CA1040812A - Methods and compositions for cleaning and bleaching plastic articles - Google Patents
Methods and compositions for cleaning and bleaching plastic articlesInfo
- Publication number
- CA1040812A CA1040812A CA210,450A CA210450A CA1040812A CA 1040812 A CA1040812 A CA 1040812A CA 210450 A CA210450 A CA 210450A CA 1040812 A CA1040812 A CA 1040812A
- Authority
- CA
- Canada
- Prior art keywords
- solution
- solutions
- lens
- article
- water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
- 238000000034 method Methods 0.000 title claims abstract description 50
- 229920003023 plastic Polymers 0.000 title claims abstract description 46
- 239000004033 plastic Substances 0.000 title claims abstract description 46
- 238000004140 cleaning Methods 0.000 title claims abstract description 45
- 239000000203 mixture Substances 0.000 title abstract description 43
- 238000004061 bleaching Methods 0.000 title abstract description 5
- 239000000243 solution Substances 0.000 claims abstract description 221
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 60
- 150000001875 compounds Chemical class 0.000 claims abstract description 32
- 230000002378 acidificating effect Effects 0.000 claims abstract description 29
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000001301 oxygen Substances 0.000 claims abstract description 28
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 28
- 239000002738 chelating agent Substances 0.000 claims abstract description 25
- 239000007864 aqueous solution Substances 0.000 claims abstract description 22
- -1 peroxy compound Chemical class 0.000 claims description 24
- 150000003839 salts Chemical class 0.000 claims description 20
- 239000002253 acid Substances 0.000 claims description 15
- 239000003599 detergent Substances 0.000 claims description 14
- 229960001922 sodium perborate Drugs 0.000 claims description 12
- YKLJGMBLPUQQOI-UHFFFAOYSA-M sodium;oxidooxy(oxo)borane Chemical compound [Na+].[O-]OB=O YKLJGMBLPUQQOI-UHFFFAOYSA-M 0.000 claims description 12
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 10
- 230000008602 contraction Effects 0.000 claims description 9
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 7
- 229910052783 alkali metal Inorganic materials 0.000 claims description 7
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 6
- 239000003929 acidic solution Substances 0.000 claims description 5
- 239000003637 basic solution Substances 0.000 claims description 4
- 229960001484 edetic acid Drugs 0.000 claims description 4
- KXDHJXZQYSOELW-UHFFFAOYSA-N Carbamic acid Chemical compound NC(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 claims description 3
- VTIIJXUACCWYHX-UHFFFAOYSA-L disodium;carboxylatooxy carbonate Chemical compound [Na+].[Na+].[O-]C(=O)OOC([O-])=O VTIIJXUACCWYHX-UHFFFAOYSA-L 0.000 claims description 3
- 239000000644 isotonic solution Substances 0.000 claims description 3
- 229940045872 sodium percarbonate Drugs 0.000 claims description 3
- URDCARMUOSMFFI-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-(2-hydroxyethyl)amino]acetic acid Chemical compound OCCN(CC(O)=O)CCN(CC(O)=O)CC(O)=O URDCARMUOSMFFI-UHFFFAOYSA-N 0.000 claims description 2
- FCKYPQBAHLOOJQ-UHFFFAOYSA-N Cyclohexane-1,2-diaminetetraacetic acid Chemical compound OC(=O)CN(CC(O)=O)C1CCCCC1N(CC(O)=O)CC(O)=O FCKYPQBAHLOOJQ-UHFFFAOYSA-N 0.000 claims description 2
- QPCDCPDFJACHGM-UHFFFAOYSA-N N,N-bis{2-[bis(carboxymethyl)amino]ethyl}glycine Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(=O)O)CCN(CC(O)=O)CC(O)=O QPCDCPDFJACHGM-UHFFFAOYSA-N 0.000 claims description 2
- 150000001340 alkali metals Chemical class 0.000 claims description 2
- NBZBKCUXIYYUSX-UHFFFAOYSA-N iminodiacetic acid Chemical compound OC(=O)CNCC(O)=O NBZBKCUXIYYUSX-UHFFFAOYSA-N 0.000 claims description 2
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 claims description 2
- 229960003330 pentetic acid Drugs 0.000 claims description 2
- 125000005342 perphosphate group Chemical group 0.000 claims description 2
- JRKICGRDRMAZLK-UHFFFAOYSA-L persulfate group Chemical group S(=O)(=O)([O-])OOS(=O)(=O)[O-] JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims description 2
- AQLJVWUFPCUVLO-UHFFFAOYSA-N urea hydrogen peroxide Chemical compound OO.NC(N)=O AQLJVWUFPCUVLO-UHFFFAOYSA-N 0.000 claims description 2
- 150000002978 peroxides Chemical class 0.000 claims 1
- 230000009471 action Effects 0.000 abstract description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 45
- 238000011282 treatment Methods 0.000 description 25
- 239000011780 sodium chloride Substances 0.000 description 24
- 229940123150 Chelating agent Drugs 0.000 description 19
- 238000009835 boiling Methods 0.000 description 19
- 125000000864 peroxy group Chemical group O(O*)* 0.000 description 16
- 229920001296 polysiloxane Polymers 0.000 description 12
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 10
- 239000008213 purified water Substances 0.000 description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 7
- 239000012530 fluid Substances 0.000 description 7
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 6
- BEFDCLMNVWHSGT-UHFFFAOYSA-N ethenylcyclopentane Chemical compound C=CC1CCCC1 BEFDCLMNVWHSGT-UHFFFAOYSA-N 0.000 description 6
- 230000007935 neutral effect Effects 0.000 description 6
- 239000004926 polymethyl methacrylate Substances 0.000 description 6
- 239000003755 preservative agent Substances 0.000 description 6
- 230000002335 preservative effect Effects 0.000 description 6
- 108090000623 proteins and genes Proteins 0.000 description 6
- 102000004169 proteins and genes Human genes 0.000 description 6
- 239000004334 sorbic acid Substances 0.000 description 6
- 235000010199 sorbic acid Nutrition 0.000 description 6
- 229940075582 sorbic acid Drugs 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 5
- 239000001103 potassium chloride Substances 0.000 description 5
- 235000011164 potassium chloride Nutrition 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 229910052708 sodium Inorganic materials 0.000 description 5
- 230000001954 sterilising effect Effects 0.000 description 5
- 238000009736 wetting Methods 0.000 description 5
- QZKRHPLGUJDVAR-UHFFFAOYSA-K EDTA trisodium salt Chemical compound [Na+].[Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O QZKRHPLGUJDVAR-UHFFFAOYSA-K 0.000 description 4
- 239000012425 OXONE® Substances 0.000 description 4
- 229910019142 PO4 Inorganic materials 0.000 description 4
- 239000002585 base Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 230000002209 hydrophobic effect Effects 0.000 description 4
- 239000004615 ingredient Substances 0.000 description 4
- HJKYXKSLRZKNSI-UHFFFAOYSA-I pentapotassium;hydrogen sulfate;oxido sulfate;sulfuric acid Chemical compound [K+].[K+].[K+].[K+].[K+].OS([O-])(=O)=O.[O-]S([O-])(=O)=O.OS(=O)(=O)O[O-].OS(=O)(=O)O[O-] HJKYXKSLRZKNSI-UHFFFAOYSA-I 0.000 description 4
- 235000021317 phosphate Nutrition 0.000 description 4
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 4
- 210000002966 serum Anatomy 0.000 description 4
- 239000004945 silicone rubber Substances 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 238000004659 sterilization and disinfection Methods 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- 239000008399 tap water Substances 0.000 description 4
- 235000020679 tap water Nutrition 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000007792 addition Methods 0.000 description 3
- 125000000217 alkyl group Polymers 0.000 description 3
- 239000007844 bleaching agent Substances 0.000 description 3
- 229920001400 block copolymer Polymers 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 239000000645 desinfectant Substances 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 150000007524 organic acids Chemical class 0.000 description 3
- 235000005985 organic acids Nutrition 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 3
- 229920002379 silicone rubber Polymers 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 description 2
- ICBJBNAUJWZPBY-UHFFFAOYSA-N 2-hydroxyethyl 3-methylbut-2-enoate Chemical compound CC(=CC(=O)OCCO)C ICBJBNAUJWZPBY-UHFFFAOYSA-N 0.000 description 2
- DBCAQXHNJOFNGC-UHFFFAOYSA-N 4-bromo-1,1,1-trifluorobutane Chemical compound FC(F)(F)CCCBr DBCAQXHNJOFNGC-UHFFFAOYSA-N 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 2
- KFSLWBXXFJQRDL-UHFFFAOYSA-N Peracetic acid Chemical compound CC(=O)OO KFSLWBXXFJQRDL-UHFFFAOYSA-N 0.000 description 2
- 229920000388 Polyphosphate Polymers 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 239000012670 alkaline solution Substances 0.000 description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 2
- 239000004327 boric acid Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000009920 chelation Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 150000001860 citric acid derivatives Chemical class 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 235000011180 diphosphates Nutrition 0.000 description 2
- 238000011067 equilibration Methods 0.000 description 2
- STVZJERGLQHEKB-UHFFFAOYSA-N ethylene glycol dimethacrylate Substances CC(=C)C(=O)OCCOC(=O)C(C)=C STVZJERGLQHEKB-UHFFFAOYSA-N 0.000 description 2
- 239000000815 hypotonic solution Substances 0.000 description 2
- 230000036512 infertility Effects 0.000 description 2
- 239000011630 iodine Substances 0.000 description 2
- 229910052740 iodine Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229940063557 methacrylate Drugs 0.000 description 2
- 150000007522 mineralic acids Chemical class 0.000 description 2
- 229920001992 poloxamer 407 Polymers 0.000 description 2
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 description 2
- 239000001205 polyphosphate Substances 0.000 description 2
- 235000011176 polyphosphates Nutrition 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 2
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 description 2
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- 230000008961 swelling Effects 0.000 description 2
- 229940033663 thimerosal Drugs 0.000 description 2
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 2
- 229960005066 trisodium edetate Drugs 0.000 description 2
- WFUGQJXVXHBTEM-UHFFFAOYSA-N 2-hydroperoxy-2-(2-hydroperoxybutan-2-ylperoxy)butane Chemical compound CCC(C)(OO)OOC(C)(CC)OO WFUGQJXVXHBTEM-UHFFFAOYSA-N 0.000 description 1
- 239000004342 Benzoyl peroxide Substances 0.000 description 1
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 description 1
- IMROMDMJAWUWLK-UHFFFAOYSA-N Ethenol Chemical compound OC=C IMROMDMJAWUWLK-UHFFFAOYSA-N 0.000 description 1
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 description 1
- 206010020852 Hypertonia Diseases 0.000 description 1
- YIVJZNGAASQVEM-UHFFFAOYSA-N Lauroyl peroxide Chemical compound CCCCCCCCCCCC(=O)OOC(=O)CCCCCCCCCCC YIVJZNGAASQVEM-UHFFFAOYSA-N 0.000 description 1
- 108010093825 Mucoproteins Proteins 0.000 description 1
- 102000001621 Mucoproteins Human genes 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000004159 Potassium persulphate Substances 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 239000004902 Softening Agent Substances 0.000 description 1
- WDJHALXBUFZDSR-UHFFFAOYSA-M acetoacetate Chemical compound CC(=O)CC([O-])=O WDJHALXBUFZDSR-UHFFFAOYSA-M 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910001508 alkali metal halide Inorganic materials 0.000 description 1
- 150000008045 alkali metal halides Chemical class 0.000 description 1
- 230000000172 allergic effect Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 230000002421 anti-septic effect Effects 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 208000010668 atopic eczema Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229960000686 benzalkonium chloride Drugs 0.000 description 1
- 235000019400 benzoyl peroxide Nutrition 0.000 description 1
- CADWTSSKOVRVJC-UHFFFAOYSA-N benzyl(dimethyl)azanium;chloride Chemical compound [Cl-].C[NH+](C)CC1=CC=CC=C1 CADWTSSKOVRVJC-UHFFFAOYSA-N 0.000 description 1
- KQNZLOUWXSAZGD-UHFFFAOYSA-N benzylperoxymethylbenzene Chemical compound C=1C=CC=CC=1COOCC1=CC=CC=C1 KQNZLOUWXSAZGD-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 210000001124 body fluid Anatomy 0.000 description 1
- 239000010839 body fluid Substances 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- HJMZMZRCABDKKV-UHFFFAOYSA-N carbonocyanidic acid Chemical compound OC(=O)C#N HJMZMZRCABDKKV-UHFFFAOYSA-N 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
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- 239000000882 contact lens solution Substances 0.000 description 1
- 230000001595 contractor effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
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- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 1
- BHDAXLOEFWJKTL-UHFFFAOYSA-L dipotassium;carboxylatooxy carbonate Chemical compound [K+].[K+].[O-]C(=O)OOC([O-])=O BHDAXLOEFWJKTL-UHFFFAOYSA-L 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical compound [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 229940009662 edetate Drugs 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
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- 230000002070 germicidal effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- LJOQGZACKSYWCH-WZBLMQSHSA-N hydroquinine Chemical compound C1=C(OC)C=C2C([C@@H](O)[C@@H]3C[C@@H]4CCN3C[C@@H]4CC)=CC=NC2=C1 LJOQGZACKSYWCH-WZBLMQSHSA-N 0.000 description 1
- 229960004251 hydroquinine Drugs 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 239000000819 hypertonic solution Substances 0.000 description 1
- 229940021223 hypertonic solution Drugs 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 229910052809 inorganic oxide Inorganic materials 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
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- 230000003993 interaction Effects 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 150000002734 metacrylic acid derivatives Chemical class 0.000 description 1
- 150000004972 metal peroxides Chemical class 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 150000007530 organic bases Chemical class 0.000 description 1
- 230000003204 osmotic effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229940021222 peritoneal dialysis isotonic solution Drugs 0.000 description 1
- 150000004965 peroxy acids Chemical class 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 229920002338 polyhydroxyethylmethacrylate Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920000193 polymethacrylate Polymers 0.000 description 1
- 229920000136 polysorbate Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000011698 potassium fluoride Substances 0.000 description 1
- 235000003270 potassium fluoride Nutrition 0.000 description 1
- 239000004323 potassium nitrate Substances 0.000 description 1
- 235000010333 potassium nitrate Nutrition 0.000 description 1
- 235000019394 potassium persulphate Nutrition 0.000 description 1
- 229910000160 potassium phosphate Inorganic materials 0.000 description 1
- 235000011009 potassium phosphates Nutrition 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
- 235000011151 potassium sulphates Nutrition 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000000069 prophylactic effect Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- PFUVRDFDKPNGAV-UHFFFAOYSA-N sodium peroxide Chemical compound [Na+].[Na+].[O-][O-] PFUVRDFDKPNGAV-UHFFFAOYSA-N 0.000 description 1
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- 229910000162 sodium phosphate Inorganic materials 0.000 description 1
- 235000011008 sodium phosphates Nutrition 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 238000005063 solubilization Methods 0.000 description 1
- 230000007928 solubilization Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000002522 swelling effect Effects 0.000 description 1
- 108010019783 tear proteins Proteins 0.000 description 1
- UEUXEKPTXMALOB-UHFFFAOYSA-J tetrasodium;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O UEUXEKPTXMALOB-UHFFFAOYSA-J 0.000 description 1
- RTKIYNMVFMVABJ-UHFFFAOYSA-L thimerosal Chemical compound [Na+].CC[Hg]SC1=CC=CC=C1C([O-])=O RTKIYNMVFMVABJ-UHFFFAOYSA-L 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000001226 triphosphate Substances 0.000 description 1
- 235000011178 triphosphate Nutrition 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- 239000012855 volatile organic compound Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G02—OPTICS
- G02C—SPECTACLES; SUNGLASSES OR GOGGLES INSOFAR AS THEY HAVE THE SAME FEATURES AS SPECTACLES; CONTACT LENSES
- G02C13/00—Assembling; Repairing; Cleaning
- G02C13/008—Devices specially adapted for cleaning contact lenses
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L12/00—Methods or apparatus for disinfecting or sterilising contact lenses; Accessories therefor
- A61L12/08—Methods or apparatus for disinfecting or sterilising contact lenses; Accessories therefor using chemical substances
- A61L12/12—Non-macromolecular oxygen-containing compounds, e.g. hydrogen peroxide or ozone
- A61L12/124—Hydrogen peroxide; Peroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/39—Organic or inorganic per-compounds
-
- G—PHYSICS
- G02—OPTICS
- G02C—SPECTACLES; SUNGLASSES OR GOGGLES INSOFAR AS THEY HAVE THE SAME FEATURES AS SPECTACLES; CONTACT LENSES
- G02C7/00—Optical parts
- G02C7/02—Lenses; Lens systems ; Methods of designing lenses
- G02C7/04—Contact lenses for the eyes
-
- C11D2111/16—
Abstract
UNITED STATES PATENT APPLICATION
OF
JOSEPH Z. KREZANOSKI
FOR
METHODS AND COMPOSITIONS FOR
CLEANING AND BLEACHING
PLASTIC ARTICLES
Plastic articles are cleaned by successively immersing them in two aqueous solutions, with each solution containing an active oxygen yield-ing per compound and preferably a chelating agent. One of the solutions is formulated to be acidic and the other is formulated to be basic. After the article is removed from the last solution, it is treated with a non-ionic cleaner and then rinsed with water. The method produces a remarkable cleaning and bleaching action on dirty, discolored plastic compositions.
This is particularly apparent when the method is applied to contact lenses.
OF
JOSEPH Z. KREZANOSKI
FOR
METHODS AND COMPOSITIONS FOR
CLEANING AND BLEACHING
PLASTIC ARTICLES
Plastic articles are cleaned by successively immersing them in two aqueous solutions, with each solution containing an active oxygen yield-ing per compound and preferably a chelating agent. One of the solutions is formulated to be acidic and the other is formulated to be basic. After the article is removed from the last solution, it is treated with a non-ionic cleaner and then rinsed with water. The method produces a remarkable cleaning and bleaching action on dirty, discolored plastic compositions.
This is particularly apparent when the method is applied to contact lenses.
Description
- ` -lQ~ lZ
This invention relates to cleaning and restoring meth-ods for synthetic plastic articles such as various contact len-ses. More particularly, this invention relates to methods for cleaning and restoring plastic articles such as soft contact lenses such as hydrophilic gel lenses made of polyhydroxylated alkyl methacrylate and hydrophobic lenses made of flexible sili-cone rubber and to methods for use with conventional hard poly-methylmethacrylate lenses.
In recent years, the advent of a great many plastic compositions has given rise to a need for cleaning and restoring articles made from them to their near-new state after they have been in use for a period of time. Many attempts have been made ;~
to restore these plastic articles to their new state with vary-ing degrees of success.
The proper care of contact lenses can be viewed as re-quiring three necessary steps. First, after removal from the eye the lenses must be cleaned to physically remove foreign matter from their surfaces. Second, the lenses must be sterilized.
Finally, the lenses must be prepared for insertion into the eye.
In the past, contact lenses have been made of hard poly-methacrylates. Proper care of these lenses has required that they be stored in specially developed cleaning and storage solu-tions to maintain them in good order when not in use. The stor-age solutions are formulated to sterilize the lenses during the lenses' storage.
Recently, a new type of contact lens known as a soft -~ lens has been developed. Soft lenses can be divided into two , .
,' .
.. . .
1~40~31Z
broad categories, namely hydrophilic soft contact lens and hydrophobic lenses.
Hydrophobic contact lenses are usually based on elas-tic and flexible silicone rubber (polysiloxane), and are gener-ally made from cross-linked dimethyl polysiloxane which is com-monly known as Antifoam A. A typical preparation of a hydropho-bic silicone contact lens is disclosed in U.S. Patent No.
3,228,741, and comprises forming a mixture of a suitable poly-` merization catalyst, up to 40% silica as a filler, and the silo-xane polymer, and then moulding and curing with heat to further polymerize the polysiloxane by cross-linking to produce the fi-nished clear lens. Clinical testing of flexible silicone rubber lenses has created a need for cleaning techniques that can be :
effectively used with these lenses.
Hydrophilic soft contact lenses are hydrated gel len-ses which can be prepared by copolymerizing hydrophilic organic monomers having an olefinic double bond with a small amount of a cross-linking agent usually having two polymerizable, olefinic double bonds. These lenses are usually based on polyhydroxylated alkyl methacrylates and contain a polyhydroxylated alkyl metha- - -crylate, such as polyhydroxyethyl methacrylate, cross-linked with, for example, a hydroxyethyl dimethylacrylate. Usually, there is about one (1) cross-linking molecule for every 200 monomer units. ~-By comparison, the conventional hard contact lens consists of polymethylmethacrylate cross-linked with hydroxyethyl dimethyl-acrylate. The absence of a hydrophilic OH group in conventional hard lenses accounts for the tremendous difference in behavior of the two materials.
:; .
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~040~31Z
Hydrated gel lenses can contain the following materi-als: (1) hydroxyethylmethacrylate (HEMA) or its analogues, (2) ethylene-glycol dimethacrylate (EGMA) or its analogues, (3) polymethylmethacrylate (PMMA) or its analogues, (4) polyvinyl-pyrrolidone (PVP), (5) traces of the respective monomers, (6) traces of inhibitors such as hydroquinine, (7) traces of cata-lysts such as benzyl peroxide, and (8) water. A more detailed description of hydrated gel lenses is found in U.S. Patent Nos.
This invention relates to cleaning and restoring meth-ods for synthetic plastic articles such as various contact len-ses. More particularly, this invention relates to methods for cleaning and restoring plastic articles such as soft contact lenses such as hydrophilic gel lenses made of polyhydroxylated alkyl methacrylate and hydrophobic lenses made of flexible sili-cone rubber and to methods for use with conventional hard poly-methylmethacrylate lenses.
In recent years, the advent of a great many plastic compositions has given rise to a need for cleaning and restoring articles made from them to their near-new state after they have been in use for a period of time. Many attempts have been made ;~
to restore these plastic articles to their new state with vary-ing degrees of success.
The proper care of contact lenses can be viewed as re-quiring three necessary steps. First, after removal from the eye the lenses must be cleaned to physically remove foreign matter from their surfaces. Second, the lenses must be sterilized.
Finally, the lenses must be prepared for insertion into the eye.
In the past, contact lenses have been made of hard poly-methacrylates. Proper care of these lenses has required that they be stored in specially developed cleaning and storage solu-tions to maintain them in good order when not in use. The stor-age solutions are formulated to sterilize the lenses during the lenses' storage.
Recently, a new type of contact lens known as a soft -~ lens has been developed. Soft lenses can be divided into two , .
,' .
.. . .
1~40~31Z
broad categories, namely hydrophilic soft contact lens and hydrophobic lenses.
Hydrophobic contact lenses are usually based on elas-tic and flexible silicone rubber (polysiloxane), and are gener-ally made from cross-linked dimethyl polysiloxane which is com-monly known as Antifoam A. A typical preparation of a hydropho-bic silicone contact lens is disclosed in U.S. Patent No.
3,228,741, and comprises forming a mixture of a suitable poly-` merization catalyst, up to 40% silica as a filler, and the silo-xane polymer, and then moulding and curing with heat to further polymerize the polysiloxane by cross-linking to produce the fi-nished clear lens. Clinical testing of flexible silicone rubber lenses has created a need for cleaning techniques that can be :
effectively used with these lenses.
Hydrophilic soft contact lenses are hydrated gel len-ses which can be prepared by copolymerizing hydrophilic organic monomers having an olefinic double bond with a small amount of a cross-linking agent usually having two polymerizable, olefinic double bonds. These lenses are usually based on polyhydroxylated alkyl methacrylates and contain a polyhydroxylated alkyl metha- - -crylate, such as polyhydroxyethyl methacrylate, cross-linked with, for example, a hydroxyethyl dimethylacrylate. Usually, there is about one (1) cross-linking molecule for every 200 monomer units. ~-By comparison, the conventional hard contact lens consists of polymethylmethacrylate cross-linked with hydroxyethyl dimethyl-acrylate. The absence of a hydrophilic OH group in conventional hard lenses accounts for the tremendous difference in behavior of the two materials.
:; .
,'' . :
, - 3 -,~ ... . . . . .
~040~31Z
Hydrated gel lenses can contain the following materi-als: (1) hydroxyethylmethacrylate (HEMA) or its analogues, (2) ethylene-glycol dimethacrylate (EGMA) or its analogues, (3) polymethylmethacrylate (PMMA) or its analogues, (4) polyvinyl-pyrrolidone (PVP), (5) traces of the respective monomers, (6) traces of inhibitors such as hydroquinine, (7) traces of cata-lysts such as benzyl peroxide, and (8) water. A more detailed description of hydrated gel lenses is found in U.S. Patent Nos.
2,976,576, 3,220,950, 3,361,858, 3,408,429, 3,496,254, and
3,499,862.
Many different cold detergent solutions have been for- -mulated and tried for cleaning plastic articles such as hard con~
tact lenses and hydrophilic gel lenses, and have met with vary-ing degrees of success. For example, the compositions disclosed in Canadian Patent No. 1,013,668, assigned to the same assignee as the present application, have a certain amount of beneficial cleaning effect. The continued and repeated use of such compo-sitions has the distinct effect of keeping dirt from accumula-ting on or in the plastic articles. These compositions, however, - -have limited restorative action on badly neglected, discolored -or severely protein encrusted plastics. Hydrophilic gel lenses `-are particularly susceptible to severe protein encrustations be-cause such lenses are often subject to a heat treatment, such as boiling in saline, to sterilize the lenses. The heat treatment - -of hydrophilic gel lenses that have not been adequately cleaned prior to the heat treatment to remove coatings of tear proteins, however, can denature the proteins and make subsequent removal of the proteins more difficult.
1~)4081Z i:
Plastic components that cannot be restored often must be discarded after a relatively short period of use despite the fact that they are not physically damaged. Many contact lenses must be discarded because of a marked decrease in light transmission or because of color development in the lenses. None of the detergents available today can reverse color changes taking place in the plastic. The dirtying and discoloration of plastic contact lenses of both the hard and flexible type is a continuing prob-lem ln the contact lens industry.
Chemical evidence indicates that debris and color found on or in contact lenses is caused primarily by the following factors: a) proteins and mucoproteins having isoelectric points at various pH's ranging from the acid end to the alkaline end of the pH scale; b) insoluble metal salts of various acidic ions; c) insoluble organic salts resulting from the interaction and precipitation of organic acids and organic bases; d) insoluble inorganic oxides, for example, Hg20 and HgO, arising through decomposition of pre-servatives like thimerosal sodium, often present in contact lens solutions as ~ -a preservative; e) organic and inorganic coloring materials found in cosmet-; ics; f) oxidation products containing chromophoric groups arising from - ingredients in tear, perspiration and other body fluids; and g) a variety of ; 20 unidentified water insoluble debris coming from the environment.
Accordingly, there has been a continuing search for a composi-tion and regimen which would clean and bleach lenses worn by patients for extended periods of time without physically destroying the lenses and without causing any physiologic damage to the cornea when the lenses are worn again after the treatment.
,~
104081;~
- SUMMARY OF THE INVENTION
It has now been found that synthetic plastic articles can be cleaned by successively contacting the article with a first aqueous solution and then a second aqueous solution, with each solution containing an active oxygen yielding per compound and one of the solutions being acidic and the other of the solutions being basic. The article is re~oved from the second solution, contacted with a non-ionic detergent, and then rinsed with water.
; Preferably, the first and second solutions each contain a chelating agent.
; When the article being treated can withstand boiling temper-atures~ such as a hydrophilic gel lens, the article preferably is boiled in both the first and second solutions. When the article being treated is a plastic that cannot be boiled, such as a conventional hard lens, it can be cleaned by eliminating the boiling steps and extending the length of time that the article is in contact with the acidic and/or basic solutions. Flexible silicone lenses can withstand boiling temperatures, but are preferably treated - -at lower temperatures, such as room temperature, for about 4 to 6 hours because boiling has a tendency to remove the hydrophilic coating that is normally applied to such lenses.
; In some instances, the ingredients of the article and basic solutions can be combined in a single solution, and the article can be cleaned -;` in this solution with one boiling cycle. In such a single solution, the acid and basic active oxygen yielding per compounds individually comprise from 0.1% to 10% of the solution. The use of a single solution, however, does-~not always produce acceptable results. The single solution can have a pN of from 2 to 11 and is usually used at an acid or basic pH. When acceptable results are . .
- -`- 1040812 not obtained, a second solution having a pH opposite that of the first can be used.
When the article being treated is a hydrophilic gel lens, it is preferably equilibrated in an isotonic environment and sterilized prior to being worn by a patient. Equilibration and sterilization can be performed as two separate steps or in a single step as described in greater detail below.
` In accordance with a preferred embodiment of the present invention, when the article is made of a hydrophilic gel plastic it is alternately expanded and contracted to aid in removing debris by controlling certain process conditions. Process condi-tions which cause expansion include the use of hypotonic solutions, alkaline solutions and heat. Process conditions which cause con-traction include the use of hypertonic conditions and acidic solutions.
The present invention restores discarded lenses routinely to their near-new state while retaining their original physical state as well as patient comfort and safety. Lenses or plastic components which are physically torn, cracked, worn or eroded, of -- -course, are not worth treating because they cannot be restored for continued use.
The invention consists in the novel compositions, methods, products and improvements shown and described. It is to be under-stood that both the foregoing general description and the following detailed description are exemplary and explanatory but are not restrictive of the invention.
Broadly, the invention relates to a method of cleaning a plastic comprising:
a) contacting the article with an acid active oxyge~
yielding compound and a basic active oxygen yielding compound, said active oxygen yielding compounds being contained in at least one aqueous solution wherein, when only one solution is employed, ' ` 1~)4(~81;~
.
the aqueous solution has a pH of from 2 to 11 and contains each of said acid and basic oxygen yielding compounds in a concentra-tion of from 0.1% to 10% by weight, and wherein when two separate aqueous solutions are employed, each solution contains an active oxygen yielding per compound in a concentration of from 0.1 to 15% by weight, with one of said solutions being acidic and the other of said solutions being basic, b) removing the article from the solution, contact-ing it with a non-ionic detergent, and rinsing it with water. .
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11)40~1Z
DETAILED DESCRIPTION OF THE INVENTION
The method of this invention includes as a first step the contacting of the article to be cleaned with a first aqueous solution conttin-ing an active oxygen yielding peroxy compound. The pH of the first solution is either alkaline or acidic, and is not neutral.
The inert nature of water, and the fact that it is a good sol-vent for-the other ingredients in the first solution, together with its ready availability, make it the desirable base material for this solution. me water used in the solution can be ordinary tap water, but preferably water purified by distillation~ filtration, ion-exchange or the like is used. It is ` especially desirable to use purified water when the article to be cleaned is a hydrophilic gel contact lens or other plastic prosthetic which makes direct contact with living tissue.
In accordance with this invention, an active oxygen yielding per compound is provided in the first solution. Active oxygen yielding compounds for use in the present invetion preferably are water soluble per-oxygen compounds and are used in the present invention in amounts ranging from 0.1 to 15% by weight~ preferably 1 to 10%, based on the total volume of the solution. The per compounds are bleaching agents that impart a high level of cleaning and bleaching power to the solution of the present inven-tion. The per compounds derive their bleaching power from the release of active oxygen. The active oxygen yielding compound can be in the form of metal peroxides, percarbonates, persulfates, perphosphates, peroxyacids, alkyl peroxides, acyl peroxides, peroxyesters and perborates such as alkali metal perborates. Exemplary of suitable active oxygen yielding compounds 104081'~
for use in this invention are hydrogen peroxide, urea peroxide, benzoyl peroxide, lauroyl peroxide, peroxyacetic acid, sodium peroxydisulfate di-tert-butyl peroxide, methyl ethyl ketone peroxide, sodium peroxide, sodium perborate, sodium and potassium percarbonate, and sodium and potassium monopersulfate. Mixtures of two or more of these compounds can be used in the first solution of this invention. The selection of a particular peroxy compound for use in the solutions of the present invention is governed by its ready availability, dissolution in water, safety, shelf-life, and the nature of the residue remaining after the release of active oxygen. Peroxy compounds that form residues that are essentially non-additive to the article being treated andlor living tissue and which can be readily removed are especially useful in the present invention.
In accordance with a preferred embodiment of the invention, the first solution contains a chelating agent. The chelating agents preferably are amino carboxylic acid compounds or water-soluble salts thereof. Examples of chelating agents which can be used in the solutions of this invention are ethylene diamine tetra-acetic acid, nitrilo triacetic acid, diethylene triamine penta-acetic acid, hydroxyethyl ethylene diamine triacetic acid, 1,2-diamino-cyclohexane tetra-acetic acid, amino diacetic acid, and hydroxyethyl amino -~
diacetic acid. These acids can be used in the form of their water-soluble salts, particularly their alkali metal salts. Especially preferred as a chelat-ing agent are the di-, tri- and tetra-sodium salts of ethylene diamine tetra-acetic acid. Other chelating agents such as citrates and polyphosphates can also be used in the present invention. The citrates which can be used in the present~invention include citric acid and its mono, di and tri alkaline metal salts. me polyphosphates which can be used include, pyrophosphates, tri-~-'' ,,.
. , . .. , ~ .
iO~081~
phosphates, tetraphosphates, trimetaphosphates, tetrametaphosphates, as well as more highly condensed phosphates in the form of the neutral or acidic alkali metal salts such as the sodium and potassium salts as well as the ammonium salt. Preferred phosphates are alkali metal triphosphates and their mixture with pyrophosphates.
The chelating agents used in the present invention act as a water softening agent and tie up divalent and trivalent cations often present in water~ thereby preventing undesirable precipitates from forming and ul-timately fogging the surface of the article being treated. This function of the chelating agent is extremely useful when treating contact lenses to bring about chelation of calcium~ iron and mercury ions and the like. The amount of chelating agent used will generally be between 0.001 to 5 weight percent, based on the volume of the solution~ and preferably is between 0.1 to 2 weight percent. As described in greater detail herefter, chelation can also be accompished by employing chelating agents in various other treating steps that can be used in the present invention.
The first solution can be conveniently prepared by forming a mixture of the chelating agent and active oxygen yielding compound, and then dissolving this mixture in an appropriate amount of water.
In accordance with the invention, the pH of the first solution is controlled to be either acidic or basic. The acidity or basicity of the - first solution can be controlled by a variety of means including using mixtures of acidic and basic peroxy compound and choosing appropriate ratios of these compounds, choosing approriate acidic or basic chelating agents, and by adting dilute solutions of inorganic and organic acids and bases. ~or .
1~)40812 example~ aqueous solutions containing 5% hydrochloric acid, 5% acetic acid of 5% sodium hydroxide can be added to the first solution to achieve an appropriate pH. The acids and bases that can be added are those that do not cause damage to the plastic article being treated and do not have a potential for adverse physiologic effect when the article is contacted with living tissue.
Tri-sodium ethylene diamine tetraacetate is especially useful in maintaining the pH of the first solution at alkaline levels when it is present in the solution at levels of 0.01 to 2%.
When the pH of the first solution is acidic, the solution should have a pH between 1 and almost but less than 7, preferably 2 to 5. When the pH of the first solution is basic, the solution should have a pH between greater than 7 and up to about 12, preferably 8.0 to 10.5. Extremely acid or extreme-ly basic solutions should be avoided because they could be detrimental to the -physical integrity of a number of plastic compositions when such solutions are -applied to articles made from these plastics at elevated temperatures, of, for example 100C or higher~ for unduly prolonged time periods of 6 or more - ~;
hours. The solutions and operating conditions of the present invention thus are formulated to routinely clean and bleach plastics but not to induce any -drastic physically destructive changes in the plastic article. -The article to be treated is contacted with the first solution by immersing it in the solution. For example, a contact lens could be immersed in from 1 to 100 ml of the first solution. The solution can be maintained at room temperature or heated up to about 100C. Preferably, when the plastic article can withstand elevated temperatures, the first solution is heated be-cause the use of elevated temperatures can loosen dirt and/or increase the rate 1~40812 of chemical reactions between the active oxygen yielding com-- pound and chromophores on the article and thereby considerably reduce the amount of time for treatment in the first solution.
Hydrophilic gel lenses can withstand elevated temperatures and generally are immersed in the first solution and boiled therein for from about two minutes to several hours such as up to 2 hours. Generally, boiling for ten to thirty minutes in the first solution produces good results. When the plastic article cannot withstand elevated or boiling temperatures, it is usually ne-cessary to leave it in the first solution for longer periods of time of from 4, preferably 6 to 48 hrs. Flexible silicone len-ses generally are treated in the first solution for about 4 to about 6 hours at temperatures below boiling, such as room temper-ature. Flexible silicone lenses can withstand boiling tempera-tures, but boiling has a tendency to remove the hydrophilic coat-ing that is normally applied to such lenses. Thus, the flexible silicone lenses can be boiled in the practice of the present in-vention, but then it may be necessary to recoat the lenses to apply a new hydrophilic coating.
In accordance with the invention, the plastic article is removed from the first solution and then contacted with a sec-ond aqueous solution containing an active oxygen yielding peroxy ; compound. The solution preferably contains a chelating agent.
The pH of the second solution is acidic when the pH of the first solution is alkaline, and is alkaline when the pH of the first solution is acidic. The second solution for treating the plastic articles is generally similar to the first solution except that the pH of the second solution is controlled to be opposite that of the first solution so that the plastic article will be sub-jected to both a basic and acidic solubilization. Thus, the same `-., . ~
, . .: . ;, . . :
, active oxygen yielding peroxy compounds and chelating agents can be incor-porated in the second solution that are used in the first solution and in the same amounts. The second solution is made acidic or basic in the same manner as the first solution, that is, by selection of suitable ratios of acidic and basic peroxy compounds, choice of acidic or basic chelating agents,and addition of dilute solutions of inorganic and organic acids and bases. The acid and basic pH ranges of the second solution correspond to those that can be used for the first solution. Thus, when the pH of the second solution is acidic, it should have a pH between l and almost but less than 7, preferably 2 to 5. When the pH of the second solution is basic, it should have a pH between tween greater than 7 and about 12, preferably 8 to 10.5.
The plastic articles generally are treated in the second solution in the same manner and for the same length of time as in the first solution.
Thus, they are immersed in the second solution, and where the article can withstand elevated temperatures, the second solution is heated and preferably boiled to bring about rapid cleaning of the article.
Dirty plastic articles, such as dirty lenses worn by different patients, often have quite different dirt compositions. Accordingly, in some usages, the bulk of dirt will be removed by either the first solution alone or the second solution alone. When the bulk of the dirt is removed by the first solution alone, boiling during the use of the second solution can be eliminated.
The method of this invention works equally as well as in producing clean articles when the first solution is acidic and the second solution basic as when the first solution is basic and the second solution is acidic.
After the article is removed from the second solution, a non-ionic detergent cleaner is applied to it to emulsify and solubilize dirt. The ' .
.
1040~12 article is then rinsed with cold water, purified water or saline until all of the nonionic detergent cleaner is rinsed away.
Preferably, the non-ionic detergent cleaner is that described in Canadian Patent No. 1,013,668. The cleaning co~position de-scribed in Canadian Patent No. 1,013,668 comprises 0.01 to 40%
of a poly(oxyethylene)-poly(oxypropylene) block copolymer, a suf-ficient amount of a germicidal composition containing sorbic acid to preserve the sterility of the solution, a sufficient amount of at least one water soluble compatible salt to provide a solution having a tonicity compatible with human tear fluid, and a balance of water. The block copolymers have a mole_ular weight between about 1700 and 15,500 and a water solubility in excess of about 10 grams per 100 ml. Additionally, these block copolymers have a cloud point in 1% aqueous solution above about 30C and a Foam Height in excess of 30 mm.
As described in Canadian Patent 1,013,668 these non-ionic detergent solutions can be formulated for use with hydro-philic gel lenses, flexible silicone lenses, and conventional hard polymethylmethacrylate lenses. A particularly useful compo-sition for hydrophilic gel lenses, hereafter referred to asCleaner A, is described in Example 4 of Canadian Patent 1,013,668 and comprises 18% polyoxyethylene-polyoxypropylene condensate (sold under the trademark Pluronic F-127 by Wyandotte Chemical Corp.), 0.1% sorbic acid N.F.XIII, 0.5% disodium EDTA as a chela- `
ting agent, 0.65% sodium chloride, 0.20% potassium chloride and ;
balance deionized water. Other commercially available composi- -P
tions containing non-ionic detergent cleaners such as Preflex '~
(Burton Parsons Co.) and Soft-Mate M (Barnes Hind Ophthalmics, Inc.) also can be used in this step of the invention to clean the ~, , .
~ - \
104()~312 ~` hydrophilic gel lenses. These latter cleaners however contain - thimerosal sodium as a preservative which may induce allergic ocular responses.
When conventional hard polymethylmethacrylate lenses are used, the cleaning composition can be any of the many commer-cially available cleaning compositions for such lenses. Prefer-ably, the cleaning composition forhard lenses is a gel form cleaning composition hereafter referred to as Cleaner B and com-prises 0.025% benzalkonium chloride U.S.P., 0.25% trisodium EDTA
as a chelating agent, 20.0% polyoxyethylene-polyoxypropylene con-densate (Pluronic F-127), and balance deionized water. Silicone lenses can be cleaned in this step of the invention with any of the cleaning compositions described in Canadian Patent No.
: 1,013,o68 as being useful for silicone lenses or with the clean-; ing compositions for conventional hard lenses just described such ;
as Cleaner B.
After the plastic article is rinsed with water, it is cleaned, bleached and has a new look approaching the original -physical state of the article. The cleaning treatment of this invention is extremely useful in restoring contact lenses to a near new state without physically polishing the lenses on a tool ~-with a polishing compound. Polishing on a tool can destroy the optics of a lens as well as the edge finish, but the rènnovating achieved by the cleaning treatment of this invention avoids these -problems. The physical dimensions and optics of lenses are not changed by the cleaning treatment of this invention.
The chelating agents of the first and second solutions can be omitted from these solutions if desired. When the chela-ting agents are omitted, however, the lenses preferably are given ''' ~
,, .
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additional treatment to insure that the lenses are cleaned.
Thus, for example, gel lenses can be maintained in the first and second solutions for longer times of from 5 to 15 minutes extra at boiling temperature. Also, the lens can be cleaned with a non-ionic cleaner containing a chelating agent and rinsed with water after it is removed from the first solution in addition to the usual application of non-ionic cleaner after removal from the second solution.
After rinsing to remove the cleaning composition applied after use of the second peroxy solution, the lens is prefer`ably treated to remove residual components that may have been imparted to the lens by the previous various treatment steps. These resi-duals can include EDTA, sulfate and borate ions, sorbic acid, polyoxyethylene glycol surfactants and the like. Preferably, the treatment to remove residuals also imparts a desired tonicity to the lens. Removal of residuals and control of tonicity to be : compatible with human serum and tear fluid is especially impor-tant when the lens is a hydrophilic gel lens. Preferably, with hydrophilic gel lenses, the tonicity is controlled to be isotonic with human serum and tear fluid, that is, they are formulated to contain the same salt concentration as that present in the serum and tear fluid of the user. The normal tonicity of human serum -~
and tear fluid is 0.9% (9.0 grams of sodium chloride per liter of ~
fluid). Tonicity control and removal of residuals can be achieved ~ -by use of isotonic solutions which contain approximately 0.9%
sodium chloride, or other salt or mixture of salts having a toni-city approximately equivalent to that of 0.9% sodium chloride.
Deviations of plus or minus 20% (0.72 - 1.08% tonicity) can be .
made, but any greater deviation would cause undesirable differ-ences in osmotic pressure between the natural fluids of the eye ` 1040~312 and the hydrophilic gel lens. The hydrophilic gel lens prefer-ably is equilibrated in an open container in 10 to 100 ml of isotonic physiologic saline solution for a minimum of 5 and preferably 10 to 20 minutes at a boiling temperature or 1 to 2 hours at room temperature.
As will be apparent to those of ordinary skill in the -art, any soluble salt or mixture of salts compatible with ocular tissue can be used to provide the desired tonicity. Preferably, sodium chloride, potassium chloride, or mixturesthereof, are used to provide the desired tonicity. It is to be understood, however, that one or more essentially neutral water soluble alkali metal salts can be substituted in whole or in part for the sodium or potassium chloride. Thus, other alkali metal halides, such as sodium bromide, potassium fluoride or potassium bromide can be used. Other salts such as sodium sulfate, potassium sulfate, sodium nitrate, sodium phosphate, potassium nitrate or potassium phosphate can also be used.
` An especially useful isotonic composition to control the tonicity of hydrophilic gel lenses and remove residuals is described in Canadian Patent Application No. 200,846 as "Solution B" and comprises 0.1% sorbic acid, 0.1% trisodium edetate, 0.75%
sodium chloride, 0.20% potassium chloride, 5% sodium hydroxide -~
solution to adjust pH to 7.4 and purified water Q.S. to make ` 100.0%. -Variations in osmolarity play a significant part in causing hydrophilic gel lenses to swell and contract. Thus, for example, hypertonicity causes a shrinking (less water) in hydrophilic gel plastics and hypotonicity causes an expansion of these plastics. Treatment of a hydrophilic - - , ,, , , ~.
1~4~381Z
gel lens to bring about a final isotonic lens help insure that the lens diameter and other physical dimensions of the treated lens will be the same or nearly the same as the new condition of the lens.
In accordance with a preferred embodiment of the invention, when the article is made from a hydrophilic gel plastic, such as a gel lens, it is alternately expanded and contracted to aid in removing debris. It has been found, in accordance with the teachings of ~he present invention that alternately changing the lens size aids in loosening and removing dirt and other debris. The lens can either be expanded and then contracted or contracted and then expanded to bring about the changes in lens size. These changes can be achieved by controlling various process steps that occur during the overall treatment of the lens.
Process conditions which cause expansion of a hydrophilic gel plastic include the use of hypotonic solutions, alkaline solutions and heat.
Process conditions which cause contraction include the use of hypertonic solutions and acidic solutions. Thus, by controlling the tonicity, alkalinity and temperature of the various solutions used during the practice of the pre-sent invention, the gel lenses can be made to alternately expand and contract from one treatment step to the next. For example, control of osmolarity preferably is performed during the treatment with the first and second peroxy containing aqueous solutions to alternately provide swelling and contraction or contraction and s~elling of the hydrophilic gel plastic. Where contraction is desired, the tonicity of either the first or second solution is controlled to contain more than the equivalent of 0.9% sodium chloride by adding to the solution inert water soluble salts~ for example, sodium chloride~ potassium --18_ 1~)4(~12 chloride, and the corresponding sulfates, phosphates, and ni-trates. The solution may be controlled to have an osmolar effect equivalent to for example 1.3% or higher to 10 to 20% sodium chloride. This extreme in osmolarity aids in shrinking a lens markedly and thus aids in loosening foreign debris tra~ped in the matrix of the plastic lens. For example, an osmolarity of 20% sodium chloride could shrink a lens having an initial lens diameter of 15 mm to a lens diameter of 9 mm. Where expansion is desired, the tonicity of either the first or second solution is controlled to contain less than the equivalent of 0.9% sodium chloride for example 0 to 0.5%, by eliminating the above men-tioned inert water soluble salts from the solution. Purified water provides an excellent hypotonic environment and causes a significant amount of swelling in a gel lens. Accordingly, when a treatment step requires that a lens be rinsed with water, puri- -fied water preferably is used when a swelling of the lens is de-sired. The tonicity of the solution generally has a greater ef-fect that the pH in determining whether it will have an expanding or contracting effect on the gel plastic.
After the desired tonicity is achieved in the cleaned, -bleached and rinsed lens, it is preferably sterilized in accord- -ance with conventional techniques. Thus, for example, hydrophil-ic gel lenses can be sterilized by boiling in saline or by chemic-al reaction. Boiling in saline to sterilize the hydrophilic gel --lens is performed in a closed system where air and other conta-minating materials cannot enter the system and is thus distin-guished from the previously described step of boiling in saline in an open system to remove residuals and control tonicity. The boiling in saline to sterilize, however, can be used to bring a-bout the desired removal of residuals and tonicity, if this step is performed with large amounts of solution at high temperature and pressure. A preferred chemical sterilization treatment is that de~cribed in Canadian Patent Application ~o. 200,84~.
lV40~31Z
sriefly, this treatment uses an aqueous antiseptic iodophor solu-tion containing from about 0.00005% to about 10% by weight iodine, from about 0.0001% to about 20% by weight of a water soluble io-dide salt, from about 0.001% to about 25% by weight polyvinyl alcohol, from about 0.001% to about 10% by weight boric acid, and the remainder solely water or other ingredients which will impart special properties. This self-sterilizing solution is desirably used in combination with an aqueous dissipating solution for dis-sipating the available iodine at a controlled rate which dissipa-ting solution comprises from about 0.01% to about 5% by weightsorbic acid or a water soluble salt thereof and from about 0.01%
to about 5% by weight ethylenediaminetetraacetic acid or a soluble salt thereof. From 1.0% to about 10% of sterilizing solution can be combined with from about 99% to about 90% by weight of dissi-pating solution to form an especially preferred solution for treating gel lenses. The lens is treated in this combined solu-tion for a minimum of about 15 minutes to 2 hours or longer. ~
Treating of silicone lenses and conventional hard lenses -to remove residuals and provide a desired tonicity ordinarily can be accomplished by applying a conventional isotonic wetting solu-tion to them after they have been rinsed free of the non-ionic cleaner that is applied after the second peroxy solution. After application of the wetting solution, the lens can be inserted in the eye. The wetting solution for these lenses need not be isoto-nic and can have tonicities equivalent to about 0.5 to 1.8% sodi- ~-um chloride. These lenses, of course can be kept in known and conventional storing and soaking solutions prior to application of the wetting solution. The known and conventional storing and soa-king solutions can sterilize these lenses.
The method of this invention achieves excellent and unex-pected results in the cleaning of dirty, discolored plastics of various compositions.
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which would otherwise have to be discarded. The cleaning method of this invention primarily is intended for use on those plastic articles which have been neglected and have been cleaned in accordance with routine or daily cleaning procedures which if follow~d would keep the articles in satisfactory condition but which cannot clean the articles once they become neglected.
The cleaning method of the present invention is a practical contact lens office procedure. Patients can bring their lenses in for rejuvination by their fitter whenever the need arises. Further, intelligent patients can be taught and allowed to treat their lenses at home every 3 to 6 months or when required, particularly if their daily prophylactic cleaning is not followed or is inade-quate.
For a clearer understandlng of the invention, specific examples of it are set forth below. These examples are merely illustrative and are not to be understood as limiting the scope and underlying principles of the invention in any way. All parts and percentages referred to in this specification and the appended claims are by weight in terms of unit volume of solution unless otherwise specifically indicated. For example, a sodium perborate content of 0.1 percent in the solution is equivalent to one gram of sodium perborate per liter of solution.
An acidic peroxy contact lens cleaning composition for hydro-philic gel lenses is prepared by forming a mixture containing, on a weight basis, 98 weight percent potassium monopersulphate and 2 weight percent -monosodium edetate and then dissolving one (1) gram of the mixture in 20 ml of water. The resulting solution is hypertonic and has a pH of about 2. A
`:
81~
dirty hydrophilic gel lens having an initial lens diameter of 15 mm in a neu-tral isotonic salt solution at room temperature is added to the solution and the solution is boiled for 15 minutes. After this treatment, the lens is re-moved and comes out considerably cleaner. The lens diameter upon removal from the acidic solution is 12.8 mm at room temeprature.
The~lens is then transferred to a hypotonic second solution having a basic pH of about 10. The second solution is made by dissoliing one (1) gram of a dry powder in 20 ml of water. The dry powder, based on its weight, consists of 98% by weight of sodium perborate and 2% by weight of tetrasodium edetate. The lens is boiled in the second solution for fifteen minutes and then taken out. The lens diameter upon removal from the second solution is 15.5 mm at room temperature.
The lens is cleaned with an isotonic nonionic cleaner (Cleaner A described above) whereupon the lens diameter returns to lS.0 mm. The lens is -hen rinsed with room temperature purified water which swells the lens diameter to 16 mm. The treated lens is now remarkably cleaner than the dirty lens. The above cycle can be repeated if desired to bring about further improvements in the lens. The lens is next placed in 15 ml of a neutral isotonic 0.9% sodium chloride solution where it is boiled for 15 minutes to accelerate equilibration and removal or residuals. Upon cooling, -the lens again returns to its original lens diameter of 15 mm. The lens is now ready for sterilization and wearing.
The above cycle is used on a number of dirtied lenses and they all exhibit good cleanliness after the treatment.
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1~40t312 _ A commercial 3% hydrogen peroxide solution containing 0.2% nitriloacetic acid and having a pH of 3 is used to clean a dirty, yellow, discarded hydrophilic gel lens. The lens is plac-ed in 30 ml of the solution, boiled in the solutionfor thirty min-utes, and removed.
The lens is then transferred to a second solution hav-ing a basic pH of 11. The second solution is made by adding two (2) grams of a mixture containing sodium percarbonate, sodium chloride and trisodiumdiethylenetriamine penta-a~etic acid to 20 ml of water. The mixture contains, based on its weight, 80 weight percent sodium percarbonate, 19 weight percent sodium chloride, and 1 weight percent of trisodiumdiethylenetriamine penta-acetic acid. The lens is boiled in the second solution for 10 minutes and then removed. The lens is then cleaned with a non-ionic clea-ner, Cleaner A, and rinsed with-water. The lens is now clean and colorless.
The lens is then equilibrated in an isotonic physiolo-- gic-saline solution, sterilized by boiling, and worn by a patient.
The patient reported that the lens looked and felt as a new lens.
A basic peroxy contact lens cleaning solution for hydro-philic gel lenses is prepared by adding 2 grams of a mixture con-taining potassium persulfate, sodium perborate and disodium ede-tate to 20 ml of water. The mixture contains, on a weight basis, 75 weight percent potassium persulphate, 20 weight percent sodium perborate and 5 weight percent disodium edetate. The resulting solution has a pH of 4.5 and is adjusted to a pH of 8.5 by addi-tion of 5 weight percent sodium hydroxide.
A dirty, discarded, hydrophilic gel lens is placed in ~ 40~3~.%
20 ml of the solution and the solution is heated at about 75"C
for thirty minutes. After this treatment, the lens is removed, The lens is then transferred to a second solution hav-ing an acidic pH of about 4Ø The second solution is prepared in an identical manner to the first solution except that the pH
is adjusted to 4.0 instead of 8.5 by addition of 5 weight per- -cent acetic acid. The lens is boiled in 20 ml of the second so-lution for 15 minutes and then removed. The lens is then cleaned with a nonionic cleaner (Cleaner A) rinsed with water, and equili- -brated in 30 ml physiologic saline for 2 hours at room tempera-ture. The lens is then placed in the transfer unit portion of a contact lens cleaning and storage device of the type shown in U.S. Patent No. 3,519,005 and U.S. Patent No. 3,645,284. Four ml of a sterile preservative dissipating solution and 4 drops of a -concentrated disinfectant solution (both described at page 26 of U.S. Serial No. 315,793) are added to the device to disinfect and sterilize the lens. The lens is kept in the combined solution overnight. The composition of the concentrated disinfectant so-lution used is:
20 Iodine 0.1 %
Potassium Iodide 0.2%
Polyvinyl alcohol (Elvanol 5105) 2.5%
Boric Acid 0.5%
Purified Water Q.S. to make100.0%
The composition of the sterile preservative dissipating solution used is:
Sorbic Acid 0.1%
Trisodium Edetate 0.1%
:
" : ' , '," '' ',' ' Sodium Chloride 1~ 40 ~ 1 2 0 75%
Potassium Chloride 0.20%
5% Sodium Hydroxide Solution to adjust pH to 7.4 Purified Water Q.S. to make 100.0%
The sterility of the preservative dissipating solution is insured by heating.
After sterilization, the lens is inserted in a patient's eye, and is remarkably comfortable and clean, almost like new.
The above cleaning cycle is repeated with eight other lenses with similar results.
This example illustrates the use of a single cleaning solution to clean a hydrophilic gel lens. Three grams of a mix-ture containing, on a weight basis, 50 weight percent potassium monopersulphate, 20 weight percent sodium chloride, 25 weight percent sodium perborate, and 5 weight percent disodium edetate are added to 50 ml of water. The pH of the resulting solution is 6.
A dirty, orange, discarded gel lens is boiled in 50 ml of the solution for 45 minutes. The lens is removed, further cleaned with a non-ionic cleaner (Cleaner A) and rinsed with water.
The thus treated lens is clean and shows no changes in its physi-cal dimensions and optics. It is equilibrated in sterile neutral isotonic solution for 1 hour and worn by à patient.
Other lenses worn by different patients, and probably containing dirts of differing compositions, did not always come out perfectly clean following this treatment. In these in-stances, additional treatment with a - 25 ~
basic peroxy composition having a pH of 7.5 to 11.0 cleaned off the remaining foreign debris.
This example illustrates the use of a single cleaning solution to clean a conventional hard contact lens. ~ne gram of a mixture containing, on a weight basis, 30 weight percent potassium monopersulphat~e, 69 weight percent sodium perborate, and 1 weight percent trisoidum edetate are added ~-to 10 ml of water. The pH of the resulting solution is 8Ø A very dirty, protein encrusted, discarded conventional hard contact lens is placed in the solution and stored in i~ for 24 hours. The lens is removed and cleaned with a commercial non-ionic cleaner (Cleaner B described above) by gentle rubb-ing and water rinsing. The lens is very clean and has a new look. A wett- ~- -ing solution is applied and the lens may be worn safely and comfortably.
A basic peroxy contact lens cleaning solution for hydrophilic ; gel lenses is prepared by adding 4 grams of sodium perborate to 80 ml of water. Twelver hydrophilic gel lenses are boiled in this solution for 15 minutes. The lenses are then transferred to a second acidic peroxy contact 20 lens cleaning solution prepared by adding 4 grams of potassium monopersul- -fate to 80 ml of water. me twelve lenses are boiled in the second solution ;
for 15 minutes and then are taken ou~. The lenses are then cleaned with a non-ionic cleaner, Cleaner A, and rinsed with cold tap water.
The lenses are equilibrated to be isotonic and residulas are removed by a variety of treatments. In one treatment, a lens is placed in --a 5 ml solution of isotonic normal saline at room temperature for 1 hour.
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~04U812 In another treatment, a lens is placed in a 5 ml of an isotonic dissipating solution comprising the disinfectant solution described in Example 3 above for 1 hour at room temperature. In still another treatment, a lens is placed in 5 ml of isotonic normal saline and kept in the solution for 5 minutes at a temperature of 100C. In still another treatment, a lens is placed in 5 ml of the dissipating solution described in Example 3 above and kept in the solution for 15 minutes at a temperature of 100C. Tests for the pre-sence of residuals show that the lenses treated in accordance with the above techniques contain a maximum of 0.0001% residuals.
The above treated lens can now be sterilized and then worn by a patient.
EXAMPLE ?
A basic peroxy contact lens cleaning solution for hydrophilic gel lenses is prepared by adding three grams of sodium perborate to 50 ml of distilled water. Twenty hydrophilic gel lenses are boiled in the solution for 15 minutes. The lenses are removed from the solution and cleaned with nonionic Cleaner A by rubbing with the index finger of one hand in the palm of the other hand. The lenses are rinsed thoroughly with distilled water.
The lenses are then placed in a second acidic peroxy contact lens cleaning solution prepared by adding 3 grams of potassium monopersul-fate ~o 50 ml of distilled water. The lenses are boiled in the second solution for 15 minutes and then are taken out. The lenses are removed from the solution and cleaned with a nonionic Cleaner A by rubbing with the index finger of one hand in the palm of the other hand. The lenses are rinsed thoroughly with distilled water. 1~4~81Z
Each lens is placed in a ml glass vial containing normal saline, U.S.P. buffered with sodium bicarbonate. The vials are closed with a silicone rubber stopper and crumped with an aluminum seal. The vials are then autoclaved for 15 minutes at 250F and 5 Ibs. pressure.
Tests for the presence of residuals show that the lenses do not contain any significant quantities of residues. The tests indicate that there are minimal levels of boron and sulfate, no sorbic acid, and no other volatile organic compounds.
EXAMPL_ 8 A basic peroxy contact lens cleaning solution is prepared by adding 1 8ram of sodium perborate to 40 ml of water. A flexible silicone lens is placed in the solution and kept in the solution for 2 hours at 60C.
The lens is removed from the solution and then cleaned with a nonionic cleaner~ Cleaner B, and rinsed with cold tap water. The lens is then trans-ferred to a second acidic peroxy contact lens cleaning solution prepared by adding one gram of potassium monopersulfate to 40 ml of water. The lens is kept in this solution~for two hours at 60C. The lens is removed from the second solution and again cleaned with Cleaner B and rinsed with cold tap water. A wetting solution is applied to the lens and it can now be worn - safely and comfortably.
The invention in its broader aspects is not limited to the -specific details shown and described and departures may be~made from such details without departing from the principles of the invention and witout sacrificing its chief advantages.
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Many different cold detergent solutions have been for- -mulated and tried for cleaning plastic articles such as hard con~
tact lenses and hydrophilic gel lenses, and have met with vary-ing degrees of success. For example, the compositions disclosed in Canadian Patent No. 1,013,668, assigned to the same assignee as the present application, have a certain amount of beneficial cleaning effect. The continued and repeated use of such compo-sitions has the distinct effect of keeping dirt from accumula-ting on or in the plastic articles. These compositions, however, - -have limited restorative action on badly neglected, discolored -or severely protein encrusted plastics. Hydrophilic gel lenses `-are particularly susceptible to severe protein encrustations be-cause such lenses are often subject to a heat treatment, such as boiling in saline, to sterilize the lenses. The heat treatment - -of hydrophilic gel lenses that have not been adequately cleaned prior to the heat treatment to remove coatings of tear proteins, however, can denature the proteins and make subsequent removal of the proteins more difficult.
1~)4081Z i:
Plastic components that cannot be restored often must be discarded after a relatively short period of use despite the fact that they are not physically damaged. Many contact lenses must be discarded because of a marked decrease in light transmission or because of color development in the lenses. None of the detergents available today can reverse color changes taking place in the plastic. The dirtying and discoloration of plastic contact lenses of both the hard and flexible type is a continuing prob-lem ln the contact lens industry.
Chemical evidence indicates that debris and color found on or in contact lenses is caused primarily by the following factors: a) proteins and mucoproteins having isoelectric points at various pH's ranging from the acid end to the alkaline end of the pH scale; b) insoluble metal salts of various acidic ions; c) insoluble organic salts resulting from the interaction and precipitation of organic acids and organic bases; d) insoluble inorganic oxides, for example, Hg20 and HgO, arising through decomposition of pre-servatives like thimerosal sodium, often present in contact lens solutions as ~ -a preservative; e) organic and inorganic coloring materials found in cosmet-; ics; f) oxidation products containing chromophoric groups arising from - ingredients in tear, perspiration and other body fluids; and g) a variety of ; 20 unidentified water insoluble debris coming from the environment.
Accordingly, there has been a continuing search for a composi-tion and regimen which would clean and bleach lenses worn by patients for extended periods of time without physically destroying the lenses and without causing any physiologic damage to the cornea when the lenses are worn again after the treatment.
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104081;~
- SUMMARY OF THE INVENTION
It has now been found that synthetic plastic articles can be cleaned by successively contacting the article with a first aqueous solution and then a second aqueous solution, with each solution containing an active oxygen yielding per compound and one of the solutions being acidic and the other of the solutions being basic. The article is re~oved from the second solution, contacted with a non-ionic detergent, and then rinsed with water.
; Preferably, the first and second solutions each contain a chelating agent.
; When the article being treated can withstand boiling temper-atures~ such as a hydrophilic gel lens, the article preferably is boiled in both the first and second solutions. When the article being treated is a plastic that cannot be boiled, such as a conventional hard lens, it can be cleaned by eliminating the boiling steps and extending the length of time that the article is in contact with the acidic and/or basic solutions. Flexible silicone lenses can withstand boiling temperatures, but are preferably treated - -at lower temperatures, such as room temperature, for about 4 to 6 hours because boiling has a tendency to remove the hydrophilic coating that is normally applied to such lenses.
; In some instances, the ingredients of the article and basic solutions can be combined in a single solution, and the article can be cleaned -;` in this solution with one boiling cycle. In such a single solution, the acid and basic active oxygen yielding per compounds individually comprise from 0.1% to 10% of the solution. The use of a single solution, however, does-~not always produce acceptable results. The single solution can have a pN of from 2 to 11 and is usually used at an acid or basic pH. When acceptable results are . .
- -`- 1040812 not obtained, a second solution having a pH opposite that of the first can be used.
When the article being treated is a hydrophilic gel lens, it is preferably equilibrated in an isotonic environment and sterilized prior to being worn by a patient. Equilibration and sterilization can be performed as two separate steps or in a single step as described in greater detail below.
` In accordance with a preferred embodiment of the present invention, when the article is made of a hydrophilic gel plastic it is alternately expanded and contracted to aid in removing debris by controlling certain process conditions. Process condi-tions which cause expansion include the use of hypotonic solutions, alkaline solutions and heat. Process conditions which cause con-traction include the use of hypertonic conditions and acidic solutions.
The present invention restores discarded lenses routinely to their near-new state while retaining their original physical state as well as patient comfort and safety. Lenses or plastic components which are physically torn, cracked, worn or eroded, of -- -course, are not worth treating because they cannot be restored for continued use.
The invention consists in the novel compositions, methods, products and improvements shown and described. It is to be under-stood that both the foregoing general description and the following detailed description are exemplary and explanatory but are not restrictive of the invention.
Broadly, the invention relates to a method of cleaning a plastic comprising:
a) contacting the article with an acid active oxyge~
yielding compound and a basic active oxygen yielding compound, said active oxygen yielding compounds being contained in at least one aqueous solution wherein, when only one solution is employed, ' ` 1~)4(~81;~
.
the aqueous solution has a pH of from 2 to 11 and contains each of said acid and basic oxygen yielding compounds in a concentra-tion of from 0.1% to 10% by weight, and wherein when two separate aqueous solutions are employed, each solution contains an active oxygen yielding per compound in a concentration of from 0.1 to 15% by weight, with one of said solutions being acidic and the other of said solutions being basic, b) removing the article from the solution, contact-ing it with a non-ionic detergent, and rinsing it with water. .
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11)40~1Z
DETAILED DESCRIPTION OF THE INVENTION
The method of this invention includes as a first step the contacting of the article to be cleaned with a first aqueous solution conttin-ing an active oxygen yielding peroxy compound. The pH of the first solution is either alkaline or acidic, and is not neutral.
The inert nature of water, and the fact that it is a good sol-vent for-the other ingredients in the first solution, together with its ready availability, make it the desirable base material for this solution. me water used in the solution can be ordinary tap water, but preferably water purified by distillation~ filtration, ion-exchange or the like is used. It is ` especially desirable to use purified water when the article to be cleaned is a hydrophilic gel contact lens or other plastic prosthetic which makes direct contact with living tissue.
In accordance with this invention, an active oxygen yielding per compound is provided in the first solution. Active oxygen yielding compounds for use in the present invetion preferably are water soluble per-oxygen compounds and are used in the present invention in amounts ranging from 0.1 to 15% by weight~ preferably 1 to 10%, based on the total volume of the solution. The per compounds are bleaching agents that impart a high level of cleaning and bleaching power to the solution of the present inven-tion. The per compounds derive their bleaching power from the release of active oxygen. The active oxygen yielding compound can be in the form of metal peroxides, percarbonates, persulfates, perphosphates, peroxyacids, alkyl peroxides, acyl peroxides, peroxyesters and perborates such as alkali metal perborates. Exemplary of suitable active oxygen yielding compounds 104081'~
for use in this invention are hydrogen peroxide, urea peroxide, benzoyl peroxide, lauroyl peroxide, peroxyacetic acid, sodium peroxydisulfate di-tert-butyl peroxide, methyl ethyl ketone peroxide, sodium peroxide, sodium perborate, sodium and potassium percarbonate, and sodium and potassium monopersulfate. Mixtures of two or more of these compounds can be used in the first solution of this invention. The selection of a particular peroxy compound for use in the solutions of the present invention is governed by its ready availability, dissolution in water, safety, shelf-life, and the nature of the residue remaining after the release of active oxygen. Peroxy compounds that form residues that are essentially non-additive to the article being treated andlor living tissue and which can be readily removed are especially useful in the present invention.
In accordance with a preferred embodiment of the invention, the first solution contains a chelating agent. The chelating agents preferably are amino carboxylic acid compounds or water-soluble salts thereof. Examples of chelating agents which can be used in the solutions of this invention are ethylene diamine tetra-acetic acid, nitrilo triacetic acid, diethylene triamine penta-acetic acid, hydroxyethyl ethylene diamine triacetic acid, 1,2-diamino-cyclohexane tetra-acetic acid, amino diacetic acid, and hydroxyethyl amino -~
diacetic acid. These acids can be used in the form of their water-soluble salts, particularly their alkali metal salts. Especially preferred as a chelat-ing agent are the di-, tri- and tetra-sodium salts of ethylene diamine tetra-acetic acid. Other chelating agents such as citrates and polyphosphates can also be used in the present invention. The citrates which can be used in the present~invention include citric acid and its mono, di and tri alkaline metal salts. me polyphosphates which can be used include, pyrophosphates, tri-~-'' ,,.
. , . .. , ~ .
iO~081~
phosphates, tetraphosphates, trimetaphosphates, tetrametaphosphates, as well as more highly condensed phosphates in the form of the neutral or acidic alkali metal salts such as the sodium and potassium salts as well as the ammonium salt. Preferred phosphates are alkali metal triphosphates and their mixture with pyrophosphates.
The chelating agents used in the present invention act as a water softening agent and tie up divalent and trivalent cations often present in water~ thereby preventing undesirable precipitates from forming and ul-timately fogging the surface of the article being treated. This function of the chelating agent is extremely useful when treating contact lenses to bring about chelation of calcium~ iron and mercury ions and the like. The amount of chelating agent used will generally be between 0.001 to 5 weight percent, based on the volume of the solution~ and preferably is between 0.1 to 2 weight percent. As described in greater detail herefter, chelation can also be accompished by employing chelating agents in various other treating steps that can be used in the present invention.
The first solution can be conveniently prepared by forming a mixture of the chelating agent and active oxygen yielding compound, and then dissolving this mixture in an appropriate amount of water.
In accordance with the invention, the pH of the first solution is controlled to be either acidic or basic. The acidity or basicity of the - first solution can be controlled by a variety of means including using mixtures of acidic and basic peroxy compound and choosing appropriate ratios of these compounds, choosing approriate acidic or basic chelating agents, and by adting dilute solutions of inorganic and organic acids and bases. ~or .
1~)40812 example~ aqueous solutions containing 5% hydrochloric acid, 5% acetic acid of 5% sodium hydroxide can be added to the first solution to achieve an appropriate pH. The acids and bases that can be added are those that do not cause damage to the plastic article being treated and do not have a potential for adverse physiologic effect when the article is contacted with living tissue.
Tri-sodium ethylene diamine tetraacetate is especially useful in maintaining the pH of the first solution at alkaline levels when it is present in the solution at levels of 0.01 to 2%.
When the pH of the first solution is acidic, the solution should have a pH between 1 and almost but less than 7, preferably 2 to 5. When the pH of the first solution is basic, the solution should have a pH between greater than 7 and up to about 12, preferably 8.0 to 10.5. Extremely acid or extreme-ly basic solutions should be avoided because they could be detrimental to the -physical integrity of a number of plastic compositions when such solutions are -applied to articles made from these plastics at elevated temperatures, of, for example 100C or higher~ for unduly prolonged time periods of 6 or more - ~;
hours. The solutions and operating conditions of the present invention thus are formulated to routinely clean and bleach plastics but not to induce any -drastic physically destructive changes in the plastic article. -The article to be treated is contacted with the first solution by immersing it in the solution. For example, a contact lens could be immersed in from 1 to 100 ml of the first solution. The solution can be maintained at room temperature or heated up to about 100C. Preferably, when the plastic article can withstand elevated temperatures, the first solution is heated be-cause the use of elevated temperatures can loosen dirt and/or increase the rate 1~40812 of chemical reactions between the active oxygen yielding com-- pound and chromophores on the article and thereby considerably reduce the amount of time for treatment in the first solution.
Hydrophilic gel lenses can withstand elevated temperatures and generally are immersed in the first solution and boiled therein for from about two minutes to several hours such as up to 2 hours. Generally, boiling for ten to thirty minutes in the first solution produces good results. When the plastic article cannot withstand elevated or boiling temperatures, it is usually ne-cessary to leave it in the first solution for longer periods of time of from 4, preferably 6 to 48 hrs. Flexible silicone len-ses generally are treated in the first solution for about 4 to about 6 hours at temperatures below boiling, such as room temper-ature. Flexible silicone lenses can withstand boiling tempera-tures, but boiling has a tendency to remove the hydrophilic coat-ing that is normally applied to such lenses. Thus, the flexible silicone lenses can be boiled in the practice of the present in-vention, but then it may be necessary to recoat the lenses to apply a new hydrophilic coating.
In accordance with the invention, the plastic article is removed from the first solution and then contacted with a sec-ond aqueous solution containing an active oxygen yielding peroxy ; compound. The solution preferably contains a chelating agent.
The pH of the second solution is acidic when the pH of the first solution is alkaline, and is alkaline when the pH of the first solution is acidic. The second solution for treating the plastic articles is generally similar to the first solution except that the pH of the second solution is controlled to be opposite that of the first solution so that the plastic article will be sub-jected to both a basic and acidic solubilization. Thus, the same `-., . ~
, . .: . ;, . . :
, active oxygen yielding peroxy compounds and chelating agents can be incor-porated in the second solution that are used in the first solution and in the same amounts. The second solution is made acidic or basic in the same manner as the first solution, that is, by selection of suitable ratios of acidic and basic peroxy compounds, choice of acidic or basic chelating agents,and addition of dilute solutions of inorganic and organic acids and bases. The acid and basic pH ranges of the second solution correspond to those that can be used for the first solution. Thus, when the pH of the second solution is acidic, it should have a pH between l and almost but less than 7, preferably 2 to 5. When the pH of the second solution is basic, it should have a pH between tween greater than 7 and about 12, preferably 8 to 10.5.
The plastic articles generally are treated in the second solution in the same manner and for the same length of time as in the first solution.
Thus, they are immersed in the second solution, and where the article can withstand elevated temperatures, the second solution is heated and preferably boiled to bring about rapid cleaning of the article.
Dirty plastic articles, such as dirty lenses worn by different patients, often have quite different dirt compositions. Accordingly, in some usages, the bulk of dirt will be removed by either the first solution alone or the second solution alone. When the bulk of the dirt is removed by the first solution alone, boiling during the use of the second solution can be eliminated.
The method of this invention works equally as well as in producing clean articles when the first solution is acidic and the second solution basic as when the first solution is basic and the second solution is acidic.
After the article is removed from the second solution, a non-ionic detergent cleaner is applied to it to emulsify and solubilize dirt. The ' .
.
1040~12 article is then rinsed with cold water, purified water or saline until all of the nonionic detergent cleaner is rinsed away.
Preferably, the non-ionic detergent cleaner is that described in Canadian Patent No. 1,013,668. The cleaning co~position de-scribed in Canadian Patent No. 1,013,668 comprises 0.01 to 40%
of a poly(oxyethylene)-poly(oxypropylene) block copolymer, a suf-ficient amount of a germicidal composition containing sorbic acid to preserve the sterility of the solution, a sufficient amount of at least one water soluble compatible salt to provide a solution having a tonicity compatible with human tear fluid, and a balance of water. The block copolymers have a mole_ular weight between about 1700 and 15,500 and a water solubility in excess of about 10 grams per 100 ml. Additionally, these block copolymers have a cloud point in 1% aqueous solution above about 30C and a Foam Height in excess of 30 mm.
As described in Canadian Patent 1,013,668 these non-ionic detergent solutions can be formulated for use with hydro-philic gel lenses, flexible silicone lenses, and conventional hard polymethylmethacrylate lenses. A particularly useful compo-sition for hydrophilic gel lenses, hereafter referred to asCleaner A, is described in Example 4 of Canadian Patent 1,013,668 and comprises 18% polyoxyethylene-polyoxypropylene condensate (sold under the trademark Pluronic F-127 by Wyandotte Chemical Corp.), 0.1% sorbic acid N.F.XIII, 0.5% disodium EDTA as a chela- `
ting agent, 0.65% sodium chloride, 0.20% potassium chloride and ;
balance deionized water. Other commercially available composi- -P
tions containing non-ionic detergent cleaners such as Preflex '~
(Burton Parsons Co.) and Soft-Mate M (Barnes Hind Ophthalmics, Inc.) also can be used in this step of the invention to clean the ~, , .
~ - \
104()~312 ~` hydrophilic gel lenses. These latter cleaners however contain - thimerosal sodium as a preservative which may induce allergic ocular responses.
When conventional hard polymethylmethacrylate lenses are used, the cleaning composition can be any of the many commer-cially available cleaning compositions for such lenses. Prefer-ably, the cleaning composition forhard lenses is a gel form cleaning composition hereafter referred to as Cleaner B and com-prises 0.025% benzalkonium chloride U.S.P., 0.25% trisodium EDTA
as a chelating agent, 20.0% polyoxyethylene-polyoxypropylene con-densate (Pluronic F-127), and balance deionized water. Silicone lenses can be cleaned in this step of the invention with any of the cleaning compositions described in Canadian Patent No.
: 1,013,o68 as being useful for silicone lenses or with the clean-; ing compositions for conventional hard lenses just described such ;
as Cleaner B.
After the plastic article is rinsed with water, it is cleaned, bleached and has a new look approaching the original -physical state of the article. The cleaning treatment of this invention is extremely useful in restoring contact lenses to a near new state without physically polishing the lenses on a tool ~-with a polishing compound. Polishing on a tool can destroy the optics of a lens as well as the edge finish, but the rènnovating achieved by the cleaning treatment of this invention avoids these -problems. The physical dimensions and optics of lenses are not changed by the cleaning treatment of this invention.
The chelating agents of the first and second solutions can be omitted from these solutions if desired. When the chela-ting agents are omitted, however, the lenses preferably are given ''' ~
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.-- ~
additional treatment to insure that the lenses are cleaned.
Thus, for example, gel lenses can be maintained in the first and second solutions for longer times of from 5 to 15 minutes extra at boiling temperature. Also, the lens can be cleaned with a non-ionic cleaner containing a chelating agent and rinsed with water after it is removed from the first solution in addition to the usual application of non-ionic cleaner after removal from the second solution.
After rinsing to remove the cleaning composition applied after use of the second peroxy solution, the lens is prefer`ably treated to remove residual components that may have been imparted to the lens by the previous various treatment steps. These resi-duals can include EDTA, sulfate and borate ions, sorbic acid, polyoxyethylene glycol surfactants and the like. Preferably, the treatment to remove residuals also imparts a desired tonicity to the lens. Removal of residuals and control of tonicity to be : compatible with human serum and tear fluid is especially impor-tant when the lens is a hydrophilic gel lens. Preferably, with hydrophilic gel lenses, the tonicity is controlled to be isotonic with human serum and tear fluid, that is, they are formulated to contain the same salt concentration as that present in the serum and tear fluid of the user. The normal tonicity of human serum -~
and tear fluid is 0.9% (9.0 grams of sodium chloride per liter of ~
fluid). Tonicity control and removal of residuals can be achieved ~ -by use of isotonic solutions which contain approximately 0.9%
sodium chloride, or other salt or mixture of salts having a toni-city approximately equivalent to that of 0.9% sodium chloride.
Deviations of plus or minus 20% (0.72 - 1.08% tonicity) can be .
made, but any greater deviation would cause undesirable differ-ences in osmotic pressure between the natural fluids of the eye ` 1040~312 and the hydrophilic gel lens. The hydrophilic gel lens prefer-ably is equilibrated in an open container in 10 to 100 ml of isotonic physiologic saline solution for a minimum of 5 and preferably 10 to 20 minutes at a boiling temperature or 1 to 2 hours at room temperature.
As will be apparent to those of ordinary skill in the -art, any soluble salt or mixture of salts compatible with ocular tissue can be used to provide the desired tonicity. Preferably, sodium chloride, potassium chloride, or mixturesthereof, are used to provide the desired tonicity. It is to be understood, however, that one or more essentially neutral water soluble alkali metal salts can be substituted in whole or in part for the sodium or potassium chloride. Thus, other alkali metal halides, such as sodium bromide, potassium fluoride or potassium bromide can be used. Other salts such as sodium sulfate, potassium sulfate, sodium nitrate, sodium phosphate, potassium nitrate or potassium phosphate can also be used.
` An especially useful isotonic composition to control the tonicity of hydrophilic gel lenses and remove residuals is described in Canadian Patent Application No. 200,846 as "Solution B" and comprises 0.1% sorbic acid, 0.1% trisodium edetate, 0.75%
sodium chloride, 0.20% potassium chloride, 5% sodium hydroxide -~
solution to adjust pH to 7.4 and purified water Q.S. to make ` 100.0%. -Variations in osmolarity play a significant part in causing hydrophilic gel lenses to swell and contract. Thus, for example, hypertonicity causes a shrinking (less water) in hydrophilic gel plastics and hypotonicity causes an expansion of these plastics. Treatment of a hydrophilic - - , ,, , , ~.
1~4~381Z
gel lens to bring about a final isotonic lens help insure that the lens diameter and other physical dimensions of the treated lens will be the same or nearly the same as the new condition of the lens.
In accordance with a preferred embodiment of the invention, when the article is made from a hydrophilic gel plastic, such as a gel lens, it is alternately expanded and contracted to aid in removing debris. It has been found, in accordance with the teachings of ~he present invention that alternately changing the lens size aids in loosening and removing dirt and other debris. The lens can either be expanded and then contracted or contracted and then expanded to bring about the changes in lens size. These changes can be achieved by controlling various process steps that occur during the overall treatment of the lens.
Process conditions which cause expansion of a hydrophilic gel plastic include the use of hypotonic solutions, alkaline solutions and heat.
Process conditions which cause contraction include the use of hypertonic solutions and acidic solutions. Thus, by controlling the tonicity, alkalinity and temperature of the various solutions used during the practice of the pre-sent invention, the gel lenses can be made to alternately expand and contract from one treatment step to the next. For example, control of osmolarity preferably is performed during the treatment with the first and second peroxy containing aqueous solutions to alternately provide swelling and contraction or contraction and s~elling of the hydrophilic gel plastic. Where contraction is desired, the tonicity of either the first or second solution is controlled to contain more than the equivalent of 0.9% sodium chloride by adding to the solution inert water soluble salts~ for example, sodium chloride~ potassium --18_ 1~)4(~12 chloride, and the corresponding sulfates, phosphates, and ni-trates. The solution may be controlled to have an osmolar effect equivalent to for example 1.3% or higher to 10 to 20% sodium chloride. This extreme in osmolarity aids in shrinking a lens markedly and thus aids in loosening foreign debris tra~ped in the matrix of the plastic lens. For example, an osmolarity of 20% sodium chloride could shrink a lens having an initial lens diameter of 15 mm to a lens diameter of 9 mm. Where expansion is desired, the tonicity of either the first or second solution is controlled to contain less than the equivalent of 0.9% sodium chloride for example 0 to 0.5%, by eliminating the above men-tioned inert water soluble salts from the solution. Purified water provides an excellent hypotonic environment and causes a significant amount of swelling in a gel lens. Accordingly, when a treatment step requires that a lens be rinsed with water, puri- -fied water preferably is used when a swelling of the lens is de-sired. The tonicity of the solution generally has a greater ef-fect that the pH in determining whether it will have an expanding or contracting effect on the gel plastic.
After the desired tonicity is achieved in the cleaned, -bleached and rinsed lens, it is preferably sterilized in accord- -ance with conventional techniques. Thus, for example, hydrophil-ic gel lenses can be sterilized by boiling in saline or by chemic-al reaction. Boiling in saline to sterilize the hydrophilic gel --lens is performed in a closed system where air and other conta-minating materials cannot enter the system and is thus distin-guished from the previously described step of boiling in saline in an open system to remove residuals and control tonicity. The boiling in saline to sterilize, however, can be used to bring a-bout the desired removal of residuals and tonicity, if this step is performed with large amounts of solution at high temperature and pressure. A preferred chemical sterilization treatment is that de~cribed in Canadian Patent Application ~o. 200,84~.
lV40~31Z
sriefly, this treatment uses an aqueous antiseptic iodophor solu-tion containing from about 0.00005% to about 10% by weight iodine, from about 0.0001% to about 20% by weight of a water soluble io-dide salt, from about 0.001% to about 25% by weight polyvinyl alcohol, from about 0.001% to about 10% by weight boric acid, and the remainder solely water or other ingredients which will impart special properties. This self-sterilizing solution is desirably used in combination with an aqueous dissipating solution for dis-sipating the available iodine at a controlled rate which dissipa-ting solution comprises from about 0.01% to about 5% by weightsorbic acid or a water soluble salt thereof and from about 0.01%
to about 5% by weight ethylenediaminetetraacetic acid or a soluble salt thereof. From 1.0% to about 10% of sterilizing solution can be combined with from about 99% to about 90% by weight of dissi-pating solution to form an especially preferred solution for treating gel lenses. The lens is treated in this combined solu-tion for a minimum of about 15 minutes to 2 hours or longer. ~
Treating of silicone lenses and conventional hard lenses -to remove residuals and provide a desired tonicity ordinarily can be accomplished by applying a conventional isotonic wetting solu-tion to them after they have been rinsed free of the non-ionic cleaner that is applied after the second peroxy solution. After application of the wetting solution, the lens can be inserted in the eye. The wetting solution for these lenses need not be isoto-nic and can have tonicities equivalent to about 0.5 to 1.8% sodi- ~-um chloride. These lenses, of course can be kept in known and conventional storing and soaking solutions prior to application of the wetting solution. The known and conventional storing and soa-king solutions can sterilize these lenses.
The method of this invention achieves excellent and unex-pected results in the cleaning of dirty, discolored plastics of various compositions.
, ' '',: ' ,; , ' , . , 1~4S~81Z
which would otherwise have to be discarded. The cleaning method of this invention primarily is intended for use on those plastic articles which have been neglected and have been cleaned in accordance with routine or daily cleaning procedures which if follow~d would keep the articles in satisfactory condition but which cannot clean the articles once they become neglected.
The cleaning method of the present invention is a practical contact lens office procedure. Patients can bring their lenses in for rejuvination by their fitter whenever the need arises. Further, intelligent patients can be taught and allowed to treat their lenses at home every 3 to 6 months or when required, particularly if their daily prophylactic cleaning is not followed or is inade-quate.
For a clearer understandlng of the invention, specific examples of it are set forth below. These examples are merely illustrative and are not to be understood as limiting the scope and underlying principles of the invention in any way. All parts and percentages referred to in this specification and the appended claims are by weight in terms of unit volume of solution unless otherwise specifically indicated. For example, a sodium perborate content of 0.1 percent in the solution is equivalent to one gram of sodium perborate per liter of solution.
An acidic peroxy contact lens cleaning composition for hydro-philic gel lenses is prepared by forming a mixture containing, on a weight basis, 98 weight percent potassium monopersulphate and 2 weight percent -monosodium edetate and then dissolving one (1) gram of the mixture in 20 ml of water. The resulting solution is hypertonic and has a pH of about 2. A
`:
81~
dirty hydrophilic gel lens having an initial lens diameter of 15 mm in a neu-tral isotonic salt solution at room temperature is added to the solution and the solution is boiled for 15 minutes. After this treatment, the lens is re-moved and comes out considerably cleaner. The lens diameter upon removal from the acidic solution is 12.8 mm at room temeprature.
The~lens is then transferred to a hypotonic second solution having a basic pH of about 10. The second solution is made by dissoliing one (1) gram of a dry powder in 20 ml of water. The dry powder, based on its weight, consists of 98% by weight of sodium perborate and 2% by weight of tetrasodium edetate. The lens is boiled in the second solution for fifteen minutes and then taken out. The lens diameter upon removal from the second solution is 15.5 mm at room temperature.
The lens is cleaned with an isotonic nonionic cleaner (Cleaner A described above) whereupon the lens diameter returns to lS.0 mm. The lens is -hen rinsed with room temperature purified water which swells the lens diameter to 16 mm. The treated lens is now remarkably cleaner than the dirty lens. The above cycle can be repeated if desired to bring about further improvements in the lens. The lens is next placed in 15 ml of a neutral isotonic 0.9% sodium chloride solution where it is boiled for 15 minutes to accelerate equilibration and removal or residuals. Upon cooling, -the lens again returns to its original lens diameter of 15 mm. The lens is now ready for sterilization and wearing.
The above cycle is used on a number of dirtied lenses and they all exhibit good cleanliness after the treatment.
,~
_22-:
' ~ ' : , :" . ,,' , , .
1~40t312 _ A commercial 3% hydrogen peroxide solution containing 0.2% nitriloacetic acid and having a pH of 3 is used to clean a dirty, yellow, discarded hydrophilic gel lens. The lens is plac-ed in 30 ml of the solution, boiled in the solutionfor thirty min-utes, and removed.
The lens is then transferred to a second solution hav-ing a basic pH of 11. The second solution is made by adding two (2) grams of a mixture containing sodium percarbonate, sodium chloride and trisodiumdiethylenetriamine penta-a~etic acid to 20 ml of water. The mixture contains, based on its weight, 80 weight percent sodium percarbonate, 19 weight percent sodium chloride, and 1 weight percent of trisodiumdiethylenetriamine penta-acetic acid. The lens is boiled in the second solution for 10 minutes and then removed. The lens is then cleaned with a non-ionic clea-ner, Cleaner A, and rinsed with-water. The lens is now clean and colorless.
The lens is then equilibrated in an isotonic physiolo-- gic-saline solution, sterilized by boiling, and worn by a patient.
The patient reported that the lens looked and felt as a new lens.
A basic peroxy contact lens cleaning solution for hydro-philic gel lenses is prepared by adding 2 grams of a mixture con-taining potassium persulfate, sodium perborate and disodium ede-tate to 20 ml of water. The mixture contains, on a weight basis, 75 weight percent potassium persulphate, 20 weight percent sodium perborate and 5 weight percent disodium edetate. The resulting solution has a pH of 4.5 and is adjusted to a pH of 8.5 by addi-tion of 5 weight percent sodium hydroxide.
A dirty, discarded, hydrophilic gel lens is placed in ~ 40~3~.%
20 ml of the solution and the solution is heated at about 75"C
for thirty minutes. After this treatment, the lens is removed, The lens is then transferred to a second solution hav-ing an acidic pH of about 4Ø The second solution is prepared in an identical manner to the first solution except that the pH
is adjusted to 4.0 instead of 8.5 by addition of 5 weight per- -cent acetic acid. The lens is boiled in 20 ml of the second so-lution for 15 minutes and then removed. The lens is then cleaned with a nonionic cleaner (Cleaner A) rinsed with water, and equili- -brated in 30 ml physiologic saline for 2 hours at room tempera-ture. The lens is then placed in the transfer unit portion of a contact lens cleaning and storage device of the type shown in U.S. Patent No. 3,519,005 and U.S. Patent No. 3,645,284. Four ml of a sterile preservative dissipating solution and 4 drops of a -concentrated disinfectant solution (both described at page 26 of U.S. Serial No. 315,793) are added to the device to disinfect and sterilize the lens. The lens is kept in the combined solution overnight. The composition of the concentrated disinfectant so-lution used is:
20 Iodine 0.1 %
Potassium Iodide 0.2%
Polyvinyl alcohol (Elvanol 5105) 2.5%
Boric Acid 0.5%
Purified Water Q.S. to make100.0%
The composition of the sterile preservative dissipating solution used is:
Sorbic Acid 0.1%
Trisodium Edetate 0.1%
:
" : ' , '," '' ',' ' Sodium Chloride 1~ 40 ~ 1 2 0 75%
Potassium Chloride 0.20%
5% Sodium Hydroxide Solution to adjust pH to 7.4 Purified Water Q.S. to make 100.0%
The sterility of the preservative dissipating solution is insured by heating.
After sterilization, the lens is inserted in a patient's eye, and is remarkably comfortable and clean, almost like new.
The above cleaning cycle is repeated with eight other lenses with similar results.
This example illustrates the use of a single cleaning solution to clean a hydrophilic gel lens. Three grams of a mix-ture containing, on a weight basis, 50 weight percent potassium monopersulphate, 20 weight percent sodium chloride, 25 weight percent sodium perborate, and 5 weight percent disodium edetate are added to 50 ml of water. The pH of the resulting solution is 6.
A dirty, orange, discarded gel lens is boiled in 50 ml of the solution for 45 minutes. The lens is removed, further cleaned with a non-ionic cleaner (Cleaner A) and rinsed with water.
The thus treated lens is clean and shows no changes in its physi-cal dimensions and optics. It is equilibrated in sterile neutral isotonic solution for 1 hour and worn by à patient.
Other lenses worn by different patients, and probably containing dirts of differing compositions, did not always come out perfectly clean following this treatment. In these in-stances, additional treatment with a - 25 ~
basic peroxy composition having a pH of 7.5 to 11.0 cleaned off the remaining foreign debris.
This example illustrates the use of a single cleaning solution to clean a conventional hard contact lens. ~ne gram of a mixture containing, on a weight basis, 30 weight percent potassium monopersulphat~e, 69 weight percent sodium perborate, and 1 weight percent trisoidum edetate are added ~-to 10 ml of water. The pH of the resulting solution is 8Ø A very dirty, protein encrusted, discarded conventional hard contact lens is placed in the solution and stored in i~ for 24 hours. The lens is removed and cleaned with a commercial non-ionic cleaner (Cleaner B described above) by gentle rubb-ing and water rinsing. The lens is very clean and has a new look. A wett- ~- -ing solution is applied and the lens may be worn safely and comfortably.
A basic peroxy contact lens cleaning solution for hydrophilic ; gel lenses is prepared by adding 4 grams of sodium perborate to 80 ml of water. Twelver hydrophilic gel lenses are boiled in this solution for 15 minutes. The lenses are then transferred to a second acidic peroxy contact 20 lens cleaning solution prepared by adding 4 grams of potassium monopersul- -fate to 80 ml of water. me twelve lenses are boiled in the second solution ;
for 15 minutes and then are taken ou~. The lenses are then cleaned with a non-ionic cleaner, Cleaner A, and rinsed with cold tap water.
The lenses are equilibrated to be isotonic and residulas are removed by a variety of treatments. In one treatment, a lens is placed in --a 5 ml solution of isotonic normal saline at room temperature for 1 hour.
, ~ ' , . ,, , . . , :
, ., .
~04U812 In another treatment, a lens is placed in a 5 ml of an isotonic dissipating solution comprising the disinfectant solution described in Example 3 above for 1 hour at room temperature. In still another treatment, a lens is placed in 5 ml of isotonic normal saline and kept in the solution for 5 minutes at a temperature of 100C. In still another treatment, a lens is placed in 5 ml of the dissipating solution described in Example 3 above and kept in the solution for 15 minutes at a temperature of 100C. Tests for the pre-sence of residuals show that the lenses treated in accordance with the above techniques contain a maximum of 0.0001% residuals.
The above treated lens can now be sterilized and then worn by a patient.
EXAMPLE ?
A basic peroxy contact lens cleaning solution for hydrophilic gel lenses is prepared by adding three grams of sodium perborate to 50 ml of distilled water. Twenty hydrophilic gel lenses are boiled in the solution for 15 minutes. The lenses are removed from the solution and cleaned with nonionic Cleaner A by rubbing with the index finger of one hand in the palm of the other hand. The lenses are rinsed thoroughly with distilled water.
The lenses are then placed in a second acidic peroxy contact lens cleaning solution prepared by adding 3 grams of potassium monopersul-fate ~o 50 ml of distilled water. The lenses are boiled in the second solution for 15 minutes and then are taken out. The lenses are removed from the solution and cleaned with a nonionic Cleaner A by rubbing with the index finger of one hand in the palm of the other hand. The lenses are rinsed thoroughly with distilled water. 1~4~81Z
Each lens is placed in a ml glass vial containing normal saline, U.S.P. buffered with sodium bicarbonate. The vials are closed with a silicone rubber stopper and crumped with an aluminum seal. The vials are then autoclaved for 15 minutes at 250F and 5 Ibs. pressure.
Tests for the presence of residuals show that the lenses do not contain any significant quantities of residues. The tests indicate that there are minimal levels of boron and sulfate, no sorbic acid, and no other volatile organic compounds.
EXAMPL_ 8 A basic peroxy contact lens cleaning solution is prepared by adding 1 8ram of sodium perborate to 40 ml of water. A flexible silicone lens is placed in the solution and kept in the solution for 2 hours at 60C.
The lens is removed from the solution and then cleaned with a nonionic cleaner~ Cleaner B, and rinsed with cold tap water. The lens is then trans-ferred to a second acidic peroxy contact lens cleaning solution prepared by adding one gram of potassium monopersulfate to 40 ml of water. The lens is kept in this solution~for two hours at 60C. The lens is removed from the second solution and again cleaned with Cleaner B and rinsed with cold tap water. A wetting solution is applied to the lens and it can now be worn - safely and comfortably.
The invention in its broader aspects is not limited to the -specific details shown and described and departures may be~made from such details without departing from the principles of the invention and witout sacrificing its chief advantages.
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Claims (27)
1. A method of cleaning a plastic article comprising:
a) successively contacting the article with a first aqueous solution and then a second aqueous solution, with each solution containing an active oxygen yielding per compound in a concentration of from 0.1 to 15 weight percent, and one of said solutions being acidic and the other of said solutions being basic; and b) removing the article from the second solution, contacting it with a non-ionic detergent, and rinsing it with water.
a) successively contacting the article with a first aqueous solution and then a second aqueous solution, with each solution containing an active oxygen yielding per compound in a concentration of from 0.1 to 15 weight percent, and one of said solutions being acidic and the other of said solutions being basic; and b) removing the article from the second solution, contacting it with a non-ionic detergent, and rinsing it with water.
2. The method of claim 1 wherein the per compound of the first and second solutions is independently selected from the group consisting of hydrogen peroxide, alkali metal perborates percarbonates, perphosphates, persulfates, and peroxides.
3. The method of claim 1 wherein the peroxy compound of the first and second solutions is independently selected from the group consisting of potassium monopersulphate, sodium perborate, urea peroxide, sodium percarbonate and hydrogen peroxide.
4. The method of claim 1 wherein the first and second solutions independently contain 0.001 to 5 weight percent of a chelating agent.
5. The method of claim 4 wherein the chelating agent of the first and second solutions is an amino carboxylic acid or a water-soluble salt thereof.
6. The method of claim 4 wherein the chelating agent is selected from the group consisting of ethylene diamine tetra-acetic acid, nitrilo triacetic acid, diethylene triamine penta-acetic acid, hydroxyethyl ethylene diamine triacetic acid, 1,2-diaminocyclohexane tetra-acetic acid, amino diacetic acid, hydroxyethyl amino diacetic acid, and their water soluble alkali metal salts.
7. The method of claim 1 wherein the first solution is heated to an elevated temperature.
8. The method of claim 7 wherein the article is boiled in the first solution.
9. The method of claim 7 wherein the second solution is heated to an elevated temperature.
10. The method of claim 9 wherein the article is boiled in the second solution.
11. The method of claim 1 wherein the acidic solution has a pH of between about 1 and less than 7 and the basic solution has a pH of between greater than 7 and about 12.
12. The method of claim 1 wherein at least one of said solutions contains an inert water soluble salt to control the tonicity of the solution.
13. A method of cleaning a hydrophilic gel lens comprising:
a) successively contacting the lens with a heated first aqueous solution and then a heated second aqueous solution, with each solution containing an active oxygen yielding per compound in a concentration of from 0.1 to 15 weight percent, and one of said solutions being acidic and the other of said solutions being basic; and b) removing the lens from the heated second solution, contacting it with a non-ionic detergent, and rinsing it with water.
a) successively contacting the lens with a heated first aqueous solution and then a heated second aqueous solution, with each solution containing an active oxygen yielding per compound in a concentration of from 0.1 to 15 weight percent, and one of said solutions being acidic and the other of said solutions being basic; and b) removing the lens from the heated second solution, contacting it with a non-ionic detergent, and rinsing it with water.
14. The method of claim 13 wherein the first and second solutions are boiled.
15. The method of claim 13 wherein after rinsing the lens is equilibrated in an isotonic solution and sterilized.
16. The method of claim 15 wherein the first and second solutions are boiled.
17. The method of claim 15 wherein the first and second solutions independently comprise from 0.1 to 15 weight percent of said per compound and 0.001 to 5 weight percent of a chelating agent.
18. The method fo claim 15 wherein the lens is alternately expanded and contracted to aid in removing debris and dirt.
19. The method of claim 18 wherein the tonicities of the first and second solutions are controlled to bring about the expansion and contraction.
20. The method of claim 18 where one of said first and second solutions is hypertonic to bring about contraction of the lens.
21. The method of claim 18 where one of said first and second solutions is hypotonic to bring about expansion of the lens.
22. The method of claim 18 where one of said first and second solutions is hypertonic to bring about contraction of the lens and the other of said first and second solutions is hypotonic to bring about expansion of the lens.
23. A method of cleaning a plastic contact lens comprising immersing the lens in an aqueous solution containing 0.1 to 10%
of an acid active oxygen yielding per compound, 0.1 to 10% of a basic active oxygen yielding per compound and an amino carboxylic acid chelating agent or a water-soluble salt thereof, said solution having a pH of 2 to 11; and removing the lens from the solution, contacting it with a non-ionic detergent, and rinsing it with water.
of an acid active oxygen yielding per compound, 0.1 to 10% of a basic active oxygen yielding per compound and an amino carboxylic acid chelating agent or a water-soluble salt thereof, said solution having a pH of 2 to 11; and removing the lens from the solution, contacting it with a non-ionic detergent, and rinsing it with water.
24. The method of claim 23 wherein the lens is a hydro-philic gel lens and the aqueous solution is boiled.
25. A method of cleaning an article made from a hydrophilic plastic comprising:
a) successively contacting the article with a heated first aqueous solution and then a heated second aqueous solution, with each solution containing an active oxygen yielding per compound in a concentration of from 0.1 to 15 weight percent, and one of said solutions being acidic and the other of said solutions being basic;
b) removing the article from the heated second solution contacting it with a non-ionic detergent, and rinsing it with water; and c) alternately expanding and contracting the article to aid in removing debris and dirt.
a) successively contacting the article with a heated first aqueous solution and then a heated second aqueous solution, with each solution containing an active oxygen yielding per compound in a concentration of from 0.1 to 15 weight percent, and one of said solutions being acidic and the other of said solutions being basic;
b) removing the article from the heated second solution contacting it with a non-ionic detergent, and rinsing it with water; and c) alternately expanding and contracting the article to aid in removing debris and dirt.
26. The method of claim 25 wherein the tonicities of the first and second solutions are controlled to bring about the expansion and contraction.
27. A method of cleaning a plastic comprising:
a) contacting the article with an acid active oxygen yielding compound and a basic active oxygen yielding compound, said active oxygen yielding compounds being contained in at least one aqueous solution wherein, when only one solution is employed, the aqueous solution has a pH of from 2 to 11 and contains each of said acid and basic oxygen yielding compounds in a concentration of from 0.1% to 10% by weight, and wherein when two separate aqueous solutions are employed, each solution contains an active oxygen yielding per compound in a concentration of from 0.1 to 15% by weight, with one of said solutions being acidic and the other of said solutions being basic, b) removing the article from the solution, contacting it with a non-ionic detergent, and rinsing it with water.
a) contacting the article with an acid active oxygen yielding compound and a basic active oxygen yielding compound, said active oxygen yielding compounds being contained in at least one aqueous solution wherein, when only one solution is employed, the aqueous solution has a pH of from 2 to 11 and contains each of said acid and basic oxygen yielding compounds in a concentration of from 0.1% to 10% by weight, and wherein when two separate aqueous solutions are employed, each solution contains an active oxygen yielding per compound in a concentration of from 0.1 to 15% by weight, with one of said solutions being acidic and the other of said solutions being basic, b) removing the article from the solution, contacting it with a non-ionic detergent, and rinsing it with water.
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US405751A US3908680A (en) | 1973-10-12 | 1973-10-12 | Methods for cleaning and bleaching plastic articles |
Publications (1)
Publication Number | Publication Date |
---|---|
CA1040812A true CA1040812A (en) | 1978-10-24 |
Family
ID=23605067
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CA210,450A Expired CA1040812A (en) | 1973-10-12 | 1974-10-01 | Methods and compositions for cleaning and bleaching plastic articles |
Country Status (9)
Country | Link |
---|---|
US (1) | US3908680A (en) |
JP (1) | JPS568675B2 (en) |
AR (1) | AR221025A1 (en) |
BR (1) | BR7408491A (en) |
CA (1) | CA1040812A (en) |
DE (1) | DE2443147C3 (en) |
FR (1) | FR2247327B1 (en) |
GB (1) | GB1472409A (en) |
IT (1) | IT1060369B (en) |
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-
1973
- 1973-10-12 US US405751A patent/US3908680A/en not_active Expired - Lifetime
-
1974
- 1974-09-10 DE DE2443147A patent/DE2443147C3/en not_active Expired
- 1974-09-18 FR FR7431512A patent/FR2247327B1/fr not_active Expired
- 1974-10-01 CA CA210,450A patent/CA1040812A/en not_active Expired
- 1974-10-11 GB GB4425774A patent/GB1472409A/en not_active Expired
- 1974-10-11 AR AR256063A patent/AR221025A1/en active
- 1974-10-11 BR BR8491/74A patent/BR7408491A/en unknown
- 1974-10-11 JP JP11623674A patent/JPS568675B2/ja not_active Expired
- 1974-10-14 IT IT28383/74A patent/IT1060369B/en active
Also Published As
Publication number | Publication date |
---|---|
GB1472409A (en) | 1977-05-04 |
BR7408491A (en) | 1975-11-04 |
US3908680A (en) | 1975-09-30 |
DE2443147B2 (en) | 1980-07-10 |
IT1060369B (en) | 1982-07-10 |
DE2443147A1 (en) | 1975-04-17 |
AU7270574A (en) | 1976-03-04 |
FR2247327B1 (en) | 1977-07-08 |
FR2247327A1 (en) | 1975-05-09 |
JPS568675B2 (en) | 1981-02-25 |
AR221025A1 (en) | 1980-12-30 |
JPS5067378A (en) | 1975-06-06 |
DE2443147C3 (en) | 1981-07-02 |
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