US2963356A - Burning rate catalysts for ammonium nitrate propellants - Google Patents
Burning rate catalysts for ammonium nitrate propellants Download PDFInfo
- Publication number
- US2963356A US2963356A US609779A US60977956A US2963356A US 2963356 A US2963356 A US 2963356A US 609779 A US609779 A US 609779A US 60977956 A US60977956 A US 60977956A US 2963356 A US2963356 A US 2963356A
- Authority
- US
- United States
- Prior art keywords
- parts
- weight
- ammonium nitrate
- propellant
- methyl
- 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 - Lifetime
Links
- 239000003380 propellant Substances 0.000 title claims description 28
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 title claims description 13
- 239000003054 catalyst Substances 0.000 title description 19
- 239000000203 mixture Substances 0.000 claims description 24
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 claims description 19
- 229920001577 copolymer Polymers 0.000 claims description 18
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 3
- 239000012279 sodium borohydride Substances 0.000 claims description 3
- 239000000463 material Substances 0.000 description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 14
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 14
- 239000011230 binding agent Substances 0.000 description 13
- 239000007800 oxidant agent Substances 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 10
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 9
- 150000001993 dienes Chemical class 0.000 description 9
- 150000001875 compounds Chemical class 0.000 description 8
- -1 i.e. Substances 0.000 description 8
- VRWKTAYJTKRVCU-UHFFFAOYSA-N iron(6+);hexacyanide Chemical compound [Fe+6].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] VRWKTAYJTKRVCU-UHFFFAOYSA-N 0.000 description 8
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- 230000001590 oxidative effect Effects 0.000 description 8
- 229920001971 elastomer Polymers 0.000 description 7
- 125000000623 heterocyclic group Chemical group 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 239000001272 nitrous oxide Substances 0.000 description 7
- 239000004449 solid propellant Substances 0.000 description 7
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 6
- DCYOBGZUOMKFPA-UHFFFAOYSA-N iron(2+);iron(3+);octadecacyanide Chemical compound [Fe+2].[Fe+2].[Fe+2].[Fe+3].[Fe+3].[Fe+3].[Fe+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] DCYOBGZUOMKFPA-UHFFFAOYSA-N 0.000 description 6
- 239000004014 plasticizer Substances 0.000 description 6
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 description 5
- 125000004432 carbon atom Chemical group C* 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 5
- 239000005060 rubber Substances 0.000 description 5
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 5
- 229920002554 vinyl polymer Polymers 0.000 description 5
- KGIGUEBEKRSTEW-UHFFFAOYSA-N 2-vinylpyridine Chemical compound C=CC1=CC=CC=N1 KGIGUEBEKRSTEW-UHFFFAOYSA-N 0.000 description 4
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 4
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 125000000217 alkyl group Chemical group 0.000 description 4
- 239000003963 antioxidant agent Substances 0.000 description 4
- 239000006229 carbon black Substances 0.000 description 4
- 239000004615 ingredient Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000004073 vulcanization Methods 0.000 description 4
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 3
- 241001441571 Hiodontidae Species 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 229910026551 ZrC Inorganic materials 0.000 description 3
- OTCHGXYCWNXDOA-UHFFFAOYSA-N [C].[Zr] Chemical compound [C].[Zr] OTCHGXYCWNXDOA-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 229910052987 metal hydride Inorganic materials 0.000 description 3
- 150000004681 metal hydrides Chemical class 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 150000003222 pyridines Chemical class 0.000 description 3
- 239000012744 reinforcing agent Substances 0.000 description 3
- 239000000344 soap Substances 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- 239000011593 sulfur Substances 0.000 description 3
- 239000000080 wetting agent Substances 0.000 description 3
- 239000011787 zinc oxide Substances 0.000 description 3
- 229910052726 zirconium Inorganic materials 0.000 description 3
- QSGNKXDSTRDWKA-UHFFFAOYSA-N zirconium dihydride Chemical compound [ZrH2] QSGNKXDSTRDWKA-UHFFFAOYSA-N 0.000 description 3
- 229910000568 zirconium hydride Inorganic materials 0.000 description 3
- SDJHPPZKZZWAKF-UHFFFAOYSA-N 2,3-dimethylbuta-1,3-diene Chemical compound CC(=C)C(C)=C SDJHPPZKZZWAKF-UHFFFAOYSA-N 0.000 description 2
- GDDNTTHUKVNJRA-UHFFFAOYSA-N 3-bromo-3,3-difluoroprop-1-ene Chemical compound FC(F)(Br)C=C GDDNTTHUKVNJRA-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 125000003545 alkoxy group Chemical group 0.000 description 2
- JOSWYUNQBRPBDN-UHFFFAOYSA-P ammonium dichromate Chemical compound [NH4+].[NH4+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O JOSWYUNQBRPBDN-UHFFFAOYSA-P 0.000 description 2
- DIKBFYAXUHHXCS-UHFFFAOYSA-N bromoform Chemical compound BrC(Br)Br DIKBFYAXUHHXCS-UHFFFAOYSA-N 0.000 description 2
- GZUXJHMPEANEGY-UHFFFAOYSA-N bromomethane Chemical compound BrC GZUXJHMPEANEGY-UHFFFAOYSA-N 0.000 description 2
- DKVNPHBNOWQYFE-UHFFFAOYSA-N carbamodithioic acid Chemical compound NC(S)=S DKVNPHBNOWQYFE-UHFFFAOYSA-N 0.000 description 2
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 125000004093 cyano group Chemical group *C#N 0.000 description 2
- 239000012990 dithiocarbamate Substances 0.000 description 2
- 238000007720 emulsion polymerization reaction Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 150000001247 metal acetylides Chemical class 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 239000006069 physical mixture Substances 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 229960003351 prussian blue Drugs 0.000 description 2
- 239000013225 prussian blue Substances 0.000 description 2
- 238000005956 quaternization reaction Methods 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- APSBXTVYXVQYAB-UHFFFAOYSA-M sodium docusate Chemical compound [Na+].CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC APSBXTVYXVQYAB-UHFFFAOYSA-M 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000010059 sulfur vulcanization Methods 0.000 description 2
- RZRJACCZWZTYJY-UHFFFAOYSA-N tert-butylsulfanyl n,n-dimethylcarbamodithioate Chemical compound CN(C)C(=S)SSC(C)(C)C RZRJACCZWZTYJY-UHFFFAOYSA-N 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- XFNJVJPLKCPIBV-UHFFFAOYSA-N trimethylenediamine Chemical group NCCCN XFNJVJPLKCPIBV-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- JDUQPSINXKBHEN-UHFFFAOYSA-N (3-ethenylisoquinolin-6-yl)methanol Chemical compound C1=NC(C=C)=CC2=CC(CO)=CC=C21 JDUQPSINXKBHEN-UHFFFAOYSA-N 0.000 description 1
- WVICRWJHVDRYSU-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;methyl prop-2-enoate Chemical compound COC(=O)C=C.C=CC1=CC=CC=C1C=C WVICRWJHVDRYSU-UHFFFAOYSA-N 0.000 description 1
- BUSCTLHHPMLZMS-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;prop-2-enoic acid;styrene Chemical compound OC(=O)C=C.C=CC1=CC=CC=C1.C=CC1=CC=CC=C1C=C BUSCTLHHPMLZMS-UHFFFAOYSA-N 0.000 description 1
- CHRJZRDFSQHIFI-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;styrene Chemical compound C=CC1=CC=CC=C1.C=CC1=CC=CC=C1C=C CHRJZRDFSQHIFI-UHFFFAOYSA-N 0.000 description 1
- PAAZPARNPHGIKF-UHFFFAOYSA-N 1,2-dibromoethane Chemical compound BrCCBr PAAZPARNPHGIKF-UHFFFAOYSA-N 0.000 description 1
- DKWHHTWSTXZKDW-UHFFFAOYSA-N 1-[2-[2-[2-(2-butoxyethoxy)ethoxymethoxy]ethoxy]ethoxy]butane Chemical compound CCCCOCCOCCOCOCCOCCOCCCC DKWHHTWSTXZKDW-UHFFFAOYSA-N 0.000 description 1
- MUEHGEQAMLEEID-UHFFFAOYSA-N 1-pentyl-2-phenylbenzene Chemical group CCCCCC1=CC=CC=C1C1=CC=CC=C1 MUEHGEQAMLEEID-UHFFFAOYSA-N 0.000 description 1
- FSECWGZNMLROOX-UHFFFAOYSA-N 2,3-dimethylhexa-1,3-diene Chemical compound CCC=C(C)C(C)=C FSECWGZNMLROOX-UHFFFAOYSA-N 0.000 description 1
- NRHMWTYCQDTKRA-UHFFFAOYSA-N 2-(5-ethenylpyridin-3-yl)phenol Chemical compound OC1=CC=CC=C1C1=CN=CC(C=C)=C1 NRHMWTYCQDTKRA-UHFFFAOYSA-N 0.000 description 1
- OWQUYBAASOSGNO-CDNKMLFNSA-N 2-[[(Z)-N-(2-hydroxy-5-sulfoanilino)-C-phenylcarbonimidoyl]diazenyl]benzoic acid Chemical compound C1=CC=C(C=C1)/C(=N/NC2=C(C=CC(=C2)S(=O)(=O)O)O)/N=NC3=CC=CC=C3C(=O)O OWQUYBAASOSGNO-CDNKMLFNSA-N 0.000 description 1
- JJVHEIJBQGMBKG-UHFFFAOYSA-N 2-ethenyl-3,4,5,6-tetramethylpyridine Chemical compound CC1=NC(C=C)=C(C)C(C)=C1C JJVHEIJBQGMBKG-UHFFFAOYSA-N 0.000 description 1
- TUPJXKPXLGTGTO-UHFFFAOYSA-N 2-ethenyl-4-ethylquinoline Chemical compound C1=CC=C2C(CC)=CC(C=C)=NC2=C1 TUPJXKPXLGTGTO-UHFFFAOYSA-N 0.000 description 1
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- IIBPRBOWHWXNCE-UHFFFAOYSA-N 3-ethenyl-2-methyl-5-undecylpyridine Chemical compound CCCCCCCCCCCC1=CN=C(C)C(C=C)=C1 IIBPRBOWHWXNCE-UHFFFAOYSA-N 0.000 description 1
- JDAPKVYHFNRFKO-UHFFFAOYSA-N 3-ethenyl-5-phenylpyridine Chemical compound C=CC1=CN=CC(C=2C=CC=CC=2)=C1 JDAPKVYHFNRFKO-UHFFFAOYSA-N 0.000 description 1
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- VYIYXBONKWPJSH-UHFFFAOYSA-N 4-benzyl-2-ethenylquinoline Chemical compound C=12C=CC=CC2=NC(C=C)=CC=1CC1=CC=CC=C1 VYIYXBONKWPJSH-UHFFFAOYSA-N 0.000 description 1
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- VJOWMORERYNYON-UHFFFAOYSA-N 5-ethenyl-2-methylpyridine Chemical compound CC1=CC=C(C=C)C=N1 VJOWMORERYNYON-UHFFFAOYSA-N 0.000 description 1
- NTFOOQDZAMZVJD-UHFFFAOYSA-N 5-ethenyl-4-nonyl-2-propan-2-ylpyridine Chemical compound CCCCCCCCCC1=CC(C(C)C)=NC=C1C=C NTFOOQDZAMZVJD-UHFFFAOYSA-N 0.000 description 1
- APCYSORWSVNLEN-UHFFFAOYSA-N 6-ethenyl-2-methyl-4-nonylquinoline Chemical compound C1=C(C=C)C=C2C(CCCCCCCCC)=CC(C)=NC2=C1 APCYSORWSVNLEN-UHFFFAOYSA-N 0.000 description 1
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- KXDHJXZQYSOELW-UHFFFAOYSA-M Carbamate Chemical compound NC([O-])=O KXDHJXZQYSOELW-UHFFFAOYSA-M 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
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- 229910002651 NO3 Inorganic materials 0.000 description 1
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- 239000002253 acid Substances 0.000 description 1
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- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 125000002877 alkyl aryl group Chemical group 0.000 description 1
- 150000001350 alkyl halides Chemical class 0.000 description 1
- 150000008051 alkyl sulfates Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 125000004104 aryloxy group Chemical group 0.000 description 1
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- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 description 1
- 239000012965 benzophenone Substances 0.000 description 1
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- 229950005228 bromoform Drugs 0.000 description 1
- 238000012662 bulk polymerization Methods 0.000 description 1
- XZKRXPZXQLARHH-UHFFFAOYSA-N buta-1,3-dienylbenzene Chemical compound C=CC=CC1=CC=CC=C1 XZKRXPZXQLARHH-UHFFFAOYSA-N 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
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- 230000007423 decrease Effects 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- NZZFYRREKKOMAT-UHFFFAOYSA-N diiodomethane Chemical compound ICI NZZFYRREKKOMAT-UHFFFAOYSA-N 0.000 description 1
- HRKQOINLCJTGBK-UHFFFAOYSA-L dioxidosulfate(2-) Chemical compound [O-]S[O-] HRKQOINLCJTGBK-UHFFFAOYSA-L 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- YAGKRVSRTSUGEY-UHFFFAOYSA-N ferricyanide Chemical compound [Fe+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] YAGKRVSRTSUGEY-UHFFFAOYSA-N 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- 125000001188 haloalkyl group Chemical group 0.000 description 1
- 125000001475 halogen functional group Chemical group 0.000 description 1
- 239000008240 homogeneous mixture Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 150000002431 hydrogen Chemical group 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 125000005027 hydroxyaryl group Chemical group 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- INQOMBQAUSQDDS-UHFFFAOYSA-N iodomethane Chemical compound IC INQOMBQAUSQDDS-UHFFFAOYSA-N 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 125000000555 isopropenyl group Chemical group [H]\C([H])=C(\*)C([H])([H])[H] 0.000 description 1
- 150000002537 isoquinolines Chemical class 0.000 description 1
- 239000004816 latex Substances 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 1
- WCYWZMWISLQXQU-UHFFFAOYSA-N methyl Chemical compound [CH3] WCYWZMWISLQXQU-UHFFFAOYSA-N 0.000 description 1
- CZXGXYBOQYQXQD-UHFFFAOYSA-N methyl benzenesulfonate Chemical compound COS(=O)(=O)C1=CC=CC=C1 CZXGXYBOQYQXQD-UHFFFAOYSA-N 0.000 description 1
- 229940102396 methyl bromide Drugs 0.000 description 1
- JZMJDSHXVKJFKW-UHFFFAOYSA-M methyl sulfate(1-) Chemical compound COS([O-])(=O)=O JZMJDSHXVKJFKW-UHFFFAOYSA-M 0.000 description 1
- SNVLJLYUUXKWOJ-UHFFFAOYSA-N methylidenecarbene Chemical group C=[C] SNVLJLYUUXKWOJ-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- QUPCNWFFTANZPX-UHFFFAOYSA-M paramenthane hydroperoxide Chemical compound [O-]O.CC(C)C1CCC(C)CC1 QUPCNWFFTANZPX-UHFFFAOYSA-M 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000000276 potassium ferrocyanide Substances 0.000 description 1
- LDQICAMJIICDLF-UHFFFAOYSA-N potassium;iron(2+);iron(3+);hexacyanide Chemical compound [K+].[Fe+2].[Fe+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] LDQICAMJIICDLF-UHFFFAOYSA-N 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 150000003248 quinolines Chemical class 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000008036 rubber plasticizer Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- XOGGUFAVLNCTRS-UHFFFAOYSA-N tetrapotassium;iron(2+);hexacyanide Chemical compound [K+].[K+].[K+].[K+].[Fe+2].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] XOGGUFAVLNCTRS-UHFFFAOYSA-N 0.000 description 1
- RYCLIXPGLDDLTM-UHFFFAOYSA-J tetrapotassium;phosphonato phosphate Chemical compound [K+].[K+].[K+].[K+].[O-]P([O-])(=O)OP([O-])([O-])=O RYCLIXPGLDDLTM-UHFFFAOYSA-J 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
- 230000000007 visual effect Effects 0.000 description 1
- 229940043798 zincon Drugs 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B45/00—Compositions or products which are defined by structure or arrangement of component of product
- C06B45/04—Compositions or products which are defined by structure or arrangement of component of product comprising solid particles dispersed in solid solution or matrix not used for explosives where the matrix consists essentially of nitrated carbohydrates or a low molecular organic explosive
- C06B45/06—Compositions or products which are defined by structure or arrangement of component of product comprising solid particles dispersed in solid solution or matrix not used for explosives where the matrix consists essentially of nitrated carbohydrates or a low molecular organic explosive the solid solution or matrix containing an organic component
- C06B45/10—Compositions or products which are defined by structure or arrangement of component of product comprising solid particles dispersed in solid solution or matrix not used for explosives where the matrix consists essentially of nitrated carbohydrates or a low molecular organic explosive the solid solution or matrix containing an organic component the organic component containing a resin
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B23/00—Compositions characterised by non-explosive or non-thermic constituents
- C06B23/007—Ballistic modifiers, burning rate catalysts, burning rate depressing agents, e.g. for gas generating
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S149/00—Explosive and thermic compositions or charges
- Y10S149/11—Particle size of a component
- Y10S149/112—Inorganic nitrogen-oxygen salt
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S149/00—Explosive and thermic compositions or charges
- Y10S149/11—Particle size of a component
- Y10S149/113—Inorganic oxygen-halogen salt
Definitions
- This invention relates to solid propellants. More particularly, this invention relates to a new class of burning rate catalysts for solid propellants.
- solid propellant materials comprising a solid oxidant such as ammonium nitrate or ammonium perchlorate, and a rubbery copolymer of butadiene and a vinylpyridine or other vinyl substituted heterocyclic nitrogen base compound, which after incorporation of the oxidant is cured by a quaternization reaction or a vulcanization reaction.
- Solid propellant mixtures of this nature and a process for their production are disclosed and claimed in copending application Serial No. 284,447, filed April 2,063,356 Patented D es. 6, teen
- An object of this invention is to provide a new class of burning rate catalysts for solid propellants prepared from ammonium nitrate and a rubbery binder.
- a further object of this invention is to provide such propellants having increased burning rates.
- the burning rate of the propellant is about 0.100 inch per second when no burning rate catalyst is used.
- Metals, metal hydrides, or metal carbides which are applicable are those which react with nitrous oxide at initial temperatures below 406 C. and which do not react with ammonium nitrate at temperatures below 60 C. These materials react with the nitrous oxide to give a glowing hot solid and act as an ignition source behind the flame, thereby increasing the burning rate of the propellants. They should not react with ammonium nitrate below 60 C., in order to eliminate the possibility of reaction in storage.
- these compounds include sodium borohydride, zirconium, zirconium hydride, zirconium carbide, titanium and cerium. These compounds are added to the solid propellant during the formulation thereof and are preferably added as finely divided materials. Broadly, the amount of these materials added is in the range of 0.5 to 10 parts per 100 parts of total propellant, 1 to 4 parts being most commonly used.
- the rubbery polymers employed as binders in the solid propellant compositions of this invention are copolymers of conjugated dienes with polymerizable heterocyclic nitrogen bases of the pyridine series. These copolymers can vary in consistency from very soft rubbers, i.e., materials which are soft at room temperature but will show retraction when relaxed, to those having a Mooney value (ML4) up to 100. Copolymers of higher Mooney value can be used if large softener loadings are used.
- the rubbery copolymers most frequently preferred have Mooney values in the range between 10 and 40. They may be prepared by any polymerization methods known to the art, e.g., mass or emulsion polymerization.
- c0- polymers One convenient method for preparing these c0- polymers is by emulsion polymerization at temperatures in the range between 0 and F. Recipes such as the iron pyrophosphate-hydroperoxide, either sugar-free or containing sugar, the sulfoxylate and the persulfate recipes are among those which are applicable. It is advantageous to polymerize to high conversion as the unreacted vinylpyridine monomer is diflicult to remove by stripping.
- the conjugated dienes employed are those containing from 4 to 6 carbon atoms per molecule and'include- 1,3- butadiene, isoprene, 2-mcthyl-l,3-butadiene, 2,3dimethyl 1,3-butadiene, and the like.
- Various alkoxy, such as methoxy and ethoxy and cyano derivatives of these conjugated dienes, are also applicable.
- dienes such as phenylbutadiene, 2,3-dimethyl-1,3-hexadien'e, 2- meth'oXy-3-ethylbutadiene, 2-ethoxy-3-ethyl l,3-ihexadiene, 2-cyano-1,3-butadiene, are also applicable in the preparation of the polymeric binders of this invention.
- conjugated diene instead of using a single conjugated diene, a mixture of conjugated dienes can be employed.
- a mixture of 1,3-butadiene and isoprene can be employed as the conjugated 'diene'porti0n of the monomer system.
- the polymerizable heterocyclic nitrogen bases which are applicable for the production of the polymeric materials are those of the pyridine, quinoline, and isoquinoline series which are copolymerizable with a conjugated diene and contain one, and only one,
- CH2 C substituent wherein R is either hydrogen or a methyl group. That is, the substituent is either a vinyl or an .alpha-methylvinyl (isopropenyl) group.
- R is either hydrogen or a methyl group. That is, the substituent is either a vinyl or an .alpha-methylvinyl (isopropenyl) group.
- R is either hydrogen or a methyl group. That is, the substituent is either a vinyl or an .alpha-methylvinyl (isopropenyl) group.
- R is either hydrogen or a methyl group. That is, the substituent is either a vinyl or an .alpha-methylvinyl (isopropenyl) group.
- the compounds of the pyridine series are of the greatest interest commercially at present.
- Various substituted derivatives are also applicable but the total number of carbon atoms in the groups attached to the carbon atoms of the heterocyclic nucleus should not be greater. than 12 because the polymer
- R is selected from the group consisting of hydrogen, alkyl, vinyl, alpha-methylvinyl, alkoxy, halo, hydroxy, cyano, aryloxy, aryl, and combinations of these groups such as haloalkyl, alkylaryl, hydroxyaryl, and the like; one and only one of said groups being selected from the group consisting of vinyl and alpha-methylvinyl; and the total number of carbon atoms in the nuclear substituted groups, in addition to the vinyl or alpha-methylvinyl group, being not greater than 12.
- Examples of such compounds are 2-vinylpyridine; 2-vinyl-5-ethylpyridine; 2-methyl-5-vinylpyridine; 4-vinylpyridine; 2,3,4-trimethy1- S-vinylpyridine; 3,4,5,6-tetra-methyl-2-vinylpyridine; 3- ethyl-S-vinylpyridine; 2,6-diethyl-4-vinylpyridine; 2-isopropyl-4-nonyl-5-vinylpyridine; 2-methyl-5-undecyl-3-vinylpyridine; 2,4-dimethyl-5,6-dipentyl-3-vinylpyridine; 2- decy1-5-(alpha-methylvinyl)pyridine; 2-vinyl-3-methyl-5- ethylpyridine; 2-methoxy-4-chloro-6-vinylpyridine; 3-vinyl-S-ethoxypyridine; 2-vinyl-4,5-dichloropyridine; 2-(alpha-methylvin
- the polymer used'as the binder in the propellant 111118 previously described was a portion of the product produced in a series of 55 runs.
- the following recipe was "'used:
- Butadiene 1 90 Z-methyl-S-vinylpyridine 10
- Water 200 Potassium fatty acid soap 6.0
- Tetra sodium salt of ethylenediamine tetracetic acid 0.005
- Tertiary dodecyl mercaptan Variable Ferrous sulfate heptahydrate
- Potassium pyrophosphate 0.253 Paramenthane hydroperoxide 0.1 or 0.135
- 'dithiocarbamate an amount of 0.15 part.
- the polymer was stabilized by adding 1.75 percent by weight based on the polymer of phenyl-beta-napthylamine.
- the latex was masterbatched with 19.5 parts of Philblack A carbon black per parts of rubber and acid coagulated.
- the crumb was caustic (potassium hydroxide) washed at a high pH to convert the organic acid to soap which was washed out to obtain a product with low organic acid and soap and subsequently dried.
- the binder for propellants 1 through 6 was as follows:
- the binder for propellant 7 was as follows:
- the polymer was placed on a roll mill and additional black was added to bring the loading to the desired level.
- the Flexamine was also added on the mill.
- the resulting mixture was placed in a Baker-Perkins mixer and the plasticizer and magnesium oxide and curatives, if used, were added and the composition mixed until a homogeneous mixture was obtained.
- the catalyst and ammonium nitrate were blended together and added to the binder in four portions, each time the mixing being continued until the mixer started drawing power. A final mixing of 5 to 10 minutes after addition of all the oxidizer was provided to insure uniformity.
- the propellant was made into strands by extruding it under a pressure of 8000 p.s.i.
- Regular propellant grade ammonium nitrate or ammonium perchlorate is used as the oxidant in the propellants of my invention. It should be finely divided, preferably in a range of 300 to 10 microns average particle size.
- the amount of oxidant is generally in the range of 50 to 90 percent by weight of the total of the oxidant and binder. If desired, however, less than 50 percent by weight can be used.
- the combustion rate catalysts of my invention can be used alone or in combination with combustion rate catalysts known in the art, such as ammonium dichromate and metal ferrocyanides and ferricyanides.
- Ferric ferrocyanides such as Prussian, Berlin, Hamburg, Chinese, Paris and Milori blue
- soluble ferric ferrocyanide such as soluble Berlin or Prussian blue which contains potassium ferric ferrocyanide
- ferric ferrocyanide which has been treated with ammonia
- Ferrous ferricyanide T urnbulls blue is also applicable.
- Milori blue is a pigment similar to Prussian blue but having a red tint and is prepared by the oxidation of a paste of potassium ferrocyanide and ferrous sulfate.
- Other metal compounds such as nickel and copper ferrocyanides can also be employed.
- the amount of burning rate catalyst used, in the propellant compositions of this invention are usually in the range of l to 60 parts per 100 parts of rubbery polymer with from 5 to 50 parts being most frequently preferred.
- the amount of combustion catalyst will usually be 0.5 to 10 parts by weight per hundred parts of oxidant and binder, with a range of l to 4 parts being preferred.
- the combination catalysts are used from 0.5 to 10 parts of the catalyst according to the present invention (metal, metal carbide, or metal hydride) is used per 100 parts by weight of propellant and from 0.25 to 5 parts of the prior art catalyst such as Milori blue are used.
- the binder contains a rubbery copolymer of the type hereinbefore described and, in addition, there can be present one or more reinforcing agents, plasticizers, wetting agents, and antioxidants.
- Other ingredients which are employed for sulfur vulcanization include a vulcanization accelerator, a vulcanizing agent such as sulfur, and an accelerator activator, such as zinc oxide.
- the copolymer comprising a conjugated diene and a polymerizable heterocyclic nitrogen base can also be cured by a quaternization reaction by incorporating therein a quaternizing agent and subjecting the resulting mixture to quaternizing conditions of temperature.
- Suitable quaternizing agents include alkyl halides such as methyl iodide, methyl bromide; alkylene halides such as methylene iodide, ethylene bromide; substituted alkanes such as chloroform, bromoform; alkyl sulfates such as methyl sulfate; and various substituted aromatic compounds such as benzoyl chloride, methyl benzene sulfonate, and the like.
- the quaternizing temperature is usually in the range zero to 175 0, although temperatures outside this range can be used.
- a general formulation for a binder composition prepared by sulfur vulcanization is given below:
- Reinforcing agent 0-50 Plasticizer 0-100 Wetting agent 0-10
- Antioxidant 0-3
- Vulcanization accelerator 0-5
- Sulfur 0-2
- Zinc oxide 0-5
- Reinforcing agents include carbon black, silica gel, lignin, and various reinforcing resins such as styrene-divinylbenzene, methyl acrylate-divinyl-benzene, acrylic acid-styrene-divinylbenzene, and methyl acrylate-acrylic acid-divinyl-benzene resins.
- any rubber plasticizers can be employed in these binder compositions.
- Materials such as Pentaryl A (amylbiphenyl), Parafiux (saturated polymerized hydrocarbon), Circosol-ZXH (petroleum hydrocarbon softener having a specific gravity of 0.940 and a Saybolt Universal viscosity at 100 F. of about 2000 seconds), di (1,4,7-trioxaundecyl)methane, and dioctyl phthalate are suitable plasticizers. Materials which provide rubber having good low temperature properties are preferred. It is also frequently preferred that the plasticizers be oxygen-containing materials.
- Wetting agents aid in deflocculating or dispersing the oxidizer, Aerosol OT (dioctyl ester of sodium sulfosuccinic acid), lechithin, and Duomeen C diacetate (the diacetate of trimethylene diamine substituted by a coconut oil product) are among the materials which are applicable.
- Antioxidants include Flexamine (physical mixture containing 65 percent of a complex diarylamine-ketone reaction product and 35 percent of N,N-diphenyl-p-phenylenediamine), phenyl-beta-naphthylamine, 2,2-methylenebis(4-methy1-6-tert-butylphenol), and the like. Rubber antioxidants, in general, may be employed or if desired may be omitted.
- vulcanization accelerators are those of the carbamate type, such as N,N-dimethyl-S-tert-butylsulfenyl dithiocarbamate and Butyl-Eight.
- Butyl Eight is a rubber accelerator of the dithiocarbamate type described in Handbook of Material Trade Names by Zimmerman and Lavine, 1953 edition, as a brown liquid; specific gravity 1.01; partially soluble in water and gasoline; and soluble in acetone, alcohol, benzol, carbon disulfide and chloroform.
- each of the various types of compounding ingredients may be used singly or mixtures of various ingredients performing a certain function may be employed. It is sometimes preferred, for example, to use mixtures of plasticizers rather than a single material.
- the various ingredients in the propellant composition may be mixed on a roll mill or an internal mixer such as a Banbury or a Baker-Perkins dispersion blade mixer may be employed.
- the binder forms a continous phase in the propellant with the oxidant as the discontinuous phase.
- Rocket grains are formed by compression molding, injection molding, or extrusion.
- the curing temperature will be limited by the oxidizer employed in some cases but will generally be in the range between 70 and 250 F., preferably between and 200 F.
- the curing time must be long enough to give required creep resistance and other mechanical properties in the propellant.
- the time will generally range from around three hours when the higher curing temperatures are employed to seven days when curing is eflect'ed at lower temperatures- A 1 v p
- all matter herein set forth is to be interpreted as illustrative and not in a limiting sense.
- A-propellant composition comprisingfrom 50 to 90 parts by weight of ammonium nitrate; from- 10 to 50parts by weight of a copolymer of'b'utadiene a'nd'Z-methyl-S- inylpyfidine to make a total of 100 parts by weight; from 0.25 to 5 parts by Weight of Milori blue; and from 0.5' to IO-parts by weightof sodiumb'orohydride.
- A-propellant composition comprising from 50 to 90 parts by-weightof ammonium nitrate; from to 50 parts by weight-o? a-copolymer of butadiene and Z-methyl-S- yinylpyridineto make a--total "of 100 parts by weight; from 0.25 to '5 parts by weight of Milori-blue; and from 0.5 to 10partsby weight of-zirconium.
- a propellant composition comprising from 50 to 90' parts by weight ofammonium nitrate; from 10 to 50 parts by'weight of a copolymer of butadiene and Z-methyl- 5-vinylpyridine to make a total of 100 parts by weight; from 0.25 to 5 parts by weight of Milori blue; and from 0.5 to 10 parts by weight of zirconium hydride.
- a propellant composition comprising from 50 to 90 parts by weight of ammonium nitrate; from- 10 to 50 parts by weight of a copolymer of butadiene and 2-methyls vinylpyridine to make a total of 100 parts by weight; from 0.25-to 5 parts by weight of Milori blue; and from 0.5 to 10 parts by weight of zirconium carbide. -5'.
- a propellant composition comprising from 5010 90 parts -by weight of ammonium nitrate; from 10 to 50 parts by Weight of a copolymer of butadiene andZ-methyl- 5-vinylpynidine to make a total of 100 parts by weight; from 0.25 to 5 parts of 100 parts by weight; from 0.25
Description
EURNING RATE CATALYSTS FOR AIMMONIUM NETRATE PROPELLANTS Eugene Daniel Guth, Bartlesville, kla., assignor to Phillips Petroleum Company, a corporation of Delawere No Drawing. Filed Sept. 13, 1956, Ser. No. 609,779
7 Claims. (Cl. 52-.5)
This invention relates to solid propellants. More particularly, this invention relates to a new class of burning rate catalysts for solid propellants.
Recently it has been discovered that superior solid propellant materials are obtained comprising a solid oxidant such as ammonium nitrate or ammonium perchlorate, and a rubbery copolymer of butadiene and a vinylpyridine or other vinyl substituted heterocyclic nitrogen base compound, which after incorporation of the oxidant is cured by a quaternization reaction or a vulcanization reaction. Solid propellant mixtures of this nature and a process for their production are disclosed and claimed in copending application Serial No. 284,447, filed April 2,063,356 Patented D es. 6, teen An object of this invention is to provide a new class of burning rate catalysts for solid propellants prepared from ammonium nitrate and a rubbery binder. A further object of this invention is to provide such propellants having increased burning rates.
Other objects and advantages of this invention will be apparent to one skilled in the art upon reading this disclosure.
It is believed that this invention can be best understood from a specific example including a series of runs employing this new group of burning rate catalysts.
In the following table a series of catalyst systems are set forth and the burning rate is given at two different pressures. In each case, the amount used is given as parts by weight per 100 parts of the propellant. The column headed temperature of reaction with N 0 refers to the temperature at which the catalyst compound begins to react with N 0. The tests with nitrous oxide were made with the catalyst, finely divided, in a tube which was inside a furnace. The nitrous oxide was passed through the tube at a flow rate sufiicient to maintain a fairly pure atmosphere over the material. The temperature was gradually increased during each run and visual observations were made to determine when the reaction occurred. The burning rate of the propellant is about 0.100 inch per second when no burning rate catalyst is used.
TABLE I Reaction of catalyst systems with nitrous oxide [Strand data. 1' vs. P curve] Tempera- 1- at 600 r at 1,000 ture of Propellant Catalyst System, Parts p.s.i. p.s.i. 12 Reaction Remarks (in/sec.) (um/sec.) w 1172] 5. 0,
Ila/@1101"; glue 0.144 0.199 0. 58 300 1 Oil l1B 2 4.0 Sodium borohydrlde 0-153 211 61 fig i ggfig g 0. 147 0. 204 0. 64 220 g g fi fi gf 0.15s 0. 225 0. 55 400 Vigorous glow.
. 011 11G 4,0 Zincon'dum carbide 0.168 0. 223 0. 52 400 D0. :8 j 0.191 0. 246 0. 51 220 D0. 4.0 Milori blue. 0.165 0. 201 300 25, 1952, and now abandoned, by W. B. Reynolds and J. E. Pritchard.
Various materials have been added to these compositions in order to increase the burning rate thereof. I have discovered that a group of metals, metal hydrides, or metal carbides will increase the burning rate of these propellants in which the ammonium nitrate is used as the oxidant. Metals, metal hydrides, or metal carbides which are applicable are those which react with nitrous oxide at initial temperatures below 406 C. and which do not react with ammonium nitrate at temperatures below 60 C. These materials react with the nitrous oxide to give a glowing hot solid and act as an ignition source behind the flame, thereby increasing the burning rate of the propellants. They should not react with ammonium nitrate below 60 C., in order to eliminate the possibility of reaction in storage. Examples of these compounds include sodium borohydride, zirconium, zirconium hydride, zirconium carbide, titanium and cerium. These compounds are added to the solid propellant during the formulation thereof and are preferably added as finely divided materials. Broadly, the amount of these materials added is in the range of 0.5 to 10 parts per 100 parts of total propellant, 1 to 4 parts being most commonly used.
Therefore, the following are objects of this invention:
It is readily obvious from the data in this table that there is a correlation between the reaction temperature of each material with nitrous oxide at atmosphere pressure and the burning rate increase. Those materials which have a low temperature of reaction with nitrous oxide increase the burning rate more than those with a high reaction temperature.
The rubbery polymers employed as binders in the solid propellant compositions of this invention are copolymers of conjugated dienes with polymerizable heterocyclic nitrogen bases of the pyridine series. These copolymers can vary in consistency from very soft rubbers, i.e., materials which are soft at room temperature but will show retraction when relaxed, to those having a Mooney value (ML4) up to 100. Copolymers of higher Mooney value can be used if large softener loadings are used. The rubbery copolymers most frequently preferred have Mooney values in the range between 10 and 40. They may be prepared by any polymerization methods known to the art, e.g., mass or emulsion polymerization. One convenient method for preparing these c0- polymers is by emulsion polymerization at temperatures in the range between 0 and F. Recipes such as the iron pyrophosphate-hydroperoxide, either sugar-free or containing sugar, the sulfoxylate and the persulfate recipes are among those which are applicable. It is advantageous to polymerize to high conversion as the unreacted vinylpyridine monomer is diflicult to remove by stripping.
The conjugated dienes employed are those containing from 4 to 6 carbon atoms per molecule and'include- 1,3- butadiene, isoprene, 2-mcthyl-l,3-butadiene, 2,3dimethyl 1,3-butadiene, and the like. Various alkoxy, such as methoxy and ethoxy and cyano derivatives of these conjugated dienes, are also applicable. Thus, other dienes, suchas phenylbutadiene, 2,3-dimethyl-1,3-hexadien'e, 2- meth'oXy-3-ethylbutadiene, 2-ethoxy-3-ethyl l,3-ihexadiene, 2-cyano-1,3-butadiene, are also applicable in the preparation of the polymeric binders of this invention.
Instead of using a single conjugated diene, a mixture of conjugated dienes can be employed. Thus, a mixture of 1,3-butadiene and isoprene can be employed as the conjugated 'diene'porti0n of the monomer system.
The polymerizable heterocyclic nitrogen bases which are applicable for the production of the polymeric materials are those of the pyridine, quinoline, and isoquinoline series which are copolymerizable with a conjugated diene and contain one, and only one,
/R'. CH2=C substituent wherein R is either hydrogen or a methyl group. That is, the substituent is either a vinyl or an .alpha-methylvinyl (isopropenyl) group. Of these, the compounds of the pyridine series are of the greatest interest commercially at present. Various substituted derivatives are also applicable but the total number of carbon atoms in the groups attached to the carbon atoms of the heterocyclic nucleus should not be greater. than 12 because the polymerization rate decreases somewhat with increasing size of the alkyl group. Compounds where the alkyl substituents are methyl and/or ethyl are available commercially.
These heterocyclic nitrogen bases have the formula where R is selected from the group consisting of hydrogen, alkyl, vinyl, alpha-methylvinyl, alkoxy, halo, hydroxy, cyano, aryloxy, aryl, and combinations of these groups such as haloalkyl, alkylaryl, hydroxyaryl, and the like; one and only one of said groups being selected from the group consisting of vinyl and alpha-methylvinyl; and the total number of carbon atoms in the nuclear substituted groups, in addition to the vinyl or alpha-methylvinyl group, being not greater than 12. Examples of such compounds are 2-vinylpyridine; 2-vinyl-5-ethylpyridine; 2-methyl-5-vinylpyridine; 4-vinylpyridine; 2,3,4-trimethy1- S-vinylpyridine; 3,4,5,6-tetra-methyl-2-vinylpyridine; 3- ethyl-S-vinylpyridine; 2,6-diethyl-4-vinylpyridine; 2-isopropyl-4-nonyl-5-vinylpyridine; 2-methyl-5-undecyl-3-vinylpyridine; 2,4-dimethyl-5,6-dipentyl-3-vinylpyridine; 2- decy1-5-(alpha-methylvinyl)pyridine; 2-vinyl-3-methyl-5- ethylpyridine; 2-methoxy-4-chloro-6-vinylpyridine; 3-vinyl-S-ethoxypyridine; 2-vinyl-4,5-dichloropyridine; 2-(alpha-methylvinyl)-4-hydroxy-6-cyanopyridine; 2-vinyl-4- phenoxy-S-methylpyridine; 2-cyano-5-(alpha methylvinyl)pyridine; 3-vinyl-5-phenylpyridine; Z-(para-methylphenyl)-3-vinyl-4-methylpyridine; 3-vinyl 5 (hydroxyphenyl)-pyridine; 2-vinylquinoline; 2-vinyl-4-ethylquinoline; 3-vinyl6,7-di-n-propylquinoline; 2-methyl-4-nonyl-6- vinylquinoline; 4-(alpha-methylvinyl)-8-dodecylquinoline; 3-viny1isoquinoline; 1,6-dimethyl-3-vinylisoquinoline; 2- vinyl-4-benzylquinoline; 3-vinyl-5-chloroethylquinoline; 3- vinyl-S,6-dichloroisoquinoline; 2-vinyl-6-ethoxy-7-methylquinoline; 3-vinyl-6-hydroxymethylisoquinoline; and the like. Mixtures of these heterocyclic nitrogen bases can be used, if desired.
The polymer used'as the binder in the propellant 111118 previously described was a portion of the product produced in a series of 55 runs. The following recipe was "'used:
Parts by weight Butadiene 1 90 Z-methyl-S-vinylpyridine 10 Water 200 Potassium fatty acid soap 6.0 KCI 0.1 Sodium alkyl aryl sulfonate 0.3 Tetra sodium salt of ethylenediamine tetracetic acid 0.005 Tertiary dodecyl mercaptan Variable Ferrous sulfate heptahydrate 0.2 Potassium pyrophosphate 0.253 Paramenthane hydroperoxide 0.1 or 0.135
'dithiocarbamate an amount of 0.15 part. The polymer was stabilized by adding 1.75 percent by weight based on the polymer of phenyl-beta-napthylamine.
The latex was masterbatched with 19.5 parts of Philblack A carbon black per parts of rubber and acid coagulated. The crumb was caustic (potassium hydroxide) washed at a high pH to convert the organic acid to soap which was washed out to obtain a product with low organic acid and soap and subsequently dried. The binder for propellants 1 through 6 was as follows:
Parts by weight Copolymer 100 Carbon black 20 ZP-2l1 1 20 Flexamine 3 3 1 5,8.11,13.16.19-hex cxa-n-tricosane.
5 A physical mixture .ontaining 65 percent of a complex dtarylamine-ketone react on product and 35 percent of N,N- diphenyl-p-phenylenedlamine.
The binder for propellant 7 was as follows:
Parts by weight Copolymer 100 Carbon black 20 Benzophenone 20 Flexamine 1 3.0
N,N-dimethyl-S-tert-butylsulfenyl dithiocarbamate 1.0 Sulfur 0.75 Zinc oxide 3.0
I 5,8,11,13,16,19-hexoxa-n-tr1cosane.
Lia K...)
The complete composition of each propellant is shown in the following table:
For each run, the polymer was placed on a roll mill and additional black was added to bring the loading to the desired level. The Flexamine was also added on the mill.
The resulting mixture was placed in a Baker-Perkins mixer and the plasticizer and magnesium oxide and curatives, if used, were added and the composition mixed until a homogeneous mixture was obtained. The catalyst and ammonium nitrate were blended together and added to the binder in four portions, each time the mixing being continued until the mixer started drawing power. A final mixing of 5 to 10 minutes after addition of all the oxidizer was provided to insure uniformity.
The propellant was made into strands by extruding it under a pressure of 8000 p.s.i.
Regular propellant grade ammonium nitrate or ammonium perchlorate is used as the oxidant in the propellants of my invention. It should be finely divided, preferably in a range of 300 to 10 microns average particle size. The amount of oxidant is generally in the range of 50 to 90 percent by weight of the total of the oxidant and binder. If desired, however, less than 50 percent by weight can be used.
The combustion rate catalysts of my invention can be used alone or in combination with combustion rate catalysts known in the art, such as ammonium dichromate and metal ferrocyanides and ferricyanides. Ferric ferrocyanides, such as Prussian, Berlin, Hamburg, Chinese, Paris and Milori blue, soluble ferric ferrocyanide, such as soluble Berlin or Prussian blue which contains potassium ferric ferrocyanide, and ferric ferrocyanide which has been treated with ammonia, are among the materials which can be used. Ferrous ferricyanide, T urnbulls blue is also applicable. Milori blue is a pigment similar to Prussian blue but having a red tint and is prepared by the oxidation of a paste of potassium ferrocyanide and ferrous sulfate. Other metal compounds such as nickel and copper ferrocyanides can also be employed.
The amount of burning rate catalyst used, in the propellant compositions of this invention, are usually in the range of l to 60 parts per 100 parts of rubbery polymer with from 5 to 50 parts being most frequently preferred. The amount of combustion catalyst will usually be 0.5 to 10 parts by weight per hundred parts of oxidant and binder, with a range of l to 4 parts being preferred. When the combination catalysts are used from 0.5 to 10 parts of the catalyst according to the present invention (metal, metal carbide, or metal hydride) is used per 100 parts by weight of propellant and from 0.25 to 5 parts of the prior art catalyst such as Milori blue are used.
The binder contains a rubbery copolymer of the type hereinbefore described and, in addition, there can be present one or more reinforcing agents, plasticizers, wetting agents, and antioxidants. Other ingredients which are employed for sulfur vulcanization include a vulcanization accelerator, a vulcanizing agent such as sulfur, and an accelerator activator, such as zinc oxide.
The copolymer comprising a conjugated diene and a polymerizable heterocyclic nitrogen base can also be cured by a quaternization reaction by incorporating therein a quaternizing agent and subjecting the resulting mixture to quaternizing conditions of temperature. Suitable quaternizing agents include alkyl halides such as methyl iodide, methyl bromide; alkylene halides such as methylene iodide, ethylene bromide; substituted alkanes such as chloroform, bromoform; alkyl sulfates such as methyl sulfate; and various substituted aromatic compounds such as benzoyl chloride, methyl benzene sulfonate, and the like.
The quaternizing temperature is usually in the range zero to 175 0, although temperatures outside this range can be used.
A general formulation for a binder composition prepared by sulfur vulcanization is given below:
Parts by weight Rubbery copolymer (as hereinbefore described) Reinforcing agent 0-50 Plasticizer 0-100 Wetting agent 0-10 Antioxidant 0-3 Vulcanization accelerator 0-5 Sulfur 0-2 Zinc oxide 0-5 Reinforcing agents include carbon black, silica gel, lignin, and various reinforcing resins such as styrene-divinylbenzene, methyl acrylate-divinyl-benzene, acrylic acid-styrene-divinylbenzene, and methyl acrylate-acrylic acid-divinyl-benzene resins.
In general, any rubber plasticizers can be employed in these binder compositions. Materials such as Pentaryl A (amylbiphenyl), Parafiux (saturated polymerized hydrocarbon), Circosol-ZXH (petroleum hydrocarbon softener having a specific gravity of 0.940 and a Saybolt Universal viscosity at 100 F. of about 2000 seconds), di (1,4,7-trioxaundecyl)methane, and dioctyl phthalate are suitable plasticizers. Materials which provide rubber having good low temperature properties are preferred. It is also frequently preferred that the plasticizers be oxygen-containing materials.
Wetting agents aid in deflocculating or dispersing the oxidizer, Aerosol OT (dioctyl ester of sodium sulfosuccinic acid), lechithin, and Duomeen C diacetate (the diacetate of trimethylene diamine substituted by a coconut oil product) are among the materials which are applicable.
Antioxidants include Flexamine (physical mixture containing 65 percent of a complex diarylamine-ketone reaction product and 35 percent of N,N-diphenyl-p-phenylenediamine), phenyl-beta-naphthylamine, 2,2-methylenebis(4-methy1-6-tert-butylphenol), and the like. Rubber antioxidants, in general, may be employed or if desired may be omitted.
Examples of vulcanization accelerators are those of the carbamate type, such as N,N-dimethyl-S-tert-butylsulfenyl dithiocarbamate and Butyl-Eight. Butyl Eight is a rubber accelerator of the dithiocarbamate type described in Handbook of Material Trade Names by Zimmerman and Lavine, 1953 edition, as a brown liquid; specific gravity 1.01; partially soluble in water and gasoline; and soluble in acetone, alcohol, benzol, carbon disulfide and chloroform.
It is to be understood that each of the various types of compounding ingredients may be used singly or mixtures of various ingredients performing a certain function may be employed. It is sometimes preferred, for example, to use mixtures of plasticizers rather than a single material.
The various ingredients in the propellant composition may be mixed on a roll mill or an internal mixer such as a Banbury or a Baker-Perkins dispersion blade mixer may be employed. The binder forms a continous phase in the propellant with the oxidant as the discontinuous phase.
Rocket grains are formed by compression molding, injection molding, or extrusion.
The curing temperature will be limited by the oxidizer employed in some cases but will generally be in the range between 70 and 250 F., preferably between and 200 F.
The curing time must be long enough to give required creep resistance and other mechanical properties in the propellant. The time will generally range from around three hours when the higher curing temperatures are employed to seven days when curing is eflect'ed at lower temperatures- A 1 v p As many. possible embodiments may be made of this invention without departing from the scopethereof, it is to be'understood that all matter herein set forth is to be interpreted as illustrative and not in a limiting sense.
I claim:
, 1. A-propellant composition comprisingfrom 50 to 90 parts by weight of ammonium nitrate; from- 10 to 50parts by weight of a copolymer of'b'utadiene a'nd'Z-methyl-S- inylpyfidine to make a total of 100 parts by weight; from 0.25 to 5 parts by Weight of Milori blue; and from 0.5' to IO-parts by weightof sodiumb'orohydride.
2. A-propellant composition comprising from 50 to 90 parts by-weightof ammonium nitrate; from to 50 parts by weight-o? a-copolymer of butadiene and Z-methyl-S- yinylpyridineto make a--total "of 100 parts by weight; from 0.25 to '5 parts by weight of Milori-blue; and from 0.5 to 10partsby weight of-zirconium.
3. A propellant composition comprising from 50 to 90' parts by weight ofammonium nitrate; from 10 to 50 parts by'weight of a copolymer of butadiene and Z-methyl- 5-vinylpyridine to make a total of 100 parts by weight; from 0.25 to 5 parts by weight of Milori blue; and from 0.5 to 10 parts by weight of zirconium hydride.
4. A propellant composition comprising from 50 to 90 parts by weight of ammonium nitrate; from- 10 to 50 parts by weight of a copolymer of butadiene and 2-methyls vinylpyridine to make a total of 100 parts by weight; from 0.25-to 5 parts by weight of Milori blue; and from 0.5 to 10 parts by weight of zirconium carbide. -5'. A propellant composition comprising from 5010 90 parts -by weight of ammonium nitrate; from 10 to 50 parts by Weight of a copolymer of butadiene andZ-methyl- 5-vinylpynidine to make a total of 100 parts by weight; from 0.25 to 5 parts of 100 parts by weight; from 0.25
'ing'upte 8 carbon" atoms 'permolecule with at'lea'st one 1 substituted heterocylic nitrogen' base selected from the group consisting of pyridine, quinoline, alkyl substituted pyridine,- and alkyl substituted quinoline, wherein the total number of carbon atoms in the nuclear alkyl substituents is not more than 12 and wherein R is selected from thegroup consisting of hydrogen and a methyl radical, to'make a total of parts by weight; from 0.25 to 5 parts by'weight'of a compound selected from the group consisting of ammonium dichromate, .ferric ferrocyanide, ferrousferricyanide, copper ferrocyanide and nickel ferrocyanideyand-from 0.5 to 10 parts by weightof a material selectedfrom the group consisting of sodium borohydride, zirconium, zirconium hydride, zirconium carbide, titanium and cerium. t r
7. The propellant ofclaim 6 wherein'said-copolymer is a copolymer of butadiene'and Z-methyl-S-vinylpyridine.
References Cited in the file of this patent UNITED STATES PATENTS
Claims (1)
1. A PROPELLANT COMPOSITION COMPRISING FROM 50 TO 90 PARTS BY WEIGHT OF AMMONIUM NITRATE, FROM 10 TO 50 PARTS BY WEIGHT OF A COPOLYMER OF BUTADIENE AND2-METHYL-5VINYLPYRIDINE TO MAKE A TOTAL OF 100 PARTS BY WEIGHT, FROM 0.25 TO 5 PARTS BY WEIGHT OF MILORI BLUE, AND FROM 0.5 TO 10 PARTS BY WEIGHT OF SODIUM BOROHYDRIDE.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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US609779A US2963356A (en) | 1956-03-26 | 1956-09-13 | Burning rate catalysts for ammonium nitrate propellants |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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US574042A US2995429A (en) | 1956-03-26 | 1956-03-26 | Solid composite rubber base ammonium nitrate propellant cured with metal oxide |
US609779A US2963356A (en) | 1956-03-26 | 1956-09-13 | Burning rate catalysts for ammonium nitrate propellants |
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US2963356A true US2963356A (en) | 1960-12-06 |
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US609779A Expired - Lifetime US2963356A (en) | 1956-03-26 | 1956-09-13 | Burning rate catalysts for ammonium nitrate propellants |
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US3159104A (en) * | 1959-11-02 | 1964-12-01 | Solid Fuels Corp | Laminated tape propellants |
US4302259A (en) * | 1979-10-31 | 1981-11-24 | The United States Of America As Represented By The Secretary Of The Army | MgH2 and Sr(NO3)2 pyrotechnic composition |
US6306232B1 (en) | 1996-07-29 | 2001-10-23 | Automotive Systems Laboratory, Inc. | Thermally stable nonazide automotive airbag propellants |
US20050257866A1 (en) * | 2004-03-29 | 2005-11-24 | Williams Graylon K | Gas generant and manufacturing method thereof |
US20090057609A1 (en) * | 2007-07-13 | 2009-03-05 | Snpe Materiaux Energetiques | Solid hydrogen source compounds and method for generating hydrogen |
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US2309978A (en) * | 1940-06-21 | 1943-02-02 | Atlas Powder Co | Propellent fuel assembly |
US2433943A (en) * | 1944-03-11 | 1948-01-06 | Aerojet Engineering Corp | Operation of jet propulsion motors with nitroparaffin |
US2555333A (en) * | 1948-05-27 | 1951-06-05 | Joseph A Grand | Solid fuel |
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US2570632A (en) * | 1948-04-01 | 1951-10-09 | Us Rubber Co | Improving the cut growth resistance of butadiene-vinyl pyridine rubbery copolymers |
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US1708186A (en) * | 1924-05-21 | 1929-04-09 | Sterner St P Meek | Tracer composition |
US2309978A (en) * | 1940-06-21 | 1943-02-02 | Atlas Powder Co | Propellent fuel assembly |
US2433943A (en) * | 1944-03-11 | 1948-01-06 | Aerojet Engineering Corp | Operation of jet propulsion motors with nitroparaffin |
GB655585A (en) * | 1947-09-29 | 1951-07-25 | Frans Tore Baltzar Bonell | Improvements in or relating to methods for producing propellent charges for rockets and the like |
US2570632A (en) * | 1948-04-01 | 1951-10-09 | Us Rubber Co | Improving the cut growth resistance of butadiene-vinyl pyridine rubbery copolymers |
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US3159104A (en) * | 1959-11-02 | 1964-12-01 | Solid Fuels Corp | Laminated tape propellants |
US4302259A (en) * | 1979-10-31 | 1981-11-24 | The United States Of America As Represented By The Secretary Of The Army | MgH2 and Sr(NO3)2 pyrotechnic composition |
US6306232B1 (en) | 1996-07-29 | 2001-10-23 | Automotive Systems Laboratory, Inc. | Thermally stable nonazide automotive airbag propellants |
US20050257866A1 (en) * | 2004-03-29 | 2005-11-24 | Williams Graylon K | Gas generant and manufacturing method thereof |
US20100269965A1 (en) * | 2004-03-29 | 2010-10-28 | Williams Graylon K | Gas generant and manufacturing method thereof |
US20090057609A1 (en) * | 2007-07-13 | 2009-03-05 | Snpe Materiaux Energetiques | Solid hydrogen source compounds and method for generating hydrogen |
US7964111B2 (en) * | 2007-07-13 | 2011-06-21 | Snpe Materiaux Energetiques | Solid hydrogen source compounds and method for generating hydrogen |
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