CN100503707C - Synthetic oil-base magnetic poly-alpha olefin liquid and its preparation - Google Patents
Synthetic oil-base magnetic poly-alpha olefin liquid and its preparation Download PDFInfo
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- CN100503707C CN100503707C CNB2006100327945A CN200610032794A CN100503707C CN 100503707 C CN100503707 C CN 100503707C CN B2006100327945 A CNB2006100327945 A CN B2006100327945A CN 200610032794 A CN200610032794 A CN 200610032794A CN 100503707 C CN100503707 C CN 100503707C
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Abstract
The present invention relates to the technical field of nanotechnology and discloses poly-alpha olefin synthetic oil-base magnetic liquid and a preparation method thereof. The magnetic liquid compriseThe present invention relates to nanometer technology, and discloses one kind of synthetic polyalpha olefin oil-base magnetic liquid and its preparation process. The magnetic liquid includes surfactans surface active agents, Fe3O4 nanometer particles and poly alpha olefin synthetic oil, wherein the surface active agents are R1CON (CH3) CH2COOH; R1 is alkyl group with 17-40 carbon atoms or alkylenet, nanometer Fe3O4 particle and synthetic polyalpha olefin oil. The surfactant is R1CON(CH3)CH2COOH, where R1 is C17-C40 alkyl or alkene radical; and the synthetic polyalpha olefin oil is H3CH(R2)-(CH; the poly alpha olefin synthetic oil is H3CH (R2)-(CH2CH (R2)) n-CH2CH2R3, and the n is from two to five; the R2 is the alkyl group with carbon number of from six to ten. The poly alpha olefin synthe2CH(R2))n-CH2CH2R2, where n=2-5 and R2 is C6-C10 alkyl radical. The synthetic polyalpha olefin oil-base magnetic liquid is homogeneous and stable and has high heat stability, high and adjustable saturtic oil magnetic liquid of the present invention has the advantages of uniformity, stability, good heat stability, high saturation magnetization, adjustable saturation magnetization, simple preparatioated magnetization intensity, simple preparation process and low cost. n process and low cost.
Description
Technical field
The present invention relates to field of nanometer technology, be specifically related to a kind of synthetic oil-base magnetic poly-alpha olefin liquid and preparation method thereof.
Background technology
Magnetic liquid is the uniform and stable colloid that the nano magnetic particle behind the tensio-active agent parcel forms in carrier fluid.The oil base magnetic liquid is mainly used in: vacuum rotary seal, loud speaker heat radiation, magnetic liquid grinding, damping shock absorption and field such as lubricated.The oil base magnetic liquid is divided into ester group magnetic liquid, keryl magnetic liquid, silicone oil based magnetic liquid, fluorine ether oil based magnetic liquid etc.The thermostability of ester group magnetic liquid and saturation magnetization are not very desirable.Do not see the report of relevant synthetic oil-base magnetic poly-alpha olefin liquid at home.
Summary of the invention
The purpose of this invention is to provide a kind of Heat stability is good, the synthetic oil-base magnetic poly-alpha olefin liquid that saturation magnetization is high.
Another object of the present invention provides the preparation method of above-mentioned synthetic oil-base magnetic poly-alpha olefin liquid; This preparation technology is simple, and cost is low.
To achieve these goals, the present invention adopts following technical scheme:
A kind of synthetic oil-base magnetic poly-alpha olefin liquid comprises tensio-active agent oleoyl sarcosine, nanometer Fe
3O
4Magnetic-particle and carrier fluid polyalphaolefin synthetic oil PAO, described tensio-active agent is R
1CON (CH
3) CH
2COOH, R
1Be that carbon atom is 17～40 alkyl or alkylene, described carrier fluid polyalphaolefin synthetic oil PAO is CH
3CH (R)-(CH
2CH (R))
n-CH
2CH
2R, n=2～5; R is that carbonatoms is 6～10 alkyl.Described nanometer Fe
3O
4The magnetic-particle diameter is about 10nm.
First kind of preparation method of synthetic oil-base magnetic poly-alpha olefin liquid is as follows:
(1) preparation and washing nano magnetic particle
Adopt chemical coprecipitation to prepare nanometer Fe
3O
4The reaction equation of magnetic-particle is:
Fe
2++2Fe
3++8OH
-＝Fe
3O
4+4H
2O
With Fe
2+, Fe
3+, OH
-Solution is hybrid reaction under high-speed stirring, Fe2
+, Fe
3+, OH
-Mol ratio be 1:2:8～16, stir, temperature of reaction is 40～90 ℃, the reaction times is 10～60 minutes, can obtain the Fe that diameter is 10nm
3O
4Magnetic-particle.Stirring velocity is 300～600r/min.
With the nanometer Fe that obtains
3O
4Magnetic-particle cleans for several times with distilled water, till the conductivity≤100 μ s/cm of washing lotion;
(2) modification of nano magnetic particle
The nanometer Fe that washing is good
3O
4Magnetic-particle distilled water constant volume stirs a certain amount of water phase surfactant mixture of adding down.Stir, 30～95 ℃ of heating in water bath, modification 30～90min makes the good nano magnetic particle of modification.Stirring velocity is 200～300r/min.
(3) washing of the nano magnetic particle that modification is good
Nano magnetic particle after the modification is successively used distilled water and washing with acetone for several times, until removing unmodified good nano magnetic particle and unnecessary tensio-active agent.Can the unmodified good nano magnetic particle of flush away with distilled water isopolarity solvent.Can the unnecessary tensio-active agent of flush away with acetone.
(4) drying of nano magnetic particle
The nano magnetic particle of step (3) preparation is made dry sample 60 ℃ of following vacuum-dryings.
(5) dispersion of nano magnetic particle
With an amount of PAO immersion 48 hours, and then ultra-sonic dispersion 24 hours made uniform and stable PAO based magnetic liquid with the sample of step (4) preparation.
The another kind of preparation method of synthetic oil-base magnetic poly-alpha olefin liquid is as follows:
(1) preparation and washing nano magnetic particle
The preparation nano magnetic particle can adopt: methods such as chemical coprecipitation, mechanical milling method, thermal decomposition method, electrical discharge machining and reduction method.
Chemical coprecipitation prepares nanometer Fe
3O
4The ion-reaction equation of magnetic-particle is:
Fe
2++2Fe
3++8OH
-＝Fe
3O
4+4H
2O
With Fe
2+, Fe
3+, OH
-Solution is hybrid reaction under high-speed stirring, Fe
2+, Fe
3+, OH
-Mol ratio be 1:2:8～16, stir, temperature of reaction is 40～90 ℃, the reaction times is 10～60 minutes, can obtain the Fe that diameter is 10nm
3O
4Magnetic-particle.Stirring velocity is 300～600r/min.
With the nanometer Fe that obtains
3O
4Magnetic-particle cleans for several times with distillation, till the conductivity≤100 μ s/cm of washing lotion;
(2) with nano magnetic particle modification in an amount of PAO, and then use washing with acetone, remove with the method for heated and stirred at last and anhydrate and acetone.
Compared with prior art, the present invention has following beneficial effect: the present invention adopts new tensio-active agent and carrier fluid to prepare a kind of new magnetic liquid.The magnetic liquid that the present invention relates to is uniform and stable, Heat stability is good, saturation magnetization height; Saturation magnetization is adjustable; The preparation method is simple, and cost is low.Magnetic liquid of the present invention is applicable to that loud speaker heat radiation, stepper-motor damping shock absorption, magnetic liquid grind, lubricated and sealing.Performance perameter: saturation magnetization 18.7～37.9emu/g (240～730Gs); Saturation magnetization is adjustable; Viscosity in the time of 27 ℃ is 36～445mPa.s; Density 1.02～1.54g/cm
3The magnetic liquid Heat stability is good, it vacuumizes 90 ℃ in vacuum drying oven down baking 234 hours is still uniform and stable, and loss amount has only 10.3%.
Description of drawings
The acupuncture structural map that Fig. 1 forms under the action of a magnetic field for synthetic oil-base magnetic poly-alpha olefin liquid;
Fig. 2 is the micro-structure diagram of magnetic liquid;
Fig. 3 is the magnetic hysteresis loop figure of magnetic liquid.
Embodiment
Embodiment 1
1. prepare and the washing nano magnetic particle:
108g FeCl
36H
2O is dissolved in the 400ml distilled water; 40g FeCl
24H
2O is dissolved in the 400ml distilled water; Mix two kinds of salts solutions.With the NH in the molysite mixing solutions adding 150ml stirring
4In the OH solution, generate the black nano magnetic-particle.NH
4NH in the OH solution
3Mass percent is 25%; The stirring velocity of mechanical stirrer is set at 400r/min.Stir heating in water bath for reaction thing 55min down, bath temperature is 70 ℃.Clean the synthetic magnetic-particle for several times with the 1500ml distillation, till the conductivity≤100 μ s/cm of washing lotion at every turn.
2. the configuration surface promoting agent aqueous solution:
The Korantin SH (oleoyl sarcosine) of 20.24g BASF is dissolved in the 400ml distilled water, adds 30ml NH again
3Mass percent is 25% NH
4OH solution, 85 ℃ of heating in water bath Korantin SH are dissolved in the water, form the surfactant soln of homogeneous transparent.
3. the modification of nano magnetic particle:
The nanometer Fe that washing is good
3O
4To 400ml, stirring velocity is to add the water phase surfactant mixture that configures under the 200r/min mechanical stirring to magnetic-particle with the distilled water constant volume.The 200r/min mechanical stirring is set modification 60min under 98 ℃ of heating in water bath.
4. the washing of the nano magnetic particle after the modification:
With the nano magnetic particle after the modification of 1500ml distilled water wash 6 times.Wash 3 times with 50ml acetone: after stirring with glass stick, ultrasonic again 1min behind the magnetic support sedimentation magnetic-particle, slowly pours out the upper strata and contains the acetone of tensio-active agent and the mixed solution of water at every turn.
5. drying nano magnetic-particle:
The sample that modification is good is put into vacuum drying oven and is carried out drying.Design temperature is 60 ℃ when dry, vacuumizes dry Ex-all acetone and water, obtains the 58g dry sample.PAO with 45ml Chevron Philips Chemical company soaked the 43.87g dry sample 48 hours, and ultra-sonic dispersion is 24 hours again, makes the uniform and stable magnetic liquid of about 50ml.Magnetic liquid forms the high acupuncture of about 1cm under the static magnetic field effect.Centrifugal sample is 2 hours under the 4000r/min, and sample is uniform and stable, and no obvious sediment is separated out.
The saturation magnetization of gained sample is 33.35emu/g (515Gs); Viscosity in the time of 27 ℃ is 109.5mPa.s; Density 1.31g/cm
3The magnetic liquid Heat stability is good (its in 90 ℃ vacuum drying oven, vacuumize the baking 234 hours still uniform and stable, loss amount has only 10.3%).The micro-structure diagram of magnetic liquid as shown in Figure 2.The acupuncture structure that magnetic liquid forms under the action of a magnetic field as shown in Figure 1.
Embodiment 2
Preparation and washing nano magnetic particle:
108g FeCl
36H
2O is dissolved in the 400ml distilled water; 40g FeCl
24H
2O is dissolved in the 400ml distilled water; Mix two kinds of iron salt solutions.With the NH in the molysite mixing solutions adding 200ml stirring
4In the OH solution, generate the black nano magnetic-particle.NH
4NH in the OH solution
3Mass percent is 25%; The stirring velocity of mechanical stirrer is set at 400r/min.Stir heating in water bath for reaction thing 20min down, bath temperature is 60 ℃.Clean the synthetic magnetic-particle for several times with the 1500ml distillation, till the conductivity≤100 μ s/cm of washing lotion at every turn.With the above-mentioned magnetic-particle of 100ml alcohol wash 3 times.
Synthesizing of nano magnetic particle surface modification and magnetic liquid:
The mixture that adds 200ml PAO and 20g Korantin SH.The 200r/min mechanical stirring is set modification 60min under 98 ℃ of heating in water bath.The magnetic liquid that the 100ml alcohol wash makes 3 times, when washing at every turn behind the ultrasonic 3min magnetic fall and slowly topple over alcohol and tensio-active agent mixed solution.The magnetic stirring apparatus heating, the mechanical stirring aforementioned sample is removed alcohol and the water in the sample.Centrifugal sample is 2 hours under the 4000r/min, and sample is uniform and stable, has small amount of precipitate to separate out.The saturation magnetization of the sample that finally obtains is 18.6emu/g (239Gs); Viscosity in the time of 27 ℃ is 36mPa.s; Density 1.02g/cm
3
Embodiment 3
The technology and the embodiment 2 of embodiment 3 preparation magnetic liquids are basic identical, and difference is: the amount of buying the PAO that executes example 3 usefulness is 90ml, and the amount of the PAO of embodiment 2 usefulness is 200ml.
The saturation magnetization of the sample that embodiment 3 makes is 28.8emu/g (446Gs); Viscosity in the time of 27 ℃ is 68.9mPa.s; Density 1.24g/cm
3
Embodiment 4
The technology and the embodiment 2 of embodiment 4 preparation magnetic liquids are basic identical, and difference is: the amount of the PAO of embodiment 4 usefulness is 60ml, and the amount of the PAO of embodiment 2 usefulness is 200ml.
The saturation magnetization of the sample that embodiment 4 makes is 37.9emu/g (732Gs); Viscosity in the time of 27 ℃ is 445mPa.s; Density 1.54g/cm
3The magnetic hysteresis loop figure of gained sample as shown in Figure 3.
Claims (1)
1, a kind of preparation method of synthetic oil-base magnetic poly-alpha olefin liquid is characterized in that being made up of following steps:
(1) preparation and washing Fe
3O
4Nano particle
With Fe
2+, Fe
3+, OH
-Solution is hybrid reaction under high-speed stirring, Fe
2+, Fe
3+, OH
-Mol ratio be 1:2:8～16, stir, temperature of reaction is 40～90 ℃, the reaction times is 10～60 minutes, can obtain Fe
3O
4Magnetic-particle; Described stirring velocity is 300～600r/min; With the nanometer Fe that obtains
3O
4Magnetic-particle cleans for several times with distilled water, till the conductivity≤100 μ s/cm of washing lotion;
(2) Fe
3O
4The modification of nano particle
The Fe that washing is good
3O
4Nano magnetic particle distilled water constant volume stirs adding water phase surfactant mixture down, stirs reaction down, 98 ℃ of bath temperatures, and modification time 30～90min makes the good nano magnetic particle of modification; The speed of described stirring is 200～600r/min; Tensio-active agent and Fe
3O
4The nano particle mol ratio is: 1:3.5～5.9;
(3) the good Fe of washing modification
3O
4Nano particle
The nano magnetic particle that modification is good is earlier with using washing with acetone, until removing unmodified good nano magnetic particle and unnecessary tensio-active agent behind the distilled water wash;
(4) drying of nano magnetic particle
Dry sample is made in the nano magnetic particle vacuum-drying of step (3) preparation;
(5) dispersion of nano magnetic particle
The sample of step (4) preparation is soaked with carrier fluid polyalphaolefin synthetic oil PAO, and then ultra-sonic dispersion, make synthetic oil-base magnetic poly-alpha olefin liquid;
Described tensio-active agent is an oleoyl sarcosine, and its structural formula is: R
1CON (CH
3) CH
2COOH, R
1Be that carbon atom is 17～40 alkyl or alkylene.
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| CN100503707C true CN100503707C (en) | 2009-06-24 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100454452C (en) * | 2006-10-10 | 2009-01-21 | 武汉理工大学 | Stable silicone oil based magnetic rheologic liquid, and preparation method |
| CN103177839B (en) * | 2012-12-28 | 2016-05-11 | 中山大学 | A kind of resistance to oxidation polyalpha olefin synthetic oil-base magnetic liquid and preparation method thereof |
| CN104479822A (en) * | 2014-11-26 | 2015-04-01 | 李铭梁 | Environment-friendly lubricating oil |
| CN108179052A (en) * | 2017-12-29 | 2018-06-19 | 常州市蓝勖化工有限公司 | A kind of nano magnetic lubricating oil and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4855079A (en) * | 1986-10-31 | 1989-08-08 | Hitachi Metals, Ltd. | Super paramagnetic fluids and methods of making super paramagnetic fluids |
| US5064550A (en) * | 1989-05-26 | 1991-11-12 | Consolidated Chemical Consulting Co. | Superparamagnetic fluids and methods of making superparamagnetic fluids |
-
2006
- 2006-01-11 CN CNB2006100327945A patent/CN100503707C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4855079A (en) * | 1986-10-31 | 1989-08-08 | Hitachi Metals, Ltd. | Super paramagnetic fluids and methods of making super paramagnetic fluids |
| US5064550A (en) * | 1989-05-26 | 1991-11-12 | Consolidated Chemical Consulting Co. | Superparamagnetic fluids and methods of making superparamagnetic fluids |
Non-Patent Citations (2)
| Title |
|---|
| 合成烃润滑油(一). 合成润滑材料，第2期. 1998 |
| 合成烃润滑油(一). 合成润滑材料，第2期. 1998 * |
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