CN1810869A - Synthetic oil-base magnetic poly-alpha olefin liquid and its prepn - Google Patents
Synthetic oil-base magnetic poly-alpha olefin liquid and its prepn Download PDFInfo
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- CN1810869A CN1810869A CN 200610032794 CN200610032794A CN1810869A CN 1810869 A CN1810869 A CN 1810869A CN 200610032794 CN200610032794 CN 200610032794 CN 200610032794 A CN200610032794 A CN 200610032794A CN 1810869 A CN1810869 A CN 1810869A
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Abstract
The 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 surfactant, 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)-(CH2CH(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 saturated magnetization intensity, simple preparation process and low cost.
Description
Technical Field
The invention relates to the technical field of nanometer, in particular to a poly α olefin synthetic oil-based magnetic liquid and a preparation method thereof.
Background
The oil-based magnetic liquid is divided into ester-based magnetic liquid, kerosene-based magnetic liquid, silicone oil-based magnetic liquid, fluoroether oil-based magnetic liquid and the like, the thermal stability and the saturation magnetization of the ester-based magnetic liquid are not ideal, and reports about poly α olefin synthetic oil-based magnetic liquid are not seen in China.
Disclosure of Invention
The invention aims to provide a poly α olefin synthetic oil-based magnetic liquid with good thermal stability and high saturation magnetization.
The invention also aims to provide a preparation method of the poly α olefin synthetic oil-based magnetic liquid, which has simple preparation process and low cost.
In order to achieve the purpose, the invention adopts the following technical scheme:
a magnetic liquid based on synthetic oil of poly α olefin contains oleoyl sarcosine as surfactant and nano Fe3O4Magnetic particles and carrier liquid poly α olefin synthetic oil PAO, and the surfactant is R1CON(CH3)CH2COOH，R1Is alkyl or alkenyl with 17-40 carbon atoms, and the carrier liquid poly α olefin synthetic oil PAO is H3CH(R2)-(CH2CH(R2))n-CH2CH2R2，n＝2～5；R2Is an alkyl group having 6 to 10 carbon atoms. The nano Fe3O4The magnetic particles have a diameter of about 10 nm.
A first preparation method of the poly α olefin synthetic oil-based magnetic liquid is as follows:
(1) preparation and washing of magnetic nanoparticles
Preparing nano Fe by chemical coprecipitation method3O4The reaction equation for magnetic particles is:
mixing Fe2+、Fe3+、OH-The solution is mixed and reacted under high-speed stirring, Fe2+、Fe3+、OH-The molar ratio of (1: 2: 8) - (16), stirring, reacting at 40-90 ℃ for 10-60 minutes to obtain the final productTo 10nm diameter of Fe3O4Magnetic particles. The stirring speed is 300-600 r/min.
The obtained nano Fe3O4Washing the magnetic particles for several times by distillation until the conductivity sigma of the washing liquid is less than or equal to 100 mu s/cm;
(2) modification of nano-magnetic particles
Washing the nanometer Fe3O4The magnetic particles are fixed to the volume by using distilled water, and a certain amount of surfactant aqueous solution is added under stirring. Stirring, heating in water bath for 30-95 ℃, and modifying for 30-90 min to obtain the modified magnetic nanoparticles. The stirring speed is 200-300 r/min.
(3) Washing of modified nano-magnetic particles
Washing the modified nano magnetic particles with distilled water and acetone for several times until the unmodified nano magnetic particles and the redundant surfactant are removed. The unmodified magnetic nanoparticles can be washed away by using a polar solvent such as distilled water. Excess surfactant can be washed off with acetone.
(4) Drying of nano-magnetic particles
And (4) drying the nano magnetic particles prepared in the step (3) at 60 ℃ in vacuum to prepare a dry sample.
(5) Dispersion of nano-magnetic particles
And (4) soaking the sample prepared in the step (4) with a proper amount of PAO for 48 hours, and then performing ultrasonic dispersion for 24 hours to prepare uniform and stable PAO-based magnetic liquid.
Another method for preparing poly α olefin synthetic oil-based magnetic liquid is as follows:
(1) preparation and washing of magnetic nanoparticles
The preparation of the nano-magnetic particles can adopt the following steps: chemical coprecipitation, mechanical grinding, thermal decomposition, spark erosion, reduction, and the like.
Preparation of nano Fe by chemical coprecipitation method3O4The ion reaction equation for magnetic particles is:
mixing Fe2+、Fe3+、OH-The solution is mixed and reacted under high-speed stirring, Fe2+、Fe3+、OH-The molar ratio of (1: 2: 8) - (16), stirring, reacting at 40-90 ℃ for 10-60 minutes to obtain Fe with the diameter of 10nm3O4Magnetic particles. The stirring speed is 300-600 r/min.
The obtained nano Fe3O4Washing the magnetic particles for several times by distillation until the conductivity sigma of the washing liquid is less than or equal to 100 mu s/cm;
(2) modifying the nano magnetic particles in a proper amount of PAO, then washing with acetone, and finally removing water and acetone by a heating and stirring method.
Compared with the prior art, the invention has the following beneficial effects: the present invention prepares a new magnetic liquid by using new surfactant and carrier liquid. The magnetic liquid involved in the invention is uniform and stable, good in thermal stability and high in saturation magnetization; the saturation magnetization is adjustable; the preparation method is simple and low in cost. The magnetic liquid is suitable for heat dissipation of a loudspeaker, damping and shock absorption of a stepping motor, grinding, lubrication and sealing of the magnetic liquid. Performance parameters: saturation magnetization of 18.7-37.9 emu/g (240-730 Gs); the saturation magnetization is adjustable; the viscosity at 27 ℃ is 36-445 mPa.s; the density is 1.02-1.54 g/cm3(ii) a The magnetic liquid has good thermal stability, is even and stable after being baked for 234 hours in a vacuum drying oven at 90 ℃ after being vacuumized, and has the loss of only 10.3 percent.
Drawings
FIG. 1 is a diagram of a needling structure formed by poly α olefin synthetic oil-based magnetic liquid under the action of a magnetic field;
FIG. 2 is a microscopic view of a magnetic liquid;
fig. 3 is a hysteresis chart of the magnetic liquid.
Detailed Description
Example 1
1. Preparing and washing the nano magnetic particles:
108g FeCl3·6H2dissolving O in 400ml of distilled water; 40g FeCl2·4H2Dissolving O in 400ml of distilled water; the two salt solutions were mixed. Adding the mixed solution of ferric salt into 150ml of NH in stirring4In OH solution, black nano magnetic particles are generated. NH (NH)4NH in OH solution3The mass percent is 25%; the stirring speed of the mechanical stirrer was set at 400 r/min. The reaction was heated in a water bath with stirring for 55min, the temperature of the water bath being 70 ℃. The synthesized magnetic particles were washed several times with 1500ml of distillation each time until the conductivity σ of the washing liquid was not more than 100 μ s/cm.
2. Preparing a surfactant aqueous solution:
20.24g of Korantin SH (oleoyl sarcosine) from BASF was dissolved in 400ml of distilled water, and 30ml of NH was added3NH with the mass percent of 25%4OH solution, Korantin SH is dissolved in water by heating in water bath at 85 ℃ to form uniform and transparent surfactant solution.
3. Modification of the nano magnetic particles:
washing the nanometer Fe3O4The magnetic particles are added with the prepared surfactant aqueous solution under the mechanical stirring with the stirring speed of 200r/min until the volume is 400ml by using distilled water. Mechanically stirring at 200r/min, and modifying for 60min under the condition of water bath heating at 98 ℃.
4. Washing the modified nano magnetic particles:
the modified nano-magnetic particles were washed 6 times with 1500ml of distilled water. Wash 3 times with 50ml acetone: stirring with a glass rod every time, performing ultrasonic treatment for 1min, settling magnetic particles with a magnetic seat, and slowly pouring out the mixture of acetone and water containing surfactant at the upper layer.
5. Drying the nano magnetic particles:
and (4) putting the modified sample into a vacuum drying oven for drying. The temperature was set at 60 ℃ during drying, and acetone and water were removed by vacuum drying to obtain 58g of a dried sample. About 50ml of a homogeneous stable magnetic liquid was prepared by soaking 43.87g of the dried sample in 45ml of PAO from Chevron Philips Chemical for 48 hours and further ultrasonic dispersing for 24 hours. The magnetic liquid forms a needle prick with the height of about 1cm under the action of a static magnetic field. And centrifuging the sample for 2 hours at 4000r/min, wherein the sample is uniform and stable, and no obvious precipitate is separated out.
The saturation magnetization of the sample obtained was 33.35emu/g (515 Gs); a viscosity at 27 ℃ of 109.5 mPa.s; density 1.31g/cm3(ii) a The magnetic liquid has good thermal stability (the magnetic liquid is uniform and stable after being vacuumized and baked for 234 hours in a vacuum drying oven at 90 ℃, and the loss is only 10.3 percent). The microstructure of the magnetic liquid is shown in FIG. 2. The acupuncture structure of the magnetic liquid under the action of the magnetic field is shown in figure 1.
Example 2
Preparing and washing the nano magnetic particles:
108g FeCl3·6H2dissolving O in 400ml of distilled water; 40g FeCl2·4H2Dissolving O in 400ml of distilled water; the two iron salt solutions were mixed. Adding the mixed solution of ferric salt into 200ml of NH in stirring4In OH solution, black nano magnetic particles are generated. NH (NH)4NH in OH solution3The mass percent is 25%; the stirring speed of the mechanical stirrer was set at 400 r/min. The reaction was heated in a water bath with stirring for 20min at a temperature of 60 ℃. The synthesized magnetic particles were washed several times with 1500ml of distillation each time until the conductivity σ of the washing liquid was not more than 100 μ s/cm. The magnetic particles were washed 3 times with 100ml of alcohol.
Surface modification of nano magnetic particles and synthesis of magnetic liquid:
a mixture of 200ml of PAO and 20g of Korantin SH was added. Mechanically stirring at 200r/min, and modifying for 60min under the condition of water bath heating at 98 ℃. The magnetic liquid prepared by 100ml of alcohol is washed for 3 times, and the mixed liquid of the alcohol and the surfactant is slowly poured out by magnetic reduction after the ultrasonic treatment is carried out for 3min during each washing. And (4) heating by a magnetic stirrer, and mechanically stirring the sample to remove the alcohol and the water in the sample. And centrifuging the sample for 2 hours at 4000r/min, wherein the sample is uniform and stable, and a small amount of precipitate is separated out. The saturation magnetization of the finally obtained sample is 18.6emu/g (239 Gs); a viscosity at 27 ℃ of 36 mPa.s; density 1.02g/cm3。
Example 3
Example 3 the process for preparing a magnetic liquid was substantially the same as in example 2, except that: the amount of PAO used in example 3 was 90ml and the amount of PAO used in example 2 was 200 ml.
The saturation magnetization of the sample prepared in example 3 was 28.8emu/g (446 Gs); a viscosity at 27 ℃ of 68.9 mPa.s; density 1.24g/cm3。
Example 4
Example 4 the process for preparing a magnetic liquid was substantially the same as in example 2, except that: the amount of PAO used in example 4 was 60ml and the amount of PAO used in example 2 was 200 ml.
The saturation magnetization of the sample obtained in example 4 was 37.9emu/g (732 Gs); viscosity at 27 ℃ of 445 mPa.s; density 1.54g/cm3. The hysteresis loop of the resulting sample is shown in FIG. 3.
Claims (6)
1. A magnetic liquid based on synthetic oil of poly α olefin contains surfactant and Fe3O4Nanoparticles and a carrier liquid, characterized in that the carrier liquid is poly α olefin synthetic oil, PAO.
2. The poly α olefin synthetic oil-based magnetic liquid of claim 1, wherein the surfactant is oleoyl sarcosine of formula R1CON(CH3)CH2COOH，R1Is a carbon atom of 17 to 40An alkyl group or an alkenyl group.
3. The poly α olefin synthetic oil-based magnetic liquid according to claim 1 or 2, wherein the poly α olefin synthetic oil PAO has the formula CH3CH(R)-(CH2CH(R))n-CH2CH2R and n are 2-5; r is C6-10 alkyl.
4. A method for preparing the poly α olefin synthetic oil-based magnetic liquid according to claim 1, comprising the steps of:
(1) preparation and washing of Fe3O4Nanoparticles
Mixing Fe2+、Fe3+、OH-The solution is mixed and reacted under high-speed stirring, Fe2+、Fe3+、OH-The molar ratio of (1: 2: 8) - (16), stirring, reacting at 40-90 ℃ for 10-60 minutes to obtain Fe3O4Magnetic particles; the stirring speed is 300-600 r/min; the obtained nano Fe3O4Washing the magnetic particles for several times by distillation until the conductivity sigma of the washing liquid is less than or equal to 100 mu s/cm;
(2)Fe3O4modification of nanoparticles
Washing the Fe3O4Fixing the volume of the nano magnetic particles by using distilled water, adding a surfactant aqueous solution while stirring, reacting while stirring, wherein the water bath temperature is 30-95 ℃, and the modification time is 30-90 min to prepare modified nano magnetic particles; the stirring speed is 200-600 r/min; surfactant and Fe3O4The mole ratio of the nano particles is as follows: 1: 3.5-5.9;
(3) washing modified Fe3O4Nanoparticles
Washing the modified nano magnetic particles with distilled water and then acetone until unmodified nano magnetic particles and redundant surfactant are removed;
(4) drying of nano-magnetic particles
Drying the nano magnetic particles prepared in the step (3) in vacuum to prepare a dry sample;
(5) dispersion of nano-magnetic particles
And (3) soaking the sample prepared in the step (4) by using carrier liquid poly α olefin synthetic oil PAO, and then performing ultrasonic dispersion to prepare the poly α olefin synthetic oil-based magnetic liquid.
5. The method according to claim 4, wherein the aqueous surfactant solution is: adding distilled water and ammonia water into the surfactant to dissolve the surfactant to form auniform and transparent surfactant aqueous solution; the ratio of oleoyl sarcosine to 25% ammonia was: 20g oleoyl sarcosine: 30ml of ammonia.
6. Another method for preparing the poly α olefin synthetic oil-based magnetic fluid of claim 1, comprising the steps of:
(1) preparing and washing the nano magnetic particles: mixing Fe2+、Fe3+、OH-The solution is mixed and reacted under stirring, Fe2+、Fe3+、OH-The molar ratio of (1: 2: 8) - (16), stirring, reacting at 40-90 ℃ for 10-60 minutes to obtain Fe3O4Magnetic particles; the stirring speed is 300-600 r/min; the obtained nano Fe3O4Washing the magnetic particles for several times by distillation until the conductivity sigma of the washing liquid is less than or equal to 100 mu s/cm;
(2) adding the washed nano magnetic particles into a mixed solution of a surfactant and carrier liquid PAO for modification, wherein the water bath temperature is 30-95 ℃, and the modification time is 30-90 min, so as to prepare modified nano magnetic particles; the stirring speed is 200-600 r/min; surfactant and Fe3O4The mole ratio of the nano particles is as follows: 1: 3.5-5.9; then washing with acetone to remove excessive surfactant, and removing water and acetone by heating and stirring.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100454452C (en) * | 2006-10-10 | 2009-01-21 | 武汉理工大学 | Stable silicone oil based magnetic rheologic liquid, and preparation method |
| CN103177839A (en) * | 2012-12-28 | 2013-06-26 | 中山大学 | Magnetic liquid based on oxidation-resistant alpha olefin synthetic oil 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 |
Family Cites Families (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
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100454452C (en) * | 2006-10-10 | 2009-01-21 | 武汉理工大学 | Stable silicone oil based magnetic rheologic liquid, and preparation method |
| CN103177839A (en) * | 2012-12-28 | 2013-06-26 | 中山大学 | Magnetic liquid based on oxidation-resistant alpha olefin synthetic oil and preparation method thereof |
| 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 |
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