CN114471391A - Self-lubricating PI microcapsule and preparation method thereof - Google Patents
Self-lubricating PI microcapsule and preparation method thereof Download PDFInfo
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- CN114471391A CN114471391A CN202210179161.6A CN202210179161A CN114471391A CN 114471391 A CN114471391 A CN 114471391A CN 202210179161 A CN202210179161 A CN 202210179161A CN 114471391 A CN114471391 A CN 114471391A
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Abstract
The invention discloses a self-lubricating PI microcapsule and a preparation method thereof, belonging to the technical field of lubricating materials, wherein the self-lubricating PI microcapsule comprises a water phase and an organic phase, and the volume ratio of the organic phase to the water phase is 1:3-5: 1; mixing a surfactant with water to obtain a water phase; adding polyimide resin and a liquid lubricating material into a volatile organic solvent to be mixed to obtain an organic phase; mixing the water phase and the organic phase, and stirring to obtain oil-in-water emulsion; mixing the oil-in-water emulsion in the presence of a stabilizer, heating, filtering, washing and drying to obtain a self-lubricating PI microcapsule water phase comprising a surfactant and water. The invention adopts the self-lubricating PI microcapsule and the preparation method thereof, overcomes the defect that the traditional self-lubricating PI microcapsule can not be used for preparing self-lubricating composite materials by injection molding, thermal spraying, medium-high temperature curing and other thermal forming processes, and the prepared microcapsule is ultrathin, good in compactness, good in mechanical strength and stability and uniform in particle size.
Description
Technical Field
The invention relates to the technical field of lubricating materials, in particular to a self-lubricating PI microcapsule and a preparation method thereof.
Background
Compared with metal, the polymer has lower friction coefficient and wear resistance, and has the advantages of light weight, easy manufacture, excellent specific strength, corrosion resistance, design flexibility and the like, so that the polymer becomes a key engineering material. However, the tribological properties of polymers are strongly influenced by their working environment and by lubricating fillers. The lubricant microencapsulated composite polymer is an effective way for preparing high-performance lubricating materials. Microcapsules are small spheres whose core material is called the core material and whose shell, consisting of a lipid or polymer, is called the wall material. When the microcapsule core material is required to play a role, a certain external force is only required to be applied to the microcapsule or the wall material is damaged by methods of increasing the temperature, ultraviolet rays and the like, so that the core material leaks to the outside to play the due role. The wall materials of the traditional microcapsules are generally epoxy resin, polystyrene, phenolic resin, urea resin and the like, and the microcapsules are damaged due to lower glass transition temperature and melting point of the wall materials when the self-lubricating composite material is prepared from the polymer base materials through thermal forming processes such as injection molding, thermal spraying, medium-high temperature curing and the like, so that the practical application of the microcapsule self-lubricating composite material is limited.
In the traditional solution, researchers mostly directly replace organic wall materials with inorganic wall materials to improve the temperature resistance of the microcapsules, but most of polymer matrixes are organic materials such as epoxy resin, polyurethane, polyimide and the like, and the inorganic wall microcapsules and the polymer matrixes have the problems of interface combination and organic-inorganic compatibility, so that the expected effect cannot be achieved, the microcapsules are agglomerated in the matrixes, and the self-repairing/lubricating performance of the composite material is greatly influenced. Therefore, it is necessary to develop an organic shell microcapsule which can withstand the thermoforming process and form a good force with the polymer matrix.
Disclosure of Invention
The invention aims to provide a self-lubricating PI microcapsule and a preparation method thereof, which overcome the defect that the traditional self-lubricating PI microcapsule can not be used for preparing self-lubricating composite materials through injection molding, thermal spraying, medium-high temperature curing and other thermal forming processes, and the prepared microcapsule is ultrathin, good in compactness, good in mechanical strength and stability and uniform in particle size.
In order to achieve the aim, the invention provides a self-lubricating PI microcapsule, which comprises an aqueous phase and an organic phase, wherein the volume ratio of the organic phase to the aqueous phase is 1:3-5: 1;
the aqueous phase includes a surfactant and water, and the organic phase includes a polyimide resin, a liquid lubricant, and a volatile organic solvent.
Preferably, the addition amount of the surfactant is 0.1-10 wt% of the total mass of the water phase.
Preferably, the surfactant is one or a mixture of sodium dodecyl sulfate, sodium fatty alcohol-polyoxyethylene ether sulfate, sodium lauryl sulfate, lauroyl glutamic acid and sodium dioctyl sulfosuccinate.
Preferably, the liquid lubricating material is any one or combination of more of fully synthetic lubricating oil, liquid paraffin, dimethyl silicone oil and 1-butyl-3-methylimidazolium hexafluorophosphate.
Preferably, the volatile organic solvent is one or a combination of acetone, N-dimethyl pyrrolidone, dichloromethane, ethyl acetate or petroleum ether.
A preparation method of a self-lubricating PI microcapsule comprises the following steps:
s1, preparing a water phase: mixing a surfactant with water to obtain a water phase;
s2, preparing an organic phase: adding polyimide resin and a liquid lubricating material into a volatile organic solvent to be mixed to obtain an organic phase;
s3, preparing oil-in-water emulsion: mixing the water phase and the organic phase, and stirring to obtain oil-in-water emulsion;
s4, preparing self-lubricating PI microcapsules: and mixing and heating the oil-in-water emulsion in the presence of a stabilizer, filtering, washing and drying to obtain the self-lubricating PI microcapsule.
Preferably, the particle size of the self-lubricating PI microcapsule is 5-25 μm.
Preferably, the mass ratio of the liquid lubricating material to the water phase added in the step S2 is 1:3-1: 8.
Preferably, the stirring speed in step S3 is 500 rpm.
Preferably, the drying in step S4 is drying or freeze drying.
Therefore, the self-lubricating PI microcapsule and the preparation method thereof have the following beneficial effects:
(1) the obtained microcapsule has excellent high temperature resistance, can be used for preparing a self-lubricating composite material with a polymer matrix through injection molding, thermal spraying, medium-high temperature curing and other thermal forming processes, can be used in a harsher environment, and widens the application range of the organic wall material microcapsule;
(2) the method adopts a solvent volatilization one-step method, has simple and convenient process, better controllability and simple post-treatment procedure, optimizes the performance and reduces the production cost at the same time.
The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
Drawings
FIG. 1 is a flow chart of the present invention for preparing self-lubricating PI microcapsules;
FIG. 2 is the relationship between the decomposition rate and the pH value of the self-lubricating PI microcapsule prepared by the present invention.
Detailed Description
FIG. 1 is a flow chart of the present invention for preparing self-lubricating PI microcapsules, wherein the present invention provides a self-lubricating PI microcapsule, which comprises an aqueous phase and an organic phase, wherein the volume ratio of the organic phase to the aqueous phase is 1:3-5: 1; the aqueous phase includes a surfactant and water, and the organic phase includes a polyimide resin, a liquid lubricant, and a volatile organic solvent. The addition amount of the surfactant is 0.1-10 wt% of the total mass of the water phase. The surfactant is one or more of sodium dodecyl sulfate, sodium fatty alcohol polyoxyethylene ether sulfate, sodium lauryl sulfate, lauroyl glutamic acid, and sodium dioctyl sulfosuccinate.
The liquid lubricating material is any one or combination of a plurality of fully synthetic lubricating oil, liquid paraffin, dimethyl silicone oil and 1-butyl-3-methylimidazole hexafluorophosphate.
The volatile organic solvent is one or more of acetone, N-dimethyl pyrrolidone, dichloromethane, ethyl acetate or petroleum ether.
A preparation method of a self-lubricating PI microcapsule comprises the following steps:
s1, preparing a water phase: mixing a surfactant with water to obtain a water phase;
s2, preparing an organic phase: adding polyimide resin and a liquid lubricating material into a volatile organic solvent, and mixing to obtain an organic phase, wherein the mass ratio of the liquid lubricating material to the water phase is 1:3-1: 8;
s3, preparing oil-in-water emulsion: mixing the water phase and the organic phase, and stirring to obtain an oil-in-water emulsion, wherein the stirring speed is 500 rpm;
s4, preparing self-lubricating PI microcapsules: mixing the oil-in-water emulsion in the presence of a stabilizer, heating, filtering, washing, and drying or freeze-drying to obtain the self-lubricating PI microcapsule.
The raw materials used in the examples of the present invention: sodium dodecyl sulfate, chemical reagent field in north of the Yangtze river of Wuhan city; sodium fatty alcohol-polyoxyethylene ether sulfate, Zibo Hailai Jingmao Co., Ltd; lauroyl glutamic acid, Chongqing Saponas science and technology Limited; lauroyl glutamic acid, dioctyl sodium sulfosuccinate, Yonghui Zhi science and technology trade, Inc., of Foshan; fully synthetic lubricating oil, liquid paraffin, tokyo chemical industry co; dimethicone, jinning hengtai chemical ltd; 1-butyl-3-methylimidazolium hexafluorophosphate, a commercially available Hongsheng fine chemical industry Co., Ltd; acetone, N-dimethylpyrrolidone, dichloromethane, ethyl acetate, petroleum ether, zhengzhou Dragon chemical trade company Limited.
The apparatus used in this example: a multifunctional stirrer, model D-8401, Waxing scientific Instrument factory, Tianjin; super constant temperature water bath, model SYC-15B, south beijing sangli electronics plant.
The technical solution of the present invention is further illustrated by the accompanying drawings and examples.
Example 1
A preparation method of a self-lubricating PI microcapsule comprises the following steps:
2g of the polyimide resin and 10g of liquid paraffin were placed in a beaker, and 40mL of acetone was poured into the beaker to dissolve the resin, thereby obtaining an organic phase.
2g of sodium dodecylsulfate was added to 100mL of water and completely dissolved to obtain an aqueous phase.
The organic phase was transferred to a four-necked flask, the aqueous phase was added with mechanical stirring at 500rpm, and heated for 4 hours while maintaining a weakly alkaline environment of the mixed emulsion with a stabilizer. And filtering the reacted solution, washing the obtained solid sample, and drying to obtain the self-lubricating PI microcapsule.
Example 2
2g of the polyimide resin and 6g of liquid paraffin were placed in a beaker, and 40mL of acetone was poured into the beaker to dissolve the resin, thereby obtaining an organic phase.
10g of sodium dodecylsulfate was added to 100mL of water and completely dissolved to obtain an aqueous phase.
The organic phase was transferred to a four-necked flask, the aqueous phase was added with mechanical stirring at 500rpm, and heated for 4 hours while maintaining a weakly alkaline environment of the mixed emulsion with a stabilizer. And filtering the reacted solution, washing the obtained solid sample, and drying to obtain the self-lubricating PI microcapsule.
In conclusion, the particle size of the self-lubricating PI microcapsule is 5-25 μm by scanning of a laser particle size analyzer; according to the TGA test, the initial decomposition temperature of the microcapsule is 330.5 ℃, and the coating rate of the microcapsule is 92.1%; according to TEM scan test, the average wall thickness of the microcapsules is 1.3 μm; according to the atomic force microscope test, the average value of the elastic modulus of the microcapsule is 0.81 +/-0.02 GPa; this type of microcapsules has proven to have good applications under neutral and alkaline conditions by testing the relationship between the rate of decomposition and the PH (figure 2).
Therefore, the self-lubricating PI microcapsule and the preparation method thereof solve the defect that the traditional self-lubricating PI microcapsule can not be used for preparing self-lubricating composite materials through injection molding, thermal spraying, medium-high temperature curing and other thermal forming processes, and the prepared microcapsule is ultrathin, good in compactness, good in mechanical strength and stability and uniform in particle size.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting the same, and although the present invention is described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that: modifications and equivalents may be made to the invention without departing from the spirit and scope of the invention.
Claims (10)
1. A self-lubricating PI microcapsule is characterized in that: comprises an aqueous phase and an organic phase, wherein the volume ratio of the organic phase to the aqueous phase is 1:3-5: 1;
the aqueous phase includes a surfactant and water, and the organic phase includes a polyimide resin, a liquid lubricant, and a volatile organic solvent.
2. The self-lubricating PI microcapsule of claim 1 and the preparation method thereof, wherein: the addition amount of the surfactant is 0.1-10 wt% of the total mass of the water phase.
3. A self-lubricating PI microcapsule according to claim 1, wherein: the surfactant is one or more of sodium dodecyl sulfate, sodium fatty alcohol-polyoxyethylene ether sulfate, sodium lauryl sulfate, lauroyl glutamic acid and sodium dioctyl sulfosuccinate.
4. A self-lubricating PI microcapsule according to claim 1, wherein: the liquid lubricating material is any one or combination of a plurality of fully synthetic lubricating oil, liquid paraffin, dimethyl silicone oil and 1-butyl-3-methylimidazole hexafluorophosphate.
5. A self-lubricating PI microcapsule according to claim 1, wherein: the volatile organic solvent is one or a combination of acetone, N-dimethyl pyrrolidone, dichloromethane, ethyl acetate or petroleum ether.
6. A process for the preparation of self-lubricating PI microcapsules according to any of claims 1 to 5 comprising the following steps:
s1, preparing a water phase: mixing a surfactant with water to obtain a water phase;
s2, preparing an organic phase: adding polyimide resin and a liquid lubricating material into a volatile organic solvent to be mixed to obtain an organic phase;
s3, preparing oil-in-water emulsion: mixing the water phase and the organic phase, and stirring to obtain oil-in-water emulsion;
s4, preparing self-lubricating PI microcapsules: and mixing and heating the oil-in-water emulsion in the presence of a stabilizer, filtering, washing and drying to obtain the self-lubricating PI microcapsule.
7. The method for preparing self-lubricating PI microcapsules of claim 6, wherein: the particle size of the self-lubricating PI microcapsule is 5-25 mu m.
8. The method for preparing self-lubricating PI microcapsules of claim 6, wherein: the mass ratio of the liquid lubricating material to the water phase added in the step S2 is 1:3-1: 8.
9. The method for preparing self-lubricating PI microcapsules of claim 6, wherein: the stirring speed in step S3 was 500 rpm.
10. The method for preparing self-lubricating PI microcapsules of claim 6, wherein: the drying in step S4 is drying or freeze drying.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115322569A (en) * | 2022-09-14 | 2022-11-11 | 明士新材料有限公司 | Polyimide film containing self-lubricating PI microcapsules and preparation method thereof |
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Cited By (1)
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| CN115322569A (en) * | 2022-09-14 | 2022-11-11 | 明士新材料有限公司 | Polyimide film containing self-lubricating PI microcapsules and preparation method thereof |
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