CN1982369A - Bi-maleimide self-lubricating nano-composite material and its production - Google Patents
Bi-maleimide self-lubricating nano-composite material and its production Download PDFInfo
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- CN1982369A CN1982369A CN 200510124559 CN200510124559A CN1982369A CN 1982369 A CN1982369 A CN 1982369A CN 200510124559 CN200510124559 CN 200510124559 CN 200510124559 A CN200510124559 A CN 200510124559A CN 1982369 A CN1982369 A CN 1982369A
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Abstract
A bimaleimide self-lubricating nano-compostie material and its production are disclosed. It consists of bimaleimide modified by diallyl bisphenol A, inorganic nanometer particle, coupling agent and carbon black. The process is carried out by adding coupling agent into acetone, adjusting pH value by acetic acid, hydrolyzing for coupling agent, adding it into solution of inorganic nanometer particle and carbon black, dispersing by ultrasonic wave, adding it into bimaleimide resin performed polymer, heating while agitating, distilling to remove acetone, pouring it into preheated mold, supplying pump to remove bubble, curing in oven, cooling to room-temperature and de-molding. It's simple and has no environmental pollution. It can be used for self-lubricating bearing, gear and compressor under high-temperature radiant environment.
Description
Technical field:
The present invention relates to a kind of bi-maleimide self-lubricating nano-composite material and preparation method thereof, belong to the manufacture field of polymkeric substance.
Background technology:
Organic-inorganic nanocomposite not only can have the characteristics and the character of inorganic materials, thermotolerance, high-temperature stability, low thermal coefficient of expansion as inorganic materials, and can be with the toughness of organic polymer, ductility with workability, therefore, nanometer particle-modified polymkeric substance becomes the focus of Materials science research.At present, the research of nano material transforms to the practical application direction of material from basic research work such as the preparation of material, sign, fundamental property analyses.
The character of matrix material is not only relevant with the character of each component, and is closely related with mutually form and interfacial property.For organic-inorganic nanocomposite, because organic constituent and inorganic component are the easy agglomeration of inconsistent and nanoparticle on thermodynamics, be unfavorable for the dispersion of inorganic particulate in organic matrix, be undoubtedly a very adverse factors for the preparation organic-inorganic nanocomposite.Therefore, prepare organic-inorganic nanocomposite, improve two alternate consistencies and seem particularly important with superperformance.Chinese patent CN1227234A has reported that original position generates the method that nano zirconium dioxide prepares organic-inorganic nanocomposite in the suspension system of polymer beads; Chinese patent CN1414037A adds the preparation method of nano-silicon nitride, nano silicon and carbon nanotube in the performed polymer of ANALYSIS OF MOLDABLE POLYIMIDES in the presence of coupling agent γ-(methacryloxypropyl) propyl trimethoxy silicane.We had once reported that the method for utilizing high speed shear and ultrasonic dispersing prepared the bismaleimides nano composite material on " tribology journal " (the 6th phase of calendar year 2001), but, influenced the tribological property of material owing to the reason nanoparticle dispersing uniformity therein of system is not fine.
Summary of the invention:
The technical problem that solves:
For fear of the deficiencies in the prior art part, the present invention proposes a kind of bi-maleimide self-lubricating nano-composite material and preparation method thereof, handle nanoparticle with amino silicane coupling agent, and suppress the sedimentation of nanoparticle in system by the generation of compound system viscosity change and resin network structure, thereby improve the dispersion state of nanoparticle in bimaleimide resin, to improve its tribological property.
Technical scheme:
Technical characterictic of the present invention is: mass fraction is made up of for 0.5～15 part 0.1～2 part of 0.5～15 part of 100 parts of bimaleimide resins, inorganic nano-particle, coupling agent and the carbon black of diallyl bisphenol modification.
Described nanoparticle is: in silicon nitride, silicon carbide, silicon-dioxide, the carbon black a kind of, two kinds, three kinds or four kinds.
Described coupling agent: γ-An Bingjisanyiyangjiguiwan, or N-β (aminoethyl)-γ-An Bingjisanjiayangjiguiwan, or N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane.
A kind of method for preparing above-mentioned materials, it is characterized in that: preparation process is as follows:
A: at first coupling agent is joined in the acetone, transfer pH value, make the coupling agent hydrolysis with acetate;
B: nanoparticle is contained in the acetone soln of coupling agent by the massfraction adding, utilized ultrasonic dispersing 10～30 minutes;
C: it is added in the performed polymer of bismaleimides, utilize the high speed homogenization stirrer to be uniformly dispersed after, join in the there-necked flask, heated and stirred, acetone is wherein removed in distillation;
D: after treating that acetone evaporated is intact, pour in the good mould of preheating, vacuumize remove bubble after, put into baking oven and be cured;
E: at last 250 ℃ of following aftertreatments 4～6 hours.
The performed polymer of described bismaleimides is by the bismaleimides of 3: 4 diallyl bisphenol modification, is prepared from by the heating and melting method.
Described curing process is: 150 ℃ solidified 2 hours, and 180 ℃ solidified 2 hours, and 220 ℃ solidified 4 hours.
Beneficial effect:
The present invention's amino silicane coupling agent solution-treated nanoparticle, drying-free is handled, and has avoided nanoparticle because of the mutual phenomenon that firmly condenses in together of the bonding effect of coupling agent, has improved the dispersiveness of nanoparticle in organic matrix.
The present invention will directly join through the acetone suspension of the nanoparticle that amino silicane coupling agent is handled in the bimaleimide resin performed polymer, and acetone can reduce the viscosity of system therein at the beginning, helps the dispersion of nanoparticle; Along with the thermal distillation that adds of acetone, the viscosity of system is increasing, and the network structure of bimaleimide resin also generating, has prevented the sedimentation of nanoparticle, can obtain the finely dispersed bi-maleimide self-lubricating nano-composite material of nanoparticle.In addition, acetone solvent adopts distillation to reclaim, and has both improved the utilization ratio of acetone, has avoided the pollution of environment again.
The present invention adds the size that coupling agent not only can significantly reduce disperse phase in bi-maleimide self-lubricating nano-composite material system, can also increase the alternate consistency of organic and inorganic two, two alternate interfaces bonding degree of improvement.Therefore, except improving the wear resistant friction reducing of bimaleimide resin, also can improve the mechanical property of bimaleimide resin, thermotolerance is also suitably improved.
Bi-maleimide self-lubricating nano-composite material of the present invention can use under particular surroundingss such as vacuum, radiation, high temperature, is suitable as self-oiling bearing, the gear in fields such as aerospace, chemical machinery, vehicle appliance, the component such as slide plate of compressor.
Preparation method of the present invention has characteristics such as operating procedure is simple, pollution-free, is the wide method for preparing organic-inorganic nanocomposite of a kind of suitability.
Description of drawings:
Fig. 1: be technological process of production figure of the present invention
Embodiment:
Now in conjunction with the accompanying drawings the present invention is further described:
Embodiment 1:
0.5 part of coupling agent γ-An Bingjisanyiyangjiguiwan is joined in the acetone, transfer pH value with acetate, after treating the γ-An Bingjisanyiyangjiguiwan hydrolysis, 2 parts of nano-silicon nitrides, 1 part nano silicon and 1 part of carbon black added contain in the acetone soln of coupling agent, utilized ultrasonic dispersing 15 minutes.Then it is joined in 100 parts the performed polymer of bimaleimide resin, utilize high speed homogenization stirrer heated and stirred 15 minutes, join in the there-necked flask, heated and stirred 30 minutes, wherein acetone is removed in distillation, treat that acetone evaporated is intact after, pour in the good mould of preheating, vacuumize remove bubble after, put into baking oven and be cured.Curing process is: after solidifying 2 hours under 150 ℃, be warming up to 180 ℃ and solidified 2 hours, be warming up to 220 ℃ again and solidify after 4 hours.After naturally cooling to the room temperature demoulding, at last 250 ℃ of following aftertreatments 4 hours.Promptly get bi-maleimide self-lubricating nano-composite material.
Embodiment 2:
0.3 part of coupling agent N-β (aminoethyl)-γ-An Bingjisanjiayangjiguiwan is joined in the acetone, transfer pH value with acetate, after treating the coupling agent hydrolysis, 2 parts of nano-silicon nitrides, 2 parts nano silicon are joined in the acetone soln that contains coupling agent, utilized ultrasonic dispersing 20 minutes.Then it is joined in 100 parts the performed polymer of bimaleimide resin, utilize high speed homogenization stirrer heated and stirred 20 minutes, join in the there-necked flask, heated and stirred 40 minutes, wherein acetone is removed in distillation, treat that acetone evaporated is intact after, pour in the good mould of preheating, vacuumize remove bubble after, put into baking oven and be cured.Curing process is: after solidifying 2 hours under 150 ℃, be warming up to 180 ℃ and solidified 2 hours, be warming up to 220 ℃ again and solidify after 4 hours.After naturally cooling to the room temperature demoulding, at last 250 ℃ of following aftertreatments 5 hours.Promptly get bi-maleimide self-lubricating nano-composite material.
Embodiment 3:
0.2 part of coupling agent N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane is joined in the acetone, transfer pH value with acetate, after treating the coupling agent hydrolysis, 1 part of nanometer silicon carbide, 2 parts nano silicon and 1 part of carbon black added contain in the acetone soln of coupling agent, utilized ultrasonic dispersing 18 minutes.Then it is joined in 100 parts the performed polymer of bimaleimide resin, utilize high speed homogenization stirrer heated and stirred 18 minutes, join in the there-necked flask, heated and stirred 40 minutes, wherein acetone is removed in distillation, treat that acetone evaporated is intact after, pour in the good mould of preheating, vacuumize remove bubble after, put into baking oven and be cured.After solidifying 2 hours under 150 ℃, be warming up to 180 ℃ and solidified 2 hours, be warming up to 220 ℃ again and solidify after 4 hours.After naturally cooling to the room temperature demoulding, at last 250 ℃ of following aftertreatments 6 hours.Promptly get bi-maleimide self-lubricating nano-composite material.
The performed polymer of the bismaleimides of the foregoing description is by the bismaleimides of 3: 4 diallyl bisphenol modification, is prepared from by the heating and melting method.
The present invention handles nanoparticle with the acetone soln of amino silicane coupling agent, directly joins in the bimaleimide resin performed polymer, and drying-free is handled, and has avoided nanoparticle because of the mutual phenomenon that firmly condenses in together of the bonding effect of coupling agent.Utilize the method for distilling acetone to change the viscosity of system, to be encapsulated in uniformly through the nanoparticle of coupling agent treatment in the network structure of bimaleimide resin, prevent the sedimentation of nanoparticle, improved dispersiveness and the two alternate consistencies of nanoparticle in organic matrix.Reclaim acetone simultaneously, avoided environmental pollution.Simple, the pollution-free and nanoparticle of this preparation method's operating procedure is uniformly dispersed, this matrix material can use under particular surroundingss such as vacuum, radiation, high temperature, is suitable as self-oiling bearing, the gear in fields such as aerospace, chemical machinery, vehicle appliance, the component such as slide plate of compressor.
The performance index of bi-maleimide self-lubricating nano-composite material of the present invention are as follows:
1. outward appearance: no significant defect
2. density:＜2.5g/cm
2
3. flexural strength:＞120Mpa
4. shock strength:＞12KJ/m
2
5. cloth the hardness:＞27kg/mm that continues
2
6. frictional coefficient:＜0.25 (GB3960-83)
7. abrasion resistance:＜2.0 * 10
-6Mm
3/ (Nm) (GB3960-83)
8. heat-drawn wire:＞270 ℃
Claims (6)
1, a kind of bi-maleimide self-lubricating nano-composite material is characterized in that: mass fraction is made up of for 0.5～15 part 0.1～2 part of 0.5～15 part of 100 parts of bimaleimide resins, inorganic nano-particle, coupling agent and the carbon black of diallyl bisphenol modification.
2, bi-maleimide self-lubricating nano-composite material according to claim 1 is characterized in that: described nanoparticle is: in silicon nitride, silicon carbide, silicon-dioxide, the carbon black a kind of, two kinds, three kinds or four kinds.
3, bi-maleimide self-lubricating nano-composite material according to claim 1, it is characterized in that: described coupling agent: γ-An Bingjisanyiyangjiguiwan, or N-β (aminoethyl)-γ-An Bingjisanjiayangjiguiwan, or N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane.
4, a kind of method for preparing above-mentioned materials, it is characterized in that: preparation process is as follows:
A: at first coupling agent is joined in the acetone, transfer pH value, make the coupling agent hydrolysis with acetate;
B: nanoparticle is contained in the acetone soln of coupling agent by the massfraction adding, utilized ultrasonic dispersing 10～30 minutes;
C: it is added in the performed polymer of bismaleimides, utilize the high speed homogenization stirrer to be uniformly dispersed after, join in the there-necked flask, heated and stirred, acetone is wherein removed in distillation;
D: after treating that acetone evaporated is intact, pour in the good mould of preheating, vacuumize remove bubble after, put into baking oven and be cured;
E: at last 250 ℃ of following aftertreatments 4～6 hours.
5, preparation method according to claim 4 is characterized in that: the performed polymer of described bismaleimides is by the bismaleimides of 3: 4 diallyl bisphenol modification, is prepared from by the heating and melting method.
6, preparation method according to claim 4 is characterized in that: described curing process is: 150 ℃ solidified 2 hours, and 180 ℃ solidified 2 hours, and 220 ℃ solidified 4 hours.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005101245596A CN100480323C (en) | 2005-12-16 | 2005-12-16 | Bi-maleimide self-lubricating nano-composite material and preparing method thereof |
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| CNB2005101245596A CN100480323C (en) | 2005-12-16 | 2005-12-16 | Bi-maleimide self-lubricating nano-composite material and preparing method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103172862A (en) * | 2013-03-28 | 2013-06-26 | 西北工业大学 | Nano-filler bismaleimide resin and preparation method thereof |
| CN103193990A (en) * | 2013-04-03 | 2013-07-10 | 中国航空工业集团公司北京航空材料研究院 | Method for eliminating surface crust during curing of bismaleimide resin and resin complex |
| CN103881379A (en) * | 2014-03-20 | 2014-06-25 | 西北工业大学 | Hydroxyl silicate/phosphorus-containing benzoxazine/bismaleimide resin composite material and preparation method thereof |
| CN103881564A (en) * | 2014-03-31 | 2014-06-25 | 嘉善友力轴承有限公司 | Method for preparing swash plate based on bismaleimide |
| CN103881565A (en) * | 2014-03-31 | 2014-06-25 | 嘉善友力轴承有限公司 | Swash plate based on bismaleimide |
| CN113755226A (en) * | 2021-10-21 | 2021-12-07 | 华亿金卫(杭州)能源有限公司 | Oil-soluble organic zirconium friction reducer and preparation method thereof |
-
2005
- 2005-12-16 CN CNB2005101245596A patent/CN100480323C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103172862A (en) * | 2013-03-28 | 2013-06-26 | 西北工业大学 | Nano-filler bismaleimide resin and preparation method thereof |
| CN103193990A (en) * | 2013-04-03 | 2013-07-10 | 中国航空工业集团公司北京航空材料研究院 | Method for eliminating surface crust during curing of bismaleimide resin and resin complex |
| CN103193990B (en) * | 2013-04-03 | 2015-09-02 | 中国航空工业集团公司北京航空材料研究院 | A kind of method and resin complexes eliminating surface skining when bismaleimide resin solidifies |
| CN103881379A (en) * | 2014-03-20 | 2014-06-25 | 西北工业大学 | Hydroxyl silicate/phosphorus-containing benzoxazine/bismaleimide resin composite material and preparation method thereof |
| CN103881379B (en) * | 2014-03-20 | 2016-05-18 | 西北工业大学 | Hydroxy silicate/phosphorous benzoxazine/bismaleimide resin composite material and preparation method thereof |
| CN103881564A (en) * | 2014-03-31 | 2014-06-25 | 嘉善友力轴承有限公司 | Method for preparing swash plate based on bismaleimide |
| CN103881565A (en) * | 2014-03-31 | 2014-06-25 | 嘉善友力轴承有限公司 | Swash plate based on bismaleimide |
| CN103881564B (en) * | 2014-03-31 | 2016-10-05 | 嘉善友力轴承有限公司 | A kind of preparation method of swash plate based on BMI |
| CN103881565B (en) * | 2014-03-31 | 2016-10-05 | 嘉善友力轴承有限公司 | A kind of swash plate based on BMI |
| CN113755226A (en) * | 2021-10-21 | 2021-12-07 | 华亿金卫(杭州)能源有限公司 | Oil-soluble organic zirconium friction reducer and preparation method thereof |
| CN113755226B (en) * | 2021-10-21 | 2022-04-29 | 华亿金卫(杭州)能源有限公司 | Oil-soluble organic zirconium friction reducer and preparation method thereof |
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|---|---|
| CN100480323C (en) | 2009-04-22 |
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