CN102911345A - Preparation method and application of epoxy resin adhesive - Google Patents
Preparation method and application of epoxy resin adhesive Download PDFInfo
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- CN102911345A CN102911345A CN2012103990752A CN201210399075A CN102911345A CN 102911345 A CN102911345 A CN 102911345A CN 2012103990752 A CN2012103990752 A CN 2012103990752A CN 201210399075 A CN201210399075 A CN 201210399075A CN 102911345 A CN102911345 A CN 102911345A
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Abstract
The invention provides a preparation method of an epoxy resin adhesive. The method comprises the following steps of: mixing bismaleimide with allyl-containing phenol, carrying out a first reaction to obtain polybismaleimide; and mixing the polybismaleimide with an epoxy resin, heating, adding an accelerant after a second reaction to obtain the epoxy resin adhesive. The invention also provides application of the prepared epoxy resin adhesive in an insufficient glue mica tape. The polybismaleimide containing active groups is reacted with the epoxy resin, and because active hydrogen is contained in the polybismaleimide molecular chain and can carry out a cross-linking reaction with an impregnating varnish material, the insufficient glue mica tape compounded by the epoxy resin adhesive has high compatibility with an impregnating resin, and an insulating structure system with a good impregnating effect is obtained.
Description
Technical field
The present invention relates to the insulating material technical field, relate in particular to preparation method and the application of epoxyn.
Background technology
The 200 class B insulation structures that at present domestic and international traction electric machine all adopts, 200 class B insulation structures mainly are divided into organic silicon insulation system and epoxy anhydride insulation system two large classes.The organic silicon insulation system is as impreg take the organosilicon solvent-free solvent impregnated resin, the major insulation that matches with it is to adopt the organosilicon low resin mica tape that is composited with uncatalyzed organic silicon adhesive, mica material and supporting material, this insulation system adopts similar organosilicon solvent impregnated resin and the organic silicon adhesive of molecular structure, can obtain whole good insulation system without air cleft after bi-material is processed through vacuum impregnation.Structural similitude principle of design based on solvent impregnated resin and mica tape adhesive, for the epoxy anhydride insulation system, as impreg, the major insulation material that matches with it is the Resins, epoxy low resin mica tape that epoxyn, mica material and the Kapton with semicure is composited with the epoxy anhydride impregnating varnish.Yet the pure epoxy resin solidification brittleness is large, and snappiness is poor, and is easy to crack, and resistance toheat only can reach the F level.Simultaneously, the pure epoxy resin low resin mica tape is easily anti-sticking, and after compound with impregnating varnish, performance is not good.Therefore, the investigator improves the major insulation material in the epoxy anhydride insulation system.
For example: publication number is that the Chinese patent of CN200910301153.9 has been reported a kind of oxatyl-containing lateral group polyarylether cured modified epoxy resin composition and preparation method thereof, its polyarylether that will contain carboxyl side group is incorporated in the Resins, epoxy molecular chain, it can effectively improve the toughness of Resins, epoxy, improves thermotolerance and insulating property.Publication number is that the CN201010135384.X Chinese patent discloses epoxy-terminated silicone oil pre-reaction thing modified epoxy resin composite and preparation and application, this patent adopts the silicone oil performed polymer modified epoxy resin take end group as epoxide group, and toughness and the thermostability of matrix material are improved.Publication number is that the Chinese patent of CN200710072800.4 has been reported the moisture-heat-proof epoxy stick, this patent prepares tackiness agent take solid-state fluorenyl Resins, epoxy and resol, bisphenol a resin as matrix resin, this tackiness agent has good resistance to elevated temperatures, its shear at high temperature strength ratio routine or modified epoxide resin adhesive are high, and water-intake rate is significantly less than conventional Resins, epoxy.Hence one can see that, and aspect the fragility and resistance toheat that solve Resins, epoxy, domestic investigator has obtained certain achievement, but the consistency of low resin mica tape epoxyn and epoxy anhydride solvent-free impregnating resin or relatively poor.
Summary of the invention
The technical problem that the present invention solves is preparation method and the application of epoxyn, the epoxyn of the present invention's preparation when being applied to low resin mica tape and the consistency of epoxy anhydride solvent impregnated resin better.
In view of this, the invention provides a kind of preparation method of epoxyn, may further comprise the steps:
With bismaleimides with contain allylic phenol and mix, obtain polybismaleimide behind the first set reaction;
Described polybismaleimide is mixed with Resins, epoxy, and heating adds promotor after the reaction for the second time, obtains epoxyn.
Preferably, described bismaleimides is N, a N ＇-penylene bismaleimides, N, N,-4,4, one or more in-diphenyl methane dimaleimide, dihydroxyphenyl propane Diphenyl Ether Bismaleimide, Bisphenol F Diphenyl Ether Bismaleimide, phenolphthalein Diphenyl Ether Bismaleimide, thymolphthalein Diphenyl Ether Bismaleimide, thymolsulfonphthalein Diphenyl Ether Bismaleimide, o-cresolphthalein Diphenyl Ether Bismaleimide, 1-naphtholphthalein Diphenyl Ether Bismaleimide and the thymolphthalein Diphenyl Ether Bismaleimide.
It is preferably, described that to contain allylic phenol be diallyl bisphenol.
Preferably, the step that obtains polybismaleimide is specially:
Lower the temperature after bismaleimides is heated to 170 ~ 200 ℃, add after temperature is down to 130 ~ 140 ℃ and contain allylic phenol, obtain polybismaleimide behind the first set reaction.
Preferably, the time of described first set reaction is 1 ~ 2h.
Preferably, described promotor is one or more of acetylacetone copper, zinc acetylacetonate, chromium acetylacetonate, acetylacetone cobalt, zinc naphthenate, aluminium acetylacetonate, 1-benzyl-2-ethyl imidazol(e), glyoxal ethyline, 2-ethyl-4-methylimidazole and 1-cyanoethyl substituted imidazole.
Preferably, the step that obtains epoxy adhesive is specially:
Described polybismaleimide is mixed with Resins, epoxy, be heated to 140 ~ 150 ℃, carry out reducing temperature after the reaction second time, temperature is added promotor after being down to 40 ~ 60 ℃, obtains epoxyn.
Preferably, the mass ratio of described Resins, epoxy, polybismaleimide and promotor is (90 ~ 110): (50 ~ 100): (0.1 ~ 5).
Preferably, described bismaleimides and the described quality that contains allylic phenol are (50 ~ 100): (25 ~ 50).
The present invention also provides the application of described epoxyn in low resin mica tape.
The invention provides a kind of preparation method of epoxyn, in the process of preparation epoxyn, at first synthesize polybismaleimide, then with described polybismaleimide and Resins, epoxy reaction, obtained the epoxyn of polybismaleimide grafting.The present invention contains polybismaleimide and the Resins, epoxy reaction of active group by employing, owing to containing active hydrogen in the polybismaleimide molecular chain of epoxyn, its can with impregnating varnish material generation crosslinking reaction, have preferably consistency thereby make by epoxyn compound low resin mica tape and solvent impregnated resin, obtain preferably insulation system system of dipping effect.Secondly, the present invention has introduced the maleimide base group of excellent heat resistance in Resins, epoxy, not only improved the resistance toheat of Resins, epoxy, and has increased the molecular weight of Resins, epoxy and improved the softening temperature of resin.
Embodiment
In order further to understand the present invention, below in conjunction with embodiment the preferred embodiment of the invention is described, but should be appreciated that these describe just as further specifying the features and advantages of the present invention, rather than to the restriction of claim of the present invention.
The embodiment of the invention discloses a kind of preparation method of epoxyn, may further comprise the steps:
With bismaleimides with contain allylic phenol and mix, obtain polybismaleimide behind the first set reaction;
Described polybismaleimide is mixed with Resins, epoxy, and heating adds promotor after the reaction for the second time, obtains epoxyn.
According to the present invention, in the process of preparation epoxyn, at first synthesized polybismaleimide.The present invention with bismaleimides with contain allylic phenol and mix, obtain polybismaleimide behind the first set reaction, described bismaleimides is preferably N, a N ＇-penylene bismaleimides, N, N,-4,4,-diphenyl methane dimaleimide, the dihydroxyphenyl propane Diphenyl Ether Bismaleimide, the Bisphenol F Diphenyl Ether Bismaleimide, the phenolphthalein Diphenyl Ether Bismaleimide, the thymolphthalein Diphenyl Ether Bismaleimide, the thymolsulfonphthalein Diphenyl Ether Bismaleimide, the o-cresolphthalein Diphenyl Ether Bismaleimide, in 1-naphtholphthalein Diphenyl Ether Bismaleimide and the thymolphthalein Diphenyl Ether Bismaleimide one or more, N more preferably, N,-4,4 ,-diphenyl methane dimaleimide, the dihydroxyphenyl propane Diphenyl Ether Bismaleimide, the phenolphthalein Diphenyl Ether Bismaleimide, the Bisphenol F Diphenyl Ether Bismaleimide, the thymolphthalein Diphenyl Ether Bismaleimide, the thymolsulfonphthalein Diphenyl Ether Bismaleimide, in o-cresolphthalein Diphenyl Ether Bismaleimide and the 1-naphtholphthalein Diphenyl Ether Bismaleimide one or more.Describedly contain allylic phenol and be preferably diallyl bisphenol.The preparation method of described polybismaleimide, specifically by the following method preparation:
In reactor, add bismaleimides, be warming up to 170 ~ 200 ℃, lower the temperature after being stirred to molten state, add after temperature is down to 130 ~ 140 ℃ and contain allylic phenol, obtain polybismaleimide behind the first set reaction.
In the process of preparation polybismaleimide, the time of described first set reaction is preferably 1 ~ 2h.Described bismaleimides and the described mass ratio that contains allylic phenol are preferably (50 ~ 100): (25 ~ 50), more preferably (65 ~ 95): (30 ~ 45).
After polybismaleimide preparation finished, then polybismaleimide and the Resins, epoxy with preparation reacted, and makes polybismaleimide graft modification Resins, epoxy, thereby obtains epoxyn.The preparation process of described epoxyn is specially:
Described polybismaleimide is mixed with Resins, epoxy, be heated to 140 ~ 150 ℃, reduce temperature after carrying out reacting 2 ~ 3h the second time, temperature is added promotor after being down to 40 ~ 50 ℃, obtains epoxyn.
According to the present invention, the quality optimization of described polybismaleimide, Resins, epoxy and described promotor is (50 ~ 100): (90 ~ 110): (0.1 ~ 5), more preferably 80:100:(0.5 ~ 5).As preferred version, the present invention has preferably added promotor at 40 ~ 50 ℃, catalyzer when described promotor is solidified as epoxyn, preferably 40 ~ 60 ℃ of addings, can avoid the tackiness agent premature setting, if and be higher than 60 ℃, promotor can cause the tackiness agent hardening, thereby mica tape can't be used.Described Resins, epoxy is preferably one or more in bisphenol A epoxide resin, bisphenol F epoxy resin, cycloaliphatic epoxy resin, bisphenol-s epoxy resin and the novolac epoxy.Described promotor is preferably one or more of acetylacetone copper, zinc acetylacetonate, chromium acetylacetonate, acetylacetone cobalt, zinc naphthenate, aluminium acetylacetonate, 1-benzyl-2-ethyl imidazol(e), glyoxal ethyline, 2-ethyl-4-methylimidazole and 1-cyanoethyl substituted imidazole, more preferably one or more in chromium acetylacetonate, zinc naphthenate, glyoxal ethyline, acetylacetone copper, zinc acetylacetonate, chromium acetylacetonate and the acetylacetone cobalt.
The present invention also provides a kind of purposes of epoxyn, and the epoxyn that the present invention is prepared is used for low resin mica tape.Above-mentioned low resin mica tape and impregnating varnish resin have preferably consistency, can access the insulation system of good integrity.According to the present invention, for the preparation of low resin mica tape, preparation method the present invention of described low resin mica tape has no particular limits, for mode well known to those skilled in the art gets final product with the epoxyn of the present invention preparation.
The present invention adopts the polybismaleimide and the Resins, epoxy reaction that contain active group in the process of preparation epoxyn, prepared a kind of polybismaleimide modified epoxide resin adhesive.By in Resins, epoxy, having introduced the maleimide base group of Good Heat-resistance, not only improved the resistance toheat of Resins, epoxy, and increased molecular weight of epoxy resin and improved the softening temperature of numerical value, improved the performance of Resins, epoxy self.On the other hand, contain active hydrogen in the poly maleimide molecular chain, its can with impreg generation crosslinking reaction, thereby make low resin mica tape and impregnating varnish resin after compound have preferably consistency, obtain good integrity without the insulation system of air cleft by vacuum pressure impregnation.Secondly, owing to contain a certain amount of hydroxyl in the epoxyn, and hydroxyl can provide cohesiveness, so epoxyn can have higher cohesiveness with mica paper and Kapton.
In order further to understand the present invention, below in conjunction with embodiment the preparation method of epoxyn provided by the invention is elaborated, protection scope of the present invention is not limited by the following examples.
Embodiment 1
The N that in three mouthfuls of round-bottomed flasks of 500mL, adds 100 weight parts, N ,-4,4, then-diphenyl methane dimaleimide is warming up to 170 ℃ and is stirred to molten state, and the 130 ℃ of diallyl bisphenols that add 50 weight parts of then lowering the temperature were 130 ℃ of lower reactions 1 hour.Then the bisphenol A epoxide resin that adds 100 weight parts is warming up to 150 ℃ and continues reaction 2 hours, is cooled to 60 ℃ of chromium acetylacetonate promotor of adding 0.5 weight part, obtains modified epoxide resin adhesive.Experimental result shows, the temperature that the epoxyn thermolysis begins is 358 ℃.With the epoxyn of the present embodiment preparation for the preparation of low resin mica tape, the performance of test low resin mica tape, as shown in table 1.
Embodiment 2
The bismaleimides (dihydroxyphenyl propane Diphenyl Ether Bismaleimide, phenolphthalein Diphenyl Ether Bismaleimide mass ratio are 50:50) that in three mouthfuls of round-bottomed flasks of 500mL, adds 100 weight parts, then be warming up to 170 ℃ and be stirred to molten state, then lower the temperature 130 ℃ and add 100 parts of diallyl bisphenols, 130 ℃ of lower reactions 1 hour.Then the bisphenol F epoxy resin that adds 100 weight parts is warming up to 150 ℃ and continues reaction 2 hours, is cooled to 60 ℃ of zinc naphthenates that add 0.5 weight part and obtains modified epoxide resin adhesive.Experimental result shows, the temperature that the epoxyn thermolysis begins is 361 ℃.
Embodiment 3
In three mouthfuls of round-bottomed flasks of 500mL, add 100 parts of bismaleimidess (mass ratio of Bisphenol F Diphenyl Ether Bismaleimide, thymolphthalein Diphenyl Ether Bismaleimide, thymolsulfonphthalein Diphenyl Ether Bismaleimide is 40:30:30), then be warming up to 170 ℃ and be stirred to molten state, then lower the temperature 130 ℃ and add 50 parts of diallyl bisphenols, 130 ℃ of lower reactions 1 hour.Then the Resins, epoxy (novolac epoxy, alicyclic epoxy mass ratio are 100:100) that adds 200 parts is warming up to 150 ℃ and continues reaction 2 hours, is cooled to 60 ℃ of glyoxal ethyline promotor of adding 1 weight part and obtains modified epoxide resin adhesive.Experimental result shows, the temperature that the epoxyn thermolysis begins is 370 ℃.
Embodiment 4
In three mouthfuls of round-bottomed flasks of 500mL, add 100 parts of bismaleimidess (1-naphtholphthalein Diphenyl Ether Bismaleimide, o-cresolphthalein Diphenyl Ether Bismaleimide mass ratio are 50:50), then be warming up to 170 ℃ and be stirred to molten state, then lower the temperature 130 ℃ and add 100 parts of diallyl bisphenols, 130 ℃ of lower reactions 1 hour.Then the bisphenol-s epoxy resin that adds 200 parts is warming up to 150 ℃ and continues reaction 2 hours, is cooled to the methyl ethyl diketone salt composite promotor of adding 5.0 weight parts after 60 ℃ and obtains modified epoxide resin adhesive.Experimental result shows, the temperature that the epoxyn thermolysis begins is 365 ℃.
The performance test data table of table 1 low resin mica tape
The Resins, epoxy low resin mica tape of epoxy anhydride solvent-free immersion paint and embodiment 1 preparation is also solidified the simulated machine of preparation through vacuum pressure impregnation, the dielectric loss of test simulation motor, insulation resistance and electrical strength, as shown in table 2, table 2 is the performance test data table of simulated machine.
The performance test data table of table 2 simulated machine
The explanation of above embodiment just is used for helping to understand method of the present invention and core concept thereof.Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of claim of the present invention.
To the above-mentioned explanation of the disclosed embodiments, make this area professional and technical personnel can realize or use the present invention.Multiple modification to these embodiment will be apparent concerning those skilled in the art, and General Principle as defined herein can be in the situation that do not break away from the spirit or scope of the present invention, in other embodiments realization.Therefore, the present invention will can not be restricted to these embodiment shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (10)
1. the preparation method of an epoxyn may further comprise the steps:
With bismaleimides with contain allylic phenol and mix, obtain polybismaleimide behind the first set reaction;
Described polybismaleimide is mixed with Resins, epoxy, and heating adds promotor after the reaction for the second time, obtains epoxyn.
2. preparation method according to claim 1, it is characterized in that, described bismaleimides is N, a N ＇-penylene bismaleimides, N, N,-4,4 ,-diphenyl methane dimaleimide, the dihydroxyphenyl propane Diphenyl Ether Bismaleimide, the Bisphenol F Diphenyl Ether Bismaleimide, the phenolphthalein Diphenyl Ether Bismaleimide, the thymolphthalein Diphenyl Ether Bismaleimide, the thymolsulfonphthalein Diphenyl Ether Bismaleimide, the o-cresolphthalein Diphenyl Ether Bismaleimide, in 1-naphtholphthalein Diphenyl Ether Bismaleimide and the thymolphthalein Diphenyl Ether Bismaleimide one or more.
3. preparation method according to claim 1 is characterized in that, described to contain allylic phenol be diallyl bisphenol.
4. preparation method according to claim 1 is characterized in that, the step that obtains polybismaleimide is specially:
Lower the temperature after bismaleimides is heated to 170 ~ 200 ℃, add after temperature is down to 130 ~ 140 ℃ and contain allylic phenol, obtain polybismaleimide behind the first set reaction.
5. preparation method according to claim 1 is characterized in that, the time of described first set reaction is 1 ~ 2h.
6. preparation method according to claim 1, it is characterized in that, described promotor is one or more of acetylacetone copper, zinc acetylacetonate, chromium acetylacetonate, acetylacetone cobalt, zinc naphthenate, aluminium acetylacetonate, 1-benzyl-2-ethyl imidazol(e), glyoxal ethyline, 2-ethyl-4-methylimidazole and 1-cyanoethyl substituted imidazole.
7. preparation method according to claim 1 is characterized in that, the step that obtains epoxy adhesive is specially:
Described polybismaleimide is mixed with Resins, epoxy, be heated to 140 ~ 150 ℃, carry out reducing temperature after the reaction second time, temperature is added promotor after being down to 40 ~ 60 ℃, obtains epoxyn.
8. preparation method according to claim 1 is characterized in that, the mass ratio of described Resins, epoxy, polybismaleimide and promotor is (90 ~ 110): (50 ~ 100): (0.1 ~ 5).
9. preparation method according to claim 1 is characterized in that, described bismaleimides and the described quality that contains allylic phenol are (50 ~ 100): (25 ~ 50).
10. each described epoxyn application in low resin mica tape of claim 1 ~ 9.
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| CN103265791A (en) * | 2013-05-29 | 2013-08-28 | 苏州生益科技有限公司 | Thermosetting resin composition for integrated circuit as well as prepreg and laminated board both fabricated by using composition |
| CN104531028A (en) * | 2015-01-24 | 2015-04-22 | 李�杰 | Preparation method of modified epoxy resin adhesive for adhesion of silicon rubber and metal |
| CN104987666A (en) * | 2015-06-30 | 2015-10-21 | 苏州洋杰电子有限公司 | Epoxy resin-polymaleimide composite semiconductor packaging material and preparation method thereof |
| CN106280445A (en) * | 2016-08-11 | 2017-01-04 | 江苏恒神股份有限公司 | A kind of liquid molding high tenacity bismaleimide resin and preparation method thereof |
| CN110964176A (en) * | 2019-12-18 | 2020-04-07 | 四川东材科技集团股份有限公司 | Preparation method of high-heat-resistance phosphorus-containing epoxy resin |
| CN112786262A (en) * | 2020-12-30 | 2021-05-11 | 苏州巨峰电气绝缘系统股份有限公司 | F-grade mica tape with less glue, preparation method and application thereof |
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| CN110964176A (en) * | 2019-12-18 | 2020-04-07 | 四川东材科技集团股份有限公司 | Preparation method of high-heat-resistance phosphorus-containing epoxy resin |
| CN112786262A (en) * | 2020-12-30 | 2021-05-11 | 苏州巨峰电气绝缘系统股份有限公司 | F-grade mica tape with less glue, preparation method and application thereof |
| CN112786262B (en) * | 2020-12-30 | 2022-08-12 | 苏州巨峰电气绝缘系统股份有限公司 | F-grade mica tape with less glue, preparation method and application thereof |
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Application publication date: 20130206 |