CN1443818A - High-strength epoxy impregnating varnish used at extremely low temperature and preparation method and use method thereof - Google Patents
High-strength epoxy impregnating varnish used at extremely low temperature and preparation method and use method thereof Download PDFInfo
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- CN1443818A CN1443818A CN 03112866 CN03112866A CN1443818A CN 1443818 A CN1443818 A CN 1443818A CN 03112866 CN03112866 CN 03112866 CN 03112866 A CN03112866 A CN 03112866A CN 1443818 A CN1443818 A CN 1443818A
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- epoxy
- low temperature
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- impregnating varnish
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- 239000004593 Epoxy Substances 0.000 title claims abstract description 54
- 239000002966 varnish Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000000034 method Methods 0.000 title claims abstract description 5
- 229920005989 resin Polymers 0.000 claims abstract description 26
- 239000011347 resin Substances 0.000 claims abstract description 26
- 239000007822 coupling agent Substances 0.000 claims abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 13
- 239000000945 filler Substances 0.000 claims abstract description 11
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 239000003822 epoxy resin Substances 0.000 claims abstract description 7
- 150000008064 anhydrides Chemical class 0.000 claims abstract description 3
- 239000005543 nano-size silicon particle Substances 0.000 claims description 20
- 150000008065 acid anhydrides Chemical class 0.000 claims description 13
- 230000003014 reinforcing effect Effects 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 125000003700 epoxy group Chemical group 0.000 claims description 4
- 238000009472 formulation Methods 0.000 claims description 4
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 3
- 239000012745 toughening agent Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 239000003973 paint Substances 0.000 abstract description 2
- 238000007598 dipping method Methods 0.000 abstract 1
- 238000005470 impregnation Methods 0.000 abstract 1
- 239000012744 reinforcing agent Substances 0.000 abstract 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 238000007872 degassing Methods 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000009413 insulation Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 3
- 238000009738 saturating Methods 0.000 description 3
- 229920003002 synthetic resin Polymers 0.000 description 3
- 239000000057 synthetic resin Substances 0.000 description 3
- 230000004927 fusion Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000008602 contraction Effects 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004172 nitrogen cycle Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
- Epoxy Resins (AREA)
Abstract
本发明公开了一种极低温下使用的高强度环氧浸渍漆及其制备方法和使用方法，其特征在于以环氧树脂和增韧环氧树脂混合物为主剂，具有增韧的酸酐为固化剂，纳米二氧化硅填料为增强剂制备而成。首先将环氧树脂和增韧环氧树脂混合，加热至150～250℃，抽真空，脱水1～4小时，再缓慢加入经偶联剂处理的纳米填料，充分搅拌后缓慢降温至室温，使纳米填料悬浮在树脂中，最后再加入酸酐固化剂。本发明既增加环氧绝缘漆在极低温下的强度和抗脆裂性能，又不影响其浸渍性能。The invention discloses a high-strength epoxy dipping paint used at extremely low temperature and its preparation method and application method. Agent, nano-silica filler is prepared as a reinforcing agent. First, mix epoxy resin and toughened epoxy resin, heat to 150-250°C, vacuumize, dehydrate for 1-4 hours, then slowly add nano filler treated with coupling agent, stir well and then cool down to room temperature slowly, so that The nano filler is suspended in the resin, and finally the anhydride curing agent is added. The invention not only increases the strength and anti-brittle performance of the epoxy insulating varnish at extremely low temperature, but also does not affect its impregnation performance.
Description
Technical field
The present invention relates to the high-strength epoxy impregnating varnish that a kind of utmost point low temperature that adds Nano filling uses down, can guarantee to flood fixedly superconducting coil in the steady running of utmost point low temperature lower magnet.Be applicable in the similar utmost point cryogenic magnet device such as large-scale superconducting magnet of magnetic confinement fusion physics facility and stressed big high-intensity magnetic field magnet.
Background technology
The superconducting intense magnetic field magnet, the large-scale superconducting magnet of magnetic confinement superconduction fusion facility is in order to guarantee the operation stability of superconducting magnet, prevent the superconducting magnet quench, the stressed sex change of magnet does not reach the design magneticstrength, and magnet is wanted impregnated insulating paint (1) fixed magnets, guarantees magnet steady running.(2) provide the magnet electric insulation.Not only intensity is low for existing common epoxy insulation varnish, and (as-263 ℃ of liquid heliums) can embrittlement under utmost point low temperature.Add filler and can suitably improve its low temperature intensity and resistance to brittle fracture energy, but the adding of common fillers improves the viscosity of insullac again, influences the saturating machine of insullac.
Summary of the invention
The objective of the invention is to use and make toughener by the Nano filling after the coupling agent treatment and cooperate Resins, epoxy and epoxy resin toughened mixture to make host, the high-strength epoxy impregnating varnish that preparation poling low temperature uses down, make it both increase intensity and the resistance to brittle fracture energy of epoxy insulation varnish under utmost point low temperature, do not influence its saturating machine again.
The present invention is the high-strength epoxy impregnating varnish that uses under a kind of utmost point low temperature, it is characterized in that with Resins, epoxy and epoxy resin toughened mixture be host, to have toughness reinforcing acid anhydrides be solidifying agent, the nano silicon filler is that toughener is prepared from.
Adopt the coupling agent treatment Nano filling, prevent that it is agglomerating because of surface action power, described coupling agent can be r-aminopropyl triethoxysilane, r-glycidyl ether oxygen propyl trimethoxy silicane, r-(metacryloxy) propyl trimethoxy silicane.
Its formulation by weight is:
80～120 parts of Resins, epoxy
5～40 parts of toughness reinforcing epoxies
50～130 parts on acid anhydrides
5～15 parts of nano silicon fillers
Its formulation by weight can also for:
80～120 parts of Resins, epoxy
5～40 parts of toughness reinforcing epoxies
50～130 parts on acid anhydrides
5～15 parts of nano silicon fillers
1～5 part of coupling agent
The preparation method of the high-strength epoxy impregnating varnish that a kind of utmost point low temperature uses down, it is characterized in that at first with Resins, epoxy and epoxy resin toughened mixing, be heated to 150～250 ℃, vacuumize, dewatered 1～4 hour, and slowly added Nano filling again, slowly be cooled to room temperature after fully stirring through coupling agent treatment, Nano filling is suspended in the resin, adds anhydride curing agent at last again.
The preparation method of the high-strength epoxy impregnating varnish that a kind of utmost point low temperature uses down is characterized in that described coupling agent treatment is meant coupling agent and Nano filling mixed to mix thoroughly.
The using method of the high-strength epoxy impregnating varnish that a kind of utmost point low temperature uses down is characterized in that condition of cure: 80～130 ℃ solidified 1～2 hour down, and 140～150 ℃ solidified 1～2 hour, and 160～190 ℃ solidified 5～15 hours.
Effect of the present invention:
The high-strength epoxy impregnating varnish that the utmost point low temperature of the present invention's preparation uses down, after measured:
(1), according to GB GB
1149-81Recording to draw and cut under the intensity room temperature greater than 13.1MPa, is greater than 15.2Mpa in the time of-196 ℃.
(2), room-temperature impact strength is greater than 16.2kg.cm/cm
2
(3), cold cycling impacts, promptly-196 ℃ five minutes, room temperature five minutes, ℃ five minutes again-196, room temperature five minutes .... greater than the not embrittlement of 20 circulation samples.
(4), cold and hot (room temperature-liquid nitrogen) shrinkage coefficient is less than 0.65%.(5) puncture of insulation, under the room temperature greater than 23.4KV/mm.(5), air content is less than 1.7%.
(6) viscosity 40 ℃ less than 63 seconds, viscosity less than time of 75 seconds greater than 10 hours.
Table 1 is listed insullac of the present invention (LH-5) and domestic Shanghai synthetic resin plant 1149,6895, external Britain rutherford experiment chamber 01,02,10,20,30, and the performance of several insullac such as CTD-101K is relatively.LH-4 is the room temperature strength height not only, and intensity is also higher during-196 ℃ of utmost point low temperature.
Table 2 is listed insullac of the present invention (LH-5) and domestic Shanghai synthetic resin plant 1149,6895, and the electric property of several insullac such as external Britain rutherford experiment chamber CTD-101K relatively.
Table 3 is listed the air content after insullac of the present invention (LH-5) saturating machine and the curing thereof.
Table 4 is listed insullac of the present invention (LH-5) and domestic Shanghai synthetic resin plant 1149,6895, external Britain rutherford experiment chamber CTD-101K, and 71A, the cold and hot shrinkage coefficient of several insullac such as 79 is relatively.
Table 1:
Table 2:
Table 3:
Table 4:
| The performance sample | Tensile strength (MPa) chamber 77K | Shearing resistance (MPa) chamber 77K | Shock strength (kg.cm/cm 2) | Room temperature liquid nitrogen cycle index |
| ?LH-5 | ＞35???＞40. | ＞13.1??????????＞15.2 | ＞16.2 | ＞20 |
| ?1149 | ?31????33.5 | ?6.0????????????7.4 | ?10.7 | ＜5 |
| ?6895 | ?34????36 | ?8.0????????????8.3 | ?13.4 | ＜5 |
| ?RAL1-PH | ?8.4±0.8???????8.9±0.6 | |||
| ?01 | ?8.7±0.8???????12±0.2 | |||
| ?02 | ?7.8±1.5???????11±1.6 | |||
| ?10 | ?8.6±0.4???????12.8±0. | |||
| ?20 | ?9.3±0.4???????9.8±1.8 | |||
| ?30 | ?6.2±0.7???????11.1±0.2 | |||
| ?CTD-101K | ?10.2???????????18.0 | ＜20 |
| The performance sample | ρ s(Ω) | ρ v(Ω.m) | E B(KV/mm) | tgδ |
| ?LH-5 | ＞3.5×10 16 | ＞2.1×10 17 | ＞28.4 | ＜0.0017 |
| ?1149 | ?1.2×10 14 | 6.5×10 16 | 30.5 | ?0.0016 |
| ?6895 | ?3.9×10 14 | 4.5×10 16 | 37.2 | ?0.012 |
| ?CTD-101K | ＞26 |
| Air content (%) | Viscosity (being coated with 4) 40 ℃ (S) | Viscosity less than time of 75S (hour) |
| ????＜1.7 | ????＜63 | ????＞10 |
| Insullac | ??LH-5 | ?1149 | ?6895 | ?CTD-101K | ?71A | ?79 |
| The cold and hot contraction of room temperature liquid nitrogen system | ＜0.0083 | ?0.011 | ?0.013 | ?0.013 | ?0.010 | ?0.011 |
Embodiment
Embodiment 1:
At first Resins, epoxy 80 grams and toughness reinforcing epoxy 5 grams are mixed and heated to 150 ~ 250 ℃, the degassing, dewater and slowly add nano silicon 5 grams after 1～4 hour again, slowly be cooled to room temperature after fully stirring, nano silicon is suspended in the Resins, epoxy, adds solidifying agent acid anhydrides 50 grams at last again and solidify condition of cure: 80～130 ℃ solidified 1～2 hour down, 140～150 ℃ solidified 1～2 hour, and 160～190 ℃ solidified 5～15 hours.
Embodiment 2:
At first Resins, epoxy 120 grams and toughness reinforcing epoxy 40 grams are mixed and heated to 150～250 ℃, the degassing, dewater and slowly add nano silicon 15 grams after 1～4 hour again, r-aminopropyl triethoxysilane 5 grams, slowly be cooled to room temperature after fully stirring, nano silicon is suspended in the Resins, epoxy, adds solidifying agent acid anhydrides 130 grams at last again and solidify.Condition of cure: 80～130 ℃ solidified 1～2 hour down, and 140～150 ℃ solidified 1～2 hour, and 160～190 ℃ solidified 5～15 hours.
Embodiment 3:
At first Resins, epoxy 100 grams and toughness reinforcing epoxy 30 grams are mixed and heated to 150～250 ℃, the degassing, dewater and slowly add nano silicon 10 grams after 1～4 hour again, r-aminopropyl triethoxysilane 1 gram, slowly be cooled to room temperature after fully stirring, nano silicon is suspended in the Resins, epoxy, adds solidifying agent acid anhydrides 100 grams at last again and solidify.Condition of cure: 80～130 ℃ solidified 1～2 hour down, and 140～150 ℃ solidified 1～2 hour, and 160～190 ℃ solidified 5～15 hours.
Embodiment 4:
At first Resins, epoxy 90 grams and toughness reinforcing epoxy 20 grams are mixed and heated to 150～250 ℃, the degassing, dewater and slowly add nano silicon 8 grams after 1～4 hour again, r-aminopropyl triethoxysilane 2 grams, slowly be cooled to room temperature after fully stirring, nano silicon is suspended in the Resins, epoxy, adds solidifying agent acid anhydrides 95 grams at last again and solidify.Condition of cure: 80～130 ℃ solidified 1～2 hour down, and 140～150 ℃ solidified 1～2 hour, and 160～190 ℃ solidified 5～15 hours.
Embodiment 5:
At first Resins, epoxy 110 grams and toughness reinforcing epoxy 35 grams are mixed and heated to 150～250 ℃, the degassing, dewater and slowly add nano silicon 7 grams after 1～4 hour again, r-aminopropyl triethoxysilane 4 grams, slowly be cooled to room temperature after fully stirring, nano silicon is suspended in the Resins, epoxy, adds solidifying agent acid anhydrides 105 grams at last again and solidify.Condition of cure: 80～130 ℃ solidified 1～2 hour down, and 140～150 ℃ solidified 1～2 hour, and 160～190 ℃ solidified 5～15 hours.
Embodiment 6:
At first Resins, epoxy 120 grams and toughness reinforcing epoxy 40 grams are mixed and heated to 150～250 ℃, the degassing, dewater and slowly add nano silicon 15 grams after 1～4 hour again, r-glycidyl ether oxygen propyl trimethoxy silicane 5 grams, slowly be cooled to room temperature after fully stirring, nano silicon is suspended in the Resins, epoxy, adds solidifying agent acid anhydrides 130 grams at last again and solidify.Condition of cure: 80～130 ℃ solidified 1～2 hour down, and 140～150 ℃ solidified 1～2 hour, and 160～190 ℃ solidified 5～15 hours.
Embodiment 7:
At first Resins, epoxy 100 grams and toughness reinforcing epoxy 30 grams are mixed and heated to 150～250 ℃, the degassing, dewater and slowly add nano silicon 10 grams after 1～4 hour again, r-(metacryloxy) propyl trimethoxy silicane 1 gram, slowly be cooled to room temperature after fully stirring, nano silicon is suspended in the Resins, epoxy, adds solidifying agent acid anhydrides 100 grams at last again and solidify.Condition of cure: 80～130 ℃ solidified 1～2 hour down, and 140～150 ℃ solidified 1～2 hour, and 160～190 ℃ solidified 5～15 hours.
Claims (7)
1, the high-strength epoxy impregnating varnish that uses under a kind of utmost point low temperature is characterized in that with Resins, epoxy and epoxy resin toughened mixture be host, and having toughness reinforcing acid anhydrides is solidifying agent, and the nano silicon filler is that toughener is prepared from.
2,, the high-strength epoxy impregnating varnish that utmost point low temperature according to claim 1 uses down, it is characterized in that adopting earlier the coupling agent treatment Nano filling, prevent that it is agglomerating because of surface action power, described coupling agent can be r-aminopropyl triethoxysilane, r-glycidyl ether oxygen propyl trimethoxy silicane, r-(metacryloxy) propyl trimethoxy silicane.
3, the high-strength epoxy impregnating varnish that uses under the utmost point low temperature according to claim 1 is characterized in that its formulation by weight is:
80～120 parts of Resins, epoxy
5～40 parts of toughness reinforcing epoxies
50～130 parts on acid anhydrides
5～15 parts of nano silicon fillers.
4, the high-strength epoxy impregnating varnish that uses under the utmost point low temperature according to claim 1 is characterized in that its formulation by weight is:
80～120 parts of Resins, epoxy
5～40 parts of toughness reinforcing epoxies
50～130 parts on acid anhydrides
5～15 parts of nano silicon fillers
1～5 part of coupling agent.
5, the preparation method of the high-strength epoxy impregnating varnish that uses under the utmost point low temperature according to claim 1, it is characterized in that at first with Resins, epoxy and epoxy resin toughened mixing, be heated to 150～250 ℃, vacuumize, dewatered 1～4 hour, and slowly added Nano filling again, slowly be cooled to room temperature after fully stirring through coupling agent treatment, Nano filling is suspended in the resin, adds anhydride curing agent at last again.
6, the preparation method of the high-strength epoxy impregnating varnish that uses down of utmost point low temperature according to claim 1 is characterized in that described coupling agent treatment is meant coupling agent and Nano filling mixed to mix thoroughly.
7, the using method of the high-strength epoxy impregnating varnish that uses down of utmost point low temperature according to claim 1, it is characterized in that condition of cure: 80～130 ℃ solidified 1～2 hour down, and 140～150 ℃ solidified 1～2 hour, and 160～190 ℃ solidified 5～15 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031128661A CN100335574C (en) | 2003-02-21 | 2003-02-21 | High-strength epoxy impregnating varnish used at extremely low temperature and preparation method and use method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031128661A CN100335574C (en) | 2003-02-21 | 2003-02-21 | High-strength epoxy impregnating varnish used at extremely low temperature and preparation method and use method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1443818A true CN1443818A (en) | 2003-09-24 |
| CN100335574C CN100335574C (en) | 2007-09-05 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB031128661A Expired - Fee Related CN100335574C (en) | 2003-02-21 | 2003-02-21 | High-strength epoxy impregnating varnish used at extremely low temperature and preparation method and use method thereof |
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|---|---|
| CN (1) | CN100335574C (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1320020C (en) * | 2004-07-02 | 2007-06-06 | 大连理工大学 | Epoxy resin complex with long chemical storage stability and temperature thixotropy |
| CN100462384C (en) * | 2006-06-22 | 2009-02-18 | 上海交通大学 | A kind of preparation method of epoxy vacuum pressure impregnation resin |
| CN101789654A (en) * | 2010-02-26 | 2010-07-28 | 株洲敏锐轨道电气有限责任公司 | Insulating method and device of oil pump motor stator of electric locomotive transformer powered up by frequency converter |
| CN102684407A (en) * | 2012-05-23 | 2012-09-19 | 永济新时速电机电器有限责任公司 | Method for protecting and fixing assembled permanent magnet in large-power permanent magnet motor |
| CN102690496A (en) * | 2012-06-08 | 2012-09-26 | 苏州巨峰电气绝缘系统股份有限公司 | Nano modified epoxy vacuum pressure impregnation resin and preparation method thereof |
| CN103555136A (en) * | 2013-10-25 | 2014-02-05 | 安徽文峰电子科技集团有限公司 | Epoxy impregnating varnish and preparation method thereof |
| CN103571301A (en) * | 2013-09-29 | 2014-02-12 | 武汉材料保护研究所 | High bonding-strength insulating paint for insulating protection layer of titanium alloy surface |
| CN108976991A (en) * | 2018-07-10 | 2018-12-11 | 丹阳市沃德立电工材料有限公司 | A kind of high resistant anticorona varnish and preparation method thereof applied to HV Electric Machine Coil |
| CN110776806A (en) * | 2019-10-21 | 2020-02-11 | 王利玲 | Hyperbranched polymer-SiO 2Modified epoxy resin insulating material and preparation method thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05287219A (en) * | 1992-04-03 | 1993-11-02 | Nippon Kayaku Co Ltd | Epoxy resin powder coating material |
| CN1197098A (en) * | 1997-04-24 | 1998-10-28 | 中国科学院低温技术实验中心 | Low temperature adhesives and curing agents for low temperature adhesives |
| JP3389533B2 (en) * | 1999-06-30 | 2003-03-24 | 株式会社日立製作所 | Epoxy resin composition and molded coil |
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2003
- 2003-02-21 CN CNB031128661A patent/CN100335574C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1320020C (en) * | 2004-07-02 | 2007-06-06 | 大连理工大学 | Epoxy resin complex with long chemical storage stability and temperature thixotropy |
| CN100462384C (en) * | 2006-06-22 | 2009-02-18 | 上海交通大学 | A kind of preparation method of epoxy vacuum pressure impregnation resin |
| CN101789654A (en) * | 2010-02-26 | 2010-07-28 | 株洲敏锐轨道电气有限责任公司 | Insulating method and device of oil pump motor stator of electric locomotive transformer powered up by frequency converter |
| CN101789654B (en) * | 2010-02-26 | 2012-12-26 | 株洲敏锐轨道电气有限责任公司 | Insulating method and device of oil pump motor stator of electric locomotive transformer powered up by frequency converter |
| CN102684407A (en) * | 2012-05-23 | 2012-09-19 | 永济新时速电机电器有限责任公司 | Method for protecting and fixing assembled permanent magnet in large-power permanent magnet motor |
| CN102690496A (en) * | 2012-06-08 | 2012-09-26 | 苏州巨峰电气绝缘系统股份有限公司 | Nano modified epoxy vacuum pressure impregnation resin and preparation method thereof |
| CN103571301A (en) * | 2013-09-29 | 2014-02-12 | 武汉材料保护研究所 | High bonding-strength insulating paint for insulating protection layer of titanium alloy surface |
| CN103571301B (en) * | 2013-09-29 | 2016-05-18 | 武汉材料保护研究所 | A kind of high bond strength coatings for titanium alloy surface insulating protective layer |
| CN103555136A (en) * | 2013-10-25 | 2014-02-05 | 安徽文峰电子科技集团有限公司 | Epoxy impregnating varnish and preparation method thereof |
| CN108976991A (en) * | 2018-07-10 | 2018-12-11 | 丹阳市沃德立电工材料有限公司 | A kind of high resistant anticorona varnish and preparation method thereof applied to HV Electric Machine Coil |
| CN110776806A (en) * | 2019-10-21 | 2020-02-11 | 王利玲 | Hyperbranched polymer-SiO 2Modified epoxy resin insulating material and preparation method thereof |
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| CN100335574C (en) | 2007-09-05 |
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