CN1443818A - High-strength epoxy impregnating varnish capable of using at ultra-low temp. and its preparation and application method - Google Patents
High-strength epoxy impregnating varnish capable of using at ultra-low temp. and its preparation and application method 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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Abstract
The present invention discloses a high-strnegth epoxy inpregnating varnish used at ultralow temp., its preparation method and application method. It is characterized by that it uses epoxy resin and toughened epoxy resin mixture as main agent, uses toughened acid anhydride as solidifying agent and uses nano silicon dioxide filling material as strengthening agent to prepare said invented product. Said preparation method includes the following steps: firstly, mixing epoxy resin and toughened epoxy resin, heating to 150-250 deg.C, evacuating, dewatering for 1-4 hr., slowly adding nano filling material treated by coupling agent, fully-stirring, then slowly cooling to room temp., making the nano filling material suspended in resin, finally adding acid anhydride solidifying agent.
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.
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CNB031128661A CN100335574C (en) | 2003-02-21 | 2003-02-21 | High-strength epoxy impregnating varnish capable of using at ultra-low temp. and its preparation and application method |
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CNB031128661A CN100335574C (en) | 2003-02-21 | 2003-02-21 | High-strength epoxy impregnating varnish capable of using at ultra-low temp. and its preparation and application method |
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Cited By (9)
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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 | Preparation method of vacuum pressurized impregnating epoxy 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)
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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 temp. adhesive and firming agent used for low temp. adhesive |
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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Cited By (11)
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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 | Preparation method of vacuum pressurized impregnating epoxy 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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