CN104160454A - 基于异己糖醇二醇二环氧甘油醚的电绝缘树脂 - Google Patents
基于异己糖醇二醇二环氧甘油醚的电绝缘树脂 Download PDFInfo
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- CN104160454A CN104160454A CN201380009442.6A CN201380009442A CN104160454A CN 104160454 A CN104160454 A CN 104160454A CN 201380009442 A CN201380009442 A CN 201380009442A CN 104160454 A CN104160454 A CN 104160454A
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- electric insulation
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- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
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- H01B3/40—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes epoxy resins
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- C08G59/20—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the epoxy compounds used
- C08G59/22—Di-epoxy compounds
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- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
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Abstract
电绝缘树脂,包括A)异己糖醇二醇二环氧甘油醚,B)硬化剂,C)任选填充剂,D)其他可选的添加剂。该异己糖醇二醇二环氧甘油醚优选是异山梨醇二环氧甘油醚、异甘露醇二环氧甘油醚或异艾杜醇二环氧甘油醚。
Description
技术领域
本发明涉及一种基于异己糖醇二醇(isohexidediol)二环氧甘油醚的电绝缘性树脂及其用途。
背景技术
基于环氧树脂的电绝缘性树脂是已知的,并常常被描述。
基于双酚A二环氧甘油醚与双酚F二环氧甘油醚的电气灌封化合物在DE4206733中有描述。这些灌封化合物包括作为填充剂的白云石以及作为硬化剂的甲基四氢邻苯二甲酸酐。该固化在80℃至100℃实施,并在130℃至140时后固化2至4小时。
DE4139877和EP545506中描述了脂环族环氧树脂。这些树脂是3,4-环氧环己基甲基3,4-环氧环己基羧酸酯和双(3,4-环氧环己基甲基)己二酸酯。白云石作为填充剂,并且四氢邻苯二甲酸酐作为硬化剂。
CH424256中描述了基于环十二烷三环氧化物的可固化浇注树脂混合物,邻苯二甲酸酐或4,4'-二氨基-3,3'-二甲基二环己基甲烷作为硬化剂。
基环氧树脂也可改性。例如在WO98/04609中描述了硅酮改性环氧树脂。
环氧树脂不用填充剂时作为浸渍剂,具有填充剂时作为浇注树脂。除了白云石,其它无机材料如白垩和氧化铝也用作环氧树脂的填充剂,也与玻璃短纤维结合,如DE1570211中的描述。橡胶粉也用作有机填充剂,如DE1495072中的描述。
环氧树脂是用二羧酸酐、二胺及它们的衍生物,并且还使用路易斯酸,如三氯化硼和三氟化硼的络合物来固化的。环氧树脂的固化尤其在书籍,如由A.M.Paquin,Springer-Verlag于1958年发表的“Epoxidverbindungen undEpoxidharze”(环氧化合物和环氧树脂)或由H.Domininghaus,VDI Verlag于1988年发表的“Die Kunststoffe und ihre Eigenschaften”(塑料及其性质)中有描述。
在电气工程领域中,环氧树脂已被证明在许多不同的应用中是有价值的。DE19809572中描述了浇注树脂变压器。DE4132982中描述了使用环氧树脂用于定子封装。DE1220500中描述了使用浇注树脂用于生产高压绝缘体。DE1209650中描述了利用浇注树脂进行绕头封装。DE1207605中描述了高压线圈的封装。另外,环氧树脂已被证明可用于浸渍牵引电动机(“Isolationssysteme für Traktionsmotoren”(用于牵引电动机的绝缘系统)VonRoll,CH-4426 Breitenbach)。
由于游离双酚A的含量,基于双酚A二环氧甘油醚的环氧树脂具有毒理学意义。此外,这些树脂在25℃具有9000到13000mPa·s的粘度,因此,对于许多应用来说粘度过高。
尽管脂环族环氧树脂具有低粘度,但它们有很强的增敏作用。
US2008/0009599A1描述了脱水糖的缩水甘油醚,如异山梨醇、异甘露醇和异艾杜醇(isoidide),以及由此通过利用脂族和芳族聚胺固化获得的树脂。
发明内容
本发明的目的是提供不具有上述缺点的电绝缘性树脂制剂。特别的,它们应该是无毒的,并具有低粘度,很短的凝胶时间,并且还有良好的固化性能和良好的粘结强度。
该目的通过电绝缘树脂实现,其包括
A)异己糖醇二醇的二环氧甘油醚
B)硬化剂
C)任选的填充剂
D)其它可选的添加剂。
我们惊奇地发现,异己糖醇二醇的二环氧甘油醚作为环氧树脂在电绝缘应用是非常有用的。
异己糖醇二醇是由来自相应的己糖醇的酸酐构造通过消除2分子的水而得到的。优先考虑的是异山梨醇、异甘露醇和异艾杜醇的二环氧甘油醚。这些都在例如US3272845中有描述。
优选考虑的是异山梨醇二环氧甘油醚。
异山梨醇(1,4:3,6-二脱水-D-山梨糖醇)是由葡萄糖制备的。异山梨醇二环氧甘油醚随后可由此通过各种方法来制备,例如在WO2008/147473中所描述的。工业用异山梨二环氧甘油醚在25℃具有的粘度约为870mPa·s,环氧当量为166EEW/g。
异甘露醇二环氧甘油醚和异艾杜醇二环氧甘油醚具有类似于异山梨醇二环氧甘油醚的性质。
根据本发明的电绝缘树脂在固化状态下具有优异的粘附性和优异的电绝缘性能。该树脂可单独用于或与固体绝缘材料(胶带等)组合用于绝缘电气装置,如电动机、变压器和发电机。
异山梨醇二环氧甘油醚以及其它的异己糖醇二醇二环氧甘油醚可用于各种电绝缘树脂配方中并用于代替例如双酚A二环氧甘油醚。根据异己糖醇二醇二环氧甘油醚和由异己糖醇二醇二环氧甘油醚代替的环氧化合物的不同环氧当量选择该异己糖醇二醇二环氧甘油醚的量。
根据本发明的电绝缘性树脂包括至少一种硬化剂B)。用于环氧树脂的合适硬化剂是二羧酸或二羧酸酐、二伯二胺或聚胺或路易斯酸。
在本发明的实施方式中,硬化剂B)包括一种或多种二羧酸酐。例如,合适的二羧酸酐或二羧酸酐硬化剂有四氢邻苯二甲酸酐、甲基四氢邻苯二甲酸酐、六氢邻苯二甲酸酐和十二烷基琥珀酸酐。优选的是四氢邻苯二甲酸酐和六氢邻苯二甲酸酐。
在一般情况下,异己糖醇二醇二环氧甘油醚的每一环氧当量使用75%至100%、优选为85%至100%的酸酐硬化剂的酸酐当量。
除了硬化剂B)外,反应促进剂可存在于树脂中。如果二羧酸酐作为硬化剂B),则优选地反应促进剂包含在其中。合适的反应促进剂是叔胺,例如苄基二甲胺、三乙胺、三乙醇胺和N-甲基吗啉。
在进一步的实施方式中,硬化剂B)包括二伯二胺或聚胺。例如,合适的硬化剂有1,6-己烯二胺、异佛尔酮二胺、苯二甲胺、二亚乙基三胺、三亚乙基四胺、四亚乙基五胺、环戊烷己胺和聚醚聚胺,如Jeffamine D 400。
在一般情况下,异己糖醇二醇二环氧甘油醚的每一环氧当量,75%至100%的等效胺量、优选85%至100%的等效胺量用作二伯二胺或聚胺。
在进一步的实施方式中,硬化剂B)包括路易斯酸。例如,适合作为硬化剂的路易斯酸有三氟化硼或三氯化硼络合物,特别是胺络合物。实例是单乙醇胺、氨,还有哌啶、三甲胺、环己烷四胺或三氟化硼的吡啶复合物,还有三氯化硼的二甲基辛胺或吡啶络合物。
在一般情况下,基于所述电绝缘树脂的总质量,使用1wt%至6wt%、优选为2wt%至5wt%的路易斯酸。
在本发明的具体实施方式中,硬化剂B)包括三氯化硼-胺络合物。
电绝缘树脂可含有一种或多种填充剂。例如,合适的填充剂选自白云石、白垩、熔融二氧化硅、石英粉、氢氧化铝、氢氧化镁及其混合物构成的组中。
基于所述电绝缘树脂的总质量,所述填充剂可以20wt%至70wt%的量存在。
如果电绝缘树脂是浇注树脂,那么其优选地包括填充剂。如果电绝缘树脂是浸渍剂,则其优选不包括填充剂。
电绝缘树脂可含有其它添加剂D)。除了已经提到的反应促进剂,添加剂还有润湿助剂、均化剂和颜料。
通常,基于所述电绝缘树脂的总质量,添加剂可以0至6wt%的量存在。
电绝缘树脂还可额外包括活性稀释剂。合适的活性稀释剂有二元醇或长链一元醇的二环氧甘油醚,例如丁二醇二环氧甘油醚、己二醇二环氧甘油醚、苯基缩水甘油醚、甲苯基缩水甘油醚、癸基缩水甘油醚、十二烷基缩水甘油醚、聚乙二醇单缩水甘油醚和聚四氢呋喃单缩水甘油醚。如果这些都存在,基于电绝缘树脂的总质量,它们可以高达20wt%的量存在,但导致了柔软的模塑材料。优选的,电绝缘树脂不含有任何活性稀释剂。
根据本发明的制剂是由当前的常规步骤,如浸渍、浸轧、滴流、浇注、真空或真空压力浸渍而引入到电机的绕组中。这之后是热固化、烘箱中固化或绕组的电阻加热或这些选项的组合。
本发明还涉及异己糖醇二醇二环氧甘油醚,特别是异山梨醇二环氧甘油醚、异甘露醇二环氧甘油醚和异艾杜醇二环氧甘油醚在电绝缘树脂中的用途,所述电绝缘树脂用于浸渍电机、用于封装变压器、电力线圈和电动机以及用于产生高压绝缘体。
本发明还涉及上述电绝缘树脂在浸渍电机、特别是浸渍高压电机中的用途。本发明进一步提供了电绝缘性树脂的用途,其用于封装变压器、电线圈、用于完全包封电动机和用于产生高压绝缘体。
本发明将参照实施例进行更详细地说明。测试是按照DIN和IEC标准进行的。
具体实施方式
实施例
本发明通过实施例进行说明,但绝不限于这些实施例。
比较例1
将53.33g的双酚A二环氧甘油醚(EEW=190)、46.53g的甲基四氢邻苯二甲酸酐和0.14g的苄基二甲胺进行混合,并在进一步的实验中使用。该制剂中含有的硬化剂理论量为100%。凝胶时间在120℃时是20′20″,在130℃时是11′19″。粘度在25℃时为656mPa.s。
实施例2
将49.88g的异山梨醇二环氧甘油醚(EEW=166)、49.97g的甲基四氢邻苯二甲酸酐和0.15g的苄基二甲胺进行混合,并在进一步的实验中使用。该制剂中含有的硬化剂理论量为100%。凝胶时间在120℃时是11′01″,在130℃时是5′12″。粘度在25℃时为421mpa.s。
固化实验
根据IEC61033,扭杆浸渍有树脂。它们在130℃时固化3小时,粘结强度确定为温度函数。
对于比较例1来说,这些为
589N(23℃),69N(155℃),42N(180℃);
对于实施例2来说,粘接强度是
632N(23℃),57N(155℃),452N(180℃)。
比较例3
将57.14g的双酚A二环氧甘油醚、42.73g的甲基四氢邻苯二甲酸酐和0.13g的苄基二甲胺进行混合,并在进一步的实验中使用。该制剂中含有的硬化剂理论量为85%。凝胶时间在120℃是22′21″,在130℃时是12′32″。粘度在25℃为805mPa.s。
实施例4
将53.91g的异山梨醇二环氧甘油醚、45.95g的甲基四氢邻苯二甲酸酐和0.14g的苄基二甲胺进行混合,并在进一步的实验中使用。该制剂含有的硬化剂理论量为85%。凝胶时间在120℃时是9′28″,在130℃时是5′00″。粘度在25℃为523mPa。
固化实验
如果比较例3在120℃时固化3小时,则模制材料具有76的肖氏D硬度。如果固化是在130℃时进行,该值是78,即没有变化。
对于来自实施例4的混合物,两种固化的相应肖氏D硬度为77。
比较例5
将52.91g的双酚A二环氧甘油醚、46.9g的甲基五氢邻苯二甲酸酐和0.14g的苄基二甲胺进行混合,并在进一步的实验中使用。该制剂中含有的硬化剂理论量为85%。凝胶时间在120℃时是19′11″,在130℃时是11″。粘度在25℃为643mPa·s。
实施例6
将49.38g的异山梨醇二环氧甘油醚、50.47g的甲基五氢邻苯二甲酸酐和0.15g的苄基二甲胺进行混合,并在进一步的实验中使用。该制剂中含有的硬化剂理论量为85%。凝胶时间在120℃时为9′22″,在130℃时为4′39″。粘度在25℃为408mPa.s。
90大小的定子浸渍有来自实施例2、4和6的树脂。在滴流阶段后,定子在160℃时固化2小时。随后他们被锯断。所有显示了铜绕组的完整、无气泡浸渍。
实施例7
在溶解器中,由108.6g不含邻苯二甲酸酯的增塑剂、526.9g异山梨醇二环氧甘油醚、1.0g锻制二氧化硅、0.1g市售的含硅酮消泡剂、342.9g白垩、20g黑色颜料膏和1.4g苄基二甲胺制备均匀的混合物。该混合物在23℃时具有4800mPa.s的年度。添加449.2g甲基四氢邻苯二甲酸酐后,将混合物均质化并制备各种标本。击穿电压为32KV/mm(根据IEC60243-1连同IEC60455-2)。跟踪指数为600(根据IEC60112连同60455-2)。耐冲击性为12kJ/m2(根据ISO 179)。
实施例8
将916g的异山梨醇二环氧甘油醚与1g润湿添加剂、1g均化助剂和37g市售的三氯化硼-胺络合物混合。已包裹有七个半重叠(14层)的市售云母/玻璃带的70×2×1cm的罗贝尔棒使用真空压力法(0.1bar真空/1小时,然后是6bar压力/5小时)浸渍该混合物。该棒在160℃时固化6小时。切开一根棒。该浸渍是均匀的并完全到达铜。
介电常数损耗因子在6KV时是0.0031,在10KV时是0.0036。介电常数损耗因子是温度依赖性的,在21℃时是0.0031,在90℃时是0.0096,在130℃时是0.0326,以及在155℃时是0.1498。
Claims (13)
1.电绝缘树脂,包括
A)异己糖醇二醇二环氧甘油醚
B)硬化剂
C)任选填充剂
D)其他可选的添加剂。
2.根据权利要求1所述的电绝缘树脂,其特征在于,所述异己糖醇二醇二环氧甘油醚是异山梨醇二环氧甘油醚、异甘露醇二环氧甘油醚或异艾杜醇二环氧甘油醚。
3.根据权利要求1或2所述的电绝缘树脂,其特征在于,所述硬化剂B)包含一种或多种二羧酸或二羧酸酐。
4.根据权利要求3所述的电绝缘树脂,其特征在于,所述硬化剂B)包括甲基四氢邻苯二甲酸酐或甲基六氢邻苯二甲酸酐。
5.根据权利要求1至4中任一项所述的电绝缘树脂,其特征在于,其包括反应促进剂。
6.根据权利要求1至5中任一项所述的电绝缘树脂,其特征在于,其包括填充剂。
7.根据权利要求6所述的电绝缘树脂,其特征在于,所述填充剂选自由白云石、白垩、熔融二氧化硅、石英粉、氢氧化铝、氢氧化镁及其混合物构成的组。
8.根据权利要求1所述的电绝缘树脂,其特征在于,所述硬化剂B)包括路易斯酸。
9.根据权利要求8所述的电绝缘树脂,其特征在于所述硬化剂B)包括三氯化硼-胺络合物。
10.异己糖醇二醇二环氧甘油醚在用于浸渍电机、用于封装变压器、线圈和电动机和用于产生高压绝缘体的电绝缘树脂中的应用。
11.根据权利要求1至9中任一项所述的电绝缘树脂在浸渍电机中的用途。
12.根据权利要求10所述的用途,所述电机为高压电机。
13.根据权利要求1至9中任一项所述的电绝缘树脂用于封装变压器和线圈、用于完全包封电动机和用于产生高压绝缘子的用途。
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US9605108B2 (en) * | 2014-04-24 | 2017-03-28 | New Jersey Institute Of Technology | Isosorbide-derived epoxy resins and methods of making same |
FR3040059B1 (fr) * | 2015-08-13 | 2019-05-17 | Roquette Freres | Utilisation d'une composition d'ethers de bis-anhydrohexitol de faible viscosite comme diluant reactif pour compositions reticulables de resines, d'adhesifs, de revetements et de matrices pour composi |
CN105931772A (zh) * | 2016-04-20 | 2016-09-07 | 南通日芝电力材料有限公司 | 环氧涂布纸生产方法 |
US11958253B2 (en) * | 2017-12-21 | 2024-04-16 | Elantas Europe S.R.L. | Use of isosorbide |
DE102020117995A1 (de) | 2020-07-08 | 2022-01-13 | Bayerische Motoren Werke Aktiengesellschaft | Elektrische Maschine für ein Kraftfahrzeug, Verwendung einer solchen elektrischen Maschine sowie Kraftfahrzeug |
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- 2012-02-14 DE DE102012202161A patent/DE102012202161A1/de not_active Ceased
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- 2013-02-08 TW TW102105068A patent/TWI612095B/zh not_active IP Right Cessation
- 2013-02-13 MY MYPI2014002355A patent/MY166177A/en unknown
- 2013-02-13 HU HUE13703619A patent/HUE029963T2/en unknown
- 2013-02-13 SI SI201330225A patent/SI2815407T1/sl unknown
- 2013-02-13 KR KR20147025263A patent/KR20140128419A/ko not_active Application Discontinuation
- 2013-02-13 ES ES13703619.0T patent/ES2578613T3/es active Active
- 2013-02-13 CN CN201380009442.6A patent/CN104160454A/zh active Pending
- 2013-02-13 EP EP13703619.0A patent/EP2815407B1/de not_active Not-in-force
- 2013-02-13 US US14/378,607 patent/US20150010697A1/en not_active Abandoned
- 2013-02-13 DK DK13703619.0T patent/DK2815407T3/en active
- 2013-02-13 BR BR112014020208A patent/BR112014020208A8/pt not_active IP Right Cessation
- 2013-02-13 WO PCT/EP2013/052824 patent/WO2013120872A2/de active Application Filing
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Also Published As
Publication number | Publication date |
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TW201336921A (zh) | 2013-09-16 |
HUE029963T2 (en) | 2017-04-28 |
BR112014020208A8 (pt) | 2017-07-11 |
MY166177A (en) | 2018-06-07 |
DE102012202161A1 (de) | 2013-08-14 |
WO2013120872A2 (de) | 2013-08-22 |
SI2815407T1 (sl) | 2016-08-31 |
KR20140128419A (ko) | 2014-11-05 |
TWI612095B (zh) | 2018-01-21 |
EP2815407B1 (de) | 2016-04-20 |
BR112014020208A2 (zh) | 2017-06-20 |
WO2013120872A3 (de) | 2014-01-09 |
ES2578613T3 (es) | 2016-07-28 |
EP2815407A2 (de) | 2014-12-24 |
DK2815407T3 (en) | 2016-08-01 |
US20150010697A1 (en) | 2015-01-08 |
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