CN116640492A - 一种储存稳定的h级高压无溶剂浸渍漆及其制备方法和应用 - Google Patents
一种储存稳定的h级高压无溶剂浸渍漆及其制备方法和应用 Download PDFInfo
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- CN116640492A CN116640492A CN202310632532.6A CN202310632532A CN116640492A CN 116640492 A CN116640492 A CN 116640492A CN 202310632532 A CN202310632532 A CN 202310632532A CN 116640492 A CN116640492 A CN 116640492A
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- epoxy resin
- diglycidyl
- impregnating varnish
- ether
- reactive
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- 239000003085 diluting agent Substances 0.000 claims abstract description 39
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 17
- 239000003999 initiator Substances 0.000 claims abstract description 10
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- 238000006116 polymerization reaction Methods 0.000 claims abstract description 7
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- 125000000524 functional group Chemical group 0.000 claims description 11
- -1 glycidyl ester Chemical class 0.000 claims description 11
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- 125000002723 alicyclic group Chemical group 0.000 claims description 7
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- 239000004641 Diallyl-phthalate Substances 0.000 claims description 3
- QUDWYFHPNIMBFC-UHFFFAOYSA-N bis(prop-2-enyl) benzene-1,2-dicarboxylate Chemical compound C=CCOC(=O)C1=CC=CC=C1C(=O)OCC=C QUDWYFHPNIMBFC-UHFFFAOYSA-N 0.000 claims description 3
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Abstract
本发明公开了一种储存稳定的H级高压无溶剂浸渍漆及其制备方法和应用。本发明的无溶剂浸渍漆包括重量份数比为20～60：90～120：2～40：0～5：0～5：0～5：0～5：20～300的耐热型环氧树脂、环氧树脂、固化剂、阻聚剂、引发剂、固化促进剂、增韧剂和活性稀释剂。该浸渍漆采用原料来源广泛，成本相对比较低廉的环氧类树脂体系，通过耐热性环氧树脂和普通环氧树脂、耐热固化剂、双官能团活性稀释剂的复配及配比设计，使得整个无溶剂浸渍漆储存稳定，粘度低，便于低温浸渍，凝胶时间短，节能环保，降低对人体健康伤害。该浸渍漆毒性小、气味小，饱和蒸汽压低，耐高温性能好，对环境友好，电气性能及储存稳定性能优异。
Description
技术领域
本发明涉及一种储存稳定的H级高压无溶剂浸渍漆及其制备方法和应用，属于电机绝缘处理技术领域。
背景技术
高压电机绕组由电磁线、对地绝缘、相绝缘、层间绝缘、槽楔和绑扎固定等各种绝缘材料和结构组合而成，是一个松散的组合体，因此要对其进行绝缘处理，使整个绕组绝缘粘结成为一个整体，提高整个绝缘结构的耐热性、导热性、电气强度、机械强度和耐环境介质侵蚀性等。
真空压力浸渍是当今高压电机主要的绝缘处理技术之一，包括中胶真空压力浸渍和少胶真空压力浸渍，其中少胶真空压力浸渍逐渐成为发展主流方向。适用于高压电机的少胶真空压力浸渍漆要求粘度小，固化收缩率低，电性能优异，耐热性能好。而目前市面上H级浸渍漆主要用于低压电机，适用于高压电机很少。
目前国内外H级无溶剂浸渍漆的品种主要有有机硅类、二苯醚类、聚酰亚胺类、耐热聚酯类、环氧类等。有机硅无溶剂漆起始粘度大，高温粘接力差，而且价格昂贵，限制其使用；二苯醚无溶剂漆固化时低分子物多，漆膜脆性大，固化温度高；聚酰亚胺无溶剂漆室温下粘度很大，需高温浸漆，使用不便；耐高温聚酯无溶剂漆收缩率大，漆膜易开裂；环氧类树脂漆采用苯乙烯类型活性稀释剂作为稀释剂，有气味严重、容易刺激皮肤和呼吸道等不良反应。出于人身健康安全考虑，欧盟正逐步取消以酸酐做固化剂的无溶剂浸渍漆的使用。
发明内容
本发明的目的是：针对目前H级无溶剂浸渍漆存在或成本昂贵，或起始粘度大，或高温粘接力差，漆膜脆性大，或机械强度低，固化收缩率大，或不够环保等缺点，限制了广泛使用；为保证原料来源广泛，降低成本，保证机械强度，提出一种H级高压无溶剂浸渍漆仍然采用环氧类树脂体系，但采用了多官能度低挥发性的活性稀释剂取代气味大、对环境污染严重的苯乙烯，具有气味小，浸渍烘焙时间短，因而环保节能；粘度小，适合室温下浸渍；胶凝时间短，固化过程中浸渍树脂流失少；贮存期长；耐候性好；其固化物机械性能好，电性能优异等特点。
为了解决上述技术问题，本发明提供了一种储存稳定的H级高压无溶剂浸渍漆，包括重量份数比为20～60：90～120：2～40：0～5：0～5：0～5：0～5：20～300的耐热型环氧树脂、环氧树脂、固化剂、阻聚剂、引发剂、固化促进剂、增韧剂和活性稀释剂；
所述耐热型环氧树脂选自缩水甘油醚类环氧树脂、缩水甘油酯类环氧树脂和缩水甘油胺类环氧树脂中的至少一种；
所述环氧树脂选自双酚类环氧树脂和脂环族环氧树脂中的至少一种；
所述活性稀释剂选自双官能团活性稀释剂，所述双官能团活性稀释剂含有两个活性官能团，其中，两个活性官能团为两个双键、双键+环氧或两个环氧官能团。
优选地，所述缩水甘油醚类环氧树脂为间苯二酚型环氧树脂、间苯二酚-甲醛型环氧树脂、邻甲酚甲醛环氧树脂、酚醛型环氧树脂、三酚基甲烷三缩水甘油醚环氧树脂和均苯三酚三缩水甘油醚环氧树脂中的至少一种；
缩水甘油酯类环氧树脂为邻苯二甲酸二缩水甘油酯、间苯二甲酸二缩水甘油酯、对苯二甲酸二缩水甘油酯、四氢邻苯二甲酸二缩水甘油酯、六氢邻苯二甲酸二缩水甘油酯、1,2-环氧环己烷-4,5-二甲酸二缩水甘油酯、内亚甲基四氢邻苯二甲酸二缩水甘油酯和均苯三酸三缩水甘油酯中的至少一种。
所述缩水甘油胺类环氧树脂为对氨基苯酚三缩水甘油基环氧树脂、氨基四官能环氧树脂、三聚氰酸环氧树脂、二甲基海因二缩水甘油胺型环氧树脂和1,3-二缩水甘油-5,5-二甲基海因环氧树脂中的至少一种。
优选地，所述双酚类环氧树脂为双酚A型环氧树脂、双酚F型环氧树脂、双酚AD型环氧树脂、双酚S型环氧树脂和氢化双酚A型环氧树脂中的至少一种；
所述脂环族环氧树脂为3,4-环氧基-6-甲基环己甲酸-3’,4’-环氧基-6’-甲基环己甲酯、3,4-环氧基环己甲酸-3’,4’-环氧基环己甲酯、二氧化乙烯基环己烯、二氧化双环戊二烯、二氧化双环戊烯基醚和二甲基代乙烯基环己烯二环氧化物中的至少一种。
优选地，所述固化剂选自线性酚醛树脂固化剂和聚酯树脂固化剂中的至少一种；
所述阻聚剂为对苯二酚、对叔丁基邻苯二酚、硝基苯和2,4,6-三硝基苯酚中的至少一种；
所述引发剂为过氧化苯甲酰、过氧化二异丙苯、过氧化二碳酸双(2-苯基乙氧基)酯和过氧化二碳酸二环己酯中的至少一种；
所述固化促进剂为乙酰丙酮铝、乙酰丙酮铬、环烷酸锌和环烷酸钴中的至少一种；
所述增韧剂为聚醚醇。
优选地，所述活性稀释剂选自二烯丙酯类活性稀释剂、二丙烯酸酯类活性稀释剂、丙烯酸缩水甘油酯类活性稀释剂、乙烯基环己烯类环氧稀释剂、乙烯基苯基缩水甘油醚活性稀释剂、烯丙基缩水甘油醚类活性稀释剂和二缩水甘油基类活性稀释剂中的至少一种。
优选地，含有两个双键活性官能团的所述活性稀释剂选自间苯二甲酸二烯丙酯、邻苯二甲酸二烯丙酯、对苯二甲酸二烯丙酯、二苯醚二甲酸二烯丙酯、1,3-丁二醇二甲基丙烯酸酯、1,4-丁二醇二甲基丙烯酸酯、1,3-丁二醇二丙烯酸酯、1,4-丁二醇二丙烯酸酯、乙二醇二甲基二丙烯酸酯、乙二醇二丙烯酸酯、二乙二醇二甲基丙烯酸酯、二乙二醇二丙烯酸酯、三乙二醇二甲基丙烯酸酯、三乙二醇二丙烯酸酯、1,6-己二醇二甲基丙烯酸酯、1,6-己二醇二丙烯酸酯、新戊二醇二甲基丙烯酸酯、新戊二醇二丙烯酸酯、二丙二醇二甲基丙烯酸酯、二丙二醇二丙烯酸酯、三丙二醇二甲基丙烯酸酯、三丙二醇二丙烯酸酯、三聚氰酸三烯丙酯、二甲基丙烯酸双酚A酯和三甲基丙烯酸三羟甲基丙烷酯中的至少一种。
优选地，含有双键+环氧活性官能团的所述活性稀释剂选自甲基丙烯酸缩水甘油酯、1，2-单环氧-4-乙烯基环己烯、1,2,8,9-双环氧-4-乙烯基环己烯、2-乙烯基苯基缩水甘油醚、4-甲基-2-乙烯基苯基缩水甘油醚和烯丙基缩水甘油醚中的至少一种。
优选地，含有两个环氧活性官能团的所述活性稀释剂选自二缩水甘油醚、聚乙醇二缩水甘油醚、聚丙二醇二缩水甘油醚、丁二醇二缩水甘油醚、二缩水甘油基苯胺、邻苯二酚二缩水甘油醚和2,6-二缩水甘油苯基缩水甘油醚中的至少一种。
本发明还提供了上述的储存稳定的H级高压无溶剂浸渍漆的制备方法，包括：将耐热型环氧树脂和环氧树脂混合加热至115-120℃，搅拌均匀后，加入固化剂，继续搅拌均匀；然后降温至75～85℃，加入引发剂、阻聚剂、固化促进剂和增韧剂，搅拌溶解均匀后，降温至55～65℃加入活性稀释剂，继续搅拌，得到H级高压无溶剂浸渍漆。
本发明还提供了上述的储存稳定的H级高压无溶剂浸渍漆在电机绝缘处理中的应用。
本发明与现有技术相比，具有如下有益效果：
本发明的浸渍漆能够达到H级耐热等级，本发明采用原料来源广泛，成本相对比较低廉的环氧树脂体系，通过耐热性环氧树脂和普通环氧树脂、耐热固化剂、双官能团活性稀释剂的复配及配比设计，使得整个无溶剂浸渍漆储存稳定，粘度低，便于低温浸渍，凝胶时间短，节能环保，降低对人体健康伤害；该浸渍漆能够用于高压电机真空浸渍，少量高压电机浸渍烘焙后，进行电机绝缘性能测试，满足性能设计要求。
具体实施方式
为使本发明更明显易懂，兹以优选实施例，作详细说明如下。
实施例1
一种储存稳定的H级高压无溶剂浸渍漆，配比如下：
制备方法：将脂环环氧树脂和酚醛型环氧树脂混合加热至120℃左右，搅拌均匀后，加入线性酚醛树脂固化剂，继续搅拌均匀；然后降温至80℃左右，加入引发剂过氧化苯甲酰和固化促进剂乙酰丙酮铬，搅拌溶解均匀后，降温至60℃左右加入活性稀释剂邻苯二甲酸二烯丙酯，继续搅拌，得到H级高压无溶剂浸渍漆。
实施例2
一种储存稳定的H级高压无溶剂浸渍漆，配比如下：
制备方法：将脂环环氧树脂和酚醛型环氧树脂混合加热至120℃左右，搅拌均匀后，加入线性酚醛树脂固化剂，继续搅拌均匀；然后降温至80℃左右，加入引发剂过氧化苯甲酰和固化促进剂乙酰丙酮铝，搅拌溶解均匀后，降温至60℃左右加入活性稀释剂三乙二醇二丙烯酸酯，继续搅拌，得到H级高压无溶剂浸渍漆。
实施例3
制备方法：将脂环环氧树脂和酚醛型环氧树脂混合加热至120℃左右，搅拌均匀后，加入线性酚醛树脂固化剂，继续搅拌均匀；然后降温至80℃左右，加入引发剂过氧化二异丙苯和固化促进剂乙酰丙酮铝，搅拌溶解均匀后，降温至60℃左右加入活性稀释剂1,4-丁二醇二甲基丙烯酸酯，继续搅拌，得到H级高压无溶剂浸渍漆。
实施例1～3中的H级高压无溶剂浸渍漆的性能测试：
粘度测试和凝胶时间的测试方法按GB/T15022进行，分别采用旋转粘度计法和自动测试仪法；
储存期的测试方法：将漆置于棕色密闭容器，放置在50±1℃恒温箱中。从该容器放入恒温箱那天开始，至容器中液体不能流动的天数为储存期。
胶片介损的测试方法：用于测试固化浸渍树脂电性能的胶片制作厚度为1mm左右，固化条件为135℃下烘4h，然后升温至160℃烘16h。测试180℃下胶片的介质损耗，施加电压为1200V。
绝缘铜排制作方法及测试方法：云母带为厚0.13mm±0.02mm的玻璃布少胶粉云母带5452-1；铜排尺寸为5.6mm×22mm×500mm。将云母带半叠包绕铜排四层，单面绝缘厚度为1.04mm，然后在中间位置平包一层低阻带。将包好的铜排用两块不易变形的钢板在厚度方向夹住，同时在铜排两侧分别放一根钢条以控制厚度，然后用螺丝将两块钢板夹紧固定。将两套这样的装置放入大小合适的铁槽中，然后在真空压力浸渍罐中抽真空，真空度达到133Pa以下开始计时抽4h，输入本发明的浸渍树脂，输完后，解除真空，用干燥氮气施加500kPa～700kPa(表压)的压力5h。然后解除压力，将该装置从浸渍树脂中取出，放入170℃烘箱中烘焙15h。烘焙结束并自然冷却后，拆钢板，取出绝缘铜排，用铝箔卷包绝缘铜排制作电极，测试常温下，施加电压为1.2kV和3.6kV时的介质损耗，并计算介质损耗增量，即3.6kV下的介质损耗减去1.2kV下的介质损耗之差除以2；测试180℃下，施加电压为3.6kV时的介质损耗；最后测试绝缘铜排的击穿强度，升压速率为1kV/s。
其中，粘度、凝胶时间、储存期和胶片介损测试结果如表1所示，绝缘铜排电性能测试结果如表2所示。
表1实施例1～3中的H级高压无溶剂浸渍漆的基本性能
表2实施例1～3中的H级高压无溶剂浸渍漆的绝缘铜排电性能
Claims (10)
1.一种储存稳定的H级高压无溶剂浸渍漆，其特征在于，包括重量份数比为20～60：90～120：2～40：0～5：0～5：0～5：0～5：20～300的耐热型环氧树脂、环氧树脂、固化剂、阻聚剂、引发剂、固化促进剂、增韧剂和活性稀释剂；
所述耐热型环氧树脂选自缩水甘油醚类环氧树脂、缩水甘油酯类环氧树脂和缩水甘油胺类环氧树脂中的至少一种；
所述环氧树脂选自双酚类环氧树脂和脂环族环氧树脂中的至少一种；
所述活性稀释剂选自双官能团活性稀释剂，所述双官能团活性稀释剂含有两个活性官能团，其中，两个活性官能团为两个双键、双键+环氧或两个环氧官能团。
2.如权利要求1所述的储存稳定的H级高压无溶剂浸渍漆，其特征在于，所述缩水甘油醚类环氧树脂为间苯二酚型环氧树脂、间苯二酚-甲醛型环氧树脂、邻甲酚甲醛环氧树脂、酚醛型环氧树脂、三酚基甲烷三缩水甘油醚环氧树脂和均苯三酚三缩水甘油醚环氧树脂中的至少一种；
缩水甘油酯类环氧树脂为邻苯二甲酸二缩水甘油酯、间苯二甲酸二缩水甘油酯、对苯二甲酸二缩水甘油酯、四氢邻苯二甲酸二缩水甘油酯、六氢邻苯二甲酸二缩水甘油酯、1,2-环氧环己烷-4,5-二甲酸二缩水甘油酯、内亚甲基四氢邻苯二甲酸二缩水甘油酯和均苯三酸三缩水甘油酯中的至少一种。
所述缩水甘油胺类环氧树脂为对氨基苯酚三缩水甘油基环氧树脂、氨基四官能环氧树脂、三聚氰酸环氧树脂、二甲基海因二缩水甘油胺型环氧树脂和1,3-二缩水甘油-5,5-二甲基海因环氧树脂中的至少一种。
3.如权利要求1所述的储存稳定的H级高压无溶剂浸渍漆，其特征在于，所述双酚类环氧树脂为双酚A型环氧树脂、双酚F型环氧树脂、双酚AD型环氧树脂、双酚S型环氧树脂和氢化双酚A型环氧树脂中的至少一种；
所述脂环族环氧树脂为3,4-环氧基-6-甲基环己甲酸-3’,4’-环氧基-6’-甲基环己甲酯、3,4-环氧基环己甲酸-3’,4’-环氧基环己甲酯、二氧化乙烯基环己烯、二氧化双环戊二烯、二氧化双环戊烯基醚和二甲基代乙烯基环己烯二环氧化物中的至少一种。
4.如权利要求1所述的储存稳定的H级高压无溶剂浸渍漆，其特征在于，所述固化剂选自线性酚醛树脂固化剂和聚酯树脂固化剂中的至少一种；
所述阻聚剂为对苯二酚、对叔丁基邻苯二酚、硝基苯和2,4,6-三硝基苯酚中的至少一种；
所述引发剂为过氧化苯甲酰、过氧化二异丙苯、过氧化二碳酸双(2-苯基乙氧基)酯和过氧化二碳酸二环己酯中的至少一种；
所述固化促进剂为乙酰丙酮铝、乙酰丙酮铬、环烷酸锌和环烷酸钴中的至少一种；
所述增韧剂为聚醚醇。
5.如权利要求1所述的储存稳定的H级高压无溶剂浸渍漆，其特征在于，所述活性稀释剂选自二烯丙酯类活性稀释剂、二丙烯酸酯类活性稀释剂、丙烯酸缩水甘油酯类活性稀释剂、乙烯基环己烯类环氧稀释剂、乙烯基苯基缩水甘油醚活性稀释剂、烯丙基缩水甘油醚类活性稀释剂和二缩水甘油基类活性稀释剂中的至少一种。
6.如权利要求1所述的储存稳定的H级高压无溶剂浸渍漆，其特征在于，含有两个双键活性官能团的所述活性稀释剂选自间苯二甲酸二烯丙酯、邻苯二甲酸二烯丙酯、对苯二甲酸二烯丙酯、二苯醚二甲酸二烯丙酯、1,3-丁二醇二甲基丙烯酸酯、1,4-丁二醇二甲基丙烯酸酯、1,3-丁二醇二丙烯酸酯、1,4-丁二醇二丙烯酸酯、乙二醇二甲基二丙烯酸酯、乙二醇二丙烯酸酯、二乙二醇二甲基丙烯酸酯、二乙二醇二丙烯酸酯、三乙二醇二甲基丙烯酸酯、三乙二醇二丙烯酸酯、1,6-己二醇二甲基丙烯酸酯、1,6-己二醇二丙烯酸酯、新戊二醇二甲基丙烯酸酯、新戊二醇二丙烯酸酯、二丙二醇二甲基丙烯酸酯、二丙二醇二丙烯酸酯、三丙二醇二甲基丙烯酸酯、三丙二醇二丙烯酸酯、三聚氰酸三烯丙酯、二甲基丙烯酸双酚A酯和三甲基丙烯酸三羟甲基丙烷酯中的至少一种。
7.如权利要求1所述的储存稳定的H级高压无溶剂浸渍漆，其特征在于，含有双键+环氧活性官能团的所述活性稀释剂选自甲基丙烯酸缩水甘油酯、1，2-单环氧-4-乙烯基环己烯、1,2,8,9-双环氧-4-乙烯基环己烯、2-乙烯基苯基缩水甘油醚、4-甲基-2-乙烯基苯基缩水甘油醚和烯丙基缩水甘油醚中的至少一种。
8.如权利要求1所述的储存稳定的H级高压无溶剂浸渍漆，其特征在于，含有两个环氧活性官能团的所述活性稀释剂选自二缩水甘油醚、聚乙醇二缩水甘油醚、聚丙二醇二缩水甘油醚、丁二醇二缩水甘油醚、二缩水甘油基苯胺、邻苯二酚二缩水甘油醚和2,6-二缩水甘油苯基缩水甘油醚中的至少一种。
9.权利要求1～8中任意一项所述的储存稳定的H级高压无溶剂浸渍漆的制备方法，其特征在于，包括：将耐热型环氧树脂和环氧树脂混合加热至115-120℃，搅拌均匀后，加入固化剂，继续搅拌均匀；然后降温至75～85℃，加入引发剂、阻聚剂、固化促进剂和增韧剂，搅拌溶解均匀后，降温至55～65℃加入活性稀释剂，继续搅拌，得到H级高压无溶剂浸渍漆。
10.权利要求1～8中任意一项所述的储存稳定的H级高压无溶剂浸渍漆在电机绝缘处理中的应用。
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