CN105622909B - 一种水性醇酸树脂的制备方法及其应用 - Google Patents
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Abstract
本发明公开了一种水性醇酸树脂的制备方法及其应用，水性醇酸树脂由适量的蓖麻油、多元醇、二元酸和/或酸酐、苯甲酸、松香以及酯化催化剂和带水剂等混合物反应得到；得到的水性醇酸树脂与氨基树脂、流平剂、消泡剂、附着力促进剂及催化剂等复配成绿色环保，耐水性、耐热性及机械性能优异的水性绝缘漆，特别适用于H级以下中小型电机、变压器的浸渍绝缘处理。
Description
技术领域
本发明涉及一种水性醇酸树脂的制备方法及其在水性浸渍绝缘漆中的应用；属于制漆技术领域。
背景技术
传统的浸渍绝缘漆一般以甲苯、二甲苯、苯乙烯、溶剂油等易燃易爆、有毒有害溶剂作稀释剂。这些有机溶剂在生产、施工和干燥过程中，直接排入大气，不仅造成环境污染，还对人体健康产生很大危害。据统计，每年由此排放到大气中的有机溶剂就达数万吨，造成极大的资源浪费，此外，溶剂型绝缘漆在使用和储存过程中还存在安全隐患。
水性浸渍绝缘漆采用水作溶剂，相对于传统溶剂型绝缘漆能极大地减少VOC的排放，有效降低了对环境的影响，降低职业病发生的潜在机率，以及减少火灾风险和储存隐患等优势。但目前水性绝缘漆存在以下几个缺点：1)耐水解性差，特别是水性醇酸类水性绝缘漆，漆加水后容易水解变混，甚至是乳白色，造成储存稳定性差；2)固化后机械强度不高，耐热性差；3)吸水率高，从而使其电绝缘性能差；4)在施工过程中容易出现漆瘤漆泡，表面效果差，虽降低固含能有效解决漆瘤漆泡等问题，但线圈的机械强度下降明显。
发明内容
针对现有的水性浸渍绝缘漆存在的缺陷，本发明的目的是要在于提供一种操作简单、高效、低成本的制备性能优异的水性醇酸树脂的方法。
本发明的另一个目的是在于提供所述的水性醇酸树脂的应用，水性醇酸树脂用于制备绿色环保，耐水性、耐热性及机械性能优异的水性浸渍绝缘漆。
为了实现上述技术目的，本发明提供了一种水性醇酸树脂的制备方法，该方法是将20～40份蓖麻油、20～40份多元醇、20～40份二元酸和/或酸酐、小于或等于9份苯甲酸、小于或等于9份松香，以及酯化催化剂和带水剂加入反应釜中，升温至165～185℃反应1.5～2.5h后，以10～15℃/h速率继续升温至195～215℃反应，待反应体系澄清后，进一步升温至210～220℃反应，直至体系的酸值为7～15mgKOH/g时，降温至150～180℃，并加入4～10份偏苯三酸酐反应，当体系酸值为25～45mgKOH/g时，终止反应，即得。
优选的方案，多元醇为三羟甲基丙烷、三羟甲基乙烷、丙三醇、三羟乙基异氰尿酸酯(赛克)中的至少一种。
优选的方案，二元酸为间苯二酸和/或对苯二酸。
优选的方案，酸酐为苯酐和/或顺酐。
优选的方案，酯化催化剂加入量为0.05～0.1份。
优选的方案，酯化催化剂为PC4100和/或PC4200(均可购于南京鼎晨科技发展有限公司)。
优选的方案，带水剂加入量为2～5份。
优选的方案，带水剂为甲基环己烷。
本发明还提供了所述方法制备的水性醇酸树脂的应用，将所述的水性醇酸树脂应用于制备水性绝缘漆。
优选的方案，水性醇酸树脂通过助溶剂稀释至固含量为70～85％，同时采用有机胺调节pH值至7.5～8.5，配成水性醇酸树脂溶液后，用于水性绝缘漆配方。
较优选的方案，助溶剂为乙二醇单丁醚和/或丙二醇单甲醚。
较优选的方案，有机胺为三乙胺和/或N,N-二甲基乙醇胺。
优选的方案，水性绝缘漆配方包括以下质量份组分：水性醇酸树脂溶液70～100份；氨基树脂15～30份；流平剂0.1～0.5份；消泡剂0.1～0.5份；附着力促进剂0.5～2份；催化剂0.1～0.5份。
较优选的方案，氨基树脂为部分甲醚化氨基树脂、全甲醚化氨基树脂、部分丁醚化氨基树脂中至少一种。
较优选的方案，流平剂为水性或水油两用的丙烯酸酯类流平剂和/或氟碳类流平剂。
较优选的方案，消泡剂为带有破泡或抑泡功能的炔二醇类消泡剂和/或有机硅类消泡剂。
较优选的方案，附着力促进剂为改性聚酯类高分子和/或氯代聚烯烃类化合物。
较优选的方案，催化剂为封闭型磺酸盐类化合物；封闭型磺酸盐类化合物优选为二甲基苯磺酸胺盐类、二壬基苯磺酸胺盐类、对甲基苯磺酸胺盐类中的至少一种。
本发明的水性绝缘漆的制备方法，包括以下步骤：
(1)按重量份计，将20～40份蓖麻油、20～40份多元醇、20～40份多元酸或酸酐、0～9份苯甲酸、0～9份松香、0.05～0.1份酯化催化剂加入反应釜中，再加入2～5份甲基环己烷作为带水剂；先加热升温至165～185℃反应1.5～2.5h后，以10～15℃/h的速度升温至195～215℃继续反应，反应体系变澄清后，进一步升温至210～220℃，反应至体系酸值7～15mgKOH/g，降温至150～180℃，加入4～10份偏苯三酸酐反应至终点酸值为25～45mgKOH/g；降温至110～140℃后，加入助溶剂稀释至固含量为70～85％，并用有机胺中和至pH值为7.5～8.5，得到水性醇酸树脂溶液；
(2)由制备的水性醇酸树脂溶液应用于制备水性绝缘漆，将以下组分按质量份计量，直接混合均匀，即得水性绝缘漆：水性醇酸树脂70～100份；氨基树脂15～30份；流平剂0.1～0.5份；消泡剂0.1～0.5份；附着力促进剂0.5～2份；催化剂0.1～0.5份。
本发明的水性绝缘漆适用于H级以下中小型电机、变压器的浸渍绝缘处理。
相对现有技术，本发明的技术方案带来的优点及效果：
(1)本发明的水性醇酸树脂的制备方法简单、高效、成本低，满足工业化生产要求。特别是酯化催化剂的加入，反应时间相对未增加酯化催化剂时至少缩短了一半以上，大大提高了反应效率，降低了生产成本。
(2)本发明的水性醇酸树脂制备的水性绝缘漆具有优异的性能：耐水解稳定性和耐热性好，表干速率快，且在常温及高温(135℃、155℃)下的粘结强度高，成膜后机械性能好，特别适用于H级以下中小型电机、变压器的浸渍绝缘处理。
(3)本发明的水性绝缘漆经济环保，使用时可按原漆兑水2.5～4.5倍使用，兑4倍水后仍能得到较强的机械强度(常态下螺旋线圈法测得数据＞100N)；使用时VOC可降低至30g/L，因此在实际应用中可大幅度降低使用成本和减少VOC排放。
具体实施方式
以下实施例旨在对本发明内容作进一步详细的描述，但本发明的权利要求保护范围不限于此。
实施例1
按重量份计，将20份的蓖麻油，26份丙三醇，24份苯酐，0.05份的PC4100加入反应釜中，加入2份的甲基环己烷作为带水剂，加热升温至170℃反应2h后，以10℃/h的速度升温至200℃，反应体系变澄清后升温至210℃，反应至酸值7mgKOH/g，降温至150℃，加入5份偏苯三酸酐反应至终点酸值为40mgKOH/g。降温至120℃后加入乙二醇单丁醚稀释至固含量约为80％，并用三乙胺中和至pH值为7.5，得到水性醇酸树脂溶液。
由上述方法制备而成的水性醇酸树脂溶液应用于水性绝缘漆，按下述比例配置：水性醇酸树脂溶液100份；全甲醚化氨基树脂CYMEL303 20份；部分甲醚化氨基树脂CYMEL325 5份；流平剂BYK340 0.1份；消泡剂BYK024 0.1份；消泡剂104E 0.1份；附着力促进剂Add-Bond DS 1300 2.0份；催化剂氰特cycat4045 0.3份。
所制得的水性浸渍绝缘漆性能：
实施例2
按重量份计，将30份的蓖麻油，25份三羟甲基丙烷，8份赛克，25份间苯二酸，5份对苯二甲酸，3份的苯甲酸；4份松香，0.1份的催化剂加入反应釜中，加入3份的甲基环己烷作为带水剂，加热升温至170℃反应2h后，以15℃/h的速度升温至200℃，反应体系变澄清后，升温至210℃，反应至酸值10mgKOH/g，降温至170℃，加入6份偏苯三酸酐反应至终点酸值为30mgKOH/g。降温至125℃后，加入丙二醇单甲醚，稀释至固含量约为70％，并用三乙胺与N,N-二甲基乙醇胺按1:1混合中和至pH值为8.0，得到水性醇酸树脂溶液。
由上述方法制备而成的水性醇酸树脂应用于水性绝缘漆，按下述比例配置：水性醇酸树脂溶液90份；全甲醚化氨基树脂CYMEL303 20份；丁醚化氨基树脂CYMEL683 10份；流平剂FS61 0.2份；流平剂BYK380 0.1份；消泡剂BYK025 0.2份；消泡剂BYK024 0.1份；AdVantis 510W 1.0份；Add-Bond DS 1300 0.5份；催化剂AC1095 0.4份。
所制得的水性浸渍绝缘漆产品性能：
实施例3
按重量份计，将40份的蓖麻油，24份三羟甲基丙烷，8份赛克，4份丙三醇，25份间苯二酸，5份顺酐，5份对苯二甲酸，4份的苯甲酸；2份松香，0.1份的催化剂加入反应釜中，加入5份的甲基环己烷作为带水剂，加热升温至170℃反应2h后，以10℃/h的速度升温至200℃，反应体系变澄清后，升温至210℃，反应至酸值15mgKOH/g，降温至180℃，加入7份偏苯三酸酐反应至终点酸值为45mgKOH/g。降温至140℃后加入乙二醇单丁醚稀释至固含量约为85％，并用N,N-二甲基乙醇胺中和至pH值为8.5，得到水性醇酸树脂溶液。
由上述方法制备而成的水性醇酸树脂应用于水性绝缘漆，按下述比例配置：水性醇酸树脂溶液90份；全甲醚化氨基树脂CYMEL303 21份；丁醚化氨基树脂CYMEL659 6份；流平剂BYK380 0.3份；流平剂FS31 0.1份；消泡剂BYK024 0.2份；附着力促进剂AdVantis510W 0.5份；附着力促进剂CP347W 1.0份；催化剂AC1080 0.4份。
所制得的水性浸渍绝缘漆产品性能：
实施例4
按重量份计，将30份的蓖麻油，27份三羟甲基丙烷，8份赛克，25份间苯二酸，5份顺酐，6份的苯甲酸；6份松香，0.1份的催化剂加入反应釜中，加入5份的甲基环己烷作为带水剂，加热升温至170℃反应2h后，以10℃/h的速度升温至200℃，反应体系变澄清后，升温至210℃，反应至酸值10mgKOH/g，降温至160℃，加入6份偏苯三酸酐反应至终点酸值为30mgKOH/g。降温至140℃后，加入乙二醇单丁醚稀释至固含约75％左右，并用N,N-二甲基乙醇胺中和至pH值为8.0，得到水性醇酸树脂溶液。
由上述方法制备而成的水性醇酸树脂应用于水性绝缘漆，按下述比例配置：水性醇酸树脂90份；部分甲醚化氨基树脂CYMEL325 20份；丁醚化氨基树脂CYMEL659 5份；流平剂FS61 0.1份；流平剂BYK340 0.4份；消泡剂BYK025 0.5份；附着力促进剂CP349W 1.5份；催化剂氰特cycat4045 0.3份。
所制得的水性浸渍绝缘漆产品性能：
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。
Claims (6)
1.一种水性醇酸树脂的应用，其特征在于：应用于制备水性绝缘漆；
所述水性醇酸树脂通过如下方法制备得到：将20～40份蓖麻油、20～40份多元醇、20～40份二元酸和酸酐或二元酸、小于或等于9份苯甲酸、小于或等于9份松香，以及酯化催化剂和带水剂加入反应釜中，升温至165～185℃反应1.5～2.5h后，以10～15℃/h速率继续升温至195～215℃反应，待反应体系澄清后，进一步升温至210～220℃反应，直至体系的酸值为7～15mgKOH/g时，降温至150～180℃，并加入4～10份偏苯三酸酐反应，当体系酸值为25～45mgKOH/g时，终止反应，即得；所述的二元酸为间苯二甲酸，或间苯二酸和对苯二酸；所述的酸酐为苯酐和/或顺酐；所述的多元醇为三羟甲基丙烷、三羟甲基乙烷、丙三醇中至少一种和三羟乙基异氰尿酸酯；
所述的水性醇酸树脂通过助溶剂稀释至固含量为70～85％，同时采用有机胺调节pH值至7.5～8.5，配成水性醇酸树脂溶液后，用于水性绝缘漆配方；
所述的水性绝缘漆配方包括以下质量份组分：
水性醇酸树脂溶液70～100份；
氨基树脂15～30份；
流平剂0.1～0.5份；
消泡剂0.1～0.5份；
附着力促进剂0.5～2份；
催化剂0.1～0.5份。
2.根据权利要求1所述的水性醇酸树脂的应用，其特征在于：所述的助溶剂为乙二醇单丁醚和/或丙二醇单甲醚；所述的有机胺为三乙胺和/或N,N-二甲基乙醇胺。
3.根据权利要求1所述的水性醇酸树脂的应用，其特征在于：所述的氨基树脂为部分甲醚化氨基树脂、全甲醚化氨基树脂、部分丁醚化氨基树脂中至少一种；所述的流平剂为丙烯酸酯类流平剂和/或氟碳类流平剂；所述的消泡剂为炔二醇类消泡剂和/或有机硅类消泡剂；所述的附着力促进剂为改性聚酯类高分子和/或氯代聚烯烃类化合物；所述的催化剂为封闭型磺酸盐类化合物。
4.根据权利要求3所述的水性醇酸树脂的应用，其特征在于：所述的封闭型磺酸盐类化合物为二甲基苯磺酸胺盐类、二壬基萘磺酸胺盐类、对甲基苯磺酸胺盐类中的至少一种。
5.根据权利要求1所述的水性醇酸树脂的应用，其特征在于：所述的酯化催化剂加入量为0.05～0.1份；所述的酯化催化剂为PC4100和/或PC4200。
6.根据权利要求1所述的水性醇酸树脂的应用，其特征在于：所述的带水剂加入量为2～5份；所述的带水剂为甲基环己烷。
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Effective date of registration: 20231018 Address after: 030000 area a, workshop 2, corundum Industrial Park, Jinxiu street, Yangqu Park, Taiyuan City, Shanxi Province Patentee after: Shanxi Qise Environmental Protection Technology Co.,Ltd. Address before: 410000 No. 101, building a4-1, Xinya entrepreneurship Park, Huashi village, Tongguan Town, Wangcheng District, Changsha City, Hunan Province Patentee before: HUNAN WOTE BANG'EN NEW MATERIAL Co.,Ltd. |
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