CN107880248A - 一种室温自交联改性水性聚氨酯树脂及其制备方法 - Google Patents

一种室温自交联改性水性聚氨酯树脂及其制备方法 Download PDF

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CN107880248A
CN107880248A CN201711167763.5A CN201711167763A CN107880248A CN 107880248 A CN107880248 A CN 107880248A CN 201711167763 A CN201711167763 A CN 201711167763A CN 107880248 A CN107880248 A CN 107880248A
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polyurethane resin
room
aqueous polyurethane
temperature self
modified aqueous
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刘巧
黄军波
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Heshan River Ben Polyfat Chemical Co Ltd
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Abstract

本发明公开了一种室温自交联改性水性聚氨酯树脂及其制备方法，由以下组分按重量份数制成：多异氰酸酯(50～80份)、多元醇(100～150份)、第一扩链剂(10～20份)、第二扩链剂(3～5份)、有机铋催化剂(0.05～0.1份)、三乙胺(10～15份)、水(300～500份)、硅烷偶联剂(10～20份)；其制备方法包括以下步骤：步骤1：多元醇和多异氰酸酯在85～95℃下反应2～3h；步骤2：加入第一扩链剂和第二扩链剂在75～85℃下反应1～3h；步骤3：加入有机铋催化剂在65～75℃下反应2～3h；步骤4：降温至35～45℃加入硅烷偶联剂，并加入三乙胺中和；步骤5：加入水，获得的产物在85～95℃下反应2～3h，真空脱出丙酮即获得所述水性聚氨酯树脂。

Description

一种室温自交联改性水性聚氨酯树脂及其制备方法
技术领域
本发明涉及高分子聚合物领域，具体公开了一种室温自交联改性水性聚氨酯树脂。
背景技术
随着人们环保意识以及环保法规的加强，环境友好的水性聚氨酯的研究、开发日益受到重视，水性聚氨酯是优秀树脂的代表，是现代水性树脂研究的热点之一。
为改善水性聚氨酯树脂的性能，业界中引用了自交联法。所谓自交联法是指在水性聚氨酯成膜后，能自动进行化学反应实现交联，提高涂膜的交联度，改善涂膜的性能。因此必须对水性聚氨酯的大分子结构进行改性，使得其在成膜后能发生自动氧化交联反应和水解缩合反应，提高综合性能。该法应用较广，市场上已有相关产品应市
根据现有技术的自交联改性水性聚氨酯树脂对研磨料金刚砂的粘附力较弱，抗撕裂强度仍有欠缺，带水打磨漆膜易破损。
发明内容
本发明的目的在于克服现有技术的缺陷，提高自交联改性水性聚氨酯树脂对研磨料的粘附力，增加抗撕裂强度，克服带水打磨漆膜易破损的问题。
本发明提出一种室温交联改性水性聚氨酯树脂，该树脂水分挥发后经过一段时间放置或简单烘烤与金刚砂反应交联，显著提高附着力和成膜的撕裂强度和耐水性。
为了实现以上目的及其他目的，本发明是通过包括以下技术方案实现的：
一种室温自交联改性水性聚氨酯树脂，由以下组分按重量份数制成：
作为以上技术方案的一种改进，所述多异氰酸酯由甲苯二异氰酸酯、异佛尔酮二异氰酸酯、二苯基甲烷二异氰酸酯、1,6-己二异氰酸酯、苯二亚甲基二异氰酸酯、萘-1,5-二异氰酸酯、多亚甲基多苯基异氰酸酯、四甲基苯二亚甲基二异氰酸酯、甲基环己基二异氰酸酯和二环己基甲烷二异氰酸酯中的一种或其任意多种组成。
作为以上技术方案的一种改进，所述多元醇由聚己内酯多元醇、聚碳酸酯多元醇、聚四氢呋喃醚多元醇、聚环氧乙烷多元醇、聚环氧丙烷多元醇、端羟基聚丁二烯、聚硅氧烷多元醇和聚酯醚多元醇中的一种或其任意多种组成。
作为以上技术方案的一种改进，所述的多元醇为二元醇。
作为以上技术方案的一种改进，所述多元醇由己内酯二元醇、聚碳酸酯二元醇、聚四氢呋喃醚二元醇、聚环氧乙烷二元醇、聚环氧丙烷二元醇、端羟基聚丁二烯和聚硅氧烷二元醇中的一种或其任意多种组成。
作为以上技术方案的一种改进，所述多异氰酸酯中多异氰酸酯基团与所述多元醇中羟基基团的摩尔数之比为0.97～0.98。
作为以上技术方案的一种改进，所述第一扩链剂由二羟甲基丙酸、二羟甲基丁酸、二羟甲基戊酸和二羟甲基辛酸中的一种或其任意多种组成。
作为以上技术方案的一种改进，所述第二扩链剂由乙二醇、一缩二乙二醇、1,4-丁二醇、2,3-丁二醇、1,6-己二醇、新戊二醇、二甘醇、甘油、山梨醇、三羟甲基丙烷和二羟甲基环己烷中的一种或其任意多种组成。
作为以上技术方案的一种改进，所述有机铋催化剂由Coscat83、有机铋1610、有机铋2010、有机铋2810和有机铋2808中的一种或其任意多种组成。
作为以上技术方案的一种改进，所述硅烷偶联剂由氨基偶联剂、环氧基偶联剂和乙烯基偶联剂的一种或其任意多种组成。
本发明还公开了一种制备如上所述室温自交联改性水性聚氨酯树脂的方法，包括以下步骤：
步骤1：多元醇和多异氰酸酯在85～95℃下反应2～3h；
步骤2：再加入第一扩链剂和第二扩链剂在75～85℃下反应1～3h；
步骤3：然后加入有机铋催化剂在65～75℃下反应2～3h；
步骤4：降温至35～45℃加入硅烷偶联剂，加入三乙胺中和；
步骤5：加入水后的产物经85～95℃下反应2～3h，真空脱出丙酮即获得所述水性聚氨酯树脂。
作为以上技术方案的一种改进，在步骤2中，加入第一扩链剂和第二扩链剂的同时加入丙酮降低粘度。
作为以上技术方案的一种改进，丙酮的作用为调整反应溶液的粘度，添加量可根据反应需要酌情添加。
作为以上技术方案的一种改进，硅烷偶联剂选择失水交联慢的牌号，水分挥发后经过一段时间放置或简单烘烤产生交联。
本发明还公开了一种如上所述室温自交联改性水性聚氨酯树脂在涂料中的用途。
所述用途为将所述水性聚氨酯树脂经增稠、润湿、消泡处理后，可直接涂布。
上述所述增稠、润湿、消泡处理步骤均采用现有技术中常用方式进行。
本发明的高温交联改性水性聚氨酯树脂，引入了可自交联的硅烷偶联剂，同时与无机材料金刚砂也有润湿和交联作用。
具体实施方式
下面对本发明的具体实施例作详细介绍。
实施例1：
取10kg甲苯二异氰酸酯、10kg异佛尔酮二异氰酸酯、10kg二苯基甲烷二异氰酸酯、10kg1,6-己二异氰酸酯、10kg苯二亚甲基二异氰酸酯、10kg萘-1,5-二异氰酸酯、5kg多亚甲基多苯基异氰酸酯、5kg四甲基苯二亚甲基二异氰酸酯、5kg甲基环己基二异氰酸酯、5kg二环己基甲烷二异氰酸酯、20kg的聚己内酯多元醇、20kg聚碳酸酯多元醇、20kg聚四氢呋喃醚多元醇、20kg聚环氧乙烷多元醇、20kg聚环氧丙烷多元醇、20kg端羟基聚丁二烯、20kg聚硅氧烷多元醇和10kg聚酯醚多元醇在85～95℃下反应2～3h；加入5kg二羟甲基丙酸、5kg二羟甲基丁酸、5kg二羟甲基戊酸、5kg二羟甲基辛酸、1kg乙二醇、1kg一缩二乙二醇、1kg1,4-丁二醇、1kg 2,3-丁二醇和1kg 1,6-己二醇，并同时加入适量的丙酮在75～85℃下反应1～3h；再加入0.01kg Coscat83、0.02kg有机铋1610、0.02kg有机铋2010、0.02kg有机铋2810和0.02kg有机铋2808在65～75℃下反应2～3h；降温至35～45℃加入10kg氨基偶联剂、5kg环氧基偶联剂和5kg乙烯基偶联剂，并加入15kg三乙胺中和；最后加入500kg水，获得的产物在85～95℃下反应2～3h，真空脱出丙酮即获得所述水性聚氨酯树脂。
实施例2
取25kg甲苯二异氰酸酯、25kg异佛尔酮二异氰酸酯、20kg内酯二元醇、20kg聚碳酸酯二元醇、20kg聚四氢呋喃醚二元醇、10kg聚环氧乙烷二元醇、10kg聚环氧丙烷二元醇、10kg端羟基聚丁二烯和10kg聚硅氧烷二元醇在85～95℃下反应2～3h；加入5kg二羟甲基丙酸、5kg二羟甲基戊酸、2kg乙二醇和2kg一缩二乙二醇，并同时加入适量的丙酮在75～85℃下反应1～3h；再加入0.05kgCoscat83和有机铋2010在65～75℃下反应2～3h；降温至35～45℃,加入5kg氨基偶联剂和5kg环氧基偶联剂，并加入10kg三乙胺中和；最后加入300kg水，获得的产物在85～95℃下反应2～3h，真空脱出丙酮即获得所述水性聚氨酯树脂。
实施例3
取20kg甲苯二异氰酸酯、20kg异佛尔酮二异氰酸酯、20kg苯二亚甲基二异氰酸酯、40kg聚己内酯多元醇、40kg聚碳酸酯多元醇和40kg聚环氧乙烷多元醇在85～95℃下反应2～3h；加入5kg二羟甲基丙酸、5kg二羟甲基丁酸、5kg二羟甲基戊酸、1kg乙二醇、1kg一缩二乙二醇和1kg 2,3-丁二醇，并同时加入适量的丙酮在75～85℃下反应1～3h；再加入003kgCoscat83、003kg有机铋1610和003kg有机铋2010在65～75℃下反应2～3h；降温至35～45℃加入7kg环氧基偶联剂和7kg乙烯基偶联剂，并加入12kg三乙胺中和；最后加入400kg水，获得的产物在85～95℃下反应2～3h，真空脱出丙酮即获得所述水性聚氨酯树脂。
实施例4
取10kg苯二亚甲基二异氰酸酯、10kg萘-1,5-二异氰酸酯、10kg多亚甲基多苯基异氰酸酯、10kg四甲基苯二亚甲基二异氰酸酯、10kg甲基环己基二异氰酸酯、10kg二环己基甲烷二异氰酸酯、40kg聚碳酸酯二元醇、40kg聚环氧丙烷二元醇和40kg聚硅氧烷二元醇在85～95℃下反应2～3h；加入7kg二羟甲基戊酸、7kg二羟甲基辛酸、1kg2,3-丁二醇、1kg新戊二醇、1kg二甘醇、1kg山梨醇和1kg三羟甲基丙烷，并同时加入适量的丙酮在75～85℃下反应1～3h；再加入有机铋2810在65～75℃下反应2～3h；降温至35～45℃加入15kg氨基偶联剂，并加入12kg三乙胺中和；最后加入400kg水，获得的产物在85～95℃下反应2～3h，真空脱出丙酮即获得所述水性聚氨酯树脂。
实施例5：
取15kg1,6-己二异氰酸酯、15kg苯二亚甲基二异氰酸酯、15kg萘-1,5-二异氰酸酯、15kg甲基环己基二异氰酸酯、60kg端羟基聚丁二烯和60kg聚酯醚多元醇在85～95℃下反应2～3h；加入10kg二羟甲基丙酸、10kg二羟甲基戊酸、1kg1,6-己二醇、1kg甘油、1kg三羟甲基丙烷和1kg二羟甲基环己烷，并同时加入适量的丙酮在75～85℃下反应1～3h；再加入0.02kgCoscat83、0.02kg有机铋2810和0.02kg有机铋2808在65～75℃下反应2～3h；降温至35～45℃,加入5kg氨基偶联剂、7kg环氧基偶联剂和2kg乙烯基偶联剂，并加入12kg三乙胺中和；最后加入400kg水，获得的产物在85～95℃下反应2～3h，真空脱出丙酮即获得所述水性聚氨酯树脂。
实施例6：
取10kg异佛尔酮二异氰酸酯、10kg1,6-己二异氰酸酯、10kg苯二亚甲基二异氰酸酯、10kg四甲基苯二亚甲基二异氰酸酯、10kg甲基环己基二异氰酸酯和10kg二环己基甲烷二异氰酸酯、30kg内酯二元醇、30kg聚四氢呋喃醚二元醇、30kg端羟基聚丁二烯和30kg聚硅氧烷二元醇在85～95℃下反应2～3h；加入7kg二羟甲基丁酸、7kg二羟甲基辛酸和1kg二甘醇、1kg三羟甲基丙烷和2kg二羟甲基环己烷，并同时加入适量的丙酮在75～85℃下反应1～3h；再加入0.06kgCoscat83和0.03kg有机铋1610在65～75℃下反应2～3h；降温至35～45℃,加入8kg氨基偶联剂、3kg环氧基偶联剂和4kg乙烯基偶联剂，并加入10kg三乙胺中和；最后加入400kg水，获得的产物在85～95℃下反应2～3h，真空脱出丙酮即获得所述水性聚氨酯树脂。
本发明的上述实施例仅仅是为清楚地说明本发明所作的举例，而并非是对本发明的实施方式的限定，对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式的变化或变动，这里无法对所有的实施方式予以穷举，凡是属于本发明的技术方案所引伸出的显而易见的变化或变动仍处于本发明的保护范围之内。

Claims (10)

1.一种室温自交联改性水性聚氨酯树脂，其特征在于：所述室温自交联改性水性聚氨酯树脂由以下组分按重量份数制成：
2.根据权利要求1所述的室温自交联改性水性聚氨酯树脂，其特征在于：所述多异氰酸酯由甲苯二异氰酸酯、异佛尔酮二异氰酸酯、二苯基甲烷二异氰酸酯、1,6-己二异氰酸酯、苯二亚甲基二异氰酸酯、萘-1,5-二异氰酸酯、多亚甲基多苯基异氰酸酯、四甲基苯二亚甲基二异氰酸酯、甲基环己基二异氰酸酯和二环己基甲烷二异氰酸酯中的一种或其任意多种组成。
3.根据权利要求1所述的室温自交联改性水性聚氨酯树脂，其特征在于：所述多元醇由聚己内酯多元醇、聚碳酸酯多元醇、聚四氢呋喃醚多元醇、聚环氧乙烷多元醇、聚环氧丙烷多元醇、端羟基聚丁二烯、聚硅氧烷多元醇和聚酯醚多元醇中的一种或其任意多种组成。
4.根据权利要求1所述的室温自交联改性水性聚氨酯树脂，其特征在于：所述的多元醇为二元醇，并由己内酯二元醇、聚碳酸酯二元醇、聚四氢呋喃醚二元醇、聚环氧乙烷二元醇、聚环氧丙烷二元醇、端羟基聚丁二烯和聚硅氧烷二元醇中的一种或其任意多种组成。
5.根据权利要求1所述的室温自交联改性水性聚氨酯树脂，其特征在于：所述多异氰酸酯中多异氰酸酯基团与所述多元醇中羟基基团的摩尔数之比为0.97～0.98。
6.根据权利要求1所述的室温自交联改性水性聚氨酯树脂，其特征在于：所述第一扩链剂由二羟甲基丙酸、二羟甲基丁酸、二羟甲基戊酸和二羟甲基辛酸中的一种或其任意多种组成；所述第二扩链剂由乙二醇、一缩二乙二醇、1,4-丁二醇、2,3-丁二醇、1,6-己二醇、新戊二醇、二甘醇、甘油、山梨醇、三羟甲基丙烷和二羟甲基环己烷中的一种或其任意多种组成。
7.根据权利要求8所述的制备室温自交联改性水性聚氨酯树脂的方法，其特征在于：所述有机铋催化剂由Coscat83、有机铋1610、有机铋2010、有机铋2810和有机铋2808中的一种或其任意多种组成。
8.根据权利要求1所述的室温自交联改性水性聚氨酯树脂，其特征在于：硅烷偶联剂由氨基偶联剂、环氧基偶联剂和乙烯基偶联剂中的一种或其任意多种组成。
9.一种制备如权利要求1-8中任一项所述的室温自交联改性水性聚氨酯树脂的方法，其特征在于：包括以下步骤：
步骤1：多元醇和多异氰酸酯在85～95℃下反应2～3h；
步骤2：再加入第一扩链剂和第二扩链剂在75～85℃下反应1～3h；
步骤3：然后加入有机铋催化剂在65～75℃下反应2～3h；
步骤4：降温至35～45℃加入硅烷偶联剂，加入三乙胺中和；
步骤5：加入水后的产物经85～95℃下反应2～3h，真空脱出丙酮即获得所述水性聚氨酯树脂；
其中步骤2还包括：加入第一扩链剂和第二扩链剂的同时加入丙酮。
10.根据权利要求1-9所述的制备室温自交联改性水性聚氨酯树脂的方法，其特征在于：本发明还公开了一种如上所述室温自交联改性水性聚氨酯树脂在涂料中的用途。
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109970940A (zh) * 2019-03-19 2019-07-05 上海工程技术大学 有机硅改性水性聚氨酯分散体和由其制备的水性指甲油
CN111019075A (zh) * 2019-11-29 2020-04-17 合肥科天水性科技有限责任公司 一种阴离子水性聚氨酯树脂、其制备方法和在涂料中的用途
CN115536802A (zh) * 2022-10-31 2022-12-30 广州海豚新材料有限公司 一种水性聚乳酸改性有机硅聚氨酯及其制备方法和应用

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109970940A (zh) * 2019-03-19 2019-07-05 上海工程技术大学 有机硅改性水性聚氨酯分散体和由其制备的水性指甲油
CN109970940B (zh) * 2019-03-19 2021-10-22 上海工程技术大学 有机硅改性水性聚氨酯分散体和由其制备的水性指甲油
CN111019075A (zh) * 2019-11-29 2020-04-17 合肥科天水性科技有限责任公司 一种阴离子水性聚氨酯树脂、其制备方法和在涂料中的用途
CN115536802A (zh) * 2022-10-31 2022-12-30 广州海豚新材料有限公司 一种水性聚乳酸改性有机硅聚氨酯及其制备方法和应用

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