CN104448213A - 一种反应性异氰酸基硅烷改性水性uv固化聚氨酯预聚物的制备方法 - Google Patents

一种反应性异氰酸基硅烷改性水性uv固化聚氨酯预聚物的制备方法 Download PDF

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CN104448213A
CN104448213A CN201410796422.4A CN201410796422A CN104448213A CN 104448213 A CN104448213 A CN 104448213A CN 201410796422 A CN201410796422 A CN 201410796422A CN 104448213 A CN104448213 A CN 104448213A
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姚伯龙
李洪萍
齐家鹏
张国标
孙常青
姜峻
高旭瑞
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Jiangnan University
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Abstract

本发明涉及本发明涉及一种反应性异氰酸基硅烷改性水性UV固化聚氨酯预聚物的制备方法，所述制备方法包括如下步骤：含有两个或两个以上异氰酸(-NCO)基团的脂肪族异氰酸酯与含亲水基团的二元醇在催化剂的作用下反应得到端羟基型聚氨酯型多元醇(A)；含有两个-NCO基团的单体与同时含有-OH和-C＝C基团的单体在催化剂作用下制得端-C＝C半封端型聚氨酯(B)，将一定比例的(B)与同时含有Si元素和-NCO基团的单体均匀，再与(A)混合，在催化剂作用和一定温度下反应，制得一种反应性异氰酸基硅烷改性水性UV固化聚氨酯预聚物。

Description

一种反应性异氰酸基硅烷改性水性UV固化聚氨酯预聚物的制备方法
技术领域
本发明涉及一种反应性异氰酸基硅烷改性水性UV固化聚氨酯预聚物的制备方法的制备方法,属于水性聚氨酯涂料领域。
背景技术
水性聚氨酯是相对于溶剂型聚氨酯而言的，它是聚氨酯粒子分散在连续相(水)中的二元胶体体系，属于(AB)n型的嵌段聚合物。其本身所具有的无毒、不易燃烧、无污染、节能、安全可靠及不易擦伤被涂饰表面等优点，且易于进行物理和化学改性。水性聚氨酯预聚物挥发性有机化合物VOC含量明显降低，顺应环保理念。含硅聚氨酯树脂通过在聚氨酯树脂中引入Si元素，降低聚氨酯的表面能，增强其耐油污性、耐候性和机械性能，且具有耐高温性能，在水性聚氨酯涂料领域有巨大潜力。
发明内容
本发明涉及本发明涉及一种反应性异氰酸基硅烷改性水性UV固化聚氨酯预聚物的制备方法的制备方法，所述制备方法包括如下步骤：含有两个或两个以上异氰酸(-NCO)基团的脂肪族异氰酸酯与含亲水基团的二元醇在催化剂的作用下反应得到端羟基型聚氨酯型多元醇(A)；含有两个-NCO基团的单体与同时含有-OH和-C＝C基团的单体在催化剂作用下制得端-C＝C半封端型聚氨酯(B)，将一定比例的(B)与同时含有Si元素和-NCO基团的单体均匀，再与(A)混合，在催化剂作用和一定温度下反应，制得一种反应性异氰酸基硅烷改性水性UV固化聚氨酯预聚物的制备方法。
1.一种反应性异氰酸基硅烷改性水性UV固化聚氨酯预聚物的制备方法，其特征在于所述同时含有Si元素和-NCO基团的单体为异氰酸丙基三乙氧基硅烷。
2.一种反应性异氰酸基硅烷改性水性UV固化聚氨酯预聚物的制备方法，其特征在于所述含亲水基团二元醇为2,2-二羟甲基丙酸(DMPA)、2,2-二羟甲基丁酸(DMBA)二羟基半酯等的一种或多种混合物。
3.一种反应性异氰酸基硅烷改性水性UV固化聚氨酯预聚物的制备方法，其特征在于所述含有两个或两个以上-NCO基团的单体为异佛尔酮二异氰酸酯(IPDI)、六亚甲基二异氰酸酯(HDI)、六亚甲基二异氰酸酯(HDI)三聚体、二苯基甲烷二异氰酸酯(MDI)、甲苯二异氰酸酯(TDI)等的一种或多种混合物。
4.一种反应性异氰酸基硅烷改性水性UV固化聚氨酯预聚物的制备方法，其特征在于所述同时含有-OH和-C＝C基团的单体为丙烯酸羟乙酯(HEA)、甲基丙烯酸羟乙酯(HEMA)、季戊四醇三丙烯酸酯(PETA)等的一种或多种混合物。
具体实施方式
下列实施实例用以更详细地描述本发明方案，但本发明并不局限于实例所描述的方案。
实施例1
(1)向带有搅拌装置的三口烧瓶中加入4.69g 2,2-二羟甲基丙酸(DMPA)和4gN,N-二甲基甲酰胺(DMF)，并加热到50℃。利用恒压滴液漏斗将5.79g六亚甲基二异氰酸酯(HDI)三聚体与0.01～0.015g二月桂酸二丁基锡(DBTDL)的混合溶液缓慢滴入三口烧瓶中，0.5h内滴加完毕并继续反应2h。
(2)向带有搅拌装置的三口烧瓶中加入5.55g异佛尔酮二异氰酸酯(IPDI)，并加热到45℃。利用恒压滴液漏斗将7.45g季戊四醇三丙烯酸酯(PETA)、4g丙酮与0.01～0.015g二月桂酸二丁基锡(DBTDL)的混合溶液缓慢滴入三口烧瓶中，0.5h内滴加完毕并继续反应2h。
(3)在步骤(1)反应完毕后，将温度调整至70℃，滴加步骤(2)的产物与1.24g异氰酸丙基三乙氧基硅烷的混合溶液，1h内滴加完毕并继续反应2h。
(4)用三乙胺中和步骤(3)的产物至pH＝7～8。加水乳化,固含量为30％～50％。
实施例2
(1)向带有搅拌装置的三口烧瓶中加入4.69g2,2-二羟甲基丙酸(DMPA)和4gN,N-二甲基甲酰胺(DMF)，并加热到50℃。利用恒压滴液漏斗将5.79g六亚甲基二异氰酸酯(HDI)三聚体与0.01～0.015g二月桂酸二丁基锡(DBTDL)的混合溶液缓慢滴入三口烧瓶中，0.5h内滴加完毕并继续反应2h。
(2)向带有搅拌装置的三口烧瓶中加入5.00g异佛尔酮二异氰酸酯(IPDI)，并加热到45℃。利用恒压滴液漏斗将6.71g季戊四醇三丙烯酸酯(PETA)、4g丙酮与0.01～0.015g二月桂酸二丁基锡(DBTDL)的混合溶液缓慢滴入三口烧瓶中，0.5h内滴加完毕并继续反应2h。
(3)在步骤(1)反应完毕后，将温度调整至70℃，滴加步骤(2)的产物与1.86g异氰酸丙基三乙氧基硅烷的混合溶液，1h内滴加完毕并继续反应2h。
(4)用三乙胺中和步骤(3)的产物至pH＝7～8。加水乳化,固含量为30％～50％。
实施例3
(1)向带有搅拌装置的三口烧瓶中加入4.69g2,2-二羟甲基丙酸(DMPA)和4gN,N-二甲基甲酰胺(DMF)，并加热到50℃。利用恒压滴液漏斗将5.79g六亚甲基二异氰酸酯(HDI)三聚体与0.01～0.015g二月桂酸二丁基锡(DBTDL)的混合溶液缓慢滴入三口烧瓶中，0.5h内滴加完毕并继续反应2h。
(2)向带有搅拌装置的三口烧瓶中加入4.44g异佛尔酮二异氰酸酯(IPDI)，并加热到45℃。利用恒压滴液漏斗将5.96g季戊四醇三丙烯酸酯(PETA)、4g丙酮与0.01～0.015g二月桂酸二丁基锡(DBTDL)的混合溶液缓慢滴入三口烧瓶中，0.5h内滴加完毕并继续反应2h。
(3)在步骤(1)反应完毕后，将温度调整至70℃，滴加步骤(2)的产物与2.47g异氰酸丙基三乙氧基硅烷的混合溶液，1h内滴加完毕并继续反应2h。
(4)用三乙胺中和步骤(3)的产物至pH＝7～8。加水乳化,固含量为30％～50％。

Claims (4)

1.一种反应性异氰酸基硅烷改性水性UV固化聚氨酯预聚物，其特征在于所述同时含有Si元素和-NCO基团的单体为异氰酸丙基三乙氧基硅烷。
2.一种反应性异氰酸基硅烷改性水性UV固化聚氨酯预聚物，其特征在于所述含亲水基团二元醇为2,2-二羟甲基丙酸(DMPA)、2,2-二羟甲基丁酸(DMBA)二羟基半酯等的一种或多种混合物。
3.一种反应性异氰酸基硅烷改性水性UV固化聚氨酯预聚物，其特征在于所述含有两个或两个以上-NCO基团的单体为异佛尔酮二异氰酸酯(IPDI)、六亚甲基二异氰酸酯(HDI)、六亚甲基二异氰酸酯(HDI)三聚体、二苯基甲烷二异氰酸酯(MDI)、甲苯二异氰酸酯(TDI)等的一种或多种混合物。
4.一种反应性异氰酸基硅烷改性水性UV固化聚氨酯预聚物，其特征在于所述同时含有-OH和-C＝C基团的单体为丙烯酸羟乙酯(HEA)、甲基丙烯酸羟乙酯(HEMA)、季戊四醇三丙烯酸酯(PETA)等的一种或多种混合物。
CN201410796422.4A 2014-12-19 2014-12-19 一种反应性异氰酸基硅烷改性水性uv固化聚氨酯预聚物的制备方法 Pending CN104448213A (zh)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111154070A (zh) * 2020-01-17 2020-05-15 中国科学院长春应用化学研究所 一种含氟聚氨酯及其制备方法
CN114958089A (zh) * 2022-05-19 2022-08-30 广东阿诺捷喷墨科技有限公司 一种用于卷尺的耐磨损uv油墨、制备方法及卷尺

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CN101314629A (zh) * 2008-05-20 2008-12-03 南通万德电子工业有限公司 光硬化树脂组合物
CN102533067A (zh) * 2011-07-01 2012-07-04 深圳市美丽华油墨涂料有限公司 一种uv固化的塑胶涂料
CN102898889A (zh) * 2011-07-27 2013-01-30 深圳市纳宇材料技术有限公司 Uv固化导光油墨及使用该油墨的导光板

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101314629A (zh) * 2008-05-20 2008-12-03 南通万德电子工业有限公司 光硬化树脂组合物
CN102533067A (zh) * 2011-07-01 2012-07-04 深圳市美丽华油墨涂料有限公司 一种uv固化的塑胶涂料
CN102898889A (zh) * 2011-07-27 2013-01-30 深圳市纳宇材料技术有限公司 Uv固化导光油墨及使用该油墨的导光板

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111154070A (zh) * 2020-01-17 2020-05-15 中国科学院长春应用化学研究所 一种含氟聚氨酯及其制备方法
CN111154070B (zh) * 2020-01-17 2021-04-27 中国科学院长春应用化学研究所 一种含氟聚氨酯及其制备方法
CN114958089A (zh) * 2022-05-19 2022-08-30 广东阿诺捷喷墨科技有限公司 一种用于卷尺的耐磨损uv油墨、制备方法及卷尺

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