CN105585690A - 一种聚二甲基硅氧烷/端羟基聚丁二烯改性uv固化超支化聚氨酯的制备方法 - Google Patents

一种聚二甲基硅氧烷/端羟基聚丁二烯改性uv固化超支化聚氨酯的制备方法 Download PDF

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CN105585690A
CN105585690A CN201510942982.0A CN201510942982A CN105585690A CN 105585690 A CN105585690 A CN 105585690A CN 201510942982 A CN201510942982 A CN 201510942982A CN 105585690 A CN105585690 A CN 105585690A
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姚伯龙
孙常青
高旭瑞
王利魁
郑春森
李洪萍
赵海平
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Jiangnan University
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Abstract

本发明涉及一种聚二甲基硅氧烷/端羟基聚丁二烯改性UV固化超支化聚氨酯的制备方法，所述制备方法包括如下步骤：在催化剂及45℃的加热搅拌条件下，将含有两个异氰酸酯基团的脂肪族多异氰酸酯与聚二甲基硅氧烷、端羟基聚丁二烯共同反应2.5h得到产物(A)；将温度升至70℃，在催化剂及加热搅拌条件下，将小分子扩链剂单体加入反应体系，继续与产物(A)反应2.5h得到产物(B)；保持温度为70℃，在催化剂及加热搅拌条件下，将同时含有-OH和-C＝C基团的单体加入反应体系，继续与产物(B)反应3h得到产物(C)；保持温度为70℃，在催化剂及加热搅拌条件下，将季戊四醇加入反应体系，继续与产物(C)反应3.5h得到产物(D)，即制得一种聚二甲基硅氧烷/端羟基聚丁二烯改性UV固化超支化聚氨酯。本发明提升了聚氨酯涂层的附着力、耐磨性、拉伸强度、耐候性等性能，同时解决了传统聚氨酯需高温固化的缺点，所得聚合物链端具有大量双键结构，这使得所制备的树脂可室温UV固化，符合节能环保涂料的要求。<!-- 2 -->

Description

一种聚二甲基硅氧烷/端羟基聚丁二烯改性UV固化超支化聚氨酯的制备方法
技术领域
本发明涉及一种聚二甲基硅氧烷/端羟基聚丁二烯改性UV固化超支化聚氨酯的制备方法，属于光固化涂料领域。
背景介绍
UV固化涂料是一种新型节能环保涂料，具有固化快、污染小、便捷高效等优点。超支化聚合物具有不同于线性聚合物分子的高度支化的三维空间结构，其分子链末端具有大量功能性基团，具有成膜性好、黏度低、反应活性高等优点，并具有良好的物理、化学性能。UV固化涂料主要由预聚物、活性单体、光引发剂及助剂组成，其中反应单体是产品物理、化学性能的主要决定因素，对材料性能有重要影响。传统涂料树脂一般为高温固化型，固化时间长、能耗高，不符合新型节能环保涂料的要求，并且其对基材的附着力、耐有机溶剂性、耐候性等性能偏差。采用异佛尔酮二异氰酸酯(IPDI)、端羟基聚丁二烯(HTPB)、聚二甲基硅氧烷(PDMS)、季戊四醇三丙烯酸酯(PETA)、甲基丙烯酸羟乙酯(HEMA)等单体制得的改性UV固化超支化聚氨酯与传统聚氨酯相比，具有较高的附着力、拉伸强度、耐油性及耐化学品性等，且分子链末端同时具有大量双键，可在室温下UV固化成膜，耐热、耐候性能良好，在光固化涂料领域有良好的应用前景。
发明内容
本发明涉及一种聚二甲基硅氧烷/端羟基聚丁二烯改性UV固化超支化聚氨酯的制备方法，其目的在于提供一种利用异氰酸酯、液体橡胶、硅油及丙烯酸单体改性合成的具有优异的化学及力学性能的超支化聚氨酯。且在该聚合物中，聚合物链端具有大量双键结构，使得所制备的树脂可在室温下UV固化，从而避免了传统聚氨酯树脂高温固化的缺点，且耐热性、耐候性、力学性能等性能优异。
本发明的技术方案是：
聚二甲基硅氧烷/端羟基聚丁二烯改性UV固化超支化聚氨酯的制备方法，包括如下步骤：
(1)将所用异氰酸酯、聚二甲基硅氧烷、端羟基聚丁二烯、小分子扩链剂、丙烯酸单体、多元醇进行脱水处理；
(2)以摩尔份数计，将共计0.1份摩尔重量的HTPB单体及PDMS单体加入干燥洁净的四口烧瓶中，加入金属有机化合物类催化剂，通入氮气保护；
(3)将上述四口烧瓶置于油浴锅中，升温至45℃，搅拌5分钟，利用恒压滴液漏斗以2s每滴的速度滴加0.2份摩尔重量的IPDI，持续搅拌，反应2.5h；
(4)第一步反应结束后，升温至70℃，利用恒压滴液漏斗以2s每滴的速度继续向体系中滴加0.05份摩尔重量的1,4-丁二醇(BDO)，反应2.5h；
(5)第二步反应结束后，保持温度70℃，利用恒压滴液漏斗以2s每滴的速度继续将0.05～0.075份摩尔重量的PETA或HEMA滴加至反应体系，反应3h；
(6)第三步反应结束后，保持温度70℃，将0.0125份摩尔重量的季戊四醇溶解于5gN,N-二甲基甲酰胺中，利用恒压滴液漏斗以2s每滴的速度继续滴加至反应体系，反应3.5h，得到所设计的聚二甲基硅氧烷/端羟基聚丁二烯改性UV固化超支化聚氨酯。
具体实施方式
实施例1
将0.01g催化剂DBTDL、168gHTPB及60gPDMS加入洁净的四口烧瓶中，插入氮气导管、搅拌棒，将烧瓶置于45℃油浴锅中，搅拌5分钟，利用恒压滴液漏斗将44.46gIPDI以2s每滴的速度缓慢加入到四口烧瓶中，持续搅拌反应2.5h；
将油浴锅升温至70℃，利用恒压滴液漏斗将4.51gBDO以2s每滴的速度缓慢加入到反应体系中，持续搅拌反应2.5h；
保持70℃，利用恒压滴液漏斗继续将16gPETA以2s每滴的速度滴加到反应体系中，持续搅拌反应3h；
保持70℃，将1.71g季戊四醇溶解于5gN,N-二甲基甲酰胺中，利用恒压滴液漏斗以2s每滴的速度继续将其滴加至反应体系中，反应3.5h，得到所设计的聚二甲基硅氧烷/端羟基聚丁二烯改性UV固化超支化聚氨酯，即产物。
实施例2
将0.01g催化剂DBTDL、168gHTPB及60gPDMS加入洁净的四口烧瓶中，插入氮气导管、搅拌棒，将烧瓶置于45℃油浴锅中，搅拌5分钟，利用恒压滴液漏斗将44.46gIPDI以2s每滴的速度缓慢加入到四口烧瓶中，持续搅拌反应2.5h；
将油浴锅升温至70℃，利用恒压滴液漏斗将4.51gBDO以2s每滴的速度缓慢加入到反应体系中，持续搅拌反应2.5h；
保持70℃，利用恒压滴液漏斗继续将8gHEMA以2s每滴的速度滴加到反应体系中，持续搅拌反应3h；
保持70℃，将1.71g季戊四醇溶解于5gN,N-二甲基甲酰胺中，利用恒压滴液漏斗以2s每滴的速度继续将其滴加至反应体系中，反应3.5h，得到所设计的聚二甲基硅氧烷/端羟基聚丁二烯改性UV固化超支化聚氨酯，即产物。

Claims (1)

1.一种聚二甲基硅氧烷/端羟基聚丁二烯改性UV固化超支化聚氨酯的制备方法，其特征步骤为：
(1)将所用异氰酸酯、聚二甲基硅氧烷、端羟基聚丁二烯、小分子扩链剂、丙烯酸单体、多元醇进行脱水处理；
(2)以摩尔份数计，将共计0.1份摩尔重量的HTPB单体及PDMS单体加入干燥洁净的四口烧瓶中，加入金属有机化合物类催化剂，通入氮气保护；
(3)将上述四口烧瓶置于油浴锅中，升温至45℃，搅拌5分钟，利用恒压滴液漏斗以2s每滴的速度滴加0.2份摩尔重量的IPDI，持续搅拌，反应2.5h；
(4)第一步反应结束后，升温至70℃，利用恒压滴液漏斗以2s每滴的速度继续向体系中滴加0.05份摩尔重量的1,4-丁二醇(BDO)，反应2.5h；
(5)第二步反应结束后，保持温度70℃，利用恒压滴液漏斗以2s每滴的速度继续将0.05～0.075份摩尔重量的PETA或HEMA滴加至反应体系，反应3h；
(6)第三步反应结束后，保持温度70℃，将0.0125份摩尔重量的季戊四醇溶解于5gN,N-二甲基甲酰胺中，利用恒压滴液漏斗以2s每滴的速度继续滴加至反应体系，反应3.5h，得到所设计的聚二甲基硅氧烷/端羟基聚丁二烯改性UV固化超支化聚氨酯；
如权利要求所述的一种聚二甲基硅氧烷/端羟基聚丁二烯改性UV固化超支化聚氨酯的制备方法，其特征在于：
步骤(5)中所述含羟基且含大量双键的功能单体为甲基丙烯酸羟乙酯(HEMA)、季戊四醇三丙烯酸酯(PETA)中的至少一种。
CN201510942982.0A 2015-12-16 2015-12-16 一种聚二甲基硅氧烷/端羟基聚丁二烯改性uv固化超支化聚氨酯的制备方法 Pending CN105585690A (zh)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109705306A (zh) * 2018-12-13 2019-05-03 江南大学 一种uv固化聚二甲基硅氧烷基改性耐候涂料的制备方法
CN111393608A (zh) * 2019-08-21 2020-07-10 杭州师范大学 一种uv固化有机硅改性超支化聚氨酯材料的制备方法
CN112608448A (zh) * 2020-12-30 2021-04-06 江南大学 一种高弹性手感耐磨多臂型光固化树脂的制备方法
CN116285851A (zh) * 2023-04-07 2023-06-23 深圳市齐进建筑工程有限公司 一种建筑接缝密封材料及其制备工艺

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