CN112646114A - 三碟烯衍生物改性聚氨酯水性树脂及其制备方法 - Google Patents

三碟烯衍生物改性聚氨酯水性树脂及其制备方法 Download PDF

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CN112646114A
CN112646114A CN202011511670.1A CN202011511670A CN112646114A CN 112646114 A CN112646114 A CN 112646114A CN 202011511670 A CN202011511670 A CN 202011511670A CN 112646114 A CN112646114 A CN 112646114A
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modified polyurethane
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张武
康伦国
姚东生
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Shaoguan Union Chemical Co Ltd
Union Foshan Chemical Co Ltd
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Union Foshan Chemical Co Ltd
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Abstract

本发明提供一种三碟烯衍生物改性聚氨酯水性树脂，按重量份计，其组成为：多异氰酸酯10.0～30.0份、多元醇2.5～10.0份、扩链剂0.5～3.0份、低聚物多元醇5.0～25.0份、二羟甲基丙酸1.5～4.5份、催化剂0.01～0.1份、2,6,14‑三氨基三蝶烯0.5～2.5份、脱水蓖麻油1.5～4.5份、丙酮6.0～15.0份、中和剂1.0～5.0份、去离子水45.0～70.0份；本发明的一种三碟烯衍生物改性聚氨酯水性树脂，具有优良的吸附能力，良好的附着力、保色性、丰满度、耐水性、耐磨性、防腐蚀性好等特点；可用于水性吸附涂料、水性木器涂料、特种功能涂料、防腐蚀涂料等。

Description

三碟烯衍生物改性聚氨酯水性树脂及其制备方法
技术领域
本发明涉及一种改性聚氨酯水性树脂及其制备方法，尤其涉及到一种三碟烯衍生物改性聚氨酯水性树脂，属于水性合成树脂技术领域。
背景技术
聚氨酯是由低聚物多元醇、小分子多元醇、多异氰酸酯和扩链剂反应而成，反应原料及工艺因素对聚氨酯材料形态有很大影响，低聚物多元醇提供软性链段，多异氰酸酯提供硬链段。聚氨酯具有良好的耐溶剂性，耐磨性和抗曲挠性，因而被广泛应用于涂料、胶黏剂、泡沫塑料、油墨及橡胶等领域。
目前，无论是家庭装修还是木器的涂饰或其他涂装等，或多或少都会产生挥发性有机物，挥发性有机物(VOCs)的无组织排放不仅会造成资源的大量浪费，还会引发环境污染，严重危害人体健康。三蝶烯及其衍生物是一类具有独特的三维刚性结构的化合物，它们在过去的20多年内受到了人们很大的关注，并已在包括分子机器、材料化学以及超分子化学等许多领域内得到了广泛的应用。利用三蝶烯丰富的反应位点和衍生位点可以制备出网状的高分子材料，而网状的自具微孔聚合物因其具有的无定形结构、高稳定性及有机微孔等特性，因而在气体吸附、氢气储存、气体分离等领域具有广泛的应用。但网状结构的自具微孔聚合物难溶于普通溶剂且易发生老化，因而大大限制了材料的推广应用。
发明内容
为解决上述所述的技术问题，本发明采用三碟烯衍生物2,6,14-三氨基三蝶烯，三碟烯能与金属离子形成配合物，其结构中含有活性基团-NH2，能与异氰酸酯反应，再引入二羟甲基丙酸DMPA，能与有机氨中和后形成稳定的水性树脂，同时加入蓖麻油，提高树脂的相容性与丰满度。
三碟烯不仅具有很好的荧光性质，同时也是一种共轭聚合物的液晶材料.另外，蝶烯具有独特的三维刚性结构，是由3个苯环通过桥连碳原子组成，其中每个苯环间的夹角均为120°，该化合物具有3个开放式富电子空腔，具有很强的配位能力。三蝶烯的骨架结构非常稳定，因此三蝶烯及其衍生物具有良好的热稳定性和化学稳定。三蝶烯的三维刚性结构可以阻止聚合物内部的聚集，从而使聚合物具有很好的溶解性，并且三蝶烯结构的引入也可以提高材料分子排列的有序性和空间上的延伸性.基于三蝶烯的多孔聚合材料，它对于氢气具有良好的吸附能力，可用作潜在的储氢材料。
本发明的首要目的提供一种三碟烯衍生物改性聚氨酯水性树脂。
本发明的另一目的提供一种三碟烯衍生物改性聚氨酯水性树脂的制备方法。
为了解决上面所述的技术问题，本发明采取以下技术方案：本发明涉及一种三碟烯衍生物改性聚氨酯水性树脂，按重量份计，其组成为：多异氰酸酯10.0～30.0份、多元醇2.5～10.0份、扩链剂0.5～3.0份、低聚物多元醇5.0～25.0份、二羟甲基丙酸1.5～4.5份、催化剂0.01～0.1份、2,6,14-三氨基三蝶烯0.5～2.5份、脱水蓖麻油1.5～4.5份、丙酮6.0～15.0份、中和剂1.0～5.0份、去离子水45.0～70.0份。
所述的多元醇为丁二醇、新戊二醇、二缩二乙二醇、1,4-环己二醇、一缩二丙二醇、2,4-二乙基-1,5-戊二醇、2-乙基-1,3-己二醇、三羟甲基丙烷、季戊四醇中的一种或几种组合。
所述的低聚物多元醇为分子量在800～3000之间的聚四氢呋喃醚二醇、聚碳酸酯多元醇、聚己内酯多元醇、聚环氧乙烷多元醇、聚醚二元醇、聚环氧丙烷多元醇中的一种或几种的组合。
所述的催化剂为二月桂酸二丁基锡。
所述的中和剂为三乙胺、氨水、二甲基乙醇胺中的一种或几种的组合。
所述的扩链剂为乙二胺、己二酸二肼、N，N-二羟基(二异丙基)苯胺中的一种或几种的组合。
所述的多异氰酸酯为甲苯二异氰酸酯、异佛尔酮二异氰酸酯、六亚甲基二异氰酸酯、苯二亚甲基二异氰酸酯、环己烷二亚甲基二异氰酸酯中的一种或几种的组合。
所述的三碟烯衍生物改性聚氨酯水性树脂的制备方法，包括以下步骤：
a、在多功能反应釜中，按配方的重量份依次加入多元醇、低聚物多元醇，加热升温至110～120℃之间真空脱水1.0～2.0h；
b、降温，然后滴加多异氰酸酯，控制温度在75℃～80℃；加入配方量的催化剂与2,6,14-三氨基三蝶烯，将温度保温在80℃～84℃反应1.5h；
c、然后加入脱水蓖麻油，将温度升温至88℃～90℃反应，视体系粘度补加丙酮，测定NCO值，当测定的值与理论设计值接近时为止；
d、继续搅拌降温，缓慢滴加中和剂，搅拌反应，加入计算量的去离子水，继续搅拌分散，在搅拌条件下加入扩链剂，先高速搅拌分散，然后改为低速搅拌，脱丙酮，过滤，即制得三碟烯衍生物改性聚氨酯水性树脂。
本发明的一种三碟烯衍生物改性聚氨酯水性树脂，具有优良的吸附能力，良好的附着力、保色性、丰满度、耐水性、耐磨性、防腐蚀性好等特点；可用于水性吸附涂料、水性木器涂料、特种功能涂料、防腐蚀涂料等。
具体实施方式
下面结合实施例对本发明的三碟烯衍生物改性聚氨酯水性树脂做进一步的描述。可以理解的是，此处所描述的具体实施例仅仅用于解释相关发明，而非对该发明的限定。
实施例1
一种三碟烯衍生物改性聚氨酯水性树脂，其制备工艺如下：
a、在多功能反应釜中，按配方的重量份依次加入1,4-环己二醇6.0份、聚四氢呋喃醚二醇16.0份，加热升温至110～120℃之间真空脱水1.5h；
b、降温，然后滴加异佛尔酮二异氰酸酯26.0份，控制温度在75℃～80℃；加入配方量的二月桂酸二丁基锡0.05份与2,6,14-三氨基三蝶烯1.2份，将温度保温在80℃～84℃反应1.5h；
c、然后加入脱水蓖麻油2.0份，将温度升温至88℃～90℃反应，视体系粘度补加丙酮12.0份，测定NCO值，当测定的值与理论设计值接近时为止；
d、继续搅拌降温，缓慢滴加三乙胺2.0份，搅拌反应，加入计算量的去离子水62.0份，继续搅拌分散，在搅拌条件下加入乙二胺1.2份，先高速搅拌分散，然后改为低速搅拌，脱丙酮，过滤，即制得三碟烯衍生物改性聚氨酯水性树脂，记为样品1。
实施例2
一种三碟烯衍生物改性聚氨酯水性树脂，其制备工艺如下：
a、在多功能反应釜中，按配方的重量份依次加入丁二醇5.0份、聚碳酸酯多元醇18.0份，加热升温至110～120℃之间真空脱水1.5h；
b、降温，然后滴加甲苯二异氰酸酯22.0份，控制温度在75℃～80℃；加入配方量的二月桂酸二丁基锡0.05份与2,6,14-三氨基三蝶烯1.0份，将温度保温在80℃～84℃反应1.5h；
c、然后加入脱水蓖麻油1.6份，将温度升温至88℃～90℃反应，视体系粘度补加丙酮11.0份，测定NCO值，当测定的值与理论设计值接近时为止；
d、继续搅拌降温，缓慢滴加氨水1.5份，搅拌反应，加入计算量的去离子水60.0份，继续搅拌分散，在搅拌条件下加入己二酸二肼1.9份，先高速搅拌分散，然后改为低速搅拌，脱丙酮，过滤，即制得三碟烯衍生物改性聚氨酯水性树脂，记为样品2。
实施例3
一种三碟烯衍生物改性聚氨酯水性树脂，其制备工艺如下：
a、在多功能反应釜中，按配方的重量份依次加入2-乙基-1,3-己二醇8.2份、聚醚二元醇20.0份，加热升温至110～120℃之间真空脱水1.5h；
b、降温，然后滴加六亚甲基二异氰酸酯30.0份，控制温度在75℃～80℃；加入配方量的二月桂酸二丁基锡0.05份与2,6,14-三氨基三蝶烯2.0份，将温度保温在80℃～84℃反应1.5h；
c、然后加入脱水蓖麻油2.4份，将温度升温至88℃～90℃反应，视体系粘度补加丙酮14.0份，测定NCO值，当测定的值与理论设计值接近时为止；
d、继续搅拌降温，缓慢滴加二甲基乙醇胺4.0份，搅拌反应，加入计算量的去离子水68.0份，继续搅拌分散，在搅拌条件下加入己二酸二肼2.2份，先高速搅拌分散，然后改为低速搅拌，脱丙酮，过滤，即制得三碟烯衍生物改性聚氨酯水性树脂，记为样品3。
性能指标测试：将上述实例中样品1、样品2、样品3与常规水性聚氨酯树脂4(对比例)，按照表1的原料配方制备成涂料，对应的涂料样品分别记为涂料1、涂料2、涂料3、涂料4，并分别测试其性能。
表1：涂料配方
原料名称 规格 用量/％
水 去离子水 15
多功能助剂 AMP-95 0.4
水性树脂 样品树脂 78.0
成膜助剂 醇酯十二 5.8
增稠剂 SN-612 0.3
消泡剂 NXZ 0.2
润湿剂 Pe100 0.3
将配置好的涂料按照相关标准，其检测的性能指标如表2所示。
附着力：按照GB/T1720-1988的规定，使用划格法进行测试；
硬度：按照GB/T6739-2006色漆和清铅笔法测定漆膜硬度；
柔韧性：按照GB/T1731-1993的规定进行检测；
耐水性：按照GB/T1733-93的规定进行检测；
耐碱性：按照GB/1763-1979的规定进行检测；
丝状腐蚀：按照丝状腐蚀(GB/T13452.4-92)的规定进行检测。
表2：涂层的性能技术指标
Figure BDA0002846583680000061
Figure BDA0002846583680000071
由表2可以看出本发明的实施例1、实施例2、实施例3样品的附着力、硬度、耐水性、柔韧性、丝状腐蚀性、丰满度等性能远远好于常规的水性聚氨酯树脂。
以上描述仅为本申请的较佳实施例以及对所运用技术原理的说明；本领域技术人员应当理解，本申请中所涉及的发明范围，并不限于上述技术特征的特定组合而成的技术方案，同时也应涵盖在不脱离所述发明构思的情况下，由上述技术特征或其等同特征进行任意组合而形成的其它技术方案。例如上述特征与本申请中公开的(但不限于)具有类似功能的技术特征进行互相替换而形成的技术方案。

Claims (8)

1.一种三碟烯衍生物改性聚氨酯水性树脂，其特征在于：所述的三碟烯衍生物改性聚氨酯水性树脂，按重量份计，其组成为：多异氰酸酯10.0～30.0份、多元醇2.5～10.0份、扩链剂0.5～3.0份、低聚物多元醇5.0～25.0份、二羟甲基丙酸1.5～4.5份、催化剂0.01～0.1份、2,6,14-三氨基三蝶烯0.5～2.5份、脱水蓖麻油1.5～4.5份、丙酮6.0～15.0份、中和剂1.0～5.0份、去离子水45.0～70.0份。
2.如权利要求1所述的一种三碟烯衍生物改性聚氨酯水性树脂，其特征在于：所述的多元醇为丁二醇、新戊二醇、二缩二乙二醇、1,4-环己二醇、一缩二丙二醇、2,4-二乙基-1,5-戊二醇、2-乙基-1,3-己二醇、三羟甲基丙烷、季戊四醇中的一种或几种组合。
3.如权利要求1所述的一种三碟烯衍生物改性聚氨酯水性树脂，其特征在于：所述的低聚物多元醇为分子量在800～3000之间的聚四氢呋喃醚二醇、聚碳酸酯多元醇、聚己内酯多元醇、聚环氧乙烷多元醇、聚醚二元醇、聚环氧丙烷多元醇中的一种或几种的组合。
4.如权利要求1所述的一种三碟烯衍生物改性聚氨酯水性树脂，其特征在于：所述的催化剂为二月桂酸二丁基锡。
5.如权利要求1所述的一种三碟烯衍生物改性聚氨酯水性树脂，其特征在于：所述的中和剂为三乙胺、氨水、二甲基乙醇胺中的一种或几种的组合。
6.如权利要求1所述的一种三碟烯衍生物改性聚氨酯水性树脂，其特征在于：所述的扩链剂为乙二胺、己二酸二肼、N，N-二羟基(二异丙基)苯胺中的一种或几种的组合。
7.如权利要求1所述的一种三碟烯衍生物改性聚氨酯水性树脂，其特征在于：所述的多异氰酸酯为甲苯二异氰酸酯、异佛尔酮二异氰酸酯、六亚甲基二异氰酸酯、苯二亚甲基二异氰酸酯、环己烷二亚甲基二异氰酸酯中的一种或几种的组合。
8.如权利要求1所述的一种三碟烯衍生物改性聚氨酯水性树脂，其特征在于：所述的制备方法，其制备工艺如下：
a、在多功能反应釜中，按配方的重量份依次加入多元醇、低聚物多元醇，加热升温至110～120℃之间真空脱水1.0～2.0h；
b、降温，然后滴加多异氰酸酯，控制温度在75℃～80℃；加入配方量的催化剂与2,6,14-三氨基三蝶烯，将温度保温在80℃～84℃反应1.5h；
c、然后加入脱水蓖麻油，将温度升温至88℃～90℃反应，视体系粘度补加丙酮，测定NCO值，当测定的值与理论设计值接近时为止；
d、继续搅拌降温，缓慢滴加中和剂，搅拌反应，加入计算量的去离子水，继续搅拌分散，在搅拌条件下加入扩链剂，先高速搅拌分散，然后改为低速搅拌，脱丙酮，过滤，即制得三碟烯衍生物改性聚氨酯水性树脂。
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