CN112646119A - 一种含三聚茚酮结构特种水性固化剂及其制备方法 - Google Patents

一种含三聚茚酮结构特种水性固化剂及其制备方法 Download PDF

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CN112646119A
CN112646119A CN202011511692.8A CN202011511692A CN112646119A CN 112646119 A CN112646119 A CN 112646119A CN 202011511692 A CN202011511692 A CN 202011511692A CN 112646119 A CN112646119 A CN 112646119A
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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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Abstract

本发明涉及一种含三聚茚酮结构特种水性固化剂，按重量份计,其组分为：三聚体60.0～80.0份、二羟甲基丙酸1.0～2.5份、低聚物多元醇5.0～10.0份、醇酸树脂6.0～12.0份、二月桂酸二丁基锡0.01～0.1份、多元醇1.0～3.0份、三聚茚酮衍生物2.0～5.0份、中和剂1.5～4.0份、惰性溶剂8.0～15.0份；其中，三聚茚酮衍生物由三聚茚酮与2‑羟基乙胺通过反应制得；本发明提供一种含三聚茚酮结构特种水性固化剂，具有优异的抗划伤性、抗菌性能好、荧光性好、耐化品性好、耐盐雾性良好等特点，与水性羟基组分配制的聚氨酯漆具有高硬度、漆膜抗划伤、流平性好、丰满度高等特点，制备成涂料时无需外加杀菌剂，制备成荧光涂料时无需外加荧光剂。

Description

一种含三聚茚酮结构特种水性固化剂及其制备方法
技术领域
本发明涉及一种水性固化剂，尤其涉及到一种具有良好荧光性能、抗菌性能好的含三聚茚酮结构特种水性固化剂及其制备方法，属于合成水性固化剂技术领域。
背景技术
随着工业的快速发展，环境恶化的问题已经逐渐显现出来，全社会对于绿色生产、绿色产品的发展均格外重视，政府也对这些产业出台相当严格的规定，作为绿色产品的代表之一，水性涂料是未来涂料发展的主要方向。
为了加快涂料的固化速度、提高漆膜的各项性能，需要在涂料中添加固化剂。作为涂料的重要组分，固化剂是决定涂料性能的重要因素。它直接决定着涂料的干性、物理机械性能、装饰性、耐介质性、耐久性、耐候性以及其他特种性能。因此，固化剂特种功能性代表着涂料的工业水平。
中国专利CN102911342A公开了一种含氟水性聚氨酯固化剂及其制备方法，由以下物质反应所得，按质量份包括：异氰酸酯或者其衍生物100份，含氟聚合物10～25份，含亲水基团化合物5～20份，溶剂50～120份，催化剂0.02～0.05份，中和剂0～3.9份；其无抗菌与荧光功能，具有一定的局限性，同时其有机溶剂含量较高。
中国专利CN108129635A公开了一种疏水阻燃型水性固化剂及其制备方法，其由六亚甲基二异氰酸酯、亲水性单体、低聚物多元醇、含羟基三聚氰胺衍生物、六氟异丙醇和溶剂在催化剂作用下反应、中和制得；其具有活性期长、贮存稳定性好等特点，但其在制备成涂料时，需要加入抗菌剂才具有抗菌效果，且不具备荧光性能。
国内最常用涂料固化剂是聚氨酯固化剂，要求其具有储存稳定性高、流平性好、易打磨等特点，但是，现有的水性聚氨酯固化剂存在活化期短、交联密度差、无抗菌性与荧光性能，在某些特殊领域具有一定的局限性。
发明内容
本发明的目的旨在提供一种含三聚茚酮结构特种水性固化剂。
本发明的另一目的提供一种含三聚茚酮结构特种水性固化剂的制备方法。
三聚茚酮因为共平面核以及C3对称的特性，使得广泛的树枝状大分子、星形分子、哑铃型分子被设计和合成。三聚茚酮作为功能单元具有良好的荧光特性，三聚茚酮在有机光电领域有甚至超过十多个领域的应用。
为解决上述问题本发明引入三聚茚酮，首先将三聚茚酮制备成三聚茚酮衍生物，三聚茚酮衍生物具有席夫碱结构，其具有良好的抗菌与杀菌性能，同时三聚茚酮具有良好的荧光性能。
本发明所述的一种含三聚茚酮结构特种水性固化剂，采取以下技术方案：按重量份计,其组分为：三聚体60.0～80.0份、二羟甲基丙酸1.0～2.5份、低聚物多元醇5.0～10.0份、醇酸树脂6.0～12.0份、二月桂酸二丁基锡0.01～0.1份、多元醇1.0～3.0份、三聚茚酮衍生物2.0～5.0份、中和剂1.5～4.0份、惰性溶剂8.0～15.0份。
其中，所述的三聚茚酮衍生物由三聚茚酮与2-羟基乙胺通过反应制得。
所述的三聚体为异佛尔酮二异氰酸酯三聚体、六亚甲基二异氰酸酯三聚体中的一种或两种的组合。
所述的低聚物多元醇为聚四氢呋喃多元醇、聚碳酸酯多元醇、聚醚二元醇、聚乙二醇中的一种或几种的组合；所述的低聚物多元醇平均分子量为600～1000。
所述的多元醇为1,4-环己烷二甲醇、1,4-丁二醇、三羟甲基丙烷中的一种或几种的组合。
所述的惰性溶剂为二乙二醇乙醚醋酸酯、N-甲基吡咯烷酮、丙二醇甲醚醋酸酯、丙二醇乙醚醋酸酯中的一种或几种的组合。
所述的中和剂为三乙胺、碳酸氢钠中的一种或两种的组合。
本发明提供一种含三聚茚酮结构特种水性固化剂的制备方法，包括以下步骤：
a)、预先对低聚物多元醇、惰性溶剂、多元醇进行除水干燥处理后备用；
b)、在反应器中通入氮气，按配方量加入低聚物多元醇、惰性溶剂、多元醇、三聚茚酮衍生物、二羟甲基丙酸、醇酸树脂升温搅拌溶解，加入三聚体，在80～82℃保温搅拌反应1.5～2.0h，滴加二月桂酸二丁基锡，升温至90～92℃保温反应1.0～1.5h，检测NCO值，当NCO值与设计值一致为止；
c)、降温，缓慢滴加中和剂中和，搅拌反应，分散均匀，过滤，出料，即得一种含三聚茚酮结构特种水性固化剂。
本发明提供一种含三聚茚酮结构特种水性固化剂，具有优异的抗划伤性、抗菌性能好、荧光性好、耐化品性好、耐盐雾性良好等特点，与水性羟基组分配制的聚氨酯漆具有高硬度、漆膜抗划伤、流平性好、丰满度高等特点，制备成涂料时无需外加杀菌剂，制备成荧光涂料时无需外加荧光剂。
具体实施方式
下面结合实施例对本发明的一种含三聚茚酮结构特种水性固化剂做进一步的描述。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
一种含三聚茚酮结构特种水性固化剂，按重量份计,其组分为：异佛尔酮二异氰酸酯三聚体75.0份、二羟甲基丙酸1.6份、聚四氢呋喃多元醇6.0份、醇酸树脂8.0份、二月桂酸二丁基锡0.05份、1,4-环己烷二甲醇1.8份、三聚茚酮衍生物4.0份、三乙胺2.0份、二乙二醇乙醚醋酸酯12.0份。
本实施例中一种含三聚茚酮结构特种水性固化剂的制备方法，包括以下步骤：
a)、预先对聚四氢呋喃多元醇、二乙二醇乙醚醋酸酯、1,4-环己烷二甲醇进行除水干燥处理后备用；
b)、在反应器中通入氮气，按配方量加入聚四氢呋喃多元醇、二乙二醇乙醚醋酸酯、1,4-环己烷二甲醇、三聚茚酮衍生物、二羟甲基丙酸、醇酸树脂升温搅拌溶解，加入异佛尔酮二异氰酸酯三聚体，在80～82℃保温搅拌反应2.0h，滴加二月桂酸二丁基锡，升温至90～92℃保温反应1.0h，检测NCO值，当NCO值与设计值一致为止；
c)、降温，缓慢滴加三乙胺中和，搅拌反应，分散均匀，过滤，出料，即得一种含三聚茚酮结构特种水性固化剂。
实施例2
一种含三聚茚酮结构特种水性固化剂，按重量份计,其组分为：六亚甲基二异氰酸酯三聚体65.0份、二羟甲基丙酸2.0份、聚醚二元醇7.0份、醇酸树脂7.0份、二月桂酸二丁基锡0.05份、1,4-丁二醇2.0份、三聚茚酮衍生物3.5份、碳酸氢钠2.0份、N-甲基吡咯烷酮13.0份。
本实施例中一种含三聚茚酮结构特种水性固化剂的制备方法，包括以下步骤：
a)、预先对聚醚二元醇、N-甲基吡咯烷酮、1,4-丁二醇进行除水干燥处理后备用；
b)、在反应器中通入氮气，按配方量加入聚醚二元醇、N-甲基吡咯烷酮、1,4-丁二醇、三聚茚酮衍生物、二羟甲基丙酸、醇酸树脂升温搅拌溶解，加入六亚甲基二异氰酸酯三聚体，在80～82℃保温搅拌反应1.5h，滴加二月桂酸二丁基锡，升温至90～92℃保温反应1.5h，检测NCO值，当NCO值与设计值一致为止；
c)、降温，缓慢滴加碳酸氢钠中和，搅拌反应，分散均匀，过滤，出料，即得一种含三聚茚酮结构特种水性固化剂。
实施例3
一种含三聚茚酮结构特种水性固化剂，按重量份计,其组分为：六亚甲基二异氰酸酯三聚体75.0份、二羟甲基丙酸2.5份、聚碳酸酯多元醇8.0份、醇酸树脂9.0份、二月桂酸二丁基锡0.06份、1,4-丁二醇1.5份、三羟甲基丙烷0.5份、三聚茚酮衍生物3.0份、三乙胺2.5份、丙二醇乙醚醋酸酯14.0份。
本实施例中一种含三聚茚酮结构特种水性固化剂的制备方法，包括以下步骤：
a)、预先对聚碳酸酯多元醇、丙二醇乙醚醋酸酯、1,4-丁二醇、三羟甲基丙烷进行除水干燥处理后备用；
b)、在反应器中通入氮气，按配方量加入聚碳酸酯多元醇、丙二醇乙醚醋酸酯、1,4-丁二醇、三羟甲基丙烷、三聚茚酮衍生物、二羟甲基丙酸、醇酸树脂升温搅拌溶解，加入六亚甲基二异氰酸酯三聚体，在80～82℃保温搅拌反应2.0h，滴加二月桂酸二丁基锡，升温至90～92℃保温反应1.5h，检测NCO值，当NCO值与设计值一致为止；
c)、降温，缓慢滴加三乙胺中和，搅拌反应，分散均匀，过滤，出料，即得一种含三聚茚酮结构特种水性固化剂。
对本发明的实施例与对比例(市售水性固化剂)与水性羟基丙烯酸树脂配制成水性罩光涂料后，按照相关标准，对漆膜性能进行对比检测，检测的性能指标如表1所示。
表1：水性罩光涂料性能技术指标
Figure BDA0002846582900000061
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 (7)

1.一种含三聚茚酮结构特种水性固化剂，其特征在于，所述的含三聚茚酮结构特种水性固化剂，按重量份计,其组分为：三聚体60.0～80.0份、二羟甲基丙酸1.0～2.5份、低聚物多元醇5.0～10.0份、醇酸树脂6.0～12.0份、二月桂酸二丁基锡0.01～0.1份、多元醇1.0～3.0份、三聚茚酮衍生物2.0～5.0份、中和剂1.5～4.0份、惰性溶剂8.0～15.0份；
其中，所述的三聚茚酮衍生物由三聚茚酮与2-羟基乙胺通过反应制得。
2.根据权利要求1所述的含三聚茚酮结构特种水性固化剂，其特征在于：所述的三聚体为异佛尔酮二异氰酸酯三聚体、六亚甲基二异氰酸酯三聚体中的一种或两种的组合。
3.根据权利要求1所述的含三聚茚酮结构特种水性固化剂，其特征在于：所述的低聚物多元醇为聚四氢呋喃多元醇、聚碳酸酯多元醇、聚醚二元醇、聚乙二醇中的一种或几种的组合；所述的低聚物多元醇平均分子量为600～1000。
4.根据权利要求1所述的含三聚茚酮结构特种水性固化剂，其特征在于：所述的多元醇为1,4-环己烷二甲醇、1,4-丁二醇、三羟甲基丙烷中的一种或几种的组合。
5.根据权利要求1所述的含三聚茚酮结构特种水性固化剂，其特征在于：所述的惰性溶剂为二乙二醇乙醚醋酸酯、N-甲基吡咯烷酮、丙二醇甲醚醋酸酯、丙二醇乙醚醋酸酯中的一种或几种的组合。
6.根据权利要求1所述的含三聚茚酮结构特种水性固化剂，其特征在于：所述的中和剂为三乙胺、碳酸氢钠中的一种或两种的组合。
7.根据权利要求1所述的含三聚茚酮结构特种水性固化剂，其特征在于：其制备工艺包括如下步骤：
a)、预先对低聚物多元醇、惰性溶剂、多元醇进行除水干燥处理后备用；
b)、在反应器中通入氮气，按配方量加入低聚物多元醇、惰性溶剂、多元醇、三聚茚酮衍生物、二羟甲基丙酸、醇酸树脂升温搅拌溶解，加入三聚体，在80～82℃保温搅拌反应1.5～2.0h，滴加二月桂酸二丁基锡，升温至90～92℃保温反应1.0～1.5h，检测NCO值，当NCO值与设计值一致为止；
c)、降温，缓慢滴加中和剂中和，搅拌反应，分散均匀，过滤，出料，即得一种含三聚茚酮结构特种水性固化剂。
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