CN104530947A - 一种新型水性聚酰胺基聚氨酯木器涂料及其制备方法 - Google Patents

一种新型水性聚酰胺基聚氨酯木器涂料及其制备方法 Download PDF

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CN104530947A
CN104530947A CN201410755409.4A CN201410755409A CN104530947A CN 104530947 A CN104530947 A CN 104530947A CN 201410755409 A CN201410755409 A CN 201410755409A CN 104530947 A CN104530947 A CN 104530947A
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polyamide resin
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李传宏
操昭云
黎群
李颖
陈桂斌
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ANQING HAOYE RESIN MATERIAL SCIENCE & TECHNOLOGY Co Ltd
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Abstract

本发明属于涂料领域，公开一种新型水性聚酰胺基聚氨酯木器涂料及其制备方法，该木器涂料由以下组分含量的原料组成：聚酰胺树脂多元醇25-35％、大分子多元醇10-20％、异氰酸酯30-40％、二元醇扩链剂3-5％、三元醇扩链剂2-4％、二羟甲基丙酸5-8％、三乙胺3-5％、后扩链剂2-4％、有机铋0.1-0.4％、有机硅偶联剂0.2-0.5％、增稠剂0.1-0.3％、流平剂0.1-0.3％。本发明产品为水性涂料，无味、节能、环保；硬度高，表面坚硬，耐磨性好，涂膜柔韧，涂膜清澈透明，具有良好的耐黄变性；耐热，耐高温，耐水解性好；附着力强、涂膜湿润，不油腻；施工简单方便。

Description

一种新型水性聚酰胺基聚氨酯木器涂料及其制备方法
技术领域
本发明属于涂料领域，涉及一种木器涂料，具体是一种新型水性聚酰胺基聚氨酯木器涂料及其制备方法。
背景技术
木材制品包括实木及人造板的制品，木制品上所用的涂料统称为木器涂料，它包括家具、门窗、护墙板、地板、日常生活用品、木制乐器、体育用品、文具、儿童玩具等所选用涂料，一般来说木器涂料以家具涂料为主。目前，高性能和低VOC含量相结合的水性聚氨酯涂料，由于聚氨酯分子具有裁剪性，结合新的合成和交联技术，可以有效控制涂料的组成和结构，从而使其具有良好的低温成膜性、耐高温回黏性、高强度、耐磨性、环保性等，因此成为发展最快的涂料品种之一。
水性木器涂料的类型主要有醇酸类、丙烯酸类、聚氨酯类及丙烯酸-聚氨酯类，其中聚氨酯类及丙烯酸-聚氨酯类是主要的。水性醇酸类具有良好的渗透性、流动性和丰满度，多用于生产色漆，但其干性较差，保光性不好。水性丙烯酸类多数是乳液型，最大优点是保光、保色性好，耐水性好，树脂分子中不含或含有亲水基，多数应用门窗等户外使用，缺点是涂膜不丰满，耐粘连性不佳、不好打磨。水性聚氨酯是综合性能优秀的合成树脂，是现代水性树脂研究的热点之一。水性聚氨酯木器涂料的某些性能与溶剂型聚氨酯木器涂料还存在一定差距，但其具有无污染、安全可靠机械性能优良，与颜料、染料的相容性好，且不易损伤被涂饰表面，易于改性等优点，如今正逐步代替溶剂型聚氨酯木器涂料。
现有技术水性涂料作为木器涂料在耐溶剂性能、耐水解性能、耐磨性能、附着力性能性能与溶剂型涂料相比还有很大的不足。
发明内容
本发明的目的在于克服一般水性涂料作为木器涂料在耐溶剂性能、耐水解性能、耐磨性能、附着力性能性能与溶剂型涂料相比的不足，提供一种新型水性聚酰胺基聚氨酯木器涂料及其制备方法。
本发明的目的可以通过以下技术方案实现：
一种新型水性聚酰胺基聚氨酯木器涂料，该木器涂料由以下组分含量的原料组成：聚酰胺树脂多元醇25-35％、大分子多元醇10-20％、异氰酸酯30-40％、二元醇扩链剂3-5％、三元醇扩链剂2-4％、二羟甲基丙酸5-8％、三乙胺3-5％、后扩链剂2-4％、有机铋0.1-0.4％、有机硅偶联剂0.2-0.5％、增稠剂0.1-0.3％、流平剂0.1-0.3％。
优选地，所述大分子多元醇为聚四氢呋喃与聚碳酸酯二醇以任意比例的混合；所述异氰酸酯为二苯甲烷二异氰酸酯；所述二元醇扩链剂为1，4丁二醇或新戊二醇；所述三元醇扩链剂为三羟甲基丙烷；所述后扩链剂为二乙烯三胺。
本发明所述聚酰胺树脂多元醇、聚四氢呋喃、聚碳酸酯二醇为分子量1000-1500范围的大分子。
本发明还提供了一种制备新型水性聚酰胺基聚氨酯木器涂料的方法，该方法包括以下具体步骤：
制备聚酰胺树脂多元醇：
向反应容器中加入二元酸，升温至140～180℃；
缓慢加入二元胺，控制反应温度为100～180℃，反应3h；
升温至180℃，脱水30min；
降温至130℃，加入醇胺和抗氧剂，反应3h；
加入吡咯烷酮，再升温至150～250℃，脱水30min；
脱水结束升温至200～230℃，抽真空1h，即得聚酰胺树脂多元醇。
制备木器涂料：
向反应容器中加入聚酰胺树脂多元醇、大分子多元醇、异氰酸酯与有机铋，80℃下，反应2小时；
加入二元醇扩链剂、三元醇扩链剂、二羟甲基丙酸，反应3.5小时，反应过程中加入溶剂二氧六环，二氧六环用量为聚酰胺树脂多元醇重量的10-15％；
冷却至50℃，加三乙胺中和，加水乳化，加入后扩链剂，继续反应1小时；
加有机硅偶联剂、增稠剂、流平剂，搅拌均匀，放料，得到半透明乳液产品，即水性聚酰胺基聚氨酯木器涂料。
优选地，二元酸与二元胺的重量比为4-6∶1，醇胺与二元酸的重量比为1∶3-6，抗氧剂的用量为二元酸重量的0.1-0.5％，吡咯烷酮用量为总重量的10-15％。
优选地，二元酸为葵二酸、二聚酸、己二酸中的一种或多种；所述二元胺为己二胺、环己二胺中的一种或两种；所述醇胺为异丙醇胺；所述抗氧剂为亚磷酸三苯酯。
本发明的有益效果：本发明产品为水性涂料，无味、节能、环保；硬度高，表面坚硬，耐磨性好，涂膜柔韧，涂膜清澈透明，具有良好的耐黄变性；耐热，耐高温，耐水解性好；附着力强、涂膜湿润，不油腻；施工简单方便。
具体实施方式
为了便于本领域技术人员理解，下面结合具体实施例对本发明作进一步的说明。
实施例1-制备聚酰胺树脂多元醇
原料：二元酸：葵二酸35克、己二酸30克、二聚酸70克；
二元胺：己二胺16克，环己二胺8克；
醇胺：异丙醇胺40克；
吡咯烷酮30毫升；
抗氧剂：亚磷酸三苯酯0.5克；
向反应器中先加入葵二酸、二聚酸和己二酸，在150℃下，加入己二胺、环己二胺，控制反应温度为150℃反应3小时，再升温至180℃，脱水30分钟，降温至130℃，加入异丙醇胺，同时加入亚磷酸三苯酯，反应3小时，反应过程加入溶剂吡咯烷酮以控制反应粘度。再升温至200℃脱水30分钟，脱水结束，升温至220℃，同时抽真空，以脱去未反应单体和溶剂。1小时后，反应结束，产品为淡桔黄色粘稠液体。设计分子量约为1300，经测试分析分子量为1270。
实施例2-制备聚酰胺树脂多元醇
原料：二元酸：葵二酸40克、己二酸40克、二聚酸64克；
二元胺：己二胺16克，环己二胺8克；
醇胺：异丙醇胺24克；
吡咯烷酮32毫升；
抗氧剂：亚磷酸三苯酯0.55克；
向反应器中先加入葵二酸、二聚酸和己二酸，在140℃下，加入己二胺、环己二胺，控制反应温度为150℃反应3小时，再升温至180℃，脱水30分钟，降温至130℃，加入异丙醇胺，同时加入亚磷酸三苯酯，反应3小时，反应过程加入溶剂吡咯烷酮以控制反应粘度。再升温至150℃脱水30分钟，脱水结束，升温至200℃，同时抽真空，以脱去未反应单体和溶剂。1小时后，反应结束，产品为淡桔黄色粘稠液体。设计分子量约为1200，经测试分析分子量为1100。
实施例3-制备聚酰胺树脂多元醇
原料：二元酸：葵二酸60克、二聚酸84克；
二元胺：己二胺20克，环己二胺16克；
醇胺：异丙醇胺48克；
吡咯烷酮45毫升；
抗氧剂：亚磷酸三苯酯0.6克；
向反应器中先加入葵二酸、二聚酸，在170℃下，加入己二胺、环己二胺，控制反应温度为180℃反应3小时，脱水30分钟，降温至130℃，加入异丙醇胺，同时加入亚磷酸三苯酯，反应3小时，反应过程加入溶剂吡咯烷酮以控制反应粘度。再升温至250℃脱水30分钟，脱水结束，升温至230℃，同时抽真空，以脱去未反应单体和溶剂。1小时后，反应结束，产品为淡桔黄色粘稠液体。设计分子量约为1400，经测试分析分子量为1410。
实施例4-制备木器涂料：
备料：本实施例大分子多元醇选自分子量1000-1500范围的大分子聚四氢呋喃、聚碳酸酯二醇。
异氰酸酯为二苯甲烷二异氰酸酯；二元醇扩链剂为新戊二醇；三元醇扩链剂为三羟甲基丙烷；后扩链剂为二乙烯三胺。
向反应器中加入聚酰胺树脂多元醇80克、聚四氢呋喃20克、聚碳酸酯二醇25克、二苯甲烷二异氰酸酯100克、有机铋0.5克，在80℃下，反应2小时，加入新戊二醇9克、三羟甲基丙烷6克、二羟甲基丙酸15克，反应3.5小时，反应过程加1.2克二氧六环控制粘度。冷却至50℃，加9克三乙胺中和，加水乳化(所加水的量根据现有技术确定即可)，加入二乙烯三胺9克，继续反应1小时，加热抽真空30分钟脱去溶剂，然后冷却，加1克有机硅偶联剂，0.5克增稠剂，0.5克流平剂，搅拌均匀，放料，得产品为半透明乳液。
实施例5-制备木器涂料：
向反应器中加入聚酰胺树脂多元醇75克、聚四氢呋喃15克、聚碳酸酯二醇15克、二苯甲烷二异氰酸酯90克、有机铋0.3克，在80℃下，反应2小时，加入1，4丁二醇12克、三羟甲基丙烷8克、二羟甲基丙酸15克，反应3.5小时，反应过程加1.0克二氧六环控制粘度。冷却至50℃，加10克三乙胺中和，加水乳化，加入二乙烯三胺6克，继续反应1小时，加热抽真空30分钟脱去溶剂，然后冷却，加0.6克有机硅偶联剂，0.3克增稠剂，0.3克流平剂，搅拌均匀，放料，得产品为半透明乳液。
实施例6-制备木器涂料：
向反应器中加入聚酰胺树脂多元醇105克、聚四氢呋喃25克、聚碳酸酯二醇35克、二苯甲烷二异氰酸酯120克、有机铋1.2克，在80℃下，反应2小时，加入1，4丁二醇15克、三羟甲基丙烷12克、二羟甲基丙酸24克，反应3.5小时，反应过程加1.5克二氧六环控制粘度。冷却至50℃，加15克三乙胺中和，加水乳化，加入二乙烯三胺12克，继续反应1小时，加热抽真空30分钟脱去溶剂，然后冷却，加1.5克有机硅偶联剂，0.9克增稠剂，0.9克流平剂，搅拌均匀，放料，得产品为半透明乳液。
根据实施例4-6所得产品，将其与国外同类产品性能比较，性能参数如下表1。
表1本发明产品与国外同类产品性能比较
RTU-3是本发明产品，对照是立邦公司净味120水性木器清漆产品。
从表1中数据可看出，本产品为交联结构主，要指标均达到新加波立邦公司产品水平。而且在耐溶剂和耐水解方面优于立邦公司产品。
以上内容仅仅是对本发明所作的举例和说明，所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代，只要不偏离发明或者超越本权利要求书所定义的范围，均应属于本发明的保护范围。

Claims (5)

1.一种新型水性聚酰胺基聚氨酯木器涂料，其特征在于，该木器涂料由以下组分含量的原料组成：聚酰胺树脂多元醇25-35％、大分子多元醇10-20％、异氰酸酯30-40％、二元醇扩链剂3-5％、三元醇扩链剂2-4％、二羟甲基丙酸5-8％、三乙胺3-5％、后扩链剂2-4％、有机铋0.1-0.4％、有机硅偶联剂0.2-0.5％、增稠剂0.1-0.3％、流平剂0.1-0.3％。
2.根据权利要求1所述的新型水性聚酰胺基聚氨酯木器涂料，其特征在于，所述大分子多元醇为聚四氢呋喃与聚碳酸酯二醇以任意比例的混合；所述异氰酸酯为二苯甲烷二异氰酸酯；所述二元醇扩链剂为1，4丁二醇或新戊二醇；所述三元醇扩链剂为三羟甲基丙烷；所述后扩链剂为二乙烯三胺。
3.一种制备权利要求1或2所述新型水性聚酰胺基聚氨酯木器涂料的方法，其特征在于，该方法包括以下具体步骤：
(1)、制备聚酰胺树脂多元醇：
向反应容器中加入二元酸，升温至140～180℃；
缓慢加入二元胺，控制反应温度为100～180℃，反应3h；
升温至180℃，脱水30min；
降温至130℃，加入醇胺和抗氧剂，反应3h；
加入吡咯烷酮，再升温至150～250℃，脱水30min；
脱水结束升温至200～230℃，抽真空1h，即得聚酰胺树脂多元醇。
(2)、制备木器涂料：
向反应容器中加入聚酰胺树脂多元醇、大分子多元醇、异氰酸酯与有机铋，80℃下，反应2小时；
加入二元醇扩链剂、三元醇扩链剂、二羟甲基丙酸，反应3.5小时，反应过程中加入溶剂二氧六环，二氧六环用量为聚酰胺树脂多元醇重量的10-15％；
冷却至50℃，加三乙胺中和，加水乳化，加入后扩链剂，继续反应1小时；
加有机硅偶联剂、增稠剂、流平剂，搅拌均匀，放料，得到半透明乳液产品。
4.根据权利要求3所述的方法，其特征在于，所述步骤(1)中二元酸与二元胺的重量比为4-6∶1，醇胺与二元酸的重量比为1∶3-6，抗氧剂的用量为二元酸重量的0.1-0.5％，吡咯烷酮用量为总重量的10-15％。
5.根据权利要求4所述的方法，其特征在于，所述二元酸为葵二酸、二聚酸、己二酸中的一种或多种；所述二元胺为己二胺、环己二胺中的一种或两种；所述醇胺为异丙醇胺；所述抗氧剂为亚磷酸三苯酯。
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