CN111995730A - 一种水性聚氨酯、水性聚氨酯涂料及其制备方法 - Google Patents

一种水性聚氨酯、水性聚氨酯涂料及其制备方法 Download PDF

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CN111995730A
CN111995730A CN202010913024.1A CN202010913024A CN111995730A CN 111995730 A CN111995730 A CN 111995730A CN 202010913024 A CN202010913024 A CN 202010913024A CN 111995730 A CN111995730 A CN 111995730A
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朱忠敏
钱泽荣
叶小明
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DONGLAI COATING TECHNOLOGY (SHANGHAI) CO LTD
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Abstract

本发明涉及一种水性聚氨酯，其制备原料包括以下组分：按重量份计，聚碳酸亚丙酯多元醇(PPC)1000份、甲苯二异氰酸酯(TDI)160‑180份、异氟尔酮二异氰酸酯(IPDI)140‑160份、二羟甲基丙酸(DMPA)40‑60份、三羟甲基丙烷(TMP)70‑90份、1,6‑己二醇(HDO)70‑90份、中和试剂25‑35份、催化剂3‑7份，以及占原料总体质量2‑10％的硅烷偶联剂。本发明采用硅烷偶联剂进行乳化反应形成含硅氧烷的基团，将基团水解后连接到水性聚氨酯分子链上。形成稳定的预聚体，解决传统水性聚氨酯耐水性不足、耐溶剂性差等缺点。

Description

一种水性聚氨酯、水性聚氨酯涂料及其制备方法
技术领域
本发明属于水性涂料领域，尤其是涉及一种水性聚氨酯、水性聚氨酯涂料及其制备方法。
背景技术
近年来，由于人们对环境保护的重视，水性技术在传统领域的应用成为一个新的热点。在传统的涂料、粘合剂领域目前还大量采用溶剂型高分子材料，这些材料在使用过程中会有大量的有机溶剂挥发进入大气，经过复杂的光化学反应最终形成所谓的光化学烟雾，影响到人的健康及农业生产。涂料以及粘合剂的水性化已经成为未来发展的一个趋势。水性聚氨酯材料由于具有良好的综合性能，同时具有环保性，因而在涂料、粘合剂、皮革涂饰剂等行业得到广泛的应用。
然而，由于水性聚氨酯分子链中含有亲水基团导致其耐水性较差，线性的水性聚氨酯分子链形成的材料，其耐溶剂性及机械性能也不理想。因此，对水性聚氨酯材料进行改性，是近年来的一大重要课题。因此，如何在合成的步骤中提高水性聚氨酯自身的性能，弥补水性聚氨酯的性能缺陷，是亟待解决的技术问题。
发明内容
本发明的目的就是为了弥补水性聚氨酯的性能缺陷而提供一种水性聚氨酯、水性聚氨酯涂料及其制备方法。
本发明的目的通过以下技术方案实现：
一种水性聚氨酯，其制备原料包括以下组分：按重量份计，聚碳酸亚丙酯多元醇(PPC)1000份、甲苯二异氰酸酯(TDI)160-180份、异氟尔酮二异氰酸酯(IPDI)140-160份、二羟甲基丙酸(DMPA)40-60份、三羟甲基丙烷(TMP)70-90份、1,6-己二醇(HDO)70-90份、中和试剂25-35份、催化剂3-7份，以及占原料总体质量2-10％的硅烷偶联剂。
优选地，其制备原料包括以下组分：按重量份计，聚碳酸亚丙酯多元醇(PPC)1000份、甲苯二异氰酸酯(TDI)170份、异氟尔酮二异氰酸酯(IPDI)150份、二羟甲基丙酸(DMPA)50份、三羟甲基丙烷(TMP)80份、1,6-己二醇(HDO)80份、中和试剂30份、催化剂5份，以及占原料总体质量10％的硅烷偶联剂。
优选地，所述的聚碳酸亚丙酯多元醇的分子量在3000±500，粘度在3000±100mpa.s/25℃，羟值在28±2。
优选地，所述中和试剂为三乙胺(TEA)，所述催化剂为二月桂酸二丁基锡(DBTDL)。
一种水性聚氨酯的制备方法，包括以下步骤：
(1)按配方备料；
(2)将聚碳酸亚丙酯多元醇(PPC)、甲苯二异氰酸酯(TDI)、异氟尔酮二异氰酸酯(IPDI)与二羟甲基丙酸(DMPA)混合反应制成预聚体Ⅰ；
(3)再加入三羟甲基丙烷(TMP)、1,6-己二醇(HDO)以及催化剂，反应制成预聚体Ⅱ；
(4)再加入硅烷偶联剂(KH550)水解缩合，加入中和试剂中和，加水乳化，制成预聚体Ⅲ，即得到所述的水性聚氨酯。
优选地，步骤(2)所述的反应温度为80-90℃。
优选地，步骤(3)所述的反应温度为65-75℃。
优选地，步骤(4)加水调节粘度在涂四杯(25℃)粘度20±5s范围。
一种水性聚氨酯涂料，包括上述的水性聚氨酯，具体包括以下重量份的组分：水性聚氨酯270份、成膜助剂8-10份、润湿剂1-1.5份、流平剂0.15-0.2份、增稠剂1-1.5份、消泡剂0.2-0.4份、分散剂2.5-3.5份、去离子水10-20份。
一种水性聚氨酯涂料的制备方法，包括以下步骤：
(1)加入水性聚氨酯并搅拌；
(2)加入成膜助剂和去离子水并搅拌；
(3)加入润湿剂、流平剂并搅拌；
(4)加入用去离子水稀释的增稠剂并搅拌；
(5)加入消泡剂、分散剂及余量水，充分搅拌均匀即得。
本发明采用硅烷偶联剂进行乳化反应形成含硅氧烷的基团，将基团水解后连接到水性聚氨酯分子链上，形成稳定的预聚体，解决传统水性聚氨酯耐水性不足、耐溶剂性差等缺点；硅氧烷基团在水的存在下可以产生水解缩合反应，反应条件极为温和，无需任何催化剂在常温下即可进行，形成的—Si—O—Si—键十分稳定，并且形成交联结构，可以有效地提高材料的耐溶剂性能以及机械性能。本发明将侧链含硅氧烷基团引入水性聚氨酯分子链中，乳化后通过硅氧烷基团的水解形成交联结构，这样同时为聚氨酯材料中引入了含硅基团与交联结构，极大地提高了树脂的耐水性、耐溶剂性能以及机械性能。
与现有技术相比，本发明具有以下特点：
1)通过对合成树脂的改性，从源头上找到解决水性聚氨酯性能不足的方法，并且能保证树脂性能的稳定性；
2)改性后的树脂性能优异，减少了不必要的助剂添加量，降低生产成本。
具体实施方式
下面结合具体实施例对本发明进行详细说明，但绝不是对本发明的限制。
本实施例的原料组分的规格详见表1：
表1原料厂家
Figure BDA0002663974060000031
Figure BDA0002663974060000041
实施例1
在装有搅拌器、温度计、回流冷凝管的三口瓶中先倒入1000gPPC，加入170gTDI、150gIPDI和50gDMPA，在85℃下反应2h。加入80gTMP和80gHDO，并加入催化剂5gDBTDL反应，用正胺滴定法判断反应终点，加入总体质量含量1％的KH550水解缩合以及30gTEA中和，加水乳化，既得改性水性聚氨酯①。
本实施例中，PPC为聚碳酸亚丙酯多元醇，TDI为甲苯二异氰酸酯，IPDI为异氟尔酮二异氰酸酯，DMPA为二羟甲基丙酸，TMP为三羟甲基丙烷，HDO为1,6-己二醇，DBTDL为二月桂酸二丁基锡。
实施例2
在装有搅拌器、温度计、回流冷凝管的三口瓶中先倒入1000gPPC，加入160gTDI、140gIPDI和40gDMPA，在85℃下反应2h。加入70gTMP和70gHDO，并加入催化剂3gDBTDL反应，用正胺滴定法判断反应终点，加入总体质量含量3％的KH550水解缩合以及25gTEA中和，加水乳化，既得改性水性聚氨酯②。
实施例3：
在装有搅拌器、温度计、回流冷凝管的三口瓶中先倒入1000gPPC，加入180gTDI、160gIPDI和60gDMPA，在85℃下反应2h。加入90gTMP和90gHDO，并加入催化剂7gDBTDL反应，用正胺滴定法判断反应终点，加入总体质量含量5％的KH550水解缩合以及35gTEA中和，加水乳化，既得改性水性聚氨酯③。
实施例4：
在装有搅拌器、温度计、回流冷凝管的三口瓶中先倒入1000gPPC，加入170gTDI、150gIPDI和50g DMPA，在85℃下反应2h。加入80gTMP和80gHDO，并加入催化剂5g DBTDL反应，用正胺滴定法判断反应终点，加入总体质量含量10％的KH550水解缩合以及30gTEA中和，加水乳化，既得改性水性聚氨酯④。
对比例1：
在装有搅拌器、温度计、回流冷凝管的三口瓶中先倒入1000gPPC，加入170gTDI、150gIPDI和50gDMPA，在85℃下反应2h。加入80gTMP和80gHDO，并加入催化剂5gDBTDL反应，用正胺滴定法判断反应终点，加入总体质量含量10％的KH560水解缩合以及30gTEA中和，加水乳化，既得改性水性聚氨酯⑤。
对比例2：
在装有搅拌器、温度计、回流冷凝管的三口瓶中先倒入1000gPPC，加入170gTDI、150gIPDI和50gDMPA，在85℃下反应2h。加入80gTMP和80gHDO，并加入催化剂5gDBTDL反应，用正胺滴定法判断反应终点，加入30gTEA中和，加水乳化，既得改性水性聚氨酯⑥。
将实施例①～④以及对比例①和②加入成膜助剂、去离子水、润湿剂、流平剂、增稠剂、消泡剂、分散剂高速混合均匀，制备方法如下：
(1)准备干净钢杯，加入制得的改性水性聚氨酯①～⑥270g，搅拌机开始搅动(转速600；转子要放在正中间)；
(2)dpnb 6g；dpm 3g；去离子水11g；三样分别加入一次性杯中，手动摇匀。吸管慢加入钢杯，搅拌15min；
(3)润湿剂加入1.2g；流平剂加入0.15-0.2g；分散剂加入3g(调速800转搅拌15min)；
(4)增稠剂1.2g*稀释倍数，用去离子水1:3稀释(800转搅拌15min)；
(5)消泡剂加0.3-0.6g(800转搅拌15min)；
(6)刮板看有无缩孔，刮板看有无开裂；
(7)停止搅拌，乳液重量*乳液固含量除以30％减实际加料总重量得出加水重量，300-200转30min；
(8)过滤底漆120幕；面漆180幕。
800～1000r/min转速下研磨分散3小时，既得分散均匀的水性聚氨酯涂料。
对水性聚氨酯涂料进行测试，测试方法为：
(1)耐水性测试：按照GB/T 1733-1993，对比例2中三块马口铁均出现起皱和脱落现象。
(2)储存稳定性测试：按照GB/T 6753.3-1986。
(3)附着力测试：按照GB 9286-88。
(4)硬度测试：用手工操作，按照GB 6739-86。
表2产品测试结果
耐水性 储存稳定性 附着力 硬度
实施例1 合格 30d未沉降 4B 2H
实施例2 合格 30d未沉降 5B 3H
实施例3 合格 30d未沉降 5B 3H
实施例4 合格 30d未沉降 5B 3H
对比例1 合格 30d未沉降 4B 2H
对比例2 不合格 30d有沉降 4B HB
经过对照试验，可知改性后的水性聚氨酯涂料在性能上有了较大提升，耐水性合格，储存稳定性30d未沉降，附着力以及硬度等机械性能比较好。
考虑到成本和效果等因素，KH550含量在2～10％时最合适，这是因为硅烷偶联剂属于较软的单体，它在使体系产生交联的同时在内部并不会形成小裂纹，但是当硅烷偶联剂用量超过以后，硬度有下降。可能的原因是随着偶联剂用量的增加，材料的交联程度增大，从而使得拉伸强度上升另一方面，硅烷偶联剂是较软的单体，在一定程度上对材料起内增塑作用，当偶联剂的含量达到一定比例的时候，这种内增塑作用超过交联作用，最终导致拉伸强度的上升幅度比低含量的时候小很多。并且，随着偶联剂含量的增加，体系中的低分子醇含量增加，这些低分子的存在导致表面力学性能下降。
上述的对实施例的描述是为便于该技术领域的普通技术人员能理解和使用发明。熟悉本领域技术的人员显然可以容易地对这些实施例做出各种修改，并把在此说明的一般原理应用到其他实施例中而不必经过创造性的劳动。因此，本发明不限于上述实施例，本领域技术人员根据本发明的揭示，不脱离本发明范畴所做出的改进和修改都应该在本发明的保护范围之内。

Claims (10)

1.一种水性聚氨酯，其特征在于，其制备原料包括以下组分：按重量份计，聚碳酸亚丙酯多元醇(PPC)1000份、甲苯二异氰酸酯(TDI)160-180份、异氟尔酮二异氰酸酯(IPDI)140-160份、二羟甲基丙酸(DMPA)40-60份、三羟甲基丙烷(TMP)70-90份、1,6-己二醇(HDO)70-90份、中和试剂25-35份、催化剂3-7份，以及占原料总体质量2-10％的硅烷偶联剂。
2.根据权利要求1所述的一种水性聚氨酯，其特征在于，其制备原料包括以下组分：按重量份计，聚碳酸亚丙酯多元醇(PPC)1000份、甲苯二异氰酸酯(TDI)170份、异氟尔酮二异氰酸酯(IPDI)150份、二羟甲基丙酸(DMPA)50份、三羟甲基丙烷(TMP)80份、1,6-己二醇(HDO)80份、中和试剂30份、催化剂5份，以及占原料总体质量10％的硅烷偶联剂。
3.根据权利要求1或2所述的一种水性聚氨酯，其特征在于，所述的聚碳酸亚丙酯多元醇的分子量在3000±500，粘度在3000±100mpa.s/25℃，羟值在28±2。
4.根据权利要求1或2所述的一种水性聚氨酯，其特征在于，所述中和试剂为三乙胺(TEA)，所述催化剂为二月桂酸二丁基锡(DBTDL)。
5.一种如权利要求1或2所述的水性聚氨酯的制备方法，其特征在于，包括以下步骤：
(1)按配方备料；
(2)将聚碳酸亚丙酯多元醇(PPC)、甲苯二异氰酸酯(TDI)、异氟尔酮二异氰酸酯(IPDI)与二羟甲基丙酸(DMPA)混合反应制成预聚体Ⅰ；
(3)再加入三羟甲基丙烷(TMP)、1,6-己二醇(HDO)以及催化剂，反应制成预聚体Ⅱ；
(4)再加入硅烷偶联剂(KH550)水解缩合，加入中和试剂中和，加水乳化，制成预聚体Ⅲ，即得到所述的水性聚氨酯。
6.根据权利要求5所述的水性聚氨酯的制备方法，其特征在于，步骤(2)所述的反应温度为80-90℃。
7.根据权利要求5所述的水性聚氨酯的制备方法，其特征在于，步骤(3)所述的反应温度为65-75℃。
8.根据权利要求5所述的水性聚氨酯的制备方法，其特征在于，步骤(4)加水调节粘度在涂四杯(25℃)粘度20±5s范围。
9.一种水性聚氨酯涂料，其特征在于，包括如权利要求1所述的水性聚氨酯，具体包括以下重量份的组分：水性聚氨酯270份、成膜助剂8-10份、润湿剂1-1.5份、流平剂0.15-0.2份、增稠剂1-1.5份、消泡剂0.2-0.4份、分散剂2.5-3.5份、去离子水10-20份。
10.一种如权利要求9所述的水性聚氨酯涂料的制备方法，其特征在于，包括以下步骤：
(1)加入水性聚氨酯并搅拌；
(2)加入成膜助剂和去离子水并搅拌；
(3)加入润湿剂、流平剂并搅拌；
(4)加入用去离子水稀释的增稠剂并搅拌；
(5)加入消泡剂、分散剂及余量水，充分搅拌均匀即得。
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