CN111303753A - 一种单组分外露型快干聚氨酯防水涂料及其制备方法 - Google Patents
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Abstract
本发明公开了一种单组分外露型快干聚氨酯防水涂料及其制备方法。所述的单组分外露型快干聚氨酯防水涂料由多异氰酸酯预聚物、苯二亚甲基二异氰酸酯、聚醚多元醇、脂肪族扩链剂、颜填料及助剂制备而成,其中多异氰酸酯预聚物为苯二亚甲基二异氰酸酯与三羟甲基丙烷反应制得。该单组分聚氨酯防水涂料具有优异的耐候性,长期使用不变色,施工简便,干燥速度快,在高端工程防水领域具有广阔的应用前景。
Description
技术领域
本发明涉及一种单组分外露型快干聚氨酯防水涂料及其制备方法,属于防水涂料领域。
背景技术
聚氨酯防水涂料具有优异的耐磨、耐溶剂、耐疲劳及耐低温性能,近些年在轨道交通、大坝防水方面应用广泛,我国在该领域起步较晚,但聚氨酯防水涂料以其优异性能被业内认为是未来高端工程防水的主要材料。目前聚氨酯类防水涂料主要以芳香族产品为主,为了达到防水涂料耐候性要求,需要在芳香族涂料表面再加涂一层脂肪族防老化面漆。
采用脂肪族异氰酸酯制备聚氨酯防水涂料可显著提升其耐候性能,直接作为外露型涂料,无需加涂防老化面漆,施工工艺简便,可显著提升施工效率。目前市面常见的脂肪族异氰酸酯产品主要有六亚甲基二异氰酸酯(HDI)、4,4'-二环己基甲烷二异氰酸酯(HMDI)、异佛尔酮二异氰酸酯(IPDI)、环己烷二亚甲基二异氰酸酯(HXDI)等。从目前公布的国内外专利来看,多数脂肪族外露型聚氨酯防水涂料以HMDI或IPDI为合成原料,分为双组分和单组分两种类型。其中单组分防水涂料施工更加简便,具有更广阔的应用前景,然而HMDI和IPDI虽然具有优异的耐候性和良好的机械性能,但反应速度较慢,制备的单组分防水涂料固化速度稍慢。
国内专利CN201510360424、CN201510360699介绍了单组分湿固化型聚氨酯防水涂料,但耐候性一般;国内专利CN103994881A、CN201510959153、CN201611121394、CN201610843230中介绍了以脂肪族异氰酸酯单体为原料的耐候外露型聚氨酯防水涂料,但均以HDI、IPDI或HMDI为原料,反应速度慢,固化速度一般;国外专利JP6397430B2中以HXDI为原料制备单组分防水涂料,但合成过程需要加入醛亚胺作为封端固化剂,合成及使用过程相对复杂。
发明内容
本发明的目的在于提供一种单组分外露型快干聚氨酯防水涂料及其制备方法,该单组分聚氨酯防水涂料采用XDI作为原料,并在反应过程中创造性地加入自制多异氰酸酯预聚物,可显著提升防水涂料干燥速度,生产工艺简单,力学性能优异,施工方便。
根据本发明的第一个方面,一种单组分外露型快干聚氨酯防水涂料,其是由以下组分制备得到:
其中组分的用量为基于单组分外露型快干聚氨酯防水涂料的质量百分量。多异氰酸酯预聚物溶液的浓度范围为例如10-35wt%,优选20-25wt%。
进一步地,本发明所述的多异氰酸酯预聚物分子结构如下:
进一步地,多异氰酸酯预聚物溶液通过以下步骤来制备:将XDI溶于溶剂中(浓度至10-40wt%),加热至50~100℃,优选60~90℃,例如约80℃,向其中滴加三羟甲基丙烷的溶液(浓度例如10-25wt%),直至反应完全,体系NCO含量达到例如4.0-7.0wt%时停止反应得到多异氰酸酯预聚物,溶剂例如可以是芳烃类如苯类、酯类或酮类溶剂中的一种或几种的任意质量比组合,如二甲苯。需要说明的是,用于合成多异氰酸酯预聚物溶液的XDI不计入单组分外露型快干聚氨酯防水涂料配方中的苯二亚甲基二异氰酸酯。
进一步地,发明中所述聚醚多元醇官能度为1.8~2.2,数均分子量为400~3000,优选800~2000。例如可以使用购自巴斯夫的PTMEG2000(聚醚多元醇,2000分子量);购自蓝星东大的PPG2000,商品名为DL-2000D(聚丙二醇,分子量2000);蓝星东大的PPG1000购自,商品名为DL-1000D(聚丙二醇,分子量1000)。
进一步地,发明中所述脂肪族扩链剂为乙二醇、丙二醇、丁二醇、戊二醇、甲基丙二醇、己二醇、一缩二乙二醇中的一种或几种的任意比例混合物。
进一步地,发明中所述催化剂为有机锡盐和有机铋盐中的一种或多种,优选二月桂酸二丁基锡、异辛酸锡、异辛酸铋中的一种或多种,更优选二月桂酸二丁基锡。
进一步地,发明中所述助剂为消泡剂、流平剂、抗氧剂、紫外线吸收剂中的一种或几种的任意质量比组合。
进一步地,所述填料为分子筛活化粉、气相二氧化硅、钛白粉、氧化钙中的两种或几种的任意质量比的组合。
根据本发明的第二个方面,提供了上述本发明所述的单组分外露型快干聚氨酯防水涂料的制备方法,包括如下步骤:
(1)多异氰酸酯预聚物制备:苯二亚甲基二异氰酸酯、三羟甲基丙烷在溶剂的存在下加热(温度例如60-90℃)反应生成多异氰酸酯预聚物;
(2)单组分防水涂料制备:将聚醚多元醇、苯二亚甲基二异氰酸酯、步骤(1)中所述多异氰酸酯预聚物、催化剂混合加热完全反应,再加入脂肪族扩链剂反应至NCO含量为1~4wt%,冷却(例如至环境温度)后加入填料及助剂搅拌均匀即可。
优选地,步骤(2)中反应温度50~100℃,优选为60~80℃。
优选地,步骤(1)中所述溶剂为苯类、酯类或酮类溶剂中的一种或几种的任意质量比组合。
本发明的优点:
本发明的单组分聚氨酯防水涂料具有优异的耐候性,长期使用不变色,施工简便,干燥速度快,在高端工程防水领域具有广阔的应用前景。
具体实施方式
为了说明本发明的效果,列举实施例对本发明作进一步详细说明,但本发明并不仅限于这些实施例。本申请中,%是指重量百分数,除非另有规定。
实施例中所使用的原料来源如下:
XDI,购自万华化学集团股份有限公司;
HMDI,购自万华化学集团股份有限公司,商品名为WANNATE HMDI;
IPDI,购自万华化学集团股份有限公司,商品名为WANNATE IPDI;
HDI三聚体,购自万华化学集团股份有限公司,商品名为WANNATE HT-100;
PTMEG2000购自巴斯夫(聚醚多元醇,2000分子量);
PPG2000购自蓝星东大,商品名为DL-2000D(聚丙二醇,分子量2000);
PPG1000购自蓝星东大,商品名为DL-1000D(聚丙二醇,分子量1000);
三羟甲基丙烷(TMP)购自阿拉丁;
丙二醇甲醚醋酸酯(PMA),1,4-丁二醇(BDO),二甲苯及丁酮购自西陇化工;
抗氧剂1010,紫外线吸收剂UV-326购自巴斯夫;
异辛酸铋购自美国领先化学,商品名BiCAT 8108;
二月桂酸二丁基锡购自购自德音化学,商品名DY-12。
实施例1
将3.75kg XDI溶于10kg二甲苯中,加热至80℃,向其中滴加TMP的二甲苯溶液(0.9kgTMP溶于5kg PMA中),直至反应完全,体系NCO含量达到4.3%左右时停止反应得到多异氰酸酯预聚物溶液。
将所得多异氰酸酯预聚物溶液、40kg PTMEG2000、12kg XDI及7g二月桂酸二丁基锡混合加热至70℃,反应至体系NCO含量达到6.4%左右加入1.5kg BDO继续反应达到终点NCO含量约4.3%。
向上一步所得浆料中加入8kg氧化钙、10kg钛白粉、0.5kg抗氧剂1010和0.5kg紫外线吸收剂UV326,混合均匀后包装得到单组分外露型聚氨酯快干防水涂料。
实施例2
将5kg XDI溶于10kg二甲苯中,加热至70℃,向其中滴加TMP的二甲苯溶液(1kgTMP溶于5kg丁酮中),直至反应完全,体系NCO含量达到6.2%左右时停止反应得到多异氰酸酯预聚物溶液。
将所得多异氰酸酯预聚物溶液、40kg PPG1000、15kg XDI及10g二月桂酸二丁基锡混合加热至60℃,反应至体系NCO含量达到6.1%左右加入2kg BDO继续反应达到终点NCO含量约3.5%。
向上一步所得浆料中加入5kg氧化钙、5kg分子筛活化粉、10kg份钛白粉、1kg抗氧剂1010和1kg重量份紫外线吸收剂UV326,混合均匀后包装得到单组分外露型聚氨酯快干防水涂料。
实施例3
将5kg XDI溶于10kg二甲苯中,加热至70℃,向其中滴加TMP的二甲苯溶液(0.8kgTMP溶于5kg PMA中),直至反应完全,体系NCO含量达到7.0%左右时停止反应得到多异氰酸酯预聚物溶液。
将所得多异氰酸酯预聚物溶液、50kg PPG2000、10kg XDI及7g二月桂酸二丁基锡混合加热至70℃,反应至体系NCO含量达到4.7%左右加入1.0kg BDO继续反应达到终点NCO含量约3.5%。
向上一步所得浆料中加入5kg氧化钙、5kg分子筛活化粉、6kg份钛白粉、1kg抗氧剂1010和1kg重量份紫外线吸收剂UV326,混合均匀后包装得到单组分外露型聚氨酯快干防水涂料。
实施例4
将4kg XDI溶于10kg二甲苯中,加热至80℃,向其中滴加TMP的二甲苯溶液(0.9kgTMP溶于6kg PMA中),直至反应完全,体系NCO含量达到4.5%左右时停止反应得到多异氰酸酯预聚物。
将所得多异氰酸酯预聚物溶液、35kg PPG1000、15kg XDI及10g二月桂酸二丁基锡混合加热至60℃,反应至体系NCO含量达到6.6%左右加入2.0kg BDO继续反应达到终点NCO含量约4.3%。
向上一步所得浆料中加入8kg氧化钙、5kg分子筛活化粉、12kg钛白粉、1kg抗氧剂1010和1kg紫外线吸收剂UV326,混合均匀后包装得到单组分外露型聚氨酯快干防水涂料。
对比例1
将50kg PTMEG2000、18kg HMDI、10g二月桂酸二丁基锡、10g二甲苯、10g PMA混合加热,80℃反应2h,再加入1.5kg BDO继续反应3h,达到理论NCO含量约3.5%。
向上一步所得浆料中加入8kg氧化钙、10kg钛白粉、1kg抗氧剂1010及1kg紫外线吸收剂UV326,混合均匀后包装得到单组分外露型聚氨酯快干防水涂料。
对比例2
将50kg PTMEG2000、15kg IPDI、4kg HDI三聚体、5g二月桂酸二丁基锡、10g二甲苯、10g PMA混合加热,80℃反应1h,再加入1kg BDO继续反应3h,达到理论NCO含量约4.4%。
向上一步所得浆料中加入8kg氧化钙、10kg钛白粉、1kg抗氧剂1010及1kg紫外线吸收剂UV326,混合均匀后包装得到单组分外露型聚氨酯快干防水涂料。
对比例3
将3.7kg HDI三聚体、40kg PTMEG2000、12kg XDI、10kg二甲苯、5kg PMA及7g二月桂酸二丁基锡混合加热至70℃,反应至体系NCO含量达到6.4%左右加入1.5kg BDO继续反应达到终点NCO含量约4.3%。
向上一步所得浆料中加入8kg氧化钙、10kg钛白粉、0.5kg抗氧剂1010和0.5kg紫外线吸收剂UV326,混合均匀后包装得到单组分外露型聚氨酯快干防水涂料。
将实施例1~4及对比例1~3制得的单组分聚氨酯防水涂料涂于干燥的玻璃板或聚四氟乙烯板上,室温下测试表干及实干时间,成膜后测试样品的拉伸强度及断裂伸长率,见表1。
表1
表干时间 | 实干时间 | 拉伸强度 | 断裂伸长率 | |
实施例1 | 4.5h | 20h | 9.2MPa | 453% |
实施例2 | 5h | 24h | 15.6MPa | 283% |
实施例3 | 6h | 24h | 6.8MPa | 574% |
实施例4 | 3.5h | 18h | 19.6MPa | 206% |
对比例1 | 12h | 48h | 5.2MPa | 657% |
对比例2 | 10h | 30h | 10.3MPa | 137% |
对比例3 | 8h | 30h | 15.3MPa | 58% |
表干时间,实干时间及拉伸性能测试按照GB/T 16777--2008标准中所述测试方法进行。从表1的结果可以看出,实施例1~4具有更好的干燥性能与较好的力学性能表现。
Claims (9)
3.根据权利要求1或2所述的单组分外露型快干防水涂料,其中,所述聚醚多元醇为官能度1.8~2.2的聚醚多元醇;和/或
所述聚醚多元醇的数均分子量为400~3000,优选800~2000。
4.根据权利要求1-3中任一项所述的单组分外露型快干防水涂料,其中,所述脂肪族扩链剂为乙二醇、丙二醇、丁二醇、戊二醇、甲基丙二醇、己二醇、一缩二乙二醇中的一种或几种的任意比例混合。
5.根据权利要求1-4中任一项所述的单组分外露型快干防水涂料,其中,所述催化剂为有机锡盐和有机铋盐中的一种或多种,优选二月桂酸二丁基锡、异辛酸锡、异辛酸铋中的一种或多种,更优选二月桂酸二丁基锡。
6.根据权利要求1-5中任一项所述的单组分外露型快干防水涂料,其中,所述助剂为消泡剂、流平剂、抗氧剂、紫外线吸收剂中的一种或几种的任意质量比组合;和/或
所述填料为分子筛活化粉、气相二氧化硅、钛白粉、氧化钙中的一种或多种的任意质量比组合。
7.权利要求1-6中任一项所述的单组分外露型快干防水涂料的制备方法,包括如下步骤:
(1)多异氰酸酯预聚物制备:苯二亚甲基二异氰酸酯、三羟甲基丙烷在溶剂的存在下混合加热反应生成多异氰酸酯预聚物;
(2)单组分防水涂料制备:将聚醚多元醇、苯二亚甲基二异氰酸酯、步骤(1)中所述多异氰酸酯预聚物、催化剂混合加热完全反应,再加入脂肪族扩链剂反应至NCO含量为1~4wt%,冷却后加入填料及助剂搅拌均匀即可。
8.根据权利要求7所述的制备方法,其中,步骤(1)及步骤(2)中反应温度为50~100℃,优选60~80℃。
9.根据权利要求7所述的制备方法,其中,步骤(1)中所述溶剂为芳烃类、酯类或酮类溶剂中的一种或几种的任意质量比组合。
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