CN104403546B - 一种阻燃聚醚型单组份聚氨酯防水涂料及其制备工艺 - Google Patents

一种阻燃聚醚型单组份聚氨酯防水涂料及其制备工艺 Download PDF

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CN104403546B
CN104403546B CN201410649197.1A CN201410649197A CN104403546B CN 104403546 B CN104403546 B CN 104403546B CN 201410649197 A CN201410649197 A CN 201410649197A CN 104403546 B CN104403546 B CN 104403546B
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王威
葛义
张冬冬
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Hongyuan Waterproof Technology Group Co ltd
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Abstract

本发明公开了一种阻燃聚醚型单组份聚氨酯防水涂料及其制备方法，所述阻燃聚醚型单组份聚氨酯防水涂料是由以下原料制成：40～50%的阻燃聚合聚醚多元醇，20.6～26.3%的液体填料，25～30%的粉体填料，3.5～4.2%的TDI和0.2%的催化剂，以上百分含量均为质量百分含量；所述液体填料为邻苯二甲酸二壬酯，所述粉体填料为碳酸钙；所述阻燃聚醚型单组份聚氨酯防水涂料的氧指数在34.8%以上，拉伸强度在2.51Mpa以上，撕裂强度在16.21N/mm以上。本发明的优点在于在聚醚多元醇中引入阻燃元素，选择合适的配比和反应条件，使得聚氨酯防水涂料有更优异、持久的阻燃效果，同时具有良好的耐热性、尺寸稳定性和强度等物理性能，其中，氧指数在34.8%以上，拉伸强度在2.51Mpa以上，撕裂强度在16.21N/mm以上。

Description

一种阻燃聚醚型单组份聚氨酯防水涂料及其制备工艺
技术领域
本发明涉及一种应用于建筑防水涂料，特别是一种阻燃聚醚型单组份聚氨酯防水涂料及其制备工艺。
背景技术
目前聚氨酯防水涂料以其优异的物理性能广泛应用于建筑物的地下室、屋面、沟池、厕浴间及化工厂地面的防水、防渗等工程。然而未经阻燃处理的聚氨酯防水涂料的氧指数为17%左右，属于易燃材料，燃烧时存在火焰大，有浓烟，释放HCN、CO等有毒气体的问题，严重威胁人们的生命财产安全。聚氨酯防水涂料的阻燃方法有添加型和反应型阻燃法两种方法。但添加阻燃剂法往往会造成涂膜的开裂，粉化或使其物理机械性能大幅下降，丧失本身所具有的性能优势，且这些阻燃剂单独添加时阻燃效果不显著。
反应型阻燃法是在生产聚氨酯防水涂料配方中加入阻燃元素的多羟基化合物等反应型阻燃剂，或在聚醚多元醇结构中引入阻燃元素而获得阻燃性能。此种方法生产聚氨酯防水涂料具有阻燃性能持久性好、对物理机械性能影响较小等优点。而在聚醚多元醇中引入阻燃元素的方法可使聚氨酯防水涂料具有较更好的耐热性、尺寸稳定性和强度，更是目前研究的重点。
发明内容
本发明的目的是提供一种阻燃聚醚型单组份聚氨酯防水涂料，具有物理性能良好，稳定性好，阻燃性能持久，氧指数高，总燃烧时间短的优点。
本发明的另一个目的是提供一种阻燃聚醚型单组份聚氨酯防水涂料的制备方法。
为解决以上技术问题，本发明采用以下技术方案：
一种阻燃聚醚型单组份聚氨酯防水涂料，所述阻燃聚醚型单组份聚氨酯防水涂料是由以下原料制成：40～50%的阻燃聚合聚醚多元醇，20.6～26.3%的液体填料，25～30%的粉体填料，3.5～4.2%的TDI和0.2%的催化剂，以上百分含量均为质量百分含量。
以下是对上述技术方案的进一步优化：
所述液体填料为邻苯二甲酸二壬酯（DINP），粉体填料为碳酸钙，催化剂为二月桂酸二丁锡。
所述阻燃聚醚型单组份聚氨酯防水涂料的氧指数在34.8%以上，拉伸强度在2.51Mpa以上，撕裂强度在16.21N/mm以上。
所述的一种阻燃聚醚型单组份聚氨酯防水涂料的制备工艺，包括以下步骤：
A. 阻燃聚合聚醚多元醇的制备；
B. 阻燃聚醚型单组份聚氨酯防水涂料的制备。
所述阻燃聚合聚醚多元醇的制备包括以下步骤:
1）甲醛溶液调制步骤
取1～2质量份的甲醛在容器中，加入适量的质量分数为10%的NaOH溶液，调整甲醛的pH值到8～9，待用，在带搅拌的容器中，温度≤40℃的条件下，加入调整好的甲醛溶液，开动搅拌；
2）加料步骤
分别加入摩尔比为3:1:0.5的三聚氰胺、双氰胺和尿素，三者总质量占聚醚多元醇量的28%；
3）加压反应步骤
缓缓升温至80℃，控制反应温度为80±2℃，充入氮气加压，控制反应压力在0.44MPa以下反应3h；加入1质量份的质量比为3:1的DL-2000D和DL-330N混合聚醚多元醇，升温至100±2℃，反应压力在0.44MPa以下反应5h；
4）真空脱除步骤
反应完后控温在115±2℃下进行真空，脱除未反应的单体和水分，降温得到阻燃聚合聚醚多元醇。
所述阻燃聚醚型单组份聚氨酯防水涂料的制备包括以下步骤:
1）真空脱水步骤
将40～50%的阻燃聚合聚醚多元醇，20.6～26.3%的液体填料，25～30%的粉体填料，混合高速搅拌均匀，在115±2℃、-0.09～-0.1MPa真空条件下脱水4h。
2）反应步骤
停真空，降温至60℃加入3.5～4.2%的TDI，保持温度80±2℃反应2h，测定反应料中—NCO含量，质量分数达到3.5～4.0%时停止反应。
3）降温出料步骤
降温至50℃，加入0.2%的催化剂搅拌均匀出料即为本发明涂料。
本发明的优点在于在聚醚多元醇中引入阻燃元素，选择合适的配比和反应条件，使得聚氨酯防水涂料有更优异、持久的阻燃效果，同时具有良好的耐热性、尺寸稳定性和强度等物理性能，其中，氧指数在34.8%以上，拉伸强度在2.51Mpa以上，撕裂强度在16.21N/mm以上。
下面结合具体实施方式对本发明作进一步说明。
具体实施方式
实施例1
A. 阻燃聚合聚醚多元醇的制备
1）甲醛溶液调制步骤
取50g甲醛在烧杯中，加入适量的质量分数为10%的NaOH溶液，调整甲醛的pH值到8，待用。在四口烧瓶中，温度≤40℃的条件下，加入调整好的甲醛溶液，开动搅拌。
2）加料步骤
分别加入摩尔比为3:1:0.5的三聚氰胺、双氰胺和尿素，三者总质量为14g。
3）加压反应步骤
缓缓升温至80℃，控制反应温度为80±2℃，充入氮气加压，控制反应压力在0.44MPa以下反应3h；加入50g的质量比为3:1的DL-2000D和DL-330N混合聚醚多元醇， 升温至100±2℃，反应压力在0.44MPa以下反应5h。
4）真空脱除步骤
反应完后控温在115±2℃进行真空脱除未反应的单体和水分，降温得到阻燃聚合聚醚多元醇。
B.单组份聚氨酯防水涂料的制备
1）真空脱水步骤
将40g制备好的阻燃聚合聚醚多元醇，26.3g的邻苯二甲酸二壬酯，30g的碳酸钙混合高速搅拌均匀，在115±2℃、-0.09～-0.1MPa真空条件下脱水4h。
2）反应步骤
停真空，降温至60℃加入3.5g的TDI，保持温度80±2℃反应2h，测定反应料中—NCO含量，质量分数达到3.5%时停止反应。
3）降温出料步骤
降温至50℃，加入0.2g的二月桂酸二丁锡搅拌均匀出料即为本发明涂料。
实施例2
A. 阻燃聚合聚醚多元醇的制备
1）甲醛溶液调制步骤
取100g甲醛在烧杯中，加入适量的质量分数为10%的NaOH溶液，调整甲醛的pH值为9，待用。在四口烧瓶中，温度≤40℃的条件下，加入调整好的甲醛溶液，开动搅拌。
2）加料步骤
分别加入摩尔比为3:1:0.5的三聚氰胺、双氰胺和尿素，三者总质量为14g。
3）加压反应步骤
缓缓升温至80℃，控制反应温度80±2℃，充入氮气加压，控制反应压力在0.44MPa以下反应3h；加入50g的质量比为3:1的DL-2000D和DL-330N混合聚醚多元醇，
升温至100±2℃，反应压力在0.44MPa以下反应5h。
4）真空脱除步骤
反应完后控温在115±2℃进行真空脱除未反应的单体和水分，降温得到阻燃聚合聚醚多元醇。
B.单组份聚氨酯防水涂料的制备
1）真空脱水步骤
将50g制备好的阻燃聚合聚醚多元醇，20.6g的邻苯二甲酸二壬酯，25g的碳酸钙混合高速搅拌均匀，在115±2℃、-0.09～-0.1MPa真空条件下脱水4h。
2）反应步骤
停真空，降温至60℃加入4.2g的TDI，保持温度80±2℃反应2h，测定反应料中—NCO含量，质量分数达到4.0%时停止反应。
3）降温出料步骤
降温至50℃，加入0.2g的二月桂酸二丁锡搅拌均匀出料即为本发明涂料。
性能验证：
将上述制备的阻燃聚醚型单组份聚氨酯防水涂料在按照GB/T19250-2003的规定下成膜养护，检测得出检测结果。
表1 阻燃聚醚型单组份聚氨酯防水涂料性能测试结果
由上可知，以上两个实施例的力学性能指标均达到甚至超过国家标准，氧指数高于标准值，火焰快速熄灭，阻燃效果良好。
以上所述为本发明最佳实施方式的举例，其中未详细述及的部分均为本领域普通技术人员的公知常识。本发明的保护范围以权利要求的内容为准，任何基于本发明的技术启示而进行的等效变换，也在本发明的保护范围之内 。

Claims (1)

1.一种阻燃聚醚型单组份聚氨酯防水涂料，其特征在于：所述阻燃聚醚型单组份聚氨酯防水涂料是由以下原料制成：40～50%的阻燃聚合聚醚多元醇，20.6～26.3%的液体填料，25～30%的粉体填料，3.5～4.2%的TDI和0.2%的催化剂，以上百分含量均为质量百分含量；
所述阻燃聚合聚醚多元醇为在聚醚多元醇中引入阻燃元素制备而成；
所述液体填料为邻苯二甲酸二壬酯，所述粉体填料为碳酸钙，所述催化剂为二月桂酸二丁锡；
所述阻燃聚醚型单组份聚氨酯防水涂料的氧指数在34.8%以上；
所述防水涂料的制备工艺，包括以下步骤：
A. 阻燃聚合聚醚多元醇的制备；
B. 阻燃聚醚型单组份聚氨酯防水涂料的制备；
所述阻燃聚合聚醚多元醇的制备包括以下步骤:
1）甲醛溶液调制步骤
取1～2质量份的甲醛在容器中，加入适量的质量分数为10%的NaOH溶液，调整甲醛的pH值到8～9，待用，在带搅拌的容器中，温度≤40℃的条件下，加入调整好的甲醛溶液，开动搅拌；
2）加料步骤
分别加入摩尔比为3:1:0.5的三聚氰胺、双氰胺和尿素，三者总质量占聚醚多元醇量的28%；
3）加压反应步骤
缓缓升温至80℃，控制反应温度为80±2℃，充入氮气加压，控制反应压力在0.44MPa以下反应3h；加入1质量份的质量比为3:1的DL-2000D和DL-330N混合聚醚多元醇， 升温至100±2℃，反应压力在0.44MPa以下反应5h；
4）真空脱除步骤
反应完后控温在115±2℃下进行真空，脱除未反应的单体和水分，降温得到阻燃聚合聚醚多元醇；
所述阻燃聚醚型单组份聚氨酯防水涂料的制备包括以下步骤:
1）真空脱水步骤
将40～50%的阻燃聚合聚醚多元醇，20.6～26.3%的液体填料，25～30%的粉体填料，混合高速搅拌均匀，在115±2℃、-0.09～-0.1MPa真空条件下脱水4h；
2）反应步骤
停真空，降温至60℃加入3.5～4.2%的TDI，保持温度80±2℃反应2h，测定反应料中—NCO含量，质量分数达到3.5～4.0%时停止反应；
3）降温出料步骤
降温至50℃，加入0.2%的催化剂搅拌均匀出料即可。
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