CN104530951A - 含磷水性聚氨酯树脂阻燃涂料的制备方法 - Google Patents

含磷水性聚氨酯树脂阻燃涂料的制备方法 Download PDF

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CN104530951A
CN104530951A CN201410804777.3A CN201410804777A CN104530951A CN 104530951 A CN104530951 A CN 104530951A CN 201410804777 A CN201410804777 A CN 201410804777A CN 104530951 A CN104530951 A CN 104530951A
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郭军红
张鹏中
杨保平
崔锦峰
包雪梅
周应萍
谢吉仁
赵秋萍
慕波
李敏睿
王心远
郭永亮
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Lanzhou University of Technology
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Abstract

含磷水性聚氨酯树脂阻燃涂料的制备方法，按质量百分数计，含磷水性聚氨酯树脂阻燃涂料配方为：含磷水性聚氨酯树脂70%~90%，颜填料5%~25%，消泡剂0.1%~0.12%， 稳定剂0.1%~0.12%；其制备步骤为：准确称量含磷水性聚氨酯树脂和颜填料，在容器中混合搅拌均匀后，倒入砂磨分散机中分散至细度小于20μm，加入消泡剂、稳定剂分散均匀，以去离子水调整粘度至合格后过滤出料，即得含磷水性聚氨酯树脂阻燃涂料，涂刷样板，经固化干燥后，检测涂层各项性能指标。

Description

含磷水性聚氨酯树脂阻燃涂料的制备方法
技术领域
本发明涉及含磷水性聚氨酯树脂阻燃涂料的制备方法，属于高分子化学及聚合物涂料组合物技术领域。
背景技术
发明CN201410499201公开了一种耐腐蚀阻燃涂料，其原料按重量份包括：改性环氧树脂78-81份，酚醛树脂12-15份，乙基纤维素5-8份，有机溶剂48-51份，颜料1.5-1.8份，消泡剂0.5-0.8份，平流剂0.8-1.2份，防霉剂0.5-0.8份，改性凹凸棒土8-9份，纳米蒙脱土2-4份，纳米氮化铝2-3份，硅烷偶联剂Si-5630.8-1.2份，壬二酸二辛酯D0Z 0.5-0.8份，三聚氰胺磷酸酯1-2份，纳米氢氧化铝0.8-1.1份，二月桂酸二丁基锡0.1-0.3份，三氯化锆0.05-0.08份。该发明具有优异的耐腐蚀、耐高温阻燃性能，而且耐冲击耐磨性能优秀，附着力良好。
发明CN201410522390涉及一种车内用水性聚氨酯涂料，由下列重量份的原料制成：水性聚氨酯乳液15-50份、阻燃剂10-20份、阻燃助剂1-10份、流平剂10-20份和水30-50份。该发明所述的车内用水性聚氨酯涂料具有增强的耐水性，可以广泛地用于在汽车车内涂覆。
聚氨酯树脂涂料应用十分广泛，在木器涂料、汽车修补涂料、防腐涂料、地坪漆、电子涂料、特种涂料、防水涂料、地板涂料、防腐涂料、预卷材涂料等产品领域都有应用。在双组分和单组分聚氨酯涂料中，因其含有易挥发有机溶剂而造成资源浪费和生产加工、施工过程中的环境污染。
发明内容
本发明的目的是提供一种含磷水性聚氨酯树脂阻燃涂料的制备方法。
本发明是含磷水性聚氨酯树脂阻燃涂料的制备方法，其制备步骤为：
（1）含磷聚酯多元醇的制备：在装有搅拌器、温度计、冷凝器、分水器的容器中加入己二酸、6-氧-6H-二苯并(c,e)(1,2)氧磷杂己环-6-酮-丁二酸、乙二醇、1，2-丙二醇、二甲苯、对甲苯磺酸，缓慢升温；固体全部熔融后，开动搅拌，继续缓慢升温至 140℃~150℃反应1h，然后继续升温至150~160℃反应1h，最后升温，控制最高温度不得超过210℃，直至酸值<10mgKOH/g时停止反应；
（2）含磷水性聚氨酯树脂的制备：将配方量的聚酯多元醇加入到装有搅拌器、冷凝器、温度计的容器中，加热升温至 45℃，缓慢滴加配方量的 TDI，搅拌30min后升温至 65℃，同时，滴加配方量的二月桂酸二丁基锡反应 2 h；升温至70℃，加入配方量的2,2-二羟甲基丁酸进行亲水扩链反应 2 h，反应至异氰酸酯基含量30min内稳定不变；降温至35℃，加入配方量的三乙胺、去离子水高速搅拌乳化，得到固含量为30%左右的水性聚氨酯树脂；
（3）含磷水性聚氨酯树脂阻燃涂料的制备：
准确称量含磷水性聚氨酯树脂和颜填料，在容器中混合搅拌均匀后，倒入砂磨分散机中分散至细度小于20μm，加入消泡剂、稳定剂分散均匀，以去离子水调整粘度至合格后过滤出料，即得含磷水性聚氨酯树脂阻燃涂料，涂刷样板，经固化干燥后，检测涂层各项性能指标。
本发明的有益之处是：通过分子设计采用含磷单体合成在聚氨酯树脂分子链上含有阻燃元素磷的聚氨酯树脂，对合成含磷聚氨酯树脂进行水性化改性，并将改性产品应用于可应用于含磷水性聚氨酯树脂涂料，得到含磷水性聚氨酯树脂阻燃涂料。通过在聚氨酯树脂分子中引入具有阻燃作用的元素磷而将其极限氧指数由小于19提高到高于32，减少火灾时因聚氨酯树脂涂料易燃而造成的人、财、物损失。
具体实施方式
本发明由以下技术方案完成，以含磷单体6-氧-6H-二苯并(c,e)(1,2)氧磷杂己环-6-酮-丁二酸（DOPOMA）合成聚酯多元醇，再与TDI反应合成聚氨酯树脂，以2,2-二羟甲基丁酸封端，三乙胺中和得到含磷水性聚氨酯树脂，将含磷水性聚氨酯树脂与颜填料、消泡剂、稳定剂等分散均匀即可得到含磷水性聚氨酯树脂阻燃涂料。
含磷水性聚氨酯树脂阻燃涂料工艺步骤如下：
（1）含磷聚酯多元醇的制备：在装有搅拌器、温度计、冷凝器、分水器的容器中加入己二酸、DOPOMA、乙二醇、1，2-丙二醇、二甲苯、对甲苯磺酸，缓慢升温；固体全部熔融后，开动搅拌，继续缓慢升温至 140℃~150℃反应1h，然后继续升温至150~160℃反应1h，最后升温，控制最高温度不得超过210℃，直至酸值<10mgKOH/g时停止反应，得到含磷聚酯多元醇；
（2）含磷水性聚氨酯树脂的制备：将配方量的聚酯多元醇转入到装有搅拌器、冷凝管、温度计的容器中，加热升温至 45℃，缓慢滴加配方量的 TDI，搅拌30min后升温至 65℃，同时，滴加配方量的二月桂酸二丁基锡反应 2 h；升温至70℃，加入配方量的2,2-二羟甲基丁酸进行亲水扩链反应 2 h，反应至异氰酸酯基含量30min内稳定不变；降温至35℃，加入配方量的三乙胺、去离子水高速搅拌乳化，得到固含量为30%左右的水性聚氨酯树脂；
（3）含磷水性聚氨酯树脂阻燃涂料的制备：
准确称量含磷水性聚氨酯树脂和颜填料，在容器中混合搅拌均匀后，倒入砂磨分散机中分散至细度小于20μm，加入消泡剂、稳定剂分散均匀，以去离子水调整粘度至合格后过滤出料，即得含磷水性聚氨酯树脂阻燃涂料，涂刷样板，经固化干燥后，检测涂层各项性能指标。
基于制备含磷聚酯多元醇总质量，按重量百分比计，其所用原料及配比为：
己二酸 14~22%，6-氧-6H-二苯并(c,e)(1,2)氧磷杂己环-6-酮-丁二酸（DOPOMA） 41~61%，乙二醇11~16%，1,2-丙二醇 5~7%，二甲苯8~12%，对甲苯磺酸 1~2%。
基于制备含磷水性聚氨酯树脂总质量，按重量百分比计，其所用原料及配比为：
含磷聚酯多元醇 12~18%，TDI 8~12%，二月桂酸二丁基锡 0.24~0.36%，2,2-二羟甲基丁酸1.68~2.52%，三乙胺 1.68~2.52%，去离子水 70%。
TDI为2,4-甲苯二异氰酸酯占80%，2,6-甲苯二异氰酸酯占20%。
基于制备含磷水性聚氨酯树脂阻燃涂料总质量，按重量百分比计，其所用原料及配比为：
含磷水性聚氨酯树脂70%~90%，颜填料5%~25%，消泡剂0.1%~0.12%， 稳定剂0.1%~0.12%；
颜填料为金红石型钛白粉，消泡剂为二甲基硅油，稳定剂为BYK-154。
以下是本发明的实施例，但本发明不局限于下列实施例中。
实施例1.
在装有搅拌器、温度计、冷凝器、分水器的容器中加入15.00g己二酸﹑52.00gDOPOMA﹑15.00g乙二醇、6.50g1,2-丙二醇、10.00g二甲苯、1.50g对甲苯磺酸，缓慢升温；固体全部熔融后，开动搅拌，继续缓慢升温至 140℃~150℃反应1h，然后继续升温至150~160℃反应1h，最后升温，控制最高温度不得超过210℃，直至酸值<10mgKOH/g时停止反应，得到含磷聚酯多元醇。
实施例2.
将15.00g含磷聚酯多元醇转入到装有搅拌器、冷凝管、温度计的容器中，加热升温至 45℃，缓慢滴加10.00g TDI，搅拌30min后升温至 65℃，同时，滴加0.30g二月桂酸二丁基锡反应 2 h；升温至70℃，加入2.30g2,2-二羟甲基丁酸进行亲水扩链反应 2 h，反应至异氰酸酯基含量30min内稳定不变；降温至35℃，加入2.40g三乙胺、70.00g去离子水高速搅拌乳化，得到固含量为30%左右的含磷水性聚氨酯树脂。
实施例3.
称量含磷水性聚氨酯树脂80份，金红石型钛白粉15份，在容器中混合搅拌均匀后，倒入砂磨分散机中分散至细度小于20μm，加入0.1份二甲基硅油消、0.1份BYK-154分散均匀，以去离子水调整粘度至合格后过滤出料，即得含磷水性聚氨酯树脂阻燃涂料，涂刷样板，经固化干燥后，检测涂层各项性能指标。

Claims (6)

1.含磷水性聚氨酯树脂阻燃涂料，其特征在于，制备步骤为：
（1）含磷聚酯多元醇的制备：在装有搅拌器、温度计、冷凝器、分水器的容器中加入己二酸、6-氧-6H-二苯并(c,e)(1,2)氧磷杂己环-6-酮-丁二酸、乙二醇、1，2-丙二醇、二甲苯、对甲苯磺酸，缓慢升温；固体全部熔融后，开动搅拌，继续缓慢升温至 140℃~150℃反应1h，然后继续升温至150~160℃反应1h，最后升温，控制最高温度不得超过210℃，直至酸值<10mgKOH/g时停止反应；
（2）含磷水性聚氨酯树脂的制备：将配方量的聚酯多元醇加入到装有搅拌器、冷凝器、温度计的容器中，加热升温至 45℃，缓慢滴加配方量的 TDI，搅拌30min后升温至 65℃，同时，滴加配方量的二月桂酸二丁基锡反应 2 h；升温至70℃，加入配方量的2,2-二羟甲基丁酸进行亲水扩链反应 2 h，反应至异氰酸酯基含量30min内稳定不变；降温至35℃，加入配方量的三乙胺、去离子水高速搅拌乳化，得到固含量为30%左右的水性聚氨酯树脂；
（3）含磷水性聚氨酯树脂阻燃涂料的制备：
准确称量含磷水性聚氨酯树脂和颜填料，在容器中混合搅拌均匀后，倒入砂磨分散机中分散至细度小于20μm，加入消泡剂、稳定剂分散均匀，以去离子水调整粘度至合格后过滤出料，即得含磷水性聚氨酯树脂阻燃涂料，涂刷样板，经固化干燥后，检测涂层各项性能指标。
2.根据权利要求1所述的含磷水性聚氨酯树脂阻燃涂料的制备方法，其特征在于：基于制备含磷聚酯多元醇总质量，按重量百分比计，其所用原料及配比为：
己二酸 14~22%，6-氧-6H-二苯并(c,e)(1,2)氧磷杂己环-6-酮-丁二酸41~61%，乙二醇11~16%，1,2-丙二醇 5~7%，二甲苯8~12%，对甲苯磺酸 1~2%。
3.根据权利要求1所述的含磷水性聚氨酯树脂阻燃涂料的制备方法，其特征在于：基于制备含磷水性聚氨酯树脂总质量，按重量百分比计，其所用原料及配比为：
含磷聚酯多元醇 12~18%，TDI 8~12%，二月桂酸二丁基锡 0.24~0.36%，2,2-二羟甲基丁酸1.68~2.52%，三乙胺 1.68~2.52%，去离子水 70%。
4.根据权利要求1所述的含磷水性聚氨酯树脂阻燃涂料的制备方法，其特征在于：基于制备含磷水性聚氨酯树脂阻燃涂料总质量，按重量百分比计，其所用原料及配比为：
含磷水性聚氨酯树脂70%~90%，颜填料5%~25%，消泡剂0.1%~0.12%， 稳定剂0.1%~0.12%。
5.根据权利要求1所述的含磷水性聚氨酯树脂阻燃涂料的制备方法，其特征在于TDI为2,4-甲苯二异氰酸酯占80%，2,6-甲苯二异氰酸酯占20%。
6.根据权利要求1所述的含磷水性聚氨酯树脂阻燃涂料的制备方法，其特征在于颜填料为金红石型钛白粉，消泡剂为二甲基硅油，稳定剂为BYK-154。
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