CN104356912B - 一种涂料的制备方法 - Google Patents
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Abstract
本发明公开了一种涂料的制备方法，在二月桂酸二丁基锡催化剂存在的条件下，将二元醇与六亚甲基二异氰酸酯混合，于70~90℃下反应1.0~3.0h，得到聚氨酯预聚体；向聚氨酯预聚体中加入亲水扩链剂、羟基硅烷和有机溶剂，于65~95℃条件下反应1.5~3.5h，加入含氮化合物于65~85℃反应1~3h，按COOH/NH2的摩尔比为0.6:1~1.2:1的比例，加入三乙胺进行中和反应30~70min，加水进行乳化，形成一种阻燃性涂料。所制备的阻燃性涂料环保、价格低廉，能满足市场需求。
Description
本申请是分案申请，原申请的申请号： 201310094271.3，申请日：2013-03-22，发明名称：一种阻燃性涂料的制备方法。
技术领域
本发明涉及一种涂料的制备方法，特别涉及一种阻燃性涂料的制备方法。
背景技术
水性聚氨酯作为涂料一个重要研究方向，其(又称水基聚氨酯)是一种在聚氨酯的分子链中含有亲水性基团的聚氨酯树脂，与水具有很强的亲和性，采用特定的工艺能使之在水中分散并形成稳定的体系。水性聚氨酯主要应用于皮革涂饰、纺织印染、造纸业、建筑涂料、胶粘剂等方面，所涉及的几乎都是易燃材料，这些材料在使用时如未经阻燃处理，必然成为引发火灾的安全隐患。水性聚氨酯的阻燃化，是水性聚氨酯功能化的重要方向之一。
发明内容
本发明实际要解决的技术问题是提供一种阻燃性水性聚氨酯涂料。
为了解决上述技术问题，本发明采用了以下技术方案。
（1)、在二月桂酸二丁基锡催化剂存在的条件下，按NCO/OH 的摩尔比为1.5:1~4.5:1，将二元醇与六亚甲基二异氰酸酯混合，于70~90℃下反应1.0~3.0h，得到聚氨酯预聚体A；所述催化剂用量为二元醇与六亚甲基二异氰酸酯总重量的0.5~0.9％；
（2)、向产物A中加入羧基含量为产物A重量1.5~3.5％的亲水扩链剂、产物A重量10.5~15.5%的羟基硅烷和产物A重量10~20％的有机溶剂，于65~95℃条件下反应1.5~3.5h，得产物B；
（3）、再往B中加入含氮化合物为产物A重量的2~6%，于65~85℃反应1~3h，按COOH/NH2 的摩尔比为0.6:1~1.2:1的比例，加入三乙胺进行中和反应30~70min，加水进行乳化，得到产物C，即为阻燃性涂料；
二元醇为水合氯醛、正丁基双（羟丙基）氧化膦中的任意一种；亲水扩链剂为马来酸、丁二酸、乙二酸中的任意一种；羟基硅烷数均分子量为600~1000g/mol；有机溶剂为吡啶、环己酮、N，N-二甲基乙酰胺中的任意一种；含氮化合物为二羟基二甲基三聚氰胺、二乙醇胺中的任意一种。
本发明具有以下特点：
（1）以阻燃性二元醇取代传统合成聚氨酯预聚体的二元醇，并发挥硅、氮、氯或硅、氮、磷协同作用，提高涂料阻燃性；
（2）以吡啶、环己酮、N，N-二甲基乙酰胺取代传统的聚氨酯的有机溶剂N,N-二甲基甲酰胺，制备工艺简单；
具体实施方式
下面结合实例进一步说明本发明。
实例一
（1)、在装有搅拌浆、温度计、冷凝管的500ml的四口烧瓶中，将水合三氯乙醛16.5g与六亚甲基二异氰酸酯33.3g混合，在二月桂酸二丁基锡催化剂0.249g存在的条件下，于70℃下反应1 h，得到49.9g聚氨酯预聚体A；
（2)、向产物A中加入亲水扩链剂马来酸0.96g、数均分子量为600 g/mol羟基硅烷5.24g和吡啶4.99g，于65℃条件下反应1.5 h，得产物B；
（3）、再往产物B中加入二羟基二甲基三聚氰胺1.0g，于65℃反应1h，加入三乙胺2.79g进行中和反应30 min，加水140g进行乳化形成202.2g阻燃性聚氨酯C。
实例二
（1)、在装有搅拌浆、温度计、冷凝管的500ml的四口烧瓶中，将正丁基双（羟丙基）氧化膦22.2g与六亚甲基二异氰酸酯75.6g混合，在二月桂酸二丁基锡催化剂0.88g存在的条件下，于90℃下反应3 h，得97.6g聚氨酯预聚体A；
（2)、向产物A中加入丁二酸4.48g、数均分子量为1000 g/mol羟基硅烷15.1g和环己酮19.5g，于95℃条件下反应3.5 h，得产物B；
（3）、再往产物B中加入二乙醇胺5.86g，反应温度85℃,反应时间3h，加入三乙胺6.39g进行中和反应70 min，加水130g进行乳化，形成275g阻燃性聚氨酯C。
实例三
（1)、在装有搅拌浆、温度计、冷凝管的500ml的四口烧瓶中，将水合三氯乙醛16.5g与六亚甲基二异氰酸酯66.6g混合，在二月桂酸二丁基锡催化剂0.58g存在的条件下，于80℃下反应2 h，得到83g聚氨酯预聚体A；
（2)、向产物A中加入乙二酸1.66g、数均分子量为800 g/mol羟基硅烷10.8g和N，N-二甲基乙酰胺12.5g，于75℃条件下反应2.5 h，得产物B；
（3）、再往B中加入二羟基二甲基三聚氰胺3.32g，反应温度75℃,反应时间2h，加入三乙胺4.1g进行中和反应50 min，加水140g进行乳化，形成245.9g阻燃性聚氨酯C；
表一和表二是本发明实例二所制备涂料所成膜所得性能指标。
膜阻燃性是通过烟密度法（最大烟密度、达到最大烟密度时间）、氧指数、垂直燃烧指标（有焰燃烧时间、无焰燃烧时间）来衡量，断裂伸长率表征其力学性能，表一是实例二所得聚氨酯乳液与市场上的阻燃性聚氨酯SPUA-352性能对比。
表一 阻燃性涂料膜阻燃效果指标
表一各项指标的检测分别依据如下标准：烟密度依据GB8323-2008来测定；氧指数采用GB/T5454-1997《纺织品 燃烧性能试验-氧指数法》测定；有焰燃烧时间和无焰燃烧时间是由GB/T 5455-1997《纺织品燃烧能试验-垂直法》来测定。
由表一可知，本发明阻燃性涂料膜点燃后，最大烟密度显著降低，达到最大烟密度时间显著延长，氧指数明显提高，燃烧时间明显缩短。
表二 阻燃性涂料膜所得断裂伸长率
表二中指标的检测方法参考（蒋维祺.皮革成品理化检验[M].中国轻工业出版社，1999，82~96），本发明阻燃性涂料所得膜断裂伸长率比市场阻燃性能最好的SPUA-352所成膜的断裂伸长率大。
Claims (1)
1.一种涂料的制备方法，其特征在于包括：
（1）、在装有搅拌浆、温度计、冷凝管的500ml的四口烧瓶中，将水合三氯乙醛16.5g与六亚甲基二异氰酸酯33.3g混合，在二月桂酸二丁基锡催化剂0.249g存在的条件下，于70℃下反应1 h，得到49.9g聚氨酯预聚体A；
（2）、向产物A中加入亲水扩链剂马来酸0.96g、数均分子量为600 g/mol羟基硅烷5.24g和吡啶4.99g，于65℃条件下反应1.5 h，得产物B；
（3）、再往产物B中加入二羟基二甲基三聚氰胺1.0g，于65℃反应1h，加入三乙胺2.79g进行中和反应30 min，加水140g进行乳化形成202.2g阻燃性聚氨酯C，即为阻燃性涂料。
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