CN104530364A - 建筑外墙保温和阻燃性聚氨酯发泡材料的制备方法 - Google Patents

建筑外墙保温和阻燃性聚氨酯发泡材料的制备方法 Download PDF

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CN104530364A
CN104530364A CN201510055422.3A CN201510055422A CN104530364A CN 104530364 A CN104530364 A CN 104530364A CN 201510055422 A CN201510055422 A CN 201510055422A CN 104530364 A CN104530364 A CN 104530364A
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Abstract

本发明公开了建筑外墙保温和阻燃性聚氨酯发泡材料的制备方法，把混合液A、B组份和C组份在20℃的室温条件下快速混合至发白，立即注入到预先准备的模温为30℃的模具模腔中，进行发泡成型，保持6h后降温冷却到室温，开模具，将泡沫从模腔中取出，室温放置1周，即可得到建筑外墙保温和阻燃性聚氨酯发泡材料，该聚氨酯发泡材料具有阻燃和保温的性能，广泛用于建筑外墙的保温层。

Description

建筑外墙保温和阻燃性聚氨酯发泡材料的制备方法
技术领域
    本发明涉及聚氨酯发泡材料的制备方法，特别涉及建筑外墙保温和阻燃性聚氨酯发泡材料的制备方法。
背景技术
聚氨酯进行合成常采用二月桂酸二丁基锡做催化剂，但由于重金属锡在随着聚氨酯的降解而对环境造成危害，筛选高效无毒的催化剂是聚氨酯合成中的一大难题。
聚氨酯硬质泡沫是以异氰酸酯和聚醚为主要原料，在发泡剂、催化剂、阻燃剂等多种助剂的作用下，通过专用设备混合，经高压喷涂现场发泡而成的高分子聚合物。聚氨酯泡有软泡和硬泡两种，软泡为开孔结构，硬泡为闭孔结构；软泡又分为结皮和不结皮两种。
聚氨酯软泡的主要功能是缓冲。聚氨酯软泡常用于沙发家具、枕头、坐垫、玩具、服装和隔音内衬。
聚氨酯硬泡体是一种具有保温与阻燃功能的新型合成材料，其导热系数低，相当于挤塑板的一半，是目前所有保温材料中导热系数最低的。硬质聚氨酯泡沫塑料主要应用在建筑物外墙保温，屋面阻燃保温一体化、冷库保温隔热、管道保温材料、建筑板材、冷藏车及冷库隔热材等。
聚氨酯泡沫作为高分子材料，由于其较大的比表面积，较小的密度，PU泡沫极易在空气中燃烧，产生有毒有害的气体，因此近年来关于阻燃PU泡沫的研究受到极大关注。
红磷阻燃剂是以红磷为代表的一种有机无卤阻燃剂，具有优良的热稳定性，不挥发性，不产生腐蚀性气体，阻燃效果好，电绝缘性佳等特点。在使用过程中没有毒性危险，添加量少，不溶解，熔点高等优点。但由于红磷容易吸潮，因此需要对其进行包覆，控制其的缓慢释放。
发明内容  
本发明所要解决的技术问题是，提供建筑外墙保温和阻燃性聚氨酯发泡材料的制备方法，选择阻燃功能材料作为催化剂，二元醇和异氰酸酯反应，环状聚二甲基硅氧烷、聚氧乙烯聚氧丙烯季戊四醇醚、菜籽油作为脱模剂和泡沫稳定剂，水、环戊烷、1-溴金刚烷作为发泡剂，盐酸多西环素、五羟基黄酮-3-鼠李糖苷、桑色素在聚氨酯泡沫材料中做阻燃成份，山柰酚-7-O-β-D-葡萄糖苷作为阻燃成份，选择有机膨润土作为泡沫的稳定成份，同时增加泡沫的强度。
建筑外墙保温和阻燃性聚氨酯发泡材料的制备方法，其特征在于：
（1）在反应器中加入玉米淀粉40g、32g磷酸、二巯基丙烷磺酸钠1.4g、二乙烯三胺五甲叉膦酸盐1.2g和2,3,6,7,10,11-六羟基三亚苯基苯1.3g，以转速60rpm进行搅拌,升温到40℃，反应3h，在烘箱中干燥，加入红磷21g和2-乙基己基硫酸酯钠盐1.4g，在50℃以转速90rpm进行搅拌混合均匀，搅拌时间40min，得混合液A；
（2） 把混合液A、B组份和C组份在20℃的室温条件下快速混合至发白，立即注入到预先准备的模温为30℃的模具模腔中，进行发泡成型，保持6h 后降温冷却到室温；
    混合液A：混合液A 2~3重量份；
B组份：由二元醇为10~24重量份、环状聚二甲基硅氧烷1~3.0重量份、聚氧乙烯聚氧丙烯季戊四醇醚2.0重量份、菜籽油1~3重量份、催化剂0.3~0.6重量份、水0.8~2.2重量份、环戊烷18~27重量份、1-溴金刚烷1~2重量份、盐酸多西环素1~2重量份、五羟基黄酮-3-鼠李糖苷2~3重量份、桑色素4~6重量份、山柰酚-7-O-β-D-葡萄糖苷2~3重量份、有机膨润土1~3重量份，所述二元醇为聚碳酸酯二醇、聚四氢呋喃醚二醇的任意一种；
C组分：异氰酸酯为25~40重量份，混合液A、B组份和C组份总重量份为100份；
（3）打开模具，将泡沫从模腔中取出，并在室温条件下放置72h，即可得到建筑外墙保温和阻燃性聚氨酯发泡材料。
催化剂为二硫化四甲基秋兰姆、二(三甲基硅基)碳酰二亚胺、磷酸伯安喹、2-[N-(间羟基)-对甲苯胺甲基]-2-咪唑啉甲磺酸盐、对甲苯磺酰胺和羧苯甲酰磺胺噻唑的任意一种；异氰酸酯为二苯基甲烷二异氰酸酯、甲苯二异氰酸酯、1,6-己二异氰酸酯中的一种。
本发明具有以下特点：
   （1）二硫化四甲基秋兰姆、二(三甲基硅基)碳酰二亚胺、磷酸伯安喹、2-[N-(间羟基)-对甲苯胺甲基]-2-咪唑啉甲磺酸盐、对甲苯磺酰胺和羧苯甲酰磺胺噻唑是一种具有功效阻燃的催化剂，降低了传统聚氨酯的常见催化剂-二月桂酸二丁基锡对环境造成的危害。
   （2）选择环状聚二甲基硅氧烷、聚氧乙烯聚氧丙烯季戊四醇醚、菜籽油作为脱模剂和泡沫稳定剂；
   （3）选择水、环戊烷、1-溴金刚烷作为发泡剂，盐酸多西环素、五羟基黄酮-3-鼠李糖苷、桑色素在聚氨酯泡沫材料中做阻燃成份，山柰酚-7-O-β-D-葡萄糖苷作为阻燃成份，选择有机膨润土作为泡沫的稳定成份，同时增加泡沫的强度。
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250ml三口瓶中加入玉米淀粉40g、32g磷酸、二巯基丙烷磺酸钠1.4g、二乙烯三胺五甲叉膦酸盐1.2g和2,3,6,7,10,11-六羟基三亚苯基苯1.3g，以转速60rpm进行搅拌,升温到40℃，反应3h，转到烘箱中102℃下烘5h，将所得干燥液体转到250ml三口烧瓶中，并向三口烧瓶中加入红磷21g和2-乙基己基硫酸酯钠盐1.4g，在50℃以转速90rpm下进行搅拌混合均匀，搅拌时间40min，得混合液A；
（2） 把混合液A、B组份和C组份在20℃的室温条件下快速混合至发白，立即注入到预先准备的模温为30℃的模具模腔中，进行发泡成型，保持6h 后降温冷却到室温；
    混合液A：混合液A 2g；
B组份：由聚碳酸酯二醇10g、环状聚二甲基硅氧烷1g、聚氧乙烯聚氧丙烯季戊四醇醚2.0g、菜籽油1g、二硫化四甲基秋兰姆0.3g、水0.8g、环戊烷18g、1-溴金刚烷1g、盐酸多西环素1g、五羟基黄酮-3-鼠李糖苷2g、桑色素4g、山柰酚-7-O-β-D-葡萄糖苷2g、有机膨润土1g；
C组份：二苯基甲烷二异氰酸酯25g；
（3）打开模具，将泡沫从模腔中取出，并在室温条件下放置72h，即可得到建筑外墙保温和阻燃性聚氨酯发泡材料。
实例二
（1）在250ml三口瓶中加入玉米淀粉40g、32g磷酸、二巯基丙烷磺酸钠1.4g、二乙烯三胺五甲叉膦酸盐1.2g和2,3,6,7,10,11-六羟基三亚苯基苯1.3g，以转速60rpm进行搅拌,升温到40℃，反应3h，转到烘箱中102℃下烘5h，将所得干燥液体转到250ml三口烧瓶中，并向三口烧瓶中加入红磷21g和2-乙基己基硫酸酯钠盐1.4g，在50℃以转速90rpm下进行搅拌混合均匀，搅拌时间40min，得混合液A；
（2） 把混合液A、B组份和C组份在20℃的室温条件下快速混合至发白，立即注入到预先准备的模温为30℃的模具模腔中，进行发泡成型，保持6h 后降温冷却到室温；
    混合液A：混合液A 3g；
B组份：由聚四氢呋喃醚二醇24g、环状聚二甲基硅氧烷3.0g、聚氧乙烯聚氧丙烯季戊四醇醚2.0g、菜籽油3g、二(三甲基硅基)碳酰二亚胺0.6g、水2.2g、环戊烷27g、1-溴金刚烷2g、盐酸多西环素2g、五羟基黄酮-3-鼠李糖苷3g、桑色素6g、山柰酚-7-O-β-D-葡萄糖苷3g、有机膨润土3g；
C组份：甲苯二异氰酸酯40g；
（3）打开模具，将泡沫从模腔中取出，并在室温条件下放置72h，即可得到建筑外墙保温和阻燃性聚氨酯发泡材料。
实例三
（1）在250ml三口瓶中加入玉米淀粉40g、32g磷酸、二巯基丙烷磺酸钠1.4g、二乙烯三胺五甲叉膦酸盐1.2g和2,3,6,7,10,11-六羟基三亚苯基苯1.3g，以转速60rpm进行搅拌,升温到40℃，反应3h，转到烘箱中102℃下烘5h，将所得干燥液体转到250ml三口烧瓶中，并向三口烧瓶中加入红磷21g和2-乙基己基硫酸酯钠盐1.4g，在50℃以转速90rpm下进行搅拌混合均匀，搅拌时间40min，得混合液A；
（2） 把混合液A、B组份和C组份在20℃的室温条件下快速混合至发白，立即注入到预先准备的模温为30℃的模具模腔中，进行发泡成型，保持6h 后降温冷却到室温；
    混合液A：混合液A 2.5g；
B组份：由聚碳酸酯二醇17g、环状聚二甲基硅氧烷2g、聚氧乙烯聚氧丙烯季戊四醇醚2g、菜籽油2g、磷酸伯安喹0.45g、水1.5g、环戊烷22.5g、1-溴金刚烷1.5g、盐酸多西环素1.5g、五羟基黄酮-3-鼠李糖苷2.5g、桑色素5g、山柰酚-7-O-β-D-葡萄糖苷2.5g、有机膨润土2g；
C组份：1,6-己二异氰酸酯32.5g；
（3）打开模具，将泡沫从模腔中取出，并在室温条件下放置72h，即可得到建筑外墙保温和阻燃性聚氨酯发泡材料。
实例四
（1）在250ml三口瓶中加入玉米淀粉40g、32g磷酸、二巯基丙烷磺酸钠1.4g、二乙烯三胺五甲叉膦酸盐1.2g和2,3,6,7,10,11-六羟基三亚苯基苯1.3g，以转速60rpm进行搅拌,升温到40℃，反应3h，转到烘箱中102℃下烘5h，将所得干燥液体转到250ml三口烧瓶中，并向三口烧瓶中加入红磷21g、2-乙基己基硫酸酯钠盐1.4g和羟基积雪草苷1.2g，在50℃以转速90rpm进行搅拌混合均匀，搅拌时间40min，得混合液A；
（2） 把混合液A、B组份和C组份在20℃的室温条件下快速混合至发白，立即注入到预先准备的模温为30℃的模具模腔中，进行发泡成型，保持6h 后降温冷却到室温；
    混合液A：混合液A 2g；
B组份：由聚碳酸酯二醇10g、环状聚二甲基硅氧烷1g、聚氧乙烯聚氧丙烯季戊四醇醚2.0g、菜籽油1g、2-[N-(间羟基)-对甲苯胺甲基]-2-咪唑啉甲磺酸盐0.4g、水0.8g、环戊烷18g、1-溴金刚烷1g、盐酸多西环素1g、五羟基黄酮-3-鼠李糖苷2g、桑色素4g、山柰酚-7-O-β-D-葡萄糖苷2g、有机膨润土1g和磺达肝癸钠1.3g；
C组分：1,6-己二异氰酸酯25g；
（3）打开模具，将泡沫从模腔中取出，并在室温条件下放置72h，即可得到建筑外墙保温和阻燃性聚氨酯发泡材料。
实例五
（1）在250ml三口瓶中加入玉米淀粉40g、32g磷酸、二巯基丙烷磺酸钠1.4g、二乙烯三胺五甲叉膦酸盐1.2g和2,3,6,7,10,11-六羟基三亚苯基苯1.3g，以转速60rpm进行搅拌,升温到40℃，反应3h，转到烘箱中102℃下烘5h，将所得干燥液体转到250ml三口烧瓶中，并向三口烧瓶中加入红磷21g、2-乙基己基硫酸酯钠盐1.4g和卡泊芬净1.8g，在50℃以转速90rpm进行搅拌混合均匀，搅拌时间40min，得混合液A；
（2） 把混合液A、B组份和C组份在20℃的室温条件下快速混合至发白，立即注入到预先准备的模温为30℃的模具模腔中，进行发泡成型，保持6h 后降温冷却到室温；
    混合液A：混合液A 3g；
B组份：由聚四氢呋喃醚二醇24g、环状聚二甲基硅氧烷3.0g、聚氧乙烯聚氧丙烯季戊四醇醚2.0g、菜籽油3g、羧苯甲酰磺胺噻唑0.6g、水2.2g、环戊烷27g、1-溴金刚烷2g、盐酸多西环素2g、五羟基黄酮-3-鼠李糖苷3g、桑色素6g、山柰酚-7-O-β-D-葡萄糖苷3g、有机膨润土3g和醋酸卡泊芬净3.2g；
C组份：二苯基甲烷二异氰酸酯40g；
（3）打开模具，将泡沫从模腔中取出，并在室温条件下放置72h，即可得到建筑外墙保温和阻燃性聚氨酯发泡材料。
  下面通过相关实验数据进一步说明本发明的有益效果：
其阻燃性通过氧指数法测定，用南京上元仪器厂氧指数测定仪，按GB/T2406-93 塑料燃烧性能试验方法-氧指数法测定测定氧指数,保温性能依据
GB/T 3399-1982进行测试，按照JIS L1099B 标准对阻燃性（以耐静水压为指标）。
表一 建筑外墙保温和阻燃性聚氨酯发泡材料性能
实验组 实例一 实例二 实例三 实例四 实例五
氧指数/% 24.2 25.6 25.4 25.3 25.7
泡沫密度/g/cm3 0.035 0.046 0.042 0.045 0.042
导热系数（w/m.K） 0.023 0.023 0.022 0.023 0.021
  从表一可以发现，发泡材料氧指数较高，泡沫密度小，很低的导热系数。

Claims (3)

1.建筑外墙保温和阻燃性聚氨酯发泡材料的制备方法，其特征在于：
（1）在反应器中加入玉米淀粉40g、32g磷酸、二巯基丙烷磺酸钠1.4g、二乙烯三胺五甲叉膦酸盐1.2g和2,3,6,7,10,11-六羟基三亚苯基苯1.3g，以转速60rpm进行搅拌,升温到40℃，反应3h，在烘箱中干燥，加入红磷21g和2-乙基己基硫酸酯钠盐1.4g，在50℃下以转速90rpm下进行搅拌混合均匀，搅拌时间40min，得混合液A；
（2） 把混合液A、B组份和C组份在20℃的室温条件下快速混合至发白，立即注入到预先准备的模温为30℃的模具模腔中，进行发泡成型，保持6h 后降温冷却到室温；
     混合液A：混合液A2~3重量份；
B组份：由二元醇10~24重量份、环状聚二甲基硅氧烷1~3.0重量份、聚氧乙烯聚氧丙烯季戊四醇醚2.0重量份、菜籽油1~3重量份、催化剂0.3~0.6重量份、水0.8~2.2重量份、环戊烷18~27重量份、1-溴金刚烷1~2重量份、盐酸多西环素1~2重量份、五羟基黄酮-3-鼠李糖苷2~3重量份、桑色素4~6重量份、山柰酚-7-O-β-D-葡萄糖苷2~3重量份、有机膨润土1~3重量份，所述二元醇为聚碳酸酯二醇、聚四氢呋喃醚二醇的任意一种；
C组份：异氰酸酯为25~40重量份，混合液A、B组份和C组份总重量份为100份；
（3）打开模具，将泡沫从模腔中取出，并在室温条件下放置72h，即可得到建筑外墙保温和阻燃性聚氨酯发泡材料。
2.如权利要求1建筑外墙保温和阻燃性聚氨酯发泡材料的制备方法，其特征在于：催化剂为二硫化四甲基秋兰姆、二(三甲基硅基)碳酰二亚胺、磷酸伯安喹、2-[N-(间羟基)-对甲苯胺甲基]-2-咪唑啉甲磺酸盐、对甲苯磺酰胺和羧苯甲酰磺胺噻唑的任意一种。
3.如权利要求1建筑外墙保温和阻燃性聚氨酯发泡材料的制备方法，其特征在于：异氰酸酯为二苯基甲烷二异氰酸酯、甲苯二异氰酸酯、1,6-己二异氰酸酯中的一种。
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