CN107880763B - 防水环保涂料及其制备方法 - Google Patents

防水环保涂料及其制备方法 Download PDF

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CN107880763B
CN107880763B CN201710947505.2A CN201710947505A CN107880763B CN 107880763 B CN107880763 B CN 107880763B CN 201710947505 A CN201710947505 A CN 201710947505A CN 107880763 B CN107880763 B CN 107880763B
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费全中
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Abstract

本发明公开了一种防水环保涂料及其制备方法,本发明防水环保涂料的制备方法,制备工艺简单,生产成本低;本发明防水环保涂料使用后,不仅能有效改善防水性能,而且具有独特防水性、高弹性和整体性,涂膜连续无任何接缝,抗渗漏,对建筑各种基材粘结性好,不易剥落,并且防腐效果优异、抗老化效果好、装饰性强,耐久性好等优点。其制备方法包括以下步骤:S1、称取各原料;S2、制备溶液A;S3、制备溶液B;S4、在溶液B中加入高岭土、碳酸钙,将合成釜的压力保持在‑0.12~‑0.08MPa,在室温条件下,搅拌2‑4小时后出料,即得。

Description

防水环保涂料及其制备方法
技术领域
本发明涉及一种防水涂料,具体来说,涉及一种防水环保涂料及其制备方法。
背景技术
防水早已不再是一个新鲜的话题,不论是隧道、桥梁、堤坝、道路、建筑还是我们日常居住的房屋,防水都不容忽视。而防水涂料经固化后形成的防水薄膜具有一定的延伸性、弹塑性、抗裂性、抗渗性及耐候性,能起到防水、防渗和保护作用。防水涂料有良好的温度适应性,操作简便,易于维修与维护。
中国专利(申请号:201110344194.3)公开了一种防水涂料,由如下成分组成:30~50%的苯丙乳液,25~30%的石粉,0~5%的重钙,1~5%的防老剂,0~5%的消泡剂,0~5%的滑石粉,3~5%的钛白粉,5~10%的聚乙烯醇,1~5%的六偏磷酸钠,10%的水。
中国专利(申请号:201510890818.X)公开了一种防水涂料,所述防水涂料包括下述重量组分:水泥10-20份、碳酸钙1-3份、石英砂5-8份、丙烯酸弹性乳液20-36份、纳米氧化硅1-5份、惰性无机粉料8-15份、分散剂1-3 份、消泡剂1-10份、阻燃剂1-5份、重质碳酸钙1-5份、硅烷偶联剂1-3份、水7-18份、乳化剂3-10份、聚乙二醇2-10份。
中国专利(申请号:201610359498.X)公开了一种防水涂料,包括由以下重量份的原料制成:聚丙烯酸树脂100份、松香15份~20份、硬脂酸锌1 份~5份、红花油6份~10份、石油6份~10份、异丁基三乙氧基硅5份~ 8份、氢氧化钾1份~5份、焦亚硫酸钠0.1份~0.2份、颜料20份~30份以及电导率小于5μS/cm的去离子水15份~20份。
然而,现有的防水涂料不能长期有效地防雨水、抗冲刷。因此,经常看到装饰和涂刷整洁美观的建筑物经不住风雨冲刷和湿气浸蚀而色彩斑驳。主要是这些涂料中缺少化学性能稳定、不溶于水的无机物质,涂料性能与建筑物本体物理性能不相近。因而,其综合防水性能效果不佳。
发明内容
本发明提供了一种防水环保涂料及其制备方法,以便实现涂料阻燃、防水功能,提高涂料使用的安全性。
技术方案如下:
一种防水环保涂料的制备方法,包括以下步骤:
S1、称取各原料:聚酯、聚醚、软化剂、高岭土、碳酸钙、偶联剂、3- 羟乙基-1,3-噁唑烷、催化剂、1,6-己二异氰酸酯;
S2、将聚醚、聚酯加入反应釜中,真空脱水后去除真空,降温至75-85℃加入1,6-己二异氰酸酯以转速为搅拌2-4小时,加入软化剂搅拌20-40分钟,得到溶液A;
S3、将溶液A抽入到合成釜中,将合成釜的压力保持在-0.12~-0.08MPa,在室温条件下,依次加入3-羟乙基-1,3-噁唑烷、催化剂、偶联剂搅拌5-15分钟,得到溶液B;
S4、在溶液B中加入高岭土、碳酸钙,将合成釜的压力保持在 -0.12~-0.08MPa,在室温条件下,搅拌2-4小时后出料,即得。
一种防水环保涂料的制备方法,包括以下步骤:
S1、按重量份称取各原料:聚酯25-30份、聚醚48-52份、软化剂1.5-4.5 份、高岭土15-25份、碳酸钙5-15份、偶联剂0.3-0.7份、3-羟乙基-1,3-噁唑烷0.4-0.9份、催化剂0.3-0.6份、1,6-己二异氰酸酯15-20份;
S2、将聚醚、聚酯加入反应釜中,将温度升至100-110℃并减压至 -0.092MPa~-0.096MPa真空脱水20-40分钟后去除真空,降温至75-85℃加入 1,6-己二异氰酸酯以转速为300-600转/分搅拌2-4小时,加入软化剂以转速为300-600转/分搅拌20-40分钟,得到溶液A;
S3、将溶液A抽入到合成釜中,将合成釜的压力保持在-0.12~-0.08MPa,在室温条件下,依次加入3-羟乙基-1,3-噁唑烷、催化剂、偶联剂以300-600 转/分搅拌5-15分钟,得到溶液B;
S4、在溶液B中加入高岭土、碳酸钙,将合成釜的压力保持在 -0.12~-0.08MPa,在室温条件下,以300-600转/分搅拌2-4小时后出料,即得。
所述偶联剂为N-(2-N-苄基氨乙基)-3-氨基丙基三甲氧基硅烷。
所述偶联剂为溴化型双酚A环氧树脂改性N-(2-N-苄基氨乙基)-3-氨基丙基三甲氧基硅烷。
所述溴化型双酚A环氧树脂改性N-(2-N-苄基氨乙基)-3-氨基丙基三甲氧基硅烷的制备过程为:将溴化型双酚A环氧树脂、丙酮按质量比为1:(2-4) 加入充满氮气的三口烧瓶中,以转速为60-180转/分搅拌5-15分钟混合均匀,再加入溴化型双酚A环氧树脂重量1.5-2.5倍的N-(2-N-苄基氨乙基)-3-氨基丙基三甲氧基硅烷在室温下以转速为60-180转/分搅拌反应50-80分钟,得到反应物;将反应物置于温度为45-55℃、真空度为-0.12~-0.09MPa下减压蒸馏去除丙酮,得到溴化型双酚A环氧树脂改性N-(2-N-苄基氨乙基)-3-氨基丙基三甲氧基硅烷。
所述催化剂为环烷酸钴、二月桂酸二丁基锡、辛酸亚锡中一种或多种的混合物。
所述软化剂为邻苯二甲酸二丁酯、邻苯二甲酸二辛酯、2,2-二甲基-3-羟基丙酸新戊二醇酯中一种或多种的混合物。在本发明的一个实施方式中,所述软化剂由23-35wt%邻苯二甲酸二辛酯和65-75wt%2,2-二甲基-3-羟基丙酸新戊二醇酯组成。
所述高岭土的粒径为1000-1500目。
所述碳酸钙为轻质碳酸钙,粒径为1000-1500目。
所述聚酯为不饱和聚酯树脂,酸值为10-30mgKOH/g。
所述聚醚的羟值为15-45mgKOH/g。
所述溴化型双酚A环氧树脂的环氧当量为300-500g/eq,溴含量为 10-30wt%。
一种防水环保涂料,由上述制备方法制备而成。
技术效果:
本发明防水环保涂料及其制备方法,制备工艺简单,生产成本低;本发明防水环保涂料使用后,不仅能有效改善防水性能,而且具有独特防水性、高弹性和整体性,涂膜连续无任何接缝,抗渗漏,对建筑各种基材粘结性好,不易剥落,并且防腐效果优异、抗老化效果好、装饰性强,耐久性好等优点。
具体实施方式
实施例中高岭土为上海跃江钛白化工制品有限公司提供的1250目煅烧高岭土,形状为白色粉末。
实施例中轻质碳酸钙为苏州名匠精细化工有限公司提供的型号为 MJ-HXQG的1250目活性轻质碳酸钙。
实施例中1,6-己二异氰酸酯,CAS号:822-06-0。
实施例中聚酯为佛山市艾迪森化工有限公司提供的型号为168-2Q的不饱和聚酯树脂,酸值为18-23mgKOH/g。
实施例中聚醚为山东蓝星东大化工有限责任公司提供的牌号为 DL-3000D的聚醚,羟值为36-39mgKOH/g。
实施例中N-(2-N-苄基氨乙基)-3-氨基丙基三甲氧基硅烷,CAS号: 209866-89-7。
实施例中溴化型双酚A环氧树脂为中国台湾南亚塑胶工业股份有限公司提供的牌号为NPEB-450A80的溴化型双酚A环氧树脂,环氧当量为410-440g/eq,溴含量为18-21wt%。
实施例中丙酮,CAS号:67-64-1。
实施例中环烷酸钴,CAS号:61789-51-3。
实施例中邻苯二甲酸二辛酯,CAS号:117-84-0。
实施例中2,2-二甲基-3-羟基丙酸新戊二醇酯,CAS号:1115-20-4。
实施例中3-羟乙基-1,3-噁唑烷,参照高峻等《3-羟乙基-1,3-噁唑烷的合成和表征及其初步应用》中1.2节的方法制备。
实施例1
防水环保涂料的制备方法,包括以下步骤:
S1、按重量份称取各原料:聚酯28份、聚醚50份、2,2-二甲基-3-羟基丙酸新戊二醇酯3份、高岭土20份、碳酸钙10份、N-(2-N-苄基氨乙基)-3- 氨基丙基三甲氧基硅烷0.5份、3-羟乙基-1,3-噁唑烷0.6份、环烷酸钴0.5份、 1,6-己二异氰酸酯18份;
S2、将聚醚、聚酯加入反应釜中,将温度升至105℃并减压至-0.095MPa 真空脱水30分钟后去除真空,降温至80℃加入1,6-己二异氰酸酯以转速为 400转/分搅拌3小时,加入2,2-二甲基-3-羟基丙酸新戊二醇酯以转速为400 转/分搅拌30分钟,得到溶液A;
S3、将溶液A抽入到合成釜中,将合成釜的压力保持在-0.1MPa,在室温25℃的条件下,依次加入3-羟乙基-1,3-噁唑烷、环烷酸钴、N-(2-N-苄基氨乙基)-3-氨基丙基三甲氧基硅烷以450转/分搅拌10分钟,得到溶液B;
S4、在溶液B中加入高岭土、碳酸钙,将合成釜的压力保持在-0.1MPa,在室温25℃的条件下,以450转/分搅拌5小时后出料,即得防水环保涂料。
实施例2
防水环保涂料的制备方法,包括以下步骤:
S1、按重量份称取各原料:聚酯28份、聚醚50份、2,2-二甲基-3-羟基丙酸新戊二醇酯3份、高岭土20份、碳酸钙10份、偶联剂0.5份、3-羟乙基-1,3-噁唑烷0.6份、环烷酸钴0.5份、1,6-己二异氰酸酯18份;
S2、将聚醚、聚酯加入反应釜中,将温度升至105℃并减压至-0.095MPa 真空脱水30分钟后去除真空,降温至80℃加入1,6-己二异氰酸酯以转速为 400转/分搅拌3小时,加入2,2-二甲基-3-羟基丙酸新戊二醇酯以转速为400 转/分搅拌30分钟,得到溶液A;
S3、将溶液A抽入到合成釜中,将合成釜的压力保持在-0.1MPa,在室温25℃的条件下,依次加入3-羟乙基-1,3-噁唑烷、环烷酸钴、偶联剂以450 转/分搅拌10分钟,得到溶液B;
S4、在溶液B中加入高岭土、碳酸钙,将合成釜的压力保持在-0.1MPa,在室温25℃的条件下,以450转/分搅拌5小时后出料,即得防水环保涂料。
所述偶联剂为溴化型双酚A环氧树脂改性N-(2-N-苄基氨乙基)-3-氨基丙基三甲氧基硅烷,所述溴化型双酚A环氧树脂改性N-(2-N-苄基氨乙基)-3- 氨基丙基三甲氧基硅烷的制备过程为:将溴化型双酚A环氧树脂、丙酮按质量比为1:3加入充满氮气的三口烧瓶中,以转速为120转/分搅拌10分钟混合均匀,再加入溴化型双酚A环氧树脂重量2倍的N-(2-N-苄基氨乙基)-3- 氨基丙基三甲氧基硅烷在室温下以转速为90转/分搅拌反应60分钟,得到反应物;将反应物置于温度为50℃、真空度为-0.1MPa下减压蒸馏去除丙酮,得到溴化型双酚A环氧树脂改性N-(2-N-苄基氨乙基)-3-氨基丙基三甲氧基硅烷。
实施例3
防水环保涂料的制备方法,包括以下步骤:
S1、按重量份称取各原料:聚酯28份、聚醚50份、邻苯二甲酸二辛酯 3份、高岭土20份、碳酸钙10份、偶联剂0.5份、3-羟乙基-1,3-噁唑烷0.6 份、环烷酸钴0.5份、1,6-己二异氰酸酯18份;
S2、将聚醚、聚酯加入反应釜中,将温度升至105℃并减压至-0.095MPa 真空脱水30分钟后去除真空,降温至80℃加入1,6-己二异氰酸酯以转速为 400转/分搅拌3小时,加入邻苯二甲酸二辛酯以转速为400转/分搅拌30分钟,得到溶液A;
S3、将溶液A抽入到合成釜中,将合成釜的压力保持在-0.1MPa,在室温25℃的条件下,依次加入3-羟乙基-1,3-噁唑烷、环烷酸钴、偶联剂以450 转/分搅拌10分钟,得到溶液B;
S4、在溶液B中加入高岭土、碳酸钙,将合成釜的压力保持在-0.1MPa,在室温25℃的条件下,以450转/分搅拌5小时后出料,即得防水环保涂料。
所述偶联剂为溴化型双酚A环氧树脂改性N-(2-N-苄基氨乙基)-3-氨基丙基三甲氧基硅烷,所述溴化型双酚A环氧树脂改性N-(2-N-苄基氨乙基)-3- 氨基丙基三甲氧基硅烷的制备过程为:将溴化型双酚A环氧树脂、丙酮按质量比为1:3加入充满氮气的三口烧瓶中,以转速为120转/分搅拌10分钟混合均匀,再加入溴化型双酚A环氧树脂重量2倍的N-(2-N-苄基氨乙基)-3- 氨基丙基三甲氧基硅烷在室温下以转速为90转/分搅拌反应60分钟,得到反应物;将反应物置于温度为50℃、真空度为-0.1MPa下减压蒸馏去除丙酮,得到溴化型双酚A环氧树脂改性N-(2-N-苄基氨乙基)-3-氨基丙基三甲氧基硅烷。
实施例4
防水环保涂料的制备方法,包括以下步骤:
S1、按重量份称取各原料:聚酯28份、聚醚50份、邻苯二甲酸二丁酯 3份、高岭土20份、碳酸钙10份、偶联剂0.5份、3-羟乙基-1,3-噁唑烷0.6 份、环烷酸钴0.5份、1,6-己二异氰酸酯18份;
S2、将聚醚、聚酯加入反应釜中,将温度升至105℃并减压至-0.095MPa 真空脱水30分钟后去除真空,降温至80℃加入1,6-己二异氰酸酯以转速为 400转/分搅拌3小时,加入邻苯二甲酸二丁酯以转速为400转/分搅拌30分钟,得到溶液A;
S3、将溶液A抽入到合成釜中,将合成釜的压力保持在-0.1MPa,在室温25℃的条件下,依次加入3-羟乙基-1,3-噁唑烷、环烷酸钴、偶联剂以450 转/分搅拌10分钟,得到溶液B;
S4、在溶液B中加入高岭土、碳酸钙,将合成釜的压力保持在-0.1MPa,在室温25℃的条件下,以450转/分搅拌5小时后出料,即得防水环保涂料。
所述偶联剂为溴化型双酚A环氧树脂改性N-(2-N-苄基氨乙基)-3-氨基丙基三甲氧基硅烷,所述溴化型双酚A环氧树脂改性N-(2-N-苄基氨乙基)-3- 氨基丙基三甲氧基硅烷的制备过程为:将溴化型双酚A环氧树脂、丙酮按质量比为1:3加入充满氮气的三口烧瓶中,以转速为120转/分搅拌10分钟混合均匀,再加入溴化型双酚A环氧树脂重量2倍的N-(2-N-苄基氨乙基)-3- 氨基丙基三甲氧基硅烷在室温下以转速为90转/分搅拌反应60分钟,得到反应物;将反应物置于温度为50℃、真空度为-0.1MPa下减压蒸馏去除丙酮,得到溴化型双酚A环氧树脂改性N-(2-N-苄基氨乙基)-3-氨基丙基三甲氧基硅烷。
实施例5
防水环保涂料的制备方法,包括以下步骤:
S1、按重量份称取各原料:聚酯28份、聚醚50份、2,2-二甲基-3-羟基丙酸新戊二醇酯2.1份、邻苯二甲酸二辛酯0.9份、高岭土20份、碳酸钙10 份、偶联剂0.5份、3-羟乙基-1,3-噁唑烷0.6份、环烷酸钴0.5份、1,6-己二异氰酸酯18份;
S2、将聚醚、聚酯加入反应釜中,将温度升至105℃并减压至-0.095MPa 真空脱水30分钟后去除真空,降温至80℃加入1,6-己二异氰酸酯以转速为 400转/分搅拌3小时,加入2,2-二甲基-3-羟基丙酸新戊二醇酯、邻苯二甲酸二辛酯以转速为400转/分搅拌30分钟,得到溶液A;
S3、将溶液A抽入到合成釜中,将合成釜的压力保持在-0.1MPa,在室温25℃的条件下,依次加入3-羟乙基-1,3-噁唑烷、环烷酸钴、偶联剂以450 转/分搅拌10分钟,得到溶液B;
S4、在溶液B中加入高岭土、碳酸钙,将合成釜的压力保持在-0.1MPa,在室温25℃的条件下,以450转/分搅拌5小时后出料,即得防水环保涂料。
所述偶联剂为溴化型双酚A环氧树脂改性N-(2-N-苄基氨乙基)-3-氨基丙基三甲氧基硅烷,所述溴化型双酚A环氧树脂改性N-(2-N-苄基氨乙基)-3- 氨基丙基三甲氧基硅烷的制备过程为:将溴化型双酚A环氧树脂、丙酮按质量比为1:3加入充满氮气的三口烧瓶中,以转速为120转/分搅拌10分钟混合均匀,再加入溴化型双酚A环氧树脂重量2倍的N-(2-N-苄基氨乙基)-3- 氨基丙基三甲氧基硅烷在室温下以转速为90转/分搅拌反应60分钟,得到反应物;将反应物置于温度为50℃、真空度为-0.1MPa下减压蒸馏去除丙酮,得到溴化型双酚A环氧树脂改性N-(2-N-苄基氨乙基)-3-氨基丙基三甲氧基硅烷。
对实施例5制备得到的防水环保涂料进行阻燃性能测试。阻火性:按 GB/T15442.4-1995的规定进行试验,耐燃时间:按GB/T15442.2-1995的规定进行试验。结果为:阻火性:质量损失为1.9g,炭化体积为8cm3;耐燃时间为40min。对实施例5制备得到的防水环保涂料,按照中华人民共和国建材行业标准JC/T894-2001进行测试,测试结果为:不透水性(0.3MPa,30分钟):不透水;潮湿基面粘结强度为1.8MPa。
测试例1
对实施例1-4制备得到的防水环保涂料进行阻燃性能测试。阻火性:按 GB/T15442.4-1995的规定进行试验,耐燃时间:按GB/T15442.2-1995的规定进行试验。具体测试数据见表1。
表1:阻火性和耐燃时间测试数据表
Figure BDA0001432071890000091
测试例2
对实施例1-4制备得到的防水环保涂料,按照中华人民共和国建材行业标准JC/T894-2001进行测试。测试结果见表2。
表2:防水性能测试结果表
Figure BDA0001432071890000092
本发明实施例2采用溴化型双酚A环氧树脂改性N-(2-N-苄基氨乙基)-3- 氨基丙基三甲氧基硅烷,阻燃和防水性能得到大幅度提高。其原因可能是在偶联剂中引入了溴元素,使得偶联剂具有很好阻燃效果,同时提高了体系的分散性。

Claims (6)

1.一种防水环保涂料的制备方法,其特征在于,包括以下步骤:
S1、按重量份称取各原料:聚酯25-30份、聚醚48-52份、软化剂1.5-4.5份、高岭土15-25份、碳酸钙5-15份、偶联剂0.3-0.7份、3-羟乙基-1,3-噁唑烷0.4-0.9份、催化剂0.3-0.6份、1,6-己二异氰酸酯15-20份;
S2、将聚醚、聚酯加入反应釜中,将温度升至100-110℃并减压至-0.092MPa~-0.096MPa真空脱水20-40分钟后去除真空,降温至75-85℃加入1,6-己二异氰酸酯以转速为300-600转/分搅拌2-4小时,加入软化剂以转速为300-600转/分搅拌20-40分钟,得到溶液A;
S3、将溶液A抽入到合成釜中,将合成釜的压力保持在-0.12~-0.08MPa,在室温条件下,依次加入3-羟乙基-1,3-噁唑烷、催化剂、偶联剂以300-600转/分搅拌5-15分钟,得到溶液B;
S4、在溶液B中加入高岭土、碳酸钙,将合成釜的压力保持在-0.12~-0.08MPa,在室温条件下,以300-600转/分搅拌2-4小时后出料,即得;所述偶联剂为溴化型双酚A环氧树脂改性N-(2-N-苄基氨乙基)-3-氨基丙基三甲氧基硅烷;
所述溴化型双酚A环氧树脂改性N-(2-N-苄基氨乙基)-3-氨基丙基三甲氧基硅烷的制备过程为:将溴化型双酚A环氧树脂、丙酮按质量比为1:(2-4)加入充满氮气的三口烧瓶中,以转速为60-180转/分搅拌5-15分钟混合均匀,再加入溴化型双酚A环氧树脂重量1.5-2.5倍的N-(2-N-苄基氨乙基)-3-氨基丙基三甲氧基硅烷在室温下以转速为60-180转/分搅拌反应50-80分钟,得到反应物;将反应物置于温度为45-55℃、真空度为-0.12~-0.09MPa下减压蒸馏去除丙酮,得到溴化型双酚A环氧树脂改性N-(2-N-苄基氨乙基)-3-氨基丙基三甲氧基硅烷;
所述软化剂由30wt%邻苯二甲酸二辛酯和70wt%2,2-二甲基-3-羟基丙酸新戊二醇酯组成。
2.根据权利要求1所述防水环保涂料的制备方法,其特征在于:所述催化剂为环烷酸钴、二月桂酸二丁基锡、辛酸亚锡中一种或多种的混合物。
3.根据权利要求1所述防水环保涂料的制备方法,其特征在于:所述高岭土的粒径为1000-1500目;所述碳酸钙为轻质碳酸钙,粒径为1000-1500目。
4.根据权利要求1所述防水环保涂料的制备方法,其特征在于:所述聚酯为不饱和聚酯树脂,酸值为10-30mgKOH/g;所述聚醚的羟值为15-45mgKOH/g;所述溴化型双酚A环氧树脂的环氧当量为300-500g/eq,溴含量为10-30wt%。
5.根据权利要求1所述防水环保涂料的制备方法,其特征在于:包括以下步骤:
S1、按重量份称取各原料:聚酯28份、聚醚50份、2,2-二甲基-3-羟基丙酸新戊二醇酯2.1份、邻苯二甲酸二辛酯0.9份、高岭土20份、碳酸钙10份、偶联剂0.5份、3-羟乙基-1,3-噁唑烷0.6份、环烷酸钴0.5份、1,6-己二异氰酸酯18份;
S2、将聚醚、聚酯加入反应釜中,将温度升至105℃并减压至-0.095MPa真空脱水30分钟后去除真空,降温至80℃加入1,6-己二异氰酸酯以转速为400转/分搅拌3小时,加入2,2-二甲基-3-羟基丙酸新戊二醇酯、邻苯二甲酸二辛酯以转速为400转/分搅拌30分钟,得到溶液A;
S3、将溶液A抽入到合成釜中,将合成釜的压力保持在-0.1MPa,在室温25℃的条件下,依次加入3-羟乙基-1,3-噁唑烷、环烷酸钴、偶联剂以450转/分搅拌10分钟,得到溶液B;
S4、在溶液B中加入高岭土、碳酸钙,将合成釜的压力保持在-0.1MPa,在室温25℃的条件下,以450转/分搅拌5小时后出料,即得防水环保涂料;
所述偶联剂为溴化型双酚A环氧树脂改性N-(2-N-苄基氨乙基)-3-氨基丙基三甲氧基硅烷,所述溴化型双酚A环氧树脂改性N-(2-N-苄基氨乙基)-3-氨基丙基三甲氧基硅烷的制备过程为:将溴化型双酚A环氧树脂、丙酮按质量比为1:3加入充满氮气的三口烧瓶中,以转速为120转/分搅拌10分钟混合均匀,再加入溴化型双酚A环氧树脂重量2倍的N-(2-N-苄基氨乙基)-3-氨基丙基三甲氧基硅烷在室温下以转速为90转/分搅拌反应60分钟,得到反应物;将反应物置于温度为50℃、真空度为-0.1MPa下减压蒸馏去除丙酮,得到溴化型双酚A环氧树脂改性N-(2-N-苄基氨乙基)-3-氨基丙基三甲氧基硅烷。
6.一种防水环保涂料,采用权利要求1-5中任一项所述制备方法制备而成。
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CN103709374A (zh) * 2013-12-26 2014-04-09 巨石集团有限公司 阻燃硅烷偶联剂的制备方法
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