CN113527570A - 一种纺织品用阻燃无氟防水剂及其制备方法 - Google Patents
一种纺织品用阻燃无氟防水剂及其制备方法 Download PDFInfo
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Abstract
本发明属于纺织助剂领域,具体涉及一种纺织品用阻燃无氟防水剂及其制备方法,该阻燃无氟防水剂包括以下重量份数的原料:总单体20‑50份、乳化剂1‑3份、PH缓冲剂0.5‑1份、引发剂0.05‑0.3份、去离子水50‑70份,并经带温带压反应得到阻燃无氟防水剂。本发明产品有效改善现有技术中防水助剂存在防水效果差、耐洗差、阻燃性差等不足。兼顾综合性能,解决了问题的同时,具有高效抗菌性和耐候性等性能。可以预见,该材料将在纺织材料迎来广阔的市场前景,尤其适用家装、汽车内饰乃至户外使用领域等。
Description
技术领域
本发明属于纺织助剂领域,具体涉及一种纺织品用阻燃无氟防水剂及其制备方法。
背景技术
织物的防水处理是通过对织物表面进行处理,以降低织物纤维的毛细管附加压力,减小纤维表面张力,从而阻止水渗透织物表面,但同时不影响织物的透气性。目前衣物穿着是否舒服是消费者选择服装的一个重要考虑因素。耐久防水处理后,能长时间阻止湿气从外表深入衣物内部,给穿着者舒适的感受。因为这个原因,耐久防水处理织物的需求量大。
防水剂分为为含氟防水剂及不含氟防水剂。由于含氟防水剂不仅具有优异的防水效果,还有高效的防油效果。但是含氟防水剂中存在如PFOA或PFOS等物质,具有毒害作用。而常用的无氟防水剂的性能,比如耐洗性等难以达到含氟防水剂的效果。因此,近年来正大力研发无氟防水剂的防水效果的挖掘以替代含氟防水剂。
另一方面,防水剂是用在织物表面处理的一种有机助剂,有机高分子大多都是易燃物;同时织物也易燃,这存在重大的安全隐患,近年来由于有机高分子易燃引发的火灾不胜其数。
为解决由上述防水剂存在的客观问题,急需开发出一种新型阻燃无氟防水剂的这项工作就显得尤为重要。
发明内容
本发明的目的是针对现有技术中防水助剂存在防水效果差、耐洗差、阻燃性差等不足,提供了一种纺织品用阻燃无氟防水剂及其制备方法。通过配方设计,解决了问题的同时,具有高效抗菌性和耐候性等性能。可以预见,该材料将在纺织材料迎来广阔的市场前景,尤其适用家装、汽车内饰乃至户外使用领域等。
为实现上述目的,本发明解决其技术问题所采用的技术方案是:
一种纺织品用阻燃无氟防水剂,包括以下重量份数的原料:
总单体20-50份、乳化剂1-3份、PH缓冲剂0.5-1份、引发剂0.05-0.3份、去离子水50-70份;
所述总单体包括氯乙烯类单体、乙烯基硅烷类单体、丙烯酸酯类单体以及功能单体。
作为优选,所述氯乙烯类单体为氯乙烯或氯乙烯与偏氯乙烯的混合物。
作为优选,所述乙烯基硅烷类单体为乙烯基三氯硅烷、乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷或乙烯基三叔丁氧基硅烷中的一种或几种。
作为优选,所述丙烯酸酯类单体为烷基碳原子数8-22的丙烯酸烷基酯或丙烯酸环烷基酯。
作为优选,所述功能单体为丙烯腈与叔碳酸乙烯酯的混合物。
作为优选,所述乳化剂为季铵盐烷基聚氧乙烯马来酸二酯。
一种纺织品用阻燃无氟防水剂的制备方法,具体包括如下的具体步骤:
(1)称取20-50份总单体,1-3份乳化剂,投入预乳化釜中,在搅拌速度为不低于200r/min的条件下,搅拌乳化1-2h,得到预乳化单体溶液;
(2)取50-70份去离子水,0.5-1份PH缓冲剂,0.05-0.3份引发剂充分搅拌溶解后加入步骤(1)预乳化釜中;
(3)反应:按体积计,先取步骤(1)预乳化单体1/6-1/5于聚合釜中,搅拌30min后升温至70-80℃,然后加入步骤(2)溶解好的引发剂1/5-1/4开始聚合反应,待聚合釜压力由初始压力降0.2MPa时开始连续补加剩余的预乳化单体和引发剂,4-6小时补加完,将反应温度升至80±1℃,继续反应至聚合釜反应压力低于0.1MPa;降温至40℃以下,抽真空至0.09MPa以下,回收未反应的氯乙烯,停真空泵,出料,过滤,包装,即得目标产物。
本发明具有如下的有益效果:
(1)本发明提供了一种纺织品用阻燃无氟防水剂,其结构中含有长链的烷基链、硅氧烷结构,长链烷基链可提供高效的疏水性;硅氧烷结构中,由于Si素的低表面张力,具有优异的疏水性,使无氟防水剂的防水性能更好。
(2)本发明提供了一种纺织品用阻燃无氟防水剂,其结构中含有氯乙烯、丙烯腈结构,一方面,卤素以及N素的协同,具有高效的阻燃性能;另一方面,强极性基团有利于在织物表面的附着,增强耐洗性。
(3)本发明提供了一种纺织品用阻燃无氟防水剂,其结构中含有叔碳酸乙烯酯结构,不仅可提供良好的耐水性还具有优异的耐候性。
(4)本发明提供了一种纺织品用阻燃无氟防水剂,其使用反应型季铵盐乳化剂,第一,反应型乳化剂可以键接到体系中而不迁移析出,防水性能、耐洗性更优;第二,季铵盐体系具有优异的广谱抗菌性。
(5)本发明提供了一种纺织品用阻燃无氟防水剂,通过配方设计,解决了传统防水助剂存在防水效果差、耐洗差、阻燃性差的问题,同时具有高效抗菌性和耐候性等性能。该材料将在纺织材料迎来广阔的市场前景,尤其适用家装、汽车内饰乃至户外使用领域等。
具体实施方式:
以下结合实施例对本发明进行详细说明。但应理解,以下实施例仅是对本发明实施方式的举例说明,而非是对本发明的范围限定。
实施例1
一种纺织品用阻燃无氟防水剂,包括以下重量份数的原料:
总单体20份:氯乙烯0.5份、偏氯乙烯0.25份、乙烯基三乙氧基硅烷1份、丙烯酸辛酯12.5份、3,3,5-三甲基甲基丙烯酸环己酯5.5份、丙烯腈0.1份、叔碳酸乙烯酯0.15份;
乳化剂:季铵盐十八烷基聚氧乙烯马来酸二酯(n=10)1份;
PH缓冲剂:碳酸氢钠0.5份;
引发剂:过硫酸铵0.05份;
去离子水70份。
一种纺织品用阻燃无氟防水剂的制备方法,具体包括如下的具体步骤:
(1)称取20份总单体,1份乳化剂,投入预乳化釜中,在搅拌速度为不低于200r/min的条件下,搅拌乳化1h,得到预乳化单体溶液;
(2)取70份去离子水,0.5份PH缓冲剂,0.05份引发剂充分搅拌溶解后加入步骤(1)预乳化釜中;
(3)反应:按体积计,先取步骤(1)预乳化单体1/6于聚合釜中,搅拌30min后升温至70-80℃,然后加入步骤(2)溶解好的引发剂1/5开始聚合反应,待聚合釜压力由初始压力降0.2MPa时开始连续补加剩余的预乳化单体和引发剂,4小时补加完,将反应温度升至80±1℃,继续反应至聚合釜反应压力低于0.1MPa;降温至40℃以下,抽真空至0.09MPa以下,回收未反应的氯乙烯,停真空泵,出料,过滤,包装,即得目标产物。
实施例2
一种纺织品用阻燃无氟防水剂,包括以下重量份数的原料:
总单体50份:氯乙烯10份、偏氯乙烯3份、乙烯基三甲氧基硅烷2份、丙烯酸二十二酯18份、丙烯酸-4-叔丁基环己酯12份、丙烯腈1.2份、叔碳酸乙烯酯3.8份;
乳化剂:季铵盐壬基酚基聚氧乙烯马来酸二酯(n=20)3份;
PH缓冲剂:碳酸氢钠1份;
引发剂:过硫酸铵0.3份;
去离子水50份。
一种纺织品用阻燃无氟防水剂的制备方法,具体包括如下的具体步骤:
(1)称取50份总单体,3份乳化剂,投入预乳化釜中,在搅拌速度为不低于200r/min的条件下,搅拌乳化2h,得到预乳化单体溶液;
(2)取50份去离子水,1份PH缓冲剂,0.3份引发剂充分搅拌溶解后加入步骤(1)预乳化釜中;
(3)反应:按体积计,先取步骤(1)预乳化单体1/5于聚合釜中,搅拌30min后升温至80℃,然后加入步骤(2)溶解好的引发剂1/4开始聚合反应,待聚合釜压力由初始压力降0.2MPa时开始连续补加剩余的预乳化单体和引发剂,6小时补加完,将反应温度升至80±1℃,继续反应至聚合釜反应压力低于0.1MPa;降温至40℃以下,抽真空至0.09MPa以下,回收未反应的氯乙烯,停真空泵,出料,过滤,包装,即得目标产物。
实施例3
一种纺织品用阻燃无氟防水剂,包括以下重量份数的原料:
总单体30份:氯乙烯0.3份、偏氯乙烯0.1份、乙烯基三甲氧基硅烷2份、丙烯酸二十酯18份、3,3,5-三甲基甲基丙烯酸环己酯8份、丙烯腈0.6份、叔碳酸乙烯酯1份;
乳化剂:季铵盐十二烷基聚氧乙烯马来酸二酯(n=10)2份;
PH缓冲剂:碳酸氢钠0.7份;
引发剂:过硫酸铵0.1份;
去离子水65份。
一种纺织品用阻燃无氟防水剂的制备方法,具体包括如下的具体步骤:
(1)称取30份总单体,2份乳化剂,投入预乳化釜中,在搅拌速度为不低于200r/min的条件下,搅拌乳化1.5h,得到预乳化单体溶液;
(2)取65份去离子水,0.7份PH缓冲剂,0.1份引发剂充分搅拌溶解后加入步骤(1)预乳化釜中;
(3)反应:按体积计,先取步骤(1)预乳化单体1/6于聚合釜中,搅拌30min后升温至70℃,然后加入步骤(2)溶解好的引发剂1/5开始聚合反应,待聚合釜压力由初始压力降0.2MPa时开始连续补加剩余的预乳化单体和引发剂,4小时补加完,将反应温度升至80±1℃,继续反应至聚合釜反应压力低于0.1MPa;降温至40℃以下,抽真空至0.09MPa以下,回收未反应的氯乙烯,停真空泵,出料,过滤,包装,即得目标产物。
实施例4
一种纺织品用阻燃无氟防水剂,包括以下重量份数的原料:
总单体40份:氯乙烯7份、乙烯基三氯硅烷4份、丙烯酸月桂酯16.5份、丙烯酸硬脂酯8.5份、丙烯腈1.3份、叔碳酸乙烯酯2.7份;
乳化剂:季铵盐壬基酚基聚氧乙烯马来酸二酯(n=20)3份;
PH缓冲剂:碳酸氢钠0.8份;
引发剂:过硫酸铵0.2份;
去离子水65份。
一种纺织品用阻燃无氟防水剂的制备方法,具体包括如下的具体步骤:
(1)称取40份总单体,3份乳化剂,投入预乳化釜中,在搅拌速度为不低于200r/min的条件下,搅拌乳化2h,得到预乳化单体溶液;
(2)取65份去离子水,0.8份PH缓冲剂,0.2份引发剂充分搅拌溶解后加入步骤(1)预乳化釜中;
(3)反应:按体积计,先取步骤(1)预乳化单体1/5于聚合釜中,搅拌30min后升温至75℃,然后加入步骤(2)溶解好的引发剂1/4开始聚合反应,待聚合釜压力由初始压力降0.2MPa时开始连续补加剩余的预乳化单体和引发剂,5小时补加完,将反应温度升至80±1℃,继续反应至聚合釜反应压力低于0.1MPa;降温至40℃以下,抽真空至0.09MPa以下,回收未反应的氯乙烯,停真空泵,出料,过滤,包装,即得目标产物。
实施例5
一种纺织品用阻燃无氟防水剂,包括以下重量份数的原料:
总单体40份:氯乙烯0.4份、偏氯乙烯0.2份、乙烯基三叔丁氧基硅烷2.2份、丙烯酸月桂酯16份、丙烯酸二十酯10份、丙烯酸硬脂酯6.5份、3,3,5-三甲基甲基丙烯酸环己酯3.5份、丙烯腈0.6份、叔碳酸乙烯酯0.6份;
乳化剂:季铵盐十二烷基聚氧乙烯马来酸二酯(n=20)2份;
PH缓冲剂:碳酸氢钠0.8份;
引发剂:过硫酸铵0.2份;
去离子水65份。
一种纺织品用阻燃无氟防水剂的制备方法,具体包括如下的具体步骤:
(1)称取40份总单体,2份乳化剂,投入预乳化釜中,在搅拌速度为不低于200r/min的条件下,搅拌乳化2h,得到预乳化单体溶液;
(2)取65份去离子水,0.8份PH缓冲剂,0.2份引发剂充分搅拌溶解后加入步骤(1)预乳化釜中;
(3)反应:按体积计,先取步骤(1)预乳化单体1/5于聚合釜中,搅拌30min后升温至80℃,然后加入步骤(2)溶解好的引发剂1/4开始聚合反应,待聚合釜压力由初始压力降0.2MPa时开始连续补加剩余的预乳化单体和引发剂,6小时补加完,将反应温度升至80±1℃,继续反应至聚合釜反应压力低于0.1MPa;降温至40℃以下,抽真空至0.09MPa以下,回收未反应的氯乙烯,停真空泵,出料,过滤,包装,即得目标产物。
实施对比例1-3均与实施例1的无氟防水剂对比:
实施对比例1
一种无氟防水剂,包括以下重量份数的原料:
总单体19.15份:乙烯基三乙氧基硅烷1份、丙烯酸辛酯12.5份、3,3,5-三甲基甲基丙烯酸环己酯5.5份、叔碳酸乙烯酯0.15份;
乳化剂:烯丙基烷基聚氧乙烯醇0.5份、十二烷基苯磺酸钠0.5份;
PH缓冲剂:碳酸氢钠0.5份;
引发剂:过硫酸铵0.05份;
去离子水70份。
一种纺织品用阻燃无氟防水剂的制备方法,具体包括如下的具体步骤:
(1)称取19.15份总单体,1份乳化剂,投入预乳化釜中,在搅拌速度为不低于200r/min的条件下,搅拌乳化1h,得到预乳化单体溶液;
(2)取70份去离子水,0.5份PH缓冲剂,0.05份引发剂充分搅拌溶解后加入步骤(1)预乳化釜中;
(3)反应:按体积计,先取步骤(1)预乳化单体1/6于聚合釜中,搅拌30min后升温至70-80℃,然后加入步骤(2)溶解好的引发剂1/5开始聚合反应,待聚合釜压力由初始压力降0.2MPa时开始连续补加剩余的预乳化单体和引发剂,4小时补加完,将反应温度升至80±1℃,继续反应至聚合釜反应压力低于0.1MPa;降温至40℃以下,抽真空至0.09MPa以下,回收未反应的氯乙烯,停真空泵,出料,过滤,包装,即得目标产物。
实施对比例2
一种纺织品用阻燃无氟防水剂,包括以下重量份数的原料:
总单体19份:氯乙烯0.5份、偏氯乙烯0.25份、丙烯酸辛酯12.5份、3,3,5-三甲基甲基丙烯酸环己酯5.5份、丙烯腈0.1份、叔碳酸乙烯酯0.15份;
乳化剂:烯丙基烷基聚氧乙烯醇0.5份、十二烷基苯磺酸钠0.5份;
PH缓冲剂:碳酸氢钠0.5份;
引发剂:过硫酸铵0.05份;
去离子水70份。
一种纺织品用阻燃无氟防水剂的制备方法,具体包括如下的具体步骤:
(1)称取19份总单体,1份乳化剂,投入预乳化釜中,在搅拌速度为不低于200r/min的条件下,搅拌乳化1h,得到预乳化单体溶液;
(2)取70份去离子水,0.5份PH缓冲剂,0.05份引发剂充分搅拌溶解后加入步骤(1)预乳化釜中;
(3)反应:按体积计,先取步骤(1)预乳化单体1/6于聚合釜中,搅拌30min后升温至70-80℃,然后加入步骤(2)溶解好的引发剂1/5开始聚合反应,待聚合釜压力由初始压力降0.2MPa时开始连续补加剩余的预乳化单体和引发剂,4小时补加完,将反应温度升至80±1℃,继续反应至聚合釜反应压力低于0.1MPa;降温至40℃以下,抽真空至0.09MPa以下,回收未反应的氯乙烯,停真空泵,出料,过滤,包装,即得目标产物。
实施对比例3
一种纺织品用阻燃无氟防水剂,包括以下重量份数的原料:
总单体19.85份:氯乙烯0.5份、偏氯乙烯0.25份、乙烯基三乙氧基硅烷1份、丙烯酸辛酯12.5份、3,3,5-三甲基甲基丙烯酸环己酯5.5份、丙烯腈0.1份;
乳化剂:烯丙基烷基聚氧乙烯醇0.5份、十二烷基苯磺酸钠0.5份;
PH缓冲剂:碳酸氢钠0.5份;
引发剂:过硫酸铵0.05份;
去离子水70份。
一种纺织品用阻燃无氟防水剂的制备方法,具体包括如下的具体步骤:
(1)称取19.85份总单体,1份乳化剂,投入预乳化釜中,在搅拌速度为不低于200r/min的条件下,搅拌乳化1h,得到预乳化单体溶液;
(2)取70份去离子水,0.5份PH缓冲剂,0.05份引发剂充分搅拌溶解后加入步骤(1)预乳化釜中;
(3)反应:按体积计,先取步骤(1)预乳化单体1/6于聚合釜中,搅拌30min后升温至70-80℃,然后加入步骤(2)溶解好的引发剂1/5开始聚合反应,待聚合釜压力由初始压力降0.2MPa时开始连续补加剩余的预乳化单体和引发剂,4小时补加完,将反应温度升至80±1℃,继续反应至聚合釜反应压力低于0.1MPa;降温至40℃以下,抽真空至0.09MPa以下,回收未反应的氯乙烯,停真空泵,出料,过滤,包装,即得目标产物。
实施对比例4
一种纺织品用阻燃无氟防水剂,包括以下重量份数的原料:
总单体20份:氯乙烯0.5份、偏氯乙烯0.25份、乙烯基三乙氧基硅烷1份、丙烯酸辛酯12.5份、3,3,5-三甲基甲基丙烯酸环己酯5.5份、丙烯腈0.1份、叔碳酸乙烯酯0.15份;
乳化剂:烯丙基烷基聚氧乙烯醇0.5份、十二烷基苯磺酸钠0.5份;
PH缓冲剂:碳酸氢钠0.5份;
引发剂:过硫酸铵0.05份;
去离子水70份。
一种纺织品用阻燃无氟防水剂的制备方法,具体包括如下的具体步骤:
(1)称取20份总单体,1份乳化剂,投入预乳化釜中,在搅拌速度为不低于200r/min的条件下,搅拌乳化1h,得到预乳化单体溶液;
(2)取70份去离子水,0.5份PH缓冲剂,0.05份引发剂充分搅拌溶解后加入步骤(1)预乳化釜中;
(3)反应:按体积计,先取步骤(1)预乳化单体1/6于聚合釜中,搅拌30min后升温至70-80℃,然后加入步骤(2)溶解好的引发剂1/5开始聚合反应,待聚合釜压力由初始压力降0.2MPa时开始连续补加剩余的预乳化单体和引发剂,4小时补加完,将反应温度升至80±1℃,继续反应至聚合釜反应压力低于0.1MPa;降温至40℃以下,抽真空至0.09MPa以下,回收未反应的氯乙烯,停真空泵,出料,过滤,包装,即得目标产物。
分别将实施例1-5、实施对比例1-4制备的无氟防水剂按其固含浓度稀释到约10wt%左右,涂覆于涤纶织物上。可采用涂布,浸渍,喷涂,轧染,辊涂或者它们的组合方法。
具体应用方法:通过将欲得固体成分浓度设定为10wt%来作为轧染浴使用,在该轧染浴中对涤纶织物进行轧染,接下来,用压浆辊除去过剩的液体,进行干燥。涤纶干燥通常在约80℃的下进行约1h左右干燥,然后在约170℃下约1min的进行熟化,结束防水处理。
分别测定本发明实施例1-5、实施对比例1-4制备的无氟防水剂的物理性能,包括防水性、阻燃性、耐候性和抗菌性,结果如表1所示。
表1各实施例物理测试性能
首先,从表1中可以看出,本发明的阻燃无氟防水剂具有更优的防水效果和阻燃效果;
第二,本发明的阻燃无氟防水剂具有更优的功能性,尤其是抗菌性和抗菌持久性;
第三,本发明的阻燃无氟防水剂具有更优的耐候性。
综合而言,与现有技术相比,本发明的阻燃无氟防水剂不仅克服现有技术中防水助剂存在防水效果差、耐洗差、阻燃性差等缺陷,在其他性能不变的情况下,还具有高效抗菌性和耐候性等性能,可以预见,该材料将在纺织材料迎来广阔的市场前景,尤其适用家装、汽车内饰乃至户外使用领域等。
其中测试方法如下:
(1)防水性:测定防水效果(依据JIS L1092-2009)进行防淋水测试。用防水性NO.表示防喷淋水性(如下述表2中所示。附在数值后的后缀“+”表示性能稍好于所述数值表示的性能)。
表2防喷淋水性
防水性NO. | 状态 |
100 | 表面没有润湿或者水滴附着 |
90 | 表面没有润湿但有小水滴附着 |
80 | 表面有独立的小水滴状润湿 |
70 | 一半表面润湿,并有渗透布匹的独立的微小湿润 |
50 | 整个表面湿润 |
0 | 整个表面前后湿润 |
防水耐久性:用40℃的洗涤液洗涤25分钟,脱水3分钟,漂洗2分钟,脱色3分钟,漂洗2分钟,脱色3分钟,进行滚筒干燥,评价之后的防水效果,重复4次,测试水洗30次后的效果。
(2)阻燃性:肉眼观察,5为最优,1为最差。
(3)耐候性:置于室外同等天数,观察表面状态及防水性测试;耐候性表示方法,5为最优,1为最差。
(4)抗菌性:参考GB/T 20944.2-2007。抗菌耐久性:测试水洗30次后的抗菌效果。
以上述依据本发明的理想实施例为启示,通过上述的说明内容,相关工作人员完全可以在不偏离本项发明技术思想的范围内,进行多样的变更以及修改。本项发明的技术性范围并不局限于说明书上的内容,必须要根据权利要求范围来确定其技术性范围。
Claims (7)
1.一种纺织品用阻燃无氟防水剂,其特征在于:包括以下重量份数的原料:
总单体20-50份、乳化剂1-3份、PH缓冲剂0.5-1份、引发剂0.05-0.3份、去离子水50-70份;
所述总单体包括氯乙烯类单体、乙烯基硅烷类单体、丙烯酸酯类单体以及功能单体。
2.根据权利要求1所述的一种纺织品用阻燃无氟防水剂,其特征在于:所述氯乙烯类单体为氯乙烯或氯乙烯与偏氯乙烯的混合物。
3.根据权利要求1所述的一种纺织品用阻燃无氟防水剂,其特征在于:所述乙烯基硅烷类单体为乙烯基三氯硅烷、乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷或乙烯基三叔丁氧基硅烷中的一种或几种。
4.根据权利要求1所述的一种纺织品用阻燃无氟防水剂,其特征在于:所述丙烯酸酯类单体为烷基碳原子数8-22的丙烯酸烷基酯或丙烯酸环烷基酯。
5.根据权利要求1所述的一种纺织品用阻燃无氟防水剂,其特征在于:所述功能单体为丙烯腈与叔碳酸乙烯酯的混合物。
6.根据权利要求1所述的一种纺织品用阻燃无氟防水剂,其特征在于:所述乳化剂为季铵盐烷基聚氧乙烯马来酸二酯。
7.一种纺织品用阻燃无氟防水剂的制备方法,其特征在于:具体包括如下的具体步骤:
(1)称取20-50份总单体,1-3份乳化剂,投入预乳化釜中,在搅拌速度为不低于200r/min的条件下,搅拌乳化1-2h,得到预乳化单体溶液;
(2)取50-70份去离子水,0.5-1份PH缓冲剂,0.05-0.3份引发剂充分搅拌溶解后加入步骤(1)预乳化釜中;
(3)反应:按体积计,先取步骤(1)预乳化单体1/6-1/5于聚合釜中,搅拌30min后升温至70-80℃,然后加入步骤(2)溶解好的引发剂1/5-1/4开始聚合反应,待聚合釜压力由初始压力降0.2MPa时开始连续补加剩余的预乳化单体和引发剂,4-6小时补加完,将反应温度升至80±1℃,继续反应至聚合釜反应压力低于0.1MPa;降温至40℃以下,抽真空至0.09MPa以下,回收未反应的氯乙烯,停真空泵,出料,过滤,包装,即得目标产物。
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CN110205818A (zh) * | 2019-07-10 | 2019-09-06 | 广东湛丰精细化工有限公司 | 一种高交联性能的无氟生态防水剂及其制备方法 |
CN112521542A (zh) * | 2020-11-18 | 2021-03-19 | 李丹丹 | 一种pvc用抗菌乳液及其制备方法 |
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CN103572603A (zh) * | 2013-10-24 | 2014-02-12 | 广东德美精细化工股份有限公司 | 纺织品无氟防水剂及其制备方法、纺织品 |
CN110205818A (zh) * | 2019-07-10 | 2019-09-06 | 广东湛丰精细化工有限公司 | 一种高交联性能的无氟生态防水剂及其制备方法 |
CN112521542A (zh) * | 2020-11-18 | 2021-03-19 | 李丹丹 | 一种pvc用抗菌乳液及其制备方法 |
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