CN107236444A - 一种疏水阻燃聚氨酯粉末涂料的制备方法 - Google Patents
一种疏水阻燃聚氨酯粉末涂料的制备方法 Download PDFInfo
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Abstract
本发明公开了一种疏水阻燃聚氨酯粉末涂料的制备方法，本发明加入的复合填料具有很好的防火阻燃性能，通过有机化改性，改善了其与聚氨酯的相容性，有效的降低团聚，提高成品涂膜表面的稳定性强度，该复合填料通过十二氟庚基丙基三甲氧基硅烷处理，在涂膜表面引入含氟离子，能够有效的提高涂膜表面的疏水性能，提高抗渗透性；本发明的涂料能够与基材形成稳定的涂膜，综合性能优越。
Description
技术领域
本发明属于涂料领域，具体涉及一种疏水阻燃聚氨酯粉末涂料的制备方法。
背景技术
聚氨酯粉末涂料正发展成为粉末涂料的主流，在粉末涂料中所占的比例越来越大，由于聚氨酯粉末涂料具有优良的耐候性、优良的物理力学性能和防腐蚀性，涂膜光亮丰满、耐磨、耐划伤、耐溶剂，流平性好、附着力强；
粉末涂料是环境友好型涂料，粉末涂料和涂装具有涂膜性能优异、工艺简便，一次涂覆可达较高厚度，节省能源和资源、减少环境污染、易实现自动化、粉末可回收的优点，一出现即可获得广泛关注，聚氨酯粉末涂料涂层不仅具有较高的装饰性和优良的物理力学性能，而且有较全面的耐化学药品性，特别是不易黄变、耐候性和耐光性。聚氨酯粉末涂料正发展成为粉末涂料的主流，在粉末涂料中所占的比例越来越大，由于聚氨酯粉末涂料具有优良的耐候性、优良的物理力学性能和防腐蚀性，涂膜光亮丰满、耐磨、耐划伤、耐溶剂，流平性好、附着力强。目前被广泛应用于冰箱、洗衣机、空调等家电及高级家具、汽车、摩托车等产业；
但是目前聚氨酯粉末涂料的阻燃性能欠佳，无机阻燃添加剂与聚氨酯的相容性差，造成涂膜表面的稳定性差，因此在火灾发生时，成膜物质往往先于脱水催化剂受热分解，产生较多的可燃的挥发性有机化合物，影响炭层的形成和结构，进而影响对基材的保护作用，同时传统聚氨酯粉末涂料的表面疏水性差，容易造成水渗透，造成涂膜的破损。
发明内容
本发明的目的在于针对现有技术中聚氨酯粉末涂料的阻燃性能欠佳，无机阻燃添加剂与聚氨酯的相容性差，造成涂膜表面的稳定性差的问题及聚氨酯粉末涂料的表面疏水性差的问题，提供一种疏水阻燃聚氨酯粉末涂料的制备方法。
为实现上述目的，本发明采用以下技术方案：
一种疏水阻燃聚氨酯粉末涂料的制备方法，包括以下步骤：
(1)取1-2重量份的硫酸亚铁铵，加入到其重量60-70倍的去离子水中，搅拌均匀，加入3-5重量份的均苯四酸二酐，在47-50℃下保温搅拌10-15分钟，加入12-16重量份的碳纳米管，磁力搅拌3-10分钟，得羧基化碳纳米管溶液；
(2)取10-14重量份的聚四氢呋喃醚二醇，在70-75℃下保温搅拌5-10分钟，加入6-8重量份的无机阻燃剂，继续保温10-20分钟，加入10-14重量份的聚乙烯吡咯烷酮，升高温度为85-90℃，加入1-2重量份的氟化钠，保温反应4-6分钟，得阻燃分散液；
(3)取0.6-1重量份的乙酰丙酮锌，加入到其重量10-13倍的无水乙醇中，搅拌均匀，加入2-3重量份的十二氟庚基丙基三甲氧基硅烷，在60-65℃下保温搅拌4-10分钟，得氟化硅烷醇分散液；
(4)取上述阻燃分散液、氟化硅烷醇分散液混合，搅拌均匀，加入上述羧基化碳纳米管溶液，送入到反应釜中，在86-90℃下保温搅拌1-2小时，出料，与2-3重量份的异氰尿酸三缩水甘油酯混合，搅拌至常温，得氟酯化阻燃分散液；
(5)取氟酯化阻燃分散液、0.8-1重量份的三乙醇胺混合，超声10-15分钟，抽滤，将沉淀水洗，常温干燥2-3小时，得氟酯化阻燃填料；
(6)取130-150重量份的聚丙二醇ppg2000，在108-110℃下真空脱水2-3小时，降低温度至55-60℃，保温备用，得预处理聚丙二醇ppg2000；
(7)取上述氟酯化阻燃填料、与100-110重量份的2,4-甲苯二异氰酸酯混合，在55-60℃下保温搅拌20-30分钟，加入上述预处理聚丙二醇ppg2000，送入到反应釜中，通入氮气，加入3-5重量份的氯化亚锡，升高温度为76-85℃，保温反应4-6小时，冷却出料，得磷化聚氨酯预聚体；
(8)取上述磷化聚氨酯预聚体，与10-15重量份的固化剂混合，在80-90℃下固化10-13小时，冷却至常温，磨成细粉，过筛，得所述疏水阻燃聚氨酯粉末涂料。
所述的无机阻燃剂为三氧化二锑、滑石粉中的一种或两种的混合物，当为两种的混合物时，三氧化二锑、滑石粉的重量比为10-14:1-2。
所述的固化剂为三羟甲基丙烷。
本发明的优点：
本发明首先将碳纳米管通过均苯四酸二酐羧基化，然后将其与阻燃分散液、氟化硅烷醇混合改性，得到无机阻燃剂、碳纳米管的复合填料，该复合填料可以在燃烧时形成均匀稳定的碳层，能够起到很好的防火阻燃性，该复合填料通过有机化改性，改善了其与聚氨酯的相容性，有效的降低团聚，提高成品涂膜表面的稳定性强度，该复合填料通过十二氟庚基丙基三甲氧基硅烷处理，在涂膜表面引入含氟离子，能够有效的提高涂膜表面的疏水性能，提高抗渗透性；本发明的涂料能够与基材形成稳定的涂膜，综合性能优越。
下面结合实施例对本发明作进一步地详细说明，但本发明的实施方式不限于此，在不脱离本发明上述技术思想情况下，根据本领域普通技术知识和惯用手段，做出各种替换和变更，均应包括在本发明的范围内。
实施例1
一种疏水阻燃聚氨酯粉末涂料的制备方法，包括以下步骤：
(1)取2重量份的硫酸亚铁铵，加入到其重量70倍的去离子水中，搅拌均匀，加入5重量份的均苯四酸二酐，在47℃下保温搅拌15分钟，加入12重量份的碳纳米管，磁力搅拌3分钟，得羧基化碳纳米管溶液；
(2)取14重量份的聚四氢呋喃醚二醇，在70℃下保温搅拌5分钟，加入6重量份的三氧化二锑，继续保温20分钟，加入10重量份的聚乙烯吡咯烷酮，升高温度为90℃，加入2重量份的氟化钠，保温反应4分钟，得阻燃分散液；
(3)取0.6重量份的乙酰丙酮锌，加入到其重量10倍的无水乙醇中，搅拌均匀，加入3重量份的十二氟庚基丙基三甲氧基硅烷，在65℃下保温搅拌4分钟，得氟化硅烷醇分散液；
(4)取上述阻燃分散液、氟化硅烷醇分散液混合，搅拌均匀，加入上述羧基化碳纳米管溶液，送入到反应釜中，在90℃下保温搅拌1小时，出料，与3重量份的异氰尿酸三缩水甘油酯混合，搅拌至常温，得氟酯化阻燃分散液；
(5)取氟酯化阻燃分散液、0.8重量份的三乙醇胺混合，超声15分钟，抽滤，将沉淀水洗，常温干燥2小时，得氟酯化阻燃填料；
(6)取150重量份的聚丙二醇ppg2000，在108℃下真空脱水2小时，降低温度至60℃，保温备用，得预处理聚丙二醇ppg2000；
(7)取上述氟酯化阻燃填料、与110重量份的2,4-甲苯二异氰酸酯混合，在60℃下保温搅拌30分钟，加入上述预处理聚丙二醇ppg2000，送入到反应釜中，通入氮气，加入3重量份的氯化亚锡，升高温度为85℃，保温反应4小时，冷却出料，得磷化聚氨酯预聚体；
(8)取上述磷化聚氨酯预聚体，与10重量份的三羟甲基丙烷混合，在80℃下固化13小时，冷却至常温，磨成细粉，过筛，得所述疏水阻燃聚氨酯粉末涂料。
实施例2
一种疏水阻燃聚氨酯粉末涂料的制备方法，包括以下步骤：
(1)取2重量份的硫酸亚铁铵，加入到其重量70倍的去离子水中，搅拌均匀，加入5重量份的均苯四酸二酐，在50℃下保温搅拌15分钟，加入16重量份的碳纳米管，磁力搅拌10分钟，得羧基化碳纳米管溶液；
(2)取14重量份的聚四氢呋喃醚二醇，在75℃下保温搅拌10分钟，加入8重量份的滑石粉，继续保温20分钟，加入14重量份的聚乙烯吡咯烷酮，升高温度为90℃，加入2重量份的氟化钠，保温反应6分钟，得阻燃分散液；
(3)取1重量份的乙酰丙酮锌，加入到其重量13倍的无水乙醇中，搅拌均匀，加入3重量份的十二氟庚基丙基三甲氧基硅烷，在65℃下保温搅拌10分钟，得氟化硅烷醇分散液；
(4)取上述阻燃分散液、氟化硅烷醇分散液混合，搅拌均匀，加入上述羧基化碳纳米管溶液，送入到反应釜中，在90℃下保温搅拌2小时，出料，与3重量份的异氰尿酸三缩水甘油酯混合，搅拌至常温，得氟酯化阻燃分散液；
(5)取氟酯化阻燃分散液、1重量份的三乙醇胺混合，超声15分钟，抽滤，将沉淀水洗，常温干燥3小时，得氟酯化阻燃填料；
(6)取150重量份的聚丙二醇ppg2000，在110℃下真空脱水3小时，降低温度至60℃，保温备用，得预处理聚丙二醇ppg2000；
(7)取上述氟酯化阻燃填料、与110重量份的2,4-甲苯二异氰酸酯混合，在60℃下保温搅拌30分钟，加入上述预处理聚丙二醇ppg2000，送入到反应釜中，通入氮气，加入5重量份的氯化亚锡，升高温度为85℃，保温反应6小时，冷却出料，得磷化聚氨酯预聚体；
(8)取上述磷化聚氨酯预聚体，与15重量份的三羟甲基丙烷混合，在90℃下固化13小时，冷却至常温，磨成细粉，过筛，得所述疏水阻燃聚氨酯粉末涂料。
实施例3
一种疏水阻燃聚氨酯粉末涂料的制备方法，包括以下步骤：
(1)取1重量份的硫酸亚铁铵，加入到其重量60倍的去离子水中，搅拌均匀，加入3重量份的均苯四酸二酐，在47℃下保温搅拌10分钟，加入12重量份的碳纳米管，磁力搅拌3分钟，得羧基化碳纳米管溶液；
(2)取10重量份的聚四氢呋喃醚二醇，在70℃下保温搅拌5分钟，加入6重量份的三氧化二锑，继续保温10分钟，加入10重量份的聚乙烯吡咯烷酮，升高温度为85℃，加入1重量份的氟化钠，保温反应4分钟，得阻燃分散液；
(3)取0.6重量份的乙酰丙酮锌，加入到其重量10倍的无水乙醇中，搅拌均匀，加入2重量份的十二氟庚基丙基三甲氧基硅烷，在60℃下保温搅拌4分钟，得氟化硅烷醇分散液；
(4)取上述阻燃分散液、氟化硅烷醇分散液混合，搅拌均匀，加入上述羧基化碳纳米管溶液，送入到反应釜中，在86℃下保温搅拌1小时，出料，与2重量份的异氰尿酸三缩水甘油酯混合，搅拌至常温，得氟酯化阻燃分散液；
(5)取氟酯化阻燃分散液、0.8重量份的三乙醇胺混合，超声10分钟，抽滤，将沉淀水洗，常温干燥2小时，得氟酯化阻燃填料；
(6)取130重量份的聚丙二醇ppg2000，在108℃下真空脱水2小时，降低温度至55℃，保温备用，得预处理聚丙二醇ppg2000；
(7)取上述氟酯化阻燃填料、与100重量份的2,4-甲苯二异氰酸酯混合，在55℃下保温搅拌20分钟，加入上述预处理聚丙二醇ppg2000，送入到反应釜中，通入氮气，加入3重量份的氯化亚锡，升高温度为76℃，保温反应4-6小时，冷却出料，得磷化聚氨酯预聚体；
(8)取上述磷化聚氨酯预聚体，与10重量份的三羟甲基丙烷混合，在80℃下固化10小时，冷却至常温，磨成细粉，过筛，得所述疏水阻燃聚氨酯粉末涂料。
性能测试：
可以得到本发明具有更好的阻燃防火性能；本发明的涂料形成的涂膜具有更高的表面疏水性能。
Claims (3)
1.一种疏水阻燃聚氨酯粉末涂料的制备方法，其特征在于，包括以下步骤：
(1)取1-2重量份的硫酸亚铁铵，加入到其重量60-70倍的去离子水中，搅拌均匀，加入3-5重量份的均苯四酸二酐，在47-50℃下保温搅拌10-15分钟，加入12-16重量份的碳纳米管，磁力搅拌3-10分钟，得羧基化碳纳米管溶液；
(2)取10-14重量份的聚四氢呋喃醚二醇，在70-75℃下保温搅拌5-10分钟，加入6-8重量份的无机阻燃剂，继续保温10-20分钟，加入10-14重量份的聚乙烯吡咯烷酮，升高温度为85-90℃，加入1-2重量份的氟化钠，保温反应4-6分钟，得阻燃分散液；
(3)取0.6-1重量份的乙酰丙酮锌，加入到其重量10-13倍的无水乙醇中，搅拌均匀，加入2-3重量份的十二氟庚基丙基三甲氧基硅烷，在60-65℃下保温搅拌4-10分钟，得氟化硅烷醇分散液；
(4)取上述阻燃分散液、氟化硅烷醇分散液混合，搅拌均匀，加入上述羧基化碳纳米管溶液，送入到反应釜中，在86-90℃下保温搅拌1-2小时，出料，与2-3重量份的异氰尿酸三缩水甘油酯混合，搅拌至常温，得氟酯化阻燃分散液；
(5)取氟酯化阻燃分散液、0.8-1重量份的三乙醇胺混合，超声10-15分钟，抽滤，将沉淀水洗，常温干燥2-3小时，得氟酯化阻燃填料；
(6)取130-150重量份的聚丙二醇ppg2000，在108-110℃下真空脱水2-3小时，降低温度至55-60℃，保温备用，得预处理聚丙二醇ppg2000；
(7)取上述氟酯化阻燃填料、与100-110重量份的2,4-甲苯二异氰酸酯混合，在55-60℃下保温搅拌20-30分钟，加入上述预处理聚丙二醇ppg2000，送入到反应釜中，通入氮气，加入3-5重量份的氯化亚锡，升高温度为76-85℃，保温反应4-6小时，冷却出料，得磷化聚氨酯预聚体；
(8)取上述磷化聚氨酯预聚体，与10-15重量份的固化剂混合，在80-90℃下固化10-13小时，冷却至常温，磨成细粉，过筛，得所述疏水阻燃聚氨酯粉末涂料。
2.根据权利要求1所述的疏水阻燃聚氨酯粉末涂料的制备方法，其特征在于，所述的无机阻燃剂为三氧化二锑、滑石粉中的一种或两种的混合物，当为两种的混合物时，三氧化二锑、滑石粉的重量比为10-14:1-2。
3.根据权利要求1所述的疏水阻燃聚氨酯粉末涂料的制备方法，其特征在于，所述的固化剂为三羟甲基丙烷。
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| CN104449323A (zh) * | 2014-11-23 | 2015-03-25 | 段宝荣 | 碳纳米管改性的导电阻燃性聚氨酯涂料与胶黏剂制备方法 |
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| CN104449323A (zh) * | 2014-11-23 | 2015-03-25 | 段宝荣 | 碳纳米管改性的导电阻燃性聚氨酯涂料与胶黏剂制备方法 |
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