CN105949431A - 一种塑胶漆用聚氨酯固化剂的制备方法 - Google Patents

一种塑胶漆用聚氨酯固化剂的制备方法 Download PDF

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CN105949431A
CN105949431A CN201610411269.8A CN201610411269A CN105949431A CN 105949431 A CN105949431 A CN 105949431A CN 201610411269 A CN201610411269 A CN 201610411269A CN 105949431 A CN105949431 A CN 105949431A
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陆国灵
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Abstract

本发明公开了一种塑胶漆用聚氨酯固化剂的制备方法,涉及固化剂制备技术领域,包括如下步骤:(1)聚氨酯合成,(2)后处理,(3)固化剂制备。本发明在聚氨酯合成阶段通过分批加料的方式,提高反应程度和原料利用率,所得聚氨酯再在助剂的协同作用下制得塑胶漆用固化剂,该固化剂的加入能缩短塑胶漆的固化时间,加快漆膜的形成和干燥,并且可有效提高漆膜的力学性能以及耐水性、耐腐蚀性和耐候性等。

Description

一种塑胶漆用聚氨酯固化剂的制备方法
技术领域:
本发明涉及固化剂制备技术领域,具体涉及一种塑胶漆用聚氨酯固化剂的制备方法。
背景技术:
塑胶漆系以树脂为基体,辅以高档适用助剂及颜料调配而成的标准型塑料油漆。该漆具有硬度高、光泽高、高分丰满度、层间附着力好、易施工等特点,广泛用于塑料底材的产品涂装,如塑料玩具、塑料日用品、电器产品、塑料工艺品等。聚氨酯固化剂是由二异氰酸酯与含有活泼氢的化合物加成反应生成的一种聚氨酯预聚物,目前常用固化剂为三羟甲基丙烷与甲苯二异氰酸酯的加成物,它在国内外聚氨酯固化剂中所占比例非常大,但三羟甲基丙烷与甲苯二异氰酸酯价格较高,且存在大量游离甲苯二异氰酸酯,固化量低,环保性差等问题。
发明内容:
本发明所要解决的技术问题在于提供一种原料利用率高、节省成本且固化效果好的塑胶漆用聚氨酯固化剂的制备方法。
本发明所要解决的技术问题采用以下的技术方案来实现:
一种塑胶漆用聚氨酯固化剂的制备方法,包括如下步骤:
(1)聚氨酯合成:将甲基丙烯酸羟乙酯、氟化钾和水混合形成底物,端氨基聚醚230、纳米氧化铝和乙醇混合形成滴加物,滴加物平均分成三批加入,先向底物中加入第一批滴加物,滴完后室温反应1h,再加入第二批滴加物,滴完后加热至回流状态保温反应2h,然后加入第三批滴加物,滴完后继续保温反应2h,即得反应液;
(2)后处理:向所得反应液中加入1/2体积二甲苯,搅拌1h,再静置1h,分层,取上层有机相,即得聚氨酯溶液;
(3)固化剂制备:将上述所得聚氨酯溶液与助剂按照重量比1:0.1混合,混合物先于超声频率40kHz、功率100W下超声处理30min,再于微波频率2450MHz、功率700W下微波处理10min,待处理物自然冷却至室温,然后于0-5℃下静置过夜,最后利用球磨机球磨至细度小于10μm即可;
所述助剂由如下重量份数的原料制成:氯磺化聚乙烯10-15份、橡胶粉7-10份、活性白土5-8份、氢化松香5-8份、石油焦4-6份、米糠蜡4-6份、纳米胶粉3-5份、三氯叔丁醇2-3份、硫脲2-3份、骨炭粉1-2份、纳米铝粉1-2份、玄明粉1-2份、亚硒酸钠0.5-1份、乙二胺二琥珀酸三钠0.5-1份,其制备方法为:先将氯磺化聚乙烯、氢化松香和石油焦充分混合,于微波频率2450MHz、功率700W下微波处理5min,再加入橡胶粉、米糠蜡和纳米胶粉,继续微波处理10min,待处理物自然冷却至80-90℃后加入活性白土、三氯叔丁醇、骨炭粉和纳米铝粉,充分混合后密封静置3h,最后加入硫脲、玄明粉、亚硒酸钠和乙二胺二琥珀酸三钠,充分研磨使其混合均匀。
所述甲基丙烯酸羟乙酯、端氨基聚醚230、氟化钾和纳米氧化铝的投料摩尔比为2.2:1:0.03:0.01。
本发明的有益效果是:本发明在聚氨酯合成阶段通过分批加料的方式,提高反应程度和原料利用率,所得聚氨酯再在助剂的协同作用下制得塑胶漆用固化剂,该固化剂的加入能缩短塑胶漆的固化时间,加快漆膜的形成和干燥,并且可有效提高漆膜的力学性能以及耐水性、耐腐蚀性和耐候性等。
具体实施方式:
为了使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解,下面结合具体实施例,进一步阐述本发明。
实施例1
(1)聚氨酯合成:将甲基丙烯酸羟乙酯、氟化钾和水混合形成底物,端氨基聚醚230、纳米氧化铝和乙醇混合形成滴加物,滴加物平均分成三批加入,先向底物中加入第一批滴加物,滴完后室温反应1h,再加入第二批滴加物,滴完后加热至回流状态保温反应2h,然后加入第三批滴加物,滴完后继续保温反应2h,即得反应液,甲基丙烯酸羟乙酯、端氨基聚醚230、氟化钾和纳米氧化铝的投料摩尔比为2.2:1:0.03:0.01;
(2)后处理:向所得反应液中加入1/2体积二甲苯,搅拌1h,再静置1h,分层,取上层有机相,即得聚氨酯溶液;
(3)固化剂制备:将上述所得聚氨酯溶液与助剂按照重量比1:0.1混合,混合物先于超声频率40kHz、功率100W下超声处理30min,再于微波频率2450MHz、功率700W下微波处理10min,待处理物自然冷却至室温,然后于0-5℃下静置过夜,最后利用球磨机球磨至细度小于10μm即可;
助剂的制备:先将10份氯磺化聚乙烯、6份氢化松香和4份石油焦充分混合,于微波频率2450MHz、功率700W下微波处理5min,再加入8份橡胶粉、4份米糠蜡和3份纳米胶粉,继续微波处理10min,待处理物自然冷却至80-90℃后加入5份活性白土、2份三氯叔丁醇、1份骨炭粉和2份纳米铝粉,充分混合后密封静置3h,最后加入2份硫脲、1份玄明粉、0.5份亚硒酸钠和0.5份乙二胺二琥珀酸三钠,充分研磨使其混合均匀。
实施例2
(1)聚氨酯合成:将甲基丙烯酸羟乙酯、氟化钾和水混合形成底物,端氨基聚醚230、纳米氧化铝和乙醇混合形成滴加物,滴加物平均分成三批加入,先向底物中加入第一批滴加物,滴完后室温反应1h,再加入第二批滴加物,滴完后加热至回流状态保温反应2h,然后加入第三批滴加物,滴完后继续保温反应2h,即得反应液,甲基丙烯酸羟乙酯、端氨基聚醚230、氟化钾和纳米氧化铝的投料摩尔比为2.2:1:0.03:0.01;
(2)后处理:向所得反应液中加入1/2体积二甲苯,搅拌1h,再静置1h,分层,取上层有机相,即得聚氨酯溶液;
(3)固化剂制备:将上述所得聚氨酯溶液与助剂按照重量比1:0.1混合,混合物先于超声频率40kHz、功率100W下超声处理30min,再于微波频率2450MHz、功率700W下微波处理10min,待处理物自然冷却至室温,然后于0-5℃下静置过夜,最后利用球磨机球磨至细度小于10μm即可;
助剂的制备:先将15份氯磺化聚乙烯、6份氢化松香和4份石油焦充分混合,于微波频率2450MHz、功率700W下微波处理5min,再加入8份橡胶粉、5份米糠蜡和3份纳米胶粉,继续微波处理10min,待处理物自然冷却至80-90℃后加入8份活性白土、2份三氯叔丁醇、1份骨炭粉和1份纳米铝粉,充分混合后密封静置3h,最后加入2份硫脲、1份玄明粉、0.5份亚硒酸钠和0.5份乙二胺二琥珀酸三钠,充分研磨使其混合均匀。
以上显示和描述了本发明的基本原理和主要特征和本发明的优点。本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。

Claims (2)

1.一种塑胶漆用聚氨酯固化剂的制备方法,其特征在于,包括如下步骤:
(1)聚氨酯合成:将甲基丙烯酸羟乙酯、氟化钾和水混合形成底物,端氨基聚醚230、纳米氧化铝和乙醇混合形成滴加物,滴加物平均分成三批加入,先向底物中加入第一批滴加物,滴完后室温反应1h,再加入第二批滴加物,滴完后加热至回流状态保温反应2h,然后加入第三批滴加物,滴完后继续保温反应2h,即得反应液;
(2)后处理:向所得反应液中加入1/2体积二甲苯,搅拌1h,再静置1h,分层,取上层有机相,即得聚氨酯溶液;
(3)固化剂制备:将上述所得聚氨酯溶液与助剂按照重量比1:0.1混合,混合物先于超声频率40kHz、功率100W下超声处理30min,再于微波频率2450MHz、功率700W下微波处理10min,待处理物自然冷却至室温,然后于0-5℃下静置过夜,最后利用球磨机球磨至细度小于10μm即可;
所述助剂由如下重量份数的原料制成:氯磺化聚乙烯10-15份、橡胶粉7-10份、活性白土5-8份、氢化松香5-8份、石油焦4-6份、米糠蜡4-6份、纳米胶粉3-5份、三氯叔丁醇2-3份、硫脲2-3份、骨炭粉1-2份、纳米铝粉1-2份、玄明粉1-2份、亚硒酸钠0.5-1份、乙二胺二琥珀酸三钠0.5-1份,其制备方法为:先将氯磺化聚乙烯、氢化松香和石油焦充分混合,于微波频率2450MHz、功率700W下微波处理5min,再加入橡胶粉、米糠蜡和纳米胶粉,继续微波处理10min,待处理物自然冷却至80-90℃后加入活性白土、三氯叔丁醇、骨炭粉和纳米铝粉,充分混合后密封静置3h,最后加入硫脲、玄明粉、亚硒酸钠和乙二胺二琥珀酸三钠,充分研磨使其混合均匀。
2.根据权利要求1所述的塑胶漆用聚氨酯固化剂的制备方法,其特征在于:所述甲基丙烯酸羟乙酯、端氨基聚醚230、氟化钾和纳米氧化铝的投料摩尔比为2.2:1:0.03:0.01。
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