CN106632879A - 一种分散体树脂的制备方法 - Google Patents

一种分散体树脂的制备方法 Download PDF

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CN106632879A
CN106632879A CN201611170978.8A CN201611170978A CN106632879A CN 106632879 A CN106632879 A CN 106632879A CN 201611170978 A CN201611170978 A CN 201611170978A CN 106632879 A CN106632879 A CN 106632879A
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王鹏
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Abstract

本发明涉及一种分散体树脂及其制备方法，属于树脂技术领域。该树脂包括异氟尔酮二异氰酸酯20‑30份、羟甲基丙烯酰胺3‑5份、三羟甲基丙烷三烯丙酯15‑20份、环氧树脂E51 20‑30份、聚醚二元醇20‑30份、甲基吡咯烷酮5‑10份、甲乙酮30‑50份、三乙醇胺3‑5份、甲基丙烯酸乙酯15‑20份、二丁基月桂酸锡3‑5份、过氧化二苯甲酰1‑3份。本发明用环氧树脂和丙烯酸酯两种物质对水性聚氨酯分散体改性，得到性能更加优异的聚氨酯‑环氧树脂‑丙烯酸酯杂化分散体，该分散体综合了聚氨酯、环氧树脂和丙烯酸酯的优点。

Description

一种分散体树脂的制备方法
技术领域
本发明涉及一种树脂及其制备方法，更具体地说，本发明涉及一种分散体树脂及其制备方法，属于树脂技术领域。
背景技术
随着环保法规的日益严格和人们环保意识的逐渐增强，溶剂型聚氨酯由于含有高VOC，对环境不利，其使用越来越受到限制。而以水为分散介质的水性聚氨酯成为环境友好聚氨酯树脂开发研究的重点。然而单一的水性聚氨酯分散体胶膜力学性能不佳，耐化学性和耐水、耐溶剂性不好，硬度较低。为改善水性聚氨酯分散体的涂膜性能、扩大水性聚氨酯分散体应用范围，就必须对水性聚氨酯分散体进行改性。有关水性聚氨酯分散体改性的报道较多，多数仅采用一种组分对其改性，导致其性能还是不能满足多方面的需求。此外，由于环氧树脂具有高模量、高强度和耐化学性好等优点，丙烯酸酯具有较好的耐水性、耐候性。
发明内容
本发明旨在解决现有水性聚氨酯分散体的性能问题，提供一种分散体树脂，该分散体树脂综合了聚氨酯、环氧树脂和丙烯酸酯的优点。
为了实现上述发明目的，其具体的技术方案如下：
一种分散体树脂，其特征在于：包括以下按照重量份数计的原料：
异氟尔酮二异氰酸酯 20-30份
羟甲基丙烯酰胺 3-5份
三羟甲基丙烷三烯丙酯 15-20份
环氧树脂E51 20-30份
聚醚二元醇 20-30份
甲基吡咯烷酮 5-10份
甲乙酮 30-50份
三乙醇胺 3-5份
甲基丙烯酸乙酯 15-20份
二丁基月桂酸锡 3-5份
过氧化二苯甲酰 1-3份。
一种分散体树脂的制备方法，其特征在于：包括以下工艺步骤：
A、将甲基吡咯烷酮、甲基丙烯酸乙酯、二丁基月桂酸锡在120℃，真空减压脱水1.5h,备用；在氮气保护下，在装有搅拌器、温度计、冷凝管的四口瓶中，加入异氟尔酮二异氰酸酯和脱水的聚醚二元醇，开动搅拌，逐渐升温到80℃，保持在此温度下反应；
B、取样测定反应物中-NCO基团的含量，当达到规定值后，加入交联剂三羟甲基丙烷三烯丙酯，保持此温度反应2h；用正丁胺滴定法判断反应终点；达到终点后加入溶有羟甲基丙烯酰胺的溶液和环氧树脂E51，保温反应5h；反应过程中视黏度的大小添加丙酮，使其符合要求；
C、最后将反应体系冷却降温至45℃以下；三乙醇胺中和，在高速剪切下加水乳化得到聚氨酯-环氧树脂杂化分散体。
D、将上述制备的分散体放入四口瓶中，在75℃下保温0.5h；75-80℃下在3h内均匀滴加过氧化二苯甲酰及过氧化二苯甲酰引发剂的丙酮溶液，进行自由基乳液聚2h；
E、滴完后过氧化二苯甲酰引发剂的甲乙酮溶液再于85-90℃保温1.5h；真空脱去反应体系中的甲乙酮及其它挥发份得到分散体树脂。
本发明带来的有益技术效果：
本发明用环氧树脂和丙烯酸酯两种物质对水性聚氨酯分散体改性，得到性能更加优异的聚氨酯-环氧树脂-丙烯酸酯杂化分散体，该分散体综合了聚氨酯、环氧树脂和丙烯酸酯的优点。
具体实施方式
实施例1
一种分散体树脂，其特征在于：包括以下按照重量份数计的原料：
异氟尔酮二异氰酸酯 20份
羟甲基丙烯酰胺 3份
三羟甲基丙烷三烯丙酯 15份
环氧树脂E51 20份
聚醚二元醇 20份
甲基吡咯烷酮 5份
甲乙酮 30份
三乙醇胺 3份
甲基丙烯酸乙酯 15份
二丁基月桂酸锡 3份
过氧化二苯甲酰 1份。
实施例2
一种分散体树脂，其特征在于：包括以下按照重量份数计的原料：
异氟尔酮二异氰酸酯 30份
羟甲基丙烯酰胺 5份
三羟甲基丙烷三烯丙酯 20份
环氧树脂E51 30份
聚醚二元醇 30份
甲基吡咯烷酮 10份
甲乙酮 50份
三乙醇胺 5份
甲基丙烯酸乙酯 20份
二丁基月桂酸锡 5份
过氧化二苯甲酰 3份。
实施例3
一种分散体树脂，其特征在于：包括以下按照重量份数计的原料：
异氟尔酮二异氰酸酯 25份
羟甲基丙烯酰胺 4份
三羟甲基丙烷三烯丙酯 18份
环氧树脂E51 25份
聚醚二元醇 25份
甲基吡咯烷酮 7份
甲乙酮 40份
三乙醇胺 4份
甲基丙烯酸乙酯 18份
二丁基月桂酸锡 4份
过氧化二苯甲酰 2份。
实施例4
一种分散体树脂的制备方法，包括以下工艺步骤：
A、将甲基吡咯烷酮、甲基丙烯酸乙酯、二丁基月桂酸锡在120℃，真空减压脱水1.5h,备用；在氮气保护下，在装有搅拌器、温度计、冷凝管的四口瓶中，加入异氟尔酮二异氰酸酯和脱水的聚醚二元醇，开动搅拌，逐渐升温到80℃，保持在此温度下反应；
B、取样测定反应物中-NCO基团的含量，当达到规定值后，加入交联剂三羟甲基丙烷三烯丙酯，保持此温度反应2h；用正丁胺滴定法判断反应终点；达到终点后加入溶有羟甲基丙烯酰胺的溶液和环氧树脂E51，保温反应5h；反应过程中视黏度的大小添加丙酮，使其符合要求；
C、最后将反应体系冷却降温至45℃以下；三乙醇胺中和，在高速剪切下加水乳化得到聚氨酯-环氧树脂杂化分散体。
D、将上述制备的分散体放入四口瓶中，在75℃下保温0.5h；75℃下在3h内均匀滴加过氧化二苯甲酰及过氧化二苯甲酰引发剂的丙酮溶液，进行自由基乳液聚2h；
E、滴完后过氧化二苯甲酰引发剂的甲乙酮溶液再于85℃保温1.5h；真空脱去反应体系中的甲乙酮及其它挥发份得到分散体树脂。
实施例5
一种分散体树脂的制备方法，包括以下工艺步骤：
A、将甲基吡咯烷酮、甲基丙烯酸乙酯、二丁基月桂酸锡在120℃，真空减压脱水1.5h,备用；在氮气保护下，在装有搅拌器、温度计、冷凝管的四口瓶中，加入异氟尔酮二异氰酸酯和脱水的聚醚二元醇，开动搅拌，逐渐升温到80℃，保持在此温度下反应；
B、取样测定反应物中-NCO基团的含量，当达到规定值后，加入交联剂三羟甲基丙烷三烯丙酯，保持此温度反应2h；用正丁胺滴定法判断反应终点；达到终点后加入溶有羟甲基丙烯酰胺的溶液和环氧树脂E51，保温反应5h；反应过程中视黏度的大小添加丙酮，使其符合要求；
C、最后将反应体系冷却降温至45℃以下；三乙醇胺中和，在高速剪切下加水乳化得到聚氨酯-环氧树脂杂化分散体。
D、将上述制备的分散体放入四口瓶中，在75℃下保温0.5h；80℃下在3h内均匀滴加过氧化二苯甲酰及过氧化二苯甲酰引发剂的丙酮溶液，进行自由基乳液聚2h；
E、滴完后过氧化二苯甲酰引发剂的甲乙酮溶液再于90℃保温1.5h；真空脱去反应体系中的甲乙酮及其它挥发份得到分散体树脂。
实施例6
一种分散体树脂的制备方法，包括以下工艺步骤：
A、将甲基吡咯烷酮、甲基丙烯酸乙酯、二丁基月桂酸锡在120℃，真空减压脱水1.5h,备用；在氮气保护下，在装有搅拌器、温度计、冷凝管的四口瓶中，加入异氟尔酮二异氰酸酯和脱水的聚醚二元醇，开动搅拌，逐渐升温到80℃，保持在此温度下反应；
B、取样测定反应物中-NCO基团的含量，当达到规定值后，加入交联剂三羟甲基丙烷三烯丙酯，保持此温度反应2h；用正丁胺滴定法判断反应终点；达到终点后加入溶有羟甲基丙烯酰胺的溶液和环氧树脂E51，保温反应5h；反应过程中视黏度的大小添加丙酮，使其符合要求；
C、最后将反应体系冷却降温至45℃以下；三乙醇胺中和，在高速剪切下加水乳化得到聚氨酯-环氧树脂杂化分散体。
D、将上述制备的分散体放入四口瓶中，在75℃下保温0.5h；78℃下在3h内均匀滴加过氧化二苯甲酰及过氧化二苯甲酰引发剂的丙酮溶液，进行自由基乳液聚2h；
E、滴完后过氧化二苯甲酰引发剂的甲乙酮溶液再于88℃保温1.5h；真空脱去反应体系中的甲乙酮及其它挥发份得到分散体树脂。

Claims (2)

1.一种分散体树脂，其特征在于：包括以下按照重量份数计的原料：
异氟尔酮二异氰酸酯 20-30份
羟甲基丙烯酰胺 3-5份
三羟甲基丙烷三烯丙酯 15-20份
环氧树脂E51 20-30份
聚醚二元醇 20-30份
甲基吡咯烷酮 5-10份
甲乙酮 30-50份
三乙醇胺 3-5份
甲基丙烯酸乙酯 15-20份
二丁基月桂酸锡 3-5份
过氧化二苯甲酰 1-3份。
2.根据权利要求1所述的一种分散体树脂的制备方法，其特征在于：包括以下工艺步骤：
A、将甲基吡咯烷酮、甲基丙烯酸乙酯、二丁基月桂酸锡在120℃，真空减压脱水1.5h,备用；在氮气保护下，在装有搅拌器、温度计、冷凝管的四口瓶中，加入异氟尔酮二异氰酸酯和脱水的聚醚二元醇，开动搅拌，逐渐升温到80℃，保持在此温度下反应；
B、取样测定反应物中-NCO基团的含量，当达到规定值后，加入交联剂三羟甲基丙烷三烯丙酯，保持此温度反应2h；用正丁胺滴定法判断反应终点；达到终点后加入溶有羟甲基丙烯酰胺的溶液和环氧树脂E51，保温反应5h；反应过程中视黏度的大小添加丙酮，使其符合要求；
C、最后将反应体系冷却降温至45℃以下；三乙醇胺中和，在高速剪切下加水乳化得到聚氨酯-环氧树脂杂化分散体；
D、将上述制备的分散体放入四口瓶中，在75℃下保温0.5h；75-80℃下在3h内均匀滴加过氧化二苯甲酰及过氧化二苯甲酰引发剂的丙酮溶液，进行自由基乳液聚2h；
E、滴完后过氧化二苯甲酰引发剂的甲乙酮溶液再于85-90℃保温1.5h；真空脱去反应体系中的甲乙酮及其它挥发份得到分散体树脂。
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