CN107163228A - 一种环保型水性环氧树脂固化剂及其制备方法 - Google Patents

一种环保型水性环氧树脂固化剂及其制备方法 Download PDF

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CN107163228A
CN107163228A CN201710490305.9A CN201710490305A CN107163228A CN 107163228 A CN107163228 A CN 107163228A CN 201710490305 A CN201710490305 A CN 201710490305A CN 107163228 A CN107163228 A CN 107163228A
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parts
curing agent
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aqueous epoxy
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邱静
阙守燕
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Sichuan Happy Trading Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/50Amines
    • C08G59/56Amines together with other curing agents
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/62Alcohols or phenols

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  • Chemical Kinetics & Catalysis (AREA)
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  • Polymers & Plastics (AREA)
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Abstract

本发明涉及一种环保型水性环氧树脂固化剂及其制备方法,属于环氧树脂技术领域。包括:羟基封端聚醚220 20份、环氧树脂E‑42 20份、OP‑10乳化剂5份、聚甲基丙烯酸二甲胺乙酯10份、固化剂590# 5份、去离子水100份。本发明采用在固化剂中引入羟基封端聚醚链段以增加树脂的水溶性,同时,以水溶性较强的聚甲基丙烯酸二甲胺乙酯作为固化剂之一,制备了水溶性环氧树脂。克服了传统环氧树脂对环境不利的缺陷。

Description

一种环保型水性环氧树脂固化剂及其制备方法
技术领域
本发明涉及一种环氧树脂固化剂及其制备方法,更具体地说,本发明涉及一种环保型水性环氧树脂固化剂及其制备方法,属于环氧树脂技术领域。
背景技术
环氧涂料性能优良,在防腐、工业地坪、建筑等领域得到了广泛的应用。但目前使用的环氧涂料主要为溶剂型涂料,近年来,随着人们环保意识的不断提高,许多国家相继颁布了限制挥发性有机溶剂(VOC)的环保法规,涂料的水性化、无溶剂化和高固体分化已成为涂料发展的必然趋势(赵新刚,“耐热型ABS共聚物的研制”,化工新型材料,2004,32(5):33-35.)。水性环氧树脂体系已经成为树脂行业研究的重点,作为水性环氧树脂体系的必要组分——水性环氧固化剂的研究开发也日趋重要。固化剂是影响双组分环氧涂料性能的关键因素之一,目前实际使用的水性环氧固化剂大多为它们的改性产物,包括酰胺化多胺(Gaofenzi Cailiao Kexue Yu Gongcheng/Polymeric Materials Science an dEngineering, 2000,16(3):160)、聚酰胺(Jim D Elmore,Derek S Kincaid,Pratap CKomar.Water-borne epoxy protective coatings for metal lJ].Journal of CoatingsTechnology,2002,74(931):63-69.)和环氧一多胺加成物(陈铤,施雪珍,顾国芳.“双组分水性环氧树脂涂料”,高分子通报,2003(12):63-70)。由于酰胺类固化剂固化后涂膜的耐水性和耐化学药品性较差,现在研究的水性环氧固化剂主要是封端的环氧一多胺类加成物J。普通的水性环氧树脂涂料的涂膜的硬度较高,但柔韧性和抗冲击性均较差。
发明内容
本发明旨在解决现有技术中的环氧树脂固化剂不够环保的问题,提供一种环保型水性环氧树脂固化剂,该环氧树脂固化剂环保无污染,且性能较佳。
为了实现上述发明目的,其具体的技术方案如下:
一种环保型水性环氧树脂固化剂,其特征在于:包括以下按照重量份数计的原料:
羟基封端聚醚220 20份
环氧树脂E-42 20份
OP-10乳化剂 5份
聚甲基丙烯酸二甲胺乙酯 10份
固化剂590# 5份
去离子水 100份。
制备工艺:
一种环保型水性环氧树脂固化剂的制备方法,其特征在于:包括以下工艺步骤:
A、将羟基封端聚醚与乳化剂、去离子水按一定比例加入具搅拌、冷凝管及加料口的三口瓶中,开动搅拌混合均匀;
B、将反应体系温度升至40℃,开动搅拌使物料进一步混合均匀;
C、将预先溶于异丙醇的环氧树脂催化剂置于恒压滴液漏斗中,缓慢滴加至三口瓶内;
D、于温度40-60℃间维持搅拌时间4h;
E、减压蒸馏脱溶剂,出料即得水性环氧树脂甲组分,备用;
F、按配方要求称取聚甲基丙烯酸二甲胺乙酯、固化剂590#、乳化剂及部分去离子水等组分,置于另一具搅拌、冷凝管及加料口的三口瓶中,开动搅拌混合均匀;
G、将温度升至60-70℃,搅拌2h;
H、将反应温度升至80-85℃,搅拌2h,得乙组分固化剂;
I、按照甲组分:乙组分为6:2的比例混合,90℃固化2h,120℃固化2h,140℃固化2h,180℃固化2h即可。
本发明带来的有益技术效果:
本发明采用在固化剂中引入羟基封端聚醚链段以增加树脂的水溶性,同时,以水溶性较强的聚甲基丙烯酸二甲胺乙酯作为固化剂之一,制备了水溶性环氧树脂。克服了传统环氧树脂对环境不利的缺陷。
具体实施方式
实施例1
一种环保型水性环氧树脂固化剂,包括以下按照重量份数计的原料:
羟基封端聚醚220 20份
环氧树脂E-42 20份
OP-10乳化剂 5份
聚甲基丙烯酸二甲胺乙酯 10份
固化剂590# 5份
去离子水 100份。
实施例2
在实施例1的基础上:
A、将羟基封端聚醚与乳化剂、去离子水按一定比例加入具搅拌、冷凝管及加料口的三口瓶中,开动搅拌混合均匀;
B、将反应体系温度升至40℃,开动搅拌使物料进一步混合均匀;
C、将预先溶于异丙醇的环氧树脂催化剂置于恒压滴液漏斗中,缓慢滴加至三口瓶内;
D、于温度40℃间维持搅拌时间4h;
E、减压蒸馏脱溶剂,出料即得水性环氧树脂甲组分,备用
F、按配方要求称取聚甲基丙烯酸二甲胺乙酯、固化剂590#、乳化剂及部分去离子水等组分,置于另一具搅拌、冷凝管及加料口的三口瓶中,开动搅拌混合均匀;
G、将温度升至60℃,搅拌2h;
H、将反应温度升至80℃,搅拌2h,得乙组分固化剂;
I、按照甲组分:乙组分为6:2的比例混合,90℃固化2h,120℃固化2h,140℃固化2h,180℃固化2h即可。
实施例3
在实施例1的基础上:
A、将羟基封端聚醚与乳化剂、去离子水按一定比例加入具搅拌、冷凝管及加料口的三口瓶中,开动搅拌混合均匀;
B、将反应体系温度升至40℃,开动搅拌使物料进一步混合均匀;
C、将预先溶于异丙醇的环氧树脂催化剂置于恒压滴液漏斗中,缓慢滴加至三口瓶内;
D、于温度60℃间维持搅拌时间4h;
E、减压蒸馏脱溶剂,出料即得水性环氧树脂甲组分,备用;
F、按配方要求称取聚甲基丙烯酸二甲胺乙酯、固化剂590#、乳化剂及部分去离子水等组分,置于另一具搅拌、冷凝管及加料口的三口瓶中,开动搅拌混合均匀;
G、将温度升至70℃,搅拌2h;
H、将反应温度升至85℃,搅拌2h,得乙组分固化剂;
I、按照甲组分:乙组分为6:2的比例混合,90℃固化2h,120℃固化2h,140℃固化2h,180℃固化2h即可。
实施例4
在实施例1的基础上:
A、将羟基封端聚醚与乳化剂、去离子水按一定比例加入具搅拌、冷凝管及加料口的三口瓶中,开动搅拌混合均匀;
B、将反应体系温度升至40℃,开动搅拌使物料进一步混合均匀;
C、将预先溶于异丙醇的环氧树脂催化剂置于恒压滴液漏斗中,缓慢滴加至三口瓶内;
D、于温度50℃间维持搅拌时间4h;
E、减压蒸馏脱溶剂,出料即得水性环氧树脂甲组分,备用;
F、按配方要求称取聚甲基丙烯酸二甲胺乙酯、固化剂590#、乳化剂及部分去离子水等组分,置于另一具搅拌、冷凝管及加料口的三口瓶中,开动搅拌混合均匀;
G、将温度升至65℃,搅拌2h;
H、将反应温度升至82℃,搅拌2h,得乙组分固化剂;
I、按照甲组分:乙组分为6:2的比例混合,90℃固化2h,120℃固化2h,140℃固化2h,180℃固化2h即可。
实施例5
在实施例1的基础上:
A、将羟基封端聚醚与乳化剂、去离子水按一定比例加入具搅拌、冷凝管及加料口的三口瓶中,开动搅拌混合均匀;
B、将反应体系温度升至40℃,开动搅拌使物料进一步混合均匀;
C、将预先溶于异丙醇的环氧树脂催化剂置于恒压滴液漏斗中,缓慢滴加至三口瓶内;
D、于温度42℃间维持搅拌时间4h;
E、减压蒸馏脱溶剂,出料即得水性环氧树脂甲组分,备用;
F、按配方要求称取聚甲基丙烯酸二甲胺乙酯、固化剂590#、乳化剂及部分去离子水等组分,置于另一具搅拌、冷凝管及加料口的三口瓶中,开动搅拌混合均匀;
G、将温度升至68℃,搅拌2h;
H、将反应温度升至81℃,搅拌2h,得乙组分固化剂;
I、按照甲组分:乙组分为6:2的比例混合,90℃固化2h,120℃固化2h,140℃固化2h,180℃固化2h即可。

Claims (2)

1.一种环保型水性环氧树脂固化剂,其特征在于:包括以下按照重量份数计的原料:
羟基封端聚醚220 20份
环氧树脂E-42 20份
OP-10乳化剂 5份
聚甲基丙烯酸二甲胺乙酯 10份
固化剂590# 5份
去离子水 100份。
2.根据权利要求1所述的一种环保型水性环氧树脂固化剂的制备方法,其特征在于:包括以下工艺步骤:
A、将羟基封端聚醚与乳化剂、去离子水按一定比例加入具搅拌、冷凝管及加料口的三口瓶中,开动搅拌混合均匀;
B、将反应体系温度升至40℃,开动搅拌使物料进一步混合均匀;
C、将预先溶于异丙醇的环氧树脂催化剂置于恒压滴液漏斗中,缓慢滴加至三口瓶内;
D、于温度40-60℃间维持搅拌时间4h;
E、减压蒸馏脱溶剂,出料即得水性环氧树脂甲组分,备用;
F、按配方要求称取聚甲基丙烯酸二甲胺乙酯、固化剂590#、乳化剂及部分去离子水等组分,置于另一具搅拌、冷凝管及加料口的三口瓶中,开动搅拌混合均匀;
G、将温度升至60-70℃,搅拌2h;
H、将反应温度升至80-85℃,搅拌2h,得乙组分固化剂;
I、按照甲组分:乙组分为6:2的比例混合,90℃固化2h,120℃固化2h,140℃固化2h,180℃固化2h即可。
CN201710490305.9A 2017-06-25 2017-06-25 一种环保型水性环氧树脂固化剂及其制备方法 Pending CN107163228A (zh)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104962176A (zh) * 2015-08-03 2015-10-07 何肖凤 一种水性环氧树脂涂料及其制备方法
CN105885628A (zh) * 2016-05-18 2016-08-24 湖北佳记合成材料股份有限公司 一种高性能水性环氧树脂汽车涂料及其制备方法
CN106366722A (zh) * 2016-10-17 2017-02-01 张莘蔓 一种新型环保太阳能贮水箱用防腐涂料

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104962176A (zh) * 2015-08-03 2015-10-07 何肖凤 一种水性环氧树脂涂料及其制备方法
CN105885628A (zh) * 2016-05-18 2016-08-24 湖北佳记合成材料股份有限公司 一种高性能水性环氧树脂汽车涂料及其制备方法
CN106366722A (zh) * 2016-10-17 2017-02-01 张莘蔓 一种新型环保太阳能贮水箱用防腐涂料

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Application publication date: 20170915