CN112759742A - 一种增韧型水性环氧树脂及其制备方法 - Google Patents
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Abstract
本发明提供的一种增韧型水性环氧树脂,其结构式如式I或式II所示。本发明还提供了上述增韧型水性环氧树脂的制备方法。本发明提供的水性环氧树脂制备工艺简单、成本较低,该树脂通过引入萘羟基、苯羟基与环氧丙醇形成高刚性的主链,从而大大增强了该树脂的韧性,主链上同时引入羟基和双键,使该环氧树脂具有一定的扩展性,能参与其他反应形成具有一定功能的环氧树脂。
Description
技术领域
本发明涉及涂料材料领域,特别涉及一种增韧型水性环氧树脂及其制备方法与应用。
背景技术
含有两个或两个以上的环氧基团的树脂称为环氧树脂,环氧基团的活泼性很高,能与很多固化剂反应形成三维交联网络结构。环氧树脂发展到今天已经走过了六十多年,产量不断增加,新品种的不断增多,环氧树脂在汽车工业、船舶及重防腐涂料、建筑业、胶粘剂以及食品、航空航天等领域都有大量应用。
环氧树脂具有大量的活性和极性基团:环氧基、醚键、轻基等,因此具有较多优良的性能和反应活性。不同种类的环氧树脂可与相应的固化剂进行交联固化,生成三维立体网状结构,通过添加各种促进剂、改性剂等以满足生产生活的各种性能要求。环氧树脂具有良好的耐热及耐化学药品性能,固化时收缩率非常小,所形成的固化物粘结性能极好,除此之外其机械和电器性能也非常优异;其缺点也非常明显,耐候性比较差,韧性也不强,施工环境极端时容易开裂、剥落。
按化学结构环氧树脂有缩水甘油醚类、脂环族类和环氧化烯烃类等几大类型,其中双酚A型环氧树脂属于缩水甘油醚类,是使用最多的环氧树脂品种。双酚A型环氧树脂的环氧基可以提高其反应活性,亚甲基链段可给予其柔韧性,醚键赋予了其耐化学药品性能,羟基提供了其粘结性,而其骨架则增强了树脂的强韧性和耐热性为拓宽环氧树脂的应用领域,克服其缺陷,国内外的研究内容主要集中在对环氧树脂进行改性以提高其水溶性,降低VOC含量以达到环保要求,其中水性环氧树脂就是一个主要的研究方向。
随着科学技术的不断进步,环氧树脂的应用领域不断被扩大,很多场合都对环氧树脂的性能提出了更加苛刻的要求。为了满足市场的需求,就必须对环氧树脂进行改性。
环氧树脂其固化物内应力大、质脆、耐冲击性和耐湿性差等。环氧树脂粘结强度较大,交联固化密度高,硬度大,柔初性差,耐热性和耐冲击损伤性差等缺点,在很大程度上限制了其应用范围通常通过化学改性引入其他基团改善性能,或者添加理想固化剂等改善环氧树脂的性能。目前增韧改性通用型环氧树脂是环氧树脂研究的热点问题之一。
发明内容
技术问题:为了解决现有技术的缺陷,本发明提供了一种增韧型水性环氧树脂及其制备方法与应用。
技术方案:本发明提供的一种增韧型水性环氧树脂,其结构式如式I或式II所示:
本发明还提供了上述增韧型水性环氧树脂的制备方法,包括以下步骤:
(1)在氢氧化钠存在下,式III所示的化合物与过量的环氧丙醇聚合反应,得式II所示的化合物;
(2)式I所示的化合物与甲基丙烯酸、苯乙烯反应,得式II所示得化合物;
反应式如下:
步骤(1)具体为:将式III所示的化合物溶于甲苯中,加入氢氧化钠水溶液,边搅拌边加热,当温度升到60-70℃时恒温搅拌并滴加环氧丙醇,于2小时内滴加完毕;提高温度,于75-85℃保持1-2h;加入蒸馏水,搅拌,静止分层除去水层,甲苯层减压蒸干即得式I所示化合物。
步骤(2)具体为:式I所示的化合物溶解于混合溶剂中,氮气保护下,缓慢滴加甲基丙烯酸、苯乙烯,再加入引发剂,升温至100-110℃,恒温反应1-2h,冷却至40-50℃,调pH至7-8,恒温反应1-2h,即得。
优选地,式III所示的化合物与环氧丙醇的摩尔比为n:(2n+2至2n+4)。
优选地,氢氧化钠水溶液中氢氧化钠的含量为0.5n-1.5n摩尔/L。
优选地,蒸馏水和甲苯的体积比为(2-4):1。
有益效果:本发明提供的水性环氧树脂制备工艺简单、成本较低,该树脂通过引入萘羟基、苯羟基与环氧丙醇形成高刚性的主链,从而大大增强了该树脂的韧性,主链上同时引入羟基和双键,使该环氧树脂具有一定的扩展性,能参与其他反应形成具有一定功能的环氧树脂。
本发明提供的水性环氧树脂制备工艺简单、成本较低,利用该树脂制得的涂料具有耐水性、耐油性、耐酸碱性、耐盐雾腐蚀性等化学特性;耐磨性、耐冲压性、耐洗刷性等优异;表面光亮、平整、美观、无接缝、易清洗、易维修保养、经久耐用。
附图说明
图1为式(I)所示的化合物的氢谱图。
图2为式(II)所示的化合物的氢谱图。
具体实施方式
下面对本发明作出进一步说明。
实施例1
将式III所示的化合物溶于甲苯中,加入氢氧化钠水溶液,边搅拌边加热,当温度升到65℃时恒温搅拌并滴加环氧丙醇,于2小时内滴加完毕;提高温度,于 80℃保持1.5h;加入蒸馏水,搅拌,静止分层除去水层,甲苯层减压蒸干得式I 所示化合物;式III所示的化合物与环氧丙醇的摩尔比为n:(2n+2至2n+4);氢氧化钠水溶液中氢氧化钠的含量为0.5n-1.5n摩尔;蒸馏水和甲苯的体积比为3:1。
得反应产物674.1g,m/z 720.31,氢谱见图1。
式I所示的化合物与溶解于混合溶剂中,氮气保护下,缓慢滴加甲基丙烯酸、苯乙烯,再加入引发剂,升温至105℃,恒温反应1.5h,冷却至45℃,调pH至7-8,恒温反应1.5h,即得。
得反应产物398.4g,m/z 1060.15,氢谱见图2。
实施例2
将式III所示的化合物溶于甲苯中,加入氢氧化钠水溶液,边搅拌边加热,当温度升到60℃时恒温搅拌并滴加环氧丙醇,于2小时内滴加完毕;提高温度,于 75℃保持2h;加入蒸馏水,搅拌,静止分层除去水层,甲苯层减压蒸干得式I所示化合物;式III所示的化合物与环氧丙醇的摩尔比为n:(2n+2至2n+4);氢氧化钠水溶液中氢氧化钠的含量为0.5n-1.5n摩尔;蒸馏水和甲苯的体积比为4:1。
得反应产物569.1g,m/z 720.31,氢谱见图1。
式I所示的化合物与溶解于混合溶剂中,氮气保护下,缓慢滴加甲基丙烯酸、苯乙烯,再加入引发剂,升温至110℃,恒温反应1h,冷却至50℃,调pH至7-8,恒温反应1h,即得。
得反应产物387.1g,m/z 1060.15,氢谱见图2。
实施例3
将式III所示的化合物溶于甲苯中,加入氢氧化钠水溶液,边搅拌边加热,当温度升到70℃时恒温搅拌并滴加环氧丙醇,于2小时内滴加完毕;提高温度,于85℃保持1h;加入蒸馏水,搅拌,静止分层除去水层,甲苯层减压蒸干得式I 所示化合物;式III所示的化合物与环氧丙醇的摩尔比为n:(2n+2至2n+4);氢氧化钠水溶液中氢氧化钠的含量为0.5n-1.5n摩尔;蒸馏水和甲苯的体积比为2:1。
得反应产物497.3g,m/z 720.31,氢谱见图1。
式I所示的化合物与溶解于混合溶剂中,氮气保护下,缓慢滴加甲基丙烯酸、苯乙烯,再加入引发剂,升温至100℃,恒温反应2h,冷却至40℃,调pH至7-8,恒温反应2h,即得。
得反应产物238.1g,m/z 1060.15,氢谱见图2。
实施例4
制得一批水性环氧树脂涂料,其配方如下表。
测试上述水性环氧涂料的性能,结果见下表。
样品1 | 样品2 | 样品3 | 对比例1 | |
表干25℃(min) | 10 | 10 | 10 | 30 |
硬干25℃(min) | 80 | 80 | 80 | 120 |
实干25℃(h) | 2.5 | 2.5 | 2.5 | 3.5 |
硬度(24h) | 3H | 3H | 3H | - |
冲击韧性KJ/m<sup>2</sup> | 45.97 | 42.60 | 41.08 | 9.00 |
弯曲强度MPa | 144.32 | 135.07 | 132.48 | 110.00 |
弯曲模量GPa | 3.31 | 3.01 | 2.88 | 2.50 |
玻璃转化温度℃ | 204.18 | 197.41 | 193.08 | 170.00 |
固体份(%) | 86.59 | 84.16 | 84.21 | 70.00 |
粘度(涂-4杯,s) | 22.45 | 22.86 | 22.59 | 142.00 |
一次涂膜厚度 | 166.76 | 147.54 | 143.78 | 104.00 |
VOC | 117.59 | 119.49 | 119.13 | 169.00 |
剥离强度N/mm | 1.68 | 1.57 | 1.53 | 1.38 |
层间粘合力N/mm | 1.17 | 1.10 | 1.10 | 0.99 |
吸湿性wt% | 0.60 | 0.60 | 0.61 | 0.67 |
Claims (7)
3.根据权利要求2所述的一种增韧型水性环氧树脂的制备方法,其特征在于:步骤(1)具体为:将式III所示的化合物溶于甲苯中,加入氢氧化钠水溶液,边搅拌边加热,当温度升到60-70℃时恒温搅拌并滴加环氧丙醇,于2小时内滴加完毕;提高温度,于75-85℃保持1-2h;加入蒸馏水,搅拌,静止分层除去水层,甲苯层减压蒸干即得式I所示化合物。
4.根据权利要求2所述的一种增韧型水性环氧树脂的制备方法,其特征在于:步骤(2)具体为:式I所示的化合物溶解于混合溶剂中,氮气保护下,缓慢滴加甲基丙烯酸、苯乙烯,再加入引发剂,升温至100-110℃,恒温反应1-2h,冷却至40-50℃,调pH至7-8,恒温反应1-2h,即得。
5.根据权利要求2所述的一种增韧型水性环氧树脂的制备方法,其特征在于:式III所示的化合物与环氧丙醇的摩尔比为n:(2n+2至2n+4)。
6.根据权利要求2所述的一种增韧型水性环氧树脂的制备方法,其特征在于:氢氧化钠水溶液中氢氧化钠的含量为0.5n-1.5n摩尔/L。
7.根据权利要求2所述的一种增韧型水性环氧树脂的制备方法,其特征在于:蒸馏水和甲苯的体积比为(2-4):1。
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