CN106634767A - 一种无氨丙烯酸/醇酸树脂留白胶及其制备方法和应用 - Google Patents
一种无氨丙烯酸/醇酸树脂留白胶及其制备方法和应用 Download PDFInfo
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Abstract
本发明公开了一种无氨丙烯酸/醇酸树脂留白胶及其制备方法和应用。本方法首先将功能性单体、亲油性乙烯基单体、醇酸树脂、催干剂在油溶性引发剂作用下进行自由基聚合,然后降温,用酸性中和剂进行中和,最后水分散得到水性丙烯酸/醇酸树脂微乳液,再与分散剂、颜料混合,充分分散并研磨至细度合格,即得无氨丙烯酸/醇酸树脂留白胶。与市场上以天然橡胶胶乳为主要成分的留白胶相比,本发明具有无刺激味、环保和保质期长的优点,同时制备工艺简单,具有广泛的市场应用前景。该留白胶可广泛的应用于水彩画留白过程中,也可以作为木材和玻璃表面的可剥离涂料使用。
Description
【技术领域】
本发明涉及水性胶黏剂及其制备方法,特别涉及一种无氨丙烯酸/醇酸树脂留白胶及其制备方法和应用。
【背景技术】
在水彩绘画中,留白胶对整个水彩画创作过程起到很重要的作用。留白胶是一种添加色素沉淀的液体,由乳胶和色料构成,用于水彩绘画中遮蔽需要保护的地方,它的使用方法是:在水彩上色之前,把需要留白的地方标记出来,然后用笔沾上水彩留白胶画在这些标记出来的地方,待干后便开始上色了,上完色待水彩纸干透后用橡皮泥或者是橡皮擦把这些涂有水彩留白胶的地方轻轻擦掉,即可显出留白画面,然后根据需要继续绘制。
目前市场上主要的水彩留白胶是水基天然乳状胶液,天然胶乳是橡胶-水基分散体系,其主要由作成膜物质的橡胶粒子和作保护胶体的非橡胶物质组成,非橡胶物质主要有糖类、蛋白质、磷脂和金属盐等。然而正是这些非橡胶物质的存在,新鲜天然乳胶如不做任何处理,一般经过6至12个小时就会发生明显的腐败现象,从而影响胶乳的质量和使用。为防止胶乳腐败,常加入氨作为保存剂,一方面氨能抑制细菌生长和酶的活性,消除或减轻细菌和酶对胶乳的腐败作用;同时氨是一种碱,可与类酯物水解所产生的高级脂肪酸发生反应,生成铵皂吸附在橡胶粒子表面,并增加橡胶粒子表面所带的负电荷和水合度,提高胶乳的稳定性。但是氨本身易挥发、刺激性大、有腐蚀性,不仅浪费大,而且使生产环境恶化还会对人体健康造成伤害,许多绘画者都在抱怨刚打开留白胶瓶盖闻到一股刺鼻的味道,就是这个原因;同时随着氨的不断挥发,胶乳表面的粒子电荷强度减小,胶乳的稳定性下降,导致留白胶在使用后期黏度变大甚至凝胶。
【发明内容】
为克服现有市场产品的不足,本发明的目的是提供一种无氨丙烯酸/醇酸树脂留白胶及其制备方法和应用,采用本发明方法制备丙烯酸/醇酸树脂留白胶过程中,不需要加入氨作为杀菌剂和稳定剂,制备出的留白胶无任何刺激味,不发生腐败,稳定性良好。
为了达到上述目的,本发明采用的技术方案是:
一种无氨丙烯酸/醇酸树脂留白胶的制备方法,包括以下步骤:
a,按重量份计,向干燥反应器中加入0.1~15份功能性单体、1~30份亲油性单体、1~20份醇酸树脂、0.01~3份催干剂和0.1~3份油溶性引发剂,反应温度50~90℃,反应时间2~7h;
b,将体系冷却至10~40℃,按重量份计,再加入0.1~2份酸性中和剂,进行中和反应;
c,在搅拌条件下,缓慢加入热水,水温为50~100℃,降温后即得到泛蓝光的丙烯酸/醇酸树脂乳液;
d,按重量份计,取水性丙烯酸/醇酸树脂乳液30~80份,分散剂0.1~2份,颜料5~20份混合,充分分散并研磨至细度合格,即得无氨丙烯酸/醇酸树脂留白胶。
所述分散剂为阳离子聚丙烯酰胺EFKA-5010、阳离子聚丙烯酸酯分散剂SN-580、非离子型润湿分散剂FX-365中一种或两种以上任意配比的混合物;
所述颜料为钴蓝、铬绿、铁红或铬黄。
所述亲油性单体为甲基丙烯酸乙酯、苯乙烯、甲基丙烯酸丁酯、丙烯酸乙酯、丙烯酸丁酯、丙烯酸异辛酯中一种或两种以上任意配比的混合物。
所述功能单体为丙烯酰胺、二甲基二烯丙基氯化铵、甲基丙烯酸二甲氨基乙酯、甲基丙烯酰氧乙基三甲基氯化铵中的一种或两种任意配比的混合物。
所述醇酸树脂为长油度醇酸树脂、中油度醇酸树脂、短油度醇酸树脂中的一种或两种任意配比的混合物。
所述催干剂为锆催干剂、锰催干剂、锌催干剂、铅催干剂、稀土催干剂中的一种或两种任意配比的混合物。
所述酸性中和剂为甲酸、乙二酸、丁酸、戊酸乙酸、盐酸、丙酸中的一种或两种任意配比的混合物。
所述油溶性引发剂为偶氮二异丁腈、偶氮二异庚腈、过氧化二苯甲酰、过氧化苯甲酸叔丁酯中的一种或两种任意配比的混合物。
一种无氨丙烯酸/醇酸树脂留白胶的制备方法制得。
一种无氨丙烯酸/醇酸树脂留白胶在水彩画留白中、木材和玻璃表面可剥离涂料中的应用。
与现有技术相比,本发明具有以下有益的技术效果:
本发明公开了一种无氨丙烯酸/醇酸树脂留白胶的制备方法,将功能性单体、亲油性乙烯基单体、醇酸树脂、催干剂在油溶性引发剂作用下进行自由基聚合,降温用酸性中和剂进行中和,水分散得到水性丙烯酸/醇酸树脂微乳液,再与分散剂、颜料混合,充分分散并研磨至细度合格,即得无氨丙烯酸/醇酸树脂留白胶。本发明以廉价的醇酸树脂代替天然橡胶乳液中的聚异戊二烯作为主要成膜物质,引入阳离子亲水单体,用阳离子丙烯酸树脂乳化剂代替非橡胶物质作为乳液稳定剂,水为溶剂,配以分散剂和颜料,采用乳化工艺制备出无氨丙烯酸/醇酸树脂留白胶。由于采用酸性中和剂,避免了引入胺类中和剂,离子性的丙烯酸树脂乳化剂分散稳定能力好于非离子性的非橡胶物质的稳定能力,制备出的留白胶具有无任何刺激味和稳定性好的优点。与市场上以天然橡胶胶乳为主要成分的留白胶相比,本发明具有无刺激味、环保和保质期长的优点,同时制备工艺简单,具有广泛的市场应用前景。
本发明产品无氨,无溶剂,具有无刺激味、稳定性好和保质期长等优点。通过60℃贮存25天贮藏测试,结果表明本发明产品具有较好的贮藏稳定性。
本发明的该留白胶可广泛的应用于水彩画留白过程中,也可以作为木材和玻璃表面的可剥离涂料使用。为水彩绘画的留白胶提供了新的材料。
【附图说明】
图1a为天然胶乳留白胶的贮藏稳定性曲线图;
图1b为无氨留白胶的贮藏稳定性曲线图。
【具体实施方式】
下面结合具体实施例对本发明做进一步详细描述:(以重量份计)
实施例1:
将水性丙烯酸/醇酸树脂乳液50份,0.2份阳离子聚丙烯酰胺EFKA-5010,6份钴蓝混合在一起,充分分散并研磨至细度合格,即得无氨丙烯酸/醇酸树脂留白胶。
其中,水性丙烯酸/醇酸树脂乳液的制备工艺如下:
1)首先,按质量分数向装有回流冷凝管、搅拌器、温度计的三口干燥烧瓶中加入10份甲基丙烯酸二甲氨基乙酯、5份丙烯酸丁酯、18份醇酸树脂、3份锆催干剂和0.8份偶氮二异丁腈,在60℃条件下均匀搅拌2h;
2)然后,将体系冷却至10℃,再加入0.5份甲酸中和,中和时间10min;
3)最后,在600转/分钟的高速搅拌条件下,缓慢加入60℃热水进行乳化分散,降温后即得到半透明泛蓝光的丙烯酸/醇酸树脂复合乳液。
4)实施例2:
将水性丙烯酸/醇酸树脂乳液80份,0.5份阳离子聚丙烯酸酯分散剂SN-580,10份铬绿混合在一起,充分分散并研磨至细度合格,即得无氨丙烯酸/醇酸树脂留白胶。
其中,水性丙烯酸/醇酸树脂乳液的制备工艺如下:
1)首先,按质量分数向装有回流冷凝管、搅拌器、温度计的三口干燥烧瓶中加入12份丙烯酰胺、8份丙烯酸乙酯、10份醇酸树脂、0.5份锰催干剂和0.8份过氧化苯甲酸叔丁酯,在60℃条件下均匀搅拌3.5h;
2)然后,将体系冷却至20℃,再加入1份丙酸,中和时间20min;
3)最后,在1000转/分钟的高速搅拌条件下,缓慢加入80℃热水进行乳化分散,降温后即得到半透明泛蓝光的丙烯酸/醇酸树脂复合乳液。
实施例3:
将水性丙烯酸/醇酸树脂乳液60份,2份非离子型润湿分散剂FX-365,8份铁红混合在一起,充分分散并研磨至细度合格,即得无氨丙烯酸/醇酸树脂留白胶。
其中,水性丙烯酸/醇酸树脂乳液的制备工艺如下:
1)首先,按质量分数向装有回流冷凝管、搅拌器、温度计的三口干燥烧瓶中加入8份甲基丙烯酰氧乙基三甲基氯化铵、17份甲基丙烯酸乙酯、15份醇酸树脂、2份稀土催干剂和1.5份偶氮二异庚腈,在70℃条件下均匀搅拌5h;
2)然后,将体系冷却至30℃,再加入2份丁酸,中和时间30min;
3)最后,在800转/分钟的高速搅拌条件下,缓慢加入90℃热水进行乳化分散,降温后即得到半透明泛蓝光的丙烯酸/醇酸树脂复合乳液。
实施例4:
将水性丙烯酸/醇酸树脂乳液70份,1.5份阳离子聚丙烯酸酯分散剂SN-580,7份铬黄混合在一起,充分分散并研磨至细度合格,即得无氨丙烯酸/醇酸树脂留白胶。
其中,水性丙烯酸/醇酸树脂乳液的制备工艺如下:
1)首先,按质量分数向装有回流冷凝管、搅拌器、温度计的三口干燥烧瓶中加入5份二甲基二烯丙基氯化铵、18份苯乙烯、12份醇酸树脂、1份铅催干剂和2份过氧化二苯甲酰,在80℃条件下均匀搅拌6h;
2)然后,将体系冷却至10℃,再加入1份戊酸乙酸,中和时间20min;
3)最后,在700转/分钟的高速搅拌条件下,缓慢加入60℃热水进行乳化分散,降温后即得到半透明泛蓝光的丙烯酸/醇酸树脂复合乳液。
实施例5:
将水性丙烯酸/醇酸树脂乳液40份,1.2份阳离子聚丙烯酰胺EFKA-5010,15份铬绿混合在一起,充分分散并研磨至细度合格,即得无氨丙烯酸/醇酸树脂留白胶。
其中,水性丙烯酸/醇酸树脂乳液的制备工艺如下:
1)首先,按质量分数向装有回流冷凝管、搅拌器、温度计的三口干燥烧瓶中加入8份丙烯酰胺、2份甲基丙烯酰氧乙基三甲基氯化铵、15份丙烯酸异辛酯、6份甲基丙烯酸丁酯、8份醇酸树脂、0.02份锌催干剂和1.8份过氧化二苯甲酰,在50℃条件下均匀搅拌7h;
2)然后,将体系冷却至20℃,再加入1.5份乙二酸,中和时间20min;
3)最后,在900转/分钟的高速搅拌条件下,缓慢加入70℃热水进行乳化分散,降温后即得到半透明泛蓝光的丙烯酸/醇酸树脂复合乳液。
实施例6:
将水性丙烯酸/醇酸树脂乳液30份,0.1份非离子型润湿分散剂FX-365,5份铬黄混合在一起,充分分散并研磨至细度合格,即得无氨丙烯酸/醇酸树脂留白胶。
其中,水性丙烯酸/醇酸树脂乳液的制备工艺如下:
1)首先,按质量分数向装有回流冷凝管、搅拌器、温度计的三口干燥烧瓶中加入20份丙烯酰胺、10份甲基丙烯酰氧乙基三甲基氯化铵、1份甲基丙烯酸丁酯、1份醇酸树脂(中油度醇酸树脂和短油度醇酸树脂)、0.01份锌催干剂和0.1份过氧化二苯甲酰,在50℃条件下均匀搅拌7h;
2)然后,将体系冷却至20℃,再加入0.1份乙二酸,中和时间20min;
3)最后,在900转/分钟的高速搅拌条件下,缓慢加入100℃热水进行乳化分散,降温后即得到半透明泛蓝光的丙烯酸/醇酸树脂复合乳液。
实施例7:
将水性丙烯酸/醇酸树脂乳液70份,1.5份阳离子聚丙烯酸酯分散剂SN-580、0.5份非离子型润湿分散剂FX-365,7份铬黄混合在一起,充分分散并研磨至细度合格,即得无氨丙烯酸/醇酸树脂留白胶。
其中,水性丙烯酸/醇酸树脂乳液的制备工艺如下:
1)首先,按质量分数向装有回流冷凝管、搅拌器、温度计的三口干燥烧瓶中加入5份二甲基二烯丙基氯化铵、10份苯乙烯、10份丙烯酸丁酯、10份丙烯酸异辛酯、20份醇酸树脂(长油度醇酸树脂和中油度醇酸树脂)、1份锰催干剂、1份锌催干剂、2份过氧化二苯甲酰和1份偶氮二异丁腈,在80℃条件下均匀搅拌2h;
2)然后,将体系冷却至40℃,再加入1份戊酸乙酸和1份盐酸,中和时间20min;
3)最后,在700转/分钟的高速搅拌条件下,缓慢加入60℃热水进行乳化分散,降温后即得到半透明泛蓝光的丙烯酸/醇酸树脂复合乳液。
实施例8:
将水性丙烯酸/醇酸树脂乳液70份,1.5份阳离子聚丙烯酸酯分散剂SN-580、0.5份阳离子聚丙烯酰胺EFKA-5010、0.1份阳离子聚丙烯酸酯分散剂SN-580,7份铬黄混合在一起,充分分散并研磨至细度合格,即得无氨丙烯酸/醇酸树脂留白胶。
其中,水性丙烯酸/醇酸树脂乳液的制备工艺如下:
1)首先,按质量分数向装有回流冷凝管、搅拌器、温度计的三口干燥烧瓶中加入5份二甲基二烯丙基氯化铵、10份甲基丙烯酸乙酯、8份丙烯酸丁酯、10份丙烯酸异辛酯、20份醇酸树脂(长油度醇酸树脂和中油度醇酸树脂)、1份锰催干剂、1份铅催干剂、2份偶氮二异丁腈和0.5份偶氮二异庚腈,在80℃条件下均匀搅拌6h;
2)然后,将体系冷却至10℃,再加入1份丁酸和0.5份戊酸乙酸,中和时间20min;
3)最后,在700转/分钟的高速搅拌条件下,缓慢加入50℃热水进行乳化分散,降温后即得到半透明泛蓝光的丙烯酸/醇酸树脂复合乳液。
应用和测试:
将本发明制备的无氨丙烯酸/醇酸树脂留白胶及市场天然胶留白胶进行存储实验(60℃贮存25天),并进行粒径测试,绘制曲线:
图1a为市场天然胶留白胶在60℃贮存25天过程中粒径变化图,由图可以看出,市场的天然胶留白胶随着存储时间的增加,留白胶的粒径出现变大的趋势。
图1b为本发明的无氨留白胶在60℃贮存25天粒径变化图,从图中可以看出本发明的无氨留白胶具有较好的贮藏稳定性,并且在存储时间的增加的情况下,粒径基本上变化不大。因此本发明制备的无氨留白胶较天然胶留白胶可做推广使用。
因此,本发明的该留白胶可广泛的应用于水彩画留白过程中,为水彩绘画的留白胶提供了新的材料。
以上内容是结合具体的优选实施方式对本发明所作的进一步详细说明,不能认定本发明的具体实施方式仅限于此,对于本发明所属技术领域的普通技术人员来说,在不隔离本发明构思的前提下,还可以做出若干简单的推演或替换,都应当视为属于本发明所提交的权利要求书确定专利保护范围。
Claims (10)
1.一种无氨丙烯酸/醇酸树脂留白胶的制备方法,其特征在于:包括以下步骤:
a,按重量份计,向干燥反应器中加入0.1~15份功能性单体、1~30份亲油性单体、1~20份醇酸树脂、0.01~3份催干剂和0.1~3份油溶性引发剂,反应温度50~90℃,反应时间2~7h;
b,将体系冷却至10~40℃,按重量份计,再加入0.1~2份酸性中和剂,进行中和反应;
c,在搅拌条件下,缓慢加入热水,水温为50~100℃,降温后即得到泛蓝光的丙烯酸/醇酸树脂乳液;
d,按重量份计,取水性丙烯酸/醇酸树脂乳液30~80份,分散剂0.1~2份,颜料5~20份混合,充分分散并研磨至细度合格,即得无氨丙烯酸/醇酸树脂留白胶。
2.根据权利要求1所述的一种无氨丙烯酸/醇酸树脂留白胶的制备方法,其特征在于:
所述分散剂为阳离子聚丙烯酰胺EFKA-5010、阳离子聚丙烯酸酯分散剂SN-580、非离子型润湿分散剂FX-365中一种或两种以上任意配比的混合物;
所述颜料为钴蓝、铬绿、铁红或铬黄。
3.根据权利要求1所述的一种无氨丙烯酸/醇酸树脂留白胶的制备方法,其特征在于:所述亲油性单体为甲基丙烯酸乙酯、苯乙烯、甲基丙烯酸丁酯、丙烯酸乙酯、丙烯酸丁酯、丙烯酸异辛酯中一种或两种以上任意配比的混合物。
4.根据权利要求1所述的一种无氨丙烯酸/醇酸树脂留白胶的制备方法,其特征在于:所述功能单体为丙烯酰胺、二甲基二烯丙基氯化铵、甲基丙烯酸二甲氨基乙酯、甲基丙烯酰氧乙基三甲基氯化铵中的一种或两种任意配比的混合物。
5.根据权利要求1所述的一种无氨丙烯酸/醇酸树脂留白胶的制备方法,其特征在于:所述醇酸树脂为长油度醇酸树脂、中油度醇酸树脂、短油度醇酸树脂中的一种或两种任意配比的混合物。
6.根据权利要求1所述的一种无氨丙烯酸/醇酸树脂留白胶的制备方法,其特征在于:所述催干剂为锆催干剂、锰催干剂、锌催干剂、铅催干剂、稀土催干剂中的一种或两种任意配比的混合物。
7.根据权利要求1所述的一种无氨丙烯酸/醇酸树脂留白胶的制备方法,其特征在于:所述酸性中和剂为甲酸、乙二酸、丁酸、戊酸乙酸、盐酸、丙酸中的一种或两种任意配比的混合物。
8.根据权利要求1所述的一种无氨丙烯酸/醇酸树脂留白胶的制备方法,其特征在于:所述油溶性引发剂为偶氮二异丁腈、偶氮二异庚腈、过氧化二苯甲酰、过氧化苯甲酸叔丁酯中的一种或两种任意配比的混合物。
9.一种无氨丙烯酸/醇酸树脂留白胶,其特征在于:由权利要求1至7任意一项所述的一种无氨丙烯酸/醇酸树脂留白胶的制备方法制得。
10.权利要求9所述的一种无氨丙烯酸/醇酸树脂留白胶在水彩画留白中、木材和玻璃表面可剥离涂料中的应用。
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CN116179069A (zh) * | 2022-12-28 | 2023-05-30 | 广东霆翊科技有限公司 | 一种无氨低气味留白胶及其制备方法 |
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Application publication date: 20170510 |