CN109535861A - 一种采用溶剂染料制备的水性荧光颜料色浆及其制备方法 - Google Patents
一种采用溶剂染料制备的水性荧光颜料色浆及其制备方法 Download PDFInfo
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Abstract
一种采用溶剂染料制备的水性荧光颜料色浆及其制备方法。涉及精细化工领域，具体涉及一种采用溶剂染料制备的水性荧光颜料色浆及其制备方法。提供了一种避免溶剂染料析出、提高色浆品质的采用溶剂染料制备的水性荧光颜料色浆及其制备方法。按质量份计，包括如下组分：质量浓度为10%的聚乙烯醇水溶液45‑55份、十二烷基苯磺酸钠15‑25份、十一碳醇二十聚氧乙烯醚15‑25份、聚合单体280‑320份、溶剂染料5.6‑6.4份、低分子量多元醇10‑15份、过硫酸铵1‑5份、去离子水570‑610份。本发明有利于染料的布朗运动，从而让染料微粒有更为充分的可能对乳胶粒进行染色。
Description
技术领域
本发明涉及精细化工领域，具体涉及一种采用溶剂染料制备的水性荧光颜料色浆及其制备方法。
背景技术
有机荧光颜料可以吸收可见光和紫外线，能把紫外线转变为一定颜色的可见光进行反射，所以总的反射光强度大大高于普通颜料，具有非常艳丽的色彩。
通常的水性荧光颜料色浆的制备方法有荧光颜料分散法和乳液聚合法。
荧光颜料分散法为先制备荧光颜料，然后再添加分散剂等助剂将荧光颜料粉末分散在水中，得到水性荧光颜料色浆。这种方法得到的色浆分散稳定性差、耐候性差，同时含有游离甲醛。
乳液聚合法采用苯乙烯、丙烯腈等单体，直接聚合得到分散稳定的乳液，同时不含游离甲醛。乳液聚合法合成水性荧光颜料色浆一般采用碱性染料进行染色，如申请号分别为200910098017.4、201010113614.2、201310492182.4和201511010399.2中国专利所述。溶剂染料的耐光性大大优于碱性染料，采用溶剂染料染色的荧光颜料具有更为优异的耐候性，但是乳液聚合中由于溶剂染料只能溶于单体相且难以跟随单体转移进入乳胶粒，从而在水相析出，产生染料颗粒。这种溶剂染料的析出颗粒物导致乳液中大颗粒物增多，产生目测可见的染色不均匀现象，是目前溶剂染料在水性荧光颜料色浆中应用的最大障碍。如专利名称为“一种制备纳米荧光颜料分散体的方法”、申请号为“201410449357.8”的中国专利，采用了细乳液聚合法制备溶剂染料染色的水性荧光颜料色浆，采用低沸点有机溶剂来协助溶剂染料的迁移，但是在80℃左右聚合温度下，丙酮、丁醇等溶剂极易在水相扩散，难以达到对溶剂染料阻隔的效果，因此聚合完成后仍需要采用500nm的微孔滤纸过滤，以除去水相存在的析出溶剂染料，仍然没能解决溶剂染料的析出问题。
发明内容
本发明针对以上问题，提供了一种避免溶剂染料析出、提高色浆品质的采用溶剂染料制备的水性荧光颜料色浆及其制备方法。
本发明的技术方案是：
一种采用溶剂染料制备的荧光颜料色浆，按质量份计，包括如下组分：质量浓度为10%的聚乙烯醇水溶液45-55份、十二烷基苯磺酸钠15-25份、十一碳醇二十聚氧乙烯醚15-25份、聚合单体280-320份、溶剂染料5.6-6.4份、低分子量多元醇10-15份、过硫酸铵1-5份、去离子水570-610份。
所述聚合单体包括苯乙烯、丙烯腈、甲基丙烯酸甲酯和甲基丙烯酸，其质量份分别为145-155份、55-60份、80-90份和2-5份。
3、根据权利要求1所述的一种采用溶剂染料制备的荧光颜料色浆，其特征在于，所述溶剂染料为溶剂黄160、溶剂黄185或溶剂黄145。
所述低分子量多元醇为乙二醇、二乙二醇、三乙二醇、丙三醇、三羟甲基丙烷、季戊四醇中的一种或多种复配。
一种权利要求1所述的采用溶剂染料制备的荧光颜料色浆的制备方法，包括如下步骤：
1）、将聚乙烯醇水溶液、十二烷基苯磺酸钠和十一碳醇二十聚氧乙烯醚溶解在490-502份的去离子水中得到水相液；
2）、将聚合单体、溶剂染料、低分子量多元醇搅拌混合溶解得到单体溶液；
3）、将单体溶液缓慢加入水相液中，高剪切乳化，得到乳液；
4）、将过硫酸铵溶解到80-108份的去离子水中得到过硫酸铵溶液；
5）、将100-110份步骤3）制得的乳液搅拌升温至90-95℃并保温，滴加剩余乳液，3h内滴加完毕，同时滴加步骤4）制得的过硫酸铵溶液，5h内滴加完毕；
6）、过滤出料，得到水性荧光颜料色浆。
本发明的有益效果是：通过在溶剂染料的单体溶液中添加低分子量多元醇，随着单体迁移聚合，析出的溶剂染料由于有低分子量多元醇的阻隔，难以团聚形成大颗粒物，同时其表面的多元醇提高了溶剂染料通过水相迁移的能力，实现了从水相到树脂相的顺利迁移。乳液聚合的温度为90-95℃，高于通常的乳液聚合温度80-85℃，更为有利于染料的布朗运动，从而让染料微粒有更为充分的可能对乳胶粒进行染色。
具体实施方式
下面结合实施例对本发明作具体说明。
实施例1
在大烧杯中依次加入去离子水495克、10%聚乙烯醇水溶液（型号为1788）50克、十二烷基苯磺酸钠（阴离子乳化剂）20克、十一碳醇二十聚氧乙烯醚（乳化剂1120，非离子乳化剂）20克，溶解得到水相液，另取一大烧杯，依次加入苯乙烯150克、丙烯腈57克、甲基丙烯酸甲酯90克、甲基丙烯酸3克、丙三醇10克和溶剂黄160 6克，搅拌溶解得到单体溶液。单体溶液缓慢加入到水相液中，高剪切乳化，得到黄色乳液。另取一烧杯，称取2克过硫酸铵和100克水，搅拌溶解。在具有搅拌器、冷凝器的三口瓶中加入上述乳液105克，搅拌升温到95℃保温，开始缓慢滴加剩余乳液，3小时内滴加完毕。同时缓慢滴加过硫酸铵溶液，5小时内滴加完毕。过滤出料（此处采用200目滤网过滤，目的是过滤掉合成过程中难免出现的大颗粒比如树脂颗粒，而对比文件201410449357.8需要采用500nm的微孔滤纸过滤，以除去水相存在的析出溶剂染料，与本案该处过滤用途不同），得到亮黄色水性荧光颜料色浆。聚合时，温度高，沸点越低的越容易转移，低分子多元醇，沸点都很高，难以转移，所以会随着溶剂染料一起析出，但是，多元醇又极易溶于水，相当于提高了溶剂染料的亲水性，所以本案中不会有溶剂染料析出。
实施例2
在大烧杯中依次加入去离子水490克、10%聚乙烯醇水溶液45克、十二烷基苯磺酸钠15克、乳化剂1120 15克，溶解得到水相液，另取一大烧杯，依次加入苯乙烯145克、丙烯腈55克、甲基丙烯酸甲酯80克、甲基丙烯酸2克、乙二醇12克和溶剂黄185 5.6克，搅拌溶解得到单体溶液。单体溶液缓慢加入到水相液中，高剪切乳化，得到黄色乳液。另取一烧杯，称取1克过硫酸铵和80克水，搅拌溶解。在具有搅拌器、冷凝器的三口瓶中加入上述乳液100克，搅拌升温到90℃保温，开始缓慢滴加剩余乳液，3小时内滴加完毕。同时缓慢滴加过硫酸铵溶液，5小时内滴加完毕。过滤出料，得到亮黄色水性荧光颜料色浆。
实施例3
在大烧杯中依次加入去离子水502克、10%聚乙烯醇水溶液55克、十二烷基苯磺酸钠25克、乳化剂1120 25克，溶解得到水相液，另取一大烧杯，依次加入苯乙烯155克、丙烯腈60克、甲基丙烯酸甲酯85克、甲基丙烯酸5克、二乙二醇5克、三乙二醇5克、三羟甲基丙烷2克、季戊四醇3克和溶剂黄145 6.4克，搅拌溶解得到单体溶液。单体溶液缓慢加入到水相液中，高剪切乳化，得到黄色乳液。另取一烧杯，称取5克过硫酸铵和108克水，搅拌溶解。在具有搅拌器、冷凝器的三口瓶中加入上述乳液110克，搅拌升温到92℃保温，开始缓慢滴加剩余乳液，3小时内滴加完毕。同时缓慢滴加过硫酸铵溶液，5小时内滴加完毕。过滤出料，得到亮黄色水性荧光颜料色浆。
对比例1
在大烧杯中依次加入去离子水502克、10%聚乙烯醇水溶液50克、十二烷基苯磺酸钠20克、乳化剂1120 20克，溶解得到水相液，另取一大烧杯，依次加入苯乙烯150克、丙烯腈57克、甲基丙烯酸甲酯90克、甲基丙烯酸3克和溶剂黄160 6克，搅拌溶解得到单体溶液。单体溶液缓慢加入到水相液中，高剪切乳化，得到黄色乳液。另取一烧杯，称取2克过硫酸铵和100克水，搅拌溶解。在具有搅拌器、冷凝器的三口瓶中加入上述乳液100克，搅拌升温到90-95℃保温，开始缓慢滴加剩余乳液，3小时内滴加完毕。同时缓慢滴加过硫酸铵溶液，5小时内滴加完毕。过滤出料，得到亮黄色水性荧光颜料色浆。
对比例2
在大烧杯中依次加入去离子水490克、10%聚乙烯醇水溶液50克、十二烷基苯磺酸钠20克、乳化剂1120 20克，溶解得到水相液，另取一大烧杯，依次加入苯乙烯150克、丙烯腈57克、甲基丙烯酸甲酯90克、甲基丙烯酸3克、丙三醇12克和溶剂黄160 6克，搅拌溶解得到单体溶液。单体溶液缓慢加入到水相液中，高剪切乳化，得到黄色乳液。另取一烧杯，称取2克过硫酸铵和100克水，搅拌溶解。在具有搅拌器、冷凝器的三口瓶中加入上述乳液100克，搅拌升温到80-85℃保温，开始缓慢滴加剩余乳液，3小时内滴加完毕。同时缓慢滴加过硫酸铵溶液，5小时内滴加完毕。过滤出料，得到亮黄色水性荧光颜料色浆。
因为溶剂染料在水相的析出物密度大于水且不能稳定分散于水中，因此可以通过稀释后沉降的方法观察是否存在析出的溶剂染料。对于实施例1、实施例2、实施例3、比较例1和比较例2，分别取100克水性荧光颜料色浆，加入去离子水400克，稀释到500克，常温静止24小时观察是否有染料颗粒物沉降，情况如表1所示。
表1 染料沉降结果
从表1中可以看出，在不加低分子量多元醇的比较例1和比较例2中，染料容易析出，而添加了低分子量多元醇的实施例1-3中无染料沉降。实施例1和比较例2对比，说明高温聚合有利于溶剂染料的染色。
Claims (5)
1.一种采用溶剂染料制备的荧光颜料色浆，其特征在于，按质量份计，包括如下组分：质量浓度为10%的聚乙烯醇水溶液45-55份、十二烷基苯磺酸钠15-25份、十一碳醇二十聚氧乙烯醚 15-25份、聚合单体280-320份、溶剂染料5.6-6.4份、低分子量多元醇10-15份、过硫酸铵1-5份、去离子水570-610份。
2.根据权利要求1所述的一种采用溶剂染料制备的荧光颜料色浆，其特征在于，所述聚合单体包括苯乙烯、丙烯腈、甲基丙烯酸甲酯和甲基丙烯酸，其质量份分别为145-155份、55-60份、80-90份和2-5份。
3.根据权利要求1所述的一种采用溶剂染料制备的荧光颜料色浆，其特征在于，所述溶剂染料为溶剂黄160、溶剂黄185或溶剂黄145。
4.根据权利要求1所述的一种采用溶剂染料制备的荧光颜料色浆，其特征在于，所述低分子量多元醇为乙二醇、二乙二醇、三乙二醇、丙三醇、三羟甲基丙烷、季戊四醇中的一种或多种复配。
5.一种权利要求1所述的采用溶剂染料制备的荧光颜料色浆的制备方法，其特征在于，包括如下步骤：
1）、将聚乙烯醇水溶液、十二烷基苯磺酸钠和十一碳醇二十聚氧乙烯醚溶解在490-502份的去离子水中得到水相液；
2）、将聚合单体、溶剂染料、低分子量多元醇搅拌混合溶解得到单体溶液；
3）、将单体溶液缓慢加入水相液中，高剪切乳化，得到乳液；
4）、将过硫酸铵溶解到80-108份的去离子水中得到过硫酸铵溶液；
5）、将100-110份步骤3）制得的乳液搅拌升温至90-95℃并保温，滴加剩余乳液，3h内滴加完毕，同时滴加步骤4）制得的过硫酸铵溶液，5h内滴加完毕；
6）、过滤出料，得到水性荧光颜料色浆。
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