CN107653704B - 一种纤维原液色浆及其制备方法 - Google Patents
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Abstract
本发明公开了一种新型环保纤维原液色浆的制备方法，该色浆由包裹颜料的预乳化液、己二酰肼水溶液、引发剂溶液为原料制备而成，添加单体和引发剂溶液时温度控制在55‑60℃，添加完毕后反应4‑5h，且采用了批量添加的方式。本发明得到的纤维原液色浆具备更优异的着色效果、优异的耐光色牢度、耐候色牢度，无需后道纤维或织物的化学染色、丝束染色或凝胶染色，最大程度上降低了对环境的污染。
Description
技术领域
本发明属于精细化工涂料技术领域，具体涉及一种新型环保纤维原液色浆的制备方法。
背景技术
随着环境危害不断的扩大，在能源和水资源日益枯竭、环保压力日益增大的社会背景下，如何避免印染过程中的高能耗、高污染是关系到纺织行业生存的重要问题。传统的纤维原料着色工艺中，阳离子染料的吸尽率较低，染料消耗多，环境污染严重；同时染料结构上的原因等，造成准确配色较困难；同时由于自身结构原因，导致着色布日晒色牢度、皂洗色牢度、摩擦色牢度较差。由于价格较为低廉，使用方便等特点，在国内依然占用绝大数份额。
中国专利申请CN201410228230《粘胶原液着色用酞菁颜料水性色浆及其制备方法》，利用了甲醛溶液，虽然性能大幅度提升，但是在生产过程中难免有残留，或对生产人员有伤害，有极大的致癌隐患。专利CN201310742922《纤维原液着色用超细炭黑水性色浆》在生产过程中采用了氯仿做溶剂，对环境和操作人员有较大的伤害。
发明内容
为解决上述现有技术存在的问题，本发明提供了一种纤维原液色浆的制备方法，该着色色浆具有优异的储存稳定性、污染极小，日晒色牢度、皂洗色牢度、摩擦色牢度。
实现本发明上述目的所采用的技术方案为：
一种纤维原液色浆，包括预乳化液、乳液和引发剂溶液；
预乳化液包括以下质量份的原料：色粉15-25份，丙烯酸酯类单体84-90份，功能单体0.6-2.0份，反应型乳化剂4.0-5.0份，分散剂0.5-1.2份，缓冲剂1-4.0份，羟乙基甲基丙烯酸磷酸酯1.0-5.0份，去离子水85-92.0份；
反应型乳化剂为SR-10、SR-20、SOFTANOL 50、SOFTANOL 30中的任意一种，或者任意几种的混合物。
己二酰肼水溶液是8wt％的己二酰肼水溶液。
引发剂溶液是由1.2质量份过硫酸钾、1.0质量份亚硫酸氢钠、12.8质量份去离子水、2.0质量份丙二醇混合得到的。
所述的分散剂为TEGO750w，为德国迪高化工公司产品。
所述的丙烯酸酯类单体为甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸正丙酯、甲基丙烯酸正丁酯、丙烯酸羟乙酯、丙烯酸羟丙酯、丙烯酸月桂酯、甲氧基聚乙二醇甲基丙烯酸酯、丙烯酸-2-乙基己酯、甲基丙烯酸中的任意一种，或者任意几种的组合。
所述的缓冲剂为碳酸氢钠。
一种纤维原液色浆的制备方法，包括如下步骤：
步骤一、配制己二酰肼水溶液、引发剂溶液：
将己二酰肼溶于水，制备浓度为8wt％的己二酰肼水溶液；
引发剂溶液是由1.2质量份过硫酸钾、1.0质量份亚硫酸氢钠、12.8质量份去离子水、2.0质量份丙二醇混合得到的；
步骤二：预乳化液的制备：
称取色粉、分散剂、反应型乳化剂、水，混合并超声分散0.5h，然后加入缓冲剂、羟乙基甲基丙烯酸磷酸酯和去离子水，混合后搅拌进行超声乳化0.5-1h，得到预分散液；
向预分散液中滴加20％的丙烯酸酯类单体，同时加热至55-60℃，缓慢滴加10％的引发剂溶液，反应0.5h后得到种子乳液；
然后继续滴加余下的丙烯酸酯类单体、引发剂溶液，同时开始滴加功能单体，直至完毕，期间控温55-60℃，反应4-5h，最后过滤，制备得到预乳化液；
步骤三：纤维原液色浆的制备：向步骤二所得预乳化液缓慢加入己二酰肼水溶液，搅拌10-30min，用滤膜过滤去除滤渣，取滤液，即纤维原液色浆。
与现有技术相比，本发明的优点和有益效果在于：
1)本发明制备着色色浆的方法新颖，首次利用采用包裹颜料的方式，利用了“核壳”乳液的制备方法，使得产品具有更优异的着色效果。
2)本发明所制备的化纤着色色浆，无论是在制备工艺，还是应用过程中，具有无毒、无害、无气味和对环境友好等优点。
3)本发明采用核壳乳液聚合方式，取部分交联物预乳液作为”种子”乳液，分批次加入含有单体和引发剂，就地聚合形成包裹色粉的超细乳液，性能具备更好的协调与互补优势。
4)所得纤维着色色浆不仅具有粒径小、不会发生颜料迁移等优点，还具备优异的日晒色牢度、皂洗色牢度、摩擦色牢度等性能，采用本发明所制备的原液着色色浆省略了后道纤维或织物的化学染色、丝束染色或凝胶染色，最大程度上降低了对环境的污染。本发明可以利用于尼龙。
附图说明
图1是实施例1所得纤维原液色浆粒径分析图。
具体实施方式
以下各实施例中原料的来源为：
甲氧基聚乙二醇甲基丙烯酸酯为沙多玛公司的甲氧基聚乙二醇(350)单丙烯酸酯；甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸正丙酯、甲基丙烯酸正丁酯、丙烯酸羟乙酯、丙烯酸羟丙酯、丙烯酸月桂酯均为台湾长兴化工有限公司产品；丙烯酸-2-乙基己酯、双丙酮丙烯酰胺为东莞永正化工有限公司提供。
TEGO750w为德国迪高化工公司产品。
反应型乳化剂：SR-10为日本艾迪科(ADEKA)产品；SOFTANOL 30为株式会社日本触媒产品；SR-20为日本艾迪科(ADEKA)产品；SOFTANOL 50为株式会社日本触媒产品。
羟乙基甲基丙烯酸磷酸酯为日本化药产品。
实施例1
一种新型纤维原液色浆，由预乳化液、己二酰肼水溶液和引发剂溶液为原料制备而成：
预乳化液由表1所示的以下质量份的原料制备而成：
表1
己二酰肼水溶液浓度是8wt％。
引发剂溶液是由1.2质量份过硫酸钾、1.0质量份亚硫酸氢钠、12.8质量份去离子水、2.0质量份丙二醇混合得到的。
一纤维原液色浆的制备方法，包括如下步骤：
1)称取色粉酞青蓝15:3、分散剂TEGO750w、反应型乳化剂、水，混合并超声分散0.5h，然后加入缓冲剂碳酸氢钠、特种单体羟乙基甲基丙烯酸磷酸酯和去离子水，混合后搅拌进行超声乳化1h，得到预分散液。
2)向预分散液中滴加20％的丙烯酸酯类单体，加热至60℃，缓慢滴加10％的引发剂溶液，反应0.5h得到种子乳液。
3)然后向种子乳液中继续滴加余下的丙烯酸酯类单体、引发剂溶液，同时开始滴加功能单体直至完毕，期间控温55℃，反应4h，最后过滤，制备预乳化液。
4)然后向上述预乳化液中缓慢加入己二酰肼水溶液，搅拌30min，用滤膜过滤去除滤渣，取滤液，即得新型纤维原液色浆。
实施例2
一种新型纤维原液色浆，由预乳化液、己二酰肼水溶液和引发剂溶液为原料制备而成：
预乳化液由表2所示的以下质量份的原料制备而成：
表2
己二酰肼水溶液是将0.8-1.6质量份己二酰肼溶解在8-10份去离子水获得的。
引发剂溶液是由1.2质量份过硫酸钾、1.0质量份亚硫酸氢钠、12.8质量份去离子水、2.0质量份丙二醇混合得到的。
一种新型纤维原液色浆的制备方法，与实施例1不同之处在于，步骤(1)超声乳化0.5h，得到预分散液。
实施例3
一种新型纤维原液色浆，由预乳化液、己二酰肼水溶液和引发剂溶液为原料制备而成：
预乳化液由表3所示的以下质量份的原料制备而成：
表3
己二酰肼水溶液是将0.8-1.6质量份己二酰肼溶解在8-10份去离子水获得的。
引发剂溶液是由1.2质量份过硫酸钾、1.0质量份亚硫酸氢钠、12.8质量份去离子水、2.0质量份丙二醇混合得到的。
制备方法，与实施例1不同之处在于，步骤(2)加入20％丙烯酸酯类单体后，加热至55℃，滴加余下的丙烯酸酯类单体、引发剂溶液，同时开始滴加功能单体时，控温60℃。
实施例4
一种新型纤维原液色浆，由预乳化液、己二酰肼水溶液和引发剂溶液为原料制备而成：
预乳化液由表4所示的以下质量份的原料制备而成：
表4
己二酰肼水溶液是将0.8-1.6质量份己二酰肼溶解在8-10份去离子水获得的。
引发剂溶液是由1.2质量份过硫酸钾、1.0质量份亚硫酸氢钠、12.8质量份去离子水、2.0质量份丙二醇混合得到的。
制备方法，与实施例1不同之处在于，步骤(3)滴加全部单体和引发剂溶液后，反应时间是5h。
将实施例1-4所得纤维原液色浆按照如下标准进行测试，结果见表5：
粒径：GB/T 19077.1-2008粒度分析激光衍射法；
耐皂洗色牢度：GB/T3921-2008纺织品色牢度耐皂洗色牢度；
耐光色牢度：GB/T 8426-1998纺织品色牢度试验耐光色牢度：日光；
耐摩擦色牢度：GB-T 3920-2008纺织品色牢度试验耐摩擦色牢度；
迁移实验：ISO 105-Z06-1998纺织品色牢度试验第Z06部分：染料和颜料泳移的评价；
表5各实施例所得原液色浆的性能测试数据
Claims (6)
1.一种纤维原液色浆的制备方法，其特征在于，步骤如下：
步骤一、配制己二酰肼水溶液、引发剂溶液：
将己二酰肼溶于水，制备浓度为8wt%的己二酰肼水溶液；
引发剂溶液是由 1.2质量份过硫酸钾、1.0质量份亚硫酸氢钠、12.8质量份去离子水、2.0质量份丙二醇混合得到的;
步骤二：预乳化液的制备：
称取色粉、分散剂、反应型乳化剂、水，混合并超声分散0.5h，然后加入缓冲剂、羟乙基甲基丙烯酸磷酸酯和去离子水，混合后搅拌进行超声乳化0.5-1h，得到预分散液；
向预分散液中滴加20%的丙烯酸酯类单体，同时加热至55-60℃，缓慢滴加10%的引发剂溶液，反应0.5h后得到种子乳液；
然后继续滴加余下的丙烯酸酯类单体、引发剂溶液，同时开始滴加功能单体，直至完毕，期间控温55-60℃，反应4-5h，最后过滤，制备得到预乳化液；
步骤三：纤维原液色浆的制备：
向步骤二所得预乳化液缓慢加入己二酰肼水溶液，搅拌10-30min，用滤膜过滤去除滤渣，取滤液，即纤维原液色浆。
2.根据权利要求1所述的纤维原液色浆的制备方法，其特征在于，步骤二中，各原料用量质量份数如下：色粉15-25份，丙烯酸酯类单体84-90份，功能单体0.6-2.0份，反应型乳化剂4-5份，分散剂0.5-1.2份，缓冲剂1-4份，羟乙基甲基丙烯酸磷酸酯1-5份，去离子水82-92份。
3.根据权利要求1所述的纤维原液色浆的制备方法，其特征在于步骤二中，所述的丙烯酸酯类单体为甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸正丙酯、甲基丙烯酸正丁酯、丙烯酸羟乙酯、丙烯酸羟丙酯、丙烯酸月桂酯、甲氧基聚乙二醇甲基丙烯酸酯和丙烯酸-2-乙基己酯、甲基丙烯酸中的任意一种，或者任意几种的组合。
4.根据权利要求1所述的纤维原液色浆的制备方法，其特征在于步骤二中，所述的功能单体是双丙酮丙烯酰胺，所述的分散剂为TEGO750w。
5.根据权利要求1所述的纤维原液色浆的制备方法，其特征在于步骤二中反应型乳化剂为SR-10、SR-20、SOFTANOL 50、SOFTANOL 30中的任意一种，或者任意几种的组合。
6.根据权利要求1所述的纤维原液色浆的制备方法，其特征在于步骤二中所述的缓冲剂为碳酸氢钠。
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