CN115595808B - 一种非水介质的活性染料棉织物染色方法 - Google Patents
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Abstract
一种非水介质的活性染料棉织物染色方法，以两种改性壳聚糖化合物溶解于DMSO/DMC中作为有机溶液介质；将活性染料溶解在水性聚氨酯乳液中得染液；将染液在高速搅拌条件下缓慢加入到有机溶液介质中，得到非水介质的活性染料液；之后进行染色吸附，以有机碱进行固色。本发明中活性染料溶解在少量的水性聚氨酯乳液中，与聚氨酯中氨基等形成氢键，提高结合牢度；之后加入到含改性壳聚糖化合物的有机溶液介质中，可以对棉织物进行有效染色，上染率高；染色工艺中条件温和，操作简单；在有机碱的存在下提高固色率，避免染色后的棉织物出现掉色现象，以有机溶液为介质，减少水的用量，有机溶液可回收，减少水污染。
Description
技术领域
本发明涉及纺织无水/少水印染技术领域，具体涉及一种非水介质的活性染料棉织物染色方法。
背景技术
纺织工业印染技术已相当成熟，染色工业通常是在水性介质中进行。然而，以水为介质的染色方法需要消耗大量的水资源，且染色后排放的废水中含难降解的化学污染物，严重影响了生态环境。为推进可持续发展理念，近几年避免使用水作为溶剂或减少水的用量的染色技术也正在研究当中。申请人在前期的工作中，以壳聚糖作为基础材料，通过对其改性获得匀染剂，在涤纶织物的印染过程中有效解决了花色、上色不均匀的问题，印染后的溶剂废水可循环使用，一定程度上满足了绿色污染的环保要求。但是，对织物的固色效果仍有待提高，且用于棉织物染色时，还需考虑到棉织物相较于涤纶织物而言，染料与棉纤维的亲和力小，因而，棉织物的上染率低，上色难。
发明内容
针对现有技术中的不足之处，本发明提供了一种非水介质的活性染料棉织物染色方法，减少印染用水量，减轻环境污染，同时满足棉织物的高染色率。
为实现上述目的，本发明提供如下技术方案：
一种非水介质的活性染料棉织物染色方法，包括如下步骤：
S1：将改性壳聚糖化合物Ⅰ和改性壳聚糖化合物Ⅱ溶解于DMSO/DMC中获得有机溶液介质；
S2：在固含量20～25％的水性聚氨酯乳液中溶解活性染料得0.5～1g/L染液；
S3：将三乙烯二胺溶解在正辛烷中得到有机碱溶液；
S3：将染液在高速搅拌条件下缓慢加入到有机溶液介质中，得到非水介质的活性染料液；将经DMSO溶胀后的棉织物浸没在活性染料液中，浴比范围1:40～1:20，于60～70℃振荡1～3h进行染色吸附；
S4：将吸附完成的棉织物取出，直接浸没在S1的有机溶液介质中；在搅拌条件下加入有机碱溶液，于60～70℃振荡1～2h；
S5：染色结束后取出棉织物，用DMSO和DMC分别清洗2-3次，后水洗，干燥；其中，
所述改性壳聚糖化合物Ⅰ为
所述改性壳聚糖化合物Ⅱ为n为8～12的整数。
进一步地，所述改性壳聚糖化合物Ⅰ的制备过程如下：
首先将壳聚糖与十二烷基硫酸钠进行静电复合保护氨基，之后置于乙二醇甲醚溶剂中，在氢氧化钠和碘化钾的催化作用下与环氧氯丙烷进行氯取代反应；反应完成后置于DMSO溶剂中，N2保护下缓慢滴加溶解有1-萘乙胺-4-磺酸钠的DMSO溶液，80℃下反应4～6h，反应完成后，旋蒸以除去溶剂，之后在Tris/甲醇溶液中沉淀，水洗后用无水乙醚洗涤，之后真空干燥即得分散剂。
进一步地，所述改性壳聚糖化合物Ⅱ的制备过程如下：N-羧甲基壳聚糖与烷基聚氧乙烯醚一同加入到反应瓶中，向其中加入溶剂甲苯以及阻聚剂对苯二酚和催化剂对甲苯磺酸，升温至120℃，搅拌反应3～4h；旋蒸除去溶剂，经提纯后得到聚氧乙烯醚接枝壳聚糖。
进一步地，所述改性壳聚糖化合物Ⅰ和改性壳聚糖化合物Ⅱ的质量比为1:1～2，DMSO/DMC的体积比为10/90，混合物在DMSO/DMC的浓度为1～2g/L。
进一步地，所述染液与有机溶液介质的体积比为0.2～0.5:1。
进一步地，所述有机碱溶液的浓度范围10～30g/L。
进一步地，步骤S4中，浴比范围1:40～1:20，有机碱溶液与有机溶液介质的体积比值为0.05～0.08。
本案中选用天然高分子材料壳聚糖作为基础材料，通过对其改性获得了改性壳聚糖化合物Ⅰ和改性壳聚糖化合物Ⅱ。壳聚糖化合物Ⅰ中含有丰富的氨基官能团，并连接有萘磺酸，具有一定的分散性能，相较于小分子的分散剂，其分散吸附性能更高，并且通过结合萘磺酸，增大空间位阻效应，避免分散剂从织物纤维表面解吸后重新聚集，而其本身的羟基和氨基官能团与活性染料中的基团结合使染料与织物纤维相互交联，提高色牢度。
改性壳聚糖化合物Ⅱ同样以N-羧甲基壳聚糖为基础原料，其在纺织印染领域具有广泛的应用，可起到固色的效果；结构式中含有丰富的聚氧乙烯醚结构，EO能与染料分子通过氢键作用很好地结合，提高色牢度。
二者混合溶于有机溶剂中形成有机溶液介质，将溶解于聚氨酯乳液中的染料与之混合得到非水介质的染料色浆，水性聚氨酯与棉纤维发生交联反应；通过壳聚糖作为架桥，壳聚糖中丰富的官能团使染料粒子在色浆中分散均匀，棉织物浸没在色浆中时，染料粒子均匀吸附在织物纤维表面，染料条件温和，染色均匀，上染率高。选择有机碱代替无机碱，在有机溶液介质中能更有效地提高固色率。
本发明的有益效果是：活性染料溶解在少量的水性聚氨酯乳液中，与聚氨酯中氨基等形成氢键，提高结合牢度；之后加入到含改性壳聚糖化合物的有机溶液介质中，可以对棉织物进行有效染色，上染率高；染色工艺中条件温和，操作简单；在有机碱的存在下提高固色率，避免染色后的棉织物出现掉色现象，以有机溶液为介质，减少水的用量，有机溶液可回收，减少水污染。
具体实施方式
下面对本发明的技术方案进行清楚、完整地描述，显然，所描述的实施例是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
此外，下面所描述的本发明不同实施方式中所涉及的技术特征只要彼此之间未构成冲突就可以相互结合。
一种非水介质的活性染料棉织物染色方法，包括如下步骤：
S1：将质量比为1:1～2的改性壳聚糖化合物Ⅰ和改性壳聚糖化合物Ⅱ溶解于DMSO/DMC(v/v＝10/90)中获得有1～2g/L机溶液介质；
改性壳聚糖化合物Ⅰ的制备过程如下：
A、称取2g壳聚糖、3g SDS，分别溶于200ml 2％醋酸溶液，完全溶剂后，将SDS溶液缓慢滴加到壳聚糖溶液中，产生大量白色絮凝沉淀，离心，依次用去离子水、丙酮洗涤真空干燥，得到氨基保护的壳聚糖；
B、将步骤A中的产物置于乙二醇甲醚溶剂中，在氢氧化钠和碘化钾的催化作用下与环氧氯丙烷进行氯取代反应；
C、将步骤B中的产物0.5g置于DMSO溶剂中，N2保护下缓慢滴加溶解有1g 1-萘乙胺-4-磺酸钠的DMSO溶液，80℃下反应4～6h，反应完成后，旋蒸以除去溶剂，之后在Tris/甲醇溶液中沉淀，水洗后用无水乙醚洗涤，之后真空干燥即得。
改性壳聚糖化合物Ⅱ的制备过程如下：N-羧甲基壳聚糖与十二烷基聚氧乙烯醚按照1.2:1的质量比一同加入到反应瓶中，向其中加入溶剂甲苯以及阻聚剂对苯二酚和催化剂对甲苯磺酸，升温至120℃，搅拌反应3～4h；旋蒸除去溶剂，经提纯后得到。
S2：在固含量20～25％的水性聚氨酯乳液中溶解活性染料得0.5～1g/L染液；
S3：将三乙烯二胺溶解在正辛烷中得到10～30g/L有机碱溶液；
S3：按体积比0.2～0.5:1将染液在高速搅拌条件下缓慢加入到有机溶液介质中，得到非水介质的活性染料液；将经DMSO溶胀后的棉织物浸没在活性染料液中，浴比范围1:40～1:20，于60～70℃振荡1～3h进行染色吸附；
S4：将吸附完成的棉织物取出，直接浸没在S1的有机溶液介质中，浴比范围1:40～1:20；在搅拌条件下加入有机碱溶液，于60～70℃振荡1～2h；有机碱溶液与有机溶液介质的体积比值为0.05～0.08。
S5：染色结束后取出棉织物，用DMSO和DMC分别清洗2-3次，后水洗，干燥。
实施例1：
S1：将质量比为1:1的改性壳聚糖化合物Ⅰ和改性壳聚糖化合物Ⅱ溶解于DMSO/DMC(v/v＝10/90)中获得有1g/L机溶液介质；
S2：在固含量25％的水性聚氨酯乳液(数均分子量为5000g/mol，购自广州享缌克新材料有限公司)中溶解活性染料(活性蓝)得0.5g/L染液；
S3：将三乙烯二胺溶解在正辛烷中得到10g/L有机碱溶液；
S3：按体积比0.3:1将染液在高速搅拌条件下缓慢加入到有机溶液介质中，得到非水介质的活性染料液；将经DMSO溶胀后的棉织物浸没在活性染料液中，浴比范围1:40，于60～70℃振荡1～3h进行染色吸附；
S4：将吸附完成的棉织物取出，直接浸没在S1的有机溶液介质中，浴比范围1:20；在搅拌条件下加入有机碱溶液，于60～70℃振荡1～2h；有机碱溶液与有机溶液介质的体积比值为0.08。
S5：染色结束后取出棉织物，用DMSO和DMC分别清洗2-3次，后水洗，干燥。
实施例2：
S1：将质量比为1:1.5的改性壳聚糖化合物Ⅰ和改性壳聚糖化合物Ⅱ溶解于DMSO/DMC(v/v＝10/90)中获得有1.5g/L机溶液介质；
S2：在固含量25％的水性聚氨酯乳液(数均分子量为5000g/mol，购自广州享缌克新材料有限公司)中溶解活性染料(活性蓝)得0.7g/L染液；
S3：将三乙烯二胺溶解在正辛烷中得到20g/L有机碱溶液；
S3：按体积比0.5:1将染液在高速搅拌条件下缓慢加入到有机溶液介质中，得到非水介质的活性染料液；将经DMSO溶胀后的棉织物浸没在活性染料液中，浴比范围1:30，于60～70℃振荡1～3h进行染色吸附；
S4：将吸附完成的棉织物取出，直接浸没在S1的有机溶液介质中，浴比范围1:20；在搅拌条件下加入有机碱溶液，于60～70℃振荡1～2h；有机碱溶液与有机溶液介质的体积比值为0.06。
S5：染色结束后取出棉织物，用DMSO和DMC分别清洗2-3次，后水洗，干燥。
实施例3：
S1：将质量比为1:2的改性壳聚糖化合物Ⅰ和改性壳聚糖化合物Ⅱ溶解于DMSO/DMC(v/v＝10/90)中获得有2g/L机溶液介质；
S2：在固含量25％的水性聚氨酯乳液(数均分子量为5000g/mol，购自广州享缌克新材料有限公司)中溶解活性染料(活性蓝)得0.8g/L染液；
S3：将三乙烯二胺溶解在正辛烷中得到20g/L有机碱溶液；
S3：按体积比0.5:1将染液在高速搅拌条件下缓慢加入到有机溶液介质中，得到非水介质的活性染料液；将经DMSO溶胀后的棉织物浸没在活性染料液中，浴比范围1:30，于60～70℃振荡1～3h进行染色吸附；
S4：将吸附完成的棉织物取出，直接浸没在S1的有机溶液介质中，浴比范围1:30；在搅拌条件下加入有机碱溶液，于60～70℃振荡1～2h；有机碱溶液与有机溶液介质的体积比值为0.08。
S5：染色结束后取出棉织物，用DMSO和DMC分别清洗2-3次，后水洗，干燥。
对比例1：
S1：将质量比为1:2的改性壳聚糖化合物Ⅰ和改性壳聚糖化合物Ⅱ溶解于DMSO/DMC(v/v＝10/90)中获得有2g/L机溶液介质；
S2：在水中溶解活性染料(活性蓝)得0.8g/L染液；
S3：将三乙烯二胺溶解在正辛烷中得到20g/L有机碱溶液；
S3：按体积比0.5:1将染液在高速搅拌条件下缓慢加入到有机溶液介质中，得到非水介质的活性染料液；将经DMSO溶胀后的棉织物浸没在活性染料液中，浴比范围1:30，于60～70℃振荡1～3h进行染色吸附；
S4：将吸附完成的棉织物取出，直接浸没在S1的有机溶液介质中，浴比范围1:30；在搅拌条件下加入有机碱溶液，于60～70℃振荡1～2h；有机碱溶液与有机溶液介质的体积比值为0.08。
S5：染色结束后取出棉织物，用DMSO和DMC分别清洗2-3次，后水洗，干燥。
对比例2：
S1：配制DMSO/DMC(v/v＝10/90)有机溶液介质；
S2：在水中溶解活性染料(活性蓝)得0.8g/L染液；
S3：将三乙烯二胺溶解在正辛烷中得到20g/L有机碱溶液；
S3：按体积比0.5:1将染液在高速搅拌条件下缓慢加入到有机溶液介质中，得到非水介质的活性染料液；将经DMSO溶胀后的棉织物浸没在活性染料液中，浴比范围1:30，于60～70℃振荡1～3h进行染色吸附；
S4：将吸附完成的棉织物取出，直接浸没在S1的有机溶液介质中，浴比范围1:30；在搅拌条件下加入有机碱溶液，于60～70℃振荡1～2h；有机碱溶液与有机溶液介质的体积比值为0.08。
S5：染色结束后取出棉织物，用DMSO和DMC分别清洗2-3次，后水洗，干燥。
上染率：(C0-C1)/C0×100％，根据分光光度计测色试样染色前浓度C0和染色后浓度C0；
固色率：酸溶解法测定，根据分光光度计测定试验吸光度计算织物表面酸溶解前后固着的染料量；
摩擦色牢度：参照GB-T3920-2008进行摩擦测试；
日晒牢度：按照GB-T8427-2008评定标准测试织物的日晒牢度；
耐洗牢度：按照GB-T3921-2008标准进行试验测试；
织物手感：以五人为一组，对固色前后的染色织物进行触摸评级，数值越大表示手感越好。上述数据记录在表1中。
表1
从上表中可以看出本案提供的非水介质的的活性染料棉织物染色方法具有较高的上染率和固色率，摩擦色牢度和耐洗牢度高，手感好。对比例1将染料直接溶于水中与有机溶液介质混合，缺少聚氨酯的氢键作用力，各项性能有所下降；对比例2则无法完成染色工艺，染料在有机溶剂中聚集，无法均匀吸附在棉织物上。
尽管本发明的实施方案已公开如上，但其并不仅仅限于说明书和实施方式中所列运用，它完全可以被适用于各种适合本发明的领域，对于熟悉本领域的人员而言，可容易地实现另外的修改，因此在不背离权利要求及等同范围所限定的一般概念下，本发明并不限于特定的细节。
Claims (5)
1.一种非水介质的活性染料棉织物染色方法，其特征在于，包括如下步骤：
S1：将改性壳聚糖化合物Ⅰ和改性壳聚糖化合物Ⅱ溶解于DMSO/DMC中获得有机溶液介质；
S2：在固含量20～25％的水性聚氨酯乳液中溶解活性染料得0.5～1g/L染液；
S3：将三乙烯二胺溶解在正辛烷中得到有机碱溶液；
S3：将染液在高速搅拌条件下缓慢加入到有机溶液介质中，得到非水介质的活性染料液；将经DMSO溶胀后的棉织物浸没在活性染料液中，浴比范围1:40～1:20，于60～70℃振荡1～3h进行染色吸附；所述染液与有机溶液介质的体积比为0.2～0.5:1；
S4：将吸附完成的棉织物取出，直接浸没在S1的有机溶液介质中；在搅拌条件下加入有机碱溶液，于60～70℃振荡1～2h；浴比范围1:40～1:20，有机碱溶液与有机溶液介质的体积比值为0.05～0.08；
S5：染色结束后取出棉织物，用DMSO和DMC分别清洗2-3次，后水洗，干燥；其中，
所述改性壳聚糖化合物Ⅰ为
所述改性壳聚糖化合物Ⅱ为n为8～12的整数。
2.如权利要求1所述的非水介质的活性染料棉织物染色方法，其特征在于，所述改性壳聚糖化合物Ⅰ的制备过程如下：
首先将壳聚糖与十二烷基硫酸钠进行静电复合保护氨基，之后置于乙二醇甲醚溶剂中，在氢氧化钠和碘化钾的催化作用下与环氧氯丙烷进行氯取代反应；反应完成后置于DMSO溶剂中，N2保护下缓慢滴加溶解有1-萘乙胺-4-磺酸钠的DMSO溶液，80℃下反应4～6h，反应完成后，旋蒸以除去溶剂，之后在Tris/甲醇溶液中沉淀，水洗后用无水乙醚洗涤，之后真空干燥即得分散剂。
3.如权利要求1所述的非水介质的活性染料棉织物染色方法，其特征在于，所述改性壳聚糖化合物Ⅱ的制备过程如下：N-羧甲基壳聚糖与烷基聚氧乙烯醚一同加入到反应瓶中，向其中加入溶剂甲苯以及阻聚剂对苯二酚和催化剂对甲苯磺酸，升温至120℃，搅拌反应3～4h；旋蒸除去溶剂，经提纯后得到聚氧乙烯醚接枝壳聚糖。
4.如权利要求1所述的非水介质的活性染料棉织物染色方法，其特征在于，所述改性壳聚糖化合物Ⅰ和改性壳聚糖化合物Ⅱ的质量比为1:1～2，DMSO/DMC的体积比为10/90，混合物在DMSO/DMC的浓度为1～2g/L。
5.如权利要求1所述的非水介质的活性染料棉织物染色方法，其特征在于，所述有机碱溶液的浓度范围10～30g/L。
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| 廖波 ; 张宾 ; 于潘芬 ; 杜小名 ; 于晓涵 ; 柳荣展 ; .壳聚糖聚醚衍生物在棉活性无盐染色中的应用.印染.2017,(第06期),6-9. * |
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