CN106478745B - 一种无甲醛水性交联剂及其制备方法和对织物的整理工艺 - Google Patents

一种无甲醛水性交联剂及其制备方法和对织物的整理工艺 Download PDF

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CN106478745B
CN106478745B CN201610899567.6A CN201610899567A CN106478745B CN 106478745 B CN106478745 B CN 106478745B CN 201610899567 A CN201610899567 A CN 201610899567A CN 106478745 B CN106478745 B CN 106478745B
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高介平
高辛格
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Abstract

本发明属于纤维素织物无甲醛交联防缩、抗皱、免烫技术领域，特别涉及一种无甲醛水性交联剂及其制备方法和对织物的整理工艺。通过两种新的水性交联剂，并选用水溶性多元羧酸酯为交联催化剂，分二步对纤维素织物处理，使纤维素织物无甲醛免烫整理技术达到一个新的高度，即在织物的强力不受损伤的同时，获得了高等级无甲醛交联防缩、抗皱、免烫整理性能，特别是经过处理后纤维素织物的湿回复角有了明显的提高。

Description

一种无甲醛水性交联剂及其制备方法和对织物的整理工艺
技术领域
本发明属于纤维素织物无甲醛交联防缩、抗皱、免烫技术领域，特别涉及一种无甲醛水性交联剂及其制备方法和对织物的整理工艺。
背景技术
纤维素(棉、麻、粘胶、莫代尔、天丝)材料制作的纺织品(服装、家纺等)具有亲肤、吸湿透气等优异舒适性能，为广大消费者所青睐，但在洗涤后会产生缩水、起皱、变形等尺寸不稳定的现象，长期以来如何使该类纺织品尺寸稳定，不断满足广大消费者不断提升的要求，是纺织产业所关注的重大课题。
目前纺织业中的乙二醛及其各类衍生物作为无甲醛免烫整理交联剂处理纤维素织物时主要面临如下几个问题：织物黄变严重、整理效果不理想、强力下降严重。
黄变的主要原因是由于乙二醛其各类衍生物与纤维素的羟基交联后，会残存大量的半缩醛羟基，在水洗前的高温热处理时会发生脱水反应生成不饱和碳碳双键或发生羟基氧化，从而变成淡黄色的化合物。
而整理效果不理想与强力下降严重始终是一对难以兼顾的矛盾：因为目前交联反应采用的催化剂为较高浓度的盐酸(HCl)、MgCl2·6H2O(六水氯化镁)、(NH4)2HPO4(磷酸氢二铵)、NH4NO3(硝酸铵)等Lewis酸(路易斯酸)，整理剂溶液的pH值一般都小于4，在该强酸性条件下纤维素大分子链容易吸酸而降解断裂，造成纤维素织物降强严重；而为了控制强力不过度下降，减少添加量又会使交联反应不充分，免烫效果差、半缩醛羟基残留多，整理效果不理想。
发明内容
本发明为解决上述技术问题首先提供了一种无甲醛水性交联剂，记作交联剂Ⅰ，成分包括
本发明还提供了一种上述交联剂Ⅰ的制备工艺：
将多羟基醛类单糖溶解于乙二醛溶液中后，先加入酸催化剂蒸馏脱水发生半缩醛化反应，再加入多元醇继续蒸馏脱水使多元醇与多羟基醛类单糖的醛基缩醛化，最后中和酸催化剂并冷却(使中和反应生成的氯盐)结晶，过滤，得到具有缩醛和半缩醛结构的混合物即无甲醛交联剂Ⅰ，
其中，多羟基醛类单糖为开链式葡萄糖，
酸催化剂为盐酸，反应后中和酸催化剂采用氢氧化钠，
多元醇为乙二醇、丙三醇、二乙二醇等，
上述无甲醛交联剂Ⅰ制备方法的具体反应式如下(多元醇选择乙二醇)：
上述反应中，葡萄糖结构上醛基缩醛化成环的过程中可以形成环与环之间的互穿(如上述反应产物的两分子互穿结构)，有利于增加弹性；并且由于葡萄糖羟基是有固定分布方式的，上述产物的其他环结构之间由于空间位阻较大的原因，发生互穿的可能性很小，因此所得产物主要还是以上述两种成分为主，且产物中，未发生互穿的成分与发生互穿的成分之间质量比为80～85：15～20。
本发明提供了另一种水性交联剂，记作交联剂Ⅱ，该交联剂Ⅱ的分子结构式为：
本发明还提供了一种上述交联剂Ⅱ的制备方法：
(1)将2，4-二氨基苯磺酸钠和氢氧化钠溶解于水，并加三聚氯嗪反应至体系呈透明状，
其中，2，4-二氨基苯磺酸钠、氢氧化钠、三聚氯嗪的用量摩尔比优选1：2：2，
加入三聚氯嗪后的反应温度控制为20℃-40℃，
反应结束后，体系中所生成中间产物的分子结构式为：
(2)向步骤(1)所得的体系中加入氢氧化钠、3-吡啶甲酸反应至体系再次呈透明状，调整体系为中性，得到交联剂Ⅱ，
其中，所加入的氢氧化钠、3-吡啶甲酸与步骤(1)所得的体系中中间产物的摩尔比为4：2：1，
采用缓冲溶液调节体系的pH值为7至8，所得的交联剂Ⅱ在50℃以下能长期保持稳定。
本发明提供了一种对织物的整理工艺：
在交联剂的水溶液中加入有机多元羧酸水溶性酯作为交联催化剂，对纤维素织物作浸轧处理，再在低温(75℃-85℃)条件下烘焙至织物保持5％-8％的含水率，然后在常温(25℃-35℃)下用塑料膜包覆堆置1-5小时，最后水洗、160℃-170℃烘干，可使纤维素织物获得良好的防缩、抗皱、免烫性能，
其中，交联剂为上述的交联剂Ⅰ，且交联剂Ⅰ与有机多元羧酸水溶性酯交联催化剂的用量质量比为4～8：1，
上述有机多元羧酸水溶性酯由水溶性多元醇与多元羧酸所合成，其中水溶性多元醇为乙二醇、丙三醇、二乙二醇中的一种或几种的组合，多元羧酸为柠檬酸、乙二酸、丙二酸、丁二酸、苹果酸、酒石酸、丁烷四羧酸中的一种或几种的组合，
该有机多元羧酸水溶性酯可与水以任意比例混溶后呈均匀透明溶液，且所得的质量浓度为1％-2％的水溶液的pH值可稳定在5-7，从而确保纤维素织物在浸轧交联剂Ⅰ和该交联催化剂时，以及织物在后续75℃-85℃热处理时，织物中的pH值始终大于5，使纤维素织物的强力损伤较小；且由于交联催化剂上的羟基活性远低于交联剂Ⅰ上的半缩醛羟基，因此其本身基本不参与醚化反应，
另外，上述交联剂Ⅰ在水溶液中的浓度为50g/L-300g/L。
本发明还提供了一种上述交联剂Ⅱ对织物的整理工艺：
在交联剂Ⅱ的水溶液中加入氧化聚乙烯蜡乳液、聚氨酯乳液、含氨基和聚醚基的有机硅氧烷乳液、抗泳移剂并混合均匀，将空白的或经过上述交联剂Ⅰ处理后的纤维素织物浸轧于该混合液中，再对织物进行95℃×30秒预烘、170℃×90秒烘焙，充分水洗后在160℃-170℃烘干，可使纤维素织物获得更加优异的防缩、抗皱、免烫性能，并且纤维素织物的强力会得到有效提升，
其中，交联剂Ⅱ在水溶液中的浓度为50g/L-250g/L，
另外，氧化聚乙烯蜡乳液、聚氨酯乳液、含氨基和聚醚基的有机硅氧烷乳液、抗泳移剂(又称“防泳移剂”)的固含量依次为20％、30％、30％、3％，
其中，抗泳移剂选自海藻酸钠。
本发明的有益效果在于：
本发明中通过两种新的水性交联剂，并选用水溶性多元羧酸酯为交联催化剂，分二步对纤维素织物处理，使纤维素织物无甲醛免烫整理技术达到一个新的高度，即在织物的强力不受损伤的同时，获得了高等级无甲醛交联防缩、抗皱、免烫整理性能，特别是经过处理后纤维素织物的湿回复角(在行业内折皱回复角虽然有两种：干回复角、湿回复角，但是所谓“免烫”是指织物洗涤受湿以后，不需要熨烫，洗涤褶皱再晾干时就能恢复平整，所以行业内判断是否具有免烫功效需要参考湿回复角的数据，一般湿回复角达到240°以上，即具有免烫功能)有了明显的提高；
交联剂Ⅰ消除了醛基，避免了后续整理过程中半缩醛羟基的产生而导致的织物变黄的现象，且自身基于特殊分子结构设计，具有优秀的交联性能，活化了其与纤维素羟基的醚化反应性(相比于本专利交联剂Ⅰ上的羟基，普通羟基之间醚化反应困难得多，例如两分子乙醇脱水成醚需要145℃下浓硫酸催化才能进行)，使得交联反应后残留羟基大大减少，一方面提高了交联效率和免烫效果，另一方面采取在较低温度(75℃-85℃)热处理，在织物含水5％-8％的含湿条件下堆置交联反应，确保了织物不发生黄变；
本发明以多元羧酸的水溶性酯(如乙二醇柠檬酸三酯)为催化剂，催化交联充分的同时使交联反应的pH值条件控制在5以上，保证了织物的强力损伤较小；
本发明设计合成了水溶性交联剂Ⅱ，借助其远距离交联特征，让纤维素的羟基通过化学键结合氧化聚乙烯蜡乳液、聚氨酯乳液、含氨基和聚醚基的有机硅氧烷乳液、抗泳移剂中的有机高分子材料，使纤维素织物得到强力补偿，并进一步提高织物的弹性，使得织物抗皱防缩、免烫性能进一步提高的同时，织物的撕破强力也得到提升。
具体实施方式
实施例1
交联剂Ⅰ的制备：
将180g葡萄糖溶解于250g溶质质量分数40％的工业级乙二醛溶液中后，先加入0.8ml溶质质量分数36.5％的浓盐酸催化剂，加热回流1.5小时发生半缩醛化反应，然后控制温度在102℃～108℃蒸馏脱水至无馏出份；再加入62g乙二醇后缓慢升温至110℃并保温至无馏出物使乙二醇与葡萄糖的醛基缩醛化，最后加入氢氧化钠中和盐酸并冷却结晶，过滤，得到多种缩醛和半缩醛的混合物，即交联剂Ⅰ。
实施例2
交联剂Ⅱ的制备：
(1)将2，4-二氨基苯磺酸钠和氢氧化钠完全溶解于水，并加三聚氯嗪于35℃反应至体系呈透明状，
2，4-二氨基苯磺酸钠、氢氧化钠、三聚氯嗪的用量摩尔比为1：2：2；
(2)向步骤(1)所得的体系中加入氢氧化钠、3-吡啶甲酸并于47℃-50℃下反应至体系再次呈透明状，采用中性缓冲溶液调节体系的pH值为7，得到交联剂Ⅱ的水溶液，并于50℃以下保存，
其中，所加入的氢氧化钠、3-吡啶甲酸与步骤(1)所得的体系中纯净中间产物的摩尔比为4：2：1。
纤维织物的预处理：
将经过退浆、煮练、漂白、丝光前处理的棉织物进行液氨处理，得到高支高密棉府绸布(经×纬组织规格：纱支80s×80s,密度685×512根/10cm)。对预处理后的织物进行室温条件下回潮测试(结果见表一)。
实施例3
将经过上述预处理的棉府绸布浸扎于实施例1所制备的交联剂Ⅰ的水溶液中(其中，交联剂Ⅰ80g/L，催化剂乙二醇柠檬酸三酯15g/L，pH值为6)，轧余率78％，再于85℃下烘干60秒使织物此时的含湿率为7％，然后在30℃下用塑料膜包覆堆置3小时，最后充分水洗并于160℃烘干，
实验过程中多次对浸扎时的溶液、布面，85℃烘干过程中的布面，堆置时的布面，以及最终160℃烘干时的布面进行检测，测得pH值都在6-7范围内，取样经冷却后室温条件下回潮测试(结果见表一)。
实施例4
将经过实施例3交联处理的棉府绸布浸扎于实施例2所制备的交联剂Ⅱ的水溶液中(其中，交联剂Ⅱ100g/L、固含量20％的氧化聚乙烯蜡乳液20g/L、固含量30％的聚氨酯乳液15g/L、固含量30％的含氨基和聚醚基的有机硅氧烷乳液20g/L、固含量3％的海藻酸钠抗泳移剂
2g/L)，轧余率75％，再进入多级连续烘箱进行95℃×30秒的预烘和170℃×90秒的焙烘，然后充分水洗并于160℃下烘干，取样经冷却后室温条件下回潮测试(结果见表一)。
对比实施例1
将实施例3中的催化剂“乙二醇柠檬酸三酯”替换为3倍摩尔数的醋酸，其余操作不变。
经处理后对织物室温条件下回潮测试(结果见表一)。
表1
(注：由于采用吸光光度法检测甲醛含量的下限为20ppm，所以世界各检测组织和制订的相关标准规定，甲醛含量低于20ppm的纺织品属于无甲醛类纺织品)

Claims (4)

1.一种水性交联剂，记作交联剂Ⅱ，其特征在于：所述交联剂Ⅱ的分子结构式为
2.一种如权利要求1所述的水性交联剂的制备方法，其特征在于：所述的制备方法为，
(1)将2，4-二氨基苯磺酸钠和氢氧化钠溶解于水，并加三聚氯嗪反应至体系呈透明状；
(2)向步骤(1)所得的体系中加入氢氧化钠、3-吡啶甲酸反应至体系再次呈透明状，调整体系为中性，得到交联剂Ⅱ。
3.一种基于权利要求1所述的水性交联剂对织物的整理工艺，其特征在于：所述的整理工艺包括，
在交联剂Ⅱ的水溶液中加入氧化聚乙烯蜡乳液、聚氨酯乳液、含氨基和聚醚基的有机硅氧烷乳液、抗泳移剂并混合均匀，将空白的或经过整理后的纤维素织物浸轧于该混合液中，再对织物进行预烘、烘焙、充分水洗、烘干。
4.如权利要求3所述的水性交联剂对织物的整理工艺，其特征在于：所述的经过整理后的纤维素织物的整理工艺包括，
在交联剂的水溶液中加入有机多元羧酸水溶性酯作为交联催化剂，对纤维素织物于上述水溶液中进行浸轧处理，再在低温条件下烘焙，然后在常温下堆置，最后水洗、烘干。
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