CN102471591B - 后清洗试剂 - Google Patents

后清洗试剂 Download PDF

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CN102471591B
CN102471591B CN201080035145.5A CN201080035145A CN102471591B CN 102471591 B CN102471591 B CN 102471591B CN 201080035145 A CN201080035145 A CN 201080035145A CN 102471591 B CN102471591 B CN 102471591B
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dyeing
aqueous solution
dye
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CN102471591A (zh
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比安卡玛丽亚·普罗佐
贾思明·克罗耳
斯特凡诺·普兰多
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Huntsman Advanced Materials Switzerland GmbH
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Abstract

一种组合物包括(a)由至少一种烯属不饱和含氮杂环化合物通过聚合反应得到的均聚物或者共聚物和(b)聚乙烯亚胺，该组合物适合用于印花过的或者染过色的纺织材料的后清洗，尤其是用活性染料染过色的或者印花过的棉纤维。

Description

后清洗试剂
技术领域
本发明涉及含有衍生自N-乙烯基杂环的聚合物和聚乙烯亚胺的组合物，以及用于印花或染色的纺织材料的后清洗(afterclearing)方法。
背景技术
使用活性染料或直接染料(substantive dyes)染色或印花纤维素纤维，通常需要重复在高达98℃温度的水浴中的漂洗步骤。因此，部分染料被清除，该部分染料仅仅是松散地结合在纤维素的表面，而且会导致其他织物的污染。
出于经济和生态方面的原因，需要减少漂洗步骤的次数，并且降低漂洗水浴的温度。
美国专利No.6039768描述了把活性染料或直接染料固定在纤维素纤维材料上的方法，该方法包括在染色之前、之中和之后用含有诸如乙烯基咪唑/乙烯基吡咯烷酮共聚物之类的N-乙烯基-N-杂环化合物的共聚物溶液(liquor)处理纤维。然而，这种方法获得的染色坚牢度性能，不能符合最高的要求。
如今发现，可以通过对染色后的纤维素纤维用含有N-乙烯基-N-杂环的至少一种均聚物或者共聚物和至少一种聚乙烯亚胺的溶液进行后清洗，克服上述缺点。
发明内容
因此本发明涉及的组合物包括
(a)由至少一种烯属不饱和含氮杂环化合物通过聚合反应得到的均聚物或者共聚物和
(b)聚乙烯亚胺。
适合作为本发明组合物组分(a)的均聚物一般可以通过以合适的方式聚合烯属不饱和含氮杂环化合物来制备。
适用于制备组分(a)中均聚物或共聚物的烯属不饱和氮含杂环是，例如，吡咯，吡咯烷，吡啶，喹啉，异喹啉，嘌呤，吡唑，咪唑，三唑，四唑，吲嗪，哒嗪，嘧啶，吡嗪，吲哚，异吲哚，噁唑，噁唑烷酮，噁唑烷，吗啉，哌嗪，哌啶，异噁唑，噻唑，异噻唑，吲哚酚(indoxyle)，吲哚醌，二氧吲哚和乙内酰脲类以及它们的衍生物。
适合作为本发明组合物组分(a)的共聚物可以，在至少有一种能进一步共聚的单体存在的情况下，通过不饱和含氮杂环的聚合反应而制备。
能进一步共聚的单体可以是其它含氮杂环或其他不饱和化合物，例如，乙烯胺，烯丙基胺(ally amine)，丙烯酸，甲基丙烯酸，丙烯酸甲酯，甲基丙烯酸甲酯，醋酸乙烯酯，丙烯酰胺和甲基丙烯酰胺。
所述聚合物的制备可以通过本身已知的方法进行，例如，由离子或者，优选是基团，引发的相应单体的聚合反应，所述相应单体的聚合反应例如在溶液悬浮液或乳液中进行。这种聚合反应优选是在具有作为自由基链引发剂的过氧化氢、过硫酸盐或者诸如K2S2O8或偶氮二异丁腈之类的偶氮化合物的溶液中进行，该自由基链引发剂的含量可为占所用的单体重量的0.005-10wt％。
优选地，本发明组合物含有作为组分(a)的聚合物，该聚合物通过N-乙烯基吡咯烷酮的均聚反应或者N-乙烯基咪唑和N-乙烯基吡咯烷酮的共聚反应制得。
尤其优选的是，作为组分(a)的聚合物，特别是由60-100摩尔％，优选为70-90摩尔％的N-乙烯基吡咯烷酮和0-40摩尔％，优选是10-30摩尔％的N-乙烯基咪唑的共聚反应制得。
不取决于溶液的比例(liquor ratio)，本发明组分(a)的均聚物或共聚物的通常用量，按纺织材料重量计，为活性成分(active content)重量的0.01-4.0wt％，优选是0.02-2.0wt％，以及尤其优选，是0.8-2.5wt％。
适合用作组分(b)的聚乙烯亚胺同样可以根据已知的方法制备。
纯聚乙烯亚胺(PEI)的分子量MW(重均(weight average))为约200克/摩尔至约5,000,000克/摩尔，其由高活性的氮杂环丙烷在酸催化下开环加成聚合而成。
通过这种方法获得的支化聚合物，具有初级、二级和三级的氨基，并可以改性，例如，与羧酸或诸如氯化物、酯类、酸酐或酰胺之类的羧酸衍生物反应，于是形成部分酰氨化的PEI。
进一步改性的聚乙烯亚胺可以通过PEI与诸如环氧乙烷或环氧丙烷之类的环氧烷反应制备，从而产生部分乙氧基化或丙氧基化的聚乙烯亚胺。
这种纯的或改性过的PEI是有市售的，例如，名称Lupasol(由巴斯夫提供)或Epomin(由Nippon Shokubai提供)的商品。
优选地，本发明组合物含有改性的聚乙烯亚胺作为组分(b)，特别是部分酰胺化的或部分烷氧基化的聚乙烯亚胺。
在进一步优选的实施例中，本发明组合物包含作为组分(b)的部分酰胺化的聚乙烯亚胺，其可以通过聚乙烯亚胺与羧酸、酸酐、酯、氯化物或酰胺反应获得。
在进一步优选的实施例中，本发明组合物包含作为组分(b)的部分乙氧基化的聚乙烯亚胺，其可以通过聚乙烯亚胺与环氧乙烷反应获得。
不取决于溶液的比例，组分(b)的PEI的通常用量，按纺织材料的重量计，是活性成分重量的0.01-4.0wt％，优选是0.05-2.0wt％，以及尤其优选，是0.1-0.25wt％。
组分(a)和(b)含量的比率可在宽的范围内变化。优选地，组分(a)的含量占组分(a)+(b)总重量的20wt％-80wt％，更优选是30-70wt％，尤其优选是40％-60wt％。
与此相对应的是，组分(b)的含量占组分(a)+(b)总重量的20wt％-80wt％，更优选是30-70wt％，尤其优选是40-60wt％。
本发明进一步的目的是用于印花或染色的纺织材料的后清洗的方法，所述纺织材料优选是纤维素织物纤维材料，该方法包括使用含有上述组合物的水溶液(aqueous liquor)处理所述印花过的或染过色的纺织材料。
本发明方法的实施优选，先用传统方式对纤维素纤维材料染色，然后再用含有包括含量为如上所述的组分(a)及(b)的组合物的新配制的水溶液进行后清洗。然后，可以对染过色的纤维素纤维材料进行脱水，而不需要进行任何额外的漂洗工艺和传统的干燥。
纤维素纤维材料可以是，例如，再生纤维素、或优选是天然纤维素、经典的粘胶短纤维、粘胶丝、大麻纤维、亚麻纤维、黄麻纤维、或优选是棉花，和也可以是诸如棉/锦纶混纺或优选是棉/涤纶混纺之类的合成纤维与纤维混纺。
纺织品可以任何表现形式使用，例如以宽松层叠(loose stack)的形式，所述宽松层叠的形式全部或部分地由原生或再生的纤维素、纱、筒子纱、绞纱、梭织(wovens)、针织或毡构成。
染色的所述是采用直接染料，或优选是用活性染料，所有合适的传统的直接和活性染料，例如在Colour Index，第三版(1971年)及其标题为“直接染料”和“活性染料”的附录中所描述的那些染料。
所述染料的典型例子是，含有磺酸基团的单偶氮化合物、多偶氮(polyazo)化合物、金属络合偶氮(metal complexazo)化合物、蒽醌、酞菁、甲(formazane)或二噁嗪染料，如果是活性染料，其携带至少一个纤维活性基团，例如卤代三嗪基(halotriazinyl)或乙烯磺酰自由基。
用染料对纤维素纤维材料的染色可以通过传统方式进行，通过竭染(exhaust process)或诸如轧染或印花及随后的固色之类的两步法。
采用直接染料的染色优选是在中性到酸性pH环境下进行竭染。
采用活性染料的染色优选是在纤维上进行竭染或随后有固色步骤的轧染。固色可以通过传统方式实现，经典的是通过汽蒸法(steamprocess)或者热熔法(thermosol process)的热作用或者，优选通过冷轧堆方法实现，浸渍的纤维材料优选是在常温下保存。
之后，被染色的材料通常是用清水在高温下漂洗，例如在40-80℃，优选是在50-70℃。
后处理优选是由竭染法进行。浴比可在较大范围内选择，通常是1∶3-1∶40，优选是，1∶5-1∶20。
不需要特别的设备。它可以使用，例如，通常的染色设备，例如开放浴槽(open bath)，绞盘染槽，卷染机，或桨喷射(paddle jet)或循环设备。
该方法可以方便地在40-80℃温度范围内进行，并且优选是50-70℃温度范围内进行。处理时间通常是10-100分钟，并且优选是30-60分钟。所述溶液的pH值范围通常是8-13，并且优选是10-12。
除了包含组分(a)和(b)的组合物之外，所述溶液还可以包含其它传统的添加剂，通常是诸如氯化钠或硫酸钠之类的电解质、分散剂、润湿剂和消泡剂。
所述新型的方法提供了活性染料或直接染料对纤维素纤维材料进行染色或者印花，该方法得到的纤维素纤维材料具有出色的对湿处理的色牢度，例如耐水洗和水的色牢度以及耐氯的色牢度，并且对得色量、色泽或日晒色牢度特性无不利影响。
尽管各种传统的后处理方法几乎都在沸腾温度下进行的，但是要成功地进行根据本发明的后清洗方法，中等温度(60-80℃)就足够了。
此外，相较于传统的现有技术方法，漂洗步骤的数量能够得到减少。
下述例子更详细地阐述发明。
具体实施方式
实施例1
一块10克重的漂白棉经编针织物用蓝色活性染料(亨斯迈提供的Novacron Blue FN-R)在浴比为1∶10(2.0BZT)的条件下以竭染法进行染色。染过色的材料从染液中取出，并在60℃的水浴中漂洗10分钟。然后，染过色的棉经编织物片用新配制的水溶液在60℃处理10分钟，该新配制的水溶液包括含有由20mol％N-乙烯基咪唑和80mol％N-乙烯吡咯烷酮制备的10wt％N-乙烯基咪唑/N-乙烯吡咯烷酮-共聚物的2克/升的水溶液，以及含有50wt％的分子量(重均)MW为750,000g/mol的改性的支化PEI的pH值为11的0.5克/升的水溶液。随后，织物在水浴中漂洗三次，每次在60℃下持续10分钟。最后，该产品在含有0.5-2.0克/升乙酸的漂洗浴中在60℃下持续处理10分钟。残浴(residual bath)是无色的。
实施例2(对照)
一块10克重的漂白棉经编针织物用蓝色活性染料(亨斯迈提供的Novacron Blue FN-R)在浴比为1∶10(2.0BZT)的条件下以竭染法进行染色。染过色的材料从染液中取出，并在40℃的水浴中漂洗10分钟。然后，染过色的棉经编织物片在含有0.5-2.0克/升醋酸的漂洗浴中在70℃处理10分钟。随后，它用含有2克/升市售皂洗剂(改性聚(丙烯酸))的水溶液在98℃处理10分钟。此后，经编织物片在80℃水浴中漂洗10分钟，然后在60℃处理10分钟，以及最后在40℃处理10分钟。残浴是略带颜色的。
染过色的样本用标准方法(ISO 105 E01)进行一些色牢度性能的测试。结果列于表1。
表1：

Claims (4)

1.用于印花或染色的纺织材料的后清洗方法，该方法包括使用含有组合物的水溶液处理所述印花过的或染过色的纺织材料，该组合物包括：
(a)按重量计20-80％的N-乙烯基咪唑/N-乙烯基吡咯烷酮共聚物和
(b)按重量计20-80％的聚乙烯亚胺；
其中所述的％是基于(a)+(b)的总重量。
2.根据权利要求1所述的方法，其中，所述水溶液的温度是50-70℃。
3.根据权利要求1或者2所述的方法，其中，所述水溶液的pH值是10-12。
4.根据权利要求1或者2所述的方法，其中，所述纺织材料是用活性染料印花过的或者染过色的。
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