CN111636223B - 一种环境友好的棉织物用活性染料低温无盐染色方法 - Google Patents
一种环境友好的棉织物用活性染料低温无盐染色方法 Download PDFInfo
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Abstract
本发明涉及了一种环境友好的棉织物用活性染料低温无盐染色方法，包括阳离子聚合物的合成，棉织物的改性处理、染色以及染料废水的絮凝等步骤。用二甲基二烯丙基氯化铵和烯丙基缩水甘油醚在过硫酸钾做引发剂的条件下合成阳离子聚合物，将棉织物浸入一定浓度的阳离子聚合物水溶液中改性处理。经改性后的棉织物可用活性染料在低温、无盐的条件下染色，提高了染料的上染率和固色率，且匀染性良好。改性棉织物的水洗液与染色残液和皂洗液混合，利用溶液里的少量阳离子聚合物将染色废水中的残余染料絮凝下来，大大减少了印染废水的排放，有利于实际生产和环境保护。
Description
技术领域
本发明属棉织物活性染料无盐染色领域。
背景技术
活性染料在染色过程中能与棉纤维形成共价键，具备优异的染色牢度，且色泽鲜艳，色谱齐全，成本低廉，应用非常广泛，已成为棉纤维纺织品染色最重要的一类染料。活性染料包括活性基团、亲水基团和染料母体三部分，其中亲水基团一般由磺酸钠盐、羟基、氨基等组成，而磺酸基对染料的亲水性有重大贡献。磺酸基团的存在有助于活性染料在水中溶解，使染色过程可以在水溶液中进行；然而，染料母体因磺酸钠盐的离解作用带上负电荷，不仅降低了对纤维负离子的结合能力，还容易被水合化形成水合物并聚集成胶团结构，使染料负离子的有效浓度下降，从而导致活性染料染色棉纤维的上染率和固色率都比较低。为解决这一问题，在染色过程中通常加入大量的无机盐来促染，但印染过程中产生的高含盐量的废水难以处理，对环境危害极大，如何实现活性染料低盐甚至无盐染色，是亟待解决的问题。
目前提高活性染料利用率，减少染色过程中无机盐使用的途径主要有：
(1)开发新型活性染料：双活性基活性染料及多官能活性染料，这类染料分子中有两个甚至多个活性基团，可有效的将活性染料利用率从50—60％提高到70—80％；阳离子活性染料可以消除染色过程中对电解质的需求，提高了染料对纤维的亲和力，可以实现无盐染色。
(2)优化染色工艺：减小染液体积可增大染液中染料和无机盐的浓度，因此减小浴比是提高染料利用率和减少无机盐使用的可行方法；轧染技术，尤其是冷-轧-堆染色工艺，不仅减少了染料和无机盐的使用，更降低了能量消耗，经济性很高。此外，固色聚合技术，胶束染色技术等新兴染色工艺也已经被研究报道。
(3)使用可生物降解的有机化合物代替无机盐：使用镁基有机化合物的混合体系在活性染料棉织物染色过程中代替无机盐，可有效防止含盐染料废水的排放；有机阳离子表面活性剂和有机酸的钠盐也可作为氯化钠和硫酸钠的替代品，不仅避免了无机盐的使用，还提高了活性染料利用率。
(4)对棉纤维进行化学改性：用含阳离子的基团在染色前对棉纤维进行预处理，可以在纤维表面引入正电荷，从而增强了纤维对活性染料的亲和力。这种方法不仅可以避免无机盐的使用，而且极大的提高了染色效率和活性染料利用率。用于棉纤维改性的阳离子试剂通常可分为两类：第一类是小分子阳离子试剂，如3-氯-2羟丙基三甲基氯化铵等，这类阳离子试剂由于其分子量小，可以很好的进入纤维内部，改性比较均匀，但用量较大，且存在一定的环境污染问题；另一类是高分子阳离子聚合物，由于其分子量大，阳离子度高，因此用量很少，但改性多限制在纤维表面，容易导致改性不均匀，从而影响染色效果。
发明内容
本发明是合成一种双功能型阳离子聚合物：二甲基二烯丙基氯化铵和烯丙基缩水甘油醚的共聚物，该共聚物既可以对棉纤维进行化学改性，也可以对染色废水进行后处理。通过控制合成条件制备出阳离子度适中、分子量较小的阳离子聚合物，能够在温和条件下对棉织物均匀改性，改性过后的棉织物可用活性染料在低温、无盐条件下进行染色，不仅大大提高染料的总利用率，而且能够获得较好的匀染效果；此外，改性棉布水洗液中的少量阳离子聚合物还可对染色废水和皂洗废水进行后处理，避免二次污染，从而实现绿色生产。
实施该发明的技术方案包括三部分，
第一部分是阳离子聚合物的合成，反应原理见附图1：按质量比7.5:1称取二甲基二烯丙基氯化铵与烯丙基缩水甘油醚加入到三口烧瓶中，然后加入单体总量1％的过硫酸钾作为引发剂，70～90℃恒温搅拌反应4h，自然冷却至室温，加入丙酮使产品析出，50℃真空干燥。
第二部分是棉纤维改性处理：合成的阳离子聚合物配制成一定浓度的水溶液，并用氢氧化钠溶液调节其pH值，将棉织物浸入该溶液，保持25℃，缓慢搅拌反应6h，水洗至中性，晾干。
第三部分是染色：采用活性染料在无盐条件下25℃浸染，并于35℃下加入碳酸钠进行固色。
经改性后的棉织物与活性染料具有很强的反应性，可在无盐条件下大幅提高染料总利用率。通过控制阳离子聚合物的合成条件，以获得阳离子度适中且分子量较小的阳离子聚合物，并在低温条件下对棉织物进行改性和染色，可获得较好的匀染效果。
本发明所涉及到的合成和改性工艺均能很好的适应印染厂现有设备，且操作简单，基本不增加现有的印染工序；所合成的阳离子聚合物用于棉织物改性，在保证匀染性的前提下大大提高了染料利用率；改性棉织物的水洗液中的少量阳离子还可以絮凝染料废水中的残余染料，经济环保，具有较高实用性。
附图说明
图1是本发明实施例技术方案阳离子聚合物-二甲基二烯丙基氯化铵和烯丙基缩水甘油醚的共聚物合成原理示意图。
具体实施方式
实施例1
(1)二甲基二烯丙基氯化铵和烯丙基缩水甘油醚共聚物的合成工艺
按照质量比7.5:1称取二甲基二烯丙基氯化铵和烯丙基缩水甘油醚加入到三口烧瓶中，然后加入单体总量1％(质量百分数，下同)的过硫酸钾作为引发剂，升温至90℃，恒温搅拌反应4h，自然冷却至室温，加入丙酮使产品析出，50℃真空干燥。
(2)棉织物改性工艺
上述合成的阳离子聚合物用去离子水配成浓度为0.7g/L的阳离子聚合物水溶液，并加入氢氧化钠溶液调节其pH值为13，将棉织物浸入该溶液，浴比1:100，保持25℃，缓慢搅拌6h，取出水洗至中性。
(3)改性棉织物染色工艺
活性黑KN-B，用量为3％(质量百分数，对棉纤维重)，浴比1:30，25℃浸染0.5h，缓慢升温至35℃，加入15g/L碳酸钠，固色4h，水洗，用1g/L的皂片水溶液95℃皂洗10min，水洗后晾干。
(4)未改性棉织物染色工艺
活性黑KN-B，用量为3％(质量百分数，对棉纤维重)，浴比1:30，氯化钠用量为60g/L，25℃浸染0.5h，缓慢升温至60℃，加入15g/L碳酸钠，固色4h，水洗，用1g/L的皂片水溶液95℃皂洗10min，水洗后晾干。
(5)染料废水和皂洗液后处理
改性棉织物用水充分清洗，水洗液与染色废水及皂洗液混合，使混合溶液中阳离子聚合物的浓度约为50mg/L，搅拌，静置沉降。通过絮凝沉降染料废水和皂洗液，絮凝脱色率达90.25％。染色废水和皂洗液得到净化处理。
经测试，采用本实施例技术方案处理的棉织物其无盐染色染料利用率高于未改性棉织物有盐染色结果，匀染性良好。
实施例2
(1)二甲基二烯丙基氯化铵和烯丙基缩水甘油醚共聚物的合成工艺
按照质量比7.5:1称取二甲基二烯丙基氯化铵和烯丙基缩水甘油醚加入到三口烧瓶中，然后加入单体总量1％的过硫酸钾作为引发剂，升温至80℃，恒温搅拌反应6h，转入小烧杯中自然冷却至室温，加入丙酮使产品析出，50℃真空干燥。
(2)棉织物改性工艺
上述合成的阳离子聚合物用去离子水配成浓度为0.7g/L的阳离子聚合物水溶液，并加入氢氧化钠溶液调节其pH值为13，将棉织物浸入该溶液，浴比1:100，保持25℃，缓慢搅拌6h，取出水洗至中性。
(3)改性棉织物染色工艺
活性艳蓝KN-R或者活性翠蓝KN-G或者活性黄3RS或者活性艳红3BSN，用量为3％(质量百分数，对棉纤维重)，浴比1:30，25℃浸染0.5h，缓慢升温至35℃，加入15g/L碳酸钠，固色4h，水洗，用1g/L的皂片水溶液95℃皂洗10min，水洗后晾干。
(4)未改性棉织物染色工艺
活性艳蓝KN-R或活性翠蓝KN-G或活性黄3RS或活性艳红3BSN，用量为3％(质量百分数，对棉纤维重)，浴比1:30，氯化钠用量为60g/L，25℃浸染0.5h，缓慢升温至60℃，加入15g/L碳酸钠，固色4h，水洗，用1g/L的皂片水溶液95℃皂洗10min，水洗后晾干。
(5)染料废水和皂洗液后处理
改性棉织物用水充分清洗，水洗液与染色废水及皂洗液混合，使混合溶液中阳离子聚合物的浓度为100mg/L，搅拌，静置沉降。通过絮凝沉降染料废水和皂洗液，絮凝脱色率达92.6％。染色废水和皂洗液得到净化处理。
经测试，采用本实施例技术方案处理的棉织物其无盐染色染料利用率高于未改性棉织物有盐染色结果，匀染性较好。
表1是采用活性染料对棉织物按照传统有盐染色工艺和阳离子改性棉织物按照无盐染色工艺分别测得的染料总利用率和K/S值结果对照表。其中染料总利用率T和K/S值分别按下式计算：
T＝E×F
式中，A0、A1、A2分别是λmax下用HP 8453紫外可见分光光度计所测得的染色前后和皂洗后染液的吸光度；R是λmax下用Ci6X分光光度仪所测得的织物反射率。
表1活性染料有盐染色、无盐染色结果对照
Claims (2)
1.一种环境友好的棉织物用活性染料低温无盐染色方法，其特征在于包括阳离子聚合物的合成、棉织物的改性处理、染色及染料废水的后处理工序，包括下列步骤：
（1）将二甲基二烯丙基氯化铵和烯丙基缩水甘油醚按质量比7.5:1的比例加入到三口烧瓶中，一次性加入单体总质量1%的过硫酸钾作为引发剂，于70~90℃下搅拌反应4h，取出，自然冷却至室温，加入丙酮使产品析出，50℃真空干燥；
（2）上述合成的阳离子聚合物用去离子水配成浓度为0.7g/L的阳离子聚合物水溶液，并加入氢氧化钠调节水溶液的pH值为13，将棉织物浸入该溶液，浴比1:100，保持25℃，缓慢搅拌6h，取出水洗至中性；
（3）改性棉织物用活性染料低温无盐染色，所述的无盐染色方法是在25℃下浸染0.5h，缓慢升温至35℃，加入15g/L碳酸钠，固色4h，水洗，用1g/L的皂片水溶液95℃皂洗10min，水洗后晾干；所述的活性染料为活性黑KN-B，活性艳蓝KN-R，活性翠蓝KN-G，活性黄3RS，活性红3BSN；
（4）利用含有阳离子聚合物的改性棉织物的水洗液絮凝处理染料废水和皂洗液，将染残液进一步净化处理，使改性工艺绿色化：棉织物用上述合成的阳离子聚合物改性后，用水充分清洗，其水洗液与染色残液、皂洗废水混合，使混合液中阳离子聚合物的浓度为50mmg/L～100mmg/L，搅拌，静置。
2.根据权利要求1所述的一种环境友好的棉织物用活性染料低温无盐染色方法，其特征在于所述的阳离子聚合物的阳离子度为3.034mmol/g，重均分子量为2315g/mol。
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