CN107227613A - 一种高吸湿羧基棉纤维的制备方法 - Google Patents
一种高吸湿羧基棉纤维的制备方法 Download PDFInfo
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Abstract
本发明公开了一种高吸湿羧基棉纤维的制备方法，涉及纺织纤维加工技术领域，包括如下步骤：(1)棉纤维预处理，(2)选择性氧化，(3)超声波处理，(4)干燥。本发明所制羧基棉纤维的羧基含量达到0.45mmol/g，从而增强吸湿性能，经试验测得其回潮率达到11.2％，从而利于将所制羧基棉纤维加工成对吸湿性要求较高的纺织品，提高纺织品的使用性能。
Description
技术领域：
本发明涉及纺织纤维加工技术领域，具体涉及一种高吸湿羧基棉纤维的制备方法。
背景技术：
棉纤维作为四大天然纤维之一，由于其柔软、保暖、舒适等独特优良的性质，一直备受人们的青睐。棉纤维的结构一般包括大分子结构、超分子结构和形态结构，棉纤维的性质基本上都有这些结构所决定的。棉纤维的主要组成物质是纤维素，其余为纤维素伴生物。棉纤维素及其伴生物的含量取决于棉纤维的成熟程度。正常成熟的棉纤维其纤维素含量占棉纤维总重量的94％左右，伴生物含量很少。由于棉纤维的组成结构及物理、化学等性能使棉纤维具有可纺性好，天然转曲多使棉纤维具有一定的抱全力，有利于纺纱工艺。
棉纤维有较好的吸湿性，在湿度状态下，棉纤维的强度会增加10％，但湿度过低时，强度较差。因此，说明对棉纤维吸湿性的适当提高会显著增强棉纤维的强度，以便于后续纺织面料加工工艺的高质进行，包括开松、除杂、梳理、伸直、牵伸、加捻和卷绕。
想要增强棉纤维的吸湿性，需要通过化学改性法在棉纤维大分子结构中引入亲水性基团，包括羟基、羧基、酰胺基、氨基等，以生成纤维素衍生物，其中氧化是非常重要的一种方法。对棉纤维进行选择性氧化，可使纤维素单元葡萄糖残基上的不同位置羟基发生反应，产生新的活性基团，以增强棉纤维的吸湿性。
目前，利用引入羧基来增强棉纤维的改性处理通常在高温、强酸或强碱介质中进行，所选用的氧化剂不仅对纤维素本身的破坏性大，而且所产生的废水对环境污染小强，需要经过多重处理后才能排放。并且在氧化过程中存在纤维素分子量减小、氧化不均匀的问题，无法保证所制羧基棉纤维的使用性能。
发明内容：
本发明所要解决的技术问题在于提供一种反应条件温和、废水污染性小且操作简便的高吸湿羧基棉纤维的制备方法。
本发明所要解决的技术问题采用以下的技术方案来实现：
一种高吸湿羧基棉纤维的制备方法，包括如下步骤：
(1)棉纤维预处理：将棉纤维浸泡在预处理液中，8-12h后抽滤，并用蒸馏水将滤渣洗涤至无预处理液残留；
(2)选择性氧化：将经预处理后的棉纤维分散于蒸馏水中，再加入4-乙酰氨基-TEMPO和溴化钠，充分混合后静置10-15min，并在搅拌下滴加50％次氯酸钠溶液，利用0.1mol/L氢氧化钠溶液控制反应体系pH值在9.5-10，待反应至pH值不变化时加入乙醇终止反应，继续搅拌5-10min，抽滤，滤渣用蒸馏水洗涤至无Cl-存在为止，即得羧基棉纤维；
(3)超声波处理：将所制羧基棉纤维分散于蒸馏水中配成悬浮液，并加入超声助剂，充分混合，再利用工作频率20kHz、输出功率600W的超声波细胞粉碎机处理3-5min，即得羧基棉纤维水溶液；
(4)干燥：将上述所得羧基棉纤维水溶液高速离心，过滤，滤渣用蒸馏水洗涤至无超声助剂残留，低温烘干，即得高吸湿羧基棉纤维。
所述4-乙酰氨基-TEMPO用量为0.1-0.2mmol每克棉纤维干重，溴化钠用量为1-2mmol每克棉纤维干重，次氯酸钠用量为1-2mmol每克棉纤维干重。
所述预处理液由如下重量份数的原料制成：月桂醇硫酸酯钠3-5份、N-羟甲基丙烯酰胺1-2份、聚天门冬氨酸0.5-1份、纳米钛白粉0.1-0.3份、抗坏血酸磷酸酯镁0.05-0.1份、甘草酸二钾0.05-0.1份、水100-150份，其制备方法为：向水中加入N-羟甲基丙烯酰胺、聚天门冬氨酸和纳米钛白粉，升温至回流状态保温搅拌30min，并以5℃/min的降温速度降温至35-40℃，然后加入月桂醇硫酸酯钠、抗坏血酸磷酸酯镁和甘草酸二钾，搅拌溶解完全后静置10min，再转入0-5℃环境中密封静置8h，再次升温至回流状态保温搅拌10min，自然冷却至室温，即得预处理液。
所述超声助剂由如下重量份数的原料制成：泊洛沙姆2-3份、聚二甲基二烯丙基氯化铵1-2份、羟乙基纤维素0.5-1份、多聚谷氨酸0.5-1份、小苏打粉0.1-0.3份、二茂铁0.01-0.02份，其制备方法为：向泊洛沙姆中加入聚二甲基二烯丙基氯化铵和二茂铁，升温至115-120℃保温研磨15min，待自然冷却至室温后加入羟乙基纤维素、多聚谷氨酸和小苏打粉，室温研磨10min，然后搅拌下向所得混合物中加入55-60℃热水，待混合物完全溶解后静置30min，最后将所得混合溶液送入喷雾干燥机中，干燥所得颗粒经超微粉碎机制成微粉，即得超声助剂。
本发明的有益效果是：
(1)通过预处理液的使用，使棉纤维内部孔径增大，并增强棉纤维的表面活性；
(2)通过4-乙酰氨基-TEMPO-NaClO-NaBr氧化体系的选择性氧化将棉纤维素分子结构中C6位的醇羟基氧化为羧基，从而在棉纤维分子中引入羧基，以赋予棉纤维高吸湿能力；
(3)通过对所制羧基棉纤维的超声波处理，并在超声助剂的协助下，促进纤维形态的改变，使所制羧基棉纤维被完全细化成均匀性强的超细纤维，从而进一步增强吸湿能力；
(4)所制羧基棉纤维的羧基含量达到0.45mmol/g，从而增强吸湿性能，经试验测得其回潮率达到11.2％，从而利于将所制羧基棉纤维加工成对吸湿性要求较高的纺织品，提高纺织品的使用性能。
具体实施方式：
为了使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解，下面结合具体实施例，进一步阐述本发明。
实施例1
(1)棉纤维预处理：将10g棉纤维浸泡在预处理液中，8h后抽滤，并用蒸馏水将滤渣洗涤至无预处理液残留；
(2)选择性氧化：将经预处理后的棉纤维分散于蒸馏水中，再加入1mmol4-乙酰氨基-TEMPO和10mmol溴化钠，充分混合后静置10min，并在搅拌下滴加50％次氯酸钠溶液(10mmol次氯酸钠固体)，利用0.1mol/L氢氧化钠溶液控制反应体系pH值在9.5-10，待反应至pH值不变化时加入乙醇终止反应，继续搅拌10min，抽滤，滤渣用蒸馏水洗涤至无Cl-存在为止，即得羧基棉纤维；
(3)超声波处理：将所制羧基棉纤维分散于蒸馏水中配成悬浮液，并加入超声助剂，充分混合，再利用工作频率20kHz、输出功率600W的超声波细胞粉碎机处理5min，即得羧基棉纤维水溶液；
(4)干燥：将上述所得羧基棉纤维水溶液高速离心，过滤，滤渣用蒸馏水洗涤至无超声助剂残留，低温烘干，即得高吸湿羧基棉纤维。
预处理液的制备：向100g水中加入1g N-羟甲基丙烯酰胺、0.5g聚天门冬氨酸和0.1g纳米钛白粉，升温至回流状态保温搅拌30min，并以5℃/min的降温速度降温至35-40℃，然后加入3g月桂醇硫酸酯钠、0.05g抗坏血酸磷酸酯镁和0.05g甘草酸二钾，搅拌溶解完全后静置10min，再转入0-5℃环境中密封静置8h，再次升温至回流状态保温搅拌10min，自然冷却至室温，即得预处理液。
超声助剂的制备：向3g泊洛沙姆中加入2g聚二甲基二烯丙基氯化铵和0.01g二茂铁，升温至115-120℃保温研磨15min，待自然冷却至室温后加入0.5g羟乙基纤维素、0.5g多聚谷氨酸和0.1g小苏打粉，室温研磨10min，然后搅拌下向所得混合物中加入55-60℃热水，待混合物完全溶解后静置30min，最后将所得混合溶液送入喷雾干燥机中，干燥所得颗粒经超微粉碎机制成微粉，即得超声助剂。
实施例2
(1)棉纤维预处理：将10g棉纤维浸泡在预处理液中，8h后抽滤，并用蒸馏水将滤渣洗涤至无预处理液残留；
(2)选择性氧化：将经预处理后的棉纤维分散于蒸馏水中，再加入1mmol4-乙酰氨基-TEMPO和10mmol溴化钠，充分混合后静置10min，并在搅拌下滴加50％次氯酸钠溶液(15mmol次氯酸钠固体)，利用0.1mol/L氢氧化钠溶液控制反应体系pH值在9.5-10，待反应至pH值不变化时加入乙醇终止反应，继续搅拌10min，抽滤，滤渣用蒸馏水洗涤至无Cl-存在为止，即得羧基棉纤维；
(3)超声波处理：将所制羧基棉纤维分散于蒸馏水中配成悬浮液，并加入超声助剂，充分混合，再利用工作频率20kHz、输出功率600W的超声波细胞粉碎机处理5min，即得羧基棉纤维水溶液；
(4)干燥：将上述所得羧基棉纤维水溶液高速离心，过滤，滤渣用蒸馏水洗涤至无超声助剂残留，低温烘干，即得高吸湿羧基棉纤维。
预处理液的制备：向150g水中加入2g N-羟甲基丙烯酰胺、1g聚天门冬氨酸和0.1g纳米钛白粉，升温至回流状态保温搅拌30min，并以5℃/min的降温速度降温至35-40℃，然后加入5g月桂醇硫酸酯钠、0.1g抗坏血酸磷酸酯镁和0.05g甘草酸二钾，搅拌溶解完全后静置10min，再转入0-5℃环境中密封静置8h，再次升温至回流状态保温搅拌10min，自然冷却至室温，即得预处理液。
超声助剂的制备：向2g泊洛沙姆中加入1g聚二甲基二烯丙基氯化铵和0.01g二茂铁，升温至115-120℃保温研磨15min，待自然冷却至室温后加入0.5g羟乙基纤维素、0.5g多聚谷氨酸和0.1g小苏打粉，室温研磨10min，然后搅拌下向所得混合物中加入55-60℃热水，待混合物完全溶解后静置30min，最后将所得混合溶液送入喷雾干燥机中，干燥所得颗粒经超微粉碎机制成微粉，即得超声助剂。
对照例1
(1)选择性氧化：将10g棉纤维分散于蒸馏水中，再加入1mmol 4-乙酰氨基-TEMPO和10mmol溴化钠，充分混合后静置10min，并在搅拌下滴加50％次氯酸钠溶液(15mmol次氯酸钠固体)，利用0.1mol/L氢氧化钠溶液控制反应体系pH值在9.5-10，待反应至pH值不变化时加入乙醇终止反应，继续搅拌10min，抽滤，滤渣用蒸馏水洗涤至无Cl-存在为止，即得羧基棉纤维；
(2)超声波处理：将所制羧基棉纤维分散于蒸馏水中配成悬浮液，并加入超声助剂，充分混合，再利用工作频率20kHz、输出功率600W的超声波细胞粉碎机处理5min，即得羧基棉纤维水溶液；
(3)干燥：将上述所得羧基棉纤维水溶液高速离心，过滤，滤渣用蒸馏水洗涤至无超声助剂残留，低温烘干，即得高吸湿羧基棉纤维。
超声助剂的制备：向2g泊洛沙姆中加入1g聚二甲基二烯丙基氯化铵和0.01g二茂铁，升温至115-120℃保温研磨15min，待自然冷却至室温后加入0.5g羟乙基纤维素、0.5g多聚谷氨酸和0.1g小苏打粉，室温研磨10min，然后搅拌下向所得混合物中加入55-60℃热水，待混合物完全溶解后静置30min，最后将所得混合溶液送入喷雾干燥机中，干燥所得颗粒经超微粉碎机制成微粉，即得超声助剂。
对照例2
(1)棉纤维预处理：将10g棉纤维浸泡在预处理液中，8h后抽滤，并用蒸馏水将滤渣洗涤至无预处理液残留；
(2)选择性氧化：将经预处理后的棉纤维分散于蒸馏水中，再加入1mmol4-乙酰氨基-TEMPO和10mmol溴化钠，充分混合后静置10min，并在搅拌下滴加50％次氯酸钠溶液(15mmol次氯酸钠固体)，利用0.1mol/L氢氧化钠溶液控制反应体系pH值在9.5-10，待反应至pH值不变化时加入乙醇终止反应，继续搅拌10min，抽滤，滤渣用蒸馏水洗涤至无Cl-存在为止，即得羧基棉纤维；
(3)超声波处理：将所制羧基棉纤维分散于蒸馏水中配成悬浮液，再利用工作频率20kHz、输出功率600W的超声波细胞粉碎机处理5min，即得羧基棉纤维水溶液；
(4)干燥：将上述所得羧基棉纤维水溶液高速离心，过滤，滤渣用蒸馏水洗涤至无超声助剂残留，低温烘干，即得高吸湿羧基棉纤维。
预处理液的制备：向150g水中加入2g N-羟甲基丙烯酰胺、1g聚天门冬氨酸和0.1g纳米钛白粉，升温至回流状态保温搅拌30min，并以5℃/min的降温速度降温至35-40℃，然后加入5g月桂醇硫酸酯钠、0.1g抗坏血酸磷酸酯镁和0.05g甘草酸二钾，搅拌溶解完全后静置10min，再转入0-5℃环境中密封静置8h，再次升温至回流状态保温搅拌10min，自然冷却至室温，即得预处理液。
实施例3
分别测定实施例1、实施例2、对照例1、对照例2所制羧基棉纤维的使用性能，并设置未经氧化改性的棉纤维作为对照例3，结果如表1所示。
表1 本发明所制羧基棉纤维的性能
| 项目 | 实施例1 | 实施例2 | 对照例1 | 对照例2 | 对照例3 |
| 羧基含量(mmol/g) | 0.43 | 0.45 | 0.38 | 0.44 | - |
| 标准回潮率(％) | 11.1 | 11.2 | 10.6 | 9.8 | 8.5 |
| 湿干断裂强度比(％) | 191 | 195 | 178 | 153 | 126 |
标准回潮率测定条件：温度20±2℃，相对湿度65±2％。
以上显示和描述了本发明的基本原理和主要特征和本发明的优点。本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的只是说明本发明的原理，在不脱离本发明精神和范围的前提下，本发明还会有各种变化和改进，这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。
Claims (4)
1.一种高吸湿羧基棉纤维的制备方法，其特征在于，包括如下步骤：
(1)棉纤维预处理：将棉纤维浸泡在预处理液中，8-12h后抽滤，并用蒸馏水将滤渣洗涤至无预处理液残留；
(2)选择性氧化：将经预处理后的棉纤维分散于蒸馏水中，再加入4-乙酰氨基-TEMPO和溴化钠，充分混合后静置10-15min，并在搅拌下滴加50％次氯酸钠溶液，利用0.1mol/L氢氧化钠溶液控制反应体系pH值在9.5-10，待反应至pH值不变化时加入乙醇终止反应，继续搅拌5-10min，抽滤，滤渣用蒸馏水洗涤至无Cl-存在为止，即得羧基棉纤维；
(3)超声波处理：将所制羧基棉纤维分散于蒸馏水中配成悬浮液，并加入超声助剂，充分混合，再利用工作频率20kHz、输出功率600W的超声波细胞粉碎机处理3-5min，即得羧基棉纤维水溶液；
(4)干燥：将上述所得羧基棉纤维水溶液高速离心，过滤，滤渣用蒸馏水洗涤至无超声助剂残留，低温烘干，即得高吸湿羧基棉纤维。
2.根据权利要求1所述的高吸湿羧基棉纤维的制备方法，其特征在于：所述4-乙酰氨基-TEMPO用量为0.1-0.2mmol每克棉纤维干重，溴化钠用量为1-2mmol每克棉纤维干重，次氯酸钠用量为1-2mmol每克棉纤维干重。
3.根据权利要求1所述的高吸湿羧基棉纤维的制备方法，其特征在于，所述预处理液由如下重量份数的原料制成：月桂醇硫酸酯钠3-5份、N-羟甲基丙烯酰胺1-2份、聚天门冬氨酸0.5-1份、纳米钛白粉0.1-0.3份、抗坏血酸磷酸酯镁0.05-0.1份、甘草酸二钾0.05-0.1份、水100-150份，其制备方法为：向水中加入N-羟甲基丙烯酰胺、聚天门冬氨酸和纳米钛白粉，升温至回流状态保温搅拌30min，并以5℃/min的降温速度降温至35-40℃，然后加入月桂醇硫酸酯钠、抗坏血酸磷酸酯镁和甘草酸二钾，搅拌溶解完全后静置10min，再转入0-5℃环境中密封静置8h，再次升温至回流状态保温搅拌10min，自然冷却至室温，即得预处理液。
4.根据权利要求1所述的高吸湿羧基棉纤维的制备方法，其特征在于，所述超声助剂由如下重量份数的原料制成：泊洛沙姆2-3份、聚二甲基二烯丙基氯化铵1-2份、羟乙基纤维素0.5-1份、多聚谷氨酸0.5-1份、小苏打粉0.1-0.3份、二茂铁0.01-0.02份，其制备方法为：向泊洛沙姆中加入聚二甲基二烯丙基氯化铵和二茂铁，升温至115-120℃保温研磨15min，待自然冷却至室温后加入羟乙基纤维素、多聚谷氨酸和小苏打粉，室温研磨10min，然后搅拌下向所得混合物中加入55-60℃热水，待混合物完全溶解后静置30min，最后将所得混合溶液送入喷雾干燥机中，干燥所得颗粒经超微粉碎机制成微粉，即得超声助剂。
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