CN111041812A - 一种自清洁纤维的制备方法 - Google Patents
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Abstract
本发明提供一种自清洁纤维及其制备方法，其中纤维以PET纤维为基材，通过原子层沉积技术在纤维表面沉积无机纳米材料，通过晶面匹配与光催化纳米材料实现结合，进一步地，通过光固化使得纳米材料牢固负载在纤维表面。本发明主要采用在纤维上形成光催化表面的方法，重点解决涂层与纤维牢固度的问题，采用原子层沉积与晶面匹配技术，同时采用光固化固定技术，实现光催化纳米材料与纤维的紧密结合。
Description
技术领域
本发明涉及功能纤维的制备领域，具体为提供一种自清洁纤维的制备方法，即在纤维表面涂覆具有光催化性能的纳米材料。
背景技术
自清洁功能纤维用在纺织领域，不仅可缓解洗涤带来的环境和能源问题，还能有效屏蔽和消解如细菌、病毒、杀虫剂、污渍等各种各样的环境污染物，避免这些污染物通过皮肤或呼吸道对人体造成伤害，所以具有自清洁功能的纤维织物可广泛应用于日常服装、生化防护服、医疗保健、环境、农场、军事等领域。
自清洁功能纤维或是织物都具备一项共同点：具有自清洁功能的表面。获得自清洁功能的途径主要包括两类：一是形成超疏水化表面，二是形成光催化表面。其中，超疏水化表面的制备方法主要包括：构建基于仿生学原理构建材料表面结构，使用低表面能的含氟、硅基团的物质对表面进行修饰或是涂层，以及利用纳米技术方法对纤维和织物进行超疏水化处理。光催化表面的制备方法主要包括：利用具有光催化效果的纳米材料如纳米二氧化钛（TiO2）整理织物，得到具有光催化的表面。但是，自清洁纤维和织物的研究现状表明，尚有许多关键问题有待进一步研发：比如超疏水自清洁表面制备方法大多需要复杂的设计、精细的控制技术或价格昂贵的氟硅化合物；光催化自清洁表面技术存在无机TiO2颗粒与纤维结合的牢度不够、易于脱落，影响纤维手感以及难以在纤维表面均匀分散等问题。因此，要开发出适用于纤维材料且高性能化、低成本化的自清洁方法还需要新的思路。
本发明主要采用在纤维上形成光催化表面的方法，重点解决涂层与纤维牢固度的问题，采用原子层沉积与晶面匹配技术，同时采用光固化固定技术，实现光催化纳米材料与纤维的紧密结合。
发明内容
针对现有技术的不足，本发明目的在于提供一种自清洁纤维的制备方法。
本发明目的通过以下方案实现：一种自清洁纤维的制备方法，以PET（聚对苯二甲酸乙二醇酯）纤维为基材，通过原子层沉积技术在纤维表面沉积无机纳米材料，通过晶面匹配与光催化纳米材料实现结合，进一步地，通过光固化使得纳米材料牢固负载在纤维表面，包括如下步骤：
（1）将PET浸泡于浓氢氧化钠（如质量浓度为20-40%）中，搅拌24小时后洗净烘干，然后置于浓度为K2Cr2O7：H2SO4：H2O =1：20：2（w/v/w）的铬酸溶液中，60℃下超声处理15min，再去离子水清洗直至水洗溶液呈中性，室温下干燥；
（2）将PET纤维通过原子层沉积技术沉积一层纳米氧化物得到，其工艺在于：将沉积室真空抽至10-16Pa，基片加热至100-150℃，向沉积室中引入金属气源，用高纯氮气清洗沉积室并向沉积室中引入水蒸气，金属气源、高纯氮气、水蒸气在沉积室内暴露时间依次为0.1s、3s、0.1s、3s；
（3）按质量百分比取下述涂层原料，纳米材料分散液10-30％、胶黏剂1-3％、分散剂5-10％、抗老化剂0.1-1％、交联剂0.1-1％、增稠剂1-5％、光引发剂0.5-2％，余量为去离子水，混合，配制成原料备用；
（4）将原料均匀涂覆在纤维表面，通过压紧装置将涂层膜与纤维压实，重复涂布、压实，得到复合膜，然后将复合膜经过低温烘干处理，将经过烘干处理的复合膜用紫外光反应仪照射3-5分钟。
金属气源为二乙基锌、三甲基铝、四氯化钛的一种。
纳米材料分散液为纳米二氧化铝、纳米二氧化硅、纳米碳酸钙、纳米氧化锌、纳米二氧化钛中的一种。
胶黏剂为聚丙烯酸酯水性粘合剂，所述分散剂为聚丙烯酸铵，所述抗老化剂为2-羟基-4-正辛氧基二苯甲酮，所述交联剂为三羟甲基丙烷三丙酸酯，所述增稠剂为羧甲基纤维素钠，所述光引发剂为二甲苯酮、烷基酮、双酮或乙酰基苯的一种。
烘干温度为50-100℃，烘干时间为10-60分钟。
本发明主要采用在纤维上形成光催化表面的方法，重点解决涂层与纤维牢固度的问题，采用原子层沉积与晶面匹配技术，同时采用光固化固定技术，实现光催化纳米材料与纤维的紧密结合。其中纤维以PET（聚对苯二甲酸乙二醇酯）为基材，通过原子层沉积技术在纤维表面沉积无机纳米材料，通过晶面匹配与光催化纳米材料实现结合，进一步地，通过光固化使得纳米材料牢固负载在纤维表面。
本发明采用原子层沉积与晶面匹配技术，同时采用光固化固定技术，实现光催化纳米材料与纤维的紧密结合。该纤维可以制备防护口罩等产品，可以有效阻挡灰尘、细菌等外来物质，发挥高效过滤的作用。本发明制备过程简单、反应易控制，稳定性好、可产业化，具有广泛的推广前景。
具体实施方式
以下通过具体的实施例对本发明的技术方案作进一步描述。以下的实施例是对本发明的进一步说明，而不限制本发明的范围。
实施例1
一种自清洁纤维，以聚对苯二甲酸乙二醇酯（PET）纤维为基材，通过原子层沉积技术在纤维表面沉积无机纳米材料，通过晶面匹配与光催化纳米材料实现结合，进一步地，通过光固化使得纳米材料牢固负载在纤维表面，按如下步骤制备：
（1）将PET纤维浸泡于浓氢氧化钠中，搅拌24小时后洗净烘干，然后置于浓度为K2Cr2O7：H2SO4：H2O =1：20：2（w/v/w）的铬酸溶液中，60℃下超声处理15min，再去离子水清洗直至水洗溶液呈中性，室温下干燥；
（2）将步骤（1）得到的PET纤维通过原子层沉积技术沉积一层纳米氧化物得到，其工艺在于：将沉积室真空抽至10Pa，基片加热至100℃，向沉积室中引入金属气源二乙基锌，用高纯氮气清洗沉积室并向沉积室中引入水蒸气，金属气源、高纯氮气、水蒸气在沉积室内暴露时间依次为0.1s、3s、0.1s、3s；
（3）按质量百分比取下述涂层原料，纳米氧化锌10％、聚丙烯酸酯水性胶黏剂1％、分散剂聚丙烯酸铵5％、抗老化剂2-羟基-4-正辛氧基二苯甲酮0.1％、交联剂三羟甲基丙烷三丙酸酯0.1％、增稠剂羧甲基纤维素钠1％、光引发剂二甲苯酮0.5％，余量为去离子水，混合，配制成原料备用；
（4）将原料均匀涂覆在纤维表面，通过压紧装置将涂层膜与纤维压实，重复涂布、压实，得到复合膜，然后将复合膜经过50℃低温烘干处理30分钟，将经过烘干处理的复合膜用紫外光反应仪照射3分钟。
涂层结合力为7.6MPa。
实施例2
一种自清洁纤维，与实施例1近似，按如下步骤制备：
（1）将PET纤维浸泡于浓氢氧化钠中，搅拌24小时后洗净烘干，然后置于浓度为K2Cr2O7：H2SO4：H2O =1：20：2（w/v/w）的铬酸溶液中，60℃下超声处理15min，再去离子水清洗直至水洗溶液呈中性，室温下干燥；
（2）将步骤（1）得到的PET纤维通过原子层沉积技术沉积一层纳米氧化物得到，其工艺在于：将沉积室真空抽至15Pa，基片加热至120℃，向沉积室中引入金属气源二乙基锌，用高纯氮气清洗沉积室并向沉积室中引入水蒸气，金属气源、高纯氮气、水蒸气在沉积室内暴露时间依次为0.1s、3s、0.1s、3s；
（3）按质量百分比取下述涂层原料，纳米氧化锌10-30％、胶黏剂聚丙烯酸酯水性粘合剂3％、分散剂聚丙烯酸铵10％、抗老化剂2-羟基-4-正辛氧基二苯甲酮1％、交联剂三羟甲基丙烷三丙酸酯1％、增稠剂、羧甲基纤维素钠5％、光引发剂烷基酮5％，余量为去离子水，混合，配制成原料备用；
（4）将原料均匀涂覆在纤维表面，通过压紧装置将涂层膜与纤维压实，重复涂布、压实，得到复合膜，然后将复合膜经过70℃低温烘干处理60分钟，将经过烘干处理的复合膜用紫外光反应仪照射5分钟。
涂层结合力为9.1MPa。
实施例3
一种自清洁纤维，与实施例1近似，按如下步骤制备：
（1）将PET纤维浸泡于浓氢氧化钠中，搅拌24小时后洗净烘干，然后置于浓度为K2Cr2O7：H2SO4：H2O =1：20：2（w/v/w）的铬酸溶液中，60℃下超声处理15min，再去离子水清洗直至水洗溶液呈中性，室温下干燥；
（2）将步骤（1）得到的PET纤维通过原子层沉积技术沉积一层纳米氧化物得到，其工艺在于：将沉积室真空抽至15Pa，基片加热至150℃，向沉积室中引入金属气源四氯化钛，用高纯氮气清洗沉积室并向沉积室中引入水蒸气，金属气源、高纯氮气、水蒸气在沉积室内暴露时间依次为0.1s、3s、0.1s、3s；
（3）按质量百分比取下述涂层原料，纳米二氧化钛30％、胶黏剂聚丙烯酸酯水性粘合剂2％、分散剂聚丙烯酸铵8％、抗老化剂2-羟基-4-正辛氧基二苯甲酮0.5％、交联剂三羟甲基丙烷三丙酸酯0.5％、增稠剂羧甲基纤维素钠3％、光引发剂乙酰基苯5％，余量为去离子水，混合，配制成原料备用；
（4）将原料均匀涂覆在纤维表面，通过压紧装置将涂层膜与纤维压实，重复涂布、压实，得到复合膜，然后将复合膜经过100℃低温烘干处理60分钟，将经过烘干处理的复合膜用紫外光反应仪照射5分钟。
涂层结合力为7.9MPa。
Claims (5)
1.一种自清洁纤维的制备方法，其特征在于以聚对苯二甲酸乙二醇酯（PET）纤维为基材，通过原子层沉积技术在纤维表面沉积无机纳米材料，通过晶面匹配与光催化纳米材料实现结合，进一步地，通过光固化使得纳米材料牢固负载在纤维表面，包括如下步骤：
（1）将PET浸泡于浓氢氧化钠中，搅拌24小时后洗净烘干，然后置于浓度为K2Cr2O7：H2SO4：H2O =1：20：2（w/v/w）的铬酸溶液中，60℃下超声处理15min，再去离子水清洗直至水洗溶液呈中性，室温下干燥；
（2）将步骤（1）得到的PET纤维通过原子层沉积技术沉积一层纳米氧化物得到，其工艺在于：将沉积室真空抽至10-16Pa，基片加热至100-150℃，向沉积室中引入金属气源，用高纯氮气清洗沉积室并向沉积室中引入水蒸气，金属气源、高纯氮气、水蒸气在沉积室内暴露时间依次为0.1s、3s、0.1s、3s；
（3）按质量百分比取下述涂层原料，纳米材料分散液10-30％、胶黏剂1-3％、分散剂5-10％、抗老化剂0.1-1％、交联剂0.1-1％、增稠剂1-5％、光引发剂0.5-5％，余量为去离子水，混合，配制成原料备用；
（4）将原料均匀涂覆在纤维表面，通过压紧装置将涂层膜与纤维压实，重复涂布、压实，得到复合膜，然后将复合膜经过低温烘干处理，将经过烘干处理的复合膜用紫外光反应仪照射3-5分钟。
2.根据权利要求1所述自清洁纤维的制备方法，其特征在于金属气源为二乙基锌、三甲基铝、四氯化钛的一种。
3.根据权利要求1所述自清洁纤维的制备方法，其特征在于纳米材料分散液为纳米二氧化铝、纳米二氧化硅、纳米碳酸钙、纳米氧化锌、纳米二氧化钛中的一种。
4.根据权利要求1所述自清洁纤维的制备方法，其特征在于胶黏剂为聚丙烯酸酯水性粘合剂，所述分散剂为聚丙烯酸铵，所述抗老化剂为2-羟基-4-正辛氧基二苯甲酮，所述交联剂为三羟甲基丙烷三丙酸酯，所述增稠剂为羧甲基纤维素钠，所述光引发剂为二甲苯酮、烷基酮、双酮或乙酰基苯的一种。
5.根据权利要求1所述自清洁纤维的制备方法，其特征在于步骤（4）中烘干温度为50-100℃，烘干时间为10-60分钟。
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