CN107724067A - 具有耐洗性能的纳米二氧化钛改性纤维素纤维及制备方法 - Google Patents
具有耐洗性能的纳米二氧化钛改性纤维素纤维及制备方法 Download PDFInfo
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Abstract
本发明公开了一种具有耐洗性能的纳米二氧化钛改性纤维素纤维及制备方法，通过在纤维素纤维的内部原位生成纳米二氧化钛颗粒和将二氧化钛纳米颗粒包覆在BSA中间，大大提高了二氧化钛纳米颗粒的附着能力。二氧化钛纳米颗粒改性后的纤维素纤维具有优异的抗菌、抗紫外、光催化、超疏水、抗皱、耐洗和自清洁性能。
Description
技术领域
本发明涉及一种具有耐洗性能的纳米二氧化钛改性纤维素纤维及制备方法，属功能纳米材料和纺织材料领域。
背景技术
从20世纪90年开始，随着测量与表征技术的提高，纳米材料和纳米科技得到了飞速的发展。纳米材料是指尺寸处于1-100nm的材料，不同与块状材料，其拥有独特的光电磁特性，在电子、材料、医药、生物、机械、纺织、印染等各个领域得到广泛的研究和应用。就纺织领域而言，将纳米材料与纺织品相结合可有效改善纺织品的固有缺陷，扩大纺织品的适用范围，提高纺织品的附加值。大量的研究结果表明，使用二氧化钛（TiO2）、氧化锌（ZnO）、石墨烯、氧化石墨烯（GO）、碳纳米管、纳米银、纳米金等纳米材料整理纺织品，可赋予纺织品优异的抗菌、抗紫外、自清洁、抗黄变、导电、抗电磁辐射等性能。
在众多类型的无机纳米材料中，纳米TiO2占据着重要的位置。纳米TiO2，亦称钛白粉，直径1-100nm，产品外观为白色疏松粉末，具有抗紫外线、抗菌、自洁净、抗老化等性能，在光催化、清洁能源、化妆品、功能纤维、塑料、油墨、涂料、油漆、精细陶瓷、光电材料等领域有着广泛的研究和应用（张伟伟. 氨基化改性纳米TiO2制备及对真丝织物抗紫外性能研究[D].苏州大学,2015）。
在纺织领域，纳米TiO2可赋予纺织品抑菌、除臭、自清洁、抗皱、紫外线屏蔽和光催化等功能。将纳米TiO2与纤维素纤维相结合可有效改善纤维素纤维固有缺陷，扩大纤维素纤维适用范围，提高纤维素纤维的附加值。以最常用的纤维素纤维——棉纤维为例，使用纳米TiO2改性棉纤维可获得抗菌、抗紫外、光催化、超疏水、抗皱、耐洗和自清洁性能（周文雅,张杨杨,施亦东. 浸轧水热法负载二氧化钛棉织物的性能研究[J]. 印染助剂,2017,34(01):23-26；张杨杨,施亦东. 纳米TiO2负载棉织物的光催化性能[J]. 印染,2015,41(11):10-13；杨璐,张辉. 棉织物水热法纳米二氧化钛表面改性[J]. 西安工程大学学报,2011,25(02):154-158+182；赵玉婷,邓桦,王蕊,谢飞翔. 棉织物的防皱防紫外复合整理[J]. 染整技术,2016,38(12):14-18；MEMON Hafeezullah,王宁宁,王珏,冯旭煌,祝成炎.负载纳米二氧化钛光催化织物的制备及其性能研究[J]. 浙江理工大学学报,2016,35(01):17-21；周顺利. 基于纳米TiO2的光催化自清洁面料的研究[D].北京服装学院,2017；卢红蓉. 纳米TiO2的制备、表面改性及其紫外屏蔽性研究[D].苏州大学,2010）。
但是目前纳米TiO2对纤维素纤维的改性主要是通过后整理法来实现。后整理法主要采用浸渍、浸轧、涂层或喷涂等方法将纳米TiO2整理到纤维上，并使之固着在纺织材料上的一种方法。后整理法具有工艺简单、可操作性强等优势。但加工过程中存在纳米材料易团聚，纳米材料在纤维和织物表面分布不均匀，纳米材料与纤维结合牢度低的问题（周顺利,王峰,熊祖江,王锐,杨春芳,张秀芹,阳明书. 基于纳米二氧化钛的光催化自清洁面料研究进展[J]. 高分子通报,2017,(04):9-18）。
发明内容
本发明针对上述不足，提供一种具有耐洗性能的纳米二氧化钛改性纤维素纤维及制备方法。
本发明通过下述技术方案予以实现：
（1）将纤维素纤维置于质量分数为10-18％的氢氧化钠溶液中，浴比1:50，70℃反应180min，用去离子水反复洗至中性，烘干后得到氢氧化钠改性纤维素；然后将上述氢氧化钠改性纤维素分散于乙醇中，浴比1:50，80℃氮气保护条件下冷凝回流60min，加入醇醚磺基琥珀酸单酯二钠盐，匀速搅拌60min后，加入偶氮二异庚腈和过氧化二苯甲酰，继续搅拌反应1-12h，过滤后使用乙醇、去离子水反复清洗，真空烘干后得到阴离子化纤维素纤维；所述醇醚磺基琥珀酸单酯二钠盐与氢氧化钠改性纤维素的质量比为1:1-1:3，所述偶氮二异庚腈的质量为氢氧化钠改性纤维素的0.01%-0.5%，所述过氧化二苯甲酰的质量为氢氧化钠改性纤维素的0.01%-0.5%。（2）将上述阴离子纤维素纤维浸渍在60℃的质量分数0.1-1%的牛血清白蛋白（BSA）溶液中60min，得到BSA改性纤维素纤维。（3）将上述BSA改性纤维素纤维浸渍在1-10g/L的钛酸四丁酯水溶液中，浴比1:50，缓慢加入十二烷基苯磺酸钠（SDBS），所述SDBS和钛酸四丁酯的质量比为2:1-1:2，超声30min后，移至高压反应釜中，200℃水热反应1-12h，反应结束后，用去离子水反复清洗、干燥处理得到纳米二氧化钛改性纤维素纤维。（4）将上述纳米二氧化钛改性纤维素纤维浸渍在60℃的质量分数0.1-1%的BSA溶液中60min，用去离子水反复清洗、真空干燥后得到具有耐洗性能的纳米二氧化钛改性纤维素纤维。
与现有技术相比，本发明的优点在于：通过原位生成二氧化钛纳米颗粒和将二氧化钛纳米颗粒包覆在BSA中间，大大提高了二氧化钛纳米颗粒的附着。二氧化钛纳米颗粒改性后的纤维素纤维具有优异的抗菌、抗紫外、光催化、超疏水、抗皱、耐洗和自清洁性能。
具体实施方式
下面结合具体实施方式，进一步阐述本发明。
实施例1：
（1）将棉布置于质量分数为10％的氢氧化钠溶液中，浴比1:50，70℃反应180min，用去离子水反复洗至中性，烘干后得到氢氧化钠改性棉；然后将上述氢氧化钠改性棉分散于乙醇中，浴比1:50，80℃氮气保护条件下冷凝回流60min，加入醇醚磺基琥珀酸单酯二钠盐，匀速搅拌60min后，加入偶氮二异庚腈和过氧化二苯甲酰，继续搅拌反应1h，过滤后使用乙醇、去离子水反复清洗，真空烘干后得到阴离子化棉纤维；所述醇醚磺基琥珀酸单酯二钠盐与氢氧化钠改性棉的质量比为1:1，所述偶氮二异庚腈的质量为氢氧化钠改性棉的0.01%，所述过氧化二苯甲酰的质量为氢氧化钠改性棉的0.01%。（2）将上述阴离子棉纤维浸渍在60℃的质量分数0.1%的牛血清白蛋白（BSA）溶液中60min，得到BSA改性棉纤维。（3）将上述BSA改性棉纤维浸渍在1g/L的钛酸四丁酯水溶液中，浴比1:50，缓慢加入十二烷基苯磺酸钠（SDBS），所述SDBS和钛酸四丁酯的质量比为2:1，超声30min后，移至高压反应釜中，200℃水热反应1h，反应结束后，用去离子水反复清洗、干燥处理得到纳米二氧化钛改性棉纤维。（4）将上述纳米二氧化钛改性棉纤维浸渍在60℃的质量分数0.1%的BSA溶液中60min，用去离子水反复清洗、真空干燥后得到具有耐洗性能的纳米二氧化钛改性棉纤维。
实施例2：
（1）将亚麻纤维置于质量分数为15％的氢氧化钠溶液中，浴比1:50，70℃反应180min，用去离子水反复洗至中性，烘干后得到氢氧化钠改性亚麻；然后将上述氢氧化钠改性亚麻分散于乙醇中，浴比1:50，80℃氮气保护条件下冷凝回流60min，加入醇醚磺基琥珀酸单酯二钠盐，匀速搅拌60min后，加入偶氮二异庚腈和过氧化二苯甲酰，继续搅拌反应5h，过滤后使用乙醇、去离子水反复清洗，真空烘干后得到阴离子化亚麻纤维；所述醇醚磺基琥珀酸单酯二钠盐与氢氧化钠改性亚麻的质量比为1:2，所述偶氮二异庚腈的质量为氢氧化钠改性亚麻的0.2%，所述过氧化二苯甲酰的质量为氢氧化钠改性亚麻的0.2%。（2）将上述阴离子亚麻纤维浸渍在60℃的质量分数0.5%的牛血清白蛋白（BSA）溶液中60min，得到BSA改性亚麻纤维。（3）将上述BSA改性亚麻纤维浸渍在5g/L的钛酸四丁酯水溶液中，浴比1:50，缓慢加入十二烷基苯磺酸钠（SDBS），所述SDBS和钛酸四丁酯的质量比为1:1，超声30min后，移至高压反应釜中，200℃水热反应6h，反应结束后，用去离子水反复清洗、干燥处理得到纳米二氧化钛改性亚麻纤维。（4）将上述纳米二氧化钛改性亚麻纤维浸渍在60℃的质量分数0.5%的BSA溶液中60min，用去离子水反复清洗、真空干燥后得到具有耐洗性能的纳米二氧化钛改性亚麻纤维。
实施例3：
（1）将竹原纤维纤维置于质量分数为18％的氢氧化钠溶液中，浴比1:50，70℃反应180min，用去离子水反复洗至中性，烘干后得到氢氧化钠改性竹原纤维；然后将上述氢氧化钠改性竹原纤维分散于乙醇中，浴比1:50，80℃氮气保护条件下冷凝回流60min，加入醇醚磺基琥珀酸单酯二钠盐，匀速搅拌60min后，加入偶氮二异庚腈和过氧化二苯甲酰，继续搅拌反应12h，过滤后使用乙醇、去离子水反复清洗，真空烘干后得到阴离子化竹原纤维纤维；所述醇醚磺基琥珀酸单酯二钠盐与氢氧化钠改性竹原纤维的质量比为1:3，所述偶氮二异庚腈的质量为氢氧化钠改性竹原纤维的0.5%，所述过氧化二苯甲酰的质量为氢氧化钠改性竹原纤维的0.5%。（2）将上述阴离子竹原纤维浸渍在60℃的质量分数1%的牛血清白蛋白（BSA）溶液中60min，得到BSA改性竹原纤维。（3）将上述BSA改性竹原纤维浸渍在10g/L的钛酸四丁酯水溶液中，浴比1:50，缓慢加入十二烷基苯磺酸钠（SDBS），所述SDBS和钛酸四丁酯的质量比为1:2，超声30min后，移至高压反应釜中，200℃水热反应12h，反应结束后，用去离子水反复清洗、干燥处理得到纳米二氧化钛改性竹原纤维。（4）将上述纳米二氧化钛改性竹原纤维浸渍在60℃的质量分数1%的BSA溶液中60min，用去离子水反复清洗、真空干燥后得到具有耐洗性能的纳米二氧化钛改性竹原纤维。
显然，本发明的上述实施例仅仅是为清楚地说明本发明所作的举例，而并非是对本发明的实施方式的限定。对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无法对所有的实施方式予以穷举。凡是属于本发明的技术方案所引申出的显而易见的变化或变动仍处于本发明的保护范围之列。
Claims (3)
1.具有耐洗性能的纳米二氧化钛改性纤维素纤维的制备方法，其特征在于：包括纤维素纤维阴离子化、BSA改性阴离子化纤维素纤维、以钛酸四丁酯为前驱体原位生成二氧化钛纳米颗粒、BSA包覆四个步骤；
步骤一：将纤维素纤维置于质量分数为10-18％的氢氧化钠溶液中，浴比1:50，70℃反应180min，用去离子水反复洗至中性，烘干后得到氢氧化钠改性纤维素；然后将上述氢氧化钠改性纤维素分散于乙醇中，浴比1:50，80℃氮气保护条件下冷凝回流60min，加入醇醚磺基琥珀酸单酯二钠盐，匀速搅拌60min后，加入偶氮二异庚腈和过氧化二苯甲酰，继续搅拌反应1-12h，过滤后使用乙醇、去离子水反复清洗，真空烘干后得到阴离子化纤维素纤维；所述醇醚磺基琥珀酸单酯二钠盐与氢氧化钠改性纤维素的质量比为1:1-1:3，所述偶氮二异庚腈的质量为氢氧化钠改性纤维素的0.01%-0.5%，所述过氧化二苯甲酰的质量为氢氧化钠改性纤维素的0.01%-0.5%；
步骤二：将上述阴离子纤维素纤维浸渍在60℃的质量分数0.1-1%的牛血清白蛋白（BSA）溶液中60min，得到BSA改性纤维素纤维；
步骤三：将上述BSA改性纤维素纤维浸渍在1-10g/L的钛酸四丁酯水溶液中，浴比1:50，缓慢加入十二烷基苯磺酸钠（SDBS），所述SDBS和钛酸四丁酯的质量比为2:1-1:2，超声30min后，移至高压反应釜中，200℃水热反应1-12h，反应结束后，用去离子水反复清洗、干燥处理得到纳米二氧化钛改性纤维素纤维；
步骤四：将上述纳米二氧化钛改性纤维素纤维浸渍在60℃的质量分数0.1-1%的BSA溶液中60min，用去离子水反复清洗、真空干燥后得到具有耐洗性能的纳米二氧化钛改性纤维素纤维。
2.根据权利要求1所述的一种具有耐洗性能的纳米二氧化钛改性纤维素纤维及制备方法，其特征在于，所述纤维素纤维包括天然纤维素纤维和再生纤维素纤维。
3.按权利要求1制备方法得到的一种具有耐洗性能的纳米二氧化钛改性纤维素纤维。
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