CN108547145A - 一种钒酸铋插层氧化石墨烯可见光催化功能织物的制备方法 - Google Patents
一种钒酸铋插层氧化石墨烯可见光催化功能织物的制备方法 Download PDFInfo
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Abstract
本发明公开了一种钒酸铋插层氧化石墨烯可见光催化功能织物的制备方法，包括：(1)将棉织物进行羧甲基壳聚糖处理，硅烷偶联剂改性，氧化石墨烯改性，制备增强石墨烯改性棉织物；(2)在搅拌条件下依次将偏矾酸钠、增强石墨烯改性棉织物、硝酸铋加入到磷酸盐缓冲溶液，搅拌30～60min得到墨绿色溶液；(3)升温至80～100℃回流10～20h，取出织物烘干即得。本发明成本低，织物强力损伤小，兼有抗菌效果，无二次污染，易于工业化生产，所得的可见光催化功能织物空气净化效果好。
Description
技术领域
本发明属光催化功能织物的制备领域，特别是涉及一种钒酸铋插层氧化石墨烯可见光催化功能织物的制备方法。
背景技术
近年来，随着我国经济的迅猛发展和人民生活的日益提高，人们开始认识到提高室内空气的品质是健康生活和工作的保障，因此，治理室内空气污染尤其是去除室内空气中的有机污染物成为国内外科技工作者研究的热点。目前，去除室内空气污染物的方法主要有：物理吸附法、化学中和法、空气负离子法、光催化法等。其中，光催化法具有明显的节能、高效、污染物降解彻底等优点且无二次污染，它已成为一种具有重要应用前景的环境治理方法，引起了国内外学者的普遍重视。至今人们对各种类型的半导体光催化反应进行了广泛的研究，取得了一定的成就。
从20世纪70年代起，钒酸铋(BiVO4)以其优越的可见光催化性能受到越来越广泛的关注。BiVO4作为光催化剂处理到玻璃、陶瓷、膨润土等刚性基材上已有人研究，但考虑到柔性基材(纤维材料)作为载体具有表面积大、易加工成型、富集污染物等等特殊性能，将光催化剂负载到柔性基材上制备柔性空气净化材料，具有更重要的实用意义。目前通过原位沉积法、浸轧法和涂层法将纳米BiVO4负载到柔性基材上也有报道，但该柔性光催化织物，存在光催化效率低，柔性基材易光降解等问题。本发明从提高光催化效率和增强纤维基材的强度角度出发，制备了钒酸铋插层氧化石墨烯可见光催化功能织物。
发明内容
发明目的：本发明所要解决的技术问题是提供一种钒酸铋插层氧化石墨烯可见光催化功能织物的制备方法，该方法成本低，无二次污染，易于工业化生产，所得的柔性空气净化材料空气净化效果好。
发明内容：本发明的一种钒酸铋插层氧化石墨烯可见光催化功能织物的制备方法，包括：
(1)将纯棉织物经羧甲基壳聚糖整理液二浸二轧后，80～100℃烘干，150～180℃焙烘1～3min，得到羧甲基壳聚糖改性棉织物；然后将羧甲基壳聚糖改性棉织物经KH-550硅烷偶联剂水溶液二浸二轧后，80～100℃烘干4～8min，得到硅烷偶联剂改性棉织物；然后将改性棉织物加入到超声分散的氧化石墨烯溶液中，调节pH值7～8.5，温度50～60℃超声反应12～24h，水洗至中性，真空烘干，得到增强石墨烯改性棉织物；
(2)在搅拌条件下依次将偏矾酸钠、增强石墨烯改性棉织物、硝酸铋加入到磷酸盐缓冲溶液，搅拌30～60min得到墨绿色溶液；其中，偏钒酸钠与硝酸铋的摩尔量比为1:2；
(3)用碱性溶液调节pH值为7～8，升温至80～100℃回流10～20h，取出织物80℃烘干，得到钒酸铋插层氧化石墨烯可见光催化功能织物。
所述步骤(1)中的纯棉织物为纯棉非织造布、纯棉机织布或纯棉针织布。
所述步骤(1)中的羧甲基壳聚糖整理液为0.1％～5％的羧甲基壳聚糖溶液。
所述步骤(1)中的KH-550硅烷偶联剂水溶液浓度为1～5g/L。
所述步骤(1)中的氧化石墨烯溶液浓度为0.1～0.5g/L。
所述步骤(2)中的磷酸盐缓冲溶液由0.1mol/L磷酸二氢钠和0.1mol/L磷酸氢钠组成，pH值为6.5～7。
所述步骤(2)中的增强石墨烯改性棉织物与偏钒酸钠用量的比例为1g：5～20mmol。
所述步骤(2)中的增强石墨烯改性棉织物与磷酸盐缓冲溶液的比例为1g：50～100mL。
所述步骤(3)中的碱性溶液为浓度为0.1～1mol/L的氢氧化钠水溶液。
有益效果：本发明制备的空气净化材料可应用于家装窗帘、医院病房、动车内部装饰、汽车内部装饰、飞机内部装饰等室内装饰领域，具有广阔的应用前景和市场前景。
本发明通过羧甲基壳聚糖处理，硅烷偶联剂改性，氧化石墨烯改性，在织物和光催化剂之间建立保护层，不仅能够增强织物强力，还能够提高催化剂稳定性，增加光电子分离，提高光催化效率，是一个可实现工业化生产和实际应用的环保工艺技术。
本发明的制备方法成本低，所用设备简单，易于工业化生产；钒酸铋插层氧化石墨烯可见光催化功能织物易加工成各种形状，使用方便；钒酸铋插层氧化石墨烯可见光催化功能织物既提高了光催化功能织物的光催化活性，又增强了光催化功能织物的强度，提升使用耐久性。
具体实施方式
具体实施例1
(1)纯棉机织布经1％羧甲基壳聚糖整理液二浸二轧后，100℃烘干，180℃焙烘1min，得到羧甲基壳聚糖改性棉织物；
(2)用分析纯磷酸一氢钠和磷酸二氢钠制备pH值为8的缓冲溶液；
(3)将0.06mol偏钒酸钠在搅拌作用下缓慢加入到30ml磷酸盐缓冲溶液中，搅拌40min，得到A液；
(4)将0.12mol硝酸铋在搅拌作用下缓慢加入到60ml磷酸盐缓冲溶液中，得到B液，然后将B液缓慢加入到A液中，得到墨绿色C液；
(5)在超声条件下，将0.1％氧化石墨烯分散于50mL磷酸盐缓冲溶液中，得到D液，然后将C液直接倒入D液；
(6)将步骤1)得到的羧甲基壳聚糖改性棉织物经润湿后加入到D液中，之后将D液升温至80℃回流20h；
(7)最后将步骤(6)得到的织物在100℃超纯水中处理30min，80℃下烘干，即得。
将本发明制得的钒酸铋插层氧化石墨烯可见光催化功能织物和普通的钒酸铋柔性光催化材料(通过原位合成法在相同织物上生长钒酸铋制得)，在同一条件下(包括光照强度，有害气体浓度、时间等)进行对比测试，其结果如下：
光催化循环10次后进行经向拉伸强力测试：测试标准参照GB/T3923.1-1997法进行，测试结果如下：
具体实施例2
(1)纯棉针织布经5％羧甲基壳聚糖整理液二浸二轧后，80℃烘干，150℃焙烘2min，得到羧甲基壳聚糖改性棉织物；
(2)用分析纯磷酸一氢钠和磷酸二氢钠制备pH值为6的缓冲溶液；
(3)将0.1mol偏钒酸钠在搅拌作用下缓慢加入到50ml磷酸盐缓冲溶液中，搅拌100min，得到A液；
(4)将0.2mol硝酸铋在搅拌作用下缓慢加入到100ml磷酸盐缓冲溶液中，得到B液，然后将B液缓慢加入到A液中，得到墨绿色C液；
(5)在超声条件下，将0.5％氧化石墨烯分散于100mL磷酸盐缓冲溶液中，得到D液，然后将C液直接倒入D液；
(6)将步骤(1)得到的羧甲基壳聚糖改性棉织物经润湿后加入到D液中，之后将D液升温至100℃回流10h；
(7)最后将步骤(6)得到的织物在100℃超纯水中处理20min，85℃下烘干，即得。
将本发明制得的钒酸铋插层氧化石墨烯可见光催化功能织物和普通的钒酸铋柔性光催化材料(通过原位合成法在相同织物上生长钒酸铋制得)，在同一条件下(包括光照强度，有害气体浓度、时间等)进行对比测试，其结果如下：
光催化循环10次后进行拉伸断裂强力测试：测试标准参照GB/T3923.1-1997标准进行，测试结果如下：
上述内容是结合具体实施例，进一步阐述本发明。应理解，这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解，在阅读了本发明讲授的内容之后，本领域技术人员可以对本发明作各种改动或修改，这些等价形式同样落于本申请所附权利要求书所限定的范围。
Claims (9)
1.一种钒酸铋插层氧化石墨烯可见光催化功能织物的制备方法，其特征在于：包括如下步骤：
(1)将纯棉织物经羧甲基壳聚糖整理液二浸二轧后，80～100℃烘干，150～180℃焙烘1～3min，得到羧甲基壳聚糖改性棉织物；然后将羧甲基壳聚糖改性棉织物经KH-550硅烷偶联剂水溶液二浸二轧后，80～100℃烘干4～8min，得到硅烷偶联剂改性棉织物；然后将改性棉织物加入到超声分散的氧化石墨烯溶液中，调节pH值7～8.5，温度50～60℃超声反应12～24h，水洗至中性，真空烘干，得到增强石墨烯改性棉织物；
(2)在搅拌条件下依次将偏矾酸钠、增强石墨烯改性棉织物、硝酸铋加入到磷酸盐缓冲溶液，搅拌30～60min得到墨绿色溶液；其中，偏钒酸钠与硝酸铋的摩尔量比为1:2；
(3)用碱性溶液调节pH值为7～8，升温至80～100℃回流10～20h，取出织物80℃烘干，得到钒酸铋插层氧化石墨烯可见光催化功能织物。
2.根据权利要求1所述一种钒酸铋插层氧化石墨烯可见光催化功能织物的制备方法，其特征在于：所述步骤(1)中的纯棉织物为纯棉非织造布、纯棉机织布或纯棉针织布。
3.根据权利要求1所述一种钒酸铋插层氧化石墨烯可见光催化功能织物的制备方法，其特征在于：所述步骤(1)中的羧甲基壳聚糖整理液为0.1％～5％的羧甲基壳聚糖溶液。
4.根据权利要求1所述一种钒酸铋插层氧化石墨烯可见光催化功能织物的制备方法，其特征在于：所述步骤(1)中的KH-550硅烷偶联剂水溶液浓度为1～5g/L。
5.根据权利要求1所述一种钒酸铋插层氧化石墨烯可见光催化功能织物的制备方法，其特征在于：所述步骤(1)中的氧化石墨烯溶液浓度为0.1～0.5g/L。
6.根据权利要求1所述一种钒酸铋插层氧化石墨烯可见光催化功能织物的制备方法，其特征在于：所述步骤(2)中的磷酸盐缓冲溶液由0.1mol/L磷酸二氢钠和0.1mol/L磷酸氢钠组成，pH值为6.5～7。
7.根据权利要求1所述一种钒酸铋插层氧化石墨烯可见光催化功能织物的制备方法，其特征在于：所述步骤(2)中的增强石墨烯改性棉织物与偏钒酸钠用量的比例为1g：0.5mmol。
8.根据权利要求1所述一种钒酸铋插层氧化石墨烯可见光催化功能织物的制备方法，其特征在于：所述步骤(2)中的增强石墨烯改性棉织物与磷酸盐缓冲溶液的比例为1g：50～100mL。
9.根据权利要求1所述一种钒酸铋插层氧化石墨烯可见光催化功能织物的制备方法，其特征在于：所述步骤(3)中的碱性溶液为浓度为0.1～1mol/L的氢氧化钠水溶液。
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