CN107185511B - 一种TiO2纳米片修饰TiO2纳米纤维膜的制备方法 - Google Patents

一种TiO2纳米片修饰TiO2纳米纤维膜的制备方法 Download PDF

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CN107185511B
CN107185511B CN201710218450.1A CN201710218450A CN107185511B CN 107185511 B CN107185511 B CN 107185511B CN 201710218450 A CN201710218450 A CN 201710218450A CN 107185511 B CN107185511 B CN 107185511B
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唐潮
房明浩
黄朝晖
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China University of Geosciences Beijing
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Abstract

本发明涉及一种TiO2纳米片修饰TiO2纳米纤维膜的制备方法，属于环境处理领域。本发明以钛酸四丁酯、聚乙烯吡络烷酮、无水乙醇、乙酸、氢氟酸为主要原料，通过静电纺丝法制备TiO2纳米纤维膜，再通过溶剂热法在纤维表面修饰TiO2纳米片，最终获得TiO2纳米片修饰TiO2纳米纤维膜材料。目前粉状的光催化材料在使用后难以回收造成二次污染，负载型光催化材料比表面积较小。TiO2纳米片修饰TiO2纳米纤维膜作为一种自支撑的具有高比表面积的光催化剂材料，可以很好的解决上述两个问题。这种制备方法还可以应用于其他光催化剂材料的制备上。

Description

一种TiO2纳米片修饰TiO2纳米纤维膜的制备方法
技术领域：
本发明涉及一种TiO2纳米片修饰TiO2纳米纤维膜的制备方法，属于环境处理领域。
背景技术：
2015年中华人民共和国环境保护部环境监测司公布的淡水资源环境数据显示我国水污染严重，其中地表水Ⅳ～Ⅴ类和劣Ⅴ类水质已占到35.5％，为不可与人体接触的水源。因此对水污染的治理已经到了迫在眉睫的地步。光催化材料作为一种新型的水和大气中有机污染物降解材料，具有无能源消耗，光催化剂无毒污染、催化活性强等优势，已经有工业化产品投入实际使用，如Degussa公司生产的P25二氧化钛粉。但是粉状的光催化材料在使用后难以回收造成二次污染，负载型光催化材料比表面积较小的劣势。因此本发明提出制备一种自支撑的具有高比表面积的光催化剂材料：TiO2纳米片修饰TiO2纳米纤维膜。该材料为纤维组成的薄膜状，易于回收再利用。纤维膜上修饰的TiO2纳米片为{001}面暴露，具有较高的光催化活性，可以大幅度提高光催化剂的光催化活性。
发明内容：
本发明是鉴于粉状的光催化材料在使用后难以回收造成二次污染，负载型光催化材料比表面积较小的劣势，提出制备一种具有自支撑性的高比表面积光催化剂材料。本发明以钛酸四丁酯、聚乙烯吡络烷酮、无水乙醇、乙酸为原料，采用电纺丝法制备TiO2纳米纤维膜，将纤维膜在水热环境下，氢氟酸作为形貌控制剂，钛酸四丁酯作为钛源，制备TiO2纳米片修饰 TiO2纳米纤维膜。该纤维膜具有高比表面积、自支撑、高催化活性，达到易回收、催化活性高的目的。
本发明提出的一种TiO2纳米片修饰TiO2纳米纤维膜的制备方法，本发明涉及一种TiO2纳米片修饰TiO2纳米纤维膜的制备方法，其特征在于：采用钛酸四丁酯、聚乙烯吡络烷酮、无水乙醇、乙酸按一定比例配置前驱体溶液，采用静电纺丝法制备TiO2纳米纤维膜。将热处理后的纤维膜与钛酸四丁酯、无水乙醇、氢氟酸混合进行溶剂热反应，获得TiO2纳米片修饰 TiO2纳米纤维膜。获得的材料微观形貌图如图1，图2所示，其中图1为TiO2纳米片修饰TiO2纳米纤维膜的5000倍扫描电镜图，图2为TiO2纳米片修饰TiO2纳米纤维膜的40000倍扫描电镜图。
前驱体溶液中钛酸四丁酯浓度为0.1％～50.0％，聚乙烯吡络烷酮的浓度为0.1％～20％。静电纺丝工艺为5～40kV，接收器与喷头距离5～20cm，前驱体供给速度为0.1～10ml/h。
TiO2纳米纤维膜的热处理温度范围为100～500℃，升温速度为0.1～20℃/min。溶剂热反应物为钛酸四丁酯、氢氟酸、无水乙醇和热处理后的TiO2纳米纤维膜，在150～200℃下反应0.1～30h。
附图说明：
图1为TiO2纳米片修饰TiO2纳米纤维膜的5000倍扫描电镜图；
图2为TiO2纳米片修饰TiO2纳米纤维膜的40000倍扫描电镜图。
具体实施方式：
本发明首先采用静电纺丝法制备TiO2纳米纤维膜，经过热处理后再采用溶剂热法在纤维表面修饰TiO2纳米片。
下面通过具体实例更详细地介绍本发明，但以下实例仅用于帮助更容易地理解本发明，本发明并不限于这些实施例。
实施例1
一种TiO2纳米片修饰TiO2纳米纤维膜的制备过程：
原料：
钛酸四丁酯、聚乙烯吡络烷酮、无水乙醇、乙酸和氢氟酸
前驱体配置：
将20ml无水乙醇，5ml乙酸，5ml钛酸四丁酯和1.5g聚乙烯吡络烷酮混合，磁力搅拌2h获得前驱体溶液。
TiO2纳米纤维膜的制备：
采用静电纺丝法制备TiO2纳米纤维膜，静电纺丝工艺为：电压为25kV，针头到接收滚筒距离为15cm，滚筒转速为120r/min，21G不锈钢针头，前驱体溶液供给量为2.0ml/h。
热处理：
将纺丝获得的TiO2纳米纤维膜以1℃/min的升温速度在300℃下热处理1h。
溶剂热制备TiO2纳米片修饰TiO2纳米纤维膜：
反应釜中加入10ml无水乙醇、1.0ml钛酸四丁酯、0.6ml氢氟酸、0.02g二氧化钛纤维，在180℃的环境下反应6h，过滤获得TiO2纳米片修饰TiO2纳米纤维膜材料。
实施例2
一种TiO2纳米片修饰TiO2纳米纤维膜的制备过程：
原料：
钛酸四丁酯、聚乙烯吡络烷酮、无水乙醇、乙酸和氢氟酸
前驱体配置：
将20ml无水乙醇，5ml乙酸，5ml钛酸四丁酯和1.5g聚乙烯吡络烷酮混合，磁力搅拌2h获得前驱体溶液。
TiO2纳米纤维膜的制备：
采用静电纺丝法制备TiO2纳米纤维膜，静电纺丝工艺为：电压为15kV，针头到接收滚筒距离为15cm，滚筒转速为120r/min，21G不锈钢针头，前驱体溶液供给量为2.0ml/h。
热处理：
将纺丝获得的TiO2纳米纤维膜以1℃/min的升温速度在300℃下热处理1h。
溶剂热制备TiO2纳米片修饰TiO2纳米纤维膜：
反应釜中加入10ml无水乙醇、1.0ml钛酸四丁酯、0.6ml氢氟酸、0.02g二氧化钛纤维，在190℃的环境下反应10h，过滤获得TiO2纳米片修饰TiO2纳米纤维膜材料。
实施例3
一种TiO2纳米片修饰TiO2纳米纤维膜的制备过程：
原料：
钛酸四丁酯、聚乙烯吡络烷酮、无水乙醇、乙酸和氢氟酸
前驱体配置：
将20ml无水乙醇，5ml乙酸，5ml钛酸四丁酯和1.5g聚乙烯吡络烷酮混合，磁力搅拌2h获得前驱体溶液。
TiO2纳米纤维膜的制备：
采用静电纺丝法制备TiO2纳米纤维膜，静电纺丝工艺为：电压为20kV，针头到接收滚筒距离为20cm，滚筒转速为120r/min，21G不锈钢针头，前驱体溶液供给量为2.0ml/h。
热处理：
将纺丝获得的TiO2纳米纤维膜以1℃/min的升温速度在300℃下热处理1h。
溶剂热制备TiO2纳米片修饰TiO2纳米纤维膜：
反应釜中加入10ml无水乙醇、1.0ml钛酸四丁酯、0.6ml氢氟酸、0.02g二氧化钛纤维，在200℃的环境下反应4h，过滤获得TiO2纳米片修饰TiO2纳米纤维膜材料。

Claims (2)

1.一种TiO2纳米片修饰TiO2纳米纤维膜的制备方法，其特征在于：采用钛酸四丁酯、聚乙烯吡咯烷酮、无水乙醇、乙酸按一定比例配置前驱体溶液，采用静电纺丝法制备TiO2纳米纤维膜；将热处理后的纤维膜与钛酸四丁酯、无水乙醇、氢氟酸混合进行溶剂热反应，获得TiO2纳米片修饰TiO2纳米纤维膜，
其中前驱体溶液中钛酸四丁酯浓度为0.1％～50.0％，聚乙烯吡咯烷酮的浓度为0.1％～20％，
静电纺丝工艺为：电压为5～40kV，接收器与喷头距离为15～20cm，前驱体供给速度为0.1～10ml/h，和
其中TiO2纳米纤维膜的热处理温度范围为100～300℃，升温速度为0.1～20℃/min，
溶剂热反应物为钛酸四丁酯、氢氟酸、无水乙醇和热处理后的TiO2纳米纤维膜，在150～200℃下反应4～10h。
2.根据权利要求1所述的TiO2纳米片修饰TiO2纳米纤维膜的制备方法，其特征在于：前驱体溶液配制和溶剂热反应物配制过程中，药品的加入顺序无先后之分。
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