CN106582611A - 一种有机污染物光降解催化剂的制备方法 - Google Patents

一种有机污染物光降解催化剂的制备方法 Download PDF

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CN106582611A
CN106582611A CN201611166581.1A CN201611166581A CN106582611A CN 106582611 A CN106582611 A CN 106582611A CN 201611166581 A CN201611166581 A CN 201611166581A CN 106582611 A CN106582611 A CN 106582611A
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李子真
杨光
李青云
李春虎
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QINGDAO HAIKE LVBANG ENVIRONMENTAL PROTECTION TECHNOLOGY Co.,Ltd.
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Abstract

本发明公开了一种有机污染物光降解催化剂的制备方法，其特征是以规整陶瓷为载体，经激光打出阵列孔和高锰酸钾活化处理后，再超声负载含BiVO4、TiO2和石墨烯的溶胶‑凝胶，真空干燥，最后经高温煅烧制备出规整陶瓷负载BiVO4‑TiO2‑石墨烯的工业有机污染物光降解催化剂。本发明的光降解催化剂在等离子发射（UV）灯辐射下，可同时具有等离子放电释放分子自由基与光催化产生超氧自由基和羟基自由基，进而高效、彻底降解各种含硫、含氮、含氨、含酚、含多环芳烃（PHAs）、含农药、含抗生素、含病毒、含细菌等有毒、有害、恶臭工业废气和工业有机污染物。

Description

一种有机污染物光降解催化剂的制备方法
技术领域
本发明涉及一种光降解催化剂的制备方法，具体涉及一种以规整陶瓷为载体的工业有机污染物光降解催化剂的制备方法。
背景技术
众所周知，工业废气和废水中的有机污染物，其物化性质大都带有恶臭、有毒，有害和致畸性等，已成为影响人们身体健康，大气雾霾的主要元凶。目前处理这类工业废气和废水的技术主要为：活性炭吸附法，光催化法，等离子体法，催化燃烧法和生物法等，采用的工艺流程大都为串联一系列这些不同的物理、化学和生物等处理技术。如，以光催化剂为例，要么以单纯TiO2光催化剂为活性组分，导致光催化剂活性只能在紫外光下相应，且TiO2光催化剂电子-空穴复合快，电子利用率低，光催化剂活性低，对键能大的工业有机污染物分子无法快速降解。
发明内容
针对上述问题，本发明专利的目的是提供一种高效简单、运行成本低的规整陶瓷负载BiVO4-TiO2-石墨烯的有机污染物光降解催化剂的制备方法。
本发明以抗酸碱腐蚀、海水腐蚀与单位体积比表面积大的规整陶瓷为载体，超声负载BiVO4、钛酸正丁酯和石墨烯三者混合而成的溶胶-凝胶液，再经高温煅烧制备出规整陶瓷负载BiVO4-TiO2-石墨烯的有机污染物光降解催化剂。在等离子（UV）灯或可见光下，均可同时在规整陶瓷负载BiVO4-TiO2-石墨烯光催化表面产生超氧自由基和羟基自由基，进而高效、彻底降解各种含硫、含氮、含氨、含酚、含多环芳烃（PHAs）、含农药、含抗生素、含病毒、含细菌等有毒、有害、恶臭工业废气和工业废水中的有机污染物。
本发明具体的技术方案如下：
一种有机污染物光降解催化剂的制备方法，其特征是包括以下步骤：（1）首先对规整陶瓷载体进行预处理：将规整陶瓷放入激光打孔机内，调整激光束的直径、阵列和功率，打出不同直径的小孔；（2）将激光打孔处理过的规整陶瓷载体放入超声反应釜中，在60-80℃下用0.2-0.4M KMnO4水溶液浸泡处理0.5~2.0h，然后放置24h，之后水洗至水洗液pH≥6.5为止；（3）将上述规整陶瓷载体进行负载处理，过程如下：将30ml钛酸四丁酯溶于100ml无水乙醇中，搅拌后加入20ml乙二醇和10ml市场上购买的石墨烯溶胶和10ml Bi(NO3)3 •5H2O与NH4VO4摩尔比为1:1的乙醇混合液，在20-60℃下搅拌2h得到混合胶体溶液，然后将处理后的规整陶瓷载体加入该胶体溶液中，35-50℃下超声真空浸渍24h；（4）取出上述在表面和微孔内负载了含TiO2、BiVO4和石墨烯前躯体溶胶-凝胶的规整陶瓷载体于110℃干燥2-4h；然后于350-650℃下焙烧2-4h，即制得规整陶瓷负载BiVO4-TiO2-石墨烯的有机污染物光降解催化剂。
所述规整陶瓷为波纹状规整陶瓷，堆密度为350~650kg/m3、体积比表面积为100~300m2/m3、水浸润性好。
所述规整陶瓷上孔的直径为Φ0.1、0.2或0.3mm，所述孔的排列是正方形阵列或者三角形阵列。
本发明的催化剂在等离子（UV）灯辐射下，可同时具有等离子放电释放分子自由基与光催化产生超氧自由基和羟基自由基，进而高效、彻底降解各种含硫、含氮、含氨、含酚、含多环芳烃（PHAs）、含农药、含抗生素、含病毒、含细菌等有毒、有害、恶臭工业废气和工业有机污染物。具有简单高效、运行成本低、无二次污染的优点，可广泛用于各种工业有机污染物的降解处理。
具体实施方式
下面结合具体实例来进一步说明本发明专利。
实施例1：
（1）首先对规整陶瓷载体进行预处理：将一定体积的规整陶瓷放入激光打孔机内，调整激光束的直径、阵列和功率，打出直径为Φ0.2 mm正方形阵列排列的小孔；（2）将激光打孔处理过的规整陶瓷载体放入超声反应釜中，在80℃下用0.2M KMnO4水溶液浸泡处理2.0h，然后放置24h，之后水洗至水洗液pH≥6.5为止；（3）将上述规整陶瓷载体进行负载处理，过程如下：将30ml钛酸四丁酯溶于100ml无水乙醇中，搅拌后加入20ml乙二醇和10ml的市场上购买的石墨烯溶胶和10ml Bi(NO3)3 •5H2O与NH4VO4（摩尔比1:1）的乙醇混合液，在30℃温度下搅拌2h得到混合胶体溶液，然后将150ml 处理后的规整陶瓷载体加入该混合胶体溶液中，50℃下超声真空浸渍24h；（4）取出上述在表面和微孔内负载了含TiO2、BiVO4和石墨烯前躯体溶胶-凝胶的规整陶瓷载体于110℃干燥4h；然后于350℃下焙烧4h，即制得规整陶瓷负载BiVO4-TiO2-石墨烯的有机污染物光降解催化剂。
实施例2：
以规整陶瓷载体负载BiVO4-TiO2-石墨烯的工业有机污染物光降解催化剂降解甲醇为例。其活性测试在Φ50 x1000mm的固定床反应器内进行，以甲醇为工业有机污染物模拟化合物，模拟工业有机污染物废气中的组成为：甲醇 800~ 2000mg/m3、O2 0~10%、水汽为0~12%，其余由N2平衡。其脱除反应温度为40℃~120℃，常压，该光催化剂的空速为800-5000 h-1，采用300W的UV发射灯和可见光灯，最终测试其甲醇降解率达99%。
实施例3：
以规整陶瓷载体负载BiVO4-TiO2-石墨烯的工业有机污染物光降解催化剂降解工业废水为例。其废水COD为1200mg/L，其COD消解活性测试在Φ50 x1000mm的固定床反应器内进行，在反应温度为20℃~60℃，常压，该光催化剂的空速为1-10 h-1，采用30W的H型UV发射灯和可见光灯，最终测试废水COD降解率达98%。
以上所述，仅为本发明的具体实施方式，但本发明的保护范围并不局限于此，任何不经过创造性劳动想到的变化或替换，都应涵盖在本发明的保护范围之内。因此，本发明的保护范围应该以权利要求书所限定的保护范围为准。

Claims (4)

1.一种有机污染物光降解催化剂的制备方法，其特征在于包括以下步骤：（1）首先对规整陶瓷载体进行预处理：将规整陶瓷放入激光打孔机内，调整激光束的直径、阵列和功率，打出不同直径的小孔；（2）将激光打孔处理过的规整陶瓷载体放入超声反应釜中，在60-80℃下用0.2-0.4M KMnO4水溶液浸泡处理0.5~2.0h，然后放置24h，之后水洗至水洗液pH≥6.5为止；（3）将上述规整陶瓷载体进行负载处理，过程如下：将30ml钛酸四丁酯溶于100ml无水乙醇中，搅拌后加入20ml乙二醇和10ml石墨烯溶胶和10ml Bi(NO3)3 •5H2O与NH4VO4摩尔比为1:1的乙醇混合液，在20-60℃下搅拌2h得到混合胶体溶液，然后将处理后的规整陶瓷载体加入该胶体溶液中，35-50℃下超声真空浸渍24h；（4）取出上述在表面和微孔内负载了含TiO2、BiVO4和石墨烯前驱体溶胶-凝胶的规整陶瓷载体于110℃干燥2-4h；然后于350-650℃下焙烧2-4h，即制得规整陶瓷负载BiVO4-TiO2-石墨烯的有机污染物光降解催化剂。
2.根据权利要求1所述的制备方法，其特征在于所述规整陶瓷为波纹状规整陶瓷，堆密度为350~650kg/m3，体积比表面积为100~300m2/m3。
3.根据权利要求1所述的制备方法，其特征在于所述孔的排列是正方形阵列或者三角形阵列。
4.根据权利要求1所述的制备方法，其特征在于所述规整陶瓷上孔的直径为Φ0.1、0.2或0.3mm。
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CN105597728A (zh) * 2016-02-25 2016-05-25 电子科技大学 二氧化钛/钛酸铋超声强化型光催化剂及其制备方法
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CN108043383B (zh) * 2017-12-15 2020-07-17 沈阳理工大学 一种光催化陶瓷波纹填料的制备方法
CN110624532A (zh) * 2019-09-19 2019-12-31 华南理工大学 一种TiO2-BiVO4-石墨烯三元复合光催化材料及其制备方法
CN110624532B (zh) * 2019-09-19 2021-08-10 华南理工大学 一种TiO2-BiVO4-石墨烯三元复合光催化材料及其制备方法
CN110813315A (zh) * 2019-11-24 2020-02-21 南京公诚节能新材料研究院有限公司 一种用于有机污水处理的光降解催化剂及其制备方法
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