CN111617633A - 一种多壳层光催化剂和活性炭复合降解VOCs的制备方法 - Google Patents
一种多壳层光催化剂和活性炭复合降解VOCs的制备方法 Download PDFInfo
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Abstract
本发明公开了一种多壳层光催化剂和活性炭复合降解VOCs的制备方法，包括以下步骤：S1制备三层空心SiO2纳米球，S2以SiO2为模板加入钛源后进行水热反应制备出多壳层的光催化剂TiO2，S3在多壳层TiO2上面负载一定比例的贵金属，S4将负载贵金属的TiO2与比例适当的活性炭均匀混合，得到复合材料。本发明方法制备的复合材料不仅可以提供较大的比表面积，而且其内部空腔可以实现光的多重反射从而产生更多的光生空虚，并结合了活性炭丰富的孔径结构，可以实现吸附和降解VOCs同时进行，是一种高效、节能的降解VOCs新型材料。
Description
技术领域
本发明涉及挥发性有机物降解技术领域，尤其是涉及一种多壳层光催化剂和活性炭复合降解VOCs的制备方法。
背景技术
挥发性有机化合物(VOCs)属于典型气态的污染物，其不仅造成环境污染，而且对人类的呼吸系统和神经系统会造成潜在的危害。因此目前对VOCs的治理是环保行业的重点工作内容之一。光催化氧化法因成本低廉、反应条件温和等优点，是当前研究处理VOCs较热门的方法之一，主要原理是利用光催化剂吸收光子产生的空穴的氧化性，将吸附在催化剂表面的VOCs进行降解处理，转化为水和二氧化碳。但传统的光催化剂材料具有较大的颗粒，入射光无法穿透过材料，所以只能吸收一小部分光照，而大部分的入射光都会被反射，极大地限制了对入射光的利用率。而且因其比表面积较小，吸附能力弱，反应位点小，不利于提高VOCs的降解率。
发明内容
发明目的：为了克服背景技术的不足，本发明公开了一种多壳层光催化剂和活性炭复合降解VOCs的制备方法。
技术方案：本发明的多壳层光催化剂和活性炭复合降解VOCs的制备方法，其特征在于，包括以下步骤：
S1合成多壳层SiO2纳米球模板
将CTAB添加到浓氨水、无水乙醇和水的混合物中搅拌均匀，再在溶液中分三次加入BTSE和TEOS的混合物，每次加入后搅拌均匀，收集有机硅球，将其重新分散在水中，并加热完成多界面转化得到三层空心SiO2纳米球模板；
S2多壳层催化剂TiO2的制备
将获得的多壳层SiO2纳米球模板超声分散在无水乙醇中，加入的十二胺和浓氨水搅拌，再加入异丙醇钛搅拌后，进行离心烘干，将样品在乙醇和盐酸的混合液中洗涤，然后用去离子水将其洗至溶液呈中性，离心烘干，将样品加入到乙醇和氨水混合进行水热反应，用去离子水洗至中性后烘干，得TiO2粉体；
S3多壳层TiO2上负载贵金属
将氯铂酸溶液加入到TiO2粉体中烘干，再进行加热；
S4光催化剂TiO2与活性炭混合
将负载了贵金属的多壳层TiO2与活性炭混合，加入无机胶黏剂搅拌均匀，得到复合的吸附降解材料。
进一步的，S1中TEOS、BTSE、CBTA、氨水、水、无水乙醇和水的混合物的摩尔比为(0.5～5)：(0.1～4)：(0.2～2)：(11～30)：(6000～8000)：1000。
进一步的，S2中十二胺和浓氨水的比例为1:(0.4-6)。
进一步的，S2中加入异丙醇钛使SiO2和TiO2的质量比为1:(0.5-6)。
进一步的，S2中用于洗涤的乙醇和盐酸按体积比为(40-100)：1混合。
进一步的，S2中用于水热反应的乙醇和氨水的体积比为(1-4):1。
进一步的，S3中所述的氯铂酸的负载量，其中Pt的质量为光催化剂的0.1-6％。
进一步的，S4中所述得活性炭为木质炭、煤质炭、果壳炭、再生炭、矿物质原料炭的一种或多种。
进一步的，S4中TiO2与活性炭的比例为1：9～4：6。
进一步的，S4中所述的无机胶黏剂使用二氧化硅溶胶、三氧化二铝溶胶、二氧化钛溶胶、磷酸盐溶液中的一种或多种。
有益效果：与现有技术相比，本发明的优点为：本发明中多壳层TiO2光催化剂可以实现较大的比表面积以及提高对光子吸收的效率，与活性炭复合后可以利用其丰富的孔径结构，可以实现活性炭吸附VOCs后光催化剂利用光照直接将其降解，提高了VOCs的降解速率和降解效率。
附图说明
图1为本发明多壳层TiO2光催化剂TEM图；
图2为本发明制备的复合材料对甲苯的降解图。
具体实施方式
下面结合附图和实施例对本发明的技术方案作进一步的说明。
实施例1
S1合成多壳层SiO2纳米球模板
将CTAB添加到浓氨水、无水乙醇和水的混合物中搅拌均匀，再在溶液中分三次加入BTSE和TEOS的混合物，TEOS、BTSE、CBTA、氨水、水、无水乙醇和水的混合物按照1：0.6：0.78：23.6：7455：1000的摩尔比进行混合，每次加入后在1100rmp的转速下搅拌均匀，收集有机硅球，将其重新分散在去离子水中，并加热完成多界面转化得到三层空心SiO2纳米球模板；
S2多壳层催化剂TiO2的制备
称取10g多壳层SiO2纳米球模板超声分散在无水乙醇中，加入体积比为1:2的十二胺和浓氨水搅拌，再加入异丙醇钛搅拌后使SiO2和TiO2的质量比为1:2，进行离心烘干，将样品在体积比为80:1的乙醇和盐酸的混合液中洗涤6次，然后用去离子水将其洗至溶液呈中性，离心烘干，将样品加入到体积比为2:1的乙醇和氨水混合进行水热反应，用去离子水洗至中性后烘干，得TiO2粉体；
S3多壳层TiO2上负载贵金属
将1wt％的氯铂酸溶液加入到TiO2粉体中烘干，再进行加热；
S4光催化剂TiO2与活性炭混合
将负载了Pt的多壳层TiO2与木质炭按照4:6的比例进行混合，加入质量比为5％的二氧化硅溶胶搅拌均匀，得到复合的吸附降解材料。
实施例2
S1合成多壳层SiO2纳米球模板
将CTAB添加到浓氨水、无水乙醇和水的混合物中搅拌均匀，再在溶液中分三次加入BTSE和TEOS的混合物，TEOS、BTSE、CBTA、氨水、水、无水乙醇和水的混合物按照0.5：0.1：0.2：11：600：1000的摩尔比进行混合，每次加入后在1100rmp的转速下搅拌均匀，收集有机硅球，将其重新分散在去离子水中，并加热完成多界面转化得到三层空心SiO2纳米球模板；
S2多壳层催化剂TiO2的制备
称取10g多壳层SiO2纳米球模板超声分散在无水乙醇中，加入体积比为1:0.4的十二胺和浓氨水搅拌，再加入异丙醇钛搅拌后使SiO2和TiO2的质量比为1:0.5，进行离心烘干，将样品在体积比为100:1的乙醇和盐酸的混合液中洗涤6次，然后用去离子水将其洗至溶液呈中性，离心烘干，将样品加入到体积比为1:1的乙醇和氨水混合进行水热反应，用去离子水洗至中性后烘干，得TiO2粉体；
S3多壳层TiO2上负载贵金属
将0.1wt％的氯铂酸溶液加入到TiO2粉体中烘干，再进行加热；
S4光催化剂TiO2与活性炭混合
将负载了Pt的多壳层TiO2与煤质炭按照1：9的比例进行混合，加入质量比为5％的三氧化二铝溶胶搅拌均匀，得到复合的吸附降解材料。
实施例3
S1合成多壳层SiO2纳米球模板
将CTAB添加到浓氨水、无水乙醇和水的混合物中搅拌均匀，再在溶液中分三次加入BTSE和TEOS的混合物，TEOS、BTSE、CBTA、氨水、水、无水乙醇和水的混合物按照5：4：2：30：8000：1000的摩尔比进行混合，每次加入后在1100rmp的转速下搅拌均匀，收集有机硅球，将其重新分散在去离子水中，并加热完成多界面转化得到三层空心SiO2纳米球模板；
S2多壳层催化剂TiO2的制备
称取10g多壳层SiO2纳米球模板超声分散在无水乙醇中，加入体积比为1:6的十二胺和浓氨水搅拌，再加入异丙醇钛搅拌后使SiO2和TiO2的质量比为1:6，进行离心烘干，将样品在体积比为40:1的乙醇和盐酸的混合液中洗涤6次，然后用去离子水将其洗至溶液呈中性，离心烘干，将样品加入到体积比为4:1的乙醇和氨水混合进行水热反应，用去离子水洗至中性后烘干，得TiO2粉体；
S3多壳层TiO2上负载贵金属
将6wt％的氯铂酸溶液加入到TiO2粉体中烘干，再进行加热；
S4光催化剂TiO2与活性炭混合
将负载了Pt的多壳层TiO2与果壳炭、再生炭、矿物质原料炭混合物按照1：2的比例进行混合，加入质量比为5％的二氧化钛溶胶、磷酸盐溶液混合物搅拌均匀，得到复合的吸附降解材料。
图1中所示为多壳层光催化剂TiO2的TEM图，可以看出按照本专利所述方法合成了3壳层的TiO2。图2所示为多壳层TiO2和活性炭的复合材料在400nm可见光下降解甲苯曲线图。
Claims (10)
1.一种多壳层光催化剂和活性炭复合降解VOCs的制备方法，其特征在于，包括以下步骤：
S1合成多壳层SiO2纳米球模板
将CTAB添加到浓氨水、无水乙醇和水的混合物中搅拌均匀，再在溶液中分三次加入BTSE和TEOS的混合物，每次加入后搅拌均匀，收集有机硅球，将其重新分散在水中，并加热完成多界面转化得到三层空心SiO2纳米球模板；
S2多壳层催化剂TiO2的制备
将获得的多壳层SiO2纳米球模板超声分散在无水乙醇中，加入的十二胺和浓氨水搅拌，再加入异丙醇钛搅拌后，进行离心烘干，将样品在乙醇和盐酸的混合液中洗涤，然后用去离子水将其洗至溶液呈中性，离心烘干，将样品加入到乙醇和氨水混合进行水热反应，用去离子水洗至中性后烘干，得TiO2粉体；
S3多壳层TiO2上负载贵金属
将氯铂酸溶液加入到TiO2粉体中烘干，再进行加热；
S4光催化剂TiO2与活性炭混合
将负载了贵金属的多壳层TiO2与活性炭混合，加入无机胶黏剂搅拌均匀，得到复合的吸附降解材料。
2.根据权利要求1所述得多壳层光催化剂和活性炭复合降解VOCs的制备方法，其特征在于：S1中TEOS、BTSE、CBTA、氨水、水、无水乙醇和水的混合物的摩尔比为(0.5～5)：(0.1～4)：(0.2～2)：(11～30)：(6000～8000)：1000。
3.根据权利要求1所述得多壳层光催化剂和活性炭复合降解VOCs的制备方法，其特征在于：S2中十二胺和浓氨水的比例为1:(0.4-6)。
4.根据权利要求1所述得多壳层光催化剂和活性炭复合降解VOCs的制备方法，其特征在于：S2中加入异丙醇钛使SiO2和TiO2的质量比为1:(0.5-6)。
5.根据权利要求1所述得多壳层光催化剂和活性炭复合降解VOCs的制备方法，其特征在于：S2中用于洗涤的乙醇和盐酸按体积比为(40-100)：1混合。
6.根据权利要求1所述得多壳层光催化剂和活性炭复合降解VOCs的制备方法，其特征在于：S2中用于水热反应的乙醇和氨水的体积比为(1-4):1。
7.根据权利要求1所述得多壳层光催化剂和活性炭复合降解VOCs的制备方法，其特征在于：S3中所述的氯铂酸的负载量，其中Pt的质量为光催化剂质量的0.1-6％。
8.根据权利要求1所述得多壳层光催化剂和活性炭复合降解VOCs的制备方法，其特征在于：S4中所述得活性炭为木质炭、煤质炭、果壳炭、再生炭、矿物质原料炭的一种或多种。
9.根据权利要求1所述得多壳层光催化剂和活性炭复合降解VOCs的制备方法，其特征在于：S4中TiO2与活性炭的比例为1：9～4：6。
10.根据权利要求1所述得多壳层光催化剂和活性炭复合降解VOCs的制备方法，其特征在于：S4中所述的无机胶黏剂使用二氧化硅溶胶、三氧化二铝溶胶、二氧化钛溶胶、磷酸盐溶液中的一种或多种。
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