CN109225181B - 一种中空硼玻璃微球@TiO2催化剂的制备方法及其用途 - Google Patents
一种中空硼玻璃微球@TiO2催化剂的制备方法及其用途 Download PDFInfo
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Abstract
本发明属于无机催化领域,提供了一种中空硼玻璃微球@TiO2催化剂的制备方法及其用途。制备步骤如下:在85℃水浴加热和搅拌的条件下向烧杯中加入去离子水和中空硼玻璃微球,同时加入一定量的NaOH溶液和TiCl4盐酸溶液,调整pH=2,反应3h,反应完全后用去离子水洗涤,样品在干燥箱烘干,制成中空硼玻璃微球@TiO2核壳结构光催化剂。该催化剂用于可见光条件下光催化降解水中的氨。本发明的显著特征在于,所采用的中空硼玻璃微球@TiO2催化剂具有很高的光催化降解氨的活性。
Description
技术领域
本发明属于无机催化领域,涉及一种中空硼玻璃微球@TiO2催化剂的制备方法和在可见光照射下催化降解氨的用途。
背景技术
随着人类进步发展,环境污染也日趋严重,清除水体中的有害物质成为环境科学界的一个重要问题。
水中无机污染物的种类常见的有氨氮、含氮氧化合物和氰离子等。我国在2015年明确规定水污染中氨氮直接排放量不大于10mg/L。水体中氨氮主要来源于生活污水、工业废水等,过多的氨化合物会恶化水的质量,对水中鱼类、植物、人体都有较大危害。游离氨对鱼类致死量仅为1mg/L,并且在硝化细菌作用下氧化成亚硝酸盐的硝酸盐,氧化1mg/L氨氮需要 4.6mg/L的溶解氧,影响了水的质量。对人体而言,硝酸盐和亚硝酸盐有可能转变为亚硝胺,对人体健康造成威胁,由此,降低水中氨氮含量成为了一项重要课题。
近年来,光催化氧化作为极具有前途的水处理工艺,是一种从水中除去污染物的高级氧化法。光催化氧化降解与其他降解氨氮方法相比有明显的优点与特点:光催化氧化可直接将氨氮氧化为氨气;无选择的降解污染物;同生物硝化降解氨氮的方法相比,提高对生物有毒的或难以生化的有机物质的可生化能力;近年来,提高光催化氧化降解氨的效率也是目前研究的热点。
发明内容
本发明采用水热法将TiO2负载在中空微球上,可见光作为光源,制作中空硼玻璃微球 @TiO2异质结复合材料来降解氨并且具有良好的催化剂活性。
本发明旨在开发一种高催化活性催化剂,在可见光照射下,用于降解水中氨。本发明所说的中空硼玻璃微球@TiO2催化剂的方法,TiO2作为催化剂的光催化效果显著,而中空微球是一种表面无孔,里面充有空气、二氧化碳等气体,成全封闭中空结构的微小球体,一般颗粒直径为10~50μm。其中,以二氧化硅、玻璃系微球最为常见。由于中空微球有比重小、导热率低、不吸水、介电常数低等特别性能,这种新型材料已受到人们的重大重视。本发明是通过如下技术方案实现的:
一种中空硼玻璃微球@TiO2催化剂,所述材料以中空硼玻璃微球作为TiO2的载体,TiO2作为光催化活性组分;TiO2质量为中空硼玻璃微球的总质量的5%~20%。
一种中空硼玻璃微球@TiO2催化剂的制备方法,包括如下步骤:
将TiCl4纯溶液缓缓加入到一定体积的稀盐酸中,得到TiCl4盐酸溶液;
称取一定量的中空硼玻璃微球,加入蒸馏水分散均匀,水浴加热,采用蠕动泵同时加入 NaOH溶液和TiCl4盐酸溶液,调节溶液pH=2;加入完毕后,继续反应;反应完成后用去离子水抽滤至中性,干燥,制备得到中空硼玻璃微球@TiO2催化剂。
TiCl4溶液的浓度为1.5mol/L,所述NaOH溶液的质量百分浓度为5wt.%。
所述产物中空硼玻璃微球@TiO2催化剂中,TiO2质量为中空硼玻璃微球的总质量的5%~20%。
水浴加热的温度为85℃。
采用蠕动泵同时加入NaOH溶液和TiCl4盐酸溶液时,加入时间控制在在半小时,加入完毕后,继续反应时间为3h。
所述干燥温度为120℃,干燥时间为24h。
将本发明制备的中空硼玻璃微球@TiO2催化剂用于光催化降解氨的用途,步骤如下:
配制不同浓度的氨溶液,然后用NaOH溶液调节pH到8~11,分别加入一定量的中空硼玻璃微球@TiO2催化剂,在光催化反应仪上进行反应。
取样测试,在25℃下连续取样11h,并在分光度计测定反应后样品的吸光度,采用水杨酸法计算其氨含量。
所述氨溶液中氨的含量为10~50mg/L,氨溶液和中空硼玻璃微球@TiO2催化剂的用量比例为200mL:0.1g。
本发明的有益效果:
(1)本发明所制备的中空硼玻璃微球@TiO2催化剂,在反应过程中具有良好的催化活性和稳定性;
(2)降解比较彻底,实验证明,只要在pH大于等于10时,只要反应足够长时间,氨都可以被完全降解。
具体实施方式
下面结合具体实施例多本发明作进一步说明:
实施例1
称取5g NaOH溶于95mL蒸馏水中配制成质量分数为5%的NaOH溶液,量取300mL 质量分数为37%浓盐酸溶液溶于700mL蒸馏水中配制成质量分数为3mol/L的稀盐酸,将165mL的TiCl4纯溶液缓缓加入500mL的稀盐酸中,滴加时需持续搅拌,再加入稀盐酸至1 L,制作完毕1.5mol/L的TiCl4盐酸溶液;
称取100g的中空硼玻璃微球和500mL的蒸馏水放入2L烧杯中,然后在85℃水浴加热和搅拌的条件下同时加入质量分数为5%的NaOH溶液和1.5mol/L的TiCl4盐酸溶液84mL,控制溶液pH=2,控制加入时间在半小时左右;加入完毕后,再反应3h;反应完成后用去离子水抽滤至中性,在120℃的干燥箱中干燥24h,制备出TiO2负载量为10%的中空硼玻璃微球@TiO2催化剂。
光催化降解氨溶液:
称取0.185g纯度为27%的氨水,加入1L的容量瓶中并稀释至1L,制成50mg/L的氨溶液;采用光催化反应装置,加入催化剂0.1g,在反应温度为25℃下,反应时溶液pH为8 下连续取样l1h,过滤出水溶液,用水杨酸法测试水中氨含量,计算转化率。测试的结果经过计算列于表1。
表1.TiO2负载量为10%的中空硼玻璃微球@TiO2(pH=8)降解50mg/L的氨溶液的不同时间段的转化率结果表
实施例2
同实施例1,但改变氨溶液的初始浓度,分别称取0.111g,0.037g氨水使氨溶液的初始浓度分别为30mg/L,10mg/L,反应11h之后的转化率所得结果见表2。
表2.TiO2负载量为10%的中空硼玻璃微球@TiO2光催化降解氨溶液的转化率结果表
实施例3
同实施例1,改变具体实施例中TiCl4溶液加入量为42mL,制备含量为5%的催化剂,反应11h之后的转化率所得结果见表3。
表3.TiO2负载量为5%的中空硼玻璃微球@TiO2光催化降解氨溶液的转化率结果表
实施例4
同实施例1,改变具体实施例中TiCl4溶液加入量为168mL,制备含量为20%的催化剂,反应11h之后的转化率所得结果见表4。
表4.TiO2负载量为20%的中空硼玻璃微球@TiO2光催化降解氨溶液的转化率结果表
实施例5
同实施例1,但改变氨溶液反应的pH值,改变降解反应时的pH,在降解反应11h后的所得结果见表5。
表5.TiO2负载量为10%的中空硼玻璃微球@TiO2光催化降解氨溶液转化率结果表
实施例6
同实施例1,改变TiO2负载量,初始浓度为50mg/L,光催化降解反应11h后的所得结果见表6。
表6.不同负载量的中空硼玻璃微球@TiO2光催化降解氨溶液转化率结果表
Claims (3)
1.一种中空硼玻璃微球@TiO2催化剂用于可见光下光催化降解氨的用途,所述中空硼玻璃微球@TiO2催化剂中,以中空硼玻璃微球作为TiO2的载体,TiO2作为光催化活性组分;TiO2质量为中空硼玻璃微球的总质量的5%~20%,其特征在于,光催化降解氨的步骤如下:
配制不同浓度的氨溶液,然后用NaOH溶液调节pH到8~11,分别加入一定量的中空硼玻璃微球@TiO2催化剂,在光催化反应仪上进行反应。
2.根据权利要求1所述的用途,其特征在于,所述的氨溶液中氨的含量为10~50mg/L,氨溶液和中空硼玻璃微球@TiO2催化剂的用量比例为200mL:0.1g。
3.根据权利要求1所述的用途,其特征在于,所述中空硼玻璃微球@TiO2催化剂的制备步骤为:将TiCl4纯溶液缓缓加入到一定体积的稀盐酸中,得到TiCl4盐酸溶液;称取一定量的中空硼玻璃微球,加入蒸馏水分散均匀,85℃水浴加热,采用蠕动泵同时加入质量百分浓度为5wt.%的NaOH溶液和浓度为1.5mol/L的TiCl4盐酸溶液,调节溶液pH=2;加入时间控制在半小时,加入完毕后,继续反应3h;反应完成后用去离子水抽滤至中性,120℃干燥24h。
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