CN113262772A - 一种高光催化效率纳米复合材料的制备方法 - Google Patents
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Abstract
本发明公开了一种高光催化效率纳米复合材料的制备方法,以石墨粉为原料、浓硫酸和高锰酸钾作为氧化剂,采用改进的Hummers法制备得到氧化石墨烯;以氧化石墨烯为前驱物与二氧化钛在水热条件下反应生成石墨烯‑二氧化钛纳米复合材料,或者在反应物中加入氮源或钒源至少一种,制备得到掺杂改性的石墨烯‑二氧化钛纳米复合材料。该光催化材料具有化学性质稳定、光催化活性高、没有毒性、容易制备且成本低廉等特点,在污水处理领域有巨大的应用潜力,具有现实意义,可以在实际应用中推广。
Description
技术领域
本发明属于光催化剂技术领域,特别是涉及一种高光催化效率纳米复合材料的制备方法。
背景技术
自然水体的污染已经成为现代社会一个主要的环境问题,尤其是印染工业,由于其产生的染料废水以及其他难处理的物质,被列为最具有污染性的工业之一,而印染工业逐年増加的废水排放量更是使环境污染问题变得异常严峻。染料废水色度髙、难降解、毒性大,对人体有潜在的致癌性,传统的水处理法处理难度比较大。
半导体光催化技术是以利用太阳能为核心,所以光催化技术是综合应对能源和环境问题挑战的重要手段。光催化是高级的氧化技术,利用光能量生成的活性自由基可以降解大部分有机污染物,尤其在染料废水处理工艺领域得到了广泛的研究与应用。因此,为了保护生态环境,缓解工业生产对水体污染的压力,避免食物链毒害事件的发生,推动人类社会可持续发展的进行,研究制备工艺简单、化性能高效的催化剂材料具有重大的实际意义。
发明内容
为了克服传统的水处理法处理污染水体的不足和提高半导体光催化技术处理污染水体的效率的问题,本发明提供了一种高光催化效率纳米复合材料的制备方法。
本发明所采用的技术方案是:
一种高光催化效率纳米复合材料的制备方法,包括如下步骤:
步骤(a):采用改进的Hummers法制备氧化石墨烯,先将石墨预氧化,再以浓硫酸和高锰酸钾作为氧化剂与预氧化石墨反应得到氧化石墨烯;
步骤(b):分别将氧化石墨烯和TiO2加到去离子水和无水乙醇中,低温超声振荡30min-50min得到氧化石墨烯和TiO2的分散液,将两种溶液混合后用氨水调节溶液pH值至9-10之间,继续超声处理40min-60min,再将混合溶液210℃水热反应8h-12h,自然冷却后得到黑色水凝胶,用去离子水洗涤3次-5次,干燥得到石墨烯-二氧化钛纳米复合材料;
步骤(c):分别以尿素、偏钒酸铵为氮源和钒源,在反应物中加入其中至少一种,采用(b)相同的方法制备得到掺杂改性的石墨烯-二氧化钛纳米复合材料。
进一步:所述的步骤(b)中反应物中加入的氧化石墨烯的质量为5wt%-20wt%。
进一步:所述的步骤(c)中反应物中加入的尿素质量满足n(N)/n(Ti)为0.5%-5%,加入的偏钒酸铵质量满足n(V)/n(Ti)为0.1%-1%。
本发明的优点如下:
1.石墨烯-二氧化钛纳米复合材料具有化学性质稳定、光催化活性高、没有毒性、容易制备且成本低廉等特点,在污水处理领域有巨大的应用潜力,具有现实意义,可以在实际应用中推广;
2.对于改善目前面临严重的水污染问题,本发明制备的材料的光催化降解性能,相比于其他水处理技术,如活性炭吸附、化学氧化、湿空气氧化、生物处理等,有更明显的优势;
3.这个催化降解过程可以使有机污染物完全的分解以达到去污,漂白和脱臭的目的,并且也不会带来二次污染;操作简便,可以在常温常压下进行,能源消耗低;
4.石墨烯-二氧化钛纳米复合材料对于降解有机污染物有普遍适用性,同时也能光催化杀灭乳杆嗜酸菌、酵母菌、大肠杆菌等细菌真菌。
附图说明
图1为本发明所述一种高光催化效率纳米复合材料的制备方法的氮掺杂改性的扫描电镜显微形貌图;
图2为本发明所述一种高光催化效率纳米复合材料的制备方法的氮掺杂改性的能谱图;
图3为本发明所述的一种高光催化效率纳米复合材料的制备方法的用紫光处理亚甲基蓝溶液得到的催化曲线图。
具体实施方式
下面对本发明作进一步的说明,但本发明并不局限于这些内容。
实施例1
采用改进的Hummers法制备氧化石墨烯,先将石墨预氧化,再以浓硫酸和高锰酸钾作为氧化剂与预氧化石墨反应得到氧化石墨烯;分别称取30mg氧化石墨烯和120mgTiO2加到去离子水和无水乙醇中,低温超声振荡40min得到氧化石墨烯和TiO2的分散液,将两种溶液混合后用氨水调节溶液pH值至9,继续超声处理60min,将混合溶液转移至100mL聚四氟乙烯内胆水热反应釜中,210℃下水热反应10h,自然冷却后得到黑色水凝胶,用去离子水洗涤3次,干燥得到石墨烯-二氧化钛纳米复合材料。
实施例2
采用改进的Hummers法制备氧化石墨烯,先将石墨预氧化,再以浓硫酸和高锰酸钾作为氧化剂与预氧化石墨反应得到氧化石墨烯;分别称取30mg氧化石墨烯和120mgTiO2加到去离子水和无水乙醇中,低温超声振荡40min得到氧化石墨烯和TiO2的分散液,将两种溶液混合后用氨水调节溶液pH值至9,加入4.5mg尿素,继续超声处理60min,将混合溶液转移至100mL聚四氟乙烯内胆水热反应釜中,210℃下水热反应10h,自然冷却后得到黑色水凝胶,用去离子水洗涤3次,干燥得到掺氮石墨烯-二氧化钛纳米复合材料。
实施例3
采用改进的Hummers法制备氧化石墨烯,先将石墨预氧化,再以浓硫酸和高锰酸钾作为氧化剂与预氧化石墨反应得到氧化石墨烯;分别称取30mg氧化石墨烯和120mgTiO2加到去离子水和无水乙醇中,低温超声振荡40min得到氧化石墨烯和TiO2的分散液,将两种溶液混合后用氨水调节溶液pH值至9,加入2.5mg偏钒酸铵,继续超声处理60min,将混合溶液转移至100mL聚四氟乙烯内胆水热反应釜中,210℃下水热反应10h,自然冷却后得到黑色水凝胶,用去离子水洗涤3次,干燥得到掺钒石墨烯-二氧化钛纳米复合材料。
实施例4
采用改进的Hummers法制备氧化石墨烯,先将石墨预氧化,再以浓硫酸和高锰酸钾作为氧化剂与预氧化石墨反应得到氧化石墨烯;分别称取30mg氧化石墨烯和120mgTiO2加到去离子水和无水乙醇中,低温超声振荡40min得到氧化石墨烯和TiO2的分散液,将两种溶液混合后用氨水调节溶液pH值至9,加入4.5mg尿素和2.5mg偏钒酸铵,继续超声处理60min,将混合溶液转移至100mL聚四氟乙烯内胆水热反应釜中,210℃下水热反应10h,自然冷却后得到黑色水凝胶,用去离子水洗涤3次,干燥得到氮、钒共掺杂石墨烯-二氧化钛纳米复合材料。
指出的是,对于本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进,这些都属于本发明的保护范围。
Claims (3)
1.一种高光催化效率纳米复合材料的制备方法,其特征在于:包括如下步骤:
步骤(a):采用改进的Hummers法制备氧化石墨烯,先将石墨预氧化,再以浓硫酸和高锰酸钾作为氧化剂与预氧化石墨反应得到氧化石墨烯;
步骤(b):分别将氧化石墨烯和TiO2加到去离子水和无水乙醇中,低温超声振荡30min-50min得到氧化石墨烯和TiO2的分散液,将两种溶液混合后用氨水调节溶液pH值至9-10之间,继续超声处理40min-60min,再将混合溶液210℃水热反应8h-12h,自然冷却后得到黑色水凝胶,用去离子水洗涤3次-5次,干燥得到石墨烯-二氧化钛纳米复合材料;
步骤(c):分别以尿素、偏钒酸铵为氮源和钒源,在反应物中加入其中至少一种,采用(b)相同的方法制备得到掺杂改性的石墨烯-二氧化钛纳米复合材料。
2.根据权利要求1所述的一种高光催化效率纳米复合材料的制备方法,其特征在于:所述的步骤(b)中反应物中加入的氧化石墨烯的质量为5wt%-20wt%。
3.根据权利要求1所述的一种高光催化效率纳米复合材料的制备方法,其特征在于:所述的步骤(c)中反应物中加入的尿素质量满足n(N)/n(Ti)为0.5%-5%,加入的偏钒酸铵质量满足n(V)/n(Ti)为0.1%-1%。
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