CN107684917A - 一种Mn1Cd3S4光催化剂的制备方法 - Google Patents
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Abstract
本发明公开一种Mn1Cd3S4光催化剂的制备方法,以无水氯化锰、硝酸镉和硫代乙酰胺为原料制备水相,以环己烷为油相,以Span85和OP‑4的混合物为乳化剂,通过反相乳液法制备Mn1Cd3S4光催化剂。本发明具有工艺稳定、能耗小、产品收率高、产品尺寸均一和产品粒径小的优点。
Description
技术领域
本发明涉及一种Mn1Cd3S4光催化剂的制备方法。
背景技术
随着人类社会的快速发展,在能源过度消耗的同时环境的的治理并未跟上步伐,因此造成了能源紧张和环境污染的问题。以半导体光催化技术为基础的光解水制氢和光催化分解成为了解决上述两个问题的最有前景的方法。硫化镉是一种重要的宽带隙半导体,其禁带宽度为2.42ev,表现出很多新奇的非线性光学性质,因而在光催化、发光、材料、生物检测、太阳能电池等领域具有广阔的应用前景。但是硫化镉存在光生空穴和光生电子的分离效率低且容易被腐蚀的缺点,使得硫化镉的应用发展受到阻碍,将与硫化锰硫化镉融合是解决这一问题的有效方法,其中Mn1Cd3S4表现出良好的催化性能。
光催化剂的催化效率不仅受禁带宽度影响,其本体的比表面积也是一个重要的印象因素,因此,一种高效、稳定的小粒径Mn1Cd3S4光催化剂的制备方法成为了解决问题的关键。
发明内容
本发明提供一种Mn1Cd3S4光催化剂的制备方法,采用反相微乳液法制备出Mn1Cd3S4,制备效率高,制备工艺稳定、可重复性好。
为解决上述技术问题,本发明采用如下技术方案:
一种Mn1Cd3S4光催化剂的制备方法,包括以下步骤:
S1.按重量份数计,取1.26份无水氯化锰和7.1份硝酸镉加入到30份水中形成A溶液,A溶液置于常温下保存;取3份硫代乙酰胺加入15份水中形成B溶液,B溶液置于常温下保存;硫代乙酰胺的稳定性与水溶性好,有利于增强本发明的工艺稳定性;
S2.按重量份数计,取450~540份环己烷加入三口烧瓶中,再向三口瓶中加入5~15份乳化剂并在常温水浴下以300~500r/min的转速搅拌,使得乳化剂与环己烷混合均匀,然后将S1中的A溶液和B溶液混合再逐滴加入到三口烧瓶中,向三口瓶中持续通氮气并将搅拌转速升至1000~1200r/min,再将水浴温度升至60~65℃反应3~5h;乳化剂用于使得A溶液和B溶液在环己烷中形成稳定的微乳液,通氮气使得反应更加稳定,有利于形成均一的Mn1Cd3S4;
S3.等S2反应结束后将搅拌转速降低至300~400r/min,然后向三口烧瓶中加入乙醇破乳,再过滤得到滤渣,将滤渣用去离子水和丙酮反复洗涤三次得,最后将滤渣冷冻干燥得到Mn1Cd3S4光催化剂;冷冻干燥能避免Mn1Cd3S4光催化剂晶粒变化。
进一步地,所述乳化剂由OP-4和Span85组成,Span85的质量占乳化剂质量的43%~66%。
进一步地,S2中水浴温度上升的时间为0.3~0.5h,这段时间能够让A溶液和B溶液加入环己烷中后充分乳化。
本发明的有益效果:
本发明的制备工艺简单,无需高温高压的反应环境,对设备要求低,生产过程的能耗低;本发明的工艺稳定,反应原料性能稳定且微乳液系统稳定,工艺的操作难度低;产品制备效率高,本发明反应时间长,反应充分因此产品收率高,反应在微乳液中进行,微乳液限定了产物的尺寸,无需担心反应时间长产品的晶粒生长;本发明制备出的Mn1Cd3S4光催化剂尺寸均一,平均粒径为6nm。
附图说明
图1为本发明Mn1Cd3S4光催化剂的扫描电镜图;
图2为本发明Mn1Cd3S4光催化剂的XRD图谱。
具体实施方式
以下参考具体实施例对本发明做进一步说明。
实施例1
一种Mn1Cd3S4光催化剂的制备方法:
S1.按重量份数计,取1.26份无水氯化锰和7.1份硝酸镉加入到30份水中形成A溶液,A溶液置于常温下保存;取3份硫代乙酰胺加入15份水中形成B溶液,B溶液置于常温下保存;
S2.按重量份数计,取450份环己烷加入三口烧瓶中,再向三口瓶中加入2.15份OP-4和2.75份Span85并在常温水浴下以500r/min的转速搅拌,然后将S1中的A溶液和B溶液混合再逐滴加入到三口烧瓶中,向三口瓶中持续通氮气并将搅拌转速升至1000r/min,再将水浴温度升至60℃反应5h,升温时间为0.3h;
S3.等S2反应结束后将搅拌转速降低至300r/min,然后向三口烧瓶中加入乙醇破乳,再过滤得到滤渣,将滤渣用去离子水和丙酮反复洗涤三次得,最后将滤渣冷冻干燥得到Mn1Cd3S4光催化剂。
实施例2
一种Mn1Cd3S4光催化剂的制备方法:
S1.按重量份数计,取1.26份无水氯化锰和7.1份硝酸镉加入到30份水中形成A溶液,A溶液置于常温下保存;取3份硫代乙酰胺加入15份水中形成B溶液,B溶液置于常温下保存;
S2.按重量份数计,取500份环己烷加入三口烧瓶中,再向三口瓶中加入6份OP-4和4份Span85并在常温水浴下以300r/min的转速搅拌,然后将S1中的A溶液和B溶液混合再逐滴加入到三口烧瓶中,向三口瓶中持续通氮气并将搅拌转速升至1100r/min,再将水浴温度升至62℃反应4h,升温时间为0.4h;
S3.等S2反应结束后将搅拌转速降低至300r/min,然后向三口烧瓶中加入乙醇破乳,再过滤得到滤渣,将滤渣用去离子水和丙酮反复洗涤三次得,最后将滤渣冷冻干燥得到Mn1Cd3S4光催化剂。
实施例3
一种Mn1Cd3S4光催化剂的制备方法:
S1.按重量份数计,取1.26份无水氯化锰和7.1份硝酸镉加入到30份水中形成A溶液,A溶液置于常温下保存;取3份硫代乙酰胺加入15份水中形成B溶液,B溶液置于常温下保存;
S2.按重量份数计,取540份环己烷加入三口烧瓶中,再向三口瓶中加入9.9份OP-4和5.1份Span85并在常温水浴下以400r/min的转速搅拌,然后将S1中的A溶液和B溶液混合再逐滴加入到三口烧瓶中,向三口瓶中持续通氮气并将搅拌转速升至1200r/min,再将水浴温度升至65℃反应3h,升温时间为0.5h;
S3.等S2反应结束后将搅拌转速降低至300r/min,然后向三口烧瓶中加入乙醇破乳,再过滤得到滤渣,将滤渣用去离子水和丙酮反复洗涤三次得,最后将滤渣冷冻干燥得到Mn1Cd3S4光催化剂。
本发明的保护范围并不仅局限于上述实施例,凡属于本发明思路下的技术方案均属于本发明的保护范围。应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理前提下的若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。
Claims (3)
1.一种Mn1Cd3S4光催化剂的制备方法,其特征在于,包括以下步骤:
S1.按重量份数计,取1.26份无水氯化锰和7.1份硝酸镉加入到30份水中形成A溶液,A溶液置于常温下保存;取3份硫代乙酰胺加入15份水中形成B溶液,B溶液置于常温下保存;
S2.按重量份数计,取450~540份环己烷加入三口烧瓶中,再向三口瓶中加入5~15份乳化剂并在常温水浴下以300~500r/min的转速搅拌,然后将S1中的A溶液和B溶液混合再逐滴加入到三口烧瓶中,向三口瓶中持续通氮气并将搅拌转速升至1000~1200r/min,再将水浴温度升至60~65℃反应3~5h;
S3.等S2反应结束后将搅拌转速降低至300~400r/min,然后向三口烧瓶中加入乙醇破乳,再过滤得到滤渣,将滤渣用去离子水和丙酮反复洗涤三次得,最后将滤渣冷冻干燥得到Mn1Cd3S4光催化剂。
2.根据权利要求1所述的一种Mn1Cd3S4光催化剂的制备方法,其特征在于,所述乳化剂由OP-4和Span85组成,Span85的质量占乳化剂质量的43%~66%。
3.根据权利要求1所述的一种Mn1Cd3S4光催化剂的制备方法,其特征在于,S2中水浴温度上升的时间为0.3~0.5h。
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CN111905761A (zh) * | 2020-07-29 | 2020-11-10 | 广西科技师范学院 | 一种Mn1Cd3S4光催化剂的制备方法 |
CN113318755A (zh) * | 2021-06-23 | 2021-08-31 | 淮北师范大学 | 一种有机无机杂化MnxCd1-xS固溶体光催化剂的制备方法 |
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