CN107282075B - 一种复合光催化剂及其制备方法 - Google Patents
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Abstract
本发明公开了一种复合光催化剂,是指钼酸铋与硫化镉复合光催化剂,该复合光催化剂能使水在太阳光的可见光照射下持续产生氢气,并公开了其制备方法。本发明所制备的钼酸铋与硫化镉复合光催化剂具有大面积接触界面,有利于载流子分离,钼酸铋与硫化镉结构稳定且带隙匹配,提高了光催化活性,催化效果稳定,具有优异的光解水产氢、光降解有机污染物及重金属离子和二氧化碳还原性能;合成方法原料普通,制备操作流程简单,工艺参数容易实现,成本低廉,操作简便,产率高,循环使用寿命长,在光解水产氢、光降解有机污染物及重金属离子和二氧化碳还原等领域具有广泛的应用前景和工业化前景。
Description
技术领域
本发明涉及一种复合光催化剂及其制备方法,属于纳米材料制备技术领域,尤其涉及一种复合纳米材料及其制备方法。
背景技术
近年来,能源危机愈演愈烈,石油日益枯竭,油价上涨,导致全球经济增长缓慢,各国为解决能源危机,实行各种政策,也有的国家为夺取原油,发动战争,伊朗革命,波斯湾战争,以及伊拉克战争都是为了争夺石油的控制权,最终目的就是为了解决能源危机。世界上为解决能源危机,也开发了很多新能源,新的方式,如光解产氢,风力发电,潮汐发电,地热发电等等,但大多数方式都是有局限性的,只能在特定的环境下实现,此时,需要寻找一种能够高效率燃烧,释放的能量大,无污染,制备容易的新型能源。
众所周知,对于地球来说,太阳光是无穷无尽的,如果能利用太阳光产生理想能源,这将是一笔巨大的财富。现有技术中,有些专利利用紫外光照射,分解水,产生氢气,氢气确实是理想的能源,在催化剂的作用下分解水产生氢气和氧气,氢气燃烧之后又产生水,对环境没有任何污染,而且产生的能量十分可观,可以用氢气代替传统的能源;也有技术论文中披露利用紫外光照射产氢,的确可以产生氢气,但是,紫外光在太阳光中占得比例只有2%,剩下的98%全都浪费了,虽说太阳光是无穷无尽的,但是如此小的比例始终不能实现大规模生产。
发明内容
为解决现有技术中存在的问题,本发明的技术目的在于,提供一种复合光催化剂及其制备方法,工艺流程简单,生产成本低,具有高效光催化活性。
为达到上述目的,本发明所采用的技术手段包括以下步骤:一种复合光催化剂,是指钼酸铋与硫化镉复合光催化剂。
进一步的,所述钼酸铋与硫化镉复合光催化剂能使水在太阳光的可见光照射下持续产生氢气。
进一步的,所述复合光催化剂的制备方法,步骤如下:
步骤一、将先将镉源和硫源分散到胺类溶剂和去离子水的混合溶剂中,水热法合成硫化镉纳米材料;
步骤二、将合成的硫化镉纳米材料、表面活性剂、钼酸盐、铋盐加入去离子水中,制成混合溶液,进行水热反应;再将水热产物洗涤后真空干燥,制得钼酸铋与硫化镉复合光催化剂。
进一步的,所述钼酸铋与硫化镉的质量比为0.05~2:1。
进一步的,所述镉源为硝酸镉、氯化镉、乙酸镉的一种或几种组合,硫源为硫脲、硫化钠、硫代乙酰胺、升华硫的一种或几种组合;所述胺类溶剂为乙二胺、二乙烯三胺、六亚甲基四胺、三乙烯四胺、环己胺、四乙烯五胺、三乙烯二胺、二甲基甲酰胺、环乙烯亚胺的一种或几种组合。
更进一步的,所述镉源和硫源的质量比为0.3~2:1;所述胺类溶剂和去离子水的体积比为0.2~10:1。
进一步的,所述钼酸盐为钼酸钠、钼酸铵、三氧化钼的一种或几种组合;所述铋盐为氯化铋、硝酸铋、次硝酸铋的一种或几种组合。
更进一步的,所述钼酸盐和铋盐的质量比为0.3~2:1。
进一步的,所述表面活性剂为乙二醇、聚乙烯吡络烷酮、月桂基磺化琥珀酸单酯二钠、苯乙烯、聚乙烯醇、吐温、十二烷基苯磺酸钠的一种或几种组合。
进一步的,所述步骤一中加热反应的温度为60℃~180℃,加热反应的时间为10~48h;所述步骤二中加热反应的温度为100℃~220℃,加热反应的时间为12~36h。
本发明的有益效果在于:钼酸铋与硫化镉复合光催化剂具有大面积接触界面,有利于载流子分离,钼酸铋与硫化镉结构稳定且带隙匹配,提高了光催化活性,催化效果稳定,具有优异的光解水产氢、光降解有机污染物及重金属离子和二氧化碳还原性能;合成方法原料普通,制备操作流程简单,工艺参数容易实现,成本低廉,操作简便,产率高,循环使用寿命长,在光解水产氢、光降解有机污染物及重金属离子和二氧化碳还原等领域具有广泛的应用前景和工业化前景。
附图说明
下面结合附图和实施例对本发明作进一步的阐述。
图1 为本发明实施例1中钼酸铋与硫化镉的TEM谱图照片。
具体实施方式
实施例1
将硝酸镉和硫代乙酰胺按0.4:1的质量比分散到40ml混合溶液中,混合溶液中三乙烯二胺和去离子水的体积比为2:1,加热至80℃反应16h,然后离心,在60℃真空干燥6h,得到CdS纳米晶。
将CdS纳米晶与15ml乙二醇、0.3g钼酸钠、0.5g硝酸铋混合加入25ml 去离子水中,将混合溶液转移至溶剂为50ml的聚四氟乙烯内衬的不锈钢反应釜中,加热至180℃反应24h,制得钼酸铋与硫化镉复合光催化剂。
如图1所示,所产生的钼酸铋与硫化镉的TEM谱图照片,经测试其产氢性能在2小时后可达到2490微摩尔。
实施例2
将20g氯化镉和15g硫化钠分散到2L混合溶液中,混合溶液中二乙烯三胺和去离子水的体积比为1:1,然后将混合溶液加热至180℃反应48 h,然后离心,真空干燥,得到CdS纳米晶。
将CdS纳米晶与0.5L吐温、30g钼酸氨、15g氯化铋混合加入5L 去离子水中,将混合溶液加热至200℃水热反应36h,制得钼酸铋与硫化镉复合光催化剂。
其光催化降解次甲基蓝染料废水效率达98%。
实施例3
将1Kg乙酸镉和1Kg升华硫分散到30L混合溶液中,混合溶液中六亚甲基四胺和去离子水的体积比为4:1,然后将混合溶液加热至110℃反应30 h,然后离心,真空干燥,得到CdS纳米晶。
将CdS纳米晶与1L月桂基磺化琥珀酸单酯二钠、900g三氧化钼、1.5Kg次硝酸铋混合加入7L 去离子水中,将混合溶液加热至220℃水热反应24h,制得钼酸铋与硫化镉复合光催化剂。
其光催化降解重金属Cr3+离子的效率达96%。
本发明公开了一种钼酸铋与硫化镉复合光催化剂,该催化剂能利用太阳光中的可见光分解水,产生氢气。由于利用的是可见光去产生氢气,可见光在太阳光中所占的比例是49%,这个比例相当可观,这大大提高了对太阳光的利用率,这是本发明的特征之一。同时,利用了钼酸铋和硫化镉复合产生的优秀光催化性能,使得在自然光的照射下,可高效的分解水,持续产生氢气,反复5次之后,钼酸铋与硫化镉的复合物仍保持98%以上,因为其重复性能好,循环使用寿命长,具有很高的使用价值,这是本发明的另一特征。
本发明制备的钼酸铋与硫化镉复合光催化剂具有大面积接触界面,有利于载流子分离,钼酸铋与硫化镉结构稳定且带隙匹配,提高了光催化活性,催化效果稳定,具有优异的光解水产氢、光降解有机污染物及重金属离子和二氧化碳还原性能;合成方法原料普通,制备操作流程简单,工艺参数容易实现,成本低廉,操作简便,产率高,循环使用寿命长,在光解水产氢、光降解有机污染物及重金属离子和二氧化碳还原等领域具有广泛的应用前景和工业化前景。
以上是本发明的实施例,但是本发明并不仅限于上述的实施例,熟悉本领域的科技人员在不违背本发明精神的前提条件下还可以作出种种等同的变形或者是替换,这些等同的变形或者替换均包含在本发明所限定的保护范围内。
Claims (3)
1.一种复合光催化剂,是指钼酸铋与硫化镉复合光催化剂,其特征在于:所述钼酸铋与硫化镉复合光催化剂能使水在太阳光的可见光照射下持续产生氢气;所述钼酸铋与硫化镉的质量比为 0.05~2:1;所述的复合光催化剂的制备方法,步骤如下:
步骤一、先将镉源和硫源分散到胺类溶剂和去离子水的混合溶剂中,水热法合成硫化镉纳米材料;
所述步骤一中水热反应的温度为60℃~180℃,水热反应的时间为10~48h;
步骤二、将合成的硫化镉纳米材料、表面活性剂、钼酸盐、铋盐加入去离子水中,制成混合溶液,进行水热反应;再将水热产物洗涤后真空干燥,制得钼酸铋与硫化镉复合光催化剂;
所述步骤二中水热反应的温度为 100℃~220℃,水热反应的时间为12~36h;
所述钼酸盐为钼酸钠、钼酸铵的一种或二种组合;所述铋盐为氯化铋、硝酸铋、次硝酸铋的一种或几种组合;
所述钼酸盐和铋盐的质量比为0.3~2:1;
所述表面活性剂为聚乙烯吡咯烷酮、月桂基磺化琥珀酸单酯二钠、聚乙烯醇、吐温、十二烷基苯磺酸钠的一种或几种组合。
2.根据权利要求1所述的复合光催化剂的制备方法,其特征在于:所述镉源为硝酸镉、氯化镉、乙酸镉的一种或几种组合,硫源为硫脲、硫化钠、硫代乙酰胺、升华硫的一种或几种组合;所述胺类溶剂为乙二胺、二乙烯三胺、六亚甲基四胺、三乙烯四胺、环己胺、四乙烯五胺、三乙烯二胺、二甲基甲酰胺、环乙烯亚胺的一种或几种组合。
3.根据权利要求2所述的复合光催化剂的制备方法,其特征在于:所述镉源和硫源的质量比为0.3~2:1;所述胺类溶剂和去离子水的体积比为0.2~10:1。
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