CN113058620A - 一种硫化钼析氢催化剂及其制备方法和应用 - Google Patents
一种硫化钼析氢催化剂及其制备方法和应用 Download PDFInfo
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Abstract
本发明涉及一种硫化钼析氢催化剂及其制备方法和应用,属于电解水领域。本发明所述制备方法包括如下步骤:1)将硫化钼粉末分散在剥离溶剂中;2)在步骤1)所得产品中合成聚苯胺,离心分离、洗涤、干燥,得到修饰聚苯胺的硫化钼;3)将修饰聚苯胺的硫化钼一步热处理使聚苯胺碳化,得到硫化钼析氢催化剂。本发明制备过程简单,操作可控,催化性能较好,易于放大,具有工业应用潜力。
Description
技术领域
本发明涉及一种硫化钼析氢催化剂及其制备方法和应用,属于电解水领域。
背景技术
在当今社会,能源危机和环境污染已日益严峻,威胁着人类的生存和发展。氢能是一种十分重要的能源,由于氢气的高能量密度以及环境友好的特点,它被认为是可持续能源存储的理想能源载体和化石燃料的替代物。而目前,氢气的生产依赖于化石燃料行业,因此也面临许多难题,如氢气纯度低、成本高;而利用电流使水分解产生氢气和氧气是非常有效的产氢方法,而且生产成本低、氢气纯度高。
电解水产氢反应被认为是大规模工业产氢的一种高效的途径。其中贵金属展现了极其优异的催化活性,例如Pt基催化剂是目前公认的性质最佳的电解水产氢催化剂,但是贵金属由于储量有限且价格昂贵因而无法大规模推广应用。硫化钼是一种二维层状结构的材料,被认为可用来替代Pt基催化剂的高效析氢催化剂。然而块体硫化钼由于暴露活性位点数较少,导电性较差的原因,析氢活性较差。
发明内容
本发明采用新方法制备的硫化钼析氢催化剂,解决了上述的问题。
本发明提供了一种硫化钼析氢催化剂的制备方法,所述制备方法包括如下步骤:1)将硫化钼粉末分散在剥离溶剂中;2)在步骤1)所得产品中合成聚苯胺,离心分离、洗涤、干燥,得到修饰聚苯胺的硫化钼;3)将修饰聚苯胺的硫化钼一步热处理使聚苯胺碳化,得到硫化钼析氢催化剂。
本发明优选为所述步骤1)中分散的方法为:液相剥离法。
本发明优选为所述步骤1)中剥离溶剂为:体积比7:3的异丙醇和水。
本发明优选为所述步骤1)中每30mL剥离溶剂加入1-2g硫化钼粉末,并超声分散2-4h。
本发明优选为所述步骤2)中聚苯胺合成的方法为:化学氧化法。
本发明优选为所述步骤2)中步骤1)所得产品加入到剥离溶剂中,并加入过硫酸铵的盐酸溶液和苯胺,在冰浴中搅拌3-4h;每20mL剥离溶剂加入1-3mL步骤1)所得产品、10mL过硫酸铵的盐酸溶液、95mg苯胺;所述过硫酸铵的盐酸溶液中过硫酸铵浓度为0.4-0.5g/mL,所述过硫酸铵的盐酸溶液中盐酸浓度为0.5-1M。
本发明优选为所述步骤3)中热处理的方法为:在氮气或氩气气氛下,500-550℃加热2-3h。
本发明另一目的为提供一种上述方法制备的硫化钼析氢催化剂。
本发明又一目的为提供一种上述硫化钼析氢催化剂在电解水析氢反应中的应用。
本发明有益效果为:
本发明利用了液相剥离法,将商业化的块体硫化钼剥离成纳米片,有助于暴露更多边缘活性位点;
本发明采用了化学氧化聚合法在硫化钼纳米片上原位合成聚苯胺,有助于防止纳米片的二次团聚;
本发明采用了热解法,使聚苯胺转化为碳材料,有助于提高催化剂的导电性;
本发明制备过程简单,操作可控,催化性能较好,易于放大,具有工业应用潜力。
附图说明
本发明附图2幅,
图1为实施例1-3和对比例1、2的LSV曲线图;
图2为实施例1制备的硫化钼析氢催化剂的SEM图。
具体实施方式
下述非限制性实施例可以使本领域的普通技术人员更全面地理解本发明,但不以任何方式限制本发明。
实施例1
配置异丙醇:水=7:3(体积比)的剥离溶剂,取1g商业化硫化钼粉末加入到30mL的剥离溶剂中,进行超声分散4h,得到硫化钼纳米片分散液;
取1mL硫化钼纳米片分散液加入到20mL的剥离溶剂中,并加入10mL 0.4g/mL过硫酸铵溶液(溶于0.5M HCl中)和95mg苯胺,在冰浴中保温并持续搅拌4h,得到聚苯胺修饰的硫化钼纳米片,离心过滤,去离子水洗涤,在真空烘箱中60℃干燥12h;
将聚苯胺修饰的硫化钼纳米片置于管式炉中,在氮气气氛下,500℃加热3h后自然冷却,得到硫化钼析氢催化剂,记为1#。
实施例2
配置异丙醇:水=7:3(体积比)的剥离溶剂,取1g商业化硫化钼粉末加入到30mL的剥离溶剂中,进行超声分散4h,得到硫化钼纳米片分散液;
取2mL硫化钼纳米片分散液加入到20mL的剥离溶剂中,并加入10mL 0.4g/mL过硫酸铵溶液(溶于0.5M HCl中)和95mg苯胺,在冰浴中保温并持续搅拌4h,得到聚苯胺修饰的硫化钼纳米片,离心过滤,去离子水洗涤,在真空烘箱中60℃干燥12h;
将聚苯胺修饰的硫化钼纳米片置于管式炉中,在氮气气氛下,500℃加热3h后自然冷却,得到硫化钼析氢催化剂,记为2#。
实施例3
配置异丙醇:水=7:3(体积比)的剥离溶剂,取1g商业化硫化钼粉末加入到30mL的剥离溶剂中,进行超声分散4h,得到硫化钼纳米片分散液;
取3mL分散液加入到20mL的剥离溶剂中,并加入10mL 0.4g/mL过硫酸铵溶液(溶于0.5M HCl中)和95mg苯胺,在冰浴中保温并持续搅拌4h,得到聚苯胺修饰的硫化钼纳米片,离心过滤,去离子水洗涤,在真空烘箱中60℃干燥12h;
将聚苯胺修饰的硫化钼纳米片置于管式炉中,在氮气气氛下,500℃加热3h后自然冷却,得到硫化钼析氢催化剂,记为3#。
对比例1
配置异丙醇:水=7:3(体积比)的剥离溶剂,取1g商业化硫化钼粉末加入到30mL的剥离溶剂中,进行超声分散4h,得到硫化钼纳米片分散液,记为ex-MoS2。
对比例2
配置异丙醇:水=7:3(体积比)的剥离溶剂,取1g商业化硫化钼粉末加入到30mL的剥离溶剂中,进行超声分散4h,得到硫化钼纳米片分散液;
取1mL硫化钼纳米片分散液用剥离溶剂稀释至20mL,加入50mg XC-72R碳黑并搅拌1h混合均匀,离心,洗涤,得到碳黑负载的硫化钼纳米片催化剂,记为ex-MoS2/CB。
电催化测试:将5mg催化剂和80μL 5%Nafion溶液分散在异丙醇溶液中超声30min,得到催化剂浆料;
移取10μL催化剂浆料于5mm直径玻碳电极上,在红外烤灯下,烘干成薄膜催化层;
在三电极体系(玻碳电极为工作电极,碳棒为对电极,甘汞电极为参比电极,0.5M硫酸溶液为电解质溶液),测量线性扫描伏安曲线,测试结果如图1。
Claims (9)
1.一种硫化钼析氢催化剂的制备方法,其特征在于:所述制备方法包括如下步骤:
1)将硫化钼粉末分散在剥离溶剂中;
2)在步骤1)所得产品中合成聚苯胺,离心分离、洗涤、干燥,得到修饰聚苯胺的硫化钼;
3)将修饰聚苯胺的硫化钼一步热处理使聚苯胺碳化,得到硫化钼析氢催化剂。
2.根据权利要求1所述硫化钼析氢催化剂的制备方法,其特征在于:所述步骤1)中分散的方法为:液相剥离法。
3.根据权利要求2所述硫化钼析氢催化剂的制备方法,其特征在于:所述步骤1)中剥离溶剂为:体积比7:3的异丙醇和水。
4.根据权利要求3所述硫化钼析氢催化剂的制备方法,其特征在于:所述步骤1)中每30mL剥离溶剂加入1-2g硫化钼粉末,并超声分散2-4h。
5.根据权利要求4所述硫化钼析氢催化剂的制备方法,其特征在于:所述步骤2)中聚苯胺合成的方法为:化学氧化法。
6.根据权利要求5所述硫化钼析氢催化剂的制备方法,其特征在于:所述步骤2)中步骤1)所得产品加入到剥离溶剂中,并加入过硫酸铵的盐酸溶液和苯胺,在冰浴中搅拌3-4h;
每20mL剥离溶剂加入1-3mL步骤1)所得产品、10mL过硫酸铵的盐酸溶液、95mg苯胺;
所述过硫酸铵的盐酸溶液中过硫酸铵浓度为0.4-0.5g/mL,所述过硫酸铵的盐酸溶液中盐酸浓度为0.5-1M。
7.根据权利要求6所述硫化钼析氢催化剂的制备方法,其特征在于:所述步骤3)中热处理的方法为:在氮气或氩气气氛下,500-550℃加热2-3h。
8.权利要求1、2、3、4、5、6或7所述方法制备的硫化钼析氢催化剂。
9.权利要求8所述硫化钼析氢催化剂在电解水析氢反应中的应用。
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