CN105688997A - 一种高选择性催化剂及其制备方法 - Google Patents
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Abstract
本发明属于催化剂材料的制备领域,特别涉及一种二氧化碳还原反应催化剂及其制备方法,其中该催化剂的粉末是由过渡族金属镍与氧、氢、碳、氮组成的复杂化合物构成,该催化剂通过以下步骤制备:采用Ni(NO3)2和苯二甲酸(TPA)的N,N’-二甲基甲酰胺(DMF)溶液在微波化学合成仪中进行微波化学合成获得的。本发明的催化剂可以催化CO2还原反应,获得单一产物CO。该催化剂的转化效果好,对CO的选择性较好。
Description
技术领域
本发明属于催化剂材料的制备领域,特别涉及一种高选择性CO2还原反应催化剂及其制备方法。
背景技术
能源短缺、CO2排放造成的温室效应带来的环境危害等问题日益严重,利用太阳光将CO2和水光催化还原成碳、氢等燃料是解决能源和环境问题的最有潜力的方法。该方法具有无污染、成本低且利用资源丰富的太阳能等优点,利用太阳能激发半导体可见光催化剂,并借助催化剂的催化活性将CO2和水转化成甲醇、甲烷、一氧化碳等燃料资源,不仅可以解决全球变暖及化石燃料枯竭等问题,同时使得CO2可以循环利用,是当前研究热点之一。
在CO2还原光催化反应过程中,首先发生催化材料反应位点上吸附CO2,然后进行光生电子-空穴与CO2之间的转化过程。虽然多电子的质子-配对转移到CO2在动力学上是较容易达到,发生反应需要很大的过电势才能发生,甚至在催化剂条件下也很难达到。热力学上CO2十分稳定,而且以CO2为原料产生的反应物均为其还原产物,完成这种转化的唯一条件是将极高的能量输入给CO2。CO2还原过程中的另一个难题就是选择性,还原CO2会生成CO、甲酸、甲醛、甲醇、甲烷或其他碳氢化合物,有目的的形成单一产物,还需要进行探索和研究。
金属有机框架材料作为一种新型的功能化、多孔、晶态复杂化合物,具有框架结构、超高孔隙率、巨大的内比表面积、结构多样易调节等特点,已有证据证明其高孔隙率可以有助于捕获CO2分子,清洁空气,保护环境。
因此,利用地球丰储材料过渡族金属开发一种具有大量孔隙的金属有机晶态材料作为CO2还原催化剂,可以捕获吸附更多的CO2分子,不仅减少CO2排放量,还可以生成有用的CO等,可用于高能效CO2还原设备,对我国环境领域和能源领域的高速发展具有十分重要意义。
发明内容
本发明的目的在于提供一种高选择性CO2还原反应催化剂及其制备方法,使催化剂在获得高催化活性的同时,还具有较好的选择性。
本发明的原理在于:采用Ni(NO3)2作为前驱体,苯二甲酸(TPA)作为连接剂,溶解在N,N’-二甲基甲酰胺(DMF)中,在微波化学合成仪中进行微波化学合成,同时磁力搅拌,获得含有超高孔隙率的晶态复杂化合物催化剂。该催化剂与传统的化学合成方法制备的催化剂结构不同,传统的化学合成方法制备的催化剂中孔隙很少;本发明方法制备的催化剂中,由于采用TPA作为连接剂,制备过程中微波辐照形成具有大量孔隙,是含有C-O基、C-H基、-NO2基和C-C基团的Ni氢氧化物的复杂化合物,有利于CO2的吸附及扩散或穿过其中的空位到达更多的还原活性金属离子位,具有高的活性。
为实现上述目的,本发明的技术方案如下:
一种高活性催化剂,由微波化学合成方法制成,该催化剂是由过渡族金属镍和氢、氧、碳、氮组成的复杂氢氧化物。
所述催化剂通过以下步骤制备:
采用Ni(NO3)2和苯二甲酸(TPA)的N,N’-二甲基甲酰胺(DMF)溶液在微波化学合成仪中进行液相化学合成反应,清洗、离心分离、干燥。
所述催化剂粉末为含有C-O基、C-H基、-NO2基和C-C基团的Ni氢氧化物的晶态复杂化合物。
一种所述的高活性催化剂的制备方法,包括如下步骤:
采用Ni(NO3)2和苯二甲酸(TPA)的N,N’-二甲基甲酰胺(DMF)溶液在微波化学合成仪中进行液相化学合成反应,清洗、离心分离、干燥。
Ni(NO3)2和苯二甲酸(TPA)的N,N’-二甲基甲酰胺(DMF)溶液浓度均为1-2mol/l,在微波化学合成仪中进行微波化学合成反应,同时磁力搅拌,反应时间为3-8min,清洗液为DMF和无水乙醇,清洗、离心分离次数为1次和2次,60℃空气环境中干燥。
本发明的有益效果在于:
本发明的CO2还原反应催化剂不仅具有好的催化性能,还具有较好的CO选择性,在CO2还原催化反应中,反应时间到6h时,CO的产率达到150μmol。,可用于高能效CO2还原反应设备。
具体实施方式
下面实施例,对本发明的具体实施方式作进一步详细描述。
本发明的高活性催化剂,由微波化学合成方法制备,该催化剂是由过渡族金属镍和氢、氧、碳、氮组成的复杂化合物;其中,所述催化剂粉末为含有C-O基、C-H基、-NO2基和C-C基团的Ni氢氧化物的晶态化合物。
该催化剂的具体制备方法如下:
采用Ni(NO3)2和苯二甲酸(TPA)的N,N’-二甲基甲酰胺(DMF)溶液在微波化学合成仪中进行微波化学合成反应,清洗、离心分离、干燥。
CO2还原反应催化剂催化性能测试方法:将催化剂颗粒10mg与适量光敏剂[Ru(bpy)3]2+混合均匀,平铺于自制反应器底部,通入5%的CO2与Ar的混合气,对反应器吹扫1h后,将流量稳定控制在2ml/min,用300W氙灯作为可见光源连续照射,反应后气体成分由GC-9560气相色谱分析仪进行检测和定量分析。
实施例1:
采用本发明的制备方法制备催化剂,首先,采用浓度2mol/lNi(NO3)2和苯二甲酸(TPA)的N,N’-二甲基甲酰胺(DMF)溶液2ml,混合均匀,放入微波化学合成仪中,在功率1000W(2.45GHz)下,进行微波化学合成反应3min,然后采用DMF、无水乙醇清洗离心分离1次和2次,在60℃烘箱干燥。在上述制备工艺条件下,所制备的高活性催化剂进行CO2还原催化反应测试,反应6h时,CO的产率达到158μmol。
实施例2:
采用本发明的制备方法制备催化剂,首先,采用浓度1mol/lCo(NO3)2和苯二甲酸(TPA)的N,N’-二甲基甲酰胺(DMF)溶液2ml,混合均匀,放入微波化学合成仪中,在功率1000W(2.45GHz)下,进行微波化学合成反应8min,然后依次采用DMF、无水乙醇清洗离心分离1次和2次,在60℃烘箱干燥。在上述制备工艺条件下,所制备的高活性催化剂进行CO2还原催化反应测试,反应6h时,CO的产率达到150μmol。
Claims (3)
1.一种催化剂,由微波化学合成方法制成,其特征在于:
该催化剂是由过渡族金属镍和氢、氧、碳、氮组成的复杂化合物;
所述催化剂通过以下步骤制备:
采用Ni(NO3)2和苯二甲酸(TPA)的N,N’-二甲基甲酰胺(DMF)溶液在微波化学合成仪中进行液相化学合成反应,清洗、离心分离、干燥。
2.如权利要求1所述的制备方法,其特征在于:
Ni(NO3)2和苯二甲酸(TPA)的N,N’-二甲基甲酰胺(DMF)溶液的浓度均为1-2mol/l,搅拌均匀后,进行微波化学合成反应,同时磁力搅拌,反应时间为3-8min,清洗液为DMF和无水乙醇,清洗、离心分离次数为DMF1次、无水乙醇2次,60℃空气环境中干燥。
3.如权利要求1所述的催化剂,其特征在于:
所述催化剂粉末为含有C-O基、C-H基、-NO2基和C-C基团的Ni氢氧化物的复杂化合物。
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CN113856690B (zh) * | 2021-09-09 | 2023-08-18 | 福州大学 | 一种用于低浓甲烷催化燃烧的钴基催化剂 |
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