CN113042066A - 一种烟气脱硝催化剂及其制备方法 - Google Patents
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Abstract
本发明涉及一种烟气脱硝催化剂及其制备方法,(1)采用静电纺丝工艺制备PVP纤维,等离子处理;将该PVP纤维放入高锰酸钾溶液,转入反应釜中,水热反应,得到三维核壳结构的PVP/MnO2复合材料;(2)将PVP/MnO2复合材料转移到含有锌盐、氨水的混合液中,搅拌,随后置于高压反应釜中,得PVP/MnO2/ZnO复合材料;将该复合材料溶解于乙醇,加入镍盐和钴盐,水热滴入氨水,水热反应,得到PVP/MnO2/ZnO/NiCo2O4的复合材料,将该复合材料采用NaOH浸泡,随后空气气氛中煅烧去除模板,得到void/MnO2/void/NiCo2O4的复合材料。催化剂拥有较大的比表面积,结构稳定性好,MnO2和NiCo2O4协同作用,具有较好的催化活性。
Description
技术领域
本发明涉及环保技术领域,具体涉及一种烟气脱硝催化剂及其制备方法。
背景技术
燃煤锅炉、玻璃炉窑和水泥炉窑等排放的氮氧化物是引起酸雨、光化学烟雾等的主要污染物之一,对大气造成了极大的污染,破坏了生态环境,并且损害人体健康。如何有效地消除氮氧化物目前已成为大气污染治理的重点和难点。选择性催化还原(SCR)脱硝技术是国际上应用最广、市场占有率最高、运行最稳定可靠的烟气脱硝技术,其原理在于在催化剂的作用下,NO与还原剂NH3发生如下反应:4NH3+4NO+O2→4N2+6H2O;而SCR技术核心技术是催化剂,其催化性能的好坏直接决定了脱硝效率;因此,开发催化性能好、稳定性高的催化剂对于脱硝技术有着重大意义。
过渡金属氧化物催化脱硝材料拥有较高的NOx催化性能,与贵金属催化材料相比其具有更高的抗氧性,而且其成本低廉。CN112473682 A公开了一种高性能中低温NH3-SCR催化剂的制备方法,其特征在于,包括以下步骤:采用共沉淀法将六水合硝酸铈、九水合硝酸铁和草酸铌溶解于蒸馏水中并在室温下均匀搅拌,然后将氨水逐滴滴加到混合溶液中,使混合溶液沉淀完全,最后经过老化、过滤、洗涤、干燥、在空气气氛下焙烧,制得高性能中低温NH3-SCR催化剂。CN111992214 A公开了一种纳米多级孔SiO2@Cu/Ni核壳材料及其制备方法与应用,其中制备方法包括:首先配制纳米级球形SiO2分散液并依次与铜源溶液及还原剂混合,得到砖红色沉淀;之后将砖红色沉淀煅烧,得到核壳材料SiO2@Cu;最后配制含有SiO2@Cu及聚乙烯醇的分散液,并与镍源混合,再依次经过加热搅拌、烘箱干燥、高温煅烧后,即得到纳米多级孔SiO2@Cu/Ni核壳材料。
发明内容
针对现有技术存在的催化剂催化活性低,比表面积小,活性差的问题,本发明所要解决的技术问题在于提供一种void/MnO2/void/NiCo2O4的复合材料烟气脱硝催化剂。
一种烟气脱硝催化剂,其特征在于,采用如下方法进行制备:
(1)采用静电纺丝工艺制备PVP纤维,对其进行等离子处理;将该PVP纤维放入溶有高锰酸钾的去离子水/乙二醇混合液中,转入反应釜中,水热反应,得到三维核壳结构的PVP/MnO2复合材料;
(2)将PVP/MnO2复合材料转移到含有锌盐、氨水的混合液中,搅拌,随后置于高压反应釜中,得PVP/MnO2/ZnO复合材料;将该复合材料溶解于乙醇,加入镍盐和钴盐,水热滴入氨水,水热反应,得到PVP/MnO2/ZnO/NiCo2O4的复合材料,将该复合材料采用NaOH浸泡,随后空气气氛中煅烧去除模板,得到void/MnO2/void/NiCo2O4的复合材料。
优选的,步骤(1)、(2)的水热反应为180-200℃下反应12-20h;
优选的,空气中煅烧温度为200-300℃,煅烧时间为0.5-1h;
优选的,MnO2/ZnO/NiCo2O4摩尔比为1:(0.5-2):(0.5-2);
优选的,镍盐和钴盐为硝酸镍和硝酸钴。
技术效果:
本申请首次提出以静电纺丝工艺制备的PVP纳米纤维-ZnO作为双模板制备独特三维双空心结构的void/MnO2/void/NiCo2O4的复合材料,该材料具有较大的比表面积,极大的增加了催化活性位点,MnO2和NiCo2O4协同作用,具有较好的催化活性;制备方法能耗低、污染小、环境友好、简便快捷、可大规模生产。
具体实施方式
实施例1
(1)采用静电纺丝工艺制备PVP三维网络纤维,对其等离子处理;取0.1mol的高锰酸钾溶于50ml,体积比为1:1的水/乙二醇的混合液中,随后将0.5g的PVP纤维放入高锰酸钾的反应釜中,180℃水热反应8h,得到三维核壳结构的PVP/MnO2复合材料;
(2)将0.4mol的硝酸锌溶于去离子水,滴入一定量的氨水,调节pH为7.8-9,加入步骤(1)的PVP/MnO2复合材料,搅拌,随后置于高压反应釜中,180℃反应6h,得PVP/MnO2/ZnO复合材料;将该复合材料溶解于乙醇,加入镍盐和钴盐,水热滴入氨水,水热反应,得到PVP/MnO2/ZnO/NiCo2O4的复合材料,将该复合材料采用NaOH浸泡,随后空气气氛中300℃下煅烧0.5h去除模板,得到void/MnO2/void/NiCo2O4的复合材料。
催化剂测试:在固定床石英管反应器中测试催化剂的反应活性,催化剂为1g,反应温度为100~450℃、以氨气为还原剂,控制气体总流量在300mL/min,空速为30,000mL·g-1h-1,脱硝效率大于88%,对N2选择性大于82%。
实施例2
(1)采用静电纺丝工艺制备PVP三维网络纤维,对其等离子处理;取0.1mol的高锰酸钾溶于体积比为1:1的50ml水/乙二醇的混合液中,随后将0.5g的PVP纤维放入高锰酸钾的反应釜中,180℃水热反应8h,得到三维核壳结构的PVP/MnO2复合材料;
(2)将0.4mol的硝酸锌溶于去离子水,滴入一定量的氨水,调节pH为7.8-9,加入步骤(1)的PVP/MnO2复合材料,搅拌,随后置于高压反应釜中,180℃反应6h,得PVP/MnO2/ZnO复合材料;将该复合材料溶解于乙醇,加入镍盐和钴盐,水热滴入氨水,水热反应,得到PVP/MnO2/ZnO/NiCo2O4的复合材料,将该复合材料采用NaOH浸泡,随后空气气氛中300℃下煅烧0.5h去除模板,得到void/MnO2/void/NiCo2O4的复合材料。
催化剂测试:在固定床石英管反应器中测试催化剂的反应活性,催化剂为1g,反应温度为100~450℃、以氨气为还原剂,控制气体总流量在200mL/min,空速为30,000mL·g-1h-1,脱硝效率大于87%,对N2选择性大于85%。
以上尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。
Claims (5)
1.一种烟气脱硝催化剂,其特征在于,采用如下方法进行制备:
(1)采用静电纺丝工艺制备PVP纤维,对其进行等离子处理;将该PVP纤维放入溶有高锰酸钾的去离子水/乙二醇混合液中,转入反应釜中,水热反应,得到三维核壳结构的PVP/MnO2复合材料;
(2)将PVP/MnO2复合材料转移到含有锌盐、氨水的混合液中,搅拌,随后置于高压反应釜中,得PVP/MnO2/ZnO复合材料;将该复合材料溶解于乙醇,加入镍盐和钴盐,水热滴入氨水,水热反应,得到PVP/MnO2/ZnO/NiCo2O4的复合材料,将该复合材料采用NaOH浸泡去除ZnO2,随后空气气氛中煅烧去除模板,得到三维网状的void/MnO2/void/NiCo2O4双空心核壳复合材料。
2.根据权利要求1所述的一种烟气脱硝催化剂,其特征在于,步骤(1)、(2)的水热反应为180-200℃下反应12-20h。
3.根据权利要求1所述的一种烟气脱硝催化剂,其特征在于,空气中煅烧温度为200-300℃,煅烧时间为0.5-1h。
4.根据权利要求1所述的一种烟气脱硝催化剂,其特征在于,MnO2/ZnO/NiCo2O4摩尔比为1:(0.5-2):(0.5-2)。
5.根据权利要求1所述的一种烟气脱硝催化剂,其特征在于,镍盐和钴盐为硝酸镍和硝酸钴。
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CN114160154A (zh) * | 2021-12-13 | 2022-03-11 | 衡水市高新区博元新能源技术研发中心 | 一种机动车尾气处理催化剂 |
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