CN113649015A - 一种烟气脱硝催化剂及其制备方法与应用 - Google Patents
一种烟气脱硝催化剂及其制备方法与应用 Download PDFInfo
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Abstract
本发明涉及一种SCR烟气脱硝催化剂,其特征在于,采用以下方法制备:称取一定量的硝酸镍、硝酸铁和L‑半胱氨酸和柠檬酸钠溶于甲醇中,180‑200℃下溶剂热反应10‑20h,将产物采用去离子水和乙醇洗涤3次,随后300‑400℃下热处理得到花状的NiFe2O4;硝酸镍、硝酸铁的摩尔比为1:2;硝酸铁、L‑半胱氨酸、柠檬酸钠的摩尔比为1:(1‑2):(1‑2);将NiFe2O4溶于去离子水和乙醇的混合溶剂中形成悬浮液,去离子水和乙醇的体积比为1:(1‑2);在悬浮液中继续加入硝酸铈、硝酸钴,然后加入四乙基氢氧化铵,混合均匀,在80‑120℃下反应2‑3h,将产物采用去离子水和乙醇洗涤3次,随后300‑400℃下热处理,得到NiFe2O4‑CeO2‑Co3O4复合材料。
Description
技术领域
本发明属于环境保护与环境催化领域,尤其涉及一种NiFe2O4-CeO2-Co3O4的SCR烟气脱硝催化剂及其制备方法与应用。
背景技术
随着当今世界经济的不断发展,大气污染问题愈发严重。大气污染物主要有易挥发性有机物、硫氧化物(SOx)、氮氧化物(NOx)、以及可吸入颗粒物等,在众多污染物中,氮氧化物是大气污染物的主要组成成分之一,其容易引起酸雨、雾霾、光化学烟雾、温室效应以及臭氧层破坏,严重威胁着人类身体健康。目前选择性催化还原(SCR)脱硝技术是工业烟气脱硝技术的主要方法,脱硝效率高,稳定性好,因此被广泛应用。SCR脱硝技术关键在于研发高催化活性的低温催化剂,目前商用钒钛催化剂需要较高的反应温度、活性温度窗口较狭窄且氮气选择性低,因此,开发一种具有高活性、温度窗口宽的低温SCR催化剂迫在眉睫。。
CN104772138A公开了一种MnOx/石墨烯低温SCR烟气脱硝催化剂及其制备方法与应用。该方法为:以含有大量含氧基团的氧化石墨烯为前驱体通过两步水溶液法将Mn负载到石墨烯上,再经过焙烧制备出MnOx/石墨烯低温SCR烟气脱硝催化剂,所述MnOx/石墨烯低温SCR烟气脱硝催化剂中,MnOx与石墨烯的质量百分比为5%~25%。本发明的催化剂是以具有独特平面延展结构及较大理论比表面积的石墨烯为载体,极大的提高了活性组分MnOx颗粒的分散性,使其获得了较好的低温SCR烟气脱硝活性。
CN108465463A公开了一种低温核壳结构Ce基催化剂及其制备方法和应用。本发明以葡萄糖为碳源,采用水热法合成纳米球模板,以六亚甲基四胺为沉淀剂,采用冷凝回流的方法合成MnO2/CeO2-MnO2纳米球,再经洗涤,干燥,焙烧制备出Ce基核壳催化剂,并研究其烃类燃烧性能。本发明制备的铈-锰纳米核壳催化剂具有良好的核壳形貌和甲苯转化率,其中,CeO2:MnO2的摩尔比为3:8时,催化剂在242℃的甲苯催化转化率达到了90%。
然而,上述催化剂活性粒子容易团聚,并且比表面积低,导致催化性能不佳。
发明内容
发明的目的在于克服现有技术的不足,提供一种活性高、稳定性好、温度窗口宽的SCR烟气脱硝催化剂及其制备方法,本申请采用花状的NiFe2O4为载体负载纳米CeO2和Co3O4,提高了催化剂的催化活性。
一种SCR烟气脱硝催化剂,其特征在于,采用以下方法制备:
称取一定量的硝酸镍、硝酸铁和L-半胱氨酸和柠檬酸钠溶于甲醇中,180-200℃下溶剂热反应10-20h,将产物采用去离子水和乙醇洗涤3次,随后300-400℃下热处理得到二维纳米片形成的花状的NiFe2O4;硝酸镍、硝酸铁的摩尔比为1:2;硝酸铁、L-半胱氨酸、柠檬酸钠的摩尔比为1:(1-2):(1-2);
将NiFe2O4溶于去离子水和乙醇的混合溶剂中形成悬浮液,去离子水和乙醇的体积比为1:(1-2);在悬浮液中继续加入硝酸铈、硝酸钴,然后加入四乙基氢氧化铵,混合均匀,在80-120℃下反应2-3h,将产物采用去离子水和乙醇洗涤3次,随后300-400℃下热处理,得到NiFe2O4-CeO2-Co3O4复合材料。
优选的,硝酸铈、硝酸钴以及四乙基氢氧化铵的摩尔比为1:(1-2):(2-3);
优选的,去离子水和乙醇的体积比为1:(1-1.5);
优选的,热处理的时间为1-2h。
技术效果:
本发明通过在溶剂热反应中引入L-半胱氨酸和柠檬酸钠,制备得到粒径为5-8微米、纳米片构成的花状的NiFe2O4,二维片结合花状多孔结构具有比表面积大、吸附性好的优点;将其作为负载体负载CeO2和Co3O4,四乙基氢氧化铵保证了纳米CeO2和Co3O4的生成,NiFe2O4纳米片有利于提高CeO2和Co3O4的负载量以及分散性,本申请精准的调控材料形貌,最大程度的暴露催化位点,将三种材料复合,将有利于扩宽催化活性的温度窗口,提升脱硝的催化性能。
附图说明
附图1为本申请的NiFe2O4的SEM图。
具体实施方式
实施例1
称取10mmol硝酸镍、20mmol的硝酸铁和25mmol的L-半胱氨酸和30mmol的柠檬酸钠溶于80ml甲醇中,200℃下溶剂热反应12h,将产物采用去离子水和乙醇洗涤3次,随后300℃下热处理得到花状的NiFe2O4;
将NiFe2O4溶于100ml的去离子水和乙醇的混合溶剂中形成悬浮液,去离子水和乙醇的体积比为1:1;接着,在悬浮液中继续加入5mmol硝酸铈、5mmol硝酸钴,然后加入10mmol四乙基氢氧化铵,混合均匀,在90℃下反应2h,将产物采用去离子水和乙醇洗涤3次,随后350℃下热处理1h,得到NiFe2O4-CeO2-Co3O4复合材料。
对比例1
称取10mmol硝酸镍、20mmol的硝酸铁和25mmol的L-半胱氨酸和30mmol的柠檬酸钠溶于80ml甲醇中,200℃下溶剂热反应12h,将产物采用去离子水和乙醇洗涤3次,随后300℃下热处理得到花状的NiFe2O4。
对比例2
以去离子水和乙醇的体积比为1:1配制混合溶剂;接着,在100ml的去离子水和乙醇的混合溶剂中加入5mmol硝酸铈、5mmol硝酸钴,然后加入10mmol四乙基氢氧化铵,混合均匀,在90℃下反应2h,将产物采用去离子水和乙醇洗涤3次,随后350℃下热处理1h,得到CeO2-Co3O4复合材料。
对比例3
以去离子水和乙醇的体积比为1:1配制混合溶剂;接着,在100ml的去离子水和乙醇的混合溶剂中加入5mmol硝酸铈,然后加入5mmol四乙基氢氧化铵,混合均匀,在90℃下反应2h,将产物采用去离子水和乙醇洗涤3次,随后350℃下热处理1h,得到CeO2。
对比例4
以去离子水和乙醇的体积比为1:1配制混合溶剂;接着,在100ml的去离子水和乙醇的混合溶剂中加入5mmol硝酸钴,然后加入5mmol四乙基氢氧化铵,混合均匀,在90℃下反应2h,将产物采用去离子水和乙醇洗涤3次,随后350℃下热处理1h,得到Co3O4。
将上述实施例1和对比例1-4所制备的脱硝催化剂粉碎,随后将其放置于反应器中测试其脱硝性能,烟气组分为NO、NH3、O2、N2,其中NO为300ppm、NH3为300ppm、O2为20%、N2为平衡气,控制气体总流量在800mL/min,空速为30,000mL·g/1h。表1为本申请实施例和对比例的催化剂在不同温度下的NOx转化率。
表1
80℃ | 120℃ | 160℃ | 200℃ | 240℃ | 280℃ | 320℃ | |
实施例1 | 80.3% | 89.5% | 90.4% | 100% | 100% | 100% | 100% |
对比例1 | 75.5% | 79.9% | 90.1% | 91.1% | 93.1% | 94.3% | 96.2% |
对比例2 | 74.8% | 76.4% | 80.9% | 82.3% | 83.3% | 84.1% | 86.3% |
对比例3 | 48.6% | 52.6% | 60.1% | 63.5% | 68.6% | 69.0% | 71.0% |
对比例4 | 51.2% | 59.1% | 62.4% | 74.8% | 76.1% | 78.0% | 78.1% |
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 (4)
1.一种SCR烟气脱硝催化剂,其特征在于,采用以下方法制备:
称取一定量的硝酸镍、硝酸铁和L-半胱氨酸和柠檬酸钠溶于甲醇中,180-200℃下溶剂热反应10-20h,将产物采用去离子水和乙醇洗涤3次,随后300-400℃下热处理得到二维纳米片形成的花状NiFe2O4;硝酸镍、硝酸铁的摩尔比为1:2;硝酸铁、L-半胱氨酸、柠檬酸钠的摩尔比为1:(1-2):(1-2);
将NiFe2O4溶于去离子水和乙醇的混合溶剂中形成悬浮液,去离子水和乙醇的体积比为1:(1-2);在悬浮液中继续加入硝酸铈、硝酸钴,然后加入四乙基氢氧化铵,混合均匀,在80-120℃下反应2-3h,将产物采用去离子水和乙醇洗涤3次,随后300-400℃下热处理,得到NiFe2O4-CeO2-Co3O4复合材料。
2.根据权利要求1所述的一种SCR烟气脱硝催化剂,硝酸铈、硝酸钴以及四乙基氢氧化铵的摩尔比为1:(1-2):(2-3)。
3.根据权利要求1所述的一种SCR烟气脱硝催化剂,去离子水和乙醇的体积比为1:(1-1.5)。
4.根据权利要求1所述的一种SCR烟气脱硝催化剂,热处理的时间为1-2h。
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CN113926466A (zh) * | 2021-11-23 | 2022-01-14 | 商河县格尔环保科技服务中心 | 一种脱硝催化剂及其制备方法 |
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 |
CN114377688A (zh) * | 2022-02-22 | 2022-04-22 | 费县塞达新材料技术中心 | 一种高效烟气脱硝催化剂及其制备方法 |
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CN113926466A (zh) * | 2021-11-23 | 2022-01-14 | 商河县格尔环保科技服务中心 | 一种脱硝催化剂及其制备方法 |
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CN114377688A (zh) * | 2022-02-22 | 2022-04-22 | 费县塞达新材料技术中心 | 一种高效烟气脱硝催化剂及其制备方法 |
CN114377688B (zh) * | 2022-02-22 | 2022-08-23 | 中国电力建设工程咨询有限公司 | 一种高效烟气脱硝催化剂及其制备方法 |
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