CN113457681A - 一种MOFs衍生的用于非甲烷总烃催化燃烧的Co-基催化剂及其制备方法和应用 - Google Patents
一种MOFs衍生的用于非甲烷总烃催化燃烧的Co-基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MOFs衍生的用于非甲烷总烃催化燃烧的Co‑基催化剂及其制备方法和应用,该催化剂包括二氧化硅和氧化铝的混合物组成的载体以及表面活性组分Co3O4,所述的载体中,二氧化硅和氧化铝质量比为5:5‑7:3;所述的活性组分Co3O4为Zif‑67衍生的Co3O4,以Co3O4质量计,为载体质量的10%。本发明催化剂采用水热法制备,使制备得到的催化剂中Co3O4颗粒尺寸较小,且分布均匀。本发明催化剂用于非甲烷总烃检测设备中检测非甲烷总烃。在292‑325 oC较低的温度区间内下,可以实现甲烷转化率低于5%,丙烷完全催化氧化转化率达95%。
Description
技术领域
本发明属于催化环保技术领域,具体涉及一种MOFs衍生的用于非甲烷总烃催化燃烧的Co-基催化剂及其制备方法和应用。
背景技术
非甲烷总烃(NMHC)是指除甲烷以外的其他所有具有挥发性的碳氢化合物的总称,如烷烃、烯烃、芳香烃和含氧碳氢化合物等。当环境中NMHC超过一定浓度时,会对人体健康产生直接危害,且很多挥发性有机物对人体有致癌作用。并且,非甲烷总烃在光照条件下会通过化学反应产生光化学烟雾及臭氧,对人类环境造成不可估量的损害。因此,从总烃中区分出非甲烷总烃,使其得以准确检测需求巨大。
目前用于非甲烷总烃(NMHC)的检测方法主要是色谱法。HJ38-2017标准中指出气相色谱法测量NMHC的含量的检测方法是将气体样品直接注入具有氢火焰离子化检测器的气相色谱仪,分别在总烃柱和甲烷柱上测得总烃和甲烷的含量,两者之差即为NMHC的含量。该方法检测繁琐,且成本较高。除此之外,气相色谱体型庞大,很难做成便携式检测器,无法进行现场监测。针对此问题,目前针对总烃中非甲烷总烃的检测发展了一种催化氧化法。催化氧化法和色谱法的主要区别在于,催化法通过催化氧化除甲烷以外的有机物对甲烷进行分析。催化氧化法的优势在于简化设备构造,方法简单,易于做成便携式检测设备。与此同时,也对非甲烷总烃催化剂的效率和温度窗口提出了更高的要求。
本发明提供一种MOFs衍生的用于非甲烷总烃催化燃烧的Co-基催化剂及其制备方法和应用,其目的在于,提供一种高效的非贵金属Co-基催化剂,从而替代贵金属,使检测仪器成本降低。
发明内容
为了克服现有技术的不足,在现有研究基础上进一步开发一种MOFs衍生的用于非甲烷总烃催化燃烧的Co-基催化剂,使其替代贵金属,使催化剂成本进一步降低,本发明目的在于提供一种MOFs衍生的用于非甲烷总烃催化燃烧的Co-基催化剂。
本发明的再一目的在于:提供一种上述MOFs衍生的用于非甲烷总烃催化燃烧的Co-基催化剂产品的制备方法。
本发明的又一目的在于:提供一种上述产品的应用。
本发明目的通过下述方案实现:一种MOFs衍生的用于非甲烷总烃催化燃烧的Co-基催化剂,包括二氧化硅和氧化铝的混合物组成的载体以及表面活性组分Co3O4,所述的载体中,二氧化硅和氧化铝质量比为5:5-7:3;所述的活性组分Co3O4为Zif-67衍生的Co3O4,以Co3O4质量计,相较于载体的质量百分数为10%。
本发明提供一种MOFs衍生的用于非甲烷总烃催化燃烧的Co-基催化剂的制备方法,采用水热法制备,主要包括以下步骤:
(1)以Co摩尔比1:4分别称取一定质量的Zif-67和Co(NO3)6H2O溶解于一定质量的甲醇溶液中,将配制好的Co(NO3)6H2O甲醇溶液倒入Zif-67甲醇溶液中,搅拌0.5h使其混合均匀,混合溶液中,Co离子总摩尔浓度为0.05mol/L;
(2)将该混合溶液转移至聚四氟乙烯不锈钢高压水热釜中,并按照质量比为5:5-7:3加入一定质量的SiO2和Al2O3,以Co3O4质量计,相较于载体的质量百分数为10%,110℃条件下水热2h,得到溶液;
(3)待溶液冷却至室温以后离心分离后用甲醇洗涤,然后于60℃条件下干燥12h,得粉末;
(4)干燥后的粉末于5%的氢氩混合气中500℃条件下还原3h后,于400℃条件下钝化12h,得到本发明所述的MOFs衍生的用于非甲烷总烃催化燃烧的Co-基催化剂。
采用本发明采用水热法制备催化剂,使制备得到的催化剂中Co3O4颗粒尺寸较小,且分布均匀。
本发明还提供了一种MOFs衍生的用于非甲烷总烃催化燃烧的Co-基催化剂的应用,用于非甲烷总烃检测设备中检测非甲烷总烃。
以甲烷/丙烷混合气模拟甲烷和非甲烷总烃污染气,将本发明催化剂用于甲烷和非甲烷总烃催化燃烧,催化燃烧所用催化剂活性评价在固定床微反应器(内径3mm石英管)中进行。催化剂的用量为100mg,温度采用K型热电偶自动控制。甲烷/丙烷标准混合气体与空气混合进入反应器进行燃烧。总流量采用质量流量计控制,甲烷和丙烷的浓度为100ppm,空气为载气,氧气浓度为10%,反应温度50-350 ℃, 在常压环境下进行。
本发明优越性在于:(1)本发明催化剂中活性组分Co3O4为MOFs衍生的Co3O4,比表面积大,活性高;(2)本发明催化剂以氧化硅和氧化铝作为载体,在还原处理过程中表面Co物种可以发生再分散,从而使催化剂性能进一步提高。本发明催化剂的制备方法简单、易操作。
具体实施方式
实施例1
一种MOFs衍生的用于非甲烷总烃催化燃烧的Co-基催化剂,采用二氧化硅和氧化铝的混合物组成的载体以及表面活性组分Co3O4,所述的载体中,二氧化硅和氧化铝质量比为7:3;所述的活性组分Co3O4为Zif-67衍生的Co3O4,以Co3O4质量计,为载体质量的10%,按下述步骤制备:
(1)分别称取0.22gZif-67和1.16gCo(NO3)6H2O溶解于50ml甲醇溶液中, 将配制好的Co(NO3)6H2O甲醇溶液倒入Zif-67甲醇溶液中,搅拌0.5h使其混合均匀得混合溶液;然后,
(2)将该混合溶液转移至150ml聚四氟乙烯不锈钢高压水热釜中,并按照质量百分数为7:3加入SiO2和Al2O3,110℃条件下水热2h;
(3)待溶液冷却至室温以后离心分离后用甲醇洗涤,然后于60℃条件下干燥12h得粉末;
(4)干燥后的粉末于5%的氢氩混合气中500℃条件下还原3h后于400℃条件下钝化12h,得到所述MOFs衍生的用于非甲烷总烃催化燃烧的Co-基催化剂,记作Co3O4/Si7Al3。
实施例2
一种MOFs衍生的用于非甲烷总烃催化燃烧的Co-基催化剂,与实施例1近似,只是二氧化硅和氧化铝质量比为6:4;所述的活性组分Co3O4为Zif-67衍生的Co3O4,以Co3O4质量计,为载体质量的10%,按下述步骤制备:
(1)分别称取0.22gZif-67和1.16gCo(NO3)6H2O溶解于50ml甲醇溶液中, 将配制好的Co(NO3)6H2O甲醇溶液倒入Zif-67甲醇溶液中,搅拌0.5h使其混合均匀得混合溶液;然后,
(2)将该混合溶液转移至150ml聚四氟乙烯不锈钢高压水热釜中,并按照质量百分数为6:4加入SiO2和Al2O3,110℃条件下水热2h;
(3)待溶液冷却至室温以后离心分离后用甲醇洗涤,然后于60℃条件下干燥12h得粉末;
(4)干燥后的粉末于5%的氢氩混合气中500℃条件下还原3h后于400℃条件下钝化12h,得到催化剂记作Co3O4/Si6Al4。
实施例3
一种MOFs衍生的用于非甲烷总烃催化燃烧的Co-基催化剂,与实施例1近似,只是二氧化硅和氧化铝质量比为5:5;所述的活性组分Co3O4为Zif-67衍生的Co3O4,以Co3O4质量计,为载体质量的10%,按下述步骤制备:
(1)分别称取0.22gZif-67和1.16gCo(NO3)6H2O溶解于50ml甲醇溶液中, 将配制好的Co(NO3)6H2O甲醇溶液倒入Zif-67甲醇溶液中,搅拌0.5h使其混合均匀得混合溶液;然后,
(2)将该混合溶液转移至150ml聚四氟乙烯不锈钢高压水热釜中,并按照质量百分数为5:5加入一定质量的SiO2和Al2O3,110℃条件下水热2h;
(3)待溶液冷却至室温以后离心分离后用甲醇洗涤,然后于60℃条件下干燥12h得粉末;
(4)干燥后的粉末于5%的氢氩混合气中500℃条件下还原3h后于400℃条件下钝化12h,得到催化剂记作Co3O4/Si5Al5。
催化剂活性测试:
以甲烷/丙烷混合气模拟甲烷和非甲烷总烃污染气,将实施例1至3所得催化剂用于甲烷和非甲烷总烃催化燃烧,用于催化燃烧所用催化剂活性评价在固定床微反应器(内径3mm石英管)中进行。催化剂的用量为100mg,温度采用K型热电偶自动控制。甲烷/丙烷标准混合气体与空气混合进入反应器进行燃烧。总流量采用质量流量计控制,甲烷和丙烷的浓度为100ppm,空气为载气,氧气浓度为10%,反应温度50-350 ℃, 在常压环境下进行。不同催化剂甲烷和丙烷反应的温度区间(丙烷完全转化,甲烷转化率低于5%的温度范围)如下表所示:
从上表可以看出,Co3O4/Si7Al3-Si5Al5系列催化剂均对总烃中非甲烷总烃催化燃烧表现出了较高的催化氧化活性,在较低的温度区间内(292-325 oC)下可以实现甲烷转化率低于5%,丙烷完全催化氧化转化率达95%。
本发明催化剂的制备方法简单易操作,催化剂成本较低。
Claims (4)
1.一种MOFs衍生的用于非甲烷总烃催化燃烧的Co-基催化剂,其特征在于,包括二氧化硅和氧化铝的混合物组成的载体以及表面活性组分Co3O4,所述的载体中,二氧化硅和氧化铝质量比为5:5-7:3;所述的活性组分Co3O4为Zif-67衍生的Co3O4,以Co3O4质量计,为载体质量的10%。
2.根据权利要求1所述MOFs衍生的用于非甲烷总烃催化燃烧的Co-基催化剂的制备方法,其特征在于,所述的二氧化硅和氧化铝质量比分别为5:5;6:4;以及7:3。
3.一种根据权利要求1或2所述MOFs衍生的用于非甲烷总烃催化燃烧的Co-基催化剂的制备方法,其特征在于,采用水热法制备,包括以下步骤:
(1)按Co摩尔比1:4分别称取Zif-67和Co(NO3)6H2O溶解于甲醇溶液中,将配制好的Co(NO3)6H2O甲醇溶液倒入Zif-67甲醇溶液中,搅拌0.5h得混合溶液,使混合溶液中Co离子总摩尔浓度为0.05mol/L;然后,
(2)将该混合溶液转移至聚四氟乙烯不锈钢高压水热釜中,并按照质量比为5:5-7:3加入一定质量的SiO2和Al2O3,以Co3O4质量计为载体质量的10%,110℃条件下水热2h;
(3)待溶液冷却至室温后离心分离后用甲醇洗涤,然后于60℃条件下干燥12h;
(4)干燥后的粉末于5%的氢氩混合气中500℃条件下还原3h后,于400℃条件下钝化12h,得到所述MOFs衍生的用于非甲烷总烃催化燃烧的Co-基催化剂。
4.一种根据权利要求1或2所述MOFs衍生的用于非甲烷总烃催化燃烧的Co-基催化剂的应用,该催化剂应用于非甲烷总烃检测设备中检测非甲烷总烃。
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