CN112495371B - 一种用于催化臭氧氧化挥发性有机物的催化剂制备方法 - Google Patents
一种用于催化臭氧氧化挥发性有机物的催化剂制备方法 Download PDFInfo
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- 229940071125 manganese acetate Drugs 0.000 claims description 2
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- 238000001179 sorption measurement Methods 0.000 description 1
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Abstract
本发明公开了一种用于催化臭氧氧化挥发性有机物的介孔二氧化锰催化剂的制备方法。该制备方法将介孔硅材料浸渍于二价锰盐溶液中,经过滤除去浸渍液后,将浸渍产物再次浸渍于高锰酸盐溶液中,除去浸渍液后干燥、煅烧得到前驱体,然后用碱溶液除去模板剂,洗涤后得到所述的介孔二氧化锰催化剂。制备的催化剂应用于催化臭氧氧化挥发性有机物,具有催化活性高、寿命长的优点。
Description
技术领域
本发明涉及环境技术领域,特别涉及一种用于催化臭氧氧化挥发性有机物的催化剂制备方法。
背景技术
挥发性有机化合物(VOCs)是一种在常温常压下,具有高蒸汽压和易挥发性的有机化学物质,是一类常见的大气污染物,减少VOCs的排放有助于改善大气环境质量、保护生态环境和保障人体健康,也是社会经济可持续发展的迫切需求。
臭氧具有强氧化性,是一种广谱杀菌剂,常用于医疗卫生、和餐饮食品行业杀菌消毒。CN101402047公开了一种臭氧分解催化剂及其制备方法,该催化剂以活性炭颗粒为载体,以锰、镍、银、铈为催化剂的活性组分。此外,如CN102513106A、CN101757933A各公开了一种臭氧分解催化剂及制备方法, 可有效去除废气中的臭氧。
介孔分子筛在催化、分离、生物及纳米材料等领域有广泛的应用前景,在催化、吸附分离以及高等无机材料等学科开拓了新的研究领域。如CN106944027A公开了一种毫米级介孔臭氧氧化催化剂的制备方法,该方法制备的毫米级介孔臭氧氧化催化剂含铈、钛、锆、氧,可显著提高臭氧氧化的矿化程度,可应用于废水处理。同时,金属氧化物也广泛用作催化臭氧氧化方法的催化剂,本发明利用介孔硅材料作为模板制备介孔二氧化锰催化剂应用于VOCs的催化臭氧氧化,优点是介孔二氧化锰的有序程度高,比表面积较大,化学稳定性好,可催化臭氧氧化VOCs,并将其降解为H2O和CO2,多余的臭氧可被催化分解为氧气,不会造成二次污染。
发明内容
本发明公开了一种用于催化臭氧氧化VOCs的催化剂制备方法,旨在提高臭氧对VOCs的深度氧化进而将VOCs降解为CO2和H2O等无害物质。
本发明所述一种用于催化臭氧氧化VOCs的催化剂制备方法包括下述步骤:
(1)采用介孔硅材料作为模板剂;
(2)将介孔硅模板浸渍于二价锰盐溶液中,过滤除去浸渍液;
(3)将步骤(2)中的浸渍产物再次浸渍于高锰酸盐溶液中,除去浸渍液后干燥、煅烧得到二氧化锰催化剂前驱体;
(4)采用碱溶液将步骤(3)中得到的二氧化锰催化剂前驱体中的介孔硅模板去除,过滤后用纯水洗涤滤饼干燥后得到介孔二氧化锰。
所述制备方法的步骤(1)所述的介孔材料为SBA-15,SBA-16,KIT-6,MCM-41中的一种或多种混合物。
所述制备方法的步骤(2)和步骤(3)中浸渍条件为机械搅拌、磁力搅拌和超声搅拌中的一种,浸渍时间为2~12小时。
所述制备方法的步骤(2)中二价锰盐溶液为氯化锰溶液、硫酸锰溶液、硝酸锰溶液、醋酸锰溶液中的一种或多种混合物,二价锰盐溶液浓度为0.015~0.6mol/L,溶液中二价锰盐的质量为硅模板质量的0.8~1.8倍。
所述制备方法的步骤(3)中高锰酸盐溶液为高锰酸钾溶液、高锰酸钠溶液中的一种或两种混合物,高锰酸盐溶液浓度为0.01~0.4mol/L。
所述制备方法的步骤(3)和步骤(4)中,干燥温度为60~100℃,干燥时间为12~16小时;煅烧温度为200~600℃,煅烧时间为4~10小时。
所述制备方法的步骤(4)中碱溶液采用氢氧化钾或氢氧化钠溶液,溶液浓度为1~2mol/L,去除模板时采用碱溶液浸渍前驱体,浸渍条件为机械搅拌、磁力搅拌和超声搅拌中的一种,浸渍3~4小时后过滤,纯水洗涤滤饼至pH为7~9。
具体实施方式
实施例1:取7ml 50%硝酸锰溶液定容至100ml,将硝酸锰溶液稀释至0.3mol/L,再取3g SBA-15浸渍于83ml浓度为0.3 mol/L的硝酸锰溶液中,超声浸渍2小时后过滤出浸渍液得到滤饼。取3.16g固体高锰酸钾溶解定容至100ml,制得0.2 mol/L的高锰酸钾溶液。将过滤后的滤饼浸渍于83ml的高锰酸钾溶液中超声浸渍2小时,后将过滤产物置于烘箱中在80℃条件下干燥12小时,然后在马弗炉中400℃煅烧4小时得到二氧化锰催化剂前驱体,然后将其溶于150ml浓度为2mol/L的氢氧化钠溶液中,搅拌浸渍4小时后过滤并用超纯水将滤饼洗涤至pH为7,将滤饼置于烘箱中70℃干燥12小时后可制得用于催化臭氧氧化VOCs的介孔二氧化锰催化剂。催化剂性能评价:催化剂的体积为0.7mL,气体流量为125ml/min,甲苯的入口浓度为60mg/m3,入口臭氧浓度为1000 mg/m3,测得甲苯净化率为100%,二氧化碳选择性为80%,出口无臭氧检出,运行50天,催化剂性能稳定。
实施例2:称取3.78g无水氯化锰固体溶于纯水配制100ml 0.3 mol/L氯化锰溶液,再取3g SBA-15浸渍于100ml浓度为0.3 mol/L氯化锰溶液中,超声浸渍2小时后过滤出去浸渍液得到滤饼。取3.16g固体高锰酸钾溶解定容至100ml,制得0.2 mol/L的高锰酸钾溶液。将过滤后的滤饼浸渍于100ml的高锰酸钾溶液中超声浸渍2小时,将过滤产物置于烘箱中干燥12小时,然后在马弗炉中400℃煅烧4小时得到二氧化锰催化剂前驱体,将其溶于150ml浓度为2mol/L的氢氧化钠溶液中,搅拌浸渍4小时后过滤并用超纯水将滤饼洗涤至pH为7,将滤饼置于烘箱中70℃干燥12小时后可制得用于催化臭氧氧化VOCs的介孔二氧化锰催化剂。催化剂性能评价:催化剂的体积为0.7mL,气体流量为125ml/min,甲苯的入口浓度为60mg/m3,入口臭氧浓度为1000 mg/m3,测得甲苯净化率为93%,二氧化碳选择性为60%,出口臭氧为100 mg/m3,运行50天,催化剂性能稳定。
实施例3:称取4.53g无水硫酸锰固体溶于纯水配制100ml 0.3 mol/L硫酸锰溶液,再取3g SBA-15浸渍于100ml浓度为0.3 mol/L硫酸锰溶液中,超声浸渍2小时后过滤出去浸渍液得到滤饼。取3.16g固体高锰酸钾溶解定容至100ml,制得0.2 mol/L的高锰酸钾溶液。将过滤后的滤饼浸渍于100ml的高锰酸钾溶液中超声浸渍2小时,将过滤产物置于烘箱中干燥12小时,然后在马弗炉中400℃煅烧4小时得到二氧化锰催化剂前驱体,将其溶于150ml浓度为2mol/L的氢氧化钠溶液中,搅拌浸渍4小时后过滤并用超纯水将滤饼洗涤至pH为7,将滤饼置于烘箱中70℃干燥12小时后可制得用于催化臭氧氧化VOCs的介孔二氧化锰催化剂。催化剂性能评价:催化剂的体积为0.7mL,气体流量为125ml/min,甲苯的入口浓度为60mg/m3,入口臭氧浓度为1000 mg/m3,测得甲苯净化率为90%,二氧化碳选择性为63%,出口臭氧为120mg/m3,运行50天,催化剂性能稳定。
以上对发明的实施例进行了详细说明,但所述内容仅为本发明的较佳实施例,不能被认为用于限定本发明的实施范围。凡依本发明申请范围所作的改进应仍归属于本发明的专利涵盖范围之内。
Claims (4)
1.一种用于催化臭氧氧化挥发性有机物的催化剂制备方法,其特征在于,所述的催化剂为介孔二氧化锰,所述催化剂的制备方法,包括步骤:
(1)采用介孔硅材料作为模板剂;
(2)将介孔硅模板浸渍于二价锰盐溶液中,过滤除去浸渍液;
(3)将步骤(2)中的浸渍产物再次浸渍于高锰酸盐溶液中,除去浸渍液后干燥、煅烧得到二氧化锰催化剂前驱体;
(4)采用碱溶液将步骤(3)中得到的二氧化锰催化剂前驱体中的介孔硅模板去除,过滤后用纯水洗涤滤饼干燥后得到介孔二氧化锰;
所述高锰酸盐溶液浓度为0.01-0.4mol/L;
所述煅烧温度为400-600℃。
2.根据权利要求书1所述的制备方法,其特征在于,步骤(2)中二价锰盐溶液为氯化锰溶液、硫酸锰溶液、硝酸锰溶液、醋酸锰溶液中的一种或多种混合物,二价锰盐溶液浓度为0.015-0.6mol/L,溶液中二价锰盐的质量为硅模板质量的0.8-1.8倍。
3.根据权利要求书1所述的制备方法,其特征在于,步骤(3)中高锰酸盐溶液为高锰酸钾溶液、高锰酸钠溶液中的一种或两种混合物。
4.根据权利要求1所述的制备方法,其特征在于,干燥温度为60-100℃,干燥时间为12-16小时;煅烧时间为4-10小时。
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