CN117443398A - 一种介孔铁基复合氧化物催化剂及其制备方法和应用 - Google Patents
一种介孔铁基复合氧化物催化剂及其制备方法和应用 Download PDFInfo
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- CN117443398A CN117443398A CN202311412284.0A CN202311412284A CN117443398A CN 117443398 A CN117443398 A CN 117443398A CN 202311412284 A CN202311412284 A CN 202311412284A CN 117443398 A CN117443398 A CN 117443398A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 102
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 89
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 38
- 239000002131 composite material Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title abstract description 12
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 174
- 238000000034 method Methods 0.000 claims abstract description 29
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 19
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- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 claims description 39
- 239000007789 gas Substances 0.000 claims description 20
- 150000003839 salts Chemical class 0.000 claims description 17
- 239000002994 raw material Substances 0.000 claims description 15
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- 229910002651 NO3 Inorganic materials 0.000 claims description 5
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 5
- 230000000630 rising effect Effects 0.000 claims description 5
- 229910052684 Cerium Inorganic materials 0.000 claims description 4
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- 229910052733 gallium Inorganic materials 0.000 claims description 4
- 239000006228 supernatant Substances 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 3
- 150000002505 iron Chemical class 0.000 claims description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 14
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- 230000000694 effects Effects 0.000 description 18
- 238000005516 engineering process Methods 0.000 description 14
- 239000000243 solution Substances 0.000 description 13
- 238000012360 testing method Methods 0.000 description 13
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 10
- 239000003546 flue gas Substances 0.000 description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 9
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- 238000001179 sorption measurement Methods 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical group [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 8
- 238000002485 combustion reaction Methods 0.000 description 8
- 239000003344 environmental pollutant Substances 0.000 description 7
- 231100000719 pollutant Toxicity 0.000 description 7
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 5
- 239000003638 chemical reducing agent Substances 0.000 description 5
- 230000006378 damage Effects 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 238000009841 combustion method Methods 0.000 description 4
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- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 238000012271 agricultural production Methods 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
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- 238000010531 catalytic reduction reaction Methods 0.000 description 2
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- CHPZKNULDCNCBW-UHFFFAOYSA-N gallium nitrate Chemical compound [Ga+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O CHPZKNULDCNCBW-UHFFFAOYSA-N 0.000 description 2
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 150000002823 nitrates Chemical class 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
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- 230000008439 repair process Effects 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- CQWVAHMJJPEGQE-UHFFFAOYSA-N CC=C.C(Cl)Cl Chemical compound CC=C.C(Cl)Cl CQWVAHMJJPEGQE-UHFFFAOYSA-N 0.000 description 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- 241000282412 Homo Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 208000012902 Nervous system disease Diseases 0.000 description 1
- 208000025966 Neurological disease Diseases 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 230000010718 Oxidation Activity Effects 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
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- 150000001555 benzenes Chemical class 0.000 description 1
- 230000001588 bifunctional effect Effects 0.000 description 1
- 238000010170 biological method Methods 0.000 description 1
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- 239000012159 carrier gas Substances 0.000 description 1
- 210000003169 central nervous system Anatomy 0.000 description 1
- QQZMWMKOWKGPQY-UHFFFAOYSA-N cerium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O QQZMWMKOWKGPQY-UHFFFAOYSA-N 0.000 description 1
- OZECDDHOAMNMQI-UHFFFAOYSA-H cerium(3+);trisulfate Chemical compound [Ce+3].[Ce+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O OZECDDHOAMNMQI-UHFFFAOYSA-H 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
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- 231100000481 chemical toxicant Toxicity 0.000 description 1
- 238000011278 co-treatment Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 1
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 1
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000003517 fume Substances 0.000 description 1
- 229940044658 gallium nitrate Drugs 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 description 1
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 description 1
- SZQUEWJRBJDHSM-UHFFFAOYSA-N iron(3+);trinitrate;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O SZQUEWJRBJDHSM-UHFFFAOYSA-N 0.000 description 1
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910001960 metal nitrate Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 210000000056 organ Anatomy 0.000 description 1
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- 238000000926 separation method Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
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- 230000001988 toxicity Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/888—Tungsten
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
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- B01D53/8625—Nitrogen oxides
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- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
- B01J37/0018—Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat)
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Abstract
本发明提供了一种介孔铁基复合氧化物催化剂及其制备方法和应用,属于环境催化净化技术领域。该铁基复合氧化物催化剂的化学式为FeaMbW(a+b)/4Oy。本发明的催化剂制备采用简单的尿素沉淀法制备,无需其他复杂操作,方法简单快捷,条件易于控制,重复性高。本发明所制备的介孔铁基复合氧化物催化剂可以用于NOx与甲苯废气协同净化处理,保持较好的脱硝性能,以及良好的甲苯氧化能力,具有很好的工业应用前景。
Description
技术领域
本发明涉及环境催化净化技术领域,尤其涉及一种介孔铁基复合氧化物催化剂及其制备方法和应用。
背景技术
我国作为世界第二大经济体,然而,在经济发展的同时也必然会导致能源的消耗,我国能源消费结构可以分为煤炭、石油、天然气、一次电力及其他能源,但由于我国的能源消费量较大,在短时间内太阳能、风能、氢能等新能源的供给远远无法满足经济发展的要求,因此,在相对较长的一段时间内,传统的化石能源依旧是能源消费结构中的核心。随着化石燃料的燃烧,燃料中的各类元素会转化成为大气污染物,烟气的排放造成严重的环境污染,环境的每况愈下直接威胁生物的生存。常见的的烟气污染物有NOx、VOCs、Hg等。其中NOx排放在大气中,再与光照作用,会发生一系列的化学反应,进而形成诸如二次有机气溶胶、硝酸盐、硫酸盐等二次污染物。二次污染物的生成会进一步引发环境污染问题,形成雾霾、光化学烟雾、酸雨等严重的环境问题。此外,NOx的存在对人体的呼吸***有着直接性的破坏,对呼吸器官造成损伤。
NOx和VOCs是PM2.5和臭氧的重要共同前体物。目前,我国大气环境中SO2、NOx得到有效治理,PM2.5、PM10污染防治成效显著,但VOCs降低不显著,导致臭氧浓度不降反升,通过对VOCs与NOx等污染物的协同控制来有效减少污染物排放,从而促进环境空气质量持续提升与改善。因此,PM2.5和臭氧的协同治理的关键就是NOx和VOCs的协同减排。
因此,开发高效协同去除甲苯和NOx净化材料和技术具有重要意义。
目前,NOx的控制技术可以划分为:(1)燃烧前脱硝,指的是去除燃料中含氮的化合物,实现源头减量;(2)燃烧中脱硝(炉内脱硝),通过调整和控制燃烧过程,减少NOx的产生;(3)燃烧后脱硝(烟气脱硝),通过化学反应对炉内产生的NOx进行脱除。炉内脱硝技术主要包括:低氮燃烧器、燃料分级燃烧、空气分级燃烧、烟气再循环等,其脱硝效率不高,一般不高于50%。选择性非催化还原技术(SNCR)是在炉膛上方,850~1100℃的温度范围内,喷入还原剂,将烟气中NO还原为N2,一般也归为炉内脱硝。常用的还原剂有氨和尿素,脱除效率在30~50%左右。SNCR技术由于设备简单,对电厂改造较小,所以应用较为广泛,但是,当还原剂喷入量过量时,会出现氨逃逸现象,造成烟道的腐蚀。
炉内脱硝技术的应用后烟气没有被脱除的NOx并不能满足排放标准的要求,因此需要借助烟气脱硝技术,进一步脱除。常见的烟气脱硝技术有选择性催化还原技术(SCR)和氧化吸收技术。氧化吸收技术是向烟气或者湿法喷淋塔中加入氧化性物质,例如,NaClOx、H2O2、KMnO4、O3、EDTA等,将NO氧化高价态NOx,最后湿法吸收。SCR技术是目前大型的燃煤电厂应用最为广泛的技术,它是借助催化剂的作用,使用还原剂将NO还原为N2。相比较于SNCR技术,它的脱除效率较高,可达90%。SCR是以NH3作还原剂,借助催化剂,使NOx和NH3在150~450℃温度区间发生归中反应转化为N2和H2O(4NH3+4NO+O2→4N2+6H2O),副产物为N2O(4NH3+4NO+3O2→4N2O+6H2O),反应温度较高时易发生NH3氧化。
工业上的VOCs种类繁多,成分复杂。VOCs的来源可分为自然源和人为源。其中,自然源包括植物释放、火山爆发等自然因素导致的VOCs的排放。人为源又包括移动源和固定源。移动源是指通过交通运输排放的VOCs,固定源是指由于工农业生产等因素导致的VOCs的排放,其中工业生产主要包括家具板材、石油加工、炼油、化工、涂料、汽修、橡胶、包装印刷和装修等行业的生产活动。农业生产活动主要包括大量农药化肥的生产和使用。在化工企业中,以甲苯为代表的苯系物是其排放的主要污染物。大部分VOCs具有毒性,会对人体造成不同的伤害。研究表明,人体接触高浓度的甲苯,会影响中枢神经***,引起神经***的紊乱。除了影响人体健康外,其排放到大气中,与大气中的NOx反应产生的光化学污染和近地面臭氧污染对生态环境造成难以修复的损害。
目前,对于VOCs的治理技术可分为源头控制和末端治理两大类。源头控制为预防性措施,对生产成本,运行方式,生产设备要求较高,以目前的技术水平很难有效去除,末端处理技术主要有燃烧法、吸附法、生物法、膜分离法和等离子体法,其中,吸附法和催化燃烧法处理量大,去除效率高,是目前为止处理燃煤烟气和工业废气等大气量烟气的两种可行方法。
(1)吸附控制技术主要通过吸附剂对废气中VOCs进行物理吸附,从而达到净化烟气的作用,是目前应用较为广泛的一种VOCs处理技术,常用的吸附剂有分子筛、活性炭、多孔矿物质。其中,活性炭由于具有较大的比表面积,丰富的孔隙结构和表面官能团等优点,得到了大量的关注。李立清等研究了酸(硝酸、硫酸、盐酸)改性活性炭对甲苯和甲醇吸附性能的影响,发现HNO3处理后活性炭的比表面积和孔容都增大,表面含氧官能团增多,吸附性能提升;解立平等制备了废弃物基活性炭,研究了其甲苯的吸附性能,发现废弃物基活性炭具有优惠型等温线平衡曲线,具有良好的吸附性能,实现了废弃物再利用。
(2)燃烧法处理VOCs废气分为三种:直接燃烧法,适用于较高浓度的VOCs废气,对于低浓度的VOCs难以根除;借助其他助燃剂,将VOCs引燃,成本较高,有二次污染;催化燃烧,借助催化剂,降低化学反应的活化能,在氧化性气氛中,直接将VOCs降解为CO2和H2O,二次污染小,反应彻底。相比于直接燃烧法和助燃法,催化燃烧不会产生NOx、SO2等二次污染,在VOCs减排也有相应的应用。
胡芸等人对比商业NH3-SCR催化剂通过浸渍法研究了双功能Cu-VWTi催化剂对NOx与甲苯、丙烯二氯甲烷与萘等协同处理的性能研究,在350℃以上催化剂对50ppm甲苯的转化率达到99%以上同时维持NOx转化率大于90%(Environ.Sci.Technol.2022,56,3719-3728);肖高飞等人采用商业催化剂的制备方法制备出V2O5-WO3/TiO2以及V2O5-MoO3/TiO2催化剂在350℃下对50ppm甲苯转化率达到90%(Chemical Engineering Journal,2022,435,134914);此外,对于NOx与甲苯协同去除,研究者还研究了Mo/Ni浸渍的VWTiOx催化剂对100ppm甲苯以及500ppm NOx之间的协同控制的反应机理,在260℃以上两种浸渍后的催化剂的甲苯的转化率达到99%,而NOx的转化率在420℃到达70%(Applied Surface Science599(2022)153986);于成龙等人研究了不同形貌的MnOx的催化剂对NOx与甲苯协同催化性能及机理,MnOx纳米棒催化剂同时去除NOx和甲苯的活性明显优于MnOx纳米立方体催化剂(Journal ofEnvironmental Chemical Engineering 10(2022)108646);张世红等通过水热法制备出Cu-SAPO-34,再通过过量浸渍法将MnOx负载在水热法制备出的载体上,从而MnOx/Cu-SAPO-34催化剂,并研究该催化剂对50ppm甲苯以及500ppmNO协同催化性能以及反应机理,在温度区间300~380℃条件下,氮氧化物和甲苯的最佳同步去除性能≥80%,同时具有较高的CO2选择性(~100%)和N2选择性(>80%),众多研究者以甲苯作为模型分子对NOx与芳香化合物的协同去除从性能和机理两方面做了初步探索。上述催化剂大部分采用具有较大毒性的金属钒,且制备步骤繁琐,且大量有毒性化学试剂的使用对人体和环境造成严重危害。
发明内容
本发明的目的在于提供一种介孔铁基复合氧化物催化剂及其制备方法和应用,用于解决催化剂毒性较大、制备工艺复杂和不能高效协同去除NOx和甲苯的技术问题。
为了实现上述发明目的,本发明提供以下技术方案:
本发明提供了一种介孔铁基复合氧化物催化剂,所述铁基复合氧化物催化剂的化学式为FeaMbW(a+b)/4Oy,其中,M为Ce、Cu、Co和Ga中的一种或几种,0≤a≤1,0≤b≤1,0≤y≤9。
本发明还提供了一种介孔铁基复合氧化物催化剂的制备方法,包括以下步骤:
(1)将铁盐、金属盐和钨盐依次加入尿素溶液中进行反应,得到前驱体溶液;
(2)将前驱体溶液静置一定时间后,倒掉上清液,对剩余物顺次进行离心、干燥和焙烧处理,即得到铁基复合氧化物催化剂;
所述金属盐为硝酸盐或硫酸盐。
进一步的,步骤(1)中,所述反应的温度为80~100℃,反应的时间为12~36h。
进一步的,步骤(1)中,所述尿素溶液的质量分数为2~5%,所述铁盐:金属盐:钨盐的质量比为1~3:0.5~2:0.4~1;
所述尿素溶液中尿素和铁盐的质量比为5~13:1~3。
进一步的,步骤(2)中,所述离心的转速为4000~6000rpm;所述干燥的温度为80~100℃,干燥的时间为20~48h;所述焙烧处理的温度为400~600℃,焙烧处理的时间为4~6h,升温速率为3~8℃/min。
本发明还提供了一种介孔铁基复合氧化物催化剂在甲苯和氮氧化物协同处理中的应用,将介孔铁基复合氧化物催化剂和混合原料气体混合后进行反应即可。
进一步的,所述混合原料气体包含400~1000ppm NH3、400~1000ppmNO、3~20%O2和100~700ppm甲苯。
进一步的,所述混合原料气体的总流量为100~400mL/min,所述介孔铁基复合氧化物催化剂用量为0.1~0.7g。
进一步的,所述反应的温度为150~500℃。
进一步的,所述混合原料气体的空速为10000~70000h-1。
本发明的有益效果:
(1)本发明的催化剂在协同反应中,可以保持较好的脱硝性能,以及良好的甲苯氧化能力,具有很好的工业应用前景;
(2)本发明的催化剂制备采用简单的尿素沉淀法制备,无需其他复杂操作,方法简单快捷,条件易于控制,重复性高,本发明所用催化剂材料来源广泛且价格相对较低,催化剂成本低廉。
附图说明
图1为实施例1所制备的催化剂的甲苯催化脱除活性图;
图2为实施例1所制备的催化剂的NOx催化脱除活性图;
图3为实施例2所制备的催化剂的甲苯催化脱除活性图;
图4为实施例2所制备的催化剂的NOx催化脱除活性图;
图5为实施例2所制备的催化剂在不同甲苯浓度下甲苯催化脱除活性图;
图6为实施例2所制备的催化剂在不同甲苯浓度下NOx协同催化脱除活性图;
图7为实施例2中所制备的催化剂在不同氧浓度下甲苯催化脱除活性图;
图8为实施例2中所制备的催化剂在不同氧浓度下NOx催化脱除活性图。
具体实施方式
本发明提供了一种介孔铁基复合氧化物催化剂,所述铁基复合氧化物催化剂的化学式为FeaMbW(a+b)/4Oy,其中,M为Ce、Cu、Co和Ga中的一种或几种,0≤a≤1,0≤b≤1,0≤y≤9。
在本发明中,所述M优选为Ce、Co和Ga中的一种或几种,进一步优选为Ce。
本发明还提供了一种介孔铁基复合氧化物催化剂的制备方法,包括以下步骤:
(1)将铁盐、金属盐和钨盐依次加入尿素溶液中进行反应,得到前驱体溶液;
(2)将前驱体溶液静置一定时间后,倒掉上清液,对剩余物顺次进行离心、干燥和焙烧处理,即得到铁基复合氧化物催化剂;
所述金属盐为硝酸盐或硫酸盐。
在本发明中,所述金属盐优选为硝酸盐。
在本发明中,步骤(1)中,所述反应的温度为80~100℃,优选为85~95℃,进一步优选为90℃;反应的时间为12~36h,优选为18~28h,进一步优选为24h。
在本发明中,步骤(1)中,所述尿素溶液的质量分数为2~5%,优选为2.3~4.8%,进一步优选为2.5~4%;所述铁盐:金属盐:钨盐的质量比为1~3:0.5~2:0.4~1,优选为1.4~2.8:0.7~1.8:0.5~0.9,进一步优选为1.6~2.5:0.8~1.5:0.6~0.8。
在本发明中,所述尿素溶液中尿素和铁盐的质量比为5~13:1~3,优选为6~11:1.5~2.9,进一步优选为7~10:1.8~2.8。
在本发明中,步骤(2)中,所述离心的转速为4000~6000rpm,优选为4200~5700rpm,进一步优选为4500~5500rpm;所述干燥的温度为80~100℃,优选为85~95℃,进一步优选为90℃;干燥的时间为20~48h,优选为23~40h,进一步优选为27~35h。
在本发明中,所述焙烧处理的温度为400~600℃,焙烧处理的时间为4~6h,升温速率为3~8℃/min;优选的,焙烧处理的温度为450~550℃,焙烧处理的时间为4.5~5.5h,升温速率为4~6℃/min;进一步优选的,焙烧处理的温度为500℃,焙烧处理的时间为5h,升温速率为5℃/min。
在本发明中,静置的时间为10~24h,优选为12~20h,进一步优选为14~18h。
本发明还提供了一种介孔铁基复合氧化物催化剂在甲苯和氮氧化物协同处理中的应用,将介孔铁基复合氧化物催化剂和混合原料气体混合后进行反应即可。
在本发明中,所述混合原料气体包含400~1000ppm NH3、400~1000ppmNO、3~20%O2和100~700ppm甲苯,优选为450~800ppm NH3、460~850ppmNO、7~18%O2和200~600ppm甲苯,进一步优选为500~600ppm NH3、500~600ppm NO、10~15%O2和300~500ppm甲苯。
在本发明中,所述混合原料气体的总流量为100~400mL/min,优选为150~350mL/min,进一步优选为200~300mL/min;所述介孔铁基复合氧化物催化剂用量为0.1~0.7g,优选为0.2~0.5g,进一步优选为0.3~0.4g。
在本发明中,所述反应的温度为150~500℃,优选为200~480℃,进一步优选为250~450℃。
在本发明中,所述混合原料气体的空速为10000~70000h-1,优选为15000~65000h-1,进一步优选为20000~60000h-1。
下面结合实施例对本发明提供的技术方案进行详细的说明,但是不能把它们理解为对本发明保护范围的限定。
实施例1
(1)将7.2g尿素溶于250mL水中,配置成尿素溶液,依次加入2.9088g九水硝酸铁、1.0421g六水硝酸铈和0.5912g偏钨酸铵,在90℃反应24h;
(2)室温下静置12h,静置后将上清液倒掉,进行离心、干燥和焙烧处理,离心的转速为5000rpm,离心的时间为6min,干燥的温度为90℃,干燥的时间为24h,放入至马弗炉中焙烧,从室温升至500℃中焙烧5h,保持升温速率为5℃/min;
(3)将步骤(2)中所制备的催化剂经压片处理成40目颗粒状得到FeCeWO,其中Fe、Ce与W的摩尔比为3:1:1,即催化剂A。
实施例2~5
按实施例1的步骤制备的催化剂,区别在于将硝酸铈换成不同的金属硝酸盐,分别为硝酸铜、硝酸钴、硝酸镓和不加硝酸铈,其摩尔占比和硝酸铈一致,从而制备出FeCuWO、FeCoWO、FeGaWO、FeWO,其中Fe、Cu与W的摩尔比为3:1:1,Fe、Co与W的摩尔比为3:1:1,Fe、Ga与W的摩尔比为3:1:1,Fe与W的摩尔比为4:1,即催化剂B、C、D、E。
测试例1
将0.4g介孔铁基复合氧化物催化剂A、B、C、D和E分别与混合原料气体进行反应,反应在微型固定床连续流动微反应器中进行,反应结束后进行NOx和甲苯协同催化脱除活性测试,测试仪器为装有FID检测器的在线气相色谱仪,测试条件为:HP-1毛细柱;载气:高纯N2;进样口温度:150℃;柱温:110℃;FID检测器温度:270℃;测试的具体条件为:通入混合原料气体为500ppm甲苯、500ppm NH3、500ppm NO和体积浓度为3%的氧气,氩气为平衡气,混合原料气的总流量为250mL/min,混合原料气的空速为36000h-1。各个催化剂在不同温度下的甲苯和NOx的转化率结果如表1和表2所示,甲苯和NOx协同反应活性如图1和图2所示。
表1不同硝酸盐的催化剂甲苯的转化率
表2不同硝酸盐的催化剂氮氧化物的转化率
从表1、表2和图1、图2可以看出,催化剂A的甲苯T90%(转化率达到90%的温度)为325℃,催化剂B的T90%为300℃,催化剂C的T90%为375℃,催化剂D的T90%为400℃,催化剂E的T90%为375℃;此外,催化剂A的氮氧化物T90%(转化率达到90%的温度)为325℃,且温度窗口较宽,催化剂B的T90%无法达到90%,催化剂C、D、E也是如此,其中催化剂A表现了最好的甲苯催化氧化活性以及NOx去除率;当温度为450℃时,催化剂A、B、C、D和E的甲苯的转化率都达到了100%,氮氧化物也具有较高的转化率。
实施例6
按实施例1的步骤制备的催化剂,其他参数均不变,仅将原料替换为7.2g尿素、1.4396g硫酸铁、0.6821g硫酸铈和0.5912g偏钨酸铵制备得到Fe3CeWO9,即催化剂F。催化剂F的甲苯和NOx的转化率和协同反应活性的测试结果与催化剂A相近。
实施例7
改变实施例1中催化剂A中硝酸铁以及硝酸铈的用量,使Fe+Ce总摩尔不变为4。根据不同的Fe/Ce的摩尔比,将催化剂分为a,b,c,d,e,f,g,h,i,其中a为Fe:Ce:W=3:1:1、b为Fe:Ce:W=3.5:0.5:1、c为Fe:Ce:W=2.5:1.5:1、d为Ce:W=4:1、e为Fe:W=4:1、f为Fe:Ce:W=2:2:1、g为Fe:Ce:W=1.5:2.5:1、h为Fe:Ce:W=1:3:1、i为Fe:Ce:W=0.5:3.5:1。
测试例2
测试的具体条件为:200ppm甲苯、500ppm NH3、500ppm NO和体积浓度为3%的氧气,氩气为平衡气,反应气流量为250mL/min,反应气体空速为36000h-1。
各个催化剂在不同温度下的甲苯和NOx的转化率结果如表3和表4所示,各个催化剂随温度变化甲苯和NOx的反应活性曲线见图3和图4。
表3不同摩尔比的Fe/Ce的催化剂的甲苯转化率
表4不同摩尔比的Fe/Ce的催化剂的氮氧化物转化率
测试例3
采用实施例1中的催化剂A,改变测试条件中的甲苯浓度,其余条件保持不变,催化剂A在不同甲苯浓度条件下不同温度点的甲苯和NOx的转化率结果如表5和表6所示,其随温度变化的反应活性曲线见图5和图6。
表5不同甲苯浓度测试的甲苯转化率
表6不同甲苯浓度测试的氮氧化物转化率
测试例4
采用实施例1中的催化剂A,改变测试条件中的氧气浓度,其余条件保持不变,催化剂A在不同氧气浓度条件下不同温度点的甲苯和NOx的转化率结果如表7和表8所示,其随温度变化的反应活性曲线见图7和图8。
表7不同氧气浓度测试的甲苯转化率
表8不同氧气浓度测试的氮氧化物转化率
由以上实施例可知,本发明提供了一种介孔铁基复合氧化物催化剂及其制备方法和应用,在协同反应中,催化剂可以保持较好的脱硝性能,以及良好的甲苯氧化能力,具有很好的工业应用前景;同时催化剂制备采用简单的尿素沉淀法制备,无需其他复杂操作,方法简单快捷,条件易于控制,重复性高,本发明所用催化剂材料来源广泛且价格相对较低,催化剂成本低廉。
以上所述仅是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。
Claims (10)
1.一种介孔铁基复合氧化物催化剂,其特征在于,所述铁基复合氧化物催化剂的化学式为FeaMbW(a+b)/4Oy,其中,M为Ce、Cu、Co和Ga中的一种或几种,0≤a≤1,0≤b≤1,0≤y≤9。
2.权利要求1所述的介孔铁基复合氧化物催化剂的制备方法,其特征在于,包括以下步骤:
(1)将铁盐、金属盐和钨盐依次加入尿素溶液中进行反应,得到前驱体溶液;
(2)将前驱体溶液静置一定时间后,倒掉上清液,对剩余物顺次进行离心、干燥和焙烧处理,即得到铁基复合氧化物催化剂;
所述金属盐包括硝酸盐或硫酸盐。
3.根据权利要求2所述的制备方法,其特征在于,步骤(1)中,所述反应的温度为80~100℃,反应的时间为12~36h。
4.根据权利要求2或3所述的制备方法,其特征在于,步骤(1)中,所述尿素溶液的质量分数为2~5%,所述铁盐:金属盐:钨盐的质量比为1~3:0.5~2:0.4~1;
所述尿素溶液中尿素和铁盐的质量比为5~13:1~3。
5.根据权利要求4所述的制备方法,其特征在于,步骤(2)中,所述离心的转速为4000~6000rpm;所述干燥的温度为80~100℃,干燥的时间为20~48h;所述焙烧处理的温度为400~600℃,焙烧处理的时间为4~6h,升温速率为3~8℃/min。
6.权利要求1所述的介孔铁基复合氧化物催化剂在甲苯和氮氧化物协同处理中的应用,其特征在于,将介孔铁基复合氧化物催化剂和混合原料气体混合后进行反应即可。
7.根据权利要求6所述的介孔铁基复合氧化物催化剂在甲苯和氮氧化物协同处理中的应用,其特征在于,所述混合原料气体包含400~1000ppmNH3、400~1000ppmNO、3~20%O2和100~700ppm甲苯。
8.根据权利要求7所述的介孔铁基复合氧化物催化剂在甲苯和氮氧化物协同处理中的应用,其特征在于,所述混合原料气体的总流量为100~400mL/min,所述介孔铁基复合氧化物催化剂用量为0.1~0.7g。
9.根据权利要求7或8所述的介孔铁基复合氧化物催化剂在甲苯和氮氧化物协同处理中的应用,其特征在于,所述反应的温度为150~500℃。
10.根据权利要求9所述的介孔铁基复合氧化物催化剂在甲苯和氮氧化物协同处理中的应用,其特征在于,所述混合原料气体的空速为10000~70000h-1。
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