CN114811624B - DMF-containing waste gas purification co-production N2O method - Google Patents
DMF-containing waste gas purification co-production N2O method Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 51
- 239000002912 waste gas Substances 0.000 title claims abstract description 36
- 238000004519 manufacturing process Methods 0.000 title claims description 19
- 238000000746 purification Methods 0.000 title claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 60
- 239000003054 catalyst Substances 0.000 claims abstract description 34
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910001868 water Inorganic materials 0.000 claims abstract description 30
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910000510 noble metal Inorganic materials 0.000 claims abstract description 20
- 239000004215 Carbon black (E152) Substances 0.000 claims abstract description 14
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 14
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 14
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 14
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 14
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000007800 oxidant agent Substances 0.000 claims abstract description 4
- 230000001590 oxidative effect Effects 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims description 43
- 239000007789 gas Substances 0.000 claims description 26
- 238000010438 heat treatment Methods 0.000 claims description 24
- 239000000463 material Substances 0.000 claims description 22
- 229910002651 NO3 Inorganic materials 0.000 claims description 17
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 15
- 230000032683 aging Effects 0.000 claims description 13
- PRKQVKDSMLBJBJ-UHFFFAOYSA-N ammonium carbonate Chemical class N.N.OC(O)=O PRKQVKDSMLBJBJ-UHFFFAOYSA-N 0.000 claims description 13
- 239000010431 corundum Substances 0.000 claims description 13
- 229910052593 corundum Inorganic materials 0.000 claims description 13
- 229910052746 lanthanum Inorganic materials 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 13
- 238000000227 grinding Methods 0.000 claims description 12
- 238000005470 impregnation Methods 0.000 claims description 12
- 238000011068 loading method Methods 0.000 claims description 12
- 239000002131 composite material Substances 0.000 claims description 5
- 229910044991 metal oxide Inorganic materials 0.000 claims description 5
- 150000004706 metal oxides Chemical class 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 229910052763 palladium Inorganic materials 0.000 claims description 2
- 229910052707 ruthenium Inorganic materials 0.000 claims description 2
- 230000007613 environmental effect Effects 0.000 abstract description 14
- 239000012535 impurity Substances 0.000 abstract description 14
- 230000008569 process Effects 0.000 abstract description 7
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 193
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 19
- 230000003197 catalytic effect Effects 0.000 description 19
- 238000006731 degradation reaction Methods 0.000 description 18
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 16
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 16
- 150000002500 ions Chemical class 0.000 description 12
- 238000004064 recycling Methods 0.000 description 10
- 230000015556 catabolic process Effects 0.000 description 9
- 229910001960 metal nitrate Inorganic materials 0.000 description 9
- 238000011156 evaluation Methods 0.000 description 8
- 239000001294 propane Substances 0.000 description 8
- 238000001179 sorption measurement Methods 0.000 description 8
- 239000001272 nitrous oxide Substances 0.000 description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- NWAHZABTSDUXMJ-UHFFFAOYSA-N platinum(2+);dinitrate Chemical compound [Pt+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O NWAHZABTSDUXMJ-UHFFFAOYSA-N 0.000 description 4
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- GTCKPGDAPXUISX-UHFFFAOYSA-N ruthenium(3+);trinitrate Chemical compound [Ru+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O GTCKPGDAPXUISX-UHFFFAOYSA-N 0.000 description 3
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- -1 ketone compound Chemical class 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 1
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- UGACIEPFGXRWCH-UHFFFAOYSA-N [Si].[Ti] Chemical compound [Si].[Ti] UGACIEPFGXRWCH-UHFFFAOYSA-N 0.000 description 1
- 239000001361 adipic acid Substances 0.000 description 1
- 235000011037 adipic acid Nutrition 0.000 description 1
- 230000003444 anaesthetic effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 238000007084 catalytic combustion reaction Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000002649 leather substitute Substances 0.000 description 1
- 230000001089 mineralizing effect Effects 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 235000013842 nitrous oxide Nutrition 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- JTJMJGYZQZDUJJ-UHFFFAOYSA-N phencyclidine Chemical compound C1CCCCN1C1(C=2C=CC=CC=2)CCCCC1 JTJMJGYZQZDUJJ-UHFFFAOYSA-N 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000002760 rocket fuel Substances 0.000 description 1
- 239000000565 sealant Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000008256 whipped cream Substances 0.000 description 1
Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
- F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
- F23G7/00—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals
- F23G7/06—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases
- F23G7/07—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases in which combustion takes place in the presence of catalytic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
- B01J23/64—Platinum group metals with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/656—Manganese, technetium or rhenium
- B01J23/6562—Manganese
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
- B01J37/086—Decomposition of an organometallic compound, a metal complex or a metal salt of a carboxylic acid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
- B01J37/088—Decomposition of a metal salt
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/20—Nitrogen oxides; Oxyacids of nitrogen; Salts thereof
- C01B21/22—Nitrous oxide (N2O)
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Thermal Sciences (AREA)
- Physics & Mathematics (AREA)
- Environmental & Geological Engineering (AREA)
- Health & Medical Sciences (AREA)
- Emergency Medicine (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a method for coproducing N 2 O by purifying waste gas containing DMF. According to the invention, a noble metal supported hexaaluminate catalyst is adopted, the expression formula is M-LaMn xAlyO19, wherein x is more than or equal to 1 and less than or equal to 4, y is more than or equal to 8 and less than or equal to 11, M is noble metal with the mass fraction of 0.1-2%, air is adopted as an oxidant, the temperature is 200-250 ℃, the concentration of DMF is 0.1-2%, DMF and organic matters in waste gas are completely mineralized under normal pressure, contained hydrocarbon is completely mineralized into carbon dioxide and water, and most nitrogen in DMF is converted into N 2 O at the same time, NH 3、NO、NO2, organic matters and other impurities are not generated, and the difficulty and cost of purifying N 2 O in the later stage are effectively reduced, so that the method is a novel process with low investment, low cost, low risk coefficient and environmental friendliness.
Description
Technical Field
The invention belongs to the technical field of catalytic combustion environment protection, and particularly relates to a method for producing N 2 O by using DMF (dimethyl formamide) -containing waste gas purification in a synergistic manner.
Background
Nitrous oxide, also known as nitrous oxide, of the formula N 2 O, also known as laughing gas, has a wide range of applications in the fields of electronics industry, food processing, medicine, energy sources, etc. Specifically, in the electronic industry, N 2 O is used as a special gas or a balance protection gas, and is widely applied to processes of integrated circuits, semiconductors, chips, phototubes, tablet computers, photovoltaic cell production and the like. In the food industry, N 2 O can be used as a foam spray for whipped cream and as a sealant for food products. In the medical field, N 2 O can be mixed with oxygen as an anesthetic for surgical and dental procedures. In the field of energy, N 2 O can be used as an auxiliary ingredient of combustion improver or rocket fuel and the like. In summary, N 2 O has wide application and very important economic value.
At present, the production method of nitrous oxide mainly comprises an ammonium nitrate thermal decomposition method, an ammonia catalytic oxidation method, a urea method and the like, but has serious explosion risks, the whole process is in a dangerous state, and the purchase, transportation, storage and use of raw materials are in strict security control. The traditional process has low productivity, requires huge equipment investment and has high production cost. Patent application number 201110387622.0 discloses a method for preparing nitrous oxide by using ketone compound, hydrogen peroxide and ammonia in the presence of titanium-silicon molecular sieve-containing catalyst, the method needs to react for 0.3-6 hours under the reaction condition of 0.1-2.0MPa to obtain mixed gas containing nitrous oxide, and the reaction needs to use dangerous raw materials such as hydrogen peroxide and ammonia, etc., and the reaction period is long. In addition, in the production of nitric acid and adipic acid, the recovery of nitrous oxide by treating the nitrous oxide-containing waste gas generated during the production process has been used, however, the impurities such as NH 3、NO、NO2 and organics in the tail gas increase the cost of purifying N 2 O to some extent. Therefore, a new process for preparing raw materials at low cost and having a low risk coefficient is demanded, the influence of impurities such as NH 3、NO、NO2 and organic matters is reduced as much as possible, and N 2 O is produced in a low-input, low-cost and environment-friendly manner, which has important significance.
Dimethylformamide (DMF) is a nitrogen-containing organic compound, and has a chemical formula of HCON (CH 3)2), which is an extremely wide-purpose chemical raw material and is also an excellent solvent with wide application, and a great amount of use and emission are available in the fields of color steel plate industry, synthetic leather industry, fiber synthesis industry, dye industry, petroleum industry, pesticide industry and the like, DMF emission not only causes serious pollution to the environment but also directly or indirectly damages human health, the patent with application number 201811184190.1 discloses a method for treating nitrogen-containing volatile organic pollutants, and although the method can effectively degrade DMF and convert nitrogen into N 2 as much as possible, thereby achieving the requirement of environmental protection, but also being a waste of potential resources for nitrogen, so that if DMF can be catalytically degraded to thoroughly mineralize, nitrogen resources in DMF can be converted into N 2 O, pollution control of waste gas can be realized, and the N 2 can be prepared by combining with the existing method for extracting N 2 from waste gas, and simultaneously, the method has good economic benefit.
Disclosure of Invention
The invention aims to provide a method for producing N 2 O by co-purification of waste gas containing DMF, which adopts hexaaluminate material loaded with noble metal as catalyst, oxygen in air as oxidant, DMF in waste gas is completely mineralized, hydrocarbon element is mineralized into carbon dioxide and water, nitrogen element is converted into N 2 O, the expression of hexaaluminate material loaded with noble metal is M-LaMn xAlyO19, wherein x is more than or equal to 1 and less than or equal to 4, y is more than or equal to 8 and less than or equal to 11, M is noble metal with mass fraction of 0.1-2%, and the noble metal is one or more of Pd, pt and Ru.
Wherein the concentration of DMF is 0.1-2%, the gas space velocity is 1000-9000 h -1, and the reaction temperature is 200-250 ℃.
Preferably, the DMF concentration is 0.1-1% and the gas space velocity is 1000-6000 h -1.
The preparation steps of the catalyst are as follows:
1) Dissolving nitrate of La, mn and Al with the mol ratio of 1:1-4:8-11 into water at 50-70 ℃;
2) Adding the solution into saturated ammonium carbonate solution, maintaining the pH to 8.5-9.5, stirring, aging for 3-6 hours, and centrifuging;
3) Drying and roasting to obtain the LaMn 1-4Al8-11O19 composite metal oxide material;
4) Loading 0.1-2% of noble metal nitrate on the LaMn 1-4Al8- 11O19 by an isovolumetric impregnation method, drying and roasting for 2-6 hours at 500-600 ℃ to obtain the hexaaluminate material catalyst loaded with noble metal.
The step 3) is specifically that the sample is firstly dried for 12-15 hours at 120-130 ℃, ground, then placed in a corundum crucible, heated to 500-600 ℃ at 5 ℃/min, maintained for 3-5 hours, and then heated to 1200-1400 ℃ at 2 ℃/min, maintained for 4-6 hours.
Preferably, the catalyst is prepared as follows:
1) Dissolving nitrate of La, mn and Al with the molar ratio of 1:1-4:8-11 into water at 70 ℃;
2) Adding the solution into saturated ammonium carbonate solution, maintaining the pH to 8.5-9.5, stirring, aging for 5 hours, and centrifuging;
3) Firstly, drying a sample at 120 ℃ for 15 hours, grinding, then placing the sample in a corundum crucible, heating to 600 ℃ at 5 ℃/min, maintaining for 3 hours, and then heating to 1300 ℃ from 600 ℃ at 2 ℃/min for 5 hours to obtain the LaMn 1-4Al8-11O19 composite metal oxide material;
4) Loading 0.1-1% of noble metal nitrate into LaMn 1-4Al8- 11O19 by an isovolumetric impregnation method, and roasting at 500 ℃ for 2 hours to obtain the noble metal-loaded hexaaluminate material catalyst.
According to the method, a hexaaluminate material loaded with noble metal is used as a catalyst, air is used as an oxidant, DMF in waste gas is completely mineralized at normal pressure within a specific temperature window of 200-250 ℃, hydrocarbon element is mineralized into carbon dioxide and water, most of nitrogen element in the waste gas is converted into N 2 O, a small amount of nitrogen element is converted into harmless N 2, N 2 O in tail gas can be discharged up to standard after being adsorbed, concentrated and recovered, wherein the selectivity of N 2 O is 50-65%, the selectivity of N 2 is 35-50%, impurities such as NH 3、NO、NO2 and organic matters are not generated, and the method has the condition of low-cost purification of N 2 O, and is a novel process for producing N 2 O with low investment, low cost, low risk coefficient and environmental friendliness.
The method provided by the invention realizes the production of N 2 O in the catalytic degradation process of DMF waste gas, avoids the environmental hazard caused by the emission of DMF into the atmosphere, realizes the recycling conversion of nitrogen element while the DMF waste gas is completely mineralized, and produces N 2 O.
The invention has the beneficial effects that
(1) The invention provides a method capable of thoroughly mineralizing DMF-containing organic waste gas, and simultaneously realizes high-value conversion of nitrogen element in the waste gas, thereby avoiding environmental hazard caused by discharging DMF into the atmosphere, realizing conversion and utilization of nitrogen resource, and having the condition of low-cost purification of N 2 O. Within the temperature window of 200-250 ℃, the hydrocarbon contained in DMF in the waste gas is completely mineralized into carbon dioxide and water, most of nitrogen element is converted into N 2 O, and a small part of nitrogen element is converted into environment-friendly nitrogen. In addition, NH 3、NO、NO2, organic matters and other impurities are not generated in the process, and conditions are provided for low-cost adsorption concentration and recovery of N 2 O.
(2) The invention is a new process for producing N 2 O with low investment, low cost, low risk coefficient and environmental protection, and has wide application prospect in the fields of DMF waste gas purification and N 2 O preparation.
Drawings
FIG. 1 is a plot of the selectivity of nitrogen-containing byproducts of example 1;
FIG. 2 is a graph of DMF conversion and selectivity to CO 2 in example 1.
Detailed Description
The following describes the embodiments of the present invention in further detail with reference to examples. The following examples are illustrative of the invention and are not intended to limit the scope of the invention.
Example 1
At 60 ℃, nitrate of La, mn and Al with the mol ratio of 1:3:9 is dissolved into water to prepare mixed ion solution, the mixed metal nitrate solution is added into saturated ammonium carbonate solution, ph is maintained to be about 7.5-9.5, and after stirring and ageing for 3 hours, the mixed ion solution is centrifuged. Drying at 120 ℃ for 12 hours, grinding the dried sample, placing the ground sample in a corundum crucible, heating to 500 ℃ at 5 ℃/min, maintaining for 5 hours, and then heating to 1200 ℃ from 500 ℃ at 2 ℃/min for 6 hours. The 1% Pd-LaMn 3Al9O19 catalyst is obtained by loading 1% (calculated as Pd, the same applies below) of palladium nitrate to LaMn 3Al9O19 by using LaMn 3Al9O19 as a carrier and roasting at 500 ℃ for 2 hours by an isovolumetric impregnation method.
Under the air reaction atmosphere, a 1% Pd-LaMn 3Al9O19 catalyst is used for the catalytic degradation of DMF. The reaction performance was evaluated in a fixed bed continuous flow reactor with DMF generating steam by bubbling at a specific temperature, the line having 120℃heat, DMF concentration of 0.5% and gas space velocity of 9000 h -1. The catalyst of 0.4 g after tabletting and sieving (40-60 meshes) is placed in a quartz reaction tube with the inner diameter of 6mm, the reactivity is tested in the temperature range of 100-400 ℃, a temperature point is set at every 50 ℃, after each temperature point is kept stable for 0.5 h, gas composition concentration data are collected, and the reactants and the products are detected on line through a GC-7890B gas chromatograph and a Fourier transform infrared spectrum gas analyzer. The result shows that 0.5% of DMF in the waste gas is completely mineralized in the air reaction atmosphere within a temperature window of 200-250 ℃, hydrocarbon is mineralized into carbon dioxide and water, the selectivity of converting most of nitrogen in DMF into N 2O,N2 O is 59-65%, the selectivity of N 2 is 35-41%, and impurities such as NH 3、NO、NO2 and organic matters are not generated, so that conditions are provided for recovering N 2 O by low-cost adsorption concentration. The method realizes the production of N 2 O in the catalytic degradation process of DMF waste gas, avoids the environmental hazard caused by the emission of DMF into the atmosphere, and simultaneously realizes the recycling conversion of nitrogen.
Example 2
At 50 ℃, nitrate of La, mn and Al with the mol ratio of 1:3:9 is dissolved into water to prepare mixed ion solution, the mixed metal nitrate solution is added into saturated ammonium carbonate solution, ph is maintained to be about 7.5-9.5, and after stirring and aging for 5 hours, the mixture is centrifuged. Drying at 130 ℃ for 15 hours, grinding the dried sample, placing the ground sample in a corundum crucible, heating to 600 ℃ at 5 ℃/min, maintaining for 5 hours, and subsequently heating to 1300 ℃ from 600 ℃ at 2 ℃/min for 5 hours. The catalyst 0.5% Pd-LaMn 3Al9O19 is obtained by loading 0.5% palladium nitrate into LaMn 3Al9O19 by using LaMn 3Al9O19 as a carrier and roasting at 500 ℃ for 2 hours by an isovolumetric impregnation method.
The prepared 0.5% Pd-LaMn 3Al9O19 catalyst material is used for the catalytic degradation and conversion of DMF with the concentration of 2%. The reaction evaluation method was the same as in example 1, and the gas space velocity was 5000 h -1. The result shows that 2% of DMF in the waste gas is completely mineralized, hydrocarbon is mineralized into carbon dioxide and water in the air reaction atmosphere within a temperature window of 200-250 ℃, the selectivity of converting most of nitrogen in DMF into N 2O,N2 O is 55-62%, the selectivity of N 2 is 38-45%, and impurities such as NH 3、NO、NO2 and organic matters are not generated, so that conditions are provided for recovering N 2 O by low-cost adsorption concentration. The method realizes the production of N 2 O in the catalytic degradation process of DMF waste gas, avoids the environmental hazard caused by the emission of DMF into the atmosphere, and simultaneously realizes the recycling conversion of nitrogen.
Example 3
At 70 ℃, nitrate of La, mn and Al with the mol ratio of 1:1:11 is dissolved into water to prepare mixed ion solution, the mixed metal nitrate solution is added into saturated ammonium carbonate solution, ph is maintained to be about 7.5-9.5, and after stirring and aging for 4 hours, the mixed ion solution is centrifuged. Drying at 130 ℃ for 13 hours, grinding the dried sample, placing the ground sample in a corundum crucible, heating to 600 ℃ at 5 ℃/min, maintaining for 4 hours, and subsequently heating to 1300 ℃ from 600 ℃ at 2 ℃/min for 5 hours. The catalyst is prepared by taking LaMn 1Al11O19 as a carrier, loading palladium nitrate, platinum nitrate and ruthenium nitrate with mass fractions of 0.2% to LaMn 1Al11O19 by an isovolumetric impregnation method, and roasting at 600 ℃ for 2 hours to obtain the catalyst of 0.2% Pd-0.2% Pt-0.2% Ru-LaMn 1Al11O19.
The prepared catalyst material of 0.2% Pd-0.2% Pt-0.2% Ru-LaMn 1Al11O19 is used for catalytic degradation and conversion of 1% DMF. The reaction evaluation method was the same as in example 1, and the gas space velocity was 2000 h -1. The result shows that DMF in the waste gas is completely mineralized, hydrocarbon is mineralized into carbon dioxide and water in the temperature window of 200-250 ℃ under the air reaction atmosphere, the selectivity of converting most of nitrogen in DMF into N 2O,N2 O is 57-63%, the selectivity of N 2 is 37-43%, and impurities such as NH 3、NO、NO2 and organic matters are not generated, so that conditions are provided for recovering N 2 O by low-cost adsorption and concentration. The method realizes the production of N 2 O in the catalytic degradation process of DMF waste gas, avoids the environmental hazard caused by the emission of DMF into the atmosphere, and simultaneously realizes the recycling conversion of nitrogen.
Example 4
At 65 ℃, nitrate of La, mn and Al with the mol ratio of 1:4:8 is dissolved into water to prepare mixed ion solution, the mixed metal nitrate solution is added into saturated ammonium carbonate solution, ph is maintained to be about 7.5-9.5, and after stirring and aging for 6 hours, the mixture is centrifuged. Drying at 125 ℃ for 14 hours, grinding the dried sample, placing the ground sample in a corundum crucible, heating to 600 ℃ at 5 ℃/min, maintaining for 3 hours, and then heating to 1200 ℃ from 600 ℃ at 2 ℃/min for 6 hours. The catalyst 0.1% Ru-LaMn 4Al8O19 is obtained by loading 0.1% ruthenium nitrate into LaMn 4Al8O19 by using LaMn 4Al8O19 as a carrier and roasting at 500 ℃ for 6 hours by an isovolumetric impregnation method.
The prepared 0.1% Ru-LaMn 4Al8O19 catalyst material is used for catalytic degradation and conversion of 0.1% DMF. The reaction evaluation method was the same as in example 1, and the gas space velocity was 1000 h -1, and the gas contained 1% acetone. The result shows that DMF and acetone in the waste gas are completely mineralized in the air reaction atmosphere within a temperature window of 200-250 ℃, hydrocarbon is mineralized into carbon dioxide and water, the selectivity of converting most nitrogen in DMF into N 2O,N2 O is 51-58%, the selectivity of N 2 is 42-49%, and impurities such as NH 3、NO、NO2 and organic matters are not generated, so that conditions are provided for recovering N 2 O by low-cost adsorption concentration. The method realizes the production of N 2 O in the catalytic degradation process of DMF waste gas, avoids the environmental hazard caused by the emission of DMF into the atmosphere, and simultaneously realizes the recycling conversion of nitrogen.
Example 5
At 70 ℃, nitrate of La, mn and Al with the mol ratio of 1:4:8 is dissolved into water to prepare mixed ion solution, the mixed metal nitrate solution is added into saturated ammonium carbonate solution, ph is maintained to be about 7.5-9.5, and after stirring and aging for 4 hours, the mixed ion solution is centrifuged. Drying at 120 ℃ for 12 hours, grinding the dried sample, placing the ground sample in a corundum crucible, heating to 500 ℃ at 5 ℃/min, maintaining for 5 hours, and then heating to 1200 ℃ from 500 ℃ at 2 ℃/min for 6 hours. The catalyst is prepared by taking LaMn 4Al8O19 as a carrier, loading platinum nitrate and ruthenium nitrate with mass fractions of 0.6% to LaMn 4Al8O19 by an isovolumetric impregnation method, and roasting at 550 ℃ for 4 hours to obtain the catalyst of 0.6% Pt-0.6% Ru-LaMn 4Al8O19.
The prepared catalyst material of 0.6% Pt-0.6% Ru-LaMn 4Al8O19% is used for catalytic degradation and conversion of 0.5% DMF. The reaction evaluation method was the same as in example 1, and the gas space velocity was 5000 h -1, and 0.2% propane was contained in the gas. The result shows that DMF and propane in the waste gas are completely mineralized in the air reaction atmosphere within the temperature window of 200-250 ℃, hydrocarbon is mineralized into carbon dioxide and water, the selectivity of converting most nitrogen in DMF into N 2O,N2 O is 55-60%, the selectivity of N 2 is 40-45%, and impurities such as NH 3、NO、NO2 and organic matters are not generated, so that conditions are provided for recovering N 2 O by low-cost adsorption concentration. The method realizes the production of N 2 O in the catalytic degradation process of DMF waste gas, avoids the environmental hazard caused by the emission of DMF into the atmosphere, and simultaneously realizes the recycling conversion of nitrogen.
Example 6
At 50 ℃, nitrate of La, mn and Al with the mol ratio of 1:4:8 is dissolved into water to prepare mixed ion solution, the mixed metal nitrate solution is added into saturated ammonium carbonate solution, ph is maintained to be about 7.5-9.5, and after stirring and aging for 5 hours, the mixture is centrifuged. Drying at 130 ℃ for 15 hours, grinding the dried sample, placing the ground sample in a corundum crucible, heating to 600 ℃ at 5 ℃/min, maintaining for 4 hours, and subsequently heating to 1400 ℃ from 600 ℃ at 2 ℃/min, and maintaining for 4 hours. The 2% Pd-LaMn 4Al8O19 catalyst is obtained by taking LaMn 4Al8O19 as a carrier, loading 2% palladium nitrate into LaMn 4Al8O19 by mass fraction through an isovolumetric impregnation method, and roasting at 500 ℃ for 4 hours.
The prepared 2% Pd-LaMn 4Al8O19 catalyst material is used for catalytic degradation and conversion of 0.5% DMF. The reaction evaluation method was the same as in example 1, and the gas space velocity was 9000 h -1, and the gas contained 0.1% propane, 0.1% acetone, 0.1% water, and 0.1% co 2. The result shows that DMF, propane and acetone in the waste gas are completely mineralized in the air reaction atmosphere within a temperature window of 200-250 ℃, hydrocarbon is mineralized into carbon dioxide and water, the selectivity of converting most of nitrogen in DMF into N 2O,N2 O is 52-61%, the selectivity of N 2 is 39-48%, and impurities such as NH 3、NO、NO2 and organic matters are not generated, so that conditions are provided for absorbing, concentrating and recycling N 2 O at low cost. The method realizes the production of N 2 O in the catalytic degradation process of DMF waste gas, avoids the environmental hazard caused by the emission of DMF into the atmosphere, and simultaneously realizes the recycling conversion of nitrogen.
Example 7
At 70 ℃, nitrate of La, mn and Al with the mol ratio of 1:3:9 is dissolved into water to prepare mixed ion solution, the mixed metal nitrate solution is added into saturated ammonium carbonate solution, ph is maintained to be about 7.5-9.5, and after stirring and aging for 4 hours, the mixture is centrifuged. Drying at 120 ℃ for 13 hours, grinding the dried sample, placing the ground sample in a corundum crucible, heating to 550 ℃ at 5 ℃/min, maintaining for 4 hours, and subsequently heating to 1250 ℃ from 550 ℃ at 2 ℃/min for 5 hours. The 1.5% Pt-LaMn 3Al9O19 catalyst is obtained by loading 2% by mass of platinum nitrate to LaMn 3Al9O19 by an isovolumetric impregnation method by taking LaMn 3Al9O19 as a carrier and roasting at 600 ℃ for 2 hours.
The prepared 1.5% Pt-LaMn 3Al9O19 catalyst material is used for catalytic degradation and conversion of 0.5% DMF. The reaction evaluation method was the same as in example 1, and the gas space velocity was 9000 h -1, and the gas contained 0.2% propane, 0.2% acetone, 3% water, and 2% co 2. The result shows that DMF, propane and acetone in the waste gas are completely mineralized in a temperature window of 200-250 ℃, hydrocarbon is mineralized into carbon dioxide and water, the selectivity of converting most of nitrogen in DMF into N 2O,N2 O is 50-55%, the selectivity of N 2 is 45-50%, and impurities such as NH 3、NO、NO2 and organic matters are not generated, so that conditions are provided for recovering N 2 O by low-cost adsorption and concentration. The method realizes the production of N 2 O in the catalytic degradation process of DMF waste gas, avoids the environmental hazard caused by the emission of DMF into the atmosphere, and simultaneously realizes the recycling conversion of nitrogen.
Example 8
At 70 ℃, nitrate of La, mn and Al with the mol ratio of 1:3:9 is dissolved into water to prepare mixed ion solution, the mixed metal nitrate solution is added into saturated ammonium carbonate solution, ph is maintained to be about 7.5-9.5, and after stirring and aging for 5 hours, the mixture is centrifuged. Drying at 120 ℃ for 13 hours, grinding the dried sample, placing the ground sample in a corundum crucible, heating to 600 ℃ at 5 ℃/min, maintaining for 3 hours, and subsequently heating to 1300 ℃ from 600 ℃ at 2 ℃/min for 5 hours. The catalyst is prepared by taking LaMn 3Al9O19 as a carrier, loading palladium nitrate and platinum nitrate with mass fractions of 0.4% into LaMn 3Al9O19 by an isovolumetric impregnation method, and roasting at 500 ℃ for 2 hours to obtain the catalyst of 0.4% Pb-0.4% Pt-LaMn 3Al9O19.
The prepared 0.4% Pb-0.4% Pt-LaMn 3Al9O19 catalyst material is used for catalytic degradation and conversion of 0.5% DMF. The reaction evaluation method was the same as in example 1, and the gas space velocity was 6000 h -1, and the gas contained 0.2% propane, 0.2% acetone, 3% water, and 2% co 2. The result shows that DMF, propane and acetone in the waste gas are completely mineralized in a temperature window of 200-250 ℃, hydrocarbon is mineralized into carbon dioxide and water, the selectivity of converting most nitrogen elements in DMF into N 2O,N2 O is 60-65%, the selectivity of N 2 is 35-40%, and impurities such as NH 3、NO、NO2 and organic matters are not generated, so that conditions are provided for recovering N 2 O by low-cost adsorption and concentration. The method realizes the production of N 2 O in the catalytic degradation process of DMF waste gas, avoids the environmental hazard caused by the emission of DMF into the atmosphere, and simultaneously realizes the recycling conversion of nitrogen.
Comparative example 1
At 60 ℃, nitrate of La, mn and Al with the mol ratio of 1:4:8 is dissolved into water to prepare mixed ion solution, and the mixed metal nitrate solution is added into saturated ammonium carbonate solution to maintain Ph to be about 7.5-9.5. After aging for 3 hours with stirring, centrifugation and drying at 120℃for 12 hours. After grinding the dried sample, placing the ground sample into a corundum crucible, heating to 500 ℃ at 5 ℃/min for 5 hours, and then heating to 1200 ℃ from 500 ℃ at 2 ℃/min for 6 hours to prepare the LaMn 4Al8O19 composite metal oxide material without carrying noble metal.
The prepared LaMn 4Al8O19 catalyst material is used for catalytic degradation and conversion of 0.5% DMF. The reaction evaluation method was the same as in example 1. The result shows that under the air reaction atmosphere, although DMF in the waste gas is completely mineralized at 200 ℃, hydrocarbon is mineralized into carbon dioxide and water, N 2 O is produced in the temperature range of 200-400 ℃, and meanwhile, NH 3、NO、NO2 and other impurities are also produced, so that the difficulty and cost of the purification of the later-stage N 2 O are increased to a certain extent.
The foregoing is merely a preferred embodiment of the present invention, and it should be noted that it will be apparent to those skilled in the art that modifications and variations can be made without departing from the technical principles of the present invention, and these modifications and variations should also be regarded as the scope of the invention.
Claims (5)
1. A method for producing N 2 O by using a waste gas purification and synergy method containing DMF is characterized in that the method adopts a hexaaluminate material loaded with noble metal as a catalyst, oxygen in air is used as an oxidant, DMF in the waste gas is completely mineralized, hydrocarbon element is mineralized into carbon dioxide and water, nitrogen element is converted into N 2 O, the expression of the hexaaluminate material loaded with noble metal is M-LaMn xAlyO19, wherein x is more than or equal to 1 and less than or equal to 4, y is more than or equal to 8 and less than or equal to 11, M is noble metal with mass fraction of 0.1-2%, and the noble metal is one or more of Pd, pt and Ru;
DMF concentration is 0.1-2%, gas space velocity is 1000-9000h -1, and reaction temperature is 200-250 ℃.
2. The method according to claim 1, wherein the DMF concentration is 0.1-1% and the gas space velocity is 1000-6000h -1.
3. The method according to claim 1, wherein the catalyst is prepared by the steps of:
1) Dissolving nitrate of La, mn and Al with a molar ratio of 1:1-4:8-11 into water at 50-70 ℃;
2) Adding the solution into saturated ammonium carbonate solution, maintaining the pH to 8.5-9.5, stirring, aging for 3-6 hours, and centrifuging;
3) Drying and roasting to obtain the LaMn 1-4Al8-11O19 composite metal oxide material;
4) Loading 0.1-2% of noble metal nitrate into LaMn 1-4Al8-11O19 by an isovolumetric impregnation method, and roasting at 500-600 ℃ for 2-6 hours to obtain the noble metal-loaded hexaaluminate material catalyst.
4. A method according to claim 3, characterized in that step 3) is performed by drying the sample at 120-130 ℃ for 12-15 hours, grinding, placing in a corundum crucible, heating to 500-600 ℃ at 5 ℃/min for 3-5 hours, and subsequently heating to 1200-1400 ℃ at 2 ℃/min for 4-6 hours.
5. The method according to claim 4, wherein the catalyst is prepared by the steps of:
1) Dissolving nitrate of La, mn and Al in a molar ratio of 1:1-4:8-11 into water at 70 ℃;
2) Adding the solution into saturated ammonium carbonate solution, maintaining the pH to 8.5-9.5, stirring, aging for 5 hours, and centrifuging;
3) Firstly, drying a sample at 120 ℃ for 15 hours, grinding, then placing the sample in a corundum crucible, heating to 600 ℃ at 5 ℃/min, maintaining for 3 hours, and then heating to 1300 ℃ from 600 ℃ at 2 ℃/min for 5 hours to obtain the LaMn 1-4Al8-11O19 composite metal oxide material;
4) Loading 0.1-1% of noble metal nitrate into LaMn 1-4Al8-11O19 by an isovolumetric impregnation method, and roasting at 500 ℃ for 2 hours to obtain the noble metal-loaded hexaaluminate material catalyst.
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| DE3442927A1 (en) * | 1984-11-24 | 1986-06-05 | Kali-Chemie Ag, 3000 Hannover | EXHAUST GAS TREATMENT METHOD |
| CN1013832B (en) * | 1988-01-26 | 1991-09-11 | 杭州大学 | Purification catalyst comprised of palladium, platinum and zeolite for organic waste gas |
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