WO2013134910A1 - 一种矿热熔融电炉尾气催化氧化净化的方法 - Google Patents
一种矿热熔融电炉尾气催化氧化净化的方法 Download PDFInfo
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- WO2013134910A1 WO2013134910A1 PCT/CN2012/072193 CN2012072193W WO2013134910A1 WO 2013134910 A1 WO2013134910 A1 WO 2013134910A1 CN 2012072193 W CN2012072193 W CN 2012072193W WO 2013134910 A1 WO2013134910 A1 WO 2013134910A1
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- Prior art keywords
- gas
- tail gas
- catalyst
- hours
- electric furnace
- Prior art date
Links
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 19
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 18
- 230000008569 process Effects 0.000 title abstract description 9
- 238000003723 Smelting Methods 0.000 title abstract 3
- 239000007789 gas Substances 0.000 claims abstract description 162
- 239000003054 catalyst Substances 0.000 claims abstract description 88
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000003513 alkali Substances 0.000 claims abstract description 30
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 24
- 238000005406 washing Methods 0.000 claims abstract description 23
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 20
- 239000001301 oxygen Substances 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 12
- 230000032683 aging Effects 0.000 claims abstract description 3
- 238000000746 purification Methods 0.000 claims description 49
- 238000006243 chemical reaction Methods 0.000 claims description 32
- 239000000243 solution Substances 0.000 claims description 30
- 238000002844 melting Methods 0.000 claims description 29
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- 239000012943 hotmelt Substances 0.000 claims description 20
- 230000003647 oxidation Effects 0.000 claims description 15
- 239000013064 chemical raw material Substances 0.000 claims description 14
- 239000007864 aqueous solution Substances 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 12
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 10
- 230000001590 oxidative effect Effects 0.000 claims description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- HWSZZLVAJGOAAY-UHFFFAOYSA-L lead(II) chloride Chemical compound Cl[Pb]Cl HWSZZLVAJGOAAY-UHFFFAOYSA-L 0.000 claims description 6
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 5
- 239000005909 Kieselgur Substances 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 229910021536 Zeolite Inorganic materials 0.000 claims description 5
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 5
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 5
- 239000011790 ferrous sulphate Substances 0.000 claims description 5
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 5
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 5
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 5
- 239000010457 zeolite Substances 0.000 claims description 5
- 238000005470 impregnation Methods 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims 2
- 239000001117 sulphuric acid Substances 0.000 claims 2
- 235000011149 sulphuric acid Nutrition 0.000 claims 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims 1
- 229910052700 potassium Inorganic materials 0.000 claims 1
- 239000011591 potassium Substances 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 23
- 239000002994 raw material Substances 0.000 abstract description 9
- 238000001816 cooling Methods 0.000 abstract description 2
- 238000001354 calcination Methods 0.000 abstract 1
- 230000003028 elevating effect Effects 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 38
- 229910052698 phosphorus Inorganic materials 0.000 description 38
- 239000011574 phosphorus Substances 0.000 description 38
- 239000012535 impurity Substances 0.000 description 28
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 27
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 23
- 239000011593 sulfur Substances 0.000 description 23
- 229910052717 sulfur Inorganic materials 0.000 description 23
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 16
- 229910052731 fluorine Inorganic materials 0.000 description 16
- 239000011737 fluorine Substances 0.000 description 16
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 15
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 14
- XDJWZONZDVNKDU-UHFFFAOYSA-N 1314-24-5 Chemical compound O=POP=O XDJWZONZDVNKDU-UHFFFAOYSA-N 0.000 description 13
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 13
- VSAISIQCTGDGPU-UHFFFAOYSA-N phosphorus trioxide Inorganic materials O1P(O2)OP3OP1OP2O3 VSAISIQCTGDGPU-UHFFFAOYSA-N 0.000 description 13
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 10
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 9
- 229910002091 carbon monoxide Inorganic materials 0.000 description 8
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 8
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 8
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 7
- 239000001569 carbon dioxide Substances 0.000 description 5
- 229910002092 carbon dioxide Inorganic materials 0.000 description 5
- 239000003344 environmental pollutant Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 231100000719 pollutant Toxicity 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000012159 carrier gas Substances 0.000 description 3
- 239000002440 industrial waste Substances 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- 230000008929 regeneration Effects 0.000 description 3
- 238000011069 regeneration method Methods 0.000 description 3
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000000443 aerosol Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000006315 carbonylation Effects 0.000 description 2
- 238000005810 carbonylation reaction Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000007602 hot air drying Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- TZIHFWKZFHZASV-UHFFFAOYSA-N methyl formate Chemical compound COC=O TZIHFWKZFHZASV-UHFFFAOYSA-N 0.000 description 2
- 231100000572 poisoning Toxicity 0.000 description 2
- 230000000607 poisoning effect Effects 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 125000001741 organic sulfur group Chemical group 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 230000009469 supplementation Effects 0.000 description 1
Classifications
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- B01D—SEPARATION
- 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
- B01D53/864—Removing carbon monoxide or hydrocarbons
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- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
- C01B3/56—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by contacting with solids; Regeneration of used solids
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- B01J2229/10—After treatment, characterised by the effect to be obtained
- B01J2229/18—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself
- B01J2229/186—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself not in framework positions
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
- C01B2203/0415—Purification by absorption in liquids
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/16—Controlling the process
- C01B2203/169—Controlling the feed
Definitions
- the invention relates to a method for catalytic oxidation purification of tail gas of a mine hot melt electric furnace.
- Carbon-based products are important organic chemical raw materials. With the reduction of petroleum resources and the rising price, the scope and quantity of carbon-based products replacing petrochemical products are expanding, and the status of carbon-based chemicals in various countries' economies is becoming more and more important. At present, carbon-chemical has become a hot spot for research and development in many countries around the world. New products, new processes, and new catalysts are emerging one after another. Carbon monoxide has almost become a chemical raw material with the same amount of basic chemical materials such as ethylene and propylene in petrochemical industry.
- the industrial waste gas is rich in carbon monoxide, and the CO in the ore-melting electric furnace is worthy of being utilized.
- Mineral hot melt When the electric furnace is used in chemical industry, it should be purified and purified first. If a 30 to 90% reduction of carbon monoxide containing carbon monoxide is used as a raw material for the production of a single carbon chemical product, high purity CO gas must first be obtained. Obviously, the presence of impurities in the tail gas of the ore-melting electric furnace greatly limits the effective utilization of the gas. In order to ensure the smooth progress of product quality and subsequent comprehensive utilization processes, it must be purified and pretreated.
- ore hot melt electric furnace exhaust gas as a raw material gas to produce a single carbon chemical product can also change the current high cost of the ore hot melt electric furnace production, and the situation in the market is weak, to achieve energy saving, energy saving, clean production.
- precious resources such as ore-melting electric furnace exhaust gas, which is rich in carbon monoxide, have been limited to drying raw materials, and most of the hot-melt electric furnace exhaust gas is directly burned and vented. The limiting factor is that the tail gas of the hot-melt electric furnace contains influences on it.
- the impurities of oxo synthesis that is, the problem of tail gas purification in the ore-melting electric furnace, have not been solved, especially the removal of phosphorus in the tail gas of the ore-melting electric furnace, which has a serious influence on the carbon monoxide carbonylation catalyst.
- the reaction is a reduction reaction occurring at a high temperature when the ore is reduced by the ore-melting electric furnace
- the impurities in the tail gas of the ore-melting electric furnace are mainly present in a reduced state.
- Phosphorus is mainly elemental phosphorus (P 4 ) and phosphine (PH 3 )
- sulfur is mainly hydrogen sulfide (H 2 S) and organic sulfur
- fluorine is mainly hydrogen fluoride (HF), silicon fluoride (SiF 4 ), etc.
- the current industry mainly uses water washing and alkaline washing to purify: 1.
- washing The reducing exhaust gas is cooled and dedusted, and fluoride and a part of elemental phosphorus, phosphine, hydrogen fluoride and hydrogen sulfide are removed. Since the vapor pressure of phosphorus rapidly decreases as the temperature decreases, some of the phosphorus in the exhaust gas is removed by condensation after the water wash is cooled, and a part of the hydrogen sulfide can be removed by dissolving in water.
- Alkali washing A large amount of acid gas such as carbon dioxide (co 2 ), hydrogen sulfide or hydrogen fluoride is removed by a chemical reaction using a 0.8 to 10% sodium hydroxide (NaOH) solution.
- acid gas such as carbon dioxide (co 2 )
- hydrogen sulfide or hydrogen fluoride is removed by a chemical reaction using a 0.8 to 10% sodium hydroxide (NaOH) solution.
- the main problems in the above methods are as follows: the removal efficiency of the elemental material is low, the removal is incomplete, and the use of various catalysts may cause poisoning of the catalyst, which cannot meet the requirements of the raw material gas of a carbon chemical.
- the invention overcomes the deficiencies of the prior art, aims to solve the problem of purification and pretreatment of the tail gas of the ore-melting electric furnace, and provides a method for catalytic oxidation purification of the tail gas of the ore-melting electric furnace, so that after purifying the tail gas of the ore-melting electric furnace, sulfur,
- concentration of typical impurities such as phosphorus and fluorine is less than 1 mg/m 3 , which makes it meet the requirements of high-value-added raw material gas for one-carbon chemical products.
- the tail gas of the ore-melting electric furnace is a reducing industrial waste gas.
- the main components are: CO 85 ⁇ 95% (V/V), C0 2 3 ⁇ 7% (V/V), H 2 1 ⁇ 8% (V/V), N 2 2 ⁇ 5% (V / V ), 0 2 0. 2 ⁇ 1% (V / V), TP 1000- 5000mg / m 3, H 2 S 1000 ⁇ 5000mg / m 3, HF 300 ⁇ 4000mg / m 3 .
- Alkaline washing can remove the typical pollutants in the elemental state in the tail gas of the ore-melting electric furnace, and convert the typical pollutants in the elemental state from the elemental state of the aerosol to the gas state, which is beneficial to the removal by the catalytic oxidation purification method;
- the reformed gas is heated to a fixed bed of catalytic oxidation, and the typical impurities in the gaseous state are removed by oxidizing a trace amount of oxygen in the tail gas of the ore-melting electric furnace.
- the tail gas of the hot-melt electric furnace is washed with an alkali-containing aqueous solution to remove impurities such as silicon fluoride, carbon dioxide and some elemental phosphorus in the tail gas.
- the reaction process is as follows:
- the washing solution containing N3 ⁇ 4C0 3 is subjected to causticization to recover NaOH and returned to the system for recycling.
- the exhaust gas still cannot meet the requirements for preparing raw materials for chemical products.
- the present invention adopts a high-efficiency purification technology of catalytic oxidation of tail gas in a mineral-melting electric furnace.
- the tail gas after the alkali washing is preheated by the preheater, and passes through the reactor from bottom to top.
- the reactor is filled with a high-efficiency catalyst, and elemental phosphorus, phosphine, and hydrogen fluoride impurities are catalytically oxidized.
- sulfur is catalytically oxidized:
- Phosphine has strong reducibility.
- the low-cost P in the exhaust gas undergoes redox reaction with high-valent metal ions (Me 3+ ), P is oxidized and converted to phosphoric acid, and metal ions (Me 3+ ) are reduced and reduced.
- the metal ions are oxidized by the 0 2 in the gas to achieve the recycling of the catalyst.
- the main reaction equation is as follows:
- the purified tail gas discharged from the reactor is cooled to 30 ° C by a cooling tower to obtain a qualified one carbon chemical raw material gas.
- the volume of oxygen in the exhaust gas obtained in the step (2) is 0. 5 ⁇ 3%, and the exhaust gas is passed from bottom to top at a rate of 300 to 600 m 3 (gas volume) / m 3 (catalyst volume).
- a catalytically oxidized fixed bed containing the high-efficiency catalyst obtained in the step (1) is subjected to a purification reaction at a reaction temperature of 50 to 100 ° C, and the purified gas is cooled to obtain a carbon chemical raw material gas.
- the catalyst carrier of the step (1) is activated alumina, zeolite, activated carbon or diatomaceous earth.
- the immersion liquid of the step (1) is a concentration of 0. 25 ⁇ 7% of sodium hydroxide, potassium hydroxide, sulfur A solution of ferrous iron, lead chloride, aluminum nitrate, sodium carbonate, copper acetate or cerium nitrate.
- the catalyst carrier When the catalyst carrier is activated alumina, it is impregnated with a cerium nitrate solution having a mass concentration of 0.35%. The catalyst carrier is impregnated with a ferrous sulfate solution having a mass concentration of 0.4%.
- the catalyst carrier When the catalyst carrier is activated carbon, it is impregnated with a potassium hydroxide solution having a mass concentration of 0.5%. When the catalyst carrier is activated carbon, it is impregnated with a sodium hydroxide solution having a mass concentration of 0.5%. The catalyst carrier is impregnated with a copper acetate solution having a mass concentration of 0.2%.
- the catalyst carrier When the catalyst carrier is activated carbon, it is impregnated with a sodium carbonate solution having a mass concentration of 7%.
- the leaching of the lead chloride was carried out with a solution having a mass concentration of 0.55%, and then impregnated with a lead chloride solution having a mass concentration of 0.25%.
- the high-efficiency catalyst of the step (3) is activated by hot air for 4-8 hours, and the adsorbed but not completely oxidized substances, such as elemental phosphorus, phosphine, phosphorus trioxide, hydrogen sulfide, are completely oxidized, and then steam is used. It is activated for 2 ⁇ 4h, then washed with water, then heated to 95 ⁇ 110°C with steam, and finally activated by drying with hot air for 24 ⁇ 48h.
- the catalytic oxidation purification can adopt two fixed bed parallel systems, wherein one fixed bed fails to be transferred to the catalyst regeneration, and the other fixed bed continues to be purified, and the catalyst regeneration time is 1/2 of the catalytic oxidation purification time of the ore heat melting electric furnace exhaust gas. 1/3, the entire system can be guaranteed to run continuously.
- the invention firstly removes typical pollutants existing in the elemental state in the tail gas of the ore heat-melting electric furnace by caustic cleaning of the tail gas of the ore-melting electric furnace, and converts the typical pollutants in the elemental state into a gas state from the elemental state of the aerosol, after the alkali washing
- the reformed gas enters the catalytic oxidation fixed bed after being heated, and the typical impurities in the gaseous state are removed by oxidizing a trace amount of oxygen in the tail gas of the ore-melting electric furnace.
- the typical impurity content in the tail gas of the ore hot-melting electric furnace is Less than 1 mg/m 3 .
- the catalyst used in the invention can greatly improve the purification efficiency of the tail gas of the ore melting electric furnace, the catalyst is easy to be regenerated, the utilization rate is high, the process flow is simple, and the purification cost is low.
- the main factors affecting the purification efficiency are the reaction temperature, the oxygen content in the exhaust gas and the carrier gas velocity.
- the influence rules are as follows:
- the oxidation reaction can be carried out at a lower temperature of 50 to 100 ° C in the presence of a catalyst.
- the increase of the reaction temperature is beneficial to the improvement of the purification efficiency.
- the reaction temperature is higher than 100 ° C and then the temperature is raised, the improvement of the purification efficiency is not obvious;
- the oxygen content in the tail gas of the ore-melting electric furnace is 0. 5 ⁇ 3%, and the purification efficiency increases as the oxygen content increases;
- the carrier gas flow rate is in the range of 300 ⁇ 600m 3 (gas volume) / m 3 (catalyst volume) ⁇ 1 ⁇ , reducing the carrier gas flow rate can improve the purification effect, but the flow rate is reduced to 300m 3 (gas volume) / m 3 ( After the catalyst volume), the purification effect has not been significantly improved.
- the adsorption capacity of the catalyst to P3 ⁇ 4 is 12 to 28%
- the adsorption capacity for elemental phosphorus is 24 to 56%
- the adsorption capacity for hydrogen sulfide is 11 to 25%
- the adsorption capacity for hydrogen fluoride is 10 to 22 %
- the content of typical impurities such as hydrogen sulfide, total phosphorus and hydrogen fluoride in the tail gas of the purified hot-melt electric furnace is less than 1mg/m 3 , which meets the requirements for the production of one-carbon chemical products.
- the invention has the following advantages:
- the purification efficiency is high, and the purified ore-melting electric furnace exhaust gas reaches the requirement of producing a carbon chemical to the raw material gas;
- Figure 1 is a process flow diagram of the present invention.
- the activated alumina was impregnated with a cerium nitrate solution having a mass concentration of 0.25% for 20 hours, aged for another 24 hours, then placed in a muffle furnace at 50 CTC for 6 hours, and finally dried at 11 CTC for 4 hours to obtain a high-efficiency catalyst;
- the volume of oxygen in the exhaust gas obtained is 0.5%, and the exhaust gas is passed from bottom to top at a rate of 500 m 3 (gas volume) / m 3 (catalyst volume) .h, in the containing step ( 1)
- the catalytically oxidized fixed bed of the obtained high-efficiency catalyst is subjected to a purification reaction at a reaction temperature of 80 ° C.
- phosphine is catalytically oxidized, and the oxidized products such as phosphorus pentoxide and phosphorus trioxide are adsorbed on the surface of the catalyst.
- Purified gas After the body is cooled, a carbon chemical raw material gas is obtained.
- the content of typical impurities such as phosphorus, sulfur and fluorine in the exhaust gas after purification is less than 1 mg/m 3 .
- the high-efficiency catalyst after the high-efficiency catalyst fails, it is activated by hot air for 4 hours, so that the adsorbed but not completely oxidized substances, such as elemental phosphorus, phosphine, phosphorus trioxide, hydrogen sulfide, are completely oxidized, then activated by steam for 2h, then washed with water, then It is heated to 110 ° C with steam and finally reconstituted after being activated by hot air drying for 24 hours.
- the adsorbed but not completely oxidized substances such as elemental phosphorus, phosphine, phosphorus trioxide, hydrogen sulfide
- the zeolite is impregnated with a ferrous sulfate solution having a mass concentration of 0.3% for 24 hours, aged for another 24 hours, calcined at 55 CTC for 6 hours, and finally dried at 110 ° C for 4 hours to obtain a high-efficiency catalyst;
- tail gas of the hot-melt electric furnace is washed with an alkali-containing aqueous solution to remove carbon dioxide and some phosphorus, sulfur and fluorine impurities, and the tail gas after alkali washing is preheated to 70 ° C ;
- the volume of oxygen in the exhaust gas obtained is 0.5%, and the exhaust gas is passed from bottom to top at a rate of 500 m 3 (gas volume) / m 3 (catalyst volume) .h, in the containing step ( 1)
- the catalytically oxidized fixed bed of the obtained high-efficiency catalyst is subjected to a purification reaction at a reaction temperature of 70 ° C.
- phosphorus and sulfur impurities are catalytically oxidized, and the oxidized products such as phosphorus pentoxide, phosphorus trioxide, sulfur, etc. are adsorbed.
- the gas is cooled to obtain a carbon chemical raw material gas.
- the content of typical impurities such as phosphorus, sulfur and fluorine in the exhaust gas after purification is less than 1 mg/m 3 .
- the high-efficiency catalyst after the high-efficiency catalyst fails, it is activated by hot air for 6h, so that the adsorbed but not completely oxidized substances, such as elemental phosphorus, phosphine, phosphorus trioxide, hydrogen sulfide, are completely oxidized, then activated by steam for 3h, then washed with water, then It is heated to 100 ° C with steam and finally re-used after being activated by hot air drying for 32 h.
- the adsorbed but not completely oxidized substances such as elemental phosphorus, phosphine, phosphorus trioxide, hydrogen sulfide
- the activated carbon was immersed in a potassium hydroxide solution with a concentration of 0.5% for 18 hours, aged for another 24 hours, calcined at 350 ° C for 12 hours, and finally dried at 110 ° C for 6 hours to obtain a high-efficiency catalyst;
- the oxygen content in the exhaust gas obtained is 0.5%, and the exhaust gas is introduced from the bottom to the bottom at a rate of 600 m 3 (gas volume) / m 3 (catalyst volume) .h, in the containing step ( 1)
- the catalytically oxidized fixed bed of the obtained high-efficiency catalyst is subjected to a purification reaction at a reaction temperature of 100 ° C.
- phosphorus and sulfur impurities are catalytically oxidized, and the oxidized products such as phosphorus pentoxide, phosphorus trioxide, sulfur, etc. are adsorbed on On the surface of the catalyst, after purification, the gas is cooled to obtain a carbon chemical raw material gas.
- the content of typical impurities such as phosphorus, sulfur and fluorine in the exhaust gas after purification is less than 1 mg/m 3 .
- the high-efficiency catalyst fails, it is activated by hot air for 8 hours, so that the adsorbed but not completely oxidized substances, such as elemental phosphorus, phosphine, phosphorus trioxide, hydrogen sulfide, are completely oxidized, then activated by steam for 4h, then washed with water, then It is heated to 110 ° C with steam and finally reconstituted after drying with hot air for 48 h.
- the diatomaceous earth was immersed in an aluminum nitrate solution with a mass concentration of 0.4% for 20 hours, aged for another 18 hours, calcined at 65 CTC for 8 hours, and finally dried at 110 ° C for 2 hours to obtain a high-efficiency catalyst;
- the volume of oxygen in the exhaust gas obtained is 0.5%, and the exhaust gas is passed from bottom to top at a rate of 400 m 3 (gas volume) / m 3 (catalyst volume) .h, in the containing step ( 1)
- the catalytic oxidation of the obtained high-efficiency catalyst is carried out in a fixed bed for purification reaction at a reaction temperature of 50 ° C.
- phosphorus and sulfur impurities are catalytically oxidized, and the oxidized products such as phosphorus pentoxide, phosphorus trioxide, sulfur, etc. are adsorbed in
- the gas is cooled to obtain a carbon chemical raw material gas.
- the content of typical impurities such as phosphorus, sulfur and fluorine in the exhaust gas after purification is less than 1 mg/m 3 .
- the high-efficiency catalyst after the high-efficiency catalyst fails, it is activated by hot air for 5 hours, and the adsorbed but not completely oxidized substances such as elemental phosphorus, phosphine, phosphorus trioxide and hydrogen sulfide are completely oxidized, and then activated by steam for 3.5 hours, and then washed with water. It is then heated to 95 ° C with steam and finally reconstituted with hot air for 40 h.
- the activated carbon was immersed in a sodium carbonate solution with a mass concentration of 7% for 10 h, and then aged for 20 h, calcined at 450 ° C for 10 h, and finally dried at 11 CTC for 8 h to obtain a high-efficiency catalyst;
- the oxygen content in the exhaust gas is 0.8%, and the exhaust gas is passed at a rate of 300 m 3 (gas volume) / m 3 (catalyst volume) ⁇ 1 ⁇ , which is highly efficient in the step (1).
- the catalyst is catalytically oxidized in a fixed bed for purification reaction, the reaction temperature is 100 ° C, and the purified gas is cooled to obtain a carbon chemical raw material gas.
- the content of typical impurities such as phosphorus, sulfur and fluorine in the exhaust gas after purification is less than 1 mg/m 3 .
- the high-efficiency catalyst after the high-efficiency catalyst fails, it is activated by hot air for 5 hours, and the adsorbed but not completely oxidized substances, such as elemental phosphorus, phosphine, phosphorus trioxide and hydrogen sulfide, are completely oxidized, then activated by steam for 3 hours, then washed with water, then It is heated to 100 ° C with steam and finally activated by drying with hot air for 30 h.
- the adsorbed but not completely oxidized substances such as elemental phosphorus, phosphine, phosphorus trioxide and hydrogen sulfide
- Example 6 The activated alumina was immersed for 14 h with a cerium nitrate solution having a mass concentration of 0.35%, aged for another 24 hours, calcined at 350 ° C for llh, and finally dried at 110 ° C for 8 h to obtain a high-efficiency catalyst;
- the oxygen content in the exhaust gas obtained is 3%, and the exhaust gas is introduced at a rate of 400 m 3 (gas volume) / m 3 (catalyst volume), in the high-efficiency catalyst containing the step (1).
- the catalytic oxidation fixed bed is subjected to a purification reaction, the reaction temperature is 90 ° C, and the purified gas is cooled to obtain a carbon chemical raw material gas.
- the content of typical impurities such as phosphorus, sulfur and fluorine in the exhaust gas after purification is less than 1 mg/m 3 .
- the zeolite was impregnated with a ferrous sulfate solution having a mass concentration of 0.4% for 16 hours, aged for another 18 hours, calcined at 65 CTC for 6 hours, and finally dried at 110 ° C for 3 hours to obtain a high-efficiency catalyst;
- the oxygen content in the exhaust gas obtained is 1%, and the exhaust gas is introduced at a rate of 500 m 3 (gas volume) / m 3 (catalyst volume) in the high-efficiency catalyst containing the step (1).
- the catalytic oxidation fixed bed is subjected to a purification reaction, the reaction temperature is 100 ° C, and the purified gas is cooled to obtain a carbon chemical raw material gas.
- the content of typical impurities such as phosphorus, sulfur and fluorine in the exhaust gas after purification is less than 1 mg/m 3 .
- the high-efficiency catalyst after the high-efficiency catalyst fails, it is activated by hot air for 5 hours, and the adsorbed but not completely oxidized substances such as elemental phosphorus, phosphine, phosphorus trioxide and hydrogen sulfide are completely oxidized, then activated by steam for 4 hours, then washed with water, then It is heated to 110 ° C with steam and finally re-used after drying with hot air for 28 h.
- the activated carbon is immersed in a sodium hydroxide solution with a concentration of 0.5% for 22 hours, aged for another 20 hours, calcined at 450 ° C for 10 hours, and finally dried at 110 ° C for 5 hours to obtain a high-efficiency catalyst;
- the volume of oxygen in the exhaust gas obtained is 2%, and the exhaust gas is introduced at a rate of 400 m 3 (gas volume) / m 3 (catalyst volume) in the high-efficiency catalyst containing the step (1).
- the catalytic oxidation fixed bed is subjected to a purification reaction, the reaction temperature is 90 ° C, and the purified gas is cooled to obtain a carbon chemical raw material gas.
- the content of typical impurities such as phosphorus, sulfur and fluorine in the exhaust gas after purification is less than 1 mg/m 3 .
- the high-efficiency catalyst after the high-efficiency catalyst fails, it is activated by hot air for 8 hours to make adsorbed but not completely oxidized substances.
- elemental phosphorus, phosphine, phosphorus trioxide and hydrogen sulfide are completely oxidized, and then activated by steam for 4 hours, then washed with water, then heated to 110 ° C with steam, and finally activated by drying with hot air for 48 hours.
- the activated carbon is immersed in a copper acetate solution with a mass concentration of 0.2% for 21 hours, aged for another 24 hours, calcined at 650 ° C for 12 hours, and finally dried at 110 ° C for 7 hours to obtain a high-efficiency catalyst;
- the oxygen content in the exhaust gas obtained is 1.2%, and the exhaust gas is introduced at a rate of 600 m 3 (gas volume) / m 3 (catalyst volume) ⁇ 1 ⁇ , which is highly efficient in the step (1).
- the catalyst is catalytically oxidized in a fixed bed for purification reaction, the reaction temperature is 100 ° C, and the purified gas is cooled to obtain a carbon chemical raw material gas.
- the content of typical impurities such as phosphorus, sulfur and fluorine in the exhaust gas after purification is less than 1 mg/m 3 .
- the diatomaceous earth was immersed in an aluminum nitrate solution with a mass concentration of 0.55% for 6 hours, then immersed in a lead chloride solution having a mass concentration of 0.25% for 10 hours, aged for another 24 hours, and then calcined at 350 ° C for 12 hours. Finally, drying at 11CTC for 4h to obtain a high-efficiency catalyst;
- the oxygen content in the exhaust gas obtained is 2.5%, and the exhaust gas is introduced at a rate of 600 m 3 (gas volume) / m 3 (catalyst volume) ⁇ 1 ⁇ , which is highly efficient in the step (1).
- the catalyst is catalytically oxidized in a fixed bed for purification reaction, the reaction temperature is 100 ° C, and the purified gas is cooled to obtain a carbon chemical raw material gas.
- the content of typical impurities such as phosphorus, sulfur and fluorine in the exhaust gas after purification is less than 1 mg/m 3 .
- the high-efficiency catalyst after the high-efficiency catalyst fails, it is activated by hot air for 4 hours, so that the adsorbed but not completely oxidized substances, such as elemental phosphorus, phosphine, phosphorus trioxide, hydrogen sulfide, are completely oxidized, then activated by steam for 4h, then washed with water, then It is heated to 95 ° C with steam and finally reconstituted after drying with hot air for 48 h.
- the adsorbed but not completely oxidized substances such as elemental phosphorus, phosphine, phosphorus trioxide, hydrogen sulfide
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CN1175920C (zh) * | 2002-04-26 | 2004-11-17 | 昆明理工大学 | 黄磷尾气固定床催化氧化净化的方法 |
CN100427390C (zh) * | 2006-02-24 | 2008-10-22 | 昆明理工大学 | 一种密闭电石炉炉气净化的方法 |
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US4474739A (en) * | 1983-06-29 | 1984-10-02 | Teledyne Industries, Inc. | Method for removing gaseous pollutants in highly dilute concentrations from air at room temperatures |
CN1175920C (zh) * | 2002-04-26 | 2004-11-17 | 昆明理工大学 | 黄磷尾气固定床催化氧化净化的方法 |
CN100427390C (zh) * | 2006-02-24 | 2008-10-22 | 昆明理工大学 | 一种密闭电石炉炉气净化的方法 |
CN101422737B (zh) * | 2008-11-24 | 2010-12-08 | 昆明理工大学 | 黄磷尾气脱磷专用催化剂tp201的制备方法 |
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