CN111579708A - Activity evaluation device and method for desulfurization catalyst - Google Patents
Activity evaluation device and method for desulfurization catalyst Download PDFInfo
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- CN111579708A CN111579708A CN202010425970.1A CN202010425970A CN111579708A CN 111579708 A CN111579708 A CN 111579708A CN 202010425970 A CN202010425970 A CN 202010425970A CN 111579708 A CN111579708 A CN 111579708A
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- hydrogen sulfide
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- 238000006477 desulfuration reaction Methods 0.000 title claims abstract description 79
- 230000023556 desulfurization Effects 0.000 title claims abstract description 79
- 239000003054 catalyst Substances 0.000 title claims abstract description 63
- 230000000694 effects Effects 0.000 title claims abstract description 43
- 238000011156 evaluation Methods 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000007789 gas Substances 0.000 claims abstract description 290
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical group S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims abstract description 154
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims abstract description 125
- 238000001179 sorption measurement Methods 0.000 claims abstract description 109
- 125000001741 organic sulfur group Chemical group 0.000 claims abstract description 78
- 230000007062 hydrolysis Effects 0.000 claims abstract description 75
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 75
- 238000001514 detection method Methods 0.000 claims abstract description 70
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 58
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 58
- 239000001301 oxygen Substances 0.000 claims abstract description 58
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 239000003463 adsorbent Substances 0.000 claims description 109
- 239000003795 chemical substances by application Substances 0.000 claims description 52
- 230000003301 hydrolyzing effect Effects 0.000 claims description 39
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 32
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 30
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 30
- 239000001257 hydrogen Substances 0.000 claims description 19
- 229910052739 hydrogen Inorganic materials 0.000 claims description 19
- 238000002156 mixing Methods 0.000 claims description 19
- 229920006395 saturated elastomer Polymers 0.000 claims description 19
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 18
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 17
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 15
- 239000001569 carbon dioxide Substances 0.000 claims description 15
- 229910052757 nitrogen Inorganic materials 0.000 claims description 15
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical class O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 150000002431 hydrogen Chemical class 0.000 claims description 8
- 230000001172 regenerating effect Effects 0.000 claims description 8
- JJWKPURADFRFRB-UHFFFAOYSA-N carbonyl sulfide Chemical compound O=C=S JJWKPURADFRFRB-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000006392 deoxygenation reaction Methods 0.000 abstract description 51
- 238000012360 testing method Methods 0.000 abstract description 12
- 230000008929 regeneration Effects 0.000 description 28
- 238000011069 regeneration method Methods 0.000 description 28
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 17
- 239000000919 ceramic Substances 0.000 description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 13
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 12
- 238000002360 preparation method Methods 0.000 description 12
- 239000011734 sodium Substances 0.000 description 11
- 230000000977 initiatory effect Effects 0.000 description 9
- 239000010453 quartz Substances 0.000 description 9
- 239000000243 solution Substances 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- 239000002131 composite material Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 239000010970 precious metal Substances 0.000 description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 5
- 239000002594 sorbent Substances 0.000 description 5
- 230000002195 synergetic effect Effects 0.000 description 5
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000011049 filling Methods 0.000 description 4
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 4
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 229910000420 cerium oxide Inorganic materials 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000000395 magnesium oxide Substances 0.000 description 3
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 3
- 238000012216 screening Methods 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- 239000011593 sulfur Substances 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000003546 flue gas Substances 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 229910052707 ruthenium Inorganic materials 0.000 description 2
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 229910001570 bauxite Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- -1 carbon monoxide Hydrogen Chemical class 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 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
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- 229910000361 cobalt sulfate Inorganic materials 0.000 description 1
- 229940044175 cobalt sulfate Drugs 0.000 description 1
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 description 1
- MULYSYXKGICWJF-UHFFFAOYSA-L cobalt(2+);oxalate Chemical compound [Co+2].[O-]C(=O)C([O-])=O MULYSYXKGICWJF-UHFFFAOYSA-L 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- INILCLIQNYSABH-UHFFFAOYSA-N cobalt;sulfanylidenemolybdenum Chemical compound [Mo].[Co]=S INILCLIQNYSABH-UHFFFAOYSA-N 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 229910000365 copper sulfate Inorganic materials 0.000 description 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 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
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- IRXRGVFLQOSHOH-UHFFFAOYSA-L dipotassium;oxalate Chemical compound [K+].[K+].[O-]C(=O)C([O-])=O IRXRGVFLQOSHOH-UHFFFAOYSA-L 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- VEPSWGHMGZQCIN-UHFFFAOYSA-H ferric oxalate Chemical compound [Fe+3].[Fe+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O VEPSWGHMGZQCIN-UHFFFAOYSA-H 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- 229910000358 iron sulfate Inorganic materials 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 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
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
- 235000011151 potassium sulphates Nutrition 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- ZNCPFRVNHGOPAG-UHFFFAOYSA-L sodium oxalate Chemical compound [Na+].[Na+].[O-]C(=O)C([O-])=O ZNCPFRVNHGOPAG-UHFFFAOYSA-L 0.000 description 1
- 229940039790 sodium oxalate Drugs 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000005987 sulfurization reaction Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/10—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using catalysis
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10K—PURIFYING OR MODIFYING THE CHEMICAL COMPOSITION OF COMBUSTIBLE GASES CONTAINING CARBON MONOXIDE
- C10K1/00—Purifying combustible gases containing carbon monoxide
- C10K1/002—Removal of contaminants
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10K—PURIFYING OR MODIFYING THE CHEMICAL COMPOSITION OF COMBUSTIBLE GASES CONTAINING CARBON MONOXIDE
- C10K1/00—Purifying combustible gases containing carbon monoxide
- C10K1/002—Removal of contaminants
- C10K1/003—Removal of contaminants of acid contaminants, e.g. acid gas removal
- C10K1/004—Sulfur containing contaminants, e.g. hydrogen sulfide
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10K—PURIFYING OR MODIFYING THE CHEMICAL COMPOSITION OF COMBUSTIBLE GASES CONTAINING CARBON MONOXIDE
- C10K1/00—Purifying combustible gases containing carbon monoxide
- C10K1/32—Purifying combustible gases containing carbon monoxide with selectively adsorptive solids, e.g. active carbon
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10K—PURIFYING OR MODIFYING THE CHEMICAL COMPOSITION OF COMBUSTIBLE GASES CONTAINING CARBON MONOXIDE
- C10K1/00—Purifying combustible gases containing carbon monoxide
- C10K1/34—Purifying combustible gases containing carbon monoxide by catalytic conversion of impurities to more readily removable materials
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- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
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Abstract
本发明属于脱硫催化剂活性评价领域，具体涉及一种脱硫催化剂的活性评价装置及方法。本发明提供的脱硫催化剂的活性评价装置，包括供气单元，还包括，反应单元，包括依次连通的脱氧单元、水解单元和吸附单元；检测单元，包括氧气检测单元、有机硫检测单元和硫化氢检测单元，所述氧气检测单元设置于所述脱氧单元和水解单元之间，所述有机硫检测单元设置于所述水解单元和吸附单元之间，所述硫化氢检测单元与所述吸附单元的出气口连接，所述供气单元与所述脱氧单元的进气口连接。本发明提供的脱硫催化剂的活性评价装置，用一次配气即可同时测试几组不同的适用于高炉煤气脱硫系列的催化剂性能，更接近催化剂的真实使用情况。
The invention belongs to the field of activity evaluation of desulfurization catalysts, and particularly relates to an activity evaluation device and method of desulfurization catalysts. The activity evaluation device of the desulfurization catalyst provided by the present invention includes a gas supply unit, and also includes a reaction unit, including a deoxygenation unit, a hydrolysis unit and an adsorption unit connected in sequence; a detection unit, including an oxygen detection unit, an organic sulfur detection unit and a hydrogen sulfide unit Detection unit, the oxygen detection unit is arranged between the deoxygenation unit and the hydrolysis unit, the organic sulfur detection unit is arranged between the hydrolysis unit and the adsorption unit, and the hydrogen sulfide detection unit is connected to the adsorption unit. The air outlet is connected, and the air supply unit is connected with the air inlet of the deoxygenation unit. The device for evaluating the activity of the desulfurization catalyst provided by the invention can simultaneously test the performance of several groups of different catalysts suitable for the desulfurization series of blast furnace gas with one gas distribution, which is closer to the actual use of the catalyst.
Description
技术领域technical field
本发明属于脱硫催化剂活性评价领域，具体涉及一种脱硫催化剂的活性评价装置及方法。The invention belongs to the field of activity evaluation of desulfurization catalysts, and particularly relates to an activity evaluation device and method of desulfurization catalysts.
背景技术Background technique
高炉煤气中含有一氧化碳、氢气、甲烷等可燃性气体，其中含有23-30％左右的一氧化碳、12-16％左右的二氧化碳、0.8-1.9％左右的氢气、0.6-1.8％左右的氧气、0.4-0.8％左右的甲烷、200mg/Nm3左右的COS、50mg/Nm3左右的H2S以及50％左右的氮气。未经脱硫处理的高炉煤气经燃烧使用后会排放出大于200mg/Nm3SO2，直接排放到大气中，将造成酸雨的形成，严重污染环境。随着人们环保意识的增加，对硫的排放限值也日益严格，每个使用高炉煤气的终端都建立起庞大的烟气脱硫装置。如此分散的脱硫装置不但大大浪费有限的钢厂空间，而且烟气脱硫的成本及二次污染也日益突显出来。Blast furnace gas contains carbon monoxide, hydrogen, methane and other combustible gases, including about 23-30% carbon monoxide, about 12-16% carbon dioxide, about 0.8-1.9% hydrogen, about 0.6-1.8% oxygen, 0.4- About 0.8% methane, about 200 mg/Nm 3 COS, about 50 mg/Nm 3 H 2 S, and about 50% nitrogen. The blast furnace gas without desulfurization treatment will emit more than 200mg/Nm 3 SO 2 after combustion, which will be directly discharged into the atmosphere, which will cause the formation of acid rain and seriously pollute the environment. With the increase of people's awareness of environmental protection, the emission limit of sulfur is becoming more and more strict. Every terminal using blast furnace gas has built a huge flue gas desulfurization device. Such scattered desulfurization devices not only greatly waste the limited steel mill space, but also the cost and secondary pollution of flue gas desulfurization are increasingly prominent.
目前针对高炉煤气的脱硫净化技术往往需要使用多种不同的催化剂，如现有技术CN110218590A公开了一种高炉煤气脱硫方法及系统，其中所述高炉煤气脱硫方法涉及用COS水解剂将高炉煤气中的有机硫转化为硫化氢，然后用硫化氢吸附剂吸附高炉煤气中的硫化氢，完成脱硫的过程。其中使用过的吸附剂等还需要用无硫干净的高炉煤气进行周期性的再生。然而在高炉煤气中如何快速筛选出可相互匹配、协同作用的不同种脱硫催化剂仍是一个亟待解决的重要技术难题。At present, the desulfurization and purification technology for blast furnace gas often needs to use a variety of different catalysts. For example, the prior art CN110218590A discloses a blast furnace gas desulfurization method and system, wherein the blast furnace gas desulfurization method involves the use of COS hydrolyzing agent. The organic sulfur is converted into hydrogen sulfide, and then the hydrogen sulfide in the blast furnace gas is adsorbed by a hydrogen sulfide adsorbent to complete the desulfurization process. The used adsorbents also need to be periodically regenerated with sulfur-free clean blast furnace gas. However, how to quickly screen out different desulfurization catalysts that can match each other and act synergistically in blast furnace gas is still an important technical problem to be solved urgently.
发明内容SUMMARY OF THE INVENTION
因此，本发明要解决的技术问题是克服现有高炉煤气脱硫工艺中无法快速筛选出可相互匹配、协同作用的不同种脱硫催化剂的缺陷，进而提供一种脱硫催化剂的活性评价装置及方法。Therefore, the technical problem to be solved by the present invention is to overcome the defect that different desulfurization catalysts that can be matched and act synergistically cannot be quickly screened in the existing blast furnace gas desulfurization process, and further provides an activity evaluation device and method for desulfurization catalysts.
为此，本发明采取的技术方案为，For this reason, the technical solution adopted in the present invention is,
一种脱硫催化剂的活性评价装置，包括供气单元，还包括，A device for evaluating the activity of a desulfurization catalyst, comprising a gas supply unit, and further comprising:
反应单元，包括依次连通的脱氧单元、水解单元和吸附单元；a reaction unit, including a deoxygenation unit, a hydrolysis unit and an adsorption unit that are connected in sequence;
检测单元，包括氧气检测单元、有机硫检测单元和硫化氢检测单元，所述氧气检测单元设置于所述脱氧单元和水解单元之间，所述有机硫检测单元设置于所述水解单元和吸附单元之间，所述硫化氢检测单元与所述吸附单元的出气口连接，所述供气单元与所述脱氧单元的进气口连接。The detection unit includes an oxygen detection unit, an organic sulfur detection unit and a hydrogen sulfide detection unit, the oxygen detection unit is arranged between the deoxygenation unit and the hydrolysis unit, and the organic sulfur detection unit is arranged between the hydrolysis unit and the adsorption unit In between, the hydrogen sulfide detection unit is connected with the air outlet of the adsorption unit, and the air supply unit is connected with the air inlet of the deoxygenation unit.
可选的，所述脱氧单元包括并联设置的第一脱氧装置和第二脱氧装置；Optionally, the deoxygenation unit includes a first deoxygenation device and a second deoxygenation device arranged in parallel;
所述吸附单元包括并联设置的第一吸附装置和第二吸附装置。The adsorption unit includes a first adsorption device and a second adsorption device arranged in parallel.
可选的，所述吸附单元的出气口与所述脱氧单元的进气口连接，所述脱氧单元的出气口与所述吸附单元的进气口连接。Optionally, the air outlet of the adsorption unit is connected to the air inlet of the deoxygenation unit, and the air outlet of the deoxygenation unit is connected to the air inlet of the adsorption unit.
可选的，所述供气单元包括依次连接的进气管路、气体混合装置和饱和水蒸气发生装置，所述饱和水蒸气发生装置的出气口与所述脱氧单元的进气口连接。Optionally, the air supply unit includes an air inlet pipeline, a gas mixing device and a saturated water vapor generating device connected in sequence, and an air outlet of the saturated water vapor generating device is connected to an air inlet of the deoxygenation unit.
可选的，所述进气管路包括一氧化碳进气管路、二氧化碳进气管路、氢气进气管路、甲烷进气管路、COS进气管路、硫化氢进气管路、氧气进气管路和氮气进气管路。Optionally, the intake pipeline includes a carbon monoxide intake pipeline, a carbon dioxide intake pipeline, a hydrogen intake pipeline, a methane intake pipeline, a COS intake pipeline, a hydrogen sulfide intake pipeline, an oxygen intake pipeline, and a nitrogen intake pipeline. .
可选的，还包括尾气处理装置，所述尾气处理装置与所述硫化氢检测单元的出气口连接。Optionally, a tail gas treatment device is also included, and the tail gas treatment device is connected to the gas outlet of the hydrogen sulfide detection unit.
可选的，所述水解单元包括水解装置，所述第一脱氧装置、第二脱氧装置、第一吸附装置、第二吸附装置和水解装置中均包括反应器以及对该反应器进行加热的加热装置。Optionally, the hydrolysis unit includes a hydrolysis device, and the first deoxygenation device, the second deoxygenation device, the first adsorption device, the second adsorption device and the hydrolysis device all include a reactor and a heating device for heating the reactor. device.
本发明还提供一种脱硫催化剂的活性评价方法，包括如下步骤：The present invention also provides a method for evaluating the activity of the desulfurization catalyst, comprising the following steps:
1)将模拟高炉煤气与脱氧剂或再生脱氧剂接触以对模拟高炉煤气进行脱氧，得到脱氧后的模拟高炉煤气，测定脱氧后的模拟高炉煤气的氧含量；1) contacting the simulated blast furnace gas with a deoxidizer or a regenerating deoxidizer to deoxidize the simulated blast furnace gas, obtaining deoxidized simulated blast furnace gas, and measuring the oxygen content of the deoxidized simulated blast furnace gas;
2)将脱氧后的模拟高炉煤气与有机硫水解剂接触以将模拟高炉煤气中的有机硫转化为硫化氢，得到水解后的模拟高炉煤气，测定水解后的模拟高炉煤气中有机硫的含量；2) contacting the deoxidized simulated blast furnace gas with an organic sulfur hydrolyzing agent to convert the organic sulfur in the simulated blast furnace gas into hydrogen sulfide, obtain the simulated blast furnace gas after the hydrolysis, and measure the content of the organic sulfur in the simulated blast furnace gas after the hydrolysis;
3)将水解后的模拟高炉煤气与硫化氢吸附剂或再生硫化氢吸附剂接触以吸附模拟高炉煤气中的硫化氢，得到脱硫后的模拟高炉煤气，测定脱硫后的模拟高炉煤气中的硫化氢含量。3) contacting the hydrolyzed simulated blast furnace gas with a hydrogen sulfide adsorbent or a regenerated hydrogen sulfide adsorbent to adsorb hydrogen sulfide in the simulated blast furnace gas, obtaining a simulated blast furnace gas after desulfurization, and measuring the hydrogen sulfide in the simulated blast furnace gas after desulfurization content.
优选的，步骤3)中将脱硫后的模拟高炉煤气依次与失活的脱氧剂、失活的硫化氢吸附剂接触以对失活的脱氧剂、失活的硫化氢吸附剂进行再生，得到再生处理后的模拟高炉煤气，测定再生处理后的模拟高炉煤气中硫化氢含量。Preferably, in step 3), the simulated blast furnace gas after desulfurization is sequentially contacted with the deactivated deoxidizer and the deactivated hydrogen sulfide adsorbent to regenerate the deactivated deoxidizer and the deactivated hydrogen sulfide adsorbent to obtain regeneration. For the simulated blast furnace gas after treatment, the hydrogen sulfide content in the simulated blast furnace gas after regeneration treatment is determined.
本发明所述模拟高炉煤气与脱氧剂或再生脱氧剂接触时的空速为500-600h-1；脱氧后的模拟高炉煤气与有机硫水解剂接触时的空速为500-700h-1；水解后的模拟高炉煤气与硫化氢吸附剂或再生硫化氢吸附剂接触时的空速为500-600h-1；脱硫后的模拟高炉煤气依次与失活的脱氧剂、失活的硫化氢吸附剂接触时的空速为500-600h-1。The space velocity of the simulated blast furnace gas in the present invention is 500-600h -1 when contacting with the deoxidizer or the regenerating deoxidizer; the space velocity when the simulated blast furnace gas after deoxidation is contacted with the organic sulfur hydrolyzing agent is 500-700h -1 ; The space velocity of the simulated blast furnace gas in contact with the hydrogen sulfide adsorbent or the regenerated hydrogen sulfide adsorbent is 500-600 h -1 ; the simulated blast furnace gas after desulfurization is contacted with the deactivated deoxidizer and the deactivated hydrogen sulfide adsorbent in turn The airspeed at 500-600h -1 .
所述模拟高炉煤气的制备方法包括将一氧化碳、二氧化碳、氢气、甲烷、羰基硫、硫化氢、氧气、氮气混合，然后在与饱和水蒸气混合，得到所述模拟高炉煤气。The preparation method of the simulated blast furnace gas includes mixing carbon monoxide, carbon dioxide, hydrogen, methane, carbonyl sulfide, hydrogen sulfide, oxygen and nitrogen, and then mixing with saturated steam to obtain the simulated blast furnace gas.
本发明技术方案，具有如下优点：The technical scheme of the present invention has the following advantages:
1、本发明提供的脱硫催化剂的活性评价装置，通过供气单元将模拟高炉煤气通过脱氧单元以脱除模拟高炉煤气中的氧气，得到脱氧处理后的模拟高炉煤气，然后将脱氧处理后的模拟高炉煤气通过氧气检测单元检测脱氧处理后的模拟高炉煤气中的氧含量，根据测得的氧含量评价脱氧单元中脱氧剂或再生脱氧剂的脱氧性能，然后在将脱氧处理后的模拟高炉煤气通过水解单元以将模拟高炉煤气中的有机硫(COS)转化为硫化氢，得到水解后的模拟高炉煤气，将水解后的模拟高炉煤气通过有机硫检测单元检测模拟高炉煤气中有机硫的含量，根据测得的有机硫含量评价水解单元中水解剂的水解性能；然后将水解后的模拟高炉煤气通过吸附单元以吸附模拟高炉煤气中的硫化氢，得到脱硫后的模拟高炉煤气，在将脱硫后的模拟高炉煤气通过硫化氢检测单元检测脱硫后的模拟高炉煤气中硫化氢的含量，根据硫化氢的含量评价吸附单元中硫化氢吸附剂或再生硫化氢吸附剂的吸附性能。本发明通过将模拟高炉煤气依次通过脱氧单元、氧气检测单元、水解单元、有机硫检测单元、吸附单元和硫化氢检测单元，可将多组高炉煤气脱硫催化剂有机地串并联起来，用一次配气即可同时测试几组不同的适用于高炉煤气脱硫系列的催化剂性能，大大缩短了催化剂的评价时间，同时还可直接实现对系列脱硫催化剂的协同作用，相互匹配的可靠性进行评价，更接近催化剂的真实使用情况。1. The device for evaluating the activity of the desulfurization catalyst provided by the present invention, passes the simulated blast furnace gas through the deoxidation unit through the gas supply unit to remove the oxygen in the simulated blast furnace gas, obtains the simulated blast furnace gas after deoxidation treatment, and then passes the simulated blast furnace gas after the deoxidation treatment. The blast furnace gas passes through the oxygen detection unit to detect the oxygen content in the deoxidized simulated blast furnace gas, and evaluates the deoxidation performance of the deoxidizer or the regenerated deoxidizer in the deoxidation unit according to the measured oxygen content, and then passes the deoxidized simulated blast furnace gas through the The hydrolysis unit converts the organic sulfur (COS) in the simulated blast furnace gas into hydrogen sulfide, and obtains the simulated blast furnace gas after hydrolysis. The measured organic sulfur content evaluates the hydrolysis performance of the hydrolyzing agent in the hydrolysis unit; then the simulated blast furnace gas after hydrolysis is passed through the adsorption unit to absorb the hydrogen sulfide in the simulated blast furnace gas, and the simulated blast furnace gas after desulfurization is obtained. The content of hydrogen sulfide in the simulated blast furnace gas after desulfurization is detected by the simulated blast furnace gas through the hydrogen sulfide detection unit, and the adsorption performance of the hydrogen sulfide adsorbent or the regenerated hydrogen sulfide adsorbent in the adsorption unit is evaluated according to the hydrogen sulfide content. By passing the simulated blast furnace gas through the deoxidation unit, the oxygen detection unit, the hydrolysis unit, the organic sulfur detection unit, the adsorption unit and the hydrogen sulfide detection unit in sequence, multiple groups of blast furnace gas desulfurization catalysts can be organically connected in series and parallel, and a single gas distribution can be used. The performance of several groups of different catalysts suitable for blast furnace gas desulfurization series can be tested at the same time, which greatly shortens the evaluation time of the catalyst, and at the same time, it can directly realize the synergistic effect of the series of desulfurization catalysts, and evaluate the reliability of mutual matching, which is closer to the catalyst. real usage.
2、本发明提供的脱硫催化剂的活性评价装置，进一步的，所述吸附单元的出气口与所述脱氧单元的进气口连接，所述脱氧单元的出气口与所述吸附单元的进气口连接。本发明通过将吸附单元的出气口与所述脱氧单元的进气口连接，所述脱氧单元的出气口与所述吸附单元的进气口连接，可有效利用脱硫后的模拟高炉煤气对脱氧单元中的失活的脱氧剂以及吸附单元中的失活的硫化氢吸附剂进行再生，然后通过阀门控制模拟高炉煤气的气体流向，将模拟高炉煤气依次通过再生脱氧剂、有机硫水解剂、再生硫化氢吸附剂，从而根据相应检测单元的检测结果评价再生脱氧剂、再生硫化氢吸附剂的再生性能，大大提高了气体的利用率，并有效地缩短催化剂的评价时间。同时通过上述连接设置可实现一次配气即可测试评价脱硫催化剂的初时活性、再生性能及其稳定性能。2. The device for evaluating the activity of the desulfurization catalyst provided by the present invention, further, the air outlet of the adsorption unit is connected to the air inlet of the deoxygenation unit, and the air outlet of the deoxygenation unit is connected to the air inlet of the adsorption unit connect. In the present invention, by connecting the gas outlet of the adsorption unit with the gas inlet of the deoxygenation unit, and the gas outlet of the deoxygenation unit is connected with the gas inlet of the adsorption unit, the simulated blast furnace gas after desulfurization can be effectively used for the deoxygenation unit. The deoxidized deoxidizer and the deactivated hydrogen sulfide adsorbent in the adsorption unit are regenerated, and then the gas flow direction of the simulated blast furnace gas is controlled by the valve, and the simulated blast furnace gas is passed through the regeneration deoxidizer, organic sulfur hydrolysis agent, regeneration sulfurization agent in turn. Therefore, the regeneration performance of the regenerated deoxidizer and the regenerated hydrogen sulfide adsorbent can be evaluated according to the detection results of the corresponding detection unit, which greatly improves the utilization rate of the gas and effectively shortens the evaluation time of the catalyst. At the same time, through the above connection arrangement, it is possible to test and evaluate the initial activity, regeneration performance and stability performance of the desulfurization catalyst with one gas distribution.
附图说明Description of drawings
为了更清楚地说明本发明具体实施方式或现有技术中的技术方案，下面将对具体实施方式或现有技术描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图是本发明的一些实施方式，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。In order to illustrate the specific embodiments of the present invention or the technical solutions in the prior art more clearly, the following briefly introduces the accompanying drawings that need to be used in the description of the specific embodiments or the prior art. Obviously, the accompanying drawings in the following description The drawings are some embodiments of the present invention. For those of ordinary skill in the art, other drawings can also be obtained based on these drawings without creative efforts.
图1为本发明的脱硫催化剂的活性评价装置示意图；Fig. 1 is the schematic diagram of the activity evaluation device of the desulfurization catalyst of the present invention;
图2为本发明实施例2脱硫催化剂的活性评价方法示意图；Fig. 2 is the schematic diagram of the activity evaluation method of the desulfurization catalyst in Example 2 of the present invention;
图3为本发明实施例3脱硫催化剂的活性评价方法示意图；3 is a schematic diagram of the activity evaluation method of the desulfurization catalyst in Example 3 of the present invention;
其中，其中附图标记表示为：Among them, the reference numerals are represented as:
1、第一脱氧装置；2、第二脱氧装置；3、氧气检测装置；4、水解装置；5、有机硫检测装置；6、第一吸附装置；7、第二吸附装置；8、供气单元；9、脱氧单元；1. First deoxygenation device; 2. Second deoxygenation device; 3. Oxygen detection device; 4. Hydrolysis device; 5. Organic sulfur detection device; 6. First adsorption device; 7. Second adsorption device; 8. Gas supply unit; 9. Deoxygenation unit;
10、吸附单元；11、硫化氢检测装置；12、尾气处理装置；13、进气管路；14、质量流量控制器；15、气体混合装置；16、水蒸气发生装置；17、第一阀门；18、第二阀门；19、第三阀门；20、第四阀门；21、第五阀门；22、第六阀门；23、第七阀门。10. Adsorption unit; 11. Hydrogen sulfide detection device; 12. Exhaust gas treatment device; 13. Intake pipeline; 14. Mass flow controller; 15. Gas mixing device; 16. Water vapor generation device; 17. First valve; 18, the second valve; 19, the third valve; 20, the fourth valve; 21, the fifth valve; 22, the sixth valve; 23, the seventh valve.
具体实施方式Detailed ways
下面对本发明的技术方案进行清楚、完整地描述，显然，所描述的实施例是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。The technical solutions of the present invention will be clearly and completely described below. Obviously, the described embodiments are part of the embodiments of the present invention, but not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.
在本发明的描述中，需要说明的是，术语“中心”、“上”、“下”、“左”、“右”、“竖直”、“水平”、“内”、“外”等指示的方位或位置关系为基于附图所示的方位或位置关系，仅是为了便于描述本发明和简化描述，而不是指示或暗示所指的装置或元件必须具有特定的方位、以特定的方位构造和操作，因此不能理解为对本发明的限制。此外，术语“第一”、“第二”、“第三”仅用于描述目的，而不能理解为指示或暗示相对重要性。In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. The indicated orientation or positional relationship is based on the orientation or positional relationship shown in the accompanying drawings, which is only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the indicated device or element must have a specific orientation or a specific orientation. construction and operation, and therefore should not be construed as limiting the invention. Furthermore, the terms "first", "second", and "third" are used for descriptive purposes only and should not be construed to indicate or imply relative importance.
在本发明的描述中，需要说明的是，除非另有明确的规定和限定，术语“安装”、“相连”、“连接”应做广义理解，例如，可以是固定连接，也可以是可拆卸连接，或一体地连接；可以是机械连接，也可以是电连接；可以是直接相连，也可以通过中间媒介间接相连，可以是两个元件内部的连通。对于本领域的普通技术人员而言，可以具体情况理解上述术语在本发明中的具体含义。In the description of the present invention, it should be noted that the terms "installed", "connected" and "connected" should be understood in a broad sense, unless otherwise expressly specified and limited, for example, it may be a fixed connection or a detachable connection Connection, or integral connection; can be mechanical connection, can also be electrical connection; can be directly connected, can also be indirectly connected through an intermediate medium, can be internal communication between two elements. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood in specific situations.
此外，下面所描述的本发明不同实施方式中所涉及的技术特征只要彼此之间未构成冲突就可以相互结合。In addition, the technical features involved in the different embodiments of the present invention described below can be combined with each other as long as they do not conflict with each other.
实施例1Example 1
如图1所示，本发明提供一种脱硫催化剂的活性评价装置，包括供气单元8，还包括，As shown in FIG. 1, the present invention provides an activity evaluation device for a desulfurization catalyst, which includes a
反应单元，包括依次连通的脱氧单元9、水解单元和吸附单元10；The reaction unit includes a
检测单元，包括氧气检测单元、有机硫检测单元和硫化氢检测单元，所述氧气检测单元设置于所述脱氧单元9和水解单元之间，所述有机硫检测单元设置于所述水解单元和吸附单元10之间，所述硫化氢检测单元与所述吸附单元10的出气口连接，所述供气单元8与所述脱氧单元9的进气口连接。The detection unit includes an oxygen detection unit, an organic sulfur detection unit and a hydrogen sulfide detection unit. The oxygen detection unit is arranged between the
本发明通过供气单元8将模拟高炉煤气通过脱氧单元9以脱除模拟高炉煤气中的氧气，得到脱氧处理后的模拟高炉煤气，然后将脱氧处理后的模拟高炉煤气通过氧气检测单元检测脱氧处理后的模拟高炉煤气中的氧含量，根据测得的氧含量评价脱氧单元9中脱氧剂或再生脱氧剂的脱氧性能，然后在将脱氧处理后的模拟高炉煤气通过水解单元以将模拟高炉煤气中的有机硫(COS)转化为硫化氢，得到水解后的模拟高炉煤气，将水解后的模拟高炉煤气通过有机硫检测单元检测模拟高炉煤气中有机硫的含量，根据测得的有机硫含量评价水解单元中水解剂的水解性能；然后将水解后的模拟高炉煤气通过吸附单元10以吸附模拟高炉煤气中的硫化氢，得到脱硫后的模拟高炉煤气，在将脱硫后的模拟高炉煤气通过硫化氢检测单元检测脱硫后的模拟高炉煤气中硫化氢的含量，根据硫化氢的含量评价吸附单元10中硫化氢吸附剂或再生硫化氢吸附剂的吸附性能。本发明通过将模拟高炉煤气依次通过脱氧单元9、氧气检测单元、水解单元、有机硫检测单元、吸附单元10和硫化氢检测单元，可将多组高炉煤气脱硫催化剂有机地串并联起来，用一次配气即可同时测试几组不同的适用于高炉煤气脱硫系列的催化剂性能，同时还可直接实现对系列脱硫催化剂的协同作用，相互匹配的可靠性进行评价，更接近催化剂的真实使用情况。In the present invention, the simulated blast furnace gas is passed through the
在一可选实施例中，所述脱氧单元9包括并联设置的第一脱氧装置1和第二脱氧装置2；所述第一脱氧装置1和第二脱氧装置2的进气口与脱氧单元的进气口连接，出气口与脱氧单元的出气口连接；所述吸附单元10包括并联设置的第一吸附装置6和第二吸附装置7；所述第一吸附装置6和第二吸附装置7的进气口与吸附单元的进气口连接，出气口与吸附单元的出气口连接。所述第一脱氧装置1和第二脱氧装置2中可择一填充脱氧剂或再生脱氧剂或失活的脱氧剂，所述失活的脱氧剂指的是随着脱氧剂对模拟高炉煤气进行催化脱氧，脱氧剂的脱氧活性下降或完全失去脱氧活性，即为失活的脱氧剂；所述再生脱氧剂指的是对失活的脱氧剂进行再生，使之提高失活的脱氧剂的脱氧活性或恢复失活的脱氧剂的脱氧活性，得到的脱氧剂即为再生脱氧剂；所述第一吸附装置6和第二吸附装置7中可择一填充硫化氢吸附剂或再生硫化氢吸附剂或失活的硫化氢吸附剂，所述失活的硫化氢吸附剂指的是随着硫化氢吸附剂对水解后的模拟高炉煤气中的硫化氢进行吸附，硫化氢吸附剂的吸附活性下降或完全失去吸附活性，即为失活的硫化氢吸附剂；所述再生硫化氢吸附剂指的是对失活的硫化氢吸附剂进行再生，使之提高失活的硫化氢吸附剂的吸附活性或恢复失活的硫化氢吸附剂的吸附活性，得到的吸附剂即为再生硫化氢吸附剂；本发明通过在第一脱氧装置1和第二脱氧装置2中择一填充脱氧剂或再生脱氧剂或失活的脱氧剂，以及在第一吸附装置6和第二吸附装置7中可择一填充硫化氢吸附剂或再生硫化氢吸附剂或失活的硫化氢吸附剂，可实现同时评价脱氧剂或再生脱氧剂的脱氧活性，以及硫化氢吸附剂或再生硫化氢吸附剂的吸附活性。In an optional embodiment, the
在一可选实施例中，所述吸附单元10的出气口与所述脱氧单元9的进气口连接，所述脱氧单元9的出气口与所述吸附单元10的进气口连接。本发明通过将吸附单元10的出气口与所述脱氧单元9的进气口连接，所述脱氧单元9的出气口与所述吸附单元10的进气口连接，可有效利用脱硫后的模拟高炉煤气对脱氧单元9中的失活的脱氧剂以及吸附单元10中的失活的硫化氢吸附剂进行再生，然后通过阀门控制模拟高炉煤气的气体流向，将模拟高炉煤气依次通过再生脱氧剂、有机硫水解剂、再生硫化氢吸附剂，从而根据相应检测单元的检测结果评价再生脱氧剂、再生硫化氢吸附剂的再生性能，大大提高了气体的利用率，并有效地缩短催化剂的评价时间。同时通过上述连接设置可实现一次配气即可测试评价脱硫催化剂的初时活性、再生性能及其稳定性能。本发明对脱硫催化剂(包括脱氧剂、有机硫水解剂和硫化氢吸附剂)的初时活性、再生性能评价指标为本领域常规评价指标。本发明所采用的评价指标具体为：氧气检测单元检测脱氧处理后的模拟高炉煤气中的氧含量低于0.2％(体积含量)，说明脱氧剂或再生脱氧剂的脱氧性能良好；有机硫检测单元检测模拟高炉煤气中有机硫的含量小于2mg/m3，说明有机硫水解剂的水解性能良好；硫化氢检测单元检测脱硫后的模拟高炉煤气中硫化氢的含量低于1mg/m3，说明硫化氢吸附剂或再生硫化氢吸附剂的吸附性能良好，或失活的硫化氢吸附剂再生完成。In an optional embodiment, the air outlet of the
在一可选实施例中，所述供气单元8包括依次连接的进气管路13、气体混合装置15和饱和水蒸气发生装置16，所述饱和水蒸气发生装置16的出气口与所述脱氧单元9的进气口连接。本发明通过将高炉煤气含有的各组分气体通过进气管路13通入气体混合装置15中进行混合，混合后再进入饱和水蒸气发生装置16，与饱和水蒸气进行混合，得到模拟高炉煤气。本发明通过依次连接的进气管路13、气体混合装置15和饱和水蒸气发生装置16，从而实现模拟高炉煤气的配制，将其应用于评价高炉煤气脱硫催化剂的活性，使其更接近催化剂的真实使用情况。可选的，所述进气管路13上设置质量流量控制器14用于控制进气管路13中气体的流量。可选的，所述饱和水蒸气发生装置16可控制模拟高炉煤气中的含水量为0-50％(体积含量)，优选为2-30％。可选的，所述进气管路13包括一氧化碳进气管路、二氧化碳进气管路、氢气进气管路、甲烷进气管路、COS进气管路、硫化氢进气管路、氧气进气管路和氮气进气管路。优选的，所述模拟高炉煤气中包括一氧化碳、二氧化碳、氢气、甲烷、羰基硫、硫化氢、氧气、氮气和饱和水蒸气。优选的，所述模拟高炉煤气中包括180-210mg/Nm3的COS，0.6-1.8％(体积含量)的氧气，23-30％(体积含量)的一氧化碳，0.8-1.9％(体积含量)的氢气，12-16％(体积含量)的二氧化碳，0.4-0.8％(体积含量)的甲烷、45-55mg/Nm3的硫化氢、40-60％(体积含量)的氮气、2-30％(体积含量)的饱和水蒸气。In an optional embodiment, the
在一可选实施例中，还包括尾气处理装置12，所述尾气处理装置12与所述硫化氢检测单元的出气口连接。所述尾气处理装置12内可内置碱液用于吸收尾气中的硫化氢，然后再将尾气排放到空气中。In an optional embodiment, an exhaust
在一可选实施例中，所述水解单元包括水解装置4，所述第一脱氧装置1、第二脱氧装置2、第一吸附装置6、第二吸附装置7和水解装置4中均包括反应器以及对该反应器进行加热的加热装置。所述反应器可为U型石英管，所述U型石英管中可内置脱硫催化剂；所述加热装置可为加热炉，用于对所述U型石英管进行加热，可选的，所述加热温度可为50-500℃。In an optional embodiment, the hydrolysis unit includes a
在一可选实施例中，所述第一脱氧装置1还包括第一阀门17，用于使气体通入所述第一脱氧装置1或阻止气体通入所述第一脱氧装置1；所述第二脱氧装置2还包括第二阀门18，用于使气体通入所述第二脱氧装置2或阻止气体通入所述第二脱氧装置2；所述氧气检测单元包括氧气检测装置3，所述氧气检测装置3包括第三阀门19，用于使气体通入所述氧气检测装置3或阻止气体通入所述氧气检测装置3；所述水解单元包括水解装置4，所述水解装置4包括第四阀门20，用于使气体通入所述水解装置4或阻止气体通入所述水解装置4；所述有机硫检测单元包括有机硫检测装置5，所述有机硫检测装置5包括第五阀门21，用于使气体通入所述有机硫检测装置5或阻止气体通入所述有机硫检测装置5；所述第一吸附装置6还包括第六阀门22，用于使气体通入所述第一吸附装置6或阻止气体通入所述第一吸附装置6；所述第二吸附装置7还包括第七阀门23，用于使气体通入所述第二吸附装置7或阻止气体通入所述第二吸附装置7。可选的，所述第一阀门17、第二阀门18、第三阀门19、第四阀门20、第五阀门21、第六阀门22、第七阀门23均可为六通阀门。可选的，所述第三阀门19还与定量环连通设置，所述第五阀门21还与定量环连通设置。In an optional embodiment, the first deoxygenation device 1 further includes a first valve 17 for allowing gas to pass into the first deoxygenation device 1 or preventing gas from passing into the first deoxygenation device 1; the The second deoxygenation device 2 further includes a second valve 18 for allowing gas to pass into the second deoxygenation device 2 or preventing gas from passing into the second deoxygenation device 2; the oxygen detection unit includes the oxygen detection device 3, so The oxygen detection device 3 includes a third valve 19, which is used to make gas pass into the oxygen detection device 3 or prevent gas from entering the oxygen detection device 3; the hydrolysis unit includes a hydrolysis device 4, and the hydrolysis device 4 includes The fourth valve 20 is used to make the gas pass into the hydrolysis device 4 or prevent the gas from passing into the hydrolysis device 4; the organic sulfur detection unit includes an organic sulfur detection device 5, and the organic sulfur detection device 5 includes a fifth The valve 21 is used to make the gas pass into the organic sulfur detection device 5 or prevent the gas from passing into the organic sulfur detection device 5; the first adsorption device 6 also includes a sixth valve 22, which is used to make the gas pass into the The first adsorption device 6 or prevent the gas from passing into the first adsorption device 6; the second adsorption device 7 further includes a seventh valve 23 for allowing the gas to pass into the second adsorption device 7 or preventing the gas from passing through. into the
本发明所述第一脱氧装置1和第二脱氧装置2内的反应器中可内置脱氧剂或再生脱氧剂或失活的脱氧剂或氧气吸附剂；所述水解装置4内的反应器中内置有机硫水解剂，所述第一吸附装置6和第二吸附装置7内的反应器中可内置硫化氢吸附剂或再生硫化氢吸附剂或失活的硫化氢吸附剂。本发明所述脱硫催化剂均为本领域常用脱硫催化剂，不对脱硫催化剂的具体种类做具体限定。可选的，所述脱氧剂选自贵金属脱氧剂、非贵金属钴钼硫型脱氧剂中的至少一种；优选的，所述贵金属脱氧剂为负载型贵金属脱氧剂，所述负载型贵金属脱氧剂中活性成分选自金、铂、钯、钌中的一种或多种，载体为氧化物载体或陶瓷载体。优选的，所述氧化物载体选自氧化铝、氧化硅、氧化镁、氧化钛、氧化锆、氧化铈中的一种或多种。所述的水解剂为负载型水解剂，所述负载型水解剂的活性成分选自氢氧化钠、氢氧化钾、碳酸钠、碳酸钾、草酸钠、草酸钾、硫酸钠、硫酸钾中的一种或多种，载体选自氮化碳、氧化铝、氧化硅、氧化镁、氧化钛、氧化锆、氧化铈中的一种或多种；所述吸附剂为负载型吸附剂，所述负载型吸附剂的活性成分选自氧化铁、氧化钴、氧化镍、氧化铜中的一种或多种，载体选自改性铝土矿、氮化碳、氧化铝、氧化硅、氧化镁、氧化钛、氧化锆、氧化铈中的一种或多种。The reactors in the
在一可选实施例中，本发明通过一氧化碳进气管路、二氧化碳进气管路、氢气进气管路、甲烷进气管路、COS进气管路、硫化氢进气管路、氧气进气管路和氮气进气管路将各组分气体按一定配比通入气体混合装置15中，所述气体混合装置15可为气体混合器，各组分气体的流量可通过进气管路上的质量流量控制器14进行控制，混合后的各组分气体通入饱和水蒸气发生装置16中与饱和水蒸气混合，得到所述模拟高炉煤气。所述饱和水蒸气发生装置16可为饱和水蒸气发生器。所述第一脱氧装置1中的第一阀门17与内置的U型石英管反应器连通，所述第二脱氧装置2中的第二阀门18与内置的U型石英管反应器连通，所述水解装置4中的第四阀门20与内置的U型石英管反应器连通，所述第一吸附装置6中的第六阀门22与内置的U型石英管反应器连通，所述第二吸附装置7中的第七阀门23与内置的U型石英管反应器连通，所述氧气检测装置3中的第三阀门19与氧气检测器连通；所述有机硫检测装置5中的第五阀门21与有机硫检测器连通。在本发明中，模拟高炉煤气通过上述七个阀门控制模拟高炉煤气是否通入相应的装置。In an optional embodiment, the present invention adopts a carbon monoxide intake pipeline, a carbon dioxide intake pipeline, a hydrogen intake pipeline, a methane intake pipeline, a COS intake pipeline, a hydrogen sulfide intake pipeline, an oxygen intake pipeline and a nitrogen intake pipeline. The gas of each component is introduced into the
在一可选实施例中，按脱硫工艺要求，在第一脱氧装置1内放置失活的脱氧剂，第二脱氧装置2内放置脱氧剂，水解装置4内放置有机硫水解剂，第一吸附装置6内放置失活的硫化氢吸附剂，第二吸附装置7内放置硫化氢吸附剂。如图2所示，配置好的模拟高炉煤气依次通过第一至第七阀门23的A、B气口；将第一阀门17、第二阀门18、第四阀门20、第六阀门22、第七阀门23的C、D气口分别与相应装置内U型石英管反应器的进气口、出气口连通；将第七阀门23的A气口与第一阀门17的E气口连通，第一阀门17的F气口与第二阀门18的E气口连通，第二阀门18的F气口与第六阀门22的F气口连通，第六阀门22的E气口与第七阀门23的F气口连通，第七阀门23的E气口与硫化氢检测装置11连通，硫化氢检测装置11与尾气处理装置12连通，第四阀门20的E气口与惰性气体连通，F气口排空，惰性气体可以平衡气的形式通入水解装置4中。第三阀门19的C、D气口与定量环连通，可用来检测氧气含量，第三阀门19的E、F气口与氧气检测器连通；第五阀门21的C、D气口与定量环连通，可用来检测有机硫含量，第五阀门21的E、F气口与有机硫检测器连通。In an optional embodiment, according to the requirements of the desulfurization process, a deactivated deoxidizer is placed in the
在一可选实施例中，配制好的模拟高炉煤气通过第一阀门17和第二阀门18的控制使模拟高炉煤气通入第一脱氧装置1或第二脱氧装置2，第一脱氧装置1或第二脱氧装置2用于脱氧剂的性能测试，其催化反应后的物流为脱氧后的模拟高炉煤气；将脱氧后的模拟高炉煤气通过第四阀门20的控制通入水解装置4，水解装置4用于有基硫水解催化剂的性能测试，其催化反应后的物流为水解后的模拟高炉煤气；水解后的模拟高炉煤气通过第六阀门22和第七阀门23的控制通入第一吸附装置6或第二吸附装置7，第一吸附装置6和第二吸附装置7用于硫化氢吸附剂或再生硫化氢吸附剂的性能测试，其催化反应后的物流为脱硫后的模拟高炉煤气，脱硫后的模拟高炉煤气通过第一阀门17和第二阀门18的控制，再次通入第一脱氧装置1或第二脱氧装置2，用于第一脱氧装置1或第一脱氧装置1内脱氧剂的再生性能评价，其评价后的物流为再生处理后的模拟高炉煤气；再生处理后的模拟高炉煤气通过第六阀门22和第七阀门23的控制，经过第一吸附装置6或第二吸附装置7，第一吸附装置6和第二吸附装置7用于硫化氢吸附剂的再生性能测试。In an optional embodiment, the prepared simulated blast furnace gas is controlled by the
在一可选实施例中，当第一脱氧装置1内的脱氧剂进行脱氧初活性评价时，第二脱氧装置2内的失活的脱氧剂可进行再生，控制第一阀门17使模拟高炉煤气通入第一脱氧装置1内，控制第二阀门18阻止模拟高炉煤气通入第二脱氧装置2；当第一脱氧装置1内的脱氧剂进行再生时，第二脱氧装置2内的脱氧剂可进行脱氧初活性评价测试，控制第一阀门17阻止模拟高炉煤气通入第一脱氧装置1内，控制第二阀门18模拟高炉煤气通入第二脱氧装置2。当水解装置4内的有机硫水解剂进行水解初活性评价时，控制第四阀门20使脱氧后的模拟高炉煤气通入水解装置4。当第一吸附装置6内的硫化氢吸附剂进行吸附初活性评价时，第二吸附装置7内的失活的硫化氢吸附剂可进行再生，控制第六阀门22使模拟高炉煤气通入第一吸附装置6内，控制第七阀门23阻止模拟高炉煤气通入第二吸附装置7；当第一吸附装置6内的硫化氢吸附剂进行再生时，第二吸附装置7内的吸附剂可进行吸附初活性评价测试，控制第六阀门22阻止模拟高炉煤气通入第一吸附装置6内，控制第七阀门23模拟高炉煤气通入第二吸附装置7。In an optional embodiment, when the deoxidizer in the
本发明所述脱氧剂均为本领域现有常规脱氧剂，所述有机硫水解剂均为本领域现有常规水解剂，所述硫化氢吸附剂均为本领域现有常规吸附剂。本领域所述脱氧剂、水解剂、吸附剂可通过市购获得，或通过本领域常规方法制备得到。可选的，所述脱氧剂的制备方法包括如下步骤：将载体置于活性组分水溶液中浸泡，然后依次进行干燥、焙烧，得到所述脱氧剂。当所述载体为复合载体时，将所述载体成分混合球磨，焙烧以制备复合载体。可选的，所述脱氧剂中活性组分与载体的质量比为(2-40)：100。所述脱氧剂的堆积密度为0.5-1.5kg/m3，所述脱氧剂的粒径为0.1-2mm。可选的，所述有机硫水解剂的制备方法包括如下步骤：将载体置于活性组分水溶液中浸泡，然后进行干燥，得到所述水解剂。当所述载体为复合载体时，将所述载体成分混合球磨，焙烧以制备复合载体。可选的，所述水解剂中活性组分与载体的质量比为(2-40)：100。所述水解剂的堆积密度为0.5-0.9kg/m3，所述水解剂的粒径为0.1-5mm。可选的，所述硫化氢吸附剂的制备方法包括如下步骤：将载体置于活性组分浸渍液中浸泡，然后依次进行干燥、焙烧，得到所述吸附剂。当所述载体为复合载体时，将所述载体成分混合球磨，焙烧以制备复合载体。可选的，所述活性组分浸渍液选自硝酸铁、硝酸钴、硝酸镍、硫酸铁、硫酸钴、硫酸镍、氯化铁、氯化钴、氯化镍、草酸铁、草酸钴、草酸镍、硝酸铜、醋酸铜、氯化铜、硫酸铜中的一种或多种水溶液。所述吸附剂中活性组分与载体的质量比为(2-40)：100。所述吸附剂的堆积密度为0.5-1.5kg/m3，所述吸附剂的粒径为0.1-5mm。The deoxidizers in the present invention are all conventional deoxidizers in the art, the organic sulfur hydrolyzing agents are all conventional hydrolyzing agents in the art, and the hydrogen sulfide adsorbents are all conventional adsorbents in the art. The deoxidizers, hydrolyzing agents and adsorbents described in the art can be obtained commercially or prepared by conventional methods in the art. Optionally, the preparation method of the deoxidizer includes the following steps: soaking the carrier in an aqueous solution of active components, and then drying and calcining in sequence to obtain the deoxidizer. When the carrier is a composite carrier, the carrier components are mixed and ball-milled and calcined to prepare a composite carrier. Optionally, the mass ratio of the active component to the carrier in the deoxidizer is (2-40):100. The bulk density of the deoxidizer is 0.5-1.5 kg/m 3 , and the particle size of the deoxidizer is 0.1-2 mm. Optionally, the preparation method of the organic sulfur hydrolyzing agent includes the following steps: soaking the carrier in an aqueous solution of active components, and then drying to obtain the hydrolyzing agent. When the carrier is a composite carrier, the carrier components are mixed and ball-milled and calcined to prepare a composite carrier. Optionally, the mass ratio of the active component to the carrier in the hydrolyzing agent is (2-40):100. The bulk density of the hydrolyzing agent is 0.5-0.9 kg/m 3 , and the particle size of the hydrolyzing agent is 0.1-5 mm. Optionally, the preparation method of the hydrogen sulfide adsorbent includes the following steps: soaking the carrier in an active component dipping solution, and then drying and calcining in sequence to obtain the adsorbent. When the carrier is a composite carrier, the carrier components are mixed and ball-milled and calcined to prepare a composite carrier. Optionally, the active component impregnation solution is selected from iron nitrate, cobalt nitrate, nickel nitrate, iron sulfate, cobalt sulfate, nickel sulfate, iron chloride, cobalt chloride, nickel chloride, iron oxalate, cobalt oxalate, oxalic acid One or more aqueous solutions of nickel, copper nitrate, copper acetate, copper chloride, and copper sulfate. The mass ratio of the active component to the carrier in the adsorbent is (2-40):100. The bulk density of the adsorbent is 0.5-1.5 kg/m 3 , and the particle size of the adsorbent is 0.1-5 mm.
本发明以下实施例2-4中所用脱氧剂、有机硫水解剂和硫化氢吸附剂均是按照如下方法制备得到。The deoxidizer, organic sulfur hydrolyzing agent and hydrogen sulfide adsorbent used in the following Examples 2-4 of the present invention are all prepared according to the following methods.
所述陶瓷载体负载钌金属脱氧剂的制备方法包括如下步骤：配制质量分数为5％的氯化钌水溶液，将陶瓷载体置于氯化钌水溶液中浸泡1小时，然后在100℃下干燥2小时，在450℃下焙烧10分钟，得到所述陶瓷载体负载钌金属脱氧剂，所述陶瓷载体负载钌金属脱氧剂中金属钌与陶瓷载体的质量比为9：50；所述陶瓷载体负载钌金属脱氧剂的堆积密度为0.8kg/m3，粒径为0.3-0.5mm。The preparation method of the ceramic carrier-supported ruthenium metal deoxidizer includes the following steps: preparing an aqueous ruthenium chloride solution with a mass fraction of 5%, immersing the ceramic carrier in the ruthenium chloride aqueous solution for 1 hour, and then drying at 100° C. for 2 hours , roasting at 450°C for 10 minutes to obtain the ceramic carrier-supported ruthenium metal deoxidizer, wherein the mass ratio of metal ruthenium to the ceramic carrier in the ceramic carrier-supported ruthenium metal deoxidizer is 9:50; the ceramic carrier supports ruthenium metal The bulk density of the deoxidizer is 0.8 kg/m 3 and the particle size is 0.3-0.5 mm.
所述Na2CO3/Al2O3的制备方法包括如下步骤：配制质量分数为10％的Na2CO3水溶液，将氧化铝载体置于Na2CO3水溶液中浸泡3小时，然后在90℃下干燥0.8小时，得到所述Na2CO3/Al2O3水解剂，所述Na2CO3/Al2O3水解剂中Na2CO3与氧化铝载体的质量比为6：58；所述Na2CO3/Al2O3水解剂的堆积密度为0.6kg/m3，粒径为2-3mm。The preparation method of the Na 2 CO 3 /Al 2 O 3 includes the following steps: preparing a Na 2 CO 3 aqueous solution with a mass fraction of 10%, placing the alumina carrier in the Na 2 CO 3 aqueous solution for 3 hours, and then immersing the alumina carrier in the Na 2
所述Fe2O3/Al2O3-C3N4吸附剂中，活性组分为Fe2O3，载体为氮化碳和氧化铝的混合载体，所述Fe2O3/Al2O3-C3N4吸附剂的制备方法包括如下步骤：In the Fe 2 O 3 /Al 2 O 3 -C 3 N 4 adsorbent, the active component is Fe 2 O 3 , the carrier is a mixed carrier of carbon nitride and alumina, and the Fe 2 O 3 /Al 2 The preparation method of O 3 -C 3 N 4 adsorbent comprises the following steps:
1)载体制备：将氮化碳粉末和氧化铝粉末等质量混合，球磨15小时，然后在900℃下焙烧5小时，制得载体，备用；1) Carrier preparation: Mix carbon nitride powder and alumina powder with equal quality, ball mill for 15 hours, and then roast at 900° C. for 5 hours to prepare a carrier for use;
2)配制质量分数为8％的硝酸铁水溶液，将载体置于硝酸铁水溶液中浸泡3小时，然后在100℃下干燥1.2小时，在800℃下焙烧30分钟，得到所述Fe2O3/Al2O3-C3N4吸附剂，所述Fe2O3/Al2O3-C3N4吸附剂中Fe2O3与载体的质量比为1：7，所述Fe2O3/Al2O3-C3N4吸附剂的堆积密度为0.9kg/m3，粒径为1-2mm。2) Prepare an aqueous ferric nitrate solution with a mass fraction of 8%, soak the carrier in an aqueous ferric nitrate solution for 3 hours, then dry at 100° C. for 1.2 hours, and bake at 800° C. for 30 minutes to obtain the Fe 2 O 3 / Al 2 O 3 -C 3 N 4 adsorbent, the mass ratio of Fe 2 O 3 to carrier in the Fe 2 O 3 /Al 2 O 3 -C 3 N 4 adsorbent is 1:7, the Fe 2 O The bulk density of the 3 /Al 2 O 3 -C 3 N 4 adsorbent is 0.9 kg/m 3 and the particle size is 1-2 mm.
实施例2Example 2
如图2所示，本实施例提供了脱硫催化剂的活性评价方法，包括如下步骤：As shown in Figure 2, this embodiment provides a method for evaluating the activity of a desulfurization catalyst, including the following steps:
1)装填催化剂：在第一脱氧装置1内填充失活的脱氧剂(所述失活的脱氧剂为失活的蜂窝状陶瓷载体负载钌金属脱氧剂)，第二脱氧装置2内填充脱氧剂(所述脱氧剂为蜂窝状陶瓷载体负载钌金属脱氧剂)，水解装置4内填充有机硫水解剂(有机硫水解剂为Na2CO3/Al2O3水解剂)，第一吸附装置6内填充失活的硫化氢吸附剂(所述失活的硫化氢吸附剂为失活的Fe2O3/Al2O3-C3N4吸附剂)，第二吸附装置7内填充硫化氢吸附剂(所述硫化氢吸附剂为Fe2O3/Al2O3-C3N4吸附剂)；1) Filling the catalyst: filling the
2)制备模拟高炉煤气：通过一氧化碳进气管路、二氧化碳进气管路、氢气进气管路、甲烷进气管路、COS进气管路、硫化氢进气管路、氧气进气管路和氮气进气管路将相应的各组气体通入气体混合器中进行混合(通过进气管路上设置的质量流量控制器14控制相应气体的流量)，混合后通入饱和水蒸气发生器中与饱和水蒸气进行再次混合，得到模拟高炉煤气(所述高炉煤气中含有200mg/Nm3的COS，1.0％(体积含量)的氧气，28％(体积含量)的一氧化碳，1.2％(体积含量)的氢气，15％(体积含量)的二氧化碳，0.6％(体积含量)的甲烷、50mg/Nm3的硫化氢、40％(体积含量)的氮气、其余为饱和水蒸气)；2) Preparation of simulated blast furnace gas: through the carbon monoxide intake pipeline, carbon dioxide intake pipeline, hydrogen intake pipeline, methane intake pipeline, COS intake pipeline, hydrogen sulfide intake pipeline, oxygen intake pipeline and nitrogen intake pipeline will be corresponding Each group of gases is passed into the gas mixer for mixing (the flow rate of the corresponding gas is controlled by the
3)将模拟高炉煤气(所述模拟高炉煤气的温度为70℃)以500h-1的体积空速通入第二脱氧装置2内与脱氧剂接触以对模拟高炉煤气进行脱氧，得到脱氧后的模拟高炉煤气，脱氧后的模拟高炉煤气可通过氧气检测装置3检测其中的氧含量，并根据氧含量评价脱氧剂的脱氧性能；脱氧后的模拟高炉煤气以500h-1的体积空速通入水解装置4与有机硫水解剂接触以将模拟高炉煤气中的有机硫转化为硫化氢，得到水解后的模拟高炉煤气，水解后的模拟高炉煤气可通过有机硫检测装置5检测其中的有机硫(COS)含量，并根据有机硫的含量计算有机硫的转化率，根据有机硫转化率评价有机硫水解剂对有机硫的水解性能；将水解后的模拟高炉煤气以500h-1的体积空速通入第二吸附装置7，与第二吸附装置7内的硫化氢吸附剂接触以吸附模拟高炉煤气中的硫化氢，得到脱硫后的模拟高炉煤气；3) The simulated blast furnace gas (the temperature of the simulated blast furnace gas is 70° C.) is passed into the second deoxidizer 2 at a volume space velocity of 500 h −1 to be contacted with the deoxidizer to deoxidize the simulated blast furnace gas, and the deoxidized gas is obtained. Simulate blast furnace gas, the oxygen content of the deoxidized simulated blast furnace gas can be detected by the
4)将脱硫后的模拟高炉煤气以500h-1的体积空速通入第一脱氧装置1内与失活的脱氧剂接触，利用脱硫后的模拟高炉煤气中的还原性气氛对失活的脱氧剂进行再生，然后再以500h-1的体积空速通入第一吸附装置6内与失活的硫化氢吸附剂接触，利用脱硫后的模拟高炉煤气中的还原性气氛对失活的硫化氢吸附剂进行再生，得到再生处理后的模拟高炉煤气，再生处理后的模拟高炉煤气可通过硫化氢检测装置11检测其中的硫化氢含量，并根据硫化氢含量评价硫化氢吸附剂的再生情况，经过硫化氢检测装置11检测后的模拟高炉煤气可通过尾气处理装置12对模拟高炉煤气进行尾气吸收处理，尾气吸收处理后排空。经测试，通过本实施例中的方法完成对脱氧剂、有机硫水解剂、硫化氢吸附剂的初始活性及再生性能评价测试相比于每次配气单独对脱氧剂、有机硫水解剂、硫化氢吸附剂的初始活性及再生性能进行评价，其时间缩短了4-5倍，可见，本实施例中的方法实现了快速筛选可相互匹配、具有协同作用的不同种脱硫催化剂的目的。4) Passing the desulfurized simulated blast furnace gas into the first deoxidizer 1 at a volume space velocity of 500 h -1 to contact with the deactivated deoxidizer, and using the reducing atmosphere in the desulfurized simulated blast furnace gas to deoxidize the deactivated The sorbent is regenerated, and then passed into the
实施例3Example 3
如图3所示，本实施例提供了脱硫催化剂的活性评价方法，包括如下步骤：As shown in Figure 3, this embodiment provides a method for evaluating the activity of a desulfurization catalyst, including the following steps:
1)装填催化剂：在第一脱氧装置1内填充脱氧剂(所述脱氧剂为蜂窝状陶瓷载体负载钌金属脱氧剂)，第二脱氧装置2内填充失活的脱氧剂(所述失活的脱氧剂为失活的蜂窝状陶瓷载体负载钌金属脱氧剂)，水解装置4内填充有机硫水解剂(有机硫水解剂为Na2CO3/Al2O3水解剂)，第一吸附装置6内填充硫化氢吸附剂(所述硫化氢吸附剂为Fe2O3/Al2O3-C3N4吸附剂)，第二吸附装置7内填充失活的硫化氢吸附剂(所述失活的硫化氢吸附剂为失活的Fe2O3/Al2O3-C3N4吸附剂)；1) Filling the catalyst: fill the
2)制备模拟高炉煤气：通过一氧化碳进气管路、二氧化碳进气管路、氢气进气管路、甲烷进气管路、COS进气管路、硫化氢进气管路、氧气进气管路和氮气进气管路将相应的各组气体通入气体混合器中进行混合(通过进气管路上设置的质量流量控制器14控制相应气体的流量)，混合后通入饱和水蒸气发生器中与饱和水蒸气进行再次混合，得到模拟高炉煤气(所述高炉煤气中含有200mg/Nm3的COS，1.0％(体积含量)的氧气，28％(体积含量)的一氧化碳，1.2％(体积含量)的氢气，15％(体积含量)的二氧化碳，0.6％(体积含量)的甲烷、50mg/Nm3的硫化氢、40％(体积含量)的氮气、其余为饱和水蒸气)；2) Preparation of simulated blast furnace gas: through the carbon monoxide intake pipeline, carbon dioxide intake pipeline, hydrogen intake pipeline, methane intake pipeline, COS intake pipeline, hydrogen sulfide intake pipeline, oxygen intake pipeline and nitrogen intake pipeline will be corresponding Each group of gases is passed into the gas mixer for mixing (the flow rate of the corresponding gas is controlled by the
3)将模拟高炉煤气(所述模拟高炉煤气的温度为90℃)以500h-1的体积空速通入第一脱氧装置1内与脱氧剂接触以对模拟高炉煤气进行脱氧，得到脱氧后的模拟高炉煤气，脱氧后的模拟高炉煤气可通过氧气检测装置3检测其中的氧含量，并根据氧含量评价脱氧剂的脱氧性能；脱氧后的模拟高炉煤气以500h-1的体积空速通入水解装置4与有机硫水解剂接触以将模拟高炉煤气中的有机硫转化为硫化氢，得到水解后的模拟高炉煤气，水解后的模拟高炉煤气可通过有机硫检测装置5检测其中的有机硫(COS)含量，并根据有机硫的含量计算有机硫的转化率，根据有机硫转化率评价有机硫水解剂对有机硫的水解性能；将水解后的模拟高炉煤气以500h-1的体积空速通入第一吸附装置6与第一吸附装置6内的硫化氢吸附剂接触以吸附模拟高炉煤气中的硫化氢，得到脱硫后的模拟高炉煤气；3) The simulated blast furnace gas (the temperature of the simulated blast furnace gas is 90° C.) is passed into the first deoxidizer 1 at a volumetric space velocity of 500 h −1 to contact with a deoxidizer to deoxidize the simulated blast furnace gas, and the deoxidized gas is obtained. Simulate blast furnace gas, the oxygen content of the deoxidized simulated blast furnace gas can be detected by the
4)将脱硫后的模拟高炉煤气以500h-1的体积空速通入第二脱氧装置2内与失活的脱氧剂接触，利用脱硫后的模拟高炉煤气中的还原性气氛对失活的脱氧剂进行再生，然后再以500h-1的体积空速通入第二吸附装置7内与失活的硫化氢吸附剂接触，利用脱硫后的模拟高炉煤气中的还原性气氛对失活的硫化氢吸附剂进行再生，得到再生处理后的模拟高炉煤气，再生处理后的模拟高炉煤气可通过硫化氢检测装置11检测其中的硫化氢含量，并根据硫化氢含量评价硫化氢吸附剂的再生情况，经过硫化氢检测装置11检测后的模拟高炉煤气可通过尾气处理装置12对模拟高炉煤气进行尾气吸收处理，尾气吸收处理后排空。经测试，通过本实施例中的方法完成对脱氧剂、有机硫水解剂、硫化氢吸附剂的初始活性及再生性能评价测试相比于每次配气单独对脱氧剂、有机硫水解剂、硫化氢吸附剂的初始活性及再生性能进行评价，其时间缩短了4-5倍，可见，本实施例中的方法实现了快速筛选可相互匹配、具有协同作用的不同种脱硫催化剂的目的。4) Pass the desulfurized simulated blast furnace gas into the second deoxidizer 2 at a volume space velocity of 500 h −1 to contact the deactivated deoxidizer, and utilize the reducing atmosphere in the desulfurized simulated blast furnace gas to deoxidize the deactivated deoxidized gas. The sorbent is regenerated, and then passed into the
实施例4Example 4
本实施例提供了脱硫催化剂的活性评价方法，包括如下步骤：The present embodiment provides an activity evaluation method for a desulfurization catalyst, comprising the following steps:
1)装填催化剂：在第一脱氧装置1内填充脱氧剂(所述脱氧剂为蜂窝状陶瓷载体负载钌金属脱氧剂)，第二脱氧装置2内填充失活的脱氧剂(所述失活的脱氧剂为失活的蜂窝状陶瓷载体负载钌金属脱氧剂)，水解装置4内填充有机硫水解剂(有机硫水解剂为Na2CO3/Al2O3水解剂)，第一吸附装置6内填充硫化氢吸附剂(所述硫化氢吸附剂为Fe2O3/Al2O3-C3N4吸附剂)，第二吸附装置7内填充失活的硫化氢吸附剂(所述失活的硫化氢吸附剂为失活的Fe2O3/Al2O3-C3N4吸附剂)；1) Filling the catalyst: fill the
2)制备模拟高炉煤气：通过一氧化碳进气管路、二氧化碳进气管路、氢气进气管路、甲烷进气管路、COS进气管路、硫化氢进气管路、氧气进气管路和氮气进气管路将相应的各组气体通入气体混合器中进行混合(通过进气管路上设置的质量流量控制器14控制相应气体的流量)，混合后通入饱和水蒸气发生器中与饱和水蒸气进行再次混合，得到模拟高炉煤气(所述高炉煤气中含有210mg/Nm3的COS，1.0％(体积含量)的氧气，30％(体积含量)的一氧化碳，1.4％(体积含量)的氢气，18％(体积含量)的二氧化碳，0.7％(体积含量)的甲烷、53mg/Nm3的硫化氢、43％(体积含量)的氮气、其余为饱和水蒸气)；2) Preparation of simulated blast furnace gas: through the carbon monoxide intake pipeline, carbon dioxide intake pipeline, hydrogen intake pipeline, methane intake pipeline, COS intake pipeline, hydrogen sulfide intake pipeline, oxygen intake pipeline and nitrogen intake pipeline will be corresponding Each group of gases is passed into the gas mixer for mixing (the flow rate of the corresponding gas is controlled by the
3)将模拟高炉煤气(所述模拟高炉煤气的温度为90℃)以700h-1的体积空速通入第一脱氧装置1内与脱氧剂接触以对模拟高炉煤气进行脱氧，得到脱氧后的模拟高炉煤气，脱氧后的模拟高炉煤气可通过氧气检测装置3检测其中的氧含量，并根据氧含量评价脱氧剂的脱氧性能；脱氧后的模拟高炉煤气以600h-1的体积空速通入水解装置4与有机硫水解剂接触以将模拟高炉煤气中的有机硫转化为硫化氢，得到水解后的模拟高炉煤气，水解后的模拟高炉煤气可通过有机硫检测装置5检测其中的有机硫(COS)含量，并根据有机硫的含量计算有机硫的转化率，根据有机硫转化率评价有机硫水解剂对有机硫的水解性能；将水解后的模拟高炉煤气以600h-1的体积空速通入第一吸附装置6与第一吸附装置6内的硫化氢吸附剂接触以吸附模拟高炉煤气中的硫化氢，得到脱硫后的模拟高炉煤气；脱硫后的模拟高炉煤气可通过硫化氢检测装置11检测其中的硫化氢含量，并根据硫化氢含量评价硫化氢吸附剂的吸附性能，经过硫化氢检测装置11检测后的模拟高炉煤气可通过尾气处理装置12对模拟高炉煤气进行尾气吸收处理，尾气吸收处理后排空。经测试，通过本实施例中的方法完成对脱氧剂、有机硫水解剂、硫化氢吸附剂的初始活性评价测试相比于每次配气单独对脱氧剂、有机硫水解剂、硫化氢吸附剂的初始活性进行评价，其时间缩短了4-5倍，可见，本实施例中的方法实现了快速筛选可相互匹配、具有协同作用的不同种脱硫催化剂的目的。3) The simulated blast furnace gas (the temperature of the simulated blast furnace gas is 90° C.) is passed into the first deoxidizer 1 at a volumetric space velocity of 700 h −1 to be contacted with a deoxidizer to deoxidize the simulated blast furnace gas, and the deoxidized gas is obtained. Simulated blast furnace gas, the oxygen content of the deoxidized simulated blast furnace gas can be detected by the
显然，上述实施例仅仅是为清楚地说明所作的举例，而并非对实施方式的限定。对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。而由此所引伸出的显而易见的变化或变动仍处于本发明创造的保护范围之中。Obviously, the above-mentioned embodiments are only examples for clear description, and are not intended to limit the implementation manner. For those of ordinary skill in the art, changes or modifications in other different forms can also be made on the basis of the above description. There is no need and cannot be exhaustive of all implementations here. And the obvious changes or changes derived from this are still within the protection scope of the present invention.
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