CN101970614A - 从烃料流中脱除汞的方法 - Google Patents
从烃料流中脱除汞的方法 Download PDFInfo
- Publication number
- CN101970614A CN101970614A CN2009801084389A CN200980108438A CN101970614A CN 101970614 A CN101970614 A CN 101970614A CN 2009801084389 A CN2009801084389 A CN 2009801084389A CN 200980108438 A CN200980108438 A CN 200980108438A CN 101970614 A CN101970614 A CN 101970614A
- Authority
- CN
- China
- Prior art keywords
- mercury
- weight
- absorption agent
- oxide
- hydrocarbon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 229910052753 mercury Inorganic materials 0.000 title claims abstract description 57
- 239000004215 Carbon black (E152) Substances 0.000 title claims abstract description 46
- 229930195733 hydrocarbon Natural products 0.000 title claims abstract description 46
- 150000002430 hydrocarbons Chemical class 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 37
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 20
- 239000001257 hydrogen Substances 0.000 claims abstract description 20
- 229910052802 copper Inorganic materials 0.000 claims abstract description 15
- 239000010949 copper Substances 0.000 claims abstract description 15
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims description 31
- 238000010521 absorption reaction Methods 0.000 claims description 30
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 17
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 13
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 10
- 239000011787 zinc oxide Substances 0.000 claims description 8
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 claims description 7
- 235000012239 silicon dioxide Nutrition 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- 229960001866 silicon dioxide Drugs 0.000 claims description 7
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 6
- 239000012876 carrier material Substances 0.000 claims description 6
- 229960004643 cupric oxide Drugs 0.000 claims description 6
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 6
- -1 hydrogen hydrocarbon Chemical class 0.000 claims description 5
- 239000000395 magnesium oxide Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 4
- 239000000725 suspension Substances 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 17
- 239000002250 absorbent Substances 0.000 abstract description 4
- 230000002745 absorbent Effects 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 description 18
- 239000000243 solution Substances 0.000 description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 11
- 229910052751 metal Inorganic materials 0.000 description 9
- 239000002184 metal Substances 0.000 description 9
- 150000001875 compounds Chemical class 0.000 description 7
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 5
- 238000005984 hydrogenation reaction Methods 0.000 description 5
- 229910052709 silver Inorganic materials 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052785 arsenic Inorganic materials 0.000 description 3
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 3
- 239000004927 clay Substances 0.000 description 3
- 229910052570 clay Inorganic materials 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 239000003915 liquefied petroleum gas Substances 0.000 description 3
- 239000003345 natural gas Substances 0.000 description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- 229910000497 Amalgam Inorganic materials 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 125000001931 aliphatic group Chemical group 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- BWFPGXWASODCHM-UHFFFAOYSA-N copper monosulfide Chemical compound [Cu]=S BWFPGXWASODCHM-UHFFFAOYSA-N 0.000 description 2
- HWMTUNCVVYPZHZ-UHFFFAOYSA-N diphenylmercury Chemical compound C=1C=CC=CC=1[Hg]C1=CC=CC=C1 HWMTUNCVVYPZHZ-UHFFFAOYSA-N 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 229910052763 palladium Inorganic materials 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 230000002829 reductive effect Effects 0.000 description 2
- 239000002594 sorbent Chemical group 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 239000005749 Copper compound Substances 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 229910052946 acanthite Inorganic materials 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 229910001854 alkali hydroxide Inorganic materials 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 238000005267 amalgamation Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 229960000892 attapulgite Drugs 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 150000001880 copper compounds Chemical class 0.000 description 1
- OMZSGWSJDCOLKM-UHFFFAOYSA-N copper(II) sulfide Chemical compound [S-2].[Cu+2] OMZSGWSJDCOLKM-UHFFFAOYSA-N 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 229940100892 mercury compound Drugs 0.000 description 1
- 150000002731 mercury compounds Chemical class 0.000 description 1
- BRMYZIKAHFEUFJ-UHFFFAOYSA-L mercury diacetate Chemical compound CC(=O)O[Hg]OC(C)=O BRMYZIKAHFEUFJ-UHFFFAOYSA-L 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical group [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
- 229910052625 palygorskite Inorganic materials 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- XEBWQGVWTUSTLN-UHFFFAOYSA-M phenylmercury acetate Chemical compound CC(=O)O[Hg]C1=CC=CC=C1 XEBWQGVWTUSTLN-UHFFFAOYSA-M 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 239000010970 precious metal 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
- 239000002994 raw material Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000010944 silver (metal) Substances 0.000 description 1
- XUARKZBEFFVFRG-UHFFFAOYSA-N silver sulfide Chemical compound [S-2].[Ag+].[Ag+] XUARKZBEFFVFRG-UHFFFAOYSA-N 0.000 description 1
- 229940056910 silver sulfide Drugs 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G25/00—Refining of hydrocarbon oils in the absence of hydrogen, with solid sorbents
- C10G25/003—Specific sorbent material, not covered by C10G25/02 or C10G25/03
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/11—Purification; Separation; Use of additives by absorption, i.e. purification or separation of gaseous hydrocarbons with the aid of liquids
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- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
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- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0233—Compounds of Cu, Ag, Au
- B01J20/0237—Compounds of Cu
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- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/041—Oxides or hydroxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
- B01J20/3202—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the carrier, support or substrate used for impregnation or coating
- B01J20/3204—Inorganic carriers, supports or substrates
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J20/30—Processes for preparing, regenerating, or reactivating
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- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
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- B01J20/3236—Inorganic material layers containing metal, other than zeolites, e.g. oxides, hydroxides, sulphides or salts
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- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/345—Regenerating or reactivating using a particular desorbing compound or mixture
- B01J20/3458—Regenerating or reactivating using a particular desorbing compound or mixture in the gas phase
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- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/3483—Regenerating or reactivating by thermal treatment not covered by groups B01J20/3441 - B01J20/3475, e.g. by heating or cooling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/86—Chromium
- B01J23/868—Chromium copper and chromium
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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Abstract
本发明涉及一种从含汞烃料流中脱除汞的方法，其中将烃料流与位于载体材料上的含铜吸收剂接触。本发明方法的特征在于在氢气存在下将烃料流与吸收剂接触。
Description
本发明涉及一种从含汞烃料流中脱除汞和/或砷的方法。
汞作为杂质存在于化学工业或石油化学工业中获得或加工的众多物料流中。这些通常是在化石原料如石油、天然气或煤的加工或热利用中以及在废料利用中获得的料流，因为这些原料或废料包含元素形式或化学结合形式的痕量汞。含有作为杂质的汞的料流也在将汞或含汞物质用作试剂或催化剂的方法中获得。可提及的实例是在通过汞齐法制备氯的过程中获得的电解氢气。由于汞的高毒性，在大多数情况下必须将该金属或含该金属的化合物从在相关方法中获得的料流中分离出去。此外，汞具有通过形成汞齐破坏铝表面的氧化层而腐蚀含铝设备的性质，因此通过由铝制成的设备或容器的料流必须几乎不含汞。另外，痕量汞会使用于例如石油化学方法中的含贵金属的催化剂中毒。
在Fuel Processing Technology 82(2003)，第89-165页中，J.H.Pavlish等概述了从燃煤发电厂获得的废气流中脱除汞的方法。在Hydrocarbon Processing，1999，第61页及以下中，S.M.Wilhelm概述了从液态烃料流中脱除汞的方法。Steve Coleman等在Feedstock Contaminants in Ethylene Plants，2005 Spring National Meeting Atlanta，GA，April 10-14，2005中概述了烯烃工厂中的汞脱除。
如果金属汞以液态形式存在于物料流中，常利用汞的高表面张力或高比重，通过倾析、借助聚结过滤器、活性炭涂覆的过滤器等的机械方法脱除汞。EP-A 0761830公开了简单且纯机械的方法，其中细碎的汞通过聚结形成易分离的更大的汞液滴而加以收集。WO 2004/048624描述了通过人工石墨过滤脱除汞的方法。
还常采用将汞与吸附剂结合的方法进行汞脱除。因此，DE-A 2643478描述了通过在具有至少250m2/g比表面积的活性碳上进行吸附将汞从液体中分离。如US 3,755,989所述，将碳基吸附剂用于，尤其是从物料流中脱除汞。US 4,500,327描述了用于从气态料流中脱除汞的硫浸渍的活性碳，而JP 52-53793描述了采用含碘化物的活性碳从液态料流中脱除汞。US4,909,926和US 4,094,777描述了采用位于载体材料如氧化铝上的含CuS或CuO或Ag2S的活性组合物从物料流中脱除汞。EP-A 0385742描述了通过将料流与存在于载体上的金属铜或铜化合物接触从包含具有至多8个碳原子的烃的液态烃料流中脱除汞的方法。
还常利用固体汞齐的形成脱除汞。用于该目的的最合适的金属是周期表中第XI族金属(Cu、Ag、Au)，其通常以吸收组合物的形式加以使用，其中所述金属均匀分布在载体上。因此，DE-A 2102039公开了从气体中脱除汞的方法，其中将含汞气体与位于多孔氧化铝载体上的含铜组合物接触。US 4,230,486公开了将液体通过位于多孔载体如活性碳或陶瓷载体上的含金属银的吸收剂之上而从液体中脱除汞的方法。DE-A 4221207教导了将溶液通过银涂覆的纤维之上而从碱金属氢氧化物溶液或碱金属醇盐溶液中脱除汞的方法。DE-A 4116890公开了用于脱除汞的吸收剂，特别地，其包含位于具有300-1000m2/g BET表面积的活性碳载体上的Cu、Ag、Fe和Bi，或Au、Sn、Zn和Pd以及金属态或氧化物或硫化物形式的所述金属的混合物。
US 4,911,825描述了从烃料流中脱除汞和砷的方法，包括：在第一步中，在氢气存在下将这些烃料流与位于氧化铝上的含镍和钯的催化剂接触，在第二步中将其与位于载体上的含硫或金属硫化物，优选为硫化铜或硫化铜和硫化银的组合的吸收剂接触。该方法也可在一个步骤中在所述催化剂和吸收剂的混合物上进行。FR-A 2310795描述了采用位于由二氧化硅、氧化铝或硅铝酸盐组成的具有40-250m2/g BET表面积的载体上的含金属金、银、铜或镍的吸收剂从气态天然气料流中脱除汞。WO 91/15559公开了通过将液态烃料流与吸收剂接触从液态烃料流中脱除汞的方法，所述吸收剂是通过将粉状氧化物(优选为选自氧化镍、氧化铜和氧化钴的氧化物)与多孔载体材料如氧化铝、二氧化硅、沸石或粘土混合，随后进行还原而制备的。
本发明的目标是提供一种从含汞烃料流中脱除汞的改进方法。
该目标通过一种从含汞烃料流中脱除汞的方法实现，其中将烃料流与位于多孔氧化物载体材料上的含铜吸收剂接触，其中在氢气存在下将烃料流与吸收剂接触。
已经发现在氢气存在下使用含铜吸收剂比无氢气时能更好地从烃料流中脱除汞，所述吸收剂包含位于载体上的铜并且也可有效地作为氢化催化剂。
本发明所用的吸收剂包含位于多孔载体材料上的铜，优选为还原态。本发明所用的吸收剂也可有效地作为氢化催化剂。合适的多孔载体材料是无定形和晶态的硅铝酸盐、氧化铝、二氧化硅、粘土和金属氧化物。合适的粘土如硅镁土、高岭土、膨润土、漂白土。合适的金属氧化物如氧化铝和二氧化硅以及氧化镁、二氧化锆、二氧化钛、氧化锌、氧化铬(III)、氧化钡及其混合物。优选的氧化铝是γ-氧化铝。
在本发明方法中可使用所有常规的活化(还原)形式的含铜氢化催化剂。
本发明所用的含铜氢化活性吸收剂可通过将氧化铜与载体材料混合并随后优选在氢气流中通过还原将铜转化为金属态而获得。本发明所用的吸收剂也可通过将载体材料用铜盐的水溶液浸渍，干燥，如果合适的话进行煅烧以及通过还原将铜转化为金属态而制备，所述还原优选采用含氢气的气流，尽管也可采用还原剂如肼。
在本发明所用的吸收剂中，铜通常以细分散在载体材料上的还原态即金属(元素)态存在。通常本发明所用的吸收剂包含位于氧化物载体材料上的10-50重量％的铜。在其基础上获得本发明所用的吸收剂的合适的组合物的实例是含氧化铜、氧化锌和氧化铝的组合物或含氧化铜、氧化镁、氧化钡、氧化铬(III)、氧化锌和二氧化硅的组合物。尤其优选10-60重量％的氧化铜、0-40重量％的氧化锌、0-20重量％的氧化铝、5-25重量％的氧化镁、10-40重量％的二氧化硅、0-5重量％的氧化铬(III)以及0-10重量％的氧化钡的混合物。
根据本发明，可从其中脱除汞的烃料流是任何可能被汞污染的烃料流。这些通常包括具有1-14个碳原子的脂族烃、芳烃、脂环烃和/或杂环烃。根据本发明，可被脱除汞的烃混合物的实例是LNG(液化天然气)、LPG(液化石油气)、石脑油以及煤油。可根据本发明的方法净化的纯净烃的实例是乙烯和丙烯以及脂族烃。
在实施本发明的方法之前，烃或烃混合物中的汞含量可至多为100ppm，但通常至多为1ppm的Hg。汞通常以有机汞化合物的形式存在。
本发明的方法可以以悬浮模式或固定床模式进行。如果以固定床模式进行，其可以以上流模式或下流模式进行。可使用气态或液态的含汞或砷的烃或烃混合物。优选使用液态的烃或烃混合物。将氢气与气态或液态的烃或烃混合物一起引入到合适的反应容器中，并使其通过(通常并流通过)存在于固定床中的颗粒状吸收剂之上。这可以以上流模式或下流模式进行。然而，也可将氢气与烃或烃混合物对流通过吸收剂床之上。吸收剂也可以以悬浮形式存在于烃或烃混合物中。通常该方法在30-250℃，优选60-180℃的温度和1-20bar的氢气压下进行。所述压力优选以使得烃或烃混合物作为液态存在的方式加以选择。引入的氢气量通常对应于10-650标准l/kg吸收剂/小时的空速。
在吸收剂耗尽后，其可通过在惰性气流或含氢气的气流中加热，通常温度为180-400℃，如200-220℃，并使气化的汞冷凝出去而热再生。
通过下文的实施例对本发明进行说明。
实施例
对比实施例1
将对应于350ppm Hg的处于500ml辛烷中的二苯汞(Ph2Hg)溶液在玻璃烧瓶中加热到60℃。在搅拌下，将1.5标准l/h的氢气通入该溶液。将5g未还原的含40重量％的CuO、40重量％的ZnO和20重量％的Al2O3的氢化催化剂以3×5mm的片剂(吸收剂A)形式加入到该溶液中。在2h和24h后从溶液中提取试样并测定试样中的汞含量。结果见表1。
对比实施例2
将对应于350ppm汞的处于500ml辛烷中的二苯汞溶液在玻璃烧瓶中加热到60℃。将事先在180℃下经H2还原和活化的5g含40重量％的CuO、40重量％的ZnO和20重量％的Al2O3的催化剂以3×5mm的片剂(吸收剂B)形式加入到该溶液中。不通入氢气。搅拌该溶液。在2h和24h后提取试样并测定其汞含量。结果见表1。
实施例1
重复对比实施例2的程序，但是通入1.5标准l/h的氢气。以固定的间隔提取试样并测定其汞含量。结果见表1。
实施例2
重复实施例1的程序，但将还原的催化剂以粉状形式(吸收剂C)加入。以固定的间隔提取试样并测定其汞含量。结果见表1。
表1
实施例3
重复实施例1的程序，但将溶液保持在25℃。以固定的间隔提取试样并测定其汞含量。结果见表2。
实施例4
重复实施例1的程序。此时温度为60℃。以固定的间隔提取试样并测定其汞含量。结果见表2。
实施例5
重复实施例1的程序，但将溶液加热到100℃。以固定的间隔提取试样并测定其汞含量。结果见表2。
表2
实施例6
在内径为6mm且总长为5m的单线(monoline)反应器中进行实验。反应器包括通过毛细管相互连接的4段。反应器以下流模式运行。将反应器各段保持在60℃。在反应器入口前将液态烃进料与氢气混合。借助于低温冷凝器将反应器输出物冷却并将气相与液相分离。所述液相用于测定汞含量，气相经由汞防护床处理。
80g含45重量％的CuO、16重量％的MgO、35重量％的SiO2、0.9重量％的Cr2O3、1.1重量％的BaO以及0.6重量％的ZnO的催化剂以3×5mm的片剂形式存在于反应器中。在各单独的片剂之间，存在直径为2mm的玻璃球。首先将催化剂在180-220℃下，在氢气流中活化。随后在氢气流中将反应器冷却到60℃。反应器在大气压下运行。
将用有机汞化合物饱和的辛烷用作进料。在部分实验中将乙酸苯汞PhHgOAc用作有机汞化合物，在另一部分试验中将乙酸汞Hg(OAc)2用作有机汞化合物。在每种情况下使用具有不同汞浓度的大量批料。计量加入100标准l/h的含汞辛烷和2标准l/h的氢气。实验结果见表3。
表3
| 实验号 | 加入的汞化合物 | 进料中汞的浓度[ppm] | 输出物中汞的浓度[ppm] |
| 1 | PhHgOAc | 80 | 0.004 |
| 2 | PhHgOAc | 90 | 0.002 |
| 3 | PhHgOAc | 80 | 0.004 |
| 4 | PhHgOAc | 60 | 0.001 |
| 5 | Hg(OAc)2 | 6 | 0.001 |
| 6 | Hg(OAc)2 | 1.4 | 0.001 |
| 7 | Hg(OAc)2 | 0.6 | 0.001 |
| 8 | Hg(OAc)2 | 2.8 | 0.001 |
| 9 | Hg(OAc)2 | 1.2 | 0.001 |
| 10 | PhHgOAc | 90 | 0.001 |
| 11 | PhHgOAc | 120 | 0.003 |
| 12 | PhHgOAc | 75 | 0.004 |
Claims (8)
1.一种从含汞烃料流中脱除汞的方法，其中将烃料流与位于载体材料上的含铜吸收剂接触，其中在氢气存在下将烃料流与吸收剂接触。
2.根据权利要求1所述的方法，其中铜存在于多孔氧化物载体材料上。
3.根据权利要求1或2所述的方法，其中吸收剂包含10-60重量％的铜。
4.根据权利要求1-3任一项所述的方法，其中吸收剂包含10-60重量％的氧化铜、0-40重量％的氧化锌、0-20重量％的氧化铝、5-25重量％的氧化镁、10-40重量％的二氧化硅、0-5重量％的氧化铬(III)以及0-10重量％的氧化钡。
5.根据权利要求1-4任一项所述的方法，其中烃料流以液态形式存在。
6.根据权利要求1-5任一项所述的方法，其中吸收剂作为固定床存在。
7.根据权利要求6所述的方法，其中将烃料流以上流模式或下流模式与吸收剂接触。
8.根据权利要求5所述的方法，其中吸收剂以悬浮形式存在于烃料流中。
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| DE2656803C2 (de) * | 1975-12-18 | 1986-12-18 | Institut Français du Pétrole, Rueil-Malmaison, Hauts-de-Seine | Verfahren zur Entfernung von in einem Gas oder in einer Flüssigkeit vorhandenem Quecksilber |
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| FR2628338B1 (fr) * | 1988-03-10 | 1991-01-04 | Inst Francais Du Petrole | Procede pour l'elimination du mercure dans les hydrocarbures |
| US4909926A (en) * | 1989-02-01 | 1990-03-20 | Mobil Oil Corporation | Method for removing mercury from hydrocarbon oil by high temperature reactive adsorption |
| JP2578514B2 (ja) * | 1989-03-03 | 1997-02-05 | 三井石油化学工業株式会社 | 液体炭化水素化合物中の水銀の除去方法 |
| FR2644472B1 (fr) * | 1989-03-16 | 1991-06-21 | Inst Francais Du Petrole | Procede pour l'elimination du mercure et eventuellement d'arsenic dans les hydrocarbures |
| US5401392A (en) * | 1989-03-16 | 1995-03-28 | Institut Francais Du Petrole | Process for eliminating mercury and possibly arsenic in hydrocarbons |
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| DE4221207A1 (de) * | 1992-06-27 | 1994-01-05 | Huels Chemische Werke Ag | Verfahren zur Entfernung von Quecksilber aus Flüssigkeiten |
| FR2701270B1 (fr) * | 1993-02-08 | 1995-04-14 | Inst Francais Du Petrole | Procédé d'élimination du mercure dans les hydrocarbures par passage sur un catalyseur présulfuré. |
| US5948726A (en) * | 1994-12-07 | 1999-09-07 | Project Earth Industries, Inc. | Adsorbent and/or catalyst and binder system and method of making therefor |
| FR2764214B1 (fr) * | 1997-06-10 | 1999-07-16 | Inst Francais Du Petrole | Procede et masses de captation pour l'elimination du mercure et de l'arsenic dans les coupes hydrocarbonees |
| JP2004167306A (ja) * | 2002-11-18 | 2004-06-17 | Ict:Kk | 排ガス浄化用触媒および排ガス浄化方法 |
| DE10255240A1 (de) * | 2002-11-26 | 2004-06-09 | Basf Ag | Verfahren zur Entfernung von Quecksilber aus mit Quecksilber verunreinigten Lösungen |
| WO2007147781A1 (de) * | 2006-06-21 | 2007-12-27 | Basf Se | Absorptionsmasse und verfahren zur entfernung von quecksilber |
-
2009
- 2009-03-09 CN CN2009801084389A patent/CN101970614A/zh active Pending
- 2009-03-09 EP EP09720628A patent/EP2265695A1/de not_active Withdrawn
- 2009-03-09 JP JP2010550151A patent/JP5455939B2/ja not_active Expired - Fee Related
- 2009-03-09 KR KR1020107021637A patent/KR20100133394A/ko not_active Application Discontinuation
- 2009-03-09 US US12/921,579 patent/US20110005975A1/en not_active Abandoned
- 2009-03-09 WO PCT/EP2009/052693 patent/WO2009112440A1/de active Application Filing
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102764655A (zh) * | 2011-12-23 | 2012-11-07 | 盐城工学院 | 一种新型脱汞催化剂 |
| CN102764655B (zh) * | 2011-12-23 | 2015-03-04 | 盐城工学院 | 一种脱汞催化剂 |
| CN104582834A (zh) * | 2012-02-06 | 2015-04-29 | 环球油品公司 | 用于汞脱除的保护吸附剂及其制备和使用方法 |
| CN105148913A (zh) * | 2015-10-08 | 2015-12-16 | 宁波海越新材料有限公司 | 一种用于仲丁醇制备甲乙酮的催化剂及其制备方法 |
| CN108249955A (zh) * | 2018-04-02 | 2018-07-06 | 中科京投环境科技江苏有限公司 | 一种脱除废、污水中汞的复合陶瓷材料及制备方法 |
| CN108249955B (zh) * | 2018-04-02 | 2020-12-29 | 中科京投环境科技江苏有限公司 | 一种脱除废、污水中汞的复合陶瓷材料的制备方法 |
| CN115698231A (zh) * | 2020-05-29 | 2023-02-03 | 埃克森美孚化学专利公司 | 含汞进料的烃热解 |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2009112440A1 (de) | 2009-09-17 |
| EP2265695A1 (de) | 2010-12-29 |
| US20110005975A1 (en) | 2011-01-13 |
| KR20100133394A (ko) | 2010-12-21 |
| JP5455939B2 (ja) | 2014-03-26 |
| JP2011513565A (ja) | 2011-04-28 |
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