CN113231004A - 一种金属硒化物汞吸附剂的常温常压制备方法和应用 - Google Patents
一种金属硒化物汞吸附剂的常温常压制备方法和应用 Download PDFInfo
- Publication number
- CN113231004A CN113231004A CN202110588946.4A CN202110588946A CN113231004A CN 113231004 A CN113231004 A CN 113231004A CN 202110588946 A CN202110588946 A CN 202110588946A CN 113231004 A CN113231004 A CN 113231004A
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- China
- Prior art keywords
- mercury
- metal selenide
- adsorbent
- normal temperature
- selenide
- 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.)
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- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 title claims abstract description 136
- 229910052753 mercury Inorganic materials 0.000 title claims abstract description 129
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 76
- 239000002184 metal Substances 0.000 title claims abstract description 76
- 150000003346 selenoethers Chemical class 0.000 title claims abstract description 62
- 239000003463 adsorbent Substances 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 21
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000011669 selenium Substances 0.000 claims abstract description 19
- 229910052711 selenium Inorganic materials 0.000 claims abstract description 17
- 238000001556 precipitation Methods 0.000 claims abstract description 10
- 239000000126 substance Substances 0.000 claims abstract description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000010949 copper Substances 0.000 claims abstract description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 3
- 239000011651 chromium Substances 0.000 claims abstract description 3
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 3
- 239000010941 cobalt Substances 0.000 claims abstract description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052802 copper Inorganic materials 0.000 claims abstract description 3
- 229910052742 iron Inorganic materials 0.000 claims abstract description 3
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims abstract description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 3
- 239000011733 molybdenum Substances 0.000 claims abstract description 3
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 3
- 229910052709 silver Inorganic materials 0.000 claims abstract description 3
- 239000004332 silver Substances 0.000 claims abstract description 3
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 3
- 239000011701 zinc Substances 0.000 claims abstract description 3
- 229940091258 selenium supplement Drugs 0.000 claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 14
- 239000002243 precursor Substances 0.000 claims description 13
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 12
- 239000003546 flue gas Substances 0.000 claims description 12
- 239000002440 industrial waste Substances 0.000 claims description 10
- 239000002699 waste material Substances 0.000 claims description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- 239000003638 chemical reducing agent Substances 0.000 claims description 9
- 238000011084 recovery Methods 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 8
- 230000032683 aging Effects 0.000 claims description 6
- 238000006722 reduction reaction Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000001784 detoxification Methods 0.000 claims description 5
- 239000012266 salt solution Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 239000004094 surface-active agent Substances 0.000 claims description 5
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 4
- 230000009471 action Effects 0.000 claims description 4
- BVTBRVFYZUCAKH-UHFFFAOYSA-L disodium selenite Chemical compound [Na+].[Na+].[O-][Se]([O-])=O BVTBRVFYZUCAKH-UHFFFAOYSA-L 0.000 claims description 4
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 4
- 238000005580 one pot reaction Methods 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- -1 selenide compound Chemical class 0.000 claims description 4
- 229960001471 sodium selenite Drugs 0.000 claims description 4
- 239000011781 sodium selenite Substances 0.000 claims description 4
- 235000015921 sodium selenite Nutrition 0.000 claims description 4
- 238000005507 spraying Methods 0.000 claims description 4
- 239000000725 suspension Substances 0.000 claims description 4
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 3
- YAZJAPBTUDGMKO-UHFFFAOYSA-L potassium selenate Chemical compound [K+].[K+].[O-][Se]([O-])(=O)=O YAZJAPBTUDGMKO-UHFFFAOYSA-L 0.000 claims description 3
- 239000012279 sodium borohydride Substances 0.000 claims description 3
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 3
- PMYDPQQPEAYXKD-UHFFFAOYSA-N 3-hydroxy-n-naphthalen-2-ylnaphthalene-2-carboxamide Chemical compound C1=CC=CC2=CC(NC(=O)C3=CC4=CC=CC=C4C=C3O)=CC=C21 PMYDPQQPEAYXKD-UHFFFAOYSA-N 0.000 claims description 2
- GFLJTEHFZZNCTR-UHFFFAOYSA-N 3-prop-2-enoyloxypropyl prop-2-enoate Chemical compound C=CC(=O)OCCCOC(=O)C=C GFLJTEHFZZNCTR-UHFFFAOYSA-N 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 125000000129 anionic group Chemical group 0.000 claims description 2
- 150000001661 cadmium Chemical class 0.000 claims description 2
- RNGFNLJMTFPHBS-UHFFFAOYSA-L dipotassium;selenite Chemical compound [K+].[K+].[O-][Se]([O-])=O RNGFNLJMTFPHBS-UHFFFAOYSA-L 0.000 claims description 2
- 239000003792 electrolyte Substances 0.000 claims description 2
- 229920000371 poly(diallyldimethylammonium chloride) polymer Polymers 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- 239000011655 sodium selenate Substances 0.000 claims description 2
- 229960001881 sodium selenate Drugs 0.000 claims description 2
- 235000018716 sodium selenate Nutrition 0.000 claims description 2
- 239000002594 sorbent Substances 0.000 claims description 2
- 239000002801 charged material Substances 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- YQMLDSWXEQOSPP-UHFFFAOYSA-N selanylidenemercury Chemical compound [Hg]=[Se] YQMLDSWXEQOSPP-UHFFFAOYSA-N 0.000 abstract description 3
- 239000004568 cement Substances 0.000 abstract description 2
- 239000003245 coal Substances 0.000 abstract description 2
- 238000005272 metallurgy Methods 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract 3
- 239000006227 byproduct Substances 0.000 abstract 1
- 229910052793 cadmium Inorganic materials 0.000 abstract 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 12
- 239000000047 product Substances 0.000 description 9
- IRPLSAGFWHCJIQ-UHFFFAOYSA-N selanylidenecopper Chemical compound [Se]=[Cu] IRPLSAGFWHCJIQ-UHFFFAOYSA-N 0.000 description 8
- 230000000694 effects Effects 0.000 description 5
- 229920005830 Polyurethane Foam Polymers 0.000 description 4
- QVYIMIJFGKEJDW-UHFFFAOYSA-N cobalt(ii) selenide Chemical compound [Se]=[Co] QVYIMIJFGKEJDW-UHFFFAOYSA-N 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000002386 leaching Methods 0.000 description 4
- 239000011496 polyurethane foam Substances 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 238000007873 sieving Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910000365 copper sulfate Inorganic materials 0.000 description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 2
- OMZSGWSJDCOLKM-UHFFFAOYSA-N copper(II) sulfide Chemical compound [S-2].[Cu+2] OMZSGWSJDCOLKM-UHFFFAOYSA-N 0.000 description 2
- 230000002354 daily effect Effects 0.000 description 2
- 238000006477 desulfuration reaction Methods 0.000 description 2
- 230000023556 desulfurization Effects 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- QHASIAZYSXZCGO-UHFFFAOYSA-N selanylidenenickel Chemical compound [Se]=[Ni] QHASIAZYSXZCGO-UHFFFAOYSA-N 0.000 description 2
- 125000003748 selenium group Chemical group *[Se]* 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- XTLZBEXMSFKWKX-UHFFFAOYSA-N [Cu].[Se]=[Fe] Chemical compound [Cu].[Se]=[Fe] XTLZBEXMSFKWKX-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 231100000693 bioaccumulation Toxicity 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- VZZSRKCQPCSMRS-UHFFFAOYSA-N dipotassium;selenium(2-) Chemical compound [K+].[K+].[Se-2] VZZSRKCQPCSMRS-UHFFFAOYSA-N 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002500 ions Chemical class 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
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 239000003077 lignite Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000002731 mercury compounds Chemical class 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000003345 natural gas Substances 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
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000002688 persistence Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003342 selenium Chemical class 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- VPQBLCVGUWPDHV-UHFFFAOYSA-N sodium selenide Chemical compound [Na+].[Na+].[Se-2] VPQBLCVGUWPDHV-UHFFFAOYSA-N 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 238000004056 waste incineration Methods 0.000 description 1
Classifications
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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
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01D53/02—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 by adsorption, e.g. preparative gas chromatography
- B01D53/04—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 by adsorption, e.g. preparative gas chromatography with stationary adsorbents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01D53/02—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 by adsorption, e.g. preparative gas chromatography
- B01D53/06—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 by adsorption, e.g. preparative gas chromatography with moving adsorbents, e.g. rotating beds
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- 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
- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- 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
- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
- B01J20/0229—Compounds of Fe
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- 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
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- 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
- B01J20/0262—Compounds of O, S, Se, Te
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/262—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon to carbon unsaturated bonds, e.g. obtained by polycondensation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/10—Destroying solid waste or transforming solid waste into something useful or harmless involving an adsorption step
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/60—Heavy metals or heavy metal compounds
- B01D2257/602—Mercury or mercury compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/02—Other waste gases
- B01D2258/0283—Flue gases
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Abstract
本发明公开了一种金属硒化物汞吸附剂的常温常压制备方法和应用；本发明采用沉淀法在常温常压下制备金属硒化物汞吸附剂。金属硒化物汞吸附剂包含铬、锰、铁、铜、钴、镍、锌、钼、银、镉中的一种或多种与硒形成的化合物及其复合物，其通过将不稳定的汞转化为稳定的硒化汞，脱除燃煤、冶金、垃圾焚烧、水泥生产等工业尾气或副产物中的汞，吸收富集含汞生活用品中的汞，实现汞资源的回收和再利用，其中待处理的汞可以单质态、游离态和/或化合物态等形式存在。由于金属硒化物具有极高的汞吸附容量和吸附速率，实现其常温常压条件下的规模化制备对汞污染防治具有重大意义，相应技术具有广阔的市场应用前景。
Description
技术领域
本发明属于环境污染防治净化技术领域，具体涉及一种金属硒化物汞吸附剂的常温常压制备方法和应用。
背景技术
汞由于其持久性、剧毒性和生物富集性，对生态环境和人类健康构成巨大危害。根据UNEP最新发布的《全球汞评估报告》，全球人为汞排放量已达约2500吨/年，远远超过了由于自然活动而排放到大自然中的汞。2017年8月全球《水俣公约》已在包含中国在内的128个签约国正式生效，其目的在于：（1）限制日益加剧的全球汞污染排放，（2）通过汞资源回收解决地壳汞资源日益枯竭的问题。因此，开发经济、高效的汞吸附剂，实现汞的脱除、解毒、富集和回收，是解决汞污和汞资源枯竭问题的关键。
金属硒化物是迄今为止吸附量最高的汞吸附剂，可将汞以很高的浓度富集在其表面，实现汞的高效解毒，利于汞的进一步回收。然而，由于可溶于水的负二价硒离子前驱体（如：硒化钠、硒化钾等）在常温常压下容易被水解，无法长期储存，金属硒化物汞吸附剂在前期研究中均只能通过水热法这种高能耗、低产能的方法制备，无法实现大规模应用。
发明内容
为了克服现有技术的不足，本发明的目的是提供一种金属硒化物汞吸附剂的常温常压制备方法及其应用。本发明的制备方法与传统水热法制备金属硒化物汞吸附剂相比，常温常压沉淀法具有能耗低、成本低、产能高、易于大规模应用的特点；所制备的金属硒化物结晶度一般低于高温高压条件下制备所得的金属硒化物，所含不饱和硒位点的比例一般高于高温高压条件制备的金属硒化物，脱汞效果优于高温高压条件下所制备的金属硒化物。
本发明利用强还原剂，将性质稳定、利于储存的高价态硒前驱体还原为负二价，与金属盐溶液在常温常压下发生沉淀反应，制备金属硒化物汞吸附剂，金属硒化物汞吸附剂是二元或多元金属硒化物或者与载体形成的金属硒化物复合物。本发明使用常温常压条件下制备的金属硒化物作为汞吸附剂，基于汞和硒原子之间很强的相互作用力，可以将单质汞、游离态汞和其它不稳定的汞化合物转化为稳定的、不溶于水的硒化汞，从而实现汞的一步固定解毒。此外，金属硒化物由于具有极高的汞吸附容量（通常大于100 mg/g），可将低富集程度的汞集中富集起来，实现汞资源的回收和再利用。其应用范围广泛，包括工业烟气的高效脱汞，工业废物和产物的净化，含汞产品/生活用品/废物中汞的富集吸收等。本发明的技术方案具体介绍如下。
本发明提供一种金属硒化物汞吸附剂的常温常压制备方法，具体步骤如下：常温常压下，以硒粉、硒酸钠、亚硒酸钠、硒酸钾或亚硒酸钾中的一种或几种作为硒前驱体，将硒前驱体在还原剂作用下发生还原反应生成负二价硒的物质，再加入可溶性金属盐溶液，发生沉淀反应，一锅法制备金属硒化物汞吸附剂；其中：可溶性金属盐选自铬、锰、铁、铜、钴、镍、锌、钼、银或镉盐中的一种或几种。
本发明中，常温是指环境温度，温度区间在0-30 ℃之间；常压是指标准大气压，沉淀老化时间不超过1 h。
本发明中，可溶性金属盐选自硝酸盐、硫酸盐或氯化物中的一种或几种。
本发明中，还原剂选自水合肼、硼氢化钠或硼氢化钾中的一种或几种；还原反应体系中，加入氢氧化钠或氢氧化钾中的一种或两种，用于促进硒前驱体在常温常压下溶解。
本发明中，在含有载体的悬浮液中加入表面活性剂或反电荷物质的体系中，加入硒前驱体和还原剂，将硒前驱体在还原剂作用下发生还原反应生成负二价硒的物质，再加入可溶性金属盐溶液，发生沉淀反应，一锅法获得金属硒化物负载于载体上的金属硒化物复合物。
本发明中，制备的金属硒化物汞吸附剂的比表面积介于0.01-2000 m2/g之间。
本发明中，表面活性剂或反电荷物质选自CTAB、PDDA、PSS或阴离子电解质中的一种。表面活性剂或反电荷物质用于调控金属硒化物的晶粒粒径并将其负载于优势载体上。
本发明还提供一种上述的常温常压制备方法制得的金属硒化物汞吸附剂。
本发明进一步提供一种上述的金属硒化物汞吸附剂的应用，应用方法包括：
（1）金属硒化物汞吸附剂以固定床形式布置于烟气道任何位置，或以喷射法直接喷入烟气道当中，实现工业烟气脱汞；
（2）将金属硒化物汞吸附剂投加到液体工业废物或产物中吸收富集液体中的汞，或直接析出固体工业废物中含有的汞，实现工业废物或产物脱汞；
（3）将金属硒化物汞吸附剂用于富集泄露、释放到空气中的汞，或直接从生活用品或废物中将汞析出并富集，实现生活用品或废物中汞的解毒和回收。
本发明中，金属硒化物汞吸附剂的应用温度介于室温到350 ℃之间。
本发明进一步提供金属硒化物汞吸附剂的应用，该金属硒化物吸附剂可实现燃煤、冶金、垃圾焚烧、水泥生产、钢铁生产、天然气生产等工业过程、废物、产物中汞的脱除、富集和回收。
用于工业烟气脱汞时，汞可以单质态、氧化态或有机态的形式存在，吸附剂可以固定床形式布置于烟气道任何位置，或以喷射法直接喷入烟气道当中。
用于工业废物或产物脱汞时，汞可以游离态、氧化态、颗粒态或有机态的形式存在，吸附剂可以投加到液体工业废物或产物中（如：污酸、脱硫液、硫酸等）吸收富集液体中的汞，或直接析出固体工业废物中含有的汞（如：脱硫石膏、飞灰、残渣等）。
该吸附剂可用于处理含汞生活用品（如：水银温度计、含汞血压计、含汞电池、含汞灯管等），实现汞的富集和回收。
用于处理生活用品/废物时，汞可以单质态、游离态、氧化态、颗粒态或有机态等形式存在，吸附剂可用于富集泄露、释放到空气中的汞，或直接从生活用品/废物中将汞析出并富集起来。
所采用的载体应利于汞和吸附剂之间的气固传质，通过气体压降测量，只要负载后的吸附剂在同等厚度情况下压降小于负载前粉末金属硒化物（粒径一般介于5 nm至1 mm之间），所采用的载体均在本发明覆盖范围内。
和现有技术相比，本发明具有以下优点：
和传统活性炭与贵金属吸附剂相比，常温制备的金属硒化物的汞吸附容量和汞吸附速率增大了至少两个数量级，脱汞成本显著降低。
和金属硫化物相比，常温常压制备的金属硒化物的汞吸附容量和吸附速率成倍增长，具备处理高浓度汞的能力。
与水热法制备的金属硒化物相比，采用常温常压条件通过沉淀法制备金属硒化物成本和能耗更低，满足规模化制备条件，可以实现批量生产以及工业化、日常化应用。
由于金属硒化物具有很大的汞吸附量，和其它吸附剂相比，从金属硒化物中回收汞是一条更加切实可行的路径。
由于产物硒化汞在水中的溶解度极低，类似于汞在自然界中的状态，含汞的废弃金属硒化物吸附剂可以直接填埋，实现汞的自然归驱。
具体实施方式
以下通过具体实施例对本发明的技术方案做进一步描述。实施例并非对保护范围的限制。
实施例1
常温常压条件下制备硒化铜吸附剂。具体步骤如下：将硒粉溶于适量水合肼的氢氧化钠溶液中，待完全溶解后，将硫酸铜溶液倒入硒溶液中(Cu：Se元素的摩尔比为1:1)，将生成的沉淀（老化时间30 min）分离、干燥、过筛后即可得硒化铜吸附剂。
将所获得的硒化铜吸附剂置于长为10 cm，内径1 cm的圆柱形石英玻璃固定床反应器中。通过汞渗透管产生汞，使用VM3000测汞仪监测反应器进出口单质汞浓度，初始单质汞浓度为1 mg/m3，通过硒化铜吸附剂后的单质汞浓度小于0.001 mg/m3，汞脱除效率达99.9%以上。本实施例充分说明了常温常压条件下制备的金属硒化物吸附剂具有优异的气相脱汞能力。
实施例2
常温常压条件下制备硒化钴吸附剂。具体步骤如下：将亚硒酸钠溶于硼氢化钠溶液中（加入适量的氢氧化钾），并将等量的氯化钴溶液倒入亚硒酸钠溶液中(Co：Se元素的摩尔比为1:1)，将生成的沉淀（老化时间30 min）分离、干燥、过筛后即可得硒化钴吸附剂。
将所获得的硒化钴吸附剂和含有0.05 mg/L汞的污酸混合，搅拌10 min后，污酸中的汞浓度低于0.001 mg/L。此外，采用TCLP法模拟含汞吸附剂暴露于环境中后的汞浸出率，发现汞从含汞的硒化钴中浸出的比例仅为0.04%，汞浸出量仅为0.0005 mg/L，远低于美国EPA规定的液体安全汞浓度上限（0.02 mg/L）。本实施例充分说明常温常压条件下制备的金属硒化物吸附剂具有优异的液相脱汞能力，含汞的金属硒化物废弃吸附剂也可以直接采取填埋处理。
实施例3
常温条件下制备金属硒化镍负载的聚氨酯泡沫吸附剂。具体步骤如下：将聚氨酯泡沫悬浮于水中，在悬浮液中加入CTAB后搅拌24 h，在上述悬浮液中加入适量硒粉的硼氢化钠-氢氧化钠溶液，继续搅拌24 h，随后加入适量的硫酸镍溶液，将生成的沉淀（老化时间1 h）分离、干燥、过筛后即可得金属硒化镍负载聚氨酯泡沫吸附剂。
将负载金属硒化物的聚氨酯泡沫塑料置于内径1 cm的圆柱形石英玻璃固定床反应器中，通过汞渗透管产生汞，使用VM3000测汞仪监测反应器进出口单质汞浓度，初始单质汞浓度为1 mg/m3，通过硒化铜吸附剂后的单质汞浓度小于0.001 mg/m3，汞脱除效率达99.9%以上。本实例充分说明常温常压条件下制备的金属硒化物可以通过加入反电荷离子负载于优势载体表面，从而采用固定床反应器实现工业烟气中汞的脱除和富集。
实施例4
常温条件下制备硒化铁铜吸附剂。具体步骤如下：将硒酸钾溶于水合肼中（加入适量的氢氧化钠），并将适量的硫酸铜和硫酸亚铁加入上述溶液中，待生成沉淀后（老化时间30 min）将其分离、干燥、过筛获得常温常压制备的硒化铁铜吸附剂。
取100 g吸附剂覆盖于体积为1 cm3左右的液态水银表面，可将体积1 cm3左右的水银完全吸收。本实例充分说明常温常压条件下制备的金属硒化物吸附剂可以处理日常生活中出现的汞泄露事故。
实施例5
在某装机容量约为6 MW的小型电厂进行了实验，燃料为褐煤，烟气量约为15000m3·min-1，汞的质量浓度为0.327 mg·m-3，分别在湿法脱硫及湿法除尘上游安装吸附剂喷射塔（温度分别为105℃和65 ℃）喷入合成的硒化铜（按实施例1所述的方法制备）。当硒化铜喷入量为8 mg·m-3，烟气中汞的脱出率达到100%，通过0.6%的醋酸溶液模拟环境浸出，浸出的汞仅为吸附汞含量的0.01%，几乎可以忽略不计。同时测试了硫化铜的汞吸附效果，当喷入硫化铜的量达到50mg m-3时，汞吸附效率效果才能达到100%，且浸出的汞达到吸附汞含量的0.7%。本实例充分说明常温常压沉淀法所制备得金属硒化物的工业应用前景。
以上实施例是对本发明的说明，不是对本发明的限定，任何对本发明进行简单修改后的方案，都属于本发明的保护范围。
Claims (9)
1.一种金属硒化物汞吸附剂的常温常压制备方法，其特征在于，常温常压下，以硒粉、硒酸钠、亚硒酸钠、硒酸钾或亚硒酸钾中的一种或几种作为硒前驱体，将硒前驱体在还原剂作用下发生还原反应生成负二价硒的物质，再加入可溶性金属盐溶液，发生沉淀反应，一锅法制备金属硒化物汞吸附剂；其中：可溶性金属盐选自铬、锰、铁、铜、钴、镍、锌、钼、银或镉盐中的一种或几种。
2.根据权利要求1所述的常温常压制备方法，其特征在于，常温是指环境温度，温度区间在0-30 ℃之间；常压是指标准大气压，沉淀老化时间不超过1 h。
3.根据权利要求1所述的常温常压制备方法，其特征在于，可溶性金属盐选自硝酸盐、硫酸盐或氯化物中的一种或几种。
4.根据权利要求1所述的常温常压制备方法，其特征在于，还原剂选自水合肼、硼氢化钠或硼氢化钾中的一种或几种；还原反应体系中，加入氢氧化钠或氢氧化钾中的一种或两种，用于促进硒前驱体在常温常压下溶解。
5.根据权利要求1所述的常温常压制备方法，其特征在于，在含有载体的悬浮液中加入表面活性剂或反电荷物质的体系中，加入硒前驱体和还原剂，将硒前驱体在还原剂作用下发生还原反应生成负二价硒的物质，再加入可溶性金属盐溶液，发生沉淀反应，一锅法获得金属硒化物负载于载体上的金属硒化物复合物。
6.根据权利要求5所述的常温常压制备方法，其特征在于，表面活性剂或反电荷物质选自CTAB、PDDA、PSS或阴离子电解质中的一种。
7.一种根据权利要求1-6之一所述的常温常压制备方法制得的金属硒化物汞吸附剂。
8.一种根据权利要求7所述的金属硒化物汞吸附剂的应用，其特征在于，应用方法包括：
（1）金属硒化物汞吸附剂以固定床形式布置于烟气道任何位置，或以喷射法直接喷入烟气道当中，实现工业烟气脱汞；
（2）将金属硒化物汞吸附剂投加到液体工业废物或产物中吸收富集液体中的汞，或直接析出固体工业废物中含有的汞，实现工业废物或产物脱汞；
（3）将金属硒化物汞吸附剂用于富集泄露、释放到空气中的汞，或直接从生活用品或废物中将汞析出并富集，实现生活用品或废物中汞的解毒与回收。
9.根据权利要求8所述的应用，其特征在于，应用温度介于室温到350℃之间。
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| CN113694909A (zh) * | 2021-08-31 | 2021-11-26 | 华中科技大学 | 一种汞回收装置 |
| CN114632499A (zh) * | 2022-03-18 | 2022-06-17 | 中南大学 | 一种用于应急处理汞污染水体的一体化成型材料及其制备方法和应用 |
| CN114920212A (zh) * | 2022-06-14 | 2022-08-19 | 蚌埠学院 | 一种硒化钼纳米材料的制备方法及其应用 |
| CN114974934A (zh) * | 2022-06-14 | 2022-08-30 | 蚌埠学院 | 一种硒化钴纳米材料的制备方法及其应用 |
| CN115025748A (zh) * | 2022-06-09 | 2022-09-09 | 上海电力大学 | 一种用于脱汞的新型硒化铜复合材料及其制备方法和应用 |
| CN115072673A (zh) * | 2022-06-14 | 2022-09-20 | 蚌埠学院 | 一种硒化镍纳米材料的制备方法及其应用 |
| CN115193389A (zh) * | 2022-06-29 | 2022-10-18 | 上海电力大学 | 一种具有片层结构的硒化物除汞吸附剂的制备方法及应用 |
| CN115245815A (zh) * | 2022-07-21 | 2022-10-28 | 中南大学 | 一种基于静电组装的吸附材料及其制备方法和应用 |
| CN115845789A (zh) * | 2022-09-13 | 2023-03-28 | 浙江慧科环保科技有限公司 | 一种硫沉积型铁基重金属吸附材料的制备方法 |
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| CN113694909A (zh) * | 2021-08-31 | 2021-11-26 | 华中科技大学 | 一种汞回收装置 |
| CN114632499A (zh) * | 2022-03-18 | 2022-06-17 | 中南大学 | 一种用于应急处理汞污染水体的一体化成型材料及其制备方法和应用 |
| CN114632499B (zh) * | 2022-03-18 | 2023-01-03 | 中南大学 | 一种用于应急处理汞污染水体的一体化成型材料及其制备方法和应用 |
| CN115025748A (zh) * | 2022-06-09 | 2022-09-09 | 上海电力大学 | 一种用于脱汞的新型硒化铜复合材料及其制备方法和应用 |
| CN115025748B (zh) * | 2022-06-09 | 2023-08-15 | 上海电力大学 | 一种用于脱汞的新型硒化铜复合材料及其制备方法和应用 |
| CN114920212A (zh) * | 2022-06-14 | 2022-08-19 | 蚌埠学院 | 一种硒化钼纳米材料的制备方法及其应用 |
| CN114974934A (zh) * | 2022-06-14 | 2022-08-30 | 蚌埠学院 | 一种硒化钴纳米材料的制备方法及其应用 |
| CN115072673A (zh) * | 2022-06-14 | 2022-09-20 | 蚌埠学院 | 一种硒化镍纳米材料的制备方法及其应用 |
| CN115193389A (zh) * | 2022-06-29 | 2022-10-18 | 上海电力大学 | 一种具有片层结构的硒化物除汞吸附剂的制备方法及应用 |
| CN115193389B (zh) * | 2022-06-29 | 2023-12-12 | 上海电力大学 | 一种具有片层结构的硒化物除汞吸附剂的制备方法及应用 |
| CN115245815A (zh) * | 2022-07-21 | 2022-10-28 | 中南大学 | 一种基于静电组装的吸附材料及其制备方法和应用 |
| CN115845789A (zh) * | 2022-09-13 | 2023-03-28 | 浙江慧科环保科技有限公司 | 一种硫沉积型铁基重金属吸附材料的制备方法 |
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