WO2016119717A1 - 一种生产高纯五氧化二钒粉体的***及方法 - Google Patents
一种生产高纯五氧化二钒粉体的***及方法 Download PDFInfo
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- WO2016119717A1 WO2016119717A1 PCT/CN2016/072518 CN2016072518W WO2016119717A1 WO 2016119717 A1 WO2016119717 A1 WO 2016119717A1 CN 2016072518 W CN2016072518 W CN 2016072518W WO 2016119717 A1 WO2016119717 A1 WO 2016119717A1
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- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 title claims abstract description 218
- 239000000843 powder Substances 0.000 title claims abstract description 63
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 19
- 239000007789 gas Substances 0.000 claims abstract description 238
- 238000005660 chlorination reaction Methods 0.000 claims abstract description 107
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 70
- 239000003546 flue gas Substances 0.000 claims abstract description 60
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 56
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 41
- 238000000034 method Methods 0.000 claims abstract description 31
- 239000000047 product Substances 0.000 claims abstract description 20
- 230000008569 process Effects 0.000 claims abstract description 17
- 238000005243 fluidization Methods 0.000 claims abstract description 15
- 239000006227 byproduct Substances 0.000 claims abstract description 5
- 230000007062 hydrolysis Effects 0.000 claims description 99
- 238000006460 hydrolysis reaction Methods 0.000 claims description 99
- ZHXZNKNQUHUIGN-UHFFFAOYSA-N chloro hypochlorite;vanadium Chemical compound [V].ClOCl ZHXZNKNQUHUIGN-UHFFFAOYSA-N 0.000 claims description 67
- 239000007788 liquid Substances 0.000 claims description 47
- CGFLRDJQEKNAGT-UHFFFAOYSA-N [V].O(Cl)Cl.[V] Chemical compound [V].O(Cl)Cl.[V] CGFLRDJQEKNAGT-UHFFFAOYSA-N 0.000 claims description 43
- 239000006096 absorbing agent Substances 0.000 claims description 43
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 37
- 229910052720 vanadium Inorganic materials 0.000 claims description 36
- 238000010992 reflux Methods 0.000 claims description 32
- 238000003860 storage Methods 0.000 claims description 32
- 238000001354 calcination Methods 0.000 claims description 27
- 239000002253 acid Substances 0.000 claims description 26
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 25
- 229910052710 silicon Inorganic materials 0.000 claims description 25
- 239000010703 silicon Substances 0.000 claims description 25
- 238000004821 distillation Methods 0.000 claims description 21
- 239000012535 impurity Substances 0.000 claims description 20
- 238000007789 sealing Methods 0.000 claims description 20
- 239000002893 slag Substances 0.000 claims description 18
- 238000009835 boiling Methods 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 13
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims description 13
- 239000000446 fuel Substances 0.000 claims description 12
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 11
- 238000002386 leaching Methods 0.000 claims description 11
- 238000000746 purification Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- 238000002485 combustion reaction Methods 0.000 claims description 7
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 6
- 239000012498 ultrapure water Substances 0.000 claims description 6
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 4
- 238000010521 absorption reaction Methods 0.000 claims description 4
- 239000000460 chlorine Substances 0.000 claims description 4
- 229910052801 chlorine Inorganic materials 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 4
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 4
- 239000000779 smoke Substances 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 3
- 239000002699 waste material Substances 0.000 claims description 3
- RCJVRSBWZCNNQT-UHFFFAOYSA-N dichloridooxygen Chemical compound ClOCl RCJVRSBWZCNNQT-UHFFFAOYSA-N 0.000 claims 1
- 239000002351 wastewater Substances 0.000 abstract description 6
- 230000008901 benefit Effects 0.000 abstract description 5
- 239000012808 vapor phase Substances 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- JBIQAPKSNFTACH-UHFFFAOYSA-K vanadium oxytrichloride Chemical compound Cl[V](Cl)(Cl)=O JBIQAPKSNFTACH-UHFFFAOYSA-K 0.000 abstract 2
- 239000007858 starting material Substances 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 37
- 239000000243 solution Substances 0.000 description 19
- 238000001556 precipitation Methods 0.000 description 14
- 239000002994 raw material Substances 0.000 description 13
- 150000003863 ammonium salts Chemical class 0.000 description 8
- 239000000126 substance Substances 0.000 description 6
- 239000003153 chemical reaction reagent Substances 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 4
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 3
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 3
- 230000033228 biological regulation Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910001510 metal chloride Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000012629 purifying agent Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- NGNBDVOYPDDBFK-UHFFFAOYSA-N 2-[2,4-di(pentan-2-yl)phenoxy]acetyl chloride Chemical compound CCCC(C)C1=CC=C(OCC(Cl)=O)C(C(C)CCC)=C1 NGNBDVOYPDDBFK-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 241000718537 Divana Species 0.000 description 1
- 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
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical group [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 206010024769 Local reaction Diseases 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229910021550 Vanadium Chloride Inorganic materials 0.000 description 1
- 229910021552 Vanadium(IV) chloride Inorganic materials 0.000 description 1
- GDQJRIJQPNLZBK-UHFFFAOYSA-A [V+5].O(Cl)Cl.[V+5].[Cl-].[V+5].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-] Chemical compound [V+5].O(Cl)Cl.[V+5].[Cl-].[V+5].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-] GDQJRIJQPNLZBK-UHFFFAOYSA-A 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- -1 ammonium ions Chemical class 0.000 description 1
- SKKMWRVAJNPLFY-UHFFFAOYSA-N azanylidynevanadium Chemical compound [V]#N SKKMWRVAJNPLFY-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- PNXOJQQRXBVKEX-UHFFFAOYSA-N iron vanadium Chemical compound [V].[Fe] PNXOJQQRXBVKEX-UHFFFAOYSA-N 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- RPESBQCJGHJMTK-UHFFFAOYSA-I pentachlorovanadium Chemical compound [Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[V+5] RPESBQCJGHJMTK-UHFFFAOYSA-I 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 229910001456 vanadium ion Inorganic materials 0.000 description 1
- JTJFQBNJBPPZRI-UHFFFAOYSA-J vanadium tetrachloride Chemical compound Cl[V](Cl)(Cl)Cl JTJFQBNJBPPZRI-UHFFFAOYSA-J 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/71—Feed mechanisms
- B01F35/717—Feed mechanisms characterised by the means for feeding the components to the mixer
- B01F35/7173—Feed mechanisms characterised by the means for feeding the components to the mixer using gravity, e.g. from a hopper
- B01F35/71731—Feed mechanisms characterised by the means for feeding the components to the mixer using gravity, e.g. from a hopper using a hopper
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/71—Feed mechanisms
- B01F35/717—Feed mechanisms characterised by the means for feeding the components to the mixer
- B01F35/71775—Feed mechanisms characterised by the means for feeding the components to the mixer using helical screws
-
- 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
- B01J6/00—Heat treatments such as Calcining; Fusing ; Pyrolysis
- B01J6/001—Calcining
- B01J6/004—Calcining using hot gas streams in which the material is moved
-
- 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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/24—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique
- B01J8/26—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique with two or more fluidised beds, e.g. reactor and regeneration installations
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L5/00—Gas handling apparatus
- B01L5/04—Gas washing apparatus, e.g. by bubbling
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/06—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents
- C01B3/061—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents by reaction of metal oxides with water
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/03—Preparation from chlorides
- C01B7/035—Preparation of hydrogen chloride from chlorides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
- C01G31/04—Halides
-
- 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
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00008—Controlling the process
- B01J2208/00017—Controlling the temperature
-
- 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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00164—Controlling or regulating processes controlling the flow
- B01J2219/00166—Controlling or regulating processes controlling the flow controlling the residence time inside the reactor vessel
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/129—Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines
Definitions
- the invention belongs to the field of chemical industry and material, and particularly relates to a system and a method for producing high-purity vanadium pentoxide powder.
- Vanadium pentoxide is one of the important industrial vanadium products, widely used in the production of alloy additives such as vanadium iron and vanadium nitride, as well as catalysts, colorants, and hard alloy additives. With the continuous development of new energy technologies, the battery industry is increasingly demanding high-purity vanadium pentoxide (purity of more than 3N5), including all-vanadium flow batteries (VRB) with good large-scale energy storage performance and vanadium for electric vehicles.
- the acid salt is a lithium ion battery or the like.
- the vanadium solution is usually obtained by leaching a vanadium solution or a vanadium-rich material (such as ammonium polyvanadate, ammonium metavanadate, industrial grade vanadium pentoxide, etc.), and is purified by chemical precipitation or (and) solvent extraction/ion.
- a vanadium-rich material such as ammonium polyvanadate, ammonium metavanadate, industrial grade vanadium pentoxide, etc.
- the impurity removal process parameters are closely related to the impurity content of the raw materials, so the adaptability to the raw materials is poor; the calcium salt, magnesium salt purifying agent or extractant used in the purification process, the acid-base reagent, and the ammonium salt for vanadium precipitation are also It is easy to introduce impurities.
- it is generally required to use an expensive reagent with a high purity, so that the cost is too high, the scale cannot be produced, and the purity of the product is difficult to be stabilized at 3N5 or more.
- the related institution also proposes to adopt the repeated precipitation method to purify and remove the vanadium solution, that is, to utilize the ammonium salt precipitation property of the vanadium-containing solution to selectively select vanadium.
- the raw material chlorination-rectification purification-subsequent treatment is a common preparation process for high-purity materials, such as high purity. Silicon (polysilicon), high purity silica, and the like.
- vanadium chloride vanadium oxychloride vanadium has a large difference from the boiling points of common impurities such as iron, calcium, magnesium, aluminum, sodium, potassium, etc., it is easy to obtain high purity vanadium oxychloride by rectification, and from high purity three High-purity vanadium pentoxide can be prepared by hydrolysis of vanadium oxychloride by hydrolysis and precipitation of ammonium salts, followed by calcination. Therefore, the preparation of high-purity vanadium pentoxide by the chlorination method has a great advantage in principle.
- the patent has the following deficiencies: (1) Similar to the aforementioned Iowa State University study, the patent actually only gives the principle of chlorination, lacking specific operational solutions, such as chlorination including both boiling chlorine And include molten salt chlorination, and molten salt chlorination and boiling chlorination are completely different chlorination methods; for example, for chlorination reactors, "rotary kiln, fluidized furnace, boiling furnace, shaft furnace, Reactors such as multi-hearth furnaces actually cover almost all common mainstream reactors in the metallurgical industry, but different reactors have very different requirements for raw materials. Shaft furnaces can only handle "coarse" particles larger than 8 mm.
- fine particles need to be treated with pellets and pre-sintering, while boiling chlorination is generally suitable for processing fine particles, so for a specific vanadium raw material, it cannot be directly applied to rotary kiln, fluidized furnace, boiling furnace, shaft furnace, and more.
- the reactor such as a crucible furnace; and the "fluidizer” and the “boiling furnace” are essentially the same, but the name is different; thus, it can be seen that the operation modes and conditions of these reactors are very different.
- vanadium raw material chlorination technology still has the following two problems: (1) vanadium raw material chlorination roasting is a strong exothermic process, and the heat generated by the chlorination reaction can satisfy the solid and gas. In addition to the preheating of the reaction material, it is still necessary to remove the heat through the furnace wall to stabilize the chlorination temperature. Therefore, the solid and the gas usually enter the reactor at a near room temperature, and the chlorination reaction generates heat to preheat before participating in the reaction.
- the local reaction efficiency of the chlorination reactor is too low; (2) due to the need to remove the heat generated by the chlorination reaction by a large amount of heat dissipation to maintain the operating temperature, the operating conditions and environmental climate changes are liable to cause chlorination temperature fluctuations, resulting in chlorination selection. Reduced sex and efficiency require a reasonable heat balance supply and temperature regulation. Therefore, it is necessary to provide a reasonable heat supply and temperature control to effectively increase the chlorination efficiency and obtain a stable chlorination temperature to ensure the selectivity of chlorination to effectively suppress the chlorination of impurities.
- the temperature regulation of the chlorination process the improvement of the direct yield of vanadium, the avoidance of ammonia nitrogen emission pollution and the reduction of production energy consumption are the key to improving the economical efficiency of the preparation of high-purity vanadium pentoxide by chlorination. .
- the present invention provides a system and method for producing high-purity vanadium pentoxide powder to ensure good selectivity of low-temperature chlorination, avoid generation of a large amount of polluted wastewater, and reduce production energy of high-purity vanadium pentoxide. Consumption and operating costs.
- the present invention adopts the following technical solutions:
- the system for producing high-purity vanadium pentoxide powder of the present invention comprising a feeding device 1, a low-temperature chlorination fluidized bed 2, a rectification purification device 3, a gas-phase hydrolysis fluidized bed 4, a calcination fluidized bed 5, Exhaust gas absorbing absorber 6, induced draft fan 7 and chimney 8;
- the feeding device 1 comprises an industrial grade vanadium pentoxide silo 1-1, an industrial grade vanadium pentoxide screw feeder 1-2, a carbon powder silo 1-3 and a carbon powder screw feeder 1-4;
- the low temperature chlorination fluidized bed 2 comprises a chlorination bed feeder 2-1, a chlorinated fluidized bed body 2-2, chlorination Bed cyclone separator 2-3, flue gas heat exchanger 2-4, flue gas condenser 2-5, chlorinated bed acid sealing tank 2-6 and chlorination bed spiral slag discharger 2-7;
- the rectification and purification device 3 includes a distillation still 3-1, a rectification column 3-2, a distillate condenser 3-3, a reflux liquid collection tank 3-4, a silicon-containing vanadium oxychloride vanadium storage tank 3-5, Distillation section acid sealing tank 3-6, high purity vanadium oxychloride vanadium condenser 3-7 and high purity vanadium oxychloride vanadium storage tank 3-8;
- the gas phase hydrolysis fluidized bed 4 comprises a hydrolysis bed air purifier 4-1, a hydrolysis bed gas heater 4-2, a vanadium oxychloride vanadium nozzle 4-3, a gas phase hydrolysis fluidized bed main body 4-4, a hydrochloric acid tail gas absorber 4-5 and hydrolysis bed discharger 4-6;
- the calcined fluidized bed 5 comprises a calcined bed air purifier 5-1, a calcined bed gas heater 5-2 and a calcined fluidized bed main body 5-3;
- the outlet of the bottom of the industrial grade vanadium pentoxide silo 1-1 is connected to the inlet of the industrial grade vanadium pentoxide screw feeder 1-2; the bottom of the carbon powder silo 1-3
- the discharge port is connected to the feed port of the carbon powder screw feeder 1-4; the discharge port of the industrial grade vanadium pentoxide screw feeder 1-2, the carbon powder screw feeder 1-
- the discharge ports of 4 are connected to the feed port of the chlorination bed feeder 2-1 through a pipe;
- the discharge port of the chlorination bed feeder 2-1 is connected to the inlet of the upper portion of the chlorinated fluidized bed main body 2-2 through a pipe; the bottom of the chlorination bed feeder 2-1
- the inlet port is connected to the nitrogen gas source manifold through a pipe;
- the chlorination bed cyclone separator 2-3 is disposed at the top center of the enlarged section of the chlorination fluidized bed main body 2-2;
- the chlorination bed cyclone separation The gas outlet at the top of the 2-3 is connected to the hot flue gas inlet of the flue gas heat exchanger 2-4 through a pipe; the cold flue gas outlet of the flue gas heat exchanger 2-4 passes through the pipe and the smoke a gas inlet of the gas condenser 2-5 is connected;
- a gas outlet of the flue gas condenser 2-5 is connected to a gas inlet of the chlorinated bed acid sealing tank 2-6 through a pipe;
- the chlorinated bed acid The gas outlet of the sealing tank 2-6 is connected
- the liquid outlet at the bottom of the flue gas condenser 2-5 is connected to the feed port of the rectification column 3-2 through a pipe; the vapor outlet of the distillation still 3-1 passes through the pipe and the rectification column 3 a vapor inlet of -2 is connected; a reflux port of the distillation pot 3-1 is connected to a liquid reflux outlet at the bottom of the rectification column 3-2 through a pipe; a gas outlet at the top of the rectification column 3-2 is passed The gas inlet of the pipe and the distillate condenser 3-3 Connecting; the liquid outlet of the distillate condenser 3-3 is connected to the liquid inlet of the reflux liquid collection tank 3-4 through a pipe; the reflux liquid outlet of the reflux liquid collection tank 3-4 is passed through a pipe and a The reflux liquid inlet at the top of the rectification column 3-2 is connected; the discharge port of the reflux liquid collection tank 3-4 is connected to the inlet of the silicon-containing vanadium oxychloride vanadium storage tank 3-5 through
- the air inlet of the hydrolysis bed air purifier 4-1 is connected to the compressed air manifold through a pipeline; the gas outlet of the hydrolysis bed air purifier 4-1 is respectively connected to the hydrolysis bed gas heater 4-2 through a pipeline a gas inlet of the gas inlet, the vanadium oxychloride nozzle 4-3, and an inlet of the bottom of the hydrolysis bed discharger 4-6; the combustion air inlet of the combustion bed gas heater 4-2 burner and The fuel inlets are respectively connected to the compressed air manifold and the fuel main pipe through pipes; the inlet ports of the hydrolysis bed gas heaters 4-2 are connected to the ultrapure water main pipe through pipes; the hydrolysis bed gas heaters 4-2 The air outlet is connected to the air inlet of the bottom of the gas phase hydrolysis fluidized bed main body 4-4 through a pipeline; the liquid outlet of the high purity vanadium oxychloride vanadium storage tank 3-8 passes through the pipeline and the vanadium oxychloride nozzle a vanadium oxychloride inlet of
- the intake port of the calcining bed air purifier 5-1 is connected to the compressed air manifold through a pipe; the gas outlet of the calcining bed air purifier 5-1 passes through the pipe and the calcined bed gas heater 5-2
- the intake ports are connected; the combustion air inlet and the fuel inlet of the burner of the calcining bed gas heater 5-2 are respectively connected to the compressed air main pipe and the fuel main pipe through a pipe; the calcining bed gas heater 5-2 is discharged
- the gas port is connected to the inlet of the bottom of the calcined fluidized bed main body 5-3 through a pipe; the gas outlet of the top of the calcined fluidized bed main body 5-3 passes through the pipe and the gas phase hydrolyzed fluidized bed main body 4-4
- the bottom air inlets are connected; the discharge port of the lower portion of the calcined fluidized bed main body 5-3 is connected to the high-purity vanadium pentoxide product silo through a pipeline;
- the gas outlet of the exhaust gas absorbing absorber 6 is connected to the gas inlet of the induced draft fan 7 through a pipe
- the gas outlet of the induced draft fan 7 is connected to the gas inlet at the bottom of the chimney 8 through a pipe.
- the method for producing high-purity vanadium pentoxide powder based on the above system of the present invention comprises the following steps:
- the industrial grade vanadium pentoxide powder in the industrial grade vanadium pentoxide silo 1-1 and the carbon powder of the carbon powder silo 1-3 are respectively passed through the industrial grade vanadium pentoxide spiral feeder 1 -2 and the carbon powder screw feeder 1-4 simultaneously enter the chlorination bed feeder 2-1 and then enter the chlorination fluidized bed main body 2-2; chlorine gas and nitrogen gas from the chlorine gas source main pipe
- the nitrogen of the gas source main pipe and the air of the compressed air main pipe are preheated by heat exchange between the flue gas heat exchanger 2-4 and the chlorinated flue gas, and then enter the chlorinated fluidized bed main body 2-2 to make vanadium pentoxide.
- the powder material such as carbon powder maintains fluidization and chemical reaction with it.
- the air causes some of the carbon powder to burn to provide heat to maintain the fluidized bed temperature.
- the chlorine gas and the carbon powder work together to chlorinate vanadium pentoxide and a small amount of impurities.
- the crude vanadium oxychloride vapor formed by the flue gas condenser 2-5 enters the rectification column 3-2 and the distillation still 3-1, and is subjected to a rectification operation to obtain a vanadium-rich scrap rich in high-boiling impurities.
- the high-purity vanadium oxychloride in the high-purity vanadium oxychloride vanadium storage tank 3-8 is introduced into the purified air from the hydrolysis bed air purifier 4-1 through the vanadium oxychloride vanadium nozzle 4-3.
- the gas phase hydrolysis fluidized bed main body 4-4 In the gas phase hydrolysis fluidized bed main body 4-4; after the ultrapure water and the purified air are preheated by the hydrolysis bed gas heater 4-2, together with the calcined flue gas from the calcined fluidized bed main body 5-3 Feeding into the gas phase hydrolysis fluidized bed main body 4-4 to maintain fluidization of the powder material, and hydrolyzing vanadium oxychloride to form vanadium pentoxide powder and hydrogen chloride-rich hydrolyzed flue gas; The divana powder is discharged into the calcined fluidized bed main body 5-3 through the hydrolysis bed discharger 4-6; the hydrolyzed flue gas is removed by the enlarged section of the gas phase hydrolysis fluidized bed main body 4-4 Thereafter, entering the hydrochloric acid exhaust gas absorber 4-5 for absorption treatment to form a by-product of the hydrochloric acid solution, and absorbing the exhaust gas into the tail gas eluting absorber 6 for treatment;
- the compressed air is sequentially preheated by the calcining bed air purifier 5-1 and the calcined bed gas heater 5-2, and then enters into the calcined fluidized bed main body 5-3 to maintain the fluidization of the vanadium pentoxide powder.
- the gas phase hydrolysis gasification bed main body 4-4 is used for the fluidized gas phase hydrolysis heating and fluidization of vanadium oxychloride; the exhaust gas leaching absorber 6 is absorbed by the alkali solution. The exhausted gas is sent to the chimney 8 via the induced draft fan 7 and then emptied.
- One of the features of the present invention is that in the chlorinated fluidized bed main body 2-2, the amount of carbon powder added in the low-temperature chlorination process is 10% to 20% of the mass of the industrial grade vanadium pentoxide powder, and chlorine
- the operating temperature is 300-500 ° C, and the average residence time of the powder is 30-80 min.
- the second feature of the present invention is that, in the rectification column 3-2, the number of trays in the rectification operation rectification section is 5 to 10, and the number of trays in the stripping section is 10 to 20; During the rectification operation, the reflux ratio (ie, the ratio of the top flow to the discharge amount) is 15 to 40.
- the third feature of the present invention is that: in the gas phase hydrolysis fluidized bed main body 4-4, vanadium pentoxide powder is directly prepared by vapor phase hydrolysis of high-purity vanadium oxychloride, the gas phase hydrolysis process is introduced into water vapor and three The mass ratio of vanadium oxychloride is 1.2 to 2.0, and the gas phase hydrolysis operation temperature is 160 to 600 °C.
- the fourth feature of the present invention is that, in the calcined fluidized bed main body 5-3, the vapor phase hydrolyzed vanadium pentoxide powder is further subjected to fluidization calcination treatment to obtain high-purity vanadium pentoxide powder, and the calcination
- the operating temperature is 400-620 ° C, and the average residence time of the powder is 30-240 min.
- the purity of the high-purity vanadium pentoxide powder produced by the invention is above 4N.
- the present invention has the following outstanding advantages:
- the chlorination gas is preheated while cooling the flue gas, so that the temperature distribution of the chlorination reactor is more uniform, and the low-temperature chlorination efficiency of the vanadium raw material is effectively improved;
- a part of the carbon powder is burned by appropriate amount of air to achieve heat balance supply and temperature regulation of the chlorination process, stabilize the chlorination operation temperature, improve the chlorination reaction efficiency and ensure good selectivity of chlorination, and avoid the formation of tetrachlorination.
- side reactions such as vanadium;
- the vanadium pentoxide powder produced by hydrolysis can be further calcined to obtain high-purity vanadium pentoxide powder.
- the body product, the generated hot flue gas is sent to the gas phase hydrolysis fluidized bed for heating and fluidization, improving heat utilization efficiency and production efficiency;
- the invention has the advantages of strong adaptability of raw materials, good selectivity of low-temperature chlorination, non-polluting wastewater discharge, low production energy consumption and low operating cost, stable product quality, and the like, and is suitable for large-scale high-purity vanadium pentoxide powder of 4N or more.
- Industrial production has good economic and social benefits.
- Figure 1 is a schematic view showing the configuration of a high purity vanadium pentoxide powder system of the present invention.
- FIG. 1 is a schematic view of a system and method for producing high purity vanadium pentoxide powder according to the present invention.
- the system for producing high-purity vanadium pentoxide powder used in the present embodiment includes a feeding device 1, a low-temperature chlorination fluidized bed 2, a rectification purification device 3, a vapor-phase hydrolyzed fluidized bed 4, and a calcination flow. a chemical bed 5, an exhaust gas absorbing absorber 6, an induced draft fan 7 and a chimney 8;
- the feeding device 1 comprises an industrial grade vanadium pentoxide silo 1-1, an industrial grade vanadium pentoxide spiral feeder 1-2, a carbon powder silo 1-3 and a carbon powder screw feeder 1-4;
- the low temperature chlorination fluidized bed 2 comprises a chlorination bed feeder 2-1, a chlorinated fluidized bed main body 2-2, a chlorinated bed cyclone 2-3, a flue gas heat exchanger 2-4, a flue gas condensation 2-5, chlorinated bed acid sealed tank 2-6 and chlorinated bed spiral slag remover 2-7;
- the rectification and purification device 3 includes a distillation still 3-1, a rectification column 3-2, a distillate condenser 3-3, a reflux liquid collection tank 3-4, a silicon-containing vanadium oxychloride vanadium storage tank 3-5, and a rectification Segment acid sealing tank 3-6, high purity vanadium oxychloride vanadium condenser 3-7 and high purity vanadium oxychloride vanadium storage tank 3-8;
- the gas phase hydrolysis fluidized bed 4 comprises a hydrolysis bed air purifier 4-1, a hydrolysis bed gas heater 4-2, a vanadium oxychloride vanadium nozzle 4-3, a gas phase hydrolysis fluidized bed main body 4-4, a hydrochloric acid tail gas absorber 4- 5 and hydrolysis bed discharger 4-6;
- the calcined fluidized bed 5 comprises a calcined bed air purifier 5-1, a calcined bed gas heater 5-2 and a calcined fluidized bed main body 5-3;
- the outlet of the bottom of the industrial grade vanadium pentoxide silo 1-1 is connected with the inlet of the industrial grade vanadium pentoxide screw feeder 1-2; the outlet of the carbon powder silo 1-3 and the charcoal
- the feed ports of the powder auger feeders 1-4 are connected; the discharge ports of the industrial grade vanadium pentoxide screw feeder 1-2, the discharge ports of the carbon powder screw feeders 1-4 are all fed with the chlorination bed
- the feed ports of the 2-1 are connected by pipes;
- the discharge port of the chlorination bed feeder 2-1 is connected to the inlet of the upper part of the chlorination fluidized bed main body 2-2 through a pipe; the inlet of the bottom of the chlorination bed feeder 2-1 is piped and The nitrogen gas source manifold is connected; the chlorination bed cyclone separator 2-3 is disposed at the top center of the enlarged section of the chlorination fluidized bed main body 2-2; the gas outlet of the chlorinated bed cyclone separator 2-3 passes through the pipeline and the smoke
- the hot flue gas inlets of the gas heat exchangers 2-4 are connected; the cold flue gas outlets of the flue gas heat exchangers 2-4 are connected to the gas inlets of the flue gas condensers 2-5 through pipes; the flue gas condensers 2 -
- the gas outlet of 5 is connected to the gas inlet of the chlorinated bed acid sealing tank 2-6 through a pipe; the chlorinated bed acid sealing tank The gas outlet of 2-6 is connected to the gas inlet of the exhaust gas leaching absorb
- the liquid outlet at the bottom of the flue gas condenser 2-5 is connected to the feed port of the rectification column 3-2 through a pipe; the vapor outlet of the distillation still 3-1 is connected to the vapor inlet of the rectification column 3-2 through a pipe; The reflux port of the still 3-1 is connected to the liquid reflux outlet at the bottom of the rectification column 3-2 through a pipe; the gas outlet at the top of the rectification column 3-2 is passed through the gas inlet of the distillate condenser 3-3 through the pipe.
- the liquid outlet of the distillate condenser 3-3 is connected to the liquid inlet of the reflux liquid collection tank 3-4 through a pipe; the reflux liquid outlet of the reflux liquid collection tank 3-4 is passed through the pipe and the top of the rectification column 3-2
- the reflux liquid inlet is connected;
- the discharge port of the reflux liquid collection tank 3-4 is connected to the inlet of the silicon-containing vanadium oxychloride vanadium storage tank 3-5 through the pipeline;
- the silicon-containing vanadium oxychloride vanadium storage tank 3-5 is lacking
- the gas outlet is connected to the gas inlet of the acid sealing tank 3-6 of the rectifying section through a pipeline;
- the gas outlet of the rectifying acid sealing tank 3-6 is connected to the gas inlet of the exhaust gas eluting absorber 6 through a pipeline;
- the rectification tower 3 -2 of the distillate outlet is connected to the gas inlet of the high purity vanadium oxychloride condenser 3-7 through a pipe;
- the air inlet of the hydrolysis bed air purifier 4-1 is connected to the compressed air main pipe through a pipeline; the air outlet of the hydrolysis bed air purifier 4-1 is respectively connected to the air inlet of the hydrolysis bed gas heater 4-2 through the pipeline, and three The gas inlet of the vanadium oxychloride nozzle 4-3 and the inlet of the bottom of the hydrolysis bed discharger 4-6 are connected; the combustion air inlet and the fuel inlet of the hydrolysis bed gas heater 4-2 are respectively passed through the pipeline and the compressed air
- the main pipe is connected with the fuel main pipe; the gas inlet of the hydrolysis bed gas heater 4-2 is connected to the ultrapure water main pipe through a pipe; the gas outlet of the hydrolysis bed gas heater 4-2 passes through the pipe and the gas phase hydrolysis fluidized bed main body 4
- the inlet ports at the bottom of the -4 are connected; the liquid outlet of the high purity vanadium oxychloride vanadium storage tank 3-8 is connected to the vanadium oxychloride inlet of the vana
- the inlet of the calcining bed air purifier 5-1 is connected to the compressed air manifold through a pipeline; the outlet of the calcining bed air purifier 5-1 is connected to the inlet of the calcined bed gas heater 5-2 through a pipe;
- the combustion air inlet and the fuel inlet of the burner of the calcining bed gas heater 5-2 are respectively connected to the compressed air main pipe and the fuel main pipe through a pipe;
- the gas outlet of the calcining bed gas heater 5-2 passes through the pipe and the calcined fluidized bed main body 5
- the inlet ports at the bottom of the -3 are connected; the gas outlet at the top of the calcined fluidized bed main body 5-3 is connected to the inlet of the bottom of the gas phase hydrolysis fluidized bed main body 4-4 through a pipe;
- the body of the fluidized bed is calcined 5-3
- the lower discharge opening is connected to the high-purity vanadium pentoxide product silo through a pipeline;
- the gas outlet of the exhaust gas eluting absorber 6 is connected to the gas inlet of the draft fan 7 through a pipe; the gas outlet of the draft fan 7 is connected to the gas inlet at the bottom of the chimney 8 through a pipe.
- the high-purity vanadium pentoxide powder is produced by using the above system, and the specific method comprises: industrial grade vanadium pentoxide powder and carbon powder silo 1-3 in the industrial grade vanadium pentoxide silo 1-1
- the carbon powder is respectively mixed into the chlorinated fluidized bed main body 2-2 by the industrial grade vanadium pentoxide screw feeder 1-2 and the carbon powder screw feeder 1-4 simultaneously entering the chlorination bed feeder 2-1;
- the chlorine gas from the chlorine gas source main pipe, the nitrogen gas of the nitrogen gas source main pipe and the air of the compressed air main pipe are preheated by the flue gas heat exchanger 2-4 and the chlorinated flue gas, and then enter the chlorinated fluidized bed main body 2-2.
- the powder material such as vanadium pentoxide or carbon powder is maintained fluidized and chemically reacted with it.
- the air causes some of the carbon powder to burn to provide heat to maintain the fluidized bed temperature.
- the chlorine gas and the carbon powder work together to make vanadium pentoxide and A small amount of impurities are chlorinated to form a chlorinated residue and a chlorinated flue gas rich in vanadium oxychloride;
- the chlorinated residue is sequentially passed through a slag discharge port of the chlorination fluidized bed main body 2-2 and a chlorination bed spiral slag discharge device 2-7 discharge;
- the chlorinated flue gas is removed by the chlorination bed cyclone 2-3 and falls back to the chlorinated fluidized bed main body 2-2
- the crude vanadium oxychloride vapor formed by the flue gas condenser 2-5 sequentially enters the rectification column 3-2 and the distillation still 3-1 to carry out a rectification operation to obtain a vanadium-rich scrap rich in high-boiling impurities and rich in low boiling point.
- the high-purity vanadium oxychloride vanadium in the high-purity vanadium oxychloride vanadium storage tank 3-8 is loaded into the gas-phase hydrolyzed fluidized bed by the purified air from the hydrolysis bed air purifier 4-1 through the vanadium oxychloride vanadium nozzle 4-3.
- vanadium oxychloride hydrolyzed to form vanadium pentoxide powder and hydrogen chloride-rich hydrolyzed flue gas
- the vanadium pentoxide powder is discharged to the calcined fluidized bed main body through the hydrolysis bed discharger 4-6.
- the hydrolyzed flue gas is removed from the dust by the expanded section of the gas-phase hydrolyzed fluidized bed main body 4-4, and then enters the hydrochloric acid exhaust gas absorber 4-5 for absorption treatment to form a by-product of the hydrochloric acid solution, and the exhaust gas is taken into the exhaust gas leaching absorber 6 for carrying out deal with;
- the compressed air is sequentially purified by the calcining bed air purifier 5-1, and the calcined bed gas heater 5-2 is preheated and then enters the calcined fluidized bed main body 5-3 to maintain the fluidization of the vanadium pentoxide powder and make it Remove water and trace volatile impurities to obtain high-purity vanadium pentoxide powder and calcined flue gas; high-purity vanadium pentoxide product is discharged and sent to high-purity product silo; calcined flue gas is removed by expanding section After entering the gas phase hydrolysis fluidized bed main body 4-4 for the fluidized gas phase hydrolysis of vanadium oxychloride to supply heat and fluidization; the gas discharged from the exhaust gas elution absorber 6 after being absorbed by the alkali solution is sent by the induced draft fan 7 Empty into the chimney 8 after evacuation.
- the industrial grade vanadium pentoxide is used as a raw material, and the chemical composition thereof is shown in Table 1.
- the treatment amount is 80 kg/h, which is obtained by low temperature chlorination, vanadium oxychloride rectification, gas phase hydrolysis and calcination. High purity vanadium pentoxide product.
- the amount of carbon powder added in the low-temperature chlorination process is 10% of the quality of the industrial grade vanadium pentoxide powder, the chlorination operation temperature is 500 ° C, and the average residence time of the powder is 30 min;
- the number of trays in the rectification section is 5, the number of trays in the stripping section is 10, and the reflux ratio in the rectification operation is 40;
- the gas phase hydrolysis fluidized bed main body 4-4 The gas phase hydrolysis process has a mass ratio of water vapor to vanadium oxychloride of 1.2, a gas phase hydrolysis operation temperature of 600 ° C; in the calcined fluidized bed main body 5-3, the calcination operation temperature is 400 ° C, and the average residence time of the powder is 240 min.
- the direct yield of vanadium is 83%, and the purity of the high-purity vanadium pentoxide product is 99.995wt% (4N5)
- the amount of carbon powder added in the low-temperature chlorination process is 20% of the quality of the industrial grade vanadium pentoxide powder, the chlorination operation temperature is 300 ° C, and the average residence time of the powder is 80 min;
- the rectification column 3-2 the number of trays in the rectification section of the rectification section is 10, the number of trays in the stripping section is 20, and the reflux ratio of the rectification operation is 15;
- the gas phase hydrolysis process has a mass ratio of water vapor to vanadium oxychloride of 2.0, a gas phase hydrolysis operation temperature of 160 ° C; in the calcined fluidized bed main body 5-3, the calcination operation temperature is 620 ° C, and the average residence time of the powder is 30 min.
- the direct yield of vanadium is 85%, and the purity of the high-purity vanadium pentoxide product is 99.999
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Abstract
Description
V2O5 | Si | Ca | Al | Ti | Fe | Mn | Na | K | S |
98.8 | 0.0150 | 0.0275 | 0.0099 | 0.0260 | 0.0971 | 0.0293 | 0.1385 | 0.0714 | 0.1274 |
Claims (8)
- 一种生产高纯五氧化二钒粉体的***,其特征在于,所述***包括加料装置(1)、低温氯化流化床(2)、精馏提纯装置(3)、气相水解流化床(4)、煅烧流化床(5)、尾气淋洗吸收器(6)、引风机(7)和烟囱(8);所述加料装置(1)包括工业级五氧化二钒料仓(1-1)、工业级五氧化二钒螺旋加料器(1-2)、炭粉料仓(1-3)和炭粉螺旋加料器(1-4);所述低温氯化流化床(2)包括氯化床进料器(2-1)、氯化流化床主体(2-2)、氯化床旋风分离器(2-3)、烟气换热器(2-4)、烟气冷凝器(2-5)、氯化床酸封罐(2-6)和氯化床螺旋排渣器(2-7);所述精馏提纯装置(3)包括蒸馏釜(3-1)、精馏塔(3-2)、馏出物冷凝器(3-3)、回流液收集罐(3-4)、含硅三氯氧钒储罐(3-5)、精馏段酸封罐(3-6)、高纯三氯氧钒冷凝器(3-7)和高纯三氯氧钒储罐(3-8);所述气相水解流化床(4)包括水解床空气净化器(4-1)、水解床气体加热器(4-2)、三氯氧钒喷嘴(4-3)、气相水解流化床主体(4-4)、盐酸尾气吸收器(4-5)和水解床排料器(4-6);所述煅烧流化床(5)包括煅烧床空气净化器(5-1)、煅烧床气体加热器(5-2)和煅烧流化床主体(5-3);所述工业级五氧化二钒料仓(1-1)底部的出料口与所述工业级五氧化二钒螺旋加料器(1-2)的进料口相连接;所述炭粉料仓(1-3)底部的出料口与所述炭粉螺旋加料器(1-4)的进料口相连接;所述工业级五氧化二钒螺旋加料器(1-2)的出料口和所述炭粉螺旋加料器(1-4)的出料口均与所述氯化床进料器(2-1)的进料口通过管道相连接;所述氯化床进料器(2-1)的排料口与所述氯化流化床主体(2-2)上部的进料口通过管道相连接;所述氯化床进料器(2-1)底部的进气口通过管道与氮气气源总管相连接;所述氯化床旋风分离器(2-3)设置于所述氯化流化床主体(2-2)的扩大段顶部中心;所述氯化床旋风分离器(2-3)顶部的出气口通过管道与所述烟气换热器(2-4)的热烟气入口相连接;所述烟气换热器(2-4)的冷烟气出口通过管道与所述烟气冷凝器(2-5)的气体入口相连接;所述烟气冷凝器(2-5)的气体出口通过管道与所述氯化床酸封罐(2-6)的气体入口相连接;所述氯化床酸封罐(2-6)的气体出口通过管道与所述尾气淋洗吸收器(6)的气体入口相连接;所述氯化流化床主体(2-2)下部的排渣口与所述氯化床螺旋排渣器(2-7) 的进料口通过管道相连接;所述氯化流化床主体(2-2)底部的进气口通过管道与所述烟气换热器(2-4)的热气体出口相连接;所述烟气换热器(2-4)的冷气体入口通过管道分别与氯气气源总管、氮气气源总管及压缩空气总管相连接;所述烟气冷凝器(2-5)底部的液体出口通过管道与所述精馏塔(3-2)的进料口相连接;所述蒸馏釜(3-1)的蒸气出口通过管道与所述精馏塔(3-2)的蒸气入口相连接;所述蒸馏釜(3-1)的回流口通过管道与所述精馏塔(3-2)底部的液体回流出口相连接;所述精馏塔(3-2)顶部的气体出口通过管道与所述馏出物冷凝器(3-3)的气体入口相连接;所述馏出物冷凝器(3-3)的液体出口通过管道与所述回流液收集罐(3-4)的液体入口相连接;所述回流液收集罐(3-4)的回流液体出口通过管道与所述精馏塔(3-2)顶部的回流液体入口相连接;所述回流液收集罐(3-4)的排料口与所述含硅三氯氧钒储罐(3-5)的入口通过管道相连接;所述含硅三氯氧钒储罐(3-5)的乏气出口通过管道与所述精馏段酸封罐(3-6)的气体入口相连接;所述精馏酸封罐(3-6)的气体出口通过管道与所述尾气淋洗吸收器(6)的气体入口相连接;所述精馏塔(3-2)的精馏物出口通过管道与所述高纯三氯氧钒冷凝器(3-7)的气体入口相连接;所述高纯三氯氧钒冷凝器(3-7)的液体出口与所述高纯三氯氧钒储罐(3-8)的液体入口通过管道相连接;所述蒸馏釜(3-1)底部设置了底流出口;所述水解床空气净化器(4-1)的进气口与压缩空气总管通过管道相连接;所述水解床空气净化器(4-1)的出气口通过管道分别与所述水解床气体加热器(4-2)的进气口、三氯氧钒喷嘴(4-3)的气体入口及水解床排料器(4-6)底部的进气口相连接;所述水解床气体加热器(4-2)燃烧嘴的助燃风入口和燃料入口分别通过管道与压缩空气总管和燃料总管相连接;所述水解床气体加热器(4-2)的进气口通过管道与超纯水总管相连接;所述水解床气体加热器(4-2)的出气口通过管道与所述气相水解流化床主体(4-4)底部的进气口相连接;所述高纯三氯氧钒储罐(3-8)的液体出口通过管道与所述三氯氧钒喷嘴(4-3)的三氯氧钒入口相连接;所述气相水解流化床主体(4-4)扩大段顶部的气体出口通过管道与所述盐酸尾气吸收器(4-5)的气体入口相连接;所述盐酸尾气吸收器(4-5)底部设置了盐酸溶液出口;所述盐酸尾气吸收器(4-5)的气体出口通过管道与所述尾气淋洗吸收器(6)的气体入口相连接;所述气相水解流化床主体(4-4)上部的出料口通过管道与所述水解床排料器(4-6)的进料口相连接;所述水解床排料器(4-6)的排料口通过管道与所述煅烧流化床主体(5-3)上部的进料口 相连接;所述煅烧床空气净化器(5-1)的进气口与压缩空气总管通过管道相连接;所述煅烧床空气净化器(5-1)的出气口通过管道与所述煅烧床气体加热器(5-2)的进气口相连接;所述煅烧床气体加热器(5-2)燃烧嘴的助燃风入口和燃料入口分别通过管道与压缩空气总管和燃料总管相连接;所述煅烧床气体加热器(5-2)的出气口通过管道与所述煅烧流化床主体(5-3)底部的进气口相连接;所述煅烧流化床主体(5-3)顶部的出气口通过管道与所述气相水解流化床主体(4-4)底部的进气口相连接;所述煅烧流化床主体(5-3)下部的排料口通过管道与高纯五氧化二钒产品料仓相连接;所述尾气淋洗吸收器(6)的气体出口通过管道与所述引风机(7)的气体入口相连接;所述引风机(7)的气体出口通过管道与所述烟囱(8)底部的气体入口相连接。
- 一种基于权利要求1所述***的生产高纯五氧化二钒粉体的方法,包括以下步骤:所述工业级五氧化二钒料仓(1-1)中的工业级五氧化二钒粉料和所述炭粉料仓(1-3)的炭粉分别经所述工业级五氧化二钒螺旋加料器(1-2)和所述炭粉螺旋加料器(1-4)同时进入所述氯化床进料器(2-1)混合后进入所述氯化流化床主体(2-2);来自氯气气源总管的氯气、氮气气源总管的氮气及压缩空气总管的空气经所述烟气换热器(2-4)与氯化烟气换热预热后进入所述氯化流化床主体(2-2)中使五氧化二钒和炭粉维持流态化并与之发生化学反应,空气使部分炭粉发生燃烧提供热量维持流化床温度,氯气与炭粉共同作用使五氧化二钒和少量杂质发生氯化,形成氯化残渣和富含三氯氧钒的氯化烟气;氯化残渣依次经所述氯化流化床主体(2-2)下部的排渣口和氯化床螺旋排渣器(2-7)排出;氯化烟气经所述氯化床旋风分离器(2-3)将粉尘脱除并落回氯化流化床主体(2-2)后,再经所述烟气换热器(2-4)预冷却并进入烟气冷凝器(2-5)中使其中的三氯氧钒冷凝形成粗三氯氧钒液体,剩余尾气经所述氯化床酸封罐(2-6)后进入所述尾气淋洗吸收器(6)中;所述烟气冷凝器(2-5)形成的粗三氯氧钒液体依次进入所述精馏塔(3-2)和所述蒸馏釜(3-1)后进行精馏操作,得到富含高沸点杂质的富钒废料、富含低沸点杂质的含硅三氯氧钒蒸气和高纯三氯氧钒蒸气;含硅三氯氧钒蒸气经所述馏出物冷凝器(3-3)冷凝至液体后,部分经回流液收集罐(3-4)回流至所述精 馏塔(3-2),其余部分进入所述含硅三氯氧钒储罐(3-5)中;含硅三氯氧钒储罐(3-5)中产生的乏气经所述精馏段酸封罐(3-6)后送往所述尾气淋洗吸收器(6)中;高纯三氯氧钒蒸气经所述高纯三氯氧钒冷凝器(3-7)冷凝至液体后进入所述高纯三氯氧钒储罐(3-8)中;所述高纯三氯氧钒储罐(3-8)中的高纯三氯氧钒经所述三氯氧钒喷嘴(4-3),由来自水解床空气净化器(4-1)的净化空气气载进入所述气相水解流化床主体(4-4)中;超纯水和净化空气经所述水解床气体加热器(4-2)预热后,与来自所述煅烧流化床主体(5-3)的煅烧烟气一起送入所述气相水解流化床主体(4-4)中使粉体物料维持流态化、并使三氯氧钒发生水解,形成五氧化二钒粉体和富含氯化氢的水解烟气;五氧化二钒粉体经所述水解床排料器(4-6)排出送入所述煅烧流化床主体(5-3)中;水解烟气经所述气相水解流化床主体(4-4)扩大段脱除粉尘后,进入所述盐酸尾气吸收器(4-5)进行吸收处理形成盐酸溶液副产品,吸收尾气进入所述尾气淋洗吸收器(6)进行处理;压缩空气依次经所述煅烧床空气净化器(5-1)净化和所述煅烧床气体加热器(5-2)预热后进入所述煅烧流化床主体(5-3)内使五氧化二钒粉体维持流态化,并使之脱除水分和微量的挥发性杂质,得到高纯五氧化二钒粉体和煅烧烟气;高纯五氧化二钒产品排出并送入高纯产品料仓;煅烧烟气经扩大段脱除粉尘后进入所述气相水解流化床主体(4-4)中用于三氯氧钒的流态化气相水解供热和流化;所述尾气淋洗吸收器(6)经碱溶液吸收处理后排出的气体经所述引风机(7)送入所述烟囱(8)后排空。
- 根据权利要求2所述的生产高纯五氧化二钒粉体的方法,其特征在于,在所述氯化流化床主体(2-2)内,所述氯化过程炭粉添加量为工业级五氧化二钒粉料质量的10%~20%。
- 根据权利要求2所述的生产高纯五氧化二钒粉体的方法,其特征在于,在所述氯化流化床主体(2-2)内,所述氯化操作温度为300~500℃,粉料的平均停留时间为30~80min。
- 根据权利要求2所述的生产高纯五氧化二钒粉体的方法,其特征在于,在所述精馏塔(3-2)内,所述精馏操作精馏段的塔板数为5~10块,提馏段的塔板数为10~20块。
- 根据权利要求2所述的生产高纯五氧化二钒粉体的方法,其特征在于, 所述精馏操作的回流比为15~40。
- 根据权利要求2所述的生产高纯五氧化二钒粉体的方法,其特征在于,在所述气相水解流化床主体(4-4)内,通过高纯三氯氧钒气相水解直接制备五氧化二钒粉体,所述气相水解过程通入水蒸气与三氯氧钒的质量比为1.2~2.0,气相水解操作温度为160~600℃。
- 根据权利要求2所述的生产高纯五氧化二钒粉体的方法,其特征在于,在所述煅烧流化床主体(5-3)内,气相水解的五氧化二钒粉体进一步进行流态化煅烧处理得到高纯五氧化二钒粉体,所述煅烧的操作温度为400~620℃,粉料的平均停留时间为30~240min。
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US20180009675A1 (en) | 2018-01-11 |
JP6404498B2 (ja) | 2018-10-10 |
RU2670866C1 (ru) | 2018-10-25 |
RU2670866C9 (ru) | 2018-12-11 |
ZA201704630B (en) | 2019-06-26 |
US10099939B2 (en) | 2018-10-16 |
BR112017015803A2 (zh) | 2018-06-19 |
AU2016212451A1 (en) | 2017-08-31 |
CA2973499A1 (en) | 2016-08-04 |
CA2973499C (en) | 2019-12-31 |
EP3252012A4 (en) | 2018-01-03 |
NZ733919A (en) | 2018-08-31 |
EP3252012B1 (en) | 2018-09-26 |
CN105984897B (zh) | 2017-05-17 |
PH12017550058A1 (en) | 2018-02-05 |
AU2016212451B2 (en) | 2018-01-18 |
JP2018509371A (ja) | 2018-04-05 |
CN105984897A (zh) | 2016-10-05 |
EP3252012A1 (en) | 2017-12-06 |
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