WO2016119716A1 - 一种制备高纯五氧化二钒粉体的系统及方法 - Google Patents
一种制备高纯五氧化二钒粉体的系统及方法 Download PDFInfo
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- WO2016119716A1 WO2016119716A1 PCT/CN2016/072517 CN2016072517W WO2016119716A1 WO 2016119716 A1 WO2016119716 A1 WO 2016119716A1 CN 2016072517 W CN2016072517 W CN 2016072517W WO 2016119716 A1 WO2016119716 A1 WO 2016119716A1
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- gas
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- vanadium
- ammonium salt
- chlorination
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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 182
- 239000000843 powder Substances 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 37
- 239000007789 gas Substances 0.000 claims abstract description 141
- 238000005660 chlorination reaction Methods 0.000 claims abstract description 109
- 150000003863 ammonium salts Chemical class 0.000 claims abstract description 99
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 59
- 239000003546 flue gas Substances 0.000 claims abstract description 51
- 238000001556 precipitation Methods 0.000 claims abstract description 50
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 41
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000001354 calcination Methods 0.000 claims abstract description 24
- 230000008569 process Effects 0.000 claims abstract description 14
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims description 55
- CGFLRDJQEKNAGT-UHFFFAOYSA-N [V].O(Cl)Cl.[V] Chemical compound [V].O(Cl)Cl.[V] CGFLRDJQEKNAGT-UHFFFAOYSA-N 0.000 claims description 41
- ZHXZNKNQUHUIGN-UHFFFAOYSA-N chloro hypochlorite;vanadium Chemical compound [V].ClOCl ZHXZNKNQUHUIGN-UHFFFAOYSA-N 0.000 claims description 38
- 229910052720 vanadium Inorganic materials 0.000 claims description 35
- 238000003860 storage Methods 0.000 claims description 34
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 34
- 238000010992 reflux Methods 0.000 claims description 32
- 238000005406 washing Methods 0.000 claims description 31
- 239000006096 absorbing agent Substances 0.000 claims description 28
- 239000002253 acid Substances 0.000 claims description 26
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 23
- 229910052710 silicon Inorganic materials 0.000 claims description 23
- 239000010703 silicon Substances 0.000 claims description 23
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 22
- 238000006243 chemical reaction Methods 0.000 claims description 22
- 238000004821 distillation Methods 0.000 claims description 21
- 238000007789 sealing Methods 0.000 claims description 21
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 19
- 239000002893 slag Substances 0.000 claims description 18
- 239000012535 impurity Substances 0.000 claims description 17
- 238000002386 leaching Methods 0.000 claims description 15
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims description 14
- 238000009835 boiling Methods 0.000 claims description 14
- 239000000047 product Substances 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 11
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 9
- 239000000446 fuel Substances 0.000 claims description 9
- 239000002244 precipitate Substances 0.000 claims description 9
- 238000000746 purification Methods 0.000 claims description 9
- 239000002002 slurry Substances 0.000 claims description 9
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000002485 combustion reaction Methods 0.000 claims description 6
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 6
- 239000012498 ultrapure water Substances 0.000 claims description 6
- 238000004065 wastewater treatment Methods 0.000 claims description 6
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 5
- 239000000460 chlorine Substances 0.000 claims description 5
- 229910052801 chlorine Inorganic materials 0.000 claims description 5
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 claims description 4
- 229910001935 vanadium oxide Inorganic materials 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 3
- 235000019270 ammonium chloride Nutrition 0.000 claims description 3
- 239000000428 dust Substances 0.000 claims description 3
- 239000011343 solid material Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 239000011268 mixed slurry Substances 0.000 claims description 2
- 239000002699 waste material Substances 0.000 claims description 2
- RCJVRSBWZCNNQT-UHFFFAOYSA-N dichloridooxygen Chemical compound ClOCl RCJVRSBWZCNNQT-UHFFFAOYSA-N 0.000 claims 1
- 229910021529 ammonia Inorganic materials 0.000 abstract description 6
- 238000005243 fluidization Methods 0.000 abstract description 6
- 230000008901 benefit Effects 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 4
- JBIQAPKSNFTACH-UHFFFAOYSA-K vanadium oxytrichloride Chemical compound Cl[V](Cl)(Cl)=O JBIQAPKSNFTACH-UHFFFAOYSA-K 0.000 abstract 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 239000007858 starting material Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 15
- 239000002994 raw material Substances 0.000 description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 5
- 239000003153 chemical reaction reagent Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 239000000779 smoke Substances 0.000 description 5
- 238000000354 decomposition reaction Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000033228 biological regulation Effects 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 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
- 239000003054 catalyst Substances 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000007599 discharging Methods 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
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 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
- 241000208125 Nicotiana Species 0.000 description 1
- 235000002637 Nicotiana tabacum Nutrition 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
- -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
- 238000006555 catalytic reaction Methods 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
- 230000007812 deficiency Effects 0.000 description 1
- 238000009826 distribution 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
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 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
- 238000004826 seaming Methods 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
- 125000005287 vanadyl group Chemical group 0.000 description 1
- 239000002351 wastewater Substances 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
- B01D3/02—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in boilers or stills
-
- 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
-
- 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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/06—Solidifying liquids
-
- 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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/245—Stationary reactors without moving elements inside placed in series
-
- 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
-
- 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
- B01J8/005—Separating solid material from the gas/liquid stream
- B01J8/0055—Separating solid material from the gas/liquid stream using cyclones
-
- 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
- B01J8/1818—Feeding of the fluidising gas
- B01J8/1827—Feeding of the fluidising gas the fluidising gas being a reactant
-
- 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
- B01J8/1836—Heating and cooling the reactor
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
- C01G31/003—Preparation involving a liquid-liquid extraction, an adsorption or an ion-exchange
-
- 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
- B01J2208/00743—Feeding or discharging of solids
- B01J2208/00752—Feeding
-
- 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
- B01J2208/00743—Feeding or discharging of solids
- B01J2208/00761—Discharging
-
- 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
- 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 preparing 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 regulation of the chlorination process the improvement of the direct yield of vanadium, the reduction of production energy consumption, and further avoiding the ammonia-containing tail gas pollution caused by the ammonium salt calcination can effectively improve the preparation of high purity five by the chlorination process. Vanadium oxide technology economy.
- the present invention provides a system and method for preparing high-purity vanadium pentoxide powder to ensure good selectivity of low-temperature chlorination, improve ammonium salt precipitation calcination decomposition efficiency, avoid ammonia-containing tail gas pollution, and reduce high Production energy consumption and operating costs of pure vanadium pentoxide.
- the present invention adopts the following technical solutions:
- the system for preparing high-purity vanadium pentoxide powder of the invention comprises the feeding device 1, the low-temperature chlorination fluidized bed 2, the rectification and purification device 3, the ammonium salt precipitation device 4, the ammonium salt feeding device 5, and the calcination Fluidized bed 6, exhaust gas leaching absorber 7, induced draft fan 8 and chimney 9;
- 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 main body 2-2, a chlorinated bed cyclone 2-3, a flue gas heat exchanger 2-4, a smoke Gas condenser 2-5, chlorinated bed acid sealed tank 2-6 and chlorination 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, 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 ammonium salt precipitation device 4 includes an ammonium salt precipitation reaction tank 4-1 and a washing filter 4-2;
- the ammonium salt feeding device 5 comprises an ammonium salt silo 5-1 and an ammonium salt screw feeder 5-2;
- the calcined fluidized bed 6 includes an air purifier 6-1, a gas heater 6-2, a calcined bed feeder 6-3, a calcined fluidized bed main body 6-4, a calcined bed cyclone separator 6-5, and ammonia.
- 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 a conduit is connected to the gas inlet of the distillate condenser 3-3; the liquid outlet of the distillate condenser 3-3 is connected to the liquid inlet of the reflux collection tank 3-4 via a conduit; The reflux liquid outlet of the reflux liquid collection tank 3-4 passes through the pipeline and the rectification column 3-2 a top reflux liquid inlet is connected; a discharge port of the reflux liquid collection tank 3-4 is connected to an inlet of the silicon-containing vanadium oxychloride vanadium storage tank 3-5 through a pipe; the silicon
- the ammonia aqueous solution inlet of the ammonium salt precipitation reaction tank 4-1 is connected to the purified ammonia water main pipe and the ammonia water outlet at the bottom of the ammonia gas condenser 6-6 through a pipe; the ammonium salt precipitates the chloride inlet of the reaction tank 4-1 Connected to the liquid outlet of the high-purity vanadium oxychloride vanadium storage tank 3-8 through a pipe; the slurry outlet of the ammonium salt precipitation reaction tank 4-1 passes through the pipeline and the slurry of the washing filter 4-2 The inlet is connected; the clean water inlet of the washing filter 4-2 is connected to the ultrapure water main pipe through a pipe; the washing liquid outlet of the washing filter 4-2 is connected to the wastewater treatment unit through a pipe; the washing and filtering The solid material outlet of the vessel 4-2 is connected to the feed port of the ammonium salt silo 5-1 through a pipeline;
- the discharge port at the bottom of the ammonium salt silo 5-1 is connected to the feed port of the ammonium salt screw feeder (5-2); the discharge port of the ammonium salt screw feeder 5-2 passes through the pipeline Connected to the feed port of the calcined bed feeder 6-3;
- the air inlet of the air purifier 6-1 is connected to the compressed air main pipe through a pipe; the air outlet of the air purifier 6-1 is respectively connected to the air inlet and the air inlet of the gas heater 6-2 through a pipe.
- the gas inlet at the bottom of the calcined bed feeder 6-3 is connected; the combustion air inlet and the fuel inlet of the gas heater 6-2 are respectively connected to the compressed air main pipe and the fuel main pipe through a pipe; the gas heating
- the gas outlet of the 6-2 is connected to the inlet of the bottom of the calcined fluidized bed main body 6-4 through a pipe; the discharge port of the calcined bed feeder 6-3 is fluidized by the pipe and the calcination a feed port at a lower portion of the bed main body 6-4 is connected; a discharge port at an upper portion of the calcined fluidized bed main body 6-4 is connected to a high-purity vanadium pentoxide product silo through a pipe; the calcined bed cyclone separat
- the gas outlet of the exhaust gas rinsing absorber 7 is connected to the gas inlet of the draft fan 8 through a pipe; the gas outlet of the draft fan 8 is connected to the gas inlet at the bottom of the chimney 9 through a pipe.
- the method for preparing 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 carbon powder maintains fluidization and chemical reaction with it, the air causes some carbon powder to burn to provide heat to maintain the fluidized bed temperature, and the chlorine gas and the carbon powder work together to chlorinate vanadium pentoxide and a small amount of impurities to form chlorination.
- a residue and a chlorinated flue gas rich in vanadium oxychloride the chlorinated residue is discharged through a slag discharge port in the lower portion of the chlorination fluidized bed main body 2-2, and the chlorination bed spiral slag discharge device 2-7; chlorine The flue gas is removed by the chlorination bed cyclone 2-3 and falls back to the chlorination fluidized bed, and then pre-cooled and enters the smoke through the flue gas heat exchanger 2-4.
- 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 vanadium-rich waste is used for subsequent recovery of vanadium
- the silicon-containing vanadium oxychloride vapor is passed through the distillate condenser 3-3 After condensing to the liquid, part of the reflux liquid collection tank 3-4 is refluxed to the rectification column 3-2, and the remainder is introduced into the silicon-containing vanadium oxychloride vanadium storage tank 3-5;
- the spent gas generated in the vanadium storage tank 3-5 is sent to the exhaust gas eluting absorber 7 through the acid sealing tank 3-6 of the rectifying section, and the silicon-containing vanadium oxychloride can be used for catalysis and other chemical fields;
- the pure vanadium oxychloride vapor is condensed into the liquid through the high-purity vanadium oxychloride condenser 3-7 and then enters the high-
- the high purity vanadium oxychloride vanadium in the high purity vanadium oxychloride vanadium storage tank 3-8 enters the ammonium salt precipitation reaction tank 4-1 and is obtained from the purified ammonia water main pipe and the ammonia gas condenser 6-6.
- the ammonia water is hydrolyzed and precipitated to form a mixed slurry of an ammonium salt precipitate containing ammonium polyvanadate or ammonium metavanadate and an ammonium chloride solution; the slurry enters the washing filter 4-2 and is washed with ultrapure water, and filtered.
- Obtaining a washing liquid and an ammonium salt precipitation powder the washing liquid is sent to the wastewater treatment unit; the ammonium salt is precipitated and sent to the ammonium salt silo 5-1;
- the ammonium salt precipitate in the ammonium salt silo 5-1 is sequentially introduced into the calcined fluidized bed main body 6-4 through the ammonium salt auger 5-2 and the calcined bed feeder 6-3;
- the compressed air is sequentially purified by the air purifier 6-1 and preheated by the gas heater 6-2 which is heated by the fuel combustion, and then sent to the calcined fluidized bed main body 6-4 to make the ammonium salt precipitated powder.
- the material maintains fluidization and thermally decomposes to form high-purity vanadium pentoxide powder and calcined flue gas rich in ammonia gas and water vapor; high-purity vanadium pentoxide powder passes through the calcined fluidized bed main body 6-4 The upper discharge opening is discharged and sent to the product silo for storage; the calcined flue gas is swirled through the calcined bed.
- the ammonia gas condenser 6-6 is condensed and recovered to obtain an aqueous ammonia solution, and then sent to the exhaust gas leaching absorber 7; the gas discharged from the exhaust gas leaching absorber 7 is passed through The induced draft fan 8 is sent into the chimney 9 and then emptied;
- One of the features of the present invention is that in the chlorinated fluidized bed main body 2-2, the chlorination process carbon powder is added in an amount of 10% to 20% by mass of the industrial grade vanadium pentoxide powder, and chlorinated.
- 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 ammonium salt precipitation reaction tank 4-1, the ammonium salt is precipitated at an operating temperature of 40 to 85 ° C and the precipitated pH is 6 to 9.
- the fourth feature of the present invention is that in the calcined fluidized bed main body 6-4, the operation temperature of the ammonium salt calcination is 400 to 600 ° C, and the average residence time of the powder is 45 to 90 min.
- the purity of the high-purity vanadium pentoxide powder obtained 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;
- ammonia aqueous solution obtained by calcination of the ammonium salt is circulated and returned to the ammonium salt precipitation step by the condensed recovery, thereby avoiding the pollution of the ammonia-containing tail gas and reducing the consumption of the purified ammonia water.
- the invention has the advantages of strong adaptability of raw materials, good selectivity of low temperature chlorination, low consumption of ammonia water, 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.
- FIG. 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 preparing a high purity vanadium pentoxide powder according to the present invention.
- the system for preparing 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, an ammonium salt precipitation device 4, and an ammonium salt feed.
- Device 5 Calcining fluidized bed 6, exhaust gas leaching absorber 7, induced draft fan 8 and chimney 9;
- 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 ammonium salt precipitation device 4 includes an ammonium salt precipitation reaction tank 4-1 and a washing filter 4-2;
- the ammonium salt feeding device 5 comprises an ammonium salt silo 5-1 and an ammonium salt screw feeder 5-2;
- the calcined fluidized bed 6 includes an air cleaner 6-1, a gas heater 6-2, a calcined bed feeder 6-3, a calcined fluidized bed main body 6-4, a calcined bed cyclone 6-5, and ammonia condensation. 6-6;
- 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 gas outlet of the chlorinated bed acid sealing tank 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 at the top of the rectification column 3-2 The outlet is connected to the gas inlet of the distillate condenser 3-3 through a conduit; the liquid outlet of the distillate condenser 3-3 is connected to the liquid inlet of the reflux collection tank 3-4 through a conduit; the reflux collection tank 3 The reflux liquid outlet of -4 is connected to the reflux liquid inlet at the top of the rectification column 3-2 through a pipe; the discharge port of the reflux liquid collection tank 3-4 and the inlet of the silicon-containing vanadium oxychloride vanadium storage tank 3-5 are passed through the pipe Connected; the spent gas outlet of the
- the ammonia solution inlet of the ammonium salt precipitation reaction tank 4-1 is connected to the ammonia water outlet of the purified ammonia water main pipe and the ammonia gas condenser 6-6 through a pipe; the chloride inlet of the ammonium salt precipitation reaction tank 4-1 passes through the pipe and the high
- the liquid outlet of the pure vanadium oxychloride vanadium storage tank 3-8 is connected;
- the slurry outlet of the ammonium salt precipitation reaction tank 4-1 is connected to the slurry inlet of the washing filter 4-2 through a pipe;
- the washing filter 4-2 The clean water inlet is connected to the ultrapure water main pipe through the pipeline;
- the washing liquid outlet of the washing filter 4-2 is connected to the wastewater treatment unit through the pipeline;
- the solid material outlet of the washing filter 4-2 is passed through the pipeline and the ammonium salt silo 5 -1 feed inlets are connected;
- the discharge port at the bottom of the ammonium salt silo 5-1 is connected to the feed port of the ammonium salt screw feeder 5-2; the discharge port of the ammonium salt screw feeder 5-2 is passed through the pipe and the calcined bed feeder 6- The feed ports of 3 are connected;
- the air inlet of the air purifier 6-1 is connected to the compressed air manifold through a pipeline; the air outlet of the air purifier 6-1 is respectively connected to the air inlet of the gas heater 6-2 and the calciner feeder 6 through the pipeline.
- 3 gas inlets at the bottom are connected; the combustion air inlet and the fuel inlet of the gas heater 6-2 are respectively connected to the compressed air main pipe and the fuel main pipe through a pipe; the gas outlet of the gas heater 6-2 passes through the pipe and the calcination flow
- the air inlets at the bottom of the chemical bed main body 6-4 are connected; the discharge port of the calcined bed feeder 6-3 is connected to the inlet of the lower portion of the calcined fluidized bed main body 6-4 through a pipe; the body of the calcined fluidized bed 6-4
- the upper discharge port is connected to the high-purity vanadium pentoxide product silo through a pipeline; the calcination bed cyclone separator 6-5 is disposed at the top center of the
- the gas outlet of the exhaust gas rinsing absorber 7 is connected to the gas inlet of the draft fan 8 through a pipe; the gas outlet of the draft fan 8 is connected to the gas inlet at the bottom of the chimney 9 through a pipe.
- the high-purity vanadium pentoxide powder is prepared 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 Carbon powder Industrial grade vanadium pentoxide screw feeder 1-2 and 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; from the chlorine gas source manifold The chlorine gas of the chlorine gas, 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 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 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.
- Part of the reflux liquid collection tank 3-4 is refluxed to the rectification column 3-2, and the remainder is introduced into the silicon-containing vanadium oxychloride vanadium storage tank 3-5; the silicon-containing vanadium oxychloride vanadium storage tank 3-5 is produced.
- the spent gas is sent to the exhaust gas leaching absorber 7 through the acid-sealing tank 3-6, and the silicon-containing vanadium oxychloride can be used in the chemical industry; the high-purity vanadium oxychloride vapor is passed through the high-purity vanadium oxychloride vanadium
- the condenser 3-7 is condensed to the liquid and then enters the high purity vanadium oxychloride vanadium storage tank 3-8;
- the high-purity vanadium oxychloride vanadium in the high-purity vanadium oxychloride vanadium storage tank 3-8 enters the ammonium salt precipitation reaction tank 4-1 and is hydrolyzed and precipitated with the ammonia water from the purified ammonia water main pipe and the ammonia gas condenser 6-6 to form a water.
- the washing liquid is sent to the wastewater treatment unit; the ammonium salt is precipitated and sent to the ammonium salt silo 5-1;
- the ammonium salt in the ammonium salt silo 5-1 is precipitated into the calcined fluidized bed main body 6-4 through the ammonium salt auger 5-2 and the calcined bed feeder 6-3; the compressed air is passed through the air purifier 6-1
- the gas heater 6-2 which purifies and relies on fuel combustion and heat supply is preheated and sent to the calcined fluidized bed main body 6-4 to maintain the fluidization of the ammonium salt precipitated powder material, and thermally decomposes to form high purity five.
- the gas is removed from the dust by the calciner bed cyclone 6-5, and then enters the ammonia gas condenser 6-6 to be condensed and recovered to obtain the ammonia aqueous solution, and then sent to the exhaust gas leaching absorber 7; the gas discharged from the exhaust gas leaching absorber 7 is introduced.
- the fan 8 is sent to the chimney 9 and then emptied.
- This embodiment uses powdered industrial grade vanadium pentoxide as raw material, and its chemical composition is listed in Table 1.
- the treatment amount is 75kg/h, and it is decomposed by low temperature chlorination, vanadium oxychloride rectification, ammonium salt precipitation and calcination. Preparation of high purity vanadium pentoxide products.
- 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 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 ammonium salt precipitation reactor 4-1 ammonium The salt precipitation operation temperature is 85 ° C, the precipitation pH value is 6.5; in the calcined fluidized bed main body 6-4, the ammonium salt calcination operation temperature is 400 ° C, the average residence time of the powder material is 90 min, the direct yield of vanadium Up to 85%, the purity of the high-purity vanadium pentoxide product is 99.996wt% (4N6).
- 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 10, the number of trays in the stripping section is 20, and the reflux ratio in the rectification operation is 15;
- the ammonium salt precipitation reactor 4-1 ammonium The salt precipitation operation temperature is 40 ° C, the precipitation pH value 9; in the calcined fluidized bed main body 6-4, the ammonium salt calcination operation temperature is 600 ° C, the average residence time of the powder material is 45 min, the direct yield of vanadium Up to 83%, the purity of the high-purity vanadium pentoxide product is 99.9993wt% (5N3).
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)
- 一种制备高纯五氧化二钒粉体的系统,其特征在于,所述系统包括加料装置(1)、低温氯化流化床(2)、精馏提纯装置(3)、铵盐沉淀装置(4)、铵盐加料装置(5)、煅烧流化床(6)、尾气淋洗吸收器(7)、引风机(8)和烟囱(9);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);所述铵盐沉淀装置(4)包括铵盐沉淀反应罐(4-1)和洗涤过滤器(4-2);所述铵盐加料装置(5)包括铵盐料仓(5-1)和铵盐螺旋加料器(5-2);所述煅烧流化床(6)包括空气净化器(6-1)、气体加热器(6-2)、煅烧床进料器(6-3)、煅烧流化床主体(6-4)、煅烧床旋风分离器(6-5)和氨气冷凝器(6-6);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、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(7)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(7)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;所述铵盐沉淀反应罐(4-1)的氨水溶液入口通过管道分别与纯化氨水总管和氨气冷凝器(6-6)底部的氨水出口相连接;所述铵盐沉淀反应罐(4-1)的氯化物入口通过管道与所述高纯三氯氧钒储罐(3-8)的液体出口相连接;所述铵盐沉淀反应罐(4-1)的浆料出口通过管道与所述洗涤过滤器(4-2)的浆料入口相连接;所述洗涤过滤器(4-2)的清水入口与超纯水总管通过管道相连接;所述洗涤过滤器(4-2)的洗涤液出口通过管道与废水处理单元相连接;所述洗涤过滤器(4-2)的固体物料出口通过管道与所述铵盐料仓(5-1)的进料口相连接;所述铵盐料仓(5-1)底部的出料口与所述铵盐螺旋加料器(5-2)的进料口相连接;所述铵盐螺旋加料器(5-2)的出料口通过管道与所述煅烧床进料器(6-3)的进料口相连接;所述空气净化器(6-1)的进气口与压缩空气总管通过管道相连接;所述空气净化器(6-1)的出气口通过管道分别与所述气体加热器(6-2)的进气口和所述煅烧床进料器(6-3)底部的气体入口相连接;所述气体加热器(6-2)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 气体加热器(6-2)的出气口通过管道与所述煅烧流化床主体(6-4)底部的进气口相连接;所述煅烧床进料器(6-3)的排料口通过管道与所述煅烧流化床主体(6-4)下部的进料口相连接;所述煅烧流化床主体(6-4)上部的出料口通过管道与高纯五氧化二钒产品料仓相连接;所述煅烧床旋风分离器(6-5)设置于所述氯化流化床主体(6-4)的扩大段顶部中心;所述煅烧床旋风分离器(6-5)的出气口通过管道与所述氨气冷凝器(6-6)的进气口相连接;所述氨气冷凝器(6-6)的气体出口通过管道与所述尾气淋洗吸收器(7)的气体入口相连接;所述尾气淋洗吸收器(7)的气体出口通过管道与所述引风机(8)的气体入口相连接;所述引风机(8)的气体出口通过管道与所述烟囱(9)底部的气体入口相连接。
- 一种基于权利要求1所述系统的制备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;氯化残渣经所述氯化流化床主体(2-2)下部的排渣口、所述氯化床螺旋排渣器(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(7)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;所述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;所述含硅三氯氧钒储罐(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(7)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)中的高纯三氯氧钒液体进入所述铵盐沉淀反应罐(4-1)后与来自纯化氨水总管及所述氨气冷凝器(6-6)的氨水发生水解沉淀,形成含多钒酸铵和偏钒酸铵的铵盐沉淀与氯化铵溶液的混合浆料;浆料进入所述洗涤过滤器(4-2)中经超纯水洗涤,过滤后得到洗涤液和铵盐沉淀粉料;洗涤液送往废水处理单元;铵盐沉淀送入所述铵盐料仓(5-1)中;所述铵盐料仓(5-1)中的铵盐沉淀依次经所述铵盐螺旋加料器(5-2)和煅烧床进料器(6-3)进入所述煅烧流化床主体(6-4)中;压缩空气依次经所述空气净化器(6-1)净化和依靠燃料燃烧供热的所述气体加热器(6-2)预热后送入所述煅烧流化床主体(6-4)中使铵盐沉淀粉体物料维持流态化,并使之发生热分解形成高纯五氧化二钒粉体,和富含氨气与水蒸气的煅烧烟气;高纯五氧化二钒粉体经所述煅烧流化床主体(6-4)上部排料口排出后送往产品料仓储存;煅烧烟气经所述煅烧床旋风分离器(6-5)脱除粉尘后进入所述氨气冷凝器(6-6)冷凝回收得到氨水溶液后,送入所述尾气淋洗吸收器(7)中;所述尾气淋洗吸收器(7)排出的气体经所述引风机(8)送入所述烟囱(9)后排空。
- 根据权利要求2所述的制备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)内进行氯化过程中,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所述的制备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所述的制备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所述的制备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所述的制备高纯五氧化二钒粉体的方法,其特征在于,在所述铵盐沉淀反应罐(4-1)内,所述铵盐沉淀的操作温度为40~85℃,沉淀pH值为6~9。
- 根据权利要求2所述的制备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(6-4)内,所述铵盐煅烧的操作温度为400~600℃,粉料的平均停留时间为45~90min。
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US10053371B2 (en) | 2018-08-21 |
EP3243798B8 (en) | 2019-05-22 |
BR112017015797A2 (zh) | 2018-06-19 |
EP3243798A1 (en) | 2017-11-15 |
US20180022616A1 (en) | 2018-01-25 |
CA2973491A1 (en) | 2016-08-04 |
CN105984900A (zh) | 2016-10-05 |
ZA201704629B (en) | 2019-06-26 |
AU2016212538B2 (en) | 2018-01-18 |
CN105984900B (zh) | 2017-06-13 |
JP2018505123A (ja) | 2018-02-22 |
RU2663777C1 (ru) | 2018-08-09 |
AU2016212538A1 (en) | 2017-08-31 |
EP3243798A4 (en) | 2018-01-03 |
JP6347903B2 (ja) | 2018-06-27 |
CA2973491C (en) | 2020-01-28 |
EP3243798B1 (en) | 2018-11-28 |
NZ733920A (en) | 2018-08-31 |
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