CN101117238A - Method for extracting vanadium pentoxide from bayer process seed precipitation solution by extraction process - Google Patents
Method for extracting vanadium pentoxide from bayer process seed precipitation solution by extraction process Download PDFInfo
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- CN101117238A CN101117238A CNA2007101186756A CN200710118675A CN101117238A CN 101117238 A CN101117238 A CN 101117238A CN A2007101186756 A CNA2007101186756 A CN A2007101186756A CN 200710118675 A CN200710118675 A CN 200710118675A CN 101117238 A CN101117238 A CN 101117238A
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- vanadium
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- vanadate
- ammonium
- bayer
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- 238000000034 method Methods 0.000 title claims abstract description 42
- 238000000605 extraction Methods 0.000 title claims abstract description 30
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000001556 precipitation Methods 0.000 title claims description 19
- 238000004131 Bayer process Methods 0.000 title claims description 16
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 70
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims abstract description 61
- 239000000284 extract Substances 0.000 claims abstract description 21
- 239000007788 liquid Substances 0.000 claims abstract description 21
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 20
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 20
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 claims abstract description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 18
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 16
- 239000013078 crystal Substances 0.000 claims abstract description 12
- CMZUMMUJMWNLFH-UHFFFAOYSA-N sodium metavanadate Chemical compound [Na+].[O-][V](=O)=O CMZUMMUJMWNLFH-UHFFFAOYSA-N 0.000 claims abstract description 12
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 10
- 239000000706 filtrate Substances 0.000 claims abstract description 10
- 239000012074 organic phase Substances 0.000 claims abstract description 10
- 208000004434 Calcinosis Diseases 0.000 claims abstract description 5
- 239000012535 impurity Substances 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 35
- 238000001914 filtration Methods 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 239000011734 sodium Substances 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 12
- WQEVDHBJGNOKKO-UHFFFAOYSA-K vanadic acid Chemical compound O[V](O)(O)=O WQEVDHBJGNOKKO-UHFFFAOYSA-K 0.000 claims description 12
- 239000012452 mother liquor Substances 0.000 claims description 11
- 238000007670 refining Methods 0.000 claims description 10
- 229910000166 zirconium phosphate Inorganic materials 0.000 claims description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 239000002244 precipitate Substances 0.000 claims description 8
- 229910052708 sodium Inorganic materials 0.000 claims description 8
- 238000002386 leaching Methods 0.000 claims description 7
- 239000012071 phase Substances 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000003350 kerosene Substances 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 4
- 150000001412 amines Chemical class 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 3
- 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 claims description 2
- 238000000151 deposition Methods 0.000 abstract description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 abstract 2
- 239000008346 aqueous phase Substances 0.000 abstract 2
- 239000002904 solvent Substances 0.000 abstract 2
- 229910021529 ammonia Inorganic materials 0.000 abstract 1
- 238000004064 recycling Methods 0.000 abstract 1
- 229910000029 sodium carbonate Inorganic materials 0.000 abstract 1
- 235000017550 sodium carbonate Nutrition 0.000 abstract 1
- 238000011084 recovery Methods 0.000 description 9
- 229910052782 aluminium Inorganic materials 0.000 description 8
- 239000013049 sediment Substances 0.000 description 8
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 7
- 229910052791 calcium Inorganic materials 0.000 description 7
- 239000011575 calcium Substances 0.000 description 7
- 229910004298 SiO 2 Inorganic materials 0.000 description 6
- 229910000831 Steel Inorganic materials 0.000 description 6
- 239000010959 steel Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 239000003245 coal Substances 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 239000003085 diluting agent Substances 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 235000010755 mineral Nutrition 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- NASFKTWZWDYFER-UHFFFAOYSA-N sodium;hydrate Chemical compound O.[Na] NASFKTWZWDYFER-UHFFFAOYSA-N 0.000 description 3
- 125000005270 trialkylamine group Chemical group 0.000 description 3
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 235000011941 Tilia x europaea Nutrition 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000004571 lime Substances 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- BPAABJIBIBFRST-UHFFFAOYSA-N [V].[V].[V].[Ga] Chemical compound [V].[V].[V].[Ga] BPAABJIBIBFRST-UHFFFAOYSA-N 0.000 description 1
- 229940037003 alum Drugs 0.000 description 1
- 229910001570 bauxite Inorganic materials 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- PNXOJQQRXBVKEX-UHFFFAOYSA-N iron vanadium Chemical compound [V].[Fe] PNXOJQQRXBVKEX-UHFFFAOYSA-N 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000005120 petroleum cracking Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000009628 steelmaking Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 150000003682 vanadium compounds Chemical class 0.000 description 1
- 229910000999 vanadium-gallium Inorganic materials 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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- Manufacture And Refinement Of Metals (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to a method for extracting vanadium pentoxide from Bayer spent liquor, in particular to an extracting method for extrating vanadium pentoxide from Bayer spent liquor, which is characterized in that the process of the invention comprises the following steps: (1) CaO is added into the Bayer spend liquor to make vanadate calcium deposit; (2) Na2CO3 solvent used for depositing is dissolved to make Sodium metavanadate solvent; (3) an organic extraction liquid is used to extract Sodium metavanadate, V205 enters an upper layer extract while other impurities enter a lower layer of aqueous phase of raffinate; (4) ammonia is used to extract an organic phase, aqueous phase is filtered to make Ammonium polyvanadate crystal which is baked to make rough V205; (5) after the rough V205 is seethed and filtered by sodium hydroxide, the filtrate is mixed with ammonium chloride, an Ammonium metavanadate to be separated out is baked to make purely refined V205; the invention is characterized in a simple process, a low cost and a high vanadium recycling rate.
Description
Technical field
A kind of method of extracting Vanadium Pentoxide in FLAKES in the Bayer-process seed-separating mother liquor is specifically related to a kind of method of extracting Vanadium Pentoxide in FLAKES with method of extraction from Bayer-process seed-separating mother liquor.
Background technology
Vanadium is a kind of important strategic goods and materials, has the characteristic of high-melting-point and easy deformation processing, is mainly used in fields such as Iron And Steel Industry, national defence sophisticated technology, chemical industry and light and textile industries.Vanadium plays the effect of crystal grain thinning in steel, add intensity and Corrosion Protection that 5/10000ths vanadium just can obviously improve steel in the steel.In foundry goods, add 0.1%～0.15% vanadium and can improve intensity, toughness and the wear resistance of foundry goods.Add 6% aluminium and 4% vanadium in the titanium-base alloy, its intensity and welding performance are improved significantly.This alloy is a material of making the air fighter gas turbine.The vanadium gallium alloy is important superconducting material.V
2O
5It is the catalyst of sulfuric acid industry, petroleum cracking industry and synthetic some macromolecular compound.There are more than 20 countries and regions to produce products such as Vanadium Pentoxide in FLAKES and vanadium iron in the world.Be South Africa, the former Soviet Union, the U.S. and China but mainly produce vanadium state.The aboundresources of vanadium is widely distributed in the world, can not supply the rich ore of exploitation but have separately, but with low-grade and other mineral paragenesis.
The Main Resources that extracts at present vanadic anhydride has bone coal, low vanadium steel slag, spent vanadium catalyst etc.Its source is wide, total amount is big.China contains the scherbinaite coal and mainly is distributed in southern all provinces, and total reserves is abundant, composes the total reserves that the vanadium of depositing estimates to surpass other national vanadium of the world.The vanadium grade is 0.3%～1.0% (with V in the Rock coal containing alum
2O
5Meter, lower same), vanadium is composed with the form of appraising at the current rate and is deposited its mineral composition complexity, separation and extraction difficulty.Low vanadium steel slag results from the steelmaking process of vanadium-bearing hot metal, the vanadium grade is generally 2%～4%, all the other are the oxide compound of iron, calcium, magnesium, aluminium etc., wherein the whole disperses of vanadium be distributed in multi mineral mutually in, be difficult to direct choosing, smelting separation, the annual total flow rate of China's (Sichuan Flos Bombacis Malabarici, Chengde, Anhui Maanshan) reaches millions of tons.Spent vanadium catalyst derives from chemistry and petroleum industry.Characteristics are that the source is wide, quantity is big, and the vanadium grade is about 8%, and wherein vanadium is mainly with V
2O
5And VOSO
4Form relatively concentrate in some specific phases.The existing traditional vanadium extraction technology from various raw materials, often owing to expensive, high pollution, long flow process, the low rate of recovery, be restricted so use always, some green separation technologies that occur, separate out technology, microorganism leaching-out technique, in-pulp electrolysis technology etc. as selectivity, be expected to use in this field achieving success.
All contain to some extent V in the bauxite
2O
5, in sintering process is produced alumina process, owing to allocated large quantities of lime in the furnace charge, make most vanadium become insoluble vanadic acid calcium and enter red mud.Lime also makes V in Bayer process
2O
5Dissolution rate reduce, vanadium circulate in seed precipitation solution and accumulates and reach finite concentration, is generally 28%～45%.Facts have proved that vanadium compound has detrimentally affect to alumina producing, if when guaranteeing that alumina producing is normally carried out, from flow process, vanadium is extracted, not only can eliminate the harm of vanadium, and can improve the economic benefit of alumina producer greatly, have crucial meaning.
The Method and process that extracts vanadium from alumina producing can be divided into three kinds of crystallisation, extraction and ion-exchanges by principle.Crystallization process technical maturity, equipment are simple, but the rate of recovery of vanadium is lower.Extraction and ion-exchange cost are lower, the rate of recovery height of vanadium, but present technological process is not mature enough, invest highlyer, also need do further improvement.
Summary of the invention
The objective of the invention is the improving of the above-mentioned method of from alumina producing, extracting vanadium, provide a kind of flow process is simple, cost is lower, vanadium recovery is high extraction process from Bayer-process seed-separating mother liquor, to extract the method for Vanadium Pentoxide in FLAKES.
The objective of the invention is to be achieved through the following technical solutions.
A kind of extraction process extracts the method for Vanadium Pentoxide in FLAKES in the Bayer-process seed-separating mother liquor, and it is levied and is that its process may further comprise the steps:
(1) add CaO in Bayer-process seed-separating mother liquor, stirring reaction makes the vanadium in the seed precipitation solution precipitate with the vanadic acid calcium form;
(2) with vanadic acid calcium form precipitation Na
2CO
3Solution dissolving makes vanadium enter with the form of vanadic acid sodium and makes sodium vanadate solution in the solution;
(3) with organic extract liquid sodium vanadate solution is extracted V
2O
5Enter the upper strata extraction phase, other impurity enter lower floor's raffinate phase water;
(4) with the ammoniacal liquor organic phase of stripping, the upper strata is that extract can be recycled, and lower floor's water is separated out ammonium poly-vanadate; Water obtains the ammonium poly-vanadate crystal after filtration, gets thick V through roasting
2O
5
5) with thick V
2O
5After boiling filtration with sodium hydrate aqueous solution, filtrate adds ammonium chloride, and the ammonium metavanadate of separating out makes the refining V of purity through roasting
2O
5
Method of the present invention, when it is characterized in that adding CaO produces vanadic acid calcium form precipitation in Bayer-process seed-separating mother liquor, the CaO add-on is 10～25g/L, is under 90～110 ℃ in temperature, behind stirring reaction 1～4h throw out filtration, washing, oven dry is made and contains the vanadium throw out;
Method of the present invention is characterized in that it being that the vanadic acid calcium deposit is added Na
2CO
3When dissolving in the solution, the vanadic acid calcium deposit adds Na
2CO
3The amount of solution is 20～50g/L, is under 95～105 ℃ in temperature, and stirring reaction 1～4h obtains vanadium leachate;
Method of the present invention is characterized in that the extraction liquid when sodium vanadate solution extracted is made up of extraction agent and thinner, and extraction agent is three basic amine R
3(wherein R is C to N
11～C
13Alkyl), thinner is with kerosene, C
6Alcohol or benzene; (volume) of extraction agent and thinner regulated leaching liquid pH=3 than being 30: 70; Be in a ratio of 1: 1～4: 1;
Method of the present invention, its feature is 5%～8% in the ammoniacal liquor weight percent concentration of reextraction organic phase, is in a ratio of 1: 1～4: 1,40～60 ℃ of reextraction temperature, the upper strata is that extract recycles, lower floor's water is separated out ammonium poly-vanadate; Water obtains the ammonium poly-vanadate crystal after filtration, at 400～600 ℃ of roasting 1～4h, makes purity and be 88%～92% thick V
2O
5
Method of the present invention is characterized in that the thick V that makes
2O
5Be to be that 15～30% sodium hydrate aqueous solution boils 2～5h with weight concentration, after the filtration, add ammonium chloride 10～20g/L filtrate, separate out ammonium metavanadate, ammonium metavanadate makes refining V at 500～700 ℃ of roasting 1～4h
2O
5
Method of the present invention be with the seed precipitation solution in the alumina producing Bayer process process through the seed precipitation solution precipitation, contain the process recovery V wherein such as leachings of vanadium precipitation, organic extract liquid extraction, back extraction, aqueous crystallization, the roasting of ammonium poly-vanadate crystal, thick vanadium be refining
2O
5Flow process is simple, cost is lower, vanadium recovery is high.
Description of drawings
Fig. 1 is the process flow sheet of method of the present invention.
Embodiment
A kind of method of extracting vanadium pentoxide from bayer process seed precipitation solution by extraction process, its process may further comprise the steps (1) and add CaO in Bayer-process seed-separating mother liquors, and stirring reaction makes the vanadium in the seed precipitation solution precipitate with the vanadic acid calcium form; (2) with vanadic acid calcium form precipitation Na
2CO
3Solution dissolving makes vanadium enter with the form of sodium vanadate and makes sodium vanadate solution in the solution; (3) with organic extract liquid sodium vanadate solution is extracted V
2O
5Enter the upper strata extraction phase, other impurity enter lower floor's raffinate phase water; (4) with the ammoniacal liquor organic phase of stripping, the upper strata is that extract can be recycled, and lower floor's water is separated out ammonium poly-vanadate; Water obtains the ammonium poly-vanadate crystal after filtration, gets thick V through roasting
2O
5(5) with thick V
2O
5After boiling filtration with sodium hydrate aqueous solution, filtrate adds ammonium chloride, and the ammonium metavanadate of separating out makes the refining V of purity through roasting
2O
5
When adding CaO produced vanadic acid calcium form precipitation in Bayer-process seed-separating mother liquor, the CaO addition was 10～25g/L, is under 90～110 ℃ in temperature, behind stirring reaction 1～4h sediment filtration, washing, oven dry was made and contained the vanadium sediment; The vanadic acid calcium precipitate is added Na
2CO
3When dissolving in the solution, the vanadic acid calcium precipitate adds Na
2CO
3The amount of solution is 20～50g/L, is under 95～105 ℃ in temperature, and stirring reaction 1～4h obtains vanadium leachate; Extract when sodium vanadate solution is extracted is made up of extractant and diluent, and extractant is three basic amine R
3(wherein R is C to N
11～C
13Alkyl), diluent is with kerosene, C
6Alcohol or benzene; (volume) of extractant and diluent regulated leaching liquid pH=3 than being 30: 70; Be in a ratio of 1: 1～4: 1; The ammoniacal liquor weight percent concentration of reextraction organic phase is 5%～8%, is in a ratio of 1: 1～4: 1,40～60 ℃ of reextraction temperature, and the upper strata is that extract recycles, lower floor's water is separated out ammonium poly-vanadate; Water obtains the ammonium poly-vanadate crystal after filtration, at 400～600 ℃ of roasting 1～4h, makes purity and be 88%～92% thick V
2O
5The thick V that makes
2O
5Be to be that 15～30% sodium hydrate aqueous solution boils 2～5h with weight concentration, after the filtration, add ammonium chloride 10～20g/L filtrate, separate out ammonium metavanadate, ammonium metavanadate makes refining V at 500～700 ℃ of roasting 1～4h
2O
5
Embodiment 1
Containing V
2O
5Adding CaO10g/L in 0.42% the seed precipitation solution, is under 100 ℃ in temperature, behind the stirring reaction 2h sediment filtration, washing, oven dry is namely got and contains the vanadium sediment, and its chemical composition is: CaO 51.32%, Al
2O
329.52%, SiO
24.61%, Na
2O 0.68%, V
2O
50.76%;
Under 100 ℃, (CaO 51.32%, Al with the vanadic acid calcium precipitate
2O
329.52%, SiO
24.61%, Na
2O 0.68%, V
2O
50.76%) adds the Na of 40g/L with the amount of 200g/L
2CO
3In the solution, stirring reaction 2h obtains vanadium leachate, and leachate vanadium concentration is 1.42g/L;
With organic extract liquid vanadium leachate is extracted, extraction liquid is a trialkylamine: kerosene=30: 70, regulate leaching liquid pH=3, and the rate of recovery that calculates vanadium is 95.8%;
Ammoniacal liquor reextraction organic phase with 6%, upper strata are that extraction liquid recycles, and lower floor's water is separated out ammonium poly-vanadate.Water obtains the ammonium poly-vanadate crystal after filtration, gets V behind 400 ℃ of roasting 2h
2O
5Purity be 89.5%;
Be 89% V with purity
2O
5Sodium hydrate aqueous solution with 20% boils 4h, and after the filtration, filtrate adds ammonium chloride 15g/L, separates out ammonium metavanadate, and ammonium metavanadate gets V at 500 ℃ of roasting 2h
2O
5Purity is 99.2% refining V
2O
5
Embodiment 2
Containing V
2O
5Adding CaO15g/L in 0.42% the seed precipitation solution, is under 102 ℃ in temperature, behind the stirring reaction 2h sediment filtration, washing, oven dry is namely got and contains the vanadium sediment, and its chemical composition is: CaO 50.36%, Al
2O
330.53%, SiO
24.08%, Na
2O 0.60%, V
2O
50.70%;
Under 100 ℃, (CaO 50.36%, Al with the vanadic acid calcium precipitate
2O
330.53%, SiO
24.08%, Na
2O 0.60%, V
2O
50.70%) adds the Na of 40g/L with the amount of 200g/L
2CO
3In the solution, stirring reaction 2h obtains vanadium leachate, and leachate vanadium concentration is 1.10g/L;
With organic extract liquid vanadium leachate is extracted, extract is trialkylamine: C
6Alcohol=30: 70 is regulated leaching liquid pH=3, and the rate of recovery that calculates vanadium is 93.8%;
Ammoniacal liquor reextraction organic phase with 7%, upper strata are that extraction liquid recycles, and lower floor's water is separated out ammonium poly-vanadate.Water obtains the ammonium poly-vanadate crystal after filtration, gets V behind 500 ℃ of roasting 2h
2O
5Purity be 91.6%;
Be 91.6% V with purity
2O
5Sodium hydrate aqueous solution with 20% boils 4h, and after the filtration, filtrate adds ammonium chloride 20g/L, separates out ammonium metavanadate, and ammonium metavanadate gets V at 600 ℃ of roasting 2h
2O
5Purity is 99.4% refining V
2O
5
Embodiment 3
Containing V
2O
5Adding CaO20g/L in 0.42% the seed precipitation solution, is under 105 ℃ in temperature, behind the stirring reaction 2h sediment filtration, washing, oven dry is namely got and contains the vanadium sediment, and its chemical composition is: CaO 50.54%, Al
2O
330.16%, SiO
23.32%, Na
2O 0..30%, V
2O
50.69%;
Under 100 ℃, (CaO 50.54%, Al with the vanadic acid calcium precipitate
2O
330.16%, SiO
23.32%, Na
2O 0.30%, V
2O
50.69%) adds the Na of 40g/L with the amount of 200g/L
2CO
3In the solution, stirring reaction 2h obtains vanadium leachate, and leachate vanadium concentration is 0.89g/L;
With organic extract liquid vanadium leachate is extracted, extraction liquid is a trialkylamine: benzene=30: 70, regulate leaching liquid pH=3, and the rate of recovery that calculates vanadium is 91.2%;
Ammoniacal liquor reextraction organic phase with 8%, upper strata are that extraction liquid recycles, and lower floor's water is separated out ammonium poly-vanadate.Water obtains the ammonium poly-vanadate crystal after filtration, gets V behind 550 ℃ of roasting 2h
2O
5Purity be 91.8%;
Be 91.8% V with purity
2O
5Sodium hydrate aqueous solution with 20% boils 4h, and after the filtration, filtrate adds ammonium chloride 20g/L, separates out ammonium metavanadate, and ammonium metavanadate gets V at 650 ℃ of roasting 2h
2O
5Purity is 99.3% refining V
2O
5
Claims (6)
1. an extraction process extracts the method for Vanadium Pentoxide in FLAKES in the Bayer-process seed-separating mother liquor, and it is levied and is that its process may further comprise the steps
(1) add CaO in Bayer-process seed-separating mother liquor, stirring reaction makes the vanadium in the seed precipitation solution precipitate with the vanadic acid calcium form;
(2) with vanadic acid calcium form precipitation Na
2CO
3Solution dissolving makes vanadium enter with the form of vanadic acid sodium and makes sodium vanadate solution in the solution;
(3) with organic extract liquid sodium vanadate solution is extracted V
2O
5Enter the upper strata extraction phase, other impurity enter lower floor's raffinate phase water;
(4) with the ammoniacal liquor organic phase of stripping, the upper strata is that extract can be recycled, and lower floor's water is separated out ammonium poly-vanadate; Water obtains the ammonium poly-vanadate crystal after filtration, gets thick V through roasting
2O
5
5) with thick V
2O
5After boiling filtration with sodium hydrate aqueous solution, filtrate adds ammonium chloride, and the ammonium metavanadate of separating out makes the refining V of purity through roasting
2O
5
2. according to according to the described method of claim 1, when it is characterized in that adding CaO produces vanadic acid calcium form precipitation in Bayer-process seed-separating mother liquor, the CaO add-on is 10～25g/L, in temperature is under 90～110 ℃, behind stirring reaction 1～4h throw out filtration, washing, oven dry is made and contains the vanadium throw out.
3. according to according to the described method of claim 1, it is characterized in that the vanadic acid calcium deposit is added Na
2CO
3When dissolving in the solution, the vanadic acid calcium deposit adds Na
2CO
3The amount of solution is 20～50g/L, is under 95～105 ℃ in temperature, and stirring reaction 1～4h obtains vanadium leachate.
4. according to according to the described method of claim 1, it is characterized in that the extraction liquid when sodium vanadate solution extracted is made up of extraction agent and thinner, extraction agent is three basic amine R
3(wherein R is C to N
11～C
13Alkyl), thinner is with kerosene, C
6Alcohol or benzene; (volume) of extraction agent and thinner regulated leaching liquid pH=3 than being 30: 70, is in a ratio of 1: 1～4: 1.
5. according to according to the described method of claim 1, its feature is 5%～8% in the ammoniacal liquor weight percent concentration of reextraction organic phase, is in a ratio of 1: 1～4: 1,40～60 ℃ of reextraction temperature, and the upper strata is that extract recycles, lower floor's water is separated out ammonium poly-vanadate; Water obtains the ammonium poly-vanadate crystal after filtration, at 400～600 ℃ of roasting 1～4h, makes purity and be 88%～92% thick V
2O
5
6. according to according to the described method of claim 1, it is characterized in that the thick V that makes
2O
5Be to be that 15～30% sodium hydrate aqueous solution boils 2～5h with weight concentration, after the filtration, add ammonium chloride 10～20g/L filtrate, separate out ammonium metavanadate, ammonium metavanadate makes refining V at 500～700 ℃ of roasting 1～4h
2O
5
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102011000A (en) * | 2010-12-09 | 2011-04-13 | 中国铝业股份有限公司 | Method for removing vanadium from gallium-enriched solution in resin-absorbed seed precipitation mother liquor |
| CN101723455B (en) * | 2009-12-29 | 2011-09-21 | 攀钢集团攀枝花钢钒有限公司 | Method for preparing sodium metavanadate |
| CN102502570A (en) * | 2011-11-29 | 2012-06-20 | 芜湖人本合金有限责任公司 | Production method of medical sodium metavanadate |
| CN103505903A (en) * | 2012-06-25 | 2014-01-15 | 中国人民解放军63971部队 | Two-stage extraction preparation method for high-purity vanadyl sulfate solution |
| CN114162865A (en) * | 2022-01-19 | 2022-03-11 | 四川轻化工大学 | High-purity ammonium metavanadate crystal and preparation method thereof |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4039614A (en) * | 1972-07-17 | 1977-08-02 | Slotvinsky Sidak Nikolai Petro | Method of preparing vanadium pentoxide from metallurgical slags containing vanadium |
| CN1724387A (en) * | 2005-06-22 | 2006-01-25 | 株洲市湘麒科技开发有限公司 | Process for extracting vanadium pentoxide from stone coal vanadium mining |
| CN100360428C (en) * | 2006-06-22 | 2008-01-09 | 姚明峰 | Method for picking up vanadium pentexide from layer silicate without oxidation in furnace |
| CN1899971B (en) * | 2006-07-01 | 2011-08-03 | 谢更生 | Method for extracting V2O5 from stone coal vanadium ore |
| CN100375716C (en) * | 2006-08-14 | 2008-03-19 | 中国铝业股份有限公司 | Method of recovering V2O5 from Bayer process mother liquid |
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2007
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101723455B (en) * | 2009-12-29 | 2011-09-21 | 攀钢集团攀枝花钢钒有限公司 | Method for preparing sodium metavanadate |
| CN102011000A (en) * | 2010-12-09 | 2011-04-13 | 中国铝业股份有限公司 | Method for removing vanadium from gallium-enriched solution in resin-absorbed seed precipitation mother liquor |
| CN102502570A (en) * | 2011-11-29 | 2012-06-20 | 芜湖人本合金有限责任公司 | Production method of medical sodium metavanadate |
| CN103505903A (en) * | 2012-06-25 | 2014-01-15 | 中国人民解放军63971部队 | Two-stage extraction preparation method for high-purity vanadyl sulfate solution |
| CN114162865A (en) * | 2022-01-19 | 2022-03-11 | 四川轻化工大学 | High-purity ammonium metavanadate crystal and preparation method thereof |
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