CN104775041B - The cleaning extraction vanadium method that a kind of vanadium liquid calcium method precipitation, mother liquor and solid waste self-loopa are utilized - Google Patents
The cleaning extraction vanadium method that a kind of vanadium liquid calcium method precipitation, mother liquor and solid waste self-loopa are utilized Download PDFInfo
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Abstract
The invention provides the cleaning extraction vanadium method that a kind of vanadium liquid calcium method precipitation, mother liquor and solid waste self-loopa are utilized, including：To after purification, vanadium liquid adds calcification additive to carry out calcium method precipitation reaction, then occurs to turn leaching reaction by the calcium vanadate for obtaining, the Ammonium Vanadate Solution for obtaining crystallization is obtained ammonium metavanadate crystal.The present invention turns the brilliant detached method of cementing using vanadium liquid calcification precipitation carbonating, can realize the regeneration of additive for extracting vanadium sodium salt and recycle；Separated by Na, V in vanadium liquid, the zero-emission and mediumization for thoroughly realizing precipitation " waste water " is utilized；The end treatment processes such as conventional precipitation technique waste water " three take off " (vanadium removal, de- chromium, deamination) are eliminated, the chromium in waste water is sold by commercialization recovery, high level；In addition to tailings in vanadium extraction, technique " solid waste " is utilized in flow process interior circulation, and tailings in vanadium extraction enters iron and steel process resourcesization and utilizes.
Description
Technical field
The invention belongs to vanadium field of chemical metallurgical technology, is related to a kind of vanadium liquid calcium method precipitation, mother liquor and solid waste self-loopa profit
Cleaning extraction vanadium method, more particularly to a kind of vanadium-containing material sodium vanadium extraction-calcium method precipitation-mother liquor and " solid waste " recycle
Chemical industry extraction vanadium method.
Background technology
The conventional method of vanadic anhydride production is vanadium slag sodium roasting-ammonium salt precipitation method, and wherein more than 65% vanadium is produced
Product come from the method.The ammonium salt precipitation method have two kinds：A kind of is that the pH value of the solution containing pentavalent vanadium is adjusted to 8.5～9.5 first, so
In solution V is pressed afterwards2O5Mass ratio 1 with ammonium salt:1.3～1.5 add ammonium salt Precipitation ammonium metavanadate；Another kind is to adopt to divide
The pH value of step solution solution adds ammonium salt Precipitation ammonium poly-vanadate to 1.5～2.5, after by the ammonium metavanadate for obtaining or many vanadium
Sour ammonium obtains vanadic anhydride through calcining.
The main deficiency of the technique is：(1) Vanadium in Vanadium Residue is mainly present with vanadium iron spinel structure, and chemical mine is mutually stable,
It is difficult to decompose；During gas-solid calcination, oxygen mass transfer effect is poor, even if adopting multiple high temp roasting, the one way of vanadium is returned
Yield also only has 80%；This technique cannot avoid the deficiency.(2) containing more siliceous low melting point in vanadium slag, improve anti-
Answer temperature cause ring formation, affect the operation of kiln, limit the further raising of reaction temperature, therefore, it is difficult to by improving temperature
Method improve vanadium recovery rate.(3) the heavy process of ammonium can produce substantial amounts of high salinity, nitrogen-containing wastewater, and unit vanadium product is (with five
V 2 O meter) for about 40 tons of waste water yield, serious environment pollution；Ton vanadium chrome waste water treatment cost is controlled at 3000 yuan or so
Reason cost is big.
CN 101157478A propose a kind of preparation method of ammonium poly-vanadate, with traditional sodium roasting-water logging technique life
It is raw material containing vanadium solution to produce, and first makes vanadium with the calcium chloride or calcium nitrate for adding and generates calcium vanadate, then turns molten with ammonium hydrogen carbonate,
Vanadium enters solution, and calcium generates the calcium carbonate of more indissoluble, and the vanadium liquid sulphur acid for adjusting pH after separating, precipitation obtain ammonium poly-vanadate.Should
Alkali content in ammonium poly-vanadate can be dropped to ammonia content drop in less than 0.1%, and vanadium wastewater compared with traditional handicraft by technique
To the 60%～75% of traditional handicraft, but there is the emission problem of ammonia nitrogen waste water.
In view of existing vanadium slag sodium roasting-water logging vanadium extraction, stone coal sodium roasting vanadium-extracting are difficult to meet vanadium using technical progress
The strategic requirement of cleaner Production in Chemical Industry, it is therefore necessary to which the method that research and development realize vanadium high efficiente callback in vanadium liquid from source, exploitation are solved
The vanadium liquid vanadium extraction clearer production technology of environmental pollution.
Content of the invention
For the problem of prior art, an object of the present invention is to provide a kind of high-efficiency cleaning extraction vanadium method, this
Bright it is a further objective that a kind of vanadium liquid calcium method precipitation is provided, the cleaning extraction vanadium method that mother liquor and solid waste self-loopa are utilized,
Methods described wastewater zero discharge, technological process are short, easy to operate, low production cost.
To achieve these goals, following technical scheme present invention employs：
The cleaning extraction vanadium method that a kind of vanadium liquid calcium method precipitation, mother liquor and solid waste self-loopa are utilized, comprises the following steps：
To after purification, vanadium liquid adds calcification additive to carry out calcium method precipitation reaction, then occurs to turn leaching by the calcium vanadate for obtaining
The Ammonium Vanadate Solution for obtaining crystallization is obtained ammonium metavanadate crystal by reaction.
Preferably, the method comprising the steps of：
(1) calcification additive is added to vanadium liquid after purification, carry out calcium method precipitation reaction, isolated vanadium in atmospheric conditions
Sour calcium precipitate and NaOH solution；
(2) calcium vanadate that step (1) is obtained is sized mixing with ammonium bicarbonate soln, carries out turning leaching reaction, isolated vanadic acid
Ammonium salt solution and precipitation of calcium carbonate；
(3) the Ammonium Vanadate Solution crystallisation by cooling that obtains step (2) adds ammonium salt crystallization, and isolated ammonium metavanadate is brilliant
Body and crystalline mother solution；
Optionally, step (4) is carried out：
(4) calcium carbonate for obtaining step (2) decomposes through high-temperature calcination, and regeneration obtains CaO, adds as calcification
Agent, prepares calcium vanadate for step (1), and calcium source is recycled.
The method that the present invention turns molten-Crystallization Separation using vanadium liquid calcification precipitation-carbonating, can realize additive for extracting vanadium sodium
The regeneration of salt with recycle.
Preferably, the calcification additive is CaO and/or Ca (OH)2.
In the present invention, the separation can be to be separated by filtration.
The processing procedure of vanadium probably includes：Roasting, leaching, purification and precipitation, the present invention be by purification after vanadium liquid
Carry out above-mentioned technique.In the present invention, it is preferred to use vanadium-containing material sodium roasting technique vanadium extraction, then leach, purify.
It is therefore preferred that after after purifying, vanadium liquid is the sodium roasting water logging vanadium extraction of raw material containing navajoite such as vanadium slag or bone coal
Contain vanadium solution.
Preferably, the calcification additive addition adds for 1.5～3 according to Ca/V mol ratios, now vanadium in vanadium liquid
Rate of deposition is 20～26wt% higher than the V element content in 95%, and calcium vanadate.The mol ratio be, for example, 1.6,1.7,1.8,
1.9th, 2.0,2.1,2.2,2.3,2.4,2.5,2.6,2.7,2.8 or 2.9.
Preferably, the calcium method precipitation reaction temperature is 40～100 DEG C, and now in vanadium liquid, the rate of deposition of vanadium is higher than 95%,
Such as 45 DEG C, 50 DEG C, 55 DEG C, 60 DEG C, 65 DEG C, 70 DEG C, 75 DEG C, 80 DEG C, 85 DEG C, 90 DEG C or 95 DEG C, the reaction time be 10～
50min, such as 15min, 20min, 25min, 30min, 35min, 40min or 45min.
Preferably, during NaOH concentration ＜ 150g/L in step (1) vanadium liquid, the NaOH solution that step (1) is obtained directly is returned
Return leaching and washing procedure, the precipitation of leaching vanadium liquid repeat step (1) for obtaining and the lock out operation of " vanadium bearing slag ".Above-mentioned
During, the NaOH media of the 8～50wt% obtained after leaching and washing procedure are stayed in leaching vanadium tailing soil, in after baking
(with Naization additive form) is directly utilized.50～92wt% (i.e. remaining) NaOH media are stayed in leaching vanadium liquid, weight
The precipitation of multiple step (1) and lock out operation, the NaOH concentration after making each circulating leaching in vanadium liquid get a promotion.
Preferably, be enriched to when the NaOH concentration in step (1) vanadium liquid >=150g/L after, be to ensure calcium method precipitation effect,
It is 40～80wt% that the NaOH solution that step (1) is obtained is concentrated by evaporation to NaOH concentration, and the NaOH solution of 40～80wt% does
For sodium additive return burden process containing vanadium mineral all of.Preferably, when the NaOH solution that step (1) is obtained contains chromium
When, chromium will crystallize precipitation in evaporation process, obtain sodium chromate product after refining.
Preferably, described turn of leaching reaction temperature is 20～100 DEG C, such as 30 DEG C, 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C
Or 90 DEG C, turn the leaching reaction time for 10～100min, such as 20min, 30min, 40min, 50min, 60min, 70min, 80min
Or 90min, it is 4 to turn leaching reaction liquid-solid ratio:1～10:1, such as 5:1、6:1、7:1、8:1 or 9:1.
Preferably, the ammonium bicarbonate soln concentration in step (2) be 1～40wt%, such as 5wt%, 10wt%,
15wt%, 20wt%, 25wt%, 30wt% or 35wt%.
Preferably, the crystallisation by cooling outlet temperature in step (3) be 0～50 DEG C, such as 5 DEG C, 10 DEG C, 15 DEG C, 20 DEG C, 25
DEG C, 30 DEG C, 35 DEG C, 40 DEG C or 45 DEG C.
Preferably, step (3) add ammonium salt to ammonium salt concentration be 5～50wt%, such as 10wt%, 15wt%, 20wt%,
25wt%, 30wt%, 35wt%, 40wt% or 45wt%.
Preferably, the crystalline mother solution that step (3) is obtained returns the calcium vanadate turn leaching for step (2).
Preferably, step (4) calcining heat is 900～1000 DEG C.
Compared with the prior art, the present invention has the advantages that：
1. additive for extracting vanadium sodium salt is regenerated and recycles；2. separated by Na, V in vanadium liquid, thoroughly realize precipitation
The zero-emission of " waste water " is utilized with mediumization；3. the ends such as conventional precipitation technique waste water " three take off " (vanadium removal, de- chromium, deamination) are eliminated
End governance process, the chromium in waste water are sold by commercialization recovery, high level；4., in addition to tailings in vanadium extraction, technique " solid waste " is in flow process
Recycle, tailings in vanadium extraction enters iron and steel process resourcesization and utilizes.5. present invention achieves efficient vanadium extracting, vanadium yield reaches 98%
More than.Therefore, method of this method for clean and effective vanadium extraction.
Description of the drawings
Fig. 1 is the process chart of the present invention.
Specific embodiment
Technical scheme is further illustrated below in conjunction with the accompanying drawings and by specific embodiment.
Embodiment 1：The cleaning extraction vanadium method processing step that the calcium method precipitation of this vanadium liquid, mother liquor and solid waste self-loopa are utilized is as follows
Described：
(1) calcification precipitation：Milk of lime is added to after purification in Leaching of Vanadium from Vanadium slag liquid, and addition is 1.5 of V moles in liquid phase
Times, precipitation temperature is 40 DEG C, reacts 100min, obtains the aqueous slkali of calcium vanadate and NaOH concentration for 150g/L, and aqueous slkali evaporates
It is 40% to NaOH concentration, obtains crystals of sodium chromate and crystalline mother solution, crystalline mother solution is used for vanadium slag sodium roasting additives, chromic acid
Sodium crystal purity after refined is 99.0%；
(2) ammonium hydrogen carbonate turns molten：Calcium vanadate adds ammonium bicarbonate soln transfer molten, obtains Ammonium Vanadate Solution and calcium carbonate,
Wherein ammonium bicarbonate soln concentration is 1%, and it is 10min to turn molten process reaction temperature for 20 DEG C, reaction time, turns molten process liquid solid
Than for 10:1；
(3) Crystallization Separation vanadium：Ammonium Vanadate Solution is cooled to 10 DEG C of crystallizations, obtains ammonium metavanadate crystal and crystalline mother solution, female
Liquid returns calcium vanadate and turns molten operation；
(4) calcium source regeneration：Calcium carbonate obtains CaO after 900 DEG C of calcinings, returns calcification precipitation operation.
After testing, calculate, in the present embodiment, vanadium comprehensive yield is 98.5%.
Embodiment 2：The cleaning extraction vanadium method processing step that the calcium method precipitation of this vanadium liquid, mother liquor and solid waste self-loopa are utilized is as follows
Described：
(1) calcification precipitation：Milk of lime is added to after purification in extracting vanadium from stone coal liquid, and addition is 3.0 of V moles in liquid phase
Times, precipitation temperature is 100 DEG C, reacts 10min, obtains the aqueous slkali of calcium vanadate and NaOH concentration for 10g/L, and aqueous slkali returns stone
Coal grog leaches operation；
(2) ammonium hydrogen carbonate turns molten：Calcium vanadate adds ammonium bicarbonate soln transfer molten, obtains Ammonium Vanadate Solution and calcium carbonate,
Wherein ammonium bicarbonate soln concentration is 10%, and it is 10min to turn molten process reaction temperature for 100 DEG C, reaction time, turns molten process liquid
Gu than being 4:1；
(3) Crystallization Separation vanadium：It is 50% that Ammonium Vanadate Solution supplements ammonium hydrogen carbonate to concentration, obtains ammonium metavanadate crystal and knot
Brilliant mother liquor, mother liquor return calcium vanadate and turn molten operation；
(4) calcium source regeneration：Calcium carbonate obtains CaO after 1000 DEG C of calcinings, returns calcification precipitation operation.
After testing, calculate, in the present embodiment, vanadium comprehensive yield is 98.3%.
Embodiment 3：The cleaning extraction vanadium method processing step that the calcium method precipitation of this vanadium liquid, mother liquor and solid waste self-loopa are utilized is as follows
Described：
(1) calcification precipitation：Quick lime is added to after purification in Leaching of Vanadium from Vanadium slag liquid, and addition is 2.0 of V moles in liquid phase
Times, precipitation temperature is 50 DEG C, reacts 50min, obtains the aqueous slkali of calcium vanadate and NaOH concentration for 35g/L, and aqueous slkali returns vanadium
Slag grog leaches operation；
(2) ammonium hydrogen carbonate turns molten：Calcium vanadate adds ammonium bicarbonate soln transfer molten, obtains Ammonium Vanadate Solution and calcium carbonate,
Wherein ammonium bicarbonate soln concentration is 30%, and it is 20min to turn molten process reaction temperature for 50 DEG C, reaction time, turns molten process liquid
Gu than being 5:1；
(3) Crystallization Separation vanadium：It is 40% that Ammonium Vanadate Solution supplements ammonium hydrogen carbonate to concentration, obtains ammonium metavanadate crystal and knot
Brilliant mother liquor, mother liquor return calcium vanadate and turn molten operation；
(4) calcium source regeneration：Calcium carbonate obtains CaO after 1000 DEG C of calcinings, returns calcification precipitation operation.
After testing, calculate, in the present embodiment, vanadium comprehensive yield is 98.8%.
Embodiment 4：The cleaning extraction vanadium method processing step that the calcium method precipitation of this vanadium liquid, mother liquor and solid waste self-loopa are utilized is as follows
Described：
(1) calcification precipitation：Quick lime is added in non-purified Leaching of Vanadium from Vanadium slag liquid, and addition is 2.5 of V moles in liquid phase
Times, precipitation temperature is 80 DEG C, reacts 50min, obtains the aqueous slkali of calcium vanadate and NaOH concentration for 100g/L；
(2) ammonium hydrogen carbonate turns molten：Calcium vanadate adds ammonium bicarbonate soln transfer molten, obtains Ammonium Vanadate Solution and calcium carbonate,
Wherein ammonium bicarbonate soln concentration is 40%, and it is 15min to turn molten process reaction temperature for 80 DEG C, reaction time, turns molten process liquid
Gu than being 6:1；
(3) Crystallization Separation vanadium：Ammonium Vanadate Solution is cooled to 50 DEG C of crystallizations, obtains ammonium metavanadate crystal and crystalline mother solution, female
Liquid returns calcium vanadate and turns molten operation；
(4) calcium source regeneration：Calcium carbonate obtains CaO after 950 DEG C of calcinings, returns calcification precipitation operation.
After testing, calculate, in the present embodiment, vanadium comprehensive yield is 98.9%.
Applicant states that the present invention illustrates the method detailed of the present invention, but the present invention not office by above-described embodiment
It is limited to above-mentioned method detailed, that is, does not mean that the present invention has to rely on above-mentioned method detailed and could implement.Art
Technical staff it will be clearly understood that any improvement in the present invention, to the equivalence replacement of each raw material of product of the present invention and auxiliary element
Interpolation, selection of concrete mode etc., within the scope of all falling within protection scope of the present invention and disclosure.
Claims (9)
1. the cleaning extraction vanadium method that a kind of vanadium liquid calcium method precipitation, mother liquor and solid waste self-loopa are utilized, comprises the following steps：
To after purification, vanadium liquid adds calcification additive to carry out calcium method precipitation reaction, the calcium vanadate for obtaining turn leaching occurs then anti-
Should, the Ammonium Vanadate Solution for obtaining crystallization is obtained ammonium metavanadate crystal；
The method comprising the steps of：
(1) calcification additive is added to vanadium liquid after purification, carry out calcium method precipitation reaction, isolated calcium vanadate in atmospheric conditions
Precipitation and NaOH solution；
(2) calcium vanadate that step (1) is obtained is sized mixing with ammonium bicarbonate soln, carries out turning leaching reaction, isolated ammonium vanadate is molten
Liquid and precipitation of calcium carbonate；
(3) the Ammonium Vanadate Solution crystallisation by cooling that obtains step (2) adds ammonium salt crystallization, isolated ammonium metavanadate crystal and
Crystalline mother solution；
Optionally, step (4) is carried out：
(4) calcium carbonate for obtaining step (2) decomposes through high-temperature calcination, and regeneration obtains CaO, as calcification additive, uses
Calcium vanadate is prepared in step (1), calcium source is recycled；
The calcification additive is CaO and/or Ca (OH)2；
As the NaOH concentration ＜ 150g/L in step (1) vanadium liquid, the NaOH solution that step (1) is obtained directly returns " ripe containing vanadium
The leaching of material " and washing procedure, the precipitation of leaching vanadium liquid repeat step (1) for obtaining and lock out operation,
The NaOH media of the 8～50wt% obtained after leaching and washing procedure are stayed in leaching vanadium tailing soil, are obtained in after baking
Directly utilize, the NaOH media of 50～92wt% are stayed in leaching vanadium liquid, the precipitation of repeat step (1) and lock out operation；
Be enriched to when the NaOH concentration in step (1) vanadium liquid >=150g/L after, the NaOH solution that step (1) is obtained is concentrated by evaporation
It is 40～80wt% to NaOH concentration, the NaOH solution of 40～80wt% is as sodium additive return burden process containing vanadium mineral
All of,
The NaOH solution when containing chromium obtained when step (1), chromium, will crystallize precipitation in evaporation process, refined after obtain sodium chromate product
Product；
The crystalline mother solution that step (3) is obtained returns the calcium vanadate turn leaching for step (2).
2. the method for claim 1, it is characterised in that vanadium liquid is the sodium roasting flooding of raw material containing navajoite after purification
After vanadium containing vanadium solution.
3. the method for claim 1, it is characterised in that the calcification additive addition according to Ca/V mol ratios is
1.5～3 add.
4. the method for claim 1, it is characterised in that the calcium method precipitation reaction temperature is 40～100 DEG C, during reaction
Between be 10～50min.
5. the method for claim 1, it is characterised in that described turn of leaching reaction temperature is 20～100 DEG C, when turning leaching reaction
Between for 10～100min, it is 4 to turn a leaching reaction liquid-solid ratio:1～10:1.
6. the method for claim 1, it is characterised in that the ammonium bicarbonate soln concentration in step (2) is 1～
40wt%.
7. the method for claim 1, it is characterised in that the crystallisation by cooling outlet temperature in step (3) is 0～50 DEG C.
8. the method for claim 1, it is characterised in that it is 5～50wt% that step (3) adds ammonium salt to ammonium salt concentration.
9. the method for claim 1, it is characterised in that step (4) calcining heat is 900～1000 DEG C.
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| TWI635184B (en) * | 2017-06-05 | 2018-09-11 | 虹京金屬股份有限公司 | Method for recovery of vanadium in vanadium-containing waste catalyst |
| CN107522218A (en) * | 2017-10-19 | 2017-12-29 | 河钢股份有限公司承德分公司 | A kind of ultrasound-enhanced calcium vanadate ammonium leaching and the method for preparing nano-calcium carbonate |
| CN107964601B (en) * | 2017-11-24 | 2019-06-14 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of method of chromium content in reduction calcium vanadate |
| CN107746078B (en) * | 2017-11-28 | 2023-08-11 | 河钢股份有限公司承德分公司 | System and method for preparing ammonium metavanadate crystals |
| CN108754125B (en) * | 2018-08-21 | 2020-08-04 | 王懿 | Clean process for extracting vanadium from vanadium-containing material through sodium salt roasting |
| CN109402401B (en) * | 2018-12-11 | 2020-12-04 | 中国科学院过程工程研究所 | Method for cleanly extracting vanadium from high-calcium vanadium-containing raw material |
| CN110668497A (en) * | 2019-11-01 | 2020-01-10 | 河钢股份有限公司承德分公司 | Method for preparing vanadium and chromium products from vanadium-chromium-containing double salt and application of vanadium and chromium-containing double salt |
| CN110835696A (en) * | 2019-11-26 | 2020-02-25 | 河钢股份有限公司承德分公司 | Preparation method of vanadium pentoxide |
| CN111748702B (en) * | 2020-07-06 | 2022-05-24 | 攀钢集团研究院有限公司 | Method for preparing vanadium oxide and circulating sodium and ammonium by using vanadium solution |
| CN114574699B (en) * | 2020-12-01 | 2024-03-12 | 中国科学院过程工程研究所 | Method for preparing ammonium metavanadate and ammonium molybdate from vanadium-molybdenum-containing solution |
| CN113979474A (en) * | 2021-11-26 | 2022-01-28 | 中国科学院过程工程研究所 | Method for internal circulation of ammonium carbonate medium in process of preparing vanadium pentoxide from calcium vanadate |
| CN115259223B (en) * | 2022-07-27 | 2023-11-14 | 中国科学院过程工程研究所 | Method for preparing ammonium metavanadate from calcium vanadate |
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| GB2456537A (en) * | 2008-01-17 | 2009-07-22 | Grimley Smith Associates | Process for vanadium recovery from residues |
| CN102912130A (en) * | 2012-11-13 | 2013-02-06 | 吉首大学 | Method for separating vanadium enriched in stone coal leaching solution |
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Address after: 067102 Luanhe Town, Shuangluan District, Chengde, Hebei Patentee after: River steel Limited by Share Ltd Chengde branch Address before: 067102 Luanhe Town, Shuangluan District, Chengde, Hebei Patentee before: Chengde Branch Co., Ltd. of Hebei Iron & Steel Group |
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