CN106591587B - A kind of method of containing vanadium and chromium reducing slag selective oxidation alkali leaching separation vanadium chromium - Google Patents

A kind of method of containing vanadium and chromium reducing slag selective oxidation alkali leaching separation vanadium chromium Download PDF

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Publication number
CN106591587B
CN106591587B CN201611235225.0A CN201611235225A CN106591587B CN 106591587 B CN106591587 B CN 106591587B CN 201611235225 A CN201611235225 A CN 201611235225A CN 106591587 B CN106591587 B CN 106591587B
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vanadium
chromium
reducing slag
alkali
selective oxidation
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CN106591587A (en
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王明玉
陈边防
黄胜
王学文
刘彪
高大雄
孟钰麒
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Central South University
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Central South University
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • C22B7/008—Wet processes by an alkaline or ammoniacal leaching
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/20—Obtaining niobium, tantalum or vanadium
    • C22B34/22—Obtaining vanadium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/30—Obtaining chromium, molybdenum or tungsten
    • C22B34/32—Obtaining chromium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/04—Working-up slag
    • 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
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Abstract

The invention discloses a kind of method that containing vanadium and chromium reducing slag selective oxidation alkali soaks separation vanadium chromium, and the solution of containing vanadium and chromium reducing slag, alkali and pentavalent vanadium source is placed in closed container and alkali soaks at 110~250 DEG C, and it is 8~14 to control alkali leaching reaction end pH；Obtain through separation of solid and liquid containing vanadium leachate and chromium slag after.The method of the present invention is using pentavalent vanadium source as oxidant, coordinate again it is of the present invention under confined conditions, the regulation and control of temperature and reaction end pH, vanadium that can be in cooperative achievement vanadium chromium reducing slag is directly separated in the form of tetravalence with chromium, compared to alkali soaking technology after existing initial oxidation, the selective higher of the method for the present invention, V leaching rate is more than 98.7%.

Description

A kind of method of containing vanadium and chromium reducing slag selective oxidation alkali leaching separation vanadium chromium
Technical field
The present invention relates to vanadium chromium reducing slag metal separation technology field, and in particular to a kind of containing vanadium and chromium reducing slag selectivity oxygen The method of choline leaching separation vanadium chromium.
Background technology
Vanadium is similar with chromium property, nature they preservation is in mineral usually in a manner of symbiosis, wherein v-ti magnetite Ore deposit is exactly the Typical Representative of this kind of mineral.The slag containing chrome alum that v-bearing titanomagnetite smelting process produces is the master of vanadic anhydride production Want raw material.The deposition vanadium mother liquid of a large amount of V containing low concentration (V) and Cr (VI) can be produced after this Leaching of Vanadium from Vanadium slag containing chromium, precipitation at present is female Liquid processing obtains a large amount of containing vanadium and chromium reducing slags, wherein vanadium is mainly with V after treatment using the mode of reduction-neutralization2O4 Form exists, remaining is with V2O3Form exist, chromium is mainly with Cr (OH)3Form exist；In reducing slag in addition to vanadium chromium also There are silicon, phosphorus etc..Phosphorous chemical industry enterprise and special steel smelt additive enterprise can also produce a large amount of containing vanadium and chromium reducing slags in production process.
The decomposition of containing vanadium and chromium reducing slag is main by the way of Ore Leaching at present, but due to the presence of silicon in vanadium chromium reducing slag So that acid leaching liquor filtration difficulty, and V (IV), V (III) and Cr (III) process complexity, flow are separated and recovered from leachate It is long, it is of high cost.Low Valent Vanadium can be oxidized to pentavalent vanadium and be realized the leaching of vanadium by hydrogen peroxide for oxidant using sodium hydroxide solution Go out, but leaching process Cr (III) can also be aoxidized, vanadium chromium inferior separating effect, and dioxygen water consumption is big, of high cost, no economy Application.Other mineral decomposition methods of containing vanadium and chromium reducing slag have sodium roasting method, calcification baking method, sub-molten salt method etc., these It is first V (V) and Cr (VI) by vanadium and chromium simultaneous oxidation that the common ground of method, which is all, then the separation and Extraction pentavalent from aqueous solution again Vanadium and Cr VI.But since V (V) is similar with the solution chemistry of Cr (VI), vanadium and chromium in separation and recovery solution are the world The problem of property.At present in solution the separation and recovery method of V (V) and Cr (VI) have it is a variety of, including solvent extraction, ion hand over Change method and the electronation precipitation method etc., but all there are the problem of of high cost, long flow path for which kind of method.
The content of the invention
For it is above-mentioned in the prior art to the various treatment technologies of containing vanadium and chromium reducing slag there are the defects of, the purpose of the present invention It is that provide a kind of leached based on selective oxidation combination alkali carries out high temperature high pressure process to vanadium chromium reducing slag, can realize that vanadium is efficient The method of Selectively leaching, this method V leaching rate is high, and vanadium chromium good separating effect, easy to operate, cost is low, disclosure satisfy that industry Change production requirement；Trivalent chromium can be recycled by Precipitation method after slag acidleach after Leaching Vanadium.
A kind of method of containing vanadium and chromium reducing slag selective oxidation alkali leaching separation vanadium chromium, by containing vanadium and chromium reducing slag, alkali and pentavalent The solution in vanadium source is placed in closed container and alkali soaks at 110~250 DEG C, and it is 8~14 to control alkali leaching reaction end pH；Passed through after Separation of solid and liquid obtains containing vanadium leachate and chromium slag.
In the present invention, using pentavalent vanadium source as oxidant, then coordinate it is of the present invention under confined conditions, temperature and anti- The regulation and control of terminal pH are answered, vanadium that can be in cooperative achievement vanadium chromium reducing slag is directly separated in the form of tetravalence with chromium, compared to existing Alkali soaking technology after initial oxidation, the selective higher of the method for the present invention, V leaching rate is more than 98.7%.
In the present invention, control alkali soaks terminal pH 8~14；Be conducive to improve V leaching rate and vanadium chromium separating effect.This hair In bright, the regulation and control of the alkali leaching terminal pH, it is believed that the OH of control alkali leaching reaction end system-Concentration is 10-6~1moL/L.
To regulate and control the pH of alkali leaching terminal well in the scope, present invention also offers a kind of preferable embodiment party Case, with the aqueous slkali that pH is 8~14 is after 1: 1.5~10g/mL is mixed by solid-to-liquid ratio by containing vanadium and chromium reducing slag；Pentavalent is added again Vanadium source, and changed into by total vanadium in vanadium chromium reducing slag1~5 times of required theoretical molar amount adds alkali；Then again close Alkali leaching is carried out under the conditions of closing.
The inventors discovered that by the preferred embodiment, the pH of alkali leaching terminal can be effectively controlled in the model In enclosing, so as to further lift the leaching rate of vanadium in vanadium chromium reducing slag, the leaching of chromium is reduced.
Preferably, the pH of alkali leaching terminal is 10~14.It that is to say, the OH of control alkali leaching reaction end-Concentration is 10-4~ 1moL/L。
In the present invention, the pentavalent vanadium source includes at least the oxide and/or salt of pentavalent vanadium.
For example, pentavalent vanadium source can be the oxide of pentavalent vanadium；And/or the water miscible salt of pentavalent vanadium；And/or pentavalent vanadium The oxide or salt that can be dissolved in alkaline aqueous solution；And/or pentavalent vanadium the oxide that can be dissolved in an acidic solution or Salt.
Preferably, the pentavalent vanadium source is V2O5, metavanadate, positive vanadate, at least one of pyrovanadate.
Metavanadate (the MVO3), positive vanadate (MVO4), pyrovanadate (MV2O7) it is preferably respective acid ion Alkali metal salt, ammonium salt.
For example, the metavanadate is preferably at least one of sodium salt, sylvite, lithium salts or ammonium salt of metavanadic acid root. The positive vanadate is preferably at least one of sodium salt, sylvite, lithium salts or ammonium salt of positive vanadic acid root.The pyrovanadate Preferably at least one of the sodium salt of pyrovanadium acid group, sylvite, lithium salts or ammonium salt.
Further preferably, the pentavalent vanadium source is selected from V2O5、Na3VO4、Na4V2O7、NaVO3、NH4VO3In at least one Kind.
In the present invention, the pentavalent vanadium source can also add in addition to it directly can add solid and include the pentavalent vanadium source Solution；The for example, acid solution in pentavalent vanadium source, alkaline solution or aqueous solution.
In the present invention, the mole that adds in pentavalent vanadium source is that V (III) in vanadium chromium reducing slag is oxidized to reason needed for V (IV) By 1~2 times of mole.
The inventors discovered that coordinate the high-selectivity oxidation agent, under confined space and pressure that the temperature is built The alkali leaching is carried out under power atmosphere, contributes to the leaching rate of further lifting vanadium.
Preferably, alkali leaching temperature is 140~180 DEG C.
In the present invention, the alkali is the hydroxide and/or carbonate of alkali metal.
The aqueous slkali is the hydroxide of alkali metal and/or the aqueous solution of carbonate.
Preferably, the aqueous slkali is at least one of sodium hydroxide, sodium carbonate, potassium hydroxide, potassium carbonate Aqueous solution.
Further preferably, the aqueous slkali is sodium hydroxide and/or the aqueous solution of sodium carbonate.
In the present invention, the alkali subsequently added is the hydroxide and/or carbonate of alkali metal；Preferably sodium hydroxide, carbon At least one of sour sodium, potassium hydroxide, potassium carbonate；More preferably sodium hydroxide and/or sodium carbonate.
In the present invention, the alkali subsequently added and identical with the alkali (alkali introduced in aqueous slkali) of vanadium chromium reducing slag hybrid reaction It is or different.
In the present invention, in confined conditions, the alkali that the dipped journey of alkali is added adds mole to make in containing vanadium and chromium reducing slag Total vanadium reaction into1~5 times of required theoretical molar amount；Preferably 1.5~3 times.
In the present invention, the alkali leaching time is 0.5~5h；The preferable alkali leaching time is 2~4h.
A kind of method for the containing vanadium and chromium reducing slag selective oxidation alkali leaching separation vanadium chromium being more highly preferred to of the present invention, including it is following Step：
Step (1)：With the aqueous slkali that pH is 8~14 it is that 1: 1.5~10g/mL is mixed by solid-to-liquid ratio by containing vanadium and chromium reducing slag, The aqueous slkali is sodium hydroxide, sodium carbonate, potassium hydroxide, at least one aqueous solution of potassium carbonate；
Step (2)：The mixed liquor of step (1) is placed in autoclave, and by V (III) oxygen in containing vanadium and chromium reducing slag Turn to 1~2 times of addition V of V (IV) theoretical amount2O5、Na3VO4、Na4V2O7、NaVO3、NH4VO3At least one of as oxidation Agent；Generated by total vanadium in containing vanadium and chromium reducing slag and alkali reaction1~5 times of theoretical amount adds sodium hydroxide, sodium carbonate, hydrogen At least one of potassium oxide, potassium carbonate alkali；After confined reaction leaches 0.5~5h at 110~250 DEG C again, separation of solid and liquid obtains Containing vanadium leachate and chromium slag.
In the present invention, most preferably containing vanadium and chromium reducing slag selective oxidation alkali soaks the method for separation vanadium chromium, wherein,
Step (1)：With the aqueous slkali that pH is 8~14 it is that 1: 2~5g/mL is mixed by solid-to-liquid ratio by containing vanadium and chromium reducing slag, institute The aqueous slkali stated is sodium hydroxide, at least one aqueous solution of sodium carbonate；
Step (2)：The mixed liquor of step (1) is placed in autoclave, and by V (III) oxygen in containing vanadium and chromium reducing slag Turn to 1~2 times of addition V of V (IV) theoretical amount2O5、NaVO3、NH4VO3At least one of be used as oxidant；Reduced by containing vanadium and chromium Total vanadium is generated with alkali reaction in slag1.5~3 times of theoretical amount add sodium hydroxide, sodium carbonate, potassium hydroxide, potassium carbonate At least one of alkali；After 2~4h is leached in reaction under the conditions of 140~180 DEG C of the confined condition again, separation of solid and liquid must contain vanadium leaching Liquid.
It is of the invention to be had the following advantages compared with existing technology and effect：
Vanadium is mainly with V in containing vanadium and chromium reducing slag2O4Form exists, and chromium is mainly with Cr (OH)3Form exists, and the present invention utilizes V2O4With Cr (OH)3Reacting generation soluble-salt with aqueous slkali, it dissolves difference existing for pH, by controlling the pH of leachate, directly The Selectively leaching for realizing V (IV) is connect, is alkali soaking technology after pentavalent vanadium compared to existing pre-oxidation Low Valent Vanadium, it is of the invention Selective higher, cost are lower；Additionally due to remaining vanadium is with V in containing vanadium and chromium reducing slag2O3Form exists, it does not dissolve in alkali, this Invention cleverly utilizes E in alkaline conditions0 Cr(III)/Cr(VI)With E0 v(IV)/v(v)Difference existing for current potential, with the compound of V (V) Or solution makees oxidant, by V (III) selective oxidations in solution into the V (IV) that can be dissolved in aqueous slkali, so as to improve vanadium Leaching rate, and Cr (III) is not oxidized.The present invention does not introduce new impurity, and the efficient selective for realizing vanadium leaches, vanadium leaching Extracting rate is more than 98.7%, and chromium leaching rate is less than 0.5%, and short with technological process, processing cost is low, easy to operate, is suitable for The advantages that industrial applications.
Embodiment
Following embodiments are intended to illustrate invention, rather than the further of protection scope of the present invention is limited.
Embodiment 1
The containing vanadium and chromium reducing slag 500g containing 6.3% vanadium and 14.1% chromium is taken by the carbonic acid that solid-to-liquid ratio 1: 3g/mL and pH is 10 Sodium solution mixes in autoclave, and the theoretical molar amount of V (IV) is then oxidized to by V (III) in containing vanadium and chromium reducing slag 1.5 times of addition V2O5, generated by total vanadium in containing vanadium and chromium reducing slag and alkali reaction2.5 times of addition hydrogen-oxygens of theoretical molar amount Change sodium, reaction leaching 3h under conditions of being 140 DEG C in temperature, pH value of solution is the 13.5 (OH of reaction end system after the completion of reaction- For 0.32moL/L), separation of solid and liquid after cooling.The leaching rate of vanadium is 99.1%, and chromium leaching rate is 0.45%.
Embodiment 2
The containing vanadium and chromium reducing slag 1000g containing 4.1% vanadium and 10.1% chromium is taken by the carbonic acid that solid-to-liquid ratio 1: 2g/mL and pH is 12 Potassium solution mixes in autoclave, and the theoretical molar amount of V (IV) is then oxidized to by V (III) in containing vanadium and chromium reducing slag 1.2 times of addition NaVO3, generated by total vanadium in containing vanadium and chromium reducing slag and alkali reaction1.5 times of addition hydrogen of theoretical molar amount Potassium oxide, reaction leaching 2h under conditions of being 180 DEG C in temperature, pH value of solution is the 13 (OH of reaction end system after the completion of reaction- For 0.1moL/L), separation of solid and liquid after cooling.The leaching rate of vanadium is 98.7%, and chromium leaching rate is 0.28%.
Embodiment 3
The containing vanadium and chromium reducing slag 500g containing 7.1% vanadium and 1.8% chromium is taken by the hydroxide that solid-to-liquid ratio 1: 5g/mL and pH is 13 Sodium solution mixes in autoclave, and the 2 of the theoretical molar amount of V (IV) is then oxidized to by V (III) in containing vanadium and chromium reducing slag NH is added again4VO3, generated by total vanadium in containing vanadium and chromium reducing slag and alkali reaction3 times of addition sodium carbonate of theoretical molar amount, 4h is leached in reaction under conditions of being 160 DEG C in temperature, and pH value of solution is the 14 (OH of reaction end system after the completion of reaction-For 1moL/ L), separation of solid and liquid after cooling.The leaching rate of vanadium is 99.5%, and chromium leaching rate is 0.11%.
Comparative example 1
Take the containing vanadium and chromium reducing slag 500g containing 6.3% vanadium and 14.1% chromium to size mixing by solid-to-liquid ratio 1: 3g/mL, then press and contain vanadium V (III) is oxidized to 1.5 times of addition V of the theoretical molar amount of V (IV) in chromium reducing slag2O5, leaching under conditions of 100 DEG C 4h, it is 13.5 during which to add sodium hydroxide and control solution terminal pH, separation of solid and liquid.The leaching rate of vanadium is 70.5%, chromium leaching rate For 0.08%.
Comparative example 2
Take the containing vanadium and chromium reducing slag 500g containing 6.3% vanadium and 14.1% chromium to size mixing by solid-to-liquid ratio 1: 3g/mL, then add double Oxygen water (30%) 25ml, leaching 4h under conditions of 100 DEG C, during which add sodium hydroxide and controls solution terminal pH as 13.5, Separation of solid and liquid.The leaching rate of vanadium is 88.1%, and chromium leaching rate is 9.8%.
Comparative example 3
The containing vanadium and chromium reducing slag 500g containing 6.3% vanadium and 14.1% chromium is taken by the carbonic acid that solid-to-liquid ratio 1: 3g/mL and pH is 10 Sodium solution mixes in autoclave, and the theoretical molar amount of V (IV) is then oxidized to by V (III) in containing vanadium and chromium reducing slag 1.5 times of addition V2O5, generated by total vanadium in containing vanadium and chromium reducing slag and alkali reaction4 times of addition hydroxides of theoretical molar amount Sodium, reaction leaching 3h under conditions of being 140 DEG C in temperature, pH value of solution is more than the 15 (OH of reaction end system after the completion of reaction-It is dense Degree is more than 10moL/L), separation of solid and liquid after cooling.The leaching rate of vanadium is 99.8%, and chromium leaching rate is 19.7%.

Claims (10)

  1. A kind of 1. method of containing vanadium and chromium reducing slag selective oxidation alkali leaching separation vanadium chromium, it is characterised in that by containing vanadium and chromium reducing slag, Alkali and the solution in pentavalent vanadium source are placed in closed container and alkali soaks at 110~250 DEG C, control alkali leaching reaction end pH be 8~ 14；Obtain through separation of solid and liquid containing vanadium leachate and chromium slag after.
  2. 2. the method for containing vanadium and chromium reducing slag selective oxidation alkali leaching separation vanadium chromium as claimed in claim 1, it is characterised in that will Containing vanadium and chromium reducing slag is after 1: 1.5~10g/mL is mixed by solid-to-liquid ratio with the aqueous slkali that pH is 8~14；Pentavalent vanadium source is added again, And changed into by total vanadium in vanadium chromium reducing slag1~5 times of required theoretical molar amount adds alkali；Then again in confined condition Lower progress alkali leaching.
  3. 3. the method for containing vanadium and chromium reducing slag selective oxidation alkali leaching separation vanadium chromium as claimed in claim 1 or 2, its feature exist In the pentavalent vanadium source includes at least the oxide and/or salt of pentavalent vanadium.
  4. 4. the method for containing vanadium and chromium reducing slag selective oxidation alkali leaching separation vanadium chromium as claimed in claim 3, it is characterised in that institute The pentavalent vanadium source stated is V2O5, metavanadate, positive vanadate, at least one of pyrovanadate.
  5. 5. the method for containing vanadium and chromium reducing slag selective oxidation alkali leaching separation vanadium chromium as claimed in claim 3, it is characterised in that institute The pentavalent vanadium source stated is selected from V2O5、Na3VO4、Na4V2O7、NaVO3、NH4VO3At least one of.
  6. 6. the method for containing vanadium and chromium reducing slag selective oxidation alkali leaching separation vanadium chromium as claimed in claim 5, it is characterised in that five The mole that adds in valency vanadium source is 1~2 times that V (III) in vanadium chromium reducing slag is oxidized to theoretical molar amount needed for V (IV).
  7. 7. the method for containing vanadium and chromium reducing slag selective oxidation alkali leaching separation vanadium chromium as claimed in claim 1, it is characterised in that alkali It is 140~180 DEG C to soak temperature.
  8. 8. the method for containing vanadium and chromium reducing slag selective oxidation alkali leaching separation vanadium chromium as claimed in claim 1, it is characterised in that alkali The pH for soaking terminal is 10~14.
  9. 9. the method for containing vanadium and chromium reducing slag selective oxidation alkali leaching separation vanadium chromium as claimed in claim 1, it is characterised in that institute The alkali stated is the hydroxide and/or carbonate of alkali metal.
  10. 10. the method for containing vanadium and chromium reducing slag selective oxidation alkali leaching separation vanadium chromium as claimed in claim 1, it is characterised in that The alkali leaching time is 0.5~5h.
CN201611235225.0A 2016-12-28 2016-12-28 A kind of method of containing vanadium and chromium reducing slag selective oxidation alkali leaching separation vanadium chromium Expired - Fee Related CN106591587B (en)

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CN107287453B (en) * 2017-06-22 2020-04-21 河钢股份有限公司承德分公司 Method for extracting vanadium from vanadium-containing steel slag by ion replacement method
CN107805710B (en) * 2017-10-23 2019-03-12 中国科学院过程工程研究所 A method of the silicate mineral synthetical recovery silicon of vanadium containing multivalent state and vanadium
CN113684376A (en) * 2021-07-19 2021-11-23 宁波双能环保科技有限公司 Method for extracting vanadium from magnesium sulfate phosphorus slag by using high-pressure kettle
CN115305357B (en) * 2022-08-17 2023-09-05 四川省银河化学股份有限公司 Method for preparing sodium chromate by taking vanadium-chromium reduction slag as raw material

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