CN114854988A - By using CO 2 Method for selectively separating vanadium and chromium in vanadium-chromium material - Google Patents

By using CO 2 Method for selectively separating vanadium and chromium in vanadium-chromium material Download PDF

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CN114854988A
CN114854988A CN202210239235.0A CN202210239235A CN114854988A CN 114854988 A CN114854988 A CN 114854988A CN 202210239235 A CN202210239235 A CN 202210239235A CN 114854988 A CN114854988 A CN 114854988A
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vanadium
chromium
solution
separation
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王丽君
刘仕元
周国治
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University of Science and Technology Beijing USTB
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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
    • C22B7/007—Wet processes by acid 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
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/005—Preliminary treatment of scrap
    • 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
    • C22B7/006—Wet processes
    • 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

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Abstract

The invention belongs to the technical field of vanadium and chromium extraction chemical industry, and relates to a method for utilizing CO 2 A method for selectively oxidizing vanadium in a vanadium-chromium-containing material to realize vanadium-chromium separation. The method specifically comprises the following steps: mixing the vanadium-chromium-containing material and the carbonate additive uniformly, briquetting, putting into a shaft furnace filled with gas, roasting in the shaft furnace for a period of time, naturally cooling the sample to room temperature to obtain a roasted sample, crushing, adding the crushed sample into the solution, mixing, filtering the mixed solution, and separating solid and liquid to obtain a vanadium-containing solution and chromium-containing residues, thereby realizing vanadium-chromium separation. The oxidant used in the present invention is CO 2 Only vanadium in the vanadium slag is oxidized, chromium in the vanadium slag cannot be oxidized, and after water leaching, leaching solution is free of chromiumChromium fundamentally solves the problem of difficult separation of vanadium and chromium, and is obviously different from the traditional roasting process; the obtained gas is CO, and can be used as fuel.

Description

By using CO 2 Method for selectively separating vanadium and chromium in vanadium-chromium material
Technical Field
The invention relates to the technical field of vanadium and chromium extraction chemical industry, in particular to a method for utilizing CO 2 A method for selectively separating vanadium and chromium in a vanadium-chromium material.
Background
Vanadium is used as a strategic metal and has important application in the industries of steel, batteries, catalysts and the like. China produces a large amount of vanadium every year, and about 85 percent of vanadium is applied to alloy steel smelting. Chromium can improve the oxidation resistance and corrosion resistance of steel and is an important alloy element of heat-resistant steel.
The vanadium titano-magnetite is a complex symbiotic mineral rich in iron, vanadium, chromium, titanium and other valuable components, and is a significant characteristic strategic resource in China. About 145 million tons of vanadium slag is generated in the vanadium titano-magnetite smelting process in China in 2020, and the vanadium slag contains valuable metals of vanadium and chromium. V in vanadium slag 2 O 3 Content 13-19 wt.%, Cr 2 O 3 Is in an amount of 1-6 wt.%. The vanadium slag mainly comprises the following phases: spinel phases (ferrovanadium spinel, vanadochium manganese spinel and ferrotitanium spinel), silicate phases (fayalite) and metallic iron phases. Vanadium exists in ferrovanadium spinel (FeV) mainly in trivalent form 2 O 4 ) In which chromium is also present mainly in trivalent form in the hercynite (FeCr) 2 O 4 ) In (1). At present, two methods of sodium roasting-water vanadium leaching and calcification roasting-acid leaching vanadium extraction are mainly used for extracting vanadium from vanadium slag in industry. The sodium roasting-water leaching vanadium extraction is that vanadium slag powder and sodium carbonate (Na) 2 CO 3 ) Powder (sodium chloride (NaCl) and sodium sulfate (Na) are sometimes added 2 SO 4 ) The mixture is roasted in a rotary kiln or a shaft furnace for about 4 hours at 780-800 ℃, and then the roasted product is leached by hot water at 95 ℃ for half an hour, so that vanadium is transferred from a solid spinel phase to an aqueous solution. The calcium roasting-acid leaching vanadium extraction is to mix vanadium slag powder with calcium carbonate (CaCO) 3 ) Or calcium oxide (CaO) powder mixture is roasted in a rotary kiln or a shaft furnace at 825 deg.C for about 4 hours, and then the roasted product is leached with 2M sulfuric acid at 95 deg.C for half an hour, so that vanadium is transferred from the solid spinel phase to the acid solution. In patent 201410730373.4 "a method for extracting vanadium and chromium from solids" vanadium slag and sodium carbonate (Na) are disclosed 2 CO 3 ) And sodium hydroxide (NaOH) mixture roasting while extracting vanadium and chromium.
Although Na is present 2 CO 3 The vanadium slag has been used as additive for roasting vanadium slag, but the above-mentioned methods are all in the presence of O 2 The introduction of oxygen is carried out under the atmosphere, and the oxygen is not only introduced into the vanadium slagThe vanadium is oxidized, chromium in the vanadium slag is also oxidized, the vanadium and the chromium enter the solution after being leached, and the vanadium and the chromium have very similar chemical properties, so that how to separate and extract the vanadium and the chromium economically and effectively becomes a worldwide problem. In order to avoid simultaneous oxidation-leaching of vanadium and chromium into solution, alternative O was sought 2 The oxidant is the key to realize that the vanadium and the chromium are not oxidized simultaneously. Therefore, it is highly desirable to develop a method of oxidizing only vanadium, but not chromium.
Disclosure of Invention
The invention discloses a method for utilizing CO 2 The method for selectively oxidizing vanadium in a vanadium-chromium-containing material to realize vanadium-chromium separation solves any one of the above and other potential problems in the prior art.
In order to solve the problems, the technical scheme of the invention is as follows: by using CO 2 The method for selectively oxidizing vanadium in a vanadium-chromium-containing material to realize vanadium-chromium separation specifically comprises the following steps:
s1) mixing the vanadium-chromium containing material and carbonate evenly, and briquetting for later use;
s2) putting the briquetted material into an alumina crucible, putting the alumina crucible into a shaft furnace, discharging air in the shaft furnace, and continuously introducing CO 2 Heating the gas to a set temperature, then preserving heat, and naturally cooling the sample to room temperature after the heat preservation is finished;
s3) crushing the sample obtained in the step S2), adding the crushed sample into the soluble solution, continuously stirring to obtain a mixed solution, filtering and separating solid and liquid to obtain a vanadium-containing solution and chromium-containing residues, and realizing vanadium-chromium separation.
Further, the vanadium-containing material in S1) comprises any one or more of vanadium slag, vanadium titano-magnetite, vanadium mica and stone coal.
Further, the carbonate in S1) is Na 2 CO 3 、NaHCO 3 、CaCO 3 、K 2 CO 3 、KHCO 3 、MnCO 3 One or more of.
Further, the vanadium-chromium-containing material in S1): the weight ratio of the carbonate additive is 100: 35-120.
Further, the briquette in S1) requires a pressure of 5 to 20MPa and a particle diameter of 30 to 300 μm.
Further, CO in S2) 2 The flow rate of (A) is 20-2000 ml/min;
further, the predetermined temperature in S2) is, when the carbonate is Na 2 CO 3、 NaHCO 3 K 2 CO 3 、KHCO 3 、MnCO 3 The temperature is 500 ℃ and 700 ℃; when being CaCO 3 The temperature is 1000-1100 ℃.
Further, the heat preservation time in S2) is 1-8 h.
Further, the soluble solution in S3) is deionized water, hydrochloric acid, or sulfuric acid.
Further, the reaction time in S3) is 20 to 300 min.
The invention has the beneficial effects that: due to the adoption of the technical scheme, the invention uses the oxidant CO 2 Only vanadium in the vanadium-chromium containing material is selectively oxidized, and chromium in the vanadium-chromium containing material is not oxidized. Na (Na) 2 CO 3 During the roasting process, the catalyst is used as a sodium electrode and is also used for generating an oxidant CO 2 The raw materials of (1).
V 2 O 3 +CO 2 +Na 2 CO 3 =2NaVO 3 +2CO
(2) The traditional sodium treatment and calcification roasting vanadium extraction process is characterized by that it contains O 2 Calcining under an atmosphere of O 2 Due to the existence of the vanadium oxide, not only vanadium in the vanadium slag is oxidized, but also chromium in the vanadium slag, pentavalent vanadium and hexavalent chromium are all water-soluble, and after water leaching, the later-stage vanadium-chromium separation is difficult. The oxidant used in the present invention is CO 2 Only vanadium in the vanadium slag is oxidized, chromium in the vanadium slag cannot be oxidized, and after water leaching, the leaching solution is chromium-free, so that the problem of difficult separation of vanadium and chromium is fundamentally solved,
(3) in the traditional sodium roasting and calcification roasting process, CO is obtained in the oxygen atmosphere 2 The gas has great harm to the environment, and the gas obtained by the method is CO and can be used as fuel.
Drawings
FIG. 1 shows the utilization of CO according to the present invention 2 Flow chart of method for selectively separating vanadium and chromium in vanadium-chromium material
Detailed Description
The specific examples described herein are for the purpose of illustrating the invention only and are not intended to limit the invention, and it will be understood by those skilled in the art that the method of the present invention is not limited to the separation of vanadium from vanadium slag, vanadium titano-magnetite, vanadium mica and stone coal.
As shown in FIG. 1, the present invention utilizes CO 2 The method for selectively oxidizing vanadium in a vanadium-chromium-containing material to realize vanadium-chromium separation specifically comprises the following steps:
s1) mixing the vanadium-chromium containing material and carbonate evenly, and briquetting for later use;
s2) putting the briquetted material into an alumina crucible, putting the alumina crucible into a shaft furnace, discharging air in the shaft furnace, and continuously introducing CO 2 Heating the gas to a set temperature, then preserving heat, and naturally cooling the sample to room temperature after the heat preservation is finished;
s3) crushing the sample obtained in the step S2), adding the crushed sample into the soluble solution, continuously stirring to obtain a mixed solution, filtering and separating solid and liquid to obtain a vanadium-containing solution and chromium-containing residues, and realizing vanadium-chromium separation.
The vanadium-containing material in the S1) comprises any one or combination of more of vanadium slag, vanadium titano-magnetite, vanadium mica and stone coal.
The vanadium-chromium-containing material in the S1): the weight ratio of the carbonate additive is 100: 35-120.
CO in said S2) 2 The flow rate of (A) is 20-2000 ml/min; the preset temperature is 500-1000 ℃, and the heat preservation time is 1-8 h.
The pressure required by the pressing block in the S1) is 5-20MPa, and the grain diameter is 30-300 um;
the carbonate in S2) is Na 2 CO 3 、NaHCO 3 、CaCO 3 、K 2 CO 3 、KHCO 3 、MnCO 3 One or more of.
The carbonate in S2) is Na 2 CO 3、 NaHCO 3 K 2 CO 3 、KHCO 3 、MnCO 3 The temperature is 500 ℃ and 800 ℃; when being CaCO 3 The temperature is 1000-1100 ℃.
The soluble solution in the S3) is deionized water, hydrochloric acid or sulfuric acid; the stirring time is 20-300 min.
The extraction method of vanadium adopts the vanadium-containing solution obtained by the method as a raw material.
The extraction method adopts the chromium-containing residue obtained by the method as a raw material.
Example 1
2 g of dried vanadium slag powder of a certain steel and iron plant in China and 1.5 g of Na 2 CO 3 Mechanically mixing the powders, pressing the powders into blocks under 15MPa, placing into a crucible, and placing the crucible in a container filled with CO 2 Heating to 700 ℃ in a gas shaft furnace, and preserving heat for 4 hours; and cooling the oxidized vanadium slag to room temperature, crushing, putting into 100mL of deionized water, uniformly mixing for 120 minutes, filtering to obtain vanadium-containing filtrate and residue, realizing vanadium-chromium separation, wherein the oxidation rate of the separated chromium is less than 5%, separating vanadium from the vanadium-containing filtrate by a precipitation method, purifying, and reducing the residue to obtain chromium alloy.
Example 2
2 g of dried vanadium slag powder of a certain steel and iron plant in China and 1.5 g of K 2 CO 3 Mechanically mixing the powders, pressing the powders into blocks under 15MPa, placing into a crucible, and placing the crucible in a container filled with CO 2 Heating to 800 ℃ in a gas shaft furnace, and preserving heat for 3 hours; and cooling the oxidized vanadium slag to room temperature, crushing, putting into 100mL of deionized water, uniformly mixing for 120 minutes, filtering to obtain vanadium-containing filtrate and residue, realizing vanadium-chromium separation, wherein the oxidation rate of the separated chromium is less than 5%, separating vanadium from the vanadium-containing filtrate by a precipitation method, purifying, and reducing the residue to obtain chromium alloy.
Example 3
2 g of dried vanadium slag powder of a certain steel and iron plant in China and 1.5 g of CaCO 3 Mechanically mixing the powders, pressing the powders into blocks under 15MPa, placing into a crucible, and placing the crucible in a container filled with CO 2 Raising the temperature to 1000 ℃ in a gas shaft furnace, and preserving the temperature for 5 hours; cooling the oxidized vanadium slag to room temperature, crushing, putting into 100mL hydrochloric acid, uniformly mixing for 120 minutes, filtering to obtain vanadium-containing filtrate and residue, realizing vanadium-chromium separation, and separating out chromiumThe oxidation rate is less than 5 percent, the obtained vanadium-containing filtrate is purified by separating vanadium by a precipitation method, and the residue is reduced to obtain the chromium alloy.
Example 4
2 g of dried vanadium slag powder of a certain steel and iron plant in China and 2 g of Na 2 CO 3 Mechanically mixing the powders, pressing the powders into blocks under 15MPa, placing into a crucible, and placing the crucible in a container filled with CO 2 Heating the gas in a shaft furnace to 700 ℃, and preserving the heat for 6 hours; and cooling the oxidized vanadium slag to room temperature, crushing, putting into 100mL sulfuric acid, uniformly mixing for 120 minutes, filtering to obtain vanadium-containing filtrate and residue, realizing vanadium-chromium separation, wherein the oxidation rate of the separated chromium is less than 5%, separating vanadium from the vanadium-containing filtrate by a precipitation method, purifying, and reducing the residue to obtain chromium alloy.
Example 5
2 g of dried vanadium slag powder of a certain domestic iron and steel plant and 2 g of MnCO 3 Mechanically mixing the powders, pressing the powders into blocks under 15MPa, placing into a crucible, and placing the crucible in a container filled with CO 2 Heating the gas in a shaft furnace to 700 ℃, and preserving the heat for 8 hours; and cooling the oxidized vanadium slag to room temperature, crushing, putting into 100mL of deionized water, uniformly mixing for 120 minutes, filtering to obtain vanadium-containing filtrate and residue, realizing vanadium-chromium separation, wherein the oxidation rate of the separated chromium is less than 5%, separating vanadium from the vanadium-containing filtrate by a precipitation method, purifying, and reducing the residue to obtain chromium alloy.
The above embodiments of the present application provide a method for utilizing CO 2 A method for selectively separating vanadium and chromium in a vanadium-chromium material is described in detail. The above description of the embodiments is only for the purpose of helping to understand the method of the present application and its core ideas; meanwhile, for a person skilled in the art, according to the idea of the present application, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present application.
As used in the specification and claims, certain terms are used to refer to particular components. As one skilled in the art will appreciate, manufacturers may refer to a component by different names. This specification and claims do not intend to distinguish between components that differ in name but not function. In the following description and in the claims, the terms "include" and "comprise" are used in an open-ended fashion, and thus should be interpreted to mean "include, but not limited to. "substantially" means within an acceptable error range, and a person skilled in the art can solve the technical problem within a certain error range to substantially achieve the technical effect. The description which follows is a preferred embodiment of the present application, but is made for the purpose of illustrating the general principles of the application and not for the purpose of limiting the scope of the application. The protection scope of the present application shall be subject to the definitions of the appended claims.
It is also noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a good or system that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such good or system. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other like elements in a commodity or system that includes the element.
It should be understood that the term "and/or" as used herein is merely one type of association that describes an associated object, meaning that three relationships may exist, e.g., a and/or B may mean: a exists alone, A and B exist simultaneously, and B exists alone. In addition, the character "/" herein generally indicates that the former and latter related objects are in an "or" relationship.
The foregoing description shows and describes several preferred embodiments of the present application, but as aforementioned, it is to be understood that the application is not limited to the forms disclosed herein, but is not to be construed as excluding other embodiments and is capable of use in various other combinations, modifications, and environments and is capable of changes within the scope of the application as described herein, commensurate with the above teachings, or the skill or knowledge of the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the application, which is to be protected by the claims appended hereto.

Claims (10)

1. By using CO 2 The method for selectively oxidizing vanadium in a vanadium-chromium-containing material to realize vanadium-chromium separation is characterized by comprising the following steps:
s1) mixing the vanadium-chromium containing material and carbonate evenly, and briquetting for later use;
s2) putting the briquetted material into an alumina crucible, putting the alumina crucible into a shaft furnace, discharging air in the shaft furnace, and continuously introducing CO 2 Heating the gas to a set temperature, then preserving heat, and naturally cooling the sample to room temperature after the heat preservation is finished;
s3) crushing the sample obtained in the step S2), adding the crushed sample into the soluble solution, continuously stirring to obtain a mixed solution, filtering and separating solid and liquid to obtain a vanadium-containing solution and chromium-containing residues, and realizing vanadium-chromium separation.
2. The method as claimed in claim 1, wherein the vanadium-containing material in S1) comprises any one or more of vanadium slag, vanadium titano-magnetite, vanadium mica and stone coal.
3. The method as claimed in claim 1, wherein the vanadium-chromium containing material in S1): the weight ratio of the carbonate addition is 100: 35-120.
4. The method as claimed in claim 1, wherein the CO in S2) 2 The flow rate of (A) is 20-2000 ml/min; the preset temperature is 500-1000 ℃, and the heat preservation time is 1-8 h.
5. The method according to claim 1, wherein the pressure required for briquetting in S1) is 5-20MPa, and the particle size is 30-300 μm.
6. The method according to claim 4, wherein the carbonate in S1) is Na 2 CO 3 、NaHCO 3 、CaCO 3 、K 2 CO 3 、KHCO 3 、MnCO 3 One or more of.
7. The method according to claim 6, wherein the carbonate in S2) is Na 2 CO 3、 NaHCO 3 K 2 CO 3 、KHCO 3 、MnCO 3 The temperature is 500 ℃ and 800 ℃; when being CaCO 3 The temperature is 1000-1100 ℃.
8. The method as claimed in claim 1, wherein the soluble solution in S3) is deionized water, hydrochloric acid or sulfuric acid; the stirring time is 20-300 min.
9. A method for extracting vanadium, which is characterized in that the method for extracting vanadium adopts the vanadium-containing solution obtained by the method of any one of claims 1 to 8 as a raw material.
10. A method for extracting chromium, characterized in that the method comprises using the chromium-containing residue obtained by the method according to any one of claims 1 to 8 as a starting material.
CN202210239235.0A 2022-03-11 2022-03-11 By using CO 2 Method for selectively separating vanadium and chromium in vanadium-chromium material Pending CN114854988A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107236870A (en) * 2017-06-22 2017-10-10 中国科学院过程工程研究所 A kind of method of v-bearing steel slag carbonization vanadium extraction
CN107254584A (en) * 2017-06-28 2017-10-17 攀钢集团攀枝花钢铁研究院有限公司 The method of roasting and separation method of chromium vanadium titanium octahedral iron ore
CN109402400A (en) * 2018-12-11 2019-03-01 河钢股份有限公司承德分公司 The method of chromium is recycled under a kind of alkaline condition from chromium-bearing sludge

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107236870A (en) * 2017-06-22 2017-10-10 中国科学院过程工程研究所 A kind of method of v-bearing steel slag carbonization vanadium extraction
CN107254584A (en) * 2017-06-28 2017-10-17 攀钢集团攀枝花钢铁研究院有限公司 The method of roasting and separation method of chromium vanadium titanium octahedral iron ore
CN109402400A (en) * 2018-12-11 2019-03-01 河钢股份有限公司承德分公司 The method of chromium is recycled under a kind of alkaline condition from chromium-bearing sludge

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