CN112981122A - Method for recovering sodium and vanadium in sodium-modified vanadium extraction tailings - Google Patents

Method for recovering sodium and vanadium in sodium-modified vanadium extraction tailings Download PDF

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CN112981122A
CN112981122A CN202110174985.XA CN202110174985A CN112981122A CN 112981122 A CN112981122 A CN 112981122A CN 202110174985 A CN202110174985 A CN 202110174985A CN 112981122 A CN112981122 A CN 112981122A
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sodium
vanadium
dealkalized
solution
leaching
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CN112981122B (en
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张廷安
豆志河
吕国志
张伟光
刘燕
赵秋月
张子木
傅大学
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Northeastern University China
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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
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G31/00—Compounds of vanadium
    • C01G31/02—Oxides
    • 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
    • C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
    • C22B26/10—Obtaining alkali metals
    • 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
    • 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
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    • 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

A method for recovering sodium and vanadium in sodium-modified vanadium extraction tailings comprises the following steps: (1) mixing a mixed solution of sodium hydroxide and sodium vanadate with tailings of sodium salt roasting vanadium extraction to leach vanadium pentoxide in the vanadium extraction tailings to obtain a leaching solution and leaching residues; (2) mixing the leached residues, hydrated lime and clear water or alkali liquor, and removing alkali in the leached residues under the condition of pressurization to obtain dealkalized residues and dealkalized liquor with sodium hydroxide as a main component; (3) returning the dealkalized slag to a blast furnace sintering system; (4) mixing the leachate and part of dealkalized solution to a mixed solution with a certain concentration, returning part of the mixed solution to the pre-sequence sodium treatment vanadium extraction process, returning the rest of the mixed solution to the pressurized alkaline leaching process for recycling, and returning the rest of the dealkalized solution to the dealkalized process for recycling. The method realizes the comprehensive recovery of sodium and vanadium in the vanadium extraction tailings, the sodium content in the obtained dealkalized slag also meets the requirement of steel smelting, and the dealkalized slag can be directly used as a smelting raw material, thereby realizing the effective utilization of multiple components in the vanadium extraction tailings.

Description

Method for recovering sodium and vanadium in sodium-modified vanadium extraction tailings
Technical Field
The invention belongs to the field of comprehensive utilization of secondary resources, and particularly relates to a method for recovering sodium and vanadium in sodium-modified vanadium extraction tailings by using a caustic leaching and lime dealkalization method.
Background
Vanadium is 'modern industrial monosodium glutamate' and is an indispensable important material for developing modern industry, modern national defense and modern scientific technology. At present, the vanadium extraction technology mainly utilizes converter vanadium slag generated in the vanadium titano-magnetite smelting process, and adopts the processes of sodium treatment roasting vanadium extraction, calcification roasting vanadium extraction, direct pressure acid leaching vanadium extraction and the like to extract, wherein the tail slag of the sodium treatment vanadium extraction generally contains 0.5-2% of vanadium pentoxide, and can be continuously used as a raw material for vanadium extraction.
Relevant workers at home and abroad carry out a great deal of research aiming at the comprehensive utilization of vanadium extraction tailings, and in a patent of 'a method for extracting vanadium from vanadium extraction tailings' with the application number of 201210562078.3, calcium fluoride accounting for 2-6 wt% of the vanadium extraction tailings is added into the vanadium extraction tailings, sulfuric acid with the volume concentration of 10% -20% is added into the vanadium extraction tailings and the calcium fluoride according to the liquid-solid ratio of 1-2L/kg, the reaction is carried out for 1.5-2.5 hours at the temperature of 90-100 ℃, and solid-liquid separation is carried out to obtain acid leaching vanadium-containing liquid and acid leaching tailings. And adjusting the pH value of the obtained vanadium-containing acid leaching solution to 4.0-5.0 by using an alkali solution, stirring for 1-10 min at room temperature, and carrying out solid-liquid separation to obtain a vanadium-containing mixture and a treatment solution. The obtained vanadium-containing mixture is mixed with the vanadium-containing converter steel slag for recycling.
In the patent of 'method and system for treating vanadium extraction tailings' with application number 201710263180.6, vanadium extraction tailings and reduction coal are mixed and molded to obtain mixed pellets; carrying out reduction roasting treatment on the mixed pellets to obtain metallized pellets; carrying out melt separation treatment on the metallized pellets to obtain vanadium-rich slag and gallium-containing molten iron; mixing the vanadium-rich slag and sodium salt, and carrying out sodium oxide roasting treatment to obtain water-soluble sodium vanadate clinker; carrying out water immersion treatment on water-soluble sodium vanadate clinker to obtain vanadium pentoxide and first tailings; pouring gallium-containing molten iron to obtain a gallium-containing iron anode, and electrolyzing the gallium-containing iron anode to obtain gallium-containing anode mud and electrolytic iron; and extracting gallium in the gallium-containing anode mud to obtain metal gallium and second tailings.
Although the method can also realize the utilization of the vanadium extraction tailings, the comprehensive recovery of sodium and vanadium in the vanadium extraction tailings is difficult to realize, and the comprehensive utilization of the tailings is difficult.
Disclosure of Invention
Aiming at the problem of efficient comprehensive utilization of vanadium and sodium in vanadium extraction tailings, the invention provides a method for recycling sodium and vanadium in sodium-modified vanadium extraction tailings by using a method of alkaline leaching and lime dealkalization.
The invention relates to a method for recovering sodium and vanadium from sodium-modified vanadium extraction tailings, which mainly comprises the following steps:
(1) and mixing the mixed solution of sodium hydroxide and sodium vanadate with the tailings of the sodium salt roasting vanadium extraction, and then carrying out alkaline leaching treatment to leach vanadium pentoxide in the vanadium extraction tailings to obtain leachate and leaching residues.
The concentration of the adopted sodium hydroxide solution is 30-200 g/L, and Na in the mixed solution+And VO3 -The molar ratio is (15-30): 1, and the leaching temperature is 40-180 ℃. The concentration of sodium hydroxide in the obtained leaching solution is 30-200 g/L, and Na in the leaching solution+And VO3 -The molar ratio is less than 15: 1.
(2) Mixing the leached residue with hydrated lime, and carrying out calcification dealkalization treatment under the pressurization condition to remove alkali in the leached residue to obtain dealkalized residue and dealkalized liquid with sodium hydroxide as a main component. The dealkalization process is carried out in clear water or alkali liquor, if clear water is adopted, the leached residue and the slaked lime solid are added into a certain amount of clear water, and the dealkalization is carried out by pressurizing; and if alkali liquor is adopted, adding the leaching residue and the slaked lime solid into a sodium hydroxide solution with the concentration of 20-150 g/L, and pressurizing for dealkalization. Wherein the addition amount of the hydrated lime is 10-30% of the mass of the leached slag, the dealkalization reaction temperature is 120-260 ℃, and the reaction time is 20-120 min.
After dealkalization treatment, the obtained dealkalized solution is a sodium hydroxide solution with the concentration of 30-200 g/L; the obtained dealkalized slag contains less than 1 percent of sodium oxide, returns to a blast furnace sintering system for batching, and then enters a blast furnace for reduction and extraction of iron therein.
(3) Mixing one part of the obtained alkali-removed liquid with the leachate obtained in the step (1), wherein the obtained mixture is a sodium hydroxide solution with the concentration of 30-200 g/L, and Na is contained in the mixed solution+And VO3 -The molar ratio is (15-30): 1. And (3) taking a part of the mixed solution to return to the sodium treatment roasting vanadium extraction process, and returning the rest part of the mixed solution to the alkaline leaching process in the step (1). The rest part of the dealkalized liquid is directly returned to the calcification dealkalization process.
Further, mixed liquor of the alkali removing liquid and the mixed liquor returned to the process of extracting vanadium by sodium salt roasting is mixed with the leaching liquid, wherein the content of sodium oxide contained in the mixed liquor is equal to the mass of the sodium oxide entering the alkali removing liquid.
Compared with the prior vanadium extraction tailings treatment technology, the method has the advantages that:
(1) sodium hydroxide is adopted in the vanadium extraction process, other impurities are not additionally introduced, and the leaching solution and the dealkalized solution are mixed and then can directly return to the preceding sodium roasting vanadium extraction process;
(2) the pressurized dealkalization process is adopted, the dealkalization efficiency is higher, and the dealkalized slag can directly return to a blast furnace batching system to enter a reduction process.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The process flow of the embodiments 1-3 of the invention is shown in FIG. 1.
In the vanadium extraction tailings adopted by the embodiment of the invention, Na is contained2O content 5.3%, V2O51.29% of Fe2O3The content of SiO is 41.9 percent2Content of 21.9%, TiO2The content is 8.61%, and the balance is Al2O3、Cr2O3The impurities of (1).
The slaked lime used is obtained by burning limestone with a CaO content of 91% and the balance comprising SiO2The impurities of (1).
The production content of the invention is not limited to the adoption of the raw materials, and any vanadium-containing raw material can be treated by adopting the method.
Example 1
A method for recovering sodium and vanadium from sodium-modified vanadium extraction tailings comprises the following specific operation steps:
(1) and mixing the mixed solution of sodium hydroxide and sodium vanadate with the tailings of the sodium salt roasting vanadium extraction, and then carrying out alkaline leaching treatment to leach vanadium pentoxide in the vanadium extraction tailings to obtain leachate and leaching slag. The concentration of the adopted sodium hydroxide is 200g/L, and Na in the mixed solution+And VO3 -The molar ratio of (A) to (B) is 15:1, and the leaching temperature is 40 ℃. The concentration of sodium hydroxide in the leaching solution is 200g/L, and Na in the leaching solution+And VO3 -Is 12.3: 1.
(2) Mixing the leached residue with hydrated lime, and carrying out calcification dealkalization treatment under the pressurization condition to remove alkali in the leached residue to obtain dealkalized residue and dealkalized liquid with sodium hydroxide as a main component. The dealkalization process is carried out in alkali liquor, and specifically, leaching residues and slaked lime solid are added into sodium hydroxide solution with the concentration of 150g/L, and dealkalization is carried out under pressure. Wherein the addition amount of the hydrated lime is 30 percent of the leached residue, the reaction temperature is 260 ℃, and the reaction time is 120 min. After dealkalization treatment, a sodium hydroxide solution with the concentration of 200g/L, namely a dealkalized solution, is obtained. The obtained dealkalized slag contains less than 1 percent of sodium oxide, returns to a blast furnace sintering system for batching, and then enters a blast furnace for reduction and extraction of iron therein.
(3) Mixing part of the obtained alkaline solution with the leachate obtained in step (1), and obtaining a mixture of 200g/L sodium hydroxide solution and Na+And VO3 -The molar ratio was 15: 1. And (3) taking a part of the mixed solution to return to the sodium treatment roasting vanadium extraction process, and returning the rest part of the mixed solution to the alkaline leaching process in the step (1). The remaining part of the lye is removedThen returning to the calcification dealkalization process. Further, mixed liquor of the alkali removing liquid and the mixed liquor returned to the process of extracting vanadium by sodium salt roasting is mixed with the leaching liquid, wherein the content of sodium oxide contained in the mixed liquor is equal to the mass of the sodium oxide entering the alkali removing liquid. After the treatment of the method, the leaching rate of vanadium in the tailings of sodium-modified vanadium extraction is 61.7%, and the removal rate of sodium oxide is 83.9%.
Example 2
A method for recovering sodium and vanadium from sodium-modified vanadium extraction tailings comprises the following specific operation steps:
(1) and mixing the mixed solution of sodium hydroxide and sodium vanadate with the tailings of the sodium salt roasting vanadium extraction, and then carrying out alkaline leaching treatment to leach vanadium pentoxide in the vanadium extraction tailings to obtain leachate and leaching slag. The concentration of the adopted sodium hydroxide is 30g/L, and Na in the mixed solution+And VO3 -The molar ratio of (A) to (B) is 30:1, and the leaching temperature is 180 ℃. The concentration of sodium hydroxide in the leaching solution is 30g/L, and Na in the leaching solution+And VO3 -Is 12.2: 1.
(2) Mixing the leached residue with hydrated lime, and carrying out calcification dealkalization treatment under the pressurization condition to remove alkali in the leached residue to obtain dealkalized residue and dealkalized liquid with sodium hydroxide as a main component. The dealkalization process is carried out in alkali liquor, and specifically, leaching residues and slaked lime solid are added into sodium hydroxide solution with the concentration of 20g/L, and dealkalization is carried out under pressure. Wherein the addition amount of the hydrated lime is 10 percent of the leached residue, the reaction temperature is 120 ℃, and the reaction time is 20 min. After dealkalization treatment, a sodium hydroxide solution with the concentration of 30g/L, namely a dealkalized solution, is obtained. The obtained dealkalized slag contains less than 1 percent of sodium oxide, returns to a blast furnace sintering system for batching, and then enters a blast furnace for reduction and extraction of iron therein.
(3) Mixing part of the obtained alkaline solution with the leachate obtained in step (1), and obtaining a mixture of 30g/L sodium hydroxide solution and Na+And VO3 -The molar ratio was 30: 1. And (3) taking a part of the mixed solution to return to the sodium treatment roasting vanadium extraction process, and returning the rest part of the mixed solution to the alkaline leaching process in the step (1). The rest part of the dealkalized liquid is directly returned to the calcification dealkalization process. Further, with leachingThe mixed solution is mixed with a dealkalized solution and a mixed solution returned to the process of extracting vanadium by sodium salt roasting, wherein the content of sodium oxide contained in the mixed solution is equal to the mass of the sodium oxide entering the dealkalized solution. After the treatment of the method, the leaching rate of vanadium in the tailings of sodium-modified vanadium extraction is 62.3%, and the removal rate of sodium oxide is 83.7%.
Example 3
A method for recovering sodium and vanadium from sodium-modified vanadium extraction tailings comprises the following specific operation steps:
(1) and mixing the mixed solution of sodium hydroxide and sodium vanadate with the tailings of the sodium salt roasting vanadium extraction, and then carrying out alkaline leaching treatment to leach vanadium pentoxide in the vanadium extraction tailings to obtain leachate and leaching slag. The concentration of the adopted sodium hydroxide is 100g/L, and Na in the mixed solution+And VO3 -At a molar ratio of 20:1 and a leaching temperature of 110 ℃. The concentration of sodium hydroxide in the leaching solution is 100g/L, and Na in the leaching solution+And VO3 -Is 13.4: 1.
(2) Mixing the leached residue with hydrated lime, and carrying out calcification dealkalization treatment under the pressurization condition to remove alkali in the leached residue to obtain dealkalized residue and dealkalized liquid with sodium hydroxide as a main component. The dealkalization process is carried out in alkali liquor, and specifically, leaching residues and slaked lime solid are added into a sodium hydroxide solution with the concentration of 60g/L, and dealkalization is carried out under pressure. Wherein the addition amount of the hydrated lime is 20 percent of the leached residue, the reaction temperature is 180 ℃, and the reaction time is 60 min. After dealkalization treatment, a sodium hydroxide solution with the concentration of 100g/L, namely dealkalized liquid, is obtained. The obtained dealkalized slag contains less than 1 percent of sodium oxide, returns to a blast furnace sintering system for batching, and then enters a blast furnace for reduction and extraction of iron therein.
(3) Mixing part of the obtained alkaline solution with the leachate obtained in step (1), and obtaining a mixture of 100g/L sodium hydroxide solution and Na+And VO3 -The molar ratio was 20: 1. And (3) taking a part of the mixed solution to return to the sodium treatment roasting vanadium extraction process, and returning the rest part of the mixed solution to the alkaline leaching process in the step (1). The rest part of the dealkalized liquid is directly returned to the calcification dealkalization process. Further, the mixed alkali solution is removed and sodium salt roasting is returned to extract vanadiumThe content of the sodium oxide in the mixed liquid is equal to the mass of the sodium oxide entering the alkali removing liquid. After the treatment of the method, the leaching rate of vanadium in the tailings of sodium-modified vanadium extraction is 61.5%, and the removal rate of sodium oxide is 84.2%.

Claims (3)

1. A method for recovering sodium and vanadium in sodium-modified vanadium extraction tailings is characterized by comprising the following steps:
(1) mixing a mixed solution of sodium hydroxide and sodium vanadate with tailings of sodium salt roasting vanadium extraction, and then carrying out alkaline leaching treatment to leach vanadium pentoxide in the vanadium extraction tailings to obtain a leaching solution and leaching residues; the concentration of the adopted sodium hydroxide solution is 30-200 g/L, and Na in the mixed solution+And VO3 -The molar ratio is (15-30): 1, and the leaching temperature is 40-180 ℃; the concentration of sodium hydroxide in the obtained leaching solution is 30-200 g/L, and Na in the leaching solution+And VO3 -The molar ratio is less than 15: 1;
(2) mixing the leached residues with hydrated lime, and carrying out calcification dealkalization treatment under the pressurization condition to remove alkali in the leached residues to obtain dealkalized residues and dealkalized solution with sodium hydroxide as a main component; the addition amount of the slaked lime is 10-30% of the mass of the leached slag, the dealkalization reaction temperature is 120-260 ℃, and the reaction time is 20-120 min; the concentration of the obtained alkali-removed liquid is 30-200 g/L;
(3) mixing one part of the obtained alkali-removed liquid with the leachate obtained in the step (1), wherein the obtained mixture is a sodium hydroxide solution with the concentration of 30-200 g/L, and Na is contained in the mixed solution+And VO3 -The molar ratio is (15-30) to 1; taking a part of the mixed solution to return to the sodium treatment roasting vanadium extraction process, and returning the rest part of the mixed solution to the alkaline leaching process in the step (1); the rest part of the dealkalized liquid is directly returned to the calcification dealkalization process.
2. The method for recovering sodium and vanadium from the sodium-modified vanadium extraction tailings according to claim 1, wherein the step (2), dealkalization is carried out in clear water or alkali liquor; adding the leached slag and the slaked lime solid into a certain amount of clear water for dealkalization by pressure; adding the leaching residue and the slaked lime solid into a sodium hydroxide solution with the concentration of 20-150 g/L by adopting an alkali solution, and pressurizing to remove alkali; the content of sodium oxide in the obtained dealkalized slag is lower than 1 percent and the obtained dealkalized slag returns to a blast furnace sintering system.
3. The method for recovering sodium and vanadium from the tailings of sodium-modified vanadium extraction according to claim 1, wherein the mixed liquor of the dealkalization liquid mixed with the leachate and the returned vanadium extraction process of sodium-modified roasting contains sodium oxide with the content equal to the mass of the sodium oxide entering the dealkalization liquid.
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CN115216635A (en) * 2022-07-18 2022-10-21 中南大学 Method for removing alkali metal by reinforced vanadium extraction tailings calcification roasting-leaching
CN115216635B (en) * 2022-07-18 2023-07-21 中南大学 Method for removing alkali metal by calcified roasting-leaching of reinforced vanadium extraction tailings

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