CN115323181B - Method for recovering vanadium from calcified vanadium extraction tailings - Google Patents
Method for recovering vanadium from calcified vanadium extraction tailings Download PDFInfo
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- CN115323181B CN115323181B CN202211121765.1A CN202211121765A CN115323181B CN 115323181 B CN115323181 B CN 115323181B CN 202211121765 A CN202211121765 A CN 202211121765A CN 115323181 B CN115323181 B CN 115323181B
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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
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/005—Preliminary treatment of scrap
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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
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention discloses a method for recovering vanadium from calcified vanadium extraction tailings, and belongs to the technical field of metallurgy. The method comprises the following steps: step one: pulping calcified vanadium extraction tailings; step two: adding calcium oxide into the slurry prepared in the step one, regulating the pH value to 10-13, and reacting for 5-15 min; step three: adding sulfuric acid into the system of the second step, regulating the pH value to 0.5-2.5, performing secondary leaching, and performing solid-liquid separation after reacting for 10-30 min to obtain vanadium-containing solution and secondary leaching tailings with low vanadium content. The invention adopts the tailings produced by the calcified roasting-sulfuric acid leaching process as raw materials, and uses calcium oxide to convert the vanadic anhydride which is not dissolved by acid in the tailings and is produced by hydrolysis and precipitation of vanadium and is not dissolved by acid into calcium vanadate dissolved by acid, and then the acid can be leached by acid, thereby having the characteristics of high vanadium recovery rate, low cost, simple operation, less slag quantity increase and the like.
Description
Technical Field
The invention belongs to the technical field of metallurgy, and particularly relates to a method for recovering vanadium from calcified vanadium extraction tailings.
Background
Vanadium is mainly applied to the field of steel, and the performance of the steel is obviously improved. At present, two processes of calcification roasting, sulfuric acid leaching, ammonium salt vanadium precipitation, sodium roasting, water leaching and ammonium salt vanadium precipitation are mainly adopted for vanadium extraction. Wherein the vanadium slag is subjected to calcified roasting-acid leaching to produce acid leaching residues, the vanadium extraction tailings produced by the vanadium industry in China are more than 120 ten thousand tons each year, the vanadium content is 1.4-1.7%, and the vanadium content is high, so that the method belongs to serious resource waste. Therefore, there are many patent documents to study how to reduce the content of TV (all vanadium) in the tailings, and most of the methods are to reduce the pH value and to calcine the tailings with calcium again.
For example, patent document CN114410988A discloses a method for deep extraction of vanadium by using vanadium extraction tailings, which specifically includes: grinding the vanadium extraction tailings, adding a carbonaceous reducing agent and a sodium salt additive, reacting for 1-5 hours at 600-750 ℃, leaching after the reaction is finished, and carrying out solid-liquid separation to obtain a vanadium-containing solution; the carbonaceous reducing agent is at least one of semi-coke or coke, the sodium salt additive is at least one of sodium vanadate or sodium chloride, the method realizes the deep vanadium extraction of vanadium extraction tailings at 600-750 ℃ and recycles valuable elements in the vanadium extraction tailings, wherein the obtained leaching slag can be directly used for blast furnace ore blending and iron making, the obtained vanadium-containing solution can be used for vanadium crystallization, and meanwhile, the process equipment is simple and easy to operate, the whole process flow is in closed cycle, and the method is clean and environment-friendly and has good economic benefit and application prospect. For another example, patent document CN112981122B discloses a method for recovering sodium and vanadium from a sodium-modified vanadium extraction tailings, comprising: (1) Mixing the mixed solution of sodium hydroxide and sodium vanadate with the tailings of the sodium roasting vanadium extraction, and leaching the vanadium pentoxide in the tailings of the vanadium extraction to obtain a leaching solution and leaching residues; (2) Mixing the leaching residue with slaked lime and clear water or alkali liquor, and removing alkali in the leaching residue under the condition of pressurization to obtain dealkalized residue and dealkalized liquor with sodium hydroxide as a main component; (3) the dealkalized slag is returned to a blast furnace sintering system; (4) The method realizes the comprehensive recovery of sodium and vanadium in the vanadium extraction tailings, and the sodium content in the obtained dealkalized slag also meets the requirements of steel smelting, can be directly used as smelting raw materials, and realizes the effective utilization of multiple components in the vanadium extraction tailings. For another example, patent document CN109355515B provides a method for extracting vanadium from calcified vanadium extraction tailings, comprising the steps of: roasting the calcified vanadium extraction tailings to obtain roasting clinker, carrying out acid leaching, collecting leaching liquid, adding a impurity removing agent, carrying out solid-liquid separation, collecting liquid phase matters, precipitating vanadium, and calcining to obtain vanadium pentoxide, wherein the vanadium extraction method can obtain a qualified product with the purity of vanadium pentoxide being more than 98%, the TV content in the tailings after vanadium extraction is less than or equal to 0.6%, and the wastewater is recycled. For another example, patent document CN109182760B discloses a method for recovering and extracting vanadium from calcified vanadium extraction tailings, comprising: controlling the water content of calcified vanadium extraction tailings to be 30-35 wt%, and drying and crushing to obtain a material A; supplementing limestone to the material A, controlling the calcium-vanadium ratio of the system to be 0.3-0.8, uniformly mixing, roasting and cooling to obtain a roasting material; the method further extracts vanadium components in the tailings by carrying out secondary roasting and leaching on the primary calcified roasting vanadium extraction tailings, so that the full recycling of vanadium in the vanadium tailings is realized, the leaching rate can reach more than 60%, the resource waste is avoided, and the method is simple and easy to use and has a value of wide popularization. For another example, patent document CN109338103B discloses a method for countercurrent acid leaching of vanadium from calcified roasting clinker, comprising the steps of: a. mixing clinker with the first-stage filtrate or/and the second-stage leaching solution, adding sulfuric acid for leaching, controlling the pH value of a first-stage leaching process system to be 2.8-3.5, and carrying out solid-liquid separation to obtain the first-stage leaching solution and solid; washing to obtain a first-stage filtrate and a solid; b. leaching the solid by using third-stage leaching liquid or/and third-stage filtrate, controlling the pH value of a second-stage leaching terminal system to be 1.8-3.5, and carrying out solid-liquid separation to obtain second-stage leaching liquid and solid; c. leaching the solid, controlling the pH value of a third-stage leaching end point system to be 1.4-2.2, and carrying out solid-liquid separation to obtain a third-stage leaching solution and the solid; the third-stage filtrate and the vanadium extraction tailings are obtained by washing, and the method has the advantages of high extraction rate and low cost.
The prior art reduces the vanadium content in the tailings by reducing the pH value or roasting the tailings again, however, the calcified vanadium extraction tailings have higher water content and higher mixing roasting difficulty, and the tailings have relatively lower TV content, so that the vanadium extraction is difficult, the overall vanadium recovery rate is not high but the cost is not low, the operation is complex, and the slag amount is increased greatly.
In view of this, the prior art is in need of improvement.
Disclosure of Invention
Aiming at the problems of the prior art, the invention provides a method for recovering vanadium from calcified vanadium extraction tailings, which has high vanadium recovery rate, low cost, no need of roasting again and little slag increase.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
according to the invention, there is provided a method for recovering vanadium from calcified vanadium extraction tailings, the method comprising the steps of: step one: pulping calcified vanadium extraction tailings; step two: adding calcium oxide into the slurry prepared in the step one, regulating the pH value to 10-13, and reacting for 5-15 min; step three: adding sulfuric acid into the system of the second step, regulating the pH value to 0.5-2.5, performing secondary leaching, and performing solid-liquid separation after reacting for 10-30 min to obtain vanadium-containing solution and secondary leaching tailings with low vanadium content.
According to one embodiment of the invention, in the first step, the pulping liquid-solid ratio is 1-2.0 ml to 1g.
According to one embodiment of the invention, in the first step, the water content of the calcified vanadium extraction tailings is 30-50%.
According to one embodiment of the invention, in the first step, the self water content of the calcified vanadium extraction tailings is calculated when the slurry solid ratio is calculated.
According to one embodiment of the invention, in step one, the beating temperature is 10-60 ℃.
According to one embodiment of the invention, in the second step, the addition amount of the calcium oxide is 1.5% -4.5% of the mass of the calcified vanadium extraction tailings.
In step three, according to one embodiment of the present invention, 25% to 50% by volume of sulfuric acid is used.
According to one embodiment of the invention, in step three, the secondary leaching temperature is 10-60 ℃.
According to one embodiment of the invention, in step three, the secondary leach tailings are washed after solid-liquid separation.
According to one embodiment of the invention, the secondary leach tailings are washed with fresh or recycled water
According to one embodiment of the invention, when the secondary leached tailings are washed, the washing water quantity is controlled according to the liquid-solid ratio of 1-2.0 ml to 1g, and the washing water returns to the step one for pulping.
By adopting the technical scheme, the invention has the following beneficial effects:
the invention adopts the tailings produced by calcification roasting-sulfuric acid leaching process as raw materials, pulps the materials according to a certain liquid-solid ratio under a certain temperature condition, and adopts calcium oxide to adjust the pH value, so that vanadium pentoxide which can not be dissolved by acid and acid-insoluble polyvanadate produced by hydrolysis and precipitation of vanadium contained in primary acid leaching slag can be converted into acid-soluble calcium vanadate through the calcium oxide, and then can be leached by acid.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
As required, detailed embodiments of the present invention are disclosed in the present specification; however, it is to be understood that the embodiments disclosed herein are merely exemplary of the invention that may be embodied in various and alternative forms. In the following description, a number of operating parameters and components are described in terms of various embodiments contemplated. These specific parameters and components are presented as examples and are not meant to be limiting.
The invention provides a method for recovering vanadium from calcified vanadium extraction tailings, which comprises the following steps:
step one: pulping calcified vanadium extraction tailings; step two: adding calcium oxide into the slurry prepared in the step one, regulating the pH value to 10-13, and reacting for 5-15 min; step three: adding sulfuric acid into the system of the second step, regulating the pH value to 0.5-2.5, performing secondary leaching, and performing solid-liquid separation after reacting for 10-30 min to obtain vanadium-containing solution and secondary leaching tailings with low vanadium content.
The "calcified vanadium extraction tailings" mentioned in the first step are acid leaching residues generated by the vanadium-containing raw material through a "calcified roasting-acid leaching" process, and are also called as "primary acid leaching residues" hereinafter. The pH value of the slurry is about 4-6 after pulping the calcified vanadium extraction tailings. The TV content in the calcified vanadium extraction tailings is 1.4-1.7%.
The mechanism of the step of adding calcium oxide is as follows: the primary acid leaching slag contains vanadic anhydride which can not be dissolved by acid, the vanadic anhydride can not be dissolved by acid, calcium oxide is used for converting the vanadic anhydride in the primary acid leaching slag into calcium vanadate, and then acid leaching can be performed. The possibility of hydrolyzing and precipitating vanadium exists in the primary leaching process, vanadium generated by hydrolyzing and precipitating vanadium cannot be dissolved in acid and can be remained in the primary acid leaching slag, so that polyvanadate generated by hydrolyzing and precipitating vanadium can be converted into calcium vanadate dissolved in acid through calcium oxide. In order to convert the vanadium pentoxide and the polyvanadate in the primary acid leaching slag into substances dissolved in acid, and simultaneously prevent other impurities from being introduced, the cost is controlled, and calcium oxide is selected. The addition of calcium oxide has the advantages that the primary acid leaching slag can reduce the total vanadium to about 0.3 percent without high-temperature roasting, and the excessive slag amount is not increased.
And in the third step, sulfuric acid is added to extract vanadium which is not extracted by one leaching, and the sulfuric acid is added to adjust the pH value to 0.5-2.5 to reduce the pH value so as to extract the vanadium which is not extracted by one leaching.
In some embodiments of the invention, in step one, the ratio of the pulping liquid to the solid is 1 to 2.0ml to 1g. Namely, the ratio of the volume (in ml) of liquid (usually water) added in pulping to the mass (in g) of calcified vanadium extraction tailings is 1-2.0:1. Preferably, the water content of the calcified vanadium extraction tailings is 30% -50%, and when the slurry solid ratio is calculated, the self water content of the calcified vanadium extraction tailings is calculated in the liquid body of the pulping device.
In some embodiments of the invention, in step one, the pulping temperature is 10-60 ℃. For example, 10 ℃, 15 ℃, 20 ℃, 25 ℃, 30 ℃, 35 ℃, 40 ℃, 45 ℃, 50 ℃, 55 ℃, 60 ℃ and the like, but the present invention is not limited to the values listed, and other values not listed in the numerical range are equally applicable.
In some embodiments of the invention, in the second step, the calcium oxide is added in an amount of 1.5% -4.5% of the mass (wet slag) of the calcified vanadium extraction tailings. For example, 1.5%, 2.0%, 2.5%, 3.0%, 3.5%, 4.0%, 4.5%, etc., but are not limited to the recited values, and other non-recited values within the range of values are equally applicable.
In some embodiments of the invention, in step three, the secondary leaching is performed using 25% to 50% volume fraction sulfuric acid. For example, 25%, 30%, 35%, 40%, 45%, 50%, etc., but are not limited to the recited values, and other non-recited values within the range of values are equally applicable.
In some embodiments of the invention, in step three, the secondary leaching temperature is 10-60 ℃. For example, 10 ℃, 15 ℃, 20 ℃, 25 ℃, 30 ℃, 35 ℃, 40 ℃, 45 ℃, 50 ℃, 55 ℃, 60 ℃ and the like, but the present invention is not limited to the values listed, and other values not listed in the numerical range are equally applicable.
In some embodiments of the invention, in step three, the secondary leach tailings are washed after solid-liquid separation. The secondary leach tailings may be washed with fresh or recycled water. The new water refers to tap water which is not used industrially, and the recycled water refers to water after participating in the reaction in the process flow, and the process requirements can be met after the water is treated by certain means. Preferably, the reuse water used in the present invention may be waste water generated in a calcium process, water used in the return process by treatment. When the secondary leached tailings are washed, the washing water quantity is controlled according to the liquid-solid ratio of 1-2.0 ml to 1g, and the washing water can be returned to the step one for pulping. The water washing amount is controlled according to the liquid-solid ratio of 1-2.0 ml to 1g, namely the ratio of the volume of water added in washing (in ml) to the mass of the secondary leaching tailings (in g) is 1-2.0 to 1.
The present invention will be specifically described with reference to the following examples.
Example 1
100g of tailings (the water content is 30 percent, and the ratio of TV to 1.4 percent) is calculated according to the liquid-solid ratio of 1:1 (the water content of the calcified vanadium extraction tailings is calculated), and pulping is carried out at the temperature of 10 ℃; adding 1.5% calcium oxide by mass of tailings (wet slag), regulating the pH value to 10.2, reacting for 5min, and adding 25% sulfuric acid by volume fraction at 10 ℃ to regulate the pH value to 0.5; after the reaction is carried out for 10min, solid-liquid separation is carried out, and a vanadium-containing solution and secondary leaching tailings with low vanadium content are obtained, the secondary leaching tailings are washed once (washing water can be clear water or reuse water), the washing water amount is controlled according to a liquid-solid ratio of 1:1, and the washing water returns to the pulping step. The secondary leaching tailings TV was 0.345%.
Example 2
200g of tailings (the water content is 30 percent, and the ratio of TV to 1.6 percent) is calculated according to the liquid-solid ratio of 1.5:1 (the water content of the calcified vanadium extraction tailings is calculated), and pulping is carried out at the temperature of 30 ℃; adding 2.5% calcium oxide by weight of tailings (wet slag), adjusting pH value to 12, reacting for 10min, and adding 35% volume fraction sulfuric acid at 30deg.C to adjust pH value to 1.0; after the reaction is carried out for 20min, solid-liquid separation is carried out, and a vanadium-containing solution and secondary leaching tailings with low vanadium content are obtained, the secondary leaching tailings are washed once (washing water can be clear water or reuse water), the washing water amount is controlled according to the liquid-solid ratio of 1.25:1, and the washing water returns to the pulping step. The secondary leaching tailings TV was 0.542%.
Example 3
300g of tailings (the water content is 30 percent, and the ratio of TV to 1.7 percent) is calculated according to the liquid-solid ratio of 2:1 (the water content of the calcified vanadium extraction tailings is calculated), and pulping is carried out at the temperature of 60 ℃; adding 4.5% calcium oxide by weight of tailings (wet slag), regulating pH value to 13.1, reacting for 15min, and adding 50% sulfuric acid by volume fraction at 60 ℃ to regulate pH value to 2.5; after 30min of reaction, carrying out solid-liquid separation to obtain vanadium-containing solution and secondary leaching tailings with low vanadium content, washing the secondary leaching tailings once (washing water can be clear water or reuse water), controlling the washing water amount according to a liquid-solid ratio of 2:1, and returning the washing water to the pulping step. The secondary leaching tailings TV was 0.757%.
Based on the above embodiments, it can be seen that: the method can reduce the content of TV in the primary acid leaching slag from 1.4-1.7% to 0.3-0.7%, thereby reducing the resource waste.
Claims (10)
1. A method for recovering vanadium from calcified vanadium extraction tailings, which is characterized by comprising the following steps:
step one: pulping calcified vanadium extraction tailings, wherein the calcified vanadium extraction tailings are acid leaching residues generated by a calcified roasting-acid leaching process of a vanadium-containing raw material;
step two: adding calcium oxide into the slurry prepared in the step one, regulating the pH value to 10-13 by adopting the calcium oxide, and reacting for 5-15 min, so that vanadium pentoxide which cannot be dissolved by acid and acid-insoluble polyvanadate generated by the hydrolysis and precipitation of vanadium contained in the calcified vanadium extraction tailings are converted into calcium vanadate dissolved in acid by the calcium oxide;
step three: directly adding sulfuric acid into the system of the second step, regulating the pH value to 0.5-2.5, carrying out secondary leaching, and carrying out solid-liquid separation after reacting for 10-30 min to obtain vanadium-containing solution and secondary leaching tailings with low vanadium content.
2. The method for recovering vanadium from calcified vanadium extraction tailings of claim 1 wherein in step one, the ratio of pulping liquid to solid is 1-2.0 ml to 1g.
3. The method for recovering vanadium from calcified vanadium extraction tailings according to claim 2, wherein in the first step, the water content of the calcified vanadium extraction tailings is 30% -50%, and the self water content of the calcified vanadium extraction tailings is calculated when the slurry solid ratio is calculated.
4. The method for recovering vanadium from calcified vanadium extraction tailings of claim 3 wherein in step one, the pulping temperature is 10-60 ℃.
5. The method for recovering vanadium from calcified vanadium extraction tailings according to claim 1, wherein in the second step, the calcium oxide is added in an amount of 1.5% -4.5% of the mass of the calcified vanadium extraction tailings.
6. The method for recovering vanadium from calcified vanadium extraction tailings according to claim 1, wherein in the third step, 25% -50% by volume of sulfuric acid is used.
7. The method for recovering vanadium from calcified vanadium extraction tailings of claim 1 wherein in step three, the secondary leaching temperature is 10-60 ℃.
8. The method for recovering vanadium from calcified vanadium extraction tailings of claim 1 wherein in step three, the secondary leach tailings are washed after solid-liquid separation.
9. The method for recovering vanadium from calcified vanadium extraction tailings of claim 8 wherein the secondary leach tailings are washed with fresh or recycled water.
10. The method for recovering vanadium from calcified vanadium extraction tailings according to claim 8, wherein the water washing amount is controlled according to a liquid-solid ratio of 1-2.0 ml to 1g when the secondary leaching tailings are washed, and the washing water is returned to the first pulping step.
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| CN114350981A (en) * | 2021-11-25 | 2022-04-15 | 攀钢集团研究院有限公司 | Method for recovering vanadium from calcified vanadium extraction tailings |
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| WO2015176429A1 (en) * | 2014-05-23 | 2015-11-26 | 中国科学院过程工程研究所 | Method for extracting vanadium by leaching vanadium-containing raw material fired clinkers with ammonium bicarbonate solution |
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