CN110983051A - Backwashing enrichment method for low-concentration vanadium liquid - Google Patents
Backwashing enrichment method for low-concentration vanadium liquid Download PDFInfo
- Publication number
- CN110983051A CN110983051A CN201911345605.3A CN201911345605A CN110983051A CN 110983051 A CN110983051 A CN 110983051A CN 201911345605 A CN201911345605 A CN 201911345605A CN 110983051 A CN110983051 A CN 110983051A
- Authority
- CN
- China
- Prior art keywords
- vanadium
- concentration
- leaching
- low
- liquid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- 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
-
- 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
-
- 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 relates to a backwashing enrichment method of low-concentration vanadium liquid. The enrichment method comprises the following steps: (1) leaching the vanadium-containing clinker by using a low-concentration vanadium solution, and filtering to obtain a high-concentration vanadium solution; (2) leaching the vanadium-containing clinker leached in the step (1) by using water, and using low-concentration leaching solution obtained by filtering for backwashing of the next batch of vanadium-containing clinker; and (3) setting the leaching temperature, the leaching time and the liquid-water ratio of the low-concentration vanadium liquid in the step (1) and the water in the step (2) according to the concentration of the low-concentration vanadium liquid in the step (1). The enrichment method utilizes the low-concentration vanadium liquid to backwash the vanadium-containing clinker, so that the equipment and capital investment in the direct vanadium extraction process are saved, and the enrichment effect of the low-concentration vanadium liquid can be realized only by adding a backwashing step in the existing vanadium leaching and extracting process flow. In addition, the low-concentration leaching solution obtained after washing can be used for backwashing the next batch of vanadium-containing clinker, thereby reducing the cost of wastewater treatment and being beneficial to environmental protection.
Description
Technical Field
The invention relates to the technical field of vanadium liquid extraction and recovery, in particular to a backwashing enrichment method of low-concentration vanadium liquid.
Background
At present, vanadium extraction from vanadium slag mainly adopts sodium oxide roasting and water vanadium extraction processes, and then vanadium pentoxide is produced. In the production process of extracting vanadium from vanadium slag, the low-concentration vanadium liquid which does not meet the requirement is often leached. On the one hand, the reasons are that the operator experiences insufficiently, the concentration cannot be distinguished according to the leaching yield and the color of the vanadium leaching solution, and the concentration of the leached vanadium solution is too low due to excessive water addition in the process of leaching the vanadium by water. When the alkalinity of the roasted clinker (or the alkalinity of the vanadium liquid) is higher, the obtained leachate has more yellow color than the leachate with the same concentration. If the concentration of the leachate is judged to be qualified according to experience, more leaching water is added, and the used leaching water is used as a diluent of the vanadium liquid, so that the vanadium concentration of the leachate is reduced. On the other hand, the method is influenced and restricted by the roasting quality of the rotary kiln, the vanadium content of the vanadium slag, the material proportion, the granularity of the leached material and the leaching speed to a great extent. Wherein, when the vanadium slag grade is low, the rotary kiln roasting conversion rate is low, the material fine particles are more, the content of soluble vanadium is less, and the vanadium concentration of the leaching solution is lower under the same leaching condition. Therefore, the low-concentration vanadium-containing leaching solution must be subjected to enrichment treatment, and then vanadium in the low-concentration vanadium-containing leaching solution is recovered.
For a long time, researchers have conducted a great deal of research on methods for enriching and recovering vanadium from low-concentration vanadium-containing leachate, mainly including a chemical precipitation method, an ion exchange method and a solution extraction method. For example, CN106282607A discloses a method for utilizing V5+A process for extracting and enriching the solution containing vanadium includes such steps as regulating the pH value of the raw liquid containing vanadium to less than 7 to generate deposit or floc, adding oxidant while stirring for reaction, and oxidizing the vanadium ions in the solution to become V5+Filtering the reaction solution to obtain filtrate as extraction stock solution; then regulating the pH value of the extraction stock solution to be below 7, and adopting an extraction organic phase with the pH value equal to that of the extraction stock solution to extract the extraction stock solutionV in liquid5+Performing countercurrent extraction to obtain enriched V5+The organic phase and the extraction residual water of the second step, the concentration of V5+The organic phase is subjected to back extraction treatment by a back extractant solution to obtain enriched V5+Is backwashed and stored to obtain a utilization V5+And extracting and enriching the vanadium-containing solution. The method is represented by V5+The valence state extraction purification and enrichment of the vanadium-containing solution do not need to repeatedly change the valence state, the vanadium recovery rate is high, but a set of independent vanadium recovery equipment needs to be established, the equipment investment is large, the process route is long, the operation cost is high, a large amount of oxidant, extractant and the like are consumed, a large amount of waste water is generated, and the environment is polluted.
CN1073414 discloses a method for separating and recovering vanadium and chromium from vanadium-chromium mixed wastewater and vanadium and chromium wastewater, wherein the method is to extract and separate vanadium and chromium respectively by using a chemical precipitation method. Wherein the process of extracting and separating vanadium comprises adjusting pH to 2-3, adding high iron, adjusting pH to 5, adding PAN non-ionic flocculant, stirring with air, rapidly precipitating vanadate, filtering to obtain vanadium slag, drying, and returning to rotary kiln for roasting to extract vanadium. Although the method has wide application range, is suitable for extracting and separating vanadium and chromium from vanadium-chromium mixed wastewater and single vanadium-or chromium-containing wastewater, has the advantages of small occupied area, small amount of sediment, easy recycling, high economic value and suitability for large, medium and small water treatment, a set of independent vanadium recovery equipment needs to be established, the equipment investment is large, the process route is long, the operation cost is high, a large amount of chemical reagents are consumed, a large amount of wastewater is generated, and the environment is polluted.
CN102676810A discloses a method for separating and recovering vanadium and chromium from a vanadate-chromate-containing solution, which utilizes weak base and strong base anion exchange resins to realize deep separation of vanadium and chromium by saturated adsorption according to the difference of anion exchange potentials formed by hexavalent chromium and pentavalent vanadium in an aqueous solution, thereby directly obtaining vanadium and chromium products. The method comprises vanadium saturation adsorption or chromium saturation adsorption, treatment of effluent liquid before a vanadium leakage point or a chromium leakage point, and treatment of vanadium-negative resin or chromium-negative resin, although the process flow is shortened to some extent, the separation effect is better, and the reagent dosage is saved, a set of independent vanadium recovery equipment needs to be established, the equipment investment is large, the operation cost is high, a large amount of ion exchange resin is consumed, a large amount of wastewater is generated, and the environment is polluted.
CN102864318A discloses a method for recovering vanadium from acidic vanadium-containing solution containing silicon and phosphorus, which comprises the steps of pH adjustment, ion exchange resin adsorption, ion exchange resin desorption, purification and silicon and phosphorus removal, vanadium precipitation treatment and vanadium-containing precipitation calcination treatment, and finally obtaining a high-concentration vanadium-containing product. Although the method has good impurity removal effect and high vanadium-containing product quality, a set of independent vanadium recovery equipment needs to be established, the equipment investment is large, the process route is long, the operation cost is high, a large amount of chemical reagents and ion exchange resins are consumed, a large amount of waste water is generated, and the environment is polluted.
CN101260467 discloses a purification and enrichment method of a low-concentration vanadium-containing aqueous solution, which comprises adding a purifying agent, adjusting pH, adsorbing by ion exchange resin, desorbing by ion exchange resin, adding the purifying agent again, and performing solid-liquid separation to obtain the purified and enriched vanadium-containing aqueous solution. Although the purification and enrichment method has the characteristics of less vanadium loss and good purification effect, a set of independent vanadium recovery equipment needs to be established, the equipment investment is large, the process route is long, the operation cost is high, a large amount of chemical reagents and ion exchange resins are consumed, a large amount of waste water is generated, and the environment is polluted.
Although some treatment methods for low-concentration vanadium liquid are disclosed in the prior art, a set of separate vanadium recovery equipment needs to be established, so that the equipment investment is large, the process route is long, the operation cost is high, a large amount of chemical reagents, ion exchange resins or extracting agents and the like are consumed, a large amount of waste water is generated, and the environment is polluted. Therefore, it is urgently needed to develop a new method for enriching a low-concentration vanadium solution.
Disclosure of Invention
In view of the problems in the prior art, the invention provides a low-concentration vanadium liquid backwashing enrichment method. The enrichment method comprises a primary leaching backwashing and a secondary leaching washing, wherein the leaching temperature, the leaching time and the liquid-water ratio of two steps are set according to the concentration of the low-concentration vanadium liquid in the primary leaching backwashing. The enrichment method utilizes the low-concentration vanadium liquid to backwash the vanadium-containing clinker to improve the vanadium concentration, not only saves the equipment and the capital investment in the direct vanadium extraction process, but also can realize the enrichment effect of the low-concentration vanadium liquid by only adding a backwashing step in the existing vanadium leaching and extracting process flow, and then carries out the next treatment according to the normal program. In addition, the low-concentration leaching solution obtained after washing can be used for backwashing the next batch of vanadium-containing clinker, thereby reducing the cost of wastewater treatment and being beneficial to environmental protection. Moreover, the enrichment method improves the overall yield of the vanadium extraction system of the vanadium slag.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention aims to provide a backwashing enrichment method of low-concentration vanadium liquid, which comprises the following steps:
(1) leaching the vanadium-containing clinker by using a low-concentration vanadium solution, and filtering to obtain a high-concentration vanadium solution;
(2) leaching the vanadium-containing clinker leached in the step (1) by using water, and using the low-concentration leaching solution obtained by filtering for backwashing of the next batch of vanadium-containing clinker.
In the production process of extracting vanadium from vanadium slag, the vanadium liquid with low concentration which does not meet the requirement is inevitably leached, and if the vanadium precipitation operation is directly carried out, the obtained V2O5The purity of the product is only 86 percent (volume of rare high melting point metal in the handbook of nonferrous metal extraction metallurgy, Beijing: the publication of metallurgy industry, 1999: 335), and the product can not meet the application requirements far away. Therefore, although the standards of the industry for low-concentration vanadium liquid are different, the vanadium liquid with the vanadium concentration lower than 20g/L is generally called low-concentration vanadium liquid, the high-concentration vanadium liquid obtained through enrichment treatment is subjected to the next vanadium precipitation operation, and the obtained V is2O5The purity of the product can reach 98 percent.
The principle of the primary leaching backwashing of the invention is that when the vanadium-containing clinker contacts with the low-concentration vanadium liquid, the water-soluble vanadium compound in the vanadium-containing clinker diffuses to the low-concentration vanadium liquid based on the molecular diffusion motion of the water-soluble vanadium compound, and the solvation of the low-concentration vanadium liquid serving as a leaching medium accelerates the diffusion of the water-soluble vanadium compound from the vanadium-containing clinker from inside to outside and enters the external leaching medium, thereby realizing the concentration enrichment effect of the low-concentration vanadium liquid. The secondary leaching washing is the action between the vanadium-containing clinker obtained by the primary leaching backwashing and water, and the principle is similar to that of the primary leaching backwashing.
In a preferred embodiment of the present invention, the solid-to-liquid ratio of the vanadium-containing clinker and the low-concentration vanadium solution in step (1) is 1:3 to 1:5, for example, 1:3, 1:3.2, 1:3.5, 1:3.7, 1:4, 1:4.3, 1:4.5, 1:4.8 or 1:5, but the present invention is not limited to the above-mentioned values, and other values not listed in the above-mentioned value range are also applicable.
Preferably, the vanadium-containing clinker in the step (1) is roasted by using sodium oxide.
As a preferred embodiment of the present invention, the vanadium-containing concentration of the low-concentration vanadium solution in step (1) is less than 15g/L, for example, 13g/L, 10g/L, 8g/L, 6g/L, 5g/L, 4g/L or 3g/L, but is not limited to the values listed above, and other values not listed above are also applicable within this range.
Preferably, the vanadium-containing concentration of the high-concentration vanadium solution in the step (1) is more than 15g/L, such as 15g/L, 16g/L, 17g/L, 19g/L, 20g/L, 22g/L, 24g/L or 25g/L, etc., but not limited to the enumerated values, and other non-enumerated values in the numerical range are also applicable, preferably 15-24 g/L.
In a preferred embodiment of the present invention, the leaching temperature is 80 to 95 ℃, for example 80 ℃, 82 ℃, 84 ℃, 85 ℃, 86 ℃, 88 ℃, 90 ℃, 92 ℃, 94 ℃ or 95 ℃, but is not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the leaching time is 2-5h, such as 2h, 2.5h, 3h, 3.5h, 4h, 4.5h or 5h, etc., but is not limited to the recited values, and other values not recited within the range of values are equally applicable.
Preferably, the ratio of the liquid to the water in step (1) between the low-concentration vanadium liquid in step (1) and the water in step (2) is 1:1 to 1:4, such as 1:1, 1:1.5, 1:2, 1:2.5, 1:3, 1:3.5 or 1:4, but not limited to the recited values, and other values not recited in the range of the recited values are also applicable.
The enrichment method is characterized in that according to the concentration of the low-concentration vanadium liquid in the step (1), the leaching temperature, the leaching time and the liquid-water ratio of the low-concentration vanadium liquid in the step (1) and the water in the step (2) are set.
As a preferable technical scheme of the invention, when the vanadium-containing concentration of the low-concentration vanadium solution in the step (1) is less than 5g/L, the leaching temperature is set to be 80-85 ℃, the leaching time is set to be 2-3h, and the liquid-water ratio is 1:1-1: 2.
As a preferable technical scheme of the invention, when the vanadium-containing concentration of the low-concentration vanadium solution in the step (1) is 5-10g/L, the leaching temperature is set to be 85-90 ℃, the leaching time is 3-4h, and the liquid-water ratio is 1:2-1: 3.
As a preferable technical scheme of the invention, when the vanadium-containing concentration of the low-concentration vanadium solution in the step (1) is 10-15g/L, the leaching temperature is set to be 90-95 ℃, the leaching time is set to be 4-5h, and the liquid-water ratio is 1:3-1: 4.
The setting principle of the leaching temperature, the leaching time and the liquid-water ratio is as follows:
the setting principle of leaching temperature is as follows: along with the increase of the concentration of the low-concentration vanadium liquid, the water-soluble vanadium compounds increase, and the resistance of the water-soluble vanadium compounds in the vanadium-containing clinker to the molecular diffusion movement of the low-concentration vanadium liquid increases. The leaching temperature is increased, so that the viscosity of the leaching solution can be reduced, the Brownian motion of soluble vanadium compound molecules is accelerated, and the diffusion speed of the soluble vanadium compound molecules into the leaching solution is increased, so that the leaching rate and the leaching speed of the soluble vanadium compound molecules can be increased;
the setting principle of leaching time is as follows: along with the increase of the concentration of the low-concentration vanadium solution, the water-soluble vanadium compounds increase, the resistance of the water-soluble vanadium compounds in the vanadium-containing clinker to the molecular diffusion movement of the low-concentration vanadium solution is increased, and the leaching time needs to be properly prolonged to increase the leaching rate of the molecules of the soluble vanadium compounds;
the principle of setting the liquid-water ratio is as follows: along with the increase of the concentration of the low-concentration vanadium liquid, the water-soluble vanadium compounds are increased, and the final dynamic balance vanadium concentration of the vanadium-containing clinker and the low-concentration vanadium liquid is increased, so that the liquid-water ratio needs to be increased, namely, the water amount for secondary leaching and washing is increased, and the soluble vanadium compounds in the vanadium-containing clinker are separated and extracted as far as possible.
In a preferred embodiment of the present invention, the vanadium-containing solution in the enrichment method has a pH of 8 to 8.5, such as 8, 8.1, 8.2, 8.3, 8.4 or 8.5, but is not limited to the values listed, and other values not listed in the range of the values are also applicable.
Preferably, the vanadium containing solution in the enrichment process is present in the form of sodium metavanadate.
Through research, the existing form of the vanadium compound in the aqueous solution is influenced by the pH value of the aqueous solution, and the vanadium compound is converted along with the change of the pH value. When the pH value is in the range of 7.5-10, the vanadium compound is present in the form of sodium metavanadate, NaVO3(ii) a When the pH value is in the range of 10-11.8, the vanadium compound is present in the form of sodium pyrovanadate, i.e. Na4V2O7(ii) a The vanadium compound is present in the form of sodium orthovanadate, i.e. Na, at a pH value in the range of 11.8 to 123VO4. In general, the pH value of the leachate obtained by the vanadium extraction process of vanadium slag by roasting sodium oxide and extracting vanadium by water is in the range of 8-8.5, so that NaVO3Is the main existing form of vanadium compound in the leaching solution. NaVO3Can be dissociated into sodium ions and metavanadate ions with strong polymerization capability in aqueous solution.
Preferably, the enrichment method adopts a vacuum filtration mode for filtration.
As a preferable technical scheme of the invention, the high-concentration vanadium solution obtained in the step (1) is subjected to impurity removal and sedimentation to obtain a qualified vanadium-containing aqueous solution.
Preferably, the impurity removal method is to add calcium chloride.
Preferably, the impurity removal is the removal of silicon and phosphorus impurities.
Preferably, the sedimentation method is stationary sedimentation.
As a preferred technical scheme of the invention, the enrichment method comprises the following steps:
(1) leaching vanadium-containing clinker from low-concentration vanadium solution with vanadium concentration less than 15g/L at a solid-liquid ratio of 1:3-1:5, and filtering to obtain high-concentration vanadium solution with vanadium concentration more than 15 g/L;
(2) leaching the vanadium-containing clinker leached in the step (1) by using water, and using low-concentration leaching solution obtained by filtering for backwashing of the next batch of vanadium-containing clinker;
setting leaching temperature, leaching time and the liquid-water ratio of the low-concentration vanadium liquid in the step (1) and the water in the step (2) according to the concentration of the low-concentration vanadium liquid in the step (1):
when the vanadium-containing concentration of the low-concentration vanadium solution in the step (1) is less than 5g/L, setting the leaching temperature to be 80-85 ℃, the leaching time to be 2-3h, and the liquid-water ratio to be 1:1-1: 2;
when the vanadium-containing concentration of the low-concentration vanadium solution in the step (1) is 5-10g/L, setting the leaching temperature to be 85-90 ℃, the leaching time to be 3-4h, and the liquid-water ratio to be 1:2-1: 3;
and (2) when the vanadium-containing concentration of the low-concentration vanadium solution in the step (1) is 10-15g/L, setting the leaching temperature to be 90-95 ℃, setting the leaching time to be 4-5h, and setting the liquid-water ratio to be 1:3-1: 4.
Compared with the prior art, the invention at least has the following beneficial effects:
(1) the enrichment method utilizes the low-concentration vanadium solution to backwash the vanadium-containing clinker to improve the vanadium concentration, only needs to add a backwashing step in the existing leaching vanadium extraction process flow to realize the enrichment effect of the low-concentration vanadium solution, and directly carries out the next treatment according to a normal program;
(2) the enrichment method comprises primary leaching backwashing and secondary leaching washing, so that soluble vanadium compounds in the vanadium-containing clinker can be separated and extracted as far as possible, and the overall yield of a vanadium slag vanadium extraction system is improved;
(3) the enrichment method does not need to establish a set of independent vanadium recovery equipment, saves equipment and capital investment in the direct vanadium extraction process, and also has the advantages of short process route, simple operation and low operation cost;
(4) the enrichment method does not adopt any chemical reagent, ion exchange resin and the like, and the low-concentration leachate generated by secondary leaching and washing can be used for backwashing of the next batch of vanadium-containing clinker without generating wastewater, thereby reducing the wastewater treatment cost and being beneficial to environmental protection.
Drawings
FIG. 1 is a flow chart of the low-concentration vanadium liquid backwashing enrichment method provided by the invention.
Detailed Description
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
FIG. 1 shows a flow chart of a low-concentration vanadium liquid backwashing enrichment method provided by the invention, which specifically comprises the following steps:
(1) leaching the vanadium-containing clinker by using a low-concentration vanadium solution, carrying out primary leaching backwashing, and carrying out impurity removal and sedimentation treatment on a high-concentration vanadium solution obtained by filtering to obtain a qualified vanadium-containing aqueous solution;
(2) leaching the vanadium-containing clinker leached in the step (1) by using water, performing secondary leaching and washing, and using low-concentration leachate obtained by filtering for backwashing of the next batch of vanadium-containing clinker;
and (3) setting the leaching temperature, the leaching time and the liquid-water ratio of the low-concentration vanadium liquid in the step (1) and the water in the step (2) according to the concentration of the low-concentration vanadium liquid in the step (1).
For the purpose of facilitating an understanding of the present invention, the present invention will now be described by way of examples.
Example 1
A backwashing enrichment method of low-concentration vanadium liquid comprises the following steps:
(1) leaching the vanadium-containing clinker roasted by sodium oxide by using a low-concentration vanadium solution with vanadium concentration of 2.41g/L, wherein the solid-liquid ratio is 1:3, the leaching temperature is 80 ℃, the leaching time is 3h, and then carrying out vacuum filtration to obtain a high-concentration vanadium solution with vanadium concentration of 18.45 g/L;
(2) leaching the vanadium-containing clinker leached in the step (1) by using water, wherein the water adding amount meets the condition that the liquid-water ratio of the low-concentration vanadium liquid in the step (1) to the water in the step (2) is 1:1, the leaching temperature is 80 ℃, the leaching time is 2.8h, filtering is carried out to obtain low-concentration leachate with the vanadium concentration of 4.06g/L, and the leachate is stored and used for backwashing of the next batch of vanadium-containing clinker;
in this embodiment, the soluble vanadium content of the vanadium-containing clinker after roasting with sodium oxide is 0.74%, and the soluble vanadium content of the filter residue obtained after the two-step treatment is 0.035%.
Example 2
A backwashing enrichment method of low-concentration vanadium liquid comprises the following steps:
(1) leaching the vanadium-containing clinker roasted by sodium oxide by using a low-concentration vanadium solution with the vanadium concentration of 3.41g/L, wherein the solid-liquid ratio is 1:3, the leaching temperature is 83 ℃, the leaching time is 2.5h, and then carrying out vacuum filtration to obtain a high-concentration vanadium solution with the vanadium concentration of 19.23 g/L;
(2) leaching the vanadium-containing clinker leached in the step (1) by using water, wherein the water adding amount meets the condition that the liquid-water ratio of the low-concentration vanadium liquid in the step (1) to the water in the step (2) is 1:1.5, the leaching temperature is 82 ℃, the leaching time is 2.5 hours, filtering is carried out to obtain low-concentration leachate with the vanadium concentration of 5.66g/L, and the leachate is stored and used for backwashing the next batch of vanadium-containing clinker;
in the embodiment, the soluble vanadium content of the vanadium-containing clinker after roasting by the sodium oxide is 0.73%, and the soluble vanadium content of the filter residue obtained after the two-step treatment is 0.029%.
Example 3
A backwashing enrichment method of low-concentration vanadium liquid comprises the following steps:
(1) leaching the vanadium-containing clinker roasted by sodium oxide by using a low-concentration vanadium solution with the vanadium concentration of 4.86g/L, wherein the solid-liquid ratio is 1:4, the leaching temperature is 85 ℃, the leaching time is 2 hours, and then carrying out vacuum filtration to obtain a high-concentration vanadium solution with the vanadium concentration of 20.61 g/L;
(2) leaching the vanadium-containing clinker leached in the step (1) by using water, wherein the water adding amount meets the condition that the liquid-water ratio of the low-concentration vanadium liquid in the step (1) to the water in the step (2) is 1:2, the leaching temperature is 85 ℃, the leaching time is 2.2 hours, filtering is carried out to obtain low-concentration leachate with the vanadium concentration of 6.21g/L, and the leachate is stored and used for backwashing the next batch of vanadium-containing clinker;
in the embodiment, the soluble vanadium content of the vanadium-containing clinker roasted by sodium oxide is 0.72 percent, and the soluble vanadium content of the filter residue obtained after the two-step treatment is 0.041 percent
Example 4
A backwashing enrichment method of low-concentration vanadium liquid comprises the following steps:
(1) leaching the vanadium-containing clinker roasted by sodium oxide by using a low-concentration vanadium solution with vanadium concentration of 5.56g/L, wherein the solid-liquid ratio is 1:4, the leaching temperature is 85 ℃, the leaching time is 3h, and then carrying out vacuum filtration to obtain a high-concentration vanadium solution with vanadium concentration of 16.37 g/L;
(2) leaching the vanadium-containing clinker leached in the step (1) with water, wherein the water adding amount meets the condition that the liquid-water ratio of the low-concentration vanadium liquid in the step (1) to the water in the step (2) is 1:2, the leaching temperature is 85 ℃, the leaching time is 3 hours, filtering is carried out to obtain a low-concentration leaching solution with the vanadium concentration of 7.96g/L, and the low-concentration leaching solution is stored and used for backwashing the next batch of vanadium-containing clinker;
in this embodiment, the soluble vanadium content of the vanadium-containing clinker after roasting with sodium oxide is 0.75%, and the soluble vanadium content of the filter residue obtained after the two-step treatment is 0.044%.
Example 5
A backwashing enrichment method of low-concentration vanadium liquid comprises the following steps:
(1) leaching the vanadium-containing clinker roasted by sodium oxide by using a low-concentration vanadium solution with vanadium concentration of 7.36g/L, wherein the solid-liquid ratio is 1:3.8, the leaching temperature is 88 ℃, the leaching time is 3.5h, and then carrying out vacuum filtration to obtain a high-concentration vanadium solution with vanadium concentration of 17.31 g/L;
(2) leaching the vanadium-containing clinker leached in the step (1) by using water, wherein the water adding amount meets the condition that the liquid-water ratio of the low-concentration vanadium liquid in the step (1) to the water in the step (2) is 1:2.6, the leaching temperature is 87 ℃, the leaching time is 3.8h, filtering is carried out to obtain low-concentration leachate with the vanadium concentration of 8.07g/L, and the leachate is stored and used for backwashing the next batch of vanadium-containing clinker;
in this embodiment, the soluble vanadium content of the vanadium-containing clinker after roasting with sodium oxide is 0.78%, and the soluble vanadium content of the filter residue obtained after the two-step treatment is 0.051%.
Example 6
A backwashing enrichment method of low-concentration vanadium liquid comprises the following steps:
(1) leaching the vanadium-containing clinker roasted by sodium oxide by using a low-concentration vanadium solution with vanadium concentration of 8.98g/L, wherein the solid-liquid ratio is 1:4.2, the leaching temperature is 90 ℃, the leaching time is 4h, and then carrying out vacuum filtration to obtain a high-concentration vanadium solution with vanadium concentration of 19.84 g/L;
(2) leaching the vanadium-containing clinker leached in the step (1) with water, wherein the water adding amount meets the condition that the liquid-water ratio of the low-concentration vanadium liquid in the step (1) to the water in the step (2) is 1:3, the leaching temperature is 90 ℃, the leaching time is 4 hours, filtering is carried out to obtain low-concentration leachate with the vanadium concentration of 10.22g/L, and the leachate is stored and used for backwashing the next batch of vanadium-containing clinker;
in this embodiment, the soluble vanadium content of the vanadium-containing clinker after roasting with sodium oxide is 0.75%, and the soluble vanadium content of the filter residue obtained after the two-step treatment is 0.039%.
Example 7
A backwashing enrichment method of low-concentration vanadium liquid comprises the following steps:
(1) leaching the vanadium-containing clinker roasted by sodium oxide by using a low-concentration vanadium solution with vanadium concentration of 11.08g/L, wherein the solid-liquid ratio is 1:5, the leaching temperature is 90 ℃, the leaching time is 4.2h, and then carrying out vacuum filtration to obtain a high-concentration vanadium solution with vanadium concentration of 20.33 g/L;
(2) leaching the vanadium-containing clinker leached in the step (1) by using water, wherein the water adding amount meets the condition that the liquid-water ratio of the low-concentration vanadium liquid in the step (1) to the water in the step (2) is 1:3.2, the leaching temperature is 90 ℃, the leaching time is 4.4h, filtering to obtain low-concentration leachate with the vanadium concentration of 11.92g/L, and storing the leachate for backwashing the next batch of vanadium-containing clinker;
in this embodiment, the soluble vanadium content of the vanadium-containing clinker after roasting with sodium oxide is 0.76%, and the soluble vanadium content of the filter residue obtained after the two-step treatment is 0.045%.
Example 8
A backwashing enrichment method of low-concentration vanadium liquid comprises the following steps:
(1) leaching the vanadium-containing clinker roasted by sodium oxide by using a low-concentration vanadium solution with the vanadium concentration of 12.57g/L, wherein the solid-liquid ratio is 1:5, the leaching temperature is 92 ℃, the leaching time is 4.5h, and then carrying out vacuum filtration to obtain a high-concentration vanadium solution with the vanadium concentration of 21.16 g/L;
(2) leaching the vanadium-containing clinker leached in the step (1) by using water, wherein the water adding amount meets the condition that the liquid-water ratio of the low-concentration vanadium liquid in the step (1) to the water in the step (2) is 1:3.5, the leaching temperature is 93 ℃, the leaching time is 4 hours, filtering is carried out to obtain low-concentration leachate with the vanadium concentration of 12.66g/L, and the leachate is stored and used for backwashing the next batch of vanadium-containing clinker;
in this embodiment, the soluble vanadium content of the vanadium-containing clinker after roasting with sodium oxide is 0.71%, and the soluble vanadium content of the filter residue obtained after the two-step treatment is 0.042%.
Example 9
A backwashing enrichment method of low-concentration vanadium liquid comprises the following steps:
(1) leaching the vanadium-containing clinker roasted by sodium oxide by using a low-concentration vanadium solution with vanadium concentration of 14.43g/L, wherein the solid-liquid ratio is 1:5, the leaching temperature is 95 ℃, the leaching time is 5h, and then carrying out vacuum filtration to obtain a high-concentration vanadium solution with vanadium concentration of 23.73 g/L;
(2) leaching the vanadium-containing clinker leached in the step (1) with water, wherein the water adding amount meets the condition that the liquid-water ratio of the low-concentration vanadium liquid in the step (1) to the water in the step (2) is 1:4, the leaching temperature is 95 ℃, the leaching time is 5 hours, filtering is carried out to obtain low-concentration leachate with the vanadium concentration of 14.92g/L, and the leachate is stored and used for backwashing the next batch of vanadium-containing clinker;
in this embodiment, the soluble vanadium content of the vanadium-containing clinker after roasting with sodium oxide is 0.75%, and the soluble vanadium content of the filter residue obtained after the two-step treatment is 0.046%.
Comparative example 1
This comparative example omits the secondary leaching water wash and the other process conditions are the same as in example 2.
In the comparative example, the soluble vanadium content of the vanadium-containing clinker after roasting with sodium oxide is 0.75%, and the soluble vanadium content of the filter residue obtained after one leaching and backwashing is 0.17%.
According to the embodiment and the comparative example, the low-concentration vanadium liquid backwashing enrichment method utilizes the low-concentration vanadium liquid to backwash the vanadium-containing clinker to improve the vanadium concentration, so that the equipment and capital investment in the direct vanadium extraction process are saved, and the enrichment effect of the low-concentration vanadium liquid can be realized only by adding a backwashing step in the existing vanadium leaching and extraction process flow. In addition, the low-concentration leaching solution obtained after washing can be used for backwashing the next batch of vanadium-containing clinker, so that the wastewater treatment cost is reduced, the environmental protection is facilitated, and the overall yield of a vanadium slag vanadium extraction system can be improved.
The applicant declares that the present invention illustrates the detailed structural features of the present invention through the above embodiments, but the present invention is not limited to the above detailed structural features, that is, it does not mean that the present invention must be implemented depending on the above detailed structural features. It should be understood by those skilled in the art that any modifications of the present invention, equivalent substitutions of selected components of the present invention, additions of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (10)
1. The backwashing enrichment method of the low-concentration vanadium liquid is characterized by comprising the following steps of:
(1) leaching the vanadium-containing clinker by using a low-concentration vanadium solution, and filtering to obtain a high-concentration vanadium solution;
(2) leaching the vanadium-containing clinker leached in the step (1) by using water, and using the low-concentration leaching solution obtained by filtering for backwashing of the next batch of vanadium-containing clinker.
2. The enrichment method according to claim 1, wherein the solid-to-liquid ratio of the vanadium-containing clinker and the low-concentration vanadium solution in the step (1) is 1:3-1: 5;
preferably, the vanadium-containing clinker in the step (1) is roasted by using sodium oxide.
3. The enrichment method according to claim 1 or 2, wherein the vanadium-containing concentration of the low-concentration vanadium liquid in the step (1) is less than 15 g/L;
preferably, the vanadium-containing concentration of the high-concentration vanadium solution in the step (1) is more than 15g/L, and preferably 15-24 g/L.
4. The enrichment method according to any one of claims 1 to 3, wherein the leaching temperature is 80-95 ℃;
preferably, the leaching time is 2-5 h;
preferably, the liquid-water ratio between the low-concentration vanadium liquid in the step (1) and the water in the step (2) is 1:1-1: 4.
5. The enrichment method according to any one of claims 1 to 4, wherein when the vanadium-containing concentration of the low-concentration vanadium liquid in the step (1) is less than 5g/L, the leaching temperature is set to be 80-85 ℃, the leaching time is set to be 2-3h, and the liquid-water ratio is 1:1-1: 2.
6. The enrichment method according to any one of claims 1 to 5, wherein when the vanadium-containing concentration of the low-concentration vanadium solution in the step (1) is 5-10g/L, the leaching temperature is set to be 85-90 ℃, the leaching time is 3-4h, and the liquid-water ratio is 1:2-1: 3.
7. The enrichment method according to any one of claims 1 to 6, wherein when the vanadium-containing concentration of the low-concentration vanadium solution in the step (1) is 10-15g/L, the leaching temperature is set to be 90-95 ℃, the leaching time is set to be 4-5h, and the liquid-water ratio is 1:3-1: 4.
8. The enrichment process according to any one of claims 1 to 7, wherein the vanadium-containing solution in the enrichment process has a pH of 8-8.5;
preferably, the vanadium containing solution in the enrichment process is in the form of sodium metavanadate;
preferably, the enrichment method adopts a vacuum filtration mode for filtration.
9. The enrichment method according to any one of claims 1 to 8, characterized in that the high-concentration vanadium solution obtained in step (1) is subjected to impurity removal and sedimentation to obtain a qualified vanadium-containing aqueous solution;
preferably, the impurity removal method is to add calcium chloride;
preferably, the impurity removal is the removal of silicon and phosphorus impurities;
preferably, the sedimentation method is stationary sedimentation.
10. The enrichment method according to any one of claims 1 to 9, wherein the enrichment method comprises the steps of:
(1) leaching vanadium-containing clinker from low-concentration vanadium solution with vanadium concentration less than 15g/L at a solid-liquid ratio of 1:3-1:5, and filtering to obtain high-concentration vanadium solution with vanadium concentration more than 15 g/L;
(2) leaching the vanadium-containing clinker leached in the step (1) by using water, and using low-concentration leaching solution obtained by filtering for backwashing of the next batch of vanadium-containing clinker;
setting leaching temperature, leaching time and the liquid-water ratio of the low-concentration vanadium liquid in the step (1) and the water in the step (2) according to the concentration of the low-concentration vanadium liquid in the step (1):
when the vanadium-containing concentration of the low-concentration vanadium solution in the step (1) is less than 5g/L, setting the leaching temperature to be 80-85 ℃, the leaching time to be 2-3h, and the liquid-water ratio to be 1:1-1: 2;
when the vanadium-containing concentration of the low-concentration vanadium solution in the step (1) is 5-10g/L, setting the leaching temperature to be 85-90 ℃, the leaching time to be 3-4h, and the liquid-water ratio to be 1:2-1: 3;
and (2) when the vanadium-containing concentration of the low-concentration vanadium solution in the step (1) is 10-15g/L, setting the leaching temperature to be 90-95 ℃, setting the leaching time to be 4-5h, and setting the liquid-water ratio to be 1:3-1: 4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911345605.3A CN110983051A (en) | 2019-12-24 | 2019-12-24 | Backwashing enrichment method for low-concentration vanadium liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911345605.3A CN110983051A (en) | 2019-12-24 | 2019-12-24 | Backwashing enrichment method for low-concentration vanadium liquid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110983051A true CN110983051A (en) | 2020-04-10 |
Family
ID=70074713
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911345605.3A Pending CN110983051A (en) | 2019-12-24 | 2019-12-24 | Backwashing enrichment method for low-concentration vanadium liquid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110983051A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112010347A (en) * | 2020-07-23 | 2020-12-01 | 中信锦州金属股份有限公司 | Method for improving yield by precipitating vanadium from high-chromium vanadium solution ammonium salt |
| CN115386742A (en) * | 2022-09-30 | 2022-11-25 | 攀钢集团西昌钒制品科技有限公司 | Method for improving concentration of vanadium in vanadium slag calcified roasting clinker leaching solution |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106048227A (en) * | 2016-06-24 | 2016-10-26 | 攀钢集团攀枝花钢钒有限公司 | Method for efficiently recycling vanadium in vanadium-containing underflow slag |
| CN109207740A (en) * | 2018-11-30 | 2019-01-15 | 攀钢集团研究院有限公司 | The extraction vanadium method of vanadium-bearing slag of high calcium and high phosphor |
| CN109338099A (en) * | 2018-11-30 | 2019-02-15 | 攀钢集团研究院有限公司 | Calcification baking vanadium extraction raw material and its extraction vanadium method |
| CN109913661A (en) * | 2019-04-25 | 2019-06-21 | 河钢股份有限公司承德分公司 | A method of from extraction sulphur and vanadium in desulfurization slag containing vanadium |
-
2019
- 2019-12-24 CN CN201911345605.3A patent/CN110983051A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106048227A (en) * | 2016-06-24 | 2016-10-26 | 攀钢集团攀枝花钢钒有限公司 | Method for efficiently recycling vanadium in vanadium-containing underflow slag |
| CN109207740A (en) * | 2018-11-30 | 2019-01-15 | 攀钢集团研究院有限公司 | The extraction vanadium method of vanadium-bearing slag of high calcium and high phosphor |
| CN109338099A (en) * | 2018-11-30 | 2019-02-15 | 攀钢集团研究院有限公司 | Calcification baking vanadium extraction raw material and its extraction vanadium method |
| CN109913661A (en) * | 2019-04-25 | 2019-06-21 | 河钢股份有限公司承德分公司 | A method of from extraction sulphur and vanadium in desulfurization slag containing vanadium |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112010347A (en) * | 2020-07-23 | 2020-12-01 | 中信锦州金属股份有限公司 | Method for improving yield by precipitating vanadium from high-chromium vanadium solution ammonium salt |
| CN112010347B (en) * | 2020-07-23 | 2022-07-26 | 中信锦州金属股份有限公司 | Method for improving yield by precipitating vanadium from high-chromium vanadium solution ammonium salt |
| CN115386742A (en) * | 2022-09-30 | 2022-11-25 | 攀钢集团西昌钒制品科技有限公司 | Method for improving concentration of vanadium in vanadium slag calcified roasting clinker leaching solution |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104498723B (en) | The method extracting Scia from titanium slag chlorized abraum salt | |
| US20200039838A1 (en) | System for extracting vanadium from leaching solution containing vanadium chromium silicon and for preparing vanadium pentoxide and processing method therefor | |
| WO2008101396A1 (en) | Preprocessing method of an organic extractant and the preprocessed product and the use thereof | |
| CN109022828B (en) | Method for extracting vanadium from waste vanadium catalyst | |
| CN104726724B (en) | The method that scandium is extracted from lateritic nickel ore | |
| US3458277A (en) | Process for the recovery of molybdenum values as high purity ammonium paramolybdate from impure molybdenum-bearing solution,with optional recovery of rhenium values if present | |
| CN108026609A (en) | The production of the concentrate containing scandium and therefrom further extraction high-purity mangesium oxide scandium | |
| CN108707753B (en) | Process for recovering rare earth-containing waste material by solvent extraction | |
| CN110983051A (en) | Backwashing enrichment method for low-concentration vanadium liquid | |
| US3966873A (en) | Uranium complex recycling method of purifying uranium liquors | |
| CN111206150B (en) | Dissolved state high-similarity rare and precious metal enrichment and separation method based on floating extraction | |
| CN117327930B (en) | Method for recovering vanadium from primary shale stone coal | |
| CN111485105B (en) | Method for recovering acid liquor and separating vanadium in process of reducing, acid leaching and vanadium-containing waste catalyst | |
| US3206276A (en) | Process for recovery of pure v2o5 from vanadium bearing materials | |
| CN110157927A (en) | A kind of no ammonium precipitation vanadium method | |
| CN111100996B (en) | Method for preparing vanadium oxide from acidic low-concentration vanadium liquid | |
| CN105671324A (en) | Method for preparing ammonium rhenate from rhenium-enriched slags | |
| CN105567986B (en) | A kind of method for reclaiming gallium germanium from zinc dust precipitation gallium germanium slag with resin | |
| CN114293033B (en) | Method for extracting vanadium from vanadium-containing carbonation leaching liquid and recycling vanadium precipitation residual liquid | |
| CN110453096A (en) | A kind of method that the Whote-wet method smelting molybdenum concentrate of environment-friendly type prepares high-purity ammonium heptamolybdate | |
| CN108342591B (en) | New method for separating molybdenum and copper | |
| CN100355917C (en) | Recovery of platinum group metals | |
| CN111020233B (en) | Method for preparing vanadium pentoxide by ammonium-free vanadium precipitation | |
| CN112662874B (en) | Method for separating and extracting rhenium and co-producing ferromolybdenum alloy from rhenium and molybdenum mixed solution | |
| CN111057875B (en) | Method for separating vanadium and chromium from solution by using microemulsion |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200410 |