CN111087019A - Method for extracting vanadium and chromium from vanadium slag vanadium extraction wastewater - Google Patents
Method for extracting vanadium and chromium from vanadium slag vanadium extraction wastewater Download PDFInfo
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- C02F1/00—Treatment of water, waste water, or sewage
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
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- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
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- C02F2101/22—Chromium or chromium compounds, e.g. chromates
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- C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
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Abstract
The invention discloses a method for extracting vanadium and chromium from vanadium slag vanadium extraction wastewater, which separates and extracts vanadium and chromium in the wastewater through ion exchange, and the residual liquid vanadium and chromium meet the requirements of vanadium industrial pollutant discharge standard. The separated vanadium liquid and chromium liquid can be used for producing products with high added values, and the obtained high-concentration vanadium liquid can be used for producing vanadium pentoxide; the obtained high-concentration chromium solution is reduced to precipitate chromium hydroxide, and the chromium sesquioxide pigment is obtained after calcination, so that the resource utilization of vanadium and chromium in the vanadium-containing wastewater is realized.
Description
Technical Field
The invention relates to a method for extracting vanadium and chromium from vanadium slag vanadium extraction wastewater, belonging to the field of vanadium chemical industry. Vanadium and chromium in the wastewater are separated and extracted through ion exchange, the obtained high-concentration vanadium liquid can be used for producing vanadium pentoxide, the obtained high-concentration chromium liquid is reduced to precipitate chromium hydroxide, and the chromium oxide pigment is obtained after calcination, so that the resource utilization of the vanadium and the chromium in the vanadium-containing wastewater is realized.
Background
According to different raw materials, vanadium slag vanadium extraction enterprises contain certain chromium, in the roasting process, part of chromium reacts with sodium salt to be converted into solution, and in the acid ammonium salt vanadium precipitation process, a small amount of vanadium and most of chromium enter production wastewater. Cr in wastewater of certain vanadium extraction enterprises6+Ion concentration of about 1.5-5 g/L, V5+The concentration is 0.05-0.2 g/L, and the daily wastewater treatment capacity reaches 1000m3The vanadium pentoxide content in the wastewater per day reaches 180-360 Kg, the chromium sesquioxide content reaches 2-7 tons, the current selling price of the vanadium pentoxide reaches 25-27 ten thousand yuan/ton, the selling price of the chromium sesquioxide pigment reaches 1.2-1.7 ten thousand yuan/ton, and the vanadium and chromium in the recovered wastewater have obvious economic benefits for enterprises.
Vanadium and chromium in the vanadium extraction wastewater are used as heavy metals and must be removed, and most vanadium extraction enterprises generally adopt a vanadium-chromium coprecipitation method: the process is characterized in that ferrous sulfate and quicklime are added into the wastewater to simultaneously precipitate vanadium and chromium, and the obtained vanadium-chromium waste residue has high impurity content, so that the vanadium and chromium are difficult to separate and extract again, the vanadium and chromium can only be stacked and stored, the comprehensive utilization of resources cannot be realized, and the chromium content of the treated wastewater cannot reach the standard. Still other enterprises employ a two-step chemical precipitation process: the process comprises the steps of firstly adding polyferric sulfate to precipitate vanadium into ferric vanadate, then reducing chromium by using a reducing agent, and then adding sodium hydroxide to precipitate chromium hydroxide.
Because hexavalent chromium belongs to a substance with strong toxicity, the state sets up the discharge standard of vanadium industrial pollutants (GB 26452-2011) in 2011, and the discharge limit value of wastewater is regulated to be V5+<1.0mg/L，Cr6+<0.5 mg/L. There are strict regulations on the chromium content in the production wastewater.
Therefore, the chromium in the recovered wastewater not only meets the requirement of environmental protection, but also can bring economic benefits for enterprises. However, at present, domestic vanadium extraction enterprises mainly adopt reduction precipitation to the wastewater to remove vanadium and chromium in the wastewater, so that the content of the vanadium and the chromium in the wastewater reaches the standard and is discharged, and the formed chromium slag containing a certain amount of chromium and a small amount of vanadium is taken as industrial waste and is subjected to comprehensive treatment by special institutions, so that the vanadium extraction enterprises are environment-friendly.
After an enterprise hands chromium slag to a mechanism special for treating industrial waste by using a method for treating the industrial waste, the treatment method of the product adopts a method of adding sodium carbonate for roasting in order to take account of other different types of industrial waste residues, low-valence vanadium and chromium in the waste residues are reoxidized at high temperature to enable the vanadium and the chromium to become high-valence soluble salts and enter an aqueous solution, an extraction method is utilized for separating the vanadium in the soluble salts, and the remaining hexavalent chromium is prepared into chromium hydroxide by a reduction precipitation method. The method carries out high-temperature oxidation on the chromium which is reduced into trivalent chromium to reform soluble hexavalent chromium, and generates and recovers the chromium hydroxide through a reduction process.
Other methods for recovering vanadium and chromium in wastewater include reducing pentavalent vanadium into tetravalent vanadium and hexavalent chromium into trivalent chromium by using sodium bisulfate, adding hydrogen peroxide to oxidize the tetravalent vanadium into the pentavalent vanadium, selectively adsorbing pentavalent vanadium ions by an ion exchange method, desorbing resin by NaOH to obtain vanadium-containing eluent, preparing ammonium metavanadate from the eluent, and calcining to obtain vanadium pentoxide. The pH value of the trivalent chromium solution is adjusted to separate out chromium in the form of hydrated chromium hydroxide, and chromium trioxide powder is obtained by calcining, but the method is not mentioned for separating and recovering vanadium and chromium from vanadium-containing wastewater.
The treatment method comprises the following steps of adjusting the pH of vanadium-containing wastewater (the content of vanadium and chromium is 20-150 mg/L, the content of other heavy metal ions is less than 50 mg/L) to 4-6, sequentially adsorbing the vanadium-containing wastewater by using chelate resin CH-90 and macroporous weak-alkaline resin A-654, desorbing the A-654 resin by using NaOH, and adjusting the pH of a desorption solution to be 6-8 to obtain a vanadium-chromium solution. Carrying out secondary adsorption and primary separation on the vanadium-chromium solution by using resin A-654 to obtain vanadium-rich resin and chromium-containing tail solution, desorbing the vanadium-rich resin to obtain vanadium solution, and carrying out ammonium salt vanadium precipitation; the chromium-containing tail solution was recovered with the strongly basic resin A-21S, but this method did not effectively recover and utilize chromium.
Other methods mainly adopt two different types of macroporous ion chelating resins to jointly adsorb vanadium, chromium and other heavy metal ions in the wastewater, and then add chemical agents to regenerate the resins for reuse, wherein the regeneration rate of the resins can reach more than 95 percent.
Disclosure of Invention
The method adopts an ion exchange method to recover vanadium and chromium aiming at a small amount of vanadium and high-concentration chromium liquid in the wastewater generated by extracting vanadium from vanadium slag.
The purpose of the invention is realized as follows:
firstly, filtering vanadium-chromium wastewater produced by extracting vanadium from vanadium slag by a filter press, and filtering out solid impurities and particle vanadium in the wastewater to obtain a clarified acidic wastewater solution. Performing three-stage adsorption on the wastewater through ion exchange resins such as D354, D301, D351 and D113, wherein the concentration of chromium ions in the effluent of a first-stage exchange column reaches 25-30 g/L, replacing the first-stage exchange column with a second-stage exchange column to form the first-stage exchange column, introducing the replaced first-stage exchange column into a desorption process, and after three-stage exchange, ensuring that the effluent quality is controlled to be Cr6+<Within 0.5 mg/L.
And adding sodium carbonate, NaOH, lime and the like into the exchanged wastewater to adjust the pH value to 8-9.5, and filtering the wastewater to reach the standard and discharge the wastewater.
And performing multistage adsorption on the resin in the first-stage exchange column, and desorbing the saturated resin by using a 5-10% NaOH solution to obtain the vanadium-containing chromium-rich solution. Since the chromium-rich solution contains vanadium, the vanadium is a valuable element, and the presence of vanadium affects the quality of the chromium hydroxide precipitation product, so that the vanadium and the chromium must be separated. Adjusting the pH value to 8-10 by using a NaOH solution, separating vanadium and chromium by using any one or more of strongly basic anion resin 717, D201, D231 and the like under an alkaline condition, and performing three-stage exchange to obtain a chromium solution, wherein the vanadium is remained in the strongly basic anion resin.
And adding one or more reducing agents such as sodium pyrosulfite, sodium bisulfite, sodium sulfite, sodium dithionite, sodium thiosulfate and hydrazine hydrate into the chromium solution, and reducing under the heating condition of 60-100 ℃ to generate chromium hydroxide precipitate. And (3) feeding the chromium hydroxide precipitate into a rotary kiln and a fluidized bed furnace for calcining at 800-1100 ℃, wherein the calcining time is 2-4 h, then respectively adding 5-10% NaOH solution and 5-10% HCl solution into the calcined material to remove impurities, and finally adding the chromium sesquioxide into a drying kiln for drying to finally obtain the high-quality chromium sesquioxide pigment product.
And (3) desorbing the vanadium ions left in the strongly basic anion resin by using a 5-10% NaOH solution after multiple times of enrichment, wherein the concentration of the vanadium is up to 15-25 g/L, the vanadium ions can be used for precipitating ammonium polyvanadate from acidic ammonium salt, and then adding the ammonium polyvanadate into a reflecting furnace or a melting furnace to melt a casting sheet to obtain a vanadium pentoxide product.
The invention has the beneficial effects that: the method has the advantages that a small amount of vanadium and high-concentration chromium liquid in the wastewater generated by vanadium extraction from vanadium slag are recycled by an ion exchange method, vanadium pentoxide and chromium oxide pigment products with high added values are further prepared from the vanadium solution and the chromium solution, and the problems of difficult resource utilization of vanadium-chromium waste residues obtained after treatment of vanadium-chromium-containing wastewater, high wastewater treatment cost and the like are solved. Meanwhile, the reducing agent, acid and alkali and other auxiliary materials used in the vanadium and chromium recovery process have less dosage and lower cost than the prior treatment method, and the Cr in the waste water after ion exchange6+、V5+Can reach the discharge standard of pollutants in vanadium industry, and solves the defect that the total chromium in the vanadium-chromium coprecipitation method in the existing vanadium extraction wastewater treatment method can not reach the standard. The method is easy to popularize, can recover trace vanadium and a large amount of chromium in the wastewater, ensures that the vanadium and chromium indexes of the vanadium extraction wastewater are qualified, has obvious economic benefit, and has important significance for treating the vanadium extraction wastewater of vanadium slag and recovering valuable elements in China.
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FIG. 1 is a schematic view of the process flow for extracting vanadium and chromium from vanadium slag vanadium extraction wastewater.
Detailed Description
The present invention is further described in detail with reference to the following examples, but the scope of the present invention is not limited to these examples.
The first embodiment is as follows: vanadium-chromium wastewater (V) produced by extracting vanadium from vanadium slag5+：0.146g/L，Cr6+: 2.87 g/L) is filtered by a filter press, solid impurities and particle vanadium in the wastewater are filtered, three-stage adsorption is carried out by D354 ion exchange resin, and the quality of the effluent is ensured to be controlled at Cr after three-stage exchange6+<Within 0.5mg/L, when the chromium ion concentration of the effluent of the first-stage exchange column reaches 25g/L, adding 8 percent NaOH solution for desorption to obtain vanadium-containing chromium-rich liquid, then regulating the pH value to 9 by using the 8 percent NaOH solution through D231 strong-base anion resin, obtaining chromium solution after three-stage exchange, adding sodium pyrosulfite into the chromium solution, and reducing the chromium solution into Cr at 80 DEG C3+And precipitating to obtain chromium hydroxide, calcining the chromium hydroxide precipitate in a rotary kiln and a fluidized bed furnace at 900 ℃ for 3h, then respectively adding 8% NaOH solution and 10% HCl solution into the calcined material to remove impurities, and finally adding chromium sesquioxide into a drying kiln for drying to finally obtain high-quality (Cr) chromium hydroxide2O3>99.5%) chromium oxide pigment product.
Vanadium ions left in the strongly basic anion resin are subjected to enrichment for multiple times, then are desorbed by 8 percent NaOH solution, the concentration of the vanadium is enriched to 20g/L, and the vanadium can be used for precipitating ammonium polyvanadate from acidic ammonium salt, and then are added into a reflecting furnace or a melting furnace to melt cast pieces to obtain a vanadium pentoxide product (V)2O5>98.7%）。
Wastewater V obtained by the first resin exchange5+<1.0 mg/L，Cr6+<0.5mg/L, and can be discharged after further treating ammonia nitrogen.
Example two: vanadium-chromium wastewater (V) produced by extracting vanadium from vanadium slag5+：0.09g/L，Cr6+: 3.52 g/L) is filtered by a filter press, solid impurities and particle vanadium in the wastewater are filtered, and then three-level adsorption is carried out by primary D301 ion exchange resin and secondary and tertiary D351, and the effluent quality is ensured to be controlled at Cr after the three-level exchange6+<Within 0.5mg/L, when the concentration of chromium ions in the effluent of the first-stage exchange column reaches 25g/L, adding 5% NaOH solution for desorption, desorbing to obtain vanadium-containing chromium-rich liquid, and passing through first-stage D231, second-stage and third-stage D201 strong-base anion treesPerforming ion exchange with lipid, adjusting pH to 8.5 with 5% NaOH solution, performing three-stage exchange to obtain chromium solution, adding hydrazine hydrate and sodium sulfite into the chromium solution, and reducing to obtain Cr at 60 deg.C3+And precipitating to obtain chromium hydroxide, calcining the chromium hydroxide precipitate in a rotary kiln and a fluidized bed furnace at 1000 ℃ for 2h, then respectively adding 5% NaOH solution and 5% HCl solution into the calcined material to remove impurities, and finally adding chromium sesquioxide into a drying kiln for drying to finally obtain high-quality (Cr) chromium hydroxide2O3>99.6%) chromium oxide pigment product.
Vanadium ions left in the strongly basic anion resin are subjected to enrichment for multiple times, then are desorbed by a 5 percent NaOH solution, the concentration of the vanadium is enriched to 15g/L, and the vanadium can be used for precipitating ammonium polyvanadate from acidic ammonium salt, and then are added into a reflecting furnace or a melting furnace to melt cast pieces to obtain a vanadium pentoxide product (V)2O5>98.7%）。
Wastewater V obtained by the first resin exchange5+<1.0 mg/L，Cr6+<0.5mg/L, and can be discharged after further treating ammonia nitrogen.
Claims (5)
1. The invention provides a resin exchange mode for separating vanadium and chromium from vanadium and chromium-containing wastewater in a combined and innovative manner, and then high-quality vanadium pentoxide and chromium oxide pigments are respectively prepared.
2. The method according to claim 1, characterized in that the vanadium extraction wastewater is subjected to three-stage adsorption through ion exchange resins such as D354, D301, D351 and D113, the chromium ion concentration of the effluent of the first-stage exchange column reaches 25-30 g/L, the effluent enters a desorption process, and the quality of the effluent is controlled to be Cr after three-stage exchange6+<Within 0.5mg/l, compared with the two-step chemical treatment process of vanadium and chromium, the invention saves a large amount of auxiliary materials, has low cost and simultaneously solves the problem that the total chromium can not reach the standard by a vanadium-chromium coprecipitation method.
3. The method of claim 1, wherein the strong base anion resin 717, D201 and D231 are used for separating vanadium and chromium under the alkaline condition, and a chromium solution is obtained after three-stage exchange, and vanadium is remained in the strong base anion resin, so that effective separation of trace vanadium and high-concentration chromium is realized.
4. The method as claimed in claim 1, wherein the chromium hydroxide precipitate is calcined in a rotary kiln and a fluidized bed furnace at 800-1100 ℃ for 2-4 hours, then the calcined material is added with 5-10% NaOH solution and 5-10% HCl solution respectively to remove impurities, and finally the chromium sesquioxide is added into a drying kiln for drying, thereby obtaining a high-quality chromium sesquioxide pigment product (Cr-containing pigment product)2O3＞99%）。
5. The method of claim 1, wherein the method is not only suitable for treating vanadium-extracting waste water from vanadium slag, but also suitable for treating chromium-containing waste water from vanadium ore, vanadium catalyst and other industries.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113416847A (en) * | 2021-07-05 | 2021-09-21 | 昆明理工大学 | Method for recycling, reducing and harmlessly treating vanadium extraction tailings |
| CN114622104A (en) * | 2022-03-21 | 2022-06-14 | 四川省银河化学股份有限公司 | Method for resource utilization of vanadium and chromium in vanadium extraction wastewater |
| CN116334414A (en) * | 2023-03-16 | 2023-06-27 | 核工业北京化工冶金研究院 | Method for selectively separating vanadium and chromium from vanadium-chromium solution |
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| CN113416847A (en) * | 2021-07-05 | 2021-09-21 | 昆明理工大学 | Method for recycling, reducing and harmlessly treating vanadium extraction tailings |
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| CN116334414A (en) * | 2023-03-16 | 2023-06-27 | 核工业北京化工冶金研究院 | Method for selectively separating vanadium and chromium from vanadium-chromium solution |
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Application publication date: 20200501 |