CN115286038B - Method for producing ammonium metavanadate by taking dephosphorization slag as raw material - Google Patents
Method for producing ammonium metavanadate by taking dephosphorization slag as raw material Download PDFInfo
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Abstract
A method for producing ammonium metavanadate by taking dephosphorization slag as raw material, which belongs to the technical field of nonferrous metallurgy, comprises the following steps of mixing dephosphorization slag and water according to a proportion, stirring and slurrying to obtain mixed solution; adding sulfuric acid into the mixed solution, controlling the pH value to be 2, stirring for 1 hour at normal temperature, leaching, performing liquid-solid separation after leaching to obtain leaching solution and filter residues, washing the filter residues, and returning the produced washing water to the leaching solution used for the pulping leaching process of the dephosphorization residues in the first step for recycling; impurity removal treatment is carried out on the leaching solution to obtain pure vanadium-containing solution; adding a vanadium precipitating agent into the pure vanadium-containing solution to precipitate vanadium, thereby obtaining the product ammonium metavanadate. The method has the advantages of short production process flow, easy control of technical operation parameters of each working procedure, no need of high temperature and high pressure, low equipment requirement, energy conservation, lower cost, high production efficiency and the like, and the purity of the obtained ammonium metavanadate is higher than 99 percent, and the direct yield of the vanadium pentoxide is as high as 92 percent.
Description
Technical Field
The invention belongs to the technical field of nonferrous metallurgy, and particularly relates to a method for producing ammonium metavanadate by taking dephosphorization slag as a raw material.
Background
Vanadium is a nonferrous metal, more than 85% of vanadium in China is used in the steel industry, and vanadium is mainly added to improve strength and toughness in steel. The alloy steel manufactured is widely applied to warships, ships, automobiles, buildings and the like. The other 10% is used for manufacturing titanium alloy which is mainly used for military industry such as submarines, airplanes and the like. The remaining minor portions are used in the chemical industry as catalysts, ceramic colorants, catalysts, and the like. The application of vanadium as an energy metal is mainly a vanadium flow battery which is recently emerging. In addition to the above fields, vanadium has a relatively wide range of applications in glass, medicine, and the like. The ammonium metavanadate can be used as upstream raw materials of vanadium alloys, vanadium chemical industry and vanadium redox flow batteries.
The method for producing ammonium metavanadate in China mainly comprises the steps of carrying out sodium roasting on vanadium-containing steel slag, carrying out wet leaching, adding sulfuric acid and other auxiliary materials into the leaching solution, preparing ammonium polyvanadate by using high Wen Chen vanadium, and purifying the ammonium polyvanadate to obtain ammonium metavanadate.
In the aspect of wet vanadium extraction, the dephosphorization slag is taken as a raw material to recover vanadium, and the Chinese patent invention discloses a process method for recovering and extracting vanadium from the dephosphorization slag in the production process of vanadium pentoxide. Firstly, removing phosphorous slag; step two, adding water into the dephosphorization slag for pulping, adding sulfuric acid for stirring and controlling the pH value to be 5-6; heating by steam at 50-60 ℃, adding ammonium sulfate, continuing heating to boil, keeping the boiling state for 45 minutes, and standing for 15 minutes to perform liquid-solid separation; settling the supernatant in the fourth step for 20-24 hours, and sending the supernatant to a settling tank; step five, adding sulfuric acid to adjust the pH value of the solution to 2-2.5, adding ammonium sulfate, and heating to boiling by using steam to obtain ammonium polyvanadate; and step six, carrying out liquid-solid separation on the supernatant and ammonium polyvanadate to obtain ammonium polyvanadate, and washing the ammonium polyvanadate with a belt type vacuum filter.
The two vanadium extraction technologies have the defects that the process flow is long, a large amount of auxiliary materials, energy sources and the like are consumed in the process of the process flow through high-temperature sodium treatment, high-temperature leaching and high Wen Chen vanadium, a large amount of smoke is generated in the pyrogenic process, a large amount of acidic ammonium salt wastewater is generated in the wet process, the purity of the produced ammonium polyvanadate vanadium pentoxide cannot be controlled, and the ammonium metavanadate product with high purity is prepared through redissolving and purifying.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: the method for producing ammonium metavanadate by taking the dephosphorization slag as the raw material solves the problems of long process flow, high production cost, non-environmental protection of industrial wastewater and the like in the prior art.
A method for producing ammonium metavanadate by taking dephosphorization slag as a raw material is characterized by comprising the following steps: comprising the following steps, which are sequentially carried out,
step one, mixing the dephosphorized slag and water according to a solid-to-liquid ratio of 3.5:1, and stirring and slurrying to obtain a mixed solution;
step two, adding sulfuric acid into the mixed solution obtained in the step one, enabling the pH value of the mixed solution to be 2, stirring for 1 hour under normal temperature condition, leaching, and obtaining leaching liquid and filter residues through solid-liquid separation;
pumping the leaching solution into a reaction kettle for impurity removal treatment, heating the reaction kettle to 30 ℃, stirring, adding sodium hydroxide, and adjusting the pH value to 9.5; continuously heating to 85 ℃, keeping the pH value to be 9.5, and reacting for 40 minutes to obtain mixed solution after impurity removal;
step four, placing the mixed solution obtained in the step three after impurity removal into a storage tank for sedimentation, and carrying out solid-liquid separation after sedimentation for 72 hours to obtain pure vanadium-containing solution and impurity removal filter residues;
and step five, adding a vanadium precipitating agent with the vanadium pentoxide metal content being 2.3 times into the pure vanadium-containing solution obtained in the step four to precipitate vanadium, reacting at normal temperature for 1 hour, detecting the concentration of vanadium pentoxide in the vanadium precipitation supernatant, performing liquid-solid separation after passing, wherein the filter cake is ammonium metavanadate, and performing wastewater treatment on the vanadium precipitation supernatant and then discharging the qualified vanadium precipitation supernatant.
Vanadium pentoxide V in the dephosphorization slag of the step one 2 O 5 30-35% of phosphorus, 0.40-0.60% of P and 5-15% of Fe.
And (3) washing the filter residues obtained in the step two, and then using the produced washing water as the phosphorus removal slag slurrying leaching liquid, and entering the next impurity removal treatment, namely, recycling the washing water.
The leaching solution obtained in the second step is vanadium pentoxide V 2 O 5 The concentration is 60g/L-75g/L.
And (3) bagging and recycling the impurity-removed filter residues obtained in the step four.
And in the fifth step, the vanadium precipitating agent is ammonium sulfate.
Through the design scheme, the invention has the following beneficial effects: the method for producing ammonium metavanadate from the dephosphorization slag has the advantages of short process flow, low production cost, capability of producing ammonium metavanadate with higher purity and good economic benefit.
The concrete further beneficial effects lie in that:
1. the method only needs one-time sulfuric acid leaching, and is carried out at normal temperature, the leaching rate of the vanadium pentoxide can reach 97%, the reaction time is only 1 hour, and the production efficiency is high;
2. the vanadium precipitation process adopts normal-temperature vanadium precipitation, so that a large amount of energy sources are saved, and the vanadium pentoxide content after calcination of the ammonium metavanadate product is more than 99%.
Detailed Description
The invention is further described in connection with the following detailed description:
embodiment 1,
Step one, taking vanadium pentoxide V 2 O 5 And mixing the dephosphorization slag with the content of 33.2%, the phosphorus content of 0.41% and the iron content of 8.75% according to the solid-to-liquid ratio of 3.5:1, and stirring and slurrying to obtain a mixed solution.
Slowly adding industrial sulfuric acid into the pulpified mixed solution, controlling the pH value to be 2, stirring and leaching for 1 hour at normal temperature, performing liquid-solid separation through filtering equipment after leaching to obtain leaching liquid and filter residues, washing the filter residues, and returning the produced washing water to the pulpified leaching process for removing the phosphorus residues in the step 1 as the leaching liquid for recycling.
Pumping the leaching solution into a reaction kettle for impurity removal treatment, heating to 30 ℃, stirring, adding sodium hydroxide, adjusting the pH value to 9.5, heating to 85 ℃, continuing to react for 40 minutes, monitoring and keeping the pH value to 9.5, and obtaining the mixed solution after impurity removal after the reaction is finished.
And step four, settling the mixed solution obtained in the step three in a storage tank for 72 hours, and then carrying out liquid-solid separation through filtering equipment to obtain pure vanadium-containing solution, and bagging the impurity-removed filter residues for subsequent recovery treatment.
And fifthly, adding ammonium sulfate serving as a vanadium precipitating agent with the vanadium pentoxide metal content being 2.3 times into the pure vanadium-containing solution to precipitate vanadium, reacting at normal temperature for 1 hour, detecting that the vanadium pentoxide concentration in the vanadium precipitation supernatant is less than 0.30 g/L, performing liquid-solid separation through filtering equipment after passing the vanadium precipitation supernatant, and obtaining ammonium metavanadate, and performing wastewater treatment on the vanadium precipitation supernatant and qualified discharge.
And step six, packaging the product ammonium metavanadate.
The obtained ammonium metavanadate is calcined to prepare vanadium pentoxide with the following components:
| composition of the components | V 2 O 5 ％ | Si％ | Fe％ | P％ |
| Content of | 99.20 | 0.105 | 0.016 | ＜0.0001 |
Embodiment II,
Step one, taking vanadium pentoxide V 2 O 5 The dephosphorization slag with the content of 30.7 percent, the phosphorus content of 0.48 percent and the iron content of 13.25 percent is mixed with water according to the solid-to-liquid ratio of 3.5:1, and the mixture is obtained by stirring and slurrying.
Slowly adding industrial sulfuric acid into the pulpified mixed solution, controlling the pH value to be 2, stirring and leaching for 1 hour at normal temperature, performing liquid-solid separation through filtering equipment after leaching to obtain leaching liquid and filter residues, washing the filter residues, and returning the produced washing water to the pulpified leaching process for removing the phosphorus residues in the step 1 as the leaching liquid for recycling.
Pumping the leaching solution into a reaction kettle for impurity removal treatment, heating to 30 ℃, stirring, adding sodium hydroxide, adjusting the pH value to 9.5, heating to 85 ℃, continuing to react for 40 minutes, monitoring and keeping the pH value to 9.5, and obtaining the mixed solution after impurity removal after the reaction is finished.
And step four, settling the mixed solution obtained in the step three in a storage tank for 72 hours, and then carrying out liquid-solid separation through filtering equipment to obtain pure vanadium-containing solution, and bagging the impurity-removed filter residues for subsequent recovery treatment.
And fifthly, adding a vanadium precipitating agent with the vanadium pentoxide metal content being 2.3 times into the pure vanadium-containing solution to precipitate vanadium, reacting at normal temperature for 1 hour, detecting that the vanadium pentoxide concentration in the vanadium precipitation supernatant is less than 0.30 g/L, performing liquid-solid separation through filtering equipment after passing the vanadium precipitation supernatant, and obtaining the product ammonium metavanadate, and performing wastewater treatment on the vanadium precipitation supernatant and then discharging the vanadium precipitation supernatant after passing the wastewater treatment.
And step six, packaging the product ammonium metavanadate.
The obtained ammonium metavanadate is calcined to prepare vanadium pentoxide with the following components:
| composition of the components | V 2 O 5 ％ | Si％ | Fe％ | P％ |
| Content of | 99.32 | 0.130 | 0.013 | ＜0.0001 |
Third embodiment,
Step one, taking vanadium pentoxide V 2 O 5 36.5 percent of dephosphorization slag with 0.54 percent of P and 10.79 percent of Fe, mixing the dephosphorization slag with water according to the solid-to-liquid ratio of 3.5:1, and stirring and slurrying to obtain mixed liquid.
Slowly adding industrial sulfuric acid into the pulpified mixed solution, controlling the pH value to be 2, stirring and leaching for 1 hour at normal temperature, performing liquid-solid separation through filtering equipment after leaching to obtain leaching liquid and filter residues, washing the filter residues, and returning the produced washing water to the pulpified leaching process for removing the phosphorus residues in the step 1 as the leaching liquid for recycling.
Pumping the leaching solution into a reaction kettle for impurity removal treatment, heating to 30 ℃, stirring, adding sodium hydroxide, adjusting the pH value to 9.5, heating to 85 ℃, continuing to react for 40 minutes, monitoring and keeping the pH value to 9.5, and obtaining the mixed solution after impurity removal after the reaction is finished.
And step four, settling the mixed solution obtained in the step three in a storage tank for 72 hours, and then carrying out liquid-solid separation through filtering equipment to obtain pure vanadium-containing solution, and bagging the impurity-removed filter residues for subsequent recovery treatment.
And fifthly, adding a vanadium precipitating agent with the vanadium pentoxide metal content being 2.3 times into the pure vanadium-containing solution to precipitate vanadium, reacting at normal temperature for 1 hour, detecting that the vanadium pentoxide concentration in the vanadium precipitation supernatant is less than 0.30 g/L, performing liquid-solid separation through filtering equipment after passing the vanadium precipitation supernatant, and obtaining the product ammonium metavanadate, and performing wastewater treatment on the vanadium precipitation supernatant and then discharging the vanadium precipitation supernatant after passing the wastewater treatment.
And step six, packaging the product ammonium metavanadate.
The obtained ammonium metavanadate is calcined to prepare vanadium pentoxide with the following components:
| composition of the components | V 2 O 5 ％ | Si％ | Fe％ | P％ |
| Content of | 99.36 | 0.150 | 0.022 | 0.012 |
According to the method, the dephosphorization slag and the water are mixed in proportion, sulfuric acid is added at normal temperature for leaching, the vanadium-containing leaching solution is subjected to impurity removal treatment and then vanadium precipitation at normal temperature, so that the ammonium metavanadate product is prepared, the purity of the obtained ammonium metavanadate is higher than 99%, the direct vanadium yield is as high as 92%, and the problems in the prior art are effectively solved.
Claims (4)
1. A method for producing ammonium metavanadate by taking dephosphorization slag as a raw material is characterized by comprising the following steps: comprising the following steps, which are sequentially carried out,
step one, mixing the dephosphorized slag and water according to a solid-to-liquid ratio of 3.5:1, and stirring and slurrying to obtain a mixed solution;
step two, adding sulfuric acid into the mixed solution obtained in the step one, enabling the pH value of the mixed solution to be 2, stirring for 1 hour under normal temperature condition, leaching, and obtaining leaching liquid and filter residues through solid-liquid separation;
pumping the leaching solution into a reaction kettle for impurity removal treatment, heating the reaction kettle to 30 ℃, stirring, adding sodium hydroxide, and adjusting the pH value to 9.5; continuously heating to 85 ℃, keeping the pH value to be 9.5, and reacting for 40 minutes to obtain mixed solution after impurity removal;
step four, placing the mixed solution obtained in the step three after impurity removal into a storage tank for sedimentation, and carrying out solid-liquid separation after sedimentation for 72 hours to obtain pure vanadium-containing solution and impurity removal filter residues;
step five, adding a vanadium precipitating agent with the metal content of vanadium pentoxide being 2.3 times into the pure vanadium-containing solution obtained in the step four to precipitate vanadium, carrying out a normal-temperature vanadium precipitation reaction for 1 hour, detecting the concentration of vanadium pentoxide in a vanadium precipitation supernatant, carrying out liquid-solid separation after passing, wherein a filter cake is ammonium metavanadate, and carrying out wastewater treatment on the vanadium precipitation supernatant and then discharging the qualified vanadium precipitation supernatant;
vanadium pentoxide V in the dephosphorization slag of the step one 2 O 5 30-35% of phosphorus, 0.40-0.60% of P and 5-15% of Fe;
the leaching solution obtained in the second step is vanadium pentoxide V 2 O 5 The concentration is 60g/L-75g/L.
2. The method for producing ammonium metavanadate from dephosphorization slag as a raw material according to claim 1, wherein the method comprises the following steps: and (3) washing the filter residue obtained in the step two, and then using the produced washing water as a phosphorus removal slag slurrying leaching liquid.
3. The method for producing ammonium metavanadate from dephosphorization slag as a raw material according to claim 1, wherein the method comprises the following steps: and (3) bagging and recycling the impurity-removed filter residues obtained in the step four.
4. The method for producing ammonium metavanadate from dephosphorization slag as a raw material according to claim 1, wherein the method comprises the following steps: and in the fifth step, the vanadium precipitating agent is ammonium sulfate.
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