CN114134344A - Method for precipitating vanadium by using ammonium metavanadate - Google Patents
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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Abstract
The invention relates to the technical field of chemical industry, and discloses a method for precipitating vanadium by using ammonium metavanadate. The method comprises the following steps: (1) adjusting the pH value of the vanadium precipitation solution to 1.8-5.0, then adding ammonium metavanadate for pulping, and adjusting the pH value of the pulping solution to 1.5-2.0, wherein the adding amount of ammonium metavanadate is NH in ammonium metavanadate4VO3The mass ratio of V in the vanadium precipitation solution to V in the vanadium precipitation solution is 1-5: 1 is the standard; (2) after the pH value of the pulping liquid is stable, the temperature of the pulping liquid is increased to 90-100 ℃ at the heating rate of 3-10 ℃/min, and the temperature is kept for precipitation to obtain ammonium polyvanadate; (3) and after filtering, washing and drying the ammonium polyvanadate, and calcining to obtain vanadium pentoxide. The method is simple to operate, the ammonium metavanadate is taken as the vanadium precipitation ammonium salt, the ammonium salt dosage can be obviously reduced, the ammonia nitrogen utilization rate is high, the influence of overhigh impurities in the vanadium liquid on the vanadium precipitation quality can be avoided, and the vanadium precipitation quality is preventedThe loss is small, and the ammonia nitrogen content in the wastewater is low.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to a method for precipitating vanadium by utilizing ammonium metavanadate.
Background
At present, the vanadium precipitation process in the industrial vanadium extraction process is mainly a chemical precipitation method, and comprises hydrolysis vanadium precipitation, ammonium salt vanadium precipitation, iron salt vanadium precipitation and calcium salt vanadium precipitation. The hydrolysis vanadium precipitation operation is simple, the production period is short, the production cost is low, the concentration of vanadium is allowed to fluctuate in a larger range, and the defects are that the red cake obtained by hydrolysis vanadium precipitation is crude vanadium, the product purity is lower, the acid consumption is large, the sewage quantity is large, and the red cake is basically replaced by ammonium salt vanadium precipitation; the precipitation amount of vanadium in calcium salt is large, and the subsequent work difficulty is large; the vanadium precipitation of calcium salt has high requirement on the purity of vanadium-containing solution, and the contents of Si and P are as low as possible; the vanadium precipitation of calcium salt is generally used as an intermediate product for enriching vanadium or used as a raw material for vanadium iron in smelting, and the application is limited. The precipitation amount of vanadium in calcium salt is large, and the subsequent work difficulty is large; the vanadium precipitation of calcium salt has high requirement on the purity of vanadium-containing solution, and the contents of Si and P are as low as possible; the vanadium precipitation of calcium salt is generally used as an intermediate product for enriching vanadium or used as a raw material for vanadium iron in smelting, and the application is limited. The vanadium precipitation amount of the iron salt is also larger, and the product purity is lower. Therefore, the prior art mainly adopts an ammonium salt vanadium precipitation process.
The ammonium consumption in the vanadium precipitation process of ammonium salt is high, the ammonia content in the wastewater is high, and the treatment is difficult.
Chinese patent CN112047379A entitled ammonium polyvanadate precipitation method provides a method for precipitating ammonium polyvanadate. Firstly, preheating a vanadium-containing solution to 60-80 ℃, adding ammonium salt, stirring and dissolving to obtain a mixed solution; adding the mixed solution into a certain amount of acid, and changing the feeding mode, and adopting a method of adding a vanadium liquid and ammonium salt mixture into a given amount of acid to realize rapid precipitation, wherein after precipitation is carried out for 15min, the vanadium precipitation rate can reach more than 99%; the ammonium-vanadium ratio can be reduced to 0.4-0.8, and the dosage of ammonium salt is reduced. The method has the advantages of low equipment requirement, convenient operation, wide application range, low cost and good social and economic benefits.
Chinese patent CN111020233B "A method for preparing vanadium pentoxide by precipitating vanadium without ammonium" includes the steps: reducing the vanadium-containing pickle liquor by using a reducing agent, and adjusting the pH of the solution by using ammonia water; extracting by adopting a cation extracting agent to obtain an organic phase loaded with vanadium oxide cations and raffinate; hydrogen peroxide and sulfuric acid are used for maintaining the pH value to be 1.5-2.5; and (3) keeping the temperature of 90-100 ℃, stirring, reacting for 15-45 min, filtering and washing to obtain the ammonium polyvanadate. The stripping agent is used for carrying out back extraction to obtain vanadium back extraction solution; after the stripping solution is placed for a period of time, peroxypolyvanadate is unstable, polyvanadate generated by decomposition is gradually separated out from a water phase, and then a vanadium pentoxide product is obtained by calcining. The method for preparing vanadium pentoxide by ammonium-free vanadium precipitation greatly simplifies the vanadium smelting process, thoroughly solves the problems of large consumption of sulfuric acid and ammonia water and large output of ammonia nitrogen wastewater in the back extraction process, has the technical characteristics of short process, environmental friendliness and high efficiency, and is easy for industrial popularization.
In view of the fact that the vanadium precipitation is carried out by adopting the mode of reducing the using amount of ammonium salt to precipitate vanadium and the mode of ammonium-free vanadium precipitation, the cost is high, the operation is complex, the ammonium metavanadate is used for replacing the traditional ammonium salt, the ammonium polyvanadate is precipitated from the vanadium liquid under the acidic condition, the operation is simple, the using amount of the ammonium salt is reduced to a certain degree, and the ammonia nitrogen utilization rate is high.
Disclosure of Invention
The invention aims to solve the problems that in the prior art, the ammonium consumption is high in the ammonium salt vanadium precipitation process, the ammonia content in the wastewater is high, the treatment is difficult, the vanadium precipitation is carried out by adopting a method of reducing the ammonium salt dosage and precipitating vanadium without ammonium, the cost is high and the operation is complex, and provides a method for precipitating vanadium by utilizing ammonium metavanadate.
In order to achieve the above object, the present invention provides a method for precipitating vanadium by using ammonium metavanadate, comprising the steps of:
(1) adjusting the pH value of the vanadium precipitation solution to 1.8-5.0, then adding ammonium metavanadate for pulping, and adjusting the pH value of the pulping solution to 1.5-2.0, wherein the adding amount of ammonium metavanadate is NH in ammonium metavanadate4VO3The mass ratio of V in the vanadium precipitation solution to V in the vanadium precipitation solution is 1-5: 1 is the standard;
(2) after the pH value of the pulping liquid is stable, the temperature of the pulping liquid is increased to 90-100 ℃ at the heating rate of 3-10 ℃/min, and the temperature is kept for precipitation to obtain ammonium polyvanadate;
(3) and after filtering, washing and drying the ammonium polyvanadate, and calcining to obtain vanadium pentoxide.
Preferably, in the step (1), the vanadium precipitation solution is a calcium-method acid leaching vanadium solution or a sodium-method water leaching vanadium solution.
Preferably, in the step (1), when the vanadium precipitation solution is a calcium-method acid leaching vanadium solution, the pH value of the vanadium precipitation solution is adjusted to 2.0-3.0; and when the vanadium precipitation solution is a sodium method water immersion vanadium precipitation solution, adjusting the pH value of the vanadium precipitation solution to 1.8-5.0.
Preferably, in the step (1), the pH value of the vanadium precipitation solution is adjusted by using 1:1 sulfuric acid.
Preferably, in step (1), the pH of the slurrying liquid is adjusted with a sulfuric acid solution.
More preferably, in step (1), 1:1 sulfuric acid solution to adjust the pH of the slurry.
Preferably, in the step (1), the beating temperature is 20-60 ℃.
Preferably, in the step (2), the heat preservation time is 30-60 min.
Preferably, in the step (3), the ammonium polyvanadate is washed with water, and the temperature of the washing water is 50-80 ℃.
Preferably, in the step (3), the drying temperature is 75-110 ℃; the drying time is more than 4 h.
Preferably, in the step (3), the calcination temperature is 500 to 550 ℃, and the calcination time is 150 to 240 min.
Compared with the prior art, the invention has the following advantages:
1) the ammonium metavanadate is used as the ammonium salt, so that the vanadium concentration in the vanadium precipitation solution can be increased, the impurity content in the vanadium precipitation solution is diluted, the V/P value is improved, the Na/V value is reduced, and the influence of overhigh impurity content in the vanadium precipitation solution on the vanadium precipitation quality is effectively avoided;
2) ammonium metavanadate is taken as precipitated vanadium ammonium salt, the dosage of the ammonium salt can be obviously reduced, and the coefficient (mass ratio) of adding the ammonium metavanadate is only NH4VO3The concentration of the ammonia nitrogen in the wastewater is 1-5, the ammonia nitrogen utilization rate is high, the ammonia nitrogen in the wastewater is less, and the cost is reduced.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The invention provides a method for precipitating vanadium by using ammonium metavanadate, which comprises the following steps:
(1) adjusting the pH value of the vanadium precipitation solution to 1.8-5.0, then adding ammonium metavanadate for pulping, and adjusting the pH value of the pulping solution to 1.5-2.0, wherein the adding amount of ammonium metavanadate is NH in ammonium metavanadate4VO3The mass ratio of V in the vanadium precipitation solution to V in the vanadium precipitation solution is 1-5: 1 is the standard;
(2) after the pH value of the pulping liquid is stable, the temperature of the pulping liquid is increased to 90-100 ℃ at the heating rate of 3-10 ℃/min, and the temperature is kept for precipitation to obtain ammonium polyvanadate;
(3) and after filtering, washing and drying the ammonium polyvanadate, and calcining to obtain vanadium pentoxide.
In the method, in the step (1), the vanadium precipitation solution is a calcium-method acid leaching vanadium solution or a sodium-method water leaching vanadium solution.
According to the method, ammonium metavanadate replaces the traditional ammonium salts such as ammonium sulfate, ammonium chloride, ammonium carbonate and ammonium bicarbonate to serve as vanadium precipitation ammonium salts, the vanadium precipitation liquid is adjusted to a specific pH value, then the ammonium metavanadate is added for pulping, loss of ammonium salts in the process of adjusting the pH value after the ammonium metavanadate is added can be avoided, the ammonium polyvanadate is precipitated at high temperature after the pH value is continuously adjusted to the optimal state of vanadium precipitation, and then the ammonium polyvanadate is filtered, washed, dried and calcined to obtain vanadium pentoxide.
The existing method mainly adopts ammonium sulfate, ammonium chloride, ammonium carbonate, ammonium bicarbonate and the like as ammonium salts to carry out vanadium precipitation, and the ammonium salts are combined with vanadate in solutionAnd generating ammonium polyvanadate under a high-temperature condition, wherein the ammonium addition coefficient of the method is 1.8-6.0 times of the mass of vanadium in the vanadium precipitation solution. And this application adopts ammonium metavanadate as heavy vanadium ammonium salt, and ammonium metavanadate adds back in heavy vanadium liquid this application after dissolving in heavy vanadium liquid under the condition, increases the vanadium content in the heavy vanadium liquid, and ammonium reacts with the vanadium in the heavy vanadium liquid again simultaneously, generates ammonium polyvanadate, and ammonium metavanadate splits under acidic regulation promptly, and partly directly generates ammonium polyvanadate, and remaining ammonium radical ion combines with the vanadate in the heavy vanadium liquid and generates ammonium polyvanadate, and it only is NH to add ammonium metavanadate mass coefficient4VO3/V＝1～5。
By adopting the method for precipitating vanadium, the ammonium-vanadium ratio in the vanadium precipitation process can be obviously reduced. For example: when the mass of vanadium in the vanadium precipitation solution is 51g (namely the vanadium is 1 mol), ammonium sulfate is used as ammonium salt (the ammonium addition coefficient is 1.8-2), and when the ammonium addition coefficient is 1.8, the molar weight of ammonium is as follows: (51 × 1.8 ÷ 132) × 2 ═ 1.40; when the ammonium addition coefficient is 2, the molar amount of ammonium is: (51 multiplied by 2 divided by 132) multiplied by 2 which is 1.54, namely the molar ratio of ammonium to vanadium is 1.4-1.54: 1 when the ammonium sulfate is used for precipitating vanadium. In the same way, when ammonium metavanadate is adopted as a vanadium precipitation ammonium salt (the ammonium addition coefficient is 1-5), and when the ammonium addition coefficient is 1, the molar weight of ammonium is as follows: 51 × 1 ÷ 117 ═ 0.44, the ammonium vanadium molar ratio: 0.44 (1+0.44) ═ 0.44:1.44 ═ 0.3: 1; when the ammonium addition coefficient is 5, the molar weight of ammonium is as follows: 51 × 5 ÷ 117 ═ 2.18, ammonium vanadium molar ratio 2.18: (1+2.18) ═ 0.685:1, namely when ammonium metavanadate is used for precipitating vanadium, the molar ratio of ammonium to vanadium is 0.3-0.685: 1. Therefore, the method for precipitating vanadium has the advantages that the molar ratio of ammonium to vanadium is obviously reduced, namely the ammonium dosage is obviously reduced and the ammonia nitrogen utilization rate is obviously improved compared with the prior art. Meanwhile, the calcium-method acid leaching vanadium liquid contains P, Mn and other impurities, the sodium-method water leaching vanadium liquid contains Si, Na, Cr and other impurities, ammonium metavanadate is used as an ammonium salt, the vanadium concentration in the vanadium precipitation liquid is increased, the impurity content in the vanadium precipitation liquid is diluted, and the influence of overhigh impurity content in the vanadium precipitation liquid on the vanadium precipitation quality can be effectively avoided.
In a specific embodiment, in step (1), when the vanadium precipitation solution is a calcium-process acid leaching vanadium solution, the pH of the vanadium precipitation solution may be adjusted to 2.0 to 3.0, for example, 2.0, 2.1, 2.2, 2.3, 2.4, 2.5, 2.6, 2.7, 2.8, 2.9, or 3.0. When the vanadium precipitation solution is a sodium method water leaching vanadium solution, the pH value of the vanadium precipitation solution is adjusted to 1.8-5.0, such as 1.8, 2.0, 2.2, 2.4, 2.6, 2.8, 3.0, 3.2, 3.4, 3.6, 3.8, 4.0, 4.2, 4.4, 4.6, 4.8 or 5.0.
In a specific embodiment, in step (1), 1:1, adjusting the pH value of the vanadium precipitation solution by sulfuric acid. Herein, the 1:1 sulfuric acid means sulfuric acid obtained by mixing water and sulfuric acid in a volume ratio of 1: 1.
In the method of the present invention, in the step (1), the pH of the slurry is adjusted with a sulfuric acid solution. Specifically, 1:1 sulfuric acid solution to adjust the pH of the slurry.
In a specific embodiment, the pH of the slurry may be adjusted to 1.5-2.0, such as 1.5, 1.6, 1.7, 1.8, 1.9 or 2.0, which is a preferable pH for vanadium precipitation, so as to prevent the quality of vanadium precipitation from being affected.
In the method of the present invention, in the step (1), the beating temperature may be 20 to 60 ℃, specifically, for example, 20 ℃, 25 ℃, 30 ℃, 35 ℃, 40 ℃, 45 ℃, 50 ℃, 55 ℃ or 60 ℃. Pulping is carried out within the temperature range of 20-60 ℃, impurities mixed in Ammonium Polyvanadate (APV) can be washed away, and meanwhile, the ammonium polyvanadate is not dissolved in the solution to cause loss.
In a specific embodiment, in step (2), the temperature rise rate may be 3 ℃/min, 4 ℃/min, 5 ℃/min, 6 ℃/min, 7 ℃/min, 8 ℃/min, 9 ℃/min, or 10 ℃/min.
In specific embodiments, the temperature of the slurrying solution may be raised to 90 ℃, 91 ℃, 92 ℃, 93 ℃, 94 ℃, 95 ℃, 96 ℃, 97 ℃, 98 ℃, 99 ℃ or 100 ℃ for precipitation.
In a preferred embodiment, in the step (2), the heat preservation time is 30-60 min, such as 30min, 35min, 40min, 45min, 50min, 55min or 60 min.
In the method of the present invention, in the step (3), the ammonium polyvanadate is washed with water, and the temperature of the washing water used is 50 to 80 ℃, specifically, the temperature of the washing water may be, for example, 50 ℃, 55 ℃, 60 ℃, 65 ℃, 70 ℃, 75 ℃ or 80 ℃. In the invention, washing with washing water at 50-80 ℃ can wash off part of impurities in the ammonium polyvanadate.
In a specific embodiment, in the step (3), the drying temperature may be 75 to 110 ℃, for example, 75 ℃, 80 ℃, 85 ℃, 90 ℃, 95 ℃, 100 ℃, 105 ℃ or 110 ℃.
In a specific embodiment, in step (3), the drying time is greater than 4h, for example, may be 5h, 6h, 7h, 8h, 9h, 10h, 11h, or 12 h.
In the method of the present invention, in the step (3), the calcination temperature may be 500 to 550 ℃, for example, 500 ℃, 505 ℃, 510 ℃, 515 ℃, 520 ℃, 525 ℃, 530 ℃, 535 ℃, 540 ℃, 545 ℃ or 550 ℃; the calcination time may be 150-240 min, such as 150min, 160min, 170min, 180min, 190min, 200min, 210min, 220min, 230min, or 240 min.
By adopting the method, the influence of overhigh impurity content in the vanadium precipitation liquid on the quality of the vanadium precipitation can be effectively reduced, and the obtained vanadium pentoxide meets the requirements of YB/T5304-2017 quality standard.
The present invention will be described in detail by way of examples, but the scope of the present invention is not limited thereto.
Example 1
100ml of acid leaching vanadium liquid by a calcium method is measured and put in a beaker, an electric stirrer is started to stir, the rotating speed is set to be 260r/min, 1:1 sulfuric acid is used for adjusting the pH value of the solution to be 2.8, and the ammonium metavanadate addition coefficient (mass ratio) is NH4VO3Adding ammonium metavanadate solid into the solution with the V being 1, pulping the solution at the temperature of 20 ℃, and then adding 1:1, the pH value of the pulping liquid is adjusted to 2.0. After the pH value is stable, heating to 95 ℃ at a heating rate of 10 ℃/min, carrying out heat preservation reaction at 95 ℃ for 30min, closing an electric stirrer to filter in time after the heat preservation time is reached, washing ammonium polyvanadate once by using tap water at 50 ℃, then drying the ammonium polyvanadate at 110 ℃, and calcining at 500 ℃ for 240min after the drying time is more than 4h to obtain vanadium pentoxide.
The vanadium precipitation rate of example 1 was 99%; the elemental composition of vanadium pentoxide was P content 0.012%, S content 0.012%, Fe content 0.10%, Si content 0.032%, K2O content 0.02%, Na2The O content is 0.021 percent, the V content is 55.6 percent, and the obtained vanadium pentoxide meets the requirements of YB/T5304-2017 quality standard.
Example 2
100ml of sodium method water immersion vanadium liquid is measured and put in a beaker, an electric stirrer is started to stir, the rotating speed is set to be 260r/min, 1:1 sulfuric acid is used for adjusting the pH value of the solution to be 5.0, and the ammonium metavanadate addition coefficient (mass ratio) is NH4VO3Adding ammonium metavanadate solid for pulping at 60 ℃ and then adding a mixture of 1:1, the pH value of the pulping liquid is adjusted to 2.0. After the pH value is stable, heating to 90 ℃ at a heating rate of 3 ℃/min, carrying out heat preservation reaction at 90 ℃ for 60min, closing an electric stirrer to filter in time after the heat preservation time is reached, washing ammonium polyvanadate once by using tap water at 80 ℃, then drying the ammonium polyvanadate at 75 ℃ for more than 4h, and calcining at 550 ℃ for 150min to obtain vanadium pentoxide.
The vanadium precipitation rate of example 2 is 99.2%; the content of vanadium pentoxide element is composed of P0.01%, S0.012%, Fe 0.01%, Si 0.01%, K2O content 0.02%, Na2The O content is 0.025 percent, the V content is 55.6 percent, and the obtained vanadium pentoxide meets the requirements of YB/T5304-2017 quality standard.
Example 3
100ml of acid leaching vanadium liquid by a calcium method is measured and put in a beaker, an electric stirrer is started to stir, the rotating speed is set to be 260r/min, 1:1 sulfuric acid is used for adjusting the pH value of the solution to be 2.8, and the ammonium metavanadate addition coefficient (mass ratio) is NH4VO3Adding ammonium metavanadate solid for pulping at 40 ℃, and then adding 1: the pH value of the pulping liquid is adjusted to 1.5 by the sulfuric acid solution of 1. After the pH value is stable, heating to 90 ℃ at a heating rate of 10 ℃/min, carrying out heat preservation reaction at 90 ℃ for 60min, closing an electric stirrer to filter in time after the heat preservation time is reached, washing ammonium polyvanadate once by using tap water at 80 ℃, then drying the ammonium polyvanadate at 110 ℃, calcining at 550 ℃ for 240min after the drying time is more than 4h, and obtaining vanadium pentoxide.
The vanadium precipitation rate of example 3 is 99.15%; element content group of vanadium pentoxideThe contents of P, S, Fe, Si, K and Si are 0.011%, 0.012%, 0.098%, 0.032% and 0.098%, respectively2O content 0.02%, Na2The O content is 0.021 percent, the V content is 55.56 percent, and the obtained vanadium pentoxide meets the requirements of YB/T5304-2017 quality standard.
Comparative example 1
The procedure is as in example 1, except that 1:1 sulfuric acid solution adjusted the pH of the slurrying to 3.0.
The vanadium deposition rate of comparative example 1 was 98.9%; the content of vanadium pentoxide element is composed of P content 0.128%, S content 0.10%, Fe content 0.20%, Si content 0.35%, K2O content 0.02%, Na2The O content is 0.021 percent, the V content is 53.68 percent, and the obtained vanadium pentoxide does not meet the quality standard requirement of YB/T5304-2017.
Comparative example 2
The procedure is as in example 1 except that the reaction is carried out at a temperature of 80 ℃ at a temperature rise rate of 10 ℃/min after the pH is stabilized, and the reaction is carried out at 80 ℃ for 30 min.
The vanadium deposition rate of comparative example 2 was 90%; the content of vanadium pentoxide element is composed of P0.218%, S0.20%, Fe 0.089%, Si 0.37%, and K2O content 0.102%, Na2The O content is 0.051 percent, the V content is 53.4 percent, and the obtained vanadium pentoxide can not meet the quality standard requirement of YB/T5304-2017.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. A method for precipitating vanadium by utilizing ammonium metavanadate is characterized by comprising the following steps:
(1) adjusting the pH value of the vanadium precipitation solution to 1.8-5.0, then adding ammonium metavanadate for pulping, and adjusting the pH value of the pulping solution to 1.5-2.0, wherein the pH value of ammonium metavanadateThe addition amount is NH in ammonium metavanadate4VO3The mass ratio of V in the vanadium precipitation solution to V in the vanadium precipitation solution is 1-5: 1 is the standard;
(2) after the pH value of the pulping liquid is stable, the temperature of the pulping liquid is increased to 90-100 ℃ at the heating rate of 3-10 ℃/min, and the temperature is kept for precipitation to obtain ammonium polyvanadate;
(3) and after filtering, washing and drying the ammonium polyvanadate, and calcining to obtain vanadium pentoxide.
2. The method according to claim 1, wherein in the step (1), the vanadium precipitation solution is a calcium method acid leaching vanadium solution or a sodium method water leaching vanadium solution.
3. The method according to claim 2, wherein in the step (1), when the vanadium precipitation solution is a calcium method acid leaching vanadium solution, the pH value of the vanadium precipitation solution is adjusted to 2.0-3.0; and when the vanadium precipitation solution is a sodium method vanadium leaching solution, adjusting the pH value of the vanadium precipitation solution to 1.8-5.0.
4. The method according to claim 1 or 2, wherein in step (1), the pH value of the vanadium precipitation solution is adjusted by using 1:1 sulfuric acid.
5. The method according to claim 1 or 2, wherein in the step (1), the pH value of the slurry is adjusted with a sulfuric acid solution;
preferably, a 1:1 sulfuric acid solution to adjust the pH of the slurry.
6. The method according to claim 1, wherein the beating temperature in step (1) is 20-60 ℃.
7. The method according to claim 1, wherein in the step (2), the holding time is 30-60 min.
8. The method according to claim 1, wherein in the step (3), the ammonium polyvanadate is washed with water, and the temperature of the washing water is 50 to 80 ℃.
9. The method according to claim 1, wherein in the step (3), the drying temperature is 75-110 ℃; the drying time is more than 4 h.
10. The method according to claim 1, wherein in the step (3), the calcination temperature is 500 to 550 ℃, and the calcination time is 150 to 240 min.
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| CN115594221A (en) * | 2022-11-15 | 2023-01-13 | 攀钢集团攀枝花钢铁研究院有限公司（Cn） | Method for preparing flaky high-density ammonium polyvanadate from vanadium liquid with low ammonium content |
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| CN112047379A (en) * | 2020-09-14 | 2020-12-08 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for precipitating ammonium polyvanadate |
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| CN115594221A (en) * | 2022-11-15 | 2023-01-13 | 攀钢集团攀枝花钢铁研究院有限公司（Cn） | Method for preparing flaky high-density ammonium polyvanadate from vanadium liquid with low ammonium content |
| CN115594221B (en) * | 2022-11-15 | 2024-03-19 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing flaky high-density ammonium polyvanadate from low ammonium content in vanadium liquid |
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