CN111410228A - Method for preparing high-purity vanadium oxychloride from ferrovanadium fine powder - Google Patents
Method for preparing high-purity vanadium oxychloride from ferrovanadium fine powder Download PDFInfo
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- CN111410228A CN111410228A CN202010245509.8A CN202010245509A CN111410228A CN 111410228 A CN111410228 A CN 111410228A CN 202010245509 A CN202010245509 A CN 202010245509A CN 111410228 A CN111410228 A CN 111410228A
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Abstract
The invention belongs to the technical field of chemical metallurgy, and particularly relates to a method for preparing high-purity vanadium oxychloride from ferrovanadium fine powder. The invention aims to solve the technical problem of providing a method for preparing high-purity vanadium oxychloride by effectively utilizing ferrovanadium fine powder. The method comprises the following steps: a. putting the ferrovanadium fine powder into a chlorination reactor, introducing nitrogen, heating to 300-600 ℃, introducing chlorine and oxygen, adjusting the total flow rate of the nitrogen, the chlorine and the oxygen, and carrying out chlorination reaction, wherein in the reaction process, volatile components in the reactor are condensed to obtain a crude product of vanadium oxytrichloride; b. after the chlorination reaction is finished, stopping introducing chlorine and oxygen, adjusting the nitrogen flow rate again, and stopping introducing nitrogen after the reactor is cooled to room temperature; c. and distilling the crude product of the vanadium oxychloride, and condensing to obtain the high-purity vanadium oxychloride. The method can prepare high-purity vanadium oxychloride products, the purity can reach more than 99.9 percent, and the chlorination efficiency of vanadium in the ferrovanadium fine powder can be improved.
Description
Technical Field
The invention belongs to the technical field of chemical metallurgy, and particularly relates to a method for preparing high-purity vanadium oxychloride from ferrovanadium fine powder.
Background
Vanadium oxychloride is an important chemical intermediate, is a catalyst or a pre-catalyst for preparing ethylene propylene rubber, can be used as an organic solvent, and is a raw material for synthesizing an organic vanadium compound. In addition, vanadium oxychloride is also an important raw material for preparing high-purity vanadium pentoxide, and the purity of the high-purity vanadium pentoxide prepared by using the vanadium oxychloride as the raw material can usually reach more than 99.99% (4N). With the continuous development of industries such as chemical industry, energy storage and the like, the demand of high-purity vanadium oxychloride is increasing day by day, and particularly in the field of vanadium battery energy storage, high-purity vanadium pentoxide is prepared by taking the high-purity vanadium oxychloride as a raw material, and then low-impurity vanadium electrolyte is prepared by taking the high-purity vanadium pentoxide as a raw material, so that the technical purpose of improving the electrolyte performance of the vanadium battery can be achieved. The raw material for preparing the vanadium oxychloride is usually vanadium oxide or vanadium-containing mineral, but the crude vanadium oxychloride prepared from the raw material usually needs to be subjected to a complicated rectification impurity removal process to prepare high-purity vanadium oxychloride, so that the preparation cost is increased, and the process feasibility is reduced to a certain extent.
In the ferrovanadium smelting process, after the prepared ferrovanadium alloy is cooled and removed from the furnace, the alloy cake needs to be crushed, a large amount of ferrovanadium fragments are generated in the crushing process, and the particle size of the ferrovanadium fragments is usually small and cannot meet the particle size standard of ferrovanadium products, so that the part of ferrovanadium fragments can be recycled only in a mode of remelting in the furnace, the energy consumption is high, and the cost is increased; meanwhile, in the process of returning and charging, part of the ferrovanadium fine powder with ultrafine grain diameter (the average grain diameter is less than 100 mu m) is easily pumped into a dust removal system, so that the loss of vanadium is caused to a certain extent. Therefore, how to fully and effectively utilize the part of ferrovanadium fine powder will affect the production efficiency and the economical efficiency of a ferrovanadium smelting system. At present, there are few reports on the recycling of ferrovanadium fine powder.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for preparing high-purity vanadium oxychloride by effectively utilizing ferrovanadium fine powder.
The technical scheme adopted by the invention for solving the technical problems is to provide a method for preparing high-purity vanadium oxychloride from ferrovanadium fine powder. The method comprises the following steps:
a. putting the ferrovanadium fine powder into a chlorination reactor, introducing nitrogen, heating to 300-600 ℃, introducing chlorine and oxygen, adjusting the total flow rate of the nitrogen, the chlorine and the oxygen, and carrying out chlorination reaction, wherein in the reaction process, volatile components in the reactor are condensed to obtain a crude product of vanadium oxytrichloride;
b. after the chlorination reaction is finished, stopping introducing chlorine and oxygen, adjusting the nitrogen flow rate again, and stopping introducing nitrogen after the reactor is cooled to room temperature;
c. and distilling the crude product of the vanadium oxychloride, and condensing to obtain the high-purity vanadium oxychloride.
Further, in the step a, the particle size of the ferrovanadium fine powder is 5-200 μm, and the vanadium content in the ferrovanadium fine powder is 40-85%.
Further, in the step a, the flow velocity of the introduced nitrogen is 0.01-0.03 m/s.
Further, in the step a, the time of chlorination reaction is 60 min-120 min.
Further, in the step a, the total flow rate of the nitrogen, the chlorine and the oxygen is adjusted to be 0.02 m/s-0.08 m/s.
Further, in the step a, the mole ratio of the introduced chlorine to the oxygen is 2-3: 1; the chlorine gas accounts for 20-50% of the volume fraction of the mixed gas of the nitrogen gas, the chlorine gas and the oxygen gas.
Further, in the step a, the tail gas in the chlorination reaction process is absorbed by a 30% sodium hydroxide aqueous solution.
Further, in the step b, the flow rate of the nitrogen is adjusted to 0.01 m/s-0.03 m/s again.
Further, in the step c, the distillation is carried out until the obtained product is 90-95% of the mass of the crude product of the vanadium oxychloride.
Preferably, the temperature of the distillation is from 125 ℃ to 130 ℃.
The invention has the beneficial effects that:
the method of the invention takes ferrovanadium alloy fine powder as a raw material, can prepare high-purity vanadium oxychloride products through chlorination process, has the purity of over 99.9 percent, can improve the added value of the products, simultaneously realizes the recycling of vanadium-containing secondary resources of a ferrovanadium smelting system, and can improve the chlorination efficiency of the ferrovanadium fine powder. The method takes ferrovanadium alloy fine powder as a raw material, chloridizes the raw material in the mixed atmosphere of chlorine, oxygen and nitrogen, chloridizes vanadium into coarse vanadium oxychloride, and then distills the obtained coarse vanadium oxychloride to prepare the high-purity vanadium oxychloride.
Detailed Description
Aiming at the defects of the prior art, the method takes the ferrovanadium fine powder as a raw material, chloridizes vanadium in the ferrovanadium fine powder into crude product vanadium oxychloride in a mixed atmosphere of chlorine, oxygen and nitrogen through a chlorination process, and then effectively removes impurities in the crude product vanadium oxychloride through simple distillation so as to prepare the high-purity vanadium oxychloride product. The method has simple steps and convenient operation, and the prepared crude product of the vanadium oxychloride has high separation and purification efficiency, and the corresponding vanadium oxychloride product has high purity, thereby being beneficial to the improvement of the application performance and the added value. By the method, the high-efficiency and high-value utilization of the ferrovanadium fine powder is realized, and a ferrovanadium fine powder recycling process method is formed. Meanwhile, the method has high process feasibility, is easy to realize industrial application, and has high application value.
Specifically, the method for preparing high-purity vanadium oxychloride from the ferrovanadium fine powder comprises the following steps:
a. putting ferrovanadium fine powder with the granularity of 5-200 mu m and the vanadium content of 40-85 percent into a chlorination reactor, introducing nitrogen with the flow rate of 0.01-0.03 m/s, heating to 300-600 ℃, introducing chlorine and oxygen, and adjusting the total flow rate of the nitrogen, the chlorine and the oxygen to be 0.02-0.08 m/s, wherein the mol ratio of the introduced chlorine to the oxygen is 2-3: 1; chlorine gas accounts for 20-50% of the volume fraction of the mixed gas of nitrogen gas, chlorine gas and oxygen gas, chlorination reaction is carried out, during the reaction process, volatile components in the reactor are condensed, and a crude product of vanadium oxychloride is obtained, wherein the chlorination reaction time is 60-120 min;
b. after the chlorination reaction is finished, stopping introducing the chlorine and the oxygen, adjusting the flow rate of the nitrogen to be 0.01-0.03 m/s again, and stopping introducing the nitrogen after the reactor is cooled to the room temperature;
c. distilling the vanadium oxychloride crude product at 125-130 ℃, distilling until the obtained product is 90-95% of the mass of the vanadium oxychloride crude product, and condensing to obtain the high-purity vanadium oxychloride.
In the step a of the invention, tail gas in the chlorination reaction process is absorbed by 30% sodium hydroxide aqueous solution, and the absorbed solution can be used as raw materials for preparing sodium chloride and sodium hypochlorite.
In step a of the invention, in order to exhaust the air in the reactor and simultaneously facilitate the stabilization of the thermal field in the reactor, the ferrovanadium fine powder is placed in a chlorination reactor and then nitrogen is introduced. The temperature is increased to 300-600 ℃, and the nitrogen flow rate is adjusted to adjust the volume fraction of the chlorine gas to play a role in dilution.
The invention can efficiently chlorinate vanadium by controlling chlorination temperature, chlorination time and chlorine content, and can inhibit chlorination of iron to the maximum extent. The chlorination temperature is controlled to be 300-600 ℃, which is beneficial to the selective chlorination of vanadium, if the temperature is too high, vanadium and iron in the ferrovanadium fine powder are both chlorinated, the consumption of chlorine is increased, and the subsequent distillation efficiency is reduced; if the temperature is too low, the chlorination reaction is slow, and neither vanadium nor iron can be chlorinated.
In the step b of the invention, after the chlorination reaction is finished, the chlorine and the oxygen are stopped to be introduced, and the nitrogen flow rate is adjusted to be 0.01-0.03 m/s again so as to cool the reactor and discharge the residual products in the reactor.
The present invention will be further illustrated by the following specific examples.
Example 1
500g of ferrovanadium fine powder is placed in a corundum crucible, the particle size of the ferrovanadium fine powder is 5-200 mu m, the vanadium content is 40%, the crucible is placed in a quartz chlorination reactor, 0.01m/s of nitrogen is introduced into the reactor, and then the reactor is placed in a tubular furnace for heating; when the furnace temperature reaches and is constant at 600 ℃, readjusting the flow rate of nitrogen in the reactor, and introducing chlorine and oxygen into the reactor, so that the total gas velocity of the nitrogen, the chlorine and the oxygen in the reactor is kept at 0.02m/s, the molar ratio of the chlorine to the oxygen is 2:1, and the volume fraction of the chlorine in the mixed gas (chlorine, nitrogen and oxygen) is 50%; in the chlorination reaction process, condensing and collecting components volatilized from a chlorination reactor to obtain a crude product of the vanadium oxychloride, and absorbing and purifying tail gas by adopting a 30% sodium hydroxide aqueous solution; stopping introducing chlorine and oxygen after reacting for 120min, adjusting the flow of introduced nitrogen to be 0.01m/s, cooling the reactor to room temperature, stopping introducing nitrogen, taking out unreacted ferrovanadium fine powder, and calculating to obtain the chlorination rates of vanadium and iron to be 95.02% and 40.34% respectively; distilling the crude product of the vanadium oxychloride at 125 ℃ for 15min until the obtained product is 90% of the mass of the crude product of the vanadium oxychloride and the purity of the obtained product of the vanadium oxychloride is 99.90%.
Example 2
Putting 200g of ferrovanadium fine powder into a corundum crucible, wherein the particle size of the ferrovanadium fine powder is 5-200 mu m, the vanadium content is 85%, putting the crucible into a quartz chlorination reactor, introducing 0.03m/s of nitrogen into the reactor, and then putting the reactor into a tubular furnace for heating; when the furnace temperature reaches and is constant at 300 ℃, readjusting the flow rate of nitrogen in the reactor, and introducing chlorine and oxygen into the reactor, so that the total gas velocity of the nitrogen, the chlorine and the oxygen in the reactor is kept at 0.05m/s, the molar ratio of the chlorine to the oxygen is 3:1, and the volume fraction of the chlorine in the mixed gas (chlorine, nitrogen and oxygen) is 30%; in the chlorination reaction process, condensing and collecting components volatilized from a chlorination reactor to obtain a crude product of the vanadium oxychloride, and absorbing and purifying tail gas by adopting a 30% sodium hydroxide aqueous solution; after the reaction is carried out for 60min, stopping introducing chlorine and oxygen, adjusting the flow rate of introduced nitrogen to be 0.03m/s, cooling the reactor to room temperature, stopping introducing nitrogen, taking out unreacted ferrovanadium fine powder, and calculating to obtain the chlorination rates of vanadium and iron to be 96.78% and 11.28% respectively; distilling the crude product of the vanadium oxychloride at 130 ℃ for 10min until the obtained product is 95% of the mass of the crude product of the vanadium oxychloride and the purity of the obtained product of the vanadium oxychloride is 99.98%.
Example 3
300g of ferrovanadium fine powder is placed in a corundum crucible, the particle size of the ferrovanadium fine powder is 5-200 mu m, the vanadium content is 50%, the crucible is placed in a quartz chlorination reactor, 0.02m/s of nitrogen is introduced into the reactor, and then the reactor is placed in a tubular furnace for heating; when the furnace temperature reaches and is constant at 500 ℃, readjusting the flow rate of nitrogen in the reactor, and introducing chlorine and oxygen into the reactor to keep the total gas velocity of the nitrogen, the chlorine and the oxygen in the reactor at 0.08m/s, wherein the molar ratio of the chlorine to the oxygen is 2.5:1, and the volume fraction of the chlorine in the mixed gas (chlorine, nitrogen and oxygen) is 20%; in the chlorination reaction process, condensing and collecting components volatilized from a chlorination reactor to obtain a crude product of the vanadium oxychloride, and absorbing and purifying tail gas by adopting a 30% sodium hydroxide aqueous solution; stopping introducing chlorine and oxygen after reacting for 90min, adjusting the flow of introduced nitrogen to be 0.02m/s, cooling the reactor to room temperature, stopping introducing nitrogen, taking out unreacted ferrovanadium fine powder, and calculating to obtain the chlorination rates of vanadium and iron to be 96.02% and 19.86% respectively; distilling the crude product of the vanadium oxychloride at 127 ℃ for 12min until the obtained product is 92% of the mass of the crude product of the vanadium oxychloride and the purity of the obtained vanadium oxychloride product is 99.95%.
Claims (9)
1. The method for preparing high-purity vanadium oxychloride from the ferrovanadium fine powder is characterized by comprising the following steps: the method comprises the following steps:
a. putting the ferrovanadium fine powder into a chlorination reactor, introducing nitrogen, heating to 300-600 ℃, introducing chlorine and oxygen, adjusting the total flow rate of the nitrogen, the chlorine and the oxygen, and carrying out chlorination reaction, wherein in the reaction process, volatile components in the reactor are condensed to obtain a crude product of vanadium oxytrichloride;
b. after the chlorination reaction is finished, stopping introducing chlorine and oxygen, adjusting the nitrogen flow rate again, and stopping introducing nitrogen after the reactor is cooled to room temperature;
c. and distilling the crude product of the vanadium oxychloride, and condensing to obtain the high-purity vanadium oxychloride.
2. The method for preparing high-purity vanadium oxychloride from the ferrovanadium fine powder as claimed in claim 1, wherein the method comprises the following steps: in the step a, the particle size of the ferrovanadium fine powder is 5-200 μm, and the vanadium content in the ferrovanadium fine powder is 40-85%.
3. The method for preparing high-purity vanadium oxychloride from the ferrovanadium fine powder as claimed in claim 1 or 2, wherein: in the step a, the flow velocity of the introduced nitrogen is 0.01-0.03 m/s.
4. The method for preparing high-purity vanadium oxychloride from the ferrovanadium fine powder according to any one of claims 1 to 3, wherein the method comprises the following steps: in the step a, the chlorination reaction time is 60-120 min.
5. The method for preparing high-purity vanadium oxychloride from the ferrovanadium fine powder according to any one of claims 1 to 4, wherein the method comprises the following steps: in the step a, the total flow rate of the nitrogen, the chlorine and the oxygen is adjusted to be 0.02 m/s-0.08 m/s.
6. The method for preparing high-purity vanadium oxychloride from the ferrovanadium fine powder according to any one of claims 1 to 5, wherein the method comprises the following steps: in the step a, the mole ratio of the introduced chlorine to the oxygen is 2-3: 1; the chlorine gas accounts for 20-50% of the volume fraction of the mixed gas of the nitrogen gas, the chlorine gas and the oxygen gas.
7. The method for preparing high-purity vanadium oxychloride from the ferrovanadium fine powder according to any one of claims 1 to 6, wherein the method comprises the following steps: in the step b, the flow velocity of the nitrogen is adjusted to 0.01 m/s-0.03 m/s again.
8. The method for preparing high-purity vanadium oxychloride from the ferrovanadium fine powder according to any one of claims 1 to 7, wherein the method comprises the following steps: in the step c, the distillation is carried out until the obtained product is 90-95% of the mass of the crude product of the vanadium oxychloride.
9. The method for preparing high-purity vanadium oxychloride from the ferrovanadium fine powder according to any one of claims 1 to 8, wherein the method comprises the following steps: in the step c, the distillation temperature is 125-130 ℃.
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| CN112142106A (en) * | 2020-09-29 | 2020-12-29 | 攀钢集团研究院有限公司 | Method for separating titanium tetrachloride from vanadium oxytrichloride crude product |
| CN114380332A (en) * | 2021-12-28 | 2022-04-22 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for purifying crude vanadium oxychloride |
| CN114380331A (en) * | 2021-12-20 | 2022-04-22 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for purifying crude vanadium oxychloride |
| CN115947370A (en) * | 2022-12-13 | 2023-04-11 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing refined vanadium oxytrichloride from vanadium-containing refined tailings |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112142106A (en) * | 2020-09-29 | 2020-12-29 | 攀钢集团研究院有限公司 | Method for separating titanium tetrachloride from vanadium oxytrichloride crude product |
| CN112142106B (en) * | 2020-09-29 | 2022-05-24 | 攀钢集团研究院有限公司 | Method for separating titanium tetrachloride from vanadium oxytrichloride crude product |
| CN114380331A (en) * | 2021-12-20 | 2022-04-22 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for purifying crude vanadium oxychloride |
| CN114380331B (en) * | 2021-12-20 | 2024-01-26 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for purifying crude vanadium oxychloride |
| CN114380332A (en) * | 2021-12-28 | 2022-04-22 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for purifying crude vanadium oxychloride |
| CN114380332B (en) * | 2021-12-28 | 2024-01-26 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for purifying crude vanadium oxychloride |
| CN115947370A (en) * | 2022-12-13 | 2023-04-11 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing refined vanadium oxytrichloride from vanadium-containing refined tailings |
| WO2024124791A1 (en) * | 2022-12-13 | 2024-06-20 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing refined vanadium oxytrichloride from vanadium-containing refined tailings |
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