CN116986631A - Method for removing sodium and potassium ions in ammonium metavanadate - Google Patents

Method for removing sodium and potassium ions in ammonium metavanadate Download PDF

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Publication number
CN116986631A
CN116986631A CN202311023439.1A CN202311023439A CN116986631A CN 116986631 A CN116986631 A CN 116986631A CN 202311023439 A CN202311023439 A CN 202311023439A CN 116986631 A CN116986631 A CN 116986631A
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ammonium metavanadate
carbonate
ammonium
sodium
potassium
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张春雨
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Hunan Zhongxin New Materials Technology Co ltd
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Hunan Zhongxin New Materials Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G31/00Compounds of vanadium
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

A method for removing sodium and potassium ions in ammonium metavanadate, comprising the following steps: (1) Dissolving ammonium metavanadate in methanol, adding ammonium carbonate, stirring for reaction, filtering, and collecting filtrate; (2) Recrystallizing the filtrate obtained in the step (1) to obtain ammonium metavanadate precipitate, and carrying out solid-liquid separation to obtain a solid substance; or evaporating the filtrate obtained in the step (1) and separating methanol from the filtrate to obtain solid matters; (3) And (3) washing the solid substance obtained in the step (2) with cold water, and drying to obtain ammonium metavanadate. The method has simple operation, the used impurity-removing raw materials are cheap and easy to obtain, and the methanol can be recycled. The obtained ammonium metavanadate has low sodium and potassium ion content, the sodium content in the ammonium metavanadate product is less than 20ppm, the potassium content is less than 20ppm, and the purity of the ammonium metavanadate is more than or equal to 99.90%.

Description

Method for removing sodium and potassium ions in ammonium metavanadate
Technical Field
The invention belongs to the technical field of chemical industry, and particularly relates to a method for removing sodium and potassium ions in ammonium metavanadate.
Background
Ammonium metavanadate with molecular formula NH 4 VO 3 White or pale yellow crystalline powder, relative density 2.326, molecular weight 116.98, slightly soluble in cold water, hot ethanol and diethyl ether, in hot water, methanol and dilute ammonium hydroxide. The vanadium pentoxide is changed into when the vanadium pentoxide is burnt in the air.
Ammonium metavanadate is an intermediate product for extracting vanadium, and is mainly used for preparing vanadium pentoxide (powder or sheet), and further producing metal vanadium, vanadium iron alloy or other vanadium-based alloy. Can also be used as chemical reagent, catalyst, drier, mordant, etc. The ceramic industry is widely used as a glaze. With the wide application of ammonium metavanadate in various industries, the requirement on the purity of ammonium metavanadate is higher and higher.
In the purification process of ammonium metavanadate, a certain amount of sodium salt or/and potassium salt is required to be added, and part of sodium potassium ions are inevitably carried in the recrystallization process, so that the quality of ammonium metavanadate products is affected. Thus, a method for removing sodium and potassium ions from ammonium metavanadate is urgently needed.
Disclosure of Invention
The invention aims to solve the technical problems of overcoming the defects of the prior art and providing a method for removing sodium and potassium ions in ammonium metavanadate.
The technical scheme adopted for solving the technical problems is that the method for removing sodium and potassium ions in ammonium metavanadate comprises the following steps:
(1) Dissolving ammonium metavanadate in methanol, adding ammonium carbonate, stirring for reaction, filtering (removing insoluble impurities such as sodium carbonate and potassium carbonate), and collecting filtrate;
further, in the step (1), depending on the solubility of ammonium metavanadate, it is preferable that ammonium metavanadate is not precipitated, and if the ambient temperature is a little higher, the ammonium metavanadate can be completely dissolved even if the amount of methanol is small; if the ambient temperature is low, the amount of methanol is increased to dissolve the ammonium metavanadate or a heating mode is adopted.
If water is used to replace methanol, sodium and potassium ions cannot be separated and removed, because sodium carbonate, potassium carbonate and ammonium carbonate are all dissolved in water, the purpose of separating from ammonium metavanadate cannot be achieved.
Further, in the step (1), the amount of ammonium carbonate to be used depends on the content of sodium and potassium ions in ammonium metavanadate, and it is preferable that the total sodium and potassium ions are removed with a slight excess. I.e. the sum of the amounts of sodium and potassium ion species contained in the ammonium metavanadate: amount of carbonate ion-containing substance contained in ammonium carbonate = 1:1.05 to 1.2.
In step (1), the reaction is preferably carried out at room temperature for 5 minutes or more (preferably 10 to 30 minutes) with stirring.
Ammonium metavanadate and ammonium carbonate are easy to dissolve in methanol, sodium and potassium in ammonium metavanadate react with ammonium carbonate to generate sodium carbonate and potassium carbonate, and sodium carbonate and potassium carbonate are insoluble in methanol and can generate precipitation and can be separated by filtration. The ammonium metavanadate is separated from the solution, wherein a very small amount of ammonium carbonate, sodium carbonate and potassium carbonate are entrained, the ammonium metavanadate is slightly dissolved in cold water, the ammonium carbonate, the sodium carbonate and the potassium carbonate are dissolved in the cold water and can be removed by washing with the cold water. The obtained ammonium metavanadate has high purity.
(2) Recrystallizing the filtrate obtained in the step (1) to obtain ammonium metavanadate precipitate, and carrying out solid-liquid separation to obtain a solid substance; or evaporating the filtrate obtained in the step (1) and separating methanol from the filtrate to obtain solid matters;
(3) Washing the solid substance obtained in the step (2) with cold water (removing impurities dissolved in water such as residual sodium carbonate, potassium carbonate and ammonium carbonate), and drying to obtain ammonium metavanadate.
Further, in step (3), the cold water is water having a temperature of less than 20 ℃ (preferably water having a temperature of less than 10 ℃). Ammonium metavanadate has a small solubility in cold water, but sodium carbonate, potassium carbonate, ammonium carbonate and the like are easily dissolved in cold water, so that the ammonium metavanadate is separated.
The method has simple operation, the used impurity-removing raw materials are cheap and easy to obtain, and the methanol can be recycled. The obtained ammonium metavanadate has low sodium and potassium ion content, the sodium content in the ammonium metavanadate product is less than 20ppm, the potassium content is less than 20ppm, and the purity of the ammonium metavanadate is more than or equal to 99.90%.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
In each of examples and comparative examples, the content of sodium in the ammonium metavanadate as a raw material was 0.12%, the content of potassium was 0.13%, and the purity of ammonium metavanadate was 99.0%.
Example 1
The method for removing sodium and potassium ions in ammonium metavanadate in the embodiment comprises the following steps:
(1) Dissolving ammonium metavanadate in methanol, adding ammonium carbonate, stirring for reaction, filtering (removing insoluble impurities such as sodium carbonate and potassium carbonate), and collecting filtrate;
in the step (1), the amount of the methanol depends on the solubility of the ammonium metavanadate, preferably, the ammonium metavanadate is not precipitated, and if the ambient temperature is higher, the ammonium metavanadate can be completely dissolved even if the amount of the methanol is smaller; if the ambient temperature is low, the amount of methanol is increased to dissolve the ammonium metavanadate or a heating mode is adopted.
In the step (1), the amount of ammonium carbonate to be used depends on the content of sodium and potassium ions in ammonium metavanadate, and it is preferable that the total sodium and potassium ions are removed with a slight excess. I.e. the sum of the amounts of sodium and potassium ion species contained in the ammonium metavanadate: amount of carbonate ion-containing substance contained in ammonium carbonate = 1:1.05.
in the step (1), the reaction was stirred at room temperature for 15 minutes.
Ammonium metavanadate and ammonium carbonate are easy to dissolve in methanol, sodium and potassium in ammonium metavanadate react with ammonium carbonate to generate sodium carbonate and potassium carbonate, and sodium carbonate and potassium carbonate are insoluble in methanol and can generate precipitation and can be separated by filtration. The ammonium metavanadate is separated from the solution, wherein a very small amount of ammonium carbonate, sodium carbonate and potassium carbonate are entrained, the ammonium metavanadate is slightly dissolved in cold water, the ammonium carbonate, the sodium carbonate and the potassium carbonate are dissolved in the cold water and can be removed by washing with the cold water. The obtained ammonium metavanadate has high purity.
(2) Recrystallizing the filtrate obtained in the step (1) to obtain ammonium metavanadate precipitate, and carrying out solid-liquid separation to obtain a solid substance; or evaporating the filtrate obtained in the step (1) and separating methanol from the filtrate to obtain solid matters;
(3) Washing the solid substance obtained in the step (2) with cold water (removing impurities dissolved in water such as residual sodium carbonate, potassium carbonate and ammonium carbonate), and drying to obtain ammonium metavanadate.
In the step (3), the cold water is water with the temperature lower than 10 ℃. Ammonium metavanadate has a small solubility in cold water, but sodium carbonate, potassium carbonate, ammonium carbonate and the like are easily dissolved in cold water, so that the ammonium metavanadate is separated.
The method has simple operation, the used impurity-removing raw materials are cheap and easy to obtain, and the methanol can be recycled. The obtained ammonium metavanadate has low sodium and potassium ion content, the sodium content in the ammonium metavanadate product is 12ppm, the potassium content is 15ppm, and the purity of the ammonium metavanadate is 99.96%.
Example 2
The method for removing sodium and potassium ions in ammonium metavanadate in the embodiment comprises the following steps:
(1) Dissolving ammonium metavanadate in methanol, adding ammonium carbonate, stirring for reaction, filtering (removing insoluble impurities such as sodium carbonate and potassium carbonate), and collecting filtrate;
further, in the step (1), depending on the solubility of ammonium metavanadate, it is preferable that ammonium metavanadate is not precipitated, and if the ambient temperature is a little higher, the ammonium metavanadate can be completely dissolved even if the amount of methanol is small; if the ambient temperature is low, the amount of methanol is increased to dissolve the ammonium metavanadate or a heating mode is adopted.
Further, in the step (1), the amount of ammonium carbonate to be used depends on the content of sodium and potassium ions in ammonium metavanadate, and it is preferable that the total sodium and potassium ions are removed with a slight excess. I.e. the sum of the amounts of sodium and potassium ion species contained in the ammonium metavanadate: amount of carbonate ion-containing substance contained in ammonium carbonate = 1:1.1.
further, in the step (1), the reaction is preferably carried out under stirring at normal temperature for 5 minutes.
Ammonium metavanadate and ammonium carbonate are easy to dissolve in methanol, sodium and potassium in ammonium metavanadate react with ammonium carbonate to generate sodium carbonate and potassium carbonate, and sodium carbonate and potassium carbonate are insoluble in methanol and can generate precipitation and can be separated by filtration. The ammonium metavanadate is separated from the solution, wherein a very small amount of ammonium carbonate, sodium carbonate and potassium carbonate are entrained, the ammonium metavanadate is slightly dissolved in cold water, the ammonium carbonate, the sodium carbonate and the potassium carbonate are dissolved in the cold water and can be removed by washing with the cold water. The obtained ammonium metavanadate has high purity.
(2) Recrystallizing the filtrate obtained in the step (1) to obtain ammonium metavanadate precipitate, and carrying out solid-liquid separation to obtain a solid substance; or evaporating the filtrate obtained in the step (1) and separating methanol from the filtrate to obtain solid matters;
(3) Washing the solid substance obtained in the step (2) with cold water (removing impurities dissolved in water such as residual sodium carbonate, potassium carbonate and ammonium carbonate), and drying to obtain ammonium metavanadate.
Further, in the step (3), the cold water is water having a temperature lower than 10 ℃. Ammonium metavanadate has a small solubility in cold water, but sodium carbonate, potassium carbonate, ammonium carbonate and the like are easily dissolved in cold water, so that the ammonium metavanadate is separated.
The method has simple operation, the used impurity-removing raw materials are cheap and easy to obtain, and the methanol can be recycled. The obtained ammonium metavanadate has low sodium and potassium ion content, the sodium content in the ammonium metavanadate product is 13ppm, the potassium content is 12ppm, and the purity of the ammonium metavanadate is 99.92%.
Example 3
The method for removing sodium and potassium ions in ammonium metavanadate in the embodiment comprises the following steps:
(1) Dissolving ammonium metavanadate in methanol, adding ammonium carbonate, stirring for reaction, filtering (removing insoluble impurities such as sodium carbonate and potassium carbonate), and collecting filtrate;
further, in the step (1), depending on the solubility of ammonium metavanadate, it is preferable that ammonium metavanadate is not precipitated, and if the ambient temperature is a little higher, the ammonium metavanadate can be completely dissolved even if the amount of methanol is small; if the ambient temperature is low, the amount of methanol is increased to dissolve the ammonium metavanadate or a heating mode is adopted.
Further, in the step (1), the amount of ammonium carbonate to be used depends on the content of sodium and potassium ions in ammonium metavanadate, and it is preferable that the total sodium and potassium ions are removed with a slight excess. I.e. the sum of the amounts of sodium and potassium ion species contained in the ammonium metavanadate: amount of carbonate ion-containing substance contained in ammonium carbonate = 1:1.2.
further, in the step (1), the reaction is preferably carried out under stirring at normal temperature for 30 minutes.
Ammonium metavanadate and ammonium carbonate are easy to dissolve in methanol, sodium and potassium in ammonium metavanadate react with ammonium carbonate to generate sodium carbonate and potassium carbonate, and sodium carbonate and potassium carbonate are insoluble in methanol and can generate precipitation and can be separated by filtration. The ammonium metavanadate is separated from the solution, wherein a very small amount of ammonium carbonate, sodium carbonate and potassium carbonate are entrained, the ammonium metavanadate is slightly dissolved in cold water, the ammonium carbonate, the sodium carbonate and the potassium carbonate are dissolved in the cold water and can be removed by washing with the cold water. The obtained ammonium metavanadate has high purity.
(2) Recrystallizing the filtrate obtained in the step (1) to obtain ammonium metavanadate precipitate, and carrying out solid-liquid separation to obtain a solid substance; or evaporating the filtrate obtained in the step (1) and separating methanol from the filtrate to obtain solid matters;
(3) Washing the solid substance obtained in the step (2) with cold water (removing impurities dissolved in water such as residual sodium carbonate, potassium carbonate and ammonium carbonate), and drying to obtain ammonium metavanadate.
Further, in the step (3), the cold water is water having a temperature lower than 20 ℃. Ammonium metavanadate has a small solubility in cold water, but sodium carbonate, potassium carbonate, ammonium carbonate and the like are easily dissolved in cold water, so that the ammonium metavanadate is separated.
The method has simple operation, the used impurity-removing raw materials are cheap and easy to obtain, and the methanol can be recycled. The obtained ammonium metavanadate has low sodium and potassium ion content, the sodium content in the ammonium metavanadate product is 16ppm, the potassium content is 17ppm, and the purity of the ammonium metavanadate is 99.92%.

Claims (6)

1. A method for removing sodium and potassium ions in ammonium metavanadate, which is characterized by comprising the following steps:
(1) Dissolving ammonium metavanadate in methanol, adding ammonium carbonate, stirring for reaction, filtering, and collecting filtrate;
(2) Recrystallizing the filtrate obtained in the step (1) to obtain ammonium metavanadate precipitate, and carrying out solid-liquid separation to obtain a solid substance; or evaporating the filtrate obtained in the step (1) and separating methanol from the filtrate to obtain solid matters;
(3) And (3) washing the solid substance obtained in the step (2) with cold water, and drying to obtain ammonium metavanadate.
2. The method for removing sodium and potassium ions from ammonium metavanadate according to claim 1, wherein in the step (1), the sum of the amounts of sodium and potassium ion substances contained in ammonium metavanadate: amount of carbonate ion-containing substance contained in ammonium carbonate = 1:1.05 to 1.2.
3. The method for removing sodium and potassium ions from ammonium metavanadate according to claim 1 or 2, wherein in the step (1), the reaction is carried out at room temperature with stirring for 5 minutes or more.
4. The method for removing sodium and potassium ions from ammonium metavanadate according to claim 3, wherein in the step (1), the reaction is carried out under stirring at room temperature for 10 to 30 minutes.
5. The method for removing sodium and potassium ions from ammonium metavanadate according to claim 1 or 2, wherein in step (3), the cold water is water having a temperature of less than 20 ℃.
6. The method for removing sodium and potassium ions from ammonium metavanadate according to claim 5, wherein in step (3), the cold water is water having a temperature of less than 10 ℃.
CN202311023439.1A 2023-08-15 2023-08-15 Method for removing sodium and potassium ions in ammonium metavanadate Pending CN116986631A (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113955801A (en) * 2021-12-09 2022-01-21 淄博凡纳蒂斯技术服务有限公司 Method for preparing high-purity ammonium metavanadate by seed crystal decomposition method

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113955801A (en) * 2021-12-09 2022-01-21 淄博凡纳蒂斯技术服务有限公司 Method for preparing high-purity ammonium metavanadate by seed crystal decomposition method

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
傅献彩 主编, 南京大学出版社: "《实用化学便览》", vol. 1, 30 September 1989, pages: 612 - 613 *
张学铭 等编, 科学技术文献出版社: "《化学小辞典(第二版)》", vol. 2, 31 August 1994, pages: 391 *

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