CN116986631A - Method for removing sodium and potassium ions in ammonium metavanadate - Google Patents
Method for removing sodium and potassium ions in ammonium metavanadate Download PDFInfo
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- 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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- Prior art keywords
- ammonium metavanadate
- carbonate
- ammonium
- sodium
- potassium
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- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 title claims abstract description 111
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 title claims abstract description 45
- 239000011734 sodium Substances 0.000 title claims abstract description 45
- 229910001414 potassium ion Inorganic materials 0.000 title claims abstract description 36
- 229910001415 sodium ion Inorganic materials 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 22
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 108
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 47
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000001099 ammonium carbonate Substances 0.000 claims abstract description 40
- 235000012501 ammonium carbonate Nutrition 0.000 claims abstract description 40
- 239000000706 filtrate Substances 0.000 claims abstract description 24
- 239000000126 substance Substances 0.000 claims abstract description 19
- 239000007787 solid Substances 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 11
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000001704 evaporation Methods 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 239000002244 precipitate Substances 0.000 claims abstract description 6
- 238000000926 separation method Methods 0.000 claims abstract description 6
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 5
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 abstract description 10
- 229910052700 potassium Inorganic materials 0.000 abstract description 10
- 239000011591 potassium Substances 0.000 abstract description 10
- 229910052708 sodium Inorganic materials 0.000 abstract description 10
- 239000000047 product Substances 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 58
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 58
- 229910000027 potassium carbonate Inorganic materials 0.000 description 29
- 229910000029 sodium carbonate Inorganic materials 0.000 description 29
- 239000012535 impurity Substances 0.000 description 8
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- 229910052720 vanadium Inorganic materials 0.000 description 3
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 229910000640 Fe alloy Inorganic materials 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- PNXOJQQRXBVKEX-UHFFFAOYSA-N iron vanadium Chemical compound [V].[Fe] PNXOJQQRXBVKEX-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 description 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- 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
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 ℃.
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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 |
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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)
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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