CN115818714A - Method for preparing potassium heptafluoroniobate - Google Patents
Method for preparing potassium heptafluoroniobate Download PDFInfo
- Publication number
- CN115818714A CN115818714A CN202211383994.0A CN202211383994A CN115818714A CN 115818714 A CN115818714 A CN 115818714A CN 202211383994 A CN202211383994 A CN 202211383994A CN 115818714 A CN115818714 A CN 115818714A
- Authority
- CN
- China
- Prior art keywords
- potassium
- heptafluoroniobate
- hydrofluoric acid
- niobium pentoxide
- purity
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- FTPUNAWAGWERLA-UHFFFAOYSA-G dipotassium;heptafluoroniobium(2-) Chemical compound [F-].[F-].[F-].[F-].[F-].[F-].[F-].[K+].[K+].[Nb+5] FTPUNAWAGWERLA-UHFFFAOYSA-G 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 29
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 62
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 23
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims abstract description 23
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 150000001450 anions Chemical class 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims abstract description 4
- 239000001257 hydrogen Substances 0.000 claims abstract description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 4
- -1 hydrogen ions Chemical class 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims description 18
- 239000010955 niobium Substances 0.000 claims description 18
- 238000002425 crystallisation Methods 0.000 claims description 12
- 230000008025 crystallization Effects 0.000 claims description 12
- 229910052758 niobium Inorganic materials 0.000 claims description 8
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 5
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 5
- 229910052700 potassium Inorganic materials 0.000 claims description 5
- 239000011591 potassium Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G33/00—Compounds of niobium
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a method for preparing potassium heptafluoroniobate, which comprises the following steps: the method comprises the following steps: providing a hydrofluoric acid solution and niobium pentoxide, and mixing and heating the hydrofluoric acid solution and the niobium pentoxide, wherein the weight ratio of the hydrofluoric acid to the niobium pentoxide in the hydrofluoric acid solution is 1.0526-3.159; step two: adding a potassium salt to the product of step one, the anion of the potassium salt being an anion capable of reacting with hydrogen ions to form water and a gas that is volatile at the heated reaction temperature; step three: and crystallizing and drying the product obtained in the second step to obtain the potassium heptafluoroniobate. The method can obtain high-purity potassium heptafluoroniobate.
Description
Technical Field
The invention relates to the technical field of potassium heptafluoroniobate chemical reagents, and in particular relates to a method for preparing potassium heptafluoroniobate.
Background
Potassium heptafluoroniobate is used as a chemical reagent in various reaction processes, and the existing preparation methods for potassium heptafluoroniobate are more, but the purity of the potassium heptafluoroniobate obtained by the preparation methods is lower, so that the application of the potassium heptafluoroniobate is limited.
Therefore, how to provide a preparation method capable of obtaining high-purity potassium heptafluoroniobate becomes a technical problem which needs to be solved urgently by the technical personnel in the field.
Disclosure of Invention
In order to realize the purpose, the invention provides a preparation method capable of obtaining high-purity potassium heptafluoroniobate, which has the following specific technical scheme:
a method for preparing potassium heptafluoroniobate, comprising the steps of:
the method comprises the following steps: providing a hydrofluoric acid solution and niobium pentoxide, and mixing and heating the hydrofluoric acid solution and the niobium pentoxide, wherein the weight ratio of the hydrofluoric acid to the niobium pentoxide in the hydrofluoric acid solution is 1.0526-3.159;
step two: adding a potassium salt to the product of step one, the anion of the potassium salt being an anion capable of reacting with hydrogen ions to form water and a volatile gas at the heated reaction temperature;
step three: and crystallizing and drying the product obtained in the second step to obtain the potassium heptafluoroniobate.
Preferably, in the second step, the potassium salt is KF, KCl, KOH or KCO 3 、KHCO 3 At least one of (1).
Preferably, the potassium salt is added in a molar ratio of niobium to potassium of 1:2.
Preferably, in the first step, the temperature for mixing and heating is 60-100 ℃.
Preferably, in the step one, the concentration of the hydrofluoric acid solution is not less than 20%.
Preferably, the crystallization process is natural cooling from the reaction temperature to room temperature.
Preferably, the crystallization process adopts water cooling, and the cooling rate is 5-10 ℃/hour.
Preferably, the purity of the niobium pentoxide is not less than 95%.
Preferably, the purity of the niobium pentoxide is 99.5%.
Preferably, the potassium salt is a solid potassium salt.
The method for preparing the potassium heptafluoroniobate provided by the invention has the following technical effects:
the weight ratio of the hydrofluoric acid to the niobium pentoxide in the hydrofluoric acid solution is limited to 1.0526-3.159, and the reaction in the range can prepare high-purity potassium heptafluoroniobate, for example, the potassium heptafluoroniobate with the purity of more than 99.9 percent can be prepared.
Preferably, the potassium salt is added in a molar ratio of niobium to potassium of 1:2 to limit the formation of unwanted impurities, such as KNbF 6 And the like.
Preferably, the purity of the niobium pentoxide is limited, so that the influence of the crystallization of part of impurities together with the potassium heptafluoroniobate on the purity of the potassium heptafluoroniobate can be avoided.
Detailed Description
The invention provides a method for preparing potassium heptafluoroniobate, which comprises the following steps:
the method comprises the following steps: providing a hydrofluoric acid solution and niobium pentoxide, and mixing and heating the hydrofluoric acid solution and the niobium pentoxide, wherein the weight ratio of the hydrofluoric acid to the niobium pentoxide in the hydrofluoric acid solution is 1.0526-3.159;
step two: adding a potassium salt to the product of step one, the anion of the potassium salt being an anion capable of reacting with hydrogen ions to form water and a gas that is volatile at the heated reaction temperature;
step three: and crystallizing and drying the product obtained in the second step to obtain the potassium heptafluoroniobate.
The weight ratio of the hydrofluoric acid to the niobium pentoxide in the hydrofluoric acid solution is limited to 1.0526-3.159, and the reaction in the range can prepare high-purity potassium heptafluoroniobate, for example, the potassium heptafluoroniobate with the purity of more than 99.9 percent can be prepared.
Wherein in the second step, the potassium salt is KF, KCl, KOH or KCO 3 、KHCO 3 At least one of (1).
The types of the selectable raw materials are more, and the raw materials are convenient to obtain.
In one embodiment, the potassium salt is added in a molar ratio of niobium to potassium of 1:2.
The potassium salt is added in a molar ratio of niobium to potassium of 1:2 to limit the formation of unwanted impurities, such as KNbF 6 And the like.
Wherein, in the first step, the temperature of mixing and heating is 60-100 ℃.
And in the first step, the concentration of the hydrofluoric acid solution is not less than 20%.
For the crystallization process, the crystallization process is to naturally cool from the reaction temperature to room temperature. Or the crystallization process adopts water cooling, and the cooling rate is 5-10 ℃/hour.
Further, the purity of the niobium pentoxide is not less than 95%.
Further, the purity of the niobium pentoxide was 99.5%.
In one embodiment, the potassium salt is a solid potassium salt.
The first embodiment is as follows:
HF in hydrofluoric acid with concentration of 40% and Nb with purity of 95% 2 O 5 When the mass ratio of (A) is 1.6527, the reaction temperature is 90 ℃, the mole ratio of Nb to K is 1:2, the mixture is naturally cooled to the room temperature from the reaction temperature, the drying temperature is 105 ℃, the mixture is dried for 4 hours, and the purity of the obtained potassium heptafluoroniobate is detected to be 99.2%.
Example two:
HF in hydrofluoric acid with concentration of 20% and Nb with purity of about 95% 2 O 5 The mass ratio of the Nb to the K is 1.0526, the reaction temperature is 60 ℃, insoluble substances are filtered, the molar ratio of Nb to K is 1:2, washing is carried out, water cooling crystallization is adopted, the cooling rate is 10 ℃/h, the drying temperature is 105 ℃, drying is carried out for 4 hours, and the purity of the potassium heptafluoroniobate reaches 99.18%.
Example three:
HF in 30% hydrofluoric acid with a purity of 99.5% Nb 2 O 5 When the mass ratio of the Nb to the K is 3.159, the reaction temperature is 100 ℃, insoluble substances are filtered, the molar ratio of Nb to K is 1:2, washing is carried out, water cooling crystallization is adopted, the cooling rate is 5 ℃/h, the drying temperature is 105 ℃, drying is carried out for 4 hours, and the purity of the potassium heptafluoroniobate reaches 99.9%.
Example four:
HF in 25% hydrofluoric acid with purity 98% Nb 2 O 5 When the mass ratio of the Nb to the K is 3.0, the reaction temperature is 85 ℃, insoluble substances are filtered, the molar ratio of the Nb to the K is 1:2, washing is carried out, water cooling crystallization is adopted, the cooling rate is 8 ℃/h, the drying temperature is 105 ℃, drying is carried out for 4 hours, and the purity of the potassium heptafluoroniobate reaches 99.8%.
Comparative example 1:
HF in hydrofluoric acid with concentration of 20% and Nb with purity of about 95% 2 O 5 At a reaction temperature of 60 ℃ when the mass ratio of (A) is 1.04, filtering insoluble substances, washing, crystallizing by water cooling at a cooling rate of 10 ℃/h, drying, wherein the molar ratio of Nb to K is 1:2The potassium heptafluoroniobate is dried for 4 hours at the temperature of 105 ℃, and the purity of the potassium heptafluoroniobate is 88 percent.
In this comparative example 1, the mass ratio of hydrofluoric acid and the niobium pentoxide in the hydrofluoric acid solution varied as compared with that in example 2, but the purity of the resulting potassium heptafluoroniobate was low.
Comparative example 2:
30% HF in hydrofluoric acid with a purity of 94% Nb 2 O 5 When the mass ratio of the Nb to the K is 3.159, the reaction temperature is 100 ℃, insoluble substances are filtered, the molar ratio of Nb to K is 1:2, washing is carried out, water cooling crystallization is adopted, the cooling rate is 5 ℃/h, the drying temperature is 105 ℃, the drying is carried out for 4 hours, and the purity of the potassium heptafluoroniobate reaches 85.4%.
The purity of niobium pentoxide varied from the comparative examples to the examples, which clearly gave potassium heptafluoroniobate of lower purity.
Claims (10)
1. A method for preparing potassium heptafluoroniobate is characterized by comprising the following steps:
the method comprises the following steps: providing a hydrofluoric acid solution and niobium pentoxide, and mixing and heating the hydrofluoric acid solution and the niobium pentoxide, wherein the weight ratio of the hydrofluoric acid to the niobium pentoxide in the hydrofluoric acid solution is 1.0526-3.159;
step two: adding a potassium salt to the product of step one, the anion of the potassium salt being an anion capable of reacting with hydrogen ions to form water and a volatile gas at the heated reaction temperature;
step three: and crystallizing and drying the product obtained in the second step to obtain the potassium heptafluoroniobate.
2. The method for preparing potassium heptafluoroniobate according to claim 1, wherein in the second step, the potassium salt is KF, KCl, KOH, KCO 3 、KHCO 3 At least one of (1).
3. The method of claim 1, wherein the potassium salt is added in a molar ratio of niobium to potassium of 1:2.
4. The method for preparing potassium heptafluoroniobate according to claim 1, wherein the temperature of the mixing heating in the first step is 60 to 100 ℃.
5. The method for preparing potassium heptafluoroniobate according to claim 1, wherein the concentration of the hydrofluoric acid solution in the first step is not less than 20%.
6. The method for preparing potassium heptafluoroniobate according to claim 1, wherein the crystallization process is a natural cooling from a reaction temperature to a room temperature.
7. The method for preparing potassium heptafluoroniobate according to claim 1, wherein the crystallization process is water cooling at a cooling rate of 5-10 ℃/hr.
8. The method for preparing potassium heptafluoroniobate according to claim 1, wherein the purity of niobium pentoxide is not less than 95%.
9. The method of claim 8, wherein the niobium pentoxide has a purity of 99.5%.
10. The method of claim 1, wherein the potassium salt is a solid potassium salt.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211383994.0A CN115818714A (en) | 2022-11-07 | 2022-11-07 | Method for preparing potassium heptafluoroniobate |
| PCT/CN2023/125664 WO2024099051A1 (en) | 2022-11-07 | 2023-10-20 | Method for preparing potassium heptafluoroniobate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211383994.0A CN115818714A (en) | 2022-11-07 | 2022-11-07 | Method for preparing potassium heptafluoroniobate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115818714A true CN115818714A (en) | 2023-03-21 |
Family
ID=85526853
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211383994.0A Pending CN115818714A (en) | 2022-11-07 | 2022-11-07 | Method for preparing potassium heptafluoroniobate |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN115818714A (en) |
| WO (1) | WO2024099051A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2024099051A1 (en) * | 2022-11-07 | 2024-05-16 | 中信金属股份有限公司 | Method for preparing potassium heptafluoroniobate |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3641190B2 (en) * | 2000-05-18 | 2005-04-20 | 三井金属鉱業株式会社 | Method for processing tantalum / niobium-containing raw materials |
| AU2002214329A1 (en) * | 2000-11-29 | 2002-06-11 | Mitsui Mining And Smelting Co. Lt.D | Process for producing potassium fluoroniobate crystal and potassium fluoroniobate crystal |
| CN105129851B (en) * | 2015-08-20 | 2018-01-30 | 宁夏东方钽业股份有限公司 | A kind of preparation method of high purity niobium oxide |
| CN107469806A (en) * | 2016-06-08 | 2017-12-15 | 中国石油化工股份有限公司 | Water-soluble niobium composition and its production and use |
| CN108910949B (en) * | 2018-07-18 | 2021-01-15 | 宁夏东方钽业股份有限公司 | Preparation method of high-purity potassium fluotantalate |
| CN113277560A (en) * | 2021-06-17 | 2021-08-20 | 宁夏东方钽业股份有限公司 | Preparation method of potassium fluoroniobate crystal |
| CN115818714A (en) * | 2022-11-07 | 2023-03-21 | 中信金属股份有限公司 | Method for preparing potassium heptafluoroniobate |
-
2022
- 2022-11-07 CN CN202211383994.0A patent/CN115818714A/en active Pending
-
2023
- 2023-10-20 WO PCT/CN2023/125664 patent/WO2024099051A1/en unknown
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2024099051A1 (en) * | 2022-11-07 | 2024-05-16 | 中信金属股份有限公司 | Method for preparing potassium heptafluoroniobate |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2024099051A1 (en) | 2024-05-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP1807354B1 (en) | Process for producing manganese fluoride | |
| JP2987713B2 (en) | Method for producing high-purity hexafluorophosphoric acid compound | |
| EP0161704B1 (en) | Process for the production of water soluble ammonium phosphates | |
| AU2014293663A1 (en) | Synthesis of hydrogen bis(fluorosulfonyl)imide | |
| US2488298A (en) | Method of producing hexafluorophosphoric acid | |
| CN115818714A (en) | Method for preparing potassium heptafluoroniobate | |
| CN101391760A (en) | Method for preparing high purity phosphorus pentafluoride gas | |
| US3421846A (en) | Production of sodium phosphates | |
| CN111592011A (en) | Method for directly synthesizing SSZ-13 zeolite molecular sieve by using TEAOH as organic template agent | |
| TW200906714A (en) | Method for producing hexafluorophosphate salt | |
| CN112592261A (en) | Preparation method of trimethylolpropane diallyl ether | |
| CN113582874B (en) | Synthesis method of bromoacetonitrile | |
| CN113929711A (en) | Preparation method of lithium difluoroborate | |
| US4041143A (en) | Process for preparing fibrous alkali metal titanate | |
| CN110862101A (en) | Preparation method of potassium nitrate | |
| RU2424187C1 (en) | Method of producing high-purity barium fluoride | |
| CN110759362B (en) | Composition containing lithium hexafluorophosphate crystal and water | |
| CN112408479A (en) | Process for preparing low-valence vanadium from ammonium metavanadate | |
| EP4108327A1 (en) | Method for producing catalyst for dehydrogenation of 3-hydroxypropionic acid, catalyst for dehydrogenation of 3-hydroxypropionic acid, and method for producing acrylic acid using same | |
| CN113321239A (en) | Cl-free2Method for preparing multiple perovskite material by method and application thereof | |
| CN112939005A (en) | Synthesis method of-CLO structure ultra-large pore aluminum phosphate and heteroatom aluminum phosphate molecular sieve | |
| US3179494A (en) | Novel process for preparing antimony oxychloride | |
| CN114873614B (en) | Method for preparing potassium nitrate byproduct potassium carnallite and magnesium chloride | |
| JPS63227593A (en) | Production of metal alkoxide solution | |
| CN103253643B (en) | Method for preparing lithium hexafluorophosphate by phase-transfer catalytic process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |