CN113086993A - Process method for preparing potassium fluoride by decomposing fluosilicic acid through electrodialysis - Google Patents
Process method for preparing potassium fluoride by decomposing fluosilicic acid through electrodialysis Download PDFInfo
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- CN113086993A CN113086993A CN202110403039.8A CN202110403039A CN113086993A CN 113086993 A CN113086993 A CN 113086993A CN 202110403039 A CN202110403039 A CN 202110403039A CN 113086993 A CN113086993 A CN 113086993A
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- CN
- China
- Prior art keywords
- potassium fluoride
- electrodialysis
- potassium
- fluoride
- decomposing
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- 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.)
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- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 title claims abstract description 82
- 239000011698 potassium fluoride Substances 0.000 title claims abstract description 41
- 235000003270 potassium fluoride Nutrition 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000000909 electrodialysis Methods 0.000 title claims abstract description 21
- 239000002253 acid Substances 0.000 title claims abstract description 16
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 42
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 21
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 17
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 16
- 239000012452 mother liquor Substances 0.000 claims abstract description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 12
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000011591 potassium Substances 0.000 claims abstract description 12
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 12
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000001103 potassium chloride Substances 0.000 claims abstract description 8
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 8
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 8
- 238000001704 evaporation Methods 0.000 claims abstract description 7
- 238000001694 spray drying Methods 0.000 claims abstract description 7
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims abstract description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 6
- 230000007062 hydrolysis Effects 0.000 claims abstract description 3
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 239000012528 membrane Substances 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 9
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 9
- 238000001914 filtration Methods 0.000 description 8
- 239000002244 precipitate Substances 0.000 description 8
- 238000001816 cooling Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- 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 description 2
- HHHPKVLNNLPPKL-UHFFFAOYSA-N benzene;hydrofluoride Chemical compound F.C1=CC=CC=C1 HHHPKVLNNLPPKL-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000010436 fluorite Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 2
- 238000004659 sterilization and disinfection Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 1
- 235000013405 beer Nutrition 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910001634 calcium fluoride Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910001610 cryolite Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 150000004683 dihydrates Chemical class 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- PYLWMHQQBFSUBP-UHFFFAOYSA-N monofluorobenzene Chemical compound FC1=CC=CC=C1 PYLWMHQQBFSUBP-UHFFFAOYSA-N 0.000 description 1
- 239000002686 phosphate fertilizer Substances 0.000 description 1
- 239000002367 phosphate rock Substances 0.000 description 1
- -1 potassium fluorosilicates Chemical class 0.000 description 1
- DHZKUVDKQZJAMV-UHFFFAOYSA-M potassium;fluoride;hydrate Chemical compound O.[F-].[K+] DHZKUVDKQZJAMV-UHFFFAOYSA-M 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/02—Fluorides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/16—Halides of ammonium
- C01C1/164—Ammonium chloride
Abstract
The invention discloses a process method for preparing potassium fluoride by decomposing fluosilicic acid through electrodialysis, wherein fluosilicic acid and potassium chloride react to prepare potassium fluosilicate and hydrochloric acid mother liquor, and the potassium fluosilicate and the hydrochloric acid mother liquor are introduced into ammonia water or liquid ammonia for hydrolysis to obtain silicon dioxide, potassium fluoride and ammonium fluoride. And separating the potassium fluoride and the ammonium fluoride by electrodialysis to obtain the potassium fluoride and the ammonium chloride. Purifying and purifying potassium fluoride, spray drying to obtain industrial potassium fluoride, evaporating and concentrating ammonium chloride, and crystallizing to obtain industrial ammonium chloride.
Description
Technical Field
The invention relates to a process method for preparing potassium fluoride by decomposing fluosilicic acid through electrodialysis, which belongs to the field of fine chemicals, wherein benzene fluoride is recycled, the residual unreacted villiaumite of the benzene fluoride is further regenerated and reused as a raw material technology; the resources in the recovery are utilized, no pollution is caused, and no three wastes are generated; the recovered intermediate can reach the market demand standard and national standard, can be directly sold, and can also produce fluorobenzene as raw material.
Background
Potassium fluosilicate belongs to a by-product in a hydrofluoric acid process, is also called silicofluoric acid, is colorless gas when anhydrous substances are not, is unstable, is easily decomposed into silicon tetrafluoride and hydrogen fluoride, is colorless when aqueous solution is in a strong acid reaction and has corrosivity, can erode glass, and is stored in containers made of wax or plastic and the like; crystals of colorless dihydrate are separated out when the concentrated solution is cooled, and the melting point is 19 ℃; the fluosilicic acid has the disinfection performance, is used for preparing fluosilicate and cryolite, and is used for electroplating, beer disinfection, wood preservation and the like. It is made up by dissolving silicon dioxide in hydrofluoric acid or mixing it with quartz powder, calcium fluoride and concentrated sulfuric acid and heating, and can also be obtained by using water to absorb silicon tetrafluoride gas escaped from phosphate fertilizer plant when decomposing phosphate rock.
It is conventional practice to produce sodium or potassium fluorosilicates by neutralization with potassium hydroxide and sodium hydroxide. The potassium fluosilicate or sodium fluosilicate has low economic value, the traditional method for producing potassium fluoride is mostly prepared by adopting a potassium hydroxide-hydrofluoric acid neutralization method, hydrofluoric acid in the traditional process is mainly prepared by reacting fluorite and sulfuric acid, the traditional process needs to consume precious resources of fluorite, the cost of the hydrofluoric acid is quite high, and the combined preparation method is adopted, so that the content of organic carbon in the potassium fluoride is greatly reduced.
The economic benefit is improved, the potassium fluoride is recycled, the villiaumite is further regenerated and reused as a raw material technology, the resources in the process of recycling are utilized, and the process is pollution-free and has no three-waste production; the recovered intermediate can reach the market demand standard and national standard, and can be directly sold.
Disclosure of Invention
The invention aims to solve the technical problem of solving the problem of separation of potassium fluoride and potassium chloride by adopting a plurality of purification means.
In order to solve the technical problems, the invention adopts the following technical scheme:
a process method for preparing potassium fluoride by decomposing fluosilicic acid by electrodialysis comprises the following steps: it comprises the following steps: wherein, the fluosilicic acid and the potassium chloride react to prepare potassium fluosilicate and hydrochloric acid mother liquor, and the potassium fluosilicate and the hydrochloric acid mother liquor are introduced into ammonia water or liquid ammonia for hydrolysis to obtain silicon dioxide, potassium fluoride and ammonium fluoride; performing electrodialysis separation on potassium fluoride and ammonium fluoride to obtain potassium fluoride and ammonium chloride; purifying and purifying potassium fluoride, spray drying to obtain industrial potassium fluoride, evaporating and concentrating ammonium chloride, and crystallizing to obtain industrial ammonium chloride.
The method comprises the following steps: the ammonia water adopts liquid ammonia component.
The method comprises the following steps: the ph is adjusted to 11 or more.
The method comprises the following steps: ph was adjusted to 13.
The method comprises the following steps: the electrodialysis adopts bipolar membrane electrodialysis.
Detailed Description
Example 1:
slowly adding 1kg of potassium chloride into 15% potassium fluosilicate until no precipitate is generated, introducing ammonia gas into the mixed solution until the precipitate becomes transparent, controlling ph to be 11, filtering to obtain silicon dioxide and mother liquor, separating the mother liquor in electrodialysis to obtain potassium fluoride and ammonium chloride, adsorbing and purifying the potassium fluoride by activated carbon, drying by adopting a spray drying method to obtain potassium fluoride, evaporating and concentrating ammonium chloride, cooling and crystallizing, and filtering to obtain industrial ammonium chloride.
Example 2:
slowly adding 1kg of potassium chloride into 15% potassium fluosilicate until no precipitate is generated, introducing ammonia gas into the mixed solution until the precipitate becomes transparent, controlling ph to be 12, filtering to obtain silicon dioxide and mother liquor, separating the mother liquor in electrodialysis to obtain potassium fluoride and ammonium chloride, adsorbing and purifying the potassium fluoride by activated carbon, drying by adopting a spray drying method to obtain potassium fluoride, evaporating and concentrating ammonium chloride, cooling and crystallizing, and filtering to obtain industrial ammonium chloride.
Example 3:
slowly adding 1kg of potassium chloride into 15% potassium fluosilicate until no precipitate is generated, introducing ammonia gas into the mixed solution until the precipitate becomes transparent, controlling ph to be 13, filtering to obtain silicon dioxide and mother liquor, separating the mother liquor in electrodialysis to obtain potassium fluoride and ammonium chloride, adsorbing and purifying the potassium fluoride by activated carbon, drying by adopting a spray drying method to obtain potassium fluoride, evaporating and concentrating ammonium chloride, cooling and crystallizing, and filtering to obtain industrial ammonium chloride.
Example 4:
slowly adding 1kg of potassium chloride into 15% potassium fluosilicate until no precipitate is generated, introducing ammonia water into the mixed solution until the precipitate becomes transparent, controlling ph to be 14, filtering to obtain silicon dioxide and mother liquor, separating the mother liquor in electrodialysis to obtain potassium fluoride and ammonium chloride, adsorbing and purifying the potassium fluoride by activated carbon, drying by adopting a spray drying method to obtain potassium fluoride, evaporating and concentrating ammonium chloride, cooling and crystallizing, and filtering to obtain industrial ammonium chloride.
Claims (5)
1. A process method for preparing potassium fluoride by decomposing fluosilicic acid through electrodialysis is characterized by comprising the following steps: wherein, the fluosilicic acid and the potassium chloride react to prepare potassium fluosilicate and hydrochloric acid mother liquor, and the potassium fluosilicate and the hydrochloric acid mother liquor are introduced into ammonia water or liquid ammonia for hydrolysis to obtain silicon dioxide, potassium fluoride and ammonium fluoride; performing electrodialysis separation on potassium fluoride and ammonium fluoride to obtain potassium fluoride and ammonium chloride; purifying and purifying potassium fluoride, spray drying to obtain industrial potassium fluoride, evaporating and concentrating ammonium chloride, and crystallizing to obtain industrial ammonium chloride.
2. The process for preparing potassium fluoride by decomposing fluosilicic acid by electrodialysis as claimed in claim 1, wherein: the ammonia water adopts liquid ammonia component.
3. The process of claim 1 for preparing potassium fluoride by decomposing fluorosilicic acid by electrodialysis, which comprises the following steps: the ph is adjusted to 11 or more.
4. The process of claim 1 for preparing potassium fluoride by decomposing fluorosilicic acid by electrodialysis, which comprises the following steps: ph was adjusted to 13.
5. The process of claim 1 for preparing potassium fluoride by decomposing fluorosilicic acid by electrodialysis, which comprises the following steps: the electrodialysis adopts bipolar membrane electrodialysis.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110403039.8A CN113086993A (en) | 2021-04-15 | 2021-04-15 | Process method for preparing potassium fluoride by decomposing fluosilicic acid through electrodialysis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110403039.8A CN113086993A (en) | 2021-04-15 | 2021-04-15 | Process method for preparing potassium fluoride by decomposing fluosilicic acid through electrodialysis |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113086993A true CN113086993A (en) | 2021-07-09 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110403039.8A Pending CN113086993A (en) | 2021-04-15 | 2021-04-15 | Process method for preparing potassium fluoride by decomposing fluosilicic acid through electrodialysis |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113086993A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113955720A (en) * | 2021-12-03 | 2022-01-21 | 浙江容跃环保科技有限公司 | Method and device for preparing hydrogen fluoride from BOE waste liquid |
| CN114180600A (en) * | 2022-01-04 | 2022-03-15 | 江苏中旗科技股份有限公司 | Separation method of ternary or quaternary mixed potassium salt |
| CN114436216A (en) * | 2022-03-03 | 2022-05-06 | 盛隆资源再生（无锡）有限公司 | Method for separating and recovering mixed acid of hydrofluoric acid and hydrochloric acid |
| CN114180600B (en) * | 2022-01-04 | 2024-04-30 | 江苏中旗科技股份有限公司 | Separation method of ternary or quaternary mixed potassium salt |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB891276A (en) * | 1959-12-11 | 1962-03-14 | Fertilizers & Chemicals Ltd | Process for the manufacture of potassium fluoride, hydrogen fluoride and silica from potassium fluosilicate |
| CN101134580A (en) * | 2006-09-01 | 2008-03-05 | 多氟多化工股份有限公司 | Method for producing potassium fluoride |
-
2021
- 2021-04-15 CN CN202110403039.8A patent/CN113086993A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB891276A (en) * | 1959-12-11 | 1962-03-14 | Fertilizers & Chemicals Ltd | Process for the manufacture of potassium fluoride, hydrogen fluoride and silica from potassium fluosilicate |
| CN101134580A (en) * | 2006-09-01 | 2008-03-05 | 多氟多化工股份有限公司 | Method for producing potassium fluoride |
Non-Patent Citations (1)
| Title |
|---|
| 刘家祺主编: "《分离过程与技术》", 31 December 2001, 天津大学出版社 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113955720A (en) * | 2021-12-03 | 2022-01-21 | 浙江容跃环保科技有限公司 | Method and device for preparing hydrogen fluoride from BOE waste liquid |
| CN114180600A (en) * | 2022-01-04 | 2022-03-15 | 江苏中旗科技股份有限公司 | Separation method of ternary or quaternary mixed potassium salt |
| CN114180600B (en) * | 2022-01-04 | 2024-04-30 | 江苏中旗科技股份有限公司 | Separation method of ternary or quaternary mixed potassium salt |
| CN114436216A (en) * | 2022-03-03 | 2022-05-06 | 盛隆资源再生（无锡）有限公司 | Method for separating and recovering mixed acid of hydrofluoric acid and hydrochloric acid |
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Application publication date: 20210709 |