CN113060745A - Preparation method for preparing potassium fluoride by using potash and potassium fluosilicate - Google Patents
Preparation method for preparing potassium fluoride by using potash and potassium fluosilicate Download PDFInfo
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- CN113060745A CN113060745A CN202110293422.2A CN202110293422A CN113060745A CN 113060745 A CN113060745 A CN 113060745A CN 202110293422 A CN202110293422 A CN 202110293422A CN 113060745 A CN113060745 A CN 113060745A
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- Prior art keywords
- potassium
- potassium fluoride
- fluosilicate
- fluoride
- solid
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- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 title claims abstract description 70
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 title claims abstract description 47
- 239000011698 potassium fluoride Substances 0.000 title claims abstract description 35
- 235000003270 potassium fluoride Nutrition 0.000 title claims abstract description 35
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 239000011591 potassium Substances 0.000 title claims abstract description 20
- 229910052700 potassium Inorganic materials 0.000 title claims abstract description 20
- 229940072033 potash Drugs 0.000 title claims abstract description 11
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 title claims abstract description 11
- 235000015320 potassium carbonate Nutrition 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims description 4
- 239000007787 solid Substances 0.000 claims abstract description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000012452 mother liquor Substances 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000006229 carbon black Substances 0.000 claims abstract description 13
- 239000002918 waste heat Substances 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 4
- 238000001694 spray drying Methods 0.000 claims description 11
- 238000002425 crystallisation Methods 0.000 claims description 8
- 230000008025 crystallization Effects 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 3
- 230000002194 synthesizing effect Effects 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 14
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 6
- 229910052731 fluorine Inorganic materials 0.000 description 6
- 239000011737 fluorine Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- 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 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 239000002686 phosphate fertilizer Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
Images
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
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
- C01B33/186—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof from or via fluosilicic acid or salts thereof by a wet process
-
- 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
-
- 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
- C01P2006/82—Compositional purity water content
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/129—Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention discloses a process method for preparing white carbon black and potassium fluoride by replacing potassium fluosilicate with potash. Reacting potassium fluosilicate with strong potassium hydroxide to obtain white carbon black, concentrating clean mother liquor, separating solid liquid to obtain potassium fluoride, returning the mother liquor to a potassium fluosilicate reaction tank to participate in reaction, wherein the potassium fluoride is spray-dried at 550 ℃ to obtain anhydrous potassium fluoride with the mass fraction of more than 98.5%, and using waste heat for concentrating and crystallizing.
Description
Technical Field
The invention relates to a preparation method for preparing potassium fluoride by using potash and potassium fluosilicate, belonging to the field of fine chemicals in chemical engineering.
Background
The fluosilicic acid is a low-value byproduct in the wet-process phosphate fertilizer production process, has few purposes, can cause serious influence on environmental protection, and is urgently needed to be solved for development and utilization. The white carbon black is used as a reinforcing material with excellent performance, and has wide market and good development prospect in the processing and application of high polymer materials; the ammonium fluoride can be used as a raw material to prepare anhydrous hydrofluoric acid, and a plurality of fluorides can be derived, so that the route is an effective way for comprehensively utilizing the fluosilicic acid. The process for preparing the white carbon black and the ammonium fluoride by the hydrofluosilicic acid ammoniation method is an intermittent process at home, and the intermittent process has the defects of low equipment utilization rate, low automation degree, small scale of single set of equipment and the like, so that the technology is not built by a large-scale industrial device at home, and the utilization of fluorine and silicon resources of a wet-process phosphoric acid enterprise at home is limited. On the other hand, the fluosilicic acid can be used as a raw material to prepare various fluorine-containing industrial products.
Disclosure of Invention
The invention aims to solve the technical problem of the prior method for preparing potassium fluoride by comprehensively utilizing potassium fluosilicate.
In order to solve the technical problems, the invention adopts the following technical scheme:
the technical scheme is as follows:
a method for preparing potassium fluoride by using potash and potassium fluosilicate comprises the following steps:
synthesizing white carbon black: reacting potassium fluosilicate with potassium hydroxide to obtain white carbon black and potassium fluoride, wherein the concentration of the potassium hydroxide is required to be more than 30%; the white carbon black is filtered by a plate filter. The solid is white carbon black, and the mother liquor is subjected to next concentration and crystallization;
concentration and crystallization: concentrating the mother liquor by using spray-dried waste heat tail gas, wherein the solid content is more than 50%;
thirdly, solid-liquid separation: filtering by using a plate filter, wherein the solid is potassium fluoride solid with the solid content of 50-65%;
spray drying: and (3) carrying out spray drying at 500-600 ℃ to obtain anhydrous potassium fluoride with the mass content of more than 98.5%, and carrying out waste heat to concentrate, crystallize and dry water.
The concentration of potassium hydroxide in the method is 48%.
The concentration of the potassium hydroxide in the method is 30%.
The temperature of the spray drying of the method is 550 ℃.
The mass fraction of the anhydrous potassium fluoride is 98.5%.
The embodiment is superior to the comparative example, the comparative example is superior in each content, and the scheme is worthy of popularization.
TABLE 1 comparison of the examples with the comparative examples
Project Specification example 1 example 2 example 3 comparative example 1
Spray temperature 1550600500450
Ammonium fluoride content% 98.598.798.690.1.
Drawings
FIG. 1 is a process flow of a process for preparing potassium fluoride using potash and potassium fluosilicate, wherein 1: potassium fluosilicate; 2: potassium hydroxide; 3: synthesizing; 4: precipitating; 5: white carbon black; 6: concentrating and crystallizing; 7: separating solid from liquid; 8: 9, spray drying; 10 parts of anhydrous potassium fluoride and 11 parts of waste heat tail gas.
Detailed Description
Example 1:
200kg of 48% potash and 150kg of potassium fluosilicate are mixed in a reaction tank, after complete reaction, silicon dioxide is filtered by a plate filter after precipitation, mother liquor is concentrated and crystallized, solid is separated by the plate filter, the solid is potassium fluoride, and the mother liquor returns to the reaction tank to react with fluorine. The solid potassium fluoride is dried at 550 ℃ by spray drying to obtain 98.5 percent anhydrous potassium fluoride. And returning the waste heat tail gas to perform mother liquor concentration and crystallization.
Example 2:
200kg of 48% potash and 150kg of potassium fluosilicate are mixed in a reaction tank, after complete reaction, silicon dioxide is filtered by a plate filter after precipitation, mother liquor is concentrated and crystallized, solid is separated by the plate filter, the solid is potassium fluoride, and the mother liquor returns to the reaction tank to react with fluorine. The solid potassium fluoride is dried by spray drying at 600 ℃ to obtain 98.7 percent anhydrous potassium fluoride. And returning the waste heat tail gas to perform mother liquor concentration and crystallization.
Example 3:
200kg of 48% potash and 150kg of potassium fluosilicate are mixed in a reaction tank, after complete reaction, silicon dioxide is filtered by a plate filter after precipitation, mother liquor is concentrated and crystallized, solid is separated by the plate filter, the solid is potassium fluoride, and the mother liquor returns to the reaction tank to react with fluorine. The solid potassium fluoride is dried at 500 ℃ by spray drying to obtain 98.6 percent anhydrous potassium fluoride. And returning the waste heat tail gas to perform mother liquor concentration and crystallization.
Comparative example 1:
200kg of 48% potash and 150kg of potassium fluosilicate are mixed in a reaction tank, after complete reaction, silicon dioxide is filtered by a plate filter after precipitation, mother liquor is concentrated and crystallized, solid is separated by the plate filter, the solid is potassium fluoride, and the mother liquor returns to the reaction tank to react with fluorine. The solid potassium fluoride is dried at 450 ℃ by spray drying to obtain 90.1 percent anhydrous potassium fluoride. And returning the waste heat tail gas to perform mother liquor concentration and crystallization.
Claims (4)
1. A preparation method for preparing potassium fluoride by using potash and potassium fluosilicate is characterized by comprising the following steps:
synthesizing white carbon black: reacting potassium fluosilicate with potassium hydroxide to obtain white carbon black and potassium fluoride, wherein the concentration of the potassium hydroxide is required to be more than 30%; filtering white carbon black by using a plate filter, wherein the solid is the white carbon black, and the mother liquor is subjected to next concentration and crystallization;
concentration and crystallization: concentrating the mother liquor by using spray-dried waste heat tail gas, wherein the solid content is more than 50%;
thirdly, solid-liquid separation: filtering by using a plate filter, wherein the solid is potassium fluoride solid with the solid content of 50-65%;
spray drying: spray drying is carried out at 500-600 ℃ to obtain anhydrous potassium fluoride with the mass content of more than or equal to 98.5%, and the water is concentrated, crystallized and dried by waste heat.
2. The process for producing potassium fluoride using potassium hydroxide and potassium fluosilicate according to claim 1, wherein: the potassium hydroxide concentration was 48%.
3. The process for producing potassium fluoride using potassium hydroxide and potassium fluosilicate according to claim 1, wherein: the spray drying temperature was 550 ℃.
4. The process for producing potassium fluoride using potassium hydroxide and potassium fluosilicate according to claim 1, wherein: the mass fraction of the anhydrous potassium fluoride is 98.5 percent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110293422.2A CN113060745A (en) | 2021-03-19 | 2021-03-19 | Preparation method for preparing potassium fluoride by using potash and potassium fluosilicate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110293422.2A CN113060745A (en) | 2021-03-19 | 2021-03-19 | Preparation method for preparing potassium fluoride by using potash and potassium fluosilicate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113060745A true CN113060745A (en) | 2021-07-02 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110293422.2A Pending CN113060745A (en) | 2021-03-19 | 2021-03-19 | Preparation method for preparing potassium fluoride by using potash and potassium fluosilicate |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101028934A (en) * | 2006-03-01 | 2007-09-05 | 多氟多化工股份有限公司 | Method for linked producing potassium fluoride white carbon black |
| CN102887531A (en) * | 2012-10-15 | 2013-01-23 | 张军航 | Technique for producing potassium fluoride from potassium fluosilicate |
| CN103663499A (en) * | 2013-11-13 | 2014-03-26 | 安徽六国化工股份有限公司 | Method for preparing potassium fluoride and coproducing ultrafine white carbon black from ammonium fluorosilicate byproduct in phosphate fertilizer production |
| CN110436485A (en) * | 2019-09-05 | 2019-11-12 | 徐小岗 | A method of potassium fluoride in high activity is produced using fluosilicic acid and potassium fluosilicate |
| CN110510640A (en) * | 2019-10-08 | 2019-11-29 | 内蒙古星汉氟都化工有限公司 | A method of it with fluosilicic acid is that raw material prepares potassium fluoride co-producing white carbon black |
-
2021
- 2021-03-19 CN CN202110293422.2A patent/CN113060745A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101028934A (en) * | 2006-03-01 | 2007-09-05 | 多氟多化工股份有限公司 | Method for linked producing potassium fluoride white carbon black |
| CN102887531A (en) * | 2012-10-15 | 2013-01-23 | 张军航 | Technique for producing potassium fluoride from potassium fluosilicate |
| CN103663499A (en) * | 2013-11-13 | 2014-03-26 | 安徽六国化工股份有限公司 | Method for preparing potassium fluoride and coproducing ultrafine white carbon black from ammonium fluorosilicate byproduct in phosphate fertilizer production |
| CN110436485A (en) * | 2019-09-05 | 2019-11-12 | 徐小岗 | A method of potassium fluoride in high activity is produced using fluosilicic acid and potassium fluosilicate |
| CN110510640A (en) * | 2019-10-08 | 2019-11-29 | 内蒙古星汉氟都化工有限公司 | A method of it with fluosilicic acid is that raw material prepares potassium fluoride co-producing white carbon black |
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| PB01 | Publication | ||
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| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210702 |
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| RJ01 | Rejection of invention patent application after publication |