CN101028934A - Method for linked producing potassium fluoride white carbon black - Google Patents
Method for linked producing potassium fluoride white carbon black Download PDFInfo
- Publication number
- CN101028934A CN101028934A CN 200610017487 CN200610017487A CN101028934A CN 101028934 A CN101028934 A CN 101028934A CN 200610017487 CN200610017487 CN 200610017487 CN 200610017487 A CN200610017487 A CN 200610017487A CN 101028934 A CN101028934 A CN 101028934A
- Authority
- CN
- China
- Prior art keywords
- carbon black
- white carbon
- potassium
- potassium fluoride
- fluoride solution
- 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.)
- Granted
Links
Landscapes
- Fertilizers (AREA)
- Silicon Compounds (AREA)
Abstract
A process for preparing potassium fluoride and white carbon black simultaneously includes such steps as reaction between fluorosilicic acid (or potassium fluorsilicate) and potassium hydroxide to obtain the slurry of white carbon black and potassium fluoride solution, filtering, washing to obtain white carbon black paste and potassium fluoride solution, and respectively preparing white carbon black and potassium fluride from them.
Description
Technical field
The present invention relates to a kind of method of producing the Potassium monofluoride co-producing white carbon black with silicofluoric acid or potassium silicofluoride.
Background technology
Potassium monofluoride, be mainly used in various alloys, metal soldering group flux, on generating, organic compound is widely used as fluorizating agent, be used to produce Tenate and monofluoroacetamide sterilant on the agricultural chemicals, pharmaceutically be used for making Norxin, it can be used as absorption agent (absorb HF and moisture), and it also is the raw material of system potassium hydrogen fluoride, also can be used for glass-engraving and food is anticorrosion.Its traditional production method is that hydrofluoric acid is making with the potassium hydroxide reaction of raw material, is raw material with hydrofluoric acid, and cost is higher.
White carbon black, the formal name used at school light silicon dioxide is mainly used the dispersion agent of used as pesticides, fire-fighting, the strengthening agent of rubber, plastics.Its traditional production method is the water glass acid hydrolyzation.
Silicofluoric acid is the by-product harmful waste of phophatic fertilizer production process, and purposes seldom and causes environment protection and to have a strong impact on, and the development process of silicofluoric acid is badly in need of solving.Potassium silicofluoride is the solid phase prod that silicofluoric acid makes, and is convenient to transportation, and its purposes is also considerably less.
Summary of the invention
The object of the present invention is to provide a kind of method of producing the Potassium monofluoride co-producing white carbon black,, turn waste into wealth effectively to utilize the by-product harmful waste of phophatic fertilizer production process.
To achieve these goals, technical program of the present invention lies in adopting a kind of method of producing the Potassium monofluoride co-producing white carbon black, with silicofluoric acid or potassium silicofluoride and potassium hydroxide raw material, potassium hydroxide and silicofluoric acid or potassium silicofluoride reaction are made white carbon black, temperature of reaction 80-100 ℃, reaction end pH value makes the slip of white carbon black precipitation and potassium fluoride solution between 8-11; With white carbon black slurry filtration, washing, obtain white carbon black ointment and potassium fluoride solution, white carbon black ointment obtains the white carbon black product through washing, drying; Potassium fluoride solution makes the Potassium monofluoride product through concentrated, spraying drying.
The concentration of silicofluoric acid is 10-40%.
The method of production Potassium monofluoride co-producing white carbon black of the present invention, with by-product harmful waste silicofluoric acid in the phophatic fertilizer production process or potassium silicofluoride is main raw material, substituted the feed hydrogen fluoric acid in traditional Potassium monofluoride production technique, and co-producing white carbon black, solved the development and use problem of silicofluoric acid or potassium silicofluoride effectively, alleviate the environmental issue of phosphate fertilizer industry, developed new fluorine resource.Adopt method of the present invention to greatly reduce production cost, solved puzzlement production of phosphate fertilizer producer effectively for a long time because the pollution problem of harmful waste silicofluoric acid has good economic worth and social value.
Reaction formula of the present invention is:
H
2SiF
6+6KOH＝6KF+SiO
2↓+4H
2O
Or K
2SiF
6+ 4KOH=6KF+SiO
2↓+2H
2O
Adopt method production Potassium monofluoride of the present invention and white carbon black product all to reach GB and customer requirement, specific targets are as follows:
Potassium monofluoride product quality analysis result
| GB | Present method | |||
| : specification | Top grade | One-level | 1# | 2# |
| Particle diameter (μ) | 1-50 | 1-50 | 43 | 46 |
| Specific surface (m2/g): | About 1.3 | About 1.3 | 1.31 | 1.23 |
| Bulk specific weight (g/cm 3): | 0.3-0.7 | 0.3-0.7 | 0.46 | 0.57 |
| Water content %: | ＜0.3 | ＜0.5 | 0.23 | 0.46 |
| Potassium monofluoride (KF) content %: | ＞99.0 | ＞98.0 | 99.3 | 98.5 |
| Clarity test: | Qualified | Qualified | Qualified | Qualified |
| Free acid (in HF) %: | ＜0.1 | ＜0.1 | 0.06 | -- |
| Free alkali (in K2CO3) %: | ＜0.05 | ＜0.5 | -- | 0.02 |
| Muriate (in KCL) %: | ＜0.2 | ＜2 | 0.15 | 0.21 |
White carbon black product quality analysis result
| Rower | Present method | ||||
| Index | BT-X | BT-M | BT-S | 1# | 2# |
| PH value | 5.0-8.0 | 5.0-8.0 | 5.0-8.0 | 6.0 | 5.5 |
| Weight loss on heating (%) | 4.0-8.0 | ≤5.0 | ≤5.0 | 4.3 | 5.8 |
| Screenings (%) | 75μm≤0.05 | 45μm≤1.0 | 0.05 | 0.08 | |
| DBP absorption value cm 3/g | ≥2.6 | 2.2-2.6 | ≥2.8 | 2.85 | 2.76 |
| Loose density g/ml | ≤0.11 | 0.11 | 0.10 | ||
| Basic metal mg/kg | ≤3.5 | 2.0 | 3.4 | ||
| Silicon-dioxide (%) | ≥90 | 93.6 | 93.2 | ||
| Burning decrement (%) | ≤7.0 | 5.4 | 4.8 | ||
| Color | Be better than or equal standard specimen | Be better than standard specimen | Be better than standard specimen | ||
| Refractive index | 1.45 | 1.43 | 1.50 | ||
| Specific surface area | 150-350 | 255 | 257 | ||
Embodiment
Embodiment 1
The method of the production Potassium monofluoride co-producing white carbon black in the present embodiment is: the concentration of silicofluoric acid is configured to 10%, potassium hydroxide and silicofluoric acid or potassium silicofluoride reacted make white carbon black, 85 ℃ of temperature of reaction, reaction end pH value is 9.0, makes the slip of white carbon black precipitation and potassium fluoride solution; With white carbon black slurry filtration, washing, obtain white carbon black ointment and potassium fluoride solution, white carbon black ointment obtains the white carbon black product through washing, drying; Potassium fluoride solution makes the Potassium monofluoride product through concentrated, spraying drying.
Embodiment 2
The method of the production Potassium monofluoride co-producing white carbon black in the present embodiment is: the concentration of silicofluoric acid is configured to 20%, potassium hydroxide and silicofluoric acid or potassium silicofluoride reacted make white carbon black, 90 ℃ of temperature of reaction, reaction end pH value is 9.5, makes the slip of white carbon black precipitation and potassium fluoride solution; With white carbon black slurry filtration, washing, obtain white carbon black ointment and potassium fluoride solution, white carbon black ointment obtains the white carbon black product through washing, drying; Potassium fluoride solution makes the Potassium monofluoride product through concentrated, spraying drying.
Embodiment 3
The method of the production Potassium monofluoride co-producing white carbon black of present embodiment is: the concentration of silicofluoric acid is configured to 30%, potassium hydroxide and silicofluoric acid or potassium silicofluoride reacted make white carbon black, 95 ℃ of temperature of reaction, reaction end pH value is 10.0, makes the slip of white carbon black precipitation and potassium fluoride solution.With white carbon black slurry filtration, washing, obtain white carbon black ointment and potassium fluoride solution, white carbon black ointment obtains the white carbon black product through washing, drying; Potassium fluoride solution makes the Potassium monofluoride product through concentrated, spraying drying.
It should be noted last that: above embodiment is the unrestricted technical scheme of the present invention in order to explanation only, although the present invention is had been described in detail with reference to the foregoing description, those of ordinary skill in the art is to be understood that: still can make amendment or be equal to replacement the present invention, and not breaking away from any modification or partial replacement of the spirit and scope of the present invention, it all should be encompassed in the middle of the claim scope of the present invention.
Claims (2)
1, a kind of method of producing the Potassium monofluoride co-producing white carbon black is characterized in that: with silicofluoric acid or potassium silicofluoride and potassium hydroxide raw material; Potassium hydroxide and silicofluoric acid or potassium silicofluoride reaction are made white carbon black, and temperature of reaction 80-100 ℃, reaction end pH value makes that white carbon black precipitates and the slip of potassium fluoride solution between 8-11; With white carbon black slurry filtration, washing, obtain white carbon black ointment and potassium fluoride solution, white carbon black ointment obtains the white carbon black product through washing, drying; Potassium fluoride solution makes the Potassium monofluoride product through concentrated, spraying drying.
2, the method for production Potassium monofluoride co-producing white carbon black according to claim 1 is characterized in that: the concentration of silicofluoric acid is 10-40%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200610017487A CN100577569C (en) | 2006-03-01 | 2006-03-01 | A kind of method of producing the Potassium monofluoride co-producing white carbon black |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200610017487A CN100577569C (en) | 2006-03-01 | 2006-03-01 | A kind of method of producing the Potassium monofluoride co-producing white carbon black |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101028934A true CN101028934A (en) | 2007-09-05 |
| CN100577569C CN100577569C (en) | 2010-01-06 |
Family
ID=38714505
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200610017487A Expired - Fee Related CN100577569C (en) | 2006-03-01 | 2006-03-01 | A kind of method of producing the Potassium monofluoride co-producing white carbon black |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100577569C (en) |
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102701236A (en) * | 2012-07-06 | 2012-10-03 | 张家港市华盛化学有限公司 | Preparation method of potassium fluoride |
| CN102887531A (en) * | 2012-10-15 | 2013-01-23 | 张军航 | Technique for producing potassium fluoride from potassium fluosilicate |
| CN103101931A (en) * | 2013-02-26 | 2013-05-15 | 山东金正大生态工程股份有限公司 | Method for preparing potassium fluoride by using potassium fluosilicate with co-production of white carbon black |
| CN103112873A (en) * | 2013-02-26 | 2013-05-22 | 山东金正大生态工程股份有限公司 | Method for preparing high-purity potassium fluoride and co-producing white carbon black by adopting potassium fluosilicate |
| CN103663474A (en) * | 2013-12-20 | 2014-03-26 | 瓮福（集团）有限责任公司 | Method for preparing white carbon black from silicon slags containing fluorine |
| CN104326475A (en) * | 2014-07-01 | 2015-02-04 | 多氟多化工股份有限公司 | Method for preparing potassium fluoride by employing fluosilicic acid with co-production of white carbon black |
| CN107973321A (en) * | 2017-12-14 | 2018-05-01 | 江西渠成氟化学有限公司 | A kind of preparation method of potassium fluoride |
| CN108083295A (en) * | 2017-12-29 | 2018-05-29 | 武汉工程大学 | A kind of method that potassium fluoride is directly prepared using wet process phosphoric acid by-product fluosilicic acid |
| CN109019984A (en) * | 2018-09-13 | 2018-12-18 | 衢州市鼎盛化工科技有限公司 | A kind of method and system recycling efficient resource from glass thinning acid pickle |
| 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 |
| CN110589854A (en) * | 2019-10-24 | 2019-12-20 | 徐小岗 | Method for producing electronic-grade fluoride salt by using fluosilicic acid and fluosilicate |
| CN111017937A (en) * | 2019-12-31 | 2020-04-17 | 贵州瓮福蓝天氟化工股份有限公司 | Method for preparing potassium fluoride and co-producing ultrafine white carbon black |
| CN111762799A (en) * | 2019-12-31 | 2020-10-13 | 承德莹科精细化工股份有限公司 | Process for co-producing high-quality white carbon black by self-producing silica gel crystal seeds in alkaline hydrolysis process during production of potassium fluoride from potassium fluosilicate |
| CN112551531A (en) * | 2020-11-24 | 2021-03-26 | 浙江巨化技术中心有限公司 | Method for coproducing hydrogen fluoride, white carbon black and potassium sulfate |
| CN113060745A (en) * | 2021-03-19 | 2021-07-02 | 严永生 | Preparation method for preparing potassium fluoride by using potash and potassium fluosilicate |
| CN113479891A (en) * | 2021-07-02 | 2021-10-08 | 多氟多新材料股份有限公司 | Method for treating fluoroethylene carbonate solid waste residue |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB647395A (en) * | 1948-11-02 | 1950-12-13 | James Wilkinson & Son Ltd | Improvements in and relating to the production of sodium fluoride from sodium silicofluoride |
| US3488702A (en) * | 1966-05-31 | 1970-01-06 | Ethyl Corp | Production of inorganic fluoro-chemicals and silicon dioxide |
| IL116144A0 (en) * | 1995-11-27 | 1996-01-31 | Harel Simcha | Production of sodium fluoride and silica |
| RU2175639C1 (en) * | 2000-05-15 | 2001-11-10 | Федеральное государственное унитарное предприятие "Сибирский химический комбинат" | Method of preparing sodium fluoride from fluosilicate compounds |
-
2006
- 2006-03-01 CN CN200610017487A patent/CN100577569C/en not_active Expired - Fee Related
Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102701236A (en) * | 2012-07-06 | 2012-10-03 | 张家港市华盛化学有限公司 | Preparation method of potassium fluoride |
| CN102887531A (en) * | 2012-10-15 | 2013-01-23 | 张军航 | Technique for producing potassium fluoride from potassium fluosilicate |
| CN102887531B (en) * | 2012-10-15 | 2014-07-02 | 张军航 | Technique for producing potassium fluoride from potassium fluosilicate |
| CN103101931A (en) * | 2013-02-26 | 2013-05-15 | 山东金正大生态工程股份有限公司 | Method for preparing potassium fluoride by using potassium fluosilicate with co-production of white carbon black |
| CN103112873A (en) * | 2013-02-26 | 2013-05-22 | 山东金正大生态工程股份有限公司 | Method for preparing high-purity potassium fluoride and co-producing white carbon black by adopting potassium fluosilicate |
| CN103663474A (en) * | 2013-12-20 | 2014-03-26 | 瓮福（集团）有限责任公司 | Method for preparing white carbon black from silicon slags containing fluorine |
| CN103663474B (en) * | 2013-12-20 | 2016-05-18 | 瓮福（集团）有限责任公司 | Method for preparing white carbon black from fluorine-containing silicon slag |
| CN104326475A (en) * | 2014-07-01 | 2015-02-04 | 多氟多化工股份有限公司 | Method for preparing potassium fluoride by employing fluosilicic acid with co-production of white carbon black |
| CN107973321A (en) * | 2017-12-14 | 2018-05-01 | 江西渠成氟化学有限公司 | A kind of preparation method of potassium fluoride |
| CN108083295A (en) * | 2017-12-29 | 2018-05-29 | 武汉工程大学 | A kind of method that potassium fluoride is directly prepared using wet process phosphoric acid by-product fluosilicic acid |
| CN109019984A (en) * | 2018-09-13 | 2018-12-18 | 衢州市鼎盛化工科技有限公司 | A kind of method and system recycling efficient resource from glass thinning acid pickle |
| 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 |
| CN110589854A (en) * | 2019-10-24 | 2019-12-20 | 徐小岗 | Method for producing electronic-grade fluoride salt by using fluosilicic acid and fluosilicate |
| CN111017937A (en) * | 2019-12-31 | 2020-04-17 | 贵州瓮福蓝天氟化工股份有限公司 | Method for preparing potassium fluoride and co-producing ultrafine white carbon black |
| CN111762799A (en) * | 2019-12-31 | 2020-10-13 | 承德莹科精细化工股份有限公司 | Process for co-producing high-quality white carbon black by self-producing silica gel crystal seeds in alkaline hydrolysis process during production of potassium fluoride from potassium fluosilicate |
| CN112551531A (en) * | 2020-11-24 | 2021-03-26 | 浙江巨化技术中心有限公司 | Method for coproducing hydrogen fluoride, white carbon black and potassium sulfate |
| CN113060745A (en) * | 2021-03-19 | 2021-07-02 | 严永生 | Preparation method for preparing potassium fluoride by using potash and potassium fluosilicate |
| CN113479891A (en) * | 2021-07-02 | 2021-10-08 | 多氟多新材料股份有限公司 | Method for treating fluoroethylene carbonate solid waste residue |
| CN113479891B (en) * | 2021-07-02 | 2023-09-22 | 多氟多新材料股份有限公司 | Treatment method of fluoroethylene carbonate solid waste residues |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100577569C (en) | 2010-01-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101028934A (en) | Method for linked producing potassium fluoride white carbon black | |
| CN100577567C (en) | Method for linked production of ammonium fluoride and white carbon black | |
| CN101028931A (en) | Method for linked producing ammonium acid fluoride and white carbon black | |
| CN101134580A (en) | Method for producing potassium fluoride | |
| CN102887532B (en) | Process for preparing potassium fluoride and co-producing white carbon black from fluosilicic acid | |
| CN104030297B (en) | A kind of production technology utilizing hexafluosilicic acid to produce sodium fluoride co-producing white carbon black | |
| CN103991882A (en) | Method for preparing potassium fluoride by using fluoride in liquid phase of wet process phosphoric acid | |
| CN103101931A (en) | Method for preparing potassium fluoride by using potassium fluosilicate with co-production of white carbon black | |
| CN101134595A (en) | Method for producing calcium fluoride | |
| CN106241834B (en) | Sodium bifluoride technology is prepared using phosphorous chemical industry fluosilicic acid as byproduct | |
| CN101134590A (en) | Method for producing aluminun fluoride with combined production of white carbon black and ammonia sulfate | |
| CN101134563A (en) | Method for producing hydrofluoric acid, waterless magnesium sulfate and sodium fluoride | |
| CN104556179A (en) | Method for producing cryolite from fluorine-containing waste gas | |
| CN102040206A (en) | Method for recycling acid sludge produced by concentrated phosphoric acid | |
| CN105366643B (en) | A kind of method that dilute fluosilicic acid of solvent extraction prepares fluoride salt co-producing white carbon black | |
| CN103435376A (en) | Method and apparatus used for preparing ammonium phosphate fertilizer from phosphoric acid sediment | |
| CN1515493A (en) | Method for simultaneously producing sodium aluminofluoride and silica white | |
| CN102897802B (en) | Method for recycling reagent-grade anhydrous sodium sulfate from basic cupric carbonate production waste liquid | |
| CN203886391U (en) | System for treating tail gas generated in production of white carbon black by adopting gas phase method | |
| CN107697939A (en) | A kind of method that ice crystal is produced using waste gas containing fluoride | |
| CN1194897C (en) | Method for producing cryolite | |
| CN101134583A (en) | Preparation method of potassium fluoride | |
| CN103738967A (en) | Method for production of sodium fluosilicate from fluorine-containing acidic wastewater | |
| CN109809483A (en) | A kind of thick zirconium chloride impurity removal and purification technique | |
| CN108083295A (en) | A kind of method that potassium fluoride is directly prepared using wet process phosphoric acid by-product fluosilicic acid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C53 | Correction of patent for invention or patent application | ||
| CB03 | Change of inventor or designer information |
Inventor after: Li Shijiang Inventor after: Li Yunfeng Inventor after: Hou Hongjun Inventor after: Yang Huachun Inventor after: Huangfu Genli Inventor after: Yan Chunsheng Inventor after: Zhang Mei Inventor after: Li Jie Inventor after: Li Yongqing Inventor after: Han Shijun Inventor before: Li Shijiang Inventor before: Hou Hongjun Inventor before: Yang Huachun Inventor before: Huangfu Genli Inventor before: Yan Chunsheng Inventor before: Zhang Mei Inventor before: Li Jie |
|
| COR | Change of bibliographic data |
Free format text: CORRECT: INVENTOR; FROM: LI SHIJIANG HOU HONGJUN YANG HUACHUN HUANGFU GENLI YAN CHUNSHENG ZHANG MEILI JIE TO: LI SHIJIANG HOU HONGJUN YANG HUACHUN HUANGFU GENLI YAN CHUNSHENG ZHANG MEI LI JIE LI YONGQING HAN SHIJUN LI YUNFENG |
|
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20100106 Termination date: 20150301 |
|
| EXPY | Termination of patent right or utility model |