CN102887530B - Production technique of potassium fluoride - Google Patents
Production technique of potassium fluoride Download PDFInfo
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- CN102887530B CN102887530B CN201210389357.4A CN201210389357A CN102887530B CN 102887530 B CN102887530 B CN 102887530B CN 201210389357 A CN201210389357 A CN 201210389357A CN 102887530 B CN102887530 B CN 102887530B
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Abstract
The invention provides a production technique of potassium fluoride, particularly a technique for producing potassium fluoride and coproducing high-purity silicon dioxide mainly from an anhydrous hydrogen fluoride production line byproduct fluosilicic acid, ammonia water and potassium hydroxide. According to the production technique of potassium fluoride, a silicon complexing reagent is added to prevent the ammonia from generating complex precipitates of ammonium fluosilicate and ammonium fluoride during desilication and enhance the separability between silicon dioxide and water; at the beginning of the potassium fluoride synthetic reaction, steam is introduced to shorten the ammonia removal reaction time; and the ammonia is used repeatedly. The invention provides a method for producing potassium fluoride from a new fluorine source anhydrous hydrogen fluoride production line byproduct fluosilicic acid instead of anhydrous hydrogen fluoride to enhance the product quality of potassium fluoride, so that 6 fluorines in the fluosilicic acid are completely released to substitute hydrofluoric acid, thereby greatly lowering the production cost of potassium fluoride and enhancing the benefits of the potassium fluoride production enterprise.
Description
Technical field
The invention belongs to chemical field, specifically a kind of production technique of Potassium monofluoride.
Background technology
Potassium monofluoride purposes is quite extensive, and for various glass etchings, food is anticorrosion, electroplate, wood preservative, welding fusing assistant, agricultural insecticide and pesticide intermediate, pharmaceutical industry raw material and organic raw material, catalyzer, absorption agent (absorbing HF and moisture) etc. fluoridized.Also be the raw material of producing potassium hydrogen fluoride.
The features such as fluorine-containing medicines has efficiently, wide spectrum, low toxicity, low residue, Drugs Containing Fluorine reaches hundreds of in the world at present, it is a very important class in synthetic drugs, there are many medicines to become the principal item for the treatment of some disease, as fluoroquinolones antibiotics Ofloxacine USP 23, antidepressant class medicine fluoxetine, diabetes class medicine sitagliptin etc.Because fluorine organic compound has special biological activity and biological fitness, the exploitation that therefore sets it as medicine is very active, and many product innovations are still among exploitation endlessly.At present, the research and development of fluoro-containing pesticide, medicine, dye well liquid crystal are in the ascendant with production, occurred a large amount of high performance fluorochemicalss, and wherein the fluorine of a lot of products gets on by Potassium monofluoride " extension ".Potassium monofluoride is as the important source material of fluorine-containing medicines intermediate, and development prospect is considerable.Mostly the method for traditional mode of production Potassium monofluoride is to adopt the reaction of potassium hydroxide-hydrofluoric acid neutralisation to make, hydrofluoric acid in traditional technology is mainly made by fluorite and sulfuric acid reaction, traditional technology need to consume valuable resource fluorite, hydrofluoric acid cost is quite high, and fluorite and sulfuric acid reaction make the by-product fluosilicic acid that hydrofluoric acid produces and never have so effective that to use.
Summary of the invention
In order to solve the problems of the technologies described above, the invention provides a kind of production technique of Potassium monofluoride.
Reaction formula of the present invention is:
H2SiF6+6NH4OH――→6NH4F+SiO2+4H2O
NH4F+KOH――→KF+NH3+H2O
A production technique for Potassium monofluoride, is characterized in that it comprises the steps:
1) silicofluoric acid is added to reactor, start stirring, add silicon complexing agent, at the uniform velocity add ammoniacal liquor, fully reaction;
2) reaction filtrate is carried out to solid-liquid separation, solid is pulled an oar to clean and is obtained high-purity silicon dioxide, after being dried, obtains white carbon black, and after liquid filtering, filtrate enters filtrate receiver;
3) reaction solution is added to Potassium monofluoride synthesis reactor, open stir, at the uniform velocity add liquid potassium hydroxide, pass into steam, reaction generate ammonia be absorbed as ammoniacal liquor through refrigeration cycle, be stored in basin, for desiliconization for subsequent use;
4) reaction liquid is added to transfer tank, precipitation 24h, clear liquid adds concentration kettle concentrated;
5) the Potassium monofluoride mother liquor after concentrated is added to groove to be painted, then squeeze into spray-drying tower by groove to be painted and spray and be dried, finished product is anhydrous potassium fluoride.
The production technique of described a kind of Potassium monofluoride, is characterized in that silicofluoric acid described in step 1) is anhydrous hydrogen fluoride production line by product, and its mass percentage concentration is 20-45%.
The production technique of described a kind of Potassium monofluoride, the amount that it is characterized in that the silicon complexing agent adding in step 1) is 0.2% of silicofluoric acid weight.
The production technique of described a kind of Potassium monofluoride, is characterized in that adding ammoniacal liquor according to 1.1-1.15 times of the required mole number of reaction in step 1), and the mass percentage concentration that adds ammoniacal liquor is 25%.
The production technique of described a kind of Potassium monofluoride, it is characterized in that reacting in step 1) to the pH value of reaction end be 8.5-9.
The production technique of described a kind of Potassium monofluoride, is characterized in that adding liquid potassium hydroxide according to 0.9-1.1 times of the required mole number of reaction in step 3).
The production technique of described a kind of Potassium monofluoride, is characterized in that passing in step 3) the temperature that steam makes reaction solution and remains on more than 110 DEG C.
The production technique of described a kind of Potassium monofluoride, it is characterized in that reacting in step 3) to the pH value of reaction end be 7.5-8.
The production technique of described a kind of Potassium monofluoride, is characterized in that the mass percentage concentration that is concentrated into solution in still in step 4) reaches 48%-50%.
The production technique of described a kind of Potassium monofluoride, is characterized in that the silicon complexing agent described in step 1) is nitrilotriacetic acid(NTA) sodium.
The production technique of a kind of Potassium monofluoride of the present invention, add silicon complexometric reagent, while preventing with ammonia desiliconization, generate the complex compound sediment of ammonium silicofluoride and Neutral ammonium fluoride, improve the separation property of silicon-dioxide and water, in the time of Potassium monofluoride building-up reactions, pass at the beginning steam, can shorten the deamination reaction time, and ammonia is to recycle, provide a kind of new fluorine source anhydrous hydrogen fluoride production line fluosilicic acid as byproduct to replace anhydrous hydrogen fluoride to produce the method for Potassium monofluoride, to improve Potassium monofluoride quality product, make 6 fluorine in silicofluoric acid all discharge, replace hydrofluoric acid, can greatly reduce the production cost of Potassium monofluoride, promote Potassium monofluoride manufacturing enterprise benefit.
Embodiment
Embodiment 1
1, the silicofluoric acid that is 20% by anhydrous hydrogen fluoride production line by product mass percentage concentration adds reactor, start stirring, add the nitrilotriacetic acid(NTA) sodium of 0.2% amount of silicofluoric acid weight, at the uniform velocity to add mass percentage concentration according to 1.1 times of the required mole number of reaction formula be 25% ammoniacal liquor, fully reaction, the pH value of reaction end is 8.5.
2, after reacting completely in reactor, reaction solution carries out solid-liquid separation, and solid is pulled an oar to clean and is high-purity silicon dioxide, can do after drying white carbon black and sell, and filtrate enters filtrate receiver.
3, reaction filtrate is added to Potassium monofluoride synthesis reactor, open and stir, at the uniform velocity add liquid potassium hydroxide according to 1.1 times of the required mole number of reaction formula, pass at the beginning steam, make more than reacting liquid temperature remains on 110 degree, this reaction needs heating at the beginning, and the water vapor that reaction generates is through cooling, vapor-liquid separation, and liquid enters condensate trap, ammonia is absorbed as ammoniacal liquor through refrigeration cycle, be stored in basin, for subsequent use for desiliconization, the pH value of reaction end is 8.
4, after reacting completely, liquid adds transfer tank, precipitation 24h, and clear liquid adds concentration kettle, the water vapor concentrating out is through cooling, vapor-liquid separation, and liquid enters condensate trap, and gas, through but circulating and be absorbed as ammoniacal liquor, is stored in basin, for subsequent use for desiliconization, in still, solution quality percentage concentration reaches 48%, concentrated end.
5, the Potassium monofluoride mother liquor after concentrated is added to groove to be painted, then it is dry to add spray-drying tower to spray by groove to be painted, finished product is anhydrous potassium fluoride.
Embodiment 2
1, the silicofluoric acid that is 30% by anhydrous hydrogen fluoride production line by product mass percentage concentration adds reactor, start stirring, add the nitrilotriacetic acid(NTA) sodium of 0.2% amount of silicofluoric acid weight, at the uniform velocity to add mass percentage concentration according to 1.1 times of the required mole number of reaction formula be 25% ammoniacal liquor, fully reaction, the pH value of reaction end is 8.5.
2, after reacting completely in reactor, reaction solution carries out solid-liquid separation, and solid is pulled an oar to clean and is high-purity silicon dioxide, can do after drying white carbon black and sell, and filtrate enters filtrate receiver.
3, reaction filtrate is added to Potassium monofluoride synthesis reactor, open and stir, at the uniform velocity add liquid potassium hydroxide according to 0.9 times of the required mole number of reaction formula, pass at the beginning steam, make more than reacting liquid temperature remains on 110 degree, this reaction needs heating at the beginning, and the water vapor that reaction generates is through cooling, vapor-liquid separation, and liquid enters condensate trap, ammonia is absorbed as ammoniacal liquor through refrigeration cycle, be stored in basin, for subsequent use for desiliconization, the pH value of reaction end is 7.5.
4, after reacting completely, liquid adds transfer tank, precipitation 24h, and clear liquid adds concentration kettle, the water vapor concentrating out is through cooling, vapor-liquid separation, and liquid enters condensate trap, and gas, through but circulating and be absorbed as ammoniacal liquor, is stored in basin, for subsequent use for desiliconization, in still, solution quality percentage concentration reaches 50%, concentrated end.
5, the Potassium monofluoride mother liquor after concentrated is added to groove to be painted, then it is dry to add spray-drying tower to spray by groove to be painted, finished product is anhydrous potassium fluoride.
Embodiment 3
1, the silicofluoric acid that is 40% by anhydrous hydrogen fluoride production line by product mass percentage concentration adds reactor, start stirring, add the nitrilotriacetic acid(NTA) sodium of 0.2% amount of silicofluoric acid weight, at the uniform velocity to add mass percentage concentration according to 1.15 times of the required mole number of reaction formula be 25% ammoniacal liquor, fully reaction, the pH value of reaction end is 9.
2, after reacting completely in reactor, reaction solution carries out solid-liquid separation, and solid is pulled an oar to clean and is high-purity silicon dioxide, can do after drying white carbon black and sell, and filtrate enters filtrate receiver.
3, reaction filtrate is added to Potassium monofluoride synthesis reactor, open and stir, at the uniform velocity add liquid potassium hydroxide according to 1.1 times of the required mole number of reaction formula, pass at the beginning steam, make more than reacting liquid temperature remains on 110 degree, this reaction needs heating at the beginning, and the water vapor that reaction generates is through cooling, vapor-liquid separation, and liquid enters condensate trap, ammonia is absorbed as ammoniacal liquor through refrigeration cycle, be stored in basin, for subsequent use for desiliconization, the pH value of reaction end is 8.
4, after reacting completely, liquid adds transfer tank, precipitation 24h, and clear liquid adds concentration kettle, the water vapor concentrating out is through cooling, vapor-liquid separation, and liquid enters condensate trap, and gas, through but circulating and be absorbed as ammoniacal liquor, is stored in basin, for subsequent use for desiliconization, in still, solution quality percentage concentration reaches 50%, concentrated end.
5, the Potassium monofluoride mother liquor after concentrated is added to groove to be painted, then it is dry to add spray-drying tower to spray by groove to be painted, finished product is anhydrous potassium fluoride.
Table 1 is the Potassium monofluoride product quality analysis result (each embodiment respectively carries out twice experiment) of utilizing method of the present invention to produce, conformance with standard HG/T 2829-2008.
The Potassium monofluoride product quality analysis result that table 1 utilizes method of the present invention to produce
Table 2 is high-purity silicon dioxide (rubber ingredients precipitated hydrated silica) mass analysis results (each embodiment respectively carries out twice experiment) of utilizing method of the present invention to produce, conformance with standard: HG/T 3061-2009.
High-purity silicon dioxide (rubber ingredients precipitated hydrated silica) the mass analysis result that table 2 utilizes method of the present invention to produce
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within being all included in protection scope of the present invention.
Claims (1)
1. a production technique for Potassium monofluoride, is characterized in that it comprises the steps:
1) silicofluoric acid is added to reactor, start stirring, add the nitrilotriacetic acid(NTA) sodium of silicofluoric acid weight 0.2% as silicon complexing agent, at the uniform velocity adding mass percentage concentration according to reaction 1.1-1.15 times of required mole number is 25% ammoniacal liquor, fully react to the pH value of reaction end be 8.5-9; Described silicofluoric acid is anhydrous hydrogen fluoride production line by product, and its mass percentage concentration is 20-45%;
2) reaction solution is carried out to solid-liquid separation, solid is pulled an oar to clean and is obtained high-purity silicon dioxide, after being dried, obtains white carbon black, and after liquid filtering, filtrate enters filtrate receiver;
3) reaction filtrate is added to Potassium monofluoride synthesis reactor, open and stir, at the uniform velocity add liquid potassium hydroxide according to 0.9-1.1 times of the required mole number of reaction, passing into the temperature that steam makes reaction solution remains on more than 110 DEG C, react to the pH value of reaction end be 7.5-8, reaction generate ammonia be absorbed as ammoniacal liquor through refrigeration cycle, be stored in basin, for desiliconization for subsequent use;
4) reaction liquid is added to transfer tank, precipitation 24h, the mass percentage concentration that clear liquid adds concentration kettle to be concentrated into solution in still reaches 48%-50%;
5) the Potassium monofluoride mother liquor after concentrated is added to groove to be painted, then squeeze into spray-drying tower by groove to be painted and spray and be dried, finished product is anhydrous potassium fluoride.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107940900A (en) * | 2017-10-12 | 2018-04-20 | 浙江工业大学 | The multilevel drying method and drying device of a kind of potassium fluoride in high activity |
| CN108675310A (en) * | 2018-07-24 | 2018-10-19 | 衢州市鼎盛化工科技有限公司 | The method for preparing ultrapure quartz sand as raw material using fluosilicic acid |
| CN110526262A (en) * | 2019-09-12 | 2019-12-03 | 内蒙古星汉氟都化工有限公司 | A kind of production line of automated production potassium fluoride |
| CN113233476A (en) * | 2021-05-14 | 2021-08-10 | 江西渠成氟化学有限公司 | Method for preparing potassium fluoride and sodium fluoride |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101049946A (en) * | 2007-05-15 | 2007-10-10 | 云南云天化国际化工股份有限公司 | Method for preparing potassium fluoride in high purity |
| CN101376509A (en) * | 2007-08-31 | 2009-03-04 | 多氟多化工股份有限公司 | Method for preparing potassium fluoride |
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| US608087A (en) * | 1898-07-26 | John-watkins | ||
| GB9300956D0 (en) * | 1993-01-19 | 1993-03-10 | British Nuclear Fuels Plc | Dehydration of mixtures |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101049946A (en) * | 2007-05-15 | 2007-10-10 | 云南云天化国际化工股份有限公司 | Method for preparing potassium fluoride in high purity |
| CN101376509A (en) * | 2007-08-31 | 2009-03-04 | 多氟多化工股份有限公司 | Method for preparing potassium fluoride |
Non-Patent Citations (2)
| Title |
|---|
| "氟化钾的制备工艺进展";于剑昆;《无机盐工业》;20100131;第42卷(第1期);第5-8页 * |
| 于剑昆."氟化钾的制备工艺进展".《无机盐工业》.2010,第42卷(第1期),第5-8页. |
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Application publication date: 20130123 Assignee: JIANGXI QUCHENG CHEMICAL Co.,Ltd. Assignor: Zhang Junhang Contract record no.: 2015360000067 Denomination of invention: Production technique of potassium fluoride Granted publication date: 20140730 License type: Exclusive License Record date: 20150603 |
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Effective date of registration: 20170210 Address after: 344800 Jiangxi city of Fuzhou province Jinxi County Industrial Park C District Patentee after: JIANGXI QUCHENG CHEMICAL Co.,Ltd. Address before: 322118 Jinhua City, Dongyang Province, Hengdian Town, Jing Jing community Jing Jing, No. 156 Patentee before: Zhang Junhang |
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