CN112174168A - Method for preparing high-purity potassium fluoride by reacting potassium water glass with fluosilicic acid or potassium fluosilicate - Google Patents
Method for preparing high-purity potassium fluoride by reacting potassium water glass with fluosilicic acid or potassium fluosilicate Download PDFInfo
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- CN112174168A CN112174168A CN202011131341.4A CN202011131341A CN112174168A CN 112174168 A CN112174168 A CN 112174168A CN 202011131341 A CN202011131341 A CN 202011131341A CN 112174168 A CN112174168 A CN 112174168A
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- 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
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- 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
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- 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
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Abstract
The invention discloses a method for preparing high-purity potassium fluoride by reacting potassium water glass with fluosilicic acid or potassium fluosilicate. Adding water into a reaction kettle, adding part or all of fluosilicic acid or potassium fluosilicate while stirring, and preparing slurry with the water; heating to 40-70 ℃, adding part of potash water glass into the slurry, and taking the silicon dioxide particles separated out by reaction as seed crystals for separating out silicon dioxide by subsequent reaction; then continuously heating to 75-95 ℃, and simultaneously adding the rest fluosilicic acid or potassium fluosilicate and potassium water glass into the slurry at a constant speed to complete the alkaline hydrolysis reaction; carrying out solid-liquid separation on the reaction liquid, and washing and drying the solid to obtain white carbon black; concentrating and spray drying the treated potassium fluoride solution to prepare anhydrous potassium fluoride. According to the method, potassium silicate is used for replacing potassium hydroxide in the process of preparing potassium fluoride, so that the negative influence of potassium hydroxide on precipitated silica particles in the alkaline hydrolysis process is avoided, high-quality potassium fluoride and white carbon black products are obtained, and the production cost is reduced.
Description
Technical Field
The invention relates to a method for preparing high-purity potassium fluoride, in particular to a method for preparing high-purity potassium fluoride by reacting potassium silicate with fluosilicic acid or potassium fluosilicate, belonging to the technical field of chemical industry.
Background
Potassium fluoride is an important inorganic fluorine compound and is widely applied to glass engraving, food corrosion prevention, electroplating, preparation of potassium bifluoride and the like; the flux is mainly used as a fluxing agent for welding various alloys or metals in the field of welding, as a fluorinating agent in the field of organic compound generation, as an absorbent for absorbing hydrogen fluoride and moisture, for producing sodium fluoroacetate and fluoroacetamide insecticides in the field of pesticides, and for preparing norfloxacin and the like in the field of medicines. The traditional production method of potassium fluoride is to take hydrofluoric acid as raw material to react with potassium hydroxide or take potassium fluosilicate to react with potassium hydroxide to prepare the potassium fluoride.
The potassium hydroxide solution reacts very readily with the silica and can even attack the glass. When potassium hydroxide is used in the reaction with fluorosilicic acid or potassium fluorosilicate, it is desirable that the silica gel nuclei formed in the initial stage of the reaction be able to serve as seed crystals for the subsequent precipitation of silica in order to produce high-quality white carbon. However, in practice, the potassium hydroxide solution added rapidly eats the silica seeds formed by the reaction, and the following side reactions occur:
2KOH+nSiO2→K2O·nSiO2+H2O (1)
this side reaction makes the silica particles precipitated by the alkaline hydrolysis reaction in an extremely unstable state, and cannot form stable silica seed crystals at the initial stage of the reaction, and further causes the silica particles precipitated by the subsequent reaction to be unable to form uniform aggregate precipitates, and thus high-quality white carbon black cannot be obtained. This has become a technical obstacle to the current process for preparing high quality white carbon black by-product.
Chinese patent document CN101049946 discloses a preparation method of high-purity potassium fluoride, which is to prepare a potassium fluoride aqueous solution by a neutralization method of hydrofluoric acid and potassium hydroxide, control the reaction end point pH and the reaction solution concentration, then settle the reaction solution, and induce crystallization to obtain the product potassium fluoride. The potassium fluoride prepared by the method has high purity, simple process flow and easy operation, but has high production cost, high price and lacks of market competitiveness.
In recent years, in order to reduce the production cost, the main process for preparing potassium fluoride by reacting potassium hydroxide with fluosilicic acid or potassium fluosilicate as a raw material, and chinese patent document CN103991882B discloses a suspension prepared by mixing potassium fluosilicate with water, and reacting the suspension with a potassium hydroxide aqueous solution. As fluosilicic acid and potassium fluosilicate are industrial byproducts, the cost is greatly reduced compared with that of hydrofluoric acid used as a fluorine source, and the byproduct white carbon black can be obtained. However, when the fluorosilicic acid or potassium fluorosilicate and potassium hydroxide are subjected to alkaline hydrolysis reaction, the reaction is not easy to control due to the excessively strong alkalinity of the potassium hydroxide, and silicon dioxide formed in the alkaline hydrolysis process is very easy to dissolve, so that the quality of the white carbon black is unstable. At present, manufacturers adopting the method to prepare potassium fluoride generally have the technical problem that high-quality white carbon black is difficult to recover.
Chinese patent document CN103112873B discloses a method for preparing potassium fluoride and white carbon black by ammonolysis of potassium fluosilicate with ammonia water and then by reaction of potassium hydroxide and ammonium fluoride. The method adopts a two-step reaction mode, wherein in the first step, ammonia water with weak basicity is used for ammonolysis to prepare white carbon black with good quality, then a potassium hydroxide solution is added into an ammonium fluoride solution to prepare potassium fluoride, and escaped ammonia is recovered. The process has the advantages of complex steps, more working procedures, and the need of using and recycling ammonia water, easily causes the problem of large production environment odor, is not beneficial to actual production and pollutes the environment.
In order to overcome the technical problem of the prior art, the invention provides a method for preparing potassium fluoride by using potassium water glass to replace strong alkali potassium hydroxide for alkaline hydrolysis reaction.
Disclosure of Invention
The invention aims to provide a method for preparing potassium fluoride by carrying out alkaline hydrolysis reaction on potassium silicate instead of strong alkali potassium hydroxide and fluosilicic acid or potassium fluosilicate. The method for preparing high-purity potassium fluoride and simultaneously producing high-quality white carbon black as a byproduct overcomes the defects of the prior art, can prepare high-quality white carbon black while producing potassium fluoride, avoids harmful gas escaping in the production process, and protects the environment.
In order to achieve the aim, the invention provides a method for preparing high-purity potassium fluoride by reacting potash water glass with fluosilicic acid or potassium fluosilicate, which mainly comprises the following steps:
A. adding water into a reaction kettle, adding part or all of fluosilicic acid or potassium fluosilicate while stirring, and preparing slurry with water;
B. heating to 40-70 ℃, adding part of potassium water glass into the slurry to generate silicon dioxide crystal seeds for subsequent reaction;
C. continuously heating to 75-95 ℃, and simultaneously adding the rest fluosilicic acid or potassium fluosilicate and potassium water glass into the slurry at a constant speed to complete the alkaline hydrolysis reaction;
D. carrying out solid-liquid separation on the reaction liquid, and washing and drying the solid to obtain white carbon black;
E. concentrating and spray drying the treated potassium fluoride solution to prepare anhydrous potassium fluoride.
Preferably, the modulus of the potash water glass is 1-2.
Preferably, the proportion of the added fluosilicic acid or potassium fluosilicate in the step A is 40-50%.
Preferably, the proportion of the potassium added water glass in the step B is 20-50%.
Preferably, the reaction temperature in the step B is 45-60 ℃.
Preferably, the reaction temperature in the step C is 80-90 degrees.
Preferably, the proportion of adding the fluosilicic acid or the potassium fluosilicate in the step A is 20 to 100 percent.
Preferably, the proportion of the potassium water glass added in the step B is 10-50%.
The invention uses potash water glass and fluosilicic acid or potassium fluosilicate to carry out alkaline hydrolysis reaction, the wet process potash water glass is from the reaction of potassium hydroxide and silicon dioxide, that is, hydroxide ions which can rapidly react with silicon dioxide particles are consumed most and have weak alkalinity in the process of the preparation reaction of the potash water glass. When the potash water glass and the fluosilicic acid or the potassium fluosilicate are used for carrying out the alkaline hydrolysis reaction, the reaction of the potash water glass and the silicon dioxide precipitated in the alkaline hydrolysis process is difficult to carry out, so that ideal silicon dioxide seed crystals obtained in the initial reaction stage can be reserved, and the growth of the silicon dioxide aggregates precipitated in the subsequent alkaline hydrolysis reaction can be in a controllable state. Thereby preparing high-quality white carbon black by-product while preparing high-purity potassium fluoride. The invention relates to a reaction formula:
H2SiF6+3K2O·nSiO2→6KF+(3n+1)SiO2+H2O (2)
K2SiF6+2K2O·nSiO2→6KF+(2n+1)SiO2 (3)
the potassium hydroxide is strong in basicity, so that the added potassium hydroxide solution is easy to rapidly generate side reaction with precipitated silicon dioxide, and particularly, a crystal seed stage is formed at the initial reaction stage, so that the quality of the white carbon black is greatly influenced.
Potassium silicate with certain concentration exists in the water glass instead of potassium hydroxide, so that side reaction is difficult to occur between the alkali hydrolysis process and the precipitated silicon dioxide, and the ordered growth of particles in the precipitation process of the silicon dioxide in the alkali hydrolysis process is ensured. The alkaline hydrolysis reaction is carried out step by step, the reaction temperature of the first step is 40-70 ℃, and the reaction temperature of the second step is 75-95 ℃. The technical measures ensure the quality of the potassium fluoride and improve the quality of the byproduct white carbon black. In addition, potassium silicate glass is used as a raw material, so that the yield of the white carbon black byproduct in a single kettle is greatly increased while the same amount of potassium fluoride product is obtained, the yield can be increased by more than 2 times, and the production cost of the white carbon black product is further reduced.
Compared with ammonolysis process, the invention avoids the escape of harmful gas in the production process, is beneficial to the production operation and protects the environment.
The modulus of the potash water glass used in the invention is 0.5-2.5, and the silicon dioxide contained in the potash water glass is simultaneously separated out with the silicon dioxide in the fluosilicic acid or the potassium fluosilicate when the alkaline hydrolysis reaction (1) or (2) is carried out, so that the yield of the white carbon black byproduct in a single kettle is greatly improved while the same amount of potassium fluoride product is obtained, the yield of the white carbon black byproduct in the single kettle can be improved by more than 2 times according to different moduli of the potash water glass, and the production cost of the silicon dioxide can be further reduced. The potassium water glass can be conveniently prepared by using potassium hydroxide and industrial byproduct active silica gel through wet reaction, and the industrial byproduct silicon resource is comprehensively utilized.
The technical difficulty of the traditional process is desiliconization and white carbon black recovery in the alkaline hydrolysis process, and the invention solves the technical problem of white carbon black recovery in the industry by introducing more silicon in the alkaline hydrolysis process in the key and creative technical scheme, and breaks through the traditional concept. Is more novel and creative.
Detailed Description
Adding water into a reaction kettle, adding part or all of fluosilicic acid or potassium fluosilicate while stirring, and preparing slurry with water; heating to 40-70 ℃, adding part of potash water glass into the slurry, and taking the silicon dioxide particles separated out by reaction as seed crystals for separating out silicon dioxide by subsequent reaction; continuously heating to 75-95 ℃, and simultaneously adding the rest fluosilicic acid or potassium fluosilicate and potassium water glass into the slurry at a constant speed to complete the alkaline hydrolysis reaction; carrying out solid-liquid separation on the reaction liquid, and washing and drying the solid to obtain white carbon black; concentrating and spray drying the treated potassium fluoride solution to prepare anhydrous potassium fluoride.
The following examples further illustrate the invention.
Example 1
A method for preparing high-purity potassium fluoride comprises the following raw materials in parts by weight:
0kg of water, 321kg of fluosilicic acid with the concentration of 40 percent and 1675kg of 25 percent potassium water glass (15 percent of potassium oxide and 10 percent of silicon dioxide).
Adding 50% of all fluosilicic acid into a reaction kettle under stirring;
heating to 50 ℃, and adding 40% potassium water glass into the slurry;
continuously heating to 85 ℃, and simultaneously adding the rest fluosilicic acid and the potassium water glass into the slurry at a constant speed to complete the alkaline hydrolysis reaction;
carrying out solid-liquid separation on the reaction liquid, washing and drying the solid to obtain the white carbon black with the specific surface area of 150m2/g；
Concentrating and spray drying the treated potassium fluoride solution to prepare anhydrous potassium fluoride.
221kg of white carbon black and 310kg of potassium fluoride are prepared through reaction, and the purity of the potassium fluoride is 99.4%.
Example 2
A method for preparing high-purity potassium fluoride comprises the following raw materials in parts by weight:
233kg of water, 200kg of 98 percent potassium fluosilicate and 1117kg of 25 percent potassium water glass (15 percent of potassium oxide and 10 percent of silicon dioxide).
Adding 233kg of water into a reaction kettle, adding 50% of potassium fluosilicate while stirring, and preparing slurry with the water;
heating to 50 ℃, and adding 25% of potassium water glass into the slurry;
continuously heating to 85 ℃, and simultaneously adding the rest fluosilicic acid and the potassium water glass into the slurry at a constant speed to complete the alkaline hydrolysis reaction;
carrying out solid-liquid separation on the reaction liquid, washing and drying the solid to obtain the white carbon black with the specific surface area of 140m2/g；
Concentrating and spray drying the treated potassium fluoride solution to prepare anhydrous potassium fluoride.
165.2kg of white carbon black, 311kg of potassium fluoride and 99.35% of potassium fluoride are prepared by reaction.
Comparative example 1
A method for preparing high-purity potassium fluoride comprises the following raw materials by weight:
934kg of water, 200kg of 98% potassium fluosilicate and 416kg of 48% potassium hydroxide.
Adding 233kg of water into a reaction kettle, adding 200kg of potassium fluosilicate while stirring, and preparing slurry with the water;
heating to 85 ℃, and adding 416kg of potassium hydroxide with the concentration of 48% into the slurry at a constant speed to complete the alkaline hydrolysis reaction.
Carrying out solid-liquid separation on the reaction liquid, washing and drying the solid to obtain the white carbon black with the specific surface area of 80m2/g
Concentrating and spray drying the treated potassium fluoride solution to prepare anhydrous potassium fluoride.
53.5kg of white carbon black, 316kg of potassium fluoride and 99.5% of potassium fluoride are prepared by reaction.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements can be made to the technical solution of the present invention by those skilled in the art without departing from the spirit of the present invention, and the technical solution of the present invention is defined by the claims.
Claims (6)
1. A method for preparing high-purity potassium fluoride is characterized in that potash water glass is used for replacing strong alkali potassium hydroxide to carry out alkaline hydrolysis reaction with fluosilicic acid or potassium fluosilicate, and comprises the following steps:
A. adding water into a reaction kettle, adding part or all of fluosilicic acid or potassium fluosilicate while stirring, and preparing slurry with water;
B. heating to 40-70 ℃, adding part of potash water glass into the slurry, and taking the silicon dioxide particles separated out by reaction as seed crystals for separating out silicon dioxide by subsequent reaction;
C. continuously heating to 75-95 ℃, and simultaneously adding the rest fluosilicic acid or potassium fluosilicate and potassium water glass into the slurry at a constant speed to complete the alkaline hydrolysis reaction;
D. carrying out solid-liquid separation on the reaction liquid, and washing and drying the solid to obtain white carbon black;
E. concentrating and spray drying the treated potassium fluoride solution to prepare anhydrous potassium fluoride.
2. The method for preparing highly pure potassium fluoride according to claim 1, wherein the potash water glass has a modulus of 0.5 to 2.5.
3. The process for producing high-purity potassium fluoride according to claim 1, wherein the alkaline hydrolysis reaction of potassium waterglass with fluorosilicic acid or potassium fluorosilicate is carried out in two stages. The reaction temperature in the first stage of step B is preferably 45-60 ℃.
4. The method for preparing highly pure potassium fluoride according to claim 1, wherein the reaction temperature in the second stage of the step C is preferably 80 to 90 ℃.
5. The method for preparing high-purity potassium fluoride according to claim 1, wherein the proportion of the fluorosilicic acid or potassium fluorosilicate added in step A is 20% to 100%.
6. The method for preparing high-purity potassium fluoride according to claim 1, wherein the potassium silicate is added in the step B in a proportion of 10% to 50%.
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Cited By (1)
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| CN116119684A (en) * | 2022-12-30 | 2023-05-16 | 承德莹科精细化工股份有限公司 | Preparation method of high-purity low-carbon crystalline potassium fluoride |
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