阅读说明：本技术 一种含高碳氯氟化钾盐联产氟化钾的工艺方法 (Process method for co-production of potassium fluoride from high-carbon potassium chlorofluoride ) 是由 严永生 于 2020-12-07 设计创作，主要内容包括：本发明公开了一种含高碳氯氟化钾盐联产氟化钾的工艺方法,其中将含有机物含量高的氟化钾和氯化钾通过多道工艺分离,提纯,干燥成氟化钾和氯化氨等物质。消耗氟硅酸,副产二氧化硅。(The invention discloses a process method for co-producing potassium fluoride from high-carbon fluorine-containing potassium chloride, wherein potassium fluoride and potassium chloride with high organic content are separated, purified and dried into potassium fluoride, ammonia chloride and other substances through multiple processes. Consumption of fluosilicic acid and by-production of silicon dioxide.)

1. A process method for co-producing potassium fluoride from high-carbon potassium chlorofluoride is characterized by comprising the following steps: it comprises the following steps:

firstly, dissolving: dissolving potassium fluoride and potassium chloride by adding water, separating potassium fluoride and potassium chloride by a centrifugal pump, adsorbing potassium chloride solid dissolved in water by activated carbon, then feeding the potassium fluoride mother liquor into an intermediate tank, evaporating and crystallizing the potassium fluoride mother liquor, centrifuging crystal slurry, dissolving crystals in the next step, and feeding the centrifuged mother liquor into a mother liquor tank;

the method comprises the following steps of: introducing hydrofluoric acid and potassium chloride into a cation exchange resin column, combining potassium ions and fluorine ions into potassium fluoride, combining hydrogen ions and chlorine ions into a hydrochloric acid solution, and dissolving the potassium fluoride solution and potassium fluoride crystals in a dissolving kettle;

carrying out reaction on the fluosilicic acid: reacting fluosilicic acid with liquid ammonia and water, pressing by a plate, wherein the filtrate is ammonium fluoride, the filter residue is silicon dioxide, and after the ammonium fluoride is settled, the supernatant passes through a precision filter and then is put into an intermediate tank;

fourthly, reacting ammonium chloride: after the ammonium fluoride and the hydrochloric acid are introduced into the ion exchange column to react, ammonium chloride and hydrofluoric acid are generated, the hydrofluoric acid participates in the regeneration process of the second part of potassium fluoride to react, and the ammonium chloride enters an evaporator to be evaporated and concentrated;

fifthly, concentrating potassium fluoride: concentrating the potassium fluoride generated in the second step into potassium fluoride concentrated solution through electrodialysis, preserving the heat of the heat preservation kettle, and drying the potassium fluoride in a spray tower;

sixthly, cyclone separation and packaging: carrying the spray-dried potassium fluoride into a material bag through material conveying, weighing and packaging;

and evaporating ammonium chloride through an evaporator, centrifuging, and drying and separating ammonium chloride solid into ammonium chloride solid through a spray tower.

2. The process for co-producing potassium fluoride and recovering potassium chloride from high-carbon potassium fluoride-containing salt as claimed in claim 1, which is characterized in that: the resin adopts cation exchange resin, potassium chloride and hydrofluoric acid take part in reaction at the resin end to generate two materials of potassium fluoride and hydrochloric acid, wherein the hydrochloric acid takes part in the reaction of ammonium fluoride.

3. The process for co-production of potassium fluoride from high-carbon chlorofluorocarbon potassium salt as claimed in claim 1, wherein said process comprises the steps of: the method is characterized in that: in the ammonium chloride reaction process, the resin adopts cation exchange resin, the ammonium fluoride and the hydrochloric acid are reacted at the resin end to generate two materials of ammonium chloride and hydrofluoric acid, wherein the hydrofluoric acid is reacted with the regeneration of the potassium fluoride.

4. The process for co-production of potassium fluoride from high-carbon chlorofluorocarbon potassium salt as claimed in claim 1, wherein said process comprises the steps of: the potassium chloride concentration adopts an electrodialysis concentration or falling film evaporation process, and the electrodialysis adopts single set or multiple sets of electrodialysis to concentrate the beryllium-containing solution singly or in series or in parallel.

Technical Field

The invention relates to a process method for co-producing potassium fluoride from high-carbon chlorofluorocarbon potassium salt, belonging to the field of fine chemicals.

Background

Potassium fluosilicate belongs to a byproduct in a hydrofluoric acid process, and is also called silicofluoric acid. The anhydrous substance is colorless gas, is unstable, and is easily decomposed into silicon tetrafluoride and hydrogen fluoride. The water solution is colorless and shows strong acid reaction. Is corrosive and can attack glass. Storing in wax or plastic container. The concentrated solution, when cooled, precipitated crystals of colorless dihydrate, melting point 19 ℃. The fluosilicic acid has the disinfection performance. Used for preparing fluorine silicate and cryolite, and used for electroplating, beer disinfection, wood preservation and the like. Is prepared by dissolving silicon dioxide in hydrofluoric acid or mixing quartz powder, calcium fluoride and concentrated sulfuric acid and then heating. Can also be obtained by absorbing silicon tetrafluoride gas escaped from phosphate rock decomposition in a phosphate fertilizer plant by water.

It is conventional practice to produce sodium or potassium fluorosilicates by neutralization with potassium hydroxide and sodium hydroxide. The potassium fluosilicate or the sodium fluosilicate has low economic value. The traditional method for producing potassium fluoride mostly adopts a potassium hydroxide-hydrofluoric acid neutralization method to react, hydrofluoric acid in the traditional process is mainly prepared by reacting fluorite and sulfuric acid, precious resources of fluorite are consumed in the traditional process, and the cost of the hydrofluoric acid is quite high. The combined preparation method is adopted, so that the content of organic carbon in potassium fluoride is greatly reduced. The economic benefit is improved.

Disclosure of Invention

The invention aims to solve the technical problem that the existing potassium fluoride process with high organic carbon content adopts multiple purification means to solve the problem of high organic carbon content.

In order to solve the technical problems, the invention adopts the following technical scheme:

a process method for co-producing potassium fluoride from high-carbon potassium chlorofluoride comprises the following steps: it comprises the following steps:

firstly, dissolving: dissolving potassium fluoride and potassium chloride by adding water, separating potassium fluoride and potassium chloride by a centrifugal pump, adsorbing potassium chloride solid dissolved in water by activated carbon, then feeding the potassium fluoride mother liquor into an intermediate tank, evaporating and crystallizing the potassium fluoride mother liquor, centrifuging crystal slurry, dissolving crystals in the next step, and feeding the centrifuged mother liquor into a mother liquor tank;

secondly, regenerating potassium fluoride: introducing hydrofluoric acid and potassium chloride into a cation exchange resin column, combining potassium ions and fluorine ions into potassium fluoride, combining hydrogen ions and chlorine ions into a hydrochloric acid solution, and dissolving the potassium fluoride solution and potassium fluoride crystals in a dissolving kettle;

thirdly, fluosilicic acid reaction: reacting fluosilicic acid with liquid ammonia and water, pressing by a plate, wherein the filtrate is ammonium fluoride, the filter residue is silicon dioxide, and after the ammonium fluoride is settled, the supernatant passes through a precision filter and then is put into an intermediate tank;

fourthly, ammonium chloride reaction: after the ammonium fluoride and the hydrochloric acid are introduced into the ion exchange column to react, ammonium chloride and hydrofluoric acid are generated, the hydrofluoric acid participates in the regeneration process of the second part of potassium fluoride to react, and the ammonium chloride enters an evaporator to be evaporated and concentrated;

fifthly, concentrating potassium fluoride: concentrating the potassium fluoride generated in the second step into potassium fluoride concentrated solution through electrodialysis, preserving the heat of the heat preservation kettle, and drying the potassium fluoride in a spray tower;

sixth, cyclone separation and packaging: carrying the spray-dried potassium fluoride into a material bag through material conveying, weighing and packaging;

and seventhly, evaporating the ammonium chloride through an evaporator, centrifuging, and drying and separating the ammonium chloride solid into the ammonium chloride solid through a spray tower.

According to the process method for recovering potassium chloride by co-producing potassium fluoride from high-carbon potassium fluoride salt, cation exchange resin is adopted as resin, potassium chloride and hydrofluoric acid are reacted at the resin end to generate two materials of potassium fluoride and hydrochloric acid, wherein the hydrochloric acid is reacted with ammonium fluoride.

In the process of ammonium chloride reaction, the resin adopts cation exchange resin, and ammonium fluoride and hydrochloric acid which are materials participate in reaction at the resin end to generate two materials, namely ammonium chloride and hydrofluoric acid, wherein the hydrofluoric acid participates in the regeneration reaction of the potassium fluoride.

The potassium chloride concentration adopts an electrodialysis concentration or falling film evaporation process, and the electrodialysis adopts single or multiple electrodialysis to concentrate the beryllium-containing solution singly or in series or in parallel.

Detailed Description

Example 1:

the process method for recovering potassium chloride by co-producing potassium fluoride from high-carbon fluorine-containing potassium salt comprises the following steps: it comprises the following steps:

firstly, dissolving: dissolving a mixture of potassium fluoride and potassium chloride by adding water, separating the potassium fluoride from the potassium chloride by a centrifugal pump, adsorbing potassium chloride solid dissolved in water by activated carbon, then feeding the potassium fluoride solid into an intermediate tank, evaporating potassium fluoride mother liquor, crystallizing, centrifuging crystal slurry, dissolving the crystal in the next step, and feeding the centrifuged mother liquor into a mother liquor tank;

secondly, regenerating potassium fluoride: introducing hydrofluoric acid and potassium chloride into a cation exchange resin column, combining potassium ions and fluorine ions into potassium fluoride, and combining hydrogen ions and chlorine ions into a hydrochloric acid solution. Dissolving the potassium fluoride solution and the potassium fluoride crystal in a dissolving kettle;

thirdly, fluosilicic acid reaction: reacting fluosilicic acid with liquid ammonia and water, pressing by a plate, wherein the filtrate is ammonium fluoride, the filter residue is silicon dioxide, and after the ammonium fluoride is settled, the supernatant passes through a precision filter and then is put into an intermediate tank;

fourthly, ammonium chloride reaction: after the ammonium fluoride and the hydrochloric acid are introduced into the ion exchange column to react, ammonium chloride and hydrofluoric acid are generated, the hydrofluoric acid participates in the regeneration process of the second part of potassium fluoride to react, and the ammonium chloride enters an evaporator to be evaporated and concentrated;

fifthly, concentrating potassium fluoride: concentrating the potassium fluoride generated in the second step into potassium fluoride concentrated solution through electrodialysis, preserving the heat of the heat preservation kettle, and drying the potassium fluoride in a spray tower;

sixth, cyclone separation and packaging: carrying the spray-dried potassium fluoride into a material bag through material conveying, weighing and packaging;

and seventhly, evaporating the ammonium chloride through an evaporator, centrifuging, and drying and separating the ammonium chloride solid into the ammonium chloride solid through a spray tower.

The resin adopts cation exchange resin, potassium chloride and hydrofluoric acid take part in reaction at the resin end to generate two materials of potassium fluoride and hydrochloric acid, wherein the hydrochloric acid takes part in the reaction of ammonium fluoride.

In the ammonium fluoride reaction process, the resin adopts cation exchange resin, the ammonium fluoride and the hydrochloric acid are reacted at the resin end to generate two materials, namely ammonium chloride and hydrofluoric acid, wherein the hydrofluoric acid is reacted with the regeneration of the potassium fluoride.

And the potassium chloride is concentrated by adopting electrodialysis, and the electrodialysis adopts single or multiple sets of electrodialysis to be used alone or in series or parallel connection for concentrating the beryllium-containing solution.