CN108033465A - A kind of preparation method of anhydrous potassium fluoride - Google Patents
A kind of preparation method of anhydrous potassium fluoride Download PDFInfo
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- CN108033465A CN108033465A CN201711341345.3A CN201711341345A CN108033465A CN 108033465 A CN108033465 A CN 108033465A CN 201711341345 A CN201711341345 A CN 201711341345A CN 108033465 A CN108033465 A CN 108033465A
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- potassium fluoride
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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
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
- C01F11/462—Sulfates of Sr or Ba
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Abstract
The present invention provides a kind of preparation method of anhydrous potassium fluoride, react to form first order reaction liquid including the thick liquid of fluosilicic acid and ammonium hydroxide, the first order reaction liquid is subjected to separation of solid and liquid and forms solid silica and second order reaction liquid, the second order reaction liquid reacts to form third-order reaction liquid with barium hydroxide, the third-order reaction liquid and potassium hydroxide are reacted, it is passed through high-temperature steam heating, stirring, obtain potassium fluoride clear liquid and ammonia, the potassium fluoride clear liquid is concentrated to form potassium fluoride mother liquor, the potassium fluoride mother liquor is passed through in spray drying tower and carries out spray drying and forms anhydrous potassium fluoride, the thick liquid of fluosilicic acid is the accessory substance on anhydrous hydrogen fluoride production line, its component includes fluosilicic acid, a small amount of sulfuric acid and a small amount of hydrofluoric acid.The present invention replaces anhydrous hydrofluoric acid by the thick liquid of fluosilicic acid, not only reduces cost of material, while can solve the comprehensive utilization of the thick liquid of fluosilicic acid, and coproduction silica and barium sulfate, improve economic benefit while the present invention produces anhydrous potassium fluoride.
Description
Technical field
The present invention relates to anhydrous potassium fluoride preparation method applied technical field, more particularly to a kind of system of anhydrous potassium fluoride
Preparation Method.
Background technology
Potassium fluoride is a kind of salt, is called the fluoride salt of potassium, it is white monoclinic crystal or crystalline powder, and taste is salty, easily inhales
It is wet, it is dissolved in water and does not dissolve in ethanol.Its aqueous solution usually can be used as various glass in alkalescence, energy etching glass and porcelain
Etching, welding fluxing agent, timber preservative, agricultural fungicides, pesticide intermediate, pharmaceuticals industry raw material and organic fluoride are former
Material, has the function that indispensable in building, chemical industry, agricultural.
In the prior art, during anhydrous potassium fluoride is produced, the hydrofluoric acid commonly using high-purity is raw material, production
Cost is higher, causes the productivity effect of enterprise low.
The content of the invention
Based on this, the object of the present invention is to provide a kind of preparation side for the anhydrous potassium fluoride that can save raw materials for production cost
Method.
A kind of preparation method of anhydrous potassium fluoride, the preparation method include the following steps：
Step S1, successively squeezes into the thick liquid of a certain amount of fluosilicic acid and ammonium hydroxide in the first reaction kettle, and stirring, it is anti-to form level-one
Answer liquid；
Step S2, carries out separation of solid and liquid by the first order reaction liquid, obtains solid silica and second order reaction liquid, lead to
Cross clear water and the solid silica is subjected to mashing cleaning, obtain high-purity silicon dioxide；
Step S3, the second order reaction liquid is squeezed into the second reaction kettle, adds a certain amount of barium hydroxide solution,
By stirring, precipitating, third-order reaction liquid is obtained；
Step S4, successively adds the third-order reaction liquid and a certain amount of potassium hydroxide solution in the 3rd reaction kettle, leads to
Enter high-temperature steam heating, stirring obtains potassium fluoride clear liquid and ammonia, and the potassium fluoride clear liquid forms fluorination by precipitation, concentration
Potassium mother liquor；
Step S5, the potassium fluoride mother liquor is squeezed into spray drying tower and is spray-dried, and forms anhydrous potassium fluoride.
Compared to the prior art, the present invention replaces anhydrous hydrofluoric acid by the thick liquid of fluosilicic acid, not only reduces cost of material,
The comprehensive utilization of the thick liquid of fluosilicic acid can be solved at the same time；By carrying out solid-liquid to first reaction solution and the 3rd reaction solution
Separation solid obtained solid silica and solid sulphuric acid barium, then by clear water be beaten made of high-purity silica
And barium sulfate, the present invention is produced anhydrous potassium fluoride, at the same can coproduction silica and barium sulfate, improve through
Ji benefit.
Further, the thick liquid of the fluosilicic acid is the accessory substance on anhydrous hydrogen fluoride production line, its concentration for 20%~
45%, its component includes silicate fluoride solution, a small amount of sulfuric acid solution and a small amount of hydrofluoric acid solution.
Further, the first order reaction liquid includes ammonium hydrogen fluoride solution, precipitation of silica and ammonium sulfate, its
PH value is 8.5~9.
Further, the second order reaction liquid includes ammonium hydrogen fluoride solution and ammonium sulfate, the third-order reaction liquid
Including barium sulfate precipitate, ammonium hydrogen fluoride solution and ammonium hydroxide.
Further, in the step S3, add the sedimentation time after the barium hydroxide solution for 20h~
30h；In the step S4, sedimentation time of the potassium fluoride clear liquid is 20h~30h, the pH value of the potassium fluoride mother liquor is
7.5~8.5.
Further, the ammonia forms ammonium hydroxide by cooling recirculation system and is stored in storage tank, for described in repetition
The operation of step S1, the concentration of the ammonium hydroxide is 25%~29%.
Further, when the concentration of the thick liquid of the fluosilicic acid is 35%, the concentration of first ammonium hydroxide is 25%, weight
For 1.05 times of the concentration of the thick liquid of the fluosilicic acid, the weight of the barium hydroxide solution is the 90% of theoretical value, described
The weight of potassium hydroxide solution is 1.1 times of theoretical value.
Further, when the concentration of the thick liquid of the fluosilicic acid is 20%, the concentration of first ammonium hydroxide is 29%, weight
For 1.05 times of the concentration of the thick liquid of the fluosilicic acid, the weight of the barium hydroxide solution is the 90% of theoretical value, described
The weight of potassium hydroxide solution is 1.05 times of theoretical value..
Further, when the concentration of the thick liquid of the fluosilicic acid is 25%, the concentration of first ammonium hydroxide is 27%, weight
For 1.1 times of the concentration of the thick liquid of the fluosilicic acid, the weight of the barium hydroxide solution is the 99% of theoretical value, the hydrogen
The weight of potassium oxide solution is 1.1 times of theoretical value.
Further, when the concentration of the thick liquid of the fluosilicic acid is 45%, the concentration of first ammonium hydroxide is 25%, weight
For 1.1 times of the concentration of the thick liquid of the fluosilicic acid, the weight of the barium hydroxide solution is the 93% of theoretical value, the hydrogen
The weight of potassium oxide solution is 1.1 times of theoretical value..
Brief description of the drawings
Fig. 1 is the process flow chart of an embodiment in the present invention.
Following embodiment will combine above-mentioned attached drawing and further illustrate the present invention.
Embodiment
For the ease of understanding the present invention, the present invention is described more fully below with reference to relevant drawings.In attached drawing
Give some embodiments of the present invention.But the present invention can realize in many different forms, however it is not limited to this paper institutes
The embodiment of description.On the contrary, the purpose for providing these embodiments is made to the disclosure more thorough and comprehensive.
It should be noted that when element is referred to as " being fixedly arranged on " another element, it can be directly on another element
Or there may also be element placed in the middle.When an element is considered as " connection " another element, it can be directly connected to
To another element or it may be simultaneously present centering elements.Term as used herein " vertical ", " horizontal ", " left side ",
" right side " and similar statement are for illustrative purposes only.
Unless otherwise defined, all of technologies and scientific terms used here by the article is with belonging to technical field of the invention
The normally understood implication of technical staff is identical.Term used in the description of the invention herein is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term as used herein " and/or " include one or more phases
The arbitrary and all combination of the Listed Items of pass.
Referring to Fig. 1, a kind of preparation method of the anhydrous potassium fluoride provided in one embodiment of the invention, the preparation method
Include the following steps：
Step S1, successively squeezes into the thick liquid of a certain amount of fluosilicic acid and ammonium hydroxide in the first reaction kettle, and stirring, it is anti-to form level-one
Answer liquid；
Step S2, carries out separation of solid and liquid by the first order reaction liquid, obtains solid silica and second order reaction liquid, lead to
Cross clear water and the solid silica is subjected to mashing cleaning, obtain high-purity silicon dioxide；
Step S3, the second order reaction liquid is squeezed into the second reaction kettle, adds a certain amount of barium hydroxide solution,
By stirring, precipitating, third-order reaction liquid is obtained, it is necessary to illustrate, when adding the precipitation after the barium hydroxide solution
Between be 20h~30h, further, add the sedimentation time most preferably 24h after the barium hydroxide solution；
Step S4, successively adds the third-order reaction liquid and a certain amount of potassium hydroxide solution in the 3rd reaction kettle, leads to
Enter high-temperature steam heating, stirring obtains potassium fluoride clear liquid and ammonia, and the potassium fluoride clear liquid forms fluorination by precipitation, concentration
Potassium mother liquor is, it is necessary to explanation, and sedimentation time of the potassium fluoride clear liquid is 20h~30h, the pH value of the potassium fluoride mother liquor is
7.5~8.5, further, the sedimentation time most preferably 24h of the potassium fluoride clear liquid, the pH value of the potassium fluoride mother liquor
Most preferably 8；
Step S5, the potassium fluoride mother liquor is squeezed into spray drying tower and is spray-dried, and forms anhydrous potassium fluoride.
Specifically, in the present embodiment, in the step S5, the temperature of the high-temperature steam is 110 DEG C.
It should be noted that the thick liquid of fluosilicic acid is the accessory substance on anhydrous hydrogen fluoride production line, its concentration is 20%
~45%, its component includes silicate fluoride solution, a small amount of sulfuric acid solution and a small amount of hydrofluoric acid solution.The first order reaction liquid includes
Ammonium hydrogen fluoride solution, precipitation of silica and ammonium sulfate, its pH value are 8.5~9.The second order reaction liquid includes fluorination
Hydrogen ammonium salt solution and ammonium sulfate.The third-order reaction liquid includes barium sulfate precipitate, ammonium hydrogen fluoride solution and ammonium hydroxide.It is described
Ammonia forms ammonium hydroxide by cooling recirculation system and is stored in storage tank, for the operation of repeating said steps S1, the ammonium hydroxide
Concentration be 25%~29%.
Specifically, in the present embodiment, it is to improve the hydrolysis degree of fluosilicic acid by the use of ammonium hydroxide as desiliconization agent, you can protect
The quality of high-purity silicon dioxide and the product quality of the anhydrous potassium fluoride are demonstrate,proved, also allows for making the ammonia inhale by the circulation
Receipts system, so as to reuse.It is to reduce cost of material, add to replace anhydrous hydrogen fluoride using the thick liquid of the fluosilicic acid
It is in order to remove the sulfuric acid that the thick liquid band of the fluosilicic acid is come, to improve the anhydrous potassium fluoride matter to enter the barium hydroxide
Amount, its addition are the 90-99% of theoretical amount.
It should be noted that when the concentration of the thick liquid of the fluosilicic acid is 35%, the concentration of first ammonium hydroxide is 25%,
Weight is 1.05 times of the concentration of the thick liquid of the fluosilicic acid, and the weight of the barium hydroxide solution is the 90% of theoretical value,
The weight of the potassium hydroxide solution is 1.1 times of theoretical value；
When the concentration of the thick liquid of the fluosilicic acid is 20%, the concentration of first ammonium hydroxide is 29%, weight is the fluorine
1.05 times of the concentration of the thick liquid of silicic acid, the weight of the barium hydroxide solution are the 90% of theoretical value, the potassium hydroxide
The weight of solution is 1.05 times of theoretical value；
When the concentration of the thick liquid of the fluosilicic acid is 25%, the concentration of first ammonium hydroxide is 27%, weight is the fluorine
1.1 times of the concentration of the thick liquid of silicic acid, the weight of the barium hydroxide solution are the 99% of theoretical value, and the potassium hydroxide is molten
The weight of liquid is 1.1 times of theoretical value；
When the concentration of the thick liquid of the fluosilicic acid is 45%, the concentration of first ammonium hydroxide is 25%, weight is the fluorine
1.1 times of the concentration of the thick liquid of silicic acid, the weight of the barium hydroxide solution are the 93% of theoretical value, and the potassium hydroxide is molten
The weight of liquid is 1.1 times of theoretical value.
Specifically, in the present embodiment, the preparation method of the ammonium acid fluoride includes following 6 chemical equations：
H2SiF6+6NH3·H2O――→6NH4F+SiO2+4H2O
H2SO4+2NH3·H2O――→(NH4)2SO4+2H2O
HF+NH3·H2O――→NH4F+H2O
(NH4)2SO4+Ba(OH)2·8H2O――→BaSO4↓+2NH3·H2O+8H2O
NH4F+KOH――→KF+NH3·H2O
To sum up, the present invention replaces anhydrous hydrofluoric acid by the thick liquid of fluosilicic acid, not only reduces cost of material, while can solve
The certainly comprehensive utilization of the thick liquid of fluosilicic acid；Obtained by carrying out separation of solid and liquid solid with the 3rd reaction solution to first reaction solution
The solid silica and solid sulphuric acid barium arrived, then by clear water be beaten made of high-purity silica and barium sulfate,
The present invention is produced anhydrous potassium fluoride, at the same can coproduction silica and barium sulfate, improve economic benefit.
Above embodiment described the technical principle of the present invention, the description is merely to explain the principles of the invention, and
The limitation of the scope of the present invention cannot be construed in any way.Based on explanation herein, those skilled in the art is not required to
Other embodiments of the present invention can be associated by paying performing creative labour, these modes fall within the present invention's
In protection domain.
Claims (10)
- A kind of 1. preparation method of anhydrous potassium fluoride, it is characterised in that：The preparation method includes the following steps：Step S1, successively squeezes into the thick liquid of a certain amount of fluosilicic acid and ammonium hydroxide in the first reaction kettle, and stirring, forms first order reaction Liquid；Step S2, carries out separation of solid and liquid by the first order reaction liquid, solid silica and second order reaction liquid is obtained, by clear The solid silica is carried out mashing cleaning by water, obtains high-purity silicon dioxide；Step S3, the second order reaction liquid is squeezed into the second reaction kettle, adds a certain amount of barium hydroxide solution, is passed through Stirring, precipitation, obtain third-order reaction liquid；Step S4, the third-order reaction liquid and a certain amount of potassium hydroxide solution are successively added in the 3rd reaction kettle, is passed through height Warm steam heating, stirring obtain potassium fluoride clear liquid and ammonia, and it is female to form potassium fluoride by precipitation, concentration for the potassium fluoride clear liquid Liquid；Step S5, the potassium fluoride mother liquor is squeezed into spray drying tower and is spray-dried, and forms anhydrous potassium fluoride.
- 2. the preparation method of anhydrous potassium fluoride according to claim 1, it is characterised in that：The thick liquid of fluosilicic acid is anhydrous Accessory substance on hydrogen fluoride production line, its concentration be 20%~45%, its component include silicate fluoride solution, a small amount of sulfuric acid solution with And a small amount of hydrofluoric acid solution.
- 3. the preparation method of anhydrous potassium fluoride according to claim 1, it is characterised in that：The first order reaction liquid includes fluorine Change hydrogen ammonium salt solution, precipitation of silica and ammonium sulfate, its pH value is 8.5~9.
- 4. the preparation method of anhydrous potassium fluoride according to claim 1, it is characterised in that：The second order reaction liquid includes fluorine Changing hydrogen ammonium salt solution and ammonium sulfate, the third-order reaction liquid includes barium sulfate precipitate, ammonium hydrogen fluoride solution and ammonium hydroxide.
- 5. the preparation method of anhydrous potassium fluoride according to claim 1, it is characterised in that：In the step S3, add Sedimentation time after the barium hydroxide solution is 20h~30h；In the step S4, the potassium fluoride clear liquid sinks Form sediment the time be 20h~30h, the pH value of the potassium fluoride mother liquor be 7.5~8.5.
- 6. the preparation method of anhydrous potassium fluoride according to claim 1, it is characterised in that：The ammonia passes through cooling cycle System forms ammonium hydroxide and is stored in storage tank, for the operation of repeating said steps S1, the concentration of the ammonium hydroxide for 25%~ 29%.
- 7. the preparation method of anhydrous potassium fluoride according to claim 1, it is characterised in that：It is dense when the thick liquid of the fluosilicic acid Spend for 35% when, the concentration of first ammonium hydroxide is 25%, 1.05 times of the concentration that weight is the thick liquid of the fluosilicic acid, described eight The weight of water barium hydroxide solution is the 90% of theoretical value, and the weight of the potassium hydroxide solution is 1.1 times of theoretical value.
- 8. the preparation method of anhydrous potassium fluoride according to claim 1, it is characterised in that：It is dense when the thick liquid of the fluosilicic acid Spend for 20% when, the concentration of first ammonium hydroxide is 29%, 1.05 times of the concentration that weight is the thick liquid of the fluosilicic acid, described eight The weight of water barium hydroxide solution is the 90% of theoretical value, and the weight of the potassium hydroxide solution is 1.05 times of theoretical value.
- 9. the preparation method of anhydrous potassium fluoride according to claim 1, it is characterised in that：It is dense when the thick liquid of the fluosilicic acid Spend for 25% when, the concentration of first ammonium hydroxide is 27%, 1.1 times of the concentration that weight is the thick liquid of the fluosilicic acid, described eight The weight of water barium hydroxide solution is the 99% of theoretical value, and the weight of the potassium hydroxide solution is 1.1 times of theoretical value.
- 10. the preparation method of anhydrous potassium fluoride according to claim 1, it is characterised in that：When the thick liquid of the fluosilicic acid When concentration is 45%, the concentration of first ammonium hydroxide is 25%, 1.1 times of the concentration that weight is the thick liquid of the fluosilicic acid, described The weight of barium hydroxide solution is the 93% of theoretical value, and the weight of the potassium hydroxide solution is 1.1 times of theoretical value.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110697735A (en) * | 2019-11-21 | 2020-01-17 | 江西渠成氟化学有限公司 | Production process of potassium fluoride |
| CN110817883A (en) * | 2019-11-21 | 2020-02-21 | 江西渠成氟化学有限公司 | Process for producing potassium fluosilicate by using byproduct calcium fluoride |
| CN112897486A (en) * | 2021-01-29 | 2021-06-04 | 中船重工（邯郸）派瑞特种气体有限公司 | Device and process for producing ammonium bifluoride and potassium fluoride as byproducts in NF3 production |
| CN118356898A (en) * | 2024-06-19 | 2024-07-19 | 内蒙古星汉新材料有限公司 | High-activity potassium fluoride automatic production line |
-
2017
- 2017-12-14 CN CN201711341345.3A patent/CN108033465A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110697735A (en) * | 2019-11-21 | 2020-01-17 | 江西渠成氟化学有限公司 | Production process of potassium fluoride |
| CN110817883A (en) * | 2019-11-21 | 2020-02-21 | 江西渠成氟化学有限公司 | Process for producing potassium fluosilicate by using byproduct calcium fluoride |
| CN112897486A (en) * | 2021-01-29 | 2021-06-04 | 中船重工（邯郸）派瑞特种气体有限公司 | Device and process for producing ammonium bifluoride and potassium fluoride as byproducts in NF3 production |
| CN118356898A (en) * | 2024-06-19 | 2024-07-19 | 内蒙古星汉新材料有限公司 | High-activity potassium fluoride automatic production line |
| CN118356898B (en) * | 2024-06-19 | 2024-09-20 | 内蒙古星汉新材料有限公司 | High-activity potassium fluoride automatic production line |
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