CN102887531B - Technique for producing potassium fluoride from potassium fluosilicate - Google Patents
Technique for producing potassium fluoride from potassium fluosilicate Download PDFInfo
- Publication number
- CN102887531B CN102887531B CN201210389440.1A CN201210389440A CN102887531B CN 102887531 B CN102887531 B CN 102887531B CN 201210389440 A CN201210389440 A CN 201210389440A CN 102887531 B CN102887531 B CN 102887531B
- Authority
- CN
- China
- Prior art keywords
- potassium
- fluoride
- liquid
- fluosilicate
- solid
- 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.)
- Active
Links
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 title claims abstract description 61
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229910052700 potassium Inorganic materials 0.000 title claims abstract description 34
- 239000011591 potassium Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000011698 potassium fluoride Substances 0.000 title claims abstract description 14
- 235000003270 potassium fluoride Nutrition 0.000 title claims abstract description 13
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 54
- 239000007788 liquid Substances 0.000 claims abstract description 38
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims abstract description 30
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 27
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- 239000011775 sodium fluoride Substances 0.000 claims abstract description 15
- 235000013024 sodium fluoride Nutrition 0.000 claims abstract description 15
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 11
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 11
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 6
- 239000010703 silicon Substances 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims description 39
- 239000007787 solid Substances 0.000 claims description 16
- 238000000926 separation method Methods 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 10
- 230000015572 biosynthetic process Effects 0.000 claims description 6
- 238000003786 synthesis reaction Methods 0.000 claims description 6
- 238000012546 transfer Methods 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- 239000006229 carbon black Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000012452 mother liquor Substances 0.000 claims description 5
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 239000007921 spray Substances 0.000 claims description 5
- 238000001694 spray drying Methods 0.000 claims description 5
- 238000003860 storage Methods 0.000 claims description 5
- 239000008139 complexing agent Substances 0.000 claims description 4
- 239000000047 product Substances 0.000 abstract description 16
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052731 fluorine Inorganic materials 0.000 abstract description 7
- 239000011737 fluorine Substances 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 4
- 239000006227 byproduct Substances 0.000 abstract description 4
- 229910000040 hydrogen fluoride Inorganic materials 0.000 abstract description 4
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 abstract description 3
- 239000002253 acid Substances 0.000 abstract description 2
- 229910021529 ammonia Inorganic materials 0.000 abstract description 2
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 2
- XJKVPKYVPCWHFO-UHFFFAOYSA-N silicon;hydrate Chemical compound O.[Si] XJKVPKYVPCWHFO-UHFFFAOYSA-N 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 2
- 230000002708 enhancing effect Effects 0.000 abstract 2
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 abstract 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 abstract 1
- 230000000536 complexating effect Effects 0.000 abstract 1
- 239000001103 potassium chloride Substances 0.000 abstract 1
- 235000011164 potassium chloride Nutrition 0.000 abstract 1
- 239000002244 precipitate Substances 0.000 abstract 1
- 239000003814 drug Substances 0.000 description 9
- 229960001866 silicon dioxide Drugs 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 6
- 229940079593 drug Drugs 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 2
- LRCFXGAMWKDGLA-UHFFFAOYSA-N dioxosilane;hydrate Chemical compound O.O=[Si]=O LRCFXGAMWKDGLA-UHFFFAOYSA-N 0.000 description 2
- 239000010436 fluorite Substances 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000575 pesticide Substances 0.000 description 2
- 229960004029 silicic acid Drugs 0.000 description 2
- RTHCYVBBDHJXIQ-MRXNPFEDSA-N (R)-fluoxetine Chemical compound O([C@H](CCNC)C=1C=CC=CC=1)C1=CC=C(C(F)(F)F)C=C1 RTHCYVBBDHJXIQ-MRXNPFEDSA-N 0.000 description 1
- ASZZHBXPMOVHCU-UHFFFAOYSA-N 3,9-diazaspiro[5.5]undecane-2,4-dione Chemical compound C1C(=O)NC(=O)CC11CCNCC1 ASZZHBXPMOVHCU-UHFFFAOYSA-N 0.000 description 1
- GSDSWSVVBLHKDQ-UHFFFAOYSA-N 9-fluoro-3-methyl-10-(4-methylpiperazin-1-yl)-7-oxo-2,3-dihydro-7H-[1,4]oxazino[2,3,4-ij]quinoline-6-carboxylic acid Chemical compound FC1=CC(C(C(C(O)=O)=C2)=O)=C3N2C(C)COC3=C1N1CCN(C)CC1 GSDSWSVVBLHKDQ-UHFFFAOYSA-N 0.000 description 1
- 229910020440 K2SiF6 Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 description 1
- 229940070337 ammonium silicofluoride Drugs 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 230000001430 anti-depressive effect Effects 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 239000000935 antidepressant agent Substances 0.000 description 1
- 229940005513 antidepressants Drugs 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 206010012601 diabetes mellitus Diseases 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- -1 fluorine organic compound Chemical class 0.000 description 1
- 125000001153 fluoro group Chemical group F* 0.000 description 1
- 229940124307 fluoroquinolone Drugs 0.000 description 1
- 229960002464 fluoxetine Drugs 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229960001699 ofloxacin Drugs 0.000 description 1
- DHZKUVDKQZJAMV-UHFFFAOYSA-M potassium;fluoride;hydrate Chemical compound O.[F-].[K+] DHZKUVDKQZJAMV-UHFFFAOYSA-M 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- MFFMDFFZMYYVKS-SECBINFHSA-N sitagliptin Chemical compound C([C@H](CC(=O)N1CC=2N(C(=NN=2)C(F)(F)F)CC1)N)C1=CC(F)=C(F)C=C1F MFFMDFFZMYYVKS-SECBINFHSA-N 0.000 description 1
- 229960004034 sitagliptin Drugs 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 239000003171 wood protecting agent Substances 0.000 description 1
Landscapes
- Silicon Compounds (AREA)
Abstract
The invention relates to a technique for producing potassium fluoride and coproducing high-purity silicon dioxide and sodium fluoride mainly from potassium fluosilicate, liquid potassium (liquid potassium hydroxide) and sodium hydroxide. The invention provides a method for producing potassium fluoride from a new fluorine source potassium fluosilicate instead of anhydrous hydrogen fluoride. All potassium for generating the potassium fluoride is derived from potassium in the potassium fluosilicate, thereby lowering the raw material cost of the 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; and the potassium fluosilicate is synthesized from the anhydrous hydrogen fluoride production line byproduct fluosilicic acid and byproduct potassium chloride, thereby enhancing the product quality of potassium fluoride, lowering the raw material cost for 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 technique that uses potassium silicofluoride to produce 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, and the hydrofluoric acid in traditional technology is mainly made by fluorite and sulfuric acid reaction, and traditional technology need to consume valuable resource fluorite, and hydrofluoric acid cost is quite high.
Summary of the invention
In order to solve the problems of the technologies described above, the invention provides a kind of technique that uses potassium silicofluoride to produce Potassium monofluoride.
Reaction formula of the present invention is:
K2SiF6+4KOH――→6KF+SiO2+4H2O
KF+NaOH――→KOH+NaF
Use potassium silicofluoride to produce a technique for Potassium monofluoride, it is characterized in that it comprises the steps:
1) liquid potassium hydroxide is added to reactor, starts stirring, add silicon complexing agent, at the uniform velocity add potassium silicofluoride solid, fully reaction;
2) reaction solution carries out solid-liquid separation, and solid is pulled an oar to clean and is high-purity silicon dioxide, obtains after drying white carbon black;
3) a part of reaction solution of second step is added to Sodium Fluoride synthesis reactor, open and stir, input sodium hydroxide at the uniform velocity, after having reacted, carry out solid-liquid separation, solid is dried and is finished product Sodium Fluoride, and liquid enters liquid potassium hydroxide storage tank, uses in order to desiliconization;
4) a part of reaction solution of second step is added to transfer tank, precipitation 24h, clear liquid adds Potassium monofluoride concentration kettle;
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.
Described a kind of technique that uses potassium silicofluoride to produce Potassium monofluoride, is characterized in that the mass percentage concentration of the liquid potassium hydroxide described in step 1) is 48%.
Described a kind of technique that uses potassium silicofluoride to produce Potassium monofluoride, the amount that it is characterized in that the silicon complexing agent adding in step 1) is 0.2% of liquid potassium hydroxide weight.
Described a kind of technique that uses potassium silicofluoride to produce Potassium monofluoride, is characterized in that adding potassium silicofluoride solid according to 0.9 times of the required mole number of reaction in step 1).
Described a kind of technique that uses potassium silicofluoride to produce Potassium monofluoride, it is characterized in that reacting in step 1) to the pH value of reaction end be 8.5-9.
Described a kind of technique that uses potassium silicofluoride to produce Potassium monofluoride, is characterized in that, in step 3), 2/3 reaction solution of second step is added to Sodium Fluoride synthesis reactor, in step 4), 1/3 remaining reaction solution of second step is added to transfer tank.
Described a kind of technique that uses potassium silicofluoride to produce Potassium monofluoride, is characterized in that adding sodium hydroxide according to 0.9-1 times of the required mole number of reaction in step 3).
Described a kind of technique that uses potassium silicofluoride to produce Potassium monofluoride, is characterized in that the mass percentage concentration that is concentrated into solution in still in step 4) reaches 48%-50%.
Described a kind of technique that uses potassium silicofluoride to produce Potassium monofluoride, is characterized in that the silicon complexing agent in step 1) is nitrilotriacetic acid(NTA) sodium.
A kind of technique that uses potassium silicofluoride to produce Potassium monofluoride of the present invention, provide a kind of new fluorine source potassium silicofluoride to replace anhydrous hydrogen fluoride to produce the method for Potassium monofluoride, the potassium that generates Potassium monofluoride all derives from the potassium in potassium silicofluoride, greatly reduce the raw materials cost of Potassium monofluoride, 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, to be that anhydrous hydrogen fluoride production line byproduct silicofluoric acid and by-product Repone K are synthetic make potassium silicofluoride, improve Potassium monofluoride quality product, reduce Potassium monofluoride material cost, promote Potassium monofluoride manufacturing enterprise benefit.
Embodiment
Embodiment 1
1, the liquid potassium hydroxide that is 48% by mass percentage concentration adds reactor, start stirring, add the nitrilotriacetic acid(NTA) sodium of 0.2% amount of liquid potassium hydroxide weight, at the uniform velocity add potassium silicofluoride solid according to 0.9 times of the required mole number of reaction formula, fully reaction, the pH value of reaction end is 8.5-9.
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.
3,2/3 reaction solution of second step is added to Sodium Fluoride synthesis reactor, open and stir, at the uniform velocity drop into sodium hydroxide according to 1 times of the required mole number of reaction formula, after having reacted, carry out solid-liquid separation, solid is dried and is finished product Sodium Fluoride, liquid enters liquid potassium hydroxide storage tank, uses in order to desiliconization.
4, the 1/3 remaining reaction solution of second step is added to transfer tank, precipitation 24h, clear liquid adds Potassium monofluoride concentration kettle, and in still, strength of solution 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 liquid potassium hydroxide that is 48% by mass percentage concentration adds reactor, start stirring, add the nitrilotriacetic acid(NTA) sodium of 0.2% amount of liquid potassium hydroxide weight, at the uniform velocity add potassium silicofluoride solid according to 0.9 times of the required mole number of reaction formula, fully reaction, the pH value of reaction end is 8.5-9.
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.
3,2/3 reaction solution of second step is added to Sodium Fluoride synthesis reactor, open and stir, at the uniform velocity drop into sodium hydroxide according to 1 times of the required mole number of reaction formula, after having reacted, carry out solid-liquid separation, solid is dried and is finished product Sodium Fluoride, liquid enters liquid potassium hydroxide storage tank, uses in order to desiliconization.
4, the 1/3 remaining reaction solution of second step is added to transfer tank, precipitation 24h, clear liquid adds Potassium monofluoride concentration kettle, and in still, strength of solution 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 liquid potassium hydroxide that is 48% by mass percentage concentration adds reactor, start stirring, add the nitrilotriacetic acid(NTA) sodium of 0.2% amount of liquid potassium hydroxide weight, at the uniform velocity add potassium silicofluoride solid according to 0.9 times of the required mole number of reaction formula, fully reaction, the pH value of reaction end is 8.5-9.
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.
3,2/3 reaction solution of second step is added to Sodium Fluoride synthesis reactor, open and stir, at the uniform velocity drop into sodium hydroxide according to 0.9 times of the required mole number of reaction formula, after having reacted, carry out solid-liquid separation, solid is dried and is finished product Sodium Fluoride, liquid enters liquid potassium hydroxide storage tank, uses in order to desiliconization.
4, the 1/3 remaining reaction solution of second step is added to transfer tank, precipitation 24h, clear liquid adds Potassium monofluoride concentration kettle, and in still, strength of solution 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.
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 Sodium Fluoride product quality analysis results (each embodiment respectively carries out twice experiment) of utilizing method of the present invention to produce, conformance with standard: GB4293-84
The Sodium Fluoride product quality analysis result that table 2 utilizes method of the present invention to produce
Table 3 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 3 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. use potassium silicofluoride to produce a technique for Potassium monofluoride, it is characterized in that it comprises the steps:
1) liquid potassium hydroxide that is 48% by mass percentage concentration adds reactor, start stirring, add 0.2% nitrilotriacetic acid(NTA) sodium of liquid potassium hydroxide weight as silicon complexing agent, at the uniform velocity add potassium silicofluoride solid according to reaction 0.9 times of required mole number, fully react to the pH value of reaction end be 8.5-9;
2) reaction solution carries out solid-liquid separation, and solid is pulled an oar to clean and is high-purity silicon dioxide, obtains after drying white carbon black;
3) 2/3 reaction solution of second step is added to Sodium Fluoride synthesis reactor, open and stir, at the uniform velocity drop into sodium hydroxide according to reaction 0.9-1 times of required mole number, after having reacted, carry out solid-liquid separation, solid is dried and is finished product Sodium Fluoride, liquid enters liquid potassium hydroxide storage tank, uses in order to desiliconization;
4) the 1/3 remaining reaction solution of second step is added to transfer tank, precipitation 24h, the mass percentage concentration that clear liquid adds Potassium monofluoride 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210389440.1A CN102887531B (en) | 2012-10-15 | 2012-10-15 | Technique for producing potassium fluoride from potassium fluosilicate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210389440.1A CN102887531B (en) | 2012-10-15 | 2012-10-15 | Technique for producing potassium fluoride from potassium fluosilicate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102887531A CN102887531A (en) | 2013-01-23 |
| CN102887531B true CN102887531B (en) | 2014-07-02 |
Family
ID=47531238
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210389440.1A Active CN102887531B (en) | 2012-10-15 | 2012-10-15 | Technique for producing potassium fluoride from potassium fluosilicate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102887531B (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104030250B (en) * | 2014-06-25 | 2016-04-27 | 江西渠成氟化学有限公司 | A kind of technique using silicofluoric acid to produce sodium bifluoride |
| CN105439160A (en) * | 2015-11-29 | 2016-03-30 | 洛阳绿仁环保设备有限公司 | Method for preparing potassium silicate from potassium feldspar |
| CN105439167A (en) * | 2015-11-29 | 2016-03-30 | 洛阳绿仁环保设备有限公司 | Method for preparing 3A molecular sieve from potassium feldspar |
| 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 |
| CN109160636A (en) * | 2018-10-15 | 2019-01-08 | 大连东泰产业废弃物处理有限公司 | A kind of technique of high-concentration fluorine-contained base extraction and recycling |
| CN113060745A (en) * | 2021-03-19 | 2021-07-02 | 严永生 | Preparation method for preparing potassium fluoride by using potash and potassium fluosilicate |
| 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 |
| CN114031100A (en) * | 2021-12-20 | 2022-02-11 | 湖北祥云(集团)化工股份有限公司 | Method for preparing fluoride salt from phosphorus ore associated fluorine |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3656894A (en) * | 1970-05-08 | 1972-04-18 | Central Glass Co Ltd | Process for the production of high quality synthetic cryolite |
| US3842161A (en) * | 1971-12-13 | 1974-10-15 | Kemira Oy | Method of refining the fluorine obtained as a by-product in the fertilizer industry |
| CN101028934A (en) * | 2006-03-01 | 2007-09-05 | 多氟多化工股份有限公司 | Method for linked producing potassium fluoride white carbon black |
| CN101376509A (en) * | 2007-08-31 | 2009-03-04 | 多氟多化工股份有限公司 | Method for preparing potassium fluoride |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009113088A2 (en) * | 2008-01-14 | 2009-09-17 | Aditya Birla Science & Technology Co. Limited | A process for manufacturing of potassium fluoride |
-
2012
- 2012-10-15 CN CN201210389440.1A patent/CN102887531B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3656894A (en) * | 1970-05-08 | 1972-04-18 | Central Glass Co Ltd | Process for the production of high quality synthetic cryolite |
| US3842161A (en) * | 1971-12-13 | 1974-10-15 | Kemira Oy | Method of refining the fluorine obtained as a by-product in the fertilizer industry |
| CN101028934A (en) * | 2006-03-01 | 2007-09-05 | 多氟多化工股份有限公司 | Method for linked producing potassium fluoride white carbon black |
| CN101376509A (en) * | 2007-08-31 | 2009-03-04 | 多氟多化工股份有限公司 | Method for preparing potassium fluoride |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102887531A (en) | 2013-01-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102887531B (en) | Technique for producing potassium fluoride from potassium fluosilicate | |
| CN103818933B (en) | Method for production of high-purity potassium fluoride by using hydrofluoric acid residual liquid | |
| CN106276829B (en) | A kind of synthetic method of double fluorine sulfimide lithiums | |
| CN103935970A (en) | Preparation methods of bis(fluorosulfonyl)imide and alkali metal salts thereof | |
| CN103044384B (en) | Preparation method of 3-fluorine-1, 3-propane sulfonic acid lactone | |
| US20140121405A1 (en) | Process for producing taurine | |
| CN102887530B (en) | Production technique of potassium fluoride | |
| CN102887528B (en) | Production technology of ammonium bifluoride | |
| CN110436485A (en) | A method of potassium fluoride in high activity is produced using fluosilicic acid and potassium fluosilicate | |
| CN103101931A (en) | Method for preparing potassium fluoride by using potassium fluosilicate with co-production of white carbon black | |
| CN102730710B (en) | Method for separating potassium chloride and potassium fluoride | |
| CN101823694B (en) | Processing method for purifying sulfur-containing chlorine hydride | |
| CN1990460B (en) | Comprehensive treatment of glycine crystallization mother liquid | |
| CN107032834A (en) | The technique that liquid phase mortar gunite method produces potassium sulfate | |
| CN102275947A (en) | Method for preparing potassium fluoborate by using mixed acid containing hydrogen fluoride | |
| CN103342646B (en) | High-selectivity synthesis method of 4-nitro-ortho-xylene | |
| CN102351694A (en) | Preparation method of trifluoroacetic acid ethyl ester | |
| CN103121699A (en) | Method for preparing potassium fluoride by utilizing potassium fluosilicate | |
| CN106587494A (en) | Method for improving ammonia-nitrogen content of H acid wastewater | |
| CN107934988A (en) | A kind of preparation method of ammonium acid fluoride | |
| CN106810476A (en) | Synthesize the method and its system of N-acetylsulfanilyl chloride as sulfonating agent with sulfur trioxide | |
| CN114380304B (en) | Short-process preparation method of raw material potassium fluoride for p-fluoronitrobenzene | |
| CN105732154A (en) | Method for preparing potassium fertilizer from potassium feldspar | |
| CN109651072A (en) | The method that chloroethanes is prepared by hydrochloric acid containing sulfur dioxide | |
| CN203269555U (en) | Apparatus for preparing hydrogen chloride by using roasting method |
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 | ||
| ASS | Succession or assignment of patent right |
Owner name: YUNNAN FLUORINE INDUSTRY ENVIRONMENTAL PROTECTION Free format text: FORMER OWNER: ZHANG JUNHANG Effective date: 20150512 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| COR | Change of bibliographic data |
Free format text: CORRECT: ADDRESS; FROM: 322118 JINHUA, ZHEJIANG PROVINCE TO: 650021 KUNMING, YUNNAN PROVINCE |
|
| TR01 | Transfer of patent right |
Effective date of registration: 20150512 Address after: 650021 Yunnan city of Kunming Province Nanping Street Century Square bldg C2 18 floor BC block Patentee after: Yunnan fluorine industry environmental protection Polytron Technologies Inc Address before: 322118 Jinhua City, Dongyang Province, Hengdian Town, Jing Jing community Jing Jing, No. 156 Patentee before: Zhang Junhang |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Technique for producing potassium fluoride from potassium fluosilicate Effective date of registration: 20170929 Granted publication date: 20140702 Pledgee: Bank of Communications Ltd Yunnan branch Pledgor: Yunnan fluorine industry environmental protection Polytron Technologies Inc Registration number: 2017530000013 |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20181212 Granted publication date: 20140702 Pledgee: Bank of Communications Ltd Yunnan branch Pledgor: Yunnan fluorine industry environmental protection Polytron Technologies Inc Registration number: 2017530000013 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right |