CN107758701B - A kind of preparation method of Potassium Hexafluorophosphate - Google Patents
A kind of preparation method of Potassium Hexafluorophosphate Download PDFInfo
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- CN107758701B CN107758701B CN201710918052.0A CN201710918052A CN107758701B CN 107758701 B CN107758701 B CN 107758701B CN 201710918052 A CN201710918052 A CN 201710918052A CN 107758701 B CN107758701 B CN 107758701B
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- HZNVUJQVZSTENZ-UHFFFAOYSA-N 2,3-dichloro-5,6-dicyano-1,4-benzoquinone Chemical compound ClC1=C(Cl)C(=O)C(C#N)=C(C#N)C1=O HZNVUJQVZSTENZ-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims abstract description 21
- 239000012043 crude product Substances 0.000 claims abstract description 19
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 10
- 239000000047 product Substances 0.000 claims abstract description 10
- ASZZHBXPMOVHCU-UHFFFAOYSA-N 3,9-diazaspiro[5.5]undecane-2,4-dione Chemical compound C1C(=O)NC(=O)CC11CCNCC1 ASZZHBXPMOVHCU-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000001103 potassium chloride Substances 0.000 claims abstract description 8
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 8
- 238000001704 evaporation Methods 0.000 claims abstract description 7
- 230000008020 evaporation Effects 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims description 20
- 239000007787 solid Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 10
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 9
- 229910052700 potassium Inorganic materials 0.000 claims description 9
- 239000011591 potassium Substances 0.000 claims description 9
- 239000000706 filtrate Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 5
- 238000000605 extraction Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 238000001953 recrystallisation Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000004090 dissolution Methods 0.000 claims description 2
- XFDJMIHUAHSGKG-UHFFFAOYSA-N chlorethoxyfos Chemical compound CCOP(=S)(OCC)OC(Cl)C(Cl)(Cl)Cl XFDJMIHUAHSGKG-UHFFFAOYSA-N 0.000 claims 3
- SGWCNDDOFLBOQV-UHFFFAOYSA-N oxidanium;fluoride Chemical compound O.F SGWCNDDOFLBOQV-UHFFFAOYSA-N 0.000 claims 2
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 abstract description 16
- 239000002994 raw material Substances 0.000 abstract description 4
- 208000036142 Viral infection Diseases 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 abstract description 2
- 150000002484 inorganic compounds Chemical class 0.000 abstract description 2
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052742 iron Inorganic materials 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- -1 Hexafluorophosphate series Chemical class 0.000 description 11
- OBCUTHMOOONNBS-UHFFFAOYSA-N phosphorus pentafluoride Chemical compound FP(F)(F)(F)F OBCUTHMOOONNBS-UHFFFAOYSA-N 0.000 description 8
- UHZYTMXLRWXGPK-UHFFFAOYSA-N phosphorus pentachloride Chemical compound ClP(Cl)(Cl)(Cl)Cl UHZYTMXLRWXGPK-UHFFFAOYSA-N 0.000 description 7
- 229910052698 phosphorus Inorganic materials 0.000 description 4
- 239000011574 phosphorus Substances 0.000 description 4
- QGHDLJAZIIFENW-UHFFFAOYSA-N 4-[1,1,1,3,3,3-hexafluoro-2-(4-hydroxy-3-prop-2-enylphenyl)propan-2-yl]-2-prop-2-enylphenol Chemical group C1=C(CC=C)C(O)=CC=C1C(C(F)(F)F)(C(F)(F)F)C1=CC=C(O)C(CC=C)=C1 QGHDLJAZIIFENW-UHFFFAOYSA-N 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000000967 suction filtration Methods 0.000 description 3
- 229910021135 KPF6 Inorganic materials 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000003682 fluorination reaction Methods 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- RHFUXPCCELGMFC-UHFFFAOYSA-N n-(6-cyano-3-hydroxy-2,2-dimethyl-3,4-dihydrochromen-4-yl)-n-phenylmethoxyacetamide Chemical compound OC1C(C)(C)OC2=CC=C(C#N)C=C2C1N(C(=O)C)OCC1=CC=CC=C1 RHFUXPCCELGMFC-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 description 2
- 239000011698 potassium fluoride Substances 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 150000004673 fluoride salts Chemical class 0.000 description 1
- 125000001153 fluoro group Chemical group F* 0.000 description 1
- 229910001506 inorganic fluoride Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 235000003270 potassium fluoride Nutrition 0.000 description 1
- 229910000160 potassium phosphate Inorganic materials 0.000 description 1
- 235000011009 potassium phosphates Nutrition 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D13/00—Compounds of sodium or potassium not provided for elsewhere
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
Abstract
The present invention relates to a kind of synthesis fields of inorganic compound, more particularly to a kind of preparation method of Potassium Hexafluorophosphate, with potassium hydrogen fluoride (or potassium chloride), anhydrous hydrogen fluoride and phosphorus oxychloride are reaction raw materials, Potassium Hexafluorophosphate crude product is obtained after initial reaction under certain condition, acidity is adjusted with potassium hydroxide again and removes iron ion, active carbon adsorption decoloration, crude product after removal of impurities recrystallizes after being concentrated by evaporation, to obtain Potassium Hexafluorophosphate finished product, the preparation method of Potassium Hexafluorophosphate of the invention, compared with traditional preparation methods, it operates simpler, it reacts more gentle, it is easily controllable, it avoids a large amount of unstable, it is corrosive, has the use of virose raw material, to reduce the risk of operation, the Potassium Hexafluorophosphate produced through this method, yield is up to 88%, purity has been more than even more 99%.
Description
Technical field
The present invention relates to a kind of synthesis field of inorganic compound, in particular to a kind of preparation method of Potassium Hexafluorophosphate.
Background technique
Hexafluorophosphate series is a kind of critically important inorganic fluoride salt, wherein Potassium Hexafluorophosphate is compared in hexafluorophosphate
More important one kind.Potassium Hexafluorophosphate can be used for preparing other hexafluorophosphates, can also be used as machine fluorine substituting agent, as light is poly-
Close catalyst.The preparation method of hexafluorophosphate is greatly developed because of the application of lithium hexafluoro phosphate, after twentieth century
Phase, some western countries chemists such as the U.S., Germany propose the imagination that Potassium Hexafluorophosphate prepares lithium hexafluoro phosphate, so that hexafluoro
The production technology of potassium phosphate is extremely improved.
Currently, the preparation of Potassium Hexafluorophosphate is mostly to be reacted using phosphorus pentafluoride gas with the potassium fluoride solution containing hydrogen fluoride
It carries out, phosphorus pentafluoride then passes through phosphorus pentachloride and is prepared with anhydrous hydrogen fluoride reaction, reaction mechanism are as follows:
HF+PCl5→PF5+HCl
PF5+KF→KPF6
Also have using potassium chloride, anhydrous hydrogen fluoride, phosphorus pentachloride reaction and prepare Potassium Hexafluorophosphate, reaction mechanism are as follows:
KCl+6HF+PCl5→KPF6+6HCl↑
In existing method, using phosphorus pentafluoride gas and fluorination nak response, then need first to prepare phosphorus pentafluoride gas, and five fluorine
Change in phosphorus gas and be mixed with HCl gas, needs to separate；Phosphorus pentafluoride and fluorination nak response, actually should be anti-with potassium hydrogen fluoride
It answers, in these reactions, labile phosphorus pentachloride solid has been used when preparing phosphorus pentafluoride, has been used when synthesizing Potassium Hexafluorophosphate
Phosphorus pentafluoride gas, so that the difficulty of reaction controlling increases, it is largely unstable, corrosive, the virose raw material of tool to make
With increasing the risk of operation.
Using potassium chloride, anhydrous hydrogen fluoride, phosphorus pentachloride reaction come when preparing Potassium Hexafluorophosphate, phosphorus pentachloride solid needs
In a small amount of mixture that potassium chloride and anhydrous hydrogen fluoride is repeatedly added, due to reacting acutely, thus control is further increased
Difficulty is easy to cause dangerous.
Therefore, it is necessary to develop a kind of novel Potassium Hexafluorophosphate preparation method, its production process is made to more tend to can control
Property.
Summary of the invention
In order to overcome the above-mentioned deficiencies of the prior art, the invention proposes a kind of preparation method of Potassium Hexafluorophosphate, make anti-
Process is answered to be more easily controlled, operation difficulty reduces, while also reducing production cost.
To achieve the goals above, the technical scheme adopted by the invention is that:
A kind of preparation method of Potassium Hexafluorophosphate, it is characterised in that: method includes the following steps:
(1) under the conditions of 0-8 DEG C, anhydrous hydrogen fluoride is added in dry potassium hydrogen fluoride or solid potassium chloride and is reacted；
(2) temperature is adjusted to -5 DEG C, opens vacuum pump and adjusts vacuum degree, made reaction condition in tiny structure, slowly drip
Add phosphorus oxychloride, control rate of addition, so that temperature is no more than -2 DEG C, after being added dropwise to complete, continue to be stirred to react 30min；
(3) temperature is adjusted to 75-85 DEG C, and vacuum degree is adjusted to 0.7-0.8Pa, by remaining hydrogen fluoride gas and life
At HCl gas extraction；
(4) it is slowly added to 50% potassium hydroxide solution into reaction, pH value is adjusted to 7；
(5) material after reaction is cooled to room temperature, Potassium Hexafluorophosphate crude product is obtained after being centrifuged；
(6) add water into Potassium Hexafluorophosphate crude product, and active carbon is added, adjust pH value to 8 with potassium hydroxide solid, heat
Stirring and dissolving；
(7) Potassium Hexafluorophosphate crude product is filtered by vacuum after being completely dissolved, and filtrate is concentrated by evaporation, when there is epitaxial in liquid level,
The cooling recrystallization of stirring；
(8) it after being cooled to room temperature, then is centrifuged, dries to obtain Potassium Hexafluorophosphate finished product.
Preferably, the dosage of anhydrous hydrogen fluoride described in step (1) is 1.8-2.0 times of theoretical amount.
It is further preferred that the dosage of anhydrous hydrogen fluoride described in step (1) is 1.8 times of theoretical amount.
Preferably, vacuum degree described in step (2) is 0.5Pa.
Preferably, the dosage of phosphorus oxychloride described in step (2) is 1.05-1.08 times of theoretical amount.
It is further preferred that the dosage of phosphorus oxychloride described in step (2) is 1.05 times of theoretical amount.
Preferably, temperature described in step (3) is 80 DEG C, and keeps the temperature 30min；
Preferably, the temperature of vacuum filtration described in step (7) is greater than 80 DEG C；
Preferably, remnants hydrogen fluoride gas described in step (3) and the HCl gas of generation are absorbed through lye.
Preferably, filtrate remaining in the step (8) can be used for producing potassium fluosilicate and potassium fluoborate.
Compared with prior art, the beneficial effects of the present invention are:
The present invention mainly uses anhydrous hydrogen fluoride dissolution potassium hydrogen fluoride or potassium chloride, obtains six after phosphorus oxychloride reaction is added dropwise
Fluorophosphoric acid potassium crude product adjusts acidity with potassium hydroxide and removes iron ion, active carbon adsorption decoloration, and the crude product evaporation after removal of impurities is dense
It is recrystallized after contracting, to obtain Potassium Hexafluorophosphate finished product, compared with the preparation method of traditional Potassium Hexafluorophosphate, operation is simpler,
React more gentle, it is easily controllable, a large amount of unstable, corrosive, the virose raw material of tool uses are avoided, to reduce
The risk of operation, the Potassium Hexafluorophosphate produced through this method, yield are up to 88%, purity be even more be more than 99%.
Specific embodiment
Specific embodiments of the present invention will be further explained below.It should be noted that for these implementations
The explanation of mode is used to help understand the present invention, but and does not constitute a limitation of the invention.In addition, invention described below
Technical characteristic involved in each embodiment can be combined with each other as long as they do not conflict with each other.
Embodiment 1
A kind of preparation method of Potassium Hexafluorophosphate, comprising the following steps:
(1) under the conditions of 0-8 DEG C, 150g anhydrous hydrogen fluoride is added in the dry potassium hydrogen fluoride solid of 78g and is reacted；
(2) temperature is adjusted to -5 DEG C, opens vacuum pump and vacuum degree is adjusted to 0.5Pa, make reaction condition in micro- negative
160g phosphorus oxychloride is slowly added dropwise in pressure, controls rate of addition, so that temperature is no more than -2 DEG C, after being added dropwise to complete, continues to be stirred to react
30min；
(3) temperature is adjusted to 80 DEG C, keeps the temperature 30min；And vacuum degree is adjusted to 0.7Pa, by remaining hydrogen fluoride gas
And the HCl gas extraction generated, it is neutralized with lye；
(4) it is slowly added to 50% potassium hydroxide solution into reaction, pH value is adjusted to 7；
(5) material after reaction is cooled to room temperature, 181g Potassium Hexafluorophosphate crude product is obtained after being centrifuged；
(6) add 300ml water into Potassium Hexafluorophosphate crude product, and proper amount of active carbon is added, adjust pH with potassium hydroxide solid
To 8, heating stirring dissolves value；
(7) Potassium Hexafluorophosphate crude product is filtered by vacuum after being completely dissolved, and filters out active carbon, to prevent hexafluoro phosphorus during filtering
Sour potassium product crystallization is precipitated, and temperature is adjusted to be greater than 80 DEG C, filtrate is concentrated by evaporation after the completion of suction filtration, epitaxial occurs to liquid level
When, stirring natural cooling recrystallization；
(8) it after being cooled to room temperature, then is centrifuged, dries to obtain 162g Potassium Hexafluorophosphate finished product, yield 88.04%, six
Fluorophosphoric acid potassium content is detected as 99.15%.
Embodiment 2
A kind of preparation method of Potassium Hexafluorophosphate, comprising the following steps:
(1) under the conditions of 0-8 DEG C, 160g anhydrous hydrogen fluoride is added in the dry potassium hydrogen fluoride solid of 78g and is reacted；
(2) temperature is adjusted to -5 DEG C, opens vacuum pump and vacuum degree is adjusted to 0.5Pa, make reaction condition in micro- negative
163g phosphorus oxychloride is slowly added dropwise in pressure, controls rate of addition, so that temperature is no more than -2 DEG C, after being added dropwise to complete, continues to be stirred to react
30min；
(3) temperature is adjusted to 80 DEG C, keeps the temperature 30min；And vacuum degree is adjusted to 0.7Pa, by remaining hydrogen fluoride gas
And the HCl gas extraction generated, it is neutralized with lye；
(4) it is slowly added to 50% potassium hydroxide solution into reaction, pH value is adjusted to 7；
(5) material after reaction is cooled to room temperature, 182g Potassium Hexafluorophosphate crude product is obtained after being centrifuged；
(6) add 300ml water into Potassium Hexafluorophosphate crude product, and proper amount of active carbon is added, adjust pH with potassium hydroxide solid
To 8, heating stirring dissolves value；
(7) Potassium Hexafluorophosphate crude product is filtered by vacuum after being completely dissolved, and filters out active carbon, to prevent hexafluoro phosphorus during filtering
Sour potassium product crystallization is precipitated, and temperature is adjusted to be greater than 80 DEG C, filtrate is concentrated by evaporation after the completion of suction filtration, epitaxial occurs to liquid level
When, stirring natural cooling recrystallization；
(8) it after being cooled to room temperature, then is centrifuged, dries to obtain 162.5g Potassium Hexafluorophosphate finished product, yield 88.32%,
Hexafluorophosphoric acid potassium content is detected as 99.18%.
Embodiment 3
(1) under the conditions of 0-8 DEG C, 167g anhydrous hydrogen fluoride is added in the dry potassium hydrogen fluoride solid of 78g and is reacted；
(2) temperature is adjusted to -5 DEG C, opens vacuum pump and vacuum degree is adjusted to 0.5Pa, make reaction condition in micro- negative
165g phosphorus oxychloride is slowly added dropwise in pressure, controls rate of addition, so that temperature is no more than -2 DEG C, after being added dropwise to complete, continues to be stirred to react
30min；
(3) temperature is adjusted to 80 DEG C, keeps the temperature 30min；And vacuum degree is adjusted to 0.8Pa, by remaining hydrogen fluoride gas
And the HCl gas extraction generated, it is neutralized with lye；
(4) it is slowly added to 50% potassium hydroxide solution into reaction, pH value is adjusted to 7；
(5) material after reaction is cooled to room temperature, 183.7g Potassium Hexafluorophosphate crude product is obtained after being centrifuged；
(6) add 300ml water into Potassium Hexafluorophosphate crude product, and proper amount of active carbon is added, adjust pH with potassium hydroxide solid
To 8, heating stirring dissolves value；
(7) Potassium Hexafluorophosphate crude product is filtered by vacuum after being completely dissolved, and filters out active carbon, to prevent hexafluoro phosphorus during filtering
Sour potassium product crystallization is precipitated, and temperature is adjusted to be greater than 80 DEG C, filtrate is concentrated by evaporation after the completion of suction filtration, epitaxial occurs to liquid level
When, stirring natural cooling recrystallization；
(8) it after being cooled to room temperature, then is centrifuged, dries to obtain 162.8g Potassium Hexafluorophosphate finished product, yield 88.48%,
Hexafluorophosphoric acid potassium content is detected as 99.20%.
Above the embodiments of the present invention are described in detail, but the present invention is not limited to described embodiments.It is right
For those skilled in the art, in the case where not departing from the principle of the invention and spirit, these embodiments are carried out more
Kind change, modification, replacement and modification, still fall in protection scope of the present invention.
Claims (10)
1. a kind of preparation method of Potassium Hexafluorophosphate, it is characterised in that: method includes the following steps:
S1, under the conditions of 0-8 DEG C, anhydrous hydrogen fluoride is added in dry potassium hydrogen fluoride or solid potassium chloride and is reacted；
S2, temperature is adjusted to -5 DEG C, opens vacuum pump and adjusts vacuum degree, made reaction condition in tiny structure, be slowly added dropwise three
Chlorethoxyfos control rate of addition, so that temperature is no more than -2 DEG C, after being added dropwise to complete, continue to be stirred to react 30min；
S3, temperature is adjusted to 75-85 DEG C, and vacuum degree is adjusted to 0.7-0.8Pa, by remaining hydrogen fluoride gas and generation
HCl gas extraction；
S4, it is slowly added to 50% potassium hydroxide solution into reaction, pH value is adjusted to 7；
S5, the material after reaction is cooled to room temperature, Potassium Hexafluorophosphate crude product is obtained after being centrifuged；
S6, add water into Potassium Hexafluorophosphate crude product, and active carbon is added, with potassium hydroxide solid adjusting pH value to 8, heating stirring
Dissolution；
S7, Potassium Hexafluorophosphate crude product are filtered by vacuum after being completely dissolved, and filtrate is concentrated by evaporation, when there is epitaxial in liquid level, stirring
Cooling recrystallization；
S8, it after being cooled to room temperature, then is centrifuged, dries to obtain Potassium Hexafluorophosphate finished product.
2. a kind of preparation method of Potassium Hexafluorophosphate according to claim 1, it is characterised in that: nothing described in step (1)
The dosage of water hydrogen fluoride is 1.8-2.0 times of theoretical amount.
3. a kind of preparation method of Potassium Hexafluorophosphate according to claim 2, it is characterised in that: nothing described in step (1)
The dosage of water hydrogen fluoride is 1.8 times of theoretical amount.
4. a kind of preparation method of Potassium Hexafluorophosphate according to claim 2, it is characterised in that: described in step (2)
Vacuum degree is 0.5Pa.
5. a kind of preparation method of Potassium Hexafluorophosphate according to claim 1, it is characterised in that: three described in step (2)
The dosage of chlorethoxyfos is 1.05-1.08 times of theoretical amount.
6. a kind of preparation method of Potassium Hexafluorophosphate according to claim 1, it is characterised in that: three described in step (2)
The dosage of chlorethoxyfos is 1.05 times of theoretical amount.
7. a kind of preparation method of Potassium Hexafluorophosphate according to claim 1, it is characterised in that: described in step (3)
Temperature is 80 DEG C, and keeps the temperature 30min；
8. a kind of preparation method of Potassium Hexafluorophosphate according to claim 1, it is characterised in that: true described in step (7)
The temperature of empty pump filter is greater than 80 DEG C.
9. a kind of preparation method of Potassium Hexafluorophosphate according to claim 1, it is characterised in that: residual described in step (3)
Remaining hydrogen fluoride gas and the HCl gas of generation are absorbed through lye.
10. a kind of preparation method of Potassium Hexafluorophosphate according to claim 1, it is characterised in that: residual in the step (8)
Remaining filtrate is for producing potassium fluosilicate and potassium fluoborate.
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| CN112456519A (en) * | 2020-12-01 | 2021-03-09 | 森田新能源材料（张家港）有限公司 | Method for recovering lithium hexafluorophosphate waste liquid |
| CN114436292B (en) * | 2022-02-21 | 2023-04-28 | 中船(邯郸)派瑞特种气体股份有限公司 | Treatment method of organic potassium salt wastewater |
| CN114590823B (en) * | 2022-03-31 | 2023-11-17 | 河南省氟基新材料科技有限公司 | Preparation method of potassium hexafluorophosphate |
| CN115974106B (en) * | 2022-12-15 | 2024-03-22 | 福建省龙德新能源有限公司 | Sodium hexafluorophosphate and recrystallization method thereof |
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| JP5254555B2 (en) * | 2007-02-08 | 2013-08-07 | ステラケミファ株式会社 | Method for producing phosphorus pentafluoride and hexafluorophosphate |
| JP2010042937A (en) * | 2008-08-08 | 2010-02-25 | Stella Chemifa Corp | Method for producing phosphorus pentafluoride and hexafluorophosphates |
| US20150044118A1 (en) * | 2012-01-19 | 2015-02-12 | Lanxess Deutschland Gmbh | Low-chloride lipf6 |
| CN102910612B (en) * | 2012-11-05 | 2014-06-18 | 中国海洋石油总公司 | Method for preparing lithium hexafluorophosphate |
| WO2015150862A1 (en) * | 2014-03-31 | 2015-10-08 | The South African Nuclear Energy Corporation Limited | Production of a hexafluorophosphate salt and of phosphorous pentafluoride |
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| CN107758701A (en) | 2018-03-06 |
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Application publication date: 20180306 Assignee: Jiangxi Sanjia Fluorochemical Co.,Ltd. Assignor: JIANGXI DONGYAN PHARMACEUTICAL Co.,Ltd. Contract record no.: X2024980012407 Denomination of invention: A preparation method of potassium hexafluorophosphate Granted publication date: 20190625 License type: Common License Record date: 20240819 |
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