CN107758701A - A kind of preparation method of Potassium Hexafluorophosphate - Google Patents
A kind of preparation method of Potassium Hexafluorophosphate Download PDFInfo
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- CN107758701A CN107758701A CN201710918052.0A CN201710918052A CN107758701A CN 107758701 A CN107758701 A CN 107758701A CN 201710918052 A CN201710918052 A CN 201710918052A CN 107758701 A CN107758701 A CN 107758701A
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- potassium hexafluorophosphate
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- hydrogen fluoride
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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 22
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000012043 crude product Substances 0.000 claims abstract description 19
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims abstract description 18
- 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 15
- 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 6
- 239000007789 gas Substances 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 15
- 239000007787 solid Substances 0.000 claims description 12
- 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
- 239000003513 alkali Substances 0.000 claims description 5
- 238000005119 centrifugation Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000010438 heat treatment 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
- 238000010521 absorption reaction 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 10
- 229910052799 carbon Inorganic materials 0.000 abstract description 5
- 229910019213 POCl3 Inorganic materials 0.000 abstract description 4
- 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
- 238000004519 manufacturing process Methods 0.000 description 4
- 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
- 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
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
Landscapes
- 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 field 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 POCl3 are reaction raw materials, Potassium Hexafluorophosphate crude product is obtained after initial reaction under certain condition, acidity is adjusted with potassium hydroxide and remove iron ion again, active carbon adsorption is decolourized, crude product after removal of impurities recrystallizes after being concentrated by evaporation, so as to obtain Potassium Hexafluorophosphate finished product, the preparation method of the Potassium Hexafluorophosphate of the present invention, compared with traditional preparation methods, operation is simpler, reaction is more gentle, it is easily controllable, avoid a large amount of unstable, it is corrosive, has the use of virose raw material, so as to reduce the danger of operation, the Potassium Hexafluorophosphate produced through this method, high income is up to 88%, purity is even more to have exceeded 99%.
Description
Technical field
The present invention relates to a kind of synthesis field of inorganic compound, more particularly to a kind of preparation method of Potassium Hexafluorophosphate.
Background technology
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, machine fluorine substituting agent can also be used as, as light gathers
Close catalyst.The preparation method of hexafluorophosphate is greatly developed because of the application of lithium hexafluoro phosphate, after twentieth century
Phase, the U.S., Germany etc., some western countries chemist proposed the imagination that Potassium Hexafluorophosphate prepares lithium hexafluoro phosphate so that hexafluoro
The production technology of potassium phosphate is extremely improved.
At present, the preparation of Potassium Hexafluorophosphate is mostly to be reacted using phosphorus pentafluoride gas and the potassium fluoride solution containing hydrogen fluoride
To carry out, phosphorus pentafluoride is then prepared by phosphorus pentachloride and anhydrous hydrogen fluoride reaction, and its reaction mechanism is：
HF+PCl5→PF5+HCl
PF5+KF→KPF6
Also have using potassium chloride, anhydrous hydrogen fluoride, phosphorus pentachloride reaction to prepare Potassium Hexafluorophosphate, its reaction mechanism is：
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, it is necessary to separate；Phosphorus pentafluoride and fluorination nak response, actually should be anti-with potassium hydrogen fluoride
Should, 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 increase of reaction controlling, it is largely unstable, corrosive, the virose raw material of tool to make
With adding the danger of operation.
During using potassium chloride, anhydrous hydrogen fluoride, phosphorus pentachloride reaction to prepare Potassium Hexafluorophosphate, phosphorus pentachloride solid needs
It is a small amount of repeatedly to add in the mixture of potassium chloride and anhydrous hydrogen fluoride, it is violent due to reacting, thus further increase control
Difficulty, easily trigger dangerous.
Therefore, it is necessary to develop a kind of new Potassium Hexafluorophosphate preparation method, its production process is set to more they tend to can control
Property.
The content of the invention
In order to overcome the above-mentioned deficiencies of the prior art, the present invention proposes a kind of preparation method of Potassium Hexafluorophosphate, makes anti-
Process is answered to be more easily controlled, operation difficulty reduces, while also reduces production cost.
To achieve these goals, the technical solution adopted in the present invention is：
A kind of preparation method of Potassium Hexafluorophosphate, it is characterised in that：This method comprises 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 reacted；
(2) -5 DEG C are adjusted to, vavuum pump is opened and adjusts vacuum, it is in tiny structure to make reaction condition, slowly drop
Add POCl3, control rate of addition, temperature is no more than -2 DEG C, after being added dropwise to complete, continue stirring reaction 30min；
(3) 75-85 DEG C is adjusted to, and vacuum is adjusted to 0.7-0.8Pa, by remaining hydrogen fluoride gas and life
Into HCl gas extract out；
(4) 50% potassium hydroxide solution is slowly added into reacting, pH value is adjusted to 7；
(5) reacted material is cooled to room temperature, Potassium Hexafluorophosphate crude product is obtained after centrifugation；
(6) toward in Potassium Hexafluorophosphate crude product plus water, and activated carbon is added, adjusts pH value to 8 with potassium hydroxide solid, heating
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,
Stirring cooling recrystallization；
(8) after being cooled to room temperature, then through centrifuging, drying 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, the vacuum described in step (2) is 0.5Pa.
Preferably, the dosage of POCl3 described in step (2) is 1.05-1.08 times of theoretical amount.
It is further preferred that the dosage of POCl3 described in step (2) is 1.05 times of theoretical amount.
Preferably, the temperature described in step (3) is 80 DEG C, and is incubated 30min；
Preferably, the temperature being filtered by vacuum described in step (7) is more than 80 DEG C；
Preferably, remaining hydrogen fluoride gas and the HCl gas of generation described in step (3) are through alkali liquor absorption.
Preferably, filtrate remaining in the step (7) can be used for production potassium fluosilicate and potassium fluoborate.
Compared with prior art, the beneficial effects of the invention are as follows：
It is of the invention that potassium hydrogen fluoride or potassium chloride are mainly dissolved using anhydrous hydrogen fluoride, obtain six after phosphorus oxychloride reaction is added dropwise
Fluorophosphoric acid potassium crude product, adjust acidity with potassium hydroxide and remove iron ion, active carbon adsorption is decolourized, and the crude product evaporation after removal of impurities is dense
Recrystallized after contracting, so as to obtain Potassium Hexafluorophosphate finished product, compared with the preparation method of traditional Potassium Hexafluorophosphate, operation is simpler,
Reaction is more gentle, easily controllable, a large amount of unstable, corrosive, the virose raw material of tool uses is avoided, so as to reduce
The danger of operation, the Potassium Hexafluorophosphate produced through this method, for high income up to 88%, purity is even more to have exceeded 99%.
Embodiment
The embodiment of the present invention is described further below.Herein it should be noted that for these implementations
The explanation of mode is used to help understand the present invention, but does not form limitation of the invention.In addition, invention described below
As long as involved technical characteristic does not form conflict can and is mutually combined each other in each embodiment.
Embodiment 1
A kind of preparation method of Potassium Hexafluorophosphate, comprises the following steps：
(1) under the conditions of 0-8 DEG C, 150g anhydrous hydrogen fluorides are added to 78g and dried in potassium hydrogen fluoride solid and are reacted；
(2) -5 DEG C are adjusted to, vavuum pump is opened and vacuum is adjusted to 0.5Pa, makes reaction condition in micro- negative
Pressure, 160g POCl3s are slowly added dropwise, control rate of addition, temperature is no more than -2 DEG C, after being added dropwise to complete, continue stirring reaction
30min；
(3) 80 DEG C are adjusted to, is incubated 30min；And vacuum is adjusted to 0.7Pa, by remaining hydrogen fluoride gas
And the HCl gas of generation is extracted out, neutralized with alkali lye；
(4) 50% potassium hydroxide solution is slowly added into reacting, pH value is adjusted to 7；
(5) reacted material is cooled to room temperature, 181g Potassium Hexafluorophosphate crude products is obtained after centrifugation；
(6) toward in Potassium Hexafluorophosphate crude product plus 300ml water, and proper amount of active carbon is added, pH is adjusted 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 activated carbon, to prevent hexafluoro phosphorus during filtering
Sour potassium product crystallization separates out, and is adjusted to be more than 80 DEG C, is concentrated by evaporation filtrate after the completion of suction filtration, treats that epitaxial occurs in liquid level
When, stirring natural cooling recrystallization；
(8) after being cooled to room temperature, then through centrifuging, drying to obtain 162g Potassium Hexafluorophosphate finished products, yield 88.04%, six
Fluorophosphoric acid potassium content is detected as 99.15%.
Embodiment 2
A kind of preparation method of Potassium Hexafluorophosphate, comprises the following steps：
(1) under the conditions of 0-8 DEG C, 160g anhydrous hydrogen fluorides are added to 78g and dried in potassium hydrogen fluoride solid and are reacted；
(2) -5 DEG C are adjusted to, vavuum pump is opened and vacuum is adjusted to 0.5Pa, makes reaction condition in micro- negative
Pressure, 163g POCl3s are slowly added dropwise, control rate of addition, temperature is no more than -2 DEG C, after being added dropwise to complete, continue stirring reaction
30min；
(3) 80 DEG C are adjusted to, is incubated 30min；And vacuum is adjusted to 0.7Pa, by remaining hydrogen fluoride gas
And the HCl gas of generation is extracted out, neutralized with alkali lye；
(4) 50% potassium hydroxide solution is slowly added into reacting, pH value is adjusted to 7；
(5) reacted material is cooled to room temperature, 182g Potassium Hexafluorophosphate crude products is obtained after centrifugation；
(6) toward in Potassium Hexafluorophosphate crude product plus 300ml water, and proper amount of active carbon is added, pH is adjusted 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 activated carbon, to prevent hexafluoro phosphorus during filtering
Sour potassium product crystallization separates out, and is adjusted to be more than 80 DEG C, is concentrated by evaporation filtrate after the completion of suction filtration, treats that epitaxial occurs in liquid level
When, stirring natural cooling recrystallization；
(8) after being cooled to room temperature, then through centrifuging, drying to obtain 162.5g Potassium Hexafluorophosphate finished products, 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 fluorides are added to 78g and dried in potassium hydrogen fluoride solid and are reacted；
(2) -5 DEG C are adjusted to, vavuum pump is opened and vacuum is adjusted to 0.5Pa, makes reaction condition in micro- negative
Pressure, 165g POCl3s are slowly added dropwise, control rate of addition, temperature is no more than -2 DEG C, after being added dropwise to complete, continue stirring reaction
30min；
(3) 80 DEG C are adjusted to, is incubated 30min；And vacuum is adjusted to 0.8Pa, by remaining hydrogen fluoride gas
And the HCl gas of generation is extracted out, neutralized with alkali lye；
(4) 50% potassium hydroxide solution is slowly added into reacting, pH value is adjusted to 7；
(5) reacted material is cooled to room temperature, 183.7g Potassium Hexafluorophosphate crude products is obtained after centrifugation；
(6) toward in Potassium Hexafluorophosphate crude product plus 300ml water, and proper amount of active carbon is added, pH is adjusted 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 activated carbon, to prevent hexafluoro phosphorus during filtering
Sour potassium product crystallization separates out, and is adjusted to be more than 80 DEG C, is concentrated by evaporation filtrate after the completion of suction filtration, treats that epitaxial occurs in liquid level
When, stirring natural cooling recrystallization；
(8) after being cooled to room temperature, then through centrifuging, drying to obtain 162.8g Potassium Hexafluorophosphate finished products, yield 88.48%,
Hexafluorophosphoric acid potassium content is detected as 99.20%.
Embodiments of the present invention are explained in detail above, but the invention is not restricted to described embodiment.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 within protection scope of the present invention.
Claims (10)
- A kind of 1. preparation method of Potassium Hexafluorophosphate, it is characterised in that：This method comprises 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 reacted；S2, -5 DEG C are adjusted to, open vavuum pump and adjust vacuum, it is in tiny structure to make reaction condition, is slowly added dropwise three Chlorethoxyfos, rate of addition is controlled, temperature is no more than -2 DEG C, after being added dropwise to complete, continue stirring reaction 30min；S3,75-85 DEG C is adjusted to, and vacuum is adjusted to 0.7-0.8Pa, by remaining hydrogen fluoride gas and generation HCl gas is extracted out；S4,50% potassium hydroxide solution is slowly added into reacting, pH value is adjusted to 7；S5, reacted material is cooled to room temperature, Potassium Hexafluorophosphate crude product is obtained after centrifugation；S6, toward in Potassium Hexafluorophosphate crude product plus water, and add activated carbon, adjust pH value to 8 with potassium hydroxide solid, heating stirring Dissolving；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, after being cooled to room temperature, then through centrifuging, drying to obtain Potassium Hexafluorophosphate finished product.
- A kind of 2. 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.
- A kind of 3. 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.
- A kind of 4. preparation method of Potassium Hexafluorophosphate according to claim 2, it is characterised in that：Described in step (2) Vacuum is 0.5Pa.
- A kind of 5. 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.
- A kind of 6. 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.
- A kind of 7. preparation method of Potassium Hexafluorophosphate according to claim 1, it is characterised in that：Described in step (3) Temperature is 80 DEG C, and is incubated 30min.
- A kind of 8. preparation method of Potassium Hexafluorophosphate according to claim 1, it is characterised in that：It is true described in step (7) The temperature that sky filters is more than 80 DEG C.
- A kind of 9. preparation method of Potassium Hexafluorophosphate according to claim 1, it is characterised in that：It is residual described in step (3) Remaining hydrogen fluoride gas and the HCl gas of generation are through alkali liquor absorption.
- A kind of 10. preparation method of Potassium Hexafluorophosphate according to claim 1, it is characterised in that：It is residual in the step (7) Remaining filtrate is used to produce potassium fluosilicate and potassium fluoborate.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN114436292A (en) * | 2022-02-21 | 2022-05-06 | 中船(邯郸)派瑞特种气体股份有限公司 | Treatment method of organic sylvite wastewater |
| CN114590823A (en) * | 2022-03-31 | 2022-06-07 | 河南省氟基新材料科技有限公司 | Preparation method of potassium hexafluorophosphate |
| CN115974106A (en) * | 2022-12-15 | 2023-04-18 | 福建省龙德新能源有限公司 | Sodium hexafluorophosphate and recrystallization method thereof |
| CN116375056A (en) * | 2023-03-31 | 2023-07-04 | 江苏泰际材料科技有限公司 | Potassium hexafluorophosphate and method for preparing potassium hexafluorophosphate |
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| CN102910612A (en) * | 2012-11-05 | 2013-02-06 | 中国海洋石油总公司 | Method for preparing lithium hexafluorophosphate |
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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 |
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| 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 |
| CN115974106A (en) * | 2022-12-15 | 2023-04-18 | 福建省龙德新能源有限公司 | Sodium hexafluorophosphate and recrystallization method thereof |
| 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 |
| CN116375056A (en) * | 2023-03-31 | 2023-07-04 | 江苏泰际材料科技有限公司 | Potassium hexafluorophosphate and method for preparing potassium hexafluorophosphate |
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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 |