CN106477541A - A kind of high-purity phosphorus pentafluoride gas preparation method - Google Patents
A kind of high-purity phosphorus pentafluoride gas preparation method Download PDFInfo
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- CN106477541A CN106477541A CN201610840216.8A CN201610840216A CN106477541A CN 106477541 A CN106477541 A CN 106477541A CN 201610840216 A CN201610840216 A CN 201610840216A CN 106477541 A CN106477541 A CN 106477541A
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- potassium
- phosphorus pentafluoride
- hydrogen fluoride
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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
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/10—Halides or oxyhalides of phosphorus
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- Inorganic Chemistry (AREA)
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Abstract
The present invention relates to a kind of new high-purity phosphorus pentafluoride gas preparation method.The present invention to prepare highly purified phosphorus pentafluoride using Potassium Hexafluorophosphate, and reaction is gently controlled, and potassium bifluoride can be with recovery, suitable industrialized production.Phosphorus pentafluoride (PF5) be widely used in the fields such as electronics industry, battery manufacture, macromolecular material and catalyst.
Description
Technical field
The present invention relates to a kind of new high-purity phosphorus pentafluoride gas preparation method, belong to technical field of fine.
Technical background
Phosphorus pentafluoride (PF5) have in the fields such as electronics industry, battery manufacture, macromolecular material and catalyst and widely should
With.With PF5LiPF for raw material preparation6It is the main electrolyte of lithium ion battery, its service life and the more traditional electricity of charging times
Solution matter dramatically increases.PF5Synthetic method be broadly divided into direct method and 2 kinds of indirect method, by making red phosphorus and F in direct method2Directly
The method of reaction can get purity and the high PF of selectivity5Product, is particularly suitable for manufacturing high-purity LiPF6Electrolyte.At present
Industrial widely used method is to make PCl5Or P2O5React with HF, the advantage of the method be raw material be easy to get, process is simple and easily
In control.Due to PF5Close with HCl boiling point it is impossible to be separated with common distillation, industrial adopt distillation under pressure or absorption more
Method is refined.These methods are difficult to industrialization, need to develop one kind and be easy to industrialized technical matters.
Content of the invention
The purpose of the present invention is a kind of synthesis technique being suitable for industrialized phosphorus pentafluoride.Its reaction equation is as follows：
KCl+2HF→KHF2+HCl
KHF2+4HF+H3PO4→KPF6↓+4H2O
KPF6+HF(g)→PF5↑+KHF2
Prepared by potassium hydrogen fluoride：The potassium chloride solution of saturation is added in the reactor of liner tetrafluoro, controls temperature to exist
80-85 DEG C, it is passed through hydrogen fluoride gas, reacts 5-6 hour, reaction produces potassium hydrogen fluoride liquid.
Prepared by Potassium Hexafluorophosphate：Potassium hydrogen fluoride liquid cooling, to room temperature, adds in the reactor of another liner tetrafluoro,
85% phosphoric acid of Deca metering, stirring at normal temperature is reacted 6 hours, has Potassium Hexafluorophosphate solid to produce, sucking filtration, filter cake distillation washing
Wash 2 times, vacuum drying obtains Potassium Hexafluorophosphate finished product.
Prepared by phosphorus pentafluoride：The Potassium Hexafluorophosphate being dried is put in the fixed bed reactors of a liner tetrafluoro, is heated to 60
DEG C, it is passed through dry hydrogen fluoride gas, produce phosphorus pentafluoride gas, through entering the condenser of logical chilled brine, then through an exsiccator,
Obtain highly purified phosphorus pentafluoride.Side-product potassium hydrogen fluoride in fixed bed reactors reclaims and is used for preparing Potassium Hexafluorophosphate.
Invention advantage:
The innovative point of the present invention is to prepare highly purified phosphorus pentafluoride using Potassium Hexafluorophosphate, and reaction is gently controlled,
Potassium bifluoride can be with recovery, suitable industrialized production.
Specific embodiment：
New high-purity phosphorus pentafluoride gas preparation method a kind of to the present invention, is specifically described by the following examples
Or be described further, its object is to be better understood from the technical connotation of the present invention, but protection scope of the present invention does not limit
In following practical range.
Embodiment 1
Add 50g potassium chloride and 150g distilled water in tetra- mouthfuls of tetrafluoro flasks of 500ml, be heated to 80 DEG C, be passed through fluohydric acid gas
Gas 81g, stirring reaction 5 hours, obtain potassium hydrogen fluoride aqueous solution.It is cooled to room temperature, be slowly added dropwise 85% phosphoric acid 75g, room temperature
Stirring reaction 6 hours, has Potassium Hexafluorophosphate solid to produce, after reaction terminates, sucking filtration, and filter cake 50ml distilled water rinsing 2 times, very
Sky is dried to obtain Potassium Hexafluorophosphate finished product 49.7g, yield 95%, product purity 99.0%.
Dry Potassium Hexafluorophosphate solid 100g is taken to be placed in the fixed bed reactors of liner tetrafluoro, fixed bed reactors are
F25 × 100, are heated to 60 DEG C, are passed through dry hydrogen fluoride gas, and reactor outlet is phosphorus pentafluoride gas and hydrogen fluoride gas
Mixed gas, mixed gas enter the condenser of logical -15 DEG C of chilled brines, then through an exsiccator, obtain highly purified five fluorinations
Phosphorus, purity is 99.5%.Side-product potassium hydrogen fluoride in fixed bed reactors reclaims and is used for preparing Potassium Hexafluorophosphate.
Embodiment 2
Add 600g potassium chloride and 250g distilled water in 5L liner tetrafluoro reaction bulb, be heated to 85 DEG C, be passed through fluohydric acid gas
Gas 1000g, stirring reaction 5 hours, obtain potassium hydrogen fluoride aqueous solution.It is cooled to room temperature, be slowly added dropwise 85% phosphatase 79 00g, often
Warm stirring reaction 6 hours, has Potassium Hexafluorophosphate solid to produce, after reaction terminates, sucking filtration, and filter cake rinses 2 with 500ml distilled water
Secondary, vacuum drying obtains Potassium Hexafluorophosphate finished product 600g, yield 97%, product purity 99.1%.
Dry Potassium Hexafluorophosphate solid 1000g is taken to be placed in the fixed bed reactors of liner tetrafluoro, fixed bed reactors
For F50 × 200, it is heated to 65 DEG C, is passed through dry hydrogen fluoride gas, reactor outlet is phosphorus pentafluoride gas and fluorination hydrogen
Body mixed gas, mixed gas enter the condenser of logical -15 DEG C of chilled brines, then through an exsiccator, obtain highly purified five fluorine
Change phosphorus, purity is 99.5%.Side-product potassium hydrogen fluoride in fixed bed reactors reclaims and is used for preparing Potassium Hexafluorophosphate.
Embodiment 3
In 5m3In the reactor of liner tetrafluoro, 500Kg potassium chloride and 2500Kg distilled water, are heated to 85 DEG C, are passed through fluorination
Hydrogen 1000kg, stirring reaction 6 hours, obtain potassium hydrogen fluoride aqueous solution.It is cooled to room temperature, be slowly added dropwise 85% phosphoric acid
1000kg, stirring at normal temperature is reacted 6 hours, has Potassium Hexafluorophosphate solid to produce, and after reaction terminates, centrifuge separates, filter cake
Rinsed 2 times with 500kg distilled water, vacuum drying obtains Potassium Hexafluorophosphate finished product 500kg, yield 95.6%, product purity
99.0%.
Dry Potassium Hexafluorophosphate solid 500kg is taken to be placed in the fixed bed reactors of liner tetrafluoro, fixed bed reactors
For F200 × 1500, it is heated to 65 DEG C, is passed through dry hydrogen fluoride gas, reactor outlet is phosphorus pentafluoride gas and fluohydric acid gas
Gas mixing gas, mixed gas enter the condenser of logical -15 DEG C of chilled brines, then through an exsiccator, obtain highly purified five
Fluorination phosphorus, purity is 99.5%.Side-product potassium hydrogen fluoride in fixed bed reactors reclaims and is used for preparing Potassium Hexafluorophosphate.
Claims (3)
1. a kind of new high-purity phosphorus pentafluoride gas preparation method, to prepare highly purified five fluorinations using Potassium Hexafluorophosphate
Phosphorus, reaction is gently controlled, and potassium bifluoride can be with recovery, suitable industrialized production.
2. high-purity phosphorus pentafluoride gas preparation method according to claim 1, Potassium Hexafluorophosphate is anti-with hydrogen fluoride gas
Should, using fixed bed reactors.
3. according to claim 2, fixed bed reactors heating-up temperature is 60-65 DEG C；By-product potassium hydrogen fluoride reclaims circulation
Using being used for preparing Potassium Hexafluorophosphate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610840216.8A CN106477541A (en) | 2016-09-21 | 2016-09-21 | A kind of high-purity phosphorus pentafluoride gas preparation method |
Applications Claiming Priority (1)
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| CN201610840216.8A CN106477541A (en) | 2016-09-21 | 2016-09-21 | A kind of high-purity phosphorus pentafluoride gas preparation method |
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| CN201610840216.8A Pending CN106477541A (en) | 2016-09-21 | 2016-09-21 | A kind of high-purity phosphorus pentafluoride gas preparation method |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101605721A (en) * | 2007-02-08 | 2009-12-16 | 斯泰拉化工公司 | The manufacture method of phosphorus pentafluoride and hexafluorophosphate |
| CN102105394A (en) * | 2008-08-08 | 2011-06-22 | 斯泰拉化工公司 | Processes for production of phosphorus pentafluoride and hexafluorophosphates |
-
2016
- 2016-09-21 CN CN201610840216.8A patent/CN106477541A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101605721A (en) * | 2007-02-08 | 2009-12-16 | 斯泰拉化工公司 | The manufacture method of phosphorus pentafluoride and hexafluorophosphate |
| CN102105394A (en) * | 2008-08-08 | 2011-06-22 | 斯泰拉化工公司 | Processes for production of phosphorus pentafluoride and hexafluorophosphates |
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Application publication date: 20170308 |
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