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Method for producing hexafluorophosphate salt

A technology of hexafluorophosphate and its manufacturing method, which is applied in lithium hexafluorophosphate, chemical instruments and methods, and phosphorus compounds, and can solve problems such as difficult control of the reaction, danger, and difficulty in removing hexafluorophosphoric acid crystals, and achieve the effect of simple operation

Inactive Publication Date: 2009-12-16
STELLA CHEMIFA CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] However, in this method, since the reaction between phosphorus pentoxide and anhydrous hydrogen fluoride is violent, it is very dangerous, and it is extremely difficult to control the reaction.
Furthermore, there is a disadvantage that the handleability is not good due to the use of extremely hygroscopic phosphorus pentoxide
That is, it is considered that from the hexafluorophosphate anion (PF 6 - ) It is very difficult to simply remove hexafluorophosphoric acid crystals (solid) from aqueous solution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0075] Put 160g of acidic potassium fluoride (KF·(HF)) and 700g of semiconductor-grade 75% by weight hydrofluoric acid (HF) into a 3L reaction tank made of fluororesin (PFA) together with the rotor, and place in an ice bath Under stirring, dissolve KF (HF). And then, measure 85% by weight of 175g phosphoric acid (H 3 PO 4), slowly drop it in for 30 minutes under ice bath, and make it react for six hours under stirring.

[0076] Thereafter, it was cooled to -5°C and crystallization was carried out for 24 hours. Next, the obtained precipitate was filtered by suction filtration. The HF concentration of the filtrate at this time was measured to be 55% by weight. In addition, the recovered crystals were washed with 400 g of pure water. Furthermore, drying was performed at 105 degreeC for 12 hours after that. The yield of the crystals obtained was 156 g (56% yield). Furthermore, XRD measurements of the resulting crystals were performed, showing that KPF 6 . Also, regarding ...

Embodiment 2

[0078] The filtrate of Example 1 was completely concentrated at 120°C over 24 hours. The concentrated liquid is a slightly viscous white cloudy liquid. Add this liquid to the reaction tank made of 3L PFA, and then add 75% by weight of 200g of H 3 PO 4 Let it dissolve. On the other hand, 550 g of semiconductor-grade 75% by weight HF was put into another container, and while cooling in an ice bath, 145 g of KF·(HF) was slowly added and dissolved under stirring. The hydrofluoric acid solution and phosphoric acid aqueous solution were respectively transferred to a separatory funnel, and were dropped while stirring in an ice bath for 15 minutes. This solution was cooled to -40°C, and crystallization was carried out for 48 hours.

[0079] Next, the obtained precipitate was filtered by suction filtration. The HF concentration of the filtrate at this time was measured to be 48% by weight. In addition, the recovered crystals were washed with 400 g of pure water. Furthermore, dry...

Embodiment 3

[0081] Put 160g of KF·(HF) and 940g of industrial grade 55% by weight HF into a reaction tank made of 3L PFA together with the rotor, and stir under an ice bath to dissolve KF(HF). Furthermore, measure 85% by weight of 175g of H in another container 3 PO 4 , while stirring in a water bath at 20° C., an aqueous phosphoric acid solution was added in one go. In this state, reaction and crystallization were carried out for 4 hours. Next, the obtained precipitate was filtered by suction filtration. The HF concentration of the filtrate at this time was measured to be 42% by weight. In addition, the recovered crystals were washed with 400 g of pure water. Furthermore, drying was performed at 105 degreeC for 24 hours after that. The results of XRD measurements on the obtained crystals are shown as KPF 6 . The output of obtained crystal is 53g, and yield is 19% (not including the KPF dissolved in the cleaning solution 6 Yield). Furthermore, regarding the obtained KPF 6 The mo...

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PUM

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Abstract

Disclosed is a method for producing a hexafluorophosphate salt (MPF6: M = Li, Na, K, Rb, Cs, NH4, Ag), which uses at least an aqueous HxPOyFz solution, an aqueous hydrofluoric acid solution and MF r(HF) as raw materials (provided that r >= 0, 0 <= x <= 3, 0 <= y <= 4 and 0 <= z <= 6). This method enables to produce a hexafluorophosphate salt (MPF6: M = Li, Na, K, Rb, Cs, NH4, Ag) having excellent workability at low cost from easily available raw materials, and the reaction can be controlled in this method.

Description

technical field [0001] The present invention relates to a method for producing hexafluorophosphate useful as an electrolyte for batteries, a catalyst in organic synthesis reactions, and the like. Background technique [0002] Hexafluorophosphate DPF 6 (D=Li, Na, K, etc.) are used as electrolyte solutions of batteries. Furthermore, when D=Ag, it attracts attention as a counter ion that generates an acid necessary for the initiation of photopolymerization and the growth reaction. Further, D=NH 4 When used, it is useful as a raw material used in the manufacture of pharmaceutical intermediates. [0003] Hexafluorophosphate DPF in solid state 6 Generally, it is a compound that is unstable to water. If there is water in the reaction system, the by-product fluorine oxyphosphate DPO will be generated. a f b , In addition, hexafluorophosphate will be decomposed into DF or DF·c(HF). Among them, especially when lithium hexafluorophosphate, silver hexafluorophosphate, etc. are pl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/455
CPCC01D13/00C01B25/455C01D15/005
Inventor 脇雅秀宫本和博青木谦治
Owner STELLA CHEMIFA CORP
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