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Process for production of hexafluorophosphates

A technology of hexafluorophosphate and manufacturing method, applied in lithium hexafluorophosphate, chemical instruments and methods, phosphorus compounds, etc., can solve the problems of expensive raw materials, high manufacturing cost, poor handling, etc., and achieve high safety and electrical characteristics. great effect

Inactive Publication Date: 2011-06-22
STELLA CHEMIFA CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] However, the methods described in Non-Patent Document 1 and Patent Document 1 have the following problems: since phosphorus pentachloride is a solid with high hygroscopicity, its handling property is deteriorated, and its operability is poor in terms of feeding raw materials into manufacturing equipment, etc. , it is also difficult to mechanize
[0009] The production method of hexafluorophosphate mentioned above has various problems such as poor operability, harsh reaction conditions, use of expensive raw materials, and disposal of by-products.
Therefore, the manufacturing cost becomes higher

Method used

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  • Process for production of hexafluorophosphates
  • Process for production of hexafluorophosphates
  • Process for production of hexafluorophosphates

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0107] 1000 g of ultrapure water was charged into a 5 L reaction tank made of fluororesin, the reaction tank was heated with an oil bath, and the ultrapure water was kept at 40°C. This ultrapure water was stirred with a rotor, while adding 800 g of commercially available acidic ammonium fluoride (NH 4 F·(HF)), to dissolve it.

[0108] Next, the temperature of the solution in the reaction tank was kept at 40°C, and at the same time, the POF 3 Air bubbles to absorb 740g POF 3 gas. The absorption amount was obtained from the increase in the weight of the reaction solution. absorbing POF 3 After degassing, stirring was continued for 2 hours to bring the temperature of the reaction liquid to 20° C., and then the liquid temperature was kept constant.

[0109] Next, the reaction tank was heated with an oil bath, and the solution in the reaction tank was evaporated to dryness. Residual crystals in the reaction tank were recovered, washed with 750 g of 75% HF aqueous solution, an...

Embodiment 2

[0112] Put 100g of acidic potassium fluoride (KF (HF)) and 500g of semiconductor grade 75% by weight hydrogen fluoride (HF) solution together with the rotor into a 3L reaction tank made of fluororesin (PFA), stir under ice bath to make KF (HF) ) dissolved. Weigh again 140g 85% by weight phosphoric acid (H 3 PO 4 ) solution in a separatory funnel, slowly drop it over 30 minutes under an ice bath, and stir to allow it to react for 6 hours.

[0113] Next, the solution was cooled at -5°C for 24 hours to precipitate crystallization. Thus, a hydrogen fluoride solution in which a precipitate was precipitated was obtained. This hydrogen fluoride solution is filtered off by suction filtration. The liquid temperature of the hydrogen fluoride solution at this time was -5°C. In addition, when the HF concentration of the filtrate was quantified, it was 46% by weight.

[0114] The recovered crystals were washed with 600 g of semiconductor grade 75% by weight hydrogen fluoride (HF) sol...

Embodiment 3

[0119] Put 210g of cesium fluoride (CsF) and 700g of semiconductor-grade 75% by weight hydrogen fluoride (HF) solution together with the rotor into a 3L PFA reaction vessel, and stir in an ice bath to dissolve the CsF. Weigh again 175g 85% by weight phosphoric acid (H 3 PO 4 ) solution in a separatory funnel, slowly drip it in 30 minutes under an ice bath, and stir to make it react for 12 hours.

[0120] Next, the solution was cooled at -5°C for 36 hours to precipitate crystallization. Thus, a solution in which a precipitate had been precipitated was obtained. The solution is then filtered off with suction. The liquid temperature of the phosphoric acid solution at this time was -5 degreeC. In addition, when the HF concentration of the filtrate was quantified, it was 55% by weight.

[0121] The recovered crystals were washed with 400 g of anhydrous hydrofluoric acid cooled to 0°C. Next, the washed filtrate was transferred to a 3L fluororesin flask, and high-purity N was b...

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Abstract

Provided are a process for production of hexafluorophosphates by which inexpensive high-quality hexafluorophosphates can be easily produced with production cost control; an electrolytic solution containing a hexafluorophosphate; and an electricity storage device equipped with the electrolytic solution. The process for production of hexafluorophosphates is characterized by reacting at least a phosphorus compound with a fluoride represented by chemical formula: MFsr(HF) [wherein 0=r=6; 1=s=3; and M is at least one selected from the group consisting of Li, Na, K, Rb, Cs, NH4, Ag, Mg, Ca, Ba, Zn, Cu, Pb, Al and Fe] to form a hexafluorophosphate represented by chemical formula: M(PF6)s.

Description

technical field [0001] The present invention relates to a method for producing hexafluorophosphoric acid and an apparatus for producing the same. More specifically, the present invention relates to a method for producing hexafluorophosphate that can be applied to an electrolytic solution of an electric storage device, an electrolytic solution containing hexafluorophosphate, and an electrolytic solution having the same Electrolyte storage element. Background technique [0002] in reducing CO as 2 Lithium-ion secondary batteries are given a position as a key device in hybrid or electric vehicles that are expected to be the killer feature of emissions. Examples of the electrolyte of this lithium ion secondary battery include lithium hexafluorophosphate, which is highly safe and has excellent electrical characteristics. Hexafluorophosphates including this lithium hexafluorophosphate are all referred to as phosphorus pentafluoride "PF 5 " is used as a starting material for man...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/455H01M10/36H01M10/0568
CPCC01B25/455C01D13/00H01M10/0525H01M10/0568Y02E60/12Y02T10/7011C01D15/005Y02E60/10H01M10/36Y02T10/70
Inventor 脇雅秀薮根辰弘宫本和博平野一孝
Owner STELLA CHEMIFA CORP
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