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Processes for producing phosphorus pentafluoride and hexafluorophosphate

A technology of hexafluorophosphate and its manufacturing method, which is applied in lithium hexafluorophosphate, chemical instruments and methods, separation methods, etc., which can solve the problems of fast reaction speed, high manufacturing cost, violent reaction, etc., 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

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Problems solved by technology

[0009] Non-Patent Document 2 (using ClF in liquid HF medium 3 Phosphorus fluorination carried out) and the reactions described in Patent Document 4 and Non-Patent Document 5 (phosphorus fluorination using fluorine gas) have such problems: the reaction rate of these reactions is fast and the reaction proceeds violently, so the control of the reaction very difficult
However, as mentioned above, the manufacturing method of phosphorus pentafluoride is complicated
And even if it starts from a low-priced raw material, it is necessary to purify the generated phosphorus pentafluoride, so the production cost of phosphorus pentafluoride is high, making hexafluorophosphate as an electrolyte an expensive substance

Method used

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  • Processes for producing phosphorus pentafluoride and hexafluorophosphate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0115] use figure 1 The apparatus shown performs the following implementations.

[0116] Commercially available potassium hexafluorophosphate (KPF 6 ) 50g and anhydrous hydrogen fluoride (HF) 2000g together with the rotor into a 5L reaction tank made of fluororesin (PFA), connected to a reflux tower made of SUS316 (20mm )superior. While heating the PFA reaction tank with a water bath so that the external temperature of the reaction tank reached 45°C, the reflux tower was cooled with -50°C brine. Furthermore, the reaction solution was stirred with a magnetic stirrer. As soon as the temperature of the water bath rises, the HF starts to reflux. At this time, the internal HF temperature was 21°C.

[0117] After 5 minutes, gas started to evolve from the reflux column, which was analyzed by FTIR. The result is that it is confirmed as PF 5 and a small amount of HF.

Embodiment 2

[0119] Lithium hexafluorophosphate (LiPF 6 ) 330g and anhydrous HF 2000g together with the rotor into the reaction tank made of 5LPFA, connected to the reflux tower made of SUS316 (20mm )superior. While heating the PFA reaction tank to 80°C with a water bath, the reflux tower was cooled with 0°C brine. Furthermore, the reaction solution was stirred with a magnetic stirrer. As soon as the temperature of the water bath rises, the HF starts to reflux. At this time, the internal HF temperature was 30°C.

[0120] The gas generated from the reflux tower was analyzed by FTIR and confirmed to be PF 5 and a small amount of HF. In addition, the gas generated at the same time was absorbed with pure water for 4 hours, the content of P in the absorption liquid was measured, and the generated PF was calculated. 5 The gas weight was 205g, and 75% was formed.

Embodiment 3

[0122] Ammonium hexafluorophosphate (NH 4 PF 6 ) 90g and anhydrous HF 2000g are added together with the rotor into a reaction tank made of 5LPFA, and the reaction solution is stirred with a magnetic stirrer. Embodiment 3 is carried out without setting the reflux tower. The generated gas was analyzed by FTIR while being absorbed by pure water. When the PFA reaction tank is heated to 65°C with a water bath, hydrogen fluoride evaporates and reacts violently with pure water as the absorbing liquid. The generated gas was analyzed by FTIR and confirmed to be PF 5 and lots of HF. Absorb with pure water for 6 hours, measure the content of P in the absorption liquid, and calculate the generated PF 5 The gas weight was 43g, and 62% was formed.

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Abstract

A process for phosphorus pentafluoride production by which high-purity phosphorus pentafluoride can be produced by a simple and economical procedure without the need of a large-scale purification apparatus or high-pressure apparatus and without generating a large amount of a by-product gas requiring a special discharge-gas treatment. The process for phosphorus pentafluoride production is characterized by introducing hydrogen fluoride and a hexafluorophosphate (MPF 6 ) into a vessel and reacting them according to the reaction shown by the scheme (1) to yield phosphorus pentafluoride. MPF 6 + uHF PF 5 + MF r(HF) (Scheme 1) In the scheme, M is at least any one of Li, Na, K, Rb, Cs, NH 4 , and Ag; 0<=r<=u; and the HF is used in an amount not smaller than the stoichiometric amount.

Description

technical field [0001] The present invention relates to a method for producing phosphorus pentafluoride and hexafluorophosphate. More specifically, it relates to a method for producing hexafluorophosphate useful as a battery electrolyte, a catalyst for organic synthesis reactions, and the like, and a method for producing phosphorus pentafluoride used as a starting material for producing hexafluorophosphate. Background technique [0002] Phosphorus pentafluoride (PF 5 ) is a substance that is a gas at room temperature and is used as a fluorinating agent in various chemical reactions in the electronics industry. Especially for the manufacture of hexafluorophosphate DPF for battery electrolyte 6 (D = Li, Na, K, etc.) starting material. In the case where D=Li, lithium hexafluorophosphate is an important substance as an electrolyte of a lithium battery. Lithium hexafluorophosphate is particularly safe and has excellent physical properties. It is considered an indispensable su...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/10B01D53/14B01D53/68B01D53/77C01B25/455
CPCC01D15/005C01B25/10C01B25/455
Inventor 脇雅秀宫本和博青木谦治
Owner STELLA CHEMIFA CORP
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