Method for producing phosphorus pentafluoride

A manufacturing method, phosphorus pentafluoride technology, applied in chemical instruments and methods, lithium hexafluorophosphate, phosphorus halide/oxyhalide, etc., can solve the problems of prolonging the residence time of the reactor, danger, unsatisfactory manufacturing method, etc.

Inactive Publication Date: 2013-06-12
DAIKIN IND LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since this method performs a three-stage reaction, the residence time in the reactor must be prolonged, and as a result, a large reactor is required, which is not ideal as an industrial-scale production method.
[0008] In the following patent document 3, a method of simultaneously reacting phosphorus trichloride, chlorine gas, and hydrogen fluoride is described, but the method specifically described is a method in which raw materials are put into a reactor with a pressure-resistant specification at one time and reacted in batches. In this method, because the heat of reaction is very large, it is extremely difficult to control the reaction temperature, which is very dangerous.
[0009] As mentioned above, with regard to the production method of phosphorus pentafluoride, a method capable of producing inexpensively and efficiently on an industrial scale has not yet been established.

Method used

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Examples

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Embodiment 1

[0059] A tubular heat-resistant and corrosion-resistant nickel-based alloy reactor with an inner diameter of 20 mm and a length of 400 mm is filled with high-alumina balls with a diameter of 4.5 mm. The reaction tube is maintained at an absolute pressure of 0.1MPa and 100°C, anhydrous hydrogen fluoride at 150ml / min (0°C, flow rate at 0.1MPa), and chlorine gas at 23ml / min (0°C, flow rate at 0.1MPa) at the same time After supplying to the reactor, phosphorus trichloride obtained by bubbling 35 ml / min (flow rate at 0° C., 0.1 MPa) of dry nitrogen into phosphorus trichloride heated to 41° C. was supplied. At this time, the supply rate of phosphorus trichloride calculated from the vapor pressure was 15 ml / min (flow rate at 0° C. and 0.1 MPa).

[0060] In order to quantify phosphorus pentafluoride, R14 (CF 4 ) gas, the gas at the outlet of the reactor was quantitatively analyzed by FT-IR, and it was confirmed that phosphorus trichloride was almost quantitatively converted into phos...

Embodiment 2

[0062] Nickel balls with a diameter of 2 mm are filled in a tubular heat-resistant and corrosion-resistant nickel-based alloy reactor with an inner diameter of 20 mm and a length of 400 mm. The reaction tube is maintained at an absolute pressure of 0.1MPa and 50°C, anhydrous hydrogen fluoride at 450ml / min (0°C, flow rate at 0.1MPa), and chlorine gas at 45ml / min (0°C, flow rate at 0.1MPa) at the same time After supplying to the reactor, phosphorus trichloride was supplied at 0.2 g / min using a liquid delivery pump.

[0063] In order to quantify phosphorus pentafluoride, R14 (CF 4 ) gas, the gas at the outlet of the reactor was quantitatively analyzed by FT-IR, and it was confirmed that phosphorus trichloride was almost quantitatively converted into phosphorus pentafluoride.

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Abstract

The present invention provides a method for producing phosphorus pentafluoride, which is characterized by having a phosphorus trihalide represented by general formula PX3 (wherein X represents F, Cl or Br) react with a molecular halogen or hydrogen fluoride that is in a gaseous state. This method is a method for efficiently producing phosphorus pentafluoride at low cost, which is applicable to the production on an industrial scale.

Description

technical field [0001] The present invention relates to a method for producing phosphorus pentafluoride and a method for producing lithium hexafluorophosphate. Background technique [0002] Phosphorus pentafluoride (PF 5 ) is a useful substance as a raw material of lithium hexafluorophosphate which can be used as an electrolyte of a lithium battery, a lithium ion secondary battery, or the like. [0003] As a method for producing phosphorus pentafluoride, for example, phosphorus pentachloride (PCl 5 ) and calcium fluoride (CaF 2 ) reaction method (Non-Patent Document 1), a method of reacting phosphorus pentachloride with hydrogen fluoride (HF) (Patent Document 1), and other methods using phosphorus pentachloride as a raw material. [0004] However, phosphorus pentachloride is not only very hygroscopic, but also easily hydrolyzed and easily reacts with moisture in the air to generate corrosive hydrogen chloride gas (HCl). As a result, the purity of phosphorus pentachloride ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/10C01B25/455
CPCC01B25/10C01D15/005Y02E60/10C01B25/455H01M4/582
Inventor 铃木敦田窪征司
Owner DAIKIN IND LTD
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