Method for preparing high purity phosphorus pentafluoride gas

A technology of phosphorus pentafluoride and phosphorus pentoxide, which is applied in the direction of phosphorus halide/oxyhalide, can solve the problems of high impurities in products, difficulties in separation and purification, and the introduction of many impurities, so as to facilitate the implementation of industrialization and process equipment Simplicity and the effect of increasing the reaction yield

Inactive Publication Date: 2009-03-25
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] Solvents are used in the traditional preparation methods. Due to the inherent characteristics of the solvent method, the prepared products have high impurities and are difficult to separate and purify; while the indirect method prepares PF 5 The process is

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Put phosphorus pentoxide into a stainless steel reaction kettle lined with polytetrafluoroethylene and equipped with stirring equipment and a cooling jacket, and use high-purity argon to drive out the air in the kettle; % of anhydrous hydrogen fluoride, the reaction time is 3h; after the reaction is completed, continue to maintain the temperature in the kettle at -20°C, and intermittently add an excess of 35% of 60% fuming sulfuric acid to the kettle while stirring until the addition is complete; After pure argon drives away the air in the closed pressure heating furnace (phosphorus pentafluoride generation furnace), the reaction intermediate product is introduced into the furnace, the temperature is controlled at 120±5°C, the gas pressure is 1.0±0.1MPa, and the reaction time is 0.5h; the heating is complete Finally, the product is introduced into a condenser to cool and remove impurities to obtain high-purity phosphorus pentafluoride; the cooling medium is industrial li...

Embodiment 2

[0027] Put phosphorus pentoxide into a stainless steel reaction kettle lined with polytetrafluoroethylene and equipped with stirring equipment and a cooling jacket, and use high-purity argon to drive out the air in the kettle; maintain the temperature in the kettle at 0°C, and feed an excess of 60% anhydrous hydrogen fluoride, and the reaction time is 5 hours; after the reaction is completed, continue to maintain the temperature in the kettle at -10°C, and intermittently add an excess of 40% of 60% fuming sulfuric acid to the kettle while stirring until the addition is complete; use high-purity After the argon gas drives away the air in the closed pressure heating furnace (phosphorus pentafluoride generation furnace), the reaction intermediate product is introduced into the furnace, the temperature is controlled at 150±5°C, the gas pressure is 1.2±0.1MPa, and the reaction time is 1.0h; after heating is complete , the product is introduced into a condenser to cool and remove imp...

Embodiment 3

[0030] Conditions as described in Example 2, adding a secondary condensation process at the end of the reaction, industrial liquid nitrogen as the cooling medium, and other reaction conditions are the same.

[0031] The reaction yield is over 98%, and the obtained product phosphorus pentafluoride can reach: PF 5 The main content is greater than 99.99%, the water content is less than 5ppm, and the HF content is less than 40ppm.

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PUM

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Abstract

The invention discloses a preparation method of high-pure phosphorus pentafluoride gas, which comprises: phosphorus pentoxide is put into a reaction container lined with PTFE and is introduced with anhydrous hydrogen fluoride, and the temperature is preserved to be minus 20 to 0 DEG C; according to the chemical reaction counting, the anhydrous hydrogen fluoride is overdosed by 50 to 60 percent; the reaction is carried out for 3 to 5 hours. After the reaction is completed, 60 percent of oleum is added in an intermittent way with stirring and the dosage of the oleum is 35 to 40 percent more than a theoretic value. The intermediate outcome of the reaction is heated for decomposing under the temperature of 120 to 150 DEG C so as to generate the phosphorus pentafluoride; the product is guided into a condenser for cooling the impurity and then the high-pure phosphorus pentafluoride is obtained. The content of PF<5> obtained by the method is greater than 99.9 percent, the content of impurity is low, the water content is less than 10ppm, HF content is less than 50ppm; moreover, the process equipment is comparatively simple, thus being beneficial to the industrial manufacturing.

Description

technical field [0001] The invention relates to the preparation of high-purity phosphorus pentafluoride gas. Background technique [0002] Phosphorus pentafluoride (PF 5 ) is a colorless and odorless gas under normal conditions, with a melting point of -93.78°C and a boiling point of -84.5°C. As a fluorinating agent, PF 5 It can perform ion transfer and is widely used in the fields of electronics industry, battery manufacturing, polymer materials and catalysts. [0003] At present, lithium hexafluorophosphate has become the mainstream as the electrolyte salt of lithium-ion batteries, while PF 5 Lithium hexafluorophosphate with excellent performance can be prepared as a raw material, making PF 5 The preparation of is more research and strategic. Domestic related PF 5 The research is almost blank, and a few companies produce commercial PF 5 All manufacturers adopt foreign technology. This has led to the fact that my country's lithium-ion batteries have been highly mono...

Claims

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Application Information

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IPC IPC(8): C01B25/10
Inventor 李新海刘建文王志兴郭华军彭文杰胡启阳
Owner CENT SOUTH UNIV
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