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Preparation method of phosphorus pentafluoride

A technology of phosphorus pentafluoride and phosphorus pentoxide, applied in the direction of phosphorus halide/oxyhalide, etc., can solve the problems of environmental pollution by reaction by-products, achieve simple process and equipment structure, non-toxic raw materials, and high reliability Effect

Inactive Publication Date: 2012-06-20
HUAHE NEW TECH DEV COMPANY RES INST OF PHYSICAL & CHEM ENG OF NUCLEAR IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] The above method was once an important method for the traditional preparation of phosphorus pentafluoride, but due to the serious environmental pollution caused by the reaction by-products, this method has now been discontinued

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0036] A preparation method of phosphorus pentafluoride, comprising the following steps:

[0037] (i) dry

[0038] Heat the horizontal reactor with stirring device to 90-110°C, keep it for 0.4-0.6 hours, and remove the moisture in the reactor and pipeline.

[0039] (ii) Feeding

[0040] In a dry environment, under the protection of an inert gas, quickly add solid powder phosphorus pentoxide and solid powder calcium fluoride into a horizontal reactor with a stirring device while hot.

[0041] (iii) Evacuation

[0042] Close the reactor, evacuate the reactor to -0.09~-0.11MPa, close the evacuation valve, observe for a period of time, if the pressure does not rise, it is considered that the reactor is not leaking, and the following operations can be performed.

[0043] (ⅳ) Synthesis reaction

[0044] Heat the reactor, the reaction temperature is controlled at 200-300°C, and the reactor pressure is controlled at

[0045] -0.1~0 MPa, the reaction time is more than 3 hours,...

Embodiment 1

[0056] The horizontal reactor with stirring device was heated to 90°C and kept for 0.4 hour to remove the moisture in the reactor and the pipeline.

[0057] In a dry environment, under the protection of an inert gas, quickly add 1 kg of phosphorus pentoxide and 0.5 kg of calcium fluoride into a horizontal reactor with a stirring device while hot, and close the reactor. Nitrogen was used as the inert gas.

[0058] Evacuate the reactor to -0.09MPa, close the evacuation valve, and observe for 10 minutes. If the pressure does not rise, it is considered that the reactor is not leaking, and the following operations can be performed.

[0059] The formal reaction was started, the reactor was heated, the reaction temperature was controlled at 200°C, the gas pressure was controlled at -0.1-0 MPa, and the reaction time was 3 hours to generate crude phosphorus pentafluoride gas.

[0060] After the heating reaction is complete, the product is cooled by a condenser to remove impurities...

Embodiment 2

[0062] Heat the horizontal reactor with stirring device to 100°C, keep it for 0.5 hour, and remove the moisture in the reactor and pipeline.

[0063] In a dry environment, under the protection of an inert gas, quickly add 2.25 kg of phosphorus pentoxide and 1 kg of calcium fluoride into a horizontal reactor with a stirring device while hot, and close the reactor. Nitrogen was used as the inert gas.

[0064] Evacuate the reactor to -0.1MPa, close the evacuation valve, and observe for 10 minutes. If the pressure does not rise, it is considered that the reactor is not leaking, and the following operations can be performed.

[0065] The formal reaction was started, the reactor was heated, the reaction temperature was controlled at 250°C, the gas pressure was controlled at -0.1-0 MPa, and the reaction time was 5 hours to generate crude phosphorus pentafluoride.

[0066] After the heating reaction is complete, the product is cooled by a condenser to remove impurities to obtain high...

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PUM

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Abstract

The invention discloses a preparation method of phosphorus pentafluoride, which includes: (i) drying: removing water in a reactor and a pipeline, (ii) material adding: adding two solid powder of phosphorus pentoxide and calcium fluoride in the reactor under protection of inert gases in dry environment, (iii) vacuuming: vacuuming the reactor to -0.09MPa to -0.11MPa, (iv) synthetic reaction: controlling the reaction temperature within 200 DEG C to 300 DEG C, controlling pressure of the reactor within -0.1MPa to 0MPa, leading reaction time to be more than 3 hours so as to generate rough phosphorus pentafluoride gas, and (v) purification. The preparation method of phosphorus pentafluoride is simple in process and device and high in reliability, the process is easy to control, raw materials are non-toxic and easy to obtain, and product purity is as high as 99.9%. Another product Ca(PO3)2 is non-toxic and harmless and can be recycled.

Description

technical field [0001] The invention belongs to a process for preparing phosphorus pentafluoride, in particular to a method for preparing phosphorus pentafluoride by utilizing the heating reaction of two solids, phosphorus pentoxide and calcium fluoride. Background technique [0002] Phosphorus pentafluoride (PF 5 ) is a colorless and odorless gas under normal conditions, which fumes violently in humid air, with a melting point of -93.78°C and a boiling point of -84°C under normal pressure. As a fluorinating agent, phosphorus pentafluoride can perform ion transfer and is widely used in the fields of electronics industry, battery manufacturing, polymer materials and catalysts. In semiconductor manufacturing, phosphorus pentafluoride becomes a plasma gas for doping under the action of microwaves, which can significantly improve semiconductor performance. [0003] In the field of polymer materials, phosphorus pentafluoride can be used as a reactant to synthesize fluorinated o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/10
Inventor 刘春雪贺邓赵娜侯姝谢文雅刘玉静
Owner HUAHE NEW TECH DEV COMPANY RES INST OF PHYSICAL & CHEM ENG OF NUCLEAR IND