A purification method and purification device for octafluoropropane

A technology of octafluoropropane and purification method, which is applied in chemical instruments and methods, disproportionation separation/purification of halogenated hydrocarbons, organic chemistry, etc. It can solve the problems of difficult purification, small adsorption capacity, and difficult removal, and achieve the reduction of impurity content, The effect of improving product yield and prolonging the required time

Active Publication Date: 2019-05-21
PERIC SPECIAL GASES CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The first type is the method of rectification, but because there are many kinds of impurities in octafluoropropane, there are often impurities with boiling points close to or azeotropic with perfluoroalkanes, so it is difficult to purify by rectification
The second type is the method of adsorption. The commonly used adsorbents are molecular sieves, activated carbon and carbon molecular sieves, etc., but some impurities have very little adsorption capacity in the adsorbents and are difficult to remove by this method.
The third category is the catalytic conversion method, which decomposes or converts impurities with a boiling point close to the boiling point of perfluoroalkane through a catalyst into impurities with a large difference in boiling point and perfluoroalkane boiling point, but this method is often only for some specific impurities efficient
[0005] The purification methods of the octafluoropropane have limitations. In the prior art, it is difficult to obtain a product with a purity greater than 99.999% by a single method of rectification, adsorption, catalytic conversion and membrane separation. Octafluoropropane

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  • A purification method and purification device for octafluoropropane

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Comparison scheme
Effect test

Embodiment 1

[0054] The rectification tower 10 is a packed rectification tower, the packing 14 is a stainless steel θ ring with a diameter of 1 mm, the rectification tower 10 is made of nickel, and the height is 15 m, and the diameter of the rectification column 13 is 50 mm.

[0055] A purification method for octafluoropropane, the steps of the purification method are as follows:

[0056] (1) Introduce crude octafluoropropane gas into cold trap 1 at a temperature of -100°C, heat it up at a rate of 1°C / min, and perform light-removal treatment at -90°C to -40°C to reduce light component impurities with low boiling points Vaporization discharge. When the temperature rises to greater than -40°C and less than or equal to -20°C, the treated crude octafluoropropane gas is introduced into the bottom of the adsorption tower 5. When the temperature rises to greater than -20°C, the flow to the bottom of the adsorption tower 5 is stopped. In, the higher boiling point heavy component impurities left in the ...

Embodiment 2

[0064] The rectification tower 10 is a packed rectification tower, and the packing 14 is a nickel Pall ring with a diameter of 5 mm. The rectification tower 10 is made of stainless steel and has a height of 8 m. The diameter of the rectification column 13 is 500 mm.

[0065] A purification method for octafluoropropane, the steps of the purification method are as follows:

[0066] (1) Introduce crude octafluoropropane gas into cold trap 1 at a temperature of -91°C, heat it up at a rate of 2°C / min, and perform light-removal treatment at -90°C to -40°C to reduce light component impurities with low boiling points Vaporization discharge. When the temperature rises to greater than -40°C and less than or equal to -20°C, the treated crude octafluoropropane gas is introduced into the bottom of the adsorption tower 5. When the temperature rises to greater than -20°C, the flow to the bottom of the adsorption tower 5 is stopped. In, the higher boiling point heavy component impurities left in t...

Embodiment 3

[0074] The rectification tower 10 is a packed rectification tower, the packing 14 is a polytetrafluoroethylene Pall ring with a diameter of 100 mm, the rectification tower 10 is made of Monel alloy with a height of 5 m, and the diameter of the rectification column 13 is 300 mm.

[0075] A purification method for octafluoropropane, the steps of the purification method are as follows:

[0076] (1) Introduce crude octafluoropropane gas into cold trap 1 at a temperature of -100°C, heat it up at a rate of 1.5°C / min, and perform light-removal treatment at -90°C to -40°C to reduce light component impurities with low boiling points Vaporization discharge. When the temperature rises to greater than -40°C and less than or equal to -20°C, the treated crude octafluoropropane gas is introduced into the bottom of the adsorption tower 5. When the temperature rises to greater than -20°C, the flow to the bottom of the adsorption tower 5 is stopped. In, the higher boiling point heavy component impur...

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Abstract

The invention relates to an octafluoropropane purifying method and a purifying apparatus thereof, which belong to the field of fine chemical engineering. The purifying method employs a cold trap for light-discharge and heavy-removal processing of an octafluoropropane crude product, the light components and heavy components impurity content are greatly reduced; an adsorbent is used for adsorption, H2O content is reduced, a part of a fluorocarbon compound is absorbed; a rectification technology is employed, the high-boiling point and low-boiling point impurity can be removed by controlling the rectification parameters, the H2O content is less than 1 ppm, the content of the organic fluorocarbon compound is less than 1 ppm, the total impurity content is less than 10 ppm, cold amount and heat consumed during the rectification process are reduced, economic performance is good, and the octafluoropropane with purity of greater than 99.999% can be obtained after being purified. The purifying apparatus mainly comprises the cold trap, an adsorption tower and a rectifying tower, and is adapted to usage of the purifying method.

Description

Technical field [0001] The invention relates to a purification method and a purification device for octafluoropropane, and belongs to the field of fine chemicals. Background technique [0002] High-purity octafluoropropane electronic gas, as a cleaning agent and etching agent for electronic devices, is used in semiconductor manufacturing and the electronics industry. As the etching accuracy of semiconductor devices becomes higher and higher, the purity requirements for octafluoropropane are also higher and higher. Generally speaking, the purity of high-purity octafluoropropane used in large-scale integrated circuits is greater than 99.999%. [0003] The main preparation method of octafluoropropane at this stage is mainly to prepare octafluoropropane by reacting hexafluoropropene or heptafluoropropane with fluorine gas. Due to the fluorination and / or high temperature reaction involved in the preparation process, a large amount of heat is released and carbon-carbon is generated. , ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C17/38C07C17/383C07C17/389C07C19/08
CPCC07C17/38C07C17/383C07C17/389C07C19/08
Inventor 黄华璠徐海云冀延治王志民商洪涛马毅斌齐航张帅
Owner PERIC SPECIAL GASES CO LTD
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