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Preparation method of ultra-high purity hexafluoroethane

A technology of pure hexafluoroethane and hexafluoroethane, applied in the field of preparation of ultra-high-purity hexafluoroethane, can solve problems such as being unsuitable for industrial production, and achieve short adsorption time, no secondary pollution, and environmental friendliness. Effect

Active Publication Date: 2017-04-12
SINOCHEM LANTIAN +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is mainly aimed at the removal of impurities in the fifth production method, that is, the direct fluorination of R161 and elemental fluorine to produce R116. It can only remove HFC-125, HFC-143a and HFC-134a, and it adopts batch operation, which is not suitable for industrial production.

Method used

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  • Preparation method of ultra-high purity hexafluoroethane
  • Preparation method of ultra-high purity hexafluoroethane
  • Preparation method of ultra-high purity hexafluoroethane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1~6

[0024] First, put a certain amount of adsorbent in a muffle furnace with a tray, heat it to 300°C for activation, keep the activation time for 3 hours, and then take it out. Weigh 300g of the activated adsorbent and place it in a 1L stainless steel cylinder, seal and vacuumize, then add 400g of crude hexafluoroethane (containing R230.0137%, R130.4588%, R143a0.2378%, R1251 to the 1L cylinder) .5163, R1150.0058%), keep the temperature at -20 °C, start the adsorption, until the adsorption equilibrium. The results after the adsorption equilibrium are shown in Table 1. Except for the special marks in Table 1, the rest are the data after adsorption for 5h.

[0025] Table 1

[0026]

[0027]

Embodiment 7~9

[0029] First, put a certain amount of activated carbon A (particle size 1-1.5mm) into an oven with a tray, heat it to 180°C for activation, keep the activation time for 3 hours, and then take it out. Weigh 130 g of activated adsorbent activated carbon A, fill it into a stainless steel gas-solid adsorption column with an inner diameter of 25 mm and a height of 90 cm, seal it, and vacuumize it. Then pass through the crude hexafluoroethane, and the impurity content of the crude product is the same as that of Example 1. Under the temperature of -30, -10, 10°C and the pressure of 0.05-0.5MPa (gauge pressure), the feed rate is 6.5g / min from the top of the adsorption bed into the adsorption fixed bed. The gas after adsorption for 11 hours was collected by condensation, and the content of each component in it was analyzed by a gas chromatograph. The results are shown in Table 2.

Embodiment 10

[0031] First, put a certain amount of 5A molecular sieve adsorbent into a muffle furnace with a tray, heat it to 300°C for activation, keep the activation time for 3 hours, and then take it out. Weigh 130 g of the activated adsorbent, fill it into a stainless steel gas-solid adsorption column with an inner diameter of 25 mm and a height of 90 cm, seal it, and vacuumize it. Then pass through the crude hexafluoroethane, and the impurity content of the crude product is the same as that of Example 1. At a temperature of -30°C and a pressure of 0.05-0.5MPa (gauge pressure), the feed rate is 4.0g / min from the top of the adsorption bed into the adsorption fixed bed. The gas adsorbed for 8 hours was collected by condensation, and the content of each component in it was analyzed with a gas chromatograph. The results are shown in Table 2.

[0032] Table 2

[0033]

[0034] Embodiments 1-6 are intermittent adsorption. The 3A type molecular sieves, 4A type molecular sieves, 5A type mol...

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Abstract

The present invention provides a method for preparing ultra-high purity hexafluoroethane through an absorption method. According to the present invention, an absorption comprising one, two or three materials selected form a 3A type molecular sieve, a 4A type molecular sieve, a 5A type molecular sieve, a NaX type molecular sieve, a CaX type molecular sieve and active carbon is adopted to remove impurities in a hexafluoroethane crude product, wherein the absorption agent is subjected to an activation treatment before absorption, the purity of the prepared hexafluoroethane can achieve 99.999%, even 99.9999% and above, and the prepared ultra-high purity hexafluoroethane can be used as the etching gas / cleaning gas in the semiconductor / electronics industry.

Description

technical field [0001] The invention belongs to the technical field of gas purification, and relates to a preparation method of ultra-high-purity hexafluoroethane. Background technique [0002] Hexafluoroethane, codenamed R116 or FC-116, is a colorless, odorless, non-flammable gas. Hexafluoroethane can be used as a refrigerant for refrigeration and air conditioning, and can also be combined with HFC-23 to form an azeotrope that does not damage the ozone layer. R-508B, R-508B can be used as a substitute for CFC-13 and R- Alternative to 503; Another major use of hexafluoroethane is as a plasma etching gas, which plays an important role in the development of the semiconductor / microelectronics industry and is a necessary medium for processing VLSI processes. Hexafluoroethane etching gas has very strict requirements on purity, often requiring more than 99.999%, or even more than 99.9999%. [0003] The production methods of hexafluoroethane mainly include: 1) Electrolytic fluori...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C19/08C07C17/389
Inventor 李盛姬柳彩波刘武灿
Owner SINOCHEM LANTIAN
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