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Ultra-high purity hexafluoroethane preparation method

A technology of pure hexafluoroethane and hexafluoroethane, which is applied in the field of preparation of ultra-high-purity hexafluoroethane, can solve problems such as being unsuitable for industrial production, and achieve the effects of short adsorption time, high adsorption efficiency and environmental friendliness

Active Publication Date: 2014-07-09
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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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1~6

[0024] First put a certain amount of adsorbent into the muffle furnace with a tray, heat 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 it, and evacuate it, then add 400g of crude hexafluoroethane (containing R230.0137%, R130.4588%, R143a0.2378%, R1251 .5163, R1150.0058%), keep the temperature at -20°C, and start to adsorb until the adsorption equilibrium. The results after adsorption equilibrium are shown in Table 1. Except for special marks in Table 1, the rest are the data after adsorption for 5 hours.

[0025] Table 1

[0026]

[0027]

Embodiment 7~9

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

Embodiment 10

[0031] First put a certain amount of 5A molecular sieve adsorbent into the muffle furnace with a tray, heat it to 300°C for activation, and keep the activation time for 3 hours before taking it out. Weigh 130 g of the activated adsorbent and 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 evacuate it. Then feed the crude hexafluoroethane, the impurity content of which is the same as in Example 1. At a temperature of -30°C and a pressure of 0.05-0.5 MPa (gauge pressure), the feed rate is 4.0 g / min from the top of the adsorption bed into the fixed adsorption bed. The gas after adsorption for 8 hours was condensed and collected, and the content of each component was analyzed by gas chromatography. The results are shown in Table 2.

[0032] Table 2

[0033]

[0034] Embodiment 1-6 is intermittent adsorption, the 3A type molecular sieve of the present invention, 4A type molecular sieve, 5A type molecu...

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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, code-named 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 form an entrainer R-508B with HFC-23 that does not damage the ozone layer. R-508B can be used as a substitute for CFC-13 and R- A substitute for 503; Another main 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, which often needs to be greater than 99.999%, or even more than 99.9999%. [0003] The production methods of hexafluoroethane mainly include: 1) ethane / ethylene electr...

Claims

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Application Information

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