Modified adsorbent and applications of modified adsorbent in ultra-high purity methyl fluoride preparation

A monofluoromethane and adsorbent technology, applied in the field of modified adsorbents, can solve the problems of requiring many raw materials, complex processes, and low purity of HFC-41, and achieve high adsorption efficiency, no secondary pollution, and large adsorption capacity. Effect

Active Publication Date: 2016-03-02
ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is complex and requires many raw materials. It is not suitable for large-scale production, and it is easy to introduce moisture and other impurities. The final HFC-41 is not high in purity, and the product cannot be used in the electronics industry.

Method used

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  • Modified adsorbent and applications of modified adsorbent in ultra-high purity methyl fluoride preparation
  • Modified adsorbent and applications of modified adsorbent in ultra-high purity methyl fluoride preparation
  • Modified adsorbent and applications of modified adsorbent in ultra-high purity methyl fluoride preparation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Weigh 10g of NaX molecular sieve raw powder, mix it with 0.1mol / L LiCl solution at a solid-to-liquid ratio of 1:3, and stir at 80°C for 4h. Filter molecular sieves, and add fresh LiCl solution with a concentration of 0.1mol / L at a solid-to-liquid ratio of 1:3 again for ion exchange. This process is repeated 4 times to ensure that Na + completely by Li + exchange. Filter the solid, wash with distilled water until Cl-free -1 . Dry at 110°C for 8 hours. Take a certain amount of sample in the gas-solid phase adsorption device, at 350 ° C, N 2 In-situ activation in the atmosphere for 2 hours, after cooling down, feed the raw material gas HFC-41 for adsorption and removal of impurities.

Embodiment 2

[0034] Weigh 10g of NaY molecular sieve raw powder, mix it with 0.1mol / L LiCl solution at a solid-to-liquid ratio of 1:3, and stir at 80°C for 4h. Filter molecular sieves, and add fresh LiCl solution with a concentration of 0.1mol / L at a solid-to-liquid ratio of 1:3 again for ion exchange. This process is repeated 4 times to ensure that Na + completely by Li + exchange. Filter the solid, wash with distilled water until Cl-free -1 . Dry at 110°C for 8 hours. Take a certain amount of sample in the gas-solid phase adsorption device, at 350 ° C, N 2 In-situ activation in the atmosphere for 2 hours, after cooling down, feed the raw material gas HFC-41 for adsorption and removal of impurities.

Embodiment 3

[0036] Weigh 10gSiO 2 and 20g LiCl solid, placed in a ball mill to grind for 60min, then take it out, and bake it at 350°C for 8h to promote LiCl on SiO 2 The surface is dispersed. Take a certain amount of sample in the gas-solid phase adsorption device, at 350 ° C, N 2 In-situ activation in the atmosphere for 2 hours, after cooling down, feed the raw material gas HFC-41 for adsorption and removal of impurities.

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Abstract

The present invention discloses an adsorbent modified through an ion exchange method, ball mill method or impregnating method, wherein the adsorbent is selected from an A type molecular sieve, an X type molecular sieve, a Y type molecular sieve, SiO2, Al2O3 or active carbon AC. According to the present invention, the modified adsorbent is suitable for removal of organic impurities from the methyl fluoride crude product so as to obtain the ultra-high purity methyl fluoride product with a purity of more than or equal to 99.999%.

Description

technical field [0001] The invention relates to an adsorbent, in particular to a modified adsorbent which can be used to prepare ultra-high-purity monofluoromethane. Background technique [0002] HFC-41 is a non-toxic, colorless, odorless, flammable liquefied gas stored in steel cylinders. It can not only be used as a raw material for the production of bromofluoromethane, but also can be used as an etchant for semiconductor dry etching technology, such as integration Plasma etching in electrical circuits, especially HDP (High Density Plasma) etching. When it is used for etching in the semiconductor industry, its purity has a decisive impact on component performance and product yield. Even a small amount of impurities entering the process will lead to a rapid increase in product failure rate. Therefore, the market has a high demand for electronic products. The purity requirements of the gas are getting higher and higher, and the basic requirement is that the organic impurity...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/08B01J20/10B01J20/18B01J20/20C07C19/08C07C17/389
Inventor 张金柯白占旗齐海何双材徐娇胡欣
Owner ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH
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