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Method for separating halogenated olefin impurities from 2-chloro-1,1,1,2-tetrafluoropropane

A technology of halogenated olefins and tetrafluoropropane, which is applied in the field of separating halogenated olefins impurities, can solve the problems of activated carbon surface pulverization, reduced service life, and large impact of activated carbon, etc., and achieves the effect of large saturated adsorption capacity

Active Publication Date: 2018-06-08
SHANDONG HUAAN NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But it only simulates the three-phase system for separation of HCFO-1233xf and HCFO-1224 isomers from HCFC-244bb
However, the actual production process also contains other components, especially unseparated complete HF, which has a greater impact on the activated carbon, which will cause the surface of the activated carbon to pulverize, affect the product components, and the service life will also be greatly reduced.

Method used

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  • Method for separating halogenated olefin impurities from 2-chloro-1,1,1,2-tetrafluoropropane
  • Method for separating halogenated olefin impurities from 2-chloro-1,1,1,2-tetrafluoropropane
  • Method for separating halogenated olefin impurities from 2-chloro-1,1,1,2-tetrafluoropropane

Examples

Experimental program
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Effect test

Embodiment 1-5

[0024] The preparation steps of embodiment 1-5 are as follows:

[0025] At 150° C., 1000 g of the adsorbent copper-modified high-silicon ZSM-5 molecular sieve was dried for 3 hours for later use. 100g of dried adsorbent is filled in the adsorption column of DN25mm×1000mm, and the composition containing 96.62% HCFC-244bb, 1.85% HCFO-1233xf, 0.12% HF and other halogenated olefins is continuously fed in the form of steam from the bottom of the adsorption column 100g, the material was recovered after 6 adsorption cycles, and the components were detected.

[0026] The preparation method of copper-modified high-silicon ZSM-5 molecular sieve is as follows: prepare saturated copper chloride solution at 60°C, add high-silicon ZSM-5 molecular sieve adsorbent into the reaction kettle, heat up to 60°C, and pump the vacuum to the reaction kettle Add an excess of saturated cupric chloride solution at 60°C; after immersion for 10 hours, filter and dry the molecular sieve to obtain the finis...

Embodiment 6-11

[0029] At 150° C., 1000 g of the adsorbent copper-modified high-silicon ZSM-5 molecular sieve was dried for 3 hours for later use. 100g of dried adsorbent is filled in the adsorption column of DN25mm×1000mm, and the excessive combination of 96.62% HCFC-244bb, 1.85% HCFO-1233xf, 0.12% HF and other halogenated olefins is continuously passed through from the bottom of the adsorption column in the form of steam until the adsorbent is saturated.

[0030] The preparation method of copper-modified high-silicon ZSM-5 molecular sieve is as follows: prepare saturated copper chloride solution at 60°C, add high-silicon ZSM-5 molecular sieve adsorbent into the reaction kettle, heat up to 60°C, and pump the vacuum to the reaction kettle Add an excess of saturated copper chloride solution at 60°C; after immersion for 13 hours, filter and dry the molecular sieve to obtain the finished product of copper-modified high-silicon ZSM-5 molecular sieve adsorbent.

[0031] See Table 2 for the raw ma...

Embodiment 12-15

[0033] After the adsorbent is saturated, heat the adsorption column to raise the temperature, and pass high-purity nitrogen that has been preheated to the same temperature as the adsorption column from the top of the adsorption column, and pass a certain amount of nitrogen to stop the desorption; the amount of nitrogen that is passed is 2000g.

[0034] See Table 3 for the temperature of the adsorption column in Examples 12-15 after heating and the related data of the adsorbent after desorption.

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Abstract

The invention relates to a method for separating halogenated olefin impurities from 2-chloro-1,1,1,2-tetrafluoropropane. The method comprises the following steps: adding the 2-chloro-1,1,1,2-tetrafluoropropane containing the halogenated olefin impurities into an adsorbent and absorbing halogenated olefins; the solid adsorbent is a copper-modified high-silicon ZSM-5 molecular sieve adsorbent. The absorption method adopted by the invention has the advantages that the saturated adsorption quantity is large, the adsorption quantity of the adsorbent for the halogenated olefins reaches 0.8, the content of HCFO-1233xf in absorbed HCFC-244bb is less than 700 ppm, the purity of the HCFC-244bb reaches above 99.6 percent, and the like. In addition, the adsorbent adopted by the invention has the advantage of HF resistance and is suitable for industrial production equipment.

Description

technical field [0001] The invention relates to a method for separating halogenated hydrocarbons, in particular to a method for separating halogenated olefin impurities from 2-chloro-1,1,1,2-tetrafluoropropane. Background technique [0002] Chinese Patent Publication No. 102001910 discloses a method for producing 2,3,3,3-tetrafluoropropene using 1,1,2,3-tetrachloropropene as a raw material. The method has three steps, in which the second step reacts the addition reaction of 2-chloro-3,3,3-trifluoropropene (HCFO-1233xf) with hydrogen fluoride to produce 2-chloro-1,1,1,2-tetrafluoropropene Fluoropropane (HCFC-244bb), HCFO-1233xf and HCFC-244bb will form an azeotropic mixture, which is difficult to separate. However, the conversion rate of HCFO-1233xf is not complete, a part of unreacted HCFO-1233xf is recycled and returned to the second-step reactor for reaction, and a part of HCFO-1233xf enters the third-step reactor along with HCFC-244bb; and a part of HCFC-244bb It will e...

Claims

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Application Information

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IPC IPC(8): C07C17/389C07C19/10
CPCC07C17/389C07C19/10
Inventor 明文勇王瑞英徐甲超王通孟翔
Owner SHANDONG HUAAN NEW MATERIAL
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