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 com

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

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Example Embodiment

[0023] Example 1-5

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

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

[0026] The preparation method of copper-modified high-silicon ZSM-5 molecular sieve is as follows: prepare a saturated copper chloride solution at 60°C, add high-silicon ZSM-5 molecular sieve adsorbent into the reaction kettle, raise the temperature to 60°C, and apply a vacuum to the reaction kettle An excess of saturated copper chloride solution at 60°C was passed into the medium; after immersing for 10 hours, the molecular sieve was filtere...

Example Embodiment

[0028] Example 6-11

[0029] At 150°C, dry 1000g of the adsorbent copper-modified high-silicon ZSM-5 molecular sieve for 3 hours. Fill the adsorption column of DN25mm×1000mm with 100g of dried adsorbent, and continuously pass the combination of 96.62% HCFC-244bb, 1.85% HCFO-1233xf, 0.12% HF and other halogenated olefins in the form of steam from the bottom of the adsorption column 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 apply a vacuum to the reaction kettle An excess of saturated copper chloride solution at 60°C was passed through it; after 13 hours of immersion, the molecular sieve was filtered and dried to obtain a finished copper-modified high-silicon ZSM-5 molecular sieve adsorbent.

[0031] The relative data of the raw material vapor adso...

Example Embodiment

[0032] Examples 12-15

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

[0034] Table 3 shows the temperature after heating and temperature rise of the adsorption column of Examples 12-15 and the relevant 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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