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Method for separating cis and trans carboxylic acids from mixed acids with cis and trans carboxylic acid isomers

An isomer and mixed acid technology, applied in the field of separating cis carboxylic acid and trans carboxylic acid, can solve the problems of difficulty in large-scale production and only use, and achieves high production cost, simple production process and low production cost. Effect

Active Publication Date: 2016-01-20
GUANGXI HAOWANG BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, the mixed acid separation technology of cis and trans carboxylic acid isomers commonly used in the chemical industry mainly includes distillation tower rectification separation, column chromatography separation, thin chromatography separation, etc. For isomer carboxylic acids that are sensitive to temperature , Distillation column distillation separation is sometimes impossible, and column chromatography separation, thin chromatography separation and other technologies are difficult to apply to industrial production, generally only used for experimental research or separation of high-value products

Method used

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  • Method for separating cis and trans carboxylic acids from mixed acids with cis and trans carboxylic acid isomers
  • Method for separating cis and trans carboxylic acids from mixed acids with cis and trans carboxylic acid isomers
  • Method for separating cis and trans carboxylic acids from mixed acids with cis and trans carboxylic acid isomers

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Effect test

example 1

[0023] Add 250ml of anhydrous ether to a 500ml dry three-necked flask (equipped with a stirrer, thermometer, calcium chloride drying tube, and ventilation tube), add 50g of 11-methoxy-3,7,11-trimethyl-2, 4E-diene dodecanoic acid (a mixture of cis-acid and trans-acid), stir to dissolve, nitrogen gas is introduced into the vent pipe, ice-salt bath, the temperature of the material liquid is lowered to -5°C, and the vent pipe is changed to dry ammonia , the mass of ammonia gas introduced is 35.0g, and the process temperature cannot exceed 5°C. Keep stirring at -5~-2°C for 2 hours. Filter while cold to obtain filter cake and filtrate A. The filter cake was slurried with 50ml of cold diethyl ether and then filtered, and dried as much as possible by suction to obtain 35g of wet product and filtrate B. Put the wet product in a 500ml beaker, add 150ml of n-hexane and 50ml of water, stir to dissolve, adjust the pH of the solution to ≤1 with 20% sulfuric acid solution, let it stand for...

example 2

[0025] Add 250ml of anhydrous n-hexane to a 500ml dry three-neck flask (equipped with a stirrer, thermometer, calcium chloride drying tube, vent tube), and add 50g of 11-methoxy-3,7,11-trimethyl-2 , 4E-diene dodecanoic acid (a mixture of cis-acid and trans-acid), stir to dissolve, nitrogen gas into the vent pipe, ice-salt bath, the temperature of the material liquid is reduced to -5 ° C, the vent pipe is changed to dry ammonia Gas, the quality of passing through the ammonia gas is 35.0g, and the process temperature cannot exceed 5°C. Keep stirring at -5~-2°C for 2 hours. Filter while cold, wait until the filter cake and filtrate A. The filter cake was slurried with 50ml of cold n-hexane and then filtered, and dried as much as possible by suction to obtain 38g of wet product and filtrate B. Put the wet product in a 500ml beaker, add 150ml of n-hexane and 50ml of water, stir to dissolve, adjust the pH of the solution to ≤1 with 20% sulfuric acid solution, let it stand for 30 m...

example 3

[0027]Add 250ml of anhydrous toluene to a 500ml dry three-necked flask (equipped with stirrer, thermometer, calcium chloride drying tube, vent tube), add 50g11-methoxyl-3,7,11-trimethyl-2, 4E-diene dodecanoic acid (a mixture of cis-acid and trans-acid), stir to dissolve, nitrogen gas is introduced into the vent pipe, ice-salt bath, the temperature of the material liquid is lowered to -5°C, and the vent pipe is changed to dry ammonia , the mass of ammonia gas introduced is 35.0g, and the process temperature cannot exceed 5°C. Keep stirring at -5~-2°C for 2 hours. Filter while cold, wait until the filter cake and filtrate A. The filter cake was slurried with 50ml of cold toluene and then filtered, and dried as much as possible to obtain 40.5g of wet product and filtrate B. Put the wet product in a 500ml beaker, add 150ml of n-hexane and 50ml of water, stir to dissolve, adjust the pH of the solution to ≤1 with 20% sulfuric acid solution, let it stand for 30 minutes, separate th...

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Abstract

The invention relates to a method for extracting cis-form carboxylic acid and trans-form carboxylic acid from mixed acid with cis-form and trans-form carboxylic acid isomers. The method includes the steps that the mixed acid with the cis-form and trans-form carboxylic acid isomers firstly reacts with ammonia gas to generate cis-form carboxylic acid ammonium salt and trans-form carboxylic acid ammonium salt, the cis-form carboxylic acid ammonium salt and the trans-form carboxylic acid ammonium salt are extracted from the mixed acid according to the characteristic that the solubility of the cis-form carboxylic acid ammonium salt in solvents and the solubility of the trans-form carboxylic acid ammonium salt in the solvents are different, and then the cis-form carboxylic acid ammonium salt and the trans-form carboxylic acid ammonium salt are reduced to be the corresponding cis-form carboxylic acid and the corresponding trans-form carboxylic acid through chemical reactions. The method can be used for industrialization mass production.

Description

technical field [0001] The invention relates to a method for separating cis-form carboxylic acid and trans-form carboxylic acid from mixed acids with cis-form and trans-form carboxylic acid isomers, belonging to the field of chemistry. Background technique [0002] At present, the mixed acid separation technology of cis and trans carboxylic acid isomers commonly used in the chemical industry mainly includes distillation tower rectification separation, column chromatography separation, thin chromatography separation, etc. For isomer carboxylic acids that are sensitive to temperature , Distillation column distillation separation is sometimes impossible, and column chromatography separation, thin chromatography separation and other technologies are difficult to apply to industrial production, generally only used for experimental research or separation of high-value products. Contents of the invention [0003] The technical problem to be solved by this invention is to provide ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/487C07C57/03
CPCC07C51/487C07C57/03
Inventor 刘松梁罗立泳
Owner GUANGXI HAOWANG BIOTECH
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