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A kind of separation method of benzene polycarboxylic acid isomer

A technology of isomers and benzene polycarboxylic acids, which is applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., to achieve the effects of increasing separation, reducing use and less investment in equipment

Active Publication Date: 2015-11-11
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But at present these separations all form liquid eutectics

Method used

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  • A kind of separation method of benzene polycarboxylic acid isomer
  • A kind of separation method of benzene polycarboxylic acid isomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Weigh a certain mass of phthalic acid and isophthalic acid mixture and dissolve it in 100mL butanone to prepare the butanone with a concentration of 1.1g / L and 1.0g / L of phthalic acid and isophthalic acid mixture respectively. solution. The solution was placed in a 150mL Erlenmeyer flask.

[0032] A small amount of tetraethylammonium chloride was added to the solution each time, magnetically stirred at room temperature for 2 hours, and then allowed to stand for 15 minutes. Get 0.1mL butanone solution and dilute to 10mL, analyze the content of phthalic acid and isophthalic acid in the solution by liquid chromatography, add tetraethylammonium chloride repeatedly, until the content of phthalic acid in the solution is no longer change. Take the raffinate rate of phthalic acid in the solution as the ordinate, and take the amount of quaternary ammonium salt added as the abscissa to obtain figure 1 .

[0033] From the results of this experiment, the amount of quaternary am...

Embodiment 2

[0035] Weigh a certain mass of phthalic acid, trimellitic acid and trimellitic acid mixture and dissolve it in 100mL of methyl ethyl ketone to prepare pyrogalloids with concentrations of 3.0g / L, 3.1g / L and 3.4g / L respectively. Solution of Formic Acid, Trimellitic Acid and Trimellitic Acid Mixture in Butanone. The solution was placed in a 150mL Erlenmeyer flask.

[0036] A small amount of tetraethylammonium chloride was added to the solution each time, magnetically stirred at room temperature for 2 hours, and then allowed to stand for 15 minutes. Get 0.1mL butanone solution and dilute it to 10mL, analyze the content of benzenetricarboxylic acid in the solution by liquid chromatography, add tetraethylammonium chloride repeatedly, until the content of benzenetrimethylcarboxylic acid in the solution no longer changes. Take the raffinate rate of benzenetricarboxylic acid in the solution as the ordinate, and take the addition amount of the quaternary ammonium salt as the abscissa t...

Embodiment 3

[0039] Weigh a certain mass of phthalic acid and isophthalic acid mixture and dissolve it in 100mL butanone to prepare the butanone with a concentration of 1.1g / L and 1.0g / L of phthalic acid and isophthalic acid mixture respectively. solution. The solution was placed in a 150mL Erlenmeyer flask.

[0040] (1) Add 0.26g of tetraethylammonium chloride to the Erlenmeyer flask, stir it magnetically for 2 hours at room temperature, and then let it stand for 15 minutes. Take 0.1mL butanone solution and dilute it to 10mL, and use liquid chromatography to analyze the content of phthalic acid and isophthalic acid in the solution. After analysis, it can be seen that 59.3% of phthalic acid is first formed with tetraethylammonium chloride. The eutectic mixture was precipitated out, while the content of isophthalic acid remained unchanged. The solution was filtered to give a butanone filtrate and a eutectic solid mixture. eutectic solid mixture at 60 o Dry in a C oven for 5 h to remove ...

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Abstract

The invention relates to a separation method for benzene polycarboxylic acid isomers. The method includes: adding a quaternary ammonium salt into a solution of benzene polycarboxylic acid isomers, conducting stirring, and making the quaternary ammonium salt interact with one of the benzene polycarboxylic acid isomers so as to form an eutectic mixture; filtering the formed eutectic mixture; drying the filtered eutectic mixture to remove the residual solvent from the eutectic mixture; mixing and stirring the dried eutectic mixture and a back extraction solvent, and performing filtering to obtain a quaternary ammonium salt containing back extraction solvent and one of the benzene polycarboxylic acid isomer; and distilling the quaternary ammonium salt containing back extraction solvent to recover the back extraction solvent and the quaternary ammonium salt.

Description

technical field [0001] The invention relates to a method for separating isomers of benzene polycarboxylic acid. Background technique [0002] Benzene polycarboxylic acid is an important chemical raw material and has a wide range of applications in industry. For example, phthalic acid is used to make dyes, polyester resins, polyester, drugs and plasticizers. Isophthalic acid is used in the production of alkyd resins, unsaturated polyester resins and other polymers. Tricarboxylic acid is used in the preparation of resins, plasticizers, dyes, crosslinking agents, etc. At present, these benzene polycarboxylic acids are mainly obtained from the catalytic oxidation of their corresponding aromatics, which are directly or indirectly obtained from petroleum. my country's oil resources are relatively scarce, and coal is relatively rich, so the production of benzene polycarboxylic acid from coal will be of great significance. However, the product obtained from coal oxidation is a c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C63/16C07C63/24C07C63/307C07C51/487
CPCC07C51/487C07C63/16C07C63/24C07C63/307
Inventor 吴卫泽李健任树行
Owner BEIJING UNIV OF CHEM TECH