Inclusion separating method and application of isomerides of 3-diphenic acid and 4-diphenic acid

A technology of isomers and diphenylformic acid, which is applied in the field of separation and purification of diphenylformic acid isomers, can solve the problems of unsuitability for large-scale production, high energy consumption of separation methods, and small processing capacity.

Inactive Publication Date: 2010-11-24
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, with the rapid development of modern production and science and technology, people's living standards continue to improve, and higher and higher requirements are placed on separation technology. These separation methods are no longer applicable to many systems and cannot meet people's needs; and traditional Separation methods are often energy-intensive, complicated to operate, small in processing capacity, and high in separation costs, and are not suitable for large-scale production

Method used

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  • Inclusion separating method and application of isomerides of 3-diphenic acid and 4-diphenic acid
  • Inclusion separating method and application of isomerides of 3-diphenic acid and 4-diphenic acid
  • Inclusion separating method and application of isomerides of 3-diphenic acid and 4-diphenic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Example 1: First prepare β-cyclodextrin into a saturated aqueous solution at 60°C, perform constant temperature magnetic stirring for 2 hours, then add the ethanol solution of diphenylcarboxylic acid dropwise to the above β-cyclodextrin with a molar material ratio of 1:1.5 In the saturated aqueous solution of dextrin, take out the Erlenmeyer flask from the water bath after reacting for 6 hours, let it stand at room temperature for 48 hours, and the inclusions are cooled and precipitated. Then the inclusions were washed three times with distilled water and absolute ethanol respectively, and the inclusions were collected. Dissolve the inclusions in ethanol solution, heat to reflux, adjust the constant temperature magnetic stirrer, control the temperature of the water bath to 88°C, adjust the speed to max, heat to reflux, and split for 2 hours; then filter twice, collect the filtrate, and use to be distilled. By distillation, the filtrate and the solvent in the mother liq...

Embodiment 2

[0031]Example 2: First make β-cyclodextrin into a saturated aqueous solution at 65°C, perform constant temperature magnetic stirring for 2.5 hours, and then add the ethanol solution of diphenylcarboxylic acid dropwise to the above β-cyclodextrin with a molar material ratio of 1:2 In the saturated aqueous solution of cyclodextrin, the conical flask was taken out from the water bath after reacting for 7 hours, and allowed to stand at room temperature for 54 hours, and the inclusion complexes were cooled and precipitated. Then the inclusions were washed three times with distilled water and absolute ethanol respectively, and the inclusions were collected. Dissolve the inclusion complex in ethanol solution, and heat to reflux, adjust the constant temperature magnetic stirrer, control the temperature of the water bath to 89°C, adjust the speed to max, heat to reflux, and split for 2.5h; then filter twice, collect the filtrate, to be distilled. By distillation, the filtrate and the ...

Embodiment 3

[0032] Example 3: First prepare the β-cyclodextrin into a saturated aqueous solution at 70°C, perform constant temperature magnetic stirring for 3 hours, and then add the ethanol solution of diphenylformic acid dropwise to the above β-cyclodextrin with a molar material ratio of 1:2.5. In the saturated aqueous solution of dextrin, take the conical flask out of the water bath after reacting for 8 hours, let it stand at room temperature for 60 hours, and the inclusion complexes are cooled and precipitated. Then the inclusions were washed three times with distilled water and absolute ethanol respectively, and the inclusions were collected. Dissolve the inclusions in ethanol solution, heat to reflux, adjust the constant temperature magnetic stirrer, control the temperature of the water bath to 90°C, adjust the speed to max, heat to reflux, and split for 3 hours; then filter twice, collect the filtrate, and use to be distilled. By distillation, the filtrate and the solvent in the m...

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Abstract

The invention relates to an inclusion separating method and application of isomerides of 3-diphenic acid and 4-diphenic acid. In the method, a mixture of 3-diphenic acid and 4-diphenic acid is separated by beta-cyclodextrin inclusion. The method comprises the following steps of: preparing an inclusion compound, (2) resolving the inclusion compound, and (3) processing the product. According to the difference between molecular structures of the 4-diphenic acid and the 3-diphenic acid, a host molecule chooses molecules which are complementary to the host molecule for inclusion and separates the molecules out in the form of crystals so as to achieve the separation purpose. On the basis of the research on the influences of material proportioning, heating temperature, inclusion time and other factors on the inclusion separating result, the optimal separating conditions for the preparation method and preparation conditions of the inclusion compound are found by orthogonal tests. The purity of the 4-diphenic acid is up to over 99%.

Description

technical field [0001] This patented technology is applicable to the disposal and recycling of benzoic acid still waste liquid produced in the process of producing benzoic acid by the toluene oxidation method and the process of synthesizing caprolactam with benzoic acid as raw material, as well as the isomers of biphenylformic acid Separation and purification. Background technique [0002] The formation of the technology of the present invention mainly comes from the residual waste of the toluene oxidation production benzoic acid unit of Shijiazhuang Oil Refining and Chemical Industry Co., Ltd. During the separation and recovery process of the residual waste of benzoic acid developed by Tianjin University, a part of 3-biphenylformic acid and 4 -The mixture of biphenyl carboxylic acid, these two kinds of chemical substances have high application value in organic synthesis, petrochemical industry, material chemistry and so on. In particular, 4-biphenylcarboxylic acid can be u...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C63/331C07C51/42
Inventor 张卫江徐姣阳彩霞
Owner TIANJIN UNIV
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