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Method for separating and purifying glutaric acid in mixed binary acid by low-carbon halogenated hydrocarbon

A technology of mixing dibasic acid and carbon halogenated alkane, which is applied in the separation/purification of carboxylic acid compounds, organic chemistry and other directions, can solve the problems of high cost, low product yield and complicated process flow.

Active Publication Date: 2017-12-29
TANGSHAN KAILUAN CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] In summary, although there are many methods for separating and purifying glutaric acid from mixed dibasic acids, the common problems are low product yield, high cost, and complicated technological process, which is not conducive to industrial production.

Method used

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  • Method for separating and purifying glutaric acid in mixed binary acid by low-carbon halogenated hydrocarbon

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Set the temperature of the constant temperature water bath to 59.4°C. After the temperature of the jacket of the dissolution kettle rises to this temperature, add 1530g of DBA raw material powder of 40 meshes after grinding and sieving and 3369ml of 1,2-dibromoethane solvent into the dissolution kettle and stir to dissolve. The speed is set to 350r / min. After the temperature displayed by the thermocouple in the dissolution kettle rises to about 59.2°C, start timing. After dissolving for 1 hour, heat-retain and filter. The filter cake is a DBA mixture, which will be used as a by-product after drying.

[0031] The filtrate was introduced into a crystallization kettle with a jacket temperature of 61.4°C, and when there were no particles in the filtrate and the thermocouple of the crystallization kettle showed that the temperature was stable at 61.2°C, the crystallization began by cooling down. During the crystallization process, the stirring speed was 290r / min, and the coo...

Embodiment 2

[0034] Set the temperature of the constant temperature water bath to 63.5°C. After the temperature of the jacket of the dissolution kettle rises to this temperature, add 1530g of DBA raw material powder of 40 meshes after grinding and sieving and 4927ml of 1,2,3-trichloropropane solvent into the dissolution kettle and stir to dissolve. The stirring speed was set at 350r / min. After the thermocouple in the dissolution kettle shows that the temperature rises to about 63.3°C, start timing. After dissolving for 1 hour, heat-preserve and filter. The filter cake is a DBA mixture, which will be used as a by-product after drying.

[0035] The filtrate was introduced into a crystallization kettle with a jacket temperature of 65.5°C. When there were no particles in the filtrate and the thermocouple of the crystallization kettle showed that the temperature was stable at 65.3°C, the crystallization began to cool down. During the crystallization process, the stirring speed was 290r / min, and...

Embodiment 3

[0038] Set the temperature of the constant temperature water bath to 57.4°C. After the temperature of the jacket of the dissolution kettle rises to this temperature, add 1530g of DBA raw material powder of 40 meshes after grinding and sieving and 4284ml of 1,4-dichlorobutane solvent into the dissolution kettle and stir to dissolve. The speed is set to 350r / min. After the temperature displayed by the thermocouple in the dissolution kettle rises to about 57.2°C, start timing. After dissolving for 1 hour, heat-retain and filter. The filter cake is a DBA mixture, which will be used as a by-product after drying.

[0039] The filtrate was introduced into a crystallization kettle with a jacket temperature of 59.4°C, and when there was no particulate matter in the filtrate and the thermocouple of the crystallization kettle showed that the temperature was stable at 59.2°C, the cooling crystallization began. During the crystallization process, the stirring speed was 290r / min, and the co...

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Abstract

The invention discloses a method for separating and purifying glutaric acid in mixed binary acid by low-carbon halogenated hydrocarbon, and belongs to the technical field of mixture separation and purification. DBA (Dibutyl Adipate) raw materials are smashed and screened; the DBA raw materials are added into low-carbon halogenated hydrocarbon solvent to be heated, stirred and dissolved; then, filtering is carried out when mixture is hot, and obtained hot filtrate is added into a crystallizer to be stirred; after the temperature of the mixture is stable, cooling is carried out to a final crystallization temperature; the temperature is maintained for certain time, and then, constant-temperature filtering is carried out to obtain a glutaric acid crystal coarse product; the glutaric acid crystal coarse product is dissolved in the fresh low-carbon halogenated hydrocarbon solvent to be recrystallized. By use of the technical scheme of the invention, pure glutaric acid can be obtained by separation.

Description

technical field [0001] The invention belongs to the technical field of separation and purification of mixtures, in particular to a method for separating and purifying glutaric acid from mixed dibasic acids. Background technique [0002] Mixed dibasic acid (DBA) is a by-product of the production process of adipic acid, the main components of which are succinic acid (SA), glutaric acid (GA) and adipic acid (AA). Generally, 50-60kg of DBA by-product is produced for every 1t of adipic acid produced. Glutaric acid is the main mixed dibasic acid, accounting for about 60%. Glutaric acid is an important chemical raw material, widely used in chemical industry, textile, medicine, agriculture and so on. [0003] At present, the price of dibasic acid in the domestic market is about 3,000 yuan / ton, and the market price of glutaric acid is about 50,000 yuan / ton. Therefore, the successful separation of glutaric acid from DBA not only has considerable economic benefits, Moreover, it can ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/43C07C55/12
CPCC07C51/43C07C55/12
Inventor 彭胜王志彦王亚涛杨大志宁利民刘莉莉于泳
Owner TANGSHAN KAILUAN CHEM TECH CO LTD
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