Liquid-liquid extraction process of dioxyethyl methane and water solution of ethanol

A technology of diethoxymethane and ethanol aqueous solution, which is applied in the fields of ether separation/purification, ether preparation, organic chemistry, etc., can solve the problems of high energy consumption and achieve the effect of low energy consumption

Inactive Publication Date: 2003-01-01
NANJING NORMAL UNIVERSITY
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Problems solved by technology

Regardless of the acid catalysis method or the chloramphenicol by-product method, in the separation process, the precision rectification method is used to separate the mixed product. Since the boiling point of DEM in the product is close to the azeotropic point of ethanol and water, the reflux ratio (R) of the rectification method is used. Controlled at about 30:1, not only consumes a lot of energy, but also can only get about 95% of DEM
At present, there are no reports on DEM extraction and purification at home and abroad, so the development of effective separation technology is not only conducive to improving product purity, but also conducive to reducing energy consumption.

Method used

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  • Liquid-liquid extraction process of dioxyethyl methane and water solution of ethanol
  • Liquid-liquid extraction process of dioxyethyl methane and water solution of ethanol
  • Liquid-liquid extraction process of dioxyethyl methane and water solution of ethanol

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Embodiment 1

[0012] Embodiment 1, with reference to figure 1 , figure 2 Shown process diagram, raw material is ethanol aqueous solution of DEM, and the content of DEM, ethanol and water is respectively 50%, 45%, 5% (mass content), and raw material is 20Kg, and pure extraction agent S1~S3 is respectively 20Kg. In the case of 298.2K, press figure 1 As shown in the process flow, the mixed liquid is sent into the extractor and fully stirred with the inflowing extractant glycerin, separated in layers, and the extract phase (E1~E3) and raffinate phase (R1~R3) are balanced in each stage of extractor state, the final extraction phase E1+E2+E3 is processed by a rectifying tower, and the composition of E1~E3 and R1~R3 after separation is shown in Table 2 (excluding the amount of solvent). The results in Table 2 show that after three extractions, the DEM yield reaches 98.9%, the purity can reach 99.6% (mass content). After the treatment, the solvent (S) is recycled, and the tower top (E) is fur...

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Abstract

Dioxyethyl methane (DEM) and water solution of ethanol are liquid-liquid extracted with polyol as extractant, and after delaminating separation, the extraction phase is refined, the processed solvent is used circularly and the raffinate contains DEM in higher purity. The optimized scheme is cross current extraction and counter current extraction process, in which material DEM and water solution of ethanol are made to contact with extractant propanetriol flowing in reverse direction in an extracting tower, with the raffinate containing DEM over 99.6%, the mixed extractant liquid being separated in refining tower and the water solution of ethanol being obtained from the tower top. The said process can separate DEM and water solution of ethanol effectively.

Description

technical field [0001] The invention relates to a chemical extraction process, in particular to a liquid-liquid extraction method of diethoxymethane (DEM) and ethanol aqueous solution. Background technique [0002] Diethoxymethane (DEM) is an important solvent and pharmaceutical intermediate, and it is generally produced by acid catalysis and chloramphenicol by-product method. Regardless of the acid catalysis method or the chloramphenicol by-product method, in the separation process, the precision rectification method is used to separate the mixed product. Since the boiling point of DEM in the product is close to the azeotropic point of ethanol and water, the reflux ratio (R) of the rectification method is used. Controlling it at about 30:1 not only consumes a lot of energy, but also only about 95% of DEM can be obtained. At present, there are no reports on DEM extraction and purification at home and abroad. Therefore, the development of effective separation technology is n...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/38C07C43/04
Inventor 顾正桂毛梅芳林军宋晓栋蔡琳娜
Owner NANJING NORMAL UNIVERSITY
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