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Aftertreatment method of chloral intermediate product synthesized by acetaldehyde aqueous solution

A technology of trichloroacetaldehyde and an aqueous solution, applied in directions such as separation/purification of carbonyl compounds, can solve the problems such as the retention of hydrated acetaldehyde products, the high cost of trichloroacetaldehyde synthesis, difficulty in improving yield and the like

Inactive Publication Date: 2011-06-15
INST OF PLANT PROTECTION CHINESE ACAD OF AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] But because the solubility of chloral in water is higher than that of organic solvent ether, ethanol, etc., so the chlorinated product of acetaldehyde aqueous solution is dissolved in raw water, and the current popular method is directly extracted from water with a water-insoluble organic solvent. Poor, a large amount of acetaldehyde hydrate products stay in water, it is difficult to increase the yield, resulting in waste; simultaneously with solvent azeotropic extraction of chloral, need to use a large amount of organic solvent, resulting in higher synthesis cost of chloral

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Example 1: In a 1000ml one-necked flask with magnetic stirring, add 250ml of 40% chloral solution, then add sodium sulfate 100g and chloroform 250ml, stir at room temperature for 10min., and leave standstill for 10min. Pour into 1000ml of liquid separation, let the stratified water layer stand and extract three times with equal volume of chloroform, combine the organic phases, rectify, collect chloral and chloroform respectively, and use the chloroform again.

Embodiment 2

[0016] Example 2: Add 250ml of 80% chloral solution in a 1000ml one-necked flask with magnetic stirring, then add sodium chloride 50g and benzene 250ml, stir at room temperature for 10min., and let stand for 10min. Pour into 1000ml of liquid separation, let the stratified water layer stand still and extract three times with equal volume of benzene, combine the organic phases, rectify, collect chloral and benzene respectively, and use the benzene again.

Embodiment 3

[0017] Example 3: In a 1000ml one-necked flask with magnetic stirring, add 250ml of 40% chloral solution, then add potassium nitrate 100g and ethyl acetate 250ml, stir at room temperature for 10min., and let stand for 10min. Pour into 1000ml of liquid separation, let the stratified water layer stand and extract three times with equal volume of ethyl acetate, combine the organic phases, rectify, collect chloral and ethyl acetate respectively, and use ethyl acetate again.

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Abstract

The invention discloses an aftertreatment method of a chloral intermediate product synthesized by an acetaldehyde aqueous solution. The method comprises the following steps of: in a system for preparing the chloral from the acetaldehyde aqueous solution, adding water-soluble inorganic salt into water in an amount differing according to the solubility of the inorganic salt in water; simultaneously, adding a water-insoluble organic solvent in an amount equal to the volume of the aqueous solution for extracting; and distilling under reduced pressure or normal pressure to obtain a mixture applied through target rectified chloral and an organic solvent.

Description

technical field [0001] The method relates to a post-processing method in the preparation process of fine chemical products, specifically a post-processing method in the preparation of pesticide and pharmaceutical intermediate chloral from acetaldehyde solution. Chloroacetaldehyde is an important organic synthesis intermediate and an important halogen derivative. It is widely used in the fields of production of pesticides, medicine, and preparation of organic raw materials. Background technique [0002] Chloral, English name Chloral, CAS NO: 75-87-6, molecular weight: 147.38, molecular formula C 2 HCl 3 O, a colorless, volatile oily liquid with a pungent odor. Melting point: -57.5, boiling point: 97.7, relative density (water=1): 1.51, relative density (air=1): 5.1, saturated vapor pressure (kPa): 4.67 / 20°C, solubility: soluble in water, ethanol , ether, chloroform, etc. Chloral is an important chemical intermediate, widely used in the preparation of pharmaceuticals (such...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/16C07C45/80
Inventor 折冬梅黄啟良李凤敏林德杰曲文岩
Owner INST OF PLANT PROTECTION CHINESE ACAD OF AGRI SCI
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