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Method for synthesizing chloroacetaldehyde

A technology of monochloroacetaldehyde and chloroacetaldehyde, applied in chemical instruments and methods, preparation of carbon-based compounds, preparation of organic compounds, etc., can solve the problem of high synthesis cost, achieve low production cost, high product purity, and good yield rate effect

Inactive Publication Date: 2011-06-29
INST OF PLANT PROTECTION CHINESE ACAD OF AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has higher synthesis cost, and the raw material vinyl chloride is a toxic substance, and long-term inhalation and exposure to vinyl chloride can cause liver cancer

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Embodiment 1: in the four-necked flask of 1000ml, add catalyzer antimony trichloride (SbCl 3 ) 2.65g and 250ml of 40% acetaldehyde solution, cooled to below 10°C, and open the ventilation valve. Introduce chlorine gas slowly at the beginning (5 bubbles / min), then speed up to 20-30 bubbles / min, turn on the stirring switch of the constant temperature magnetic stirrer, let the cold acetaldehyde aqueous solution stir quickly, break the chlorine gas bubbles, Make it fully contact with acetaldehyde. Control of reaction temperature: control the temperature of the reaction system below 20°C, preferably around 15°C.

[0012] The reaction process was detected by gas chromatography. Control of reaction time: The end of the reaction is regarded as the relative content of the product no longer increasing. After the reaction was finished, distilled under atmospheric pressure and collected fractions to obtain 142.9 g of the product with a yield of 80.1%.

Embodiment 2

[0013] Embodiment 2: in the four-necked flask of 1000ml, add the mixture of catalyzer iron trichloride 5.6g and aluminum trichloride 4.8g, add the 85% acetaldehyde solution of 250ml again, be cooled to below 10 ℃, open ventilation valve. Introduce chlorine gas slowly (10 bubbles / min) at the beginning, then speed up to 30-40 bubbles / min, turn on the stirring switch of the constant temperature magnetic stirrer, let the cold acetaldehyde aqueous solution stir quickly, break the chlorine gas bubbles, Make it fully contact with acetaldehyde. Reaction temperature control: ice-water bath, so that the temperature of the reaction system is controlled below 20°C, preferably around 15°C.

[0014] The reaction process was detected by gas chromatography. Control of reaction time: The end of the reaction is regarded as the relative content of the product no longer increasing. After the reaction, the solid was filtered by suction and dried to obtain 269.2 g of chloroacetaldehyde, with a yi...

Embodiment 3

[0015] Embodiment 3: in the four-necked flask of 1000ml, add the mixture of catalyzer mercury sulfate 7.5g and the vitriol oil 4.8g, add the 20% acetaldehyde solution of 250ml again, be cooled to below 5 ℃, open ventilation valve. Introduce chlorine gas slowly (5 bubbles / min) at the beginning, then speed up to 20-40 bubbles / min, turn on the stirring switch of the constant temperature magnetic stirrer, let the cold acetaldehyde aqueous solution stir quickly, break the chlorine gas bubbles, Make it fully contact with acetaldehyde. Reaction temperature control: ice-water bath, so that the temperature of the reaction system is controlled below 10°C, preferably around 5°C.

[0016] The reaction process was detected by gas chromatography. Control of reaction time: The end of the reaction is regarded as the relative content of the product no longer increasing. After the reaction was finished, distilled under atmospheric pressure and collected fractions to obtain 57.1 g of the produ...

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PUM

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Abstract

The invention discloses a method for synthesizing chloroacetaldehyde through catalysis of aqueous solution of aldehyde. In the method, the aqueous solution of aldehyde is taken as a raw material, and the aldehyde is subjected to chlorination by controlling reaction temperature in the presence of a single or mixed catalyst; and after the reaction is finished, the product is subjected to distillation or suction filtration, and high-purity chloroacetaldehyde is obtained. The method has the advantages of high yield and light environmental pollution, and can be applied to preparation of a small amount of chloroacetaldehyde in a laboratory and industrial production.

Description

technical field [0001] The method relates to a preparation method of a fine chemical product, specifically a method for preparing a pesticide and a pharmaceutical intermediate monochloroacetaldehyde. Chloroacetaldehyde is an important organic synthesis intermediate and an important halogen derivative. It is widely used in the production of pesticides, medicines, and the preparation of organic raw materials. Background technique [0002] Chloroacetaldehyde, English name Chloroacetaldehyde, CAS NO: 107-20-0, molecular weight: 78.5, molecular formula C 2 h 3 ClO, a flammable and toxic liquid with a pungent pungent smell. The boiling point is 85-86°C. The flash point is 87.78°C. flammable. poisonous. Soluble in water, ether, methanol, acetone. 40% aqueous solution is a colorless transparent liquid. The relative density is 1.19. The boiling point is 99-100°C. The refractive index is 1.397. When the concentration in water is greater than 50%, the hemihydrate flake cryst...

Claims

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Application Information

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IPC IPC(8): C07C47/14C07C45/63B01J27/10B01J27/128B01J27/053
Inventor 折冬梅黄啟良李凤敏
Owner INST OF PLANT PROTECTION CHINESE ACAD OF AGRI SCI
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