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Production technology of trichloroacetyl chloride

A technology for the production of trichloroacetyl chloride, which is applied in the field of preparing trichloroacetyl chloride, can solve the problems of incomplete reaction, environmental pollution, and separation difficulties, and achieve the effects of low production cost, high reaction yield and simple process

Pending Publication Date: 2015-12-16
山东谦诚工贸科技有限公司
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AI Technical Summary

Problems solved by technology

But above-mentioned preparation method has some problems in varying degrees, as: higher pressure, incomplete reaction, greater toxicity, difficult separation, problems such as environmental pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0011] Step 1: Chloroacetic acid waste liquid refining

[0012] Throw in 3.5t of chloroacetic acid waste liquid, turn on condensed water and brine, heat up and distill at atmospheric pressure, collect the distillate into four altars or let it go directly, take an instantaneous sample as water when the kettle temperature is 130°C, and stop atmospheric distillation when the water content is less than 30%. After 3 hours of normal fractionation, take an instant sample to test the water content. If the water content is less than 1-3%, the distillation is stopped, the temperature is lowered to 50°C, and the mother liquor is introduced into the storage tank.

[0013] Step 2: Acid Chlorination

[0014] Put in 3000kg of refined mother liquor and 390kg of sulfur, adjust the valves according to the order of the main and auxiliary kettles, open the condensed water, and freeze the brine. If the temperature of the main kettle is first raised to 75°C when feeding materials for the first ti...

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Abstract

The invention relates to a production technology of trichloroacetyl chloride. Chloroacetic acid waste liquor is used as a raw material and belongs to the technical field of organic chemicals and preparation. The production method comprises steps as follows: (1) the chloroacetic acid waste liquor refined by a rectifying column is pumped into an acylation kettle with vacuum, a certain amount of sulfur is added, chlorine is fed at a certain temperature for a reaction, cross chlorination with main and auxiliary tanks is adopted to enable the chlorine to fully react, and mixed acyl chloride is produced through the reaction; (2) the mixed acyl chloride is added to a chlorination kettle, pyridine is used as a catalyst, 4-dimethylamino pyridine is used as a promoter, the chlorine is fed for a reaction at a certain temperature, and the trichloroacetyl chloride is produced. The raw material is wide in source, the production cost is low, and the production technology is suitable for industrial production.

Description

technical field [0001] The invention relates to a production process for preparing trichloroacetyl chloride, which uses chloroacetic acid waste liquid as a raw material, and belongs to the technical field of organic chemicals and preparation. Background technique [0002] Trichloroacetyl chloride is an important organic chemical raw material, which is widely used in pharmaceutical, pesticide, dye, daily chemical, petroleum, fine chemical and other industries. The method of synthetic trichloroacetyl chloride has multiple, as (1) trichloroacetic acid is in CsCl, KCl, K 2 CO 3 And quaternary ammonium salt and other catalysts in the presence of thermal decomposition reaction. (2) Trichloroacetic acid reacts with thionyl chloride in the presence of activated carbon or DMF. (3) with CCl 4 , CO as raw material, in the catalyst such as CuCl, AlCl 3 react in the presence of . (4) Trichloroacetic acid is obtained by acylation with phosgene in the presence of DMF. However, the a...

Claims

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Application Information

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IPC IPC(8): C07C51/62C07C51/60C07C53/48
CPCC07C51/62C07C51/60C07C53/48
Inventor 段维亮李斌
Owner 山东谦诚工贸科技有限公司
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