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Novel process for producing trichloro-acetic chloride

A technology of trichloroacetyl chloride and acid chloride, which is applied in the preparation of carboxylate, organic compound, organic chemistry, etc., can solve the problems of incomplete reaction, difficult separation, environmental pollution, etc., and achieve low production cost, simple process, The effect of high reaction yield

Inactive Publication Date: 2013-05-08
SHANXI SANWEI FENGHAI CHEM
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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

[0010] Step 1: Chloroacetic acid waste liquid refining

[0011] 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.

[0012] Step 2: Acid Chlorination

[0013] 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 method for preparing trichloro-acetic chloride by using chloroacetic acid waste liquid as a raw material, and belongs to the field of organic chemicals and preparation technology. The method comprises the following steps of (1) pumping chloroacetic acid waste liquid refined by a rectifying tower into an acylation kettle, adding a proper amount of sulphur, and passing a chlorine gas at a certain temperature for reaction, and thus mixed acid chloride is obtained after the reaction, wherein to make the chlorine gas reacted adequately, cross chloride is adopted by using a main kettle and an assistant kettle; and (2) adding the mixed acid chloride into a chlorination reaction vessel, reacting by using pyridine as a catalyst and 4-dimethylamino pyridine as a cocatalyst and passing the chlorine gas for reaction at a certain temperature, and thus trichloro-acetic chloride is formed. The novel process has wide raw material source and low production cost and is suitable for industrialized production.

Description

technical field [0001] The invention relates to a method 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 above-mention...

Claims

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Application Information

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IPC IPC(8): C07C53/48C07C51/62
Inventor 薛振海
Owner SHANXI SANWEI FENGHAI CHEM
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