Synthesizing method of chloride

A synthesis method and technology of acyl chlorides, which are applied in the preparation of acyl halides, chemical recovery, organic chemistry, etc., can solve problems such as harsh working environment, not pleasant enough, unstable product quality, etc., achieve high yield and improve the effect of working environment

Inactive Publication Date: 2007-09-19
江苏强盛功能化学股份有限公司
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  • Summary
  • Abstract
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  • Application Information

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Problems solved by technology

But both also have their own deficiencies, such as the unstable product quality of the former, the reaction produces two parts of hydrogen chloride; the latter produces one part of hydrogen chloride
Since both have hydrogen chloride gas, it is not only necessary to increase the tail gas absorption device, but also the operating environment is harsh and not pleasant enough. In addition, the product contains more hydrogen chloride

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 391 g (2.0 mol) of raw material trichlorotoluene and 0.13 g (0.001 mol) of catalyst aluminum trichloride into the reactor, adjust the temperature to 100° C., drip 452 g (2.0 mol) of benzoic anhydride that melts, and maintain the temperature of the reactor. The temperature is 110-118°C, and the dropwise addition is completed in about 2 hours. After the dropwise addition of benzoic anhydride, the reaction was maintained at 140° C. for 4 hours. Sampling analysis: the yield of benzoyl chloride is 98.8%. Then the finished product of benzoyl chloride is collected by distillation under reduced pressure in the rectification tower; the aluminum trichloride catalyst is recovered from the still residue.

[0021] Result: bp.140-145℃ / 180mm, benzoyl chloride, colorless to light yellow liquid, GC content 99.22%.

Embodiment 2

[0023] Add 460g (2.0mol) of raw material p-chlorobenzotrichloride and 0.98g (0.01mol) of catalyst phosphoric acid into the reactor, adjust the temperature to 100-110°C, add 200g (1.96mol) of acetic anhydride dropwise, and maintain the temperature of reactor 1 The temperature is 105-110°C, and the dropwise addition is completed in about 2 hours. After the dropwise addition of acetic anhydride, the reaction was continued for 1 hour and the first fraction was collected. P-chlorotrichlorotoluene and acetic anhydride react rapidly under the action of catalyst phosphoric acid to generate acetyl chloride, which is separated from the reactor as the first fraction from the top of the rectification tower.

[0024] Then add 10 g of crude acetyl chloride (or equivalent to 6 g of acetic anhydride) into the reactor, and continue the reaction at 110° C. for 1 hour. Sampling analysis: the yield of p-chlorobenzoyl chloride was 98.3%. Then the crude product of acetyl chloride is distilled thr...

Embodiment 3

[0030] Add 460g (2.0mol) of the raw material o-chlorobenzotrichloride and 1.62g (0.01mol) of the catalyst iron trichloride into the reactor, adjust the temperature to 120°C, add 265g (2.04mol) of propionic anhydride dropwise, and maintain the temperature of the reactor The temperature was 80°C, and the dropwise addition was completed in about 2 hours. After adding propionic anhydride dropwise, the insulation reaction was continued for 3 hours. O-chlorotrichlorotoluene and propionic anhydride react rapidly under the action of catalyst ferric chloride to generate propionyl chloride, which is separated from the reaction kettle from the top of the rectifying tower as the first component.

[0031] Then the reaction solution was transferred to a reaction kettle, and the reaction was continued at 130° C. for 2 hours. Sampling analysis: the yield of o-chlorobenzoyl chloride is 98.6%. Then the crude product of propionyl chloride is distilled under reduced pressure in the rectifying t...

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Abstract

A synthetic method of acyl chloride belongs to the synthetic technical field of the intermediate for the chemical products, consisting of two steps firstly catalyzing the halogenated trichlorotoluene compound and the carboxylic anhydride to produce a single or complex acyl chloride in the effect of the catalyzer, and secondly getting corresponding acyl chloride after rectification. The inventive synthetic method of the acyl chloride can improve the working environment because there provides no excitant gas chlorine hydride. The catalyzer can be recycled. The yield is high in unit period because the produced carbonyl chloride with the low boiling point can be drived off in time.

Description

technical field [0001] The invention belongs to the technical field of synthesis of intermediates used in chemical products, and more specifically relates to a synthesis method of acid chlorides. Background technique [0002] Acid chlorides are important intermediates in organic synthesis, and are important acylation and benzylation reagents in the production of chemical products such as pesticides, medicines, dyes, organic peroxides, surfactants, and auxiliary agents. At present, the methods for preparing acid chlorides from α, α, and α-trichlorotoluene (hereinafter referred to as trichlorotoluene) mainly include trichlorotoluene hydrolysis and co-heating of trichlorotoluene and carboxylic acid. Both have certain practicability, such as the former is simple in process; the latter has high yield and low cost. But both also have their own deficiencies, such as the unstable product quality of the former, the reaction produces two parts of hydrogen chloride; the latter produce...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C63/70C07C63/04C07C53/42C07C53/38C07C51/58
CPCY02P20/584
Inventor 应志耀陆靖曲大伟
Owner 江苏强盛功能化学股份有限公司
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