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Preparation method and preparation device of trichloroacetyl chloride

A technology of trichloroacetyl chloride and preparation device, which is applied in the directions of acid halide preparation, organic compound preparation, feeding device, etc., can solve the problems of complex production process of trichloroacetyl chloride preparation device, etc., and achieves the solution of complex and simplified production process. The effect of the production process

Pending Publication Date: 2021-07-09
JIANGSU QIHENG AGRI & CHEM TECHCO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The object of the present invention is to provide a preparation method and a preparation device of trichloroacetyl chloride, aiming to solve the problem that the production process of the preparation method of trichloroacetyl chloride and the preparation device is complicated

Method used

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  • Preparation method and preparation device of trichloroacetyl chloride
  • Preparation method and preparation device of trichloroacetyl chloride
  • Preparation method and preparation device of trichloroacetyl chloride

Examples

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Embodiment 1

[0025] Example 1, see figure 1 , the invention provides a kind of preparation method of trichloroacetyl chloride, comprising:

[0026] S101, the temperature of the gas phase reactor 6 loaded with the pretreated activated carbon catalyst is raised to 130° C.;

[0027] The pretreatment method of activated carbon is to add preferred activated carbon into a pipe with a diameter of 25-100MM, and slowly heat it to 150°C under vacuum until no water is released. Nitrogen was introduced to normal pressure, and then chlorine gas was slowly introduced at 150°C for activation until the temperature of the activated carbon layer was stable, and then the temperature was lowered.

[0028] S102, the raw material ketene is passed into the gas phase reactor 6 at 50 g / hour, and the chlorine gas vaporized by liquid chlorine is passed into the gas phase reactor 6 at 265 g / hour;

[0029] Chlorine vaporized by ketene and liquid chlorine are both calibrated by flowmeters and then controlled for mete...

Embodiment 2

[0032] Example 2, see figure 2 , the invention provides a kind of preparation method of trichloroacetyl chloride, comprising:

[0033] S201, the temperature of the gas phase reactor 6 loaded with the pretreated activated carbon catalyst is raised to 130° C.;

[0034] The pretreatment method of activated carbon is to add preferred activated carbon into a pipe with a diameter of 25-100MM, and slowly heat it to 150°C under vacuum until no water is released. Nitrogen was introduced to normal pressure, and then chlorine gas was slowly introduced at 150°C for activation until the temperature of the activated carbon layer was stable, and then the temperature was lowered.

[0035] S202, raw material vinyl ketone is passed into gas-phase reactor 6 with 52 grams / hour, and the chlorine gas of liquid chlorine vaporization is passed into gas-phase reactor 6 with 275 grams / hour;

[0036] Chlorine vaporized by ketene and liquid chlorine are both calibrated by flowmeters and then controlle...

Embodiment 3

[0039] Example 3, see image 3 , the invention provides a kind of preparation method of trichloroacetyl chloride, comprising:

[0040] S301. Add 200 g of diketene and 0.2 g of pyridine into the reactor;

[0041] The reactor is 100ml.

[0042] S302. When the temperature of the reactor is 10-120° C., feed chlorine gas until it is no longer absorbed to obtain the primary product of trichloroacetyl chloride.

[0043] About 1100g of chlorine gas was introduced, and the content of the initial product was trichloroacetyl chloride: 96.7%, monochloroacetyl chloride: 0.8%, dichloroacetyl chloride: 0.5%, carbon tetrachloride: 0.7% and others: 1.3%.

[0044] see Figure 4, the present invention also provides a preparation device for trichloroacetyl chloride, comprising a ketene intake pipe 1, a buffer tank 3, a vaporizer 2, a gas phase reactor 6, a first chlorine gas intake pipe 16, a condenser 7, a receiving tank 8, Absorption mechanism 9, hydrochloric acid tank 10, delivery mechanis...

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Abstract

The invention discloses a preparation method and a preparation device of trichloroacetyl chloride. The preparation method comprises the following steps: simultaneously carrying out a catalytic gas-phase reaction on gas-phase ketene or gas-phase ketene dimer and chlorine, or introducing chlorine into liquid ketene or ketene dimer in the presence of an organic base catalyst to finish a liquid reaction; collecting a reaction product, and carrying out atmospheric distillation; and collecting the distillate of the temperature of 116-118 DEG C to obtain trichloroacetyl chloride. The invention provides the novel trichloroacetyl chloride synthesis method, the production process is simplified, and the problem that a preparation method and a preparation device of trichloroacetyl chloride are complex in production process is solved.

Description

technical field [0001] The invention relates to the technical field of fine organic chemicals, in particular to a preparation method and a preparation device of trichloroacetyl chloride. Background technique [0002] Trichloroacetyl chloride is an excellent acylating agent and organic synthesis intermediate, widely used in the synthesis of pesticides, medicines, organic intermediates and fine chemical products. The existing production process of trichloroacetyl chloride is complicated. Contents of the invention [0003] The object of the present invention is to provide a kind of preparation method and preparation device of trichloroacetyl chloride, aim to solve the problem that the production process of the preparation method of trichloroacetyl chloride and preparation device is complicated. [0004] To achieve the above object, the invention provides a kind of preparation method of trichloroacetyl chloride, comprising: [0005] Simultaneously catalyzing gas phase reacti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/58C07C51/64C07C53/48B01J4/00B01J12/00
CPCC07C51/58C07C51/64B01J4/001B01J12/00C07C53/48
Inventor 袁绍志
Owner JIANGSU QIHENG AGRI & CHEM TECHCO
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