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Process and device for producing tetrachloro-2-cyanopyridine with liquid chromatography

A cyanopyridine and a production process technology are applied in the field of liquid-phase chlorination reaction processes and devices to achieve the effects of low energy consumption, improved safety and operability, and reduced processing load

Active Publication Date: 2017-11-07
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Aiming at the problems existing in the existing gas-phase chlorination process, the present invention proposes a new process and device capable of overcoming the disadvantages of the above-mentioned gas-phase chlorination process, that is, adopting a new liquid-phase chlorination process

Method used

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  • Process and device for producing tetrachloro-2-cyanopyridine with liquid chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Fill 20kg of FeCl loaded with 5% (wt) in the first microbubble generator (C-1) and the second microbubble generator (C-2) respectively 3Activated carbon was used as a pre-reaction catalyst and a main reaction catalyst. After the liquid 2-cyanopyridine is preheated to 30°C, it enters the first gas-liquid enhanced reaction tower (R-1) at a rate of 125kg / h through pipeline 1 to fully mix with chlorine gas, and the gas-liquid mixture passes through pipeline 16 and the first cycle The pump (P-1) enters the first microbubble generator (C-1), and the pre-reaction is carried out in the first microbubble generator (C-1), and part of the gas phase material can also enter the first microbubble generator through the pipeline 15 The device (C-1) completes the circulation of the gas phase material. The material from the first microbubble generator (C-1) enters the first gas-liquid intensified reaction tower (R-1) through pipeline 18 and fully mixes with chlorine gas. The first gas-...

Embodiment 2

[0039] In the first microbubble generator (C-1) and the second microbubble generator (C-2), respectively fill 18 kg with 5% (wt) FeCl 3 Activated carbon was used as a pre-reaction catalyst and a main reaction catalyst. After the liquid 2-cyanopyridine is preheated to 70°C, it enters the first gas-liquid enhanced reaction tower (R-1) at a rate of 130kg / h through pipeline 1 to fully mix with chlorine gas, and the gas-liquid mixture passes through pipeline 16 and the first cycle The pump (P-1) enters the first microbubble generator (C-1), and the pre-reaction is carried out in the first microbubble generator (C-1), and part of the gas phase material can also enter the first microbubble generator through the pipeline 15 The device (C-1) completes the circulation of the gas phase material. The material from the first microbubble generator (C-1) enters the first gas-liquid intensified reaction tower (R-1) through pipeline 18 and fully mixes with chlorine gas. The first gas-liquid ...

Embodiment 3

[0041] Fill the first microbubble generator (C-1) and the second microbubble generator (C-2) with 25 kg of FeCl loaded with 5% (wt) 3 Activated carbon was used as a pre-reaction catalyst and a main reaction catalyst. After the liquid 2-cyanopyridine is preheated to 110°C, it enters the first gas-liquid enhanced reaction tower (R-1) at a rate of 130kg / h through pipeline 1 to fully mix with chlorine gas, and the gas-liquid mixture passes through pipeline 16 and the first cycle The pump (P-1) enters the first microbubble generator (C-1), and the pre-reaction is carried out in the first microbubble generator (C-1), and part of the gas phase material can also enter the first microbubble generator through the pipeline 15 The device (C-1) completes the circulation of the gas phase material. The material from the first microbubble generator (C-1) is fully mixed with chlorine gas through the first gas-liquid enhanced reaction tower (R-1) in pipeline 18. The first gas-liquid enhanced ...

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Abstract

The invention relates to a process for producing tetrachloro-2-cyanopyridine. The process comprises steps as follows: liquid 2-cyanopyridine is preheated, flows into a gas-liquid reinforcement pre-reactor and pre-reacts with chlorine under the action of a pre-reaction catalyst; after the reaction, a gas-phase material is washed and flows into an absorption device to be absorbed; a liquid-phase material after pre-reaction enters a gas-liquid reinforcement main reactor and has a chlorination reaction with the chlorine under the action of a main reaction catalyst; the liquid-phase material discharged from the main reactor is introduced into an evaporator for separation, and finally a tetrachloro-2-cyanopyridine solid is obtained. The process has the advantages that the production flow of tetrachloro-2-cyanopyridine is shortened, and safety and operability of the production process are improved; the utilization rate of the chlorine is increased, and the exhaust gas treatment load is reduced; the chlorination reaction temperature is reduced, the problem that the catalyst is prone to coking is solved, and the service life of the catalyst is prolonged; the yield and content of the product are increased, the difficulty of product purification is reduced, the reaction temperature is low, energy consumption is small; the process is green and environment-friendly.

Description

technical field [0001] The invention relates to a liquid-phase chlorination reaction process and device of tetrachloro-2-cyanopyridine, which belongs to the technical field of fine chemical industry. Background technique [0002] Pyridine chlorides have high biological activity and are widely used as intermediates in the synthesis of pesticides, medicines and dyes. Using tetrachloro-2-cyanopyridine as raw material, a series of pesticides such as insecticides and herbicides can be developed and synthesized. These pesticides usually have the advantages of less useful amount, high selectivity, low toxicity, small residual amount, and short residual period. , which is of great significance to the sustainable use of soil, agricultural development and environmental protection. In recent years, the development, application range and demand of downstream products using tetrachloro-2-cyanopyridine as raw materials are all growing rapidly. [0003] At present, the production method ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/84
CPCC07D213/84
Inventor 周政张志炳王宝荣杨国强刘甲杜惠媛刘承智
Owner NANJING UNIV
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