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Production method of 4-chloro-2-cyanopyridine

The technology of a cyanopyridine and a production method is applied in the production field of tetrachloro-2-cyanopyridine, and can solve the problems of reducing catalyst activity, easily occurring high-temperature polymerization, shortening the service life of the catalyst, etc., so as to suppress harmful side reactions, improve the Product yield, effect of reducing chlorination temperature

Active Publication Date: 2014-03-26
JIANGYIN SULI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

European patent EP182111 introduced the reaction of 2-cyanopyridine and chlorine in a fluidized bed reactor equipped with activated carbon at 500°C to prepare tetrachloro-2-cyanopyridine. The main defect of this method is that due to the high reaction temperature, The fluidized bed reaction is not easy to control, and high temperature polymerization is prone to occur, and the produced polymer adheres to the catalyst layer, resulting in coking of the catalyst surface, reducing the catalyst activity and reducing the service life of the catalyst
Chinese patent CN100579964C also uses 2-cyanopyridine and chlorine as raw materials, and adopts activated carbon impregnated with ferric chloride and hydrochloric acid as the main catalyst to synthesize tetrachloro-2-cyanopyridine through gas phase chlorination reaction. The problem of low rate and poor product quality

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Embodiment 1: fluidized bed and fixed bed all do not add the coconut shell activated carbon catalyst of modification

[0026] Add 1000kg of ordinary coconut shell activated carbon catalyst of 24 meshes into the fluidized bed, and add 1200kg of ordinary coconut shell activated carbon catalysts mixed with 3 different particle sizes into the fixed bed, among which the particle size is 150kg for 16 meshes, 450kg for 25 meshes, and 600kg for 38 meshes. Check the airtightness of the reactor and the pipeline of the whole system to ensure that there is no air leakage and start heating to raise the temperature. When the temperature reaches 200°C, start to feed chlorine gas until the temperature of each point of the two reactors is stable and no trace is detected in the tail gas. HCl is released, and the activation is completed. The activation time is generally 3 hours, and the activation temperature is controlled within the range of 200-250°C.

[0027] After the catalyst is acti...

Embodiment 2

[0028] Embodiment 2: (only add the modified coconut shell activated carbon catalyst in the fluidized bed)

[0029]Embodiment 2 basic process is as described in example 1, and the added catalyzer of fluidized bed is modified coconut shell gac catalyst, and it has added 0.8% lanthanum chloride, 0.2% cerium chloride in the common coconut shell gac catalyst of 1000kg24 purpose, The fixed bed still uses common coconut shell activated carbon catalysts mixed with three different particle sizes, including 150kg for 16 meshes, 450kg for 25 meshes, and 600kg for 38 meshes. The fluidized bed reaction temperature is controlled at 200-300°C, and the fixed bed reaction temperature is controlled at 240-320°C. The tetrachloro-2-cyanopyridine content of the obtained product is 98.8%, the impurity content of pentachloropyridine is 2.5%, and the service life of the catalyst is 50 days.

Embodiment 3

[0030] Embodiment 3: (the coconut shell active carbon catalyst that only adds modification in the fixed bed)

[0031] The basic process of embodiment 3 is as described in Example 1. The fluidized bed is still 1000kg24 purpose coconut shell activated carbon catalyst, and the catalyst added by the fixed bed is a modified catalyst, which is 16 orders, 25 orders and 38 orders in 1200kg. 1% lanthanum chloride and 0.2% cerium chloride were added to the coconut shell activated carbon catalyst mixed 1:3:4. The fluidized bed reaction temperature is controlled at 200-300°C, and the fixed bed reaction temperature is controlled at 240-320°C. The obtained product The tetrachloro-2-cyanopyridine content of the obtained product is 98.5%, the impurity content of pentachloropyridine is 2.6%, and the service life of the catalyst is 46 days.

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Abstract

The invention relates to a production method of 4-chloro-2-cyanopyridine. The method comprises the following steps: taking 2-cyanopyridine and chlorine gas as raw materials, evaporating 2-cyanopyridine and preheated chlorine gas through an evapourizer, mixing evaporated 2-cyanopyridine and preheated chlorine gas to obtain a mixture, causing the mixture to sequentially pass through a fluidized bed reactor and a fixed bed reactor, which are filled with modified cocoanut active charcoal catalysts and connected in series to generate gas-phase catalytic chlorination to prepare 4-chloro-2-cyanopyridine, and achieving the production of 4-chloro-2-cyanopyridine. The modified cocoanut active charcoal catalysts are used in the reaction process, the reaction temperature is lowered, the activities of the catalysts is improved, the problem that the catalysts are liable to coking is solved, the service lives of the catalysts are prolonged, and meanwhile, the yield and the content of 4-chloro-2-cyanopyridine are increased.

Description

technical field [0001] The invention relates to a production method of tetrachlorocyanopyridine compounds, in particular to a production method of tetrachloro-2-cyanopyridine. It belongs to the field of organic chemical technology. technical background [0002] Tetrachlorocyanopyridine compounds have high biological activity and can be used as synthetic intermediates of pesticides, medicines and dyes. A series of pesticides developed and synthesized with tetrachloro-2-cyanopyridine, especially herbicides, have the characteristics of low dosage, high selectivity, low toxicity, small residual amount and short residual period in soil and plants. Development and ecological protection are of great significance. In recent years, with the continuous development of its downstream products, the scope of application and demand have grown rapidly. [0003] The production method of tetrachloro-2-cyanopyridine mainly uses 2-cyanopyridine and chlorine as raw materials, and is prepared ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/84
Inventor 缪金凤黄岳兴王成宇
Owner JIANGYIN SULI CHEM
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