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Method for producing high-purity pentachloro benzonitrile

The technology of a kind of pentachlorobenzonitrile and its production method is applied in the production field of high-purity pentachlorobenzonitrile, which can solve the problems of low pentachlorobenzonitrile content, high reaction temperature, and low conversion rate of benzonitrile, and achieve improved selectivity , increase the content, overcome the effect of clothing and unloading difficulties

Active Publication Date: 2018-01-19
JIANGYIN SULI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] For the problems existing in the technical background, the object of the present invention is to overcome the problems such as the high reaction temperature encountered in the process of producing pentachlorobenzonitrile, the low content of produced pentachlorobenzonitrile and the low conversion rate of benzonitrile

Method used

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Examples

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Effect test

preparation example Construction

[0029] The preparation of graphene oxide includes the following steps: first step, weigh 6g of potassium permanganate and 1g of graphite powder in a beaker and stir evenly to form a mixture. In the second step, 120 mL of concentrated sulfuric acid and 10 mL of phosphoric acid were successively added into a three-neck flask, and stirred for 10 min. In the third step, slowly add the mixture of potassium permanganate and graphite powder prepared in the first step into the three-necked flask in the second step, and stir for 12 hours under the condition of a water bath at a temperature of 48°C. The fourth step is to take another beaker, add an appropriate amount of ice cubes and 6mL hydrogen peroxide into the beaker, and then transfer the reactants of the third step to the beaker with ice cubes and hydrogen peroxide, and let it stand for 24 hours. If stratification occurs, remove the yellow solution in the lower layer, add distilled water repeatedly, stir, centrifuge, and test the ...

Embodiment 1

[0031] Embodiment 1: (fluidized bed and fixed bed add modified active carbon catalyst at the same time)

[0032]Add 1000kg of activated carbon A1 into the fluidized bed, and 1000kg of activated carbon B1 into the fixed bed to check the airtightness of the system pipeline. When the airtightness is ensured, feed the carrier gas (nitrogen) and heat up to 120 ℃, keep constant temperature for 1h. Then the temperature is raised to 230°C, and chlorine gas is introduced to activate the activated carbon until the temperature of each point of the two reactors is stable, and hydrogen chloride gas cannot be detected in the tail gas. The activation time is generally 3 hours. After the catalyst activation is completed, the raw material benzonitrile is pumped into the vaporizer through a metering pump, and at the same time, the preheated nitrogen gas is passed into the vaporizer at a temperature of 250°C to vaporize the benzonitrile, and the mole of benzonitrile and nitrogen is The ratio is...

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Abstract

The invention relates to a method for producing high-purity pentachloro benzonitrile. The method comprises the following steps: a, preparing graphene oxide; b, preparing a modified activated carbon catalyst; c, activating the modified activated carbon catalyst; d, pre-vaporizing cyanobenzene; e, performing a chlorination reaction; and f, performing trapping. According to the method, optimization selection is performed on the catalyst, the catalyst is modified, and the modified activated carbon catalyst is fully catalyzed; meanwhile, an improved compound bed process is adopted; and through improvement of the catalyst and the production process, the temperature required for the chlorination reaction is greatly reduced, the product content (more than or equal to 99.6%) is improved, and service life of the catalyst is prolonged to 720 h.

Description

technical field [0001] The invention belongs to the technical field of organic chemical industry, in particular to a production method of high-purity pentachlorobenzonitrile. technical background [0002] Pentachlorobenzonitrile is an important intermediate used in the production of fine chemical products such as pesticides, medicines, dyes, coatings, and functional materials. Domestic Zhejiang and Hunan have respectively built 100-ton industrial production test devices, but there are no relevant written reports. The survey shows that the current domestic market capacity of pentachlorobenzonitrile is about 5,000 tons per year, and currently it mainly relies on imports to meet the needs of the domestic market. In addition, pentachlorobenzonitrile has a large profit potential. Therefore, it is particularly necessary to develop a method to realize the large-scale production of pentachlorobenzonitrile to replace imported products. [0003] Ruetman reported that N-methylanili...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/06B01J37/02B01J37/24B01J37/12B01J21/18B01J35/10C07C253/30C07C253/34C07C255/50
Inventor 缪金凤汪静莉黄岳兴王成宇鲍丽平
Owner JIANGYIN SULI CHEM
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