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Method for re-activating inactivated catalyst through catalytic chlorination of pyridine nitrile

A catalyst, pyridine nitrile technology, applied in physical/chemical process catalysts, chemical instruments and methods, chemical recovery and other directions, can solve problems such as easy deactivation of catalysts, and achieve the effects of small equipment investment, obvious economic benefits, and improved utilization value

Inactive Publication Date: 2011-07-27
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Because the catalyst is easily deactivated in the reaction process, a large amount of deactivated catalyst activated carbon is produced in the process of producing tetrachloropyridine nitrile. The conventional method adopts incineration treatment, which produces a large amount of waste gas

Method used

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  • Method for re-activating inactivated catalyst through catalytic chlorination of pyridine nitrile
  • Method for re-activating inactivated catalyst through catalytic chlorination of pyridine nitrile
  • Method for re-activating inactivated catalyst through catalytic chlorination of pyridine nitrile

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] In a fixed-bed reactor equipped with 38.4g of pyridine nitrile catalytic chlorination deactivation catalyst activated carbon, under the protection of nitrogen with a flow rate of 2-4L / h, the material is heated to 550±5°C by electric heating, and kept for 20min; The gaseous product was condensed to normal temperature to obtain a white solid powder product with a mass of 5.7 g; wherein the mass fraction of tetrachloropyridinenitrile was 64.32%, and that of pentachloropyridine was 32.16%. Continue to raise the temperature to 850±5°C, stop feeding nitrogen, change to feed water vapor, the flow rate is 0.6g / min, activate at 850±5°C for 60min, the physical properties of activated carbon before and after regeneration are shown in Table 1.

[0019] Table 1 Comparison of catalysts before and after regeneration

[0020]

Embodiment 2

[0022] In a fixed-bed reactor equipped with 38.4g pyridine nitrile catalytic chlorination deactivation catalyst activated carbon, under the protection of carbon dioxide with a flow rate of 5-6L / h, the material was heated to 400±5°C by microwave heating and kept for 60min; The gas phase product was condensed to normal temperature to obtain a white solid powder product with a mass of 5.9 g; wherein the mass fraction of tetrachloropyridine nitrile was 66.42%, and that of pentachloropyridine was 31.83%. Continue to heat up to 900±5°C, and activate at this temperature for 40 minutes. The physical properties of activated carbon before and after regeneration are shown in Table 2.

[0023] Table 2 Comparison of catalysts before and after regeneration

[0024]

Embodiment 3

[0026] In a fixed-bed reactor equipped with 38.4g of pyridine nitrile catalytic chlorination deactivation catalyst activated carbon, add carbon dioxide with an oxygen content of 5% and a flow rate of 5-6L / h, heat the material to 300°C by microwave heating, and stop Heating, the temperature of the material was slowly raised to 600°C, and kept for 40 minutes; the gas phase product was condensed to room temperature to obtain a white solid powder product with a mass of 5.8g. Wherein the mass fraction of tetrachloropyridine nitrile is 68.42%, and the mass fraction of pentachloropyridine is 30.83%. Continue to heat up to 700±5°C, and activate at this temperature for 60 minutes. The physical properties of activated carbon before and after regeneration are shown in Table 3.

[0027] Table 3 Comparison of catalysts before and after regeneration

[0028]

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PUM

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Abstract

The invention discloses a method for re-activating an inactivated catalyst through catalytic chlorination of pyridine nitrile. The method comprises the following steps of: introducing an oxygen-containing inert gas and heating inactivated activated carbon to rise the temperature to 300 DEG C to 600 DEG C; and condensing a gas phase product to obtain a crystal mixture which mainly contains tetrachloro pyridine nitrile. With the adoption of the method, high-value products can be recycled from the waste catalyst, the pollution of the inactivated activated carbon to the environment is reduced simultaneously, the activated carbon is further heated for activation, and then the performance of the activated carbon can be completely recovered.

Description

technical field [0001] The invention relates to a method for recovering tetrachloropyridine nitrile from an active carbon catalyst deactivated by catalytic chlorination of pyridine nitrile and reviving the catalyst. Background technique [0002] The chemical name of tetrachloropyridinecarbonitrile is 3,4,5,6-tetrachloropyridine-2-carbonitrile. It is an important organic intermediate that can be used in the synthesis of dyes, pesticides, plastic additives, etc. At present, the main method of synthesizing tetrachloropyridine nitrile is: in a fixed-bed reactor, activated carbon is used as a catalyst, and the gases of chlorine, nitrogen and 2-cyanopyridine are introduced to react at 280 ° C to 350 ° C, and the mixed gas is cooled, The product tetrachloropyridine nitrile was obtained by crystallization and separation. [0003] Because the catalyst is easily deactivated in the reaction process, a large amount of deactivated catalyst activated carbon is produced in the process of...

Claims

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Application Information

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IPC IPC(8): B01J21/20B01J21/18C07D213/84
CPCY02P20/584
Inventor 罗和安艾秋红王浩新王良芥黄荣辉
Owner XIANGTAN UNIV
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