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Method for synthesizing 2,6-dichlorobenzonitrile by ammoxidation

A dichlorobenzonitrile and ammoxidation technology, which is applied in the preparation of hydrocarbon ammoxidation, chemical instruments and methods, organic chemistry, etc., can solve the problems of long residence time, long process flow and high catalyst activity, and achieves reasonable design and operability. The effect of strong performance and high overall yield

Inactive Publication Date: 2015-02-04
SUZHOU JONATHAN NEW MATERIALS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has long process flow, high cost, large amount of waste water and serious pollution
[0003] More advanced technology is to apply o-chlorobenzonitrile fluidized bed technology and catalyst mechanically at present, as Chinese patent ZL97109006.8, but, because of the sp

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] A method for synthesizing 2,6-dichlorobenzonitrile by ammoxidation. The method uses 2,6-dichlorotoluene, ammonia and air as raw materials, and a catalyst is filled in a fixed bed. At a temperature of 350° C. and a pressure of 0.02 MPa, One-step synthesis of 2,6-dichlorobenzonitrile; the molar ratio of raw materials is 2,6-dichlorotoluene:ammonia=1:2.8, and the standard air volume is 0.2m 3 / liter of catalyst L h;

[0016] The preparation method of the catalyst is that the soluble salts of the active ingredient ammonium metavanadate, ammonium molybdate, ammonium chromate, phosphoric acid and potassium carbonate are formulated into a uniform solution, and the carrier γ-Al 2 o 3 Immerse it in it, age it at room temperature, put it into an electric furnace for activation after drying, and obtain a catalyst with a loading rate of 8%;

[0017] The process is as follows: control the temperature of the fixed bed catalyst at 365±1°C, the temperature of the premixed raw materi...

Embodiment 2

[0019] A method for synthesizing 2,6-dichlorobenzonitrile by ammoxidation. The method uses 2,6-dichlorotoluene, ammonia and air as raw materials, and a catalyst is filled in a fixed bed. At a temperature of 350° C. and a pressure of 0.02 MPa, One-step synthesis of 2,6-dichlorobenzonitrile; the molar ratio of raw materials is 2,6-dichlorotoluene:ammonia=1:2.8, and the standard air volume is 0.2m 3 / liter of catalyst L h;

[0020] The preparation method of the catalyst is that the soluble salts of the active ingredient ammonium metavanadate, ammonium molybdate, ammonium chromate, phosphoric acid and potassium carbonate are formulated into a uniform solution, and the carrier γ-Al 2 o 3 Immerse it in it, age at room temperature, put it into an electric furnace for activation after drying, and obtain a catalyst with a loading rate of 6%;

[0021] The process is as follows: control the temperature of the fixed bed catalyst at 365±1°C, the temperature of the premixed raw material ...

Embodiment 3

[0023] A method for synthesizing 2,6-dichlorobenzonitrile by ammoxidation. The method uses 2,6-dichlorotoluene, ammonia and air as raw materials, and a catalyst is filled in a fixed bed. At a temperature of 350° C. and a pressure of 0.02 MPa, One-step synthesis of 2,6-dichlorobenzonitrile; the molar ratio of raw materials is 2,6-dichlorotoluene:ammonia=1:2.8, and the standard air volume is 0.2m 3 / liter of catalyst L h;

[0024] The preparation method of the catalyst is that the soluble salts of the active ingredient ammonium metavanadate, ammonium molybdate, ammonium chromate, phosphoric acid and potassium carbonate are formulated into a uniform solution, and the carrier γ-Al 2 o 3 Immerse it in it, age at room temperature, put it into an electric furnace for activation after drying, and obtain a catalyst with a loading rate of 12%;

[0025] The process is as follows: control the temperature of the fixed bed catalyst at 365±1°C, the temperature of the premixed raw material...

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PUM

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Abstract

The invention relates to a method for synthesizing 2,6-dichlorobenzonitrile by ammoxidation, which comprises the following step: by using 2,6-dichlorotoluene, ammonia and air as raw materials, carrying out one-step synthesis in a catalyst-filled fixed bed at 350-375 DEG C under the pressure of 0.02-0.1 MPa to obtain the 2,6-dichlorobenzonitrile, wherein the mole ratio of the 2,6-dichlorotoluene to the ammonia is 1:(2.8-5), the standard state air quantity is 0.2-0.5 m<3>/L catalyst L.h, and the catalyst is P-V-Mo-Cr-K-O/gamma-Al2O3. The method has the advantages of reasonable design, high operability and high overall yield. The brand-new ammoxidation catalyst is adopted to obtain favorable effect, so that the conversion rate of the 2,6-dichlorotoluene is up to 99.5%, and the mole yield of the 2,6-dichlorobenzonitrile is up to 95.0%.

Description

technical field [0001] The invention relates to a method for synthesizing 2,6-dichlorobenzonitrile by ammoxidation. Background technique [0002] 2,6-Dichlorobenzonitrile can be used in pesticides, medicines, pigments, dyes and other industries. The traditional synthesis method of 2,6-dichlorobenzonitrile is: 6-chloro-o-nitrotoluene reacts with chlorine gas, chlorates and removes the nitro group to obtain 2,6-dichloro-chlorobenzyl chloride mixture; Chlorochlorobenzyl chloride mixture is hydrolyzed into 2,6-dichlorobenzaldehyde in formic acid and zinc chloride aqueous solution; 2,6-dichlorobenzaldehyde reacts with hydroxylamine hydrochloride and dehydrates into 2,6-dichlorobenzonitrile. This method has long process flow, high cost, large amount of waste water and serious pollution. [0003] More advanced technology is to apply o-chlorobenzonitrile fluidized bed technology and catalyst mechanically at present, as Chinese patent ZL97109006.8, but, because of the special struc...

Claims

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Application Information

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IPC IPC(8): C07C255/50C07C253/28B01J27/199
Inventor 李卓才李苏杨
Owner SUZHOU JONATHAN NEW MATERIALS TECH
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