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Method for producing o-chlorobenzonitrile

A technology of o-chlorobenzonitrile and o-chlorotoluene, applied in the preparation of hydrocarbon ammoxidation, organic chemistry, etc., can solve the problems of reactor load reduction, reactor amplification effect, and difficulty in removing heat from the reaction, so as to increase the reaction load, The effect of improving selectivity and overcoming the amplification effect

Inactive Publication Date: 2005-03-16
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] The technical problem to be solved by the present invention is to overcome problems such as reactor amplification effect and reaction heat removal difficulty caused by using a fixed bed in the method for the production of o-chlorobenzonitrile introduced in previous documents, and generally also need to add water in the process to reduce the load of the reactor The problem of providing a new method for the production of o-chlorobenzonitrile

Method used

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  • Method for producing o-chlorobenzonitrile
  • Method for producing o-chlorobenzonitrile
  • Method for producing o-chlorobenzonitrile

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Catalyst preparation:

[0053] 224g V 2 o 5 Add it into a solution at a temperature of 80-90° C. consisting of 490 milliliters of water and 468 grams of oxalic acid, stir well, and react to obtain a vanadium oxalate solution.

[0054] The weight percent concentration is 40% SiO 2 1250 grams of silica sol are slowly added in the above-mentioned solution under stirring, then add respectively by 864 grams of Cr (NO 3 ) 3 9H 2 O. 12.4 g KNO 3 , 71.6 g Co(NO 3 )·6H 2 A solution of O and 500 ml of water, 76.4 g of H 3 BO 3 , a solution composed of 85.1 grams of 85% phosphoric acid and 500 milliliters of water and 43.5 grams (NH 4 ) 6 Mo 7 o 24 4H 2 O and the solution that 100 milliliters of waters form, stir, heat and evaporate to solid content 40% (weight), obtain viscous slurry.

[0055] The above slurry was spray-dried in a spray dryer to shape, and the formed catalyst precursor was pre-calcined at 300°C for 2 hours, and then fired at 650°C for 4.5 hours to ...

Embodiment 2～10

[0066] The catalyst preparation method is the same as in Example 1, and the proportioning or composition of the catalyst is changed to obtain the catalyst composition in Table 1, and the catalyst evaluation method in Example 1 is used for evaluation. Its result list 1.

[0067]

Embodiment 11

[0074] According to the catalyst preparation method and composition of Example 1, 3.0 tons of industrial catalysts are produced, once filled in the 1000 tons / year o-chlorobenzonitrile fluidized bed reactor, and carried out industrial production according to the process evaluation conditions of Example 1, the catalyst is processed by half a year. Industrial operation calibration shows that the catalyst has good activity and stability. The results are shown in Table 2 below:

[0075] project

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Abstract

The present invention relates to a method for producing o-chlorobenzonitrile, and is characterized by that it adopts the fluidized bed catalyst process using vanadium-chromium-born as main active components, its operation conditions are as follows: reaction temp. is 300-500 deg.C, reaction process is normal pressure to 0.05 MPa, residence time is 0.2-20 sec. and the role ratio of reaction raw materials is: tolylchloride: ammonia: air=1:2-13:10-50.

Description

technical field [0001] The present invention relates to a process for the production of o-chlorobenzonitrile. Background technique [0002] O-chlorobenzonitrile is an important intermediate for dyes, medicines, pesticides and spices. For example, 2-cyano-4-nitroaniline, an important intermediate of multi-purpose azo disperse dyes, can be produced through nitration ammonolysis reaction of o-chlorobenzonitrile; biphenyl compound can be synthesized with halogenated benzene for the preparation of non-peptide anti-vascular Tensin can also prepare a variety of anti-inflammatory and bactericidal drugs. [0003] The most convenient and advanced method for preparing o-chlorobenzonitrile is the direct ammoxidation process of o-chlorotoluene developed and matured in the past 30 years. Because of its short process flow, easy operation, good product quality and high yield, it has developed rapidly in recent years . [0004] Main reaction formula: [0005] <...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C253/28C07C255/50
Inventor 陈金华顾龙勤施惠肖景娴胡永君
Owner CHINA PETROLEUM & CHEM CORP