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Method for ammoxidation preparation of 2,4-dichlorobenzonitrile

A technology of dichlorobenzonitrile and ammoxidation is applied in the preparation of hydrocarbon ammoxidation, chemical instruments and methods, organic chemistry, etc., and can solve the problems of low fixed-bed evaluation yield, poor fluidization quality, and high production cost, Achieve the effect of improving fluidization quality, reducing production cost and reducing channel flow

Inactive Publication Date: 2012-10-24
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved by the present invention is that there is poor fluidization quality in the fluidized bed reactor in the past production technology, resulting in low yield; or the use of fixed bed evaluation yield is still low, high production cost, providing a new Method for preparing 2,4-dichlorobenzonitrile by ammoxidation

Method used

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  • Method for ammoxidation preparation of 2,4-dichlorobenzonitrile
  • Method for ammoxidation preparation of 2,4-dichlorobenzonitrile
  • Method for ammoxidation preparation of 2,4-dichlorobenzonitrile

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Experimental program
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Effect test

Embodiment 1

[0037] Catalyst preparation:

[0038] 201 g V 2 o 5 Add it into a solution at a temperature of 80-90° C. consisting of 440 milliliters of water and 420 grams of oxalic acid, stir well, and react to obtain a vanadium oxalate solution.

[0039] 40% (weight) SiO 2 1250 grams of silica sol were slowly added to the above solution under stirring, and then respectively added by 798 grams of Cr (NO 3 ) 3 9H 2 A solution composed of O and 300 ml of water, 68.6 g of H 3 BO 3 and 560 ml of water and 39.2 g (NH 4 ) 6 Mo 7 o 24 4H 2 A solution consisting of O and 50 ml of water, 0.11 molar phosphoric acid solution, and finally 9.4 g of NaNO 3 and 20 milliliters of water, then add 113.7 grams of 30% (by weight) TiCl 3 Hydrochloric acid solution, stirred and mixed, heated and evaporated to a solid content of 42% (weight), to obtain a viscous slurry.

[0040] The above slurry is sprayed into shape, the gas inlet temperature of the sprayer is 250°C, the outlet temperature is 130°...

Embodiment 2～5

[0047] Using the same catalyst preparation process and ammoxidation reaction process parameters as in Example 1, the obtained catalyst and its properties are shown in Table 1.

[0048] The influence of table 1 catalyst composition on 2,4-dichlorobenzonitrile yield

[0049]

Embodiment 6

[0051] Use the same catalyzer and catalyst amount of embodiment 1, same reaction pressure, reaction load and reaction raw material ratio, change temperature of reaction, evaluate reaction process condition in embodiment 1, its evaluation result is listed in following table 2.

[0052] The influence of table 2 temperature on reaction

[0053]

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Abstract

The invention relates to a method for the ammoxidation synthesis of 2,4-dichlorobenzonitrile to mainly solve problems of bad fluidization quality and low yield, or low yield and high production cost after using a fixed bed existing in fluidized bed reactors in present production technologies. The method which adopts 2,4-dichlorotoluene, ammonia and air as raw materials comprises a step that the raw materials contact and react with a catalyst in a fluidized bed under conditions that the raw material ratio of the 2,4-dichlorotoluene to the ammonia to the air is 1:2-10:4-40, the reaction temperature is 300-500DEG C, the reaction pressure is 0.01-0.1Mpa and the catalyst load (WWH) is 0.03-0.1h<-1> to generate the 2,4-dichlorobenzonitrile. The method well solves the problems and can be used for the industrial production of the ammoxidation synthesis of the 2,4-dichlorobenzonitrile.

Description

technical field [0001] The invention relates to a method for preparing 2,4-dichlorobenzonitrile by ammoxidation. Background technique [0002] 2,4-dichlorobenzonitrile (abbreviated as 2,4-DCN) is a fine chemical intermediate with a wide range of uses; 2,4-difluorobenzonitrile, 2,4 -Dichlorobenzoic acid, etc. are important organic intermediates, which can be widely used in industries such as medicine, pesticides, pigments, dyes, and photosensitive materials. [0003] In the previous 2,4-dichlorobenzonitrile synthesis technology, the European patent technology EP441004 is a chemical synthesis method, which is obtained by the reaction of raw materials α, α, α,-2,4-pentachlorotoluene and ammonia; Japan Patent Ping 01-96163 reports that 2,4-dichlorobenzoyl chloride is used as raw material to react to generate corresponding carboxylic acid, which is then prepared by reacting with urea. These chemical synthesis methods all have the disadvantages of expensive raw materials, diffic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/50C07C253/28B01J27/199
Inventor 顾龙勤陈亮
Owner CHINA PETROLEUM & CHEM CORP
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