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Method for synthesizing 2,3-dichlorobenzonitrile by catalytic ammonia oxidation method and dedicated catalyst

A technique for the synthesis of dichlorobenzonitrile, which is applied in metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, preparation of hydrocarbon ammoxidation, etc., and can solve the problems of low selectivity and active loading, and catalysts Easy deactivation, short service life and other problems, to achieve the effect of reducing solid waste pollution, reducing raw material consumption, and long service life

Inactive Publication Date: 2013-02-27
应城市澳赛斯化工有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0020] If the existing ammoxidation catalyst system is used for the preparation of 2,3-dichlorobenzonitrile, the catalyst is easily deactivated, the service life is short, the selectivity and active load are not high, and the conversion rate of the reaction is not high
Like this, limit the development of the industrialized production of 2,3-dichlorobenzonitrile prepared by ammoxidation

Method used

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  • Method for synthesizing 2,3-dichlorobenzonitrile by catalytic ammonia oxidation method and dedicated catalyst
  • Method for synthesizing 2,3-dichlorobenzonitrile by catalytic ammonia oxidation method and dedicated catalyst
  • Method for synthesizing 2,3-dichlorobenzonitrile by catalytic ammonia oxidation method and dedicated catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0056] 125kgV 2 O 5 (Molecular weight: 181.88) Pour into 250kg deionized water at 70℃, heat the deionized water to 70℃ and mix evenly, add 700kg of oxalic acid to 125kg V 2 O 5 In the solution, control the reaction temperature to 80℃, wait until V 2 O 5 Dissolve completely to dark blue, add 200kg of potassium antimony tartrate (molecular weight 667.86) with a content of more than 99%, stir to dissolve and keep warm to 85℃, add 30kg of boric acid with a content of more than 99% to the reactor to dissolve in the solution, and then add 80kg of titanic acid to dissolve Pour into the reaction kettle in 300kg deionized water, keep it at 85°C, fully stir and dissolve, add deionized water to the mother liquor volume of 1300 liters, and keep it for 1.5 hours.

[0057] Cool the 40~140 mesh coarse-pored microsphere silica gel roasted to 800℃ to 50℃, then pour it into the mother liquor and stir evenly until the silica gel is completely submerged, keep it at 80℃ for 24 hours, take it out and dr...

Embodiment 2

[0066] 125kgV 2 O 5 (Molecular weight: 181.88) Pour into 250kg deionized water at 70℃, heat the deionized water to 70℃ and mix evenly, add 700kg of oxalic acid to 125kg V 2 O 5 In the solution, control the reaction temperature to 80℃ and wait until V 2 O 5 Dissolve completely to dark blue, add 350kg of potassium antimony tartrate (molecular weight 667.86) with a content of more than 99%, stir to dissolve and keep warm to 85℃, add 55kg of boric acid with a content of more than 99% to the reactor to dissolve in the solution, then add 100kg of titanic acid to dissolve Pour into the reaction kettle in 300kg deionized water, keep it at 85°C, fully stir and dissolve, add deionized water to the mother liquor volume of 1300 liters, and keep it for 1.5 hours.

[0067] Cool the 40~140 mesh coarse-pored microsphere silica gel roasted to 800℃ to 50℃, then pour it into the mother liquor and stir evenly until the silica gel is completely submerged, keep it at 80℃ for 24 hours, take it out and dr...

Embodiment 3

[0076] 125kgV 2 O 5 (Molecular weight: 181.88) Pour into 250kg deionized water at 70℃, heat the deionized water to 70℃ and mix evenly, add 700kg of oxalic acid to 125kg V 2 O 5 In the solution, control the reaction temperature to 80℃, wait until V 2 O 5 Dissolve completely to dark blue, add more than 99% potassium antimony tartrate (molecular weight 667.86) 550kg, fully stir and dissolve and keep to 85℃, add 80kg of boric acid with a content of more than 99% to the reaction kettle to dissolve in the solution, and then add 120kg of titanic acid to dissolve Pour into the reaction kettle in 300kg deionized water, keep it at 85°C, fully stir and dissolve, add deionized water to the mother liquor volume of 1300 liters, and keep it for 1.5 hours.

[0077] Cool the 40~140 mesh coarse-pored microsphere silica gel roasted to 800℃ to 50℃, then pour it into the mother liquor and stir evenly until the silica gel is completely submerged, keep it at 80℃ for 24 hours, take it out and dry it into ...

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Abstract

The invention provides a catalyst for synthesizing 2,3-dichlorobenzonitrile by catalytic ammonia oxidation method. The catalyst disclosed herein adopts microspheric silica gel as a carrier, and is characterized in that: the active component of the catalyst is TiaVbSbcBdOx, wherein a represents 1, b represents 0.5-1, c represents 0.3-1.5, d represents 0.2-1, and x represents 0.3-0.35, and the active component accounts for 70wt% of the weight of the whole catalyst. According to the invention, the catalyst is used in the industrial synthetic method of 2,3-dichlorobenzonitrile, and the devices of the industrial synthetic method is improved; the conversion rate and product yield are raised, and simultaneously the product quality is raised, and the production cost is reduced. By using ammonia oxidation of the novel catalyst to conduct one-step synthesis of 2,3-dichlorobenzonitrile, the conversion rate can reach 100%, the selectivity is higher than 96%, the yield is higher than 95%, the product quality is raised, and the production cost is reduced.

Description

technical field [0001] The invention relates to a catalytic synthesis of an organic intermediate, in particular to a method for synthesizing 2,3-dichlorobenzonitrile by catalytic ammoxidation and a special catalyst. Background technique [0002] 2,3-Dichlorobenzonitrile is an important organic intermediate and belongs to the field of chemical pesticide intermediates. It is widely used as a rare source intermediate and is widely used in pesticides, medicines, pigments and other fields. [0003] Since the molecule of 2,3-dichlorobenzonitrile contains carbon-nitrogen triple bonds, it is much more active than amido compounds, and can undergo many reactions such as hydrolysis, alcoholysis, ammonolysis and chlorine reduction. For example, in the aspect of pesticides, it is used to synthesize new pesticides that are expected to remove pyrethroids with high efficiency, low toxicity, no residue and easy degradation. At the same time, the herbicide XDE can be synthesized, which is a p...

Claims

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Application Information

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IPC IPC(8): B01J23/22C07C255/50C07C253/28
Inventor 程冬秀黄雯黄兵红饶彬鹏
Owner 应城市澳赛斯化工有限责任公司