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Method for efficiently preparing p-tert-butyl benzonitrile by utilizing liquid-phase ammonia oxidation process

A technology of tert-butylbenzonitrile and p-tert-butyltoluene, which is applied in the field of efficient preparation of p-tert-butylbenzonitrile, can solve the problems of affecting the economic benefits of industrialization and low conversion rate, so as to avoid product loss, reduce consumption, reduce The effect of preparation costs

Inactive Publication Date: 2017-12-08
ANHUI ZHIBO NEW MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Patent CN 1660499A discloses a preparation method and application of a composite oxide-supported catalyst. Cobalt, nickel and cocatalyst raw materials are loaded on alumina or silica in the form of oxides by impregnation method and high-temperature calcination method to obtain Composite oxide supported catalyst, the catalyst is used in the liquid-phase ammoxidation of p-tert-butyltoluene to prepare p-tert-butylbenzonitrile in the examples, and p-tert-butyltoluene is converted in Examples 1-3 and Comparative Example 1 The rate is respectively 58%, 54%, 50.5%, 51%, and the p-tert-butylbenzonitrile selectivity is respectively 98.56%, 91.56%, 93.56%, 95.56%, and the average transformation rate of its p-tert-butyltoluene is calculated 53% and the average selectivity of p-tert-butylbenzonitrile is 94.81%, thus it can be seen that although this catalyst can improve the selectivity of p-tert-butylbenzonitrile to more than 94%, the conversion rate of p-tert-butyltoluene is very low Low, which means that there is a large amount of unreacted p-tert-butyltoluene, which will directly greatly limit the output of p-tert-butylbenzonitrile for industrial production, thereby affecting the economic benefits of industrialization

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 2mol p-tert-butyltoluene, 10mol m-xylene and 0.08mol loaded metal catalyst into a stainless steel autoclave, heat up to 150-160° C. and keep stirring, then feed the mixed gas of air and ammonia (the mixture of air and ammonia The feeding molar ratio is 12:1), keep the pressure of the reaction system at 0.5MPa, take samples regularly for detection, stop feeding the mixed gas after the reaction is completed, and open the pressure relief valve when the temperature of the kettle is naturally cooled to below 50°C. After the pressure relief is completed Open the reaction kettle, and take out the reaction solution, then add water to the reaction solution, so that the volume ratio of the reaction solution to water reaches 3:1, after stirring evenly, the water phase is separated to recover the catalyst, and the obtained organic phase is concentrated under reduced pressure to recover m-xylene , The concentrated residue is p-tert-butylbenzonitrile. After testing, the conversio...

Embodiment 2

[0026] Add 2mol p-tert-butyltoluene, 15mol m-xylene and 0.1mol loaded metal catalyst into a stainless steel autoclave, heat up to 150-160° C. and keep stirring, then feed the mixed gas of air and ammonia (the mixture of air and ammonia The feeding molar ratio is 12:1), keep the pressure of the reaction system at 0.5MPa, take samples regularly for detection, stop feeding the mixed gas after the reaction is completed, and open the pressure relief valve when the temperature of the kettle is naturally cooled to below 50°C. After the pressure relief is completed Open the reaction kettle, and take out the reaction solution, then add water to the reaction solution, so that the volume ratio of the reaction solution to water reaches 3:0.5, after stirring evenly, separate the water phase to recover the catalyst, and the obtained organic phase is concentrated under reduced pressure to recover m-xylene , The concentrated residue is p-tert-butylbenzonitrile. After testing, the conversion r...

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Abstract

The invention discloses a method for efficiently preparing p-tert-butyl benzonitrile by utilizing a liquid-phase ammonia oxidation process and relates to the technical field of chemical synthesis. The method comprises the following steps: by taking p-tert-butyl methylbenzene as a reaction raw material, m-xylene as a reaction solvent and a stainless steel autoclave as a reaction container, introducing a mixture of air and ammonia gas into the reaction container under the existence of a loading type metal catalyst; and preparing the p-tert-butyl benzonitrile by utilizing the liquid-phase ammonia oxidation process. According to the preparation steps in the invention, the average conversion rate of the raw material to p-tert-butyl methylbenzene is 80% or above, the average selectivity of the product for p-tert-butyl benzonitrile is 98% or above, and meanwhile, the reaction time is obviously shortened, the adopted catalyst can be easily recycled and the dosage of noble metal is less.

Description

Technical field: [0001] The invention relates to the technical field of chemical synthesis, in particular to a method for efficiently preparing p-tert-butylbenzonitrile by using a liquid-phase ammoxidation method. Background technique: [0002] Aromatic nitrile is an important intermediate for the synthesis of dyes, pesticides, medicines and various materials, and has a wide range of uses. At present, the simplest and most economical method for synthesizing aromatic nitriles is to use toluene and its derivatives as raw materials, and synthesize them in one step by gas-phase ammoxidation under the action of a catalyst, but the reaction temperature of gas-phase ammoxidation is generally 400-500°C , while most of the toluene derivatives are structurally unstable at this temperature, and the selectivity of the product nitrile compounds is low, such as tert-butyl substituted toluene and hydroxyl substituted toluene. [0003] The liquid-phase ammoxidation method is usually carrie...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/28C07C255/50B01J31/06B01J23/755
CPCB01J23/755B01J31/06C07C253/28C07C255/50Y02P20/584
Inventor 汪六一宋从发
Owner ANHUI ZHIBO NEW MATERIAL TECH CO LTD