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A kind of preparation method for synthesizing aromatic nitrile catalyst and the synthetic method of aromatic nitrile

A synthesis method and catalyst technology, which are applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of increasing synthesis cost, large environmental impact, and difficulty in obtaining metal complex catalysts, and achieve easy and efficient products. Excellent catalytic performance

Active Publication Date: 2022-06-17
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that it needs to use toxic cyanide reagents, such as KCN, Zn(CN) 2 , NaCN and CuCN, etc., the yield is generally 66.0-90%, but a large amount of reaction waste liquid containing metal is produced after the reaction, which has a great impact on the environment
The disadvantage of this method is that the metal complex catalyst used is difficult to obtain, and a large amount of additives are added to the system, which makes it difficult to purify and separate the target product and increase the cost of synthesis

Method used

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  • A kind of preparation method for synthesizing aromatic nitrile catalyst and the synthetic method of aromatic nitrile
  • A kind of preparation method for synthesizing aromatic nitrile catalyst and the synthetic method of aromatic nitrile
  • A kind of preparation method for synthesizing aromatic nitrile catalyst and the synthetic method of aromatic nitrile

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Experimental program
Comparison scheme
Effect test

preparation example Construction

[0029] The preparation method of Pd / ZSM-5 is:

[0030] Weigh 2.0g of ZSM-5 carrier into a 150mL beaker, add 80mL of distilled water, weigh 0.1026g of Pd(NO) 3 ) 2 ·2H 2 O was added to the beaker and stirred at room temperature for 72h. After filtration and washing, the obtained catalyst sample was dried in an oven at 50° C. for 72 h to obtain a Pd / ZSM-5 catalyst.

specific Embodiment 1

[0031] Benzamide (2 mmol, 0.24 g), Pd / ZSM-5 (0.1 g) and 20 mL of acetonitrile were sequentially added to a 50 mL reaction kettle, the reaction temperature was controlled at 100 °C, and the reaction was vigorously stirred for 4 h. After the reaction was completed, it was cooled to room temperature, the reaction system was centrifuged, and the reaction solution was subjected to chromatographic analysis. All the reactants were converted, and the selectivity of benzonitrile was 100%; After several experiments, yields of 92-97% were obtained).

[0032] The equation involved in the reaction is as follows:

[0033]

specific Embodiment 2

[0034] Benzamide (2 mmol, 0.24 g), Pd / ZSM-5 (0.1 g) and 20 mL of acetonitrile were sequentially added to a 50 mL reaction kettle, the reaction temperature was controlled at 80 °C, and the reaction was vigorously stirred for 6 h. After the reaction was completed, it was cooled to room temperature, the reaction system was centrifuged, and the reaction solution was analyzed by chromatography. All the reactants were converted, and the selectivity of benzonitrile was 100%. Benzonitrile can be obtained by distillation under reduced pressure, and benzonitrile ~ 0.19 g (yield 92-97%) can be obtained by distillation under reduced pressure.

[0035] The equation involved in the reaction is as follows:

[0036]

[0037] The above-mentioned catalysts, under the same reaction conditions, partially expand R, all obtain better catalytic effects: higher conversion rate and product selectivity, and the target product and catalytic performance are:

[0038]

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Abstract

The invention belongs to the technical field of aromatic nitrile synthesis, and discloses a method for preparing a catalyst for synthesizing aromatic nitriles and a method for synthesizing aromatic nitriles. The present invention adopts the method of ion exchange to obtain Pd / ZSM‑5 as a catalyst, and then uses the catalyst to synthesize aromatic nitriles, specifically: aryl formamide is dissolved in acetonitrile solvent, and the reaction is catalyzed at a reaction temperature of 60‑120 °C After 3-5 hours, aromatic nitriles are obtained. Compared with the existing technology, this method does not need to introduce acid-base additives, ligands, and metal catalysts containing ligands. Using this catalyst, with acetonitrile solvent, the conversion rate of aryl formamide and the selectivity of aromatic nitrile target products are high , high yield, simple operation, easy purification, less impact on the environment, has potential industrial value, and is worthy of popularization and application.

Description

technical field [0001] The invention belongs to the field of fine chemicals, and relates to a preparation method for synthesizing an aromatic nitrile catalyst and a method for synthesizing an aromatic nitrile. Background technique [0002] Aromatic nitrile is an effective organic intermediate, which is widely used in the synthesis of pesticides, pharmaceuticals, and dye chemicals. The structural motifs of aromatic nitrile molecules have also been found in biological activities and natural products. extensive attention. At present, there are two common methods for synthesizing aromatic nitriles: the first method is to use aryl aldehydes as raw materials, and synthesize them through the cyanation reaction of p-aryl aldehydes. The disadvantage of this method is that it requires the use of toxic cyanating reagents, such as KCN, Zn(CN) 2 , NaCN and CuCN, etc., the yield is generally 66.0-90%, but a large amount of metal-containing reaction waste liquid produced after the reacti...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/44B01J29/12B01J29/74C07C253/20C07C255/50C07C255/53C07C255/54C07C255/33C07C255/34
CPCB01J29/44B01J29/126B01J29/123B01J29/7415B01J29/7484C07C253/20B01J2229/18C07C255/50C07C255/53C07C255/54C07C255/33C07C255/34
Inventor 张磊唐天地陈中淼傅雯倩才国仁陈群
Owner CHANGZHOU UNIV
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