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Catalyst for synthesizing 2-cyano pyrazine and preparation method of catalyst

A cyanopyrazine and a catalyst technology are applied to the catalyst for synthesizing 2-cyanopyrazine and the field of preparation thereof, and can solve the problems of difficult application, poor thermal stability, phase structure change and the like, and achieve improved selectivity and yield, The effect of improving catalyst activity and good use effect

Inactive Publication Date: 2019-03-19
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Some researchers try to load it on the carrier (such as SiO 2 ) to improve its thermal stability, however, due to the poor solubility of ammonium phosphomolybdate and the dispersive loading process is not easy to operate and control, making this method difficult to apply
[0005] Based on the above studies, it can be seen that although heteropolyacid compounds have good activity and selectivity for low-temperature ammoxidation, their poor thermal stability has become a problem in application. At high temperatures for a long time, the framework structure of heteropolyacids decomposes, and the phase structure Changes that affect the use of the catalyst

Method used

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  • Catalyst for synthesizing 2-cyano pyrazine and preparation method of catalyst
  • Catalyst for synthesizing 2-cyano pyrazine and preparation method of catalyst
  • Catalyst for synthesizing 2-cyano pyrazine and preparation method of catalyst

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 20g V 2 o 5React with 300mL isobutanol at 109°C for 3h, then add 95% pyrophosphoric acid to the system to make P:V=1.1, and react at 109°C for 12h after the addition, after the reaction is completed, naturally cool to room temperature, and reduce the reactant Pressure filtration with a vacuum of 0.05 MPa. The filter cake is then washed with isobutanol to remove soluble impurities from the solid surface. Substance A was obtained after washing and drying at 110°C for 12 hours.

[0034] Substance A was calcined in an oxygen atmosphere, the temperature was raised from room temperature to 650 °C at a rate of 5 °C / min, calcined for 4 hours, and cooled to room temperature to obtain Substance B.

[0035] The ammonium molybdate salt solution with a mass fraction of 10% was prepared by using ammonium molybdate, and the pH of the solution was controlled to be 1 by using nitric acid. Add 10g of substance B into 25g of the above solution to fully impregnate, impregnate for 3 hou...

Embodiment 2

[0038] 20g V 2 o 5 React with 160mL of isobutanol at 80°C for 5h, then add 95% pyrophosphoric acid to the system to make P:V=0.8, and react at 80°C for 5h after adding, after the reaction is completed, naturally cool to room temperature, and reduce the reactant Pressure filtration, the vacuum degree is 0.01MPa. The filter cake is then washed with isobutanol to remove soluble impurities from the solid surface. Substance A was obtained after washing and drying at 100°C for 12 hours.

[0039] Substance A was calcined in an oxygen atmosphere, the temperature was raised from room temperature to 500 °C at a rate of 5 °C / min, calcined for 6 hours, and cooled to room temperature to obtain Substance B.

[0040] The ammonium molybdate salt solution with a mass fraction of 5% was prepared by using ammonium molybdate, and the pH of the solution was controlled to be 3 by using nitric acid. Add 10g of substance B into 10g of the above solution to fully impregnate, impregnate for 3 hours...

Embodiment 3

[0042] 20g V 2 o 5 React with 500mL of isobutanol at 200°C for 3h, then add 95% pyrophosphoric acid to the system to make P:V=1.5, and react at 200°C for 10h after adding, after the reaction is completed, naturally cool to room temperature, and reduce the reactant Pressure filtration, the vacuum degree is 0.09MPa. The filter cake is then washed with isobutanol to remove soluble impurities from the solid surface. Substance A was obtained after washing and drying at 120°C for 10 hours.

[0043] Substance A was calcined in an oxygen atmosphere, the temperature was raised from room temperature to 700 °C at a rate of 5 °C / min, calcined for 3 hours, and cooled to room temperature to obtain Substance B.

[0044] The ammonium molybdate salt solution with a mass fraction of 15% was prepared by using ammonium molybdate, and the pH of the solution was controlled to be 2 by using nitric acid. Add 10g of substance B to 40g of the above solution to fully impregnate, impregnate for 3 hou...

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Abstract

The invention relates to a catalyst for synthesizing 2-cyano pyrazine and a preparation method of the catalyst. The catalyst comprises, in weight percent, 3%-30% of MoO3, 40%-55% of V2O5, 25%-44% of P2O5 and 0.75%-2.5% of NO2. The invention further provides a preparation method of the catalyst. The catalyst is used for oxidizing 2-methylpyrazine gas-phase ammonia to form the 2-cyano pyrazine and has the advantages of good reaction activity and heat stability, high product selectivity and yield, long service life and the like.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a catalyst for synthesizing 2-cyanopyrazine and a preparation method thereof. Background technique [0002] Cyanopyrazine and its derivatives are relatively complex nitrogen-containing heterocyclic aromatic nitrile compounds, and are important organic chemical raw materials and intermediates. 2-cyanopyrazine is the basic raw material for the synthesis of pyrazinamide anti-tuberculosis medicines. There are many methods for the synthesis of 2-cyanopyrazine, among which the ammoxidation of 2-methylpyrazine to synthesize 2-cyanopyrazine is the preferred synthetic method at present. The key of this process is to develop high conversion rate and high selectivity catalyst. Forni et al. reported SbVMnO and VMoPO ammoxidation catalysts, but the yields were not high, most of them were around 80%, the highest was 85%, and the reaction temperature was above 400°C. [0003] V ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/19B01J37/28B01J37/08B01J37/02C07D241/24
CPCC07D241/24B01J23/002B01J27/19B01J37/0201B01J37/08B01J37/28B01J35/30
Inventor 刘新宇王海波宋丽芝乔凯王领民
Owner CHINA PETROLEUM & CHEM CORP