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Catalyst for preparing 2-cyanopyridine by ammoxidation

A technology of ammoxidation reaction and cyanopyridine, which is applied in the direction of physical/chemical process catalyst, catalyst activation/preparation, organic chemistry, etc., to achieve the effect of convenient preparation and high selectivity

Active Publication Date: 2018-01-05
HIGH & NEW TECH RES CENT OF HENAN ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent CN 103467370 B reports the ammoxidation of vanadium-titanium catalyst to prepare picoline and its derivatives, the catalyst consists of 6-18% V 2 o 5 , 1.5-6.5% Sb 2 o 3 and 80-92% TiO 2 Composition, the yield of 2-cyanopyridine is 82.7%; Dong-Koo Lee, et al. Korean J. Chem. Eng ., 20(2), 279-283 (2003) reported a powder amorphous MoPO catalyst, which catalyzed 2-picoline to generate 2-cyanopyridine with a selectivity of 95%, and the catalytic results were satisfactory, but the literature only Limited to the case of unsupported powder MoPO as catalyst

Method used

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Effect test

Embodiment 1

[0018] A preparation method for a catalyst for preparing 2-cyanopyridine by ammoxidation, comprising the steps of:

[0019] 1) Preparation of titania support:

[0020] 200 g of metatitanic acid was taken and calcined at 500 °C for 4 h to obtain 170 g of titanium dioxide powder. Take 100 g of this titanium dioxide powder, add 25 g of PVA-1788 aqueous solution with a mass concentration of 5%, 4 g of citric acid, 1 g of glycerin and 30 g of water, stir and mix evenly, and then extrude on an extrusion machine to obtain a diameter of φ3- 6mm, 4-10mm long columnar body, air at room temperature for 1 day. Then bake at 120°C for 6 hours, and then calcined at 900°C for 6 hours to obtain a titanium dioxide carrier.

[0021] 2) MoO 3 -P 2 o 5 / TiO 2 Catalyst preparation:

[0022] Take 2.1 g ammonium tetramolybdate ((NH 4 ) 2 Mo 4 o 13· 2H 2 O), add 7 g deionized water and 4 g ammonia water (25wt%), add 2.9g phosphoric acid (85wt%), stir and mix and dissolve to obtain an impre...

Embodiment 2

[0025] A method for preparing a catalyst for ammoxidation reaction to prepare 2-cyanopyridine, comprising the steps of:

[0026] 1) Preparation of titania support:

[0027] Take 200 g of metatitanic acid and calcinate at 500 °C for 5 h to obtain 169 g of titanium dioxide powder. Take 100 g of this titanium dioxide powder, add 25 g of 5% PVA-1788 aqueous solution, 4 g of citric acid, 1 g of glycerin and 30 g of water, stir and mix well, and then extrude on the extruder to obtain a diameter of φ3-6mm 1. A columnar green body with a length of 4-10mm is left to air at room temperature for 1 day, then dried at 120°C for 6 hours, and then calcined at 850°C for 9 hours to obtain a titanium dioxide carrier.

[0028] 2) MoO 3 -P 2 o 5 / TiO 2 Catalyst preparation:

[0029] Take 3.1 g of ammonium tetramolybdate, add 14 g of deionized water and 6 g of ammonia water (25%), add 5.2 g of phosphoric acid (85%), stir and mix to dissolve to obtain an impregnation solution, then put 60 g o...

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PUM

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Abstract

The invention relates to a catalyst for preparing 2-cyanopyridine by ammoxidation. The catalyst is prepared by taking TiO2 as a carrier and loading MoO3 and P2O5 by an impregnation method. The catalyst comprises 2.8-8.3% of MoO3 and 2.8-12.2% of P2O5 by mass percentage. The invention further discloses 2-cyanopyridine prepared by using the catalyst to catalyze the ammoxidation of 2-picoline. A testproves that a conversion rate of 2-picoline can reach above 98%, and the selectivity of 2-cyanopyridine can reach above 90% by the action of the catalyst.

Description

technical field [0001] The invention belongs to the technical field of catalytic synthesis, and in particular relates to a catalyst for preparing 2-cyanopyridine by gas-phase ammoxidation reaction and a preparation method thereof. Background technique [0002] 2-cyanopyridine can be used as a herbicide intermediate. 2-cyanopyridine is mainly prepared from 2-picoline through ammoxidation reaction. The key to the preparation of 2-picoline is the ammoxidation catalyst. Although there are many studies on picoline ammoxidation catalysts, they mainly focus on the preparation of 3-cyanopyridine (nicotinonitrile) by ammoxidation of 3-picoline. Because nicotinamide can be hydrolyzed to produce bulk raw material nicotinamide (VB 3 ), it is easier for people to focus on it. [0003] Due to the difference between the substitution at the 2-position and the substitution at the 3-position of pyridine, the selectivity of the product 2-cyanopyridine is not high when the catalyst of 3-picoli...

Claims

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Application Information

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IPC IPC(8): B01J27/19B01J37/02B01J37/08C07D213/84
Inventor 王利敏陈彤程森祥
Owner HIGH & NEW TECH RES CENT OF HENAN ACAD OF SCI
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