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Catalyst for producing 3-cyano pyridine as well as preparation method and use thereof

A technology of cyanopyridine and catalyst, which is applied in the field of catalyst for producing 3-cyanopyridine and its preparation and application, can solve the problems of high energy consumption, high use temperature, and low energy consumption, and achieve high yield, The effect of low reaction temperature

Inactive Publication Date: 2009-05-20
ZHEJIANG NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a low temperature and low energy consumption catalyst for the existing 3-picoline ammoxidation to produce 3-cyanopyridine catalysts, which have the disadvantages of high temperature and high energy consumption. Catalyst for producing 3-cyanopyridine by ammoxidation of 3-picoline and its preparation method and application

Method used

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  • Catalyst for producing 3-cyano pyridine as well as preparation method and use thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] 0.1%Cr 2 o 3 -5%V 2 o 5 / TiO 2 Catalyst preparation

[0014] Weigh NH 4 VO 3 1.084g, dissolved in 60.0g double-distilled water and 1.668g oxalic acid mixture, heated and stirred to 50°C for NH 4 VO 3 Dissolve completely, then add 0.0894g Cr 2 o 3 , forming an orange liquid, and the solution was gradually cooled to 20 ° C, at this temperature, slowly added 16 g of anatase TiO with a particle size of 100 mesh 2 Add the solid powder in the above solution, continue to stir to form a suspension, and adjust the pH value of the above slurry to 6 with an appropriate amount of oxalic acid, continue to stir for 12 hours, and then evaporate the solvent to dryness at 90°C for the resulting suspension. Dry at ℃ for 12h, place in a muffle furnace and bake at 400℃ for 5h to obtain a sample with 0.1% Cr 2 o 3 -5%V 2 o 5 / TiO 2 catalyst.

[0015] Weigh 0.5 g of the above-mentioned solid catalyst and apply it to the gas-phase ammoxidation of 3-picoline to produce 3-cyanop...

Embodiment 2

[0017] 0.25%K 2 O-7.5%V 2 o 5 / TiO 2 Catalyst preparation and catalytic performance

[0018] Weigh NH 4 VO 3 1.668g, dissolved in 60.0g double-distilled water and 1.668g oxalic acid mixture, heated and stirred to 70°C for NH 4 VO 3 Dissolve completely, then add 0.0927g KNO 3 , forming an orange liquid, and the solution was gradually cooled to 50 ° C, at this temperature, slowly added 16 g of anatase TiO with a particle size of 140 mesh 2 Add the solid powder in the above solution, continue to stir to form a suspension, and adjust the pH value of the above slurry to 5 with an appropriate amount of oxalic acid, continue to stir for 12 hours, and then evaporate the solvent to dryness at 90°C for the resulting suspension, at 110 Dry at ℃ for 12h, place in a muffle furnace and bake at 500℃ for 7h to obtain a sample of 0.25% K 2 O-7.5%V 2 o 5 / TiO 2 catalyst.

[0019] Weighed 1 g of the above solid catalyst and applied it to the gas-phase ammoxidation of 3-picoline to p...

Embodiment 3

[0021] 0.5% MoO 3 -10%V 2 o 5 / TiO 2 Catalyst preparation and catalytic performance

[0022] Weigh NH 4 VO 3 2.298g, dissolved in 60.0g double-distilled water and 1.668g oxalic acid mixture, heated and stirred to 90°C for NH 4 VO 3 Dissolve completely, then add 0.0894gMoO3 , forming an orange liquid, and the solution was gradually cooled to 50 ° C, at this temperature, slowly added 16 g of anatase TiO with a particle size of 150 mesh 2 Add the solid powder in the above solution, continue to stir to form a suspension, and adjust the pH value of the above slurry to 3 with an appropriate amount of oxalic acid, continue to stir for 12 hours, and then evaporate the solvent to dryness at 90°C for the resulting suspension. Dry at ℃ for 12h, place in a muffle furnace and bake at 600℃ for 10h to obtain a sample of 0.5% MoO 3 -10%V 2 o 5 / TiO 2 catalyst.

[0023] Weighed 2 g of the above solid catalyst and applied it to the gas-phase ammoxidation of 3-picoline to produce 3-c...

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Abstract

The invention relates to a catalyst for producing 3-cyanopyridine and a preparation method and application thereof. Aiming at that the prior catalyst for producing the 3-cyanopyridine by ammoxidizing 3-methylpyridine has the disadvantages of higher service temperature and large energy consumption, the invention provides a catalyst which has low service temperature and small energy consumption and is used for producing the 3-cyanopyridine by ammoxidizing the 3-methylpyridine, and a preparation method and application thereof. A carrier of the catalyst adopts anatase TiO2, an active constituent adopts V2O5, and an auxiliary agent adopts one or more than one of transition metal oxide or alkali metal oxide; the method for preparing the catalyst comprises the following steps: the carrier, the active constituent and a predecessor of the auxiliary agent are weighed according to the mixture ratio, and are placed into an oxalic acid solution to be mixed evenly, the pH value of a mixed liquid is controlled, the mixed liquid is evaporated to obtain solid powder, and the solid powder is baked to obtain the catalyst. The catalyst is used for producing the 3-cyanopyridine by ammoxidizing the 3-pyridylamine in a gas phase.

Description

technical field [0001] The invention relates to a catalyst for producing 3-cyanopyridine, its preparation method and application. In particular, a catalyst for producing 3-cyanopyridine by ammoxidation of 3-picoline and its preparation method and application. Background technique [0002] In the petrochemical industry, the partial oxidation and ammoxidation of methyl aromatic compounds to synthesize aldehydes and nitriles is directly related to the development and production of mid- and downstream products, such as medicine, pesticides, and dyes. As vitamin B series products, two substances, niacinamide and niacin, play an important role in the metabolism of humans and animals, and are important food additives and feed additives. Among them, nicotinic acid can be converted into 3-cyanopyridine by gas-phase ammoxidation of 3-picoline, and then obtained by hydrolysis. Among them, the 3-picoline ammoxidation process has the technical problem of low yield of the target product...

Claims

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Application Information

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IPC IPC(8): B01J23/26B01J23/22B01J23/16B01J21/06C07D213/85
Inventor 钟依均张富民陈菲方文程朱伟东
Owner ZHEJIANG NORMAL UNIVERSITY
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