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A kind of catalyst for preparing 3-cyanopyridine and preparation method thereof

A cyanopyridine and catalyst technology, which is applied to the catalyst for preparing 3-cyanopyridine and the field of preparation thereof, can solve the problems of poor selectivity, high reaction temperature, low yield and the like, and achieves mild process conditions, simple preparation process and high yield. high rate effect

Active Publication Date: 2021-01-15
BROTHER ENTERPRISES HLDG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the problems of high reaction temperature, poor selectivity and low yield of existing 3-cyanopyridine catalysts, the invention provides a catalyst for preparing 3-cyanopyridine

Method used

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  • A kind of catalyst for preparing 3-cyanopyridine and preparation method thereof
  • A kind of catalyst for preparing 3-cyanopyridine and preparation method thereof
  • A kind of catalyst for preparing 3-cyanopyridine and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0045]Catalyst preparation: heat and dry the raw material titanium dioxide, then place it in a rotary kiln for calcination at 200-300°C for 2 hours, and then calcine at 500-800°C for 3-4 hours, then lower the temperature. Acidic solution choose V (acetic acid / oxalic acid) = 50:50 mixed acid solution. Weigh 100g of vanadium pentoxide, 10g of niobium oxalate, 5g of cesium nitrate, 82g of phosphorus pentoxide, 90g of potassium chloride, 55g of antimony trioxide, 100g of DMF, 1.1g of molybdenum trioxide, and add 300g of mixed acid aqueous solution at 40°C Stir at low temperature for 2 hours to fully dissolve. After mixing evenly, add 700g of treated titanium dioxide and continue to heat and stir. After mixing for 50 minutes, grind for 10 hours, and then stand for 40 hours. The ground active TiO 2 The particles are sprayed onto 3500g of silicon carbide carrier, the spraying temperature is 280-300°C, and cooled after spraying to ensure that the weight gain of the prepared catalys...

Embodiment 2

[0048] Catalyst preparation: heat and dry the raw material titanium dioxide, then place it in a rotary kiln for calcination at 250-300°C for 5 hours, then calcine at 500-800°C for 10 hours, and lower the temperature. The acidic solution is a mixed acid solution of V (formic acid / acetic acid) = 50:50. Weigh 95g of vanadium pentoxide, 10g of niobium carbonate, 7.7g of cesium oxalate, 167g of potassium dihydrogen phosphate, 55g of antimony trioxide, 10.8g of silver nitrate, 5.2g of nickel sulfate, and 100g of acetamide into 350g of mixed acid aqueous solution at 60 Stir at ℃ for 4 hours to fully dissolve. After mixing evenly, add 680g of treated titanium dioxide and continue to heat and stir. After mixing for 2 hours, grind for 14 hours and stand for 24 hours. The ground active TiO 2 The particles are sprayed onto 4000g of silicon carbide carrier, the spraying temperature is 300-350°C, and cooled after spraying to ensure that the weight gain of the prepared catalyst is about 20%...

Embodiment 3

[0051] Catalyst preparation: heat and dry the raw material titanium dioxide, then place it in a rotary kiln for calcination at 280-300°C for 4 hours, then calcine at 500-800°C for 6 hours, and lower the temperature. Acid solution choose oxalic acid solution. Weigh 104g of vanadium pentoxide, 12.6g of ferrous sulfate, 6.4g of rubidium sulfate, 67g of potassium sulfate, 46.7g of antimony trioxide, 10.8g of silver nitrate, 5.2g of nickel sulfate, and 120g of propionamide into 300g of oxalic acid aqueous solution at 60 Stir at ~70°C for 2-4 hours to fully dissolve, mix evenly, add 770g of treated titanium dioxide and continue to heat and stir, mix for 3-5 hours, grind for 14-16 hours, and stand for 24-36 hours. The ground active TiO 2 The particles are sprayed onto 4000g of silicon carbide carrier, the spraying temperature is 300-350°C, and cooled after spraying to ensure that the weight gain of the prepared catalyst is about 25%.

[0052] Catalyst application example: 3-picolin...

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Abstract

The invention relates to a catalyst, in particular to a catalyst for preparing 3-cyanopyridine and a preparation method thereof. The catalyst for preparing 3-cyanopyridine comprises a carrier, a mainactive component and an auxiliary active component, wherein an active material is sprayed on the carrier to obtain the catalyst; the total weight of the main active component and the auxiliary activecomponent accounts for 15-40% of the total weight of the catalyst; the carrier is silicon carbide, an SMA maleic anhydride catalyst carrier, SiO2, or Al2O3; the main active component is a combinationof modified titanium dioxide and vanadium pentoxide; and a modification method of the modified titanium dioxide comprises: drying titanium dioxide, calcining the dried titanium dioxide at 100-300 DEGC for 1-10 hours, calcining the titanium dioxide at 300-800 DEG C for 1-20 hours, and carrying out cooling to obtain the modified titanium dioxide. After being modified at a high temperature, titaniumdioxide can effectively reduce organic residues, change crystal forms, and effectively improve the activity and the service life of the catalyst.

Description

technical field [0001] The invention relates to a catalyst, in particular to a catalyst for preparing 3-cyanopyridine and a preparation method thereof, belonging to the field of catalysts. Background technique [0002] 3-cyanopyridine, also known as nicotinonitrile, as an important pharmaceutical and chemical intermediate, is the main raw material for the preparation of vitamin B3 nicotinic acid and nicotinamide, and vitamin B3 is currently widely used in industries such as medicine, food and feed additives. Huge market potential. At present, the production of 3-cyanopyridine mainly uses 3-picoline as raw material through ammoxidation synthesis. The ammoxidation reaction process is complicated, which is characterized by high reaction conversion rate, many side reactions, and low reaction selectivity. The difficulty lies in the catalyst technology. . [0003] Studies have shown that although the conversion rate of the existing 3-cyanopyridine catalysts can be close to 100%,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/228B01J27/199C07D213/85
CPCB01J27/199B01J27/228C07D213/85
Inventor 潘炎烽高海燕周中平钱志达
Owner BROTHER ENTERPRISES HLDG CO LTD
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