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3-cyanopyridine production method

A production method and cyanopyridine technology are applied in the production field of tricyanopyridine to achieve the effects of simple process, low cost and wide application

Inactive Publication Date: 2016-07-06
JIANGSU WEUNITE FINE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

According to existing reports, the synthetic method of international and domestic tricyanopyridines has the following routes: 1. nicotinamide method, nicotinamide method refers to nicotinamide and catalyst P2O5 react in molten state to prepare 3-cyanopyridine, The reaction yield is 83% to 84%. Although the yield of 3-cyanopyridine produced by this method is relatively high, we can see from the source of raw materials and the reaction process that this method is only suitable for laboratory use; 2.2- Methylglutaronitrile oxidation method, 2-methylglutaronitrile is directly oxidized to produce 3-cyanopyridine. The raw materials of this process route are relatively easy to obtain, and the by-products of adiponitrile produced from acrylonitrile are rationally utilized. At the same time, the reaction The device is a fixed bed reactor, which can be produced continuously and has good industrialization prospects, but there are few reports at present; 3. Ammoxidation method, ammoxidation refers to the reaction of olefins, aromatics, alkanes and their derivatives with air (oxygen), ammonia A type of reaction in which gas is mixed and reacted on a catalyst to obtain cyanide compounds

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] The 3-picoline of formula quantity is sent into vaporizer to vaporize, and after 3-picoline is vaporized, the oxygen of formula quantity is taken out of vaporizer and enters fluidized bed after mixing with the ammonia gas of formula quantity in the mixer, and flow The temperature in the chemical bed is adjusted to 320°C, the pressure is 0.05Mpa, and the recipe amount of self-made catalyst is added to make it react. The ratio of the four raw materials is 3-picoline, ammonia, oxygen, self-made catalyst==1:4 : 12: 1.5, the time is 12 minutes after the reaction ends, the gas after the reaction is cooled and sent to the receiver, and the product tricyanopyridine is obtained after condensation, the yield of the product is 60%-70%, and the purity is 90% Send the condensed and solidified tricyanopyridine into a dryer, dry at 60°C for 2.0 hours, then send the dried product into a pulverizer, and pulverize it into powder to obtain the finished product.

Embodiment 2

[0019] The 3-picoline of formula quantity is sent into vaporizer to vaporize, and after 3-picoline is vaporized, the oxygen of formula quantity is taken out of vaporizer and enters fluidized bed after mixing with the ammonia gas of formula quantity in the mixer, and flow The temperature in the chemical bed is adjusted to 335°C, the pressure is 0.075Mpa, and the formulated amount of self-made catalyst is added to make it react. The ratio of the four raw materials is 3-picoline, ammonia, oxygen, self-made catalyst==1:9 : 26: 2.0, the time is 11 minutes after the reaction ends, the gas after the reaction is cooled and sent to the receiver, and the product tricyanopyridine is obtained after condensation. The yield of the product is 60%-70%, and the purity is 90%. Send the condensed and solidified tricyanopyridine into a dryer, dry at 65°C for 1.75 hours, then send the dried product into a pulverizer, and pulverize it into powder to obtain the finished product.

Embodiment 3

[0021] The 3-picoline of formula quantity is sent into vaporizer to vaporize, and after 3-picoline is vaporized, the oxygen of formula quantity is taken out of vaporizer and enters fluidized bed after mixing with the ammonia gas of formula quantity in the mixer, and flow The temperature in the chemical bed is adjusted to 350°C, the pressure is 0.05Mpa-0.10Mpa, and the recipe amount of self-made catalyst is added to make it react. The ratio of the four raw materials is 3-picoline, ammonia, oxygen, self-made catalyst== 1:14:40:2.5, the reaction time is 12 minutes and the reaction ends. After the reaction gas is cooled, it is sent to the receiver, and the product tricyanopyridine is obtained after condensation. The yield of the product is 60%-70%, and the purity is 90%; send the condensed and solidified tricyanopyridine into a dryer, dry at 70°C for 2.0 hours, then send the dried product into a pulverizer, and pulverize it into powder to obtain the finished product.

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PUM

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Abstract

The present invention discloses a 3-cyanopyridine production method, which belongs to the technical field of fine chemical production, raw material molar ratio is as follows: 3-methylpyridine:ammonia:oxygen:homemade catalyst is 1: 4-14: 12-40: 1.5-2.5; and key points of the production method are as follows: 1, selection of the raw material ratio; 2, selection of appropriate temperature, to be more specific, the temperature is as low as possible under possible conditions;3, selection of reaction time; and 4, selection of a catalyst, to be more specific, the catalyst is selected for more full reaction to obtain a highest yield. The 3-cyanopyridine production method has the advantages of simple production process, low production cost and no pollution, the product yield can reach 70%, the content can reach 90%; the main use of the product is as follows: 1. 3-cyanopyridine is used as a dye intermediate; 2. the 3-cyanopyridine is used as a pesticide pymetrozine intermediate, rodenticide pyridyl phenylcarbamates and mieshujing intermediate; 3. and the 3-cyanopyridine is used as a pharmaceutical intermediate, pigment intermediate, resin intermediate, and the like, and also used as an important chemical intermediate.

Description

Technical field: [0001] The invention belongs to the field of pesticide production, in particular to a production method of tricyanopyridine. Background technique: [0002] Tricyanopyridine, Chinese alias 3-pyridinecarbonitrile, niconitrile, etc., molecular formula C6H4N2, molecular weight 104.11, appearance: white crystal, capable of sublimation, soluble in ethanol, ether, chloroform, benzene and petroleum ether, slightly soluble in water . According to existing reports, the synthetic method of international and domestic tricyanopyridines has the following routes: 1. nicotinamide method, nicotinamide method refers to nicotinamide and catalyst P2O5 react in molten state to prepare 3-cyanopyridine, The reaction yield is 83% to 84%. Although the yield of 3-cyanopyridine produced by this method is relatively high, we can see from the source of raw materials and the reaction process that this method is only suitable for laboratory use; 2.2- Methylglutaronitrile oxidation metho...

Claims

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Application Information

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IPC IPC(8): C07D213/85
Inventor 蒙健
Owner JIANGSU WEUNITE FINE CHEM CO LTD
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