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Method of synthesis of 2-picoline through 5-ketohexanenitrile

A technology of methyl pyridine and base capronitrile, which is applied in chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, organic chemistry, etc., can solve the problems of low purity, unstable acetylene, and explosive polymerization. , to achieve the effect of strong operability, safe operation and reasonable design

Active Publication Date: 2013-02-13
连云港阳方催化科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

2-Methylpyridine came from the pyridine fraction in coal tar in the early stage, the output is too small, the purity is very low, and it is far from meeting the demand
The biggest disadvantage of this process is that acetylene is not stable, and it is prone to explosive polymerization under this condition.

Method used

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  • Method of synthesis of 2-picoline through 5-ketohexanenitrile
  • Method of synthesis of 2-picoline through 5-ketohexanenitrile
  • Method of synthesis of 2-picoline through 5-ketohexanenitrile

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Example 1, a method for synthesizing 2-picoline from 5-ketocapronitrile, the method uses 5-ketocapronitrile (acetylbutyronitrile) as raw material, and in the presence of hydrogen, a granular catalyst is packed in a fixed bed , at a temperature of 380°C and a pressure of 0.02MPa, one-step synthesis of 2-picoline; the load of 5-ketocapronitrile is 40g / liter catalyst L·h, and the standard hydrogen circulation in the tail gas is 0.08m 3 / liter of catalyst L h;

[0022] Each active component of the granular catalyst is counted as:

[0023] Zn 1.0 Cr a Cu b mn c K d o e

[0024] The value of a ranges from 0.1 to 1.2;

[0025] The b value ranges from 0.1 to 0.6;

[0026] The value of c ranges from 0.05 to 0.5;

[0027] The range of d value is 0.01~0.08;

[0028] e is the sum of the oxygen required to satisfy the oxides of each element.

Embodiment 2

[0029] Example 2, a method for synthesizing 2-picoline from 5-ketocapronitrile, the method uses 5-ketocapronitrile (acetylbutyronitrile) as raw material, and in the presence of hydrogen, a granular catalyst is packed in a fixed bed , at a temperature of 420°C and a pressure of 0.1 MPa, 2-picoline was synthesized in one step; the load of 5-ketocapronitrile was 180 g / liter catalyst L·h, and the standard hydrogen circulation in the tail gas was 0.2 m 3 / liter of catalyst L h;

[0030] Each active component of the granular catalyst is counted as:

[0031] Zn 1.0 Cr a Cu b mn c K d o e

[0032] The value of a ranges from 0.1 to 1.2;

[0033] The b value ranges from 0.1 to 0.6;

[0034] The value of c ranges from 0.05 to 0.5;

[0035] The range of d value is 0.01~0.08;

[0036] e is the sum of the oxygen required to satisfy the oxides of each element.

Embodiment 3

[0037] Example 3, a method for synthesizing 2-picoline from 5-ketocapronitrile, the method uses 5-ketocapronitrile (acetylbutyronitrile) as raw material, and in the presence of hydrogen, a granular catalyst is packed in a fixed bed , at a temperature of 400°C and a pressure of 0.06 MPa, one-step synthesis of 2-picoline; the load of 5-ketocapronitrile is 100 g / liter catalyst L·h, and the standard hydrogen circulation in the tail gas is 0.12 m 3 / liter of catalyst L h;

[0038] Each active component of the granular catalyst is counted as:

[0039] Zn 1.0 Cr a Cu b mn c K d o e

[0040] The value of a ranges from 0.1 to 1.2;

[0041] The b value ranges from 0.1 to 0.6;

[0042] The value of c ranges from 0.05 to 0.5;

[0043] The range of d value is 0.01~0.08;

[0044] e is the sum of the oxygen required to satisfy the oxides of each element.

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Abstract

The invention provides a method of synthesis of 2-picoline through 5-ketohexanenitrile. According to the method, 5-ketohexanenitrile (acetyl butyronitrile) is utilized as raw materials, with the existence of hydrogen, a particle catalyst is filled in a fixed bed, at the temperature of 380-420 DEG C, under the pressure of 0.02-0.1Mpa, the 2-picoline is synthesized in one step, and each active component of the particle catalyst is Zn1.0CraCubMncKdOe in terms of atomicity. According to the method, with the existence of hydrogen, the 5-ketohexanenitrile raw materials are subjected to hydrogenation, ring closure and dehydrogenation to generate the 2-picoline meanwhile. The method is reasonable in design, high in operability and safe to operate. Due to the method, waster water, waste and waste solid are not generated, and requirement of environment-friendly chemical industry at present is met. According to the method, composite zinc-chromium-manganese-potassium is used as a catalyst, conversion ratio of the 5-ketohexanenitrile can reach 99.0%, molar yield of the 2-picoline can reach 99.0%, and the method can be directly used for synthesizing 2-cyanopridine.

Description

technical field [0001] The invention relates to a preparation method of 2-picoline, in particular to a method for synthesizing 2-picoline from 5-ketocapronitrile. Background technique [0002] 2-picoline can be used in pesticide, medicine, cord fabric and other industries. 2-Methylpyridine comes from the pyridine fraction in coal tar in the early stage, and the yield is too small and the purity is very low, which is far from meeting the demand. The industrial by-product of synthetic pyridine is 2-picoline, and the output is 6-8% of the pyridine content. Since the maximum use of pyridine is to synthesize the pesticide paraquat, and paraquat is limited and phased out, the output of pyridine has shrunk dramatically. In the production of diphenylamine, a very small amount of 2-picoline is also produced by-product, and the yield is 0.6% of that of diphenylamine. At present, the relatively advanced technology is that acetonitrile and acetylene are catalyzed by cyclopentadienyl-c...

Claims

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Application Information

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IPC IPC(8): C07D213/16C07D213/09B01J23/889
Inventor 杨永恒
Owner 连云港阳方催化科技有限公司
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