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2-vinylpyridine produced by catalyst distillation of heteropoly acid

A technology of vinylpyridine and heteropolyacids, which is applied in physical/chemical process catalysts, chemical industry, organic chemistry, etc. It can solve the problems of high energy consumption, pollution of the catalyst environment, etc., and achieve the effect of simple process

Inactive Publication Date: 2008-07-23
于景东
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process has high energy consumption and the catalyst pollutes the environment. Therefore, a new process method is urgently needed to replace the existing process.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Weigh the by-product 2-picoline and formaldehyde of diphenylamine, so that the molar ratio of the two is 1:2, then weigh the catalyst phosphotungstic acid (HPW), make phosphotungstic acid (HPW) and 2-picoline The mass ratio of the sum of formaldehyde and formaldehyde is 0.001. The above-mentioned raw materials are put into a four-stage serial stirring reactor at a feed rate of 100-500Kg / h, and the paddle type is stirred at a speed of 60-150RPM. Among them: the reaction temperature of the first-stage reactor is 60-160°C, and the pressure is 0.1-0.3MPa; the reaction temperature of the second-stage reactor is 60-160°C, normal pressure; the reaction temperature of the third-stage reactor is 120-260°C , the pressure is 20-80mmHg; the reaction temperature of the four-stage reactor is 80-200°C, and the pressure is 10-50mmHg. Finally, the distillate product with a boiling range of 120-150°C is obtained. According to gas chromatography analysis, the single pass conversion rate ...

Embodiment 2

[0016] Weigh the by-product 2-picoline and paraformaldehyde of diphenylamine, make the molar ratio of the two be 1: 3, then weigh the catalyst phosphomolybdic acid (HPMo), make phosphomolybdic acid (HPMo) and 2-formaldehyde The mass ratio of the sum of pyridine and paraformaldehyde is 0.008, and the above-mentioned raw materials are put into a four-stage serial stirring reactor at a feed rate of 100-500Kg / h, and the paddle type is stirred at a speed of 60-150RPM. Among them: the reaction temperature of the first-stage reactor is 60-160°C, and the pressure is 0.1-0.3MPa; the reaction temperature of the second-stage reactor is 60-160°C, normal pressure; the reaction temperature of the third-stage reactor is 120-260°C , the pressure is 20-80mmHg; the reaction temperature of the four-stage reactor is 80-200°C, and the pressure is 10-50mmHg. Finally, a fraction product with a boiling range of 120-150°C is obtained, and the selectivity of 2-vinylpyridine reaches 97.00%; then the rem...

Embodiment 3

[0018] Weigh the by-product 2-picoline and formaldehyde of diphenylamine, so that the molar ratio of the two is 1:2.5, then weigh the catalyst phosphotungstic acid (HPW), make phosphotungstic acid (HPW) and 2-picoline The mass ratio of the sum of formaldehyde and formaldehyde is 0.005, and the above-mentioned raw materials are put into a four-stage serial stirring reactor at a feed rate of 100-500Kg / h, and the paddle type is stirred at a speed of 60-150RPM. Among them: the reaction temperature of the first-stage reactor is 60-160°C, and the pressure is 0.1-0.3MPa; the reaction temperature of the second-stage reactor is 60-160°C, normal pressure; the reaction temperature of the third-stage reactor is 120-260°C , the pressure is 20-80mmHg; the reaction temperature of the four-stage reactor is 80-200°C, and the pressure is 10-50mmHg. Finally, the distillate product with a boiling range of 120-150°C is obtained. The selectivity of 2-vinylpyridine reaches 97.00%. The remaining un...

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Abstract

The invention discloses a method of using heteropolyacid catalyst to prepare 2-vinylpyridine, which comprises: (1). 2-methylpyridine and formaldehyde or paraformaldehyde with molar ratio of 1:2 to 3 are used as raw material; mass ratio between added heteropolyacid catalyst and the raw material is 0.001 to 0.008; 4-stage series type stirring reactor is arranged and material feeding speed is 100 to 500kg / h; (2). The raw material and the catalyst are reacted in the 4-stage series type stirring reactor to collect final fraction product with boiling range of 120 to 150 DEG C, thereby getting 2-vinylpyridine; (3). The rest fractions are collected and returned to stage-1 reactor to increase conversion rate of 2-methylpyridine. The conversion rate of 2-methylpyridine reaches 95% and the selectivity of the 2-vinylpyridine reaches 97.00%, thereby realizing effective use of byproduct. The preparation method for 2-vinylpyridine by using heteropolyacid catalyst has the advantages of simple technique and non-pollution upon environment.

Description

technical field [0001] The invention relates to a preparation method of 2-vinylpyridine, in particular to a method for one-step synthesis and preparation of 2-vinylpyridine using an environment-friendly catalyst. Background technique [0002] What take 2-picoline as raw material to produce the operational route of 2-vinylpyridine at present adopts two-step method production, intermittent operation; What catalyst used is benzoic acid, chloroacetic acid or acetic acid. This process has high energy consumption and the catalyst pollutes the environment. Therefore, a new process method is urgently needed to replace the existing process. Contents of the invention [0003] In view of the deficiencies in the prior art, the purpose of the present invention is to provide a new preparation method for 2-vinylpyridine using 2-picoline as raw material and heteropoly acid as a catalyst. The method has simple process and no pollution to the environment . [0004] Goal of the invention o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/06C07D213/127B01J27/188
CPCY02P20/10
Inventor 于景东
Owner 于景东
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