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Method for industrial scale preparation of 4-vinylpyridine

A vinylpyridine, industrial-scale technology, applied in the field of industrial-scale preparation of 4-vinylpyridine, can solve the problems of high requirements, high reaction temperature, and high unit consumption, meets general equipment requirements, simple production process, and no danger. Effect

Inactive Publication Date: 2016-10-12
淄博张店东方化学股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The disadvantage of this method is that the reaction temperature is relatively high (400-500°C), and the reaction pressure is relatively high (1.5MPa, equivalent to 15kg / cm 3 ), the reactor is a pipeline type, easy to block, and the equipment needs to be pressure-resistant and anti-corrosion, and the requirements are high; the unit consumption of 4-picoline is high (1 ton of 4-vinylpyridine consumes 1.4 tons of 4-picoline), and the yield is only About 63%; the product 4-vinylpyridine entrains the intermediate 4-hydroxyethylpyridine, which affects the quality of the product 4-vinylpyridine

Method used

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  • Method for industrial scale preparation of 4-vinylpyridine

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The weight ratio of 4-hydroxyethylpyridine to catalyst calcium chloride is 1:1.

[0023] Feeding amount:

[0024] 4-Hydroxyethylpyridine (content 98.57%) 1247.84kg, converted to pure 1230kg;

[0025] Calcium chloride (content 94%) 1031.58kg, converted to pure 970kg;

[0026] Put the catalyst into the reaction kettle, under stirring, gradually heat up to 180°C, and time the reaction, gradually add 4-hydroxyethylpyridine dropwise, and at the same time, vacuumize the reaction kettle, and the reaction solution will undergo dehydration reaction immediately, and the reaction product (reaction generated 4-vinylpyridine and water) are distilled from the steam outlet, reacted at 185±5°C for 5 minutes, collected fractions with a boiling range of 60-100°C / 10-150 mmHg, and separated the reaction water contained in the fractions by alkali analysis , the reaction generates water and dissolves solid sodium hydroxide or sodium chloride for alkali analysis, and the lower layer is NaOH...

Embodiment 2

[0029] The weight ratio of 4-hydroxyethylpyridine to catalyst magnesium chloride is 1:1.

[0030] Feeding amount:

[0031] 4-Hydroxyethylpyridine (content 98.57%) 1247.84kg, converted to pure 1230kg;

[0032] Magnesium chloride (content 46%) 1031.58kg, converted to pure 475kg;

[0033] The reaction temperature is 185±5°C, and the reaction time is 30 minutes;

[0034] Obtain finished product 900.55kg, content 98.28%, convert pure 885.06kg, yield 84.29%; Moisture 0.48%, all the other are with embodiment 1.

Embodiment 3

[0036] The weight ratio of 4-hydroxyethylpyridine to catalyst sodium acetate is 1:1.

[0037] Feeding amount:

[0038] 4-Hydroxyethylpyridine (content 98.57%) 1247.84kg, converted to pure 1230kg;

[0039] Sodium acetate (content 98%) 421.05kg, converted to pure 413kg;

[0040] Reaction temperature 185±5℃, reaction time 10min;

[0041] Obtain finished product 920.85kg, content 98.58%, convert pure 907.77kg, yield 86.46%; Moisture content 0.51%, all the other are the same as embodiment 1.

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Abstract

Belonging to the field of preparation of pyridine compounds, the invention in particular relates to a process for industrial scale preparation of 4-vinylpyridine. The process consists of: taking 4-hydroxyethylpyridine as the starting raw material, in the presence of a catalyst, carrying out dehydration reaction, firstly collecting fraction with a boiling range of 60-100DEG C / 10-150mmHg, separating the reaction generated water mingled in the fraction by means of alkali washing or salting-out to obtain a crude product; then conducting reduced pressure distillation on the crude product, and collecting fraction with a boiling range of 60-100DEG C / 90-150mmHg, thus obtaining the 4-vinylpyridine product. The catalyst is one of calcium chloride, magnesium chloride or sodium acetate. The catalyst adopted by the invention is an ordinary chemical product and non-hazardous; the reaction condition is atmospheric pressure, the process involves a kettle reactor and has general requirements for equipment; and the production process is simple, and has high yield.

Description

technical field [0001] The invention belongs to the field of preparation of pyridine compounds, in particular to a process for preparing 4-vinylpyridine on an industrial scale. Background technique [0002] In the prior art, 4-picoline is used as a starting material to produce 4-vinylpyridine, and its process route is a one-step method: the input raw material is 4-picoline, and the product obtained after the reaction is 4-vinylpyridine , the intermediate 4-hydroxyethylpyridine was not isolated. [0003] The disadvantage of this method is that the reaction temperature is relatively high (400-500°C), and the reaction pressure is relatively high (1.5MPa, equivalent to 15kg / cm 3 ), the reactor is a pipeline type, easy to block, and the equipment needs to be pressure-resistant and anti-corrosion, and the requirements are high; the unit consumption of 4-picoline is high (1 ton of 4-vinylpyridine consumes 1.4 tons of 4-picoline), and the yield is only About 63%; the intermediate ...

Claims

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Application Information

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IPC IPC(8): C07D213/127C07D213/16
CPCC07D213/127C07D213/16
Inventor 王宝庆仇传禄王刚孔凡平
Owner 淄博张店东方化学股份有限公司
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