High-efficiency environment-friendly 2-vinyl pyridine preparation method

A technology of vinylpyridine and hydroxyethylpyridine, which is applied in the direction of sustainable manufacturing/processing, chemical industry, climate sustainability, etc., can solve the problems of low equipment corrosion, serious equipment corrosion, slow reaction speed, etc., and achieve equipment Low requirements, low environmental pollution and low production cost

Inactive Publication Date: 2014-11-05
SOUTHEAST UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Purpose of the invention: the purpose of the present invention is to provide a novel 2-vinylpyridine preparation process in order to overcome the large pollution in the prior art, serious equipment corrosion, low yie

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 123kg of 2-hydroxyethylpyridine and 20kg of KF / Mg-Al HT solid base were added to the reaction still, and dehydration reaction distillation was carried out at 100mmHg and 80°C, and the mixed solution of 2-vinylpyridine and water was continuously distilled. After 3 hours, the reaction was stopped. 115 kg of a mixed solution of 2-vinylpyridine and water was obtained.

[0023] 100kg of sodium hydroxide was added to the mixed solution of 2-vinylpyridine and water, fully dissolved, and then allowed to stand for 3 hours for stratification, and the upper layer was a 2-vinylpyridine-rich layer (oil layer).

[0024] The oil layer was put into the still, and distilled under reduced pressure at 25 mmHg, and the fractions at 60°C to 62°C were collected to obtain 2-vinylpyridine with a purity of 99.9% and a yield of 89%.

Embodiment 2

[0026] 300kg 2-hydroxyethylpyridine, 45kg KNO 3 / Ca-Mg-Al HT solid base was added to the reaction still, at 80 mmHg, dehydration reaction distillation was carried out at 70 ° C, and the mixed solution of 2-vinylpyridine and water was continuously distilled. After 4 hours, the reaction was stopped to obtain 280kg of the mixed solution of 2-vinylpyridine and water.

[0027] 200kg of sodium hydroxide was added to the mixed solution of 2-vinylpyridine and water, fully dissolved, and then allowed to stand for 5 hours to separate layers, and the upper layer was a 2-vinylpyridine-rich layer (oil layer). The oil layer was put into the still, and distilled under reduced pressure at 50 mmHg, and the fractions at 70°C to 72°C were collected to obtain 2-vinylpyridine with a purity of 99.9% and a yield of 90%.

Embodiment 3

[0029] 200kg of 2-hydroxyethyl pyridine and 30kg of KF / Ca-Al HT solid base were added to the reaction still, dehydration reaction distillation was carried out at 150mmHg and 100°C, and the mixed solution of 2-vinylpyridine and water was continuously distilled. After 2 hours, the reaction was stopped. 195 kg of a mixed solution of 2-vinylpyridine and water was obtained.

[0030] 190 kg of sodium hydroxide was added to the mixed solution, fully dissolved, and then allowed to stand for 3 hours to separate layers, and the upper layer was a 2-vinylpyridine-rich layer (oil layer). The oil layer was put into the still, and distilled under reduced pressure at 25 mmHg, and the fractions at 60°C to 62°C were collected to obtain 2-vinylpyridine with a purity of 99.9% and a yield of 90%.

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Abstract

The invention discloses a high-efficiency environment-friendly 2-vinyl pyridine preparation method. According to the method, 2-hydroxyethyl pyridine and a catalyst are subjected to reactive distillation at a pressure equivalent to 60-160mmHg, such that a mixed liquid of 2-vinyl pyridine and water is continuously produced by distillation; strong alkali is added, and the mixture is allowed to stand and is stratified, such that a 2-vinyl pyridine-rich oil layer is obtained; reduced-pressure distillation is carried out, and a fraction at a temperature of 30-130 DEG C is collected, such that a 2-vinyl pyridine finished product is obtained. According to the preparation method, reaction raw materials and optimal dose ratios, and especially the optimal catalyst and a dose thereof are screened through a large amount of experiments. The optimal reaction temperature, reaction time and reaction pressure are also screened through large amounts of experiments. The entire process is reasonable; environment pollution is low; reaction temperature is low; reaction time is short; reaction efficiency is high; requirements on equipment is low; production cost is low; yield is high; and produced 2-vinyl pyridine has high purity. With the method, various deficiencies of prior arts can be overcome.

Description

technical field [0001] The invention belongs to the preparation of pyridine compounds, in particular to a new preparation process of 2-vinylpyridine. Background technique [0002] 2-Vinylpyridine is mainly used to synthesize fenbutadiene latex, and also used to manufacture drugs such as kesilpine and betadine hydrochloride. At present, only a few countries in the world such as the United States, Japan and China produce it. At present, 2-vinylpyridine is mainly produced by the method of catalytic dehydration by 2-hydroxyethylpyridine, and the catalyst used in the production process is the key to the process. The Chinese patent with publication number CN102863375A uses 50% aqueous NaOH solution as a catalyst; the Chinese patent with publication number CN1580045A uses homogeneous liquid catalysts such as sulfuric acid, phosphoric acid, sodium hydroxide, potassium hydroxide to catalyze 2-hydroxyethylpyridine; The Chinese patent No. CN101225071A uses heteropolyacids as catalysts...

Claims

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Application Information

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IPC IPC(8): C07D213/16C07D213/127
CPCC07D213/127C07D213/16Y02P20/10
Inventor 肖国民高李璟张进宋坤忠薛中群丁木生
Owner SOUTHEAST UNIV
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