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Process for large-scale preparation of 2-vinyl pyridine

A vinylpyridine and preparation process technology, applied in the direction of organic chemistry and the like, can solve the problems of high requirements, high reaction temperature, high unit consumption, and achieve the effects of general equipment requirements, high yield and simple production process

Active Publication Date: 2005-02-16
淄博张店东方化学股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 is equivalent to 15kg / cm 2 ), the reactor is a pipeline type, easy to block, and the equipment needs pressure resistance and anti-corrosion, which have high requirements; the unit consumption of 2-picoline is high (1 ton of 2-vinylpyridine consumes 1.4 tons of 2-picoline), and the yield is only 63%±; the product 2-vinylpyridine entrains the intermediate 2-hydroxyethylpyridine, which affects the quality of the product 2-vinylpyridine

Method used

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  • Process for large-scale preparation of 2-vinyl pyridine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1. The dehydration reaction equation is as follows:

[0023]

[0024] In the presence of inorganic acid or inorganic base, 2-hydroxyethylpyridine removes a molecule of water to generate 2-vinylpyridine.

[0025] 2. Specific process operation

[0026] 1. Raw material situation

[0027] 2-Hydroxyethylpyridine, content ≥ 98.50%, 2-methylpyridine ≤ 1.0%, moisture ≤ 1%, self-made; sulfuric acid commercially available as an industrial product.

[0028] 2 ratio

[0029] The weight ratio of the raw materials is 2-hydroxyethylpyridine: sulfuric acid = 1: 1; the reaction temperature is 180-190°C;

[0030] The specific quantity is: 2-hydroxyethylpyridine (content 98.57%) 1247.84kg, equivalent to pure 1230kg;

[0031] Sulfuric acid (content 95%) 1031.58kg, converted to pure 980kg;

[0032] 3. Specific operation

[0033] Proportional sulfuric acid is added to the reaction kettle, under stirring, the temperature is gradually raised to 180 ° C, and the reaction ti...

Embodiment 2

[0035] The weight ratio of raw materials is 2-hydroxyethylpyridine:phosphoric acid=1:1; reaction 180~190°C / 30min;

[0036] The specific quantity is: 2-hydroxyethylpyridine (content 98.57%) 1247.84kg, equivalent to pure 1230kg;

[0037] Phosphoric acid (content 95%) 1031.58kg, converted to pure 980kg,

[0038] Finished product 900.55kg, content 98.28%, convert pure 885.06kg, yield 84.29%; Moisture content 0.48%, all the other are the same as Example 1.

Embodiment 3

[0040] The weight ratio of raw materials is 2-hydroxyethylpyridine: sodium hydroxide = 1: 1; reaction 180~190°C / 10min;

[0041] The specific quantity is: 2-hydroxyethylpyridine (content 98.57%) 1247.84kg, equivalent to pure 1230kg;

[0042] Sodium hydroxide (content 95%) 421.05kg, converted to pure 400kg,

[0043] 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 Example 1.

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Abstract

The invention refers to the technique to produce 2- vinyl pyridine with the scale of industrial production. It chooses the 2-ethoxyl pyridine as the starting material, dehydrates a molecule of water to produce 2-vinyl pyridine with the existence of the catalyzer; keep the weight ratio of 2-ethoxyl pyridine:catalyzer=1:0.05-1.0 and chooses the vitriol, phosphoric acid, sodium hydroxide or potassium hydroxide as the catalyzer. The reaction condition is as follows: whisk it for between 5min and 30min at the temperature of between 100deg.C and 190deg.C, collect the fractions with boiling range of 60-100deg.C / 10-150mm / Hg, separate the water of the imputities by alkaliingout method or saltingout method to get the crude product; distill it with lower pressure, collect the fractions with boiling range of 60-100deg.C / 90-150mm / Hg and get the turnoff of the 2- vinyl pyridine. Compared with today's technology, the invention is featured by the following aspects: normal pressure, tank reactor, ecumenic requirements to the equipments, simpler production technique and higher yield.

Description

technical field [0001] The invention belongs to the preparation of pyridine compounds, in particular to a process for preparing 2-vinylpyridine on an industrial scale. Background technique [0002] In the prior art, 2-picoline is used as a starting material to produce 2-vinylpyridine, and its process route is a one-step process; that is, the input raw material is 2-picoline, and the product obtained after the reaction is 2-vinylpyridine. Pyridine, the intermediate 2-hydroxyethylpyridine is 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 is equivalent to 15kg / cm 2 ), the reactor is a pipeline type, easy to block, and the equipment needs pressure resistance and anti-corrosion, which have high requirements; the unit consumption of 2-picoline is high (1 ton of 2-vinylpyridine consumes 1.4 tons of 2-picoline), and the yield is only 63%±; the intermediate ...

Claims

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Application Information

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IPC IPC(8): C07D213/127
Inventor 王宝庆仇传禄赵学冉邹长征
Owner 淄博张店东方化学股份有限公司
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