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Process for large-scale preparation of 2-hydroxyethyl pyridine

A technology of hydroxyethylpyridine and industrial scale, which is applied in the technical field of preparing 2-hydroxyethylpyridine on an industrial scale, can solve the problems such as the lack of supply of industrial-scale 2-hydroxyethylpyridine products, and achieve simple and convenient production process and high yield Effect

Active Publication Date: 2006-04-26
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

[0002] In the prior art, there is no industrial scale 2-hydroxyethylpyridine product supply

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1 1

[0015] Embodiment 1 one, reaction equation is as follows:

[0016]

[0017] 2. Specific process operation

[0018] Using 2-methylpyridine as the starting material, it condenses with paraformaldehyde in the presence of a catalyst to generate 2-hydroxyethylpyridine.

[0019] 1. Raw material situation

[0020] 2-Methylpyridine (2-methylpyridine) is commercially available, with a content ≥ 99% and a moisture content ≤ 0.2%;

[0021] Paraformaldehyde (Paraformaldehyde, also known as solid formaldehyde) is commercially available, solid particles, content 90-95%, formic acid content ≤ 0.03%;

[0022] Benzoic acid (benzoic acid, commercially available industrial product, content ≥ 98.5%) is used as catalyst.

[0023] 2. Weight ratio

[0024] 2-picoline:paraformaldehyde:catalyst=1:0.12:0.012

[0025] Feeding quantity is: 2-picoline (content 99.5%, w / w) 93.5kg, pure 93.0kg

[0026] Paraformaldehyde (content 90.5%, w / w) 12.33kg, pure 11.16kg

[0027] Benzoic acid (content 98.5%...

Embodiment 2

[0030] Embodiment 2 catalyst is commercially available chloroacetic acid (monochloroacetic acid), monochloroacetic acid content ≥ 99%, dichloroacetic acid content ≤ 0.5%,

[0031] 2-picoline: paraformaldehyde: catalyst=1: 0.03: 0.003;

[0032] Feeding quantity is: 2-picoline (content 99.5%, w / w) 93.5kg, pure 93.0kg

[0033] Paraformaldehyde (content 91.5%, w / w) 3.05kg, pure 2.79kg

[0034] Chloroacetic acid (content 99.5%, w / w) 0.2804kg, pure 0.28kg

[0035] The reaction temperature is 90-100°C, the reaction time is 10-12 hours, and the finished product of 2-hydroxyethylpyridine is obtained. The finished product has a yield of 107.52kg, a content of 98.12%, and a pure conversion of 105.50kg, based on 2-picoline, with a yield of 85.77%; a light yellow transparent liquid with a moisture content of 0.48%; the rest are the same as in Example 1.

Embodiment 3

[0036] Embodiment 3 Catalyst uses commercially available commodity acetic acid (acetic acid), acetic acid content ≥ 96%,

[0037] 2-picoline: paraformaldehyde: catalyst=1: 0.12: 0.003;

[0038] Feeding quantity is: 2-picoline (content 99.5%) 93.5kg, convert pure 93.0kg

[0039] Paraformaldehyde (content 90.5%) 12.33kg, pure 11.16kg

[0040] Acetic acid (content 96.5%) 0.2804kg, converted to pure 0.28kg

[0041] The reaction temperature is 170-180°C, the reaction time is 15 hours, the yield of the finished product is 115.96kg, the content is 98.58%, and the pure product is 114.31kg. Based on 2-picoline, the yield is 92.94%. It is a colorless and transparent liquid with a water content of 0.48%. The rest With embodiment 1.

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Abstract

The invention relates to a process for preparing 2-hydroxyethylpyridine on an industrial scale. 2-methylpyridine is used as the starting material; in the presence of catalyst benzoic acid, chloroacetic acid or acetic acid, it is condensed with paraformaldehyde to generate 2-hydroxyethylpyridine; the weight ratio of raw materials is: 2-methylpyridine : Paraformaldehyde: Catalyst=1: 0.03~0.12: 0.0024~0.012; Reaction condition: 90~180 ℃ / 10~30h under agitation: Reaction is finished, vacuum distillation, collection boiling range 60~150 ℃ / 10~100mmHg distillate Parts, to obtain 2-hydroxyethylpyridine finished product. It fills the gap in the country, and the production process is simple; the yield is high, and the yield can reach 84-94.85% based on 2-picoline.

Description

technical field [0001] The invention belongs to the preparation of pyridine compounds, in particular to a process for preparing 2-hydroxyethylpyridine on an industrial scale. Background technique [0002] In the prior art, there is no industrial scale 2-hydroxyethylpyridine product supply. Only in the process of producing 2-vinylpyridine from 2-picoline as the starting material, 2-hydroxyethylpyridine is generated in the intermediate reaction; but the prior art does not separate the intermediate 2-hydroxyethylpyridine , but continue the reaction to prepare the final product 2-vinylpyridine. Contents of the invention [0003] The purpose of the present invention is to separate and obtain 2-hydroxyethylpyridine (2-hydroxyethylpyridine) product on the basis of prior art. [0004] The technical scheme of the present invention is as follows: develop a kind of industrial-scale preparation 2-hydroxyethylpyridine technique, it is characterized in that be that starting material i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/64
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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