A kind of preparation method of efficient and environment-friendly 2-hydroxyethylpyridine

A technology of hydroxyethylpyridine and picoline, which is applied in the field of new preparation technology of 2-hydroxyethylpyridine, can solve the problems of long reaction time, high reaction temperature, strong corrosion and the like, and achieves short reaction time and low reaction temperature. , the effect of low equipment requirements

Inactive Publication Date: 2016-08-24
SOUTHEAST UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Purpose of the invention: the purpose of the present invention is to generally adopt paraformaldehyde as raw material in the preparation technology of existing 2-hydroxyethylpyridine, take liquid acid as catalyzer, have long reaction time, high reaction temperature, large pollution, corrosion Strong and other problems, the present invention provides a novel process for the preparation of 2-hydroxyethylpyridine, through a large number of experimental screening, using solid superacid instead of liquid acid catalyst, less pollution, and can be produced in a shorter reaction time and lower 2-Hydroxyethylpyridine with high purity is prepared at high temperature, the present invention has high yield, strong environmental performance and low production cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] A kind of preparation method of efficient environment-friendly 2-hydroxyethylpyridine, it comprises the following steps:

[0021] 300kg 2-picoline, 115kg mass concentration is 40% formaldehyde solution and 6kg SO 4 2- / ZrO 2 The loaded benzoic acid was added into the autoclave, and the temperature was raised to 140° C. for 60 minutes. When the reaction time is up, quickly cool the autoclave to room temperature, press filter to remove the solid, put the liquid in the still, and distill unreacted formaldehyde, 2-picoline and water under reduced pressure at 40mmHg to obtain 99.8% purity 2-hydroxyethylpyridine, yield 90%.

Embodiment 2

[0023] A kind of preparation method of efficient environment-friendly 2-hydroxyethylpyridine, it comprises the following steps:

[0024] 150kg 2-picoline, 130kg 20% ​​formaldehyde solution and 6kg SO 4 2- / TiO 2 The loaded benzoic acid was added into the autoclave, and the temperature was raised to 180° C. for 30 minutes. When the reaction time is up, quickly cool the autoclave to room temperature, press filter to remove the solid, put the liquid in the still, and distill unreacted formaldehyde, 2-picoline and water under reduced pressure at 40mmHg to obtain 99.9% purity 2-hydroxyethylpyridine, yield 90%.

Embodiment 3

[0026] A kind of preparation method of efficient environment-friendly 2-hydroxyethylpyridine, it comprises the following steps:

[0027] 400kg 2-picoline, 200kg 40% formaldehyde solution and 4kg BA / SiO 2 The loaded benzoic acid was added into the autoclave, and the temperature was raised to 120° C. for 80 minutes. When the reaction time is up, the autoclave is quickly cooled to room temperature, the solid is removed by pressure filtration, the liquid is placed in a still, and the unreacted formaldehyde, 2-picoline and water are distilled under reduced pressure at 40 mmHg to obtain 99.9% purity 2-hydroxyethylpyridine, yield 91%.

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Abstract

The invention discloses a high-efficiency environment-friendly preparation method of 2-hydroxyethylpyridine, which comprises the following steps: proportionally adding 2-methylpyridine and formaldehyde into a high-pressure autoclave, adding a solid superhigh acid catalyst, heating while stirring to react, quickly cooling the high-pressure autoclave, filtering out the solid superhigh acid catalyst, distilling the mixed solution under reduced pressure, and distilling off unreacted 2-methylpyridine, formaldehyde and water under the pressure of 10-100 mmHg to obtain the 2-hydroxyethylpyridine end product. Abundant experiments are performed to screen out the optimal proportion of the reactant raw material to the catalyst thereof; and abundant experiments are performed to screen out the optimum reaction temperature, reaction time and reaction pressure. The whole method has the advantages of reasonable technique, small environmental pollution, low reaction temperature, short reaction time, high reaction efficiency, low production cost, high yield and high purity of the prepared 2-hydroxyethylpyridine.

Description

technical field [0001] The invention belongs to the preparation of pyridine compounds, in particular to a new preparation process of 2-hydroxyethylpyridine. Background technique [0002] 2-Hydroxyethylpyridine is an important chemical raw material, which is widely used in the synthesis and production of organic synthesis and pharmaceutical intermediates. The patent with the publication number CN1580046A provides a process for preparing 2-hydroxyethylpyridine on an industrial scale, using 2-picoline and paraformaldehyde as raw materials, and benzoic acid, chloroacetic acid or acetic acid as a catalyst. The patent with the publication number CN102731372A provides an efficient and environmentally friendly preparation method of 2-hydroxyethylpyridine, using tetrahydrofuran as a solvent, 2-picoline and paraformaldehyde as raw materials, and organic base catalysis. [0003] The above method mainly adopts paraformaldehyde as a reactant, because the decomposition temperature of par...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/30
CPCC07D213/30
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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