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Process of separating methyl pyridine mixture

A technology of methyl pyridine and separation method, applied in directions such as organic chemistry, can solve the problems of low product purity, difficulty in operation and control, and high cost

Inactive Publication Date: 2007-11-07
EAST CHINA UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the entrainer used in the existing azeotropic distillation separation technology is water, so that the boiling point of each azeotrope (formed by each component and water) is almost the same (the azeotrope of 2,6-lutidine and water The boiling point of the mixture fraction is 95.6°C, the boiling point of the azeotrope of 3-picoline and water is 96.7°C, and the boiling point of the azeotrope fraction of 4-picoline and water is 97°C), resulting in difficulties in operation and control, and product purity Low and high cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 100kg containing 34wt% 2, the mixture of 6-lutidine, 34wt% 4-picoline, 30wt% 3-picoline is put into the distillation still, then drops into 360kg methyl alcohol and 40kg water, as entrainer, heating This solution is rectified by a rectification tower (tray number 20). Under normal pressure, at 62-63 ° C, the azeotrope of 2,6-lutidine and methanol / water flows out from the top of the tower, and the boiling point is collected. The distillate 220kg (gas chromatography analysis: containing 15wt% of 2,6-lutidine, 76.5wt% of methanol, 8.5wt% of water).

[0021] The still temperature is cooled to room temperature, then add 170.1kg methyl alcohol and 18.9kg water, then carry out rectification, collect boiling point and be 65-66 ℃ cut 300kg (gas chromatography analysis: contain 3-picoline 9wt%, methyl alcohol 81.9wt% %, water 9.1wt%).

[0022] The still temperature is cooled to room temperature, then add 90kg methanol and 10kg water, then carry out rectification, collect 66-68 ℃...

Embodiment 2

[0026] 100kg containing 34wt% 2, the mixture of 6-lutidine, 34wt% 4-picoline, 30wt% 3-picoline is dropped into still still, then drops into 400kg 95v / v% ethanol as entrainer, heating This solution is rectified through a rectification tower (number of plates: 20). Under normal pressure, at 69-71 ° C, the azeotrope of 2,6-lutidine and ethanol flows out from the top of the tower, and the boiling point fraction is collected. 200kg (gas chromatography analysis: containing 16.5wt% of 2,6-lutidine, 83.5wt% of 95v / v% ethanol).

[0027] The still temperature is cooled to room temperature, then add 150kg 95v / v% ethanol aqueous solution, then carry out rectification, collect the cut 250kg that boiling point is 72.5-74 ℃ (gas chromatographic analysis: contain 3-picoline 11.2wt%, 95v / v v% ethanol 88.8 wt%).

[0028] The still temperature is cooled to room temperature, then add 70kg 95v / v% ethanol aqueous solution, then carry out rectification, collect 76-77 ℃ cut 100kg (gas chromatography...

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PUM

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Abstract

The present invention relates to process of separating mixture of methyl pyridine isomer and / or homologous compound. The separating process includes the main steps of: normal pressure rectification of the methyl pyridine mixture in the presence of C1-C6 monobasic alcohol water solution as the first azeotropic agent and collecting the fraction comprising the required component and the first azeotropic agent; and the subsequent normal pressure azeotropic rectification of the collected fraction with benzene as the second azeotropic agent to obtain the target product. The present invention can obtain components with purity not lower than 99 wt%, and has cheap material, easy control and low cost.

Description

technical field [0001] The present invention relates to a method for separating a mixture mainly composed of picoline isomers or / and homologues. Background technique [0002] So far, there are various methods for separating mixtures composed of picoline isomers and / or homologs that have been disclosed, mainly divided into three categories. One is: adopt the adsorption separation method to separate the mixture composed of picoline isomers or / and homologs (as reported in EP 173440 or U.S.Pat.No.3,064,002); the other is: chemical conversion method, that is, specific Add the compound of picoline isomers or / and homologues into the mixture, so that the added compound forms corresponding derivatives with one or more picolines, and utilizes the characteristics that these derivatives are easier to separate to achieve Separation purposes (such as the method described in U.S.Pat.No.2,516,370 or JP60214775); the third is: azeotropic distillation separation method, that is, the mixture ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/06
Inventor 沈永嘉朱健明王成云裘海啸
Owner EAST CHINA UNIV OF SCI & TECH
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