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Method for realizing 2-picoline dehydration by side withdrawal from azeotropic distillation column

A technology of azeotropic distillation column and picoline, which is applied in the direction of sustainable manufacturing/processing, chemical industry, climate sustainability, etc., can solve the problems of high moisture content of 2-picoline affecting recycling, etc., and achieve product High recovery rate, good separation effect and simple operation

Active Publication Date: 2018-06-22
淄博高新技术产业开发区精细化工和高分子材料研究院 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In order to overcome the defects in the prior art, the present invention provides a method for realizing 2-picoline dehydration by using the side line extraction of an azeotropic rectification tower, which can solve the problem of 2-picoline moisture in the production process of 2-vinylpyridine. Excessive content affects the problem of recycling

Method used

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  • Method for realizing 2-picoline dehydration by side withdrawal from azeotropic distillation column
  • Method for realizing 2-picoline dehydration by side withdrawal from azeotropic distillation column

Examples

Experimental program
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Embodiment 1

[0021] as attached figure 1 As shown, the 2-picoline / water solution with a mass fraction of 8% is continuously fed to an azeotropic distillation column containing 15 trays, the flow rate is 200kg / h, and the feeding position is the 9th tray; The entrainer cyclohexane is continuously fed to the rectification column from the first tray, the flow rate is 1472kg / h, and the amount of the entrainer is 8 times of the water quality at this time; the tower still heating device is turned on. The operating pressure of the rectification tower is 101.325kPa, the temperature at the top of the tower is 65°C, and the temperature at the bottom of the tower is 125°C.

[0022] Extraction and follow-up operations are as follows:

[0023] (1) All the gas phase at the top of the tower is taken out, then cooled to a liquid phase by heat exchanger 1, and then carried out in a phase separator for phase separation operation, and the phase separation time is 5 hours;

[0024] The gas phase at the top o...

Embodiment 2

[0029] The difference between this embodiment and embodiment one is that the 2-picoline / water solution with a mass fraction of 50% is continuously fed to an azeotropic rectification column containing 30 trays, with a flow rate of 100kg / h, The feeding position is the 11th tray; the entrainer cyclohexane is continuously fed to the rectification column from the first tray, the flow rate is 300kg / h, and the amount of the entrainer is 6 times the water quality ; Turn on the tower kettle heating device. The operating pressure of the rectification tower is 101.325kPa, the temperature at the top of the tower is 55°C, and the temperature at the bottom of the tower is 128°C.

[0030] Extraction and follow-up operations are as follows:

[0031] (1) All the gas phase at the top of the tower is taken out, then cooled to a liquid phase by heat exchanger 1, and then carried out in a phase separator for phase separation operation, and the phase separation time is 3 hours;

[0032] The gas p...

Embodiment 3

[0037] The difference between this embodiment and embodiment two is that the 2-picoline / water solution with a mass fraction of 99% is continuously fed to an azeotropic rectification column containing 10 trays, and the flow rate is 100kg / h. The feeding position is the fifth tray; the entrainer cyclohexane is continuously fed from the first tray to the rectification column at a flow rate of 10kg / h, and the amount of the entrainer is 10 times the water mass ; Turn on the tower kettle heating device. The operating pressure of the rectification tower is 101.325kPa, the temperature at the top of the tower is 62°C, and the temperature at the bottom of the tower is 130°C.

[0038] Extraction and follow-up operations are as follows:

[0039] (1) The gas phase at the top of the tower is all extracted, and then cooled to a liquid phase by heat exchanger 1, and then carried out in a phase separator for phase separation operation, and the phase separation time is 0.5h;

[0040] The gas pha...

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Abstract

The invention provides a method for realizing 2-picoline dehydration by side withdrawal from an azeotropic distillation column. According to the method, cyclohexane is taken as an entrainer, a new lowazeotrope is formed from cyclohexane and water and breaks azeotropy of 2-picoline and water. A cyclohexane and water gas-phase mixture is obtained from top of the azeotropic distillation column, vapor rich in 2-picoline is withdrawn from the side of a column plate close to the column bottom and condensed into a liquid by a heat exchanger, a small amount of 2-picoline containing impurities is withdrawn from the column bottom, and accordingly, separation of 2-picoline and water is realized with the distillation method. The method is applicable to continuous distillation operation, 2-picoline with higher purity can be obtained by side withdrawal, 2-picoline is prevented from being heated at the column bottom for too long time to produce side effects, only one substance, namely, the entraineris introduced in the whole process, the entrainer can be efficiently recycled, and the method is a separation method with high efficiency and low energy consumption and cost.

Description

technical field [0001] The invention belongs to the technical method of the chemical industry separation process, and relates to a method for realizing the dehydration of 2-picoline by azeotropic rectification. Background technique [0002] 2-Methylpyridine is an important chemical intermediate and an important raw material for the synthesis of medicines and dyes. At present, 2-picoline is widely used to synthesize 2-vinylpyridine, and the latter is used to produce butylpyridine latex. Butylpyridine latex is the skeleton material of rubber products such as tires and conveyor belts. my country's annual demand is tens of thousands of tons, and the demand is year by year At present, domestic butylpyridine latex mainly depends on imports, and refined 2-picoline plays an important role in the synthesis of butylpyridine latex. [0003] The process of synthesizing 2-vinylpyridine with 2-picoline is as follows: 2-picoline and paraformaldehyde are catalytically added in liquid phase ...

Claims

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Application Information

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IPC IPC(8): C07D213/127C07D213/16
CPCC07D213/127C07D213/16Y02P20/10
Inventor 吕灵娟杜振江刘宁那平白鹏
Owner 淄博高新技术产业开发区精细化工和高分子材料研究院
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