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Method of dehydrating 2-methylpyridine by coupling extraction and rectification operations

A picoline and extraction technology, applied in the separation field of 2-picoline dehydration, can solve the problem of high moisture content, achieve the effects of low energy consumption, wide application range and good separation effect

Pending Publication Date: 2018-09-28
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

[0007] In order to overcome the defects in the prior art, the present invention provides a method for removing water in 2-picoline by extraction operation and rectification operation, which can solve the problem of 2-picoline in the production process of 2-vinylpyridine The problem of excessive moisture content in the recycling process

Method used

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  • Method of dehydrating 2-methylpyridine by coupling extraction and rectification operations

Examples

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Effect test

Embodiment 1

[0019] Embodiment 1: the application example of dehydration method of the present invention in batch rectification mode of operation

[0020] Take by weighing 100g 2-picoline respectively, 150g water, 600g carbon tetrachloride, now extractant consumption is 6 times of 2-picoline quality, material is placed in separating funnel, it is sealed with glass stopper, Shake the separatory funnel to mix the materials evenly, then let it stand for 2h, and you can see obvious stratification, wherein the upper layer is an aqueous phase, and the lower layer is an organic phase containing 2-picoline and carbon tetrachloride; The phase mass is 149.5g, and the mass fractions of water, 2-picoline, and carbon tetrachloride are 99.2%, 0.74%, and 0.06%, respectively.

[0021] Release the organic phase from the valve below the separatory funnel, feed it to the bottom of the batch distillation tower containing 30 trays at one time, turn on the condensate water, turn on the heating device of the bot...

Embodiment 2

[0024] The application example of the dehydration method of the present invention in the continuous rectification operation mode.

[0025] 2-picoline / aqueous solution and extraction agent are all continuous feeding, and wherein in 2-picoline / aqueous solution, the mass fraction of 2-picoline is 50%, feed flow rate is 200kg / h, extraction agent four The feed flow rate of carbon chloride is 800kg / h. At this time, the amount of extractant is 8 times the mass of 2-picoline. After the two are mixed evenly by the mixer, they enter the phase separation tank for phase separation to ensure that the materials are phase separated. The time can reach 1h, and the aqueous phase and organic phase can be continuously extracted. The produced water phase flow rate is 99.8kg / h, and the organic phase flow rate is 900.2 kg / h.

[0026] The organic phase extracted from the phase separation tank is preheated to 60°C through a heat exchanger, and is continuously fed to the rectification tower with 40 t...

Embodiment 3

[0029] When the dehydration method of the present invention is low in feed concentration, the application example in the continuous rectification mode of operation:

[0030] 2-picoline / aqueous solution and extraction agent are all continuous feeding, and wherein in 2-picoline / aqueous solution, the mass fraction of 2-picoline is 10%, feed flow rate is 200kg / h, extraction agent four The feed flow rate of chlorinated carbon is 200kg / h. At this time, the amount of extractant is 10 times the mass of 2-picoline. After the two are mixed evenly by the mixer, they enter the phase separation tank for phase separation to ensure that the materials are phase separated. The time can reach 5h, and the aqueous phase and organic phase can be continuously extracted. The flow rate of the aqueous phase is 181.2 kg / h, and the flow rate of the organic phase is 218.8 kg / h.

[0031] The organic phase extracted from the phase separation tank is preheated to 50°C through a heat exchanger, and is conti...

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Abstract

A method of dehydrating 2-methylpyridine by coupling extraction and rectification operations includes the following steps: 1) mixing an extraction agent with a 2-methylpyridine / water solution to perform extraction; 2) allowing the mixture liquid in the step 1) to stand in a phase separation tank for phase separation, then layering the mixture to obtain a water phase being water and an organic phase being a mixture liquid of the 2-methylpyridine and the extraction agent; 3) preheating the organic phase to 50-60 DEG C, feeding the organic phase into a rectification column for separation, whereinthe extraction agent is withdrawn from the column top and the 2-methylpyridine is withdrawn from the column bottom. The method can prepare high-purity 2-methylpyridine and extraction agent just withone rectification column, solves the problem of influence on recycling use due to high water content of the 2-methylpyridine in a production process of 2-vinylpyridine, has good separation effect, islow in energy consumption and cost, has extensive application range, and is suitable for both batch rectification process and continuous rectification process.

Description

technical field [0001] The invention relates to a separation technology for dehydration of 2-picoline. 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 under high pressure or normal pressure to synthesize 2-hydroxyethylpyridine, and the latter is obtained by d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/127C07D213/16
CPCC07D213/127C07D213/16
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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