Synthesis of DMF and device

A heat exchange device and cooling medium technology, applied in the preparation of organic compounds, organic chemistry, chemical instruments and methods, etc., can solve the problems of low synthesis efficiency and short production cycle, reduce the frequency of equipment start-up and stop, and improve the reaction Efficiency, reduction of maintenance and cleaning costs and the effect of pollutant emissions

Active Publication Date: 2009-01-07
HENAN JUNHUA DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The object of the present invention is to provide a kind of DMF synthesis method, solve the problem that synthesis efficiency is low, production period is short in current DMF synthesis

Method used

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  • Synthesis of DMF and device

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Experimental program
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Effect test

Embodiment 1

[0026] Such as figure 1 As shown, the DMF reaction device is composed of a DMF reactor 1, a desalinated water heat exchanger 2, a desalted water circulation pump 3 (one of which is a standby pump), and a buffer tank 4; wherein the outlet of the DMF reactor 1 cooling medium is connected to the buffer tank, The buffer tank is connected to the desalinated water circulating pump 3, and the circulating pump 3 is connected to the desalinated water heat exchanger 2, and the desalted water heat exchanger 2 is connected to the cooling medium inlet of the DMF reactor 1. Wherein the reactor 1 is provided with a U-shaped heat exchange tube 5 .

[0027] In the reactor, the outside of the U-shaped tube 5 is a mixed liquid phase such as dimethylamine, sodium methoxide methanol solution, etc. CO bubbles through the sparger to react with dimethylamine to produce DMF; desalted water is used as the cooling medium of the DMF reactor, and it goes through U The tube side of type tube 5 conducts he...

Embodiment 2

[0029] In the reactor, outside the U-shaped tube is a mixed liquid phase such as dimethylamine, sodium methoxide and methanol solution, and CO is bubbled through the sparger to react with dimethylamine to produce DMF; desalted water is used as the cooling medium of the DMF reactor, and it follows a U-shaped The tube side and the liquid phase and gas phase in the reactor conduct heat exchange between the walls, absorb the heat generated by the synthesis reaction, and at the same time increase the temperature of the desalted water; the temperature of the desalted water entering the reactor is 90 ° C, and the temperature of the exiting reactor reaches 94 ° C. The desalinated water is sent to the buffer tank, through the circulation pump at 500m 3 / h flow rate to the desalinated water heat exchanger. The desalinated water goes through the shell side and exchanges heat with the tube side circulating water. After being cooled to 90°C by the circulating water, it is sent to the cooli...

Embodiment 3

[0031] In the reactor, outside the U-shaped tube is a mixed liquid phase such as dimethylamine, sodium methoxide and methanol solution, and CO is bubbled through the sparger to react with dimethylamine to produce DMF; desalted water is used as the cooling medium of the DMF reactor, and it follows a U-shaped The tube side and the liquid phase and gas phase in the reactor conduct heat exchange between the walls, absorb the heat generated by the synthesis reaction, and at the same time increase the temperature of the desalted water; the temperature of the desalted water entering the reactor is 93 ° C, and the temperature of the exiting reactor reaches 98 ° C. The desalinated water is sent to the buffer tank, through the circulation pump at 550m 3 / h flow rate to the desalinated water heat exchanger. The desalted water goes through the shell side, exchanges heat with the tube side circulating water, is cooled to 93°C by the circulating water, and then sent to the cooling medium in...

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Abstract

The invention belongs to the synthesis field for industrial chemicals, and particularly relates to the synthesis of DMF (dimethylformamide), which comprises the following steps: CO and dimethylamine react in a reactor to synthesize DMF in one step and the heat generated in the reactor is taken away through a cooling medium, wherein, the temperature for the cooling medium to enter the reactor is controlled to 90 to 94 DEG C, and the temperature for the cooling medium to come out is controlled to 94 to 98 DEG C. The synthesis avoids that precipitation is separated out from sodium methoxide through crystallization and the inner wall of a U-shaped tube bundle of the reactor is jammed because of scale formation, increases the reaction efficiency, reduces the startup and shutdown frequency of equipment, reduces the repairing and cleaning cost as well as pollutant discharge, and facilitates planned overhaul and maintenance for equipment operation.

Description

(1) Technical field [0001] The invention belongs to the field of synthesis of chemical raw materials, in particular to a synthesis of DMF (dimethylformamide). (2) Background technology [0002] DMF is an important raw material for the production of polyurethane synthetic leather, polyacrylonitrile spinning and medicine. There are 8 kinds of common DMF synthesis process routes in China, and the more common one is the one-step synthesis method of carbon monoxide. The chemical reaction equation is as follows: [0003] CO+NH(CH 3 ) 2 →HCON(CH 3 ) 2 [0004] The method uses sodium methoxide as a catalyst, and has simple technological process, low investment and good product quality. Carbon monoxide as the raw material can be separated and extracted by semi-water gas from the ammonia plant. The source of raw material is wide and the product cost is low. The current leading device for its synthesis reactor is an internal cooling reactor, which has the advantages of uniform d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C233/03C07C231/10
Inventor 汤广斌甘世杰刘灏
Owner HENAN JUNHUA DEV
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