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Rectification device and process for purifying ethyl difluoroacetate efficiently

A high-efficiency technology of ethyl difluoroacetate, applied in the field of high-efficiency purification of ethyl difluoroacetate rectification equipment, can solve the problems of lack of preparation research on fluorine-containing compounds, unsuitable for industrial applications, waste of raw materials and purity, and achieve low operating costs , Low equipment cost, simple process effect

Inactive Publication Date: 2013-02-13
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The extraction method needs to introduce third-party reagents, which causes waste of raw materials and the problem of low purity; membrane separation technology is a relatively new technology in recent years, and the efficient purification of fluorine-containing compounds such as ethyl difluoroacetate lacks the corresponding membrane technology. Preparative studies; chromatography is suitable for laboratory research, not for industrial applications

Method used

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  • Rectification device and process for purifying ethyl difluoroacetate efficiently

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Product feed content 90%:

[0018] Feed material at bubble point of light removal tower 1, processing capacity: 30kg / hr, the fourth heat exchanger 10 turns on low-pressure steam, when condensate distills out from the top of light removal tower 1, the top of the tower starts to fully reflux, and when the temperature at the top of the tower reaches At 45-50°C, the intermediates are mined, and the second feed pump 5 is started to feed the finished product tower 2. The sixth heat exchanger 12 turns on the low-pressure steam, and when condensate distills out from the top of the finished product tower 2, the top of the tower begins to reflux, and when the temperature at the top of the tower reaches 98-99°C, the finished product ethyl difluoroacetate is collected, with a content of 99.97% . Only key control points are listed, and other conditions are detailed in the specific implementation section, the same below.

Embodiment 2

[0020] Product feed content 96.67%:

[0021] Feed material at bubble point of light removal tower 1, processing capacity: 50kg / hr, the fourth heat exchanger 10 turns on low-pressure steam, when condensate distills out from the top of light removal tower 1, the top of the tower starts to fully reflux, and when the temperature at the top of the tower reaches At 45-50°C, the intermediates are mined, and the second feed pump 5 is started to feed the finished product tower 2. The sixth heat exchanger 12 turns on the low-pressure steam, and when condensate distills out from the top of the finished product tower 2, the top of the tower begins to reflux, and when the temperature at the top of the tower reaches 98-99°C, the finished product ethyl difluoroacetate is collected, with a content of 99.98% .

Embodiment 3

[0023] Product feed content 95%:

[0024]Feed material at bubble point of light removal tower 1, processing capacity: 70kg / hr, the fourth heat exchanger 10 turns on low-pressure steam, when condensate distills out from the top of light removal tower 1, the top of the tower starts to fully reflux, and when the temperature at the top of the tower reaches At 45-50°C, the intermediates are mined, and the second feed pump 5 is started to feed the finished product tower 2. The sixth heat exchanger 12 turns on the low-pressure steam, and when condensate distills out from the top of the finished product tower 2, the top of the tower begins to reflux, and when the temperature at the top of the tower reaches 98-99°C, the finished product ethyl difluoroacetate is collected, with a content of 99.95% .

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Abstract

The invention discloses a rectification device and a process for purifying ethyl difluoroacetate efficiently. The device comprises a light component removal tower, a finished product tower, an intermediate product recovery tower, a first charging pump, a second charging pump, a third charging pump, a first heat exchanger, a second heat exchanger, a third heat exchanger, a fourth heat exchanger, a fifth heat exchanger, a sixth heat exchanger, a seventh heat exchanger, an eighth heat exchanger, a first storage tank, a second storage tank, a third storage tank, a fourth storage tank, a fifth storage tank and a sixth storage tank. Bubble point charging is conducted in the light component removal tower, the a fourth heat exchanger starts low-pressure steam, total reflux is conducted at the top of the tower, intermediate bodies are collected when the temperature of the top of the tower reaches 45-50 DEG C, then the second charging pump is started, and charging is conducted in the finished product tower. The sixth heat exchanger starts the low-pressure steam, total reflux is conducted at the top of the tower when condensate is distilled out of the top of the finished product tower, finished products of the ethyl difluoroacetate are collected when the temperature of the top of the tower reaches 98-99 DEG C, and the content is in a range of 99.95-99.98%. By the aid of the device and the process, high-purity ethyl difluoroacetate products can be obtained, the process is simple, and industrial production requirements can be met.

Description

technical field [0001] The invention relates to a rectification device and method for efficiently purifying ethyl difluoroacetate. Background technique [0002] The fluorine chemical industry is a sub-industry of the chemical industry. Due to the variety of products, excellent performance and wide application fields, this industry has become an important industry with rapid development in recent years. Due to the problems of incomplete conversion and many side reactions in the organic synthesis reaction, there are many by-products in the product, and the purity is not high. How to obtain high-purity fluoride products is a problem faced by many enterprises. The separation methods of organic mixtures mainly include rectification, extraction, membrane separation technology, and chromatography. The extraction method needs to introduce third-party reagents, which causes waste of raw materials and the problem of low purity; membrane separation technology is a relatively new tec...

Claims

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Application Information

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IPC IPC(8): B01D3/14
Inventor 朱明乔胡红定吴晓晋王树华安立梅雷志刚
Owner ZHEJIANG UNIV
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