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Preparation appaPratus for perfluoroisobutyryl fluoride

A technology for the preparation of perfluoroisobutyryl, which is applied in the field of fluorine chemistry, can solve problems such as difficult industrialization, low output, and complicated separation procedures, and achieve the effects of facilitating industrialization, increasing yield, and simple design

Inactive Publication Date: 2019-11-12
TIANJIN CHANGLU CHEM NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] There are many methods for preparing perfluorobutyryl fluoride, such as electrochemical method or chemical synthesis method. Among them, the reaction kettle liquid phase method is a commonly used compound synthesis method. Its advantage is that it is simple to operate, but it is reacted due to the one-pot method of feeding materials. Therefore, the output is often low
For the preparation of perfluoroisobutyryl fluoride by one-pot reaction, the yield is low, the separation process is complicated and difficult to industrialize and other defects, so there is an urgent need for a simple and convenient preparation device for perfluoroisobutyryl fluoride

Method used

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  • Preparation appaPratus for perfluoroisobutyryl fluoride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1: The gas feedstock hexafluoropropylene and carbonyl fluoride are fed into the gas feed port according to the amount of components in the reactor. The molar ratio is 1:1.5. The addition of a small amount of carbonyl fluoride is beneficial to the reaction. Liquid feed The liquid solvent mixed with the catalyst is DMF, and the catalyst is KF; the reaction temperature of the reactor is set to 75-85°C. The concentration of the basic fluoride in DMF is 0.08 mol / L, and perfluoroisobutyryl fluoride is prepared by the above-mentioned preparation device. After 12 hours of continuous reaction, the yield of the product perfluoroisobutyryl fluoride reaches more than 96%. Due to the high boiling point of DMF, there is only a small amount of product and raw material gas overflow at the reaction temperature, while perfluoroisobutyryl fluoride and raw material gas hexafluoropropylene and carbonyl fluoride pass through the valve as the reaction progresses Control the overflow fr...

Embodiment 2

[0018] Example 2: Example 2 is the same as Example 1, except that the initial feed molar concentration of the feed gas is 1:1. The catalyst is CsF with a molar concentration of 0.05 mol / L.

Embodiment 3

[0019] Example 3: Example 3 is the same as Example 1, except that the initial feed molar concentration of the raw gas is 1:2. The catalyst is NaF with a molar concentration of 0.1 mol / L.

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Abstract

The invention particularly relates to a preparation apparatus for perfluoroisobutyryl fluoride, belonging to the field of fluorine chemistry. The preparation apparatus for perfluoroisobutyryl fluoridecomprises a reaction kettle and a cooling reflux device, wherein the reaction kettle comprises a kettle body, a gas feed inlet, a liquid feed inlet and an exhaust port all arranged in the top of thekettle body, and a waste discharging port arranged in the bottom of the kettle body; the exhaust port communicates with the cooling reflux device through a valve; and the cooling reflux device includes a shell, a coiled condensation pipe arranged in the shell, a feed gas inlet formed in one side of the shell and connected with the exhaust port, a feed gas outlet formed in the other side of the shell, and a product outlet formed in the bottom of the shell. The preparation apparatus for perfluoroisobutyryl fluoride provided by the invention utilizes the kinetic balance of a reaction to continuously remove a product, so the concentration of raw materials is maintained high at all times while the concentration of the product is maintained low, and the reaction is carried out along forward direction, thereby increasing the yield of the product; and the preparation apparatus is simple in design and is beneficial for industrialization.

Description

Technical field [0001] The invention belongs to the field of fluorine chemistry, and specifically relates to a preparation device of perfluoroisobutyryl fluoride. Background technique [0002] Perfluoroisobutyryl fluoride is an important fluorine-containing compound with a wide range of applications. It can be used in cleaning agents, etching agents, pesticide intermediates, fluorine-containing material monomers, etc. in the electronics industry. [0003] There are many methods for preparing perfluorobutyryl fluoride, such as electrochemical method or chemical synthesis method. Among them, the reactor liquid phase method is a commonly used compound synthesis method, which has the advantage of simple operation, but due to the one-pot method for feeding and reacting, So the output is often low. In view of the shortcomings of low yield, complicated separation process and difficulty in industrialization when preparing perfluoroisobutyryl fluoride by one-pot reaction, a simple and conv...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J19/00C07C51/58C07C53/50
CPCB01J19/002C07C51/58C07C53/50
Inventor 汤峤永姚素梅贺光瑞
Owner TIANJIN CHANGLU CHEM NEW MATERIAL CO LTD