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Treatment method of perfluoroalkyl acyl fluoride waste

A technology of perfluoroalkyl acyl fluoride and a treatment method, which is applied in the field of perfluoroalkyl acyl fluoride waste treatment, can solve the problems of consuming reaction materials, large amount of materials, unfavorable commercialization and the like, and achieves simple operation and economical cost. , the effect of reducing the discharge of waste

Active Publication Date: 2013-05-08
ZHEJIANG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Large consumption of expensive reaction materials and considerable amounts of material produced hinder the commercialization of the method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] This embodiment discloses a method for treating perfluoroalkyl fluoride waste, and the specific steps are as follows:

[0045] (1) Introduce 50ml of perfluoroalkyl fluoride waste into a 500ml jacketed reaction kettle, through which condensed water at a temperature of 5°C is passed through the jacket. After the temperature in the reactor and the temperature of the condensed water reach equilibrium , the configured 1mol / L K 2 CO 3 About 150ml of the solution was slowly added dropwise to the perfluoroalkyl fluoride waste while stirring continuously. A large amount of heat is released during this process, and the temperature in the reactor needs to be kept below 25°C. After the dropwise addition of the alkali solution is completed, the stirring is continued for 5 hours to ensure complete hydrolysis of the perfluoroalkyl acid fluoride and complete acid-base neutralization reaction. Then stop stirring and let it stand for 2h to separate the water phase and the oil phase. ...

Embodiment 2

[0049] This embodiment discloses a method for treating perfluoroalkyl fluoride waste, and the specific steps are as follows:

[0050] (1) Introduce 50ml of perfluoroalkyl fluoride waste into a 500ml jacketed reaction kettle, through which condensed water at a temperature of 5°C is passed through the jacket. After the temperature in the reactor and the temperature of the condensed water reach equilibrium , the configured 1mol / L Na 2 CO 3 About 150ml of the solution was slowly added dropwise to the perfluoroalkyl fluoride waste while stirring continuously. A large amount of heat is released during this process, and the temperature in the reactor needs to be kept below 10°C. At the same time, due to the low solubility of NaF in water (4.06g / 100g water (20°C), a large amount of NaF precipitated during the dropping process. After the dropwise addition of the alkali solution is completed, the stirring is continued for 5 hours to ensure complete hydrolysis of the perfluoroalkyl ac...

Embodiment 3

[0054] This embodiment discloses a method for treating perfluoroalkyl fluoride waste, and the specific steps are as follows:

[0055] (1) Introduce 25ml of perfluoroalkyl fluoride waste into a 500ml jacketed reaction kettle, and pass through the jacket with condensed water at a temperature of 5°C. After the temperature in the reactor and the temperature of the condensed water reach equilibrium , the configured 1mol / L KHCO 3 About 300ml of the solution was slowly added dropwise to the perfluoroalkyl fluoride waste while stirring continuously. A large amount of heat is released during this process, and the temperature in the reactor needs to be kept below 25°C. After the dropwise addition of the alkali solution is completed, the stirring is continued for 5 hours to ensure complete hydrolysis of the perfluoroalkyl acid fluoride and complete acid-base neutralization reaction. Then stop stirring and let it stand for 2h to separate the water phase and the oil phase. Then take out...

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PUM

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Abstract

The invention discloses a treatment method of perfluoroalkyl acyl fluoride waste. The method comprises the following steps of: first, adding aqueous alkali to the perfluoroalkyl acyl fluoride waste, adjusting the pH value to 7-8, standing and separating to obtain a water phase and an oil phase; then, separating and purifying the water phase to obtain perfluorocarboxylate; and finally, separating and purifying the oil phase to obtain inertial fluorocarbon. The perfluoroalkyl acyl fluoride waste is treated in grades in the following steps of: adding aqueous alkali to separate the perfluoroalkyl acyl fluoride waste into the water and oil phases, and respectively separating and purifying the water and oil phases; and obtaining high purity perfluorocarboxylate after separation and purification of the water phase and obtaining high purity inertial fluorocarbon after separation and purification of the oil phase. The treatment condition is mild and the treatment effect is good.

Description

technical field [0001] The invention relates to the technical field of waste treatment produced in the electrochemical fluorination production process, in particular to a treatment method for perfluoroalkyl fluoride waste. Background technique [0002] At present, the Simons method is mostly used for the production of acyl fluoride products. First, perfluorocyclohexyl fluoride is produced by electrochemical fluorination of benzoyl chloride, and then the crude product of acyl fluoride is separated by distillation and purification. Some low-boiling perfluorinated compounds (PFCs) separated by rectification have a boiling point between 40 and 80 °C. That is, perfluoroalkyl fluoride waste. Perfluoroalkyl fluoride waste contains part of perfluorocyclohexyl fluoride, and other by-products, including other configurations of perfluoroacyl fluoride and inert fluorocarbons (perfluorocarbons and perfluorocyclic ethers mixture), etc. [0003] The structure of perfluoroalkyl fluoride ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/04C07C51/42C07C17/395C07C17/38
Inventor 鲍宗必楼军任其龙杨亦文邢华斌苏宝根
Owner ZHEJIANG UNIV
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