Comprehensive utilization method of solvent and by-product in preparation of HFPO by oxygen oxidation method

A technology for oxygen oxidation and by-products, applied in chemical instruments and methods, amino compound preparation, organic compound preparation, etc., can solve the problems of unavailable systems, equipment corrosion, and inability to obtain high-purity solvents, etc., to reduce equipment costs and The cost of waste liquid treatment, avoiding the accumulation of by-products, and the effect of simple process route

Active Publication Date: 2020-07-24
SHANDONG DONGYUE WEILAI HYDROGEN ENERGY MATERIAL CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Using different solvent systems will generate different types of by-products, whose physical properties are very different, and the same treatment method cannot be applied to all systems
[0005] Patent CN109678700A discloses a method for the comprehensive utilization of HFPO by-products, using ultraviolet light irradiation can eliminate peroxides in the by-products in the system, but cannot obtain high-purity Solvent, the obtained carboxylic acid solution has a high acidity, which seriously corrodes the equipment, and carbonyl fluoride is a highly toxic, strong oxidizing, and strong corrosive chemical, which will have a greater safety risk
In addition, the patent does not describe the mentioned solvent in detail, and only expresses it as a fluorinated solvent. In fact, the perfluorinated saturated hydrocarbon and ether system is used without peroxide formation.
[0006] Aiming at the problems that the above-mentioned process has relatively high safety risks, by-products are highly toxic and acidic, and cannot be applied to systems of perfluorinated saturated hydrocarbons and ethers, the present invention provides a simple and mild process, which is safe, Environmental protection and economic benefits are more obvious

Method used

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  • Comprehensive utilization method of solvent and by-product in preparation of HFPO by oxygen oxidation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Oxygen oxidation method prepares the comprehensive utilization method of solvent and by-product in HFPO, and the steps are as follows:

[0050] (1) Separation: Oxygen is used as oxidant, hexafluoropropylene is used as raw material, HFPO is prepared by oxygen oxidation method, DY-01 is used as solvent, and after 50 kettles of intermittent reaction, the fluorocarbon to be purified containing acyl fluoride by-products is taken out Solvent, the by-product was found to be mainly CF 3 O(CF(CF 3 ) CF 2 O) 2 CF 2 COF and CF 3 CF 2 O(CF 2 CF 2 O) 2 CF(CF 3 ) COF, the total content is 26wt%.

[0051] (2) Alcohol washing: mix the fluorocarbon solvent to be purified with absolute ethanol in a volume ratio of 1:1, figure 1 Mix in the washing device shown, turn on the stirring, and pass in circulating water to control the temperature of the washing tank below 40°C. After stirring for 6 hours, start to stand still. After standing for 2 hours, the liquid separation is comple...

Embodiment 2

[0060] (1) Separation: Oxygen is used as oxidant, hexafluoropropylene is used as raw material, and HFPO is prepared by oxygen oxidation method, and DY-02 is used as solvent. After 30 kettles of intermittent reaction, the fluorocarbon to be purified containing acyl fluoride by-products is taken out Solvent, the by-product was found to be mainly CF 3 CF 2 CF 2 O(CF 2 CF 2 O) 2 CF(CF 3 ) COF, the total content is 19wt%.

[0061] (2) Alcohol washing: the fluorocarbon solvent to be purified and absolute ethanol in a volume ratio of 2:1, in figure 1 Mix in the washing device shown, turn on the stirring, and pass in circulating water to control the temperature of the washing tank below 40°C. After stirring for 6 hours, start to stand still. After standing for 2 hours, the liquid separation is completed, and the fluorocarbon solvent after alcohol washing and Hydrogen fluoride ethanol solution;

[0062] The hydrogen fluoride content in the hydrogen fluoride ethanol solution is ...

Embodiment 3

[0070] (1) Separation: Oxygen is used as oxidant, hexafluoropropylene is used as raw material, HFPO is prepared by oxygen oxidation method, DY-03 is used as solvent, and after 30 kettles of intermittent reaction, the fluorocarbon to be purified containing acyl fluoride by-products is taken out Solvent, the by-product was found to be mainly CF 3 OCF 2 CF 2 OCF (CF 3 ) CF 2 OCF (CF 3 ) COF, the total content is 20wt%.

[0071] (2) Alcohol washing: mix the fluorocarbon solvent to be purified with anhydrous propanol at a volume ratio of 0.5:1, in figure 1 Mix in the washing device shown, turn on the stirring, and pass in circulating water to control the temperature of the washing tank below 40°C. After stirring for 5 hours, start to stand still. After standing for 2 hours, the liquid separation is completed, and the fluorocarbon solvent after alcohol washing and Hydrogen fluoride propanol solution;

[0072] The hydrogen fluoride content in the hydrogen fluoride-propanol sol...

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Abstract

The invention relates to the technical field of fluorine chemical industry, in particular to a method for comprehensive utilization of a solvent and by-products in preparation of HFPO through an oxygen oxidation process. According to the comprehensive utilization method, a to-be-purified fluorocarbon solvent containing acyl fluoride by-products generated in the preparation of the HFPO through theoxygen oxidation process is sequentially subjected to separation, alcohol washing, rectification, alkali washing and drying to obtain the fluorocarbon solvent with a purity of 99wt% or above. The method is simple in process route; an important fluorination reagent in the fluorine chemical industry can be obtained; the fluorocarbon solvent can be continuously used in the reaction for preparing HFPOafter being purified; and more importantly, the byproducts are converted into stable and neutral esters rather than carboxylic acids, and can be applied or converted in a wider scope, so the purposeof comprehensive utilization of all the byproducts is achieved.

Description

technical field [0001] The invention relates to the technical field of fluorine chemical industry, in particular to a method for comprehensive utilization of solvents and by-products in the preparation of HFPO by an oxygen oxidation method. Background technique [0002] Oxygen oxidation method to prepare hexafluoropropylene oxide (HFPO) is the most common process for preparing hexafluoropropylene oxide by oxidizing hexafluoropropylene in a fluorocarbon solvent with oxygen as the oxidant. [0003] Commonly used solvents for preparing hexafluoropropylene oxide by oxygen oxidation are chlorofluorocarbons (such as: CFC-113, etc.) and perfluorocarbons or ethers, and perfluorocarbons and ethers also contain perfluorocarbons. Saturated hydrocarbons or ethers and saturated hydrocarbons or ethers. [0004] The production process of producing hexafluoropropylene oxide by oxygen oxidation method is divided into batch method and continuous method. The fluorocarbon solvent in the two me...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D303/48C07D301/06C07D301/32C07C51/64C07C59/135C07C67/14C07C67/54C07C69/708C07C209/00C07C211/05
CPCC07C51/64C07C67/14C07C67/54C07C209/00C07D301/06C07D301/32C07D303/48C07C59/135C07C69/708C07C211/05
Inventor 宋昌平崔永文王克珊郑魁星刘丰宇史翔王振华赵彬冯威张永明
Owner SHANDONG DONGYUE WEILAI HYDROGEN ENERGY MATERIAL CO LTD
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