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Preparation method of brominated perfluoroalkane

The technology of iodo perfluoroalkane and perfluoroalkane is applied in the field of production of fluorine-containing fine chemicals, can solve the problems of incapable of continuous industrialized production, high reaction temperature, and high equipment requirements, and achieves high production efficiency, safe equipment operation, and low cost. The effect of energy consumption

Pending Publication Date: 2021-02-09
SHANDONG ZHONGSHAN PHOTOELECTRIC MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] In view of the disadvantages of low product purity, high reaction temperature, high equipment requirements, complicated operation, and incapable of industrial continuous production in the production methods of brominated perfluoroalkanes in the prior art, the present invention provides a kind of industrialized brominated perfluoroalkanes Continuous production method to solve the above problems

Method used

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  • Preparation method of brominated perfluoroalkane
  • Preparation method of brominated perfluoroalkane
  • Preparation method of brominated perfluoroalkane

Examples

Experimental program
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Effect test

Embodiment 1

[0047] A preparation method of brominated perfluorooctane, the specific steps are as follows:

[0048] (1) Heat the quartz reaction tube to keep the temperature in the tube between 70°C, turn on the light source of the photochemical reactor, and set the wavelength to 254nm;

[0049] (2) Turn on the sampling pump, adjust the flow rate of perfluoroiodooctane to 5mL / min, and the flow rate of bromine to 1.5mL / min, and enter the photochemical reactor for continuous reaction;

[0050] (3) The reaction mixture flows into the phase separation tank for preliminary separation, bromine and the iodine bromide generated are layered with the product, and the lower layer is the bromine and iodine bromide layer. After every 36 hours, the bromine is released once in the recovery tank , while releasing the crude product of the target product in the upper layer to flow into the washing tank;

[0051] (4) the crude product of the target product flowing into the washing tank is treated with 30% s...

Embodiment 2

[0058] A preparation method of brominated perfluorohexane, the specific steps are as follows:

[0059] (1) Heat the quartz reaction tube to keep the temperature in the tube between 60°C, turn on the light source of the photochemical reactor, and set the wavelength to 254nm;

[0060] (2) Turn on the injection pump, adjust the flow rate of perfluoroiodohexane to 5mL / min, and the flow rate of bromine to 1.5mL / min, and enter the photochemical reactor for continuous reaction;

[0061] (3) The reaction mixture flows into the phase separation tank for preliminary separation, bromine and the iodine bromide generated are layered with the product, and the lower layer is the bromine and iodine bromide layer. After every 36 hours, the bromine is released once in the recovery tank , while releasing the crude product of the target product in the upper layer to flow into the washing tank;

[0062] (4) the crude product of the target product flowing into the washing tank is treated with 30% ...

Embodiment 3

[0070] A preparation method of bromoperfluorodecane, the specific steps are as follows:

[0071] (1) Heat the quartz reaction tube to keep the temperature in the tube between 70°C, turn on the light source of the photochemical reactor, and set the wavelength to 254nm;

[0072] (2) Turn on the injection pump, adjust the flow rate of perfluoroiododecane to 5mL / min, and the flow rate of bromine to 1.5mL / min, and enter the photochemical reactor for continuous reaction;

[0073] (3) The reaction mixture flows into the phase separation tank for preliminary separation, bromine and the iodine bromide generated are layered with the product, and the lower layer is the bromine and iodine bromide layer. After every 36 hours, the bromine is released once in the recovery tank , while releasing the crude product of the target product in the upper layer to flow into the washing tank;

[0074] (4) the crude product of the target product flowing into the washing tank is treated with 30% sodium...

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Abstract

The invention relates to a preparation method of brominated perfluoroalkane, and belongs to the technical field of fluorine-containing fine chemical production. Perfluoroalkyl iodide and bromine are used as raw materials, a photochemical reaction is performed under a normal pressure condition to synthesize a target product, then a reaction mixture is treated with alkali liquor, and finally, rectification and purification are performed to obtain the target product. The method has the advantages of mild preparation process conditions, simple equipment, high key raw material conversion rate, hightarget product selectivity, and easy realization of industrial continuous production.

Description

technical field [0001] The invention belongs to the technical field of production of fluorine-containing fine chemicals, and in particular relates to a preparation method of brominated perfluoroalkane. Background technique [0002] With the development of synthesis and application of fluorine-containing compounds, brominated perfluoroalkanes are more and more widely used in the field of medicine, and have important uses in artificial blood, contrast agents, tumor treatment drugs, assisted pulmonary cavity ventilation, and ophthalmic surgical instruments. . [0003] In the prior art, the preparation methods of brominated perfluoroalkanes mainly include the following: [0004] (1) Decarboxylation method [0005] The patent US2678953 discloses a reaction between silver salt of polyfluorocarboxylic acid and bromine to prepare brominated perfluoroalkanes, but the raw materials used in this method are difficult to obtain, expensive, and have no practical industrial application v...

Claims

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Application Information

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IPC IPC(8): C07C17/20C07C17/38C07C17/383C07C19/14
CPCC07C17/204C07C17/38C07C17/383C07C19/14
Inventor 方治文王毅刘晓贾裕康
Owner SHANDONG ZHONGSHAN PHOTOELECTRIC MATERIAL CO LTD
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