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Preparation method of perfluoroheptanoic acid

A technology of perfluoroheptanoic acid and fluoroheptanoic acid, applied in the preparation of acyl halides, organic chemistry, etc., can solve the problems of high energy consumption, low yield, and heavy pollution, and achieve low energy consumption, high yield, and no pollution Effect

Active Publication Date: 2017-06-13
济南齐氟新材料技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the problems of low yield, high energy consumption and heavy pollution in the preparation of perfluoroheptanoic acid in the above prior art, the present application discloses a perfluoroheptanoic acid with high yield, low energy consumption, no pollution and easy operation. The preparation method of fluoroheptanoic acid

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) In a 500ml reaction kettle, add 100 grams of dodecafluoroheptanol, 100 grams of water, and 0.5 grams of tetrabutylammonium bromide. The temperature was raised to 70°C with stirring, and 66 grams of potassium permanganate was added in batches within 3 hours, and the reaction was continued for 5 hours. Remove the solid by filtration while hot, acidify with 50% sulfuric acid, separate the lower layer, extract the upper aqueous phase with an equal amount of ether, combine the lower layers, rectify and recover the ether, and obtain 86 grams of dodecafluoroheptanoic acid, with a yield of 93%.

[0026] (2) Add the obtained dodecafluoroheptanoic acid into another 500ml reaction kettle, and add 80g of dimethylformamide. 40 g of thionyl chloride was added dropwise with stirring. After the dropwise addition, the temperature was raised to 60° C., and the reaction was kept for 2.5 hours. Rectification obtains dodecafluoroheptanoyl chloride 80 grams, yield 91%,

[0027] (3) Ad...

Embodiment 2

[0030] (1) In a 500ml reaction kettle, add 150 grams of dodecafluoroheptanol, 63 grams of 65% concentrated nitric acid, and 0.3 grams of ferric chloride. The temperature was raised to 125° C. under stirring, and the pressure was 0.23 MPa, and the reaction was continued for 5 hours. Cool down, separate the lower layer for rectification, and obtain 122 grams of product dodecafluoroheptanoic acid, with a yield of 88%.

[0031] (2) Add the obtained dodecafluoroheptanoic acid into another 500ml reaction kettle, and add 95 grams of tetrahydrofuran. 52 g of thionyl chloride were added dropwise with stirring. After the dropwise addition, the temperature was raised to 60° C., and the reaction was kept for 2.5 hours. Rectification obtains dodecafluoroheptanoyl chloride 120 grams, yield 93%,

[0032] (3) Add the obtained above product into a 250ml fluorination reaction kettle, stir and heat up to 60°C, and feed 25% fluorine gas from the bottom of the material at a rate of 250ml / min. ...

Embodiment 3

[0035] (1) Take 115 grams of dodecafluoroheptanoic acid obtained in Reference Example 2, add 72 grams of diethyl ether, keep the temperature below 30°C, add 50 grams of thionyl chloride dropwise, after the addition is complete, stir overnight at room temperature. Distillation to remove ether and excess thionyl chloride,

[0036] (2) The obtained product is put into a fluorination reaction kettle at a temperature of 50° C., and 25% fluorine gas is introduced from the bottom of the reaction kettle at a rate of 200 ml / min. Continue to ventilate for 25 hours, take samples and test, and the raw materials are completely reacted. Receiving 112 grams, yield 96%,

[0037] The temperature of the fluorinated product was raised to 50° C., 9 g of deionized water was added, and the stirring was continued for 3 hours. Negative pressure rectification gave 89 grams of product with a purity of 96.2%. The comprehensive yield is 75.6%.

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Abstract

The invention relates to the technical field of fluorochemical preparation, particularly a preparation method of perfluoroheptanoic acid. The method comprises the following steps: oxidizing dodecafluoroheptanol to obtain dodecafluoroheptanoic acid, carrying out reaction on the dodecafluoroheptanoic acid and thionyl chloride to obtain dodecafluoroheptanoyl chloride, carrying out fluorination on the dodecafluoroheptanoyl chloride to obtain perfluoroheptanoyl chloride, and hydrolyzing to obtain the perfluoroheptanoic acid. The technical process of preparing perfluoroheptanoic acid from dodecafluoroheptanol has the advantages of low energy consumption, no pollution and high yield (up to 75% or above), is easy to operate, and has higher competitive edges than the existing perfluoroheptanoic acid production technique.

Description

technical field [0001] The invention relates to the technical field of preparation of fluorine-containing compounds, in particular to a preparation method of perfluoroheptanoic acid. Background technique [0002] Perfluoroheptanoic acid is a very important new fluorine-containing material, which is mainly used in emulsifiers and dispersants of fluoropolymers, as well as leveling agents for inks and coatings. At present, perfluorooctanoic acid (PFOA) is mainly used as fluorinated emulsifier, but because of its bioaccumulation and refractory properties, it has been gradually banned in Europe, America and other places. As its substitute, perfluoroheptanoic acid has broad application prospects. [0003] Generally, the preparation method similar to perfluoroheptanoic acid adopts electrolytic fluorination method. For example, CN 104910302A discloses that after purification of perfluoroheptanoyl fluoride prepared by electrolytic fluorination method, the perfluoroheptanoic acid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/04C07C53/21
Inventor 张立亭
Owner 济南齐氟新材料技术有限公司
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