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Preparation process of perfluoroheptanoic acid

A technology of perfluoroheptanoic acid and preparation process, which is applied in the preparation of carboxylate, the preparation of organic compounds, the preparation of acyl halides, etc., can solve the problems of low product yield, heavy pollution, large energy consumption, etc., and achieve high yield , low energy consumption, easy to operate

Pending Publication Date: 2021-02-12
JIANGXI GUOHUA IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In view of the problems existing in the prior art, the purpose of the present invention is to provide a preparation process of perfluoroheptanoic acid, which solves the problem that the existing preparation method of perfluoroheptanoic acid adopts electrolytic fluorination method, and obtains perfluoroheptanoic acid through transformation Acid products or perfluoroheptanoate products, this method has obvious deficiencies, the product yield is too low, only 10-20%, high energy consumption, heavy pollution, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A preparation process for perfluoroheptanoic acid, comprising the following steps:

[0027] Step 1, oxidation: add potassium permanganate, organic weak acid solution and quaternary ammonium salt catalyst in the reaction vessel, the quality of organic weak acid solution is 1 times of potassium permanganate quality, the molar number of quaternary ammonium salt catalyst is permanganate 8% of potassium moles, in the reaction vessel, slowly drip into dodecafluoroheptanol, the mol ratio of potassium permanganate and dodecafluoroheptanol is 5: 3, after dropping, control reaction temperature at 70 ℃, After reacting for another 1 hour, the reaction solution was filtered with suction, after the filtrate was acidified, the acidified liquid was extracted with an extractant ketone, the organic phase was separated, and the organic phase was distilled to collect a fraction at 192°C to obtain dodecafluoroheptanoic acid;

[0028] Oxidation of dodecafluoroheptanol gives dodecafluorohepta...

Embodiment 2

[0039] A preparation process for perfluoroheptanoic acid, comprising the following steps:

[0040] Step 1, oxidation: add potassium permanganate, organic weak acid solution and quaternary ammonium salt catalyst in reaction vessel, the quality of organic weak acid solution is 1.5 times of potassium permanganate quality, and the molar number of quaternary ammonium salt catalyst is permanganate 10% of the moles of potassium, slowly drop dodecafluoroheptanol into the reaction vessel, the molar ratio of potassium permanganate and dodecafluoroheptanol is 5:3, after the dropwise addition, control the reaction temperature at 80°C, After reacting for another 0.75 hours, the reaction solution was suction-filtered, and after the filtrate was acidified, the acidified liquid was extracted with an extractant ketone, the organic phase was separated, and the organic phase was distilled to collect fractions at 192°C to obtain dodecafluoroheptanoic acid;

[0041] Oxidation of dodecafluoroheptan...

Embodiment 3

[0053] A preparation process for perfluoroheptanoic acid, comprising the following steps:

[0054] Step 1, oxidation: add potassium permanganate, organic weak acid solution and quaternary ammonium salt catalyst in the reaction vessel, the quality of organic weak acid solution is 2 times of potassium permanganate quality, the molar number of quaternary ammonium salt catalyst is permanganate 12% of the moles of potassium, in the reaction vessel, slowly drip dodecafluoroheptanol, the mol ratio of potassium permanganate and dodecafluoroheptanol is 5:3, after the dropwise addition, control the reaction temperature at 85°C, After reacting for another 0.5 hour, the reaction solution was filtered with suction, after the filtrate was acidified, the acidified liquid was extracted with an extractant ketone, the organic phase was separated, and the organic phase was distilled to collect a fraction at 192°C to obtain dodecafluoroheptanoic acid;

[0055] Oxidation of dodecafluoroheptanol gi...

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Abstract

The invention belongs to the field of fluorine-containing compound preparation, and discloses a perfluoroheptanoic acid preparation process, which comprises: 1, oxidation: adding potassium permanganate, an organic weak acid solution and a quaternary ammonium salt catalyst to a reaction container, slowly adding dodecafluoroheptanol to the reaction container in a dropwise manner, controlling the reaction temperature at 70-85 DEG C after the dropwise addition is completed, carrying out suction filtration on reaction liquid after reacting for 0.5-1 hour, acidifying filtrate, extracting the acidified liquid with an extractant ketone, separating out an organic phase, distilling the organic phase, and collecting 192 DEG C fraction to obtain dodecafluoroheptanoic acid. The application field of thedodecafluoroheptanol is limited, and the use of the dodecafluoroheptanol is greatly limited. The perfluoroheptanoic acid is prepared from the dodecafluoroheptanol as a raw material through oxidation,chlorination, fluorination, hydrolysis and other reactions, the process has wider application prospects, the technological process for preparing the perfluoroheptanoic acid from the dodecafluoroheptanol is low in energy consumption, free of pollution, easy to operate and high in yield, the comprehensive yield can reach 75% or above, and the process has stronger competitive advantages.

Description

technical field [0001] The invention relates to the technical field of preparation of fluorine-containing compounds, in particular to a preparation process 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] The existing preparation method of perfluoroheptanoic acid adopts the electrolytic fluorination method to obtain perfluoroheptanoic acid products or perfluoroheptanoic acid salt products through transformation. This method has obvious shortcomings, and the product yield is too ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C53/21C07C51/04
CPCC07C51/04C07C51/58C07C51/60C07C51/16C07C53/21C07C53/50
Inventor 陈红斌祝金玲
Owner JIANGXI GUOHUA IND CO LTD
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