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Preparation method of perfluoro caprylic acid

A technology of perfluorooctanoic acid and sodium perfluorooctanoate, which is applied in the preparation of acyl halides and organic chemistry, and can solve the problems of low linear chain content, numerous operation steps, and low yields

Inactive Publication Date: 2007-07-18
SHANDONG HUAXIA SHENZHOU NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The chemical synthesis method is complex, with many operation steps and huge investment; the electrolysis method is simple, requires less investment, and can obtain a very versatile by-product: fluorocarbon
But also exist yield is not high, the deficiencies such as the linear chain content of gained product is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Example 1: The weight of the electrolyte is 85KG, 18L of 30% liquid caustic soda is added, and 100L of water is added, while stirring continuously. After standing still for 45 minutes, the fluorocarbon in the lower layer and the sodium fluoride in the middle layer were separated. Acidify the perfluorooctanoic acid sodium salt solution, add 17L of 98% concentrated sulfuric acid, stir at a rate of less than 20 rpm for 10 minutes, and stand for 40 to 50 minutes to obtain a yellow-brown precipitate (perfluorooctanoic acid containing impurities), which is rectified Finally, 14.2KG perfluorooctanoic acid was obtained. White crystals, the detected straight chain content is 91%.

Embodiment 2～4

[0032] Embodiment 2~4: operation steps are all the same as embodiment 1. The difference is that the amount of electrolyte and the amount of adding liquid caustic soda, sulfuric acid, and water have changed, and the specific amounts are as follows:

[0033] serial number

[0034] Comparative analysis:

Embodiment 2

[0035] Embodiment 2, embodiment 3 add the amount of liquid caustic soda, sulfuric acid, water according to the ratio, after rectifying, all obtain the product that appearance is white crystal, and straight chain content is 90.1% and 91.3%. Example 2 output is 14.4KG; Example 3 output is 15.4KG. Embodiment 4 did not add in proportion when carrying out post-treatment alkali hydrolysis, and only collected the product 2.3KG that appearance is white crystal when rectifying. The rest are yellow or pale yellow crystals.

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Abstract

This invention relates to a perfluorooctanoic acid preparation method, belong to fluorine chemicals technology field. It takes electrolysis fluorine hydride and octanoyl chlorine electrolyte as materials, the main ingredients is perfluorooctanoic acid fluoride. First use liquid alkali to alkaline hydrolyze electrolyte containing perfluorooctanoic acid fluorine, isolate part of sodium fluoride and the main byproduct of fluorocarbon, obtain perfluorooctanoic acid solution of sodium, then use sulfate for acidification, gain perfluorooctanoic acid. Through organic and water phase separation to remove some of the residual hydrogen fluoride, the organic phase by means of distillation purification, to obtain perfluorooctanoic acid products. The invention can improve the yield of perfluorooctanoic acid products while enhancing straight chain content.

Description

technical field [0001] The invention relates to a preparation method of perfluorooctanoic acid, which belongs to the technical field of fluorine chemical industry. Background technique [0002] The ammonium or sodium salt of perfluorooctanoic acid is an anionic surfactant with excellent performance, an efficient metal cleaning agent, and a synthetic fluororesin (such as dispersed polytetrafluoroethylene resin, polyvinylidene fluoride resin, polyperfluoroethylene propylene resin, etc.) Resin) and fluororubber are indispensable and irreplaceable raw materials. Perfluorooctanoic acid is also used as an intermediate in the synthesis of water-repellent and oil-repellent leather, paper, and fiber treatment agents. Perfluorooctanoic acid is a fine fluorinated product with high added value and a wide range of uses. [0003] At present, the methods for producing PFOA mainly include synthesis and electrolysis. These two methods are to obtain perfluorooctanoyl fluoride through the p...

Claims

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Application Information

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IPC IPC(8): C07C51/04C07C53/21
Inventor 薛念强李鑫王汉利高洪光
Owner SHANDONG HUAXIA SHENZHOU NEW MATERIAL
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