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Perfluoropolyether carboxylic acid with low HF content and preparation method thereof

A technology of perfluoropolyether carboxylic acid and perfluorocarboxylic acid, applied in the field of fluorine chemical industry, can solve problems such as affecting the quality of perfluoropolyether carboxylic acid, and achieve the effect of reducing HF and improving efficiency

Pending Publication Date: 2020-05-08
TIANJIN CHANGLU CHEM NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Perfluoropolyether carboxylic acid is usually prepared by reacting perfluoroacyl fluoride with water, but a large amount of hydrofluoric acid will be produced during the preparation process, and these hydrofluoric acids are easily soluble in perfluoropolyether carboxylic acid, thereby affecting perfluoropolyether carboxylic acid. sour quality

Method used

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  • Perfluoropolyether carboxylic acid with low HF content and preparation method thereof
  • Perfluoropolyether carboxylic acid with low HF content and preparation method thereof

Examples

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Effect test

Embodiment 1

[0015] Example 1: In a reaction tank, add 100 grams of perfluoropolyetheracyl fluoride CF3CF2CF2OCF(CF3)-COF at 0°C to 10°C, keep the temperature and add 115g of NaF in a saturated aqueous solution at a speed of 1-10ml / min, Without stirring, after the reaction is over, open the partition in the reaction tank, the reaction product flows into the absorption tower containing the NaF recovery agent through the filter screen set on the partition, and a small amount of NaHF2 stays on the filter screen, and a large amount of HF generated The gas enters the NaOH recovery tank through the gas outlet above the reaction tank to complete the recovery of a large amount of HF gas. The product CF3CF2CF2OCF(CF3)-COOH containing a small amount of HF enters the absorption tower, and HF reacts with NaF to generate NaHF2. After absorbing HF, the gas CF3CF2CF2OCF(CF3)-COOH enters the storage tank of perfluoropolyether carboxylic acid, and the content of HF in the final CF3CF2CF2OCF(CF3)-COOH is les...

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Abstract

The invention belongs to the field of fluorine chemical industry. The invention relates to a preparation method of perfluoropolyether carboxylic acid with low HF content. The preparation method comprises the following steps that a saturated sodium fluoride aqueous solution is dropwise added into a reaction tank containing perfluoropolyether acyl fluoride at the speed of 1-10 ml / min, a product flows into an absorption tower containing a NaF recycling agent to absorb HF after the reaction is finished, and therefore perfluorocarboxylic acid with the HF content smaller than 0.1% is obtained. Perfluoropolyether acyl fluoride reacts with a saturated sodium fluoride aqueous solution to generate perfluoropolyether carboxylic acid and hydrogen fluoride, hydrogen fluoride and sodium fluoride generate sodium bifluoride which is less dissolved in water, sodium bifluoride is filtered, dried and heated (160 DEG C) to obtain sodium fluoride again, and sodium fluoride can be recycled.

Description

technical field [0001] The invention belongs to the field of fluorine chemical industry, and in particular relates to a preparation method of perfluoropolyether carboxylic acid with low HF content. Background technique [0002] Low-molecular-weight perfluoropolyether carboxylic acids and carboxylates are important fluorocarbon surfactants, which can be used as dispersants to disperse polymerized fluorinated monomers in aqueous polymerization media to prepare various fluororesins. Due to the environmental problems caused by the traditional fluorosurfactant perfluorooctanoic acid and salt, perfluoropolyether carboxylic acid and carboxylate are regarded as an important new green and environmentally friendly fluorocarbon surfactant because they are more easily degraded. Fluoropolymer preparation, waterproof and oil-proof, petroleum exploration and other fields have a wide range of application values. [0003] Perfluoropolyether carboxylic acid is usually prepared by reacting pe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/04C07C51/42C07C59/135C08G65/324B01D53/14B01D53/18
CPCC07C51/04C07C51/42C07C59/135B01D53/1456B01D53/1425B01D53/18C08G65/324B01D2252/10B01D2257/2047Y02C20/30
Inventor 肖鑫姚素梅
Owner TIANJIN CHANGLU CHEM NEW MATERIAL CO LTD
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