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Method for separating perfluoroalkylethylene from perfluoroalkyl ethyl acrylate crude product

A technology of perfluoroalkyl ethyl acrylate and perfluoroalkyl ethylene, which is applied in the field of separation and recovery of perfluoroalkyl ethylene, can solve the problems of complex treatment process and high energy consumption, and achieve the effect of improving utilization efficiency and reducing emissions

Active Publication Date: 2016-03-30
SICHUAN XIAIFU TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The traditional process is to mix the by-product olefins with unqualified solvents for incineration treatment. This treatment method not only consumes a lot of energy, but also has a complicated treatment process. In the end, only about 30% of hydrofluoric acid can be obtained.

Method used

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  • Method for separating perfluoroalkylethylene from perfluoroalkyl ethyl acrylate crude product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Flow the liquid phase material in the 100Kg perfluoroalkyl ethyl acrylate reactor through the pipeline to the filter, and place 108Kg of the obtained filtrate in the rectification tower, and the operating pressure in the tower is about 20KPa, Collect 38Kg of solvent crude fraction at 40-80°C, 6Kg of perfluoroalkylethylene crude fraction at 90-110°C, and 64Kg of perfluoroalkyl ethyl acrylate crude fraction as the bottom material.

[0035] (2) Place the perfluoroalkylethylene crude fraction obtained in step (1) in a washing tank, add a KOH solution with a mass percent concentration of 5% to it at a rate of 5Kg / min for washing (the amount of KOH solution is about 10Kg ) with constant stirring. After the lye washing is finished, add deionized water to it at a certain speed for washing until it is neutral (the amount of deionized water is about 15Kg).

[0036] (3) Add 50 g of activated alumina powder (40 mesh) to the crude fraction of perfluoroalkylethylene obtained in ...

Embodiment 2

[0040](1) Flow the liquid phase material in the 100Kg perfluoroalkyl ethyl acrylate reactor to the filter 2 through the pipeline, and place 112Kg of the obtained filtrate in the rectification tower, and the operating pressure in the tower is about 30KPa , respectively collected 45Kg of solvent crude fraction at 40-60°C, 6.2Kg of perfluoroalkylethylene crude fraction at 90-100°C, and 60.8Kg of perfluoroalkyl ethyl acrylate crude fraction as the bottom material.

[0041] (2) Put the solvent crude fraction obtained in step (1) in a rectification tower, the operating pressure in the tower is about 20KPa, collect 42Kg of the solvent crude fraction at 40-60°C, and the tower bottom material mainly contains perfluoroalkyl The crude fraction of ethyl acrylate crude fraction 3Kg;

[0042] (3) Put the crude fraction of perfluoroalkyl ethyl acrylate obtained in step (1) in a rectification tower, the operating pressure in the tower is about 20KPa, and the rectification temperature is 90°C....

Embodiment 3

[0047] (1) Flow the liquid phase material in the 100Kg perfluoroalkyl ethyl acrylate reaction kettle to the filter 2 through the pipeline, and place 110Kg of the obtained filtrate in the rectification tower, and the operating pressure in the tower is about 40KPa , respectively collected 45Kg of solvent crude fraction at 40-90°C, 6.2Kg of perfluoroalkylethylene crude fraction at 90-110°C, and 58.8Kg of perfluoroalkyl ethyl acrylate crude fraction as the bottom material.

[0048] (2) Place the solvent crude fraction obtained in step (1) in a rectification tower, the operating pressure in the tower is about 40KPa, collect 41.5Kg of the solvent crude fraction at 40-90°C, and the tower bottom material mainly contains perfluoroalkane Crude distillate 3.5Kg of ethyl ethyl acrylate;

[0049] (3) Put the crude fraction of perfluoroalkyl ethyl acrylate obtained in step (1) in a rectification tower, the operating pressure in the tower is about 40KPa, and the rectification temperature is ...

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Abstract

The invention relates to a method for separating perfluoroalkyl ethylene from a perfluoroalkylethyl acrylate crude product, which comprises the following steps: rectifying the perfluoroalkylethyl acrylate crude product to obtain a primary rectification solution containing perfluoroalkyl ethylene; adding an alkali solution into the obtained primary rectification solution for washing, adding activated alumina for decolorization, and carrying out water-oil-solid three-phase separation to obtain an oil phase containing perfluoroalkyl ethylene; and adding a small amount of polymerization inhibitor into the oil phase containing perfluoroalkyl ethylene, and rectifying to obtain the perfluoroalkyl ethylene. The separation method provided by the invention can purify the perfluoroalkyl ethylene in the perfluoroalkylethyl acrylate crude product to 99.9% above, and the perfluoroalkyl ethylene can be directly sold as a high-added-value product. The method enhances the utilization efficiency of chemical raw materials and reduces the emissions of the chemical raw materials.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a method for separating and recovering perfluoroalkylethylene from a crude product of perfluoroalkyl ethyl acrylate. Background technique [0002] Perfluoroalkylethylene (perfluoroalkylethylene iodide adduct) is an important intermediate of fluorine-containing surfactants, which can generate various surfactants such as perfluorocarboxylic acid after oxidation, so this substance has broad market space. The general method for synthesizing perfluoroalkylethylene is to perform addition reaction of perfluoroalkyl iodide and ethylene, and then carry out elimination reaction under alkaline conditions to generate perfluoroalkylethylene. [0003] Perfluoroalkyl ethylene acrylate is a very important fluorine-containing surfactant. Because of its special hydrophobic and oleophobic properties, it is widely used as a three-proof finishing agent in the fields of textiles and leather. The mai...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C21/18C07C17/38C07C17/383
Inventor 张金刚胡有荣李瑞涛陈千友
Owner SICHUAN XIAIFU TECH