Method for separating difluoroethanol and water with porous liquid as extracting agent

A technology of difluoroethanol and extractant, which is applied in the field of chemical separation, can solve the problems of operator safety and health threats, high equipment costs, and high energy consumption, and achieves strong circulation extraction capabilities, repeated use, and high extraction efficiency Effect

Active Publication Date: 2021-04-09
SHANDONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] There are defects and deficiencies in the above-mentioned existing separation technologies: (1) extractive distillation and azeotropic distillation separate difluoroethanol and water, the equipment cost is high, and the energy consumption is relatively large
(2) The entrainer toluene is highly toxic, affects human health, and is flammable and explosive, all of which pose a threat to the safety and health of operators

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The imidazole porous liquid is formed by combining 1-butyl-3-methylimidazole bistrifluoromethanesulfonimide and ZIF-8. The mass ratio of the porous liquid to the mixture of difluoroethanol and water is 0.5:1, the extraction temperature is 25°C, and the stirring time is 30min. Take 2.55g of the porous liquid in a sample bottle and add 5.1g of the mixture of difluoroethanol and water. , stirred for 30 minutes, and left to stand for 30 minutes. The difluoroethanol in the upper raffinate phase was measured by GC. After the porous liquid was circulated and extracted 10 times, the extraction rate of difluoroethanol was 64.2%. The porous liquid in the lower layer of the extract was recovered with ethyl acetate. The recovery rate of difluoroethanol obtained after distillation of the stripping agent phase was 83.3%, and the extraction rate did not decrease significantly after 10 times of circular extraction of the porous liquid.

Embodiment 2

[0028] The pyridine porous liquid is formed by the combination of n-butylpyridine bistrifluoromethanesulfonimide and ZIF-8. The mass ratio of the porous liquid to the mixture of difluoroethanol and water is 2:1. The extraction temperature is 25°C. Stir The time is 40min, at 25°C, take a mixture of 5.045g difluoroethanol and water into a sample bottle, add 10.09g porous liquid, stir for 40min, let stand for 40min, use GC to measure the concentration of difluoroethanol in the upper raffinate phase, porous liquid Circular extraction for 9 times, the extraction rate of difluoroethanol was 89.3%, the porous liquid in the lower extraction phase was reclaimed with ethyl acetate, and after the rectification of the upper layer stripping agent phase, the recovery rate of difluoroethanol was 90.1%. The extraction rate did not decrease significantly after liquid circulation extraction for 9 times.

Embodiment 3

[0030] The pyridine porous liquid is formed by the combination of n-butylpyridine bistrifluoromethanesulfonimide and ZIF-8, the mass ratio of the porous liquid to the mixture of difluoroethanol and water is 5:1, the extraction temperature is 35°C, stirring The time is 40min, at 35°C, take 2g of difluoroethanol and water mixture into the sample bottle, add 10g of porous liquid, stir for 40min, let it stand for 40min, use GC to measure the concentration of difluoroethanol in the upper raffinate phase, and extract the porous liquid circularly 11 times, the extraction rate of difluoroethanol was 92.4%. The porous liquid in the lower extraction phase was reclaimed with ethyl acetate. After the rectification of the upper layer stripping agent phase, the recovery rate of difluoroethanol was 91.6%, and the porous liquid was recycled. The extraction rate did not drop significantly after 11 extractions.

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Abstract

The invention relates to a method for extracting and separating difluoroethanol and water by utilizing porous liquid. According to the method, the porous liquid is synthesized by utilizing ZIF-8 and hydrophobic ionic liquid and is used as the extracting agent to extract and separate a mixture of difluoroethanol and water. The method comprises the following steps: firstly, stirring mixed porous liquid, difluoroethanol and water, and conducting standing to obtain two layered phases; separating out an upper-layer raffinate phase and a lower-layer extraction phase in a liquid separation manner; then carrying out back extraction on the lower-layer extraction phase by using ethyl acetate, and carrying out rectification treatment on a back-extracted phase obtained after back-extraction to obtain difluoroethanol; and carrying out cyclic extraction on the upper-layer raffinate phase by using the regenerated porous liquid. The porous liquid used in the method has the same characteristics as a porous material and an ionic liquid, and is high in separation efficiency, high in cyclic extraction capacity, friendly to environment and capable of being repeatedly used.

Description

technical field [0001] The invention relates to a method for extracting and separating difluoroethanol and water by using a porous liquid, belonging to the technical field of chemical separation. Background technique [0002] Difluoroethanol (DFE) is an important fluorinated aliphatic intermediate. Due to its special structure, difluoromethyl has different chemical properties from other alcohols and can participate in a variety of organic synthesis reactions, especially in fluorinated pesticides, pharmaceuticals, fluoropolymers and cleaning agents. Aqueous solutions of DFE are produced during the application and preparation of difluoroethanol. DFE and water can form an azeotrope. The polarity of difluoroethanol is very similar to that of water, and it is more difficult to separate than the azeotropic system of fluoroalcohols such as tetrafluoropropanol and octafluoropentanol and water. Liquid-liquid extraction is a common method for separating azeotropes and is performed ...

Claims

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Application Information

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IPC IPC(8): C07C29/86C07C31/38
CPCC07C29/86C07C31/38Y02P20/582
Inventor 徐冬梅吴绪敏马艺心
Owner SHANDONG UNIV OF SCI & TECH
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