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Liquid-phase reaction preparation method of fluorides

A liquid-phase reaction and fluoride technology, which is applied in chemical instruments and methods, hydrolysis preparation, halogenated hydrocarbon preparation, etc., can solve the problems of low reaction yield and long reaction time

Active Publication Date: 2014-04-09
JIANGSU BLUESTAR GREEN TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But this method reaction yield is low, and reaction time is long

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The content is composed of 300 kg of aqueous solution of 17% potassium chloride, 4% potassium formate, 15% potassium fluoride and CHF 2 CH 2 30 kg of Cl is continuously sent to the respective coil preheaters for preheating with their corresponding high-pressure metering pumps at a mass ratio of 10:1, and then overheated through their respective coil superheaters. The overheated two-phase materials are mixed in the mixer and then enter the reactor for reaction. The reaction temperature is 260-270°C, the reaction pressure is 11-12MPa, and the reaction residence time is 35 minutes. The reaction product is cooled by a cooler, collected, distilled, and rectified to obtain the product trifluoroethane and difluoroethanol, and the unreacted CHF 2 CH 2 Cl then continues to return to the reactor for reaction. The one-time yield of difluoroethanol reaches 52%, and the one-time yield of trifluoroethane reaches 23%.

Embodiment 2

[0027] The content is composed of 300 kg of aqueous solution of 30% potassium chloride, 4.3% potassium carbonate, 5% potassium fluoride and CHF 2 CH 2 60 kg of Cl is continuously sent to the respective coil preheaters for preheating with their corresponding high-pressure metering pumps at a mass ratio of 5:1, and then overheated through their respective coil superheaters. The overheated two-phase materials are mixed in the mixer and then enter the reactor for reaction. The reaction temperature is 280-290°C, the reaction pressure is 10-11MPa, and the reaction residence time is 60 minutes. The reaction product is cooled by a cooler, collected, distilled, and rectified to obtain the product trifluoroethane and difluoroethanol, and the unreacted CHF 2 CH 2 Cl then continues to return to the reactor for reaction. The one-time yield of difluoroethanol reaches 60.5%, and the one-time yield of trifluoroethane reaches 6.4%. .

Embodiment 3

[0029] The content is composed of 300 kg of aqueous solution of 18% ammonium chloride, 3.7% ammonium bicarbonate, 14.2% potassium fluoride and CHF 2 CH 2 50 kg of Cl is continuously sent to the respective coil preheaters for preheating with respective corresponding high-pressure metering pumps at a mass ratio of 6:1, and then overheated through the respective coil superheaters. The overheated two-phase materials are mixed in the mixer and then enter the reactor for reaction. The reaction temperature is 300-305° C., the reaction pressure is 12-13 MPa, and the reaction residence time is 25 minutes. The reaction product is cooled by a cooler, collected, distilled, and rectified to obtain the product trifluoroethane and difluoroethanol, and the unreacted CHF 2 CH 2 Cl then continues to return to the reactor for reaction. The one-time yield of difluoroethanol was 50.8%, and the one-time yield of trifluoroethane was 16.7%.

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Abstract

The invention relates to a liquid-phase reaction preparation method of fluorides. The liquid-phase reaction preparation method comprises the following steps: raw material mixing: mixing a potassium fluoride water solution and CHF2CH2Cl according to the weight ratio of (1-10): 1, wherein the concentration of the potassium fluoride water solution is 1%-6%; reaction: performing chemical reaction on the mixed raw materials, wherein the reaction temperature is 80-360 DEG C, the reaction pressure is 0.1-25MPa, and the reaction retention time is 10-90min; cooling, and receiving the materials so as to obtain trifluoroethane and difluoroethanol. According to the liquid-phase reaction preparation method of the fluorides, provided by the invention, the one-time yield of difluoroethanol can achieve 30-60%, and the one-time yield of trifluoroethane can achieve 5-25%.

Description

technical field [0001] The invention relates to a liquid-phase reaction preparation method of fluoride. Background technique [0002] Trifluoroethane is a fluorine-containing refrigerant that can also be used as a foaming agent and cleaning agent. [0003] Difluoroethanol is an important aliphatic fluorine-containing intermediate. It is a colorless liquid with an alcohol smell at room temperature. It is stable and can be freely miscible with water and various organic solvents. Due to its unique physical and chemical properties and molecular structure, it has different properties from other alcohols and can participate in various organic chemical reactions, so it has broad prospects for development and utilization. Difluoroethanol is mainly used in the synthesis of fluorine-containing medicines, pesticides and dyes. [0004] At present, the development and research of difluoroethanol in the world is still at the primary level. It is mainly obtained by reducing fluorine-cont...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/38C07C29/09C07C19/08C07C17/20
CPCC07C17/208C07C29/09C07C31/38C07C19/08
Inventor 陈建海李建民吴建军荆忠俊顾小兵张伟华
Owner JIANGSU BLUESTAR GREEN TECH
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