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The Synthetic Method and Application of Bis(2,2,2-Trifluoroethyl) Ether

The technology of a trifluoroethyl group and a synthesis method is applied in the application of lithium battery electrolyte solution and the field of fluorinated organic solvent fluorinated ether, which can solve the problems of difficult storage of production raw materials, less than 99% purity, and high equipment performance requirements, Achieve the effect of increasing competitiveness, reducing production costs and reducing equipment costs

Active Publication Date: 2022-03-29
JIANGSU BLUESTAR GREEN TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The traditional method for preparing bis(2,2,2-trifluoroethyl) ether, such as the bis(2,2,2-trifluoroethyl) ether of U.S. Patent No. 3,363,006 and its preparation method, uses 2,2, 2-Trifluoroalcohol and dioxane prepare nucleophilic 2,2,2-trifluoroethylsodium, and then react with tosylate to generate (2,2,2-trifluoroethyl)ether, prefabricated 2,2,2-Trifluoroethylsodium needs to be carried out from metal sodium in dioxane environment. The production process is complex and requires high equipment performance. The production raw materials are not easy to store and are not environmentally friendly. In addition, through this The purity of bis(2,2,2-trifluoroethyl) ether produced by the method cannot reach more than 99%

Method used

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Examples

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preparation example Construction

[0029] The synthetic method of two (2,2,2-trifluoroethyl) ethers comprises the following steps:

[0030] 1) Preparation of 1,1,1-trifluoro-2-chloroethane;

[0031] Preferably, as an implementable manner, the preparation of 1,1,1-trifluoro-2-chloroethane also includes the following steps:

[0032] S1 Add the catalyst to the 1,1,1-trifluoro-2-chloroethane reactor first, and when the temperature of the reactor reaches 100°C with steam, feed hydrogen fluoride, trichloroethylene, and chlorine gas into the reactor at a certain rate Continuously add raw materials to the reactor, control the pressure of the reactor to 0.7-0.8Mpa, and control the reaction temperature to 100-115°C.

[0033] It should be noted that the catalyst used in this step is a catalyst commonly used for halogenated alkanes, which may be antimony pentachloride or other metal halides.

[0034] Preferably, in this step, the ventilation rate is: hydrogen fluoride<250L / h, trichlorethylene<180L / h, chlorine gas 12-15Kg...

Embodiment 1

[0049]The catalyst antimony pentachloride is added to the 1,1,1-trifluoro-2-chloroethane reactor in advance, and when the temperature of the reactor is heated to 100°C with steam, hydrogen fluoride <250L / h, trichloroethylene <180L / h, chlorine gas 12-15Kg / h, continuously add raw materials into the reactor, control the pressure of the reactor to 0.7-0.8Mpa, and the reaction temperature to 100-115°C. Open the valve to the gas buffer tank, and control the temperature of the reaction bubbler to be 65-85°C. Open the water inlet valve of the condenser and control the top temperature of the condenser to 40-45°C. Start the cryogenic system to cool and collect the exhaust gas. The collected crude 1,1,1-trifluoro-2-chloroethane is rectified in a rectification tower to remove alkali and washed with water, and then sent to the alkali hydrolysis section.

[0050] Add 550kg ethylene glycol, 1.1kg potassium hydroxide, 100kg trifluoroethanol in the pressure reactor, seal the reactor, and pa...

Embodiment 2

[0052] The catalyst antimony pentachloride is added to the 1,1,1-trifluoro-2-chloroethane reactor in advance, and when the temperature of the reactor is heated to 100°C with steam, hydrogen fluoride <250L / h, trichloroethylene <180L / h, chlorine gas 12-15Kg / h, continuously add raw materials into the reactor, control the pressure of the reactor to 0.7-0.8Mpa, and the reaction temperature to 100-115°C. Open the valve to the gas buffer tank, and control the temperature of the reaction bubbler to be 65-85°C. Open the water inlet valve of the condenser and control the top temperature of the condenser to 40-45°C. Start the cryogenic system to cool and collect the exhaust gas. The collected crude 1,1,1-trifluoro-2-chloroethane is rectified in a rectification tower to remove alkali and washed with water, and then sent to the alkali hydrolysis section.

[0053] Add 500kg ethylene glycol, 1.0kg potassium hydroxide, 100kg trifluoroethanol to the pressure reactor, seal the reactor, and p...

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Abstract

The invention provides a method for synthesizing bis(2,2,2-trifluoroethyl) ether, comprising the following steps: preparing 1,1,1-trifluoro-2-chloroethane; Add 500-550 parts by weight of ethylene glycol, 0.9-1.1 parts by weight of potassium hydroxide, and 100 parts by weight of trifluoroethanol, seal the reactor, and feed 1,1,1-trifluoro-2-chloroethane 110-130 parts by weight part, stirred and heated to at least 70-80°C for 2-4 hours; the system temperature was controlled between 70-90°C, a polar solvent was added to the system, stirred evenly, and the potassium chloride solid precipitate was filtered to obtain the filtrate; the filtrate fine The product with a purity of more than 99.98% is obtained by distillation, and its application in the field of lithium batteries as an electrolyte solution for lithium batteries is provided. This process has the advantages of easy access to raw materials, no supply restrictions, simple equipment requirements, no special material requirements, simple process, fully meets production needs, clean production, reduces equipment costs, increases the competitiveness of the company's products, and improves economic benefits.

Description

technical field [0001] The invention relates to the field of production of lithium battery electrolyte solution, in particular to a production method of fluorinated organic solvent fluorinated ether and its application as lithium battery electrolyte solution. Background technique [0002] Fluorinated organic solvents have long been used in lithium-ion batteries, and fluorinated solvents can bring various benefits to electrolytes compared with conventional electrolytes without fluorinated solvents. Bis(2,2,2-trifluoroethyl)ether is an electrolyte solution for lithium batteries with high oxidation resistance, good flame retardancy and good compatibility with graphite negative electrodes. By adding bis(2,2,2-trifluoroethyl) ether to the lithium battery electrolyte, the oxidation resistance, flame retardancy and good compatibility with graphite negative electrodes of the entire lithium battery system can be significantly improved. Bis(2,2,2-trifluoroethyl)ether helps to form an...

Claims

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Application Information

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IPC IPC(8): C07C41/16C07C43/12H01M10/0569
CPCC07C41/16H01M10/0569C07C17/21C07C43/123C07C19/12Y02E60/10
Inventor 徐祥松高国军陈建海李建民何金峰刘俊
Owner JIANGSU BLUESTAR GREEN TECH
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