Preparation method of fluoroethylene carbonate

A technology of fluoroethylene carbonate and chloroethylene carbonate, which is applied in the field of preparation of fluoroethylene carbonate, can solve the problems of increased reaction operation complexity, long time, high reaction temperature, etc., and achieve enhanced nucleophilicity and room temperature reaction The effect of mild conditions and high reaction yield

Active Publication Date: 2014-05-07
武汉市瑞华新能源科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to suppress the occurrence of side effects, some people use R 3 The fluorinating agent of N·nHF class (as CN101774923), but increased the complexity of reaction operation (due to using highly toxic reagent hydrogen fluoride)
In addition, in the prior art, usually the reaction temperature is higher and the time is longer

Method used

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  • Preparation method of fluoroethylene carbonate
  • Preparation method of fluoroethylene carbonate
  • Preparation method of fluoroethylene carbonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] In a 250ml three-necked flask, add 24.5g (0.2mol) of chloroethylene carbonate (Cl-EC), then add successively relative to 1.3 times the fluorinating reagent KF of chloroethylene carbonate consumption, 10mol% bis(tri-EC) Fluoromethylsulfonyl) imidized 1-methyl-3-ethylimidazolium (Im-1,2-TFSI, 7.8g) ionic liquid catalyst, and 60ml of acetonitrile. Stir magnetically and react at 25°C for 12h. Filter off the solid, collect the filtrate, remove the organic solvent in the filtrate by rotary evaporation, and carry out vacuum distillation on the remaining liquid, collect 18g of 70~72℃ / 2~3mm Hg fraction, the yield is 85%; the water content is 15ppm (measured by coulometric method) . The light yellow residue remaining in the bottle after distillation is ionic liquid (ionic liquid cannot be distilled out by ordinary distillation methods due to its extremely low volatility), weighing about 8g. The recovered ionic liquid is directly used in the next cycle reaction.

[0024] The ch...

Embodiment 2

[0026] The ionic liquid recovered in Example 1 was directly used in the catalytic reaction to prepare fluoroethylene carbonate (F-EC). Except using the recovered ionic liquid of Example 1 for the catalytic reaction, the remaining reaction steps and reagent consumption were the same as in Example 1 to obtain 18 g of fluoroethylene carbonate (F-EC) with a yield of 85%. Following examples 1 and 2, the ionic liquid recovered after each reaction was used for the next reaction to catalyze the preparation of fluoroethylene carbonate, and 10 consecutive reactions were carried out like this. As a result, the yield of fluoroethylene carbonate (F-EC) was 82 to 85%. After ten reactions, the ionic liquid was yellow, washed with water, dried and weighed, and the weight of the ionic liquid was 6.5 g. Therefore, the recovery of the ionic liquid was 83% after 10 catalytic reactions. It was confirmed by nuclear magnetic characterization that the ionic liquid did not decompose after 10 reactio...

Embodiment 3-24

[0036] Examples 3-29 show the preparation methods and yields of F-EC under different reaction conditions. In all the examples, the amount of Cl-EC is 24.5g (0.2mol), and the amount of the catalyst ionic liquid is calculated according to the percentage molar ratio of the amount of Cl-EC.

[0037] Table 1 Preparation methods and results of F-EC under different reaction conditions

[0038]

[0039]

[0040] Explanation: Im, N, PY, Py and Pl represent (a) imidazole, (b) tetraalkyl quaternary ammonium, (c) tetrahydropyrrole, (d) pyridine and piperidine (e) in formula 1 respectively in the table ) parent structure. The substituents methyl, ethyl, n-propyl, n-butyl, n-pentyl and n-hexyl on the nitrogen atom are represented by numbers 1, 2, 3, 4, 5 and 6 respectively (such as PY-12 represents N- methyl-N-ethyltetrahydropyridinium cation).

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Abstract

The invention discloses a preparation method of fluoroethylene carbonate. The preparation method comprises the following steps of by adopting imidazole type and quarternary ammonium type ion liquid of fluorosulfimide anions as a catalyst, carrying out nucleophilic substitution reaction on chloroethylene carbonate and an alkali-metal fluorinating agent in an organic solvent so as to generate fluoroethylene carbonate. The preparation method has the advantages that the yield is high, the reaction condition is mild and the ion liquid catalyst can be recycled and the like.

Description

technical field [0001] The invention belongs to the field of organic fluorine chemical industry, and in particular relates to a method for preparing fluoroethylene carbonate by using ionic liquid as a catalyst. Background technique [0002] 4-Fluoro-1,3-dioxolane-2-one, also known as fluoroethylene carbonate (hereinafter referred to as F-EC), is an important electrolyte solvent or additive for lithium-ion batteries. Its main function is to form a protective film on the surface of carbon-based materials such as graphite negative electrodes in lithium-ion batteries, which can significantly improve the performance of lithium batteries (such as cycle life, high and low temperature performance and safety, etc.) while inhibiting the decomposition of the electrolyte. . Therefore, exploring the preparation method of F-EC is one of the hotspots in electrolyte materials in recent years. [0003] In the prior art, there are mainly three kinds of preparation methods related to FEC: (1...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/42B01J31/02
CPCY02P20/584C07D317/42
Inventor 陈瀚林陈世忠周志彬
Owner 武汉市瑞华新能源科技有限公司
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