Synthesis method of trifluoroethanol acetate

A technology of trifluoroethanol acetate and its synthesis method, which is applied to the preparation of carboxylic acid halides, the manufacture of final products, organic chemistry, etc., and can solve the problems of poor purity, imperfect manufacturing and purification methods of trifluoroethanol acetate, and low production capacity, etc. problems, to achieve the effects of improving yield and purity, inhibiting side reactions, and simplifying the reaction process

Pending Publication Date: 2022-05-20
SHIJIAZHUANG SAN TAI CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the production and purification methods of trifluoroethanol acetate are not perfect, and the uncertainty of various parameters in the production process leads to low production capacity and relatively poor purity.

Method used

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  • Synthesis method of trifluoroethanol acetate
  • Synthesis method of trifluoroethanol acetate
  • Synthesis method of trifluoroethanol acetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Synthesis method of trifluoroethanol acetate, the synthesis steps of which are as follows:

[0021] Take 86.35g (1.1mol) acetyl chloride dissolved in 200mL of dichloromethane to give dichloromethane solution of acetyl chloride;

[0022]Take 100g (1mol) of trifluoroethanol to cool down to 0 °C, maintain 0 °C slowly add dichloromethane solution of acetyl chloride (drop time is 1h), after the drop is completed, 0 °C stirring reaction for 1h, and then add 183.98g (1.82 mol) of triethylamine in 4 batches (triethylamine is generally added in 3 to 4 batches), two drops of triethylamine are stirred between the acylation reaction for 1h, triethylamine drops are completed, and then maintain the 0 °C reaction for 1h, add 19.27g (0.18mol) Sodium carbonate, continue to maintain 0 °C reaction for 1h, then heated to 5 °C reaction 1h, and then heated to 10 °C reaction to trifluoroethanol all reaction completely, and then add 200mL of water washing, phase separation, the resulting organic p...

Embodiment 2

[0025] Synthesis method of trifluoroethanol acetate, the synthesis steps of which are as follows

[0026] Take 78.5 g (1mol) of acetyl chloride dissolved in 180mL of dichloromethane to give dichloromethane solution of acetyl chloride;

[0027] Take 100g (1mol) of trifluoroethanol to cool down to -5 °C, maintain -5 °C slowly add dichloromethane solution of acetyl chloride (drop time is 1h), after the drop is completed, -5 °C stirring reaction 0.5h, and then add 160.22g (1.58 mol) of triethylamine in 3 batches (triethylamine is generally added in 3 to 4 batches), the two drops of triethylamine are stirred to carry out the acylation reaction for 0.5h, after the triethylamine drops are completed, then maintain the -5 °C reaction 0.5h, add 33.57g (0.32mol) sodium carbonate, continue to maintain -5 °C reaction 0.5h, then heat up to 8 °C reaction 0.5h, and then heat up to 15 °C reaction to trifluoroethanol all reaction completely, and then add 200mL of water washing, phase separation, th...

Embodiment 3

[0029] Synthesis method of trifluoroethanol acetate, the synthesis steps of which are as follows:

[0030] Take 82.43g (1.05mol) acetyl chloride dissolved in 190mL of dichloromethane to give dichloromethane solution of acetyl chloride;

[0031]Take 100g (1mol) of trifluoroethanol to cool down to -1 °C, maintain -1 °C slowly add acetyl chloride dichloromethane solution (drop time is 1h), after the drop is completed, -1 °C stirring reaction 0.6h, and then add 162.78g (1.61 mol) of triethylamine in 3 batches (triethylamine is generally added in 3 to 4 batches), the two drops of triethylamine are stirred to carry out the acylation reaction for 0.6h, after the completion of the triethylamine drop,then maintain the -1 °C reaction 0.6h, add 25.58g (0.24mol) sodium carbonate, continue to maintain -1 °C reaction 0.6h, then heated to 7 °C reaction 0.6h, and then heated to 12 °C reaction to trifluoroethanol all reaction completely, and then added 200mL of water washing, phase separation, the...

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Abstract

The invention discloses a synthesis method of trifluoroethanol acetate, and relates to the technical field of battery electrolyte additives, and the synthesis method comprises the following steps: taking trifluoroethanol and acetyl chloride, and under the action of an acid capturing agent composed of triethylamine and sodium carbonate, carrying out acylation reaction to obtain the trifluoroethanol acetate. According to the invention, by selecting the appropriate acid capturing agent composition, the side reaction of trifluoroethanol and acetyl chloride is effectively inhibited, and the yield and purity of the product are improved; the esterification reaction is carried out in a gradient heating manner, so that the reaction difficulty is reduced, and the forward proceeding of the reaction is promoted. According to the method, the reaction process is simple, raw materials used in the reaction are easy to obtain, the reaction process is milder and safer compared with the prior art, the product yield and the product purity in the production process are ensured to be maximized by controlling the reaction conditions in each stage, and the product yield and the product purity are further improved by reasonably controlling the use amount of the reaction raw materials and the reaction process.

Description

Technical field [0001] The present invention relates to the technical field of battery electrolyte additives, in particular, a synthesis method of trifluoroethanol acetate. Background [0002] Since the commercialization of lithium batteries in the 1990s, it has been applied in all aspects of life and production because of its high energy density, small pollution and long life. However, with the continuous development of the times, the higher performance requirements and wider application areas of the battery have gradually restricted the subsequent development of lithium batteries. How to improve the safety and stability of lithium batteries has become the focus of current research, and the key factor affecting the performance of lithium batteries lies in all aspects of the performance of the organic electrolyte, in the production of batteries in the electrolyte to add electrolyte additives containing trifluoroethanol acetate to increase the concentration of hydrogen ions in the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/14C07C69/14
CPCC07C67/14C07C69/14Y02P70/50
Inventor 彭鹏鹏郝俊侯荣雪王军葛建民
Owner SHIJIAZHUANG SAN TAI CHEM CO LTD
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