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Synthesis method of alkali metal trifluoromethanesulfonate

A technology of trifluoromethanesulfonic acid base and synthesis method, which is applied in the preparation of sulfonate, the preparation of sulfonate, organic chemistry, etc., can solve the problem that the purity of lithium trifluoromethanesulfonate cannot reach the standard, the conductivity of the battery is affected, and the moisture cannot be Complete removal of problems such as avoiding the introduction of impurities, low cost and mild conditions

Active Publication Date: 2020-05-08
PERIC SPECIAL GASES CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But there is following problem in this preparation method: one, when lithium hydroxide is not enough, can generate trifluoromethanesulfonic acid
Even a small amount of trifluoromethanesulfonic acid in lithium trifluoromethanesulfonate will affect the characteristics of the battery and reduce its stability
Two, if LiOH is excessive, because lithium hydroxide can form hydrate, therefore can cause moisture to be removed completely; On the other hand, lithium hydroxide purity is low, and the purity of the lithium trifluoromethanesulfonate that generates also can't reach the standard, will have a negative impact on The performance of the battery affects
In addition, lithium trifluoromethanesulfonate can also be prepared by reacting trifluoromethanesulfonic acid with lithium carbonate, but this reaction is likely to cause lithium carbonate residue, which seriously affects the electrical conductivity of the battery.

Method used

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  • Synthesis method of alkali metal trifluoromethanesulfonate
  • Synthesis method of alkali metal trifluoromethanesulfonate

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Add 111g (1.0mol) of anhydrous calcium chloride and 64g (2mol) of methanol into reactor I equipped with a thermometer, a distillation device, and mechanical stirring, evacuate the system to -0.095MPa, cool the system to -40°C, and Add 380 g (2.5 mol) of trifluoromethanesulfonyl fluoride. Stir mechanically, control the temperature of the system at 0°C, and the pressure at 0.1 MPa, and react for 2.5 hours. After the reaction, slowly open the outlet valve of the system to release excess trifluoromethanesulfonyl fluoride and collect it by cooling. After the pressure in the reaction vessel I was reduced to normal pressure, the temperature of the system was slowly raised for distillation, and the fractions at a temperature of 90-105°C were collected to obtain 304 g of methyl trifluoromethanesulfonate with a yield of 92.7%.

[0030] Take 164g (1.0mol) of methyl trifluoromethanesulfonate in reactor II equipped with a thermometer and mechanical stirring, and add 44g (1.0mol) of...

Embodiment 2

[0032] Add 111g (1.0mol) of calcium chloride and 96.6g (2.1mol) of ethanol into reactor I equipped with a thermometer, a distillation device, and mechanical stirring, evacuate the system to -0.095MPa, cool the system to -40°C, and Add 380 g (2.5 mol) of trifluoromethanesulfonyl fluoride. Stir mechanically, control the temperature of the system at 0°C, and the pressure at 0.05 MPa, and react for 3 hours. After the reaction, slowly open the outlet valve of the system to release excess trifluoromethanesulfonyl fluoride and collect it by cooling. After the pressure in the reaction vessel I was reduced to normal pressure, the temperature of the system was slowly raised for distillation, and the fractions at a temperature of 90-105°C were collected to obtain 316.8 g of ethyl trifluoromethanesulfonate with a yield of 88.9%.

[0033] Get 178g (1.0mol) of ethyl trifluoromethanesulfonate in reactor II equipped with a thermometer and mechanical stirring, add 40g (1.0mol) of sodium hydro...

Embodiment 3

[0035] Add 111g (1.0mol) of calcium chloride and 64g (2.0mol) of methanol into the reactor I equipped with a thermometer, a distillation device, and mechanical stirring, and evacuate the system to -0.095MPa. 245 g (2.5 mol) of sulfonyl fluoride. Stir mechanically, control the temperature of the system at 68°C, and react at a pressure of 0.1MPa for 2h. After the reaction, slowly open the outlet valve of the system to release excess methanesulfonyl fluoride and collect it under cooling. Slowly raise the system temperature and distill under reduced pressure, the pressure is -0.095MPa, and the fractions with a temperature of 90-95°C are collected to obtain 204g of methyl methanesulfonate, with a yield of 92.7%.

[0036] Take 110 g (1.0 mol) of methyl methanesulfonate in reactor II equipped with a thermometer and mechanical stirring, and add 44 g (1.0 mol) of lithium hydroxide monohydrate. Stir mechanically, control the temperature of the system at 50°C, and react at a pressure o...

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Abstract

The invention relates to a synthesis method of alkali metal trifluoromethanesulfonate, and belongs to the technical field of fine chemical engineering. The method comprises the following steps: firstly, adding anhydrous calcium chloride and alcohol into a reactor, vacuumizing, controlling the temperature in the reactor to be -40-25 DEG C, introducing excessive a sulfonyl fluoride compound, stirring, controlling the temperature to be -40-70 DEG C and the pressure to be 0.05-0.15 MPa, and reacting for 2-3 h; discharging the unreacted sulfonyl fluoride compound after the reaction is finished, anddistilling to obtain an ester compound; and adding an alkali metal hydroxide into the ester compound, stirring, reacting for 2-5 h under the pressure of 0.05-0.15 MPa at the temperature of 20-70 DEGC, filtering after the reaction is finished, and drying to obtain the alkali metal trifluoromethanesulfonate. The reaction yield is effectively improved, and introduction of impurities in a conventional method is avoided; and post-reaction treatment is simple, and pollution in the synthesis process is reduced.

Description

technical field [0001] The invention relates to a method for synthesizing alkali metal trifluoromethanesulfonate, belonging to the technical field of fine chemicals. Background technique [0002] Alkali metal triflate salts include lithium triflate, sodium triflate, potassium triflate and rubidium triflate, where lithium triflate (CF 3 SO 3 When Li) is used as a solid electrolyte, its stable anion will improve the structure and composition of the passivation layer between the electrolyte and the cathode material interface, which is conducive to the stability of the electrolyte, passivation film and motor, so its production and application have become a research hotspot . [0003] At present, the production technology of lithium trifluoromethanesulfonate is mainly controlled by Japan and the United States. Foreign manufacturers include Japan's Chuo Glass and the US 3M Company, etc., but few technologies have been disclosed. The production method proposed in the Japanese pu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/32C07C309/06
CPCC07C303/32C07C303/28C07C309/06C07C309/65
Inventor 花莹曦姚刚商洪涛户帅帅罗建志郝春辉袁瑞玲史紫微吕灵华杨雷雷
Owner PERIC SPECIAL GASES CO LTD
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