阅读说明：本技术 一种三氟甲磺酸锂的制备方法 (Preparation method of lithium trifluoromethanesulfonate ) 是由 陈红斌 祝金玲 黄素玉 于 2019-11-19 设计创作，主要内容包括：本发明一种三氟甲磺酸锂的制备方法,包括以下步骤：步骤一：三氟甲基卤化锌的制备：氮气保护下,向锌粉和四氢呋喃的悬浮溶液中通入三氟卤代甲烷,然后再加入适量的单质碘,缓慢加热反应,加入三氟卤代甲烷继续反应4-10h,制得三氟甲基卤化锌反应液；步骤二：三氟甲烷磺酸卤化锌的制备：在三氟甲基卤化锌反应液中,加入三氧化硫固体,得到三氟甲烷磺酸卤化锌反应液；骤三：三氟甲磺酸锂的制备：将三氟甲烷磺酸卤化锌反应液用氢氧化锂溶液中和,过滤,蒸干滤液的三氟甲磺酸锂。(The invention relates to a preparation method of lithium trifluoromethanesulfonate, which comprises the following steps: the method comprises the following steps: preparation of trifluoromethyl zinc halide: under the protection of nitrogen, introducing trifluorohalomethane into a suspension solution of zinc powder and tetrahydrofuran, then adding a proper amount of elemental iodine, slowly heating for reaction, adding trifluorohalomethane, and continuing to react for 4-10h to prepare a trifluoromethyl zinc halide reaction solution; step two: preparation of zinc trifluoromethanesulfonate halide: adding sulfur trioxide solid into the trifluoromethyl zinc halide reaction liquid to obtain trifluoromethanesulfonic acid zinc halide reaction liquid; step three: preparation of lithium trifluoromethanesulfonate: and (3) neutralizing the zinc trifluoromethanesulfonate halide reaction liquid with a lithium hydroxide solution, filtering, and evaporating lithium trifluoromethanesulfonate in the filtrate to dryness.)

1. A preparation method of lithium trifluoromethanesulfonate is characterized by comprising the following steps: the method comprises the following steps:

the method comprises the following steps: preparation of trifluoromethyl zinc halide: under the protection of nitrogen, introducing trifluorohalomethane into a suspension solution of zinc powder and tetrahydrofuran, then adding a proper amount of elemental iodine, slowly heating for reaction, adding trifluorohalomethane, and continuing to react for 4-10h to prepare a trifluoromethyl zinc halide reaction solution;

step two: preparation of zinc trifluoromethanesulfonate halide: adding sulfur trioxide solid into the trifluoromethyl zinc halide reaction liquid to obtain trifluoromethanesulfonic acid zinc halide reaction liquid;

step three: preparation of lithium trifluoromethanesulfonate: and (3) neutralizing the zinc trifluoromethanesulfonate halide reaction liquid with a lithium hydroxide solution, filtering, and evaporating lithium trifluoromethanesulfonate in the filtrate to dryness.

2. The method for producing lithium trifluoromethanesulfonate according to claim 1, wherein: 20% -35%.

3. The method for producing lithium trifluoromethanesulfonate according to claim 1, wherein: the reaction temperature of the methyl zinc halide reaction liquid is 40-80 ℃.

4. The preparation method of lithium trifluoromethanesulfonate described in claim 1 is characterized in that: and reacting the zinc powder with trifluorohalomethane at the temperature of 60 ℃ for 1 h.

5. The method for producing lithium trifluoromethanesulfonate according to claim 1, wherein: the reaction temperature of the methyl zinc halide reaction liquid is 40-80 ℃.

Technical Field

The invention relates to the technical field of electrolyte, in particular to a preparation method of lithium trifluoromethanesulfonate.

Background

Lithium trifluoromethanesulfonate can be used as an electrolyte of a lithium battery, and anions of the lithium trifluoromethanesulfonate can improve a passivation layer structure between an electrolyte and a cathode material interface, so that the lithium trifluoromethanesulfonate is favorable for stabilizing the electrolyte and a passivation film. At present, two methods for producing lithium trifluoromethanesulfonate are available, one method is that methanesulfonyl fluoride and liquid hydrogen fluoride are added into an electrolytic bath for electrolysis to produce trifluoromethanesulfonyl fluoride, and the trifluoromethanesulfonyl fluoride reacts with lithium carbonate to generate lithium trifluoromethanesulfonate; the other method is that trifluoromethanesulfonyl fluoride reacts with lithium hydroxide to prepare lithium trifluoromethanesulfonate, trifluoromethanesulfonic acid is generated when lithium hydroxide is insufficient, and battery characteristics are affected and stability is reduced when trifluoromethanesulfonic acid is contained in lithium trifluoromethanesulfonate.

Disclosure of Invention

The invention aims to provide a preparation method of lithium trifluoromethanesulfonate.

In order to achieve the purpose, the invention adopts the following technical scheme: a preparation method of lithium trifluoromethanesulfonate comprises the following steps:

the method comprises the following steps: preparation of trifluoromethyl zinc halide: under the protection of nitrogen, introducing trifluorohalomethane into a suspension solution of zinc powder and tetrahydrofuran, then adding a proper amount of elemental iodine, slowly heating for reaction, adding trifluorohalomethane, and continuing to react for 4-10h to prepare a trifluoromethyl zinc halide reaction solution;

step two: preparation of zinc trifluoromethanesulfonate halide: adding sulfur trioxide solid into the trifluoromethyl zinc halide reaction liquid to obtain trifluoromethanesulfonic acid zinc halide reaction liquid;

step three: preparation of lithium trifluoromethanesulfonate: and (3) neutralizing the zinc trifluoromethanesulfonate halide reaction liquid with a lithium hydroxide solution, filtering, and evaporating lithium trifluoromethanesulfonate in the filtrate to dryness.

Further preferably, the concentration of the lithium hydroxide solution is from 20% to 35%.

The reaction temperature of the trifluoromethyl zinc halide reaction liquid is 40-80 ℃.

The zinc powder and trifluorohalomethane react at the temperature of 60 ℃ for 1 h.

The reaction temperature of the trifluoromethyl zinc halide reaction liquid is 40-80 ℃.

The invention has the beneficial effects that: on the basis of the existing preparation process of zinc trifluoromethanesulfonate halide in the company, the zinc trifluoromethanesulfonate halide is subjected to a neutralization reaction with a lithium hydroxide solution to obtain lithium trifluoromethanesulfonate, and a novel process of the lithium trifluoromethanesulfonate is provided, wherein the yield can reach 70%.

Detailed Description

The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.

Example 1:

the method comprises the following steps: preparation of trifluoromethyl zinc halide: under the protection of nitrogen, 30g of trifluorohalogenated methane is introduced into a suspension solution of 106g of zinc powder and 500ml of tetrahydrofuran, then 5g of elemental iodine is added, the mixture is slowly heated to 40 ℃ for reaction for 2 hours, and the trifluorohalogenated methane is added for continuous reaction for 4 hours to prepare a trifluoromethyl zinc halide reaction solution.

Step two: preparation of zinc trifluoromethanesulfonate halide: 130g of sulfur trioxide solid is added into the trifluoromethyl zinc halide reaction liquid to obtain the trifluoromethanesulfonic acid zinc halide reaction liquid.

Step three: preparation of lithium trifluoromethanesulfonate: and (3) neutralizing the zinc halide trifluoromethanesulfonate reaction solution with a 20% lithium hydroxide solution until no precipitate is separated out, filtering, and evaporating the filtrate to dryness to obtain lithium trifluoromethanesulfonate.

Example 2:

the method comprises the following steps: preparation of trifluoromethyl zinc halide: under the protection of nitrogen, 30g of trifluorohalogenated methane is introduced into a suspension solution of 106g of zinc powder and 500ml of tetrahydrofuran, then 5g of elemental iodine is added, the mixture is slowly heated to 60 ℃ for reaction for 1 hour, and the trifluorohalogenated methane is added for continuous reaction for 6 hours to prepare a trifluoromethyl zinc halide reaction solution.

Step two: preparation of zinc trifluoromethanesulfonate halide: and adding 230g of sulfur trioxide solid into the trifluoromethyl zinc halide reaction liquid to obtain the trifluoromethanesulfonic acid zinc halide reaction liquid.

Step three: preparation of lithium trifluoromethanesulfonate: and (3) neutralizing the zinc halide trifluoromethanesulfonate reaction liquid with a 25% lithium hydroxide solution until no precipitate is separated out, filtering, and evaporating the filtrate to dryness to obtain lithium trifluoromethanesulfonate.

Example 3:

the method comprises the following steps: preparation of trifluoromethyl zinc halide: under the protection of nitrogen, 30g of trifluorohalogenated methane is introduced into a suspension solution of 106g of zinc powder and 500ml of tetrahydrofuran, then 5g of elemental iodine is added, the mixture is slowly heated to 80 ℃ for reaction for 1 hour, and the trifluorohalogenated methane is added for continuous reaction for 10 hours to prepare a trifluoromethyl zinc halide reaction solution.

Step two: preparation of zinc trifluoromethanesulfonate halide: 350g of sulfur trioxide solid is added into the trifluoromethyl zinc halide reaction liquid to obtain the trifluoromethane sulfonic acid zinc halide reaction liquid.

Step three: preparation of lithium trifluoromethanesulfonate: and (3) neutralizing the zinc halide trifluoromethanesulfonate reaction solution with 35% lithium hydroxide solution until no precipitate is separated out, filtering, and evaporating the filtrate to dryness to obtain lithium trifluoromethanesulfonate.

The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.