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Preparation method of difluoro-sulfimide and lithium difluoro-sulfimide

A technology of lithium bisfluorosulfonimide and bisfluorosulfonimide, which is applied in the field of fluorine chemical synthesis, can solve the problems of long production process, difficulty in ensuring purity, and difficulty in controlling the reaction process, so as to meet the requirements of yield and quality. The needs of the production equipment, the residual impurity content is easy to control, and the effect of reducing the requirements of the production equipment

Inactive Publication Date: 2017-02-01
718TH RES INST OF CHINA SHIPBUILDING INDAL CORP
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  • Abstract
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AI Technical Summary

Problems solved by technology

[0004] (1) The first type of preparation method: first synthesize dichlorosulfonimide, which is fluorinated and lithium-containing substance lithiated to obtain lithium bisfluorosulfonimide (US4315935; CN102786452); The preparation method involves three or even four steps of chemical reactions and related purification steps. The process is long and the product has high impurities. The impurities introduced during the synthesis process, especially chloride ions, are difficult to effectively remove, and the presence of chloride ions will significantly increase the concentration of difluorosulfonyl oxide. The corrosiveness of lithium amine to aluminum electrodes commonly used in lithium batteries (Abouimrane A et al, J Power Sources 2009, 693; Han H B et al, J Power Sources 2011, 3623), seriously affects the industrial application of lithium bisfluorosulfonyl imide
[0005] (2) The second type of preparation method: prepare bisfluorosulfonimide salt by reacting sulfuryl fluoride and ammonia gas, and then lithiate lithium-containing substances to obtain lithium bisfluorosulfonimide (EP2415757, EP2439173, US20120020867); In the preparation method, the reactants are all in gaseous state, and the reaction needs to be carried out under high pressure. During the reaction process, heat is released violently, and solid salt is formed. It is difficult to transfer heat quickly, the reaction process is difficult to control, and there are high risks in the preparation process. Defects such as large investment in equipment
[0006] (3) The third type of preparation method: lithium salt (such as lithium perchlorate (LiClO 4 ) etc.) and bisfluorosulfonimide potassium salt etc. in an organic solvent by ion exchange reaction to obtain bisfluorosulfonimide lithium salt (CN101747242), however, in the product obtained by ion exchange, due to a small amount of LiClO 4 The presence of impurities makes it difficult to guarantee purity
[0007] In summary, the preparation method reported in the prior art has problems such as long production process flow, high impurity content, low product yield and high manufacturing cost. large-scale application, especially hindering its becoming the mainstream electrolyte material in new energy sources such as lithium-ion batteries and supercapacitors

Method used

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  • Preparation method of difluoro-sulfimide and lithium difluoro-sulfimide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] (1) Under stirring, add 97.1g of sulfamic acid (1mol) and fluorosulfonic acid into the dry 1L reactor, and flow 1.5m into the reactor 3 h -1 Slow introduction of sulfoxide fluoride SOF 2 Reaction, wherein, sulfamic acid: fluorosulfonic acid: SOF 2 The molar ratio is 1:1.5:6, the reaction temperature is 160°C, and the reaction pressure is 1MPa. After the introduction is completed, the reaction is continued for 18 hours to obtain the product, which is detected as bisfluorosulfonimide;

[0053] (2) Recrystallize and filter the bisfluorosulfonimide prepared in step (1) in the solvent diethyl carbonate at -100°C to obtain purified bisfluorosulfonimide with a yield of 90% , with a purity of 95%;

[0054] (3) Add the solvent nitromethane, and slowly add 31.2g of lithium-containing substance lithium fluoride (1.2mol) into the 1L reactor containing the bisfluorosulfonimide prepared in step (2) under stirring. The molar ratio of sulfonylimide and lithium-containing substance ...

Embodiment 2

[0057] (1) The raw materials are sulfamoyl fluoride, fluorosulfonic acid and SOClF, the molar ratio of sulfamoyl fluoride: fluorosulfonic acid: SOClF is 1:0.5:2, the reaction temperature is 80°C, the reaction pressure is -0.09MPa, and the rest With embodiment 1 step (1);

[0058] (2) Distilling the bisfluorosulfonimide prepared in step (1) under reduced pressure at 169° C. to obtain purified bisfluorosulfonimide with a yield of 90% and a purity of 92%;

[0059] (3) Add solvent dimethyl carbonate, the molar ratio of bisfluorosulfonimide and lithium-containing substance lithium oxide is 1:10, the reaction temperature is 0°C, and the reaction pressure is -0.09MPa, and the rest are the same as in Example 1 ( 3);

[0060] (4) adding solvent to the reaction product prepared in step (3) is tetrahydrofuran, adding 200 g of solvent tetrahydrofuran and recrystallizing at normal temperature for 2 hours, the yield is 93%, and the purity is more than or equal to 99.5%. Ion content<0.4ppm...

Embodiment 3

[0062] (1) Raw material sulfamic acid: fluorosulfonic acid: SOF 2 The mol ratio is 1:0.8:4, and the temperature of reaction is 100 DEG C, and the reaction pressure is 0MPa, and all the other are with embodiment 1 step (1);

[0063] (2) The bisfluorosulfonimide prepared in step (1) was distilled under reduced pressure at 60°C to obtain purified bisfluorosulfonimide with a yield of 91% and a purity of 93%;

[0064] (3) adding solvent isopentane, the ratio of bisfluorosulfonimide and lithium-containing substance lithium sulfide is 1:0.8, and the rest are the same as step (3) of Example 1;

[0065] (4) add solvent to the reaction product that step (3) makes is acetonitrile, add solvent acetonitrile 200g recrystallization 2h at normal temperature, productive rate is 94%, purity >=99.5%, wherein, chloride ion content<0.1ppm, fluorine Ion content<0.4ppm, water content<10ppm, sodium ion content<1ppm, potassium ion content<1ppm, all the other are the same as step (4) of embodiment 1. ...

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Abstract

The invention relates to a preparation method of difluoro-sulfimide and lithium difluoro-sulfimide, and belongs to the field of fluorine chemical synthesis. The preparation method comprises the steps that difluoro-sulfimide is obtained by adding fluoro-sulfoxide into a mixture of sulfamic acid or amino sulfonyl fluoride and fluorosulfuric acid for reacting and then subjected to recrystallization and filtration which are conducted at the temperature of minus 100 DEG C to 16 DEG C and / or reduced / normal-pressure distillation and purification which are conducted at the temperature of 60 DEG C to 169 DEG C; difluoro-sulfimide and a lithium-containing substance react in a solvent to obtain lithium difluoro-sulfimide, and then recrystallization, filtration and purification are conducted. According to the preparation method, difluoro-sulfimide can be prepared through one step, lithium difluoro-sulfimide is obtained through lithiation, and the prepared products can be purified; few steps are needed, the technology is simple, the process is easy to control, the requirement on production devices is low, the production efficiency, the product yield and the purity are high, and large-scale production and application can be achieved.

Description

technical field [0001] The invention relates to a preparation method of bisfluorosulfonimide and lithium bisfluorosulfonimide, belonging to the field of fluorine chemical synthesis. Background technique [0002] Bisfluorosulfonimide (chemical formula is HN(SO 2 F) 2 , referred to as HFSI) is the preparation of lithium bisfluorosulfonyl imide (chemical formula is LiN(SO 2 F) 2 , referred to as LiFSI) as the main raw material, with a boiling point of 170°C and a melting point of 17°C. Lithium bisfluorosulfonyl imide is an important fluorine-containing organic ion compound. It has suitable conductivity, high thermal stability, high electrochemical stability, and low probability of side reactions. It is an electrolyte substance with wide application prospects. Ion batteries, ionic liquid catalysts and supercapacitors all have important industrial application value. [0003] In the prior art, the preparation method of lithium bisfluorosulfonyl imide is mainly as follows: ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/096C01B21/086
CPCC01B21/096C01B21/086C01P2006/80
Inventor 蒋玉贵郗少杰杨献奎孟祥军李翔宇张净普
Owner 718TH RES INST OF CHINA SHIPBUILDING INDAL CORP
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