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Preparation method for difluorosulfimide lithium salt

A technology of bisfluorosulfonimide lithium salt and bisfluorosulfonimide is applied in the field of preparation of bisfluorosulfonimide lithium salt, which can solve the problem that LiF and LiFSI are not easily separated, the purity of LiFSI cannot be guaranteed, and it is not suitable for Industrial production and other problems, to achieve the effect of low cost, convenient recycling and application, and ensuring quality and purity

Active Publication Date: 2015-09-23
SHANGHAI CHEMSPEC CORP +1
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Problems solved by technology

[0003] Most of the synthetic methods of LiFSI are to synthesize bischlorosulfonimide (HClSI) first, and then react with MFn (M is the 11-15 group, the 4th-6th period element) to prepare the corresponding metal or organic base. The salt intermediate of bisfluorosulfonimide, and then with LiOH or Li 2 CO 3 Carry out cation exchange reaction and make LiFSI (US2013331609, US2012041233, EP2415757, US2011034716), the shortcoming of these methods is, it is difficult to carry out completely after exchange reaction reaches an equilibrium, and unreacted intermediate MSFI (M refers to metal cation, organic base Cations) are difficult to completely separate from LiSFI to obtain high-quality products
[0004] When using HClSI to directly react with LiF to prepare LiFSI (US2004097757), a large amount of corrosive gas HF will be produced, and the excess LiF and LiFSI are not easy to separate
[0005] Although it has also been reported that with purified potassium bisfluorosulfonimide (KFSI) and LiClO 4 LiFSI is prepared by metal exchange, but the potassium ions in the product are often high, which affects its practical application, and LiClO 4 and the resulting KClO 4 , there is a certain risk of explosion (Electrochimical Acta, 2012, 66, PP.320-324, Polyhedron, 2006, 25, PP. 1292-1298, CN101747242, CN101747243, CN101654229)
In addition, since LiClO 4 Generally, a slight excess is required to participate in the reaction, but due to its strong hygroscopicity, the final product contains a small amount of LiClO 4 Cannot be removed, so that the purity of the final product LiFSI cannot be guaranteed
[0006] US8377406 discloses the method that bisfluorosulfonimide (HFSI) directly reacts with lithium carbonate to prepare LiFSI in an aqueous solution, but this method also has obvious deficiencies, when HFSI dissolves in water, it exotherms violently, thereby causing the decomposition of HFSI, the The patent adopts the method of preparing HFSI aqueous solution at ultra-low temperature (-78°C) to solve the technical problem of violent heat release when HFSI dissolves in water, but this method increases a lot of energy consumption, and more importantly, LiFSI has a very good water solubility property, the extraction efficiency is very low, not suitable for industrial production

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  • Preparation method for difluorosulfimide lithium salt
  • Preparation method for difluorosulfimide lithium salt
  • Preparation method for difluorosulfimide lithium salt

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preparation example Construction

[0047] The invention provides a kind of preparation method of bisfluorosulfonyl imide lithium salt (LiFSI), comprising the following steps:

[0048] (1) Fluorination reaction: The intermediate bisfluorosulfonimide (HFSI) is synthesized from bischlorosulfonimide (HClSI) and hydrogen fluoride (HF) under the action of a catalyst. The reaction equation is as follows:

[0049]

[0050] In the step 1, the specific method of the fluorination reaction is: placing HClSI and the catalyst in the reaction device, and feeding HF gas to carry out the reaction.

[0051] In said step 1, the catalyst is preferably a Lewis acid, more preferably SbCl 5 , TiCl 4 , SnCl 4 , MoCl 5 The combination of one or more of them, the molar ratio of HClSI to catalyst is preferably 1:0.05‰~1:1‰, more preferably 1:0.1‰~1:0.5‰.

[0052] In the step 1, the molar ratio of HClSI to HF is preferably 1:1.4-1:4, more preferably 1:1.7-1:2.

[0053] In the step 1, the reaction temperature of the reaction system...

Embodiment 1

[0073] In the 1000mL reaction bottle, add HClSI 1235g, SbCl 5 0.5g, heat up to 100-105°C, slowly pass in about 230g of HF gas under stirring, cool down to room temperature after 20 hours of reaction, blow nitrogen for 15 hours, and obtain about 900g of crude product, short-distilled to obtain 865.6g of product, yield 82.8% .

Embodiment 2

[0075] In the 1000mL reaction bottle, add HClSI 1230g, MoCl 5 0.47g, heat up to 100-105°C, slowly pass in about 216g of HF gas under stirring, cool down to room temperature after 22 hours of reaction, blow nitrogen for 15 hours, and obtain about 896g of crude product, short-distilled to obtain 864.8g of product, yield 83.1% .

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Abstract

The invention relates to the field of lithium batteries and lithium capacitors, in particular to a preparation method for difluorosulfimide lithium salt and application of the difluorosulfimide lithium salt. The preparation method for the difluorosulfimide lithium salt, provided by the invention, comprises the following steps: (1) performing fluorination reaction: synthetizing midbody difluorosulfimide from dichlorosulfimide and hydrogen fluoride under the action of a catalyst; (2) performing reaction between the difluorosulfimide obtained in the step 1 and alkaline lithium, and performing solid-liquid separation after the reaction to obtain an LiFSI product. The preparation method for the difluorosulfimide lithium salt, provided by the invention, is low in cost, few in by-product and simple in post-treatment, and the quality and the purity of the product are ensured, therefore the preparation method which is capable of obtaining the high-quality and high-purity product and is economic and practical is provided; the preparation method is suitable for industrial production.

Description

technical field [0001] The invention relates to the field of lithium batteries and lithium capacitors, in particular to a preparation method and application of bisfluorosulfonimide lithium salt. Background technique [0002] In the periodic table, fluorine is the most electronegative element. Often after a compound is introduced with fluorine, its physical and chemical properties change significantly. Therefore, many fluorine-containing lithium compounds, such as lithium bistrifluoromethanesulfonylimide (LiTFSI) and lithium hexafluorophosphate (LiPF 6 ), are widely used to improve the electrical properties of batteries and capacitors. U.S. Patent US5916475 discloses a ratio of LiTFSI and LiPF 6 Lithium bisfluorosulfonyl imide (LiFSI), a fluorine-containing lithium salt with better thermal and chemical stability, higher electrical conductivity and lower corrosion rate, is considered to have the potential to replace LiPF 6 A bisfluorolithium salt of , will have excellent ap...

Claims

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Application Information

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IPC IPC(8): C01B21/096
CPCC01B21/0935C01B21/086C01B21/096
Inventor 何立杨东林盛平刘俊蔡国荣刘辉孙元健汤晓敏
Owner SHANGHAI CHEMSPEC CORP
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