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Bis(fluorosulfonyl)imide metal salt and method for preparing same

A technology of bisfluorosulfonimide and manufacturing method, which is applied in the fields of final product manufacturing, nitrogen and non-metallic compounds, sustainable manufacturing/processing, etc., can solve the problems such as unrecorded lithium salt molding methods, and achieve the goal of not being easy to scatter, not easy to Moisture absorption, easy handling effect

Active Publication Date: 2019-04-02
NIPPON SHOKUBAI CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the molding method for the obtained lithium salt is not described

Method used

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  • Bis(fluorosulfonyl)imide metal salt and method for preparing same
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  • Bis(fluorosulfonyl)imide metal salt and method for preparing same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0135] 11.70 g (0.45 mol) of LiF was weighed into the PFA reaction container. The reaction container was ice-cooled, and 95.9 g (0.53 mol) of HFSI [bisfluorosulfonimide] was charged. The reaction solution was heated to 120° C., and reacted for 1.5 hours. The reaction solution was heated under reduced pressure at 10 hPa, 140-145° C. for 2 hours. As a result, 73 g (molten state) of LiFSI was obtained.

[0136] The obtained LiFSI was sucked up with a glass pipette while maintaining the temperature of 140 to 145° C., and quickly dropped on a SUS304 plate heated to 60° C., and solidified to obtain pellets. The mass average particle diameter of the cured pellets was 4.8 mm. Moisture content was 54 mass ppm. In addition, the residual solvent amount was not more than the detection limit (1 mass ppm or less). The bulk specific gravity of the obtained pellets was 1.12. The above reactions and operations are carried out in a dry room with a dew point below -50°C.

Embodiment 2

[0138] 905 g (5.00 mol) of HFSI [bisfluorosulfonimide] and 132 g (5.10 mol) of LiF were charged into a stainless steel reaction vessel equipped with a nitrogen gas inlet tube and a reflux tube. While stirring the reaction solution, it heated to 150 degreeC. Thereafter, the pressure was reduced, and the reaction solution was heated at 10 hPa at 145 to 150° C. for 2 hours. As a result, 890 g (4.76 mol) of LiFSI (molten state) was obtained.

[0139] The reaction solution obtained in this way was connected to a transmission steel belt type granulation device (ROTOFORMM1) manufactured by SANDVIK Co., Ltd. through a heating pipe, and was pressure-fed thereto. The melt is extruded onto the transmission steel belt under certain conditions. Scrape the molten liquid extruded until the transmission steel belt makes one revolution directly with a scraper, and obtain pellets after one revolution. At this time, the crystal nucleation time was 1 minute, the crystal growth time was 2 minut...

Embodiment 3

[0142] 905 g (5.00 mol) of HFSI [bisfluorosulfonimide] and 129 g (4.98 mol) of LiF were charged into a stainless steel reaction vessel equipped with a nitrogen gas inlet tube and a reflux tube. Stirring the reaction solution, it heated at 150 degreeC, and reacted for 1.5 hours. The reaction solution was heated under reduced pressure at 10 hPa, 145-150° C. for 2 hours. As a result, 890 g (4.76 mol) of LiFSI (molten state) was obtained.

[0143]A pipe for taking out was connected to this reactor, and the LiFSI melt was taken out by pressurizing from a nitrogen gas introduction pipe. The melt was drawn into a mold having a depth of 1 cm, a width of 1.75 cm, and a width of 2 cm, and the mold was cooled at 50° C. to obtain a massive LiFSI shaped body. The obtained LiFSI shaped body was measured with a caliper, and the minimum length was 10 mm. In addition, the water content was 7 mass ppm. In addition, the residual solvent amount was not more than the detection limit. The abov...

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Abstract

This bis(fluorosulfonyl)imide metal salt is an alkali metal salt or alkaline earth metal salt of bis(fluorosulfonyl)imide, has an average particle size of at least 0.1 mm, and has an average moistureabsorption rate of 2.5 mass ppm / cm2 min when sealed in a PE bag having a thickness of 80 [mu]m for 30 minutes at 23 DEG C and 65% humidity.

Description

technical field [0001] The present invention relates to a bisfluorosulfonimide metal salt and a method for producing the metal salt. Background technique [0002] Salts of fluorosulfonimides, derivatives thereof as having N(SO 2 F) group or N(SO 2 f) 2 It is useful as an intermediate of a compound based on an electrolyte, an additive to an electrolyte of a fuel cell, a selective electrophilic fluorinating agent, a photoacid generator, a thermal acid generator, a near-infrared absorber Pigments and the like are compounds useful for various purposes. [0003] Salts of fluorosulfonimides generally have high hygroscopicity and tend to absorb moisture or scatter easily when they are made into fine powders. Therefore, there is a problem that it is difficult to handle. [0004] Patent Document 1 describes a method for producing granules or powders of a disulfonamide alkali metal salt having a mode particle diameter of 80 μm or less. However, in the production method of the dis...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/086H01M8/10
CPCH01M8/10C01B21/086C01P2004/20C01P2004/32C01P2004/60C01P2006/90C01P2004/30C01P2004/90Y02E60/50Y02E60/10H01M8/1016C01P2004/61C01P2006/40Y02P70/50
Inventor 山田宪侍清水大嗣胜山裕大水野弘行奥村康则板山直彦深田幸宏佐藤裕一樋口泰弘山内隆广
Owner NIPPON SHOKUBAI CO LTD
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