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Preparation method of fluoroalkyl sultone

A technology of fluoroalkyl sultone and fluoroalkyl sulfonic acid, which is applied in the field of synthesis of electrolyte additives, can solve the problems of difficult acquisition of raw materials, excessive three wastes, cumbersome post-processing, etc., and achieve low cost and original The effect of simple excipients and simple preparation methods

Pending Publication Date: 2021-10-26
四川研一新材料有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Alcohol substrates containing fluorine and bromine in this route are not easy to obtain and have a high cost of raw materials, and the reaction requires a large amount of water or alkali to remove by-products of sulfurous acid and bromide
There are many three wastes, and the post-processing is cumbersome

Method used

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  • Preparation method of fluoroalkyl sultone
  • Preparation method of fluoroalkyl sultone

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preparation example Construction

[0023] A method for preparing fluoroalkyl sultones, comprising the following steps: putting alkyl sultones, initiators, acid-binding agents, and solvents into a high-pressure reaction kettle, and nitrogen atmosphere replacement protection; The mixed gas of sulfuryl fluoride and nitrogen is quantified, and after being sealed, the heat preservation reaction is carried out before the temperature rise reaction; after the reaction is completed, the liquid in the kettle is washed, extracted, and devolatilized to obtain a concentrated liquid, and the concentrated liquid is subjected to vacuum distillation to obtain fluoroalkyl sulfonic acid Lactone.

[0024] The molar ratio of alkyl sultone, initiator, and acid-binding agent is 1: (0.001-0.1): (0.5-5); the amount of solvent used is 3-10 times the molar amount of alkyl sultone; A certain amount of sulfuryl fluoride gas is fed into the reaction first, and then a quantitative amount of nitrogen gas is fed to dilute and pressurize; when ...

Embodiment 1

[0043] Add 1,3-propane sultone (12.2g, 0.1mol), azobisisobutyronitrile (16mg, 0.0001mol) and triethylamine (5.06g, 0.05mol), acetonitrile (12.2g, 0.3mol), nitrogen atmosphere replacement protection, the temperature of the kettle is down to -20 ℃, after sealing, feed high-purity sulfuryl fluoride (10.2g, 0.1mol), the flow rate is 5ml / min, then feed high-purity nitrogen (28g, 1mol), seal the reactor, the pressure of the autoclave is 2.4Mpa, start stirring, the holding time is 1 hour, the temperature is raised to 0°C and the reaction is held for 8 hours, and the reaction is over Afterwards, the pressure is released, the still liquid is filtered, the solvent is recovered under reduced pressure, the concentrated solution is obtained through water washing, extraction, and volatilization, and the concentrated solution is subjected to vacuum distillation to obtain 3-fluoro-1,3-propane sultone ( 10.85g, 0.0774mol), selectivity 83.6%, yield 77.4%, purity 99.82% (GC), moisture content 12...

Embodiment 2

[0045] At 30°C, 1,3-propane sultone (12.2 g, 0.1 mol), azobisisobutyronitrile (1.64 g, 0.01 mol), pyridine (39.6 g, 0.5mol), sulfolane (36.05g, 0.3mol), nitrogen atmosphere replacement protection, after sealing, pass into high-purity sulfuryl fluoride (51.03g, 0.5mol), flow rate is 5ml / min, then pass into high-purity nitrogen (1.4g , 0.05mol), the reactor is sealed, the pressure of the autoclave is 1.5Mpa, the stirring is started, the holding time is 8 hours, the temperature is raised to 180°C and the reaction is held for 8 hours, after the reaction is completed, the pressure is released, and the still liquid is filtered and reduced The solvent was recovered under pressure, washed with water, extracted, and devolatilized to obtain a concentrated solution, and the concentrated solution was subjected to vacuum distillation to obtain perfluoro-1,3-propane sultone (19.833g, 0.0862mol), with a selectivity of 92.7%, The yield is 86.2%, the purity is 99.93% (GC), the water content is...

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Abstract

A preparation method of fluoroalkyl sultone comprises the following steps: adding alkyl sultone, an initiator, an acid-binding agent and a solvent into a high-pressure reaction kettle, and carrying out nitrogen atmosphere replacement protection; introducing quantitative mixed gas of sulfuryl fluoride and nitrogen at low temperature, sealing, carrying out heat preservation reaction, and then carrying out heating reaction; and after the reaction is finished, washing, extracting and devolatilizing kettle liquid to obtain a concentrated solution, and rectifying the concentrated solution under reduced pressure to obtain the fluoroalkyl sultone. The preparation method is simple and easy to operate, raw materials and auxiliary materials are simple and easy to obtain, the cost is low, and the prepared fluoroalkyl sultone is high in purity and can meet the application of lithium battery electrolyte.

Description

technical field [0001] The invention relates to a synthesis method of an electrolyte additive, in particular to a preparation method of fluoropropane sultone. Background technique [0002] The S-containing electrolyte additive can form a film on the surface of the positive and negative electrodes of the lithium-ion battery to improve the high-temperature cycle and storage performance under high-voltage and high-nickel systems (ACS Appl. Energy Mater. 2018, 1, 2582-2591); Similar substances such as FEC can form an organic-inorganic composite SEI film on the surface of the negative electrode to improve the cycle stability of the Si negative electrode (Energy Storage Materials 2017, 6, 26-35). [0003] Patent document KR10-0908570 reports a synthetic route of fluorosultone, which uses a chlorinated reagent to replace the sultone, and then performs a halogen displacement reaction. The first step of the reaction is chlorination, the product is chlorosultone, and the reaction sel...

Claims

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Application Information

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IPC IPC(8): C07D327/04C07D327/06C07D327/02H01M10/0525H01M10/0567
CPCC07D327/04C07D327/06C07D327/02H01M10/0567H01M10/0525H01M2300/0025Y02E60/10
Inventor 刘新平钱超岳敏
Owner 四川研一新材料有限责任公司
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