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Preparation method of pentafluorophenyl methanesulfonate

A technology of pentafluorophenyl methanesulfonate and methanesulfonic anhydride is applied in the field of preparation of pentafluorophenyl methanesulfonate, and can solve the problems of easily causing danger, potential safety hazard, easy introduction of chloride ions, and the like, To achieve the effect of easy transportation and storage, reduced difficulty and cost, and simple purification process

Inactive Publication Date: 2018-12-07
SHANSHAN ADVANCED MATERIALS QUZHOU CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] However, this method has the following disadvantages: firstly, methanesulfonyl chloride is a flammable liquid and is a highly toxic chemical, which has many safety hazards during transportation, use and storage; secondly, the reactivity of methanesulfonyl chloride is too high. High, it is difficult to control in the reaction, and it is easy to cause danger; third, it is easy to introduce chloride ions in the reaction process, and chloride ions are very harmful to lithium-ion batteries, and the purification cost is relatively high
The reaction activity of this method is too low, and the reaction conversion rate is low, resulting in great difficulty in purification.

Method used

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  • Preparation method of pentafluorophenyl methanesulfonate
  • Preparation method of pentafluorophenyl methanesulfonate
  • Preparation method of pentafluorophenyl methanesulfonate

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Embodiment

[0037] (1) Synthesis of Pentafluorophenyl Methanesulfonate

[0038] Take by weighing 50g pentafluorophenol (0.272mol) and certain quality methanesulfonic anhydride (by the proportioning in the specific example in the table) respectively in the glove box, and be dissolved in the organic solvent of 200ml respectively; Pentafluorophenol / Organic solvent was added to a three-necked flask, and 80ml of acid-binding agent was added at the same time; under normal temperature and nitrogen protection, methanesulfonic anhydride / organic solvent was added dropwise, and the dropping time was 5h. After the dropwise addition, adjust the temperature to 50°C and continue the reaction for 24h.

[0039] (2) purification of pentafluorophenyl methanesulfonate

[0040] There are two main purification methods of pentafluorophenyl methanesulfonate:

[0041] Method 1: After the crude pentafluorophenyl methanesulfonate is prepared, the temperature of the reaction solution is lowered to -5-5°C, the rea...

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Abstract

The invention discloses a preparation method of pentafluorophenyl methanesulfonate. The preparation method comprises the steps of with methane sulfonic anhydride as a sulfonating reagent, dissolving methane sulfonic anhydride into an organic solvent for later use; dissolving pentafluorophenol into the organic solvent, simultaneously adding an acid-binding agent, dropwise adding the organic solventdissolved with methane sulfonic anhydride so as to prepare a pentafluorophenyl methanesulfonate crude product, and purifying and drying the crude product, so as to obtain a pentafluorophenyl methanesulfonate finished product. The preparation method has the beneficial effects that the use risk of highly toxic chemicals is avoided, and the sulfonating reagent, namely methane sulfonic anhydride, isa white crystalline solid and is convenient to transport and store; the reaction activity of methane sulfonic anhydride is between the reaction activities of methylsufonyl chloride and methanesulfonicacid, and reaction conditions are mild; chloride ions are not generated in the reaction, so that the purifying difficulty of the chloride ions is reduced, and the purifying cost is lowered; and besides, the purifying process is simple, and hydrolysis of sulfonate is reduced by virtue of an ice water extraction manner, so that the yield is increased.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a preparation method of pentafluorophenyl methanesulfonate. Background technique [0002] With the rapid development of the new energy industry, the market share of lithium-ion batteries is gradually increasing, and the importance of lithium battery materials is becoming increasingly prominent. In the development of lithium-ion battery electrolytes, in order to adapt to the development conditions of high specific energy and high voltage, research on new electrolyte additives for high nickel high voltage and silicon carbon negative electrodes has become a hot spot. [0003] Fluoroethylene carbonate (FEC) is an excellent additive that can well form an SEI film on the surface of the negative electrode, prevent the embedding of solvent molecules in the graphite negative electrode, and protect the negative electrode material. However, with the increase in energy density requirements,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/66C07C303/28C07C303/44
CPCC07C303/28C07C303/44C07C309/66
Inventor 杜建委钟子坊杨冰周彤吴财平
Owner SHANSHAN ADVANCED MATERIALS QUZHOU CO LTD
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