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Preparation method of alkyl lithium sulfate

A technology of lithium alkyl sulfate and silicon alkyl sulfate is applied in the field of preparation of lithium ion battery electrolyte additive lithium alkyl sulfate, which can solve the problem that the transesterification efficiency is difficult to reach 100%, the reaction of lithium chlorosulfonate is incomplete, and the Lithium chlorosulfonate is difficult to purify and other problems, to achieve the effect of loose reaction conditions, difficult to remove and easy to obtain

Pending Publication Date: 2022-02-25
山东永浩新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] However, the disadvantage of this method is that, firstly, in the first step of lithiation process, dihydrocarbyl sulfate is easy to react in an environment with water to produce sulfate, which makes it difficult to purify the product, and both sulfate and acidity will increase; secondly , when preparing alkyl sulfates modified by special groups, first, there is no corresponding dihydrocarbyl sulfate one-step reaction preparation, and second, if it is prepared by transesterification, the transesterification efficiency is difficult to reach 100%, that is, the product may contain Saturated alkyl lithium sulfate and alkyl lithium sulfate with special group modification, more difficult to separate
[0006] In addition, by reacting chlorosulfonic acid with the corresponding lithium salt, lithium chlorosulfonate is prepared, and then the corresponding alkyl alcohol is removed from HCl under the action of an acid-binding agent, and the corresponding alkyl lithium sulfate can also be prepared, but this In this method, there is still the incomplete situation of the lithium chlorosulfonate reaction, which causes the product to be mixed with lithium chlorosulfonate and is difficult to purify

Method used

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  • Preparation method of alkyl lithium sulfate

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Effect test

Embodiment 1

[0035] A preparation method for alkyl lithium sulfate, comprising the following steps:

[0036] 1) Add 116.5 g (1 mol) of chlorosulfonic acid and 400 ml of dichloromethane to the flask under 0°C ice-water bath and nitrogen protection, and gradually add 102 g (1 mol) of triethylamine to the chlorosulfonic acid and trimethylchlorosilane 108.6 g (1 mol) mixed solution, after the dropwise addition, the temperature was raised to normal temperature, and the reaction was continued for 12 h until no precipitation occurred; after the reaction was completed, filtered to remove the insoluble triethylamine hydrochloride , After removing dichloromethane by rotary evaporation, re-filter, and then carry out rectification operation on the filtrate, collect the fraction at 60~70°C to obtain silicon chlorosulfonate.

[0037] 2) Put 94 g (0.5 mol) of silicon chlorosulfonate into a flask, and add 200 ml of dichloromethane after dehydration in an ice-water bath at 0°C under the protection of nitro...

Embodiment 2

[0041] A kind of preparation method of alkyl lithium sulfate, on the basis of embodiment 1, step 1) adopts following method:

[0042]1) Add 142 g (1.05 mol) of sulfonyl chloride into the flask under the protection of nitrogen in an ice-water bath at 0°C, and add zinc chloride with a molar fraction of 3%, then gradually add hexamethyl dichloride dropwise to the sulfonyl chloride Siloxane 162 g (1 mol), after the dropwise addition, raise the temperature to normal temperature, and continue to react for 12 h; after the reaction, filter, and then carry out rectification operation on the filtrate, remove the previous fraction (below 50°C), and collect Distillate at 60~70°C to obtain silicon chlorosulfonate.

[0043] Step 2) and step 3) are the same as in Example 1.

[0044] It was characterized by proton nuclear magnetic spectrum and ion chromatography, and the analysis and calculation showed that the yield of the product was 78.5%, and the purity was greater than 99.5% (characteri...

Embodiment 3

[0046] A preparation method of alkyl lithium sulfate, on the basis of Example 1, step 2) propylene alcohol is replaced by butenyl alcohol, the obtained in step 2) is silicon butenyl sulfate, and the final product obtained in step 3) is butane Lithium Alkenyl Sulfate.

[0047] Characterized by proton nuclear magnetic spectrum and ion chromatography, analysis and calculation can be obtained, the product yield is 79.6%, and the purity is greater than 99.5% (NMR characterization).

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Abstract

The invention discloses a preparation method of alkyl lithium sulfate, and relates to the technical field of lithium ion battery manufacturing, in particular to a preparation method of alkyl lithium sulfate serving as an electrolyte additive of a lithium ion battery. Alkyl lithium sulfate is speculated to possibly have the effects of reducing the internal resistance of the battery and improving the high-temperature storage performance and the cycle performance of the battery, while existing preparation methods generally have the problems of low reaction exchange efficiency and difficulty in product purification. According to the method, silicon chlorosulfonate reacts with alkyl alcohol and an acid-binding agent to obtain silicon alkyl sulfate ester, then the silicon alkyl sulfate ester reacts with a lithium source to obtain lithium alkyl sulfate, a thought of introducing sulfonate radicals into a high-molecular polymer material is provided, the method is suitable for preparing lithium alkyl sulfonate modified by various different groups, the cost is low, the conversion rate is high, the purification process is simple, the purity is high, and the method is suitable for industrial large-scale production of the alkyl lithium sulfate.

Description

technical field [0001] The invention discloses a preparation method of alkyl lithium sulfate, which relates to the technical field of manufacturing lithium ion batteries, and in particular relates to a preparation method of alkyl lithium sulfate, an electrolyte additive for lithium ion batteries. Background technique [0002] Lithium battery electrolyte is the carrier of ion transmission in the battery. It is usually prepared from high-purity organic solvents, electrolyte lithium salts, additives and other raw materials under certain conditions and in a certain proportion. However, during the cycle, unstable components in the electrolyte, such as carbonate solvents, are prone to redox reactions at the positive and negative electrodes of the lithium battery and decompose or deposit on the electrode surface. The gas generated by the decomposition will cause the battery to expand. The bulging reduces the service life of the battery and affects the safety of the battery; the loo...

Claims

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Application Information

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IPC IPC(8): C07C305/04C07C303/24C07F7/08H01M10/0567
CPCC07C303/24H01M10/0567C07F7/0834C07C305/04Y02E60/10
Inventor 牛会柱牛超
Owner 山东永浩新材料科技有限公司
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