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Preparation method for synthesizing pentaerythritol bicyclic sulfate

A technology of pentaerythritol and synthesis method, which is applied in the direction of organic chemistry, etc., can solve the problems such as the influence of battery electrical performance, great harm, and poor safety.

Pending Publication Date: 2019-08-23
杨记
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] (2) Synthesis of 3,3,9,9-tetroxide-2,4,8,10-tetraoxa-3,9-dithiaspiro[5.5] in the next step with pentaerythritol and sulfone dichloride as a catalyst Undecane, the 3,3,9,9-tetroxide-2,4,8,10-tetraoxa-3,9-dithiaspiro[5.5]undecane produced by the above method contains chlorine impurities, As a lithium battery material, it has an impact on the electrical performance of the battery. In addition, thionyl chloride or thionyl chloride is relatively harmful to the human body and has poor safety. The HCl produced is corrosive and requires high equipment requirements.

Method used

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  • Preparation method for synthesizing pentaerythritol bicyclic sulfate
  • Preparation method for synthesizing pentaerythritol bicyclic sulfate
  • Preparation method for synthesizing pentaerythritol bicyclic sulfate

Examples

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Effect test

Embodiment 1

[0020] Add 252g of dimethyl sulfate, 0.1g of catalyst titanate, and 500g of benzene solvent into a 2L four-necked bottle at room temperature, pass through nitrogen protection, stir and heat up to 60 degrees to completely dissolve, and continue to heat up to 120 degrees after the dissolution is completed. Add pentaerythritol in batches within 10 hours. Since pentaerythritol is an insoluble white powder, pentaerythritol will disappear only through reaction. Observe the disappearance of pentaerythritol every time to judge the reaction termination point. Methanol will be produced during the reaction, and it will be fractionated by circulating nitrogen and condensation The methanol gas is taken out of the reactor for recovery. When 136~200g of pentaerythritol is added, no powder disappears, indicating that the reaction has reached the end point, and the excess pentaerythritol is cooled and filtered, and then rectified to obtain 3,3,9,9-tetraoxo-2,4,8,10-tetraoxo- The crude product ...

Embodiment 2

[0022] Add 504g of dimethyl sulfate, 0.1g of catalyst p-toluenesulfonic acid, and 800g of benzene solvent into a 3L four-necked bottle at normal temperature, and pass through nitrogen protection, stir and heat up to 80 degrees to completely dissolve, and continue to heat up to 150 degrees after the dissolution is completed. Add pentaerythritol in batches within 10 hours. Since pentaerythritol is an insoluble white powder, pentaerythritol will only disappear through reaction. Observe the disappearance of pentaerythritol every time to judge the end point of the reaction. Methanol will be produced during the reaction. Through circulating nitrogen and condensation Fractional distillation recovers methanol. When 272~400g of pentaerythritol is added, no powder disappears, indicating that the reaction has reached the end point, and the excess pentaerythritol is cooled and filtered, and then rectified to obtain 3,3,9,9-tetraoxo-2,4,8,10-tetraoxo- The crude product of 3,9-dithiaspiro[5...

Embodiment 3

[0024] Add 252g of dimethyl sulfate, 0.1g of catalyst titanium sulfate, and 500g of benzene solvent into a 2L four-necked bottle at normal temperature, pass through nitrogen protection, stir and heat up to 80 degrees to completely dissolve, and continue to heat up to 150 degrees after the dissolution is completed. Add pentaerythritol in batches within an hour. Since pentaerythritol is an insoluble white powder, pentaerythritol will only disappear through reaction. Observe the disappearance of pentaerythritol every time to judge the reaction termination point. Methanol will be produced during the reaction, and it will be recovered by circulating nitrogen and condensation fractionation Methanol. When 130~200g of pentaerythritol is added, no powder disappears, indicating that the reaction has reached the end point, and the excess pentaerythritol is cooled and filtered, and then rectified to obtain 3,3,9,9-tetraoxo-2,4,8,10-tetraoxo- The crude product of 3,9-dithiaspiro[5.5]undeca...

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Abstract

The invention discloses a preparation method for synthesizing pentaerythritol bicyclic sulfate from dimethyl sulfate and pentaerythritol by a one-step synthesis process under the action of a catalyst.The method which adopts the pentaerythritol and dimethyl sulfate as raw materials comprises the following steps: heating a solvent, the dimethyl sulfate and the catalyst to 60-65 DEG C under the protection of nitrogen to achieve full dissolving, adding the pentaerythritol in batches while refluxing at 70 DEG C to start a reaction, continuously reacting and heating to 150 DEG C, carrying out condensation refluxing to separate a reactant methanol in order to obtain crude pentaerythritol bicyclic sulfate, filtering and distilling the crude product obtained by the reaction, washing and purifyingthe distilled crude product with a solvent, and performing vacuum drying to obtain the target product that is purified pentaerythritol bicyclic sulfate. The compound prepared by the method has the advantages of novel structure, high product purity, low raw material cost, simplicity and high efficiency in one-step synthesis, easiness in disposal of wastes, and high economical property of the reaction process, and can be used for lithium ion battery electrolyte additives to improve the comprehensive performances of batteries.

Description

technical field [0001] The invention relates to a novel sulfur-containing electrolyte additive 3,3,9,9-tetroxide-2,4,8,10-tetraoxa-3,9-dithiaspiro[ 5.5] Synthetic preparation method of undecane. Background technique [0002] 3,3,9,9-tetroxide-2,4,8,10-tetraoxa-3,9-dithiaspiro[5.5]undecane is a raw material for organic synthesis and can be used as a lithium ion Secondary battery electrolyte additives, the current synthesis methods are as follows: [0003] (1) Use pentaerythritol and thionyl chloride nucleophilic substitution reaction to synthesize pentaerythritol dithionyl, and then continue to react under the action of oxidant and catalyst to obtain 3,3,9,9-tetroxide-2,4,8,10- Tetraoxa-3,9-dithiaspiro[5.5]undecane; [0004] (2) Synthesis of 3,3,9,9-tetroxide-2,4,8,10-tetraoxa-3,9-dithiaspiro[5.5] in the next step with pentaerythritol and sulfone dichloride as a catalyst Undecane, the 3,3,9,9-tetroxide-2,4,8,10-tetraoxa-3,9-dithiaspiro[5.5]undecane produced by the above m...

Claims

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Application Information

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IPC IPC(8): C07D497/10
CPCC07D497/10
Inventor 杨记
Owner 杨记
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