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Preparation method of pentaerythritol sulfate

A technology of pentaerythritol sulfate and pentaerythritol, which is applied in the field of preparation of pentaerythritol sulfate, can solve the problems of high reaction temperature, poor safety, and long reaction time, and achieve the effects of mild reaction conditions, avoiding corrosion, and short reaction time

Pending Publication Date: 2022-05-13
湖北澳格森化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The ubiquitous problem of this method is that due to the use of thionyl chloride in the reaction process, the introduced chloride ions are difficult to remove and affect the quality of the product, and thionyl chloride is relatively harmful to the human body, has poor safety, and the hydrochloric acid produced has corrosion to equipment. In addition, the oxidation system uses more NaIO 4 -RuCl 3 .3H 2 O system requires the use of catalysts containing rare metals rubidium and titanium and the oxidant NaIO 4 , the cost is too high, which is not conducive to the realization of large-scale industrial production
This method needs to be reacted at 60-150°C for 10 hours, and then kept at 120-150°C for 3-6 hours. There are problems of high reaction temperature and long reaction time. In addition, this process also needs to add a catalyst

Method used

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  • Preparation method of pentaerythritol sulfate
  • Preparation method of pentaerythritol sulfate
  • Preparation method of pentaerythritol sulfate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Put 13.6g of pentaerythritol, 8.0g of sulfur trioxide pyridine complex, and 250mL of dichloroethane distilled to remove water into a 500mL three-necked flask. After fully stirring and mixing, pass in nitrogen gas and react at room temperature for 4 hours. The liquid phase monitors the pentaerythritol raw material There is basically no residue, add 60g of anhydrous magnesium sulfate to the three-necked flask, heat up to 80°C for 4 hours, cool the reaction solution to room temperature and filter, the filtrate is distilled under reduced pressure, and the solid is separated by petroleum ether through a silica gel column, the target polarity The eluate concentration of the eluent is dried, can obtain the pentaerythritol sulfate ester of 20.4g white powder, yield 78%, liquid chromatography measures purity 99.57%, through the proton spectrum identification of mass spectrometry and nuclear magnetic resonance, be determined to be the pentaerythritol of target Sulfate compounds. ...

Embodiment 2

[0033] Into a 500mL three-necked flask, put 13.6g of pentaerythritol, 9.5g of sulfur trioxide pyridine complex, and 250mL of dichloroethane after molecular sieve dehydration was added. After fully stirring and mixing, nitrogen gas was introduced, and the reaction was carried out at room temperature for 2 hours. Liquid phase monitoring There is basically no pentaerythritol raw material left. Add 27g of dicyclohexylcarbodiimide to the three-necked flask, raise the temperature to 65°C and react for 6h, cool the reaction solution to room temperature and filter it. The filtrate is distilled under reduced pressure, and the solid is passed through a silica gel column with petroleum ether. Separation, the eluent concentration of target polarity, drying, can obtain the pentaerythritol sulfate ester of 18.2g white powder, yield 70%, liquid chromatography measures purity 99.45%, through the proton spectrum identification of mass spectrometry and nuclear magnetic resonance, Identify the ta...

Embodiment 3

[0037] Into a 500mL three-necked flask, put 13.6g of pentaerythritol, 7.0g of trimethylamine complex of sulfur trioxide, and 100mL of dichloroethane dried over anhydrous magnesium sulfate, stir and mix thoroughly, then pass in nitrogen gas, and react at room temperature for 2.5h, There is basically no remaining pentaerythritol raw material in the liquid phase monitoring. Add 36g of anhydrous magnesium sulfate to the three-necked flask, raise the temperature to 80°C for 4 hours, cool the reaction solution to room temperature and filter it. The filtrate is distilled under reduced pressure, and the solid is passed through a silica gel column with petroleum ether. Separation, the eluent of target polarity is concentrated, dried, can obtain the pentaerythritol sulfate ester of 19.5g white powder, yield 75%, liquid chromatography measures purity 99.76%, through the proton spectrum identification of mass spectrometry and nuclear magnetic resonance, Identify the target pentaerythritol ...

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Abstract

The invention discloses a preparation method of pentaerythritol sulfate, and belongs to the technical field of organic synthesis. The method comprises the following steps: carrying out sulfonation reaction on pentaerythritol and a sulfur trioxide Lewis base complex in a solvent under the protection of inert gas, adding a dehydrating agent to carry out ring closing reaction after the sulfonation reaction is completed, and carrying out post-treatment after the ring closing reaction is completed to obtain pentaerythritol sulfate, the molar ratio of the pentaerythritol to the sulfur trioxide Lewis base complex to the dehydrating agent is 1: (0.4-0.6): (2-5), the temperature of the sulfonation reaction is 0-35 DEG C, and the temperature of the ring closing reaction is 65-80 DEG C. According to the method, the product can be prepared through a one-pot method, the process steps are simple, the reaction conditions are milder, the raw material cost is greatly reduced, the product purity of the pentaerythritol sulfate is guaranteed, and the method is more suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method of pentaerythritol sulfate. Background technique [0002] Electrolyte additives refer to a small amount of additives added to the electrolyte to improve the electrochemical performance of the electrolyte and improve the quality of cathodic deposition. Electrolyte additives are some natural or synthetic organic or inorganic compounds, generally do not participate in the electrode reaction of the electrolysis process, but can improve the electrochemical performance of the electrolyte system, affect the discharge conditions of ions, and make the electrolysis process in a better state. The amount of electrolyte additives is generally small, but it is an indispensable part of the electrolyte system. [0003] The compound of pentaerythritol sulfate contains a sulfate group, and its structural formula is as follows: [0004] . [0005] Pentaerythritol...

Claims

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Application Information

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IPC IPC(8): C07D497/10
CPCC07D497/10
Inventor 周调杨
Owner 湖北澳格森化工有限公司