Sulfate preparation method

A sulfuric acid ester and sulfuryl fluoride technology, which is applied in the field of sulfuric acid ester preparation, can solve the problems of high investment in environmental protection, high manufacturing cost, and affecting product quality.

Active Publication Date: 2018-08-17
SHANGHAI CHEMSPEC CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The ubiquitous problem of this method is that due to the use of thionyl chloride in the reaction process, the introduction of chloride ions is difficult to remove, which affects the quality of the product, and the oxidation step operation and material costs are high.
The method is cumbersome to operate, the oxidizing reagent is expensive, and

Method used

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preparation example Construction

[0049] The present invention provides a kind of preparation method of sulfuric acid ester on the one hand, the chemical structural formula of described sulfuric acid ester is shown in formula I, and the preparation method of described sulfuric acid ester can comprise: formula II compound is mixed with sulfur under the condition that reaction solvent exists Acyl fluoride reaction, preparation obtains the compound of formula I, and reaction equation is as follows:

[0050]

[0051]Among them, n can be selected from 0, 1, 2, 3 or 4; M can be selected from Li, Na, K; R1, R2, R3, R4, R5, R6 can be independently selected from H, C1~C4 alkyl , C6-C18 aryl, C1-C4 alkoxy, chlorine or bromine. The C1-C4 alkyl group may be, for example, methyl, ethyl, propyl, n-propyl, isopropyl, butyl, n-butyl, isobutyl, sec-butyl, tert-butyl and the like. The C6-C18 aryl group may be, for example, phenyl, naphthyl, fluoranthenyl, fluorenyl, tetrahydronaphthyl, indanyl, anthracenyl and the like. Th...

Embodiment 1

[0071] Preparation of vinyl sulfate:

[0072] Put 200ml of toluene, 75g of ethylene glycol (1.2mol) and 80g (2mol) of sodium hydroxide into the reaction bottle equipped with a water separator, heat up to the reflux temperature and react, and observe that water continuously distills out in the water separator. After 20 hours, the reaction was completed, and the solvent in the system was evaporated to dryness to obtain ethylene glycol disodium salt, which weighed 107.3 g and was set aside.

[0073] In a 1000mL reaction flask, under the protection of nitrogen, add 106.0g of ethylene glycol disodium salt and 500mL of dichloromethane prepared in the above steps, keep the internal temperature at -10~10°C and slowly pass in 148.7g (1.47mol) of sulfuryl fluoride gas, keep warm React for 1.5 hours, blow nitrogen gas for 1 hour, filter, and desolvate the filtrate under reduced pressure at 40°C to obtain the crude solid. Cool down to room temperature, filter and dry to obtain 91.5 g of ...

Embodiment 2

[0075] Preparation of propylene sulfate:

[0076] Drop into 200ml toluene, 1,3-propanediol 100g (1.31mol) and 110g sodium methylate (2.04mol) in the reaction bottle that water separating device is housed, stir and be warming up to the low boiler in reflux separation system, slowly cool down after 15 hours, Add 200ml of dichloromethane to form a sodium salt suspension for later use.

[0077] In a 2000mL autoclave, replace the air with nitrogen. After adding 500ml of dichloromethane, 145.3g of sulfuryl fluoride was introduced into the autoclave under the protection of nitrogen to maintain an internal temperature of -10-0°C, and the sodium salt suspension was dropped into the autoclave, and kept for 2 hours for reaction. After the reaction, blow the system with nitrogen to remove excess sulfuryl fluoride gas, filter the reaction solution, and precipitate it to dryness under reduced pressure. Add 300ml of methyl tert-butyl ether, 15-crown-50.05g, 18-crown-6 0.05g to the crude pro...

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Abstract

The invention relates to the field of organic synthesis, and especially relates to a sulfate preparation method. The invention provides a sulfate preparation method. According to the preparation method, a compound represented by a formula (II) reacts with sulfuryl fluoride in the presence of a reaction solvent to prepare a compound represented by a formula (I). During the sulfate preparation process, the introduction of water and chlorine ions is avoided effectively, the situation that the product is degraded and the chlorine ion content is high is avoided therefore; moreover, the steps of thepreparation method are simple and short, the raw material are common chemical products on the market, the kinds of raw materials and the side reactions are few, and the yield is high. The manufacturing cost is low, only recyclable organic solvents are used, the reaction byproduct is a single inorganic salt solid and can be easily recovered, no wastewater is generated, the environment is better protected, and the sulfate preparation method is green and environmentally friendly and is suitable for industrial large scale production.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a preparation method of sulfuric acid ester. Background technique [0002] In recent years, with the widespread application of lithium-ion batteries in the field of electric vehicles, the temperature adaptability of lithium-ion batteries has attracted more and more attention. In most parts of our country, the temperature in summer can reach about 38°C, while in winter it can be as low as about -10°C, which poses a severe test to the high and low temperature performance of batteries. Sulfate ester compounds have a wide range of uses, especially cyclic sulfate ester compounds are increasingly used as new additives for solid electrolyte phase interface films of lithium batteries and lithium electronic electrolytes to improve high and low temperature performance of batteries. Studies have shown that cyclic sulfate esters can be reduced in the electrolyte to produce sulfite compounds...

Claims

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Application Information

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IPC IPC(8): C07D327/10
CPCC07D327/10C07C29/70C07C31/30
Inventor 何立李晓亮田中杨建华
Owner SHANGHAI CHEMSPEC CORP
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