Preparation method of ethylene sulfate

A technology of vinyl sulfate and vinyl sulfite, which is applied in the field of preparation of vinyl sulfate, can solve the problems of high cost, low yield, and unsuitability for industrial production, and achieve the effects of low cost, less side reactions, and safe reaction

Active Publication Date: 2019-07-09
福建博鸿新能源科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] (3) obtain vinyl sulfate by dibromoethane and silver sulfate reaction, reaction formula is shown in formula III, and this reaction yield is only 23%, uses a large amount of silver sulfate simultaneously, and cost is high, and yield is low, is not suitable for suitability for suitability for industrialized production

Method used

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  • Preparation method of ethylene sulfate
  • Preparation method of ethylene sulfate
  • Preparation method of ethylene sulfate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] A kind of preparation method of vinyl sulfate, described preparation method comprises the following steps:

[0035] 1) Add 2500g of ethylene glycol into a 5000mL flask and stir in a normal temperature water bath (to avoid exothermic reaction to increase the reaction temperature), then add 4820g of thionyl chloride dropwise from the dropping funnel to react, and the dropping time is 1.5h , Continue to react for 2 hours after the dropwise addition is completed, and the tail gas generated during the reaction process is absorbed by water. After the reaction was completed, 15ml of 20% sodium hydroxide solution was added dropwise to neutralize slowly, and the reaction solution was detected to be neutral. The reaction solution was directly distilled under reduced pressure to obtain 4190 g of vinyl sulfite product with a GC purity of 99.8% and a yield of 96.2%.

[0036] 2) Add 900g dimethyl carbonate, 500g vinyl sulfite, 2g ditriphenylphosphine palladium chloride, 1g cuprous c...

Embodiment 2

[0039] 1) Under normal temperature water bath conditions, add 2500g of ethylene glycol into a 5000mL flask and stir, add 4792g of thionyl chloride dropwise from the dropping funnel to react, the dropping time is 1.5h, continue to react for 2h after the dropping is completed, the reaction process The exhaust gas produced is absorbed by water. After the reaction was completed, 15ml of 20% sodium hydroxide solution was added dropwise to neutralize slowly, and the reaction solution was detected to be neutral. The reaction solution was directly distilled under reduced pressure to obtain 4172 g of vinyl sulfite product with a GC purity of 99.8% and a yield of 95.8%.

[0040] 2) add 1100g dimethyl carbonate in the high pressure reactor, 500g vinyl sulfite, the catalyst 5.8g that embodiment 1 filters and obtains, and the reactor is filled with oxygen, and the pressure in the high pressure reactor is controlled to be 0.3Mpa (normal temperature), and the reaction The reaction was carri...

Embodiment 3

[0043] 1) Under normal temperature water bath conditions, add 2500g of ethylene glycol into a 5000mL flask and stir, add 5031g of thionyl chloride dropwise from the dropping funnel to react, the dropwise addition time is 1.5h, continue to react for 2h after the dropwise addition is completed, the reaction process The exhaust gas produced is absorbed by water. After the reaction was completed, 15ml of 20% sodium hydroxide solution was added dropwise to neutralize slowly, and the reaction solution was detected to be neutral. The reaction solution was directly distilled under reduced pressure to obtain 4233 g of vinyl sulfite product with a GC purity of 99.8% and a yield of 97.2%.

[0044] 2) Add 1000g dimethyl carbonate, 500g vinyl sulfite, ditriphenylphosphine palladium chloride 2g, cuprous chloride 1g in the high-pressure reactor, and the reactor is filled with compressed air, and the pressure in the high-pressure reactor is controlled to be 0.2Mpa (normal temperature), the r...

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Abstract

The invention discloses a preparation method of ethylene sulfate. The method comprises the following steps: firstly, ethylene glycol and thionyl chloride are used as raw materials to synthesize ethylene sulfite, the ethylene sulfite and air or oxygen are subjected to a direct oxidation reaction under the action of a catalyst to form ethylene sulfate, filtration is performed, washing is performed by using water, concentration is performed, crystallization is performed, and therefore the finished-product ethylene sulfate is obtained. The method provided by the invention adopts the novel catalystand uses the air or the oxygen as an oxidant, thereby effectively reducing use costs of the catalyst and the oxidant; and the method has less waste water, thereby being more in line with concepts ofenergy saving, greenness and environmental protection.

Description

technical field [0001] The present invention relates to the synthetic method of organic compound, relate in particular to a kind of preparation method of vinyl sulfate. Background technique [0002] Vinyl sulfate is a new type of electrolyte additive for lithium batteries. Its function is to inhibit the decline of the initial capacity of the battery, increase the initial discharge capacity, reduce the expansion of the battery after high temperature storage, and improve the charge and discharge performance and cycle times of the battery. At the same time, vinyl sulfate can be used as a hydroxyethylation reagent in organic synthesis to synthesize pharmaceutical intermediates, and can also be used as a raw material for synthesizing certain heterocyclic compounds for gelatin hardening, antihypertensive drugs, and new double surfactants. Therefore, it has broad research and development prospects. [0003] The preparation method of vinyl sulfate mainly comprises the following ste...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D327/10
CPCC07D327/10
Inventor 张茂华蒋永飞胡嗣敏
Owner 福建博鸿新能源科技有限公司
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