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Method for preparing ethylene sulfite

A technology of vinyl sulfite and ethylene oxide, applied in the field of catalytic synthesis of vinyl sulfite, to achieve the effect of improving purity and yield and low price

Active Publication Date: 2011-06-15
BYD CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But in CN85100162A, there is no any teaching or revelation that this catalyst can be used for the preparation of vinyl sulfite

Method used

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  • Method for preparing ethylene sulfite

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preparation example Construction

[0008] The preparation method of vinyl sulfite of the present invention comprises carrying out contact reaction of sulfur dioxide and ethylene oxide under the condition that the complex compound of polyethylene glycol (PEG) and metal halide is used as a catalyst. The reaction is shown in the following formula.

[0009]

[0010] The usage amount of the catalyst can be 0.01-0.5 times, preferably 0.05-0.2 times of the weight of ethylene oxide.

[0011] Polyethylene glycol (PEG) has the effect of complexing alkali metal and alkaline earth metal ions, thereby improving the catalytic ability of negative ions. The catalyst used in the present invention can be a complex formed by polyethylene glycol (PEG) and metal halide, wherein the molar ratio of polyethylene glycol (PEG) to metal halide is (1.0-4.0): 1 . The molecular weight range of the polyethylene glycol (PEG) may be 190-880. The metal halide may be an alkali metal halide and / or an alkaline earth metal halide, preferably ...

Embodiment 1

[0016] In 200 milliliters of autoclaves with electromagnetic stirring, add 108 grams of vinyl sulfite and 6.0 grams of catalyst (produced by 5.0 grams of polyethylene glycol (PEG) 200 (produced by Guangzhou Jietu Chemical Company) and 1.0 grams of potassium iodide Mixed complex), after replacing the air with nitrogen, add 100 grams of ethylene oxide. Then, heat the temperature-raising reaction mixture, and when the reaction temperature rises to 130° C., feed sulfur dioxide to 5 MPa, and react for about 2 hours while maintaining the temperature and pressure. Pass cooling water in the autoclave, cool to 50 ℃, emit the product in the still, obtain the thick product of the vinyl sulfite of 347.9 grams. The resulting crude product was purified by vacuum distillation to obtain 341.4 grams of vinyl sulfite, which was analyzed by chromatography with a purity of 99.5% and a yield of 94.6% (relative to ethylene oxide).

Embodiment 2

[0018] In a 200 ml autoclave with electromagnetic stirring, add 80 grams of vinyl sulfite and 8.0 grams of catalyst (produced by 6.4 grams of polyethylene glycol (PEG) 400 (produced by Guangzhou Jietu Chemical Company) and 1.6 grams of bromine A complex formed by mixing sodium chloride), after replacing the air with nitrogen, add 100 grams of ethylene oxide. Then, heat the temperature-raising reaction mixture, and when the reaction temperature rises to 150° C., feed sulfur dioxide to 4 MPa, and react for about 2 hours while maintaining the temperature and pressure. Pass cooling water in the autoclave, be cooled to 50 ℃, emit the product in the still, obtain the thick product of the vinyl sulfite of 332.2 grams. The obtained crude product was subjected to vacuum distillation and purification to obtain 323.5 grams of vinyl sulfite. Through chromatographic analysis, the purity was 99.2%, and the yield was 98.4% (relative to ethylene oxide).

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Abstract

The invention relates to a method for catalyzing and synthesizing ethylene sulfite through the reaction between sulfur dioxide and epoxy ethane. The preparation method of the ethylene sulfite provided by the invention comprises that the sulfur dioxide is contact reacted with the epoxy ethane under the existence of catalyst, and is characterized in that the catalyst is complex compound synthesizedby polyethylene glycol (PEG) and metal halide. According to the preparation method of the ethylene sulfite of the invention, less catalyst that is complexly synthesized by the low-price and safe and non-toxic polyethylene glycol (PEG) and metal halide is employed to facilitate reaction under the mild conditions, thus improving the purity and the yield of the ethylene sulfite.

Description

technical field [0001] The present invention relates to the catalytic synthesis of vinyl sulfite through the reaction of sulfur dioxide and ethylene oxide. Background technique [0002] Vinyl sulfite is an important organic chemical product and an intermediate in the synthesis of other chemical products. It can be used as an additive for organic electrolytes in lithium-ion secondary batteries. [0003] The preparation method of known vinyl sulfite is at present, with oxirane, sulfur dioxide is raw material, uses the halide of alkali metal halide, alkaline earth metal halide or iron, cobalt, nickel as catalyzer, at high temperature (220 ℃~300℃) and high pressure (above 10MPa) to prepare vinyl sulfite. The disadvantage of this method is that the reaction conditions are high, the yield is low, and there are many by-products generated. [0004] CN85100162A discloses a method for synthesizing ethylene carbonate, which uses ethylene oxide and carbon dioxide as raw materials, and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D327/10
Inventor 周刚
Owner BYD CO LTD
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