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The preparation method of 1,3-propane sultone

A technology of propane sultone and allyl alcohol, applied in the direction of organic chemistry and the like, can solve the problems of low reaction yield, low total yield, high cost and the like, and achieves the effect of simple process and no pollution

Active Publication Date: 2012-02-08
ZHANGJIAGANG HUASHENG CHEM CO LTD
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  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

[0004] About the preparation method of 1,3-propane sultone, there are reports both at home and abroad, such as the direct dehalogenation of sodium halopropane sulfonate to prepare 1,3-propane sultone, but this method is rare due to the presence of raw materials And the price is expensive, and factors such as low reaction yield simultaneously bring a lot of inconvenience to production
In addition, the Chinese patent specification with application number 200710048316.8 discloses a method for synthesizing 1,3-propane sultone. In the method, sodium bisulfite and allyl alcohol are used as raw materials, and 3-hydroxyl is catalyzed by infrared irradiation. -1-propanesulfonate, then neutralized in the presence of concentrated hydrochloric acid to generate 3-hydroxyl-1-propanesulfonic acid, and then extracted with n-butanol and then molecularly distilled to obtain the target substance. The disadvantage of this method is that the steps are long and the total The yield is low, only 70%

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  • The preparation method of 1,3-propane sultone

Examples

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Effect test

Embodiment 1

[0026] In a three-necked flask containing 12g of ammonium sulfite, 120g of water, and 62g of polyethyl ether-18-crown-62g, add dropwise an aqueous solution of 58g of allyl alcohol, 20g of ammonium sulfite and 98g of ammonium bisulfite while stirring at 40°C A total of 500g, the dropping time is 1 hour, and the temperature is kept for 4 hours. After the reaction was completed, 200g of water was distilled off, and the filtrate was obtained by cooling and filtration. The filtrate was distilled to obtain a solid hydroxypropanesulfonate amine, and 400g of absolute ethanol was added, stirred into a white paste, and 36.5g of dry hydrogen chloride gas was introduced, and the temperature was kept at 50°C. After the reaction is completed, cool and filter to obtain an ethanol solution of hydroxypropanesulfonic acid. First remove the ethanol by distillation under reduced pressure, and then collect 110g of fractions at 150-160°C / 10mmHg by high-vacuum rectification. Analyze by GC / MS mass spe...

Embodiment 2

[0028] In a three-neck flask filled with 15g of sodium sulfite, 150g of water, and 12-crown-42g, 58g of allyl alcohol, 28g of sodium sulfite and 112g of sodium bisulfite were added dropwise while stirring at 50°C. hours, keep warm for 4 hours. After the reaction was completed, 300g of water was distilled off, and the filtrate was obtained by cooling and filtration. The filtrate was distilled to dryness to obtain a solid sodium hydroxypropanesulfonate, and 500g of absolute ethanol was added, stirred into a white paste, and 36.5g of dry hydrogen chloride gas was introduced, and the temperature was maintained at 50°C. After the reaction is completed, cool and filter to obtain the ethanol solution of hydroxypropanesulfonic acid. First, the ethanol is removed by vacuum distillation, and then high vacuum distillation collects 112g of 150-160°C / 10mmHg fraction, which is analyzed by GC / MS mass spectrometry, m / z: 122, 58, proved to be Molecular ion characteristic fragments are measur...

Embodiment 3

[0030] In a three-neck flask filled with 16 g of potassium sulfite, 160 g of water, and 62 g of dicyclohexane-18-crown-62 g, 58 g of allyl alcohol, 40 g of potassium sulfite and potassium bisulfite were added dropwise while stirring at 100°C. A total of 800 g of 200 g of aqueous solution was added dropwise for 1 hour, and the temperature was kept for 4 hours. After the reaction was completed, 400g of water was distilled off, and the filtrate was obtained by cooling and filtration. The filtrate was evaporated to dryness to obtain a solid of potassium hydroxypropanesulfonate, and 600g of absolute ethanol was added, stirred into a white paste, and 36.5g of dry hydrogen chloride gas was introduced, and the temperature was maintained at 50°C. After the reaction is completed, cool and filter to obtain ethanol solution of hydroxypropanesulfonic acid. First, remove the ethanol by distillation under reduced pressure, and then collect 115g of 150-160°C / 10mmHg fraction by high-vacuum rect...

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Abstract

The invention discloses a preparation method of 1,3-propane sultone, which uses hydrogen sulfite, sulfite and allyl alcohol as raw materials, water as a medium, and crown ether as a catalyst to react at a certain temperature to form The reaction mixture of hydroxypropanesulfonate, the obtained reaction mixture containing hydroxypropanesulfonate is reacted under acidifying agent and solvent environment to generate the reaction mixture containing hydroxypropanesulfonic acid, and then the hydroxypropanesulfonic acid obtained by the above reaction is The acid reaction mixture is subjected to high-temperature rectification to obtain the target product 1,3-propane sultone. The advantages of the present invention are: the raw materials are cheap and easy to obtain, the raw materials are not highly toxic and explosive, have no pollution to the environment, and the process is simple , the purity reaches more than 99.95%, and the yield is as high as more than 90%.

Description

technical field [0001] The present invention relates to a process for the preparation of 1,3-propane sultone. Background technique [0002] 1,3-propane sultone is mainly used in fuel, medicine, lithium battery and other fields, and its structural formula is: [0003] [0004] About the preparation method of 1,3-propane sultone, there are reports both at home and abroad, such as the direct dehalogenation of sodium halopropane sulfonate to prepare 1,3-propane sultone, but this method is rare due to the presence of raw materials And the price is expensive, and factors such as low reaction yield simultaneously bring a lot of inconvenience to production. In addition, the Chinese patent specification with application number 200710048316.8 discloses a method for synthesizing 1,3-propane sultone. In the method, sodium bisulfite and allyl alcohol are used as raw materials, and 3-hydroxyl is catalyzed by infrared irradiation. -1-propanesulfonate, then neutralized in the presence ...

Claims

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Application Information

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IPC IPC(8): C07D327/04
Inventor 张先林刘东杨志勇林刚李伟峰
Owner ZHANGJIAGANG HUASHENG CHEM CO LTD
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