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Preparation method of 1,3-propane sulfone

A technology of propane sultone and sodium hydroxypropanesulfonate, applied in 1 field, can solve the problems of increased chloride ion content, large amount of solid waste, influence on product purity, etc., and achieves reduction of chloride ions, simple reaction raw materials, and improved conversion. rate effect

Active Publication Date: 2016-11-23
ZHANGJIAGANG HICOMER CHEM CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The shortcoming of above-mentioned preparation method is: (1) reaction temperature is high, and by-product is more, and molar yield is not high; (2) still residue after high-temperature rectification is no longer processed, so solid waste is more; (3) Acidification with hydrochloric acid will increase the chloride ion content of the reactants, which will affect the purity of the product

Method used

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  • Preparation method of 1,3-propane sulfone
  • Preparation method of 1,3-propane sulfone
  • Preparation method of 1,3-propane sulfone

Examples

Experimental program
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Embodiment 1

[0022] (1) Add 104g (1mol) of sodium bisulfite and 312g of deionized water into a three-neck flask with mechanical stirring, thermometer, dropping device, and condenser, and stir, then add 58g of allyl alcohol dropwise at 30°C (1mol) and initiator, thereby reaction generates sodium 3-hydroxypropanesulfonate, initiator is mixed by sodium persulfate 11.9g, hydrogen peroxide 1.7g, ferrous sulfate 3.8g and deionized water 69.6g, drips Time 1 hour, be incubated 7 hours, analyze and sample then, after propenyl alcohol is reacted to below 0.2% of its consumption, reaction completes; (2) add sulfuric acid 50g ( 0.5mol) to carry out acidification, the acidification temperature is 50 ℃, and the acidification time is 2 hours, distills out excess water 254.4g after acidification finishes, then adds 600g dehydrated alcohol and carries out extraction and cooling filtration, thereby obtains the 3-hydroxypropanesulfonic acid Ethanol solution; (3) the ethanol solution of 3-hydroxypropanesulfon...

Embodiment 2

[0024] (1) Add 208g (2mol) of sodium bisulfite and 624g of deionized water into a three-neck flask with mechanical stirring, thermometer, dropping device, and condenser, and stir, then add 58g of allyl alcohol dropwise at 80°C (1mol) and initiator, thus react and generate sodium 3-hydroxypropanesulfonate, initiator is mixed by sodium persulfate 2.4g, hydrogen peroxide 0.34g, ferrous sulfate 0.76g and deionized water 14g, dropwise time 1 hour, insulation 2 hours, analysis and sampling then, after propenyl alcohol is reacted to below 0.2% of its consumption, the reaction is complete; (2) add sulfuric acid 50g (0.5 g) in the aqueous solution containing 3-hydroxy propane sulfonate that reaction obtains mol) for acidification, the acidification temperature is 60°C, and the acidification time is 1 hour. After the acidification ends, 320 g of excess water is distilled off, and then 800 g of absolute ethanol is added for extraction and cooled and filtered to obtain an ethanol solution ...

Embodiment 3

[0026](1) Add 156g (1.5mol) of sodium bisulfite and 468g of deionized water into a three-neck flask with mechanical stirring, thermometer, dropping device, and condenser, and stir, then add propenyl alcohol dropwise at 50°C 58g (1mol) and initiator, thus react and generate sodium 3-hydroxypropanesulfonate, initiator is mixed by sodium persulfate 7.2g, hydrogen peroxide 1.0g, ferrous sulfate 2.3g and deionized water 42g, dropwise Time 1 hour, insulation 4 hours, analysis and sampling then, after propenyl alcohol is reacted to below 0.2% of its consumption, reaction completes; (2) add sulfuric acid 50g ( 0.5mol) for acidification, the acidification temperature is 50°C, and the acidification time is 2 hours. After the acidification ends, 270 g of excess water is distilled off, and then 1200 g of absolute ethanol is added for extraction and cooling and filtration, thereby obtaining ethanol of 3-hydroxypropanesulfonic acid solution; (3) the ethanol solution of 3-hydroxypropanesulfo...

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Abstract

The invention discloses a preparation method of 1,3-propane sulfone. The preparation method comprises the following steps: firstly, using propenol and sodium hydrogen sulfite as raw materials, taking deionized water as a medium, and reacting under catalytic addition reaction of an initiator to generate 3-sodium hydroxy propanesulfate; secondly, adding sulfuric acid into a reaction solution for acidating, then removing excessive water by distilling, subsequently adding anhydrous ethanol, and extracting and filtering to obtain an ethanol solution of 3-hydroxy propanesulfate; thirdly, distilling the ethanol solution of the 3-hydroxy propanesulfate at normal pressure first to remove ethanol, and then rectifying to obtain the 1,3-propane sulfone; fourthly, adding an aqueous solution of sodium hydroxide into cauldron bottom residue to carry out hydrolysis, then adding sulfuric acid for acidating, subsequently adding anhydrous ethanol, extracting and filtering to obtain an ethanol solution of 3-hydroxy propanesulfonic acid, then distilling the ethanol solution of the 3-hydroxy propanesulfonic acid at normal pressure to remove ethanol, and then rectifying to obtain the 1,3-propane sulfone. According to the preparation method, the reaction temperature is reduced; in addition, a product is high in mole yield and few in solid wastes; the high-purity product is easily obtained.

Description

technical field [0001] The invention relates to the field of electrolyte additives for lithium ion batteries, in particular to a preparation method for 1,3-propane sultone which can be used as an additive for electrolytes of lithium ion batteries. Background technique [0002] The structural formula of 1,3-propane sultone is: 1,3-propane sultone is a new type of additive that can make the electrolyte of lithium-ion batteries more effective. A 1,3-propane sulfonic acid is disclosed in the Chinese invention patent with the application number CN200810234140.X The preparation method of lactone, the preparation method is: using bisulfite, sulfite and propenyl alcohol as raw materials, water as medium, crown ether as catalyst, reacting at a temperature of 40 to 100°C to produce hydroxyl-containing propanesulfone acid salt reaction mixture, then add hydrochloric acid to the reaction mixture containing hydroxypropanesulfonate for acidification, then add absolute ethanol to extract...

Claims

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Application Information

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IPC IPC(8): C07D327/04
CPCC07D327/04
Inventor 姚双开庞靖李苑许国荣许逸达刘冬
Owner ZHANGJIAGANG HICOMER CHEM CO LTD
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