Method for preparing 1,3-propane sultone

A technology of propane sultone and sodium allyl sulfonate, applied in the direction of organic chemistry and the like, can solve the problems of high cost, high price of finished PS, restrict downstream application of PS, etc., and achieves low cost, simple equipment and mild process conditions. Effect

Active Publication Date: 2015-07-29
RONGCHENG QINGMU CHEM MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The methods for synthesizing PS introduced in the above-mentioned documents and patents have all carried out beneficial experiments and broadened the thinking, but there are also shortcomi

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 1) Sulfonation process:

[0030] Add 144g of sodium metabisulfite into a three-necked flask equipped with a thermometer, a condenser, and a stirring device, inject 268g of deionized water into it, and raise the temperature to 50°C until the sodium metabisulfite is completely dissolved. 76.5 g of allyl chloride was slowly added dropwise. After the dropwise addition, use sodium hydroxide solution to control the pH=8~9, when there is no reflux of allyl chloride in the reaction, it proves that the reaction has reached the end. The reaction solution was distilled under reduced pressure until a white solid was precipitated, then cooled and filtered. The filtrate was dried to obtain 143 g of sodium allyl sulfonate in the form of white powder.

[0031] 2) Reverse Markov addition and acidification process:

[0032] Add allyl sodium sulfonate 143g in step 1 in the there-necked flask equipped with thermometer, condensing tube, stirring device, inject massfraction wherein into 5...

Embodiment 2

[0036] 1) Sulfonation process:

[0037] Add 189g of sodium sulfite into a three-necked flask equipped with a thermometer, a condenser, and a stirring device, inject 200g of deionized water into it, and raise the temperature to 50°C until the sodium sulfite is completely dissolved. 76.5 g of allyl chloride was slowly added dropwise. After the dropwise addition, use NaOH solution to control the pH=8~9, when there is no reflux of allyl chloride in the reaction, it proves that the reaction has reached the end point. The reaction solution was distilled under reduced pressure until a white solid was precipitated, then cooled and filtered. The filtrate was dried to obtain 141 g of sodium allyl sulfonate in the form of white powder.

[0038] 2) Reverse Markov addition and acidification process:

[0039] Add 141g of sodium allyl sulfonate in step 1 to the there-necked flask equipped with a thermometer, condenser, and stirring device, inject 450g of sulfuric acid aqueous solution wit...

Embodiment 3

[0043] 1) Sulfonation process:

[0044]Add 240 g of potassium sulfite into a three-necked flask equipped with a thermometer, a condenser, and a stirring device, inject 500 g of deionized water into it, and raise the temperature to 50° C. until the potassium sulfite is completely dissolved. 76.5 g of allyl chloride was slowly added dropwise. After the dropwise addition, use NaOH solution to control the pH=8~9, when there is no reflux of allyl chloride in the reaction, it proves that the reaction has reached the end point. The reaction solution was distilled under reduced pressure until a white solid was precipitated, then cooled and filtered. The filtrate was dried to obtain 143 g of sodium allyl sulfonate in the form of white powder.

[0045] 2) Reverse Markov addition and acidification process:

[0046] Add 143g of sodium allyl sulfonate in step 1 to a three-neck flask equipped with a thermometer, a condenser tube, and a stirring device, inject 380g of a 40% aqueous soluti...

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Abstract

The invention provides a method for preparing 1,3-propane sultone (PS). The method comprises the following steps: dripping allyl chloride into a certain quantity of a sodium metabisulfite aqueous solution to prepare sodium allyl sulfonate; carrying out reaction between sodium allyl sulfonate and sulfuric acid under the existence of a catalyst; carrying out hydrolysis under an alkali condition; carrying out acidation to prepare 3-hydroxypropanesulfonic acid; conducting cyclodehydration under the existence of an inert dehydrating agent to prepare 1,3-propane sultone. The method has the advantages that allyl chloride which is cheap is taken as a raw material; the target product with relatively high yield is prepared according to the four steps of substitution, addition reaction, hydrolysis and cyclization; the reaction condition is mild; the suitability for mass production is realized.

Description

technical field [0001] The invention belongs to the technical field of fine chemical synthesis, and in particular relates to a preparation method of 1,3-propane sultone using allyl chloride as a raw material. Background technique [0002] 1,3-Propane sultone (hereinafter referred to as PS) is a colorless liquid or white crystal in appearance. PS is a very important intermediate in organic synthesis, which has strong reactivity with alcohols, phenols, thiols, amines, etc., and can replace the required substituent -(CH 2 ) 3 SO 3 The introduction of H into O, S, and N can improve the surface properties of substances, and is also an important raw material for the synthesis of cationic or zwitterionic surfactants. The most important thing is that the non-hydrolyzed solution of lithium-ion batteries added by PS can improve the cycle life and storage stability, so the PS market prospect is very broad. [0003] At present, the main methods for producing 1,3-propane sultone (PS)...

Claims

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Application Information

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IPC IPC(8): C07D327/04
CPCC07D327/04
Inventor 刘晓波李维平张晓宁李晓明王芳芳孙朋波
Owner RONGCHENG QINGMU CHEM MATERIALS
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