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The preparation method of 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 price of finished PS, high cost, restriction of downstream application of PS, etc., and achieves low cost, mild process conditions and simple equipment. Effect

Active Publication Date: 2016-07-06
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 shortcomings: the above-mentioned methods all use propylene alcohol as a raw material, and the cost is relatively high, resulting in higher prices for finished PS. Limits the downstream application of PS

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 1) Sulfonation process:

[0030] 144g of sodium metabisulfite was added to the three-necked flask equipped with a thermometer, a condenser and a stirring device, 268g of deionized water was injected into it, and the temperature was raised to 50° C. until the sodium metabisulfite was completely dissolved. 76.5 g of allyl chloride was slowly added dropwise. After the dropwise addition, use sodium hydroxide solution to control pH=8~9. When the reaction does not have allyl chloride reflux, it proves that the reaction reaches 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 white powdery sodium allyl sulfonate.

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

[0032] In the there-necked flask equipped with a thermometer, a condenser and a stirring device, add 143 g of sodium allyl sulfonate in step 1, inject 352 g of a 50% aqueo...

Embodiment 2

[0036] 1) Sulfonation process:

[0037] 189g of sodium sulfite was added to the three-necked flask equipped with a thermometer, a condenser and a stirring device, 200 g of deionized water was injected into it, and the temperature was raised to 50° C. until the sodium sulfite was completely dissolved. 76.5 g of allyl chloride was slowly added dropwise. After the dropwise addition, use NaOH solution to control pH=8~9, when there is no allyl chloride reflux in the reaction, it proves that the reaction reaches 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 white powdery sodium allyl sulfonate.

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

[0039] Add 141 g of sodium allyl sulfonate in step 1 to the there-necked flask equipped with a thermometer, a condenser and a stirring device, inject 450 g of a 40% aqueous sulfuric acid soluti...

Embodiment 3

[0043] 1) Sulfonation process:

[0044]Add 240 g of potassium sulfite to the three-necked flask equipped with a thermometer, a condenser and a stirring device, inject 500 g of deionized water into it, and heat it 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 pH=8~9, when there is no allyl chloride reflux in the reaction, it proves that the reaction reaches 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 white powdery sodium allyl sulfonate.

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

[0046] Add 143 g of sodium allyl sulfonate in step 1 to the there-necked flask equipped with a thermometer, a condenser and a stirring device, inject 380 g of a 40% aqueous sulfuric acid solution by mass fraction into i...

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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 specifically relates to a preparation method of 1,3-propane sultone using allyl chloride as 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. It has strong reactivity with alcohols, phenols, thiols, amines, etc., and can convert the required substituents - (CH 2 ) 3 SO 3 The introduction of H to 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. What is particularly important is that the addition of PS to the non-hydrolytic solution of lithium-ion batteries can improve cycle life and storage stability, so the PS market prospect is very broad. [0003] The main methods currently used to produce 1,3-propane sultone...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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