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Preparation method of 1,3-propane sultone

A technology of propane sultone and sodium polyacrylate, which is applied in the direction of organic chemistry, can solve the problems of high equipment requirements and high cost of reaction conditions, and achieve the effect of stable crystal lattice, low equipment requirements and simple operation

Inactive Publication Date: 2018-12-14
SUZHOU GAIDE FINE MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But above-mentioned method is raw material with propylene alcohol, and cost is high, and reaction condition is high to equipment requirement

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A preparation method of 1,3-propane sultone, comprising the following steps:

[0028] (1) Calcium chloride is dissolved in deionized water and stirred until the solid is dissolved to obtain a calcium chloride solution with a mass concentration of 15%; citric acid is added to the calcium chloride solution and continued to stir until the solid is dissolved to obtain a mixed solution A; Wherein, the mass ratio of described calcium chloride, citric acid is 5:0.3;

[0029] (2) Sodium polyacrylate is dissolved in deionized water and stirred to obtain a sodium polyacrylate solution with a mass concentration of 3%, and it is slowly added to the mixed solution A prepared above. Under the state of stirring 30min, mixed solution B is obtained; Wherein, the rate of addition of the polyacrylic acid sodium solution is 1ml / L; The mass ratio of polyacrylic acid sodium, calcium chloride is 0.1:1;

[0030] (3) preparing a mass concentration of 20% sodium carbonate solution, then quickly...

Embodiment 2

[0035] A preparation method of 1,3-propane sultone, comprising the following steps:

[0036] (1) Calcium chloride is dissolved in deionized water and stirred until the solid is dissolved to obtain a calcium chloride solution with a mass concentration of 35%; citric acid is added to the calcium chloride solution and continued to stir until the solid is dissolved to obtain a mixed solution A; Wherein, the mass ratio of described calcium chloride, citric acid is 7:0.3;

[0037] (2) Sodium polyacrylate is dissolved in deionized water and stirred to obtain a sodium polyacrylate solution with a mass concentration of 8%, and it is slowly added to the above-mentioned mixed solution A, and after the addition is completed, the solution is heated at 5000 rpm Stir 50min under the state, make mixed solution B; Wherein, the drip rate of described polyacrylic acid sodium solution is 5ml / L; The mass ratio of polyacrylic acid sodium, calcium chloride is 0.6:1;

[0038] (3) preparing a mass co...

Embodiment 3

[0043] A preparation method of 1,3-propane sultone, comprising the following steps:

[0044] (1) Calcium chloride is dissolved in deionized water and stirred until the solid is dissolved to obtain a calcium chloride solution with a mass concentration of 20%; citric acid is added to the calcium chloride solution and continued to stir until the solid is dissolved to obtain a mixed solution A; Wherein, the mass ratio of described calcium chloride, citric acid is 5.5:0.3;

[0045](2) Sodium polyacrylate is dissolved in deionized water and stirred to obtain a sodium polyacrylate solution with a mass concentration of 4%, and it is slowly added to the mixed solution A prepared above. Stir 35min under the state, make mixed solution B; Wherein, the drip rate of described polyacrylic acid sodium solution is 2ml / L; The mass ratio of polyacrylic acid sodium, calcium chloride is 0.2:1;

[0046] (3) preparing a mass concentration of 20% sodium carbonate solution, then quickly adding the ab...

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Abstract

The invention discloses a preparation method of 1,3-propane sultone. The preparation method comprises the steps as follows: firstly, preparing a calcium chloride solution, adding citric acid to prepare a mixed solution A, mixing the mixed solution A with a sodium polyacrylate to prepare a mixed solution B, then, quickly adding the mixed solution B to a sodium carbonate solution for precipitation to prepare porous calcium carbonate, and soaking the porous calcium carbonate in a peroxybenzoic acid solution to prepare a catalyst; mixing sodium allylsulfonate and a sulfuric acid solution, adding the catalyst for a reaction, adding an ethanol solution of sodium hydroxide for a reaction, and finally, adding hydrochloric acid for acidization to prepare 3-hydroxypropanesulfonic acid; mixing prepared 3-hydroxypropanesulfonic acid and n-hexane, adding the mixture to a three-neck flask to be stirred to react, cooling a product to the room temperature after the reaction, and performing reduced pressure distillation to prepare the target product 1,3-propane sultone. The method is simple to operate, low in energy consumption and high in product yield.

Description

Technical field: [0001] The invention relates to the field of organic synthesis, in particular to a preparation method of 1,3-propane sultone. Background technique: [0002] 1,3-propane sultone is a new functional fine chemical material. It can react with many kinds of compounds under very mild conditions, and accurately provide sulfonic acid groups, thereby endowing these compounds with new properties (such as hydrophilicity, antistatic properties, etc.), and is an excellent general-purpose sulfonic acid It is also a key raw material for the synthesis of important electroplating additive intermediates PPS, UPS, DPS, MPS, ZPS, POPS, SP and other products. It is an important pharmaceutical intermediate, and is also used in brighteners, dyes, diionic surfactants, sulfonating agents, lithium batteries, etc. [0003] At present, the preparation methods for producing 1,3-propane sultone mainly include the following: (1) using propylene alcohol as a raw material, reacting with s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D327/04
CPCC07D327/04
Inventor 李晓明
Owner SUZHOU GAIDE FINE MATERIALS CO LTD
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