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Preparation method of trimercapto compound monomer

A technology of compound and trimercapto, which is applied in the field of preparation of monomers of trimercapto compounds, can solve the problems of cumbersome operation and long process route, and achieve the effect of cumbersome operation, long process route and large pollution

Inactive Publication Date: 2021-02-02
JIANGHAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The invention provides a preparation method of trimercapto compound monomer, which solves the technical problems of long process route and cumbersome operation in the preparation method of polythiol in the prior art, and realizes simple reaction, high efficiency, high yield and energy saving Environmentally friendly technical effects

Method used

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  • Preparation method of trimercapto compound monomer
  • Preparation method of trimercapto compound monomer
  • Preparation method of trimercapto compound monomer

Examples

Experimental program
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Effect test

Embodiment 1

[0037] Add 47.58g of parent reactant 0.11mol pentaerythritol tetramercaptoacetate into a 500ml three-necked flask equipped with a condenser, thermometer, water separator, and oil bath, use 300mL ethyl acetate as a solvent, stir mechanically, and heat in an oil bath at 50°C After the pentaerythritol tetramercaptoacetate in the there-necked flask was completely dissolved, 0.19 g of 0.0019 mol of triethylamine catalyst was added dropwise therein, and then 18.52 g of 0.1 mol of cyclotrimethylolpropane methylal acrylate was measured with a graduated cylinder. Add the three-necked flask and continue to stir the reaction for 10 h, until TLC (TLC is the English abbreviation of thin layer chromatography, the same hereinafter) confirms that the reaction is complete, and the stirring is stopped.

Embodiment 2

[0039] Add 56.24g of parent reactant 0.13mol pentaerythritol tetramercaptoacetate into a 500ml three-necked flask equipped with a condenser, thermometer, water separator, and oil bath, use 300mL ethyl acetate as solvent, stir mechanically, and heat in an oil bath at 60°C After the pentaerythritol tetramercaptoacetate in the there-necked flask was completely dissolved, 0.56 g of 0.0056 mol of triethylamine catalyst was added dropwise therein, and 18.52 g of 0.1 mol of cyclotrimethylolpropane methylal acrylate was measured with a graduated cylinder. Add the three-necked flask and continue to stir the reaction for 12h until TLC confirms that the reaction is complete, then stop stirring.

Embodiment 3

[0041] Add 64.89g of parent reactant 0.15mol pentaerythritol tetramercaptoacetate into a 500ml three-necked flask equipped with a condenser, thermometer, water separator, and oil bath, use 300mL ethyl acetate as a solvent, stir mechanically, and heat in an oil bath at 70°C After the pentaerythritol tetramercaptoacetate in the there-necked flask was completely dissolved, 0.93 g of 0.0093 mol of triethylamine catalyst was added dropwise, and then 18.52 g of 0.1 mol of cyclotrimethylolpropane methylal acrylate was measured with a graduated cylinder. Add the three-necked flask and continue to stir the reaction for 14h until TLC confirms that the reaction is complete, then stop stirring.

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Abstract

The invention relates to a preparation method of a trimercapto compound monomer. The preparation method comprises the following steps: using pentaerythritol tetramercaptoacetate as a parent reactant and ethyl acetate as a solvent, forming a parent reactant solution, mechanically stirring, heating in an oil bath, using triethylamine as a catalyst and carrying out Michael nucleophilic addition reaction with cyclotrimethylolpropane methylal acrylate to prepare the trimercapto compound monomer. According to the preparation method, the required super-dendritic polymercaptan compound can be successfully synthesized through one-step reaction, and the preparation method is simple and efficient in reaction, relatively high in yield, energy-saving and environment-friendly.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to a preparation method of a trimercapto compound monomer. Background technique [0002] In organic chemistry, a class of non-aromatic compounds containing mercapto functional groups (-SH) is called thiols. From a structural point of view, it can be seen that the oxygen in ordinary alcohols is replaced by sulfur. Mercaptans can be used as drugs, antidotes and rubber vulcanization accelerators. [0003] The traditional methods for preparing mercaptans, especially polythiols, have long process routes, high energy consumption, heavy pollution, low yields, and cumbersome operations. For example, the traditional thiourea hydrolysis method is used to prepare mercaptans. The process is mainly divided into three steps: generation of isothiouronium salts; alkali hydrolysis; acidification to generate mercaptans. [0004] The synthesis of polythiol compounds requires us to optimize...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D319/06C08G75/045
CPCC07D319/06C08G75/045
Inventor 尤庆亮肖本雄钱新华蒋湛黄园刘志宏邹立勇刘继延肖标高淑豫刘学清曹一平周瑞雪胡思前
Owner JIANGHAN UNIVERSITY
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