Preparation method of dodecanethiol compound monomer

A technology of mercapto compounds and monomers, which is applied in the field of preparation of dodecyl mercapto compound monomers, can solve the problems of long process route, complicated operation and the like, and achieve the effects of long process route, complicated operation and large pollution.

Pending Publication Date: 2021-03-19
JIANGHAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The invention provides a method for preparing a dodecyl mercapto 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, Technical effect of energy saving and environmental protection

Method used

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  • Preparation method of dodecanethiol compound monomer
  • Preparation method of dodecanethiol compound monomer
  • Preparation method of dodecanethiol compound monomer

Examples

Experimental program
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Effect test

Embodiment 1

[0038] Add 194.67g of parent reactant 0.45mol 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 three-necked flask was completely dissolved, 0.35 g of 0.0035 mol of triethylamine catalyst was added dropwise therein, and 35.20 g of 0.1 mol of pentaerythritol tetraacrylate was measured with a graduated cylinder, and then added into the three-necked flask to continue stirring and reacting for 10 h , until TLC determined that the reaction was complete, and the stirring was stopped.

Embodiment 2

[0040] Add 216.3g of parent reactant 0.5mol pentaerythritol tetramercaptoacetate into a 500mL three-neck 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 60°C After the pentaerythritol tetramercaptoacetate in the three-necked flask was completely dissolved, 1.06 g of 0.0106 mol of triethylamine catalyst was added dropwise therein, and 35.20 g of 0.1 mol of pentaerythritol tetraacrylate was measured with a graduated cylinder, and then added into the three-necked flask to continue stirring for 12 hours. , until TLC determined that the reaction was complete, and the stirring was stopped.

Embodiment 3

[0042] Add 237.93g of parent reactant 0.55mol pentaerythritol tetramercaptoacetate into a 500mL three-neck 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 three-necked flask was completely dissolved, 1.06 g of 0.0106 mol of triethylamine catalyst was added dropwise therein, and then 35.20 g of 0.1 mol of pentaerythritol tetraacrylate was measured with a graduated cylinder, and added into the three-necked flask to continue stirring the reaction 14h, until TLC confirms that the reaction is complete, stop stirring.

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Abstract

The invention relates to a preparation method of a dodecamercapto compound monomer. The preparation method comprises the following steps of: by using pentaerythritol tetramercaptoacetate as a parent reactant and ethyl acetate as a solvent, forming a parent reactant solution, mechanically stirring the solution, heating the parent reactant solution in an oil bath; and carrying out Michael nucleophilic addition reaction on the solution and pentaerythritol tetraacrylate or di-(trimethylolpropane) tetraacrylate to prepare the dodecamercapto compound monomer. According to the preparation method, therequired 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 dodecyl mercapto 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 opt...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C319/18C07C323/52
CPCC07C319/18C07C323/52
Inventor 尤庆亮蒋湛钱新华肖本雄黄园曹一平刘志宏邹立勇刘继延肖标高淑豫刘学清周瑞雪胡思前
Owner JIANGHAN UNIVERSITY
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