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Preparation method of semi-aromatic polythioesters

A polythioester and semi-aromatic technology, which is applied in the field of preparation of semi-aromatic polythioester, can solve the problems of unsuitability for large-scale production and high energy consumption of the synthesis route, and achieve the improvement of mechanical properties and optical properties, The effect of mild reaction conditions and a wide range of sources

Active Publication Date: 2019-05-03
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since the reaction process requires high temperature, high pressure and removal of small molecular compounds, the synthetic route consumes a lot of energy and is not suitable for large-scale production

Method used

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  • Preparation method of semi-aromatic polythioesters
  • Preparation method of semi-aromatic polythioesters
  • Preparation method of semi-aromatic polythioesters

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Dry the 100mL pressure-resistant glass bottle equipped with a magnet at 130°C for more than 12 hours, vacuumize it until it cools down to room temperature, and flush it with nitrogen to prepare for use. Under nitrogen protection, a certain amount of catalyst 3a and cocatalyst bis(triphenylphosphoryl)ammonium chloride were weighed at room temperature, and the molar ratio of catalyst to cocatalyst was 1 / 1. Then add alkylene oxide 1a and thioanhydride 2a, the molar ratio of epoxy hydrocarbon, thioanhydride and chromium metal catalyst is 2000 / 1000 / 1. It was then placed in an oil bath at 25°C and magnetic stirring was started. Reaction 4h, stop stirring. A very small amount of the reaction mixture was removed for the 1 H NMR and GPC tests. 1 H NMR test showed that the conversion rate of thioanhydride was >99%, and GPC test showed that the polymer molecular weight was 35600 g / mol. Purify the remaining reaction polymer. Purification of the polymer: first dissolve the crude...

Embodiment 2

[0035] Dry the 100mL pressure-resistant glass bottle equipped with a magnet at 130°C for more than 12 hours, vacuumize it until it cools down to room temperature, and flush it with nitrogen to prepare for use. Under nitrogen protection, a certain amount of catalyst 3a and cocatalyst bis(triphenylphosphoryl)ammonium chloride were weighed at room temperature, and the molar ratio of catalyst to cocatalyst was 1 / 2. Then add alkylene oxide 1b and thioanhydride 2a, the molar ratio of alkylene oxide, thioanhydride and chromium metal catalyst is 2000 / 1000 / 1. Then put it into an oil bath at 50°C and start magnetic stirring. Reaction 16h, stop stirring. A very small amount of the reaction mixture was removed for the 1 H NMR and GPC tests. 1 H NMR test showed that the conversion rate of thioanhydride was >99%, and GPC test showed that the polymer molecular weight was 41200 g / mol. Purify the remaining reaction polymer. Purification of the polymer: first dissolve the crude product in a...

Embodiment 3

[0037] Dry the 100mL pressure-resistant glass bottle equipped with a magnet at 130°C for more than 12 hours, vacuumize it until it cools down to room temperature, and flush it with nitrogen to prepare for use. Under nitrogen protection, a certain amount of catalyst 3a and cocatalyst bis(triphenylphosphoryl)ammonium chloride were weighed at room temperature, and the molar ratio of catalyst to cocatalyst was 1 / 2. Then add alkylene oxide 1c and thioanhydride 2a, the molar ratio of alkylene oxide, thioanhydride and chromium metal catalyst is 2000 / 1000 / 1. Then put it into an oil bath at 10°C and start magnetic stirring. Reaction 2h, stop stirring. A very small amount of the reaction mixture was removed for the 1 H NMR and GPC tests. 1 H NMR test showed that the conversion rate of thioanhydride was >99%, and GPC test showed that the polymer molecular weight was 37800 g / mol. Purify the remaining reaction polymer. Purification of the polymer: first dissolve the crude product in a ...

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Abstract

The invention provides a preparation method of semi-aromatic polythioesters, and belongs to the technical field of polymeric materials. The method comprises the following steps: adding alkylene oxide,thiophthalic anhydride, a catalyst and a cocatalyst into a dry reaction container, carrying out a reaction at 0-40 DEG C for 0.5-24 h, and purifying and drying the obtained reaction product to obtainthe semi-aromatic polythioesters. Compared with previously reported polythioester preparation methods, the method provided by the invention has the advantages of cheap and easily available raw materials, large variety number of products, and simplicity and easy operation of a polymerization process. The generated semi-aromatic polythioesters have good thermal stability and good refractive index,and have potential uses in the field of special optical materials.

Description

technical field [0001] The invention belongs to the field of polymer materials, and in particular relates to a preparation method of semi-aromatic polythioester. Background technique [0002] Polythioester is a type of polymer similar in structure to polyester, that is, a type of heterochain polymer in which the oxygen atoms in the ester groups on the polyester main chain are replaced by sulfur atoms. The sulfur atoms introduced in the main chain make polythioester exhibit unique properties in terms of optical properties, chemical stability, and heavy metal ion adsorption while retaining the characteristics of polyester materials. Therefore, polythioester materials have broad application prospects in the manufacture of high-performance optical fiber, adhesives, and wastewater treatment containing heavy metal ions. At present, semi-aromatic polythioesters are mainly synthesized by polycondensation of dithiols and diacids in organic solvents. Since the reaction process requi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/26
Inventor 任伟民王丽阳乐天俊吕小兵
Owner DALIAN UNIV OF TECH
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