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Aliphatic polythioester preparation method

A polythioester and aliphatic technology is applied in the field of preparation of aliphatic polythioesters, which can solve problems such as being unsuitable for large-scale production of polythioesters, and achieve precise regulation of polymer structure and simple and easy polymerization method. The effect of various operations and product types

Active Publication Date: 2019-03-08
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Neither method is suitable for large-scale production of polythioesters

Method used

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  • Aliphatic polythioester preparation method
  • Aliphatic polythioester preparation method
  • Aliphatic polythioester preparation method

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 the protection of nitrogen, weigh a certain amount of initiator bis(triphenylphosphoryl) ammonium chloride, cyclothioalkane 1a and aliphatic thioanhydride 2a at room temperature, cyclothioalkane, aliphatic thioanhydride and initiator The molar ratio 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 aliphatic thioanhydride was >99%, and GPC test showed that the polymer molecular weight was 23400 g / mol. Purify the remaining reaction polymer. Purification of the polymer: first dissolve the crude product in a small amount of dichloromethane, then add a large amou...

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, take by weighing a certain amount of initiator bis(triphenylphosphoryl) ammonium acetate, epithioalkane 1a and aliphatic thioanhydride 2c at room temperature, the mixture of epithioalkane, aliphatic thioanhydride and initiator The molar ratio 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 aliphatic thioanhydride was >99%, and GPC test showed that the polymer molecular weight was 31200 g / mol. Purify the remaining reaction polymer. Purification of the polymer: first dissolve the crude product in a small amount of dichloromethane, then ad...

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, room temperature takes by weighing a certain amount of initiator bis(triphenylphosphoryl) ammonium nitrate, epithioalkane 1b and aliphatic thioanhydride 2a, the mixture of epithioalkane, aliphatic thioanhydride and initiator The molar ratio is 2000:1000:1. Then put it into an oil bath at 40°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 aliphatic thioanhydride was >99%, and GPC test showed that the polymer molecular weight was 40800 g / mol. Purify the remaining reaction polymer. Purification of the polymer: first dissolve the crude product in a small amount of dichloromethane, then add a large amo...

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Abstract

The invention belongs to the field of high polymer materials and particularly relates to an aliphatic polythioester preparation method. Raw materials including epithioalkane and aliphatic thioanhydride and an initiator namely quaternary ammonium salt are subjected to bulk polymerization or solution polymerization reaction, wherein the reaction temperature is 0-120 DEG C, and reaction time is 0.1-24h. The method has advantages of precision in polymer structure control, product diversification, simplicity and easiness in operation of a polymerization method and the like, and generated aliphaticpolythioester is high in thermal stability and refractive index and has a potential application 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 aliphatic 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 enable polythioesters to exhibit unique properties in terms of optical properties, chemical resistance, and heavy metal ion adsorption while retaining the characteristics of polyester materials. Therefore, polythioester materials have broad application prospects in high-performance optical fiber manufacturing, adhesives, and wastewater treatment containing heavy metal ions. At present, the synthesis methods of polythioester mainly include two kinds: polycondensation method and ring-opening polymerization method. The polycondensation m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/26
CPCC08G75/26
Inventor 任伟民乐天俊张明潮吕小兵
Owner DALIAN UNIV OF TECH
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