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Preparation method of crystalline polymonothiocarbonate

A monothiocarbonate and crystallinity technology, which is applied in the field of preparation of crystalline polymonothiocarbonate, can solve the problems of single monomer, limited practical application of materials, low polymer melting temperature, etc., and achieves improved optical properties. , controllable structure, high polymer selectivity effect

Active Publication Date: 2018-09-21
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, although there is a method for preparing crystalline polymonothiocarbonate (CN106243336A), the melting temperature of the resulting polymer is low, which limits the practical application of this type of material; in addition, the monomers used are relatively single

Method used

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  • Preparation method of crystalline polymonothiocarbonate
  • Preparation method of crystalline polymonothiocarbonate
  • Preparation method of crystalline polymonothiocarbonate

Examples

Experimental program
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Embodiment 1

[0042]A 100 mL autoclave equipped with a magnet was dried at 130 °C for more than 12 h, vacuumed until it was cooled to room temperature, and flushed with nitrogen to prepare for use. Under nitrogen protection, a certain amount of catalyst 2a and cocatalyst bis(triphenylphosphoranyl)ammonium chloride were weighed at room temperature and placed in a Xulink flask, and the molar ratio of catalyst to cocatalyst was 1:2. Then add meso alkylene oxide 1a, the molar ratio of meso alkylene oxide to catalyst is 2000:1, stir for 5 minutes to completely dissolve, and transfer the above solution into an autoclave with a dry syringe. The kettle is charged with carbonyl sulfide at a specified pressure, and the molar ratio of carbonyl sulfide to meso-alkane oxide is 1.2:1. It was then placed in an oil bath at 25°C and magnetic stirring was turned on. When the reaction reaches the appointed time, the stirring is stopped, and the remaining carbonyl sulfide gas is slowly released. A very small...

Embodiment 2

[0044] A 100 mL autoclave equipped with a magnet was dried at 130 °C for more than 12 h, vacuumed until it was cooled to room temperature, and flushed with nitrogen to prepare for use. Under nitrogen protection, a certain amount of catalyst 2b and cocatalyst bis(triphenylphosphoranyl)ammonium chloride were weighed at room temperature and placed in a Xulink flask, and the molar ratio of catalyst to cocatalyst was 1:2. Then add meso alkylene oxide 1a, the molar ratio of meso alkylene oxide to catalyst is 2000:1, stir for 5 minutes to completely dissolve, and transfer the above solution into an autoclave with a dry syringe. The kettle is charged with carbonyl sulfide at a specified pressure, and the molar ratio of carbonyl sulfide to meso-alkane oxide is 1.2:1. It was then placed in an oil bath at 25°C and magnetic stirring was turned on. When the reaction reaches the appointed time, the stirring is stopped, and the remaining carbonyl sulfide gas is slowly released. A very smal...

Embodiment 3

[0046] A 100 mL autoclave equipped with a magnet was dried at 130 °C for more than 12 h, vacuumed until it was cooled to room temperature, and flushed with nitrogen to prepare for use. Under nitrogen protection, a certain amount of catalyst 2c and cocatalyst tetrabutylammonium chloride were weighed at room temperature and placed in a Xulink bottle, and the molar ratio of catalyst to cocatalyst was 1:2. Then add meso alkylene oxide 1a, the molar ratio of meso alkylene oxide to catalyst is 2000:1, stir for 5 minutes to completely dissolve, and transfer the above solution into an autoclave with a dry syringe. The kettle is charged with carbonyl sulfide at a specified pressure, and the molar ratio of carbonyl sulfide to meso-alkane oxide is 1.2:1. It was then placed in an oil bath at 25°C and magnetic stirring was turned on. When the reaction reaches the appointed time, the stirring is stopped, and the remaining carbonyl sulfide gas is slowly released. A very small amount of the...

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Abstract

The invention belongs to the field of polymer materials, and relates to a preparation method of a crystalline polymonothiocarbonate. An an asymmetric copolymerization reaction takes place between mesomeric epoxyalkane and carbonyl sulfide under the action of a chiral catalyst to form the crystalline polymonothiocarbonate with a highly isotactic structure. The content of monothiocarbonate units ina polymer chain of the crystalline polymonothiocarbonate is 99% or more than 99%; the Isotactic degree of the polymer is 75% to 99%; and a semi-crystalline material can be obtained after the polymer is simply heat-treated. The crystalline polymonothiocarbonate is prepared by polymerizing the carbonyl sulfide and the mesomeric epoxyalkane, and the mesomeric epoxyalkane is wide in sources, so that aplurality of crystalline polymonothiocarbonates can be prepared; the preparation method is mild in reaction conditions, high in catalyst activity, and high in polymer selectivity; and the prepared polymonothiocarbonate is controllable in structure, complete in alternation, and relatively high in melting temperature, has no oxygen-sulfur exchange, and has the advantages of high possibility of crystallization, strong resistance to thermal deformation, high refractive index and the like.

Description

technical field [0001] The invention belongs to the field of polymer materials, and in particular relates to a preparation method of crystalline polymonothiocarbonate. Background technique [0002] Polythiocarbonate is a class of copolymers similar in structure to polycarbonate, that is, all or part of the oxygen atoms in the polycarbonate segment structure are replaced by sulfur atoms. The introduction of sulfur atoms in the main chain enables polythiocarbonates to exhibit unique optical properties while retaining the characteristics of polycarbonate materials. Originally, polythiocarbonates were formed by polycondensation of dithiols with phosgene or by ring-opening polymerization of cyclic thiocarbonates. However, when phosgene is used as the reaction raw material, the requirements for the reaction equipment are higher, and the process does not meet the "green" chemical characteristics; while the cyclic thiocarbonate has very low activity in the ring-opening polymerizati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/28
CPCC08G75/28
Inventor 任伟民乐天俊顾格阁吕小兵
Owner DALIAN UNIV OF TECH
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