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Preparation method of cyclic polyester oligomer

A technology for cyclic polyester and oligomers, which is applied in the field of preparation of cyclic polyester oligomers, and can solve problems such as unfavorable product performance and accelerated curing time

Inactive Publication Date: 2012-09-19
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Organotin or organotitanium catalysts are usually used in the production of cyclic polyester oligomers. These catalysts will initiate ring-opening polymerization of cyclic polyester oligomers when heated, and further accelerate the curing time during injection molding. Not conducive to controlling product performance

Method used

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  • Preparation method of cyclic polyester oligomer
  • Preparation method of cyclic polyester oligomer
  • Preparation method of cyclic polyester oligomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] In a 50ml three-necked reaction flask equipped with a mechanical stirring device, add 20 milliliters of dry chlorobenzene and 0.15 grams of polybutylene terephthalate (PBT, Mw=45000, styrene standard), replace with nitrogen three times, stir and heat to 140°C, make the PBT dissolution system into a transparent solution, then add 0.02g of dimethyl tin oxide, react for 240 minutes, cool to 25°C, heat filter, and vacuum the filtrate to dry the solvent to obtain a white solid. The white solid was dissolved in dichloromethane, the solution was removed by column chromatography to remove the residual organotin catalyst, and the final product was obtained after drying. The reaction yield was 24%.

Embodiment 2

[0023] In a 100ml three-necked reaction flask equipped with a mechanical stirring device, add 40 milliliters of dry o-dichlorobenzene and 0.5 gram of polytrimethylene terephthalate (PTT, Mw=128000, styrene standard), replace with nitrogen three times, stir and heat to 190°C, make the PTT dissolution system become a transparent solution, then add 0.25g of dibutyltin oxide, react for 180 minutes, cool to 50°C, heat filter, and vacuum the filtrate to dry the solvent to obtain a white solid. The white solid was dissolved in chloroform, the solution was removed by column chromatography to remove the residual organotin catalyst, and the final product was obtained after drying. The reaction yield was 37%.

Embodiment 3

[0025] In a 500ml three-necked reaction flask equipped with a mechanical stirring device, add 250ml of dry naphthalene and 3g of polyethylene terephthalate PET (Mw=82000, styrene standard), replace with nitrogen three times, stir and heat to 210°C , so that the PET solution system becomes a transparent solution, then add 0.3g 1,1,6,6-tetra-n-methyl-1,6-ditin-2,5,7,10-tetraoxcyclodecane, and react for 45 minutes Afterwards, cool to 100°C, heat filter, and vacuum the filtrate to dry the solvent to obtain a white solid. The white solid was dissolved in ether, the solution was removed by column chromatography to remove the residual organotin catalyst, and the final product was obtained after drying. The reaction yield was 83%.

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Abstract

The invention relates to a preparation method of a cyclic polyester oligomer. The traditional method has the problems of difficulty in recycling halogen and side products of ammonium salts, and the like, thereby being difficult to be used in production. The preparation method comprises the steps of: firstly, dissolving linear poly dihydricalcohol terephthalate into a high-boiling point organic solvent, heating and stirring to form a transparent solution of the poly dihydricalcohol terephthalate; then adding an organic tin catalyst into the transparent solution of the poly dihydricalcohol terephthalate, cracking and cyclizing to form a solution of the poly dihydricalcohol terephthalate; and cooling the solution, filtering and drying to obtain the poly dihydricalcohol terephthalate, removing remained organic tin catalyst from the solution through column chromatography, and drying to obtain the cyclic polyester oligomer without containing the organic tin catalyst. The cyclic polyester oligomer prepared by using the method can not generate self-polymerizing side reactions in a normal temperature storage period and a processing temperature-raising process.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and relates to a method for preparing cyclic polyester oligomers, in particular to a method for preparing cyclic polyester oligomers from a linear polyester organic solution in the presence of an organotin catalyst. Background technique [0002] Aromatic polyesters are a class of synthetic polymer materials developed in the 1950s. They have many advantages such as excellent mechanical properties, high thermal stability, chemical corrosion resistance, and low price. They have been widely used in the fields of fibers, films, and engineering plastics. Widely used, its main representatives are PET (polyethylene terephthalate), PTT (polytrimethylene terephthalate) and PBT (polybutylene terephthalate). Aromatic polyesters are mainly obtained through polycondensation reactions between derivatives of aromatic dibasic acids or esters and aliphatic or alicyclic diols. This polyester can be proce...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/183C08G63/85C08G63/90
Inventor 史佳鑫蒋志强黎俊江盛鸿王宗宝陈鹏顾群
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI