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Molecular weight controllable poly epsilon-caprolactone and preparation method thereof

A technology of caprolactone and molecular weight, which is applied in the field of preparing polyε-caprolactone, can solve the problems of difficult removal of metal residues and inapplicability

Inactive Publication Date: 2016-03-02
YUNNAN MINZU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Such as CN1814644, US5235031, US5357034, US4057537, etc. have reported that metal catalysts such as tin salts are used to catalyze ε-caprolactone and lactide to carry out ring-opening polymerization to prepare poly ε-caprolactone and polylactic acid. But the polymerization prepared by this type of method Biomaterials cannot be used in some specific fields such as biomedicine and microelectronics because it is extremely difficult to remove metal residues

Method used

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  • Molecular weight controllable poly epsilon-caprolactone and preparation method thereof
  • Molecular weight controllable poly epsilon-caprolactone and preparation method thereof
  • Molecular weight controllable poly epsilon-caprolactone and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0017] In a 1 liter glass bottle, add 300 grams of ε-caprolactone, 2 grams of ethylene glycol, replace it with high-purity nitrogen three times, and add 0.05 grams of 4-methyl-1-(4-sulfonate butane) under the protection of nitrogen. Base) pyridine tetrafluoroborate, heated to 120-140 degrees for 12 hours and then cooled to room temperature. Dissolve the product with 2000 ml of chloroform, precipitate with 5000 ml of ethanol to obtain 280 g of polyε-caprolactone. The weight is measured by GPC The average molecular weight is 30,000 and the molecular weight distribution is 1.3.

Embodiment 2

[0019] Add 15 kilograms of ε-caprolactone to a 20-liter stainless steel stirred reactor, add 0.15 kilograms of butanediol, fill with nitrogen and replace the air three times, and add 1,1'-(butane-1,4- Diyl)bis[3-(4-sulfonylbutyl)-imidazole]tetrafluoroborate 75g, polymerize at 130-150°C for 12 hours, then vacuum at this temperature (vacuum degree 1-10mmHg) The unreacted monomer was removed, and 14.5 kg of polyε-caprolactone was obtained. The weight average molecular weight was 10,000 and the molecular weight distribution was 1.2 by GPC.

Embodiment 3

[0021] Add 15 kg of ε-caprolactone and 0.75 kg of 1,2-propanediol into a 20-liter stainless steel reactor with stirring. Fill with nitrogen and replace the air three times. Add 1,1'-(butane-1,4) under nitrogen protection. -Diyl)bis[3-(4-sulfobutyl)-imidazole]tetrafluoroborate 15g, polymerize at 90-120 degrees for 12 hours, then vacuum at this temperature (vacuum degree 1-10mmHg) Unreacted monomers and impurities were removed to obtain 14.8 kg of polyε-caprolactone, with a weight average molecular weight of 2500 and a molecular weight distribution of 1.24 as determined by GPC.

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Abstract

The invention discloses a molecular weight controllable poly epsilon-caprolactone and a preparation method thereof. The method includes: mixing epsilon-caprolactone with an alcohol molecular weight regulator in proportion, adding 4-methyl-1-(4-sulfobutyl)pyridine tetrafluoro-borate or 1, 1'-(butane-1, 4-diyl)bis[3-(4-sulfobutyl)-imidazole]tetrafluoroborate to serve as the catalyst, and conducting ring opening polymerization at 60-180DEG C and under anhydrous and oxygen-free conditions, thus obtaining poly epsilon-caprolactone.

Description

Technical field [0001] The invention belongs to the field of polymer materials, and specifically relates to a method for preparing polyε-caprolactone. Background technique [0002] Polyε-caprolactone has good flexibility, processability and biodegradability, especially shape memory, and has good application prospects in the fields of radiotherapy positioning plates, tapes, bandages, and orthotics in the biomedical field It is also widely used to modify and toughen other polymer materials such as polylactic acid. As a new and high-grade polyurethane material, hydroxyl-terminated low molecular weight polycaprolactone has good elasticity and has replaced polyether polyols in high-end adhesives, polyurethane foam, sponges and polyurethane paints. [0003] There have been a lot of researches on the preparation method of polyε-caprolactone. The main method is to carry out ring-opening polymerization of ε-caprolactone under the action of a catalyst. Various catalysts have become the rese...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/08C08G63/84
Inventor 李宏利袁明龙袁明虎唐志道袁明伟蒋琳钏永明郭俊明彭金辉
Owner YUNNAN MINZU UNIV
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