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Preparation method of poly epsilon-caprolactone

A technology of caprolactone and catalyst is applied in the field of preparing polyε-caprolactone, which can solve the problems of difficult removal of metal residues and inability to apply

Active 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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  • Preparation method of poly epsilon-caprolactone
  • Preparation method of poly epsilon-caprolactone
  • Preparation method of poly epsilon-caprolactone

Examples

Experimental program
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Embodiment 1

[0017] In a 1-liter glass bottle, add 300 grams of ε-caprolactone, 2 grams of ethylene glycol, and after three replacements with high-purity nitrogen, add 0.05 grams of 1-(4-sulfonic acid)butyl-3- Methylimidazole tetrafluoroborate, heated to 120-140 degrees, reacted for 12 hours, cooled to room temperature, dissolved the product with 2000 ml of chloroform, and precipitated with 5000 ml of ethanol to obtain 280 g of polyε-caprolactone. The weight average was determined by GPC The molecular weight is 30,000, and the molecular weight distribution is 1.3.

Embodiment 2

[0019] Add 15 kg of ε-caprolactone to a 20-liter stainless steel reactor with stirring, add 0.15 kg of butanediol, fill with nitrogen and replace the air three times, add 1-(4-sulfonic acid) butyl-3 under nitrogen protection - 75 grams of methylpyrazine tetrafluoroborate, polymerized at 130-150 degrees for 12 hours, then vacuum (vacuum degree 1-10mmHg) at this temperature to remove unreacted monomers to obtain 14.5 kilograms of polyε-hexane Lactone, measured by GPC, has a weight average molecular weight of 10,000 and a molecular weight distribution of 1.2.

Embodiment 3

[0021] Add 15 kg of ε-caprolactone and 0.75 kg of 1,2-propanediol to a 20-liter stainless steel reactor with stirring, fill with nitrogen and replace the air three times, and add 1-(4-sulfonic acid) butyl- 15 grams of 3-methylpyrazine tetrafluoroborate, polymerized at 90-120 degrees for 12 hours, then vacuum (vacuum degree 1-10mmHg) at this temperature to remove unreacted monomers and impurities to obtain 14.8 kilograms of polyε -Caprolactone, the weight average molecular weight measured by GPC is 2500, and the molecular weight distribution is 1.24.

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Abstract

The invention discloses a preparation method of poly epsilon-caprolactone. The method includes: mixing epsilon-caprolactone with an alcohol molecular weight regulator in proportion, then adding 1-(4-sulfonyl)butyl-3-methylpyrazine tetrafluoroborate or 1-(4-sulfonyl)butyl-3-methylimidazole tetrafluoroborate as the catalyst, and at a temperature of 60-180DEG C, carrying out ring opening polymerization under anhydrous and oxygen-free conditions to obtain poly epsilon-caprolactone.

Description

technical field [0001] The invention belongs to the field of polymer materials, in particular to a method for preparing polyε-caprolactone. Background technique [0002] Poly ε-caprolactone has good flexibility, processability and biodegradability, especially shape memory, and has good application prospects in the fields of radiotherapy positioning plates, tapes, bandages, orthoses, etc. in the biomedical field , is also widely used to modify and toughen other polymer materials such as polylactic acid. As a new and high-grade polyurethane material, low molecular weight polycaprolactone with hydroxyl end has good elasticity and has been used as a substitute for polyether polyol in the fields of high-end adhesives, polyurethane foams, sponges and polyurethane paints. [0003] The preparation method of polyε-caprolactone has been extensively studied, among which the main method is the ring-opening polymerization of ε-caprolactone under the action of a catalyst, and various cat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/08C08G63/84
Inventor 袁明龙李宏利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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