A kind of preparation method of polycaprolactone and application of used initiator

A technology of polycaprolactone and initiator, which is applied in the field of polymer polycaprolactone preparation, can solve the problems of limited application and toxicity, and achieve the effects of convenient fixing and disassembly, fast reaction speed and high catalytic activity

Active Publication Date: 2016-04-13
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of this method are that the cocatalysts trialkylphosphine and triphenylphosphine used are highly toxic, which limits their application in medicine.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Weigh 114g of ε-caprolactone and pour it into a three-necked flask. Weigh 0.088g of ethylene oxide (the molar ratio of the monomer to 500), 0.439g of dibutyltin diacetate (the molar ratio of the monomer to 800), 0.054g of benzyl alcohol (the molar ratio of the monomer to 500), the initiator, Mix the catalyst and molecular weight regulator and inject it into the three-necked flask, install the nitrogen conduit, mercury thermometer, condenser tube, metal stirring rod, etc., feed nitrogen, open the inlet and outlet of condensed water, start the stirring device, and confirm that the system is sealed. Heat up the oil bath, control the temperature of the liquid in the three-necked flask at 130-160°C, react for 30-75 minutes, and discharge the product after the rod climbing phenomenon occurs. The color of the product is pure white. Molecular weight and molecular weight distribution index are measured by GPC gel chromatography, and the weight average molecular weight of the pro...

Embodiment 2

[0021] Weigh 114g of ε-caprolactone and pour it into a three-necked flask. Weigh 0.029g of propylene oxide (monomer to its molar ratio of 2000), 0.130g of dibutyltin dibenzoate (monomer to its molar ratio of 3000), 0.122g of phenylethyl alcohol (monomer to its molar ratio of 1000), will trigger After mixing the agent, catalyst and molecular weight regulator, pour it into the three-necked flask, install the nitrogen conduit, mercury thermometer, condenser tube, metal stirring rod, etc., pass in nitrogen, open the inlet and outlet of condensed water, start the stirring device, and confirm that the system is sealed. , heat up the oil bath, control the temperature of the liquid in the three-necked flask at 130-160°C, react for 30-75 minutes, and discharge the product after the rod climbing phenomenon occurs. The color of the product is pure white. Molecular weight and molecular weight distribution index are measured by GPC gel chromatography, and the weight average molecular weigh...

Embodiment 3

[0023] Weigh 114g of ε-caprolactone and pour it into a three-necked flask. Weigh 0.088g of 1,2-epoxyoctadecane (monomer and its molar ratio 4000), 0.104g dibutyltin diacetate (monomer and its molar ratio 5000), 0.068g 3-phenylpropanol (monomer and its molar ratio 2000), mix the initiator, catalyst, and molecular weight regulator and inject it into a three-necked flask, install a nitrogen conduit, a mercury thermometer, a condenser tube, a metal stirring rod, etc., feed nitrogen, open the inlet and outlet of condensed water, start the stirring device, and determine After the system is sealed, heat up the oil bath, control the temperature of the liquid in the three-necked flask at 120-160°C, and react for 30-75 minutes. After the rod climbing phenomenon occurs, the product is discharged. The color of the product is pure white. Molecular weight and molecular weight distribution index are measured by GPC gel chromatography, and the weight average molecular weight of the product ob...

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Abstract

The invention discloses a preparation method of polycaprolactone and applications of initiator used therein. The polycaprolactone is synthesized trough the reaction which employs Epsilon-caprolactone as a monomer, alkylene oxide as an initiator, organic metal salt as a catalyst, and C7-C11 aromatic alcohol as a molecular weight modifier, at the temperature of 120-190 DEG C and under the protection of nitrogen; the carbon chain length of alkyl group in the alkylene oxide is 2-20. The preparation method provided by the invention is simple in production technology, low in conditions required by reaction, rapid in reaction speed, short in reaction time, good in product chromaticity and adjustable in molecular weight according to requirements.

Description

technical field [0001] The invention relates to a preparation method of polymer polycaprolactone. Background technique [0002] Polycaprolactone is a synthetic aliphatic polyester. Due to its good biodegradability, biocompatibility, drug permeability, and low melting point, it is widely used in biomaterials and pharmaceutical fields. , such as medical bandages, orthotics, sutures, drug release agents, medical fixed brackets, etc. [0003] At present, there are many kinds of initiators and catalysts used for ε-caprolactone polymerization, and some of the disclosed initiation-catalysis systems have poor catalytic effects. Although some disclosed initiators and catalysts have relatively high initiation activity, they have relatively large Cytotoxicity limits its application in biomedicine. [0004] 02110858.7 discloses a method for preparing high-molecular-weight branched polycaprolactone, which is characterized in that EVOH is used as an initiator and ε-caprolactone is used ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/08C08G63/87C08G63/82C08G63/85C08G63/83A61L31/06
Inventor 李长存黎树根韩娟刘洪武李勇军李君罗际安李勇华
Owner CHINA PETROLEUM & CHEM CORP
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