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A preparation method of polycaprolactone, a biodegradable polymer material for medicine

A polymer material, polycaprolactone technology, applied in the field of drug preparation, can solve the problems of complex synthesis steps, low product yield, long reaction time, etc., to achieve low reaction requirements, simple production process, and short reaction time Effect

Active Publication Date: 2020-11-17
山东采采医疗科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Metals in common metal compound catalysts include magnesium, calcium, tin, aluminum, zinc, iron, titanium, etc.; however, in existing metal complex catalysts, the selection of ligands and metals is very important for the ring-opening polymerization. The speed and the performance of the resulting product are very critical. In the case of the same metal, the replacement and selection of the ligand often show unexpected catalytic effects. In the case of the same ligand, the replacement of the metal will also produce different results. Catalytic effect
[0005] In addition to the above-mentioned metal compound coordination catalyst systems, there are organoaluminum compound coordination catalysts and rare earth compound catalysts. The organoaluminum compound coordination catalysts mainly include alkyl aluminum, alkoxy aluminum, porphyrin aluminum and their derivatives. Among them, aluminum isopropoxide is the most effective catalyst, the reaction conditions are mild, and the molecular weight of the obtained polymer is high, but the reaction time is long, the product yield is low, the molecular weight distribution is wide, and the organoaluminum compound has certain toxicity, which limits its application in the market. Biomedical Applications
[0006] Rare earth catalysts such as halide rare earth compounds, rare earth alkoxy compounds and rare earth aryl oxide compounds can also catalyze the ring-opening polymerization of caprolactone, and its mechanism is similar to the catalytic mechanism of alkoxy aluminum (belonging to the coordination-insertion mechanism), However, the catalyst is unstable and easily hydrolyzed in the air, and the synthesis steps are too complicated

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A preparation method of polycaprolactone, a biodegradable polymer material for medicine, comprising the following steps:

[0029] Weigh 200g ε-caprolactone monomer, pour it into a three-necked flask, weigh 0.094g tetraphenyltin (the molar ratio of caprolactone monomer to tetraphenyltin is 8000:1) and 0.65g n-dodecyl alcohol ( The molar ratio of caprolactone monomer and n-dodecyl alcohol is 500:1), mix evenly, pour into the three-necked flask, pass nitrogen gas, start the stirring device, make sure the system is sealed and then raise the temperature, control the temperature of the liquid in the three-necked flask 120-170°C, after 4-6 hours of reaction, the material is discharged. The color of the product is pure white. The crude product is dissolved and precipitated three times, and vacuum-dried to constant weight to obtain the finished product. The weight average molecular weight of the obtained product is 68288, the molecular weight distribution index is 1.52, and the ...

Embodiment 2

[0031] A preparation method of polycaprolactone, a biodegradable polymer material for medicine, comprising the following steps:

[0032] Weigh 200g ε-caprolactone monomer, pour it into a three-necked flask, weigh 0.094g tetraphenyltin (the molar ratio of caprolactone monomer to tetraphenyltin is 8000:1) and 0.626g n-tetradecyl alcohol ( The molar ratio of caprolactone monomer and n-tetradecyl alcohol is 600:1), mix evenly, pour into the three-necked flask, pass nitrogen gas, start the stirring device, make sure that the system is sealed and then raise the temperature, and control the temperature of the liquid in the three-necked flask. 120-170°C, after 4-6 hours of reaction, the color of the discharged product is pure white. The crude product is dissolved in a solvent, precipitated three times, and vacuum-dried to constant weight to obtain the finished product. The weight average molecular weight of the obtained product is 75049, the molecular weight distribution index is 1.40...

Embodiment 3

[0034] A preparation method of polycaprolactone, a biodegradable polymer material for medicine, comprising the following steps:

[0035] Weigh 200g ε-caprolactone monomer, pour it into a three-necked flask, weigh 0.0625g dibutyltin diphenylacetate (the molar ratio of caprolactone monomer to dibutyltindiphenylacetate is 10000:1) and 0.267 g phenylethanol (caprolactone monomer to phenylethanol molar ratio 800:1) is mixed evenly, injected into the three-necked flask, fed with nitrogen, started the stirring device, confirmed that the system has been sealed, then raised the temperature, and controlled the temperature of the liquid in the three-necked flask After reacting at 120-170°C for 4-6 hours, the material is discharged. The color of the product is pure white. It is dissolved in a solvent, precipitated for 3 times, and vacuum-dried to constant weight to obtain the finished product. The weight average molecular weight of the obtained product is 91987, and the molecular weight d...

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PUM

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Abstract

The invention relates to a preparation method of medical biodegradable high-polymer material polycaprolactone. According to the method, an organometal compound is taken as a catalyst, polycaprolactoneis prepared with a bulk polymerization method, the production process is simple, conditions required for a reaction are lower, the reaction speed is high, the reaction time is short, the product chromaticity is good, and the molecular weight can be regulated as required; and an organometal compound catalysis system is an efficient catalysis system, the reaction time is short, the weight-average molecular weight of a product can be adjusted, the smallest molecular weight dispersion index can be 1.40, and polycaprolactone is high in catalysis activity and basically non-toxic.

Description

technical field [0001] The invention relates to a preparation method of polycaprolactone, a biodegradable polymer material used in medicine, and belongs to the technical field of medicine preparation. Background technique [0002] Since the 1960s, polycaprolactone (PCL polycaprolactone) has attracted widespread attention due to its good biocompatibility, biodegradability and memory, and its related research has also developed rapidly. PCL is a semi-crystalline polymer with a melting point of 59-64°C and a glass transition temperature of -60°C. It is rubbery at room temperature, which makes it possible to have better drug permeability than other polyesters, and can be used for implant materials in the body and sustained-release capsules of drugs. The molecular chain of PCL is relatively regular, flexible, and easy to crystallize, so it has better hydrophobicity than polyglycolide and polylactide, and it degrades slowly in the body, so it is one of the ideal implant materials...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G69/14C08G69/20
CPCC08G69/14C08G69/20C08G2230/00
Inventor 苏红清赵春华秦昌袁文博李建
Owner 山东采采医疗科技有限公司
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