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Preparation method of ethylenediamine modified maleic anhydride polylactide-glycolide polymer

A technology of maleic anhydride and polylactide, applied in the field of preparation of modified polylactide, which can solve the problems of skin and nervous system irritation

Active Publication Date: 2014-12-03
HUNAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Due to its strong alkalinity and strong hygroscopicity, free aliphatic diamines can have adverse stimulating effects on the respiratory tract, skin and nervous system of animals, or are said to be cytotoxic, but there is no known cytotoxicity of bound aliphatic diamines. to report

Method used

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  • Preparation method of ethylenediamine modified maleic anhydride polylactide-glycolide polymer
  • Preparation method of ethylenediamine modified maleic anhydride polylactide-glycolide polymer

Examples

Experimental program
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Embodiment 1

[0022] Dissolve 10g of MPLGA in 27ml of chloroform to prepare 20wt% MPLGA in chloroform, and mix equal volumes of ethylenediamine and chloroform to prepare 38wt% ethylenediamine in chloroform. Add the chloroform of MPLGA into a three-necked flask equipped with a stirrer and a thermometer, add 2ml of ethylenediamine in chloroform under stirring, and control the system temperature below 10°C with an ice bath. After the dropwise addition was completed and kept warm for 5 min, the temperature was raised to room temperature and reacted for 60 min. The product was dropped into an excess ethanol solution to precipitate and was washed with deionized water to become neutral. The product was vacuum-dried at 40 °C to constant weight to obtain a yellow EMPLGA solid. The resulting product M w =27775, M w / M n =1.70.

Embodiment 2

[0024] 10g of MPLGA was dissolved in 16ml of chloroform to prepare a 30wt% MPLGA solution in chloroform, and equal volumes of ethylenediamine and chloroform were mixed to prepare a 38wt% ethylenediamine solution in chloroform. Add the chloroform of MPLGA into a three-necked flask equipped with a stirrer and a thermometer, add 1ml of ethylenediamine in chloroform solution under stirring conditions, and control the system temperature below 10°C with an ice bath. After the dropwise addition was completed and kept warm for 10 min, the temperature was raised to room temperature and reacted for 30 min. The product was dropped into an excess ethanol solution to precipitate and was washed with deionized water to become neutral. The product was vacuum-dried at 40 °C to constant weight to obtain a yellow EMPLGA solid. The resulting product M w =33262, M w / M n =1.65.

Embodiment 3

[0026] Dissolve 10g of MPLGA in 20ml of chloroform to prepare 25wt% MPLGA in chloroform, and mix equal volumes of ethylenediamine and chloroform to prepare 38wt% ethylenediamine in chloroform. Add the chloroform of MPLGA into a three-necked flask equipped with a stirrer and a thermometer, add 2ml of ethylenediamine in chloroform under stirring, and control the system temperature below 10°C with an ice bath. After the dropwise addition was completed and kept warm for 5 min, the temperature was raised to room temperature and reacted for 40 min. The product was dropped into an excess ethanol solution to precipitate and was washed with deionized water to become neutral. The product was vacuum-dried at 40 °C to constant weight to obtain a yellow EMPLGA solid. The resulting product M w =30347, M w / M n =1.71.

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Abstract

The invention provides a preparation method of an ethylenediamine modified maleic anhydride polylactide-glycolide polymer disclosed as Formula (I), which comprises the following steps: by using D,L-lactide, glycolide and maleic anhydride as raw materials, stannous octanoate as a catalyst and benzoperoxide as an initiator, carrying out polymerization in an ampoule bottle under high-vacuum conditions to prepare maleic anhydride polylactide-glycolide (MPLGA), adding a trichloromethane solution of ethylenediamine into a trichloromethane solution of the MPLGA while stirring, keeping the temperature at lower than 10 DEG C for 5-10 minutes, reacting at room temperature for 30-60 minutes, dropwisely adding the product into excessive solvent, precipitating, washing with deionized water to a neutral state, and carrying out vacuum drying to constant weight, thereby obtaining the ethylenediamine modified maleic anhydride polylactide-glycolide polymer solid. The product has higher hydrophilicity and biocompatibility.

Description

technical field [0001] The invention relates to the technical field of production of degradable biomedical polymer materials, in particular to a preparation method of modified polyglycolide with good hydrophilic performance and controllable degradation rate. Background technique [0002] Polylactide (PLGA) is widely used in slow-release materials, surgical sutures, tissue engineering, etc. because of its good biocompatibility, complete biodegradability in vivo, and controllable degradation rate. The hydrophobicity, lack of abundant active groups and other defects limit its application. Maleic anhydride polylactide (MPLGA) can be prepared by free radical polymerization using the tertiary carbon hydrogen in the main chain of PLGA and the carbon-carbon double bond in maleic anhydride. MPLGA has good hydrophilic properties and mechanical properties, and the introduction of anhydride bonds can also provide active groups for subsequent modification of materials. However, the int...

Claims

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Application Information

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IPC IPC(8): C08F283/02C08F222/06C08F8/32C08G63/08
Inventor 周智华黄慧华曹大福周虎刘清泉刘立华陈建
Owner HUNAN UNIV OF SCI & TECH
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