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A kind of preparation method of polylactic acid compound grafted on the surface of carboxylated graphene oxide

A graphene surface, carboxylation technology, applied in the field of biomedical polymer materials, can solve problems such as limited application, achieve the effects of mild experimental conditions, improved application prospects, and high grafting rate

Active Publication Date: 2020-12-08
DALIAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Polylactic acid (PLLA) has high crystallinity and strong hydrophobicity, which largely limits its application in medical drug release carrier materials

Method used

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  • A kind of preparation method of polylactic acid compound grafted on the surface of carboxylated graphene oxide
  • A kind of preparation method of polylactic acid compound grafted on the surface of carboxylated graphene oxide
  • A kind of preparation method of polylactic acid compound grafted on the surface of carboxylated graphene oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Take 0.01g of GO-COOH ultrasonically dissolved in 10mL of deionized water to obtain GO-COOH solution; add 0.02g of PLLA-PEG-PLLA to 40mL of dichloromethane to obtain PLLA-PEG-PLLA solution; GO-COOH After the solution was mixed with PLLA-PEG-PLLA solution, 50mL of ethanol was added to make it uniformly dispersed, and then 0.04g of EDC and 0.02g of DMAP were added to the mixed solution, protected by nitrogen, and stirred at 70°C for 5h. After the reaction, the The reaction solution was put into a dialysis bag, dialyzed for 5 days, and freeze-dried to obtain a product of polylactic acid copolymer grafted with carboxylated graphite oxide (GO-COOH-PLLA-PEG-PLLA), with a grafting rate of 99.13%.

Embodiment 2

[0027] Take 0.01g of GO-COOH ultrasonically dissolved in 10mL of deionized water to obtain GO-COOH solution; add 0.02g of PLLA-PEG-PLLA to 10mL of dichloromethane to obtain PLLA-PEG-PLLA solution; GO-COOH After the solution was mixed with the PLLA-PEG-PLLA solution, 50mL of ethanol was added to make it uniformly dispersed, and then 0.04g of EDC and 0.02g of DMAP were added to the mixed solution, protected by nitrogen, and stirred at 85°C for 15h. After the reaction, the The reaction solution was put into a dialysis bag, dialyzed for 5 days, and freeze-dried to obtain a product of polylactic acid copolymer grafted with carboxylated graphite oxide (GO-COOH-PLLA-PEG-PLLA), with a grafting rate of 96.58%.

Embodiment 3

[0029] Take 0.01g of GO-COOH ultrasonically dissolved in 10mL of deionized water to obtain GO-COOH solution; add 0.02g of PLLA-PEG-PLLA to 60mL of dichloromethane to obtain PLLA-PEG-PLLA solution; GO-COOH After the solution was mixed with PLLA-PEG-PLLA solution, 50mL of ethanol was added to make it uniformly dispersed, and then 0.05g of EDC and 0.01g of DMAP were added to the mixed solution, protected by nitrogen, and stirred at 55°C for 20h. After the reaction, the The reaction solution was put into a dialysis bag, dialyzed for 5 days, and freeze-dried to obtain a product of polylactic acid copolymer grafted with carboxylated graphite oxide (GO-COOH-PLLA-PEG-PLLA), with a grafting rate of 98.82%.

[0030] figure 2 It is an infrared spectrogram of the carboxylated graphene oxide surface-grafted polylactic acid composite obtained in Example 1. In the figure: (a) The characteristic peaks of GO-COOH appear at 1736cm-1 (carbonyl-C=O stretching vibration peak in carboxylic acid),...

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Abstract

The invention relates to a preparation method of a carboxylated graphene oxide surface grafted polylactic complex. The carboxylated graphene oxide surface grafted polylactic complex (GO-COOH-PLLA-PEG-PLLA) is prepared by taking carboxylated graphene oxide (GO-COOH) as a raw material by means of an improved Steglish esterification reaction method. The structure of the complex is represented by means of infrared spectrum (FTIR) and nuclear magnetic resonance spectrum (1HNMR), and the synthesized molecules are consistent with target molecular structures. By grafting the graphene oxide with polylactic by means of the method, the grafting rate reaches up to 99.13%. The preparation method is mild in experimental condition, easy to operate and free of byproducts in reaction process, so that the purity of the polymer is greatly improved. No organic solvents are left, the experimental cost is low, and the application prospect of the complex in the biomedical field is improved.

Description

technical field [0001] The invention relates to the field of biomedical polymer materials, in particular to a method for preparing a polylactic acid compound grafted on the surface of carboxylated graphene oxide. [0002] technical background [0003] Polylactic acid (PLLA) has high crystallinity and strong hydrophobicity, which greatly limits its application in medical drug release carrier materials. In order to improve the performance of PLLA, in recent years, the functional modification of PLLA has been extensively studied by material scientists at home and abroad. At present, the modification of PLLA mainly includes chemical modification and physical filling modification. Chemical modification is mainly by copolymerizing lactic acid and other substances, and then extending the chain to form a block complex; or adding a multifunctional cross-linking agent, such as dioctyl phthalate (DOP), to PLLA for cross-linking modification. or through the esterification reaction betw...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00
CPCC08G83/001
Inventor 詹世平闫思圻张娇宫蕾
Owner DALIAN UNIV
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