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Polylactic acid grafted quaternized chitosan material and its stereocomposite crystalline nanofiber membrane and their preparation method and application

A technology of quaternized chitosan and composite nanofibers, which is applied in the fields of fiber chemical characteristics, conjugated synthetic polymer artificial filaments, and pharmaceutical formulations, and can solve problems such as the need to improve the crystallinity of stereocomplexes and the degradation of polylactic acid. , achieve broad biomedical application prospects, avoid degradation, and have strong dispersion effects

Active Publication Date: 2022-07-12
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In 2006, Tsuji reported for the first time that the nanospinning with stereocomplex crystallinity of 20% was obtained by mixing two polylactic acid enantiomers and electrospinning (see H.Tsuji, M.Nakano, M.Hashimoto , K.Takashima, S.Katsura, A.Mizuno.Biomacromolecules 2006, 7(12), 3316-3320), but the amorphous region and homogeneous crystals still account for the main part, and the degree of stereocomplex crystallinity still needs to be improved
Studies have shown that heating can effectively increase the crystallinity of stereocomplex crystals, but excessively high temperatures can easily cause degradation of polylactic acid, so how to increase the crystallinity of stereocomplex crystals at lower temperatures is more meaningful

Method used

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  • Polylactic acid grafted quaternized chitosan material and its stereocomposite crystalline nanofiber membrane and their preparation method and application
  • Polylactic acid grafted quaternized chitosan material and its stereocomposite crystalline nanofiber membrane and their preparation method and application
  • Polylactic acid grafted quaternized chitosan material and its stereocomposite crystalline nanofiber membrane and their preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] (1) Preparation of QCS-PLLA

[0050] Under nitrogen protection, the QCS powder prepared and purified by the prior art and L-lactide were added to sulfuric acid in a molar ratio of 1:12 to prepare an acid solution with a solid content of 8% (w / v). The reaction was stirred for 2 h. After the reaction, the reaction solution was poured into a buffer solution composed of 10M sodium hydroxide and 0.2M dipotassium hydrogen phosphate in a pre-ice bath with a mixing ratio of 1:4. After the product was precipitated, it was filtered and purified with water. After thorough washing, the QCS-PLLA was obtained by freeze-drying.

[0051] (2) Preparation of stereocomposite crystalline nanofiber membranes

[0052] D-polylactic acid (weight average molecular weight 100KDa, optical purity 98%), QCS-PLLA and QCS were mixed in a mass ratio of 50:40:10, in hexafluoroisopropanol and dichloromethane (4:1, v / v) to dissolve in, prepare a solution with a solid content of 8% (w / v) concentration,...

Embodiment 2

[0054] (1) Preparation of QCS-PDLA

[0055] Under nitrogen protection, the QCS powder prepared and purified by the prior art and D-lactide were added together in sulfuric acid according to a molar ratio of 1:36 to prepare an acid solution with a solid content of 15% (w / v). The reaction was stirred at ℃ for 6 h. After the reaction was completed, the reaction solution was poured into a buffer solution consisting of 10M sodium hydroxide and 0.2M dipotassium hydrogen phosphate mixed in a ratio of 1:4 in an ice bath. After thorough washing with water, the QCS-PDLA was obtained by freeze-drying.

[0056] (2) Preparation of stereocomposite crystalline nanofiber membranes

[0057] L-polylactic acid (weight average molecular weight 250KDa, optical purity 98%), QCS-PDLA and QCS were mixed in a mass ratio of 70:20:10, in hexafluoroisopropanol and dichloromethane (5:1, v / v ), dissolved in 10% (w / v) concentration of solid content, then added lithium bromide whose total mass was 0.5% and ...

Embodiment 3

[0059] (1) Preparation of QCS-PDLA

[0060] Under nitrogen protection, the QCS powder prepared and purified by the prior art and D-lactide are added together in methanesulfonic acid according to a molar ratio of 1:36 to prepare an acid solution with a solid content of 10% (w / v), The reaction was stirred at 55°C for 6 hours. After the reaction was completed, the reaction solution was poured into a buffer solution consisting of 10M sodium hydroxide and 0.2M dipotassium hydrogen phosphate in a pre-ice bath with a mixing ratio of 1:4. After the product was precipitated, it was filtered. The QCS-PLLA was obtained by washing with pure water and freeze-drying.

[0061] (2) Preparation of stereocomposite crystalline nanofiber membranes

[0062] L-polylactic acid (weight average molecular weight 200KDa, optical purity 98%), QCS-PDLA and QCS were mixed in a mass ratio of 60:30:10 in hexafluoroisopropanol and THF (1:1, v / v) Dissolve, prepare a solution with a solid content of 14% (w / v)...

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Abstract

The present invention not only discloses the polylactic acid-grafted quaternized chitosan with the following structure: first, the quaternized chitosan and D-lactide or L-lactide are added to an acidic solvent for stirring reaction, and then poured into buffer Precipitated in the solution, filtered, washed and freeze-dried: the above-mentioned polylactic acid grafted quaternized chitosan is also used to prepare a stereocomposite crystal nanofiber membrane and its application. Because the polylactic acid-modified quaternized chitosan disclosed in the present invention can be better compatible with polylactic acid, and can also be paired with polylactic acid for a short time at a lower temperature to form a stereocomposite crystal nanofiber film, which can avoid The degradation of polylactic acid can make the surface of the nanofiber membrane rich in quaternary ammonium groups, giving it stronger antibacterial properties, so it can be used in anti-infective wound dressings, food packaging, oil-water separation, filtration and sewage treatment. application prospects.

Description

technical field [0001] The invention belongs to the technical field of quaternized chitosan and high-voltage electrospinning fibers and their application, and in particular relates to a polylactic acid-grafted quaternized chitosan, and a polylactic acid-containing polylactic acid prepared by the high-voltage electrospinning technology. Stereocomposite crystal nanofiber membranes of grafted quaternized chitosan, and their preparation methods and applications. Background technique [0002] Chitosan is a natural cationic alkaline polysaccharide that exists in nature. It has the characteristics of non-irritant, good biocompatibility and biodegradability, so it is widely used in the field of biomaterials. However, due to the hydrogen bonds formed between the amino groups and hydroxyl groups in the chitosan structure or the rigid crystalline structure between hydrogen bonds, the water solubility of chitosan is poor, thus limiting its spinnability and practical application in the f...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G81/00D01F8/14D01F8/16D01F8/18D04H1/4382D04H1/728A61L15/26A61L15/44A61L15/46
CPCC08G81/00D04H1/4382D04H1/728D01F8/14D01F8/16D01F8/18A61L15/26A61L15/44A61L15/46A61L2400/12A61L2300/404A61L2300/412C08L87/00
Inventor 郭刚任杨梅陈海锋顾迎春
Owner SICHUAN UNIV
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