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Preparation method of high intensity biodegradable supramolecule hydrogel

A supramolecular hydrogel and biodegradation technology, applied in the field of preparation of high-strength biodegradable supramolecular hydrogel, can solve the problems of low strength, inappropriateness, low strength, etc., and achieve a simple preparation method and fast application. Effect

Inactive Publication Date: 2008-10-22
WUHAN TEXTILE UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the supramolecular physical gel obtained in the above-mentioned method still has the following disadvantages: 1. the stability is poor, and the original network of the supramolecular physical gel changes when the external environment changes (such as shearing, pH value change and temperature change, etc.). The structure will change; ②The strength is not high. The supramolecular physical gel is formed by the clathrate crystal domain as the physical cross-linking point. When the external environment changes, it is easy to be damaged, so the strength is low, and it is not suitable as a tissue engineering scaffold. Material
[0005] "Synthesis and characterization of photopolymerized α-CD assembled supramolecular structure hydrogel" in the journal "Chemical Journal of Chinese Universities" 2003 Issue 24 introduced the use of photopolymerization cross-linking technology to prepare stable supramolecular hydrogels, which can avoid The use of chemical cross-linking agents is eliminated, but the preparation process needs to be carried out in organic solvents, and the resulting gel lacks stimuli responsiveness

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0019] Add 10g of dry F68 (a Pluronic block copolymer with an average molecular weight of 8400) to a 50ml clean single-necked round bottom flask, and add 1.09g of freshly distilled ε-caprolactone monomer and 3mg of For stannous octoate, after evacuating for 10 minutes, introduce argon gas, and repeat evacuation-ventilation for 3 times, and finally, under the protection of argon gas and magnetic stirring, the bulk polymerization reaction is carried out at 130°C for 12 hours, after cooling, it is dissolved in chloroform, and Precipitate with anhydrous ether, filter, and vacuum-dry the precipitate at 30°C to constant weight to obtain a water-soluble F68 / PCL block copolymer.

[0020]Add 5 g of the F68 / PCL block copolymer synthesized above to a 100 ml single-necked round-bottomed flask containing 60 ml of dry dichloromethane, place the single-necked round-bottomed flask in an ice bath and cool it to 0°C, and first add 0.5 ml of triethyl ether amine, then add 0.26ml of acryloyl chlo...

Embodiment 2

[0023] Add 60ml of toluene and 10g of F127 (a Pluronic block copolymer with an average molecular weight of 12600) to a 100ml clean single-necked round-bottomed flask, azeotropically distill 30ml of toluene under the protection of argon, and add 0.36g of toluene after cooling to room temperature Freshly distilled ε-caprolactone monomer and 10 mg stannous octoate were refluxed at 110°C for 18 hours under the protection of argon and magnetic stirring. Drying under vacuum to a constant weight yields a water-soluble F127 / PCL block copolymer.

[0024] Add 5 g of the F127 / PCL block copolymer synthesized above to a 100 ml single-necked round-bottomed flask containing 60 ml of dry dichloromethane, place the single-necked round-bottomed flask in an ice bath and cool it to 0°C, and first add 0.3 ml of triethyl ether amine, then add 0.22ml of methacryloyl chloride dropwise, react at 0°C for 12h, and then continue to react at 25°C for 12h, filter to remove by-products, and precipitate with...

Embodiment 3

[0027] Add 50ml of toluene and 10g of F68 (a Pluronic block copolymer with an average molecular weight of 8400) to a 100ml clean single-necked round-bottomed flask, azeotropically distill 25ml of toluene under the protection of argon, and cool to room temperature under argon Add 0.81g of freshly distilled ε-caprolactone monomer and 7mg of stannous octoate under protection, under the protection of argon and magnetic stirring, reflux reaction at 110°C for 24h, the reactant is cooled and precipitated with anhydrous ether, filtered , vacuum-dried to constant weight at 40°C to obtain a water-soluble F68 / PCL block copolymer.

[0028] Add 5 g of the F68 / PCL block copolymer synthesized above, 0.16 g of acrylic acid, 0.13 g of 4-methylaminopyridine and 0.34 g of N , N'-dicyclohexanecarbodiimide. The reaction system was reacted at 25° C. for 24 hours. After filtration, the filtrate was precipitated with petroleum ether, and the product was vacuum-dried at 40° C. to constant weight to o...

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Abstract

The invention belongs to the field of a biological medical polymeric material and relates to a preparation method of biodegradable supermolecular hydrogel with high strength. The preparation method is that firstly, Pluronic block copolymer and stannous octoate are used as coinitiator to initiate Epsilon-caprolactone monomer ring-opening polymerization and acrylate or methacrylate is terminated to obtain a photopolymerisable macromonomer. Then, macromonomer solution which is mixed with micro-photo initiator is mixed with Alpha-cyclodextrin solution of certain concentration to rapidly form the precursor of supermolecular physical gel. The precursor of physical gel can rapidly form the supermolecular hydrogel with high strength in situ after the irradiation of ultraviolet. The preparation method of the invention relates no organic solvent, cross linking agent and related reaction. The preparation method is simple and can be applied rapidly. And the strength and the temperature responsive property of the supermolecular hydrogel can be regulated and controlled. The obtained biodegradable supermolecular hydrogel with high strength can be widely applied to the field of the biological medical engineering material.

Description

technical field [0001] The invention belongs to the field of biomedical polymer materials, in particular to a preparation method of high-strength biodegradable supramolecular hydrogel. Background technique [0002] Polymer hydrogels have been widely used in the fields of biomedical materials such as drug release, tissue engineering, and other engineering technology fields due to their good biocompatibility, permeability, and non-inactivation of drug loading. According to the different connection methods of hydrogel network, hydrogel can be divided into chemical gel and physical gel. Chemical gels are often formed by covalent bonds formed by chemical reactions under the action of chemical cross-linking agents; physical gels are formed through non-covalent interactions, such as hydrogen bonds, hydrophobic interactions, chain entanglements, and crystallization. role formation. [0003] Injectable physical gels formed in situ have attracted extensive attention in the fields of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61L31/04A61L31/14A61K47/30
Inventor 赵三平徐卫林
Owner WUHAN TEXTILE UNIV
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