CN103600521A - Controllable-property collagen nanometer fibre non-woven fabric preparation method - Google Patents
Controllable-property collagen nanometer fibre non-woven fabric preparation method Download PDFInfo
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- CN103600521A CN103600521A CN201310586160.4A CN201310586160A CN103600521A CN 103600521 A CN103600521 A CN 103600521A CN 201310586160 A CN201310586160 A CN 201310586160A CN 103600521 A CN103600521 A CN 103600521A
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Abstract
The invention relates to a controllable-property collagen nanometer fibre non-woven fabric preparation method. The controllable-property collagen nanometer fibre non-woven fabric preparation method is characterized in that a gradient type in-situ crosslinking gelatin nanometer fiber (CGN) prepared by active static spinning and a multi-hole layer as well as thermoplasticity non-crosslinking biodegradable polyester non-woven fabric are laminated together in a multifunctional model support system; the mechanical strength, biodegradation speed rate and a biological function of the crosslinking gelatin nanometer fibre/poly-caprolactone/crosslinking gelatin nanometer fibre (CGN/PCL/CGN) layered creature composite material prepared by the invention are regulated through regulating and controlling the kind, composition, fiber diameter, air porosity, number and sequence of each layer; CGN/PCL multi-layer creature composite material can be cut into different shapes according to the need and is connected to a tissue through a surgery sewing operation, the requirements of different patients are realized, and the medical extensive use is realized.
Description
Technical field
The present invention relates to build the model support material of soft tissue regeneration, relate in particular to a kind of preparation method of Static Spinning collagen nanofiber nonwoven.
Background technology
Regenerative medicine be one in the fast-developing field of the multidisciplinary intersection in material science, bioengineering, cell biological and biological medicine forward position.The very large challenge that at present cell engineering Material Field faces is exactly can analog cell epimatrix (ECM) and promote the research of the timbering material as three-dimensional template of regeneration, the structure similar with fibrous cell's epimatrix with and the size of nanoscale make nano fiber non-woven fabric and micrometer/nanometer hybrid nonwoven cloth be considered to the very promising candidate material for above-mentioned timbering material.For the timbering material of traditional large scale or micro-dimension, thereby collagen nanofiber nonwoven needs less cell concentration to realize effective cell seeding, cell adherence and Cell Differentiation.And the dispersion of the growth of cell, nutrition and oxygen does not only occur in the surface of support, but be diffused in whole support.
In numerous Polymer Processing technology, electrostatic spinning has represented a kind of technology of guided bone.The cost of electrostatic spinning is lower, and especially outstanding be that electrostatic spinning technique can be used for design functionality nanofiber and nonwoven fabric construct, between dispensing end and receiving terminal, the polymer solution early capillary place of syringe forms the superfine fibre of random deposition Cheng Gan on injected current and then receiving system, thereby forms nano fiber non-woven fabric.Utilize electrostatic spinning can prepare nanometer or the micrometer fibers of a variety of polymer.Electrostatic spinning has successfully been used for preparing bionical protein nano fibrous framework material, electrostatic spinning synthetic or natural polymer has been used to design class like the nonwoven system of extracellular matrix, for example, Biodegradable high-molecular polycaprolactone (PCL) and PLA (PLA), although the polymer of electrostatic spinning has good mechanical property, but the cell adhesion of synthetic polymer and Cell Differentiation performance are not as natural biological macromolecule, therefore, the synthetic macromolecule of the natural biological macromolecule such as gelatin and picture polycaprolactone and this class of PLA, after mixing, carry out again electrostatic spinning, the another kind of method that improves synthesized polymer physical performance is that gelatin is grafted on synthetic fibers.With synthetic fibers, compare, the performance of composite fibre and graft fibres all improves significantly.Mixing of natural biological copolymer nanofiber provides extraordinary biocompatibility and cell adhesion, but its meeting swelling in water, and the mechanical strength in water is very low, is its maximum weakness.
Summary of the invention
The present invention relates to the controlled collagen nanofiber nonwoven preparation method of a kind of performance, concrete preparation method is as follows:
(1) electrostatic spinning of gelatin solution: the acetic acid that gelatin powder is dissolved in to 1:2:1, in the mixed solution of ethyl acetate and water, stir the solution (25wt%) that 3h obtains clarification, before carrying out electrostatic spinning, solution mixes with a certain amount of glyoxal solution, mixed solution is transferred in syringe provides power to advance spinning solution (advancing speed 0.9～1.8mL/h) with syringe pump, the diameter of spinning head is 0.6mm, dispensing end connects high-voltage power apparatus, voltage is 14～18kV, the electrostatic spinning nano fiber felt obtaining is placed 3～4h and is obtained cross-linked gelatin nanofiber at 70～75 ℃.
(2) micro-the extruding of three-dimensional of polycaprolactone (PCL): in 3D fiber laydown device, polycaprolactone (PCL, Mw=75000～85000g/mol, viscosity: 1.03～1.12dl/g) be transferred in the extrusion device of heating, extruded velocity is 400～500mm/min, temperature is 140～170 ℃, and pressure is 0.96bar, and nozzle diameter is 0.6mm.
In the present invention, in a multi-functional model support system, the in-situ cross-linked gelatine nano fiber of gradient type (CGN) that active electro-spinning is standby and many hole layers and the uncrosslinked biodegradable polyester non-woven fabric of thermoplasticity are laminated together; In Static Spinning process, in nontoxic mixed solvent (acetic acid/ethyl acetate/water, 5:3:2, w/w/w), add dialdehyde that gelatin is carried out in-situ cross-linked.Thereby not fluorine-containing interconnected system has been eliminated the step that traditional cross-linked gelatin nanofiber has been simplified in crosslinked post processing.Thereby the existence of glyoxal makes gelatin little by little be cross-linked the concentration that increases gradually gelatin solution, and the diameter of electrostatic spinning nano fiber increases to 680nm from 90nm gradually; Then in the process of lamination, micro-micron polycaprolactone (PCL) fabric nonwoven cloth and the cross-linked gelatin nanofiber layer of extruding of 3D mixes.
The specific embodiment
In order to deepen the understanding of the present invention, below in conjunction with specific embodiment, the present invention is described in further detail.
(1) electrostatic spinning of gelatin solution: gelatin powder is dissolved in the mixed solution of acetic acid, ethyl acetate and water of 1/2/1 (v/v), stir the solution (25wt%) that 3h obtains clarification, before carrying out electrostatic spinning, solution mixes with the glyoxal solution of 10mL, and mixed solution is transferred in syringe provides power to advance spinning solution (advancing speed 0.9mL/h) with syringe pump.The diameter of spinning head is 0.6mm, and dispensing end connects high-voltage power apparatus, and high pressure is 14kV.The electrostatic spinning nano fiber felt obtaining 3h at 70 ℃ obtains cross-linked gelatin nanofiber.
(2) micro-the extruding of three-dimensional of polycaprolactone (PCL): in 3D fiber laydown device, polycaprolactone (PCL, Mw=82000g/mol, viscosity: 1.09dl/g) be transferred in the extrusion device of heating, extruded velocity is 500mm/min, temperature is 140 ℃, and pressure is 0.96bar, and nozzle diameter is 0.6mm.
Claims (2)
1. a preparation method for the controlled collagen nanofiber nonwoven of performance, its step is as follows:
(1) electrostatic spinning of gelatin solution:
Gelatin powder is dissolved in the mixed solution of 1/2/1 acetic acid, ethyl acetate and water, stir the solution (25wt%) that 3h obtains clarification, before carrying out electrostatic spinning, solution mixes with a certain amount of glyoxal solution, mixed solution is transferred in syringe provides power to advance spinning solution (advancing speed 0.9～1.8mL/h) with syringe pump, the diameter of spinning head is 0.6mm, dispensing end connects high-voltage power apparatus, voltage is 14～18kV, and the electrostatic spinning nano fiber felt obtaining is placed 3～4h and obtained cross-linked gelatin nanofiber at 70～75 ℃;
(2) micro-the extruding of three-dimensional of polycaprolactone (PCL):
In 3D fiber laydown device, polycaprolactone (PCL, Mw=75000～85000g/mol, viscosity: 1.03～1.12dl/g) be transferred in the extrusion device of heating, extruded velocity is 400～500mm/min, and temperature is 140～170 ℃, pressure is 0.96bar, and nozzle diameter is 0.6mm.
2. collagen nanofiber nonwoven preparation method as claimed in claim 1, is characterized in that: described spinning voltage is 15kV.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310586160.4A CN103600521B (en) | 2013-11-15 | 2013-11-15 | Controllable-property collagen nanometer fibre non-woven fabric preparation method |
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| CN201310586160.4A CN103600521B (en) | 2013-11-15 | 2013-11-15 | Controllable-property collagen nanometer fibre non-woven fabric preparation method |
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| CN103600521A true CN103600521A (en) | 2014-02-26 |
| CN103600521B CN103600521B (en) | 2015-07-15 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110404110A (en) * | 2019-08-21 | 2019-11-05 | 华南理工大学 | A kind of collagen-based cornea regeneration repair materials of resistance to suture and preparation method thereof |
| WO2021227395A1 (en) * | 2020-05-15 | 2021-11-18 | 成都硕屋科技有限公司 | Production process for nanoporous composite material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1403163A (en) * | 2002-10-23 | 2003-03-19 | 东南大学 | Absorbable fiber reinforced multilayer film material and its prepn |
| WO2012136701A1 (en) * | 2011-04-05 | 2012-10-11 | Universitätsklinikum Freiburg | Biocompatible and biodegradable gradient layer system for regenerative medicine and for tissue support |
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2013
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1403163A (en) * | 2002-10-23 | 2003-03-19 | 东南大学 | Absorbable fiber reinforced multilayer film material and its prepn |
| WO2012136701A1 (en) * | 2011-04-05 | 2012-10-11 | Universitätsklinikum Freiburg | Biocompatible and biodegradable gradient layer system for regenerative medicine and for tissue support |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110404110A (en) * | 2019-08-21 | 2019-11-05 | 华南理工大学 | A kind of collagen-based cornea regeneration repair materials of resistance to suture and preparation method thereof |
| CN110404110B (en) * | 2019-08-21 | 2021-10-22 | 华南理工大学 | Suture-resistant collagen-based cornea regeneration repair material and preparation method thereof |
| WO2021227395A1 (en) * | 2020-05-15 | 2021-11-18 | 成都硕屋科技有限公司 | Production process for nanoporous composite material |
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| CN103600521B (en) | 2015-07-15 |
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