CN103993425A - Preparing method of polycaprolactone-keratin composite nano fiber film - Google Patents
Preparing method of polycaprolactone-keratin composite nano fiber film Download PDFInfo
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- CN103993425A CN103993425A CN201410263724.5A CN201410263724A CN103993425A CN 103993425 A CN103993425 A CN 103993425A CN 201410263724 A CN201410263724 A CN 201410263724A CN 103993425 A CN103993425 A CN 103993425A
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Abstract
The invention relates to a preparing method of a polycaprolactone-keratin composite nano fiber film. The preparing method comprises the steps that polycaprolactone is dissolved in a solvent, dissolution by stirring is carried out, and a polycaprolactone solution is obtained; keratin is dissolved in a solvent, dissolution by stirring is carried out, and a keratin solution is obtained; and the polycaprolactone solution and the keratin solution are mixed according to the weight ratio of 95 : 5-5 : 95, blending by stirring is carried out, a spinning solution is obtained, then electrostatic spinning is carried out, and the composite nano fiber film is obtained. The nano fiber film is prepared by the natural biomacromolecule material keratin and the polycaprolactone in a composite mode through an electrostatic spinning method, so that the nano fiber film has high porosity, and meanwhile good mechanical property and good biological property are achieved.
Description
Technical field
The invention belongs to the preparation field of nano fibrous membrane, particularly a kind of preparation method of polycaprolactone-keratin composite nano-fiber membrane.
Background technology
Keratin is a kind of insoluble fibrous animal protein, is the structural proteins of ectoderm cell, is extensively present in animal skin and cutaneous appendage, as hair, hoof, shell, pawl, angle, scale etc.Large quantity research in recent years shows, keratin is a kind of good biocompatibility and the high-quality bio-medical material that do not repelled by immunity of organism, has broad application prospects.At present, carry out basic research and the animal experiment study about keratin biomaterials in a large number both at home and abroad, at wound dressing [Wound Repair and Regeneration, 2012,20:236-242], artifical bone [Journal of Bioactive and Compatible Polymers, 2013,28:141-153] and the neural aspects such as [Biomaterials34 (2013) 5907-5914] of repairing all obtained good result, and there have portioned product to be applied to be clinical.
But existing studies have shown that, because keratic molecular weight is lower, the membrane material that single keratin material is made is conventionally more crisp, and mechanical strength is not high, and its application is restricted.Therefore, at present, most keratin based biomaterial often adopts keratin and natural polymer or artificial macromolecule compound, so both can keep improving the poor deficiency of single keratin mechanical property, as fibroin albumen [Biomacromolecules, 2008, 9, 1299 – 1305], PVA[Advances in Materials Science and Engineering, 2014, Article ID163678], PLGA[Journal of Bioactive and Compatible Polymers, 2013, 28:141-153], PLLA[Biomed.Mater.2013, 8:1-9] etc.Polycaprolactone (PCL) is a kind of business-like; Medical macromolecular materials, have good biocompatibility and degradability,, by the approval of Bureau of Drugs Supervision of the U.S., are widely used in the bio-medical fields such as pharmaceutical carrier, soft tissue repair, tissue engineering material.Therefore, the present invention has developed a kind of composite based on polycaprolactone and keratin bi-material.Meanwhile, in order to obtain the film material with high porosity, the present invention adopts the method for electrostatic spinning to prepare polycaprolactone and keratin composite membrane.Electrostatic spinning technique refers to and utilizes high voltage electric field environment to make polymer dope form charged injection stream, and this injection stream is elongated under electric field action, and solvent evaporates finally forms the nanofiber of certain form on receiving system.In recent ten years, this technology has become one of effective way of preparing nano-fiber material, and gained nanofiber porosity is high, and form is controlled, is widely used in the field such as medical dressing, tissue engineering bracket.The prepared polycaprolactone-keratin composite nano-fiber membrane of the present invention has kept the biologically active that keratin is good, possesses again toughness and mechanical strength that polycaprolactone is good, is expected to be applied to the fields such as medical dressing.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation method of polycaprolactone-keratin composite nano-fiber membrane, this invention is by the method for electrostatic spinning, by natural biological macromolecular material keratin and the compound nano fibrous membrane that is prepared into of polycaprolactone, make this nano fibrous membrane in possessing high porosity, demonstrate good mechanics and biology performance.
The preparation method of a kind of polycaprolactone-keratin composite nano-fiber membrane of the present invention, comprising:
(1) polycaprolactone is dissolved in solvent, stirring and dissolving, obtains polycaprolactone solution;
(2) keratin is dissolved in solvent, stirring and dissolving, obtains keratin solution;
(3) by polycaprolactone solution with keratin solution in mass ratio for 95:5-5:95 mixes, stir and evenly mix, obtain spinning solution, then carry out electrostatic spinning, obtain polycaprolactone-keratin composite nano-fiber membrane.
In described step (1), solvent is acetic acid or acetic/formic acid mixed solution; Wherein the quality concentration expressed in percentage by volume of acetic acid is more than or equal to 80%, and in acetic/formic acid mixed liquor, the volume ratio of acetic acid and formic acid is 1:9-9:1.
In described step (1), the mean molecule quantity of polycaprolactone is 70,000-90,000.
In described step (1), the concentration of polycaprolactone solution is 80-100mg/ml.
In described step (2), solvent is formic acid or acetic/formic acid mixed solution; Wherein the quality concentration expressed in percentage by volume of formic acid is more than or equal to 80%, and in acetic/formic acid mixed liquor, the volume ratio of acetic acid and formic acid is 1:9-9:1.
In described step (2), the concentration of keratin solution is 10-20mg/ml.
In described step (2), keratin is the keratin that adopts reducing process, oxidizing process, Hydrolyze method to obtain.
In described step (2), keratin is the keratin that animal extraction keratin or gene recombination technology obtain.
Described keratin can extract and obtain from human or animal's hairs such as human hair, wool, poultry feather, ox hairs, can be also to derive from other animal bodies of having reported such as hagfish, can be also the keratin product that gene recombination technology obtains.
In described step (2), keratic molecular weight is 3-300kDa.
In described step (3), electrostatic spinning process parameter is: voltage 13-35kV, and receiving range 8-22cm, spinning speed is 0.5-1.5ml/h, spinneret orifice internal diameter is 0.7-0.9mm, spinning temperature 20-30 DEG C, spinning humidity 45-65%; Receive nano silk with aluminium foil or cloth.
In described step (3), polycaprolactone-keratin composite nano-fiber membrane of gained is for medical wound dressing.
In described step (3), the nano fibrous membrane of gained is tridimensional network, and fibre diameter is 50-800nm.
beneficial effect
The present invention, by the method for electrostatic spinning, by natural biological macromolecular material keratin and the compound nano fibrous membrane that is prepared into of polycaprolactone, makes this nano fibrous membrane in possessing high porosity, demonstrates good mechanics and biology performance.
Detailed description of the invention
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.In addition should be understood that those skilled in the art can make various changes or modifications the present invention after having read the content of the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
Be 0.8g by quality, molecular weight ranges is 70,000-90, and 000 polycaprolactone is dissolved in the acetic/formic acid mixed liquor that 10ml, volume ratio are 30/70, carries out magnetic agitation to dissolving completely under room temperature, and obtaining concentration is the polycaprolactone solution of quality 80mg/ml.0.2g keratin solid is dissolved in to 10ml formic acid, under room temperature, carries out magnetic agitation to dissolving completely, obtain the keratin solution that concentration is 20mg/ml.Above-mentioned polycaprolactone is mixed according to the ratio of mass ratio 60:40 with keratin solution, and magnetic agitation is to mixing.Above-mentioned gained polycaprolactone/keratin solution is carried out to electrostatic spinning, and electrostatic spinning parameter is voltage 15kV, receiving range 12cm, and spinning speed is 0.5ml/h, spinneret orifice internal diameter is 0.7mm, 25 DEG C of spinning temperatures, spinning humidity 50%.Receive and spray the nano silk producing taking aluminium foil as receiver, obtain polycaprolactone-keratin composite nano-fiber membrane.
Embodiment 2
Be 1.0g by quality, molecular weight ranges is 70,000-90, and 000 polycaprolactone is dissolved in 10ml acetic acid, carries out magnetic agitation to dissolving completely under room temperature, and obtaining concentration is the polycaprolactone solution of quality 100mg/ml.0.15g keratin solid is dissolved in pure formic acid, under room temperature, carries out magnetic agitation to dissolving completely, obtain the keratin solution that concentration is 15mg/ml.Above-mentioned polycaprolactone is mixed according to the ratio of mass ratio 50:50 with keratin solution, and magnetic agitation is to mixing.Above-mentioned gained polycaprolactone/keratin solution is carried out to electrostatic spinning, and electrostatic spinning parameter is voltage 13kV, receiving range 10cm, and spinning speed is 0.8ml/h, spinneret orifice internal diameter is 0.7mm, 30 DEG C of spinning temperatures, spinning humidity 65%.Receive and spray the nano silk producing taking aluminium foil as receiver, obtain polycaprolactone-keratin composite nano-fiber membrane.
Embodiment 3
Be 1.0g by quality, molecular weight ranges is 70,000-90, and 000 polycaprolactone is dissolved in the acetic/formic acid mixed liquor that 10ml, volume ratio are 10/90, carries out magnetic agitation to dissolving completely under room temperature, and obtaining concentration is the polycaprolactone solution of quality 100mg/ml.0.15g keratin solid is dissolved in the acetic/formic acid mixed liquor that 10ml, volume ratio are 10/90, under room temperature, carries out magnetic agitation to dissolving completely, obtain the keratin solution that concentration is 15mg/ml.Above-mentioned polycaprolactone is mixed according to the ratio of mass ratio 95:5 with keratin solution, and magnetic agitation is to mixing.Above-mentioned gained polycaprolactone/keratin solution is carried out to electrostatic spinning, and electrostatic spinning parameter is voltage 13kV, receiving range 8cm, and spinning speed is 1.5ml/h, spinneret orifice internal diameter is 0.9mm, 20 DEG C of spinning temperatures, spinning humidity 45%.Receive and spray the nano silk producing taking aluminium foil as receiver, obtain polycaprolactone-keratin composite nano-fiber membrane.
Embodiment 4
Be 0.8g by quality, molecular weight ranges is 70,000-90, and 000 polycaprolactone is dissolved in the acetic/formic acid mixed liquor that 10ml, volume ratio are 90/10, carries out magnetic agitation to dissolving completely under room temperature, and obtaining concentration is the polycaprolactone solution of quality 80mg/ml.0.2g keratin solid is dissolved in the acetic/formic acid mixed liquor that 10ml, volume ratio are 90/10, under room temperature, carries out magnetic agitation to dissolving completely, obtain the keratin solution that concentration is 20mg/ml.Above-mentioned polycaprolactone is mixed according to the ratio of mass ratio 5:95 with keratin solution, and magnetic agitation is to mixing.Above-mentioned gained polycaprolactone/keratin solution is carried out to electrostatic spinning, and electrostatic spinning parameter is voltage 35kV, receiving range 22cm, and spinning speed is 1.5ml/h, spinneret orifice internal diameter is 0.9mm, 20 DEG C of spinning temperatures, spinning humidity 55%.Receive and spray the nano silk producing taking cloth as receiver, obtain polycaprolactone-keratin composite nano-fiber membrane.
Embodiment 5
Be 0.8g by quality, molecular weight ranges is 70,000-90, and 000 polycaprolactone is dissolved in 10ml acetic acid, carries out magnetic agitation to dissolving completely under room temperature, and obtaining concentration is the polycaprolactone solution of quality 80mg/ml.0.15g keratin solid is dissolved in to 10ml acetic acid, under room temperature, carries out magnetic agitation to dissolving completely, obtain the keratin solution that concentration is 15mg/ml.Above-mentioned polycaprolactone is mixed according to the ratio of mass ratio 95:5 with keratin solution, and magnetic agitation is to mixing.Above-mentioned gained polycaprolactone/keratin solution is carried out to electrostatic spinning, and electrostatic spinning parameter is voltage 15kV, receiving range 12cm, and spinning speed is 1.0ml/h, spinneret orifice internal diameter is 0.7mm, 15 DEG C of spinning temperatures, spinning humidity 55%.Receive and spray the nano silk producing taking aluminium foil as receiver, obtain polycaprolactone-keratin composite nano-fiber membrane.
Embodiment 6
Be 1.0g by quality, molecular weight ranges is 70,000-90, and 000 polycaprolactone is dissolved in 10ml, volume ratio is 30/70
Acetic/formic acid mixed liquor, under room temperature, carry out magnetic agitation to completely dissolve, obtaining concentration is the polycaprolactone solution of quality 100mg/ml.0.2g keratin solid is dissolved in to 10ml acetic acid, under room temperature, carries out magnetic agitation to dissolving completely, obtain the keratin solution that concentration is 20mg/ml.Above-mentioned polycaprolactone is mixed according to the ratio of mass ratio 90:10 with keratin solution, and magnetic agitation is to mixing.Above-mentioned gained polycaprolactone/keratin solution is carried out to electrostatic spinning, and electrostatic spinning parameter is voltage 15kV, receiving range 12cm, and spinning speed is 1.2ml/h, spinneret orifice internal diameter is 0.7mm, 15 DEG C of spinning temperatures, spinning humidity 55%.Receive and spray the nano silk producing taking aluminium foil as receiver, obtain polycaprolactone-keratin composite nano-fiber membrane.
Embodiment 7
Prepare polycaprolactone-keratin composite nano-fiber membrane according to the preparation method described in embodiment 1, measure by analysis, the fracture strength of composite nano-fiber material under drying regime is 1.4MPa, and elongation at break is 60%, porosity 93%.Taking vascular endothelial cell as cell model, adopt sem observation cell to stick form on material, and by mtt assay, the propagation behavior of cell is evaluated, result shows, endothelial cell shows good stick form and propagation behavior on composite nano-fiber material, has significant difference compared with single polycaprolactone nano fibrous membrane.According to the preparation method described in embodiment 1, the nano fibrous membrane of preparing with single keratin under drying regime fragility by force, easily broken.
Claims (11)
1. a preparation method for polycaprolactone-keratin composite nano-fiber membrane, comprising:
(1) polycaprolactone is dissolved in solvent, stirring and dissolving, obtains polycaprolactone solution;
(2) keratin is dissolved in solvent, stirring and dissolving, obtains keratin solution;
(3) by polycaprolactone solution with keratin solution in mass ratio for 95:5-5:95 mixes, stir and evenly mix, obtain spinning solution, then carry out electrostatic spinning, obtain polycaprolactone-keratin composite nano-fiber membrane.
2. the preparation method of a kind of polycaprolactone-keratin composite nano-fiber membrane according to claim 1, is characterized in that: in described step (1), solvent is acetic acid or acetic/formic acid mixed solution; Wherein the quality concentration expressed in percentage by volume of acetic acid is more than or equal to 80%, and in acetic/formic acid mixed liquor, the volume ratio of acetic acid and formic acid is 1:9-9:1.
3. the preparation method of a kind of polycaprolactone-keratin composite nano-fiber membrane according to claim 1, is characterized in that: in described step (1), the mean molecule quantity of polycaprolactone is 70,000-90,000.
4. the preparation method of a kind of polycaprolactone-keratin composite nano-fiber membrane according to claim 1, is characterized in that: in described step (1), the concentration of polycaprolactone solution is 80-100mg/ml.
5. the preparation method of a kind of polycaprolactone-keratin composite nano-fiber membrane according to claim 1, is characterized in that: in described step (2), solvent is formic acid or acetic/formic acid mixed solution; Wherein the quality concentration expressed in percentage by volume of formic acid is more than or equal to 80%, and in acetic/formic acid mixed liquor, the volume ratio of acetic acid and formic acid is 1:9-9:1.
6. the preparation method of a kind of polycaprolactone-keratin composite nano-fiber membrane according to claim 1, is characterized in that: in described step (2), the concentration of keratin solution is 10-20mg/ml.
7. the preparation method of a kind of polycaprolactone-keratin composite nano-fiber membrane according to claim 1, is characterized in that: in described step (2), keratin is the keratin that adopts reducing process, oxidizing process, Hydrolyze method to obtain.
8. the preparation method of a kind of polycaprolactone-keratin composite nano-fiber membrane according to claim 1, is characterized in that: in described step (2), keratin is the keratin that animal extraction keratin or gene recombination technology obtain.
9. the preparation method of a kind of polycaprolactone-keratin composite nano-fiber membrane according to claim 1, is characterized in that: in described step (2), keratic molecular weight is 3-300kDa.
10. the preparation method of a kind of polycaprolactone-keratin composite nano-fiber membrane according to claim 1, it is characterized in that: in described step (3), electrostatic spinning process parameter is: voltage 13-35kV, receiving range 8-22cm, spinning speed is 0.5-1.5ml/h, spinneret orifice internal diameter is 0.7-0.9mm, spinning temperature 20-30 DEG C, spinning humidity 45-65%; Receive nano silk with aluminium foil or cloth.
The preparation method of 11. a kind of polycaprolactone-keratin composite nano-fiber membranes according to claim 1, is characterized in that: in described step (3), polycaprolactone-keratin composite nano-fiber membrane of gained is for medical wound dressing.
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| CN104784744A (en) * | 2015-05-09 | 2015-07-22 | 南京师范大学 | Compound method for preparing wound dressing by utilizing human hair keratin |
| CN104784758A (en) * | 2015-05-09 | 2015-07-22 | 南京师范大学 | Preparation method of polymer/keratin composite anticoagulation vascular tissue engineering scaffold |
| CN107519524A (en) * | 2017-09-21 | 2017-12-29 | 滨州医学院 | A kind of polycaprolactone/collagen/quaternary ammonium salt electrospun composite fibers film and preparation method thereof |
| CN108179547A (en) * | 2017-12-19 | 2018-06-19 | 东华大学 | A kind of preparation method of the fluorescent nano-fiber film as heavy metal antimony Visual retrieval device |
| CN114427119A (en) * | 2022-01-21 | 2022-05-03 | 华中科技大学 | Preparation method and application of frozen electrostatic spinning of polymer fiber membrane |
| CN116084085A (en) * | 2021-11-05 | 2023-05-09 | 亚格生技股份有限公司 | Method for manufacturing nanofiber film |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108179547A (en) * | 2017-12-19 | 2018-06-19 | 东华大学 | A kind of preparation method of the fluorescent nano-fiber film as heavy metal antimony Visual retrieval device |
| CN116084085A (en) * | 2021-11-05 | 2023-05-09 | 亚格生技股份有限公司 | Method for manufacturing nanofiber film |
| CN114427119A (en) * | 2022-01-21 | 2022-05-03 | 华中科技大学 | Preparation method and application of frozen electrostatic spinning of polymer fiber membrane |
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