CN104511045A - Polyvinyl alcohol/chitosan nano fiber film dressing containing nano silver and preparation thereof - Google Patents
Polyvinyl alcohol/chitosan nano fiber film dressing containing nano silver and preparation thereof Download PDFInfo
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Abstract
The invention relates to a polyvinyl alcohol/chitosan nano fiber film dressing containing nano silver and preparation thereof. The nano fiber film dressing is prepared by the following steps: taking a mixture of polyvinyl alcohol and chitosan as the base material, then mixing nano silver into the polyvinyl alcohol/chitosan nano fiber film through an electrostatic spinning technology, and finally adding glutaraldehyde to crosslink the nano fiber film so as to obtain the target product. The obtained dressing has the characteristics that the preparation technology is simple; a wet environment can be achieved for promoting wound healing; and the dressing has an antiseptic function.
Description
Technical field
The present invention relates to a kind of Biomedical Textiles, specifically a kind of polyvinyl alcohol/chitosan nano fiber membrane dressing containing nanometer silver and preparation.
Background technology
Within 1962, Britain professor Winter proposes moisture treatment theory, and confirm and the drier wounds environment facies ratio be exposed in air, the moist environment that moistening and medical dressing application that is that have permeability is formed afterwards, can promote the formation of epithelium, accelerating wound healing.Various moist dressing arises at the historic moment since then, and research shows that desirable medical dressing should have following functions: 1. can absorb wound fluid, keeps wound surface moistening, prevents the loss of body fluid and moisture; 2. resist the invasion of antibacterial, protect from infection; 3. the adhesion of granulation and epithelial tissue and growth etc. are promoted.
In order to keep the wettability of wound surface, many water-soluble high-molecular materials are used as the raw material of medical dressing, comprise polyvinyl alcohol, polyvinylpyrrolidone, poly(ethylene oxide) etc., containing a large amount of hydroxyls in these molecules, a large amount of hydrogen bond can be formed with hydrone, therefore, prepared medical dressing can absorb moisture, for wound healing provides the environment of moistening.Simple water soluble polymer makes medical dressing, in use to scatter and disappear because of high molecular dissolving its stability, therefore, often blended with polysaccharide macromolecule (as chitosan, sodium alginate, collagen protein etc.), and carry out the crosslinked stability that could keep its pattern with cross-linking agent.
With the medical dressing that hydrophilic high molecular material is made, wet environment can be provided for wound healing, the chance of wound circumference bacterial infection also can be caused to increase simultaneously, therefore, also will strengthen the antibiotic property of medical dressing.Silver has broad spectrum antibacterial, adds the antibiotic property that nanometer silver can give dressing in dressing.Make nano-Ag particles activity with nanotechnology form and become large, easily agglomeration occurs, be difficult to directly add in dressing.
Adopt method of electrostatic spinning that nanometer silver and nanofiber can be made once-forming, make nanometer silver be evenly distributed in dressing, effectively the coming off and agglomeration of minimizing nanometer silver.Meanwhile, it is simple that method of electrostatic spinning prepares nanofiber technique, and structure-controllable, prepared nano fibrous membrane has the features such as specific surface area is large, porosity is large, is conducive to adhesion and the growth of wound cells.
Application number 200710171324.1, name is called the Chinese invention patent application of " for medical dressing composite nanometer fiber felt containing nano silver gelatin/chitosan and preparation ", discloses a kind of composite nanometer fiber felt be made up of the gelatin/chitosan nanofiber containing nanometer silver.Its preparation method is: be solvent with formic acid, is mixed according to a certain percentage by gelatin solution, adds silver nitrate, make nanofiber mats with method of electrostatic spinning with chitosan solution; The silver ion reduction in fiber is made to become Argent grain with irradiation under ultraviolet ray.The nano-Ag particles diameter adopting the method obtained is very little, and is evenly distributed in fiber felt, utilizes the strong antimicrobial effect of nanometer silver to can be made into medical dressing.Because the water absorbing capacity of gelatin itself is lower, so this composite nanometer fiber felt absorption transudate ability is not high.
Application number is 201010248219.5, the Chinese invention patent application that name is called " a kind of preparation method of the chitosan/polyvinyl alcohol sponge dressing containing nanometer silver ", disclose a kind of preparation method of the chitosan/polyvinyl alcohol sponge dressing containing nanometer silver: in Polyvinyl acetal reaction, add nanometer silver/polyglycol solution, and polyvinyl alcohol/chitosan alcohol blended liquid, the obtained chitosan/polyvinyl alcohol sponge dressing containing nanometer silver.Adopt the dressing that obtains of the method to have good biocompatibility, water absorption and antibiotic property, but this sponge dressing specific surface area is little, porosity is little, to the adhesion of wound cells and growth-promoting effect limited.
Summary of the invention
Technical problem to be solved by this invention is the defect overcoming prior art existence, a kind of polyvinyl alcohol/chitosan nano fiber membrane dressing containing nanometer silver and preparation are provided, this nano fibrous membrane with polyvinyl alcohol and chitosan compound for base material, by electrostatic spinning, nanometer silver is incorporated in polyvinyl alcohol/chitosan composite nano fibre film, then utilizes glutaraldehyde that nano fibrous membrane is cross-linked and obtain.
Described polyvinyl alcohol/chitosan nano fiber membrane the dressing containing nanometer silver, concrete preparation method is as follows:
(1) poly-vinyl alcohol solution is prepared
By water-soluble for polyvinyl alcohol with in the mixed solvent (water: ethanol mass ratio is 8:15) of ethanol, magnetic agitation, to dissolving completely, obtains the poly-vinyl alcohol solution that concentration is 8 ~ 20%.
(2) chitosan solution is prepared
Be dissolved in by chitosan in acetum (mass concentration 1%), magnetic agitation, to dissolving completely, obtains the chitosan solution that concentration is 3 ~ 10%.
(3) nano silver colloidal sol is prepared
Be precursor power nano silver colloidal sol according to following reaction with silver nitrate:
Polyvinylpyrrolidone (stabilizing agent as nanometer silver) is dissolved in DMF (as solvent and reducing agent), is made into reducing solution.By AgNO
3solution dropwise joins in reducing solution while stirring, dropwises, and continues to stir 6h, makes nano silver colloidal sol.
(4) polyvinyl alcohol/chitosan/nanometer silver spinning liquid is prepared
Get poly-vinyl alcohol solution and chitosan solution, 100:4 mixes in mass ratio, and dropwise add nano silver colloidal sol after magnetic agitation is even, the mass ratio of poly-vinyl alcohol solution and nano silver colloidal sol is 100:6, dropwises, and continues to stir 2h, is made into spinning liquid.
(5) electrostatic spinning
Polyvinyl alcohol/chitosan/nanometer silver the spinning liquid of preparation in step (4) is carried out electrostatic spinning and obtains nano fibrous membrane, employing aluminium foil receives, and electrostatic spinning process parameter is: voltage is 10kV, and syringe pump fltting speed is 20uL/min, receiving range is 12cm, and temperature is room temperature.
(6) glutaraldehyde cross-linking
The nano fibrous membrane of preparation in step (5) is placed in the crosslinked 1 ~ 3h of glutaraldehyde steam sealing.
Advantage of the present invention is: the present invention adopt method of electrostatic spinning to prepare containing nanometer silver polyvinyl alcohol/chitosan nano fiber membrane dressing, have preparation technology simple, can moistening environment be provided for wound healing and there is the features such as antibiotic property.
The present invention utilizes N, dinethylformamide is as solvent and reducing agent, polyvinylpyrrolidone is as the stabilizing agent of nanometer silver, by the presoma of nanometer silver---silver nitrate joins polyvinylpyrrolidone/N, in dinethylformamide solution, make silver ion reduction become nano silver colloidal sol, the nanometer silver diameter obtained like this is very little, avoids and directly adds nano silver powder.Adopt method of electrostatic spinning can make nanometer silver and nanofiber once-forming, nano-Ag particles is allowed to be attached to polyvinyl alcohol/chitosan composite nano fibre surface or to embed in fiber, effectively can reduce coming off and agglomeration of nanometer silver like this, the nanometer silver of formation is more uniformly distributed in nanofiber.Utilize the broad spectrum antibacterial of nanometer silver, composite nano-fiber membrane prepared by the present invention can be used as medical dressing.Polyvinyl alcohol is a kind of water soluble polymer, containing a large amount of hydroxyls, a large amount of hydrogen bond can be formed with hydrone, therefore, composite nano-fiber membrane prepared by the present invention can absorb moisture, for wound healing provides the environment of moistening, and utilize glutaraldehyde carry out crosslinked after, the stability of nano fibrous membrane under wet environment is also improved.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph containing nanometer silver composite nano-fiber membrane that embodiment 1 obtains
Fig. 2 is the scanning electron microscope (SEM) photograph containing nanometer silver composite nano-fiber membrane that embodiment 2 obtains
Fig. 3 is the scanning electron microscope (SEM) photograph containing nanometer silver composite nano-fiber membrane that embodiment 3 obtains
Fig. 4 be embodiment 1 obtained in PBS buffer, soak 1h containing nanometer silver composite nano-fiber membrane after scanning electron microscope (SEM) photograph
Fig. 5 be embodiment 2 obtained in PBS buffer, soak 1h containing nanometer silver composite nano-fiber membrane after scanning electron microscope (SEM) photograph
Fig. 6 be embodiment 3 obtained in PBS buffer, soak 1h containing nanometer silver composite nano-fiber membrane after scanning electron microscope (SEM) photograph
Fig. 7 is the x-ray photoelectron spectroscopy figure containing nanometer silver composite nano-fiber membrane that embodiment 3 obtains
As can be seen from Fig. 1 ~ 3, along with the prolongation of crosslinking time, the adhesion degree between nanofiber increases, and the hole of composite nano-fiber membrane reduces.
As can be seen from Fig. 4 ~ 6, along with the prolongation of crosslinking time, the maintenance fiber morphology stability of composite nano-fiber membrane strengthens.
As seen from Figure 7, there is nanometer silver in the surface of composite nano-fiber membrane.
Detailed description of the invention
Below in conjunction with example, the present invention is described further, but the scope of protection of present invention is not limited to the scope of case representation.
Containing polyvinyl alcohol/chitosan nano fiber membrane dressing and the preparation of nanometer silver, detailed description of the invention is as follows:
Embodiment 1
Take 8g polyvinyl alcohol to be dissolved in the mixed solvent (water: ethanol mass ratio is 8:15) of 92g water and ethanol, be made into the poly-vinyl alcohol solution that 100g mass fraction is 8%.Take the acetum that 0.24g chitosan is dissolved in 7.76g1%, be made into the chitosan solution that 8g mass fraction is 3%.In boiling water bath, be that the silver nitrate solution of 400g/L dropwise adds polyvinylpyrrolidone/N while stirring by 0.6ml concentration, (0.6g polyvinylpyrrolidone is dissolved in 5.4mL N to dinethylformamide solution, dinethylformamide) in, continue insulated and stirred 6h and make nano silver colloidal sol.After above-mentioned PVOH and chitosan solution mixing, dropwise add above-mentioned nano silver colloidal sol while stirring, dropwise, continue to stir 2h and be made into spinning liquid.Utilize electrostatic spinning apparatus to carry out spinning and obtain nano fibrous membrane, voltage is 10kV, and syringe pump fltting speed is 20uL/min, and adopt aluminium foil to receive, receiving range is 12cm.The glutaraldehyde measuring 50mL50% adds in the exsiccator of 180mm, 60 DEG C of preheatings after one hour, the crosslinked 1h of sealing on dividing plate nano fibrous membrane being placed in the inner porous of exsiccator, then by the dry 72h of vacuum drying oven that the nano fibrous membrane after crosslinked is placed in, namely obtained containing nanometer silver composite nano-fiber membrane sample A
1.
Embodiment 2
The concentration of poly-vinyl alcohol solution is expanded as 20%, and the sealing crosslinking time of nano fibrous membrane extends to 2h, other reagent and consumption and process conditions constant, repeat embodiment 1, namely obtained containing nanometer silver composite nano-fiber membrane sample A
2.
Embodiment 3
The concentration of chitosan solution is expanded as 10%, and the sealing crosslinking time of nano fibrous membrane extends to 3h, other reagent and consumption and process conditions constant, repeat embodiment 1, namely obtained containing nanometer silver composite nano-fiber membrane sample A
3.
Above-mentioned sample adopts following method to test its steady dissolution:
Concentration (is the KH of 0.1mol/L by the PBS buffer solution sample after crosslinked being immersed in respectively PH=7.4
2pO
4the Na of solution and 0.1mol/L
2hPO
4solution is by volume for 1:4 is obtained by mixing) in process 1h, with distilled water cleaning after taking-up, being placed in vacuum drying oven under the condition of 40 DEG C dries 24h.Then, utilize scanning electron microscope sem (NoVaNaVo SEM430, FEI Co.) to observe sample and soak the microscopic appearance before and after PBS buffer solution.
Claims (4)
1., containing polyvinyl alcohol/chitosan nano fiber membrane dressing of nanometer silver, it is characterized in that preparing nano fibrous membrane by method of electrostatic spinning with polyvinyl alcohol, chitosan, nanometer silver for raw material, then make nano fibrous membrane occur crosslinked with glutaraldehyde and obtain.
2., containing a preparation for the polyvinyl alcohol/chitosan nano fiber membrane dressing of nanometer silver, comprise the following steps:
(1) poly-vinyl alcohol solution is prepared
By water-soluble for polyvinyl alcohol with in the mixed solvent (water: ethanol mass ratio is 8:15) of ethanol, magnetic agitation, to dissolving completely, obtains the poly-vinyl alcohol solution that concentration is 8 ~ 20%.
(2) chitosan solution is prepared
Be dissolved in by chitosan in acetum (mass concentration 1%), magnetic agitation, to dissolving completely, obtains the chitosan solution that concentration is 3 ~ 10%.
(3) nano silver colloidal sol is prepared
Polyvinylpyrrolidone (stabilizing agent as nanometer silver) is dissolved in DMF (as solvent and reducing agent), is made into reducing solution.By AgNO
3solution dropwise joins in reducing solution while stirring, dropwises, and continues to stir 6h, makes nano silver colloidal sol.
(4) polyvinyl alcohol/chitosan/nanometer silver spinning liquid is prepared
Get poly-vinyl alcohol solution and chitosan solution, 100:4 mixes in mass ratio, and dropwise add nano silver colloidal sol after magnetic agitation is even, the mass ratio of poly-vinyl alcohol solution and nano silver colloidal sol is 100:6, dropwises, and continues to stir 2h, is made into spinning liquid.
(5) electrostatic spinning
Polyvinyl alcohol/chitosan/nanometer silver the spinning liquid of preparation in step (4) is carried out electrostatic spinning and obtains nano fibrous membrane, adopt aluminium foil to receive
(6) glutaraldehyde cross-linking
The nano fibrous membrane of preparation in step (5) being placed in glutaraldehyde steam, to carry out sealing crosslinked.
3. preparation method according to claim 2, is characterized in that: described electrostatic spinning process parameter, and voltage is 10kV, and syringe pump fltting speed is 20uL/min, and receiving range is 12cm, and temperature is room temperature.
4. preparation method according to claim 2, is characterized in that: the described glutaraldehyde cross-linking time is 1 ~ 3h.
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| CN106048892A (en) * | 2016-07-15 | 2016-10-26 | 东华大学 | Preparation method of GO/SA/PVA composite nanofiber membrane carrying nano silver particles |
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| CN113529278B (en) * | 2021-06-21 | 2022-06-21 | 五邑大学 | Crosslinking type nanofiber membrane and preparation method and application thereof |
| CN114892342A (en) * | 2022-04-26 | 2022-08-12 | 自然资源部第三海洋研究所 | Preparation method and application of antibacterial nanofiber membrane |
| CN115976735A (en) * | 2022-12-19 | 2023-04-18 | 南京理工大学 | Composite polylactic acid fiber membrane containing self-charged nano antibacterial agent, preparation method and application thereof |
| CN115976735B (en) * | 2022-12-19 | 2023-12-08 | 南京理工大学 | Composite polylactic acid fiber membrane containing self-charged nano antibacterial agent, preparation method and application thereof |
| CN116173283A (en) * | 2023-02-02 | 2023-05-30 | 江苏恰瑞生物科技有限公司 | Chitosan-polyvinyl alcohol SOD enzyme hydrogel dressing |
| CN116173283B (en) * | 2023-02-02 | 2024-02-27 | 江苏恰瑞生物科技有限公司 | Chitosan-polyvinyl alcohol SOD enzyme hydrogel dressing |
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