CN104511045B - A kind of preparation method of the polyvinyl alcohol containing nano silver/chitosan nano fiber membrane dressing - Google Patents
A kind of preparation method of the polyvinyl alcohol containing nano silver/chitosan nano fiber membrane dressing Download PDFInfo
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Abstract
The present invention relates to a kind of polyvinyl alcohol containing nano silver/chitosan nano fiber membrane dressing and preparation.Nano silver is incorporated into polyvinyl alcohol/chitosan nano fiber membrane by the nanofiber film dressing using polyvinyl alcohol and chitosan compound as base material, by electrostatic spinning, then makes nano fibrous membrane be crosslinked to obtain using glutaraldehyde.The dressing that the present invention obtains has the characteristics that the environment that preparation process is simple, can provide moistening for wound healing and has antibiotic property.
Description
Technical field
The present invention relates to a kind of Biomedical Textiles, specifically a kind of polyvinyl alcohol/chitosan containing nano silver
The preparation method of nanofiber film dressing.
Background technology
Britain professor Winter in 1962 proposes moisture treatment theory, and the dry wound for confirming and being exposed in air
Choma border is compared, and the moist environment for moistening and being formed after the medical dressing application with permeability can promote the formation of epithelium,
Accelerating wound healing.Various moist dressings come into being since then, research shows that ideal medical dressing should have following work(
Energy：1. wound fluid can be absorbed, surface of a wound wetting is kept, the loss of body fluid and moisture is prevented；2. resisting the invasion of bacterium, prevent
Infection；3. promoting the adherency and growth etc. of granulation and epithelial tissue.
In order to keep the wetability of the surface of a wound, many water-soluble high-molecular materials are used as the raw material of medical dressing, including gather
Vinyl alcohol, polyvinylpyrrolidone, polyethylene oxide etc. contain a large amount of hydroxyl in these molecules, can be formed with hydrone greatly
Hydrogen bond is measured, therefore, prepared medical dressing can absorb moisture, and the environment of wetting is provided for wound healing.Merely with water-soluble
Property macromolecule medical dressing is made, in use can because of it is high molecular dissolving and scatter and disappear its stability therefore often want
It is blended with polysaccharide family macromolecule (such as chitosan, sodium alginate, collagen), it could be kept by being used in combination crosslinking agent to carry out crosslinking
The stability of pattern.
The medical dressing made of hydrophilic high molecular material can provide wet environment for wound healing, while can also lead
It causes the chance of wound circumference bacterial infection to increase, therefore, also to enhance the antibiotic property of medical dressing.Silver has broad spectrum antibacterial,
Nano silver is added in dressings can assign the antibiotic property of dressing.Nano-Ag particles activity is made in the form of nanotechnology to become larger, holds
Agglomeration easily occurs, it is difficult to be directly added into dressing.
Nano silver can be made once-forming with nanofiber using method of electrostatic spinning, nano silver is made to be evenly distributed in dressing
In, effectively reduce nano silver fall off and agglomeration.Meanwhile method of electrostatic spinning prepares that nanofiber is simple for process, and structure can
Control, prepared nano fibrous membrane have the characteristics that large specific surface area, porosity are big, are conducive to the adherency and life of wound cells
It is long.
Application number 200710171324.1, it is entitled " fine for medical dressing composite Nano containing nano silver gelatin/chitosan
Tie up felt and preparation " Chinese invention patent application, disclose and a kind of be made of the gelatin/chitosan nanofiber containing nano silver
Composite nanometer fiber felt.Preparation method is：Using formic acid as solvent, gelatin solution is mixed according to a certain percentage with chitosan solution
It closes, silver nitrate is added, nanofiber mats are made with method of electrostatic spinning；Make the silver ion reduction Cheng Yin in fiber with ultraviolet light
Particle.It using nano-Ag particles diameter very little made from this method, and is evenly distributed in fine felt, utilizes the strong antibacterial of nano silver
Effect can be made into medical dressing.Because the water absorbing capacity of gelatin itself is relatively low, this composite nanometer fiber felt absorbs exudation
Liquid energy power is not high.
Application No. is 201010248219.5, it is entitled " a kind of chitosan/polyvinyl alcohol sponge dressing containing nano silver
The Chinese invention patent application of preparation method " discloses a kind of preparation of the chitosan/polyvinyl alcohol sponge dressing containing nano silver
Method：In Polyvinyl acetal reaction, nano silver/polyglycol solution is added and polyvinyl alcohol/chitosan alcohol is blended
The chitosan/polyvinyl alcohol sponge dressing containing nano silver is made in liquid.There is good biofacies using the dressing that this method obtains
Capacitive, water imbibition and antibiotic property, but this sponge dressing specific surface area is small, porosity is small, adherency and growth to wound cells
Facilitation is limited.
Invention content
The technical problem to be solved by the present invention is to overcome defect of the existing technology, provide a kind of poly- containing nano silver
Vinyl alcohol/chitosan nano fiber membrane dressing and preparation, the nano fibrous membrane using polyvinyl alcohol and chitosan compound as base material,
Nano silver is incorporated into polyvinyl alcohol/chitosan composite nano fibre film by electrostatic spinning, then makes to receive using glutaraldehyde
Rice tunica fibrosa is crosslinked to obtain.
Polyvinyl alcohol containing the nano silver/chitosan nano fiber membrane dressing, specific preparation method are as follows：
(1) poly-vinyl alcohol solution is prepared
Polyvinyl alcohol is dissolved in the mixed solvent (water of water and ethyl alcohol：Ethyl alcohol mass ratio is 8：15) in, magnetic agitation is to complete
Fully dissolved obtains a concentration of 8~20% poly-vinyl alcohol solution.
(2) chitosan solution is prepared
Chitosan is dissolved in acetum (mass concentration 1%), magnetic agitation to being completely dissolved, obtain a concentration of 3~
10% chitosan solution.
(3) nano silver colloidal sol is prepared
According to following reactions nano silver colloidal sol is prepared by presoma of silver nitrate：
Polyvinylpyrrolidone (stabilizer as nano silver) is dissolved in n,N-Dimethylformamide (as solvent and also
Former agent) in, it is made into reducing solution.By AgNO3Solution is added dropwise in reducing solution while stirring, is added dropwise, and continues to stir 6h,
Nano silver colloidal sol is made.
(4) polyvinyl alcohol/chitosan/nano silver spinning solution is prepared
Take poly-vinyl alcohol solution and chitosan solution, in mass ratio 100：4 are mixed, and are added dropwise after magnetic agitation is uniform
Enter nano silver colloidal sol, the mass ratio of poly-vinyl alcohol solution and nano silver colloidal sol is 100：6, it is added dropwise, continues to stir 2h, be made into
Spinning solution.
(5) electrostatic spinning
Polyvinyl alcohol/the chitosan prepared in step (4)/nano silver spinning solution is subjected to electrostatic spinning and obtains nanofiber
Film is received using aluminium foil, and electrostatic spinning process parameter is：Voltage is 10kV, and syringe pump fltting speed is 20uL/min, receive away from
From for 12cm, temperature is room temperature.
(6) glutaraldehyde cross-linking
The nano fibrous membrane prepared in step (5) is placed in 1~3h of sealing crosslinking in glutaraldehyde steam.
It is an advantage of the invention that：The present invention uses polyvinyl alcohol containing nano silver/chitosan nano prepared by method of electrostatic spinning
Fiber film dressing has the characteristics that the environment that preparation process is simple, can provide moistening for wound healing and has antibiotic property.
The present invention is using n,N-Dimethylformamide as solvent and reducing agent, and polyvinylpyrrolidone is as nano silver
Stabilizer, presoma-silver nitrate of nano silver is added in polyvinylpyrrolidone/n,N-Dimethylformamide solution,
Make silver ion reduction at nano silver colloidal sol, the nano silver diameter very little obtained in this way avoids and is directly added into nano silver powder.It adopts
Nano silver can be made once-forming with nanofiber with method of electrostatic spinning, allow nano-Ag particles to be attached to polyvinyl alcohol/chitosan multiple
Close in nanofiber surface or embedded fiber, can effectively reduce in this way nano silver fall off and agglomeration, make the nanometer to be formed
Silver is more uniformly distributed in nanofiber.Using the broad spectrum antibacterial of nano silver, composite nano-fiber membrane prepared by the present invention
It can be used as medical dressing.Polyvinyl alcohol is a kind of water soluble polymer, and containing a large amount of hydroxyl, a large amount of hydrogen can be formed with hydrone
Key, therefore, composite nano-fiber membrane prepared by the present invention can absorb moisture, and the environment of wetting is provided for wound healing, and sharp
After being crosslinked with glutaraldehyde, stability of the nano fibrous membrane under wet environment is also improved.
Description of the drawings
It, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical solution in the prior art
Embodiment or attached drawing needed to be used in the description of the prior art are briefly described, it should be apparent that, in being described below
Attached drawing is some embodiments of the present invention, for those of ordinary skill in the art, before not making the creative labor
It puts, other drawings may also be obtained based on these drawings.
Fig. 1 is the scanning electron microscope (SEM) photograph of the composite nano-fiber membrane containing nano silver made from embodiment 1；
Fig. 2 is the scanning electron microscope (SEM) photograph of the composite nano-fiber membrane containing nano silver made from embodiment 2；
Fig. 3 is the scanning electron microscope (SEM) photograph of the composite nano-fiber membrane containing nano silver made from embodiment 3；
Fig. 4 is that composite nano-fiber membrane containing nano silver made from embodiment 1 impregnates the scanning electricity after 1h in PBS buffer solution
Mirror figure；
Fig. 5 is that composite nano-fiber membrane containing nano silver made from embodiment 2 impregnates the scanning electricity after 1h in PBS buffer solution
Mirror figure；
Fig. 6 is that composite nano-fiber membrane containing nano silver made from embodiment 3 impregnates the scanning electricity after 1h in PBS buffer solution
Mirror figure；
Fig. 7 is the x-ray photoelectron spectroscopy figure of the composite nano-fiber membrane containing nano silver made from embodiment 3；It can be with by Fig. 1~3
Find out, with the extension of crosslinking time, the adhesion degree between nanofiber increases, and the hole of composite nano-fiber membrane is reduced.
As the extension of crosslinking time, the holding fiber morphology of composite nano-fiber membrane are stablized it can be seen from Fig. 4~6
Property enhancing.
As seen from Figure 7, there are nano silvers on the surface of composite nano-fiber membrane.
Specific implementation mode
With reference to example, the present invention is described further, but the scope of protection of present invention is not limited to example
The range of expression.
A kind of polyvinyl alcohol containing nano silver/chitosan nano fiber membrane dressing and preparation, specific implementation mode are as follows：
Embodiment 1
Weigh the mixed solvent (water that 8g polyvinyl alcohol is dissolved in 92g water and ethyl alcohol：Ethyl alcohol mass ratio is 8：15) it in, is made into
The poly-vinyl alcohol solution that 100g mass fractions are 8%.The acetum that 0.24g chitosans are dissolved in 7.76g1% is weighed, 8g is made into
The chitosan solution that mass fraction is 3%.In boiling water bath, while stirring by the silver nitrate solution of a concentration of 400g/L of 0.6ml
Polyvinylpyrrolidone/n,N-Dimethylformamide solution is added dropwise, and (0.6g polyvinylpyrrolidones are dissolved in 5.4mL N, N-
Dimethylformamide) in, continue insulated and stirred 6h and nano silver colloidal sol is made.After above-mentioned polyethanol and chitosan solution are mixed,
Above-mentioned nano silver colloidal sol is added dropwise while stirring, is added dropwise, continues stirring 2h and is made into spinning solution.Utilize electrostatic spinning apparatus
It carries out spinning and obtains nano fibrous membrane, voltage 10kV, syringe pump fltting speed is 20uL/min, is received using aluminium foil, is received
Distance is 12cm.The glutaraldehyde for measuring 50mL50% is added in the drier of 180mm, after being preheated one hour at 60 DEG C, by nanometer
Tunica fibrosa is placed in inside drier sealing crosslinking 1h on a porous partition board, is then placed in the nano fibrous membrane after crosslinking
Dry 72h, obtains the sample of composite nano-fiber membrane containing nano silver A1 in vacuum drying chamber.
Embodiment 2
The concentration of poly-vinyl alcohol solution is expanded as 20%, the sealing crosslinking time of nano fibrous membrane extends to 2h, other
Reagent and dosage and process conditions are constant, repeat embodiment 1, obtain the sample of composite nano-fiber membrane containing nano silver A2.
Embodiment 3
The concentration of chitosan solution is expanded as 10%, the sealing crosslinking time of nano fibrous membrane extends to 3h, other examinations
Agent and dosage and process conditions are constant, repeat embodiment 1, obtain the sample of composite nano-fiber membrane containing nano silver A3.
Above-mentioned sample tests its steady dissolution using following methods：
Sample after crosslinking is separately immersed in the PBS buffer solutions of PH=7.4 (by the KH2PO4 of a concentration of 0.1mol/L
The Na2HPO4 solution of solution and 0.1mol/L are 1 by volume：4 are obtained by mixing) in handle 1h, after taking-up wash with distilled water,
Vacuum drying oven is placed in dry for 24 hours under conditions of 40 DEG C.Then, using scanning electron microscope sem, (NoVaNaVo SEM430, FEI are public
Department) microscopic appearance of the observation sample before and after impregnating PBS buffer solutions.
Claims (3)
1. a kind of preparation method of the polyvinyl alcohol containing nano silver/chitosan nano fiber membrane dressing, which is characterized in that with poly- second
Enol, chitosan, nano silver are raw material, prepare nano fibrous membrane by method of electrostatic spinning, then make nanofiber with glutaraldehyde
Film is crosslinked and is made；Include the following steps：
(1) poly-vinyl alcohol solution is prepared
Polyvinyl alcohol is dissolved in the in the mixed solvent of water and ethyl alcohol, magnetic agitation obtains a concentration of 8~20% to being completely dissolved
The mass ratio of the in the mixed solvent of poly-vinyl alcohol solution, wherein water and ethyl alcohol, water and ethyl alcohol is 8:15；
(2) chitosan solution is prepared
Chitosan is dissolved in the acetum of mass concentration 1%, magnetic agitation obtains a concentration of 3~10% to being completely dissolved
Chitosan solution；
(3) nano silver colloidal sol is prepared
It will be dissolved in the N as solvent and reducing agent, N- dimethyl formyls as the polyvinylpyrrolidone of the stabilizer of nano silver
In amine, it is made into reducing solution；By AgNO3Solution is added dropwise in reducing solution while stirring, is added dropwise, and continues to stir 6h, system
At nano silver colloidal sol；
(4) polyvinyl alcohol/chitosan/nano silver spinning solution is prepared
Take poly-vinyl alcohol solution and chitosan solution, in mass ratio 100：4 are mixed, and are added dropwise and are received after magnetic agitation is uniform
The mass ratio of rice silver sol, poly-vinyl alcohol solution and nano silver colloidal sol is 100：6, it is added dropwise, continues to stir 2h, be made into spinning
Liquid；
(5) electrostatic spinning
Polyvinyl alcohol/the chitosan prepared in step (4)/nano silver spinning solution is subjected to electrostatic spinning and obtains nano fibrous membrane,
It is received using aluminium foil；
(6) glutaraldehyde cross-linking
The nano fibrous membrane prepared in step (5) is placed in glutaraldehyde steam and is sealed crosslinking.
2. preparation method according to claim 1, it is characterised in that：The electrostatic spinning process parameter, voltage 10kV,
Syringe pump fltting speed is 20uL/min, and it is 12cm to receive distance, and temperature is room temperature.
3. preparation method according to claim 1, it is characterised in that：The glutaraldehyde cross-linking time is 1~3h.
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