CN106757785A - Silver-loaded chitosan/polyvinyl alcohol micron belt and preparation method and application thereof - Google Patents
Silver-loaded chitosan/polyvinyl alcohol micron belt and preparation method and application thereof Download PDFInfo
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- CN106757785A CN106757785A CN201611078308.3A CN201611078308A CN106757785A CN 106757785 A CN106757785 A CN 106757785A CN 201611078308 A CN201611078308 A CN 201611078308A CN 106757785 A CN106757785 A CN 106757785A
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- silver
- polyvinyl alcohol
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- chitosan
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Artificial Filaments (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Materials For Medical Uses (AREA)
Abstract
The invention relates to a silver-loaded chitosan/polyvinyl alcohol micro-belt and a preparation method and application thereof, wherein the micro-belt is a chitosan/polyvinyl alcohol belt-shaped composite fiber film with silver nano-particles uniformly distributed, the diameter of the micro-belt is 0.3-2 mu m, and the particle size of the silver nano-particles is 5-60 nm. Mixing the polyvinyl alcohol solution and the lactic acid solution of the chitosan, adding ethanol, uniformly stirring, adding silver nitrate, stirring for 40-50h in a dark place to prepare a spinning solution, and then carrying out electrostatic spinning to obtain the silver-loaded chitosan/polyvinyl alcohol micro-belt. The micro-belt of the invention has the advantages of one-dimensional and two-dimensional nano materials, has higher specific surface area, porosity and water absorption, and effectively reduces the phenomena of shedding, agglomeration and the like of nano silver by attaching or embedding nano silver particles in the micro-belt, so that the formed nano silver is more uniformly distributed in the micro-belt, and the lethality of the micro-belt to escherichia coli is 100%.
Description
Technical field
The present invention relates to composite nano-fiber material field, more particularly to a kind of load silver shitosan with anti-microbial property/
Polyvinyl alcohol micron band and preparation method and application.
Background technology
Noble silver is used as high-efficiency antimicrobial material because of its unique photoelectric characteristic, high chemical stability and catalysis activity
Material.Nano material has big specific surface area and catalysis activity high, has preferably catalysis and sterilization compared to its block materials
Etc. performance.In recent years, people prepare the Argent grain of nanoscale by various means, and this Nano Silver has more excellent antibacterial
Performance.But, it is small-sized due to Nano Silver, during exclusive use, it is easy to be lost in, therefore, typically will in practical application
It is carried on carrier material, to play its excellent sterilizing ability.By in nano-silver loaded to nanofiber, you can to utilize
The great specific surface area increase Nano Silver of nanofiber and the contact area of bacterium, can effectively prevent silver during use again
Loss, it is more more efficient than many conventional methods.
One-dimensional chitosan-based material has the design feature that specific surface area is big, porosity is high and the good life of chitosan material
Thing medical performance, is a kind of green fiber with good environmental-protecting performance.Due to shitosan, viscosity is higher in an acidic solution, band
Positive charge, and intramolecular and the effect of intermolecular strong chemical bond, cause it to be difficult to move freely during electrostatic spinning, cause
Fiber is discontinuous, containing pearl, or even spinning fracture.And electrostatic blended spinning technology can be obtained high-specific surface area, continuous flawless
Nanofiber, more tough and tensile more durable than tunica fibrosa prepared by chitosan alone, cost of material is also lower.Polyvinyl alcohol 1788
(PVA) grease resistance and solvent resistance with good chemical stability and physical and mechanical properties and brilliance.Further, since
PVA has good biocompatibility and degradability, frequently as biomimetic material extensive use.High-molecular polyvinyl alcohol passes through
Hydrogen bond action is combined with shitosan, has better electrostatic spinning performance than other polymer.
Chinese patent document CN104511045A (application numbers：201310441908.1) disclose a kind of containing Nano Silver
The preparation method of chitosan/polyvinyl alcohol nanofiber film dressing, the nanofiber film dressing is mixed with polyvinyl alcohol and shitosan
Compound is base material, by the way that silver sol is added dropwise, chitosan/polyvinyl alcohol nano fibrous membrane, Ran Houli is obtained using method of electrostatic spinning
It is crosslinked with glutaraldehyde and nano fibrous membrane and obtains water-resistance anti-bacterial fibre.
Chinese patent document CN103705969A (application numbers：201410001923.9) a kind of shitosan base load silver is disclosed
The preparation method of composite antibacterial type superfine fibre film, specific steps include：The first step：It is the acetic acid of 50-90% in mass fraction
Silver nitrate powder is added in the aqueous solution, stirring dissolves it, weigh shitosan and polyethylene glycol oxide or pva powder is added
To in above-mentioned solution, stirring obtains spinning solution；Second step：Spinning solution is added into electrostatic spinning apparatus, voltage be 10-20kV,
Spinning solution injects speed 0.1-1.0mL/h, receives distance for 8-30cm, spinning temperature are that 20-50 DEG C and relative humidity are 10-
Electrostatic spinning is carried out under conditions of 55%, the white nano fibrous membrane vacuum drying 12-36h that will be obtained removes the solvent of residual,
Obtain chitosan-based silver-loaded composite antimicrobial superfine fiber membrane.
But, tunica fibrosa specific surface area, porosity, pick up, the absorption of Nano Silver that above-mentioned two patent documents are obtained
Ability and bacteriostasis property all have much room for improvement.
Monodimension nanometer material is widely paid close attention to due to its excellent physical and chemical performance, two-dimension nano materials due to
Stratiform and the characteristic such as controllable and furtherd investigate.The characteristics of micron carrying material has had a peacekeeping two-dimension nano materials concurrently, is current
Forward position material in Nanometer scale science and technology research and development, is relatively new knot between a peacekeeping two-dimensional nanostructure
Structure, with rectangular section, flakiness ratio has the property of uniqueness than larger；This very thin strip nanostructured, neither
It is same as the hollow structure of nanotube, and the different solid cylinder structures with nano wire.Micro belt Material Manufacturing Process is easily controlled,
When production in enormous quantities material structure can unify, internal structure is perfect, surface is clean smooth and no internal flaw, dislocation,
Purity is higher, and these properties enable it to put into industrial production earlier.
At present, the silver-colored chitosan/polyvinyl alcohol micro belt of load is directly prepared using electrostatic spinning technique, relevant report is had no.
The content of the invention
In view of the shortcomings of the prior art, silver-colored chitosan/polyvinyl alcohol micro belt and its preparation are carried the invention provides one kind
Silver nitrate is added mixed liquor, polyvinyl alcohol by method with application, the micro belt with polyvinyl alcohol and chitosan compound as base material
Used as reducing agent, shitosan prepares the chitosan/polyvinyl alcohol micro belt containing Nano Silver as stabilizer.
Technical scheme is as follows：
One kind carries silver-colored chitosan/polyvinyl alcohol micro belt, the micro belt be evenly distributed with the shitosan of silver nano-grain/
Polyvinyl alcohol banding composite cellulosic membrane, a diameter of 0.3-2 μm of micro belt, the particle diameter of silver nano-grain is 5-60nm.
, according to the invention it is preferred to, described micron tape thickness is 100-300nm.
, according to the invention it is preferred to, 0.5-1.5 μm of the micro belt diameter, silver nano-grain particle diameter is 5-40nm.
According to the present invention, the preparation method of above-mentioned load silver chitosan/polyvinyl alcohol micro belt, including step is as follows：
Ethanol is added after the lactic acid solution of poly-vinyl alcohol solution and shitosan is mixed, silver nitrate is stirring evenly and then adding into,
Lucifuge stirs 40-50h, is made into spinning solution, and then electrostatic spinning obtains carrying silver-colored chitosan/polyvinyl alcohol micro belt.
Preparation in accordance with the present invention, it is preferred that the mass concentration of described poly-vinyl alcohol solution is 10-20%, institute
The lactic acid solution mass concentration of the shitosan stated is 2-8%；
Preferably, the mass ratio of poly-vinyl alcohol solution, the lactic acid solution of shitosan and ethanol is (90-70)：(10-30)：
(5-10)。
Preparation in accordance with the present invention, it is preferred that the addition of silver nitrate is the 2 of polyvinyl alcohol and shitosan gross mass
~8%.
Preparation in accordance with the present invention, it is preferred that the condition of electrostatic spinning is：
Received using aluminium foil, voltage is 15-20kV, syringe pump fltting speed is 1.5-3mL/h, it is 12- to receive distance
18cm, temperature is 20-25 DEG C.
According to the present invention, application of the above-mentioned load silver chitosan/polyvinyl alcohol micro belt in medical dressing is prepared.
The present invention, using shitosan as stabilizer, silver nitrate is added by the use of polyvinyl alcohol as the reducing agent of silver ion
To in chitosan/polyvinyl alcohol mixed liquor, silver ion is set to be reduced into Nano Silver, prepared by the method for this " from bottom to top " receives
Rice Argent grain diameter is smaller, it is to avoid be directly added into skewness after nano-silver powder, the problems such as particle diameter is uneven.Using electrostatic spinning
Method can make Nano Silver once-forming with micro belt, allow nano-Ag particles to adhere to or be embedded in chitosan/polyvinyl alcohol micro belt
In, coming off and the phenomenon such as reunite for Nano Silver is effectively reduced, make the Nano Silver to be formed distribution in micro belt evenly.
Using the broad spectrum antibacterial of Nano Silver, micro belt prepared by the present invention can be used as medical dressing.Polyvinyl alcohol is water-soluble high score
Son, containing substantial amounts of hydroxyl, can form substantial amounts of hydrogen bond with hydrone, therefore, compound micro belt prepared by the present invention can absorb
Moisture, is environment that wound can provide wetting.
Beneficial effects of the present invention：
1st, the advantage for carrying silver-colored chitosan/polyvinyl alcohol micro belt with a peacekeeping two-dimension nano materials of the invention, both
Solid nanofiber is different from again different from nanotube, and compared to existing nanofiber, micro belt possesses ratio table higher
Area, porosity and water absorption rate, nano-Ag particles adhere to or are embedded in chitosan/polyvinyl alcohol micro belt, due to bandwidth
Than relatively thin, it is to avoid excessive Nano Silver is embedded in inside, coming off and the phenomenon such as reunite for Nano Silver is effectively reduced, makes shape
Into distribution of the Nano Silver in micro belt evenly.
It is 2nd, of the invention that to carry silver-colored chitosan/polyvinyl alcohol micro belt preparation technology simpler, by the use of polyvinyl alcohol as
Reducing agent, used as stabilizer, in-situ reducing is into Nano Silver for shitosan.And selected base material is all degradability and biocompatibility
Green material, improve the pattern of film, the chitosan/polyvinyl alcohol micro belt of argentiferous is prepared, with broad spectrum antibacterial
Feature, the fatal rate to Escherichia coli is 100%.
Brief description of the drawings
Fig. 1 is the ultra-violet absorption spectrum of lucifuge stirring different time in silver nitrate addition polyvinyl alcohol in embodiment 1.
Fig. 2 is the XRD spectra of the silver-colored chitosan/polyvinyl alcohol micro belt of the load obtained in embodiment 2.In figure a be shitosan/
The XRD curves of polyvinyl alcohol；B is the XRD curves for carrying silver-colored chitosan/polyvinyl alcohol.
Fig. 3 is the scanning electron microscopic picture of the silver-colored chitosan/polyvinyl alcohol micro belt of the load obtained in embodiment 2.
Fig. 4 is the load silver chitosan/polyvinyl alcohol micro belt transmission electron microscope picture obtained in embodiment 2.A is low power in figure
Transmission photo；B is that high power transmits photo.
Fig. 5 is the fungistatic effect figure of the silver-colored chitosan/polyvinyl alcohol micro belt of the load obtained in embodiment 2.A is antibacterial in figure
Before；After b is antibacterial.
Specific embodiment
Below by specific embodiment and with reference to accompanying drawing, the invention will be further described, but not limited to this.
Shitosan used is white or off-white powder, deacetylation in embodiment>95%, rank medical grade.It is used
Polyvinyl alcohol be white particle, model 1788, molecular weight 44.05MW.
Embodiment 1
Weigh 10g polyvinyl alcohol to be dissolved in 90g water, magnetic agitation heating for dissolving, it is 10% to be made into 100g mass fractions
Poly-vinyl alcohol solution.Weigh 0.2g shitosans to be dissolved in lactic acid, be made into the shitosan lactic acid solution that 10g mass fractions are 2%.Will
Above-mentioned polyvinyl alcohol and chitosan solution are with 70:After 30 mass ratio mixing, polyvinyl alcohol and shitosan gross mass 2% are added
Silver nitrate, lucifuge stirring 48h after be made into spinning solution.Spinning is carried out using electrostatic spinning apparatus, voltage is 20kV, and syringe pump is pushed away
Enter speed for 2.26mL/h, received using aluminium foil, it is 15cm to receive distance.It is obtained and carries silver-colored chitosan/polyvinyl alcohol micro belt.
, with the increase of mixing time, UV absorption intensity is as shown in figure 1, with mixing time for obtained spinning solution
Increase, UV absorption intensity gradually strengthens, it was demonstrated that the reproducibility to silver ion of polyvinyl alcohol.
Embodiment 2
The mass concentration of poly-vinyl alcohol solution is expanded as 20%, other reagents and consumption and process conditions are constant, repeated
Embodiment 1, that is, obtain carrying silver-colored chitosan/polyvinyl alcohol micro belt.The XRD of obtained micro belt is as shown in Fig. 2 20 ° or so
It is the unbodied peak of shitosan, the peak of indexing is the peak of elemental silver, illustrates that the silver in micro belt is elemental silver.Substrate carrier silver
Respectively as shown in Figure 3,4, obtained composite membrane is ribbon-like fibre, a diameter of 0.6-1 μm, is carried for front and rear scanning and transmission photo
Ribbon-like fibre surface has uniformly been covered with silver nano-grain, particle diameter 5-60nm after silver.
Embodiment 3
The mass concentration of chitosan solution is expanded as 8%, other reagents and consumption and process conditions are constant, repeat to implement
Example 1, that is, obtain carrying silver-colored chitosan/polyvinyl alcohol micro belt.
Test example
The sample of embodiment 2 is tested into its bactericidal property using following methods：
The bactericidal property test of silver-colored chitosan/polyvinyl alcohol micro belt is carried according to the examination of Appendix B in GB/T21510-2008
Proved recipe method, test strain is most representational Escherichia coli in gramnegative bacterium.Experiment uses shake-flask method, cut-parts
It is affixed in conical flasks of the 250mL equipped with bacteria suspension, under the conditions of 25 DEG C, after 150r/min vibrations 2min, according to remaining in flask
Strain, test its bactericidal property.
Resulting bactericidal effect is survived after sterilization as shown in figure 5, there is 504 E. coli clones before sterilized in flask
Bacterium colony be 0, it is known that the sterilizing rate for carrying silver-colored chitosan/polyvinyl alcohol micro belt is 100%.
Claims (10)
1. it is a kind of to carry silver-colored chitosan/polyvinyl alcohol micro belt, it is characterised in that the micro belt is to be evenly distributed with silver nano-grain
Chitosan/polyvinyl alcohol banding composite cellulosic membrane, a diameter of 0.3-2 μm of micro belt, the particle diameter of silver nano-grain is 5-60nm.
2. it is according to claim 1 to carry silver-colored chitosan/polyvinyl alcohol micro belt, it is characterised in that described micron tape thickness
It is 100-300nm to spend.
3. it is according to claim 1 to carry silver-colored chitosan/polyvinyl alcohol micro belt, it is characterised in that the micro belt diameter
0.5-1.5μm。
4. it is according to claim 1 to carry silver-colored chitosan/polyvinyl alcohol micro belt, it is characterised in that the silver nano-grain
Particle diameter is 5-60nm.
5. the preparation method of the silver-colored chitosan/polyvinyl alcohol micro belt of load described in any one of claim 1-4, including step is such as
Under：
Ethanol is added after the lactic acid solution of poly-vinyl alcohol solution and shitosan is mixed, silver nitrate, lucifuge is stirring evenly and then adding into
Stirring 40-50h, is made into spinning solution, and then electrostatic spinning obtains carrying silver-colored chitosan/polyvinyl alcohol micro belt.
6. preparation method according to claim 5, it is characterised in that the mass concentration of described poly-vinyl alcohol solution is
10-20%, the lactic acid solution mass concentration of described shitosan is 2-8%.
7. preparation method according to claim 5, it is characterised in that poly-vinyl alcohol solution, the lactic acid solution of shitosan and
The mass ratio of ethanol is (90-70)：(10-30)：(5-10).
8. preparation method according to claim 5, it is characterised in that the addition of silver nitrate is polyvinyl alcohol and shitosan
The 2~8% of gross mass.
9. preparation method according to claim 5, it is characterised in that the condition of electrostatic spinning is：
Received using aluminium foil, voltage is 15-20kV, syringe pump fltting speed is 1.5-3mL/h, it is 12-18cm, temperature to receive distance
Spend is 20-25 DEG C.
10. load silver-colored chitosan/polyvinyl alcohol micro belt the answering in medical dressing is prepared described in any one of claim 1-4
With.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107691969A (en) * | 2017-09-21 | 2018-02-16 | 华南协同创新研究院 | A kind of low molecular chitosan@silver nano-grains composite membrane and preparation method and application |
| CN108633879A (en) * | 2018-04-20 | 2018-10-12 | 袁杰 | A kind of circulating water sterilizing agent |
| CN109169706A (en) * | 2018-07-19 | 2019-01-11 | 大美泰康（天津）生态科技有限公司 | Complex antimicrobials and antibacterial bacteriostatic type multifunctional inorganic ecologic coating obtained |
| CN112962216A (en) * | 2021-02-07 | 2021-06-15 | 宁波工程学院 | Preparation method of nylon 6/chitosan/precious metal nano-fiber |
| CN116617439A (en) * | 2023-06-05 | 2023-08-22 | 江苏益通生物科技有限公司 | Chitosan composite hemostatic dressing and manufacturing method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107691969A (en) * | 2017-09-21 | 2018-02-16 | 华南协同创新研究院 | A kind of low molecular chitosan@silver nano-grains composite membrane and preparation method and application |
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| CN109169706A (en) * | 2018-07-19 | 2019-01-11 | 大美泰康（天津）生态科技有限公司 | Complex antimicrobials and antibacterial bacteriostatic type multifunctional inorganic ecologic coating obtained |
| CN112962216A (en) * | 2021-02-07 | 2021-06-15 | 宁波工程学院 | Preparation method of nylon 6/chitosan/precious metal nano-fiber |
| CN112962216B (en) * | 2021-02-07 | 2022-02-01 | 宁波工程学院 | Preparation method of nylon 6/chitosan/precious metal nano-fiber |
| CN116617439A (en) * | 2023-06-05 | 2023-08-22 | 江苏益通生物科技有限公司 | Chitosan composite hemostatic dressing and manufacturing method thereof |
| CN116617439B (en) * | 2023-06-05 | 2023-10-20 | 江苏益通生物科技有限公司 | Chitosan composite hemostatic dressing and manufacturing method thereof |
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