CN101096424A - Glutin nano fabric film containing nano silver and preparation and application thereof - Google Patents
Glutin nano fabric film containing nano silver and preparation and application thereof Download PDFInfo
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- CN101096424A CN101096424A CNA2007100428245A CN200710042824A CN101096424A CN 101096424 A CN101096424 A CN 101096424A CN A2007100428245 A CNA2007100428245 A CN A2007100428245A CN 200710042824 A CN200710042824 A CN 200710042824A CN 101096424 A CN101096424 A CN 101096424A
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Abstract
The invention relates to a nanometer silver gelatine nanometer fiber film, which comprises the following parts: a gelatine nanometer fiber and a nanometer silver distributed in gelatine nanometer fiber homogeneously, wherein the nanometer silver particle attaches the surface of the gelatine nanometer fiber or in the fiber, the mean diameter of the gelatine nanometer fiber is 60-220nm, and the mean diameter of the nanometer silver is 4-50nm. The electrostatic spinning method comprises the following steps: making the spinning liquid by adding silver nitrate in gelatin-formic acid solution; getting the nanometer fiber film with silver ion by electrostatic spinning; deacidizing the silver ion in the fiber into the nanometer silver particle with ultraviolet irradiation method. The nanometer silver gelatine nanometer fiber film is used to make the artificial skin, the medical dressing, the hemostatic material and the sanitary cotton.
Description
Technical field
The present invention relates to nano fibrous membrane, be specifically related to a kind of gelatine nano fiber film that contains nanometer silver and its production and application.
Background technology
The manufacturing of nanofiber at present one of is the focus of world attention.Nanofiber has less diameter and bigger specific surface area, therefore makes nanofiber have purposes widely.The non-woven fabrics that utilizes nanofiber to make has the feature of highly air-permeable, adds nanofiber and has big surface-area, is commonly used to make medical dressing and restores to promote wound.Nano fibrous membrane has high porosity, helps the evaporation of wound fluid, avoids the surface of a wound long-pending; And oxygen sees through easily, helps the growth and the regeneration of wound tissue cellular respiration, epithelium, accelerates the healing of wound.In addition, nanofiber also can be used to make high efficiency filtering material, protective clothing etc.
Silver has the effect of broad-spectrum antimicrobial, is a kind of natural antibacterial material, uses also relatively safety, therefore has use range widely.At present make or form the nanometer-level silver fine particle in the mode of nanotechnology, can make the activity of silver become big, antibacterial effect strengthens.With nanometer silver attached to becoming antibacterial fiber and antibiotic facing material on the fiber.Nanometer silver is compound to makes antiseptic dressing in the medical dressing, have many effects such as sterilization, anti-inflammatory, promotion wound healing.On nanofiber, adhere to nanometer silver, usually adopt the mode of dipping and coating, nanometer silver is attached on the nanofiber and forms nano silver fibre.These methods with dipping or coating are difficult to obtain the little silver-colored particle to several nanometers of diameter, and the distribution of silver-colored particle on fiber surface be difficult to reach very even, and the usage quantity of nanometer silver is increased.Adopt the method for electrostatic spinning can in nanofiber, mix nanometer silver, strengthen antibacterial effect.
Relate to the fibrous reticulum that contains nanometer silver with the method for electrostatic spinning preparation in patent CN1851087A, its method is that the nano-Ag particles uniform mixing is formed spinning solution in polypropylene solution, carries out electrostatic spinning again nano-Ag particles is mixed in the fiber.The shortcoming that contains two aspects of nano silver fibre existence that this method makes: the one, the diameter of nano-Ag particles is bigger, is 100~500 nanometers; The 2nd, nano silver powder is reunited in the mixing process of polymers soln easily, is difficult to be uniformly dispersed.
The present invention is the presoma with nanometer silver---Silver Nitrate joins and makes uniform spinning solution in the gelatin solution, by electrostatic spinning silver ions is sneaked in the fiber, and the method by photoreduction becomes nano-Ag particles with the silver ion reduction in the fiber then.The nano-Ag particles diameter can be very little like this, is low to moderate several nanometers, and nano-Ag particles can be evenly distributed in the tunica fibrosa, can utilize the antibacterial effect of nanometer silver to make products such as artificial skin, medical dressing, hemostatic material, cotton wool.
Summary of the invention
One of the technical problem to be solved in the present invention is that to overcome in the prior art nano particle bigger, nano silver powder is difficult to finely dispersed defective, provide a kind of nano-Ag particles diameter very little, nano-Ag particles can be evenly distributed in the gelatine nano fiber film that contains nanometer silver in the tunica fibrosa.The gelatine nano fiber film that contains nanometer silver provided by the invention comprises gelatine nano fiber and is evenly distributed in the nanometer silver of gelatine nano fiber, utilize this natural macromolecular material of gelatin, method by electrostatic spinning embeds nanometer silver or makes nanometer silver attached on the fiber surface in nanofiber, the gelatine nano fiber diameter is 60~200 nanometers, nano-Ag particles mean diameter 4~50nm.
Another technical problem to be solved by this invention has provided a kind of preparation method who contains the gelatine nano fiber film of nanometer silver, and this preparation method adopts electrospinning process, comprises the following steps:
(1) preparation gelatin solution: gelatin is dissolved in the formic acid, and magnetic agitation is transparent, glassy yellow liquid, i.e. gelatin-formic acid solution to dissolving fully;
(2) preparation gelatin-silver nitrate solution: in the gelatin-formic acid solution of (1) preparation, add the Silver Nitrate powder, continue to stir 1 hour, dissolve fully to Silver Nitrate;
(3) carry out electrostatic spinning in the gelatin-silver nitrate solution immigration plastics needle tubing with preparation in (2), the electrostatic spinning process condition is: static voltage is 14~32 kilovolts, and accepting distance is 6~24 centimetres, and spinning speed is 0.4 milliliter/hour, 0.7 millimeter of orifice internal diameter, spinning is at room temperature carried out;
(4) nano fibrous membrane that electrostatic spinning is made carries out photoreduction with UV-irradiation, makes the silver ions in the fiber become nano-Ag particles, and wherein the nano-Ag particles major part is distributed in the surface of fiber;
Formic acid mass concentration in the step (1) is 70%~90%; Gained gelatin-formic acid solution concentration is 14%~22% (grams per milliliter);
In the step (2) to add the Silver Nitrate powder concn be 0.3%~6%.
The nano silver fibre film of electrospinning process preparation of the present invention can make nanometer silver and nanofiber once-forming, allow nano-Ag particles attached to the nanofiber of gelatin surface or embed in the fiber and form the nano silver fibre film, can reduce coming off and agglomeration of nanometer silver effectively, avoided direct adding nano silver powder, and can reduce the silver-colored addition of making nano silver fibre, the nanometer silver of formation is distributed in tunica fibrosa more equably.
Utilize the antibacterial effect of nanometer silver, the gelatine nano fiber film that contains nanometer silver of the present invention can be applicable to make products such as artificial skin, medical dressing, hemostatic material, cotton wool.
Description of drawings
The sem photograph of Fig. 1 embodiment 1 prepared micro/nano fibrous membrane material;
The sem photograph of Fig. 2 embodiment 2 prepared micro/nano fibrous membrane materials;
The transmission electron microscope picture of Fig. 3 embodiment 1 prepared micro/nano fibrous membrane material;
The transmission electron microscope picture of Fig. 4 embodiment 2 prepared micro/nano fibrous membrane materials.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
Accurately taking by weighing 1.5 gram medical grade gelatin is dissolved in 10 milliliters of formic acid strong solutions, formic acid concn is 88%, sealing back normal temperature lower magnetic force stirs, treat that gelatin dissolves the Silver Nitrate powder that the back adds 0.0075 gram fully, continue magnetic agitation at normal temperatures after the sealing, treat that Silver Nitrate dissolves the back fully and forms the glassy yellow transparent liquid, leave standstill after 15 minutes spinning solution is transferred in the plastic injector, voltage is 22kV, the syringe pump fltting speed is 0.4ml/h, the employing aluminium foil receives, and receiving range is 14cm, and orifice diameter is 0.7mm, on aluminium foil, obtain static and spin gelatin/silver-colored nano fibrous membrane, 40 ℃ of following vacuum-drying 24h place irradiation 3h under the ultraviolet lamp, obtain containing the gelatine nano fiber film of nanometer silver.The average fibre diameter that obtains is 105nm, and silver-colored particulate mean diameter is 11nm.
Embodiment 2
Accurately taking by weighing 1.5 gram medical grade gelatin is dissolved in 10 milliliters of formic acid strong solutions, formic acid concn is 88%, sealing back normal temperature lower magnetic force stirs, treat that gelatin dissolves the Silver Nitrate powder that the back adds 0.0150 gram fully, continue magnetic agitation at normal temperatures after the sealing, treat that Silver Nitrate dissolves the back fully and forms the glassy yellow transparent liquid, leave standstill after 15 minutes spinning solution is transferred in the plastic injector, voltage is 22kV, the syringe pump fltting speed is 0.4ml/h, the employing aluminium foil receives, and receiving range is 14cm, and orifice diameter is 0.7mm, on aluminium foil, obtain static and spin gelatin/silver-colored nano fibrous membrane, 40 ℃ of following vacuum-drying 24h place irradiation 3h under the ultraviolet lamp, obtain containing the gelatine nano fiber film of nanometer silver.The average fibre diameter that obtains is 126nm, and silver-colored particulate mean diameter is 13nm.
Embodiment 3
Accurately taking by weighing 1.5 gram medical grade gelatin is dissolved in 10 milliliters of formic acid strong solutions, formic acid concn is 88%, sealing back normal temperature lower magnetic force stirs, treat that gelatin dissolves the Silver Nitrate powder that the back adds 0.0300 gram fully, continue magnetic agitation at normal temperatures after the sealing, treat that Silver Nitrate dissolves the back fully and forms the glassy yellow transparent liquid, leave standstill after 15 minutes spinning solution is transferred in the plastic injector, voltage is 22kV, the syringe pump fltting speed is 0.4ml/h, the employing aluminium foil receives, and receiving range is 14cm, and orifice diameter is 0.7mm, on aluminium foil, obtain static and spin gelatin/silver-colored nano fibrous membrane, 40 ℃ of following vacuum-drying 24h place irradiation 3h under the ultraviolet lamp, obtain containing the gelatine nano fiber film of nanometer silver.The average fibre diameter that obtains is 165nm, and silver-colored particulate mean diameter is 17nm.
Embodiment 4
Accurately taking by weighing 1.5 gram medical grade gelatin is dissolved in 10 milliliters of formic acid strong solutions, formic acid concn is 88%, sealing back normal temperature lower magnetic force stirs, treat that gelatin dissolves the Silver Nitrate powder that the back adds 0.0450 gram fully, continue magnetic agitation at normal temperatures after the sealing, treat that Silver Nitrate dissolves the back fully and forms the glassy yellow transparent liquid, leave standstill after 15 minutes spinning solution is transferred in the plastic injector, voltage is 22kV, the syringe pump fltting speed is 0.4ml/h, the employing aluminium foil receives, and receiving range is 14cm, and orifice diameter is 0.7mm, on aluminium foil, obtain static and spin gelatin/silver-colored nano fibrous membrane, 40 ℃ of following vacuum-drying 24h place irradiation 3h under the ultraviolet lamp, obtain containing the gelatine nano fiber film of nanometer silver.The average fibre diameter that obtains is 189nm, and silver-colored particulate mean diameter is 23nm.
Claims (9)
1. gelatine nano fiber film that contains nanometer silver, comprise gelatine nano fiber and the nanometer silver that is evenly distributed in gelatine nano fiber, in the nanofiber surface or embedding fiber of nano-Ag particles attached to gelatin, the gelatine nano fiber mean diameter is 60~200nm, and the nano-Ag particles mean diameter is 4~50nm.
2. a kind of gelatine nano fiber film that contains nanometer silver as claimed in claim 1 is characterized in that: the gelatine nano fiber mean diameter is 105,126,165 or 189nm, and the nano-Ag particles mean diameter is 11,13,17 or 23nm.
3. a preparation method who contains the gelatine nano fiber film of nanometer silver is characterized in that adopting electrospinning process, comprises the following steps:
(1) preparation gelatin solution: gelatin is dissolved in the formic acid, and magnetic agitation is transparent, glassy yellow liquid, i.e. gelatin-formic acid solution to dissolving fully;
(2) preparation gelatin-silver nitrate solution: in the gelatin-formic acid solution of (1) preparation, add the Silver Nitrate powder, continue to stir 1 hour, dissolve fully to Silver Nitrate;
(3) carry out electrostatic spinning in the gelatin-silver nitrate solution immigration plastics needle tubing with preparation in (2);
(4) nano fibrous membrane that electrostatic spinning is made carries out photoreduction with UV-irradiation, makes the silver ions in the fiber become nano-Ag particles.
4. a kind of preparation method who contains the gelatine nano fiber film of nanometer silver as claimed in claim 3, it is characterized in that: the formic acid mass concentration in the step (1) is 70%~90%.
5. a kind of preparation method who contains the gelatine nano fiber film of nanometer silver as claimed in claim 7, it is characterized in that: the formic acid mass concentration is 88%.
6. a kind of preparation method who contains the gelatine nano fiber film of nanometer silver as claimed in claim 6 is characterized in that: the gained gelatin-formic acid solution concentration is 14%~22% (grams per milliliter) in the step (1).
7. a kind of preparation method who contains the gelatine nano fiber film of nanometer silver as claimed in claim 6 is characterized in that: in the step (2) to add the Silver Nitrate powder concn be 0.3%~6%.
8. a kind of preparation method who contains the gelatine nano fiber film of nanometer silver as claimed in claim 6, it is characterized in that: the electrostatic spinning process condition is in the step (3): static voltage is 14~32 kilovolts, accepting distance is 6~24 centimetres, spinning speed is 0.4 milliliter/hour, 0.7 millimeter of orifice internal diameter, spinning is at room temperature carried out.
9. a gelatine nano fiber film that contains nanometer silver is applied to make artificial skin, medical dressing, hemostatic material, cotton wool.
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CNA2007100428245A CN101096424A (en) | 2007-06-27 | 2007-06-27 | Glutin nano fabric film containing nano silver and preparation and application thereof |
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