CN101864670A - Method for preparing nano silver-containing anti-bacterial fabric by immersion process - Google Patents
Method for preparing nano silver-containing anti-bacterial fabric by immersion process Download PDFInfo
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Abstract
The invention relates to a method for preparing a nano silver-containing anti-bacterial fabric by an immersion process. The method comprises the following steps: dissolving dopamine hydrochloride in Tris buffer solution; adjusting the pH value of solution to be between 7 and 10 by using hydrochloric acid; immerging a fabric into prepared dopamine solution in a bath ratio of 1:30; after stirring for reacting at the temperature of between 20 and 40 DEG C for 20 to 30 hours, taking the fabric out and washing to obtain a poly dopamine film-coated fabric; putting the fabric into silver nitrate aqueous solution; and after immerging for 8 to 10 hours, washing and drying the fabric to obtain the nano silver-containing fabric. The nano silver-containing fabric prepared by the method has the characteristics of high soaping fastness resistance and lasting antibiotic property; a sterilizing rate is still up to 100 percent after the fabric is washed with water for 30 times; and the preparation method has the characteristics of simple process, no pollution to the environment, low cost and large-scale production.
Description
Technical field
The invention belongs to the arrangement preparation field of nanometer silver antimicrobial fabric, particularly a kind of method for preparing nano silver-containing anti-bacterial fabric with impregnation technology.
Background technology
Along with growth in the living standard, people require to improve gradually to the health taking of textiles, and the piece market with antibacterial functions is also enlarging gradually.At present, antiseptic can be divided into inorganic serial antiseptic and organic series antiseptic two big classes substantially.Organic antibacterial agent can not satisfy market demands because of himself characteristics poor chemical stability, poor heat resistance.In recent years, the inorganic nano material development is rapid, but the great majority report is to go up loaded with nano level silver, zinc, copper, rare earth element etc. at carrier material (as molecular sieve, imvite, calcium carbonate etc.), and its shortcoming is that carrier material does not have antibiotic property, antibiotic effective ingredient is few, and the antiseptic consumption is big etc.
Recently, scientist finds that mussel can freely be adsorbed on wet body surface.By to the discovering of its foot structure, the protein of mussel foot contains a large amount of dopamines in forming.Discover that dopamine can polymerization reaction take place under alkali condition, the poly-dopamine of formation has certain adhesiveness.Thereby make people expect utilizing functional polymer film that dopamine forms at big body surface platform, body surface is carried out further modification handle as secondary response.
Summary of the invention
Technical problem to be solved by this invention provides a kind of method for preparing nano silver-containing anti-bacterial fabric with impregnation technology, the carrying nano silver fabric of this method preparation has the antibiotic property of fastness to soaping and high-efficient and lasting preferably, after through 30 washings, silver content still remains on 15mg/g, and sterilizing rate still can reach 100%; And preparation technology is simple, and environment is not polluted, and cost is low, is fit to large-scale production.
Of the present inventionly a kind ofly prepare the method for nano silver-containing anti-bacterial fabric, comprising with impregnation technology:
(1) compound concentration is the Tris cushioning liquid of 20g/L, then Dopamine hydrochloride is dissolved in the Tris cushioning liquid, is mixed with the dopamine solution that concentration is 0.05-0.25mol/L, with hydrochloride adjusted solution pH value to the scope of 7-10;
(2) fabric that will clean impregnated in the dopamine solution of above-mentioned preparation with 1: 30 bath raio, and control reaction temperature is 20-40 ℃, takes out behind the stirring reaction 20-30h, cleans, and obtains applying the fabric of poly-dopamine film;
(3) fabric of the poly-dopamine film of the coating that above-mentioned reaction is made is put into the silver nitrate aqueous solution that concentration is 0.05-0.35mol/L; bath raio is 1: 60, takes out behind the dipping 8-10h, after water is rinsed well; vacuum drying under 40 ℃ of conditions obtains the carrying nano silver fabric.
Tris cushioning liquid in the described step (1) is the aqueous solution of trishydroxymethylaminomethane;
The concentration of the dopamine solution in the described step (1) is 0.1-0.2mol/L;
Dopamine solution pH value in the described step (1) is 8~9;
Fabric in the described step (2) is hydrophilic fabrics or water-repellent fabrics;
Preferred hydrophilic fabrics is cotton, hair, silk fabrics; Preferred water-repellent fabrics is terylene, acrylic fibers;
The concentration of the silver nitrate aqueous solution in the described step (3) is 0.1-0.3mol/L;
Described nano silver-containing anti-bacterial fabric, its silver content be distributed as 1-60mg/g, the particle mean size of silver particles is 10-150nm.
Because not only can forming poly-dopamine film on hydrophilic fabrics (as cotton, hair, silk fabrics) surface, Dopamine hydrochloride can also form poly-dopamine film on water-repellent fabrics (as terylene, acrylic fibers) surface.In course of reaction, poly-dopamine has not only played the effect of reductant, and the silver ion reduction in the solution is become nano silver particles, simultaneously nano silver particles is sticked to fabric face, need not to add extra adhesive or reductant.Poly-simultaneously dopamine is not only the physical adherence effect to the combination of Nano silver grain, also has the binding effect to nano silver particles of adjacent hydroxyl structure of catechol and amido, so antibiotic fabric has very high washing resistance.
Beneficial effect
The carrying nano silver fabric of the present invention preparation has the antibiotic property of fastness to soaping and high-efficient and lasting preferably, and after through 30 washings, sterilizing rate still can reach 100%; And preparation method's technology is simple, and environment is not polluted, and cost is low, is fit to large-scale production.
Description of drawings
Fig. 1 is the x-ray photoelectron energy spectrogram of the embodiment of the invention 1 Central Plains COTTON FABRIC, dopamine arrangement back COTTON FABRIC and carrying nano silver antibiotic fabric, wherein, and the COTTON FABRIC of the former COTTON FABRIC of A, B dopamine arrangement back COTTON FABRIC, C loaded with nano silver particles;
Fig. 2 is the scanning electron microscope diagram of the embodiment of the invention 1 Central Plains COTTON FABRIC, dopamine arrangement back COTTON FABRIC and carrying nano silver antibiotic fabric, wherein, and the COTTON FABRIC of the former COTTON FABRIC of A, B dopamine arrangement back COTTON FABRIC, C loaded with nano silver particles;
Fig. 3 is the washing resistance of carrying nano silver antibiotic fabric in the embodiment of the invention 1;
Fig. 4 is the antibiotic property of carrying nano silver antibiotic fabric in the embodiment of the invention 1, wherein, A handle through dopamine but not the COTTON FABRIC of the COTTON FABRIC of loaded with nano silver particles, B loaded with nano silver particles without washing handle, the COTTON FABRIC washing of C loaded with nano silver particles 30 times; (a) sample behind " 0 " sample contact time, (b) cultivation 24h.
The specific 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
Take by weighing the 3g trishydroxymethylaminomethane and be dissolved in preparation Tris cushioning liquid in the 150ml water, Dopamine hydrochloride is dissolved in the Tris cushioning liquid, the concentration of dopamine solution is 0.2mol/L, with hydrochloride adjusted solution pH value to 8.5, the COTTON FABRIC of getting then after 5g cleans is put into reactive bath technique, control reaction temperature is 30 ℃, taking out behind the reaction 24h under the condition of magnetic agitation, clean up with distilled water, put it into then in the liquor argenti nitratis ophthalmicus that concentration is 0.3mol/L; bath raio is 1: 60, take out behind the dipping 8h, with the clean back of distilled water flushing vacuum drying under 40 ℃ of conditions.Can obtain containing the COTTON FABRIC with antibacterial functions of nano silver particles.
Fig. 1 puts back COTTON FABRIC (B) in order for former COTTON FABRIC (A), the dopamine of present embodiment preparation and contains the x-ray photoelectron energy spectrogram of the COTTON FABRIC (C) of nano silver particles.Can judge dopamine surface of cotton fabric Already in by the appearance at N1s peak for dopamine arrangement back COTTON FABRIC.In addition, the position by Ag3d (368.4eV) peak in the x-ray photoelectron power spectrum can prove that the silver on the COTTON FABRIC is that form with silver particles is present in fabric face.
Fig. 2 is the scanning electron microscope diagram of the COTTON FABRIC (C) of former COTTON FABRIC (A), dopamine modified cotton fabric (B) and load Nano silver grain.Can prove under alkali condition by spectrogram in conjunction with the x-ray photoelectron of dopamine modified cotton fabric, dopaminergic spontaneous at the surface of cotton fabric polymerization reaction take place, and form the coarse poly-dopamine film of one deck at surface of cotton fabric.From Fig. 2 .B as can be seen on the COTTON FABRIC of dopamine arrangement back the silver particles of load belong to Nano grade, particle diameter is about 80nm and be evenly distributed.
After the fabric washability that Fig. 3 carries out according to the ISO105-C10 testing standard for the COTTON FABRIC of loaded with nano silver particles is tested, fabric sample is cleared up the fabric face silver content that records.Can prove and use the carrying nano silver fabric of this method preparation to have fabulous fastness to soaping, after through 30 washings, silver content still remains on about 15mg/g.
The antibiotic property test that Fig. 4 carries out according to AATCC (U.S. textile dyeing man and chemist association) 100-2004 testing standard for COTTON FABRIC.Can prove that from the contrast of figure A and B only the COTTON FABRIC of handling through dopamine does not possess antibiotic property substantially, and the fabric sterilizing rate of load Nano silver grain can reach 100%, so nano silver particles is the main cause of antibacterial fabric.Find out that from figure four C fabric can prove that still reaching 100% through 30 washing back sterilizing rates the carrying nano silver antibiotic fabric of this method preparation has the antibiotic property of high-efficient and lasting.
Embodiment 2
Prepare the carrying nano silver antibiotic fabric according to embodiment 1 described method, the concentration of dopamine solution is adjusted into 0.1mol/L, silver nitrate concentration is adjusted into 0.1mol/L, and other condition is constant.The content of nanometer silver of the surface of cotton fabric load with antibacterial functions that contains nano silver particles of preparation is 27mg/g, and after standing 30 washings, silver content still can reach 11mg/g, and sterilizing rate can reach 100%.
Embodiment 3
Prepare the carrying nano silver antibiotic fabric according to embodiment 1 described method, change the COTTON FABRIC of flooding into hydrophobic dacron, other condition is constant.The content of nanometer silver of the dacron area load with antibacterial functions that contains nano silver particles of preparation is 10mg/g, and after standing 30 washings, silver content still can reach 3mg/g, and sterilizing rate can reach 100%.
Embodiment 4
Prepare the carrying nano silver antibiotic fabric according to embodiment 1 described method, change the COTTON FABRIC of flooding into hydrophobic dacron, dopamine concentration is adjusted into 0.1mol/L, and other condition is constant.The content of nanometer silver of the dacron area load with antibacterial functions that contains nano silver particles of preparation is 9mg/g, and after standing 30 washings, silver content still can reach 2mg/g, and sterilizing rate can reach 100%.
Claims (8)
1. one kind prepares the method for nano silver-containing anti-bacterial fabric with impregnation technology, comprising:
(1) compound concentration is the Tris cushioning liquid of 20g/L, then Dopamine hydrochloride is dissolved in the Tris cushioning liquid, is mixed with the dopamine solution that concentration is 0.05-0.25mol/L, with hydrochloride adjusted solution pH value to the scope of 7-10;
(2) fabric that will clean impregnated in the dopamine solution of above-mentioned preparation with 1: 30 bath raio, and control reaction temperature is 20-40 ℃, takes out behind the stirring reaction 20-30h, cleans, and obtains applying the fabric of poly-dopamine film;
(3) fabric of the poly-dopamine film of the coating that above-mentioned reaction is made is put into the silver nitrate aqueous solution that concentration is 0.05-0.35mol/L; bath raio is 1: 60, takes out behind the dipping 8-10h, after water is rinsed well; vacuum drying under 40 ℃ of conditions obtains the carrying nano silver fabric.
2. according to claim 1ly a kind ofly prepare the method for nano silver-containing anti-bacterial fabric with impregnation technology, it is characterized in that: the Tris cushioning liquid in the described step (1) is the aqueous solution of trishydroxymethylaminomethane.
3. according to claim 1ly a kind ofly prepare the method for nano silver-containing anti-bacterial fabric with impregnation technology, it is characterized in that: the concentration of the dopamine solution in the described step (1) is 0.1-0.2mol/L.
4. according to claim 1ly a kind ofly prepare the method for nano silver-containing anti-bacterial fabric with impregnation technology, it is characterized in that: the dopamine solution pH value in the described step (1) is 8~9.
5. according to claim 1ly a kind ofly prepare the method for nano silver-containing anti-bacterial fabric with impregnation technology, it is characterized in that: the fabric in the described step (2) is hydrophilic fabrics or water-repellent fabrics.
6. according to claim 5ly a kind ofly prepare the method for nano silver-containing anti-bacterial fabric with impregnation technology, it is characterized in that: described hydrophilic fabrics is cotton, hair or silk fabrics; Water-repellent fabrics is terylene or acrylic fibers.
7. according to claim 1ly a kind ofly prepare the method for nano silver-containing anti-bacterial fabric with impregnation technology, it is characterized in that: the concentration of the silver nitrate aqueous solution in the described step (3) is 0.1-0.3mol/L.
8. according to claim 1ly a kind ofly prepare the method for nano silver-containing anti-bacterial fabric, it is characterized in that with impregnation technology: described nano silver-containing anti-bacterial fabric, its silver content be distributed as 1-60mg/g, the particle mean size of silver particles is 10-150nm.
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