CN102864443A - Coating method of matrix - Google Patents
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- CN102864443A CN102864443A CN2011101869538A CN201110186953A CN102864443A CN 102864443 A CN102864443 A CN 102864443A CN 2011101869538 A CN2011101869538 A CN 2011101869538A CN 201110186953 A CN201110186953 A CN 201110186953A CN 102864443 A CN102864443 A CN 102864443A
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Abstract
The invention provides a coating method of a matrix, comprising the following steps: contacting the matrix with a first solution, mixing the contacted matrix with a second solution, and drying the mixed matrix, wherein the first solution contains a first coupling agent and a first solvent, the second solution contains nano silver particles, a second coupling agent and a second solvent. The method disclosed herein carries out coating treatment on the matrix to let the coated matrix have high-efficiency lasting antibacterial function. The results of test cases of the invention show that the antibacterial function of a product which is processed by a 24-hour treatmentcan reach to more than 99.9998%. In addition, the method has the advantages of wide application, simple preparation method, no environmental pollution, and low cost, and is suitable for large-scale production.
Description
Technical field
The present invention relates to a kind of film coating method of matrix.
Background technology
Along with the day by day raising of standard of living, in recent years, the nano-antibacterial coating technique worldwide begins to be able to the marketization, and its applied research at medicine equipment and sanitation and health-care field has obtained significant progress.For example, " Acticoat ", a kind of wound dressings product based on the nanometer silver coating technique (Nucryst, Wakefield, MA, USA), the sales volume in 2004 has reached 25,000,000 dollars.With it simultaneously, the market capacity of antimicrobial product is huge, according to estimates, will reach 45,000,000,000 dollars to the sales volume of nano-antibacterial product in 2012.The nanometer silver antimicrobial technology has shown powerful growth vigor because it has environmental protection, efficiently reaches the characteristics such as low-cost in antimicrobial product market.
Current, the nanometer silver antimicrobial technology also is in starting and the stage of growth in China, and powerful vigor and the market space are arranged, but lacks relevant preparation and the production technology with independent intellectual property right.
The core of nanometer silver antimicrobial technology comprises nano-Ag particles material preparation and the application art in product.Current existing several different methods can prepare the nano-Ag particles material, but the application art technology of nano silver material in product lacks very much.Existing magnetron sputtering and nano material blending technology exist production prices costliness, complex process, unstable properties, antibiotic many drawbacks such as not lasting.
Summary of the invention
The objective of the invention is to overcome the defects of prior art, a kind of film coating method of matrix is provided.
The invention provides a kind of film coating method of matrix, it is characterized in that, the method comprises this matrix is contacted with the first solution, and the matrix after will contacting is mixed with the second solution, mixed matrix is carried out drying, wherein, described the first solution contains the first coupling agent and the first solvent, and described the second solution contains nano-Ag particles, the second coupling agent and the second solvent.
Method of the present invention is carried out coating film treatment to matrix, so that the matrix behind the plated film has efficient, lasting antibacterial, can find out from the test result according to test case of the present invention, through 24 hours processing, the anti-microbial property of the product after method of the present invention is processed can reach more than 99.9998%.
In addition, being widely used of this technology, preparation technology is simple, and environment is not polluted, and cost is low, is fit to scale operation.
Embodiment
The invention provides a kind of film coating method of matrix, it is characterized in that, the method comprises this matrix is contacted with the first solution, and the matrix after will contacting is mixed with the second solution, mixed matrix is carried out drying, wherein, described the first solution contains the first coupling agent and the first solvent, and described the second solution contains nano-Ag particles, the second coupling agent and the second solvent.
According to the present invention, preferably, take the total amount of the first solution as benchmark, the content of the first coupling agent is the 0.01-40 % by weight in described the first solution, and the content of the first solvent is the 60-99.99 % by weight.Further preferred, take the total amount of the first solution as benchmark, the content of the first coupling agent is the 0.1-20 % by weight in described the first solution, and the content of the first solvent is the 80-99.9 % by weight.Most preferably, take the total amount of the first solution as benchmark, the content of the first coupling agent is the 0.2-10 % by weight in described the first solution, and the content of the first solvent is the 90-99.8 % by weight.
According to the present invention, preferably, described the first solution is by the first coupling agent and the first solvent composition.
According to the present invention, preferably, take the total amount of the second solution as benchmark, the content of nano-Ag particles is the 0.01-30 % by weight in described the second solution, and the content of the second coupling agent is the 0.01-20 % by weight, and the content of the second solvent is the 50-99.9 % by weight.Further preferably, take the total amount of the second solution as benchmark, the content of nano-Ag particles is the 0.05-10 % by weight in described the second solution, and the content of the second coupling agent is the 0.05-10 % by weight, and the content of the second solvent is the 80-99.9 % by weight.Most preferably, take the total amount of the second solution as benchmark, the content of nano-Ag particles is the 0.1-5 % by weight in described the second solution, and the content of the second coupling agent is the 0.2-5 % by weight, and the content of the second solvent is the 90-99.7 % by weight.
According to the present invention, preferably, described the second solution is by nano-Ag particles, the second coupling agent and the second solvent composition.
According to the present invention, described nano-Ag particles is preferably the nano-Ag particles that granularity is the 1-1000 nanometer, and further preferably, the granularity of described nano-Ag particles is the 5-500 nanometer, and most preferably, the granularity of described nano-Ag particles is the 10-100 nanometer.
Among the present invention, the term granularity is well known in the art, refers to the size of particle, and the granularity of spherical particles represents with diameter usually.
Described nano-Ag particles can be loaded nano silver particle and/or non-loading type nano-Ag particles.Described loaded nano silver particle can be for various loaded nano silver particles well known in the art, such as the immobilized nano-Ag particles of inorganic salt.
According to the present invention, preferably, described the first coupling agent comprises at least a in silane coupling agent, titanate coupling agent, aluminate coupling agent, bimetal coupling agent, xylogen coupling agent and the tin coupling agent.Further preferably, described the first coupling agent is silane coupling agent and/or titanate coupling agent.
According to the present invention, preferably, described the second coupling agent comprises at least a in silane coupling agent, titanate coupling agent, aluminate coupling agent, bimetal coupling agent, xylogen coupling agent and the tin coupling agent.Further preferably, described the second coupling agent is silane coupling agent and/or titanate coupling agent.
Described the first coupling agent and the second coupling agent can be identical or different, and preferably, the two is identical.
According to the present invention, described the first solvent is preferably water and/or organic solvent, and further preferably, described organic solvent is at least a in the acid amides of the nitrile of furans, C2-C8 of acid, the C4-C14 of ketone, the C2-C8 of alcohol, the C3-C14 of C1-C6 and C1-C6; Most preferably be at least a in water, methyl alcohol, ethanol and the acetone.
Described the second solvent also is preferably water and/or above-mentioned organic solvent.Described the first solvent and the second solvent can be identical or different, and preferably, the two is identical.
According to the present invention, also preferably contain the first auxiliary agent in described the first solution, and take the weight of the first solution as benchmark, the content of auxiliary agent is preferably the 0.001-5 % by weight in described the first solution, more preferably the 0.01-1 % by weight; Preferably, described the first auxiliary agent is at least a in tensio-active agent, defoamer, dispersion agent, sequestrant and the thickening material.For example, described tensio-active agent is at least a in sodium laurylsulfonate, lauryl sulfosuccinate monoesters disodium, stearic acid and the glycerin fatty acid ester; Described defoamer is at least a in glycerine trihydroxy-polyethers, polydimethylsiloxane, myrcene and the firpene; Described dispersion agent is at least a in Sodium hexametaphosphate 99, sodium polyphosphate, white oil and the methanonaphthalene sodium sulfonate; Described sequestrant is citric acid, tartrate, fumaric acid, polymethyl acrylic acid and at least a in the polyacrylic acid is arranged; Described thickening material is at least a in Xylo-Mucine, sodium alginate and the Natvosol.
According to the present invention, add suitable auxiliary agent and can effectively help and improve coupling agent and the nano silver material dispersion effect in solution.
According to the present invention, preferably, described the first solution is by the first coupling agent, the first auxiliary agent and the first solvent composition.
Same, the second solution also can comprise the second auxiliary agent, and take the weight of the second solution as benchmark, the content of the second auxiliary agent is the 0.001-5 % by weight in described the second solution, more preferably the 0.01-1 % by weight; Preferably, described the second auxiliary agent is at least a in tensio-active agent, defoamer, dispersion agent, sequestrant and the thickening material.The optional scope of described tensio-active agent, defoamer, dispersion agent, sequestrant and thickening material does not repeat them here as hereinbefore.
Described the first auxiliary agent and the second auxiliary agent can be identical or different, and preferably, the two is identical.
According to the present invention, preferably, described the second solution is by nano-Ag particles, the second coupling agent, the second auxiliary agent and the second solvent composition.
According to the present invention, if mixed matrix is cleaned, can access better coating effects, preferably, before drying, comprise also with the 3rd solvent mixed matrix cleaned that described the 3rd solvent is water and/or organic solvent, preferably, at least a for in the acid amides of the nitrile of the furans of the acid of the ketone of the alcohol of C1-C6, C3-C14, C2-C8, C4-C14, C2-C8 and C1-C6 of described organic solvent; The ketone of the pure and mild C3-C14 of water, C1-C6 more preferably; Most preferably be water, methyl alcohol, ethanol, acetone.
Same, matrix before contacting is washed pre-treatment also can obtain preferably coating effects, the 4th used solvent of described washing is water and/or organic solvent, preferably, at least a for in the nitrile of the acid of the ketone of the alcohol of C1-C6, C3-C14, C2-C8, C4-C14 furans, C2-C8 and the C1-C6 acid amides of described organic solvent, the more preferably ketone of the pure and mild C3-C14 of water, C1-C6.
According to the present invention, the condition of described contact can in very large range change, and preferred, described contact is carried out under agitation condition, the condition of described contact comprises, temperature is 0-150 ℃, and the time is 1 second-10000 hours, further preferably, temperature is 20-100 ℃, time is 1 minute-50 hours, and most preferably, the time is 1-10 hour; The present inventor finds under study for action, when the condition that contacts can obtain better coating effects in above-mentioned scope.
According to the present invention, after the matrix after the described contact refers to that contact process finishes, with the matrix after the first solution separating, the condition of described mixing can in very large range change, and preferred, described being blended under the agitation condition carried out, the condition of described mixing comprises, temperature is 0-150 ℃, and the time is 1 second-10000 hours, further preferably, temperature is 20-100 ℃, time is 1 minute-50 hours, and most preferably, the time is 1-10 hour; The present inventor finds under study for action, when the condition of mixing can obtain better coating effects in above-mentioned scope.
Among the present invention, described stirring can be for this area various alr modes commonly used, such as mechanical stirring, and induction stirring etc.The mode of described contact and mixing can contact for this area is various and the mode of mixing, among the present invention, and described contact and mix and all be preferably immersion.
According to the present invention, after described mixed matrix refers to that mixing process finishes, with the matrix after the second solution separating, the temperature of described drying can in very large range change, only otherwise the character of destroying matrix gets final product, usually, the temperature of described drying is 0-300 ℃, and preferably, the temperature of described drying is 20-150 ℃, most preferably, the temperature of described drying is 40-120 ℃.The time of described drying is as the criterion with the complete desolvation of matrix.
According to the present invention, the purpose of described drying is in order to make the matrix desolvation, the various situations that need use to meet matrix.The means of described drying also can be for multiple, at least a in, vacuum-drying dry such as dry air, sunlight and the nitrogen protection drying.
According to the present invention, described matrix is the various materials that need plated film to reach antibacterial, and for example, described matrix includes but not limited in textiles, plastics, macromolecular material, metallic substance and the paper at least a.
Described matrix can have variform, includes but not limited to strip, fibrous, sheet, at least a in membranaceous and thread.
Matrix after the described dried contact, namely final product can have the colors such as white, yellow, green, black.
Below, by following examples the present invention is done more detailed description.Should be understood that these embodiment only to be used for explanation the present invention 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 reading the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Used all chemical reagent are analytical pure in the embodiment of the invention.
Embodiment 1
Taking by weighing 0.5 gram APTES is mixed in and is configured to the first solution in the 200ml distilled water, get the immobilized nano-Ag particles of 0.5 gram silicon-dioxide (available from U.S. AgION nano-silver ionic series, granularity is the 50-80 nanometer) be mixed in the 200ml distilled water, obtain the second solution.Then get 10 cotton fabrics crossed of gram cleaning, dryings and place the first solution, the control temperature is at 60 ℃, after soaking 5h under the condition of magnetic agitation, take out, then this cotton fabric is taken out and be placed in the second solution, the control temperature is at 80 ℃, take out after soaking 3h under the condition of magnetic agitation, use distilled water flushing, then oven dry namely obtained to have the product P 1 of antibacterial in one hour under 80 ℃ of conditions.
Embodiment 2
Take by weighing 1.5 gram Union carbide A-162s, 0.2 the gram sodium laurylsulfonate is mixed in and is configured to the first solution in the 200ml distilled water, get the immobilized nano-Ag particles of 0.1 gram silicon-dioxide (available from U.S. AgION nano-silver ionic series, granularity is the 50-80 nanometer) and 0.1 the gram Sodium hexametaphosphate 99 be mixed in the 200ml distilled water, obtain the second solution.Then get 10 cotton fabrics crossed of gram cleaning, dryings and place the first solution, the control temperature is at 40 ℃, after soaking 5h under the condition of magnetic agitation, take out, then this cotton fabric is taken out and be placed in the second solution, the control temperature is at 90 ℃, take out after soaking 3h under the condition of magnetic agitation, with mixing solutions (5: the 1) cleaning of distilled water and acetone, then oven dry namely obtained to have the product P 2 of antibacterial in one hour under 120 ℃ of conditions.
Embodiment 3
Taking by weighing 1.5 gram isopropyl triisostearoyl titanates and 0.15 gram lauryl sulfosuccinate monoesters disodium is mixed in and is configured to the first solution in the 200ml distilled water; get 0.2 gram nano silver powder (available from the positive nanometer silver in Shanghai, Shanghai Science and Technology Ltd.; granularity is the 20-30 nanometer) and 0.1 the gram sodium laurylsulfonate be mixed in the 200ml tetrahydrofuran (THF), obtain the second solution.Then get 30 cotton fabrics crossed of gram cleaning, dryings and place the first solution, the control temperature is at 90 ℃, after soaking 3h under the condition of magnetic agitation, take out, then this cotton fabric is taken out and be placed in the second solution, the control temperature is at 40 ℃, take out after soaking 6h under the condition of magnetic agitation, with the mixing solutions flushing of distilled water and ethanol (1: 1), then oven dry namely obtained to have the product P 3 of antibacterial in one hour under 40 ℃ of conditions.
Embodiment 4
Taking by weighing 1.0 gram isopropyl triisostearoyl titanates and 0.15 gram lauryl sulfosuccinate monoesters disodium is mixed in and is configured to the first solution in the 200ml distilled water; get 0.2 gram nano silver powder (available from the positive nanometer silver in Shanghai, the Shanghai granularity 20-30 of Science and Technology Ltd. nanometer), 0.1 gram sodium laurylsulfonate and 0.1 gram Sodium hexametaphosphate 99 and be mixed in the distilled water of 200ml and the mixing solutions of ethanol (1: 2), obtain the second solution.Then get 30 cotton fabrics crossed of gram cleaning, dryings and place the first solution, the control temperature is at 90 ℃, after soaking 3h under the condition of magnetic agitation, take out, then this cotton fabric is taken out and be placed in the second solution, the control temperature is at 40 ℃, take out after soaking 6h under the condition of magnetic agitation, use distilled water flushing, then oven dry namely obtained to have the product P 4 of antibacterial in one hour under 40 ℃ of conditions.
Test case 1
The product P 1-P4 for preparing among the embodiment 1-4 is carried out germ resistance test according to AATCC (U.S. textile dyeing man and chemist association) 100-1996 testing standard to representative bacterium together with the sample DP1 (as negative comparative sample) that does not carry out the nanometer silver processing, comprise streptococcus aureus and pneumobacillus.It has represented extraordinary antibacterial effect, its result shown in following table 1 and table 2, (method of calculation of anti-microbial property are: 1-(the bacterium number that detects in the bacterium number that detects in the product/negative comparative sample)):
Table 1
Table 1 has shown the product of the method according to this invention processing and the test result of negative contrast product anti-Staphylococcus aureus.
Table 2
Table 2 has shown the product of the method according to this invention processing and the test result of the anti-pneumobacillus of negative contrast product.
Can be found out by table 1 and table 2, after 24 hours, with only detecting less than 10 on the product P 1-P4 after the method processing of the present invention
6Individual bacterium, and the number of bacteria in the negative comparative sample has reached 10
7-10
9Sample after method of the present invention is processed, in 24 hours, anti-microbial property all can reach more than 99.94%.This illustrates that substrate coating method of the present invention can make matrix have fabulous anti-microbial property, and method preparation technology of the present invention is simple simultaneously, and environment is not polluted, and cost is low, is fit to scale operation.
Claims (13)
1. the film coating method of a matrix, it is characterized in that, the method comprises this matrix is contacted with the first solution, and the matrix after will contacting is mixed with the second solution, mixed matrix is carried out drying, wherein, described the first solution contains the first coupling agent and the first solvent, and described the second solution contains nano-Ag particles, the second coupling agent and the second solvent.
2. method according to claim 1, wherein, take the total amount of the first solution as benchmark, the content of the first coupling agent is the 0.01-40 % by weight in described the first solution, the content of the first solvent is the 60-99.99 % by weight.
3. method according to claim 1, wherein, take the total amount of the second solution as benchmark, the content of nano-Ag particles is the 0.01-30 % by weight in described the second solution, the content of the second coupling agent is the 0.01-20 % by weight, and the content of the second solvent is the 50-99.9 % by weight.
4. according to claim 1 or 3 described methods, wherein, the granularity of described nano-Ag particles is the 1-1000 nanometer.
5. according to claim 1 or 3 described methods, wherein, described nano-Ag particles is loaded nano silver particle and/or non-loading type nano-Ag particles.
6. method according to claim 1, wherein, described the first coupling agent comprises at least a in silane coupling agent, titanate coupling agent, aluminate coupling agent, bimetal coupling agent, xylogen coupling agent and the tin coupling agent, described the second coupling agent comprises at least a in silane coupling agent, titanate coupling agent, aluminate coupling agent, bimetal coupling agent, xylogen coupling agent and the tin coupling agent, and described the first coupling agent and the second coupling agent are identical or different.
7. method according to claim 1, wherein, described the first solvent is water and/or organic solvent, preferably, and at least a in the nitrile of the acid of the alcohol of described organic solvent C1-C6, the ketone of C3-C14, C2-C8, the furans of C4-C14, C2-C8 and the acid amides of C1-C6; Described the second solvent is water and/or organic solvent, and described the first solvent and the second solvent are identical or different.
8. method according to claim 1 wherein, also contains the first auxiliary agent in described the first solution, and take the weight of the first solution as benchmark, the content of the first auxiliary agent is the 0.001-5 % by weight in described the first solution; Preferably, described the first auxiliary agent is at least a in tensio-active agent, defoamer, dispersion agent, sequestrant and the thickening material; Also contain the second auxiliary agent in described the second solution, take the weight of the second solution as benchmark, the content of the second auxiliary agent is the 0.001-5 % by weight in described the second solution; Preferably, described the second auxiliary agent is at least a in tensio-active agent, defoamer, dispersion agent, sequestrant and the thickening material, and described the first auxiliary agent and the second auxiliary agent are identical or different.
9. the described method of any one according to claim 1-8 wherein, before drying, also comprises with the 3rd solvent mixed matrix is cleaned; Described the 3rd solvent is water and/or organic solvent, and preferably, described organic solvent is at least a in the acid amides of the nitrile of furans, C2-C8 of acid, the C4-C14 of ketone, the C2-C8 of alcohol, the C3-C14 of C1-C6 and C1-C6.
10. the described method of any one according to claim 1-8, wherein, described contact is carried out under agitation condition, and the condition of described contact comprises that temperature is 0-150 ℃, and the time is 1 second-10000 hours.
11. the described method of any one according to claim 1-8, wherein, described being blended under the agitation condition carried out, and the condition of described mixing comprises that temperature is 0-150 ℃, and the time is 1 second-10000 hours.
12. the described method of any one according to claim 1-8, wherein, the temperature of described drying is 0-300 ℃.
13. the described method of any one according to claim 1-8, wherein, described matrix is at least a in textiles, plastics, macromolecular material, metallic substance and the paper.
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Application publication date: 20130109 |