CN102816440A - Isolated soy protein-nano silver antibacterial composite membrane and preparation method thereof - Google Patents
Isolated soy protein-nano silver antibacterial composite membrane and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of nano materials and antibacterial materials, and particularly relates to an isolated soy protein-nano silver antibacterial composite membrane and a preparation method thereof. The preparation method includes mixing the isolated soy protein with silver nitrate, in-situ reducing precursors of silver into silver nano particles in the absence of sunlight or simulated sunlight, and preparing the particles into a composite membrane material; or preparing the isolated soy protein into a membrane material, soaking the membrane into a silver nitrate aqueous solution, and then in-situ reducing precursors of the silver into silver nano particles in the absence of the sunlight or the simulated sunlight. According to the antibacterial composite membrane and the preparation method thereof, the isolated soy protein serves as the base material, the reducing agent of silver ions and the stabilizer of nano silver simultaneously, other chemical reagents are not needed, and the preparation process is simple, energy-saving and environment-friendly; and the prepared composite membrane has efficient, broad-spectrum and durable antibacterial effects, and is suitable for fields of food packaging, hygienic products, daily necessities, medical materials and the like.
Description
Technical field
The invention belongs to nano material, anti-biotic material technical field, be specifically related to a kind of soybean protein isolate-nanometer silver antimicrobial composite package and preparation method thereof.
Background technology
Anti-biotic material is meant can kill or hinder microorganism growth breeding and active one type of functional materials thereof.Along with development in science and technology and people to healthy living require increasingly highly, antimicrobial technology and anti-biotic material have received concern more and more widely.Anti-biotic material relatively more commonly used at present comprises inorganic system and organic system two big classes.Inorganic owner will refer to all kinds of metallicss and its esters etc., mainly comprises metal_based material, natural mineral, thomel etc.; The principal item of organic system has quaternary ammonium salts, biguanides, alcohols, phenols, pyridines, imidazoles, halogen amine etc.Inorganic antibacterial material is compared with the organic anti-bacterial material, has wide spectrum, durable, safe characteristics, and wherein silver is that anti-biotic material has become present most widely used inorganic antibacterial material.Silver is that anti-biotic material has a long history; Just bring into use silverware to deposit food ancient Roman even epoch people more early and prevent corruption, but common silvery agent sterilizing power is not strong, antimicrobial spectrum is wideless yet; The appearance of nanotechnology has broken through the weak bottleneck of common silvery agent sterilizing power.
Nanometer silver is to be the novel product that foundation development forms with the nanotechnology, has very excellent characteristic at aspects such as electricity, optics and catalysis.Simultaneously because surface effects, volume effect, quantum size effect and macro quanta tunnel effect; It is the incomparable antibacterial effect of anti-biotic material that nanometer silver has conventional silver; The nanometer silver of minute quantity can make mikrobe comprise that the growth of bacterium, fungi, yeast etc. and breeding keep lower level, and renders a service lastingly.Based on this, nano silver antibacterial material has very application prospects, comprises various antibiotic dress ornaments, antibacterials, toy for children, personal-care supplies etc.
The preparation of nanometer silver can be divided into two types of direct method and indirect methods.Directly preparation method mainly is the physics preparation method, and methods such as laser ablation method, microwave reduction method, sputtering method and mechanical milling method are arranged, but the physics preparation method is had relatively high expectations the productive expense costliness to plant and instrument.Preparation method can be divided into chemical reduction method and biological reducing method indirectly.Chemical reduction method is in the presoma of silver, to add a certain amount of reductive agent, like Peng Qinghuana, Trisodium Citrate, Hydrazine Hydrate 80, xitix etc., presoma is reduced to simple substance silver, and the further growth of simple substance silver is silver-colored particle.Silver particles is prone to reunion, therefore often needs to add certain amount of stabilizer or dispersion agent, waits like polyoxyethylene glycol, thiol derivatives, aniline, long-chain amine, tensio-active agent and reduces silver-colored particulate reunion.But the used chemical reagent of chemical method commonly used all has harm to human body or environment to a certain extent, stablizer that has or dispersion agent even carinogenicity is arranged.Therefore, low consumption, oligosaprobic biological reducing method have just received increasing concern.This method is for one type to utilize the biological activity reducing metal ion of mikrobe, and another kind of is the reducing substances reducing metal ion that utilizes natural materials itself to contain.Based on the latter, increasing people is devoted to select a kind of natural materials with good biocompatibility, and adopts simple, green method to prepare nanometer silver.
It is matrix that the present invention adopts the soybean protein isolate of green natural, utilizes tyrosine in the soybean protein isolate good reductibility under alkaline condition, and the presoma of silver is reduced to silver-colored simple substance; Because groups such as the amino that enrich on the soybean protein isolate surface, carboxyl have good affinity to silver, make the nano silver particles that generates to stablize for a long time, thereby obtain stable soybean protein isolate-nano-ag composite simultaneously.Utilize the excellent processability of soybean protein isolate at last, prepare have efficient, wide spectrum, the soybean protein isolate-nanometer silver antimicrobial composite package of persistent antibacterial effect.Soybean protein isolate need not to add any other chemical reagent simultaneously as reductive agent and stablizer in whole process of preparation, and is green non-poisonous, simple and convenient, easy handling.Simultaneously, soybean protein isolate wide material sources, with low cost, good biocompatibility, therefore this method for preparing soybean protein isolate-nanometer silver antimicrobial composite package has suitable feasibility and practical significance.
Summary of the invention
The object of the present invention is to provide and a kind ofly prepare that process is simple, energy-conserving and environment-protective, have soybean protein isolate-Nano silver grain antimicrobial compound film of good anti-microbial property and preparation method thereof.
The preparation method of soybean protein isolate provided by the present invention-nanometer silver antimicrobial composite package specifically can be divided into 2 kinds:
(1) soybean protein isolate in-situ reducing Silver Nitrate prepares nanometer silver, and further prepares soybean protein isolate-nanometer silver antimicrobial composite package, and concrete steps are following:
(1) preparation quality concentration is 0.25 ~ 6% the soybean protein isolate aqueous solution, stirs dropwise to add sodium hydroxide, regulator solution pH to 9 ~ 12 down;
(2) stirring adds Silver Nitrate down in step (1) gained solution, obtains the mixed solution that silver nitrate concentration is 2 ~ 50 mmol/L, continues to stir 25 ~ 40 min;
(3) mixing solutions that step (2) is obtained is exposed under sunshine or the simulated solar irradiation, and illumination action time is 0.5 ~ 24 h, obtains uniform soybean protein isolate-nanometer silver mixing solutions;
(4) it is in 1 ~ 6% the soybean protein isolate solution that the soybean protein isolate that step (3) is obtained-nanometer silver mixing solutions joins massfraction; The add-on of control silver is 0.05 ~ 2% of a soybean protein isolate consumption, is prepared into soybean protein isolate-nanometer silver antimicrobial composite package then.
(2) preparation soy protein isolate film, and utilize soy protein isolate film in-situ reducing Silver Nitrate to prepare soybean protein isolate-nanometer silver antimicrobial composite package, concrete steps are following:
(1) preparation quality concentration is 0.25 ~ 6% the soybean protein isolate aqueous solution, stirs down dropwise to add sodium hydroxide, and regulator solution pH to 9-12 prepares soy protein isolate film then;
(2) soy protein isolate film that step (1) is obtained is immersed in the silver nitrate solution that concentration is 2 ~ 50 mg/mL, and soak time is 0.5 –, 5 h;
(3) immersion that step (2) is obtained has the soy protein isolate film of silver nitrate solution to be exposed under sunshine or the simulated solar irradiation; Illumination action time is 0.5 ~ 24 h; Use deionized water wash then 4 ~ 6 times, room temperature is dried, and obtains soybean protein isolate-nanometer silver antimicrobial composite package.
The concrete operations step of aforesaid method is following:
1. a soybean protein isolate in-situ reducing Silver Nitrate prepares nanometer silver; And further prepare the method for soybean protein isolate-nanometer silver antimicrobial composite package: 10 g soybean isolate protein powder ends are dissolved in the aqueous solution of 100 g Guanidinium hydrochlorides and 25 mg WR 34678s; Dialysis is after 72 hours, again with the extremely approaching neutrality of deionized water dialysis in the aqueous sodium hydroxide solution of pH=11.Adopt the centrifugal insolubles of removing minute quantity in 10 minutes of speed of 9000 r/min; Obtain mass concentration and be about 2% the soybean protein isolate aqueous solution, then through concentrate or the deionized water dilution to obtain mass concentration be 0.25 ~ 6% the soybean protein isolate aqueous solution.Stir down dropwise dropping sodium and regulate soybean protein isolate pH value of solution to 9 ~ 12, the Silver Nitrate solids that add different amounts then obtain the soybean protein isolate that silver nitrate concentration is 2 ~ 50 mmol/L-Silver Nitrate mixed solution, continue to mix 30 min.This mixing solutions is exposed to irradiation 0.5 ~ 24 h under sunshine or the simulated solar irradiation, obtains uniform soybean protein isolate-nanometer silver mixing solutions.It is in 1 ~ 6% the soybean protein isolate solution that the gained mixed solution is joined massfraction, and the add-on of control silver is 0.05 ~ 2% of a soybean protein isolate consumption, then with this soybean protein isolate-nanometer silver mixing solutions casting film, drying at room temperature.Prepared film is 60
oCrosslinked 1 h under the C water bath condition (crosslinked fluid is for the epoxy chloropropane volumetric concentration is 1%, the ethanol volumetric concentration is 70% the aqueous solution); Then with film with deionized water wash 5 times to remove unreacted Silver Nitrate, epoxy chloropropane; Drying at room temperature can make soybean protein isolate-nanometer silver antimicrobial composite package.
2. one kind prepares soy protein isolate film; Utilize soy protein isolate film in-situ reducing Silver Nitrate to prepare the method for soybean protein isolate-nanometer silver antimicrobial composite package then: 10 g soybean isolate protein powder ends are dissolved in the aqueous solution of 100 g Guanidinium hydrochlorides and 25 mg WR 34678s; Dialysis is after 72 hours, again with the extremely approaching neutrality of deionized water dialysis in the aqueous sodium hydroxide solution of pH=11.Adopting the centrifugal insolubles of removing minute quantity in 10 minutes of speed of 9000 r/min to obtain mass concentration is about 2% the soybean protein isolate aqueous solution, then through concentrate or the deionized water dilution to obtain mass concentration be 0.25 ~ 6% the soybean protein isolate aqueous solution.Dropwise dropping sodium solution is regulated soybean protein isolate pH value of solution to 9 ~ 12, with this mixing solutions casting film, drying at room temperature.With the film that makes 60
oCrosslinked 1 h under the C water bath condition (crosslinked fluid is for the epoxy chloropropane volumetric concentration is 1%, the ethanol volumetric concentration is 70% the aqueous solution); With film with deionized water wash 5 times to remove unreacted Silver Nitrate, epoxy chloropropane; Drying at room temperature makes soy protein isolate film.Then soy protein isolate film is immersed in the silver nitrate solution that concentration is 2 ~ 50 mg/mL, soaks 0.5 ~ 5 h; Have the immersion that obtains the soy protein isolate film of silver nitrate solution to be exposed under sunshine or the simulated solar irradiation, illumination action time is 0.5 ~ 24 h; Take out with deionized water wash 5 times, normal temperature dries, and obtains soybean protein isolate-nanometer silver antimicrobial composite package.
Compared with prior art, the present invention has following characteristics:
Soybean protein isolate need not to add other chemical reagent simultaneously as the reductive agent of Silver Nitrate and the stablizer of nanometer silver, pollutes few.
Required illumination condition can be sunshine or simulated solar illumination, conveniently is easy to get.
Reaction conditions is gentle, need not severe condition such as HTHP, good energy-conserving effect.
Prepared nanometer silver particle diameter little (about 5-7 nm), size distribution are even.Little particle diameter has higher specific surface area, also just means higher anti-microbial activity and lower consumption.
The nanometer silver good stability, placement still can keep good dispersiveness half a year, and can dissolve each other with plurality of reagents, and therefore Application Areas is widely arranged.
Soybean protein isolate is as mould material matrix, and biocompatibility and biological degradability are good.
Antibiotic high efficiency.Silver amount concentration is that sterilizing rate can reach more than 99.9% in 1% material 2 h.
Broad-spectrum antibacterial property.Prepared anti-biotic material has all shown excellent resistance for gram-positive microorganism and Gram-negative bacteria.
Embodiment
Below utilize embodiment further explain the present invention, but can not think to limit scope of invention.
Embodiment 1: get mass concentration and be 0.25% soybean protein isolate solution 5 mL; Stir following dropwise dropping sodium and regulate its pH to 10; Drip silver nitrate solution; Obtaining silver nitrate concentration is soybean protein isolate-Silver Nitrate mixed solution of 25 mmol/L, stirs 30 min and makes Silver Nitrate and soybean protein isolate thorough mixing, and this mixing solutions is exposed to illumination 2 h under the sunshine.Obtain soybean protein isolate-nanometer silver mixed solution.It is in 6% the soybean protein isolate solution that the gained mixed solution is joined massfraction, and the add-on of control silver is 0.1% of a soybean protein isolate consumption, stirs 10 min, makes it thorough mixing, it is watered to cast from the film forming container then, at room temperature drying and forming-film.With the film that makes 60
oCrosslinked 1 h under the C water bath condition (crosslinked fluid is for the epoxy chloropropane volumetric concentration is 1%, the ethanol volumetric concentration is 70% the aqueous solution); Then with film with in the deionized water washing 5 times to remove unreacted Silver Nitrate, epoxy chloropropane; Room temperature is dried, and can make soybean protein isolate-nanometer silver antimicrobial composite package.
Operate preparation intestinal bacteria suspension-s according to the antibacterial experiment standard method; It is inoculated into above-mentioned gained soybean protein isolate-nanometer silver antimicrobial composite package surface, act on 2 h after, bacterium liquid is transferred in the 25 mL PBS damping fluids dilution, coated plate, 37 together with antibacterial film
oCount after cultivating 24 h in the C bio-incubator.The result shows, gained soybean protein isolate-nanometer silver antimicrobial composite package contacts and in 2 h, can reach more than 80% colibacillary sterilizing rate when antibiotic.
Embodiment 2: get mass concentration and be 0.5% soybean protein isolate solution 5 mL; Stir following dropwise dropping sodium and regulate its pH to 10; Drip silver nitrate solution; Obtaining silver nitrate concentration is soybean protein isolate-Silver Nitrate mixed solution of 25 mmol/L, stirs 30 min and makes Silver Nitrate and soybean protein isolate thorough mixing, this mixing solutions is exposed to illumination 4 h under the incandescent light of 100 W.It is in 2% the soybean protein isolate solution that the gained mixed solution is joined massfraction, and the add-on of control silver is 1% of a soybean protein isolate consumption, stirs 30 min, makes it thorough mixing, it is watered to cast from the film forming container then, at room temperature drying and forming-film.With the film that makes 60
oCrosslinked 1 h under the C water bath condition (crosslinked fluid is for the epoxy chloropropane volumetric concentration is 1%, the ethanol volumetric concentration is 70% the aqueous solution); Then with film with in the deionized water washing 5 times to remove unreacted Silver Nitrate, epoxy chloropropane; Room temperature is dried, and can make soybean protein isolate-nanometer silver antimicrobial composite package.
Operate according to the antibacterial experiment standard method, prepare golden yellow grape ball suspension-s; It is inoculated into above-mentioned gained soybean protein isolate-nanometer silver antimicrobial composite package surface, act on 2 h after, bacterium liquid is transferred in the 25 mL PBS damping fluids dilution, coated plate, 37 together with antibacterial film
oCount after cultivating 24 h in the C bio-incubator.The result shows, gained soybean protein isolate-nanometer silver antimicrobial composite package contacts when antibiotic that sterilizing rate to streptococcus aureus can reach 99.9% in 2 h.
Embodiment 3: get mass concentration and be 4% soybean protein isolate solution 10 mL, stir down dropwise dropping sodium and regulate its pH to 11, this soybean protein isolate aqueous solution is watered cast from the film forming container, at room temperature drying and forming-film.Prepared film is 60
oCrosslinked 1 h under the C water bath condition (crosslinked fluid is for the epoxy chloropropane volumetric concentration is 1%, the ethanol volumetric concentration is 70% the aqueous solution), then with film with deionized water wash 5 times with after removing unreacted epoxy chloropropane, dry under the room temperature.Then this soy protein isolate film is immersed in the silver nitrate solution that concentration is 25 mg/mL and leaves standstill 2 h, subsequently whole reaction system is exposed to irradiation 12 h under the sunshine.With its taking-up,, dry under the room temperature with deionized water wash 5 times with after removing unreacted Silver Nitrate, can make soybean protein isolate-nanometer silver antimicrobial composite package.
Operate preparation streptococcus aureus suspension-s according to the antibacterial experiment standard method; It is inoculated into above-mentioned gained soybean protein isolate-nanometer silver antimicrobial composite package surface, act on 12 h after, bacterium liquid is transferred in the 25 mL PBS damping fluids dilution, coated plate, 37 together with antibacterial film
oCount after cultivating 24 h in the C bio-incubator.The result shows, gained soybean protein isolate-nanometer silver antimicrobial composite package contacts when antibiotic that sterilizing rate to streptococcus aureus reaches 90% in 2 h, in 12 h, can reach 99.9%.
Embodiment 4: get mass concentration and be 6% soybean protein isolate solution 8 mL, stir down dropwise dropping sodium and regulate its pH to 12, this soybean protein isolate aqueous solution is watered cast from the film forming container, at room temperature drying and forming-film.Prepared film is 60
oCrosslinked 1 h under the C water bath condition (crosslinked fluid is for the epoxy chloropropane volumetric concentration is 1%, the ethanol volumetric concentration is 70% the aqueous solution), then with film with deionized water wash 5 times with after removing unreacted epoxy chloropropane, dry under the room temperature.Then this soy protein isolate film is immersed in the silver nitrate solution that concentration is 50 mg/mL and leaves standstill 4 h, subsequently whole reaction system is exposed to the following irradiation of incandescent light 24 h of 100 W.With its taking-up,, dry under the room temperature with deionized water wash 5 times with after removing unreacted Silver Nitrate, can make soybean protein isolate-nanometer silver antimicrobial composite package.
Operate preparation intestinal bacteria suspension-s according to the antibacterial experiment standard method; It is inoculated into above-mentioned gained soybean protein isolate-nanometer silver antimicrobial composite package surface, act on 2 h after, bacterium liquid is transferred in the 25 mL PBS damping fluids dilution, coated plate, 37 together with antibacterial film
oCount after cultivating 24 h in the C bio-incubator.The result shows, gained soybean protein isolate-nanometer silver antimicrobial composite package contacts and in 2 h, can reach 99.9% to colibacillary sterilizing rate when antibiotic.
Embodiment 5: get mass concentration and be 2% soybean protein isolate solution 5 mL; Stir following dropwise dropping sodium and regulate its pH to 10; Drip silver nitrate solution; Obtaining silver nitrate concentration is soybean protein isolate-Silver Nitrate mixed solution of 25 mmol/L, stirs 30 min and makes Silver Nitrate and soybean protein isolate thorough mixing, and this mixing solutions is exposed to illumination 4 h under the sunshine.Obtain soybean protein isolate-nanometer silver mixed solution.It is in 3% the soybean protein isolate solution that the gained mixed solution is joined massfraction, and the add-on of control silver is 0.1% of a soybean protein isolate consumption, stirs 10 min, makes it thorough mixing, it is watered to cast from the film forming container then, at room temperature drying and forming-film.With the film that makes 60
oCrosslinked 1 h under the C water bath condition (crosslinked fluid is for the epoxy chloropropane volumetric concentration is 1%, the ethanol volumetric concentration is 70% the aqueous solution); Then with film with in the deionized water washing 5 times to remove unreacted Silver Nitrate, epoxy chloropropane; Room temperature is dried, and can make soybean protein isolate-nanometer silver antimicrobial composite package.
Operate preparation streptococcus aureus suspension-s according to the antibacterial experiment standard method; Soybean protein isolate-nanometer silver antimicrobial composite package is dipped in the 30 mL inoculums, place vibrator vibration (200 r/min) 2 h after, dilution, coated plate, 37
oCount after cultivating 24 h in the C bio-incubator.The result shows, gained soybean protein isolate-nanometer silver antimicrobial composite package vibrates when antibiotic, and sterilizing rate to streptococcus aureus can reach 99.9% in 2 h.
Embodiment 6: gets mass concentration and is 6% soybean protein isolate solution 10 mL, stir down dropwise dropping sodium and regulate its pH to 10, and, this soybean protein isolate aqueous solution watered cast from the film forming container, at room temperature drying and forming-film.Prepared film is 60
oCrosslinked 1 h under the C water bath condition (crosslinked fluid is for the epoxy chloropropane volumetric concentration is 1%, the ethanol volumetric concentration is 70% the aqueous solution), then with film with deionized water wash 5 times with after removing unreacted epoxy chloropropane, dry under the room temperature.Then this soy protein isolate film is immersed in the silver nitrate solution that concentration is 50 mg/mL and leaves standstill 5 h, subsequently whole reaction system is exposed to irradiation 12 h under the sunshine.With its taking-up,, dry under the room temperature with deionized water wash 5 times with after removing unreacted Silver Nitrate, can make soybean protein isolate-nanometer silver antimicrobial composite package.
Operate preparation intestinal bacteria bacterium suspension-s according to the antibacterial experiment standard method; Soybean protein isolate-nanometer silver antimicrobial composite package is dipped in the 30 mL inoculums, place vibrator vibration (200 r/min) 2 h after, dilution, coated plate, 37
oCount after cultivating 24 h in the C bio-incubator.The result shows, gained soybean protein isolate-nanometer silver antimicrobial composite package vibrates and in 2 h, can reach 99.9% to colibacillary sterilizing rate when antibiotic.
Claims (3)
1. the preparation method of soybean protein isolate-nanometer silver antimicrobial composite package is divided into 2 kinds:
(1) soybean protein isolate in-situ reducing Silver Nitrate prepares nanometer silver, and further prepares soybean protein isolate-nanometer silver antimicrobial composite package, and concrete steps are following:
(1) preparation quality concentration is 0.25 ~ 6% the soybean protein isolate aqueous solution, stirs dropwise to add sodium hydroxide, regulator solution pH to 9 ~ 12 down;
(2) stirring adds Silver Nitrate down in step (1) gained solution, obtains the mixed solution that silver nitrate concentration is 2 ~ 50 mmol/L, continues to stir 25 ~ 40 min;
(3) mixing solutions that step (2) is obtained is exposed under sunshine or the simulated solar irradiation, and illumination action time is 0.5 ~ 24 h, obtains uniform soybean protein isolate-nanometer silver mixing solutions;
(4) soybean protein isolate that step (3) is obtained-nanometer silver mixing solutions joins in the soybean protein isolate solution that massfraction is 1%-6%; The add-on of control silver is 0.05% ~ 2% of a soybean protein isolate consumption, is prepared into soybean protein isolate-nanometer silver antimicrobial composite package then;
(2) preparation soy protein isolate film, and utilize soy protein isolate film in-situ reducing Silver Nitrate to prepare soybean protein isolate-nanometer silver antimicrobial composite package, concrete steps are following:
(1) preparation quality concentration is the soybean protein isolate aqueous solution of 0.25-6%, stirs down dropwise to add sodium hydrate regulator solution pH to 9-12, prepares soy protein isolate film then;
(2) soy protein isolate film that step (1) is obtained is immersed in the silver nitrate solution that concentration is 2 ~ 50 mg/mL, and soak time is 0.5 –, 5 h;
(3) immersion that step (2) is obtained has the soy protein isolate film of silver nitrate solution to be exposed under sunshine or the simulated solar irradiation, and illumination action time is 0.5 ~ 24 h; With deionized water wash 4-6 time, room temperature is dried; Obtain soybean protein isolate-nanometer silver antimicrobial composite package.
2. soybean protein isolate-nanometer silver antimicrobial matrix material that preparation method as claimed in claim 1 obtains.
3. the soybean protein isolate as claimed in claim 2-application of nanometer silver antimicrobial matrix material in food product pack, sanitary product, medical material.
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| CN103141514A (en) * | 2013-03-06 | 2013-06-12 | 广西中医药大学 | Silver-containing antimicrobial agent and preparation method thereof |
| CN103642070A (en) * | 2013-11-11 | 2014-03-19 | 青岛文创科技有限公司 | Antibiotic composite membrane of nano-silk fibroin-chitosan-nano-silver |
| CN103665894A (en) * | 2013-11-11 | 2014-03-26 | 青岛佰众化工技术有限公司 | Nanometer silk fibroin-nano-silver antibacterial composite material |
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| CN108359140A (en) * | 2018-03-27 | 2018-08-03 | 陕西杨凌陕特农业发展有限公司 | A kind of nanometer silver antimicrobial film and preparation method thereof containing honey |
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| CN114573846A (en) * | 2022-03-22 | 2022-06-03 | 哈尔滨学院 | Preparation method of soybean protein antibacterial biomembrane with high mechanical strength |
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| CN103141514B (en) * | 2013-03-06 | 2015-05-13 | 广西中医药大学 | Silver-containing antimicrobial agent and preparation method thereof |
| CN103642070A (en) * | 2013-11-11 | 2014-03-19 | 青岛文创科技有限公司 | Antibiotic composite membrane of nano-silk fibroin-chitosan-nano-silver |
| CN103665894A (en) * | 2013-11-11 | 2014-03-26 | 青岛佰众化工技术有限公司 | Nanometer silk fibroin-nano-silver antibacterial composite material |
| CN104817706A (en) * | 2015-03-12 | 2015-08-05 | 浙江海洋学院 | Preparation method for Setipinna tenuifilis protein nano-silver antibacterial film |
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| CN106279744A (en) * | 2016-09-22 | 2017-01-04 | 东北农业大学 | A kind of controlled release biocidal property eats composite membrane and preparation method thereof |
| CN107739055A (en) * | 2017-11-02 | 2018-02-27 | 太原工业学院 | A kind of method that biological template method prepares nanometer titanium dioxide manganese material |
| CN108359140A (en) * | 2018-03-27 | 2018-08-03 | 陕西杨凌陕特农业发展有限公司 | A kind of nanometer silver antimicrobial film and preparation method thereof containing honey |
| CN114376067A (en) * | 2022-01-18 | 2022-04-22 | 大连工业大学 | Modified protein nano-particle, preparation method and application thereof |
| CN114573846A (en) * | 2022-03-22 | 2022-06-03 | 哈尔滨学院 | Preparation method of soybean protein antibacterial biomembrane with high mechanical strength |
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| WO2024069222A1 (en) * | 2022-10-01 | 2024-04-04 | Heidarisoureshjani Maryam | Clothing with soy fibers for butterfly patients |
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