CN102816440B - 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-nano silver antibacterial composite membrane and preparation method thereof.
Background technology
Anti-biotic material refers to the class functional materials can killing or hinder microbial growth and activity thereof.Along with development in science and technology and the requirement of people to healthy living more and more higher, antimicrobial technology and anti-biotic material receive to be paid close attention to more and more widely.Anti-biotic material relatively more conventional at present comprises inorganic system and the large class of organic system two.Inorganic owner will refer to all kinds of metallics and its esters etc., mainly comprises metal_based material, natural mineral, carbon fiber etc.; The principal item of organic system has quaternary ammonium salts, biguanides, alcohols, phenols, pyridines, imidazoles, halogen amine etc.Inorganic antibacterial material, compared with organic anti-bacterial material, has wide spectrum, durable, safe feature, and wherein silver system anti-biotic material has become current most widely used inorganic antibacterial material.Silver system anti-biotic material has a long history, in ancient Roman, epoch people even more early just bring into use silverware storing food to prevent corruption, but common silvery agent sterilizing power is not strong, and antimicrobial spectrum is wideless yet, the appearance of nanotechnology, breaches the bottleneck that common silvery agent sterilizing power is weak.
Nanometer silver is the novel product developed based on nanotechnology, in electricity, optics and catalysis etc., have very excellent characteristic.Simultaneously due to surface effects, volume effect, quantum size effect and macro quanta tunnel effect, nanometer silver has the incomparable antibacterial effect of conventional silver system anti-biotic material, the Growth and reproduction that the nanometer silver of minute quantity can make microorganism comprise bacterium, fungi, yeast etc. keeps lower level, and effect is lasting.Based on this, nano silver antibacterial material has application prospect widely, comprises various antibacterial dress ornament, antibacterials, toy for children, personal-care supplies etc.
The preparation of nanometer silver can be divided into direct method and indirect method two class.Direct preparation method is physics preparation method mainly, has the methods such as laser ablation, Microwave reduction method, sputtering method and mechanical milling method, but physics preparation method requires higher to plant and instrument, and productive expense is expensive.Indirect preparation method can be divided into chemical reduction method and biological reducing method.Chemical reduction method adds a certain amount of reductive agent in the presoma of silver, and as sodium borohydride, Trisodium Citrate, hydrazine hydrate, xitix etc., presoma is reduced to elemental silver, elemental silver further growth is Argent grain.Silver particles is easily reunited, and therefore often need add a certain amount of stablizer or dispersion agent, as polyoxyethylene glycol, thiol derivatives, aniline, long-chain amine, tensio-active agent etc. reduce the reunion of Argent grain.But the chemical reagent commonly using chemical method used has harm to human body or environment to a certain extent, and some stablizers or dispersion agent even have carinogenicity.Therefore, low consumption, oligosaprobic biological reducing method just receive increasing concern.The method one class is the biological activity reducing metal ion utilizing microorganism, and another kind of is the reducing substances reducing metal ion utilizing 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.
The present invention adopts the soybean protein isolate of green natural to be matrix, utilizes the reductibility that the tyrosine in soybean protein isolate is excellent in the basic conditions, the presoma of silver is reduced to silver-colored simple substance; Simultaneously because the group such as amino, carboxyl that soybean protein isolate surface is abundant has good affinity to silver, make the nano silver particles that generates can long-time stable, thus obtain stable soybean protein isolate-nano-ag composite.Finally utilize the processability of soybean protein isolate excellence, prepare and there is efficient, wide spectrum, lasting antibacterial effect soybean protein isolate-nano silver antibacterial composite membrane.In whole preparation process, soybean protein isolate is simultaneously as reductive agent and stablizer, without the need to adding any other chemical reagent, green non-poisonous, simple and convenient, easy handling.Meanwhile, soybean protein isolate wide material sources, with low cost, good biocompatibility, therefore this method preparing soybean protein isolate-nano silver antibacterial composite membrane has suitable feasibility and practical significance.
Summary of the invention
The object of the present invention is to provide that a kind of preparation process is simple, energy-conserving and environment-protective, the soybean protein isolate-Nano silver grain antimicrobial compound film with good anti-microbial property and preparation method thereof.
The preparation method of soybean protein isolate-nano silver antibacterial composite membrane provided by the present invention, specifically can be divided into 2 kinds:
(1) soybean protein isolate in-situ reducing Silver Nitrate prepares nanometer silver, and prepares soybean protein isolate-nano silver antibacterial composite membrane further, and concrete steps are as follows:
(1) preparation quality concentration is the soybean separation protein white water solution of 0.25 ~ 6%, dropwise adds sodium hydroxide under stirring, regulator solution pH to 9 ~ 12;
(2) in step (1) gained solution, add Silver Nitrate under stirring, obtain the mixed solution that silver nitrate concentration is 2 ~ 50 mmol/L, continue stirring 25 ~ 40 min;
(3), under the mixing solutions that step (2) obtains being exposed to sunlight or simulated solar irradiation, illumination action time is 0.5 ~ 24 h, obtains uniform soybean protein isolate-nanometer silver mixing solutions;
(4) soybean protein isolate-nanometer silver mixing solutions that step (3) obtains being joined massfraction is in the soybean protein isolate solution of 1 ~ 6%, the add-on controlling silver is 0.05 ~ 2% of soybean protein isolate consumption, is then prepared into soybean protein isolate-nano silver antibacterial composite membrane.
(2) prepare soy protein isolate film, and utilize soy protein isolate film in-situ reducing Silver Nitrate to prepare soybean protein isolate-nano silver antibacterial composite membrane, concrete steps are as follows:
(1) preparation quality concentration is the soybean separation protein white water solution of 0.25 ~ 6%, dropwise adds sodium hydroxide under stirring, and regulator solution pH to 9-12, then prepares soy protein isolate film;
(2) soy protein isolate film that step (1) obtains being immersed in concentration is in the silver nitrate solution of 2 ~ 50 mg/mL, and soak time is 0.5 – 5 h;
(3) under the soy protein isolate film immersed with silver nitrate solution that step (2) obtains being exposed to sunlight or simulated solar irradiation, illumination action time is 0.5 ~ 24 h, then deionized water wash is used 4 ~ 6 times, room temperature is dried, and obtains soybean protein isolate-nano silver antibacterial composite membrane.
The concrete operation step of aforesaid method is as follows:
1. a soybean protein isolate in-situ reducing Silver Nitrate prepares nanometer silver, and prepare the method for soybean protein isolate-nano silver antibacterial composite membrane further: 10 g soybean isolate protein powder ends are dissolved in the aqueous solution of 100 g Guanidinium hydrochlorides and 25 mg dithiothreitol (DTT), after dialysing 72 hours in the aqueous sodium hydroxide solution of pH=11, then with deionized water dialysis to close neutral.Adopt the insolubles of centrifugation 10 minutes removing minute quantities of 9000 r/min, obtain the soybean separation protein white water solution that mass concentration is about 2%, then obtain by concentrated or deionized water dilution the soybean separation protein white water solution that mass concentration is 0.25 ~ 6%.Dropwise drip sodium hydroxide under stirring and regulate soybean protein isolate pH value of solution to 9 ~ 12, the Silver Nitrate solid then adding different amount obtains soybean protein isolate-Silver Nitrate mixed solution that silver nitrate concentration is 2 ~ 50 mmol/L, continues to be uniformly mixed 30 min.Irradiate 0.5 ~ 24 h under this mixing solutions being exposed to sunlight or simulated solar irradiation, obtain uniform soybean protein isolate-nanometer silver mixing solutions.Gained mixed solution being joined massfraction is in the soybean protein isolate solution of 1 ~ 6%, and the add-on controlling silver is 0.05 ~ 2% of soybean protein isolate consumption, then by this soybean protein isolate-nanometer silver mixing solutions casting film, and drying at room temperature.Obtained film is 60
ounder C water bath condition, crosslinked 1 h(crosslinked fluid is epoxy chloropropane volumetric concentration is 1%, ethanol contend concentration is the aqueous solution of 70%), then by film deionized water wash 5 times to remove unreacted Silver Nitrate, epoxy chloropropane, drying at room temperature, can obtain soybean protein isolate-nano silver antibacterial composite membrane.
2. prepare soy protein isolate film for one kind, then soy protein isolate film in-situ reducing Silver Nitrate is utilized to prepare the method for soybean protein isolate-nano silver antibacterial composite membrane: to be dissolved in the aqueous solution of 100 g Guanidinium hydrochlorides and 25 mg dithiothreitol (DTT) by 10 g soybean isolate protein powder ends, after dialysing 72 hours in the aqueous sodium hydroxide solution of pH=11, then with deionized water dialysis to close neutral.Adopt the insolubles of centrifugation 10 minutes removing minute quantities of 9000 r/min to obtain the soybean separation protein white water solution that mass concentration is about 2%, then obtain by concentrated or deionized water dilution the soybean separation protein white water solution that mass concentration is 0.25 ~ 6%.Dropwise drip sodium hydroxide solution and regulate soybean protein isolate pH value of solution to 9 ~ 12, by this mixing solutions casting film, drying at room temperature.By obtained film 60
ounder C water bath condition, crosslinked 1 h(crosslinked fluid is epoxy chloropropane volumetric concentration is 1%, ethanol contend concentration is the aqueous solution of 70%), by film deionized water wash 5 times to remove unreacted Silver Nitrate, epoxy chloropropane, drying at room temperature, obtained soy protein isolate film.Then soy protein isolate film being immersed in concentration is in the silver nitrate solution of 2 ~ 50 mg/mL, soaks 0.5 ~ 5 h; Under the soy protein isolate film immersed with silver nitrate solution obtained is exposed to sunlight or simulated solar irradiation, illumination action time is 0.5 ~ 24 h; Take out and use deionized water wash 5 times, normal temperature dries, and obtains soybean protein isolate-nano silver antibacterial composite membrane.
Compared with prior art, the present invention has following features:
Soybean protein isolate, simultaneously as the reductive agent of Silver Nitrate and the stablizer of nanometer silver, without the need to other chemical reagent additional, pollutes few.
Required illumination condition can be sunlight or simulated solar illumination, is conveniently easy to get.
Reaction conditions is gentle, without the need to severe condition such as High Temperature High Pressure, and good energy-conserving effect.
Prepared nanometer silver particle diameter little (5-7 about nm), even particle size distribution.Little particle diameter has higher specific surface area, also just means higher anti-microbial activity and lower consumption.
Nanometer silver good stability, places and still can keep good dispersiveness, and can dissolve each other with plurality of reagents, therefore have Application Areas widely half a year.
Soybean protein isolate as mould material matrix, biocompatibility and biological degradability good.
Antibacterial high efficiency.Silver mass concentration be 1% material 2 h in sterilizing rate can reach more than 99.9%.
Broad-spectrum antibacterial property.Prepared anti-biotic material all shows excellent resistance for gram-positive microorganism and Gram-negative bacteria.
Embodiment
Below utilize embodiment to further describe the present invention, but can not think to limit scope of invention.
Embodiment 1: get soybean protein isolate solution 5 mL that mass concentration is 0.25%, dropwise drip sodium hydroxide under stirring and regulate its pH to 10, drip silver nitrate solution, obtain soybean protein isolate-Silver Nitrate mixed solution that silver nitrate concentration is 25 mmol/L, stirring 30 min makes Silver Nitrate fully mix with soybean protein isolate, this mixing solutions is exposed to illumination 2 h under sunlight.Obtain soybean protein isolate-nanometer silver mixed solution.Gained mixed solution being joined massfraction is in the soybean protein isolate solution of 6%, and the add-on controlling silver is 0.1% of soybean protein isolate consumption, stirs 10 min, makes it abundant mixing, then watered and cast from film forming container, at room temperature drying and forming-film.By obtained film 60
ounder C water bath condition, crosslinked 1 h(crosslinked fluid is epoxy chloropropane volumetric concentration is 1%, ethanol contend concentration is the aqueous solution of 70%), then 5 times will be washed in film deionized water to remove unreacted Silver Nitrate, epoxy chloropropane, room temperature is dried, and can obtain soybean protein isolate-nano silver antibacterial composite membrane.
Operate according to antibacterial experiment standard method, prepare E. coli suspension; Be inoculated into above-mentioned gained soybean protein isolate-nano silver antibacterial composite membrane surface, after acting on 2 h, bacterium liquid transferred in 25 mL PBS damping fluids together with antibacterial film, dilution, coated plate, 37
ocount after cultivating 24 h in C bio-incubator.Result shows, gained soybean protein isolate-nano silver antibacterial composite membrane contact can reach more than 80% to colibacillary sterilizing rate time antibacterial in 2 h.
Embodiment 2: get soybean protein isolate solution 5 mL that mass concentration is 0.5%, dropwise drip sodium hydroxide under stirring and regulate its pH to 10, drip silver nitrate solution, obtain soybean protein isolate-Silver Nitrate mixed solution that silver nitrate concentration is 25 mmol/L, stirring 30 min makes Silver Nitrate fully mix with soybean protein isolate, this mixing solutions is exposed to illumination 4 h under the incandescent light of 100 W.Gained mixed solution being joined massfraction is in the soybean protein isolate solution of 2%, and the add-on controlling silver is 1% of soybean protein isolate consumption, stirs 30 min, makes it abundant mixing, then watered and cast from film forming container, at room temperature drying and forming-film.By obtained film 60
ounder C water bath condition, crosslinked 1 h(crosslinked fluid is epoxy chloropropane volumetric concentration is 1%, ethanol contend concentration is the aqueous solution of 70%), then 5 times will be washed in film deionized water to remove unreacted Silver Nitrate, epoxy chloropropane, room temperature is dried, and can obtain soybean protein isolate-nano silver antibacterial composite membrane.
Operate according to antibacterial experiment standard method, prepare Staphylococcus aureus suspension; Be inoculated into above-mentioned gained soybean protein isolate-nano silver antibacterial composite membrane surface, after acting on 2 h, bacterium liquid transferred in 25 mL PBS damping fluids together with antibacterial film, dilution, coated plate, 37
ocount after cultivating 24 h in C bio-incubator.Result shows, gained soybean protein isolate-nano silver antibacterial composite membrane contact can reach 99.9% to the sterilizing rate of streptococcus aureus time antibacterial in 2 h.
Embodiment 3: get soybean protein isolate solution 10 mL that mass concentration is 4%, dropwise drip sodium hydroxide and regulate its pH to 11 under stirring, casts in one-tenth film container, at room temperature drying and forming-film by this soybean separation protein white water solution.Obtained film is 60
ounder C water bath condition, crosslinked 1 h(crosslinked fluid is epoxy chloropropane volumetric concentration is 1%, ethanol contend concentration is the aqueous solution of 70%), then by film deionized water wash 5 times with after removing unreacted epoxy chloropropane, dry under room temperature.Then this soy protein isolate film being immersed in concentration is leave standstill 2 h in the silver nitrate solution of 25 mg/mL, irradiates 12 h under subsequently whole reaction system being exposed to sunlight.Taken out, with deionized water wash 5 times with after removing unreacted Silver Nitrate, dry under room temperature, soybean protein isolate-nano silver antibacterial composite membrane can be obtained.
Operate according to antibacterial experiment standard method, preparation streptococcus aureus suspension; Be inoculated into above-mentioned gained soybean protein isolate-nano silver antibacterial composite membrane surface, after acting on 12 h, bacterium liquid transferred in 25 mL PBS damping fluids together with antibacterial film, dilution, coated plate, 37
ocount after cultivating 24 h in C bio-incubator.Result shows, gained soybean protein isolate-nano silver antibacterial composite membrane contact reaches 90% to the sterilizing rate of streptococcus aureus time antibacterial, can reach 99.9% in 12 h in 2 h.
Embodiment 4: get soybean protein isolate solution 8 mL that mass concentration is 6%, dropwise drip sodium hydroxide and regulate its pH to 12 under stirring, casts in one-tenth film container, at room temperature drying and forming-film by this soybean separation protein white water solution.Obtained film is 60
ounder C water bath condition, crosslinked 1 h(crosslinked fluid is epoxy chloropropane volumetric concentration is 1%, ethanol contend concentration is the aqueous solution of 70%), then by film deionized water wash 5 times with after removing unreacted epoxy chloropropane, dry under room temperature.Then this soy protein isolate film being immersed in concentration is leave standstill 4 h in the silver nitrate solution of 50 mg/mL, irradiates 24 h under subsequently whole reaction system being exposed to the incandescent light of 100 W.Taken out, with deionized water wash 5 times with after removing unreacted Silver Nitrate, dry under room temperature, soybean protein isolate-nano silver antibacterial composite membrane can be obtained.
Operate according to antibacterial experiment standard method, prepare E. coli suspension; Be inoculated into above-mentioned gained soybean protein isolate-nano silver antibacterial composite membrane surface, after acting on 2 h, bacterium liquid transferred in 25 mL PBS damping fluids together with antibacterial film, dilution, coated plate, 37
ocount after cultivating 24 h in C bio-incubator.Result shows, gained soybean protein isolate-nano silver antibacterial composite membrane contact can reach 99.9% to colibacillary sterilizing rate time antibacterial in 2 h.
Embodiment 5: get soybean protein isolate solution 5 mL that mass concentration is 2%, dropwise drip sodium hydroxide under stirring and regulate its pH to 10, drip silver nitrate solution, obtain soybean protein isolate-Silver Nitrate mixed solution that silver nitrate concentration is 25 mmol/L, stirring 30 min makes Silver Nitrate fully mix with soybean protein isolate, this mixing solutions is exposed to illumination 4 h under sunlight.Obtain soybean protein isolate-nanometer silver mixed solution.Gained mixed solution being joined massfraction is in the soybean protein isolate solution of 3%, and the add-on controlling silver is 0.1% of soybean protein isolate consumption, stirs 10 min, makes it abundant mixing, then watered and cast from film forming container, at room temperature drying and forming-film.By obtained film 60
ounder C water bath condition, crosslinked 1 h(crosslinked fluid is epoxy chloropropane volumetric concentration is 1%, ethanol contend concentration is the aqueous solution of 70%), then 5 times will be washed in film deionized water to remove unreacted Silver Nitrate, epoxy chloropropane, room temperature is dried, and can obtain soybean protein isolate-nano silver antibacterial composite membrane.
Operate according to antibacterial experiment standard method, preparation streptococcus aureus suspension; Soybean protein isolate-nano silver antibacterial composite membrane is dipped in 30 mL inoculums, after being placed in vibrator vibration (200 r/min) 2 h, dilution, coated plate, 37
ocount after cultivating 24 h in C bio-incubator.Result shows, gained soybean protein isolate-nano silver antibacterial composite membrane vibration can reach 99.9% to the sterilizing rate of streptococcus aureus time antibacterial in 2 h.
Embodiment 6: get soybean protein isolate solution 10 mL that mass concentration is 6%, dropwise drip sodium hydroxide under stirring and regulate its pH to 10, this soybean separation protein white water solution is cast in one-tenth film container, at room temperature drying and forming-film.Obtained film is 60
ounder C water bath condition, crosslinked 1 h(crosslinked fluid is epoxy chloropropane volumetric concentration is 1%, ethanol contend concentration is the aqueous solution of 70%), then by film deionized water wash 5 times with after removing unreacted epoxy chloropropane, dry under room temperature.Then this soy protein isolate film being immersed in concentration is leave standstill 5 h in the silver nitrate solution of 50 mg/mL, irradiates 12 h under subsequently whole reaction system being exposed to sunlight.Taken out, with deionized water wash 5 times with after removing unreacted Silver Nitrate, dry under room temperature, soybean protein isolate-nano silver antibacterial composite membrane can be obtained.
Operate according to antibacterial experiment standard method, preparation intestinal bacteria bacterium suspension; Soybean protein isolate-nano silver antibacterial composite membrane is dipped in 30 mL inoculums, after being placed in vibrator vibration (200 r/min) 2 h, dilution, coated plate, 37
ocount after cultivating 24 h in C bio-incubator.Result shows, gained soybean protein isolate-nano silver antibacterial composite membrane vibration can reach 99.9% to colibacillary sterilizing rate time antibacterial in 2 h.
Claims (3)
1. a preparation method for soybean protein isolate-nano silver antibacterial composite membrane, is divided into 2 kinds:
(1) soybean protein isolate in-situ reducing Silver Nitrate prepares nanometer silver, and prepares soybean protein isolate-nano silver antibacterial composite membrane further, and concrete steps are as follows:
(1) preparation quality concentration is the soybean separation protein white water solution of 0.25 ~ 6%, dropwise adds sodium hydroxide under stirring, regulator solution pH to 9 ~ 12;
(2) in step (1) gained solution, add Silver Nitrate under stirring, obtain the mixed solution that silver nitrate concentration is 2 ~ 50 mmol/L, continue stirring 25 ~ 40 min;
(3), under the mixing solutions that step (2) obtains being exposed to sunlight or simulated solar irradiation, illumination action time is 0.5 ~ 24 h, obtains uniform soybean protein isolate-nanometer silver mixing solutions;
(4) soybean protein isolate-nanometer silver mixing solutions that step (3) obtains being joined massfraction is in the soybean protein isolate solution of 1%-6%, the add-on controlling silver is 0.05% ~ 2% of soybean protein isolate consumption, is then prepared into soybean protein isolate-nano silver antibacterial composite membrane;
(2) prepare soy protein isolate film, and utilize soy protein isolate film in-situ reducing Silver Nitrate to prepare soybean protein isolate-nano silver antibacterial composite membrane, concrete steps are as follows:
(1) preparation quality concentration is the soybean separation protein white water solution of 0.25-6%, dropwise adds sodium hydrate regulator solution pH to 9-12, then prepare soy protein isolate film under stirring;
(2) soy protein isolate film that step (1) obtains being immersed in concentration is in the silver nitrate solution of 2 ~ 50 mg/mL, and soak time is 0.5 – 5 h;
(3), under the soy protein isolate film immersed with silver nitrate solution that step (2) obtains being exposed to sunlight or simulated solar irradiation, illumination action time is 0.5 ~ 24 h; With deionized water wash 4-6 time, room temperature is dried; Obtain soybean protein isolate-nano silver antibacterial composite membrane;
Wherein, soybean separation protein white water solution is obtained by following steps: be dissolved in the aqueous solution of 100 g Guanidinium hydrochlorides and 25 mg dithiothreitol (DTT) by 10 g soybean isolate protein powder ends, after dialysing 72 hours in the aqueous sodium hydroxide solution of pH=11, then with deionized water dialysis to close neutral; Adopt the insolubles of centrifugation 10 minutes removing minute quantities of 9000 r/min, obtain the soybean separation protein white water solution that mass concentration is about 2%, then obtain by concentrated or deionized water dilution the soybean separation protein white water solution that mass concentration is 0.25-6%.
2. soybean protein isolate-nano silver antibacterial composite membrane of obtaining of a preparation method as claimed in claim 1.
3. the application of soybean protein isolate-nano silver antibacterial composite membrane in food product pack and sanitary product as claimed in claim 2.
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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 |
| CN105755050B (en) * | 2016-05-06 | 2021-09-03 | 华中农业大学 | Method for biologically synthesizing nano silver by using illicium verum leaf extract |
| CN106279744B (en) * | 2016-09-22 | 2019-05-07 | 东北农业大学 | A kind of controlled release biocidal property eats the preparation method of composite membrane |
| 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 |
| CN114573846B (en) * | 2022-03-22 | 2024-01-09 | 哈尔滨学院 | Preparation method of soybean protein antibacterial biological film with high mechanical strength |
| WO2024069222A1 (en) * | 2022-10-01 | 2024-04-04 | Heidarisoureshjani Maryam | Clothing with soy fibers for butterfly patients |
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