CN102935521A - Method for preparing fibroin nano-silver hydrosol - Google Patents
Method for preparing fibroin nano-silver hydrosol Download PDFInfo
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- CN102935521A CN102935521A CN2012105222023A CN201210522202A CN102935521A CN 102935521 A CN102935521 A CN 102935521A CN 2012105222023 A CN2012105222023 A CN 2012105222023A CN 201210522202 A CN201210522202 A CN 201210522202A CN 102935521 A CN102935521 A CN 102935521A
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Abstract
The invention discloses a method for preparing fibroin nano-silver hydrosol. The method comprises the following steps of: dissolving or dispersing soluble amylose in deionized water, stirring the mixture until the amylose is completely gelatinized to obtain a starch solution, adding a silver nitrate solution, and then mixing the mixture with a fibroin solution to obtain a fibroin-starch-silver nitrate ternary complex solution; adjusting the pH value of the ternary complex solution to be at 8-10 by ammonia water, and fully mixing at the temperature condition of 20-80 DEG C to obtain the fibroin nano-silver hydrosol with the silver particle size being 1-100nm. According to the method, micromolecule fibroin peptide is used as a capturing agent and a reducing agent, the soluble starch is used as a dispersing agent and a protective agent, and the micromolecule fibroin peptide and the soluble starch are used for reducing and preparing nano-silver. The prepared nano-silver hydrosol is small in silver particle size, uniform in distribution and good in stability, in the prepared process, the reaction is mild, the operation is convenient, the green and environment-friendly aim is realized, and the fibroin nano-silver hydrosol can be widely used as a functional nano-material.
Description
Technical field
The present invention relates to a kind of preparation method of the fibroin Nano Silver hydrosol, belong to technical field of nano material.
Background technology
Nano Silver is that particle diameter is at nano level argent simple substance, nano silver material possesses special skin effect, small-size effect, quantum size effect and macro quanta tunnel effect, present many unusual physicochemical properties, especially obvious in aspect performance advantages such as electronics, optics, antibiotic and catalysis, be widely used in catalyst material, battery electrode material, low temperature Heat Conduction Material, electrocondution slurry, anti-biotic material and medical material, have a extensive future.
Usually the preparation method of Nano Silver is physical method and chemical method, the Nano Silver good dispersion of chemical method because making wherein, particle diameter is concentrated, pattern is evenly and by more use, but reducing agent (hydrazine hydrate, borohydride salts etc.) or stabilizing agent (polyvinylpyrrolidone, lauryl sodium sulfate, metaphosphate etc.) that its preparation process is introduced are all toxic even carcinogenic, and environmental and biological materials is had potential hazard.The standby Nano Silver of the biological reducing legal system of in recent years rising, because of raw material extensively, reaction temperature and, equipment requirement is low, product is stable and advantages of environment protection, advocated energetically, wherein adopt natural polymer reduction to prepare Nano Silver and caused extensive concern as a kind of method of environmental protection.
In the Chinese invention patent (CN102228995A) " a kind of polysaccharide-nano silver sol and preparation method thereof ", a kind of polysaccharide-nano silver sol and preparation method thereof is disclosed, be specifically related to a kind of preparation method of carboxymethyl chitosan quaternary ammonium salt-nano silver colloidal sol, method is first with AgNO
3Be converted into more active [Ag (NH
3)
2] OH, use again carboxymethyl chitosan quaternary ammonium salt as reducing agent and stabilizing agent, adopt microwave heating method aqueous phase under normal pressure to prepare carboxymethyl chitosan quaternary ammonium salt-nano silver colloidal sol, preparation process meets " Green Chemistry " theory.
China is the maximum production state of silk, all produces a large amount of useless silks every year, and silk weight 20～30% be sericin, be a kind of native protein resource of preciousness, it is directly discharged as refuse, has both caused environmental pollution, especially the huge wasting of resources.Therefore, utilize the series of products of silk-fibroin exploitation high-tech content, high added value, can not only take full advantage of the resources advantage of China, can also " turn waste into wealth ", bring considerable economic benefit.Sericin is as a kind of globular preteins, and is higher with the amino acid content of polar residues, and design feature has determined that it can have good complexing and reducing power to silver ion, can be used as reducing agent and prepares Nano Silver.
Starch is as a kind of polysaccharide reproducibility natural polymer, and wide material sources are cheap.Soluble starch mainly is amylose, be to contain the macromolecule that enriches hydroxyl by what a plurality of glucose units consisted of, can by in the molecule and intermolecular hydrogen bond action form " capsule " of molecular level, for the growth of metal nanoparticle provides template.
Summary of the invention
The object of the present invention is to provide a kind of fibroin Nano Silver hydrosol and preparation method thereof, the Nano Silver particle diameter that obtains is little, be evenly distributed, good stability, and the preparation process reaction temperature and, easy to operate, environmental protection.
Technical scheme of the present invention provides a kind of preparation method of the fibroin Nano Silver hydrosol, comprises the steps:
(1) solid nitric acid silver is dissolved or dispersed in the deionized water, obtains the liquor argenti nitratis ophthalmicus that concentration is 0.01～0.5mol/L;
(2) amylose with solubility is dissolved or dispersed in the deionized water, is stirred to complete gelatinization under 60～100 ℃ temperature conditions, obtains the starch solution that concentration is 0.1～5wt%;
(3) the solubility fibroin is dissolved or dispersed in the deionized water, being mixed with concentration is the fibroin solution of 0.5～5 wt%;
(4) with described starch solution and described liquor argenti nitratis ophthalmicus by volume 1:6～1:1 mix, obtain starch-silver nitrate binary composite solution;
(5) 1:2～10:1 mixes described fibroin solution with starch-silver nitrate binary solution by volume, obtains the tri compound solution of fibroin-starch-silver nitrate; The pH value of regulating tri compound solution with ammoniacal liquor is 8～10, stirs 5min～12h under 20～80 ℃ temperature conditions, and obtaining silver granuel directly is the fibroin sodium rice silver hydrosol of 1～100nm.
The amylose of described solubility comprises one or more in cornstarch, wheat kind of starch, tapioca, starch from sweet potato, sweet potato starch, farina, Lotus Root Starch, water caltrop starch and the Chinese Water Chestnut Starch.
The small-molecular weight silk-fibroin peptide that described solubility fibroin is molecular weight 1～5KDa comprises sericin peptide or fibroin albumen peptide; Its preparation method is: 1:50～1:10 mixes protease and silk protein solution in mass ratio, cessation reaction after under stirring condition, being hydrolyzed 30～120min, the solution that obtains is through the filtering with microporous membrane of 0.22～0.65 μ m, and obtaining molecular weight after concentrating filter liquor, the drying is the silk-fibroin peptide powder of 1～5KDa.Described protease is papain, neutral proteinase, trypsase, one or more in chymotrypsin, pepsin, subtilopeptidase A, the thermolysin.
The present invention with little molecule silk-fibroin peptide as agent for capturing and reducing agent; soluble starch is dispersant and protective agent; be used for reduction preparation Nano Silver; its principle is: silk gum is a kind of globular preteins; amino acid content with polar residues is higher; some α spirals that form it overstock in inside with the β-pleated sheet structure and the relative fine and close internal structure of formation more; then the distributing corner of regularity relative mistake of silk gum periphery; ring-type and " random " coiled structure; fibroin is higher because of its β-pleated sheet structural content; its compound with regular structure; degree of crystallinity is relatively high; the two design feature all makes the active group of its surface distributed relatively less; if it is not ideal enough to be directly used in its effect of reduction preparation Nano Silver; the large molecule of silk-fibroin is carried out suitable enzymolysis processing can obtain little molecule silk-fibroin peptide, at this moment active group (OH;-NH
2,-COOH etc.) come out in a large number, metal ion is demonstrated good complexing and reducing power; When starch with after sericin contacts, can be with the silk-fibroin Uniform Dispersion, the two is by forming " capsule " of numerous molecular levels with intermolecular hydrogen bond action in the molecule simultaneously, for the growth of nano-Ag particles provides good template, can realize Uniform Dispersion, complexing seizure and in-situ reducing to silver ion, thus the silk-fibroin Nano Silver hydrosol that obtains having good stability.
Compared with prior art, the invention has the beneficial effects as follows:
(1) the little molecule silk-fibroin peptide behind the employing enzymolysis is as agent for capturing and reducing agent, and the natural polysaccharide soluble starch serves as dispersant and protective agent, and reduction preparation Nano Silver possesses the advantages such as raw material is extensive, asepsis environment-protecting, meets the theory of " Green Chemistry ".
(2) utilize the molecular characterization of silk-fibroin and starch, by silver ion with simple mixing of protective agent, reducing agent can obtain the Nano Silver hydrosol, the preparation method is simply effective, easily realizes large-scale production.
(3) the Nano Silver hydrosol for preparing is uniformly dispersed and good stability, can be used as functional nanomaterials and is widely used.
Description of drawings
The uv-visible absorption spectra figure (UV-Vis figure) of the fibroin Nano Silver hydrosol that Fig. 1 provides for the embodiment of the invention;
The fibroin Nano Silver hydrosol that Fig. 2 provides for the embodiment of the invention is through the observable Nano Silver form of transmission electron microscope (TEM) grain-size graph;
Fig. 3 records wherein Nano Silver particle diameter distribution results figure for the fibroin Nano Silver hydrosol that the embodiment of the invention provides through laser particle instrument (DLS).
The specific embodiment
Below in conjunction with embodiment technical solution of the present invention is described in detail.
Embodiment 1:
Get the 0.2g cornstarch and be scattered in the 10ml deionized water, be stirred to gelatinization under 80 ℃ to get corn starch solution, it is added in the liquor argenti nitratis ophthalmicus that 10ml concentration is 0.05mol/L, mix and obtain starch-silver nitrate binary composite solution.
1:20 mixes papain with sericin solution in mass ratio, regulate pH value and temperature to the active optimum condition of corresponding protein enzyme, cessation reaction behind the hydrolysis 40min under stirring condition, the solution that obtains is through the filtering with microporous membrane of 0.22～0.65 μ m, and obtaining molecular weight after concentrating filter liquor, the drying is the sericin peptide powder of 1～5KDa.
Getting the little molecule sericin of 2.4g peptide powder is dissolved in the 120ml deionized water, obtaining concentration is the sericin peptide solution of 2 wt %, it is added in above-mentioned starch-silver nitrate composite solution, mix to get the tri compound solution of sericin peptide-starch-silver nitrate, regulator solution pH value to 9.0, be to stir 240min under 60 ℃ the condition in temperature, obtain particle diameter at the Nano Silver hydrosol of 5～30nm.
Embodiment 2:
Get the 0.15g tapioca and be scattered in the 5ml deionized water, be stirred to gelatinization under 90 ℃ to get tapioca solution, it is added in the liquor argenti nitratis ophthalmicus that 20ml concentration is 0.2mol/L, mix and obtain starch-silver nitrate binary composite solution.
The little molecule fibroin albumen peptide powder of getting the 3g molecular weight and be 1～5KDa is dissolved in the 100ml deionized water, obtaining concentration is the fibroin albumen peptide solution of 3wt %, it is added in above-mentioned starch-silver nitrate composite solution, mix to get the tri compound solution of fibroin albumen peptide-starch-silver nitrate, regulator solution pH value to 9.2,70 ℃ of lower 180min that stir obtain particle diameter at the Nano Silver hydrosol of 3～25nm.
Referring to accompanying drawing 1, it is the uv-visible absorption spectra figure (UV-Vis figure) of the resulting fibroin Nano Silver of the present embodiment hydrosol, as seen from Figure 1, typical Nano Silver characteristic absorption peak occurred at the 408nm place, proved to have generated the spherical nano-silver particle in the product water colloidal sol.
Referring to accompanying drawing 2, it be the resulting fibroin Nano Silver of the present embodiment hydrosol through the observable Nano Silver form of transmission electron microscope (TEM) grain-size graph, Fig. 2 shows that Nano Silver is spheric granules in the gained hydrosol.
Referring to accompanying drawing 3, it records wherein Nano Silver particle diameter distribution results figure for the resulting fibroin Nano Silver of the present embodiment hydrosol through laser particle instrument (DLS); Nano Silver particle diameter shown in Figure 3 is at 3～25nm.
Embodiment 3:
Get the 0.1g wheaten starch and be scattered in the 10ml deionized water, be stirred to gelatinization under 90 ℃ to get wheat starch solution, it is added in the liquor argenti nitratis ophthalmicus that 20ml concentration is 0.1mol/L, mix and obtain starch-silver nitrate binary composite solution.Getting the 1.2g molecular weight is that the little molecule sericin peptide of 1～5KDa and the composite powder of little molecule fibroin albumen peptide are dissolved in the preparation 60ml deionized water, obtaining concentration is the silk-fibroin peptide solution of 2 wt %, it is added in above-mentioned starch-silver nitrate composite solution, mix to get the tri compound solution of silk-fibroin peptide-starch-silver nitrate, regulator solution pH value to 9.5,80 ℃ of lower 120min that stir obtain particle diameter at the Nano Silver hydrosol of 2～20nm.
Claims (5)
1. the preparation method of a fibroin Nano Silver hydrosol is characterized in that comprising the steps:
(1) solid nitric acid silver is dissolved or dispersed in the deionized water, obtains the liquor argenti nitratis ophthalmicus that concentration is 0.01～0.5mol/L;
(2) amylose with solubility is dissolved or dispersed in the deionized water, is stirred to complete gelatinization under 60～100 ℃ temperature conditions, obtains the starch solution that concentration is 0.1～5wt%;
(3) the solubility fibroin is dissolved or dispersed in the deionized water, being mixed with concentration is the fibroin solution of 0.5～5 wt%;
(4) with described starch solution and described liquor argenti nitratis ophthalmicus by volume 1:6～1:1 mix, obtain starch-silver nitrate binary composite solution;
(5) 1:2～10:1 mixes described fibroin solution with starch-silver nitrate binary solution by volume, obtains the tri compound solution of fibroin-starch-silver nitrate; The pH value of regulating tri compound solution with ammoniacal liquor is 8～10, stirs 5min～12h under 20～80 ℃ temperature conditions, and obtaining silver granuel directly is the fibroin sodium rice silver hydrosol of 1～100nm.
2. the preparation method of a kind of fibroin Nano Silver hydrosol according to claim 1, it is characterized in that: the amylose of described solubility comprises one or more in cornstarch, wheat kind of starch, tapioca, starch from sweet potato, sweet potato starch, farina, Lotus Root Starch, water caltrop starch and the Chinese Water Chestnut Starch.
3. the preparation method of a kind of fibroin Nano Silver hydrosol according to claim 1, it is characterized in that: the small-molecular weight silk-fibroin peptide that described solubility fibroin is molecular weight 1～5KDa comprises sericin peptide or fibroin albumen peptide.
4. the preparation method of a kind of fibroin Nano Silver hydrosol according to claim 3, it is characterized in that: the preparation method of described small-molecular weight silk-fibroin peptide, 1:50～1:10 mixes protease and silk protein solution in mass ratio, cessation reaction after under stirring condition, being hydrolyzed 30～120min, the solution that obtains is through the filtering with microporous membrane of 0.22～0.65 μ m, and obtaining molecular weight after concentrating filter liquor, the drying is the silk-fibroin peptide powder of 1～5KDa.
5. the preparation method of a kind of fibroin Nano Silver hydrosol according to claim 5, it is characterized in that: described protease is papain, neutral proteinase, trypsase, one or more in chymotrypsin, pepsin, subtilopeptidase A, the thermolysin.
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| CN103203469A (en) * | 2013-04-28 | 2013-07-17 | 黑龙江大学 | Preparation method of Ag-Ag2O hetero-structure silver material |
| CN103406548A (en) * | 2013-08-08 | 2013-11-27 | 广西大学 | Silver nano particle and preparation method and application thereof |
| CN103495738A (en) * | 2013-09-24 | 2014-01-08 | 东华大学 | Water-soluble nano silver preparation method based on waste keratin degradation products |
| CN104498534A (en) * | 2015-01-07 | 2015-04-08 | 广西大学 | Application of silver nanoparticles in controlling major contaminating bacteria in fuel ethanol fermentation production process |
| CN104551010A (en) * | 2015-01-19 | 2015-04-29 | 青岛农业大学 | Method for preparing water-soluble nano-silver by using short amylose as template |
| CN104817706A (en) * | 2015-03-12 | 2015-08-05 | 浙江海洋学院 | Preparation method for Setipinna tenuifilis protein nano-silver antibacterial film |
| CN105435300A (en) * | 2015-12-25 | 2016-03-30 | 重庆理工大学 | Nano-silk-fibroin-containing antibacterial medical dressing |
| CN106238748A (en) * | 2016-08-31 | 2016-12-21 | 华南理工大学 | The synthetic method of ball shaped nano Argent grain and ball shaped nano Argent grain |
| CN106751920A (en) * | 2016-12-01 | 2017-05-31 | 西南大学 | Preparation method of the enhanced laminated film anti-biotic material of polyvinyl alcohol silk gum Nano Silver and products thereof and application |
| CN107186224A (en) * | 2017-06-20 | 2017-09-22 | 北印（青岛）研究院有限公司 | A kind of method that enzyme decomposition technique prepares nano-silver powder |
| CN107498067A (en) * | 2017-09-21 | 2017-12-22 | 厦门医学院 | The quick method for preparing nano silver colloidal sol of Bao internal organ degradation product green |
| CN109794616A (en) * | 2019-01-15 | 2019-05-24 | 南通纺织丝绸产业技术研究院 | The preparation of the silver nanoclusters of sericin package and fluorescence probe |
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| CN113647409A (en) * | 2021-08-11 | 2021-11-16 | 武汉纺织大学 | Silver-loaded silk fibroin nanoparticle antibacterial agent, preparation method and application |
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| CN103203469A (en) * | 2013-04-28 | 2013-07-17 | 黑龙江大学 | Preparation method of Ag-Ag2O hetero-structure silver material |
| CN103406548A (en) * | 2013-08-08 | 2013-11-27 | 广西大学 | Silver nano particle and preparation method and application thereof |
| CN103406548B (en) * | 2013-08-08 | 2015-11-18 | 广西大学 | Nano silver grain and preparation method thereof and application |
| CN103495738A (en) * | 2013-09-24 | 2014-01-08 | 东华大学 | Water-soluble nano silver preparation method based on waste keratin degradation products |
| CN103495738B (en) * | 2013-09-24 | 2015-11-18 | 东华大学 | A kind of preparation method of the water-soluble nano silver based on discarded keratin degrading thing |
| CN104498534A (en) * | 2015-01-07 | 2015-04-08 | 广西大学 | Application of silver nanoparticles in controlling major contaminating bacteria in fuel ethanol fermentation production process |
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| CN106751920A (en) * | 2016-12-01 | 2017-05-31 | 西南大学 | Preparation method of the enhanced laminated film anti-biotic material of polyvinyl alcohol silk gum Nano Silver and products thereof and application |
| CN106751920B (en) * | 2016-12-01 | 2019-07-09 | 西南大学 | Preparation method of the enhanced laminated film anti-biotic material of polyvinyl alcohol-silk gum-nano silver and products thereof and application |
| CN107186224A (en) * | 2017-06-20 | 2017-09-22 | 北印（青岛）研究院有限公司 | A kind of method that enzyme decomposition technique prepares nano-silver powder |
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| CN107498067A (en) * | 2017-09-21 | 2017-12-22 | 厦门医学院 | The quick method for preparing nano silver colloidal sol of Bao internal organ degradation product green |
| CN109794616A (en) * | 2019-01-15 | 2019-05-24 | 南通纺织丝绸产业技术研究院 | The preparation of the silver nanoclusters of sericin package and fluorescence probe |
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| CN113647409A (en) * | 2021-08-11 | 2021-11-16 | 武汉纺织大学 | Silver-loaded silk fibroin nanoparticle antibacterial agent, preparation method and application |
| CN113647409B (en) * | 2021-08-11 | 2023-03-07 | 武汉纺织大学 | Silver-loaded silk fibroin nanoparticle antibacterial agent, preparation method and application |
| CN115305262A (en) * | 2022-07-25 | 2022-11-08 | 集美大学 | Preparation method and application of abalone viscera zymolyte nano-silver |
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