CN104923805A - Micro-nano-silver base material preparation method and micro-nano-silver base material thereof - Google Patents
Micro-nano-silver base material preparation method and micro-nano-silver base material thereof Download PDFInfo
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Abstract
The invention discloses a micro-nano-silver base material preparation method and a micro-nano-silver base material thereof. Extracting solutions of naturally-green green tea and pu'er tea are used as a reducing agent and a stabilizing agent for silver nanoparticles, the operation is simple and fast, the preparation process has the advantages of being green and environmentally friendly and fast and high-efficient, the average grain diameter of the prepared silver nanoparticles is 30 nm, the particle morphology is uniform, and the dispersity is good. The silver nanoparticles synthetized by the micro-nano-silver base material preparation method has good application prospect in the fields of biology, pharmacy, catalysis and the like.
Description
Technical field
The present invention relates to Material Field, be specifically related to a kind of preparation method and micro-nano silver sill thereof of micro-nano silver sill.
Background technology
In various metallic, the silver particles of micron and nano-scale has been subject to the concern of people since coming out always deeply, this is not only because it has unique characteristic such as electronics, optics, catalysis, and has good antibiotic property, bio-compatibility and surface and the many merits such as easily to modify.Micro-nano silver particle has been widely used in the aspects such as photomechanical production, bio-medical material, chemical catalyst, ceramic material, electrocondution slurry, sewage disposal, construction material, lubricant, light absorbing material, coating, sensor and high performance electrode material.
For adapting to different demands, people explore the new method preparing micro-nano silver particle all the time in recent years.Due to many restrictions of Silver Nanoparticles itself, such as synthesize high, the poor stability of cost etc., micro nanometer silver particle then with its excellent combination property, good stability, low cost, the simple advantage such as synthesis technique and the easy recycling use of product, becomes study hotspot in recent years gradually.At present, the method preparing spherical micron Argent grain mainly contains silver salt decomposition method, electrolysis heat, evaporation and chemical liquid phase reducing process etc.
Chemical method is the preparation method of Nano silver grain the most frequently used at present, more reducing agent is used to have sodium borohydride, hydrazine hydrate, dimethyl formamide etc., but these toxicity of compound are strong, seriously polluted, serious harm is all existed to human body and environment, therefore, " greenization " of nano material preparation process just seems particularly important, and replace traditional, poisonous organic compound with the green solvent of safety, environmental protection, nontoxic reducing agent and macromolecule stabilizer, just become the important research direction of Green Chemistry.
Summary of the invention
For solving the problem, the invention provides a kind of preparation method and micro-nano silver sill thereof of micro-nano silver sill, with low cost, preparation process is fast, productive rate is high, environmental protection and energy saving.
For achieving the above object, the technical scheme that the present invention takes is:
A preparation method for micro-nano silver sill, comprises the steps:
S1, the green tea 55 ~ 65g taking cleaned drying, Pu'er tea 60 ~ 70g are placed in steam-explosion jar, and first passing into pressure in nitrogen to steam-explosion jar is 0.7 ~ 1.3MPa, explosion treatment 8 ~ 25min; Then passing into rapidly pressure in steam to steam-explosion jar is 1.3 ~ 1.7MPa, Steam explosion treatment 0.5 ~ 2.5min, filters, obtains leaching liquor;
S2, select China fir wood chip through acid-base pretreatment as column chromatography filler, leaching liquor is adsorbed, then carries out wash-out with pure water, collect the eluent of different component, after mixing, be spray dried to powder, obtain Tea Polyphenols powder;
S2, take 4 ~ 6.08g silver nitrate and be dissolved in 1000ml deionized water, lucifuge stirs, and obtains liquor argenti nitratis ophthalmicus;
S3, slowly to be added by the liquor argenti nitratis ophthalmicus of step S2 gained in the Tea Polyphenols powder that is under stirring, after interpolation, mixed liquor is heated to 35 ~ 45 DEG C, isothermal reaction 2h, obtains crude product:
S4, by the crude product of gained after centrifuge is separated, collecting precipitation product, adds turpentine derivatives and carries out ultrasonic cleaning in precipitated product, and centrifugation collecting precipitation product after cleaning, obtain finished product.
Wherein, described turpentine derivatives is isomery, the disproportionation products of firpene.
Wherein, in described step S4, the rotating speed of centrifuge is 5300r/min.
A kind of preparation method as above-mentioned micro-nano silver sill and the micro-nano silver sill for preparing.
The present invention has following beneficial effect:
Adopt the green tea of natural green and Pu'er tea extract as the reducing agent of Nano silver grain and stabilizing agent, simple and quick, preparation process has the advantage such as environmental protection, convenient and efficient, and the average grain diameter of prepared Nano silver grain is 30nm, granule-morphology is homogeneous, favorable dispersibility; The silver nano-grain of this method synthesis has applications well prospect in fields such as biology, pharmacy, catalysis.
Detailed description of the invention
In order to make objects and advantages of the present invention clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
The isomery that the turpentine derivatives used in following examples is firpene, disproportionation products, in step S4, the rotating speed of centrifuge is 5300r/min.
Embodiment 1
S1, the green tea 55g taking cleaned drying, Pu'er tea 60g are placed in steam-explosion jar, and first passing into pressure in nitrogen to steam-explosion jar is 0.7MPa, explosion treatment 8min; Then passing into rapidly pressure in steam to steam-explosion jar is 1.3MPa, Steam explosion treatment 0.5min, filters, obtains leaching liquor;
S2, select China fir wood chip through acid-base pretreatment as column chromatography filler, leaching liquor is adsorbed, then carries out wash-out with pure water, collect the eluent of different component, after mixing, be spray dried to powder, obtain Tea Polyphenols powder;
S2, take 4g silver nitrate and be dissolved in 1000ml deionized water, lucifuge stirs, and obtains liquor argenti nitratis ophthalmicus;
S3, slowly to be added by the liquor argenti nitratis ophthalmicus of step S2 gained in the Tea Polyphenols powder that is under stirring, after interpolation, mixed liquor is heated to 35 DEG C, isothermal reaction 2h, obtains crude product:
S4, by the crude product of gained after centrifuge is separated, collecting precipitation product, adds turpentine derivatives and carries out ultrasonic cleaning in precipitated product, and centrifugation collecting precipitation product after cleaning, obtain finished product.
Embodiment 2
S1, the green tea 65g taking cleaned drying, Pu'er bitter edible plant 70g are placed in steam-explosion jar, and first passing into pressure in nitrogen to steam-explosion jar is 1.3MPa, explosion treatment 25min; Then passing into rapidly pressure in steam to steam-explosion jar is 1.7MPa, Steam explosion treatment 2.5min, filters, obtains leaching liquor;
S2, select China fir wood chip through acid-base pretreatment as column chromatography filler, leaching liquor is adsorbed, then carries out wash-out with pure water, collect the eluent of different component, after mixing, be spray dried to powder, obtain Tea Polyphenols powder;
S2, take 6.08g silver nitrate and be dissolved in 1000ml deionized water, lucifuge stirs, and obtains liquor argenti nitratis ophthalmicus;
S3, slowly to be added by the liquor argenti nitratis ophthalmicus of step S2 gained in the bitter edible plant polyphenol powder that is under stirring, after interpolation, mixed liquor is heated to 45 DEG C, isothermal reaction 2h, obtains crude product:
S4, by the crude product of gained after centrifuge is separated, collecting precipitation product, adds turpentine derivatives and carries out ultrasonic cleaning in precipitated product, and centrifugation collecting precipitation product after cleaning, obtain finished product.
Embodiment 3
S1, the green tea 60g taking cleaned drying, Pu'er tea 65g are placed in steam-explosion jar, and first passing into pressure in nitrogen to steam-explosion jar is 1MPa, explosion treatment 17min; Then passing into rapidly pressure in steam to steam-explosion jar is 1.5MPa, Steam explosion treatment 1.5min, filters, obtains leaching liquor;
S2, select China fir wood chip through acid-base pretreatment as column chromatography filler, leaching liquor is adsorbed, then carries out wash-out with pure water, collect the eluent of different component, after mixing, be spray dried to powder, obtain Tea Polyphenols powder;
S2, take 5.04g silver nitrate and be dissolved in 1000ml deionized water, lucifuge stirs, and obtains liquor argenti nitratis ophthalmicus;
S3, slowly to be added by the liquor argenti nitratis ophthalmicus of step S2 gained in the Tea Polyphenols powder that is under stirring, after interpolation, mixed liquor is heated to 40 DEG C, isothermal reaction 2h, obtains crude product:
S4, by the crude product of gained after centrifuge is separated, collecting precipitation product, adds turpentine derivatives and carries out ultrasonic cleaning in precipitated product, and centrifugation collecting precipitation product after cleaning, obtain finished product
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (4)
1. a preparation method for micro-nano silver sill, is characterized in that, comprises the steps:
S1, the green tea 55 ~ 65g taking cleaned drying, Pu'er tea 60 ~ 70g are placed in steam-explosion jar, and first passing into pressure in nitrogen to steam-explosion jar is 0.7 ~ 1.3MPa, explosion treatment 8 ~ 25min; Then passing into rapidly pressure in steam to steam-explosion jar is 1.3 ~ 1.7MPa, Steam explosion treatment 0.5 ~ 2.5min, filters, obtains leaching liquor;
S2, select China fir wood chip through acid-base pretreatment as column chromatography filler, leaching liquor is adsorbed, then carries out wash-out with pure water, collect the eluent of different component, after mixing, be spray dried to powder, obtain Tea Polyphenols powder;
S2, take 4 ~ 6.08g silver nitrate and be dissolved in 1000ml deionized water, lucifuge stirs, and obtains liquor argenti nitratis ophthalmicus;
S3, slowly to be added by the liquor argenti nitratis ophthalmicus of step S2 gained in the Tea Polyphenols powder that is under stirring, after interpolation, mixed liquor is heated to 35 ~ 45 DEG C, isothermal reaction 2h, obtains crude product:
S4, by the crude product of gained after centrifuge is separated, collecting precipitation product, adds turpentine derivatives and carries out ultrasonic cleaning in precipitated product, and centrifugation collecting precipitation product after cleaning, obtain finished product.
2. the preparation method of a kind of micro-nano silver sill according to claim 1, is characterized in that, described turpentine derivatives is isomery, the disproportionation products of firpene.
3. the preparation method of a kind of micro-nano silver sill according to claim 1, is characterized in that, in described step S4, the rotating speed of centrifuge is 5300r/min.
4. the preparation method based on the micro-nano silver sill described in any one of claims 1 to 3 and the micro-nano silver sill prepared.
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Cited By (7)
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|---|---|---|---|---|
| CN105458283A (en) * | 2015-11-24 | 2016-04-06 | 太原理工大学 | Method for green synthesis of nanometer zero-valent iron-copper bi-metal material and application |
| CN105665737A (en) * | 2016-01-27 | 2016-06-15 | 陕西科技大学 | Biosynthesis method of nano Ag |
| CN106945489A (en) * | 2017-03-05 | 2017-07-14 | 华南理工大学 | A kind of vehicular air purifier using Nano Silver tealeaf residue biological carbon as main filtrate |
| CN108161024A (en) * | 2018-01-24 | 2018-06-15 | 东北大学 | A kind of preparation method of the micro-nano metallic copper of threadiness |
| CN109909513A (en) * | 2019-04-26 | 2019-06-21 | 中国科学院西双版纳热带植物园 | A kind of method and purposes with comospore Glochidion puberum biosynthesis nano silver particles |
| US10500645B1 (en) | 2019-01-07 | 2019-12-10 | King Saud University | Method of synthesizing silver nanoparticles using mint extract |
| CN113084182A (en) * | 2021-03-04 | 2021-07-09 | 福建农林大学 | Method for preparing nano-silver by using tea leaching solution as raw material |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105458283A (en) * | 2015-11-24 | 2016-04-06 | 太原理工大学 | Method for green synthesis of nanometer zero-valent iron-copper bi-metal material and application |
| CN105458283B (en) * | 2015-11-24 | 2018-02-16 | 太原理工大学 | A kind of method and purposes of green syt nano zero-valence iron-copper bi-metal material |
| CN105665737A (en) * | 2016-01-27 | 2016-06-15 | 陕西科技大学 | Biosynthesis method of nano Ag |
| CN106945489A (en) * | 2017-03-05 | 2017-07-14 | 华南理工大学 | A kind of vehicular air purifier using Nano Silver tealeaf residue biological carbon as main filtrate |
| CN108161024A (en) * | 2018-01-24 | 2018-06-15 | 东北大学 | A kind of preparation method of the micro-nano metallic copper of threadiness |
| US10500645B1 (en) | 2019-01-07 | 2019-12-10 | King Saud University | Method of synthesizing silver nanoparticles using mint extract |
| CN109909513A (en) * | 2019-04-26 | 2019-06-21 | 中国科学院西双版纳热带植物园 | A kind of method and purposes with comospore Glochidion puberum biosynthesis nano silver particles |
| CN109909513B (en) * | 2019-04-26 | 2022-03-04 | 中国科学院西双版纳热带植物园 | Method for biologically synthesizing nano silver particles by using glochidion pubescens and application |
| CN113084182A (en) * | 2021-03-04 | 2021-07-09 | 福建农林大学 | Method for preparing nano-silver by using tea leaching solution as raw material |
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Application publication date: 20150923 |