CN103706803A - Method for using grapefruit juice to restore silver ions in silver nitrate solution - Google Patents
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- CN103706803A CN103706803A CN201310496515.0A CN201310496515A CN103706803A CN 103706803 A CN103706803 A CN 103706803A CN 201310496515 A CN201310496515 A CN 201310496515A CN 103706803 A CN103706803 A CN 103706803A
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Abstract
The invention discloses a method for using grapefruit juice to restore silver ions in silver nitrate solution. The method includes: well mixing about 20mL of freshly squeezed grapefruit juice with about 20mL of 0.01-0.1mol/L silver nitrate solution under the constant-temperature water bath at about 30 DEG C, allowing the two to react in a 50mL small beaker, standing the reaction liquid for 48 hours, using a high-speed centrifuge to separate sedimentation, washing the sedimentation with anhydrous ethanol, and centrifuging the washed sedimentation with the high-speed centrifuge to obtain the products.
Description
Technical field
The invention belongs to nano-Ag particles and manufacture field, relate in particular to a kind of method of utilizing grape fruit juice to restore the silver ion in liquor argenti nitratis ophthalmicus.
Background technology
Along with developing rapidly of nano material, the application of nano material is also more and more extensive, as at nano paint, and CNT, Nano semiconductor, catalysis material, and at aspects such as medicine, household electrical appliances, weaving, environmental protection.And in recent years, the research aspect Nano Silver has obtained abundant achievement especially.No matter be that Nano Silver is undoubtedly one of a kind of research material the most extensively and profoundly from preparation, character or application.Nano silver material is except possessing the characteristic of general nano material, aspect optical material, the significant surface plasmon resonance effect of nano-Ag particles, this effect can strengthen the electromagnetic field of nano-Ag particles inside and peripheral region thereof, can be used for developing photon crystal material, as Nano Silver semiconductor.Meanwhile, because nano-Ag particles has very strong fluorescence emitting characteristics, can be used for the exploitation of biological detection, mark and biological and chemical sensor etc.; Aspect macroscopic property, demonstrate dimensional effect and form effect.Along with the combination energy that reduces nano silver material of nano silver material size, melt enthalpy and corresponding standard thermodynamic functions as
with
all reduce, and K
Θincrease etc.Nano silver material macroscopic property all has certain otherness with block ag material in every respect, and the macroscopic property of therefore studying nano silver material has extremely important scientific meaning and using value.
Traditional preparation method of Nano Silver mainly comprises the integrated approach of Physical, chemical method and physical chemistry combination.The method of preparing the earliest Nano Silver is Physical, and the purity of Nano Silver prepared by the method is higher, but yields poorly, fund input is large, energy consumption is large.Main preparation methods has high-energy mechanical ball milling method, luminescence method, radiation method, arc process, using vaporization condensation process etc.Xu J, Yin J S etc. carries out high-energy mechanical ball milling to silver powder under the ultralow temperature of-196 ℃, obtained the nano-Ag particles that average grain diameter is about 20nm; Du Yong etc. are placed on argent under the Nd:YAG laser instrument of wavelength 1064nm, prepare the Ag colloid particle of 5-20nm by the controlled light time.The stability of prepared silver colloid is fine, places and does not also occur coagulation thing several weeks; It is to utilize ionising radiation that radiation method is prepared nano material, is generally that the γ high-energy ray that utilizes co-60 radiation source to produce makes water generates ionization and excites, and generates reproducibility particle H free radical and aqueous electron and oxidisability particle OH free radical.Utilizing these reproducibility particles can be progressively nano-Ag particles silver ion reduction.The people such as Cui Guoshi adopt gamma Rays liquid-phase reduction to prepare nano silver colloidal sol.The nano silver colloidal sol of be conducive to obtain average grain diameter less (10-30nm) at lower absorbed dose of radiation, higher polyvinyl alcohol concentration (7.5%), lower silver nitrate concentration (0.01mol/L) and suitable isopropyl alcohol concentration (0.5mol/L), singly disperse, nothing being assembled; Silver powder prepared by the DC arc plasma evaporation equipment that the employings such as Duan Zhiwei are developed is voluntarily pure pollution-free, belongs to polymorphic structure, is ball chain form.Average grain diameter is within the scope of 38-220nm.Narrow diameter distribution.Maximum yield has improved nearly 17 times than similar result of study.
The Wei Zhi employing anodic arc discharging plasma evaporation condensation method such as by force prepares silver nanoparticle powder, under optimum process condition: silver nanoparticle powder diameter prepared by thermal power 3kw, air pressure 0.3-2kPa, Ar atmosphere, arc voltage 20-30V, arc current 70-150A, water-cooled is in 20nm left and right and purity is high, good dispersion.
In the face of physical-chemical process, prepare the various drawbacks that nano-Ag particles exists, add low-carbon (LC) and environmental protection life that society is pursued.Nano-Ag particles is prepared in green reduction becomes the direction that people pursue.
Summary of the invention
The object of the invention is to propose a kind of method of utilizing grape fruit juice to restore the silver ion in liquor argenti nitratis ophthalmicus.
The present invention adopts following technical scheme to achieve these goals:
Utilize grape fruit juice to restore a method for the silver ion in liquor argenti nitratis ophthalmicus, it is characterized in that, comprise the following steps:
(1) get fresh grape fruit, peeling, gets 30g left and right grape fruit fruit grain and adds after the distilled water squeezing of 60g left and right, with Buchner funnel suction filtration, obtain juice, and making supernatant with centrifuge low-speed centrifugal, gained supernatant is existing squeezing grape fruit juice, is all placed on sealing in beaker and saves backup;
(2) in the water bath with thermostatic control of 30 ℃ of left and right, get about 20mL and now squeeze after grape fruit juice mixes with the liquor argenti nitratis ophthalmicus of the 0.01-0.1mol/L of 20mL left and right and react in the small beaker of 50mL, above-mentioned reactant liquor was placed after 48 hours, with supercentrifuge, isolate precipitation, then with after absolute ethanol washing precipitation and through the centrifugal product that obtains of supercentrifuge.
A kind of described method of utilizing grape fruit juice to restore the silver ion in liquor argenti nitratis ophthalmicus, is characterized in that, comprises the following steps:
(1) get fresh grape fruit, peeling, gets 30g grape fruit fruit grain and adds after the squeezing of 60g distilled water, with Buchner funnel suction filtration, obtain juice, and making supernatant with centrifuge low-speed centrifugal, gained supernatant is existing squeezing grape fruit juice, is all placed on sealing in beaker and saves backup;
(2) in the water bath with thermostatic control of 30 ℃, getting 20mL now squeezes after grape fruit juice mixes with the liquor argenti nitratis ophthalmicus of the 0.01-0.1mol/L of 20mL and reacts in the small beaker of 50mL, above-mentioned reactant liquor was placed after 48 hours, with supercentrifuge, isolate precipitation, then with after absolute ethanol washing precipitation and through the centrifugal product that obtains of supercentrifuge.
Silver nano-grain forms the discussion of mechanism:
In grape fruit juice, mainly contain carrotene, B family vitamin, vitamin C, the biomolecule such as carbohydrate, volatile oil, protein, glutamic acid (Glu), aspartic acid (Asp), lysine (Lys), arginine (Arg), threonine (Thr) and organic acid etc.Because the biomolecule such as vitamin C and partial amino-acid have reproducibility, can be simple substance silver by monovalence silver ion reduction.The silver atoms generating is in forming the process that nucleus and nucleus constantly grow up, be subject to absorption and the package action of biomolecule in grape fruit juice, reduced surperficial energy, limited thereby crystal grain continues to grow up, the final spherical granule of class that is of a size of 50-100 nanometer that forms.
Beneficial effect of the present invention:
(1) the present invention restores the silver ion in liquor argenti nitratis ophthalmicus with the grape fruit juice of fresh squeezing, and easy and simple to handle, step is simple, and not only environmental protection but also safety and the Nano Silver that obtains had good stability.Raw material easily obtains and nonhazardous, has a good application prospect.
(2) utilize the reproducibility organic-biological molecule containing in grape fruit juice, can under temperate condition (30 ℃, normal pressure), restore the monovalence silver ion in liquor argenti nitratis ophthalmicus; Product is shown through multiple analytical test, and obtain the simple substance silver of the centroid cubic crystal system of class spherical morphology, particle diameter is between 50-100nm; The organic reducing biomolecule containing in grape fruit juice plays the effect of template and reducing agent to the generation of nano-Ag particles, the generation of induction and regulation and control Nano silver grain.
Accompanying drawing explanation
Fig. 1 is the infrared spectrogram of the grape fruit juice of embodiment 1;
Fig. 2 is the ultraviolet-visible spectrogram of the grape fruit juice of embodiment 1;
Fig. 3 is the ultraviolet-visible spectrogram of the reactant liquor of embodiment 1;
Fig. 4 is the scanning electron microscope (SEM) photograph of the product of the present invention of embodiment 1;
Fig. 5 is the x-ray diffraction pattern of the product of the present invention of embodiment 1.
The specific embodiment
1 experiment reagent and instrument
Reagent: silver nitrate, absolute ethyl alcohol, iodine, KI, is more than analysis pure; Redistilled water; Test fruit grape fruit used and be purchased from local fruit shop;
Instrument: U.S. Nicolet870 type Fourier transformation infrared spectrometer, solid K Br compressing tablet (sweep limits: 4000 ~ 400cm
-1, scan resolution ratio 4cm 32 times
-1);
TU-1901 dual-beam ultraviolet-visible spectrophotometer, Beijing is general analyse all purpose instrument Limited Liability (sweep limits: 190 ~ 800nm, sampling interval: 1nm, spectral bandwidth: 2nm, sweep speed: middling speed, scanning times: once, luminosity pattern: Abs);
The desk-top multitube autobalance of TD6 centrifuge, ordinary Instrument Ltd. in Changsha (accelerating potential is 80kV);
MAP18XAHF type X-ray diffractometer, Dandong ray instrument industrial group (test voltage is 40kV, and electric current is 100mA, and sweep speed is 4 °/min, continuous sweep);
KYKY-EM3200 type digital scanning electron microscope, Beijing KYKY Technology Development Co., Ltd.'s (accelerating potential: 30kV);
Electronic balance (AB104-N, Max=101g, d=0.1mg);
HH-S6 thermostat water bath, Jintan City Xin Nuo laboratory apparatus factory (water temperature is controlled at 30 ℃).
The extraction of 2 grape fruit juice
Get fresh grape fruit, peeling, gets 30g shaddock fruit grain and adds 60g distilled water and squeeze into fruit juice.With Buchner funnel suction filtration, obtain fruit juice, and make 80mL supernatant with centrifuge low-speed centrifugal.By the parallel 5-10 group of carrying out of this experiment, gained supernatant is all placed on sealing in beaker and saves backup.
Producing of 3 silver nano-grains
Get a certain amount of silver nitrate (1.6990g) solid, be placed in beaker and add after distilled water dissolving, be transferred to the liquor argenti nitratis ophthalmicus that is mixed with 0.1mol/L in the volumetric flask that specification is 100mL.The concentration that becomes volume to be 50mL this solution dilution is not less than a series of liquor argenti nitratis ophthalmicuses of 0.01mol/L.In 30 ℃ of waters bath with thermostatic control, get 20mL and now squeeze in the small beaker that grape fruit juice and the liquor argenti nitratis ophthalmicus of 20mL0.1-0.01mol/L be blended in 50mL and react.The ultra-violet absorption spectrum of timing assaying reaction liquid.Above-mentioned reactant liquor is placed after 48h, with centrifuge high speed centrifugation, isolated precipitation, then with after absolute ethanol washing precipitation and through the centrifugal product that obtains of centrifuge.By the parallel 10-20 group of carrying out of above-mentioned experiment, to obtain enough products, dry laggard line scanning electron microscope, infrared spectrum and X-ray diffraction test.
The rough calculation of 4Vc content
Get 20mL and now squeeze grape fruit juice, 100mL intermediate water, 10mL2mol/L HAc and 10mL0.5% starch, they are all joined in 250mL conical flask, after mixing, use I
2standard liquid [1/2(I
2)=0.1mol/L] carry out titration, to determine the content of Vc in above-mentioned grape fruit juice.Parallel titration three times.I used
2the volume of standard liquid is respectively: 1.51mL, 1.57mL, 1.63mL, average external volume is 1.57mL.
Therefore, Vc content is: Vc%=C
i2v
i2176.12/20=0.1543mg/mL.
5 results and discussion
5.1 the infrared spectrum analysis of grape fruit juice
In grape fruit juice, there is various biomolecules perhaps, as protein, vitamin and polysaccharide etc.Fig. 1 be grapefruit juice juice drop on KBr solid, dry the measured infrared spectrogram of rear compressing tablet.1621cm in figure
-1place's absworption peak is corresponding to the stretching vibration of the C=O group of albumen acid amides I band, 1250cm
-1place absworption peak for albumen acid amides III with on C-N flexural vibrations.1413cm
-1and 1055cm
-1place's absworption peak may be respectively the flexural vibrations of C-OH group in albumen, vitamin or polysaccharide molecule and the asymmetric stretching vibration of C-O-C group.2930cm
-1place may be the feature stretching vibration absorption band of methyl.3379cm
-1place may be the characteristic absorption band of hydrogen bond in NH.
The ultraviolet-visible analysis of spectrum of 5.2 grape fruit juice
Fig. 2 is the ultraviolet-visible spectrogram of the grape fruit juice that records.As can be seen from the figure, at 210nm and 280nm place, two absworption peaks have been there are, respectively π-π on the electron transition of C=O base n-π * and protein-tyrosine, tryptophan or phenylalanine residue on the peptide bond such as corresponding protein or amino acid
*electron transition, show to contain in grape fruit juice the biomolecule such as protein, amino acid.
The ultraviolet-visible analysis of spectrum of 5.3 reactant liquors
Fig. 3 is the ultraviolet-visible spectrogram of the reactant liquor of the placement different time that records.As can be seen from the figure, at 440nm place, obviously there is an absworption peak, and the increase in the intensity reaction time of this absworption peak and strengthening gradually.This absworption peak is considered to the characteristic absorption peak of silver nano-grain, and it is to cause because the radial surface of silver nano-grain in solution strengthens resonance Raman.This explanation is along with the prolongation in reaction time, and the amount of product silver nano-grain is in continuous increase.
The scanning electron microscope analysis of 5.4 products
Fig. 4 reacts the scanning electron microscope (SEM) photograph of 48 hours products therefroms for containing the reactant liquor of 0.05mol/L silver nitrate and grape fruit juice under 30 ℃ of conditions.As can be seen from the figure, product is the spherical granule of class, and particle size is between 50-100nm.The particle compared with large occurring in figure is to form because little nano particle occurs to assemble.
The X-ray diffraction analysis of 5.5 products
Fig. 5 reacts the x-ray diffraction pattern of 48 hours products therefroms for containing the reactant liquor of 0.05mol/L silver nitrate and grape fruit juice under 30 ℃ of conditions.As seen from the figure, when being 38.24 °, 44.43 °, 64.66 °, 77.63 °, 81.78 °, 2 θ there are 5 diffraction maximums, reference standard card (JCPDS87-0720) can be found (111), (200), (220) of corresponding center of area Cubic silver simple substance respectively, the feature diffraction of (311) and (222) face, shows that product is the silver-colored simple substance of face-centred cubic structure.
5.6 silver nano-grains form the discussion of mechanism
In grape fruit juice, mainly contain carrotene, B family vitamin, vitamin C, the biomolecule such as carbohydrate, volatile oil, protein, glutamic acid (Glu), aspartic acid (Asp), lysine (Lys), arginine (Arg), threonine (Thr) and organic acid etc.Because the biomolecule such as vitamin C and partial amino-acid have reproducibility, can be simple substance silver by monovalence silver ion reduction.The silver atoms generating is in forming the process that nucleus and nucleus constantly grow up, be subject to absorption and the package action of biomolecule in grape fruit juice, reduced surperficial energy, limited thereby crystal grain continues to grow up, the final spherical granule of class that is of a size of 50-100 nanometer that forms.
6 conclusions
Utilize the various biomolecules containing in grape fruit juice, under temperate condition, (30 ℃, normal pressure) are simple substance silver by the monovalence silver ion reduction in liquor argenti nitratis ophthalmicus.After multiple analytical test, find, the simple substance silver that products therefrom is centroid cubic crystal system, particle diameter is between 50-100nm.Formation mechanism to silver nano-grain is inquired into, and shows that the biomolecule containing in grape fruit juice plays the effect of template and reducing agent, the generation of induction and regulation and control Nano silver grain to the generation of simple substance silver particle.
A kind of described method of utilizing grape fruit juice to restore the silver ion in liquor argenti nitratis ophthalmicus, comprises the following steps:
(1) get fresh grape fruit, peeling, gets 30g grape fruit fruit grain and adds after the squeezing of 60g distilled water, with Buchner funnel suction filtration, obtain juice, and making supernatant with centrifuge low-speed centrifugal, gained supernatant is existing squeezing grape fruit juice, is all placed on sealing in beaker and saves backup;
(2) in the water bath with thermostatic control of 30 ℃, getting 20mL now squeezes after grape fruit juice mixes with the liquor argenti nitratis ophthalmicus of the 0.01-0.1mol/L of 20mL and reacts in the small beaker of 50mL, above-mentioned reactant liquor was placed after 48 hours, with supercentrifuge, isolate precipitation, then with after absolute ethanol washing precipitation and through the centrifugal product that obtains of supercentrifuge.
Claims (2)
1. utilize grape fruit juice to restore a method for the silver ion in liquor argenti nitratis ophthalmicus, it is characterized in that, comprise the following steps:
(1) get fresh grape fruit, peeling, gets 30g left and right grape fruit fruit grain and adds after the distilled water squeezing of 60g left and right, with Buchner funnel suction filtration, obtain juice, and making supernatant with centrifuge low-speed centrifugal, gained supernatant is existing squeezing grape fruit juice, is all placed on sealing in beaker and saves backup;
(2) in the water bath with thermostatic control of 30 ℃ of left and right, get about 20mL and now squeeze after grape fruit juice mixes with the liquor argenti nitratis ophthalmicus of the 0.01-0.1mol/L of 20mL left and right and react in the small beaker of 50mL, above-mentioned reactant liquor was placed after 48 hours, with supercentrifuge, isolate precipitation, then with after absolute ethanol washing precipitation and through the centrifugal product that obtains of supercentrifuge.
2. a kind of method of utilizing grape fruit juice to restore the silver ion in liquor argenti nitratis ophthalmicus according to claim 1, is characterized in that, comprises the following steps:
(1) get fresh grape fruit, peeling, gets 30g grape fruit fruit grain and adds after the squeezing of 60g distilled water, with Buchner funnel suction filtration, obtain juice, and making supernatant with centrifuge low-speed centrifugal, gained supernatant is existing squeezing grape fruit juice, is all placed on sealing in beaker and saves backup;
(2) in the water bath with thermostatic control of 30 ℃, getting 20mL now squeezes after grape fruit juice mixes with the liquor argenti nitratis ophthalmicus of the 0.01-0.1mol/L of 20mL and reacts in the small beaker of 50mL, above-mentioned reactant liquor was placed after 48 hours, with supercentrifuge, isolate precipitation, then with after absolute ethanol washing precipitation and through the centrifugal product that obtains of supercentrifuge.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104889419A (en) * | 2015-05-18 | 2015-09-09 | 湖州品创孵化器有限公司 | Biological synthesis method for spherical silver nanoparticle |
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| CN102941348A (en) * | 2012-12-05 | 2013-02-27 | 苏州大学 | Method for preparing nano-silver hydrosol by using plant extract |
| CN103302306A (en) * | 2013-06-19 | 2013-09-18 | 东南大学 | Method for reducing and preparing functionalized nano-silver based on polyphenol |
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2013
- 2013-10-21 CN CN201310496515.0A patent/CN103706803A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005095031A1 (en) * | 2004-03-31 | 2005-10-13 | Council Of Scientific And Industrial Research | A process for the synthesis of mono and bimetallic nanoparticles using palnt extract |
| CN102202815A (en) * | 2008-05-16 | 2011-09-28 | 维鲁泰克技术股份有限公司 | Green synthesis of nanometals using plant extracts and use thereof |
| CN102941348A (en) * | 2012-12-05 | 2013-02-27 | 苏州大学 | Method for preparing nano-silver hydrosol by using plant extract |
| CN103302306A (en) * | 2013-06-19 | 2013-09-18 | 东南大学 | Method for reducing and preparing functionalized nano-silver based on polyphenol |
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| CN104889419A (en) * | 2015-05-18 | 2015-09-09 | 湖州品创孵化器有限公司 | Biological synthesis method for spherical silver nanoparticle |
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