CN101225533A - Electrolytic preparation method of high-activity long-life electrically positive colloid nano silver - Google Patents
Electrolytic preparation method of high-activity long-life electrically positive colloid nano silver Download PDFInfo
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- CN101225533A CN101225533A CNA2007100662859A CN200710066285A CN101225533A CN 101225533 A CN101225533 A CN 101225533A CN A2007100662859 A CNA2007100662859 A CN A2007100662859A CN 200710066285 A CN200710066285 A CN 200710066285A CN 101225533 A CN101225533 A CN 101225533A
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Abstract
The invention relates to an electrolysis preparation method of high activity and long life positive silver colloids, which is characterized in that: two silver rods of the diameter of 4 to 6 mm and the length of 90 to 110 mm are used as two electrodes; the Na3C6H5O72H2O of the concentration of 0.476 to 1.16 mmol/l or the polyvinyl alcohol solution containing the silver nitrate (molecular weight: 169.87) of 20 to 60 mg in per 1000 ml is used as electrolyte; two silver rods of the diameter of 4 to 5 mm and the length of 90 to 110 mm are inserted during preparing; the control voltage is 6 to 9 V; the electrolysis time is 50 to 60 seconds, so as to obtain the positive silver colloids. The electrolysis preparation method of high activity and long life positive silver colloids has the advantages of strong stability, good reliability, long preservation time and stronger surface reinforced spectral effect.
Description
Technical field
The present invention relates to a kind of electrolytic process and prepare high reactivity, long-life electrically positive colloid nano silver and using method, belong to nanotechnology, metal colloidal state preparation of nanoparticles and Application Areas.
Background technology
Colloid nano silver is widely used in surperficial enhanced spectrum research, aspects such as police criminal detection and medical jurisprudence, biologic pharmacological science.Traditional silver colloid has several preparation methods, and the most frequently used is chemical reduction method, promptly by the colloid nano silver (also claiming grey elargol) of the surperficial positively charged of trisodium citrate reduction preparation; Prepare colloid nano silver (also claiming yellow elargol) with the potassium borohydride reduction Silver Nitrate.People also adopt pulsed laser irradiation metal (gold, silver, copper etc.) to produce nano-metal particle recently, and are distributed to the method that obtains elargol in the aqueous solution.The particle size of silver does not wait to nanometers up to a hundred from the number nanometer in the elargol of these method preparations.The silver coating of particles also has sphere, needle-like, hex crystal shape not to wait, and these elargol have been widely used in surperficial enhanced spectrum research.Yet the elargol of traditional method preparation is very unstable.Under room temperature environment, store, generally only stablize about 2 weeks to 2 month, just reunite, precipitate.And the many character of colloidal all are on the turn during this period, and this brings great inconvenience to use, also often result of use are produced uncertain.Such as repeatability, the reliability of SERS, police criminal detection and Forensic detection result's stability, reliability.The objective of the invention is to invent a kind of method of preparation and use of novel colloid nano silver, use the colloid nano silver of the method preparation under room temperature environment, to keep in Dark Place more than a year and a half, still do not reunite, do not precipitate, and stronger surperficial enhanced spectrum effect is arranged.By changing the composition of electrolytic solution, can obtain variable grain size, the band ionic charge colloid nano silver different simultaneously with composition.In colloid nano silver, except that nano-Ag particles, also have some other ion and molecule (as sodium ion, nitrate ion, citrate ion, solvent molecule etc.), these ions and molecule are measured molecule to some does not have influence, but to other molecule influential (Raman peaks of reinforcing effect or mensuration molecule disappears), like this, just can select different electrolytes to prepare variable grain size, the band ionic charge colloid nano silver different with composition.As not containing nitrate ion in the colloid nano silver take trisodium citrate as electrolyte, like this, the molecule of some and the competitive absorption of nitrate ion just can not be influenced; And do not contain citrate in the Nano Silver that the electrolyte of preparing with silver nitrate and polyvinyl alcohol prepares, can avoid the citrate Raman peaks to measuring the impact of some molecule Raman peaks.
Summary of the invention
Purpose of the present invention provides a kind of high reactivity, long-life electrically positive colloid nano silver electrolytic preparation method for the weak point that overcomes above-mentioned prior art existence just.The electrically positive colloid nano silver that the inventive method makes has that stability is strong, good reliability, the shelf time is long and the remarkable advantage of stronger surperficial enhanced spectrum effect is arranged.
The objective of the invention is to realize by following technical solution.
Preparation method of the present invention is: take diameter as 4～6 millimeters, length is that two silver rods of 90～110 millimeters are positive and negative electrode, two hydration trisodium citrate (Na take concentration as 0.476～1.16mmol/L
3C
6H
5O
7.2H
2O) or contain 20～60 milligrams of silver nitrates in per 1000 milliliters (molecular weight: poly-vinyl alcohol solution 169.87) is electrolyte; Inserting two diameters during preparation is 4～6 millimeters, and length is that 90～110 millimeters silver rod is positive and negative electrode, and control voltage is 6～9V, and electrolysis 50～60 minutes can make high activity, long-life electrically positive colloid nano silver in electrolytic solution.
Experimental water is common distilled water during preparation, can obtain the colloid nano silver of energy long preservation different-grain diameter, excellent in uniform (more than 1 year) by changing electrolysis time and control voltage.Electrolysis time is long, and the particle diameter of silver-colored particle is more big; Control voltage is more high, and the particle diameter of silver-colored particle is also more big; Preparation condition of the present invention is simple, and common lab all can prepare.Cost of manufacture is low, does not need expensive experimental equipment.The Positive silver colloid for preparing is shown as uniform spheroidal or ellipsoidal particle through transmission electron microscope, particle diameter forms with electrolyte and concentration is different changes, the particle diameter of silver particle changes in 20～80 nanometer range, the Nano Silver that particle diameter is little, higher concentration can obtain greater particle size of the general obtainable silver-colored particle of low concentration.At ambient temperature, to divide airtight preservation among the Brown Glass Brown glass bottles and jars only (must not use the cleaning agent that contains fluorescer to clean) that installs to through repeatedly cleaning after keeping in Dark Place about one month.Electrically positive colloid nano silver after the packing is statically placed in lucifuge, in the anti-environment that jolts.
Further set forth content of the present invention below in conjunction with drawings and Examples.
Embodiment
Embodiment one is take diameter as 4 millimeters, and length is that 90 millimeters silver rod is electrode, two hydration trisodium citrate (Na take concentration as 1.16mmol/L
3C
6H
5O
7.2H
2O) solution is electrolyte; Inserting two silver rods during preparation is electrode, and control voltage is 6V, and electrolysis 50 minutes namely makes high activity, long-life electrically positive colloid nano silver in electrolyte.
Embodiment two is take diameter as 6 millimeters, and length is that 110 millimeters silver rod is electrode, two hydration trisodium citrate (Na take concentration as 0.476mmol/L
3C
6H
5O
7.2H
2O) solution is electrolyte; Inserting two silver rods during preparation is electrode, and control voltage is 7V, and electrolysis 60 minutes namely makes high activity, long-life electrically positive colloid nano silver in electrolyte.
Embodiment three is take diameter as 6 millimeters, and length is that 90 millimeters silver rod is electrode, and (molecular weight: poly-vinyl alcohol solution 169.87) is as electrolyte to contain 40 milligrams of silver nitrates in per 1000 milliliters; Inserting two silver rods during preparation is electrode, and control voltage is 7V, and electrolysis 55 minutes namely makes high activity, long-life electrically positive colloid nano silver in electrolyte.
This electrically positive colloid nano silver prepared in August, 2005, dividing packs into is with in the Brown Glass Brown glass bottles and jars only of rubber plug, behind black plastics bag parcel, be positioned over laboratory room temperature preservation (about 5～30 ℃ of temperature), in May, 2007, study surface enhanced Raman scattering with it, and compare the year before, still keep active preferably, the Raman peaks (as Yamamoto Methylene Blue ZF, to magenta) with a part is had good circulation ratio.Explanation can keep its Raman active in the room temperature lucifuge more than a year and a half in the anti-environment that jolts.
The present invention is a kind of long lifetime, highly active electrically positive colloid nano silver, belong to nanotechnology, metal nanoparticle colloid for preparing field, after the colloid of preparation kept in Dark Place one month at normal temperatures, be divided in through cleaning for several times in the airtight Brown Glass Brown glass bottles and jars only of (can not use the detergent that contains fluorescent agent), normal temperature is kept in the anti-environment that jolts of lucifuge before using.Its characteristics also are the colloid nano silver through above-mentioned art breading, can be under room temperature environment (5～30 ℃) leave standstill and preserve more than a year and a half, and do not reunite, do not precipitate, still keep strengthening preferably the effect of Raman toughener, the Raman peaks with a part is had good circulation ratio.Its characteristics three are: as required, form and electrolysis time by changing electrolyte, can obtain to contain in the solution colloid nano silvers different ions, that particle diameter is different.The colloid nano silver particle of this method preparation is spheroidal or elliposoidal, and positive charge is worn through the electrophoresis experiment verification table in the surface.The present invention can be widely used in SERS research and to drugs, medicine, dye molecule, and the evaluation of agricultural chemicals.
Claims (1)
1. high activity, long-life electrically positive colloid nano silver electrolytic preparation method is characterized in that: take diameter as 4～6 millimeters, length is that two silver rods of 90～110 millimeters are electrode, two hydration trisodium citrate (Na take concentration as 0.476～1.16mmol/L
3C
6H
5O
7.2H
2O) or contain 20～60 milligrams of silver nitrates in per 1000 milliliters (molecular weight: poly-vinyl alcohol solution 169.87) is electrolyte; Inserting two diameters during preparation is 4～6 millimeters, and length is that 90～110 millimeters silver rod is electrode, and control voltage is 6～9V, electrolysis 50～60 minutes.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100662859A CN101225533A (en) | 2007-10-17 | 2007-10-17 | Electrolytic preparation method of high-activity long-life electrically positive colloid nano silver |
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|---|---|---|---|
| CNA2007100662859A CN101225533A (en) | 2007-10-17 | 2007-10-17 | Electrolytic preparation method of high-activity long-life electrically positive colloid nano silver |
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|---|---|
| CN101225533A true CN101225533A (en) | 2008-07-23 |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102031539A (en) * | 2010-12-21 | 2011-04-27 | 北京化工大学 | Method for preparing metallic silver nano particles with controllable shapes in batch |
| CN102181885A (en) * | 2011-04-07 | 2011-09-14 | 东南大学 | Method for preparing nano silver solution by electrolysis |
| RU2452498C2 (en) * | 2010-07-20 | 2012-06-10 | Общество с ограниченной ответственностью "Научно-производственное объединение "Ликом" | Method for preparing anti-tuberculosis drug |
| CN103060854A (en) * | 2013-01-11 | 2013-04-24 | 东南大学 | Method for electrochemical synthesis of colloidal silver solution |
| CN103084580A (en) * | 2013-01-11 | 2013-05-08 | 东南大学 | Method for synthesizing water-solubility fluorescence silver nanocluster by electrochemistry |
| RU2602741C2 (en) * | 2015-03-23 | 2016-11-20 | Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский Томский политехнический университет" | Method of producing water-soluble composition of silver nanoparticles |
| CN106283123A (en) * | 2016-09-30 | 2017-01-04 | 天津宝兴威科技有限公司 | A kind of preparation method of nanometer silver coating |
| CN111889832A (en) * | 2020-06-28 | 2020-11-06 | 合肥百诺金科技股份有限公司 | Method for synthesizing silver nanoparticles by liquid-phase electric spark with clean surface and controllable size |
| CN112021340A (en) * | 2020-07-28 | 2020-12-04 | 北京工业大学 | Preparation and application of nano composite bactericidal antiviral material |
| CN112609208A (en) * | 2020-11-28 | 2021-04-06 | 欧之萌(武汉)国际贸易有限公司 | Method for preparing low-concentration nano-silver antibacterial spray through electrolysis |
-
2007
- 2007-10-17 CN CNA2007100662859A patent/CN101225533A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2452498C2 (en) * | 2010-07-20 | 2012-06-10 | Общество с ограниченной ответственностью "Научно-производственное объединение "Ликом" | Method for preparing anti-tuberculosis drug |
| CN102031539A (en) * | 2010-12-21 | 2011-04-27 | 北京化工大学 | Method for preparing metallic silver nano particles with controllable shapes in batch |
| CN102181885A (en) * | 2011-04-07 | 2011-09-14 | 东南大学 | Method for preparing nano silver solution by electrolysis |
| CN103060854A (en) * | 2013-01-11 | 2013-04-24 | 东南大学 | Method for electrochemical synthesis of colloidal silver solution |
| CN103084580A (en) * | 2013-01-11 | 2013-05-08 | 东南大学 | Method for synthesizing water-solubility fluorescence silver nanocluster by electrochemistry |
| RU2602741C2 (en) * | 2015-03-23 | 2016-11-20 | Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский Томский политехнический университет" | Method of producing water-soluble composition of silver nanoparticles |
| CN106283123A (en) * | 2016-09-30 | 2017-01-04 | 天津宝兴威科技有限公司 | A kind of preparation method of nanometer silver coating |
| CN111889832A (en) * | 2020-06-28 | 2020-11-06 | 合肥百诺金科技股份有限公司 | Method for synthesizing silver nanoparticles by liquid-phase electric spark with clean surface and controllable size |
| CN112021340A (en) * | 2020-07-28 | 2020-12-04 | 北京工业大学 | Preparation and application of nano composite bactericidal antiviral material |
| CN112609208A (en) * | 2020-11-28 | 2021-04-06 | 欧之萌(武汉)国际贸易有限公司 | Method for preparing low-concentration nano-silver antibacterial spray through electrolysis |
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Open date: 20080723 |