CN103060854A - Method for electrochemical synthesis of colloidal silver solution - Google Patents
Method for electrochemical synthesis of colloidal silver solution Download PDFInfo
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- CN103060854A CN103060854A CN201310009840XA CN201310009840A CN103060854A CN 103060854 A CN103060854 A CN 103060854A CN 201310009840X A CN201310009840X A CN 201310009840XA CN 201310009840 A CN201310009840 A CN 201310009840A CN 103060854 A CN103060854 A CN 103060854A
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Abstract
The invention relates to a method for the continuous electrochemical synthesis of a colloidal silver solution. The method comprises the following steps: stabilizers with the concentration of 2.5 mg/mL to 10 mg/mL are continuously injected into a silver electrolysis reactor; the electrode of a silver rod is enabled to perform an electrolytic reaction in the continuous flowing stabilizers at the temperature of 30 DEG C to 90 DEG C and the stirring speed of 1V to 20V; and when the reactor is full of the solution, a product flows out, i.e. the colloidal silver solution is obtained. The method is suitable for the preparation of colloidal silver used as the stabilizers such as spolyvinylpyrrolidone, polyvinyl alcohol, sodium citrate and the like; and nanosilver particles with different sizes can be obtained by regulating and controlling the colloidal silver. In addition, as the method is used, various silver salts and reducing agents are not required; and only the stabilizers are utilized, so that the product is higher in purity. The experimental equipment is simple, easy to control, environment-friendly and free of pollution. Therefore, the method provided by the invention has a prospect for the batch synthesis of the nanosilver.
Description
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Technical field
The present invention relates to the preparing technical field of noble metal nanometer material, particularly relate to a kind of electrochemistry method for continuously synthesizing of colloidal silver solution.
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Background technology
In more than ten years, nanometer silver is at catalysis, antibiotic, optics in the past, and the many-sides such as electronics, biomarker, figure image intensifying show good application prospect.At present, the preparation method of nanometer silver mainly contains physical method, chemical process and biological method.
The advantage of physical method is to prepare relatively largely, and product impurity is few, and purity is higher; Shortcoming is that plant and instrument is had relatively high expectations, and productive expense is expensive.The advantage of chemical process is comparatively versatile and flexible, easy handling; Shortcoming is that reaction process and processing condition are not easy to control well, and a certain ad hoc approach can only be prepared the nanometer silver of a certain specific median size, and used chemical reagent can produce harm to human body or environment usually.The advantage of biological method is that this class material product has more biocompatibility and environment friendly, wide such as the microorganism raw material sources, cheap and easy to get, the bioreduction mild condition, the chemical reagent that reaction process adds and generation have toxic byproduct few, and the product nano particle is attached to and is difficult on the thalline reuniting; Shortcoming is that to adopt microorganism system to prepare the condition of nano particle like that artificial controlled not as physical-chemical reaction.
With regard to present present Research, the industrialization production of nanometer silver and application still are subject to the restriction of following point: particle is very easily reunited, and is difficult to obtain the mono-dispersed nano particle; The nanometer silver output that size distribution is little, pattern is single has much room for improvement, especially for the chemical method that generally uses now, although simple to operate, with low cost, but because the parameter of required regulation and control is too much in preparation process, and higher to its accuracy requirement, thereby so that the output of single shape nanometer silver is lower.Therefore, improve the output of nanometer silver, the preparation structure is more meticulous, even the nanometer silver of the required specific microtexture of synthetic people, and these all are the important directions of nanometer silver research and development.
The production technology of following nanometer silver should be to low cost, low consumption, the low future development that pollutes.Compare the traditional chemical method, utilize electrochemical method prepare nano material have equipment simple, easy to operate, be easy to the advantages such as control, reaction conditions is gentle, quick, the resulting nano particle purity of reaction is high, environmental pollution is few.Just because of the electrochemical method investment is low, productive rate is high, and technical difficulty is less, and technique is flexible, is easy to control, easily turns to industrialization by the laboratory.Therefore, electrochemical synthesis is a kind of up-and-coming nanometer silver preparation method.
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Summary of the invention
The technical problem that solves:The purpose of this invention is to provide the continuously method of synthetic colloidal silver solution of a kind of electrochemistry.
Technical scheme:A kind of electrochemistry is the method for synthetic colloidal silver solution continuously, by being that the stablizer of 2.5mg/mL-10mg/mL successively injects silver-colored electrolysis reactor with concentration, under the condition that 30 ℃-90 ℃, 1V-20V stir, make silver-colored bar electrode in the stablizer of continuous flow, electrolytic reaction occur, when solution is full of in the reactor, product flows out, and obtains colloidal silver solution.
Reaction electrode in the described silver-colored electrolysis reactor is purity 99.99%, the silver rod of diameter 2-3mm, interelectrode distance 8-10mm, reactor volume 10mL.
The optimum concentration range of described stablizer is 5mg/mL-10mg/mL.
Described temperature range is 60 ℃-90 ℃.
The every 30sec-1min of electrode current direction of described silver-colored electrolysis reactor exchanges 1 time automatically.
Described stablizer is polyvinylpyrrolidone (PVP), polyvinyl alcohol (PVA) or Trisodium Citrate.
When making stablizer, the optimum range of response voltage is 7V-10V with polyvinylpyrrolidone (PVP).
Described silver-colored electrolysis reactor is two electrodes or four pairs of electrodes.
During two electrolysis, the stablizer flow velocity is 30mL/h-100mL/h; During eight electrolysis, the stablizer flow velocity is 200mL/h-1000mL/h.
Described silver-colored electrolysis reactor is connected with input unit, electrolysis control device, take-off equipment respectively, and silver-colored electrolysis reactor is located on the magnetic force heating stirrer; Input unit is micrometeor syringe pump or peristaltic pump, the electrolysis control device is comprised of D.C. regulated power supply and sense of current controller, take-off equipment is comprised of spiral cold-finger and solution collection container, input unit is connected by pipeline with silver-colored electrolysis reactor with take-off equipment, and the electrolysis control device links to each other by electric wire with electrode in the silver-colored electrolysis reactor.
Beneficial effect:The invention provides the continuously method of synthetic colloidal silver solution of a kind of electrochemistry.By the method, can obtain simply, rapidly the colloidal silver solution of high yield, and owing to having avoided use reductive agent and silver salt, silver nano-grain purity is higher in the product.The method can by changing the size of the regulation and control silver nano-grains such as flow velocity, response voltage, temperature and stablizer, obtain the different size nanometer silver from 1-2 nanometer to 70 ~ 80 nanometers, for the controlled preparation of the magnanimity of nanometer silver provides a kind of good scheme.
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Description of drawings
Fig. 1 is the continuously device schematic diagram of synthetic colloidal silver solution of electrochemistry; 1 for connecting the wire of D.C. regulated power supply and sense of current controller, 2 for connecting the wire of sense of current controller and electrode, 3 for connecting the fine duct of input unit and silver-colored electrolysis reactor, and 4 for connecting the fine duct of silver-colored electrolysis reactor and take-off equipment, and 5 for connecting the fine duct of spiral cold-finger and solution collection container, 6 is D.C. regulated power supply, 7 is sense of current controller, and 8 is input unit, and 9 is the magnetic force heating stirrer, 10 is silver-colored electrolysis reactor, and 11 is take-off equipment;
Fig. 2 is the XRD figure of synthetic silver nano-grain;
Fig. 3 is the uv-visible absorption spectra figure of synthetic silver nano-grain;
Fig. 4 is transmission electron microscope picture and the particle diameter statistical graph of synthetic silver nano-grain;
Fig. 5 is colloidal silver solution 20nm electromicroscopic photograph;
Fig. 6 is colloidal silver solution 100nm electromicroscopic photograph.
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Embodiment
Below by specific embodiment method of the present invention is described.Method described in the following embodiment if no special instructions, is ordinary method; Described reagent and material if no special instructions, all can obtain from commercial channels.
The device explanation: silver-colored electrolysis reactor 10 is connected with input unit 8, electrolysis control device, take-off equipment 11 respectively, and silver-colored electrolysis reactor is located on the magnetic force heating stirrer 9; Input unit is micrometeor syringe pump or peristaltic pump, the electrolysis control device is comprised of D.C. regulated power supply 6 and sense of current controller 7, take-off equipment is comprised of spiral cold-finger and solution collection container, input unit is connected by pipeline with silver-colored electrolysis reactor with take-off equipment, and the electrolysis control device links to each other by electric wire with electrode in the silver-colored electrolysis reactor.
Adopt two electrode reaction devices (volume is 10mL approximately), the PVP solution of configuration 5mg/mL injects reaction unit with the 100mL/h flow velocity, the 15V electrolytic reaction, and 60 ℃ of temperature of reaction, 1min changes the one-time electrode sense of current.Output terminal is collected product, composes as can be known according to XRD figure among Fig. 2 that product is fine silver, further according to UV-Vis spectrum among Fig. 3 as can be known product be nanometer silver, the pattern of nanometer silver and size are shown in Fig. 4 (a).Reaction electrode is purity 99.99%, the silver rod of diameter 2-3mm, interelectrode distance 8-10mm.
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Adopt two electrode reaction devices (volume is 10mL approximately), the PVP solution of configuration 5mg/mL injects reaction unit with the 50mL/h flow velocity, the 9V electrolytic reaction, and 60 ℃ of temperature of reaction, 1min changes the one-time electrode sense of current.Output terminal is collected product and is colloidal silver solution, shown in Fig. 4 (b).Reaction electrode is purity 99.99%, the silver rod of diameter 2-3mm, interelectrode distance 8-10mm.
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Adopt two electrode reaction devices (volume is 10mL approximately), the PVP solution of configuration 10mg/mL injects reaction unit with the 30mL/h flow velocity, the 10V electrolytic reaction, and 80 ℃ of temperature of reaction, 1min changes the one-time electrode sense of current.Output terminal is collected product and is colloidal silver solution, shown in Fig. 4 (c).Reaction electrode is purity 99.99%, the silver rod of diameter 2-3mm, interelectrode distance 8-10mm.
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Adopt eight electrode reaction devices (volume is 70mL approximately), the PVP solution of configuration 5mg/mL injects reaction unit with the 380mL/h flow velocity, the 7V electrolytic reaction, and 50 ℃ of temperature of reaction, 1min changes the one-time electrode sense of current.Output terminal is collected product and is colloidal silver solution, as shown in Figure 5.Reaction electrode is purity 99.99%, the silver rod of diameter 2-3mm, interelectrode distance 8-10mm.
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Embodiment 5
Adopt eight electrode reaction devices (volume is 70mL approximately), the PVP solution of configuration 5mg/mL injects continuous synthesizer with the 540mL/h flow velocity, the 8.5V electrolytic reaction, and 70 ℃ of temperature of reaction, 1min changes the one-time electrode sense of current.Output terminal is collected product and is colloidal silver solution, as shown in Figure 6.Reaction electrode is purity 99.99%, the silver rod of diameter 2-3mm, interelectrode distance 8-10mm.
Claims (10)
1. the continuous method of synthetic colloidal silver solution of an electrochemistry, it is characterized in that: by being that the stablizer of 2.5mg/mL-10mg/mL successively injects silver-colored electrolysis reactor with concentration, under the condition that 30 ℃-90 ℃, 1V-20V stir, make silver-colored bar electrode in the stablizer of continuous flow, electrolytic reaction occur, when solution is full of in the reactor, product flows out, and obtains colloidal silver solution.
2. electrochemistry according to claim 1 is synthesized the method for colloidal silver solution continuously, it is characterized in that reaction electrode is purity 99.99% in the silver-colored electrolysis reactor, the silver rod of diameter 2-3mm, interelectrode distance 8-10mm, reactor volume 10mL.
3. electrochemistry according to claim 1 is synthesized the method for colloidal silver solution continuously, and the optimum concentration range that it is characterized in that stablizer is 5mg/mL-10mg/mL.
4. electrochemistry according to claim 1 is synthesized the method for colloidal silver solution continuously, it is characterized in that described temperature range is 60 ℃-90 ℃.
5. electrochemistry according to claim 1 is synthesized the method for colloidal silver solution continuously, it is characterized in that the every 30sec-1min of electrode current direction of silver-colored electrolysis reactor exchanges 1 time automatically.
6. electrochemistry according to claim 1 is synthesized the method for colloidal silver solution continuously, it is characterized in that stablizer is polyvinylpyrrolidone (PVP), polyvinyl alcohol (PVA) or Trisodium Citrate.
7. electrochemistry according to claim 6 is synthesized the method for colloidal silver solution continuously, and it is characterized in that: when making stablizer, the optimum range of response voltage is 7V-10V with polyvinylpyrrolidone (PVP).
8. electrochemistry according to claim 1 is synthesized the method for colloidal silver solution continuously, it is characterized in that silver-colored electrolysis reactor is two electrodes or four pairs of electrodes.
9. electrochemistry according to claim 8 is synthesized the method for colloidal silver solution continuously, and when it is characterized in that two electrolysis, the stablizer flow velocity is 30mL/h-100mL/h; During eight electrolysis, the stablizer flow velocity is 200mL/h-1000mL/h.
10. electrochemistry according to claim 1 is synthesized the method for colloidal silver solution continuously, it is characterized in that described silver-colored electrolysis reactor (10) is connected with input unit (8), electrolysis control device, take-off equipment (11) respectively, silver-colored electrolysis reactor is located on the magnetic force heating stirrer (9); Input unit is micrometeor syringe pump or peristaltic pump, the electrolysis control device is comprised of D.C. regulated power supply (6) and sense of current controller (7), take-off equipment is comprised of spiral cold-finger and solution collection container, input unit is connected by pipeline with silver-colored electrolysis reactor with take-off equipment, and the electrolysis control device links to each other by electric wire with electrode in the silver-colored electrolysis reactor.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107855122A (en) * | 2017-10-31 | 2018-03-30 | 绍兴文理学院 | A kind of preparation method of noble metal platinum nano catalyst |
| CN108486611A (en) * | 2018-05-09 | 2018-09-04 | 河南海王星科技发展有限公司 | A kind of colloidal silver generator |
| 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 |
| CN112609209A (en) * | 2020-11-28 | 2021-04-06 | 欧之萌(武汉)国际贸易有限公司 | Electrolytic bath device for preparing colloid nano silver by low-current mobile phase |
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| US3843491A (en) * | 1971-12-28 | 1974-10-22 | Snam Progetti | Process for the preparation of silver base catalyst |
| CN101225533A (en) * | 2007-10-17 | 2008-07-23 | 楚雄师范学院 | Electrolytic preparation method of high-activity long-life electrically positive colloid nano silver |
| CN101554597A (en) * | 2009-05-12 | 2009-10-14 | 厦门大学 | Method for preparing Pt/C nanometer catalyst and device thereof |
| CN102181885A (en) * | 2011-04-07 | 2011-09-14 | 东南大学 | Method for preparing nano silver solution by electrolysis |
| CN102367582A (en) * | 2010-09-15 | 2012-03-07 | 北京奈艾斯新材料科技有限公司 | Method for preparing nanoscale metal particles by bimetallic electrode pulse direct-current bias electrodeposition |
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2013
- 2013-01-11 CN CN201310009840XA patent/CN103060854A/en active Pending
Patent Citations (5)
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| US3843491A (en) * | 1971-12-28 | 1974-10-22 | Snam Progetti | Process for the preparation of silver base catalyst |
| CN101225533A (en) * | 2007-10-17 | 2008-07-23 | 楚雄师范学院 | Electrolytic preparation method of high-activity long-life electrically positive colloid nano silver |
| CN101554597A (en) * | 2009-05-12 | 2009-10-14 | 厦门大学 | Method for preparing Pt/C nanometer catalyst and device thereof |
| CN102367582A (en) * | 2010-09-15 | 2012-03-07 | 北京奈艾斯新材料科技有限公司 | Method for preparing nanoscale metal particles by bimetallic electrode pulse direct-current bias electrodeposition |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107855122A (en) * | 2017-10-31 | 2018-03-30 | 绍兴文理学院 | A kind of preparation method of noble metal platinum nano catalyst |
| CN108486611A (en) * | 2018-05-09 | 2018-09-04 | 河南海王星科技发展有限公司 | A kind of colloidal silver generator |
| 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 |
| CN112609209A (en) * | 2020-11-28 | 2021-04-06 | 欧之萌(武汉)国际贸易有限公司 | Electrolytic bath device for preparing colloid nano silver by low-current mobile phase |
| CN112609209B (en) * | 2020-11-28 | 2022-06-07 | 欧之萌(武汉)国际贸易有限公司 | Electrolytic bath device for preparing colloid nano silver by low-current mobile phase |
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Application publication date: 20130424 |