CN101811724A - Method for preparing silver peroxide superfine powder - Google Patents
Method for preparing silver peroxide superfine powder Download PDFInfo
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- CN101811724A CN101811724A CN 201010153697 CN201010153697A CN101811724A CN 101811724 A CN101811724 A CN 101811724A CN 201010153697 CN201010153697 CN 201010153697 CN 201010153697 A CN201010153697 A CN 201010153697A CN 101811724 A CN101811724 A CN 101811724A
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Abstract
The invention discloses a method for preparing silver peroxide (AgO) superfine powder, which comprises: firstly, heating solution of silver nitrate to 25 to 55 DEG C and adding solution of sodium hydroxide into the solution of silver nitrate with stirring at a speed of 2,000r/min to obtain mixed solution, wherein brown active Ag2O micro crystals precipitate in the mixed solution; and introducing ozone into the mixed solution containing the Ag2O micro crystals for 1 to 5 hours under the condition that the reaction temperature is controlled to be 25 to 55 DEG C to obtain a black precipitate, filtering the precipitate to obtain AgO wet powder, washing the AgO wet powder with deionized water, drying the AgO wet powder at 70 to 100 DEG C for 3 to 5 hours to obtain dry AgO powder with a particle size of 200 nanometer. The AgO superfine powder prepared by the method has the advantages of high purity, complete crystal form, small particle size, simple operation process and preparation equipment and no pollutant discharge.
Description
Technical field
The invention belongs to ultra-fine inorganic oxide powder preparing technical field, be specifically related to a kind of method for preparing silver peroxide superfine powder.
Background technology
The research sterilizing ability is strong, stability is high, be a hot subject of sterilization material research to the effect of human body safety non-toxic evil, sterilant that bacterium is not developed immunity to drugs.Organic bactericide is owing to exist security (as toxic side effect, some monomer even carcinogenesis is arranged), poor heat resistance, easily decompose and problem such as work-ing life is short and fading out from practical application gradually.Natural bactericidal agent is owing to be subjected to resource limit, application that certain difficulty is arranged.Therefore inorganic fungicide research is risen, and mainly concentrates on titanium dioxide optical catalyst and nanometer silver, monovalence is carried silver-colored sterilization material.The photocatalysis efficiency of titanium dioxide is low, and the germicidal action of silver is relevant with the valent state of self, and the high more sterilizing ability of valence state is strong more.Existing result of study shows that the silver peroxide of high price has extremely strong sterilizing ability, and the sterilization speed and the sterilization effect of high price silver peroxide are all good than monovalence silver suboxide.
Silver has multiple oxidation valence state, is mainly the Ag(I), the Ag(II), the Ag(III), oxidation state is that the silver compound of+1 valency is more common, oxidation state for+2 and+3 silver compound be rare or unstable compounds, AgO is considered to the mixed valence compound.Silver peroxide (AgO) has than strong oxidizing property, electromagnetic property and electrochemical activity as a kind of novel inorganic functional material, has been successfully applied to fields such as water purifier, organic synthesis, superconductor and heavy-duty battery.Existing preparation silver peroxide method is to adopt strong oxidizer Potassium Persulphate or bromine water oxidation Silver Nitrate or silver suboxide reaction in strong alkali solution to make, and adopting the electrolysis process preparation, mainly there are problems such as particle diameter is big, purity is lower in the silver peroxide that obtains so.And invent the patent of invention (application number 200610000059.6 of people such as artificial Zhang Yu application, patent name is " preparation method of a kind of nano oxidized Gao Yin ", open day is on July 11st, 2007), adopt the highly purified nano phase ag_2 o of clorox and sodium hydroxide mixed chemical solution oxidation silver nitrate solution preparation, this patent requires temperature of reaction at 5～35 ℃, the naoh concentration of reaction is 20%～45%, because oxidizing reaction is thermopositive reaction, this reaction must could realize temperature control by means of cooling system; The amount of sodium hydroxide that reaction adds is too big, so the reaction process complexity, naoh concentration height in the waste liquid of discharging, and environmental pollution is serious.
Summary of the invention
The object of the invention provides a kind of method for preparing silver peroxide superfine powder, prepare ultra-fine AgO powder by the ozone oxidation method, solved the complicated process of preparation that exists in the prior art, the silver peroxide particle diameter of preparing is big, purity is low, the problem of poor stability, severe reaction conditions.
The technical solution adopted in the present invention is that a kind of method for preparing silver peroxide superfine powder comprises following operation steps:
Step 1,
Preparation concentration is that 0.10mol/L～0.20mol/L silver nitrate solution and concentration are the sodium hydroxide solution of 0.6mol/L～5.6mol/L, and the volume ratio of silver nitrate solution and sodium hydroxide solution is 4:1;
Step 2,
Silver nitrate solution is heated to 25 ℃～55 ℃, under the stirring velocity of 2000r/min, sodium hydroxide solution is added in the silver nitrate solution, obtain mixing solutions, the pale brown look active A g that separates out is arranged in this mixing solutions
2The O crystallite;
Step 3,
Be controlled in temperature of reaction under 25～55 ℃ the condition, toward having analysed Ag
2Fed ozone 1～5 hour in the mixing solutions of O crystallite, obtain black precipitate, filtering precipitate obtains the AgO wet-milling, with washed with de-ionized water AgO wet-milling, dried 3～5 hours under 70～100 ℃ of conditions, promptly obtaining the exsiccant particle diameter is the silver peroxide powder of 200nm again.
The invention has the beneficial effects as follows that by the AgO ultrafine powder of this method preparation, it is little to have a purity height, complete in crystal formation, particle diameter, operating procedure and preparation equipment are simple, the advantage of non-pollutant discharge.Particularly, make that germ-killing efficiency height, sterilization speed are fast, the sterilant consumption is little because AgO ultrafine powder purity height, the particle diameter of preparation are little, economic benefit is obvious, can do water treatment and the required sterilant of other germicidal applications, also can be used for the occasion that some other needs AgO,, silver battery material synthetic etc. as organic oxidation.
Description of drawings
Fig. 1 is that the ultra-fine silver peroxide powder of the inventive method preparation adopts Tianjin, island XRD-7000S type X-ray diffractometer to analyze the XRD figure spectrum of its crystalline structure gained;
Fig. 2 is that the ultra-fine silver peroxide powder of the inventive method preparation adopts JSM-6700FXIB type scanning electronic microscope its pattern, size to be analyzed the SEM figure of gained;
Fig. 3 is that the ultra-fine silver peroxide powder of the inventive method preparation adopts CPY-2P type high temperature difference thermal analyzer that its thermal decomposition process is carried out the DTA graphic representation that institute gets.
Embodiment
The present invention is described in detail below in conjunction with the drawings and specific embodiments.
The method for preparing silver peroxide superfine powder provided by the invention comprises following operation steps:
Step 1,
Preparation concentration is that silver nitrate solution and the concentration of 0.10mol/L～0.20mol/L is the sodium hydroxide solution of 0.6mol/L～5.6mol/L, and the volume ratio of silver nitrate solution and sodium hydroxide solution is 4:1;
Step 2,
Silver nitrate solution is moved in the three hole reactors, be heated to 25 ℃～55 ℃, start agitator simultaneously, under the stirring velocity of 2000r/min, sodium hydroxide solution is slowly added in the silver nitrate solution, obtain mixing solutions, the pale brown look active A g that separates out is arranged in this mixing solutions
2The O crystallite;
Step 3,
To analyse Ag
2The mixing solutions of O crystallite moves in the gas-liquid reactor, be controlled in temperature of reaction under 25～55 ℃ the condition, in gas-liquid reactor, feed ozone 1～5h by ozonizer, obtain black precipitate, filtering precipitate obtains the AgO wet-milling, with washed with de-ionized water AgO wet-milling, under 70～100 ℃ of conditions, dried 3～5 hours again, promptly obtain the ultra-fine silver peroxide powder of exsiccant.
By above-mentioned preparation method, obtain particle diameter and be the AgO powder about 200nm; Measuring its purity with inferior mn ion method is 50%～89%.
The method for preparing the AgO powder provided by the invention, by feed ozone in the Silver Nitrate basic solution, ozone and monovalence silver ions generation oxidizing reaction obtain purity height, few, the free of contamination ultra-fine silver peroxide powder of foreign ion.The method of comparing the existing AgO of preparation not only simple, the required cost of processing condition low, do not discharge pollutants, and purity height just can obtain having highly purified ultra-fine AgO powder as long as ozone feeds the time sufficiently long.In addition, the AgO powder of the present invention's preparation has very high stability at normal temperatures, just begins slowly to decompose when envrionment temperature is elevated to 170 ℃ to lose the Ag that oxygen forms+1 valency
2O, this ultra-fine AgO powder that shows that the present invention prepares has very high stability at normal temperatures.
Fig. 1 is that the ultra-fine silver peroxide powder of the inventive method preparation adopts Tianjin, island XRD-7000S type X-ray diffractometer to analyze the XRD figure spectrum of its crystalline structure gained.The Cu target is used in test, and tube voltage is 40kV, and electric current is 30mA, 10 °/min of sweep velocity, and the scanning angle scope is 20 °～90 °.The XRD data and the JCPDS standard card of test gained are compared, find this diffractogram and monoclinic AgO(PDF#43-1038) the diffractogram coupling, thereby confirm that the powder of preparation is monocline AgO.
Fig. 2 is that the ultra-fine silver peroxide powder of the inventive method preparation adopts JSM-6700FXIB type scanning electronic microscope its pattern, size to be analyzed the SEM figure of gained.As can be seen from the figure powder has the corynebacterium pattern, and its most of particulate diameter is about 200nm.
Fig. 3 is that the ultra-fine silver peroxide powder of the inventive method preparation adopts CPY-2P type high temperature difference thermal analyzer that its thermal decomposition process is carried out the DTA graphic representation that institute gets.As can be seen from the figure Zhi Bei AgO powder has very high stability at normal temperatures, just begins slowly to decompose when envrionment temperature is elevated to 170 ℃ to lose the Ag that oxygen forms+1 valency
2O, this shows that ultra-fine AgO has very high stability at normal temperatures.
Embodiment 1
The 0.10mol/L silver nitrate solution of 200mL is added in the three hole reactors of 500mL and place thermostat water bath to be heated to 25 ℃, start agitator simultaneously, under the 2000r/min stirring velocity, slowly add in silver nitrate solution by feeder the sodium hydroxide solution of the 0.6mol/L of 50mL, obtain mixing solutions, the pale brown look active A g that separates out is arranged in this mixing solutions
2The O crystallite.To analyse Ag then
2The mixing solutions of O crystallite moves in the gas-liquid reactor, be controlled in temperature of reaction under 25 ℃ the condition, in gas-liquid reactor, feed ozone 1h by ozonizer, obtain black precipitate, filtering precipitate obtains the AgO wet-milling, with washed with de-ionized water AgO wet-milling, under 70 ℃ of conditions, dried wet-milling 5 hours again, promptly obtain the ultra-fine silver peroxide powder of exsiccant.The content of AgO is 50.1% in inferior mn ion reduction method assay determination products therefrom.
Embodiment 2
The 0.15mol/L silver nitrate solution of 200mL is added in the three hole reactors of 500mL and place thermostat water bath to be heated to 35 ℃, start agitator simultaneously, under the 2000r/min stirring velocity, slowly add in silver nitrate solution by feeder the sodium hydroxide solution of the 3.6mol/L of 50mL, obtain mixing solutions, the pale brown look active A g that separates out is arranged in this mixing solutions
2The O crystallite.To analyse Ag then
2The mixing solutions of O crystallite moves in the gas-liquid reactor, be controlled in temperature of reaction under 35 ℃ the condition, in gas-liquid reactor, feed ozone 3h by ozonizer, obtain the precipitation of black, filtering precipitate obtains the AgO wet-milling, with washed with de-ionized water AgO wet-milling, under 90 ℃ of conditions, dried wet-milling 4 hours again, promptly obtain the ultra-fine silver peroxide powder of exsiccant.The content of AgO is 72% in inferior mn ion reduction method assay determination products therefrom.
Embodiment 3
The 0.2mol/L silver nitrate solution of 200mL is added in the three hole reactors of 500mL and place thermostat water bath to be heated to 55 ℃, start agitator simultaneously, under the 2000r/min stirring velocity, slowly add in silver nitrate solution by feeder the sodium hydroxide solution of the 5.6mol/L of 50mL, obtain mixing solutions, the pale brown look active A g that separates out is arranged in this mixing solutions
2The O crystallite.To analyse Ag then
2The mixing solutions of O crystallite moves in the gas-liquid reactor, be controlled in temperature of reaction under 55 ℃ the condition, in gas-liquid reactor, feed ozone 5h by ozonizer, obtain the precipitation of black, filtering precipitate obtains the AgO wet-milling, with washed with de-ionized water AgO wet-milling, the powder that oven dry obtains under 100 ℃ of conditions is 3 hours then, promptly obtains the ultra-fine silver peroxide powder of exsiccant.The content of AgO is 89% in inferior mn ion reduction method assay determination products obtained therefrom.
Claims (1)
1. a method for preparing silver peroxide superfine powder is characterized in that, comprises following operation steps:
Step 1,
Preparation concentration is that silver nitrate solution and the concentration of 0.10mol/L～0.20mol/L is the sodium hydroxide solution of 0.6mol/L～5.6mol/L, and the volume ratio of silver nitrate solution and sodium hydroxide solution is 4:1;
Step 2,
Silver nitrate solution is heated to 25 ℃～55 ℃, under the stirring velocity of 2000r/min, sodium hydroxide solution is added in the silver nitrate solution, obtain mixing solutions, the pale brown look active A g that separates out is arranged in this mixing solutions
2The O crystallite;
Step 3,
Temperature of reaction is controlled under 25～55 ℃ the condition, analysed Ag toward what step 2 obtained
2Fed ozone 1～5 hour in the mixing solutions of O crystallite, obtain black precipitate, filtering precipitate obtains the AgO wet-milling, with washed with de-ionized water AgO wet-milling, dries 3～5 hours under 70～100 ℃ of conditions again, promptly obtains exsiccant silver peroxide powder.
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| CN 201010153697 CN101811724A (en) | 2010-04-23 | 2010-04-23 | Method for preparing silver peroxide superfine powder |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102581289A (en) * | 2012-03-15 | 2012-07-18 | 中南大学 | Method for preparing monodisperse high-crystallinity silver powder |
| CN104263948A (en) * | 2014-10-16 | 2015-01-07 | 云南驰宏锌锗股份有限公司 | Method for recovering sliver from silver-bearing waste liquor |
| CN110563022A (en) * | 2019-08-29 | 2019-12-13 | 西安理工大学 | Monodisperse AgO hollow porous microsphere and preparation method and application thereof |
| CN114620690A (en) * | 2022-03-07 | 2022-06-14 | 中南大学 | Preparation method of silver peroxide positive electrode material for water-activated battery |
| CN115849431A (en) * | 2022-10-11 | 2023-03-28 | 贵州梅岭电源有限公司 | Zinc-silver battery and high-specific-capacity AgO positive electrode material thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59182228A (en) * | 1983-03-31 | 1984-10-17 | Mitsui Mining & Smelting Co Ltd | Silver (ii) peroxide and cell using the same |
| CN1994891A (en) * | 2006-01-06 | 2007-07-11 | 北京化工大学 | Chemical oxidation method for producing nano high valence silver oxide |
-
2010
- 2010-04-23 CN CN 201010153697 patent/CN101811724A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59182228A (en) * | 1983-03-31 | 1984-10-17 | Mitsui Mining & Smelting Co Ltd | Silver (ii) peroxide and cell using the same |
| CN1994891A (en) * | 2006-01-06 | 2007-07-11 | 北京化工大学 | Chemical oxidation method for producing nano high valence silver oxide |
Non-Patent Citations (1)
| Title |
|---|
| 《Polyhedron》 19821231 R. Dallenbach et al. Synthesis of silver (Ⅱ) oxide by oxidation of silver or silver oxide by means of ozone 183－186 1 第1卷, 第2期 2 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102581289A (en) * | 2012-03-15 | 2012-07-18 | 中南大学 | Method for preparing monodisperse high-crystallinity silver powder |
| CN104263948A (en) * | 2014-10-16 | 2015-01-07 | 云南驰宏锌锗股份有限公司 | Method for recovering sliver from silver-bearing waste liquor |
| CN110563022A (en) * | 2019-08-29 | 2019-12-13 | 西安理工大学 | Monodisperse AgO hollow porous microsphere and preparation method and application thereof |
| CN110563022B (en) * | 2019-08-29 | 2022-01-07 | 西安理工大学 | Monodisperse AgO hollow porous microsphere and preparation method and application thereof |
| CN114620690A (en) * | 2022-03-07 | 2022-06-14 | 中南大学 | Preparation method of silver peroxide positive electrode material for water-activated battery |
| CN115849431A (en) * | 2022-10-11 | 2023-03-28 | 贵州梅岭电源有限公司 | Zinc-silver battery and high-specific-capacity AgO positive electrode material thereof |
| WO2024077829A1 (en) * | 2022-10-11 | 2024-04-18 | 贵州梅岭电源有限公司 | Zinc-silver battery and high specific capacity ago positive electrode material thereof |
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Application publication date: 20100825 |