CN102259905A - Preparation method of superfine silver oxide - Google Patents
Preparation method of superfine silver oxide Download PDFInfo
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- CN102259905A CN102259905A CN2010101892671A CN201010189267A CN102259905A CN 102259905 A CN102259905 A CN 102259905A CN 2010101892671 A CN2010101892671 A CN 2010101892671A CN 201010189267 A CN201010189267 A CN 201010189267A CN 102259905 A CN102259905 A CN 102259905A
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- silver oxide
- sodium hydroxide
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- superfine
- silver
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Abstract
The invention discloses a preparation method of superfine silver oxide, comprising the following steps of: (1) dissolving silver nitrate into deionized water to prepare a silver nitrate solution; (2) weighing sodium hydroxide, and dissolving the sodium hydroxide into the deionized water to prepare a sodium hydroxide solution; (3) weighing dispersant rosin, adding the rosin into the sodium hydroxide solution, stirring and heating, standing after a saponification reaction to obtain mixed liquor; (4) adding the silver nitrite solution into the mixed liquor while stirring, and continuously stirring unit the reaction is completed so as to obtain a reaction mixture; (5) placing the reaction mixture into a filter, and washing the reaction mixture with the deionized water until the pH is close to be neutral so as to obtain a filtrate; and (6) carrying out centrifugal separation on the filtrate obtained in the step (4) to obtain silver oxide, and then drying the silver oxide in a vacuum drying oven to obtain the superfine silver oxide. In the invention, cheap rosin is taken as the dispersant, the superfine silver oxide with the grain size less than or equal to 5mu m can be prepared, and the preparing cost is lower.
Description
Technical field
The present invention relates to a kind of preparation method of superfine silver oxide.
Background technology
At present, ultrafine particulate and ultrafine powder become increasingly active in the application and the research of every field such as chemical industry, medicine, electronic technology.In the preparation process of ultrafine particle, dispersion agent is that the control particle size is in one of key factor of micron, nano level scope, also be the important factor of control coacervate size and distribution, use different dispersion agents can directly influence ultrafine particle size and character.In the process of preparation superfine silver oxide, people select a kind of as dispersion agent among polyvinyl alcohol (PVA), polyvinylpyrrolidone (PVP), alkyl sulfhydryl (RSH) or the polyethylene kind non-ionic dispersing agent DJ2004 mostly for use, yet these several dispersion agents all are not easy to obtain, the price comparison costliness, cause preparation cost higher, be not easy to promote.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of superfine silver oxide selects for use inexpensive rosin as dispersion agent, can make the superfine silver oxide of particle diameter≤5 μ m, and preparation cost is lower.
The object of the present invention is achieved like this:
A kind of preparation method of superfine silver oxide may further comprise the steps:
(1) Silver Nitrate is dissolved in the deionized water, is mixed with the silver nitrate solution that silver content is 40～60g/L;
(2) press Silver Nitrate: the weight ratio weighing sodium hydroxide of sodium hydroxide=1: 0.28～0.3, it is dissolved in the deionized water, be mixed with sodium hydroxide solution;
(3) by Silver Nitrate: the weight ratio of rosin=1: 0.005～0.01 takes by weighing rosin as disperser, and rosin is added in the middle prepared sodium hydroxide solution of step (2), and stirring heating leaves standstill after the saponification reaction, obtains mixed solution;
(4) in the mixed solution that in whipping step (3), prepares, the silver nitrate solution for preparing in the step (1) is added wherein, continue to be stirred to after adding and react completely, obtain reaction mixture;
(5) reaction mixture that obtains in the step (4) is put into strainer, extremely approaching neutral with deionized water wash simultaneously, obtain filtrate;
(6) filtrate that obtains in the step (4) is carried out obtaining silver suboxide after the centrifugation, put it into then and carry out drying in the vacuum drying oven, obtain superfine silver oxide.
Preferably, in the step of the present invention (2), the concentration of sodium hydroxide solution is 20～30%.
Preferably, in the step of the present invention (3), the temperature of heating is 50～80 ℃.The time of described saponification reaction is 0.5～1 hour.
Preferably, in the step of the present invention (4), the temperature the during mixed solution for preparing in the whipping step (3) is 50～80 ℃; Speed when adding Silver Nitrate is 1～3L/min, and the too fast words of adding speed can cause silver oxide particle inhomogeneous; The time of continuing to stir is 1.5～2 hours.
Preferably, in the step of the present invention (6), the temperature of vacuum drying oven is 80～90 ℃.
Therefore compared with prior art, the present invention has following beneficial effect:
The present invention adopts rosin can make the superfine silver oxide of particle diameter≤5 μ m as dispersion agent, and the rosin less expensive, obtains easily, so preparation cost is lower, promotes easily.
Embodiment
Describe the present invention in detail below in conjunction with specific embodiment, be used for explaining the present invention in this illustrative examples of the present invention and explanation, but not as a limitation of the invention.
Embodiment one
Prepare superfine silver oxide according to the following step:
(1) Silver Nitrate is dissolved in the deionized water, is mixed with the silver nitrate solution that silver content is 40g/L;
(2) press Silver Nitrate: the weight ratio weighing sodium hydroxide of sodium hydroxide=1: 0.28, it is dissolved in the deionized water, be mixed with concentration and be 30% sodium hydroxide solution;
(3) by Silver Nitrate: the weight ratio of rosin=1: 0.005 takes by weighing rosin as disperser, and rosin is added in the step (2) in the prepared sodium hydroxide solution, and stirring heating, Heating temperature are 50 ℃, and saponification reaction left standstill after 1 hour, obtained mixed solution;
(4) in the mixed solution that in whipping step (3), prepares, temperature during stirring is 50 ℃, and the silver nitrate solution for preparing in the step (1) is added wherein, and adding speed is 3L/min, continue after adding to stir 2 hours, obtain reaction mixture to reacting completely;
(5) reaction mixture that obtains in the step (4) is put into strainer, with deionized water wash extremely approaching neutral (pH value is near 7), obtain filtrate simultaneously;
(6) filtrate that obtains in the step (4) is carried out obtaining silver suboxide after the centrifugation, put it into temperature then and be in 90 ℃ the vacuum drying oven and carry out drying, obtain superfine silver oxide.
Embodiment two
Prepare superfine silver oxide according to the following step:
(1) Silver Nitrate is dissolved in the deionized water, is mixed with the silver nitrate solution that silver content is 60g/L;
(2) press Silver Nitrate: the weight ratio weighing sodium hydroxide of sodium hydroxide=1: 0.3, it is dissolved in the deionized water, be mixed with concentration and be 30% sodium hydroxide solution;
(3) by Silver Nitrate: the weight ratio of rosin=1: 0.01 takes by weighing rosin as disperser, and rosin is added in the step (2) in the prepared sodium hydroxide solution, and stirring heating, Heating temperature are 80 ℃, and saponification reaction left standstill after 0.5 hour, obtained mixed solution;
(4) in the mixed solution that in whipping step (3), prepares, temperature during stirring is 80 ℃, and the silver nitrate solution for preparing in the step (1) is added wherein, and adding speed is 1L/min, continue after adding to stir 1.5 hours, obtain reaction mixture to reacting completely;
(5) reaction mixture that obtains in the step (4) is put into strainer, with deionized water wash extremely approaching neutral (pH value is near 7), obtain filtrate simultaneously;
(6) filtrate that obtains in the step (4) is carried out obtaining silver suboxide after the centrifugation, put it into temperature then and be in 80 ℃ the vacuum drying oven and carry out drying, obtain superfine silver oxide.
Embodiment three
Prepare superfine silver oxide according to the following step:
(1) Silver Nitrate is dissolved in the deionized water, is mixed with the silver nitrate solution that silver content is 50g/L;
(2) press Silver Nitrate: the weight ratio weighing sodium hydroxide of sodium hydroxide=1: 0.29, it is dissolved in the deionized water, be mixed with concentration and be 25% sodium hydroxide solution;
(3) by Silver Nitrate: the weight ratio of rosin=1: 0.008 takes by weighing rosin as disperser, and rosin is added in the step (2) in the prepared sodium hydroxide solution, and stirring heating, Heating temperature are 60 ℃, and saponification reaction left standstill after 0.6 hour, obtained mixed solution;
(4) in the mixed solution that in whipping step (3), prepares, temperature during stirring is 70 ℃, and the silver nitrate solution for preparing in the step (1) is added wherein, and adding speed is 2L/min, continue after adding to stir 1.6 hours, obtain reaction mixture to reacting completely;
(5) reaction mixture that obtains in the step (4) is put into strainer, with deionized water wash extremely approaching neutral (pH value is near 7), obtain filtrate simultaneously;
(6) filtrate that obtains in the step (4) is carried out obtaining silver suboxide after the centrifugation, put it into temperature then and be in 85 ℃ the vacuum drying oven and carry out drying, obtain superfine silver oxide.
Embodiment four
Prepare superfine silver oxide according to the following step:
(1) Silver Nitrate is dissolved in the deionized water, is mixed with the silver nitrate solution that silver content is 56g/L;
(2) press Silver Nitrate: the weight ratio weighing sodium hydroxide of sodium hydroxide=1: 0.295, it is dissolved in the deionized water, be mixed with concentration and be 24% sodium hydroxide solution;
(3) by Silver Nitrate: the weight ratio of rosin=1: 0.009 takes by weighing rosin as disperser, and rosin is added in the step (2) in the prepared sodium hydroxide solution, and stirring heating, Heating temperature are 70 ℃, and saponification reaction left standstill after 0.8 hour, obtained mixed solution;
(4) in the mixed solution that in whipping step (3), prepares, temperature during stirring is 60 ℃, and the silver nitrate solution for preparing in the step (1) is added wherein, and adding speed is 2.5L/min, continue after adding to stir 1.8 hours, obtain reaction mixture to reacting completely;
(5) reaction mixture that obtains in the step (4) is put into strainer, with deionized water wash extremely approaching neutral (pH value is near 7), obtain filtrate simultaneously;
(6) filtrate that obtains in the step (4) is carried out obtaining silver suboxide after the centrifugation, put it into temperature then and be in 88 ℃ the vacuum drying oven and carry out drying, obtain superfine silver oxide.
More than the technical scheme that the embodiment of the invention provided is described in detail, used specific case herein the principle and the embodiment of the embodiment of the invention are set forth, the explanation of above embodiment only is applicable to the principle that helps to understand the embodiment of the invention; Simultaneously, for one of ordinary skill in the art, according to the embodiment of the invention, the part that on embodiment and range of application, all can change, in sum, this description should not be construed as limitation of the present invention.
Claims (8)
1. the preparation method of a superfine silver oxide is characterized in that may further comprise the steps:
(1) Silver Nitrate is dissolved in the deionized water, is mixed with the silver nitrate solution that silver content is 40～60g/L;
(2) press Silver Nitrate: the weight ratio weighing sodium hydroxide of sodium hydroxide=1: 0.28～0.3, it is dissolved in the deionized water, be mixed with sodium hydroxide solution;
(3) by Silver Nitrate: the weight ratio of rosin=1: 0.005～0.01 takes by weighing rosin as disperser, and rosin is added in the middle prepared sodium hydroxide solution of step (2), and stirring heating leaves standstill after the saponification reaction, obtains mixed solution;
(4) in the mixed solution that in whipping step (3), prepares, the silver nitrate solution for preparing in the step (1) is added wherein, continue to be stirred to after adding and react completely, obtain reaction mixture;
(5) reaction mixture that obtains in the step (4) is put into strainer, extremely approaching neutral with deionized water wash simultaneously, obtain filtrate;
(6) filtrate that obtains in the step (4) is carried out obtaining silver suboxide after the centrifugation, put it into then and carry out drying in the vacuum drying oven, obtain superfine silver oxide.
2. the preparation method of superfine silver oxide according to claim 1, it is characterized in that: in the described step (2), the concentration of sodium hydroxide solution is 20～30%.
3. the preparation method of superfine silver oxide according to claim 1, it is characterized in that: in the described step (3), the temperature of heating is 50～80 ℃.
4. the preparation method of superfine silver oxide according to claim 1, it is characterized in that: in the described step (3), the time of saponification reaction is 0.5～1 hour.
5. the preparation method of superfine silver oxide according to claim 1 is characterized in that: in the described step (4), the temperature the during mixed solution for preparing in the whipping step (3) is 50～80 ℃.
6. the preparation method of the described superfine silver oxide of claim 1 is characterized in that: in the described step (4), the speed when adding Silver Nitrate is 1～3L/min.
7. the preparation method of the described superfine silver oxide of claim 1 is characterized in that: in the described step (4), the time of continuing to stir is 1.5～2 hours.
8. the preparation method of the described superfine silver oxide of claim 1, it is characterized in that: in the described step (6), the temperature of vacuum drying oven is 80～90 ℃.
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| CN2010101892671A CN102259905A (en) | 2010-05-26 | 2010-05-26 | Preparation method of superfine silver oxide |
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| CN2010101892671A CN102259905A (en) | 2010-05-26 | 2010-05-26 | Preparation method of superfine silver oxide |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103058260A (en) * | 2012-12-29 | 2013-04-24 | 安徽师范大学 | Preparation method for belt-shaped silver oxide nano array |
| CN104787795A (en) * | 2015-04-14 | 2015-07-22 | 东华理工大学 | Method for preparing micro silver oxide |
| CN107433139A (en) * | 2017-06-07 | 2017-12-05 | 常州市绿意管道有限公司 | A kind of preparation method of anti-clogging antibacterial type charged nanofiltration membrane |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1308102A (en) * | 2001-02-07 | 2001-08-15 | 南京大学 | Nanometer level silver oxide and its production process |
| CN1565976A (en) * | 2003-06-10 | 2005-01-19 | 中国乐凯胶片集团公司 | Nano-class silver oxide and preparation method thereof |
| CN101707062A (en) * | 2009-12-03 | 2010-05-12 | 北京有色金属研究总院 | Nano-silver powder, manufacturing method and application thereof |
-
2010
- 2010-05-26 CN CN2010101892671A patent/CN102259905A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1308102A (en) * | 2001-02-07 | 2001-08-15 | 南京大学 | Nanometer level silver oxide and its production process |
| CN1565976A (en) * | 2003-06-10 | 2005-01-19 | 中国乐凯胶片集团公司 | Nano-class silver oxide and preparation method thereof |
| CN101707062A (en) * | 2009-12-03 | 2010-05-12 | 北京有色金属研究总院 | Nano-silver powder, manufacturing method and application thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103058260A (en) * | 2012-12-29 | 2013-04-24 | 安徽师范大学 | Preparation method for belt-shaped silver oxide nano array |
| CN103058260B (en) * | 2012-12-29 | 2014-10-15 | 安徽师范大学 | Preparation method for belt-shaped silver oxide nano array |
| CN104787795A (en) * | 2015-04-14 | 2015-07-22 | 东华理工大学 | Method for preparing micro silver oxide |
| CN104787795B (en) * | 2015-04-14 | 2016-08-31 | 东华理工大学 | A kind of method preparing micron silver oxide |
| CN107433139A (en) * | 2017-06-07 | 2017-12-05 | 常州市绿意管道有限公司 | A kind of preparation method of anti-clogging antibacterial type charged nanofiltration membrane |
| CN107433139B (en) * | 2017-06-07 | 2020-06-16 | 深圳市益嘉昇科技有限公司 | Preparation method of anti-blocking bacteriostatic charged nanofiltration membrane |
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Application publication date: 20111130 |