CN1244497C - Prepn of nano silver oxide particle - Google Patents
Prepn of nano silver oxide particle Download PDFInfo
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- CN1244497C CN1244497C CN 03151210 CN03151210A CN1244497C CN 1244497 C CN1244497 C CN 1244497C CN 03151210 CN03151210 CN 03151210 CN 03151210 A CN03151210 A CN 03151210A CN 1244497 C CN1244497 C CN 1244497C
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- silver
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- deionized water
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Abstract
The present invention discloses a method for preparing nano silver oxide particles, which comprises the following steps that silver nitrate is dissolved in deionized water to prepare a solution with the concentration of 0.2 mol/L to 4.0 mol/L; an organic dispersing agent with the proportion of 1% to 10% by weight ratio is added into the solution; then, the solution is stirred violently, and simultaneously 5% to 15% of ammonia water by weight ratio with the weight percentage concentration of 25% is dropped into the solution to form a silver-ammonia complex ion solution; subsequently, the silver-ammonia complex ion solution is stirred violently, and simultaneously is dropped into an alkali solution with the concentration of 0.5 mol/L to 3.0 mol/L to form precipitates; the precipitates are taken out through centrifugal separation, washed with deionized water for a plurality of times, frozen and dried. The nano silver oxide particles prepared by the method of the present invention have the advantages of high purity and high stability; the particle size is between 10 nm to 100 nm, and basically no agglomeration phenomenon occurs.
Description
Technical field
The present invention relates to prepare nano phase ag_2 o particulate method.
Background technology
Silver suboxide (Ag2O) can be widely used in electronic devices and components, button cell, sanitas, antiseptic-germicide, glass colorant and industries such as abrasive and chemical catalyst.Wherein silver suboxide is in the consumption maximum of electronic devices and components industry.The production of current silver suboxide mainly is the silver suboxide precipitation that obtains with the reaction of silver nitrate solution and sodium hydroxide solution, washs, separates and drying obtains silver oxide particle.The subject matter that exists in the silver suboxide production at present is:
1) purity of silver suboxide product is not high enough, often contains partial impurities;
2) granularity of silver oxide particle is big and size-grade distribution is inhomogeneous.And in the practical application, no matter be as the silver slurry or as antiseptic-germicide, chemical catalyst, all require silver suboxide to have little granularity.
Summary of the invention
The object of the present invention is to provide preparation nano phase ag_2 o particulate method, to obtain purity height, nano phase ag_2 o particle stable, that disperse better and narrow particle size distribution.
Preparation nano phase ag_2 o particulate method of the present invention may further comprise the steps:
Silver Nitrate is dissolved in is mixed with the solution that concentration is 0.2mol/L～4.0mol/L in the deionized water, 1%～10% ratio adds organic dispersing agent by weight in this solution, then in vigorous stirring by weight 5%～15% ratio to drip weight percent concentration be that 25% ammoniacal liquor forms silver ammino ion solution; After this in vigorous stirring, this drips of solution is added in the alkaline solution that concentration is 0.5mol/L～3.0mol/L, forms precipitation; Take out precipitation and for several times by centrifugation again with deionized water wash, lyophilize, the nano phase ag_2 o particle.
Above-mentioned organic dispersing agent can be the polyacrylic acid of molecular weight between 200～30000, molecular weight between 200～40000 polyoxyethylene glycol or molecular weight at 1000～30000 polyvinyl alcohol.Alkaline solution can adopt sodium hydroxide solution or potassium hydroxide solution.
The present invention adopts wet-chemical to make a kind of nano phase ag_2 o particle comparatively easily in conjunction with heat-treating methods, its granular size is between 10 nanometer to 100 nanometers, and granule stability is good, less reunion, narrow particle size distribution, and granularity can be controlled by the variation of experiment condition.Owing to adopt organic dispersing agent, solved the problem that particle is easily grown up and primary particle is easy to reunite that is settled out in the co-precipitation effectively.Simultaneously, adopt freeze-drying to solve the problem of particle agglomeration in the drying process effectively in the preparation process.Therefore, the grain graininess of finally preparing is little and even, does not have agglomeration substantially.
Embodiment
Further specify the present invention below in conjunction with example.
Embodiment 1
Silver Nitrate is dissolved in the solution that forms 0.3mol/L in the deionized water, in silver nitrate solution by weight 4% ratio to add molecular weight be 1000 polyacrylic acid, forming behind the mixing solutions therein 5% ratio by weight, to add weight percent concentration be 25% ammoniacal liquor, forms silver ammino ion solution; Dissolution of sodium hydroxide in going to form 1.0mol/L solution in dried up, is added to the silver ammino ion drips of solution in the sodium hydroxide solution in the vigorous stirring sodium hydroxide solution, forms precipitation.To precipitate with centrifugal separation and take out, with deionized water wash three times, through lyophilize, the nano phase ag_2 o particle of particle diameter between 10 nanometers～30 nanometers.
Embodiment 2
Silver Nitrate is dissolved in the solution that forms 1.5mol/L in the deionized water, in silver nitrate solution by weight 7% ratio to add molecular weight be 5000 polyoxyethylene glycol, forming behind the mixing solutions therein 10% ratio by weight, to add weight percent concentration be 25% ammoniacal liquor, forms silver ammino ion solution; Dissolution of sodium hydroxide in going to form 1.5mol/L solution in dried up, is added to the silver ammino ion drips of solution in the sodium hydroxide solution in the vigorous stirring sodium hydroxide solution, forms precipitation.To precipitate with centrifugal separation and take out, with deionized water wash three times, through lyophilize, the nano phase ag_2 o particle of particle diameter between 30 nanometers～60 nanometers.
Embodiment 3
Silver Nitrate is dissolved in the solution that forms 0.5mol/L in the deionized water, in silver nitrate solution by weight 5% ratio to add molecular weight be 2000 polyacrylic acid, forming behind the mixing solutions therein 5% ratio by weight, to add weight percent concentration be 25% ammoniacal liquor, forms silver ammino ion solution; Potassium hydroxide is dissolved in the dried up middle 1.0mol/L of formation solution, in the vigorous stirring sodium hydroxide solution, the silver ammino ion drips of solution is added in the sodium hydroxide solution, form precipitation.To precipitate with centrifugal separation and take out, with deionized water wash three times, through lyophilize, the nano phase ag_2 o particle of particle diameter between 20 nanometers～60 nanometers.
Embodiment 4
Silver Nitrate is dissolved in the solution that forms 2.0mol/L in the deionized water, in silver nitrate solution by weight 9% ratio to add molecular weight be 10000 polyvinyl alcohol, forming behind the mixing solutions therein 10% ratio by weight, to add weight percent concentration be 25% ammoniacal liquor, forms silver ammino ion solution; Dissolution of sodium hydroxide in going to form 2.0mol/L solution in dried up, is added to the silver ammino ion drips of solution in the sodium hydroxide solution in the vigorous stirring sodium hydroxide solution, forms precipitation.To precipitate with centrifugal separation and take out, with deionized water wash three times, through lyophilize, the nano phase ag_2 o particle of particle diameter between 60 nanometers～90 nanometers.
Claims (2)
1. one kind prepares nano phase ag_2 o particulate method, it is characterized in that may further comprise the steps:
Silver Nitrate is dissolved in is mixed with the solution that concentration is 0.2mol/L～4.0mol/L in the deionized water, 1%～10% ratio adds polyacrylic acid, polyoxyethylene glycol or polyvinyl alcohol by weight in this solution, then in vigorous stirring by weight 5%～15% ratio to drip weight percent concentration be that 25% ammoniacal liquor forms silver ammino ion solution; After this in vigorous stirring, this drips of solution is added in the alkaline solution that concentration is 0.5mol/L～3.0mol/L, forms precipitation; Take out precipitation and for several times by centrifugation again with deionized water wash, lyophilize gets the nano phase ag_2 o particle, and said polyacrylic molecular weight is between 200～30000, the molecular weight of polyoxyethylene glycol is between 200～40000, and the molecular weight of polyvinyl alcohol is between 1000～30000.
2. preparation nano phase ag_2 o particulate method according to claim 1 is characterized in that said alkaline solution is sodium hydroxide solution or potassium hydroxide solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03151210 CN1244497C (en) | 2003-09-23 | 2003-09-23 | Prepn of nano silver oxide particle |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03151210 CN1244497C (en) | 2003-09-23 | 2003-09-23 | Prepn of nano silver oxide particle |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1526643A CN1526643A (en) | 2004-09-08 |
| CN1244497C true CN1244497C (en) | 2006-03-08 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
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| CN 03151210 Expired - Fee Related CN1244497C (en) | 2003-09-23 | 2003-09-23 | Prepn of nano silver oxide particle |
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| CN (1) | CN1244497C (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100500573C (en) * | 2007-04-04 | 2009-06-17 | 厦门大学 | Shape and size controllable preparation method of micro-nano silver oxide |
| CN101698500B (en) * | 2009-11-03 | 2011-12-28 | 宁波晶鑫电子材料有限公司 | Method for preparing micron-sized silver oxide powder with porous structure |
| CN107577090B (en) * | 2017-09-26 | 2021-02-19 | 京东方科技集团股份有限公司 | Display panel, manufacturing method thereof and display device |
| CN108452591A (en) * | 2018-04-27 | 2018-08-28 | 佛山市日日圣科技有限公司 | A kind of preparation method of antibacterial type water purification carbon fiber |
| CN109497049A (en) * | 2018-11-12 | 2019-03-22 | 上海聚治新材料科技有限公司 | A kind of preparation method of high efficiency preparation high concentration silver antibacterial water |
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2003
- 2003-09-23 CN CN 03151210 patent/CN1244497C/en not_active Expired - Fee Related
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| CN1526643A (en) | 2004-09-08 |
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Owner name: SHANGHAI HUASHI NANO MATERIALS CO., LTD. Free format text: FORMER OWNER: WENG WENJIAN; HUANG DEHUAN; HAN GAORONG Effective date: 20061013 |
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Effective date of registration: 20061013 Address after: 201108, A building, Xin Mei Industrial Zone, No. 260, Cao Cao Road, Shanghai, Minhang District Patentee after: Shanghai Huashi Nano Material Co., Ltd. Address before: 310031 No. 20, Zhejiang Road, Hangzhou, Zhejiang, Xihu District Co-patentee before: Huang Dehuan Patentee before: Weng Wenjian Co-patentee before: Han Gaorong |
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Granted publication date: 20060308 Termination date: 20110923 |