CN1244497C - Prepn of nano silver oxide particle - Google Patents
Prepn of nano silver oxide particle Download PDFInfo
- Publication number
- 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
- Authority
- CN
- China
- Prior art keywords
- solution
- silver
- concentration
- weight
- deionized water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
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- 239000002245 particle Substances 0.000 title claims abstract description 22
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 14
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Substances [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 title abstract description 7
- 229910001923 silver oxide Inorganic materials 0.000 title abstract description 5
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 150000002500 ions Chemical class 0.000 claims abstract description 12
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 44
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 42
- 229910052709 silver Inorganic materials 0.000 claims description 11
- 239000004332 silver Substances 0.000 claims description 11
- 238000001556 precipitation Methods 0.000 claims description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- 229920002125 Sokalan® Polymers 0.000 claims description 4
- 239000012670 alkaline solution Substances 0.000 claims description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 4
- 239000004584 polyacrylic acid Substances 0.000 claims description 4
- -1 polyoxyethylene Polymers 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000000926 separation method Methods 0.000 abstract description 5
- 239000002270 dispersing agent Substances 0.000 abstract description 4
- 238000005054 agglomeration Methods 0.000 abstract description 3
- 230000002776 aggregation Effects 0.000 abstract description 3
- PLKATZNSTYDYJW-UHFFFAOYSA-N azane silver Chemical compound N.[Ag] PLKATZNSTYDYJW-UHFFFAOYSA-N 0.000 abstract 2
- 239000002244 precipitate Substances 0.000 abstract 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- 239000003513 alkali Substances 0.000 abstract 1
- 229910000108 silver(I,III) oxide Inorganic materials 0.000 description 8
- 238000002156 mixing Methods 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
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 |
|---|---|---|---|
| CN 03151210 Expired - Fee Related CN1244497C (en) | 2003-09-23 | 2003-09-23 | Prepn of nano silver oxide particle |
Country Status (1)
| Country | Link |
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| CN (1) | CN1244497C (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100500573C (en) * | 2007-04-04 | 2009-06-17 | 厦门大学 | A preparation method with controllable shape and size 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 |
| CN118620429A (en) * | 2024-06-27 | 2024-09-10 | 广东砂鸵涂料科技有限公司 | Inorganic coating with antibacterial and antiviral functions and preparation method thereof |
-
2003
- 2003-09-23 CN CN 03151210 patent/CN1244497C/en not_active Expired - Fee Related
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| Publication number | Publication date |
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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 |