CN1557163A - Nano antiseptic silver powder preparation method using metallic silver - Google Patents
Nano antiseptic silver powder preparation method using metallic silver Download PDFInfo
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- CN1557163A CN1557163A CNA200410016340XA CN200410016340A CN1557163A CN 1557163 A CN1557163 A CN 1557163A CN A200410016340X A CNA200410016340X A CN A200410016340XA CN 200410016340 A CN200410016340 A CN 200410016340A CN 1557163 A CN1557163 A CN 1557163A
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- silver
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- aqueous solution
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 24
- 239000004332 silver Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 230000002421 anti-septic effect Effects 0.000 title abstract 5
- 239000002245 particle Substances 0.000 claims abstract description 30
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims abstract description 19
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 16
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 7
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 38
- 239000007864 aqueous solution Substances 0.000 claims description 36
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 19
- 239000000243 solution Substances 0.000 claims description 18
- 239000002202 Polyethylene glycol Substances 0.000 claims description 12
- 229920001223 polyethylene glycol Polymers 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 239000011734 sodium Substances 0.000 claims description 10
- 229910052708 sodium Inorganic materials 0.000 claims description 10
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 8
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 8
- 239000010977 jade Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 6
- 238000002161 passivation Methods 0.000 claims description 6
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 6
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 6
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 6
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims description 4
- 239000012752 auxiliary agent Substances 0.000 claims description 4
- 235000019830 sodium polyphosphate Nutrition 0.000 claims description 4
- 239000002671 adjuvant Substances 0.000 claims description 2
- 239000000843 powder Substances 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 239000004744 fabric Substances 0.000 abstract description 2
- 229920003023 plastic Polymers 0.000 abstract description 2
- 239000004033 plastic Substances 0.000 abstract description 2
- 239000000919 ceramic Substances 0.000 abstract 1
- 239000003638 chemical reducing agent Substances 0.000 abstract 1
- 230000015271 coagulation Effects 0.000 abstract 1
- 238000005345 coagulation Methods 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 239000003973 paint Substances 0.000 abstract 1
- 229920000151 polyglycol Polymers 0.000 abstract 1
- 239000010695 polyglycol Substances 0.000 abstract 1
- 239000007921 spray Substances 0.000 abstract 1
- 230000000844 anti-bacterial effect Effects 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000010946 fine silver Substances 0.000 description 4
- 238000001914 filtration Methods 0.000 description 3
- 239000003242 anti bacterial agent Substances 0.000 description 2
- 229940088710 antibiotic agent Drugs 0.000 description 2
- 230000003115 biocidal effect Effects 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- 231100000957 no side effect Toxicity 0.000 description 2
- 229920000137 polyphosphoric acid Polymers 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002147 killing effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- -1 pottery Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
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- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The preparation process of nano antiseptic silver powder with metal silver features that solution containing nano sliver particle is first obtained with metal silver, nitric acid and polyglycol as main material, hydrazine hydrate as reductant, and proper amount of surface assistant; and then deactivated and spray dried to obtain nano antiseptic silver powder with silver content of 60-90 %. The process has easy-to-obtain material, simple operation, low cost and easy application in industrial production, and the prepared nano silver powder has no coagulation and nano sliver size of 10-100 nm. The nano antiseptic silver powder may be used in antiseptic fabric, plastic, ceramic, paint, medical dressing and other fields.
Description
Technical field
The present invention relates to a kind of method for preparing nano-antibacterial silver powder, particularly prepare the method for nano-antibacterial silver powder with argent.
Background technology
Mercury, silver are the strongest metals of sterilization functions.Because mercury all has serious harm to human body and environment, can not be used as anti-biotic material.Therefore, silver becomes the optimal selection of preparation anti-biotic material.Silver has very strong antibacterial ability, and bacterium, fungi, mould etc. are all had very strong killing action, the people is had no side effect, its antibacterial functions have wide spectrum, long-acting, safely, characteristics such as have no side effect, thereby be subjected to the attention of height.When the silver particles diameter was reduced to nano-scale, its specific surface area increased greatly, increased activity, and antibacterial efficacy also strengthens thereupon.Therefore, little, the finely disseminated silver powder of prepared sizes is the key that improves silver-colored antibacterial efficacy.At present, when preparing nano-silver powder, adopt precipitation, filtration, oven drying method to obtain silver powder with chemical method.In fact, finely disseminated nano-silver powder can not precipitate in considerable time, can not with common filtration method with itself and moisture from.Have only big when silver particles, just can precipitate after reuniting, also could with filtration method with itself and moisture from.On the other hand, when preparing nano-silver powder, be raw material with the silver nitrate usually with chemical method, cost is higher.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing nano-antibacterial silver powder with argent.
Method step is as follows
1) be that 0.01～3.0% surperficial adjuvant water solution and concentration are that to add concentration be behind 0.01～3.0% the silver nitrate aqueous solution for 0.01～3.0% the polyethylene glycol aqueous solution with mass percent concentration, in stirring, add concentration lentamente and be 0.001～1.0% hydrazine hydrate aqueous solution, the mol ratio of silver nitrate, surperficial auxiliary agent, polyethylene glycol, hydrazine hydrate is 1.0: 0.001～0.2: 0.0001～0.015: 0.5～1.5, when the pH value reaches 6.5～7.5, stop to add hydrazine hydrate aqueous solution, continue to stir 10～30 minutes, obtain to contain the solution of nano silver particles;
2) with the above-mentioned solution left standstill that contains nano silver particles 6 to 12 hours, the passivation nano silver particles;
3) atomized drying obtains silver content 60～90% nano-antibacterial silver powder, and the granularity of silver particles is 10～100nm;
2. according to claim 1ly a kind ofly prepare the method for nano-antibacterial silver powder, it is characterized in that said silver nitrate aqueous solution is formed by argent and dilute nitric acid reaction with argent, the reaction later stage, solution is heated to 40～60 ℃, stop until reaction;
3. according to claim 1ly a kind ofly prepare the method for nano-antibacterial silver powder, it is characterized in that said surperficial auxiliary agent is one or more in polyvinylpyrrolidone, sodium polyphosphate, lauryl sodium sulfate, the dodecyl semi-annular jade pendant acid sodium with argent.
Advantage of the present invention is: be feedstock production nano-antibacterial silver powder with the argent, raw material are easy to get, preparation technology is simple, lower, the easy industrialization of cost.The nano-silver powder of this method preparation can not take place to reunite in depositing and particle is grown up, and is convenient to preserve and use.The granularity of the silver particles of preparation is 10～100nm, good dispersion, can be used on fields such as antibacterial fabric, plastics, pottery, coating, Medical dressing.
Description of drawings
Fig. 1 is the X-ray diffractogram of Nano Silver in the embodiment of the invention 1, and the diffraction maximum of mark " * " number is the diffraction maximum of silver;
Fig. 2 is the transmission electron micrograph of Nano Silver in the embodiment of the invention 1, and the upper right corner of figure is the SEAD figure of this zone silver particles.
Embodiment
Embodiment 1
1) the 10g fine silver being put into 25.5ml concentration is 15% nitric acid, is heated to 60 ℃, stops until reaction, obtains mass percent concentration and be 39.2% silver nitrate aqueous solution;
2) with the 50ml mass percent concentration be 0.05% the polyvinylpyrrolidone aqueous solution, 10ml concentration is 0.01% lauryl sodium sulfate aqueous solution, 10ml concentration is that to join 50ml concentration be behind 0.2% the silver nitrate aqueous solution for 0.01% the polyethylene glycol aqueous solution, add deionized water to 200ml, in stirring, add 200ml concentration lentamente and be 0.008% hydrazine hydrate aqueous solution, silver nitrate, polyvinylpyrrolidone, lauryl sodium sulfate, polyethylene glycol, the mol ratio of hydrazine hydrate is 1.0: 0.0042: 006: 0.0002: 0.54, when the pH value reaches 7.0, stop to add hydrazine hydrate aqueous solution, continue to stir 10 minutes, obtain to contain the solution of nano silver particles;
3) with the above-mentioned solution left standstill that contains nano silver particles 12 hours, the passivation nano silver particles;
4) obtain the nano-antibacterial silver powder of silver content 90% after the drying, the granularity of silver particles is 28nm;
Embodiment 2
1) the 10g fine silver being put into 25.5ml concentration is 15% nitric acid, is heated to 55 ℃, stops until reaction, obtains mass percent concentration and be 39.2% silver nitrate aqueous solution;
2) with the 20ml mass percent concentration be 0.2% polyphosphoric acids sodium water solution, 50ml concentration is 0.05% dodecyl semi-annular jade pendant acid sodium aqueous solution, 20ml concentration is that to join 50ml concentration be behind 0.5% the silver nitrate aqueous solution for 0.2% the polyethylene glycol aqueous solution, add deionized water to 200ml, in stirring, add 200ml concentration lentamente and be 0.03% hydrazine hydrate aqueous solution, silver nitrate, sodium polyphosphate, dodecyl semi-annular jade pendant acid sodium, polyethylene glycol, the mol ratio of hydrazine hydrate is 1.0: 0.074: 0.062: 0.0003: 0.82, when the pH value reaches 7.0, stop to add hydrazine hydrate aqueous solution, continue to stir 10 minutes, obtain to contain the solution of nano silver particles;
3) with the above-mentioned solution left standstill that contains nano silver particles 12 hours, the passivation nano silver particles;
4) obtain the nano-antibacterial silver powder of silver content 60% after the drying, the granularity of silver particles is 26nm;
Embodiment 3
1) the 10g fine silver being put into 21.3ml concentration is 18% nitric acid, is heated to 50 ℃, stops until reaction, obtains mass percent concentration and be 46.9% silver nitrate aqueous solution;
2) with the 20ml mass percent concentration be 0.1% the polyvinylpyrrolidone aqueous solution, 10ml concentration is 0.01% dodecyl semi-annular jade pendant acid sodium aqueous solution, 10ml concentration is that to join 50ml concentration be behind 0.2% the silver nitrate aqueous solution for 0.003% the polyethylene glycol aqueous solution, add deionized water to 200ml, in stirring, add 200ml concentration lentamente and be 0.01% hydrazine hydrate aqueous solution, silver nitrate, polyvinylpyrrolidone, dodecyl semi-annular jade pendant acid sodium, polyethylene glycol, the mol ratio of hydrazine hydrate is 1.0: 0.0034: 0062: 0.0001: 0.68, when the pH value reaches 7.0, stop to add hydrazine hydrate aqueous solution, continue to stir 10 minutes, obtain to contain the solution of nano silver particles;
3) with the above-mentioned solution left standstill that contains nano silver particles 12 hours, the passivation nano silver particles;
4) obtain the nano-antibacterial silver powder of silver content 75% after the drying, the granularity of silver particles is 25nm.
Embodiment 4
1) the 10g fine silver being put into 19.1ml concentration is 20% nitric acid, is heated to 50 ℃, stops until reaction, obtains mass percent concentration and be 52.4% silver nitrate aqueous solution;
2) with the 20ml mass percent concentration be 0.2% polyphosphoric acids sodium water solution, 50ml concentration is 0.05% dodecyl semi-annular jade pendant acid sodium aqueous solution, 20ml concentration is that to join 50ml concentration be behind 0.2% the silver nitrate aqueous solution for 0.02% the polyethylene glycol aqueous solution, add deionized water to 200ml, in stirring, add 200ml concentration lentamente and be 0.05% hydrazine hydrate aqueous solution, silver nitrate, sodium polyphosphate, dodecyl semi-annular jade pendant acid sodium, polyethylene glycol, the mol ratio of hydrazine hydrate is 1.0: 0.074: 0.062: 0.0003: 1.37, when the pH value reaches 7.0, stop to add hydrazine hydrate aqueous solution, continue to stir 10 minutes, obtain to contain the solution of nano silver particles;
3) with the above-mentioned solution left standstill that contains nano silver particles 12 hours, the passivation nano silver particles;
4) obtain the nano-antibacterial silver powder of silver content 60% after the drying, the granularity of silver particles is 30nm.
Claims (3)
1. one kind prepares the method for nano-antibacterial silver powder with argent, it is characterized in that the step of method is
1) be that 0.01～3.0% surperficial adjuvant water solution and concentration are that to add concentration be behind 0.01～3.0% the silver nitrate aqueous solution for 0.01～3.0% the polyethylene glycol aqueous solution with mass percent concentration, in stirring, add concentration lentamente and be 0.001～1.0% hydrazine hydrate aqueous solution, the mol ratio of silver nitrate, surperficial auxiliary agent, polyethylene glycol, hydrazine hydrate is 1.0: 0.001～0.2: 0.0001～0.015: 0.5～1.5, when the pH value reaches 6.5～7.5, stop to add hydrazine hydrate aqueous solution, continue to stir 10～30 minutes, obtain to contain the solution of nano silver particles;
2) with the above-mentioned solution left standstill that contains nano silver particles 6 to 12 hours, the passivation nano silver particles;
3) atomized drying obtains silver content 60～90% nano-antibacterial silver powder, and the granularity of silver particles is 10～100nm;
2. according to claim 1ly a kind ofly prepare the method for nano-antibacterial silver powder, it is characterized in that said silver nitrate aqueous solution is formed by argent and dilute nitric acid reaction with argent, the reaction later stage, solution is heated to 40～60 ℃, stop until reaction;
3. according to claim 1ly a kind ofly prepare the method for nano-antibacterial silver powder, it is characterized in that said surperficial auxiliary agent is one or more in polyvinylpyrrolidone, sodium polyphosphate, lauryl sodium sulfate, the dodecyl semi-annular jade pendant acid sodium with argent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200410016340XA CN1299578C (en) | 2004-02-13 | 2004-02-13 | Nano antiseptic silver powder preparation method using metallic silver |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200410016340XA CN1299578C (en) | 2004-02-13 | 2004-02-13 | Nano antiseptic silver powder preparation method using metallic silver |
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| Publication Number | Publication Date |
|---|---|
| CN1557163A true CN1557163A (en) | 2004-12-29 |
| CN1299578C CN1299578C (en) | 2007-02-14 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB200410016340XA Expired - Fee Related CN1299578C (en) | 2004-02-13 | 2004-02-13 | Nano antiseptic silver powder preparation method using metallic silver |
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| Country | Link |
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| CN (1) | CN1299578C (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101862837A (en) * | 2010-07-02 | 2010-10-20 | 中国乐凯胶片集团公司 | Preparation method for silver powder |
| CN102114546A (en) * | 2011-03-29 | 2011-07-06 | 兰州金川新材料科技股份有限公司 | Method for preparing spherical silver powder |
| CN102220045A (en) * | 2010-04-16 | 2011-10-19 | 上海亿金纳米科技有限公司 | Low-temperature-sintered solvent-based nano-silver electroconductive ink and preparation process thereof |
| CN103355349A (en) * | 2013-06-27 | 2013-10-23 | 南京市荣达树脂有限公司 | Preparation method of antibacterial powders for antibacterial coating |
| CN106176810A (en) * | 2016-07-13 | 2016-12-07 | 长沙迪谷纳米生物科技有限公司 | Medicinal nano material compositions DG 5 is for the purposes of antimicrobial agent |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63213606A (en) * | 1987-03-02 | 1988-09-06 | Daido Steel Co Ltd | Production of fine silver powder |
| CZ279525B6 (en) * | 1991-08-23 | 1995-05-17 | Glazura S.P. | Process for producing silver powder |
| JPH07118868A (en) * | 1993-10-20 | 1995-05-09 | Sumitomo Metal Mining Co Ltd | Production of palladium-coated spherical silver powder |
| CN1266761A (en) * | 2000-03-23 | 2000-09-20 | 南京大学 | Process for preparing nm-class silver powder |
-
2004
- 2004-02-13 CN CNB200410016340XA patent/CN1299578C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102220045A (en) * | 2010-04-16 | 2011-10-19 | 上海亿金纳米科技有限公司 | Low-temperature-sintered solvent-based nano-silver electroconductive ink and preparation process thereof |
| CN101862837A (en) * | 2010-07-02 | 2010-10-20 | 中国乐凯胶片集团公司 | Preparation method for silver powder |
| CN102114546A (en) * | 2011-03-29 | 2011-07-06 | 兰州金川新材料科技股份有限公司 | Method for preparing spherical silver powder |
| CN103355349A (en) * | 2013-06-27 | 2013-10-23 | 南京市荣达树脂有限公司 | Preparation method of antibacterial powders for antibacterial coating |
| CN106176810A (en) * | 2016-07-13 | 2016-12-07 | 长沙迪谷纳米生物科技有限公司 | Medicinal nano material compositions DG 5 is for the purposes of antimicrobial agent |
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| Publication number | Publication date |
|---|---|
| CN1299578C (en) | 2007-02-14 |
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Effective date of registration: 20090206 Address after: A, Mei Mei Industrial Park, 260 Cao Cao Road, Shanghai, Minhang District: 201108 Patentee after: Shanghai Huashi Nano Material Co., Ltd. Address before: Room 301, 13 lane, 288 lane, Macao Road, Putuo District, Shanghai, zip code: 200060 Co-patentee before: Li Zongquan Patentee before: Huang de Huan |
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