CN100384947C - Process for preparing silver-based polynary nano composite powder - Google Patents
Process for preparing silver-based polynary nano composite powder Download PDFInfo
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- CN100384947C CN100384947C CNB2004100163397A CN200410016339A CN100384947C CN 100384947 C CN100384947 C CN 100384947C CN B2004100163397 A CNB2004100163397 A CN B2004100163397A CN 200410016339 A CN200410016339 A CN 200410016339A CN 100384947 C CN100384947 C CN 100384947C
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Abstract
The present invention discloses a making method for silver-base polynary nanometer composite powder, which comprises: mixing a 0.01 to 5.0% (mass) silver nitrate water solution, a of 0.01 to 5.0% (mass) zinc nitrate water solution, a 0.01 to 5.0% (mass) ferric nitrate water solution and a 0.01 to 5.0% (mass) cupric nitrate water solution; adding an amount of a surface auxiliary agent; adding a 0.001 to 1.0% (mass) hydrazine hydrate water solution without stopping stirring; continuously stirring for 10 to 30 minutes so as to obtain a solution containing polynary nanometer composite particles; and passivating, separating, washing and drying the solution containing polynary nanometer composite particles so as to obtain the silver-base polynary nanometer composite silver-zinc-ferrum-copper powder with the silver content of 40 to 99.6%. The present invention has the advantages that the method can be used for making silver-base polynary nanometer composite powder with the granularity of 10 to 100 nm; the variety and the quantity of the composite elements can be combined according to needs, and therefore, the ingredients of the silver-base polynary nanometer composite powder are even; the present invention has the advantages of easy acquirement of raw materials, simple preparation process, low cost and easy industrial production; and the silver-base polynary nanometer composite powder is wide in application range, and can be used in the aspects of nanometer antibacterial powder, special electric conducting materials, etc. When used as an antibacterial material, the nanometer composite silver-zinc-ferrum-copper powder can increase the efficacy and enhance the wide popularization performance and the high efficiency owing to the polynary synergistic effect.
Description
Technical field
The present invention relates to a kind of matrix material of silver, particularly money base polynary nanometer composite granule.
Background technology
Argent has very strong antibiotic effect, and when the grain Trail of silver particles Zai Satisfied meter ruler was very little, it was antibiotic, sterilization usefulness improves greatly.Characteristics ， Satisfied rice silver antibacterial agents such as You Yu Satisfied rice silver has wide spectrum, efficient, environmental protection, have no side effect are subjected to the great attention of domestic and international scientific and technological circle and industrial community.Outside the desilver, metallic elements such as zinc, copper also have the excellent antibiotic effect.Compound silver-the zinc of applying nano-iron/copper powder is as anti-biotic material, because polynary synergistic effect can improve its usefulness and increase its wide spectrum, high efficiency.In addition, money base polynary nanometer composite granule also has very high using value at aspects such as extraordinary electro-conductive materials.
Summary of the invention
The object of the present invention is to provide a kind of money base polynary nanometer composite granule.
Money base polynary nanometer composite granule composition is:
80.0～99.8％Ag-0.1～20.0％Zn-0.001％Fe-0.001％Cu、80.0～99.8％Ag-0.001％Zn-0.1～20.0％Fe-0.001％Cu、60.0～99.7％Ag-0.1～20.0％Zn-0.1～20.0％Fe-0.001％Cu、60.0～99.7％Ag-0.1～20.0％Zn-0.001％Fe-0.1～20.0％Cu、60.0～99.7％Ag-0.001％Zn-0.1～20.0％Fe-20.0-0.1％Cu、40.0～99.6％Ag-0.1～20.0％Zn-0.1～20.0％Cu-0.1～20.0％Fe；
Its preparation method's step is as follows:
1) with mass percent concentration is 0.01～5.0% silver nitrate aqueous solution, concentration is 0.001～5.0% zinc nitrate aqueous solution, concentration is 0.001～5.0% iron nitrate aqueous solution, concentration is after 0.001～5.0% copper nitrate aqueous solution mixes, adding concentration is 0.01～5.0% surperficial adjuvant water solution, in stirring, add concentration lentamente and be 0.001～1.0% hydrazine hydrate aqueous solution, Silver Nitrate, zinc nitrate, iron nitrate, cupric nitrate, the surface auxiliary agent, the mol ratio of hydrazine hydrate is 1.0: 0.001～0.31: 0.001～0.48: 0.001～0.43: 0.001～1.0: 0.5～4.5, 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 polynary nanometer composite particles;
2) above-mentioned reaction product is left standstill 6 to 12 hours, make the nano silver particles passivation, through separation, washing, cryodrying, obtain the money base polynary nanometer composite granule of silver content 40～99.6%, powder granularity is 10～100nm.
Advantage of the present invention is: can prepare money base polynary nanometer composite granule, powder granularity is 10 to 100nm, and complex element kind and quantity can make up as required, and composition is even; Starting material are easy to get, preparation technology is simple, cost is low, easy industrialization; Money base polynary nanometer composite granule purposes is wide, can be used on aspects such as antiseptic nano powder and extraordinary electro-conductive material.Compound silver-the zinc of applying nano-iron/copper powder is as anti-biotic material, because polynary synergistic effect can improve its usefulness and increase its wide spectrum, high efficiency.
Description of drawings
Fig. 1 is the transmission electron microscope photo of silver particles powder in the embodiment of the invention 1;
Fig. 2 is the transmission electron microscope photo of silver particles powder in the embodiment of the invention 2;
Fig. 3 is the transmission electron microscope photo of silver particles powder in the embodiment of the invention 3.
Embodiment
The composition of money base polynary nanometer composite granule of the present invention is
80.0～99.8％Ag-0.1～20.0％Zn-0.001％Fe-0.001％Cu、80.0～99.8％Ag-0.001％Zn-0.1～20.0％Fe-0.001％Cu、60.0～99.7％Ag-0.1～20.0％Zn-0.1～20.0％Fe-0.001％Cu、60.0～99.7％Ag-0.1～20.0％Zn-0.001％Fe-0.1～20.0％Cu、60.0～99.7％Ag-0.001％Zn-0.1～20.0％Fe-20.0-0.1％Cu、40.0～99.6％Ag-0.1～20.0％Zn-0.1～20.0％Cu-0.1～20.0％Fe。
The surface auxiliary agent comprises sodium lauryl sulphate, dodecyl semi-annular jade pendant acid sodium, polyvinylpyrrolidone, sodium polyphosphate, can use wherein a kind ofly, also can use multiple simultaneously.
Embodiment 1
1) with the 50ml mass percent concentration is 0.2% silver nitrate aqueous solution, 10ml concentration is 0.2% zinc nitrate aqueous solution, 10ml concentration is 0.001% iron nitrate aqueous solution, 10ml concentration is after 0.001% copper nitrate aqueous solution mixes, adding 50ml concentration is 0.1% the polyvinylpyrrolidone aqueous solution, 20ml concentration is 0.1% lauryl sodium sulfate aqueous solution, add deionized water to 200ml, in stirring, add 200ml concentration lentamente and be 0.01% hydrazine hydrate aqueous solution, Silver Nitrate, zinc nitrate, iron nitrate, cupric nitrate, polyvinylpyrrolidone, sodium lauryl sulphate, the mol ratio of hydrazine hydrate is 1.0: 0.18: 0.0007: 0.0009: 0.0085: 0.12: 0.68, 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 polynary nanometer composite particles;
2) above-mentioned reaction product was left standstill 12 hours, make the nano silver particles passivation, through separation, washing, cryodrying, obtain the composite nano-powder of 90.1% silver medal-9.8% zinc and trace iron, copper, the mean particle size of powder is 20nm.
Embodiment 2
1) with the 50ml mass percent concentration is 0.2% silver nitrate aqueous solution, 11.5ml concentration is 0.2% zinc nitrate aqueous solution, 10ml concentration is 0.001% iron nitrate aqueous solution, 11.7ml concentration is 0.2% copper nitrate aqueous solution mix after, adding 50ml concentration is 0.1% polyphosphoric acid sodium water solution, 50ml concentration is 0.1% dodecyl semi-annular jade pendant acid sodium aqueous solution, add deionized water to 200ml, in stirring, add 180ml concentration lentamente and be 0.015% hydrazine hydrate aqueous solution, Silver Nitrate, zinc nitrate, iron nitrate, cupric nitrate, polyvinylpyrrolidone, sodium lauryl sulphate, the mol ratio of hydrazine hydrate is 1.0: 0.21: 0.0007: 0.21: 0.23: 0.0.31: 0.92, when the pH value reaches 7.0, stop to add hydrazine hydrate aqueous solution, continue to stir 15 minutes, obtain to contain the solution of polynary nanometer composite particles;
2) above-mentioned reaction product was left standstill 12 hours, make the nano silver particles passivation, through separation, washing, cryodrying, obtain the composite nano-powder of 79.8% silver medal-10.1% zinc-0.2% iron-9.9% bronze medal, the mean particle size of powder is 18nm.
Embodiment 3
1) with the 30ml mass percent concentration is 0.8% silver nitrate aqueous solution, 15ml concentration is 0.5% zinc nitrate aqueous solution, 10ml concentration is 0.5% iron nitrate aqueous solution, 10ml concentration is after 0.001% copper nitrate aqueous solution mixes, adding 25ml concentration is 0.5% the polyvinylpyrrolidone aqueous solution, 20ml concentration is 0.5% lauryl sodium sulfate aqueous solution, add deionized water to 200ml, in stirring, add 200ml concentration lentamente and be 0.04% hydrazine hydrate aqueous solution, Silver Nitrate, zinc nitrate, iron nitrate, cupric nitrate, polyvinylpyrrolidone, sodium lauryl sulphate, the mol ratio of hydrazine hydrate is 1.0: 0.28: 0.15: 0.0038: 0.0089: 0.25: 1.13, when the pH value reaches 7.0, stop to add hydrazine hydrate aqueous solution, continue to stir 15 minutes, obtain to contain the solution of polynary nanometer composite particles;
2) above-mentioned reaction product was left standstill 12 hours, make the nano silver particles passivation, through separation, washing, cryodrying, obtain the composite nano-powder body of 80.2% silver medal-13.6% zinc-6.1% iron-0.1% bronze medal, the mean particle size of powder is 26nm.
Embodiment 4
1) with the 20ml mass percent concentration is 0.5% silver nitrate aqueous solution, 18ml concentration is 0.5% zinc nitrate aqueous solution, 27ml concentration is 0.5% iron nitrate aqueous solution, 18ml concentration is after 0.5% copper nitrate aqueous solution mixes, adding 20ml concentration is 0.8% the polyvinylpyrrolidone aqueous solution, 20ml concentration is 0.8% lauryl sodium sulfate aqueous solution, add deionized water to 200ml, in stirring, add 200ml concentration lentamente and be 0.055% hydrazine hydrate aqueous solution, Silver Nitrate, zinc nitrate, iron nitrate, cupric nitrate, polyvinylpyrrolidone, sodium lauryl sulphate, the mol ratio of hydrazine hydrate is 1.0: 0.81: 0.95: 0.82: 0.027: 0.96: 3.71, when the pH value reaches 7.0, stop to add hydrazine hydrate aqueous solution, continue to stir 15 minutes, obtain to contain the solution of polynary nanometer composite particles;
2) above-mentioned reaction product was left standstill 12 hours, make the nano silver particles passivation,, obtain the composite nano-powder of 40.7% silver medal-19.9% zinc-19.9% iron-19.5% bronze medal through separation, washing, cryodrying.
Embodiment 5
1) with the 50ml mass percent concentration is 0.2% silver nitrate aqueous solution, 20ml concentration is 0.1% zinc nitrate aqueous solution, 20ml concentration is 0.1% iron nitrate aqueous solution, 20ml concentration is after 0.1% copper nitrate aqueous solution mixes, adding 30ml concentration is 0.5% the polyvinylpyrrolidone aqueous solution, 20ml concentration is 0.5% lauryl sodium sulfate aqueous solution, add water to 200ml, in stirring, add 200ml concentration lentamente and be 0.015% hydrazine hydrate aqueous solution, Silver Nitrate, zinc nitrate, iron nitrate, cupric nitrate, polyvinylpyrrolidone, sodium lauryl sulphate, the mol ratio of hydrazine hydrate is 1.0: 0.18: 0.0141: 0.18: 0.026: 0.62: 1.01, when the pH value reaches 7.0, stop to add hydrazine hydrate aqueous solution, continue to stir 15 minutes, obtain to contain the solution of polynary nanometer composite particles;
2) above-mentioned reaction product was left standstill 12 hours, make the nano silver particles passivation,, obtain the composite nano-powder of 77.6% silver medal-8.4% zinc-5.7% iron-8.3% bronze medal through separation, washing, cryodrying.
Claims (1)
1. a money base polynary nanometer composite granule is characterized in that its composition is
80.0～99.8％Ag-0.1～20.0％Zn-0.001％Fe-0.001％Cu、
80.0～99.8％Ag-0.001％Zn-0.1～20.0％Fe-0.001％Cu、
60.0～99.7％Ag-0.1～20.0％Zn-0.1～20.0％Fe-0.001％Cu、
60.0～99.7％Ag-0.1～20.0％Zn-0.001％Fe-0.1～20.0％Cu、
60.0～99.7％Ag-0.001％Zn-0.1～20.0％Fe-20.0-0.1％Cu、
40.0～99.6％Ag-0.1～20.0％Zn-0.1～20.0％Cu-0.1～20.0％Fe；
Its preparation method's step is as follows:
1) with mass percent concentration is 0.01～5.0% silver nitrate aqueous solution, concentration is 0.001～5.0% zinc nitrate aqueous solution, concentration is 0.001～5.0% iron nitrate aqueous solution, concentration is after 0.001～5.0% copper nitrate aqueous solution mixes, adding concentration is 0.01～5.0% surperficial adjuvant water solution, in stirring, add concentration lentamente and be 0.001～1.0% hydrazine hydrate aqueous solution, Silver Nitrate, zinc nitrate, iron nitrate, cupric nitrate, the surface auxiliary agent, the mol ratio of hydrazine hydrate is 1.0: 0.001～0.31: 0.001～0.48: 0.001～0.43: 0.001～1.0: 0.5～4.5, 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 polynary nanometer composite particles;
2) above-mentioned reaction product is left standstill 6 to 12 hours, make the nano silver particles passivation, through separation, washing, cryodrying, obtain the money base polynary nanometer composite granule of silver content 40～95%, powder granularity is 10～100nm.
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| CN103430960A (en) * | 2013-06-27 | 2013-12-11 | 南京市荣达树脂有限公司 | Antibacterial powder for antibacterial coating material |
| CN113463152A (en) * | 2021-07-12 | 2021-10-01 | 广东工业大学 | Surface passivation treatment method for silver particles |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1197708A (en) * | 1998-03-03 | 1998-11-04 | 浙江大学 | Preparation of nanometer silver-copper alloy powder |
| CN1310248A (en) * | 2000-12-04 | 2001-08-29 | 中国人民解放军***联勤部卫生防疫队 | Aluminium utensils capable of killing bacteria and replenishing zinc automatically and its manufacture |
| CN1341358A (en) * | 2000-09-07 | 2002-03-27 | 刘建忠 | Silver zinc combined antimicrobial agent |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1197708A (en) * | 1998-03-03 | 1998-11-04 | 浙江大学 | Preparation of nanometer silver-copper alloy powder |
| CN1341358A (en) * | 2000-09-07 | 2002-03-27 | 刘建忠 | Silver zinc combined antimicrobial agent |
| CN1310248A (en) * | 2000-12-04 | 2001-08-29 | 中国人民解放军***联勤部卫生防疫队 | Aluminium utensils capable of killing bacteria and replenishing zinc automatically and its manufacture |
Non-Patent Citations (4)
| Title |
|---|
| 化学还原法制备纳米金属粉的几点考虑. 彭少方.四川有色金属，第2期. 2003 |
| 化学还原法制备纳米金属粉的几点考虑. 彭少方.四川有色金属，第2期. 2003 * |
| 高分子保护银超微粒子分散液的制备及其导电性. 赵斌.化东理工大学学报，第21卷第4期. 1995 |
| 高分子保护银超微粒子分散液的制备及其导电性. 赵斌.化东理工大学学报，第21卷第4期. 1995 * |
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Effective date of registration: 20081114 Address after: A, Mei Mei Industrial Park, 260 Lian Cao Road, Shanghai, Minhang District, China: 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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