CN1281126C - Nanometer silver antiseptic powder preparation method - Google Patents
Nanometer silver antiseptic powder preparation method Download PDFInfo
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- CN1281126C CN1281126C CN 200410016338 CN200410016338A CN1281126C CN 1281126 C CN1281126 C CN 1281126C CN 200410016338 CN200410016338 CN 200410016338 CN 200410016338 A CN200410016338 A CN 200410016338A CN 1281126 C CN1281126 C CN 1281126C
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 239000000843 powder Substances 0.000 title claims abstract description 35
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 28
- 239000004332 silver Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 230000002421 anti-septic effect Effects 0.000 title 1
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 34
- 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
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 10
- 239000011707 mineral Substances 0.000 claims abstract description 10
- 239000002245 particle Substances 0.000 claims abstract description 7
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 5
- 229910010272 inorganic material Inorganic materials 0.000 claims abstract description 5
- 239000011147 inorganic material Substances 0.000 claims abstract description 5
- 239000007864 aqueous solution Substances 0.000 claims description 26
- 230000000845 anti-microbial effect Effects 0.000 claims description 13
- 239000000243 solution Substances 0.000 claims description 13
- 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 11
- 239000011734 sodium Substances 0.000 claims description 11
- 229910052708 sodium Inorganic materials 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 10
- 230000010355 oscillation Effects 0.000 claims description 10
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 9
- 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 9
- 239000010977 jade Substances 0.000 claims description 9
- 229910052625 palygorskite Inorganic materials 0.000 claims description 7
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 7
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 7
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 7
- 238000010908 decantation Methods 0.000 claims description 6
- 239000011259 mixed solution Substances 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 5
- 239000004113 Sepiolite Substances 0.000 claims description 5
- 239000011858 nanopowder Substances 0.000 claims description 5
- 229910052624 sepiolite Inorganic materials 0.000 claims description 5
- 235000019355 sepiolite Nutrition 0.000 claims description 5
- 235000019830 sodium polyphosphate Nutrition 0.000 claims description 5
- 238000007654 immersion Methods 0.000 claims description 4
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 3
- 239000002671 adjuvant Substances 0.000 claims description 3
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims description 3
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052622 kaolinite Inorganic materials 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 2
- 238000001694 spray drying Methods 0.000 claims description 2
- 239000000969 carrier Substances 0.000 abstract description 3
- 239000011248 coating agent Substances 0.000 abstract description 3
- 238000000576 coating method Methods 0.000 abstract description 3
- 229920003023 plastic Polymers 0.000 abstract description 3
- 239000004033 plastic Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 230000000844 anti-bacterial effect Effects 0.000 abstract 7
- 239000000919 ceramic Substances 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 230000003115 biocidal effect Effects 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 229920000137 polyphosphoric acid Polymers 0.000 description 2
- -1 pottery Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 239000004599 antimicrobial Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 231100000957 no side effect Toxicity 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000000926 separation method 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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Abstract
The present invention discloses a preparation method for antibacterial powder carrying nanometer silver. Ultrafine carriers are added in water solution of silver nitrate with the concentration of 0.01 to 5.0% by mass percentage, and after supersonic vibration is carried out on the water solution of silver nitrate for 0.5 to 4 hours, water solution of surface auxiliary agents with the concentration of 0.01 to 5.0% is added; water solution of hydrazine hydrate with the concentration of 0.001 to 1.0% is added in the water solution of silver nitrate when the water solution of silver nitrate is stirred, the water solution of silver nitrate continues to be stirred for 10 to 30 minutes, and solution containing the powder carrying nanometer silver is obtained; the solution containing the powder carrying nanometer silver is separated, washed and dried, and then the antibacterial powder carrying nanometer silver with the silver content of 0.1 to 20% is obtained. The present invention has the advantages that different types of antibacterial powder carrying nanometer silver can be prepared, carriers can be natural mineral powder and can also be artificially synthesized nanometer inorganic materials, and the amount of carried silver can be regulated according to the needs; the granularity of nanometer silver particles is from 10 nm to 100 nm, and the components of the antibacterial powder are even. The antibacterial powder has the advantages of easy acquisition of raw materials, simple preparation method, low cost and easy industrialized production, and the products are convenient to preserve and apply; the antibacterial powder containing nanometer silver can be used in the fields of antibacterial plastics, ceramics, coating materials, medical dressings, etc.
Description
Technical field
The present invention relates to a kind of preparation method of antimicrobial powder, particularly the preparation method of carrying nano silver antimicrobial powder.
Background technology
Jin Shu Silver has very strong antibiotic effect, and when silver particles during at nano-scale, it is antibiotic, sterilization usefulness improves greatly.Owing to Na Mi Silver has wide spectrum, efficient, environmental protection, reason such as have no side effect, Na Mi Silver antibacterial agent is subjected to the great attention of domestic and international scientific and technological circle and industrial circle.Pure Na Mi Silver powder is easy to reunite, and is difficult to evenly disperse in materials such as plastics, pottery, coating, medicine.If with some inorganic material or natural minerals powder is the carrier of Nano Silver, then can overcomes and receive a meter Silver powder and easily reunite, disperse difficulties such as inhomogeneous.The n-SiO of synthetic
2, n-TiO
2, n-CaCO
3, n-Al
2O
3, n-ZnO etc., have advantages such as specific surface area is big, Stability Analysis of Structures, can be as the carrier of Nano Silver.Some have the natural minerals of special construction such as palygorskite, sepiolite, kaolinite, montmorillonite etc. and have nanoscale structures, and its nano pore all has remarkable advantages at aspects such as absorption silver particles, specific surface area and dispersivenesses, is the important carrier of Nano Silver.On the other hand, behind the use carrier, the separation of silver-carrying nano powder and application become and are more prone to; Wherein, some carriers have certain water storage function, help improving the effect of nano silver antimicrobials.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of carrying nano silver antimicrobial powder.
The step of method is as follows
1) be that nanometer～micron-sized natural minerals or people's synthetic inorganic material superfine powder are as carrier with granularity, at mass percent concentration is to soak 4 to 12 hours in 0.01～5.0% the silver nitrate aqueous solution, used ultrasonic oscillation then 0.5 to 2 hour, wherein synthetic nano-powder immersion 4 to 6 hours, ultrasonic oscillation 0.5 to 1.0 hour, natural nano-mineral immersion 6 to 12 hours, ultrasonic oscillation 1 to 2 hour;
2) be that 0.01～5.0% surperficial adjuvant water solution joins in the mixed solution of step 1) with 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, hydrazine hydrate is 1.0: 0.001～1.0: 0.5～1.5, when the pH value reaches 6.8～7.8, stop to add hydrazine hydrate aqueous solution, continue to stir 10～30 minutes, surperficial auxiliary agent is one or more in polyvinylpyrrolidone, sodium polyphosphate, lauryl sodium sulfate, the dodecyl semi-annular jade pendant acid sodium;
3) with step 2) solution left standstill that obtains 6 to 12 hours, decantation spends deionised water 2 to 3 times;
4) the solution spray drying that step 3) is obtained obtains the carrying nano silver antimicrobial powder of silver content 0.1～20%, and the granularity of silver particles is 10～100nm.
Advantage of the present invention is: can prepare different types of carrying nano silver antimicrobial powder, carrier can be the natural minerals powder, also can be the nano inorganic material of synthetic, and silver carrying amount can be regulated as required; The granularity of nanometer silver granuel is 10 to 100nm, and the antimicrobial powder composition is even; Raw material are easy to get, the preparation method is simple, cost is low, easy industrialization, are convenient to preserve and use; The carrying nano silver antimicrobial powder can be used on fields such as antibiotic plastic, pottery, coating, Medical dressing.
Description of drawings
Fig. 1 is carrying nano silver SiO
2The X-ray diffractogram of antimicrobial powder, figure acceptance of the bid " * " number diffraction maximum be silver-colored diffraction maximum;
Fig. 2 is the X-ray diffractogram of carrying nano silver palygorskite antimicrobial powder, figure acceptance of the bid " * " number diffraction maximum be the diffraction maximum of silver, mark " * " number diffraction maximum be the diffraction maximum of palygorskite.
Embodiment
Carrier of the present invention is the natural minerals powder and the synthetic n-SiO of palygorskite, sepiolite, kaolinite, montmorillonite
2, n-TiO
2, n-CaCO
3, n-Al
2O
3, the n-ZnO nano-powder, and their mixture;
The surface auxiliary agent is one or more in polyvinylpyrrolidone, sodium polyphosphate, lauryl sodium sulfate, the dodecyl semi-annular jade pendant acid sodium.
Embodiment 1
1) with 0.4g synthetic nanometer SiO
2As carrier, be to soak 4 hours in 0.2% the silver nitrate aqueous solution at 35ml, mass percent concentration, used ultrasonic oscillation then 1 hour;
2) be that 0.1% the polyvinylpyrrolidone aqueous solution, 50ml concentration are that 0.05% lauryl sodium sulfate aqueous solution joins in the mixed solution of step 1) with 50ml concentration, add deionized water to 200ml, in stirring, add 200ml concentration lentamente and be 0.006% hydrazine hydrate aqueous solution, the mol ratio of silver nitrate, polyvinylpyrrolidone, lauryl sodium sulfate, hydrazine hydrate is 1.0: 0.012: 0.21: 0.58, when the pH value reaches 7.0, stop to add hydrazine hydrate aqueous solution, continue to stir 10 minutes;
3) with step 2) solution left standstill that obtains 12 hours, decantation spends deionised water 3 times;
4) the product drying that step 3) is obtained obtains the carrying nano silver SiO of silver content 10%
2Powder, the granularity of silver particles are 28nm.
Embodiment 2
1) with 0.4g micron order palygorskite powder as carrier, be to soak 12 hours in 0.4% the silver nitrate aqueous solution at the 40ml mass percent concentration, used ultrasonic oscillation then 4 hours;
2) be that 0.2% polyphosphoric acids sodium water solution, 30ml concentration are that 0.2% dodecyl semi-annular jade pendant acid sodium aqueous solution joins in the mixed solution of step 1) with 40ml concentration, add deionized water to 200ml, in stirring, add 200ml concentration lentamente and be 0.012% hydrazine hydrate aqueous solution, the mol ratio of silver nitrate, sodium polyphosphate, dodecyl semi-annular jade pendant acid sodium, hydrazine hydrate is 1.0: 0.23: 0.23: 0.51, when the pH value reaches 7.0, stop to add hydrazine hydrate aqueous solution, continue to stir 15 minutes;
3) with step 2) solution left standstill that obtains 12 hours, decantation spends deionised water 3 times;
4) the product drying that step 3) is obtained obtains the carrying nano silver palygorskite powder of silver content 20%, and the granularity of silver particles is 30nm.
Embodiment 3
1) with 0.2g synthetic n-Al
2O
3As carrier, be to soak 12 hours in 0.1% the silver nitrate aqueous solution at the 20ml mass percent concentration, used ultrasonic oscillation then 2 hours;
2) be that 0.1% polyphosphoric acids sodium water solution, 10ml concentration are that 0.01% dodecyl semi-annular jade pendant acid sodium aqueous solution joins in the mixed solution of step 1) with 20ml concentration, add deionized water to 200ml, in stirring, add 100ml concentration lentamente and be 0.003% hydrazine hydrate aqueous solution, the mol ratio of silver nitrate, sodium polyphosphate, dodecyl semi-annular jade pendant acid sodium, hydrazine hydrate is 1.0: 0.046: 0.031: 0.51, when the pH value reaches 7.0, stop to add hydrazine hydrate aqueous solution, continue to stir 15 minutes;
3) with step 2) solution left standstill that obtains 12 hours, decantation spends deionised water 3 times;
4) the product drying that step 3) is obtained obtains the carrying nano silver n-Al of silver content 6.0%
2O
3Powder.
Embodiment 4
1) with 1.0g micron order sepiolite powder as carrier, be to soak 12 hours in 0.04% the silver nitrate aqueous solution at the 50ml mass percent concentration, used ultrasonic oscillation then 4 hours;
2) be that 0.02% the polyvinylpyrrolidone aqueous solution, 50ml concentration are that 0.05% dodecyl semi-annular jade pendant acid sodium aqueous solution joins in the mixed solution of step 1) with 50ml concentration, add deionized water to 200ml, in stirring, add 100ml concentration lentamente and be 0.004% hydrazine hydrate aqueous solution, the mol ratio of silver nitrate, polyvinylpyrrolidone, dodecyl semi-annular jade pendant acid sodium, hydrazine hydrate is 1.0: 0.0085: 0.78: 0.68, when the pH value reaches 7.0, stop to add hydrazine hydrate aqueous solution, continue to stir 15 minutes;
3) with step 2) solution left standstill that obtains 12 hours, decantation spends deionised water 3 times;
4) the product drying that step 3) is obtained obtains the carrying nano silver sepiolite powder of silver content 1.6%.
Claims (2)
1. the preparation method of a carrying nano silver antimicrobial powder is characterized in that the step of method is as follows
1) be that nanometer～micron-sized natural minerals or synthetic inorganic material superfine powder are as carrier with granularity, at mass percent concentration is to soak 4 to 12 hours in 0.01～5.0% the silver nitrate aqueous solution, used ultrasonic oscillation then 0.5 to 2 hour, wherein synthetic nano-powder immersion 4 to 6 hours, ultrasonic oscillation 0.5 to 1.0 hour, natural nano-mineral immersion 6 to 12 hours, ultrasonic oscillation 1 to 2 hour;
2) be that 0.01～5.0% surperficial adjuvant water solution joins in the mixed solution of step 1) with concentration, in stirring, add concentration lentamente and be 0.001～1.0% hydrazine hydrate aqueous solution, the mol ratio of silver nitrate aqueous solution, surperficial adjuvant water solution, hydrazine hydrate aqueous solution is 1.0: 0.001～1.0: 0.5～1.5, when the pH value reaches 6.8～7.8, stop to add hydrazine hydrate aqueous solution, continue to stir 10～30 minutes, surperficial auxiliary agent is one or more in polyvinylpyrrolidone, sodium polyphosphate, lauryl sodium sulfate, the dodecyl semi-annular jade pendant acid sodium;
3) with step 2) solution left standstill that obtains 6 to 12 hours, decantation spends deionised water 2 to 3 times;
4) the solution spray drying that step 3) is obtained obtains the carrying nano silver antimicrobial powder of silver content 0.1～20%, and the granularity of silver particles is 10～100nm.
2. the preparation method of a kind of carrying nano silver antimicrobial powder according to claim 1 is characterized in that said carrier is the natural minerals powder and the synthetic n-SiO of palygorskite, sepiolite, kaolinite, montmorillonite
2, n-TiO
2, n-CaCO
3, n-Al
2O
3, the n-ZnO nano-powder, and their mixture.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410016338 CN1281126C (en) | 2004-02-13 | 2004-02-13 | Nanometer silver antiseptic powder preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410016338 CN1281126C (en) | 2004-02-13 | 2004-02-13 | Nanometer silver antiseptic powder preparation method |
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| Publication Number | Publication Date |
|---|---|
| CN1557150A CN1557150A (en) | 2004-12-29 |
| CN1281126C true CN1281126C (en) | 2006-10-25 |
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|---|---|---|---|
| CN 200410016338 Expired - Fee Related CN1281126C (en) | 2004-02-13 | 2004-02-13 | Nanometer silver antiseptic powder preparation method |
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| Country | Link |
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Cited By (1)
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| CN101138342B (en) * | 2007-09-28 | 2011-05-25 | 上海师范大学 | Method for preparing nanometer mesoporous cerium oxide carrying silver antimicrobials |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101138342B (en) * | 2007-09-28 | 2011-05-25 | 上海师范大学 | Method for preparing nanometer mesoporous cerium oxide carrying silver antimicrobials |
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| CN1557150A (en) | 2004-12-29 |
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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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Owner name: SHANGHAI HUASHI NANOMETER MATERIALS CO., LTD. Free format text: FORMER OWNER: HUANG DEHUAN Effective date: 20090206 |
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Granted publication date: 20061025 Termination date: 20130213 |