CN1557150A - Nanometer silver antiseptic powder preparation method - Google Patents
Nanometer silver antiseptic powder preparation method Download PDFInfo
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- CN1557150A CN1557150A CNA2004100163382A CN200410016338A CN1557150A CN 1557150 A CN1557150 A CN 1557150A CN A2004100163382 A CNA2004100163382 A CN A2004100163382A CN 200410016338 A CN200410016338 A CN 200410016338A CN 1557150 A CN1557150 A CN 1557150A
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Abstract
The preparation process of nano silver carrying antiseptic powder includes: adding superfine carrier into sliver nitrate aqua of 0.01-5.0 wt% concentration, ultrasonic vibration for 0.5-4 hr, adding surface assistant aqua of 0.01-5.0 wt% concentration, adding hydrazine hydrate aqua of 0.001-1.0 wt% concentration under stirring, stirring further for 10-30 min to obtain solution of nano silver carrier, separation, washing, and drying to obtain the nano silver carrying antiseptic powder with silver content of 0.1-20 wt%. The present invention can prepare nano silver carrying antiseptic powder of different kinds of carrier, which may be natural mineral powder or artificially synthesized nano inorganic material, and with adjustable silver content and nano sliver size of 10-100 nm. The nano silver carrying antiseptic powder may be used in antiseptic plastic, ceramic, paint, dressing and other fields.
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 Zai Satisfied meter ruler was very little, it was antibiotic, sterilization usefulness improves greatly.Reason ， Satisfied Mi Silver antibacterial agents such as You Yu Satisfied Mi 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 circle.Chun Satisfied 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 restrains clothes Satisfied rice 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;
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 (3)
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;
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;
3. the preparation method of a kind of carrying nano silver antimicrobial powder according to claim 1 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.
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|---|---|---|---|
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| CN102783498A (en) * | 2011-05-16 | 2012-11-21 | 常州英中纳米科技有限公司 | Method for producing nano-silver composite antibacterial agent through spray drying |
| CN103271942A (en) * | 2013-05-27 | 2013-09-04 | 浙江大学 | Method for preparing nano silver-kaolinite compound by using hydrated kaolinite as carrier |
| CN104585235A (en) * | 2014-12-31 | 2015-05-06 | 芜湖恒杰膨润土科技有限公司 | Silver-loaded bentonite and preparation method thereof |
| CN104987051A (en) * | 2015-06-02 | 2015-10-21 | 安徽省含山瓷业股份有限公司 | Antibacterial and bactericidal ceramic bowl and preparation method thereof |
| CN105079862A (en) * | 2015-09-23 | 2015-11-25 | 江苏蓝湾生物科技有限公司 | Medical anti-microbial dressing and preparation method thereof |
| CN105126155A (en) * | 2015-09-23 | 2015-12-09 | 江苏蓝湾生物科技有限公司 | Medical antibacterial swelling relieving material and preparation method of medical antibacterial swelling relieving material |
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| CN105638731A (en) * | 2016-01-30 | 2016-06-08 | 湘潭大学 | Preparation method of antibacterial sepiolite powder |
| CN106270479A (en) * | 2015-05-21 | 2017-01-04 | 中国石油化工股份有限公司 | A kind of attapulgite-nanometer silver composite inorganic powder and preparation method |
| CN106621850A (en) * | 2015-10-28 | 2017-05-10 | 中国石油化工股份有限公司 | Antibacterial composite nanofiltration membrane, and preparation method and application thereof |
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| CN106757074A (en) * | 2016-12-16 | 2017-05-31 | 安徽宝恒新材料科技有限公司 | A kind of processing method for improving stainless steel antibiotic property |
| CN107602898A (en) * | 2017-10-10 | 2018-01-19 | 深圳大学 | A kind of antibiotic plastic and preparation method |
| CN108129066A (en) * | 2017-12-30 | 2018-06-08 | 常州新之雅装饰材料有限公司 | A kind of preparation method for carrying silver-colored palygorskite heat resistant type liquid wallpaper |
| CN108627528A (en) * | 2018-05-02 | 2018-10-09 | 山东非金属材料研究所 | Nano silver reference materials for particle size analysis and preparation method thereof |
| CN109880037A (en) * | 2019-01-14 | 2019-06-14 | 广东恩浩内衣实业有限公司 | A kind of polyurethane foam and its mold cup of high content of nanometer silver |
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| CN102783498A (en) * | 2011-05-16 | 2012-11-21 | 常州英中纳米科技有限公司 | Method for producing nano-silver composite antibacterial agent through spray drying |
| CN103271942A (en) * | 2013-05-27 | 2013-09-04 | 浙江大学 | Method for preparing nano silver-kaolinite compound by using hydrated kaolinite as carrier |
| WO2015192676A1 (en) * | 2014-06-18 | 2015-12-23 | 陈文旻 | Antibacterial coating and preparation method therefor |
| CN104585235A (en) * | 2014-12-31 | 2015-05-06 | 芜湖恒杰膨润土科技有限公司 | Silver-loaded bentonite and preparation method thereof |
| CN104585235B (en) * | 2014-12-31 | 2017-09-01 | 芜湖恒杰膨润土科技有限公司 | Carry silver-colored bentonite and preparation method thereof |
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| CN105126155A (en) * | 2015-09-23 | 2015-12-09 | 江苏蓝湾生物科技有限公司 | Medical antibacterial swelling relieving material and preparation method of medical antibacterial swelling relieving material |
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| CN112625324A (en) * | 2020-11-30 | 2021-04-09 | 江西力达塑胶管业有限公司 | Anti-aging antibacterial PE water supply pipe |
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