CN1759962A - Method for preparing Nano silver sol - Google Patents
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- CN1759962A CN1759962A CN 200510110310 CN200510110310A CN1759962A CN 1759962 A CN1759962 A CN 1759962A CN 200510110310 CN200510110310 CN 200510110310 CN 200510110310 A CN200510110310 A CN 200510110310A CN 1759962 A CN1759962 A CN 1759962A
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Abstract
A process for preparing nano-Ag sol includes such steps as preparing the reverse-phase microemulsion from glucolipide-type surfactant, mixing the microemulsion containing reducer with the microemulsion containing silver nitrate while high-speed stirring, preparing Ag nanoparticles, demulsifying, separating, washing, and distributing them in nonpolar solvent. Its advantages are high stability and high antibacterial effect.
Description
Technical field
The present invention relates to a kind of preparation method of nano silver colloidal sol, particularly relating to a kind of is template with reverse microemulsion shape liquid, need not to add the preparation method of any other protectant nano silver colloidal sol.
Background technology
The generation of Nano Silver has had nearly 30 years history, because it all demonstrates superiority in various fields such as mechanics, calorifics, electricity, optics, thereby is subjected to broad research.In recent years, along with the progressively raising of people to health demand, antibiotic, the antibacterial effect of silver has been subjected to paying close attention to widely, and compares with common silver, and the antibacterial action of Nano Silver has produced qualitative leap, uses the silver of minute quantity just can produce very strong bactericidal effect.Though multiple metal ion all has antibiotic effect as mercury, lead, chromium, nickel, cobalt, copper, zinc etc., but mercury, lead, chromium are to the murder by poisoning of human body lastingly; Nickel, cobalt, copper have coloration and influence attractive in appearance object; Though zinc has certain antibacterial effect, its antibacterial strength only is 1/1000 of a silver ion.Studies show that Nano Silver demonstrates the excellent antibacterial ability as a kind of antiseptic to Gram-positive and negative bacteria, fungi and bacillus, can be widely used in fields such as textile chemical fiber, health care, environmental protection, daily electrical home appliance, fruit freshness preserving.
At present, the method for preparing nano silver colloidal sol has multiple, comprises direct-reduction process, chemical deposition, galvanoplastic and microemulsion method etc.Wherein, microemulsion method can be controlled the particle size and the degree of scatter of Nano Silver well by the proportioning of control solvent, silver salt, reducing agent, surfactant concentration and micro emulsion.But will introduce the reunion that protective agent prevents nano silver colloidal sol in traditional microemulsion method, and wherein residual chemical surfactant has chemical toxicity, influenced the performance of nano silver colloidal sol.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of nano silver colloidal sol, the nano silver colloidal sol of adopt this method can obtain a kind of form stable, be uniformly dispersed, particle diameter is less; This method can conveniently be controlled the particle diameter of nano silver colloidal sol simultaneously, need not introduce protective agent, can overcome the microemulsion method complicated process of preparation, the shortcoming of residual chemical noxious material in the nano silver colloidal sol.
Purpose of the present invention can be achieved through the following technical solutions: a kind of preparation method of nano silver colloidal sol is characterized in that this method is that template prepares with reverse microemulsion shape liquid; Its processing step is as follows:
(1) produces respectively micro emulsion that contains silver nitrate and the micro emulsion that contains reducing agent;
(2) micro emulsion that will contain silver nitrate under agitation is added drop-wise in the micro emulsion that contains reducing agent, the micro emulsion that perhaps will contain reducing agent under agitation is added drop-wise in the micro emulsion that contains silver nitrate, after dropwising, continue to stir 1～3 hour, obtain containing the micro emulsion of Nano Silver;
(3) demulsifier under agitation is added drop-wise in the micro emulsion that contains Nano Silver, produces black precipitate;
(4) solution separation, washing, the drying that step (3) is obtained, ultrasonic again being distributed in the non-polar solven obtains nano silver colloidal sol.
Reverse microemulsion shape fluid component and content (weight portion) as template are as follows:
Oil phase 1～95, (2) surfactant phase 1～98, (3) water 1～50.5;
Described oil phase is selected from one or more the mixture in alkane, cycloalkane, the aromatic hydrocarbon;
Described surfactant comprises (a) glycolipid type biological surfactant mutually, (b) water-soluble or oil-soluble straight chain alcohol, and its weight is 1～4 times of biosurfactant, (c) alkali, its weight is 0.05～1 times of biosurfactant;
Described water is the silver nitrate aqueous solution of 0.05～0.1mol/L or the reducing agent aqueous solution of 0.05～0.1mol/L.
The mixture of one or more in described alkane, cycloalkane, the aromatic hydrocarbon comprises one or more mixtures in normal heptane, isooctane, the cyclohexane.
The more weak hydroxy-acid group of described biosurfactant band polarity, hydrophilic radical are sugar, polysaccharide.
Described water miscible straight chain alcohol is a normal propyl alcohol, and described oil-soluble straight chain alcohol is selected from one or more in n-butanol, n-amyl alcohol, n-hexyl alcohol, the n-heptanol.
Described alkali is NaOH, potassium hydroxide or its mixture.
Described reducing agent is selected from one or more in sodium borohydride, hydrazine hydrate, trisodium citrate or the ascorbic acid.
Described demulsifier is ethanol or acetone.
Described non-polar solven is the mixture of one or more non-polar solvens.
Described nano silver colloidal sol average grain diameter is less than 50nm.
Compared with prior art, the present invention has following characteristics:
1. the nano silver colloidal sol among the present invention is formed in the water nuclear of reverse micro emulsion, controls the size of nano silver colloidal sol by the size of control water nuclear, can control particle diameter less than 50nm.
2. do not introduce other any protective agent among the present invention; utilization remains in the formed space structure of electronegative biosurfactant in the nano silver colloidal sol; positively charged silver ion stably is scattered in wherein; limited silver-colored growth by the outside hydrophobic group of biosurfactant and the space of inner hydrophilic base formation; make nano silver colloidal sol be in stable state for a long time, be evenly distributed.
3. residual is the glycolipid type biological surfactant in the nano silver colloidal sol of the present invention, the consumption of this type biological surfactant in the preparation nano silver colloidal sol is few, nontoxic, itself have excellent antibiotic and antiviral activity, can not influence the antibacterial action of nano silver colloidal sol.
4. the centrifugal raffinate of breakdown of emulsion can not polluted environment by complete biodegradable in the nano silver colloidal sol of the present invention.
The specific embodiment
The invention will be further described below in conjunction with specific embodiment.
Embodiment 1
A kind of prescription of reverse microemulsion shape liquid is as follows:
| Component | The component title | Gram |
| Oil phase | Normal heptane | 9 |
| Alkali | NaOH | 0.25 |
| Water | Silver nitrate aqueous solution or sodium borohydride aqueous solution | 1 |
| Biosurfactant | Rhamnolipid | 3 |
| Cosurfactant | N-butanol | 6 |
The preparation method of Nano Silver is as follows:
Silver nitrate, sodium borohydride are dissolved in respectively in the deionized water, produce concentration and be respectively the silver nitrate aqueous solution of 0.1mol/L and the sodium borohydride aqueous solution of 0.1mol/L.With the mixture of biosurfactant and cosurfactant is that 9: 1 ratio is mixed with silver nitrate aqueous solution and sodium borohydride aqueous solution with mass ratio respectively, adding and the biosurfactant oil phase suitable with the co-surfactant blend quality makes microemulsion that contains silver nitrate and the microemulsion that contains sodium borohydride respectively again.The microemulsion that under agitation will contain silver nitrate is added drop-wise in the microemulsion that contains sodium borohydride, after dropwising, continues to stir 2 hours.Under agitation demulsifier ethanol is added drop-wise in the micro emulsion that contains Nano Silver, separation, washing, dry, ultrasonic being distributed in the normal heptane get the brown nano silver colloidal sol of 15～40nm.
Embodiment 2
A kind of prescription of reverse microemulsion shape liquid is as follows:
| Component | The component title | Gram |
| Oil phase | Isooctane | 4 |
| Alkali | Potassium hydroxide | 0.09 |
| Water | The silver nitrate aqueous solution or the hydrazine hydrate aqueous solution | 1 |
| Biosurfactant | The marine alga glycolipid | 1.33 |
| Cosurfactant | N-amyl alcohol | 2.66 |
The preparation method of Nano Silver is as follows:
Silver nitrate, hydrazine hydrate are dissolved in respectively in the deionized water, produce concentration and be respectively the silver nitrate aqueous solution of 0.1mol/L and the hydrazine hydrate aqueous solution of 0.1mol/L.With the mixture of biosurfactant and cosurfactant is that 8: 2 ratio is mixed with silver nitrate aqueous solution and the hydrazine hydrate aqueous solution with mass ratio respectively, adding and the biosurfactant oil phase suitable with the co-surfactant blend quality makes microemulsion that contains silver nitrate and the microemulsion that contains hydrazine hydrate respectively again.The microemulsion that under agitation will contain silver nitrate is added drop-wise in the microemulsion that contains hydrazine hydrate, after dropwising, continues to stir 2 hours.Under agitation demulsifier ethanol is added drop-wise in the micro emulsion that contains Nano Silver, separation, washing, dry, ultrasonic being distributed in the isooctane get the brown nano silver colloidal sol of 15～50nm.
Embodiment 3
A kind of prescription of reverse microemulsion shape liquid is as follows:
| Component | The component title | Gram |
| Oil phase | Cyclohexane | 7 |
| Alkali | NaOH | 0.20 |
| Water | Silver nitrate aqueous solution or trisodium citrate aqueous solution | 3 |
| Biosurfactant | Sophorolipid | 2.33 |
| Cosurfactant | Normal propyl alcohol | 4.66 |
The preparation method of Nano Silver is as follows:
Silver nitrate, trisodium citrate are dissolved in respectively in the deionized water, produce concentration and be respectively the silver nitrate aqueous solution of 0.1mol/L and the trisodium citrate aqueous solution of 0.1mol/L.With the mixture of biosurfactant and cosurfactant is that 7: 3 ratio is mixed with silver nitrate aqueous solution and trisodium citrate aqueous solution with mass ratio respectively, adding and the biosurfactant oil phase suitable with the co-surfactant blend quality makes microemulsion that contains silver nitrate and the microemulsion that contains trisodium citrate respectively again.The microemulsion that under agitation will contain silver nitrate is added drop-wise in the microemulsion that contains trisodium citrate, after dropwising, continues to stir 2 hours.Under agitation demulsifier ethanol is added drop-wise in the micro emulsion that contains Nano Silver separation, washing, dry, the ultrasonic brown nano silver colloidal sol of cyclohexane 20～50nm that is distributed to.
Embodiment 4
A kind of prescription of reverse microemulsion shape liquid is as follows:
| Component | The component title | Gram |
| Oil phase | N-hexane | 9 |
| Alkali | NaOH | 0.25 |
| Water | Silver nitrate aqueous solution or aqueous ascorbic acid | 1 |
| Biosurfactant | Ornithine fat | 3 |
| Cosurfactant | N-heptanol | 6 |
The preparation method of Nano Silver is as follows
Silver nitrate, ascorbic acid are dissolved in respectively in the deionized water, produce concentration and be respectively the silver nitrate aqueous solution of 0.05mol/L and the aqueous ascorbic acid of 0.1mol/L.With the mixture of biosurfactant and cosurfactant is that 9: 1 ratio is mixed with silver nitrate aqueous solution and aqueous ascorbic acid with mass ratio respectively, adding and the biosurfactant oil phase suitable with the co-surfactant blend quality makes microemulsion that contains silver nitrate and the microemulsion that contains ascorbic acid respectively again.The microemulsion that under agitation will contain silver nitrate is added drop-wise in the microemulsion that contains ascorbic acid, after dropwising, continues to stir 2 hours.Under agitation demulsifier acetone is added drop-wise in the micro emulsion that contains Nano Silver, separation, washing, dry, ultrasonic being distributed in the n-hexane get the faint yellow nano silver colloidal sol of 5～10nm.
Embodiment 5
A kind of prescription of reverse microemulsion shape liquid is as follows:
| Component | The component title | Gram |
| Oil phase | Isoheptane | 4 |
| Alkali | Potassium hydroxide | 0.09 |
| Water | The silver nitrate aqueous solution or the hydrazine hydrate aqueous solution | 1 |
| Biosurfactant | Seminolipid | 1.33 |
| Cosurfactant | N-octyl alcohol | 2.66 |
The preparation method of Nano Silver is as follows:
Silver nitrate, hydrazine hydrate are dissolved in respectively in the deionized water, produce concentration and be respectively the silver nitrate aqueous solution of 0.05mol/L and the hydrazine hydrate aqueous solution of 0.1mol/L.With the mixture of biosurfactant and cosurfactant is that 8: 2 ratio is mixed with silver nitrate aqueous solution and the hydrazine hydrate aqueous solution with mass ratio respectively, adding and the biosurfactant oil phase suitable with the co-surfactant blend quality makes microemulsion that contains silver nitrate and the microemulsion that contains hydrazine hydrate respectively again.The microemulsion that under agitation will contain silver nitrate is added drop-wise in the microemulsion that contains hydrazine hydrate, after dropwising, continues to stir 2 hours.Under agitation demulsifier acetone is added drop-wise in the micro emulsion that contains Nano Silver, separation, washing, dry, ultrasonic being distributed in the isoheptane get 5～25nm Yellow nanometer silver sol.
Embodiment 6
A kind of prescription of reverse microemulsion shape liquid is as follows:
| Component | The component title | Gram |
| Oil phase | Hexadecane | 7 |
| Alkali | NaOH | 0.20 |
| Water | Silver nitrate aqueous solution or trisodium citrate aqueous solution | 3 |
| Biosurfactant | Cellobiose fat | 2.33 |
| Cosurfactant | N-hexyl alcohol | 4.66 |
The preparation method of Nano Silver is as follows:
Silver nitrate, trisodium citrate are dissolved in respectively in the deionized water, produce concentration and be respectively the silver nitrate aqueous solution of 0.05mol/L and the trisodium citrate aqueous solution of 0.1mol/L.With the mixture of biosurfactant and cosurfactant is that 7: 3 ratio is mixed with silver nitrate aqueous solution and trisodium citrate aqueous solution with mass ratio respectively, adding and the biosurfactant oil phase suitable with the co-surfactant blend quality makes microemulsion that contains silver nitrate and the microemulsion that contains trisodium citrate respectively again.The microemulsion that under agitation will contain silver nitrate is added drop-wise in the microemulsion that contains trisodium citrate, after dropwising, continues to stir 2 hours.Under agitation demulsifier acetone is added drop-wise in the micro emulsion that contains Nano Silver, separation, washing, dry, ultrasonic being distributed in the hexadecane get 10～30nm nano silver colloidal sol.
Claims (10)
1. the preparation method of a nano silver colloidal sol is characterized in that, this method is that template prepares with reverse microemulsion shape liquid; Its processing step is as follows:
(1) produces respectively micro emulsion that contains silver nitrate and the micro emulsion that contains reducing agent;
(2) micro emulsion that will contain silver nitrate under agitation is added drop-wise in the micro emulsion that contains reducing agent, the micro emulsion that perhaps will contain reducing agent under agitation is added drop-wise in the micro emulsion that contains silver nitrate, after dropwising, continue to stir 1～3 hour, obtain containing the micro emulsion of Nano Silver;
(3) demulsifier under agitation is added drop-wise in the micro emulsion that contains Nano Silver, produces black precipitate;
(4) solution separation, washing, the drying that step (3) is obtained, ultrasonic again being distributed in the non-polar solven obtains nano silver colloidal sol.
2. the preparation method of a kind of nano silver colloidal sol according to claim 1 is characterized in that, and is as follows as the reverse microemulsion shape fluid component and the content (weight portion) of template:
Oil phase 1～95, (2) surfactant phase 1～98, (3) water 1～50.5;
Described oil phase is selected from one or more the mixture in alkane, cycloalkane, the aromatic hydrocarbon;
Described surfactant comprises (a) glycolipid type biological surfactant mutually, (b) water-soluble or oil-soluble straight chain alcohol, and its weight is 1～4 times of biosurfactant, (c) alkali, its weight is 0.05～1 times of biosurfactant;
Described water is the silver nitrate aqueous solution of 0.05～0.1mol/L or the reducing agent aqueous solution of 0.05～0.1mol/L.
3. the preparation method of a kind of nano silver colloidal sol according to claim 2 is characterized in that, the mixture of one or more in described alkane, cycloalkane, the aromatic hydrocarbon comprises one or more mixtures in normal heptane, isooctane, the cyclohexane.
4. the preparation method of a kind of nano silver colloidal sol according to claim 2 is characterized in that, the more weak hydroxy-acid group of described biosurfactant band polarity, hydrophilic radical are sugar, polysaccharide.
5. the preparation method of a kind of nano silver colloidal sol according to claim 2 is characterized in that, described water miscible straight chain alcohol is a normal propyl alcohol, and described oil-soluble straight chain alcohol is selected from one or more in n-butanol, n-amyl alcohol, n-hexyl alcohol, the n-heptanol.
6. the preparation method of a kind of nano silver colloidal sol according to claim 2 is characterized in that, described alkali is NaOH, potassium hydroxide or its mixture.
7. the preparation method of a kind of nano silver colloidal sol according to claim 1 is characterized in that, described reducing agent is selected from one or more in sodium borohydride, hydrazine hydrate, trisodium citrate or the ascorbic acid.
8. the preparation method of a kind of nano silver colloidal sol according to claim 1 is characterized in that, described demulsifier is ethanol or acetone.
9. the preparation method of a kind of nano silver colloidal sol according to claim 1 is characterized in that, described non-polar solven is the mixture of one or more non-polar solvens.
10. the preparation method of a kind of nano silver colloidal sol according to claim 1 is characterized in that, described nano silver colloidal sol average grain diameter is less than 50nm.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2008100163A1 (en) | 2007-02-13 | 2008-08-21 | Instytut Wlókien Naturalnych | Method of manufacturing silver nanoparticles, cellulosic fibers and nanofibers containing silver nanoparticles, fibers and nanofibers containing silver nanoparticles, use of silver nanoparticles to the manufacture of cellulosic fibers and nanofibers, and wound dressing containing silver nanoparticles |
| CN101898250A (en) * | 2010-07-20 | 2010-12-01 | 复旦大学 | Original ecology separation and redispersion method of nano metallic colloid |
| CN102228995A (en) * | 2011-06-30 | 2011-11-02 | 华南理工大学 | Polysaccharide-nano silver sol and preparation method thereof |
| CN102990079A (en) * | 2012-12-05 | 2013-03-27 | 中国科学院合肥物质科学研究院 | Method for preparing silver nanoparticles with different sizes and particle assemblies with different shapes |
| CN105268988A (en) * | 2015-10-26 | 2016-01-27 | 昆明理工大学 | Method for preparing ultrafine spherical silver powder |
| CN105980055A (en) * | 2014-02-04 | 2016-09-28 | 拓自达电线株式会社 | Process for manufacturing supported nanocolloidal particles, and supported nanocolloidal particles |
| CN108453268A (en) * | 2018-02-08 | 2018-08-28 | 南京工业大学 | Core-shell type micron silver and preparation method and application thereof |
| CN109530717A (en) * | 2018-12-03 | 2019-03-29 | 安徽工业大学 | The method of microemulsion method controlledly synthesis Ag metal nano material in original position from Ag-containing solution |
| CN111364095A (en) * | 2020-03-18 | 2020-07-03 | 青岛大学 | Method for synthesizing small-size metal nanocrystalline |
| CN111838179A (en) * | 2020-07-23 | 2020-10-30 | 中国药科大学 | Turbulence-enhanced continuously-prepared broad-spectrum drug-resistant bacterium killing preparation as well as preparation method and application thereof |
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| US5147841A (en) * | 1990-11-23 | 1992-09-15 | The United States Of America As Represented By The United States Department Of Energy | Method for the preparation of metal colloids in inverse micelles and product preferred by the method |
| CN1202531C (en) * | 2003-01-14 | 2005-05-18 | 中山大学 | Low-content nanometer conducting silver paste and its prepn |
| CN1233447C (en) * | 2003-12-24 | 2005-12-28 | 华东理工大学 | Micro lactescence and its preparing method |
| JP4096061B2 (en) * | 2004-03-31 | 2008-06-04 | 独立行政法人産業技術総合研究所 | Method for producing metal nanoparticles using microemulsion in supercritical carbon dioxide |
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- 2005-11-11 CN CNB200510110310XA patent/CN100415413C/en not_active Expired - Fee Related
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| WO2008100163A1 (en) | 2007-02-13 | 2008-08-21 | Instytut Wlókien Naturalnych | Method of manufacturing silver nanoparticles, cellulosic fibers and nanofibers containing silver nanoparticles, fibers and nanofibers containing silver nanoparticles, use of silver nanoparticles to the manufacture of cellulosic fibers and nanofibers, and wound dressing containing silver nanoparticles |
| CN101898250A (en) * | 2010-07-20 | 2010-12-01 | 复旦大学 | Original ecology separation and redispersion method of nano metallic colloid |
| CN102228995A (en) * | 2011-06-30 | 2011-11-02 | 华南理工大学 | Polysaccharide-nano silver sol and preparation method thereof |
| CN102990079A (en) * | 2012-12-05 | 2013-03-27 | 中国科学院合肥物质科学研究院 | Method for preparing silver nanoparticles with different sizes and particle assemblies with different shapes |
| CN102990079B (en) * | 2012-12-05 | 2014-10-01 | 中国科学院合肥物质科学研究院 | Method for preparing silver nanoparticles with different sizes and particle assemblies with different shapes |
| CN105980055A (en) * | 2014-02-04 | 2016-09-28 | 拓自达电线株式会社 | Process for manufacturing supported nanocolloidal particles, and supported nanocolloidal particles |
| CN105980055B (en) * | 2014-02-04 | 2019-09-06 | 拓自达电线株式会社 | The manufacturing method and its loaded article of nano-colloid particulate load object |
| CN105268988A (en) * | 2015-10-26 | 2016-01-27 | 昆明理工大学 | Method for preparing ultrafine spherical silver powder |
| CN105268988B (en) * | 2015-10-26 | 2018-03-06 | 昆明理工大学 | A kind of preparation method of superfine spherical silver powder |
| CN108453268A (en) * | 2018-02-08 | 2018-08-28 | 南京工业大学 | Core-shell type micron silver and preparation method and application thereof |
| CN109530717A (en) * | 2018-12-03 | 2019-03-29 | 安徽工业大学 | The method of microemulsion method controlledly synthesis Ag metal nano material in original position from Ag-containing solution |
| CN111364095A (en) * | 2020-03-18 | 2020-07-03 | 青岛大学 | Method for synthesizing small-size metal nanocrystalline |
| CN111838179A (en) * | 2020-07-23 | 2020-10-30 | 中国药科大学 | Turbulence-enhanced continuously-prepared broad-spectrum drug-resistant bacterium killing preparation as well as preparation method and application thereof |
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