CN103691966A - Method for preparing silver nanoparticles based on poly(2-acrylamino-2-methyl propanesulfonic acid) - Google Patents
Method for preparing silver nanoparticles based on poly(2-acrylamino-2-methyl propanesulfonic acid) Download PDFInfo
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- CN103691966A CN103691966A CN201410004754.4A CN201410004754A CN103691966A CN 103691966 A CN103691966 A CN 103691966A CN 201410004754 A CN201410004754 A CN 201410004754A CN 103691966 A CN103691966 A CN 103691966A
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- panesulfonic acid
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Abstract
The invention discloses a method for preparing silver nanoparticles based on poly(2-acrylamino-2-methyl propanesulfonic acid). The method comprises the steps of adding poly(2-acrylamino-2-methyl propanesulfonic acid) to water to prepare emulsion, adding a sodium hypophosphite solution to the emulsion, stirring evenly, and then heating the emulsion, dropwise adding a silver nitrate solution into the emulsion, performing reduction reaction, and then demulsifying, centrifuging, washing and drying to obtain silver nanoparticles. The method is simple and effective and applicable to industrial production, and reaction conditions are easily-controllable; the prepared silver nanoparticles are even in distribution of morphologies and particle sizes, unlikely to gather and extensive in application potentiality in fields of medicine, chemical industry, electronic devices and conductive composite materials, and the like.
Description
Technical field
The present invention relates to a kind of method of preparing nano silver particles based on poly-(2-acrylamide-2-methylpro panesulfonic acid); Belong to metal nano material field.
Background technology
Nano material is described as important new material of 21 century, is one of current study hotspot.In metal nano material field, nano silver material has the characteristics such as high electric conductivity, strong bactericidal properties, catalytic, be widely used in the fields such as electronic device, bio-sensing, bactericide, catalyst, become an important part in metal nanoparticle research.
The preparation method of nano silver particles has multiple, and thermal decomposition method, condensation of gas method, electrochemical process, biochemical process, chemical reduction method etc. are the several methods adopting at present.Wherein, chemical reduction method is one of the simplest, effective method.The main reducing agent that uses in chemical reduction method, as sodium hypophosphite, sodium borohydride, trisodium citrate etc., the aqueous solution of reduction silver nitrate obtains.In prior art, by surfactant, can make the nano silver particles of polymolecularity, small particle diameter, as polyvinyl alcohol, neopelex etc.But the nano silver particles making is very easily reunited, pattern is irregular, particle diameter distributes wide in range.
Summary of the invention
The present invention is directed to nano silver particles prepared by method of the prior art exist very easily reunite, pattern is irregular, particle diameter distributes wide in range defect, object is to be to provide a kind of to prepare pattern rule and particle diameter is evenly distributed, the method that is difficult for the nano silver particles of reunion, the method is simply effective, easy to control, be applicable to suitability for industrialized production.
The invention provides a kind of method of preparing nano silver particles based on poly-(2-acrylamide-2-methylpro panesulfonic acid), the method is poly-(2-acrylamide-2-methylpro panesulfonic acid) to be added to the water to preparation to obtain mass fraction be poly-(2-acrylamide-2-methylpro panesulfonic acid) emulsion of 5～30%, in described emulsion, add sodium hypophosphite solution, make the mass concentration of sodium phosphate in described emulsion reach 0.003～0.009g/mL, after stirring, described emulsion is warming up to 35～45 ℃, to dripping concentration in described emulsion, be simultaneously that the liquor argenti nitratis ophthalmicus of 0.1～0.3g/mL carries out reduction reaction, after reduction reaction completes, breakdown of emulsion, centrifugal, washing, dry, obtain nano silver particles, the mol ratio of described sodium hypophosphite and silver nitrate is 1～1.5:2.
In preferred poly-(2-acrylamide-2-methylpro panesulfonic acid) emulsion, the mass fraction of poly-(2-acrylamide-2-methylpro panesulfonic acid) is 5～15%.
Described liquor argenti nitratis ophthalmicus rate of addition is 15～20/min.
The described reduction reaction time is 1～1.5h.
Described poly-(2-acrylamide-2-methylpro panesulfonic acid) (PAAMPS) be the 2-acrylamide-2-methylpro panesulfonic acid aqueous solution that is 15～25% by mass percent under 60～70 ℃ of conditions, by polymerisation, make; Described polymerization reaction time is 3～5h.
Described nano silver particles average grain diameter is 80～120nm; Be preferably 90～110nm.
Beneficial effect of the present invention: the present invention adopts poly-(2-acrylamide-2-methylpro panesulfonic acid) to pass through reduction method for preparing nanometer silver particles as surfactant first, the nano silver particles pattern rule and the particle diameter that make are evenly distributed, have the advantages that to be difficult for reunion, the nano silver particles making from the embodiment of the present invention 1 and comparative example 1 particle diameter distribution normal curve figure can find out: (a of Fig. 3, there is narrower spike in the nano silver particles particle diameter narrow distribution that the embodiment of the present invention 1 makes, in Fig. 4, can find out near nano silver particles 100nm the Nano Silver that occupies whole preparation 57.373%, particle diameter occupies 82.132% at the following particle of 106nm, illustrate that particle diameter is most near 100nm, particle diameter narrow distribution), particle diameter little (can find out in a of Fig. 3 that average grain diameter is in 100nm left and right), pattern rule (Fig. 2 can see the spherical particle of even particle size), and the nano silver particles particle diameter wider distribution that comparative example 1 makes (occurring wider bimodal in the b of Fig. 3), particle diameter large (can find out in the b of Fig. 3 that average grain diameter is in 1000nm left and right), the nano silver particles agglomeration that comparative example 1 makes is obvious.
Accompanying drawing explanation
XRD figure of the nano silver particles that [Fig. 1] makes for standard crystalline state silver and the embodiment of the present invention 1: a is standard crystalline state silver collection of illustrative plates, b is that the XRD of the nano silver particles that makes of embodiment 1 schemes.
The scanning electron microscope diagram of the nano silver particles that [Fig. 2] makes for embodiment 1: a is 30,000 * image, b is 50,000 * image.
The particle diameter distribution normal curve that [Fig. 3] is the nano silver particles prepared in emulsion: a is the particle diameter distribution normal curve figure of the nano silver particles of embodiment 1 preparation, the particle diameter distribution normal curve figure that b is the nano silver particles that makes in comparative example 1.
[Fig. 4] is the histogram of particle size distribution of the nano silver particles of embodiment 1 preparation.
The specific embodiment
Following specific embodiment is intended to further illustrate content of the present invention, and unrestricted the scope of protection of the invention.Embodiment 1
In 5wt%PAAMPS emulsion, prepare nano silver particles
Get 30.0g2-acrylamide-2-methylpro panesulfonic acid (AAMPS) and join in 120g distilled water, add 0.015g APS after dissolving, be slowly warming up to 65 ℃ after stirring and dissolving, isothermal reaction 4h, finally obtains PAAMPS.
Get 5.0g PAAMPS and join that in 95.0g distilled water, to be configured to mass fraction be 5% PAAMPS emulsion, 0.44g sodium hypophosphite is dissolved in 10mL distilled water and joins in the emulsion of PAAMPS of 100mL mass fraction 5%, subsequently after electric stirring 15 minutes, reaction system is warming up to 40 ℃, the liquor argenti nitratis ophthalmicus 10mL that dropping contains 1.42g, rate of addition is controlled at 15～20 droplets/minute, 90 minutes reaction time; Add subsequently acetone breakdown of emulsion, centrifugal, washing, dry obtain nano silver particles, nano silver particles XRD scheme as shown in Figure 1, and as shown in Figure 2, particle diameter distributes as shown in Fig. 3 (a) and Fig. 4 scanning electron microscope diagram, and nano silver particles average grain diameter is about 100nm.
In 10wt%PAAMPS emulsion, prepare nano silver particles
Get 30.0g2-acrylamide-2-methylpro panesulfonic acid (AAMPS) and join in 120g distilled water, add 0.015g APS after dissolving, be slowly warming up to 65 ℃ after stirring and dissolving, isothermal reaction 4h, finally obtains PAAMPS.
Get 10.0g PAAMPS and join that in 90.0g distilled water, to be configured to mass fraction be 10% PAAMPS emulsion, 0.44g sodium hypophosphite is dissolved in 10mL distilled water and joins in the emulsion of PAAMPS of 100mL mass fraction 10%, subsequently after electric stirring 15 minutes, reaction system is warming up to 40 ℃, the liquor argenti nitratis ophthalmicus 10mL that dropping contains 1.42g, rate of addition is controlled at 15～20 droplets/minute, 70 minutes reaction time; Add subsequently acetone breakdown of emulsion, centrifugal, washing, the dry nano silver particles that obtains, nano silver particles average grain diameter is 100nm left and right.
Example 1 is executed in contrast
In 5wt% neopelex emulsion, prepare nano silver particles
Get 5.0g neopelex and join that in 95.0g distilled water, to be configured to mass fraction be emulsion in 5% neopelex emulsion, 0.44g sodium hypophosphite is dissolved in 10mL distilled water and joins in the emulsion in the neopelex emulsion of 100mL mass fraction 5%, subsequently after electric stirring 15 minutes, reaction system is warming up to 40 ℃, the liquor argenti nitratis ophthalmicus 10mL that dropping contains 1.42g, rate of addition is controlled at 15～20 droplets/minute, 90 minutes reaction time; Add subsequently acetone breakdown of emulsion, centrifugal, washing, dry obtain nano silver particles, particle diameter distributes as shown in Figure 3 (b).
Claims (6)
1. a method of preparing nano silver particles based on poly-(2-acrylamide-2-methylpro panesulfonic acid), it is characterized in that, to gather (2-acrylamide-2-methylpro panesulfonic acid) is added to the water preparation to obtain mass fraction is poly-(2-acrylamide-2-methylpro panesulfonic acid) emulsion of 5～30%, in described emulsion, add sodium hypophosphite solution, make the mass concentration of sodium phosphate in described emulsion reach 0.003～0.009g/mL, after stirring, described emulsion is warming up to 35～45 ℃, to dripping concentration in described emulsion, be simultaneously that the liquor argenti nitratis ophthalmicus of 0.1～0.3g/mL carries out reduction reaction, after reduction reaction completes, breakdown of emulsion, centrifugal, washing, dry, obtain nano silver particles, the mol ratio of described sodium hypophosphite and silver nitrate is 1～1.5:2.
2. the method for claim 1, is characterized in that, in described poly-(2-acrylamide-2-methylpro panesulfonic acid) emulsion, the mass fraction of poly-(2-acrylamide-2-methylpro panesulfonic acid) is 5～15%.
3. the method for claim 1, is characterized in that, described liquor argenti nitratis ophthalmicus rate of addition is 15～20/min.
4. the method for claim 1, is characterized in that, the described reduction reaction time is 1～1.5h.
5. the method for claim 1, it is characterized in that, poly-(2-acrylamide-2-methylpro panesulfonic acid) aqueous solution that described poly-(2-acrylamide-2-methylpro panesulfonic acid) is is 15～25% by mass percent, under 60～70 ℃ of conditions, makes by polymerisation.
6. the method as described in claim 1～5 any one, is characterized in that, described nano silver particles average grain diameter is 80～120nm.
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| CN106219592A (en) * | 2016-07-27 | 2016-12-14 | 常州大学 | The formation of nanoscale silver oxide and process for dispersing |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005220435A (en) * | 2003-10-22 | 2005-08-18 | Mitsuboshi Belting Ltd | Method of producing metal nanoparticle and dispersion of metal nanoparticle |
| JP2006328472A (en) * | 2005-05-26 | 2006-12-07 | Mitsui Chemicals Inc | Production method of silver nanoparticle, silver nanoparticle and application thereof |
| JP2008031518A (en) * | 2006-07-28 | 2008-02-14 | Furukawa Electric Co Ltd:The | Nanorod, and method for producing nanorod |
| US20080087137A1 (en) * | 2006-07-06 | 2008-04-17 | Samsung Electro-Mecanics Co., Ltd. | Method for manufacturing metal nanoparticles |
| WO2009024312A2 (en) * | 2007-08-17 | 2009-02-26 | Albert-Ludwigs-Universität Freiburg | Method for the production and stabilization of functional metal nanoparticles in ionic liquids |
| CN101921443A (en) * | 2010-08-06 | 2010-12-22 | 浙江大学 | Preparation method of high-strength intelligent hydrogel doped with nanoparticles in homogeneous manner |
| CN102985452A (en) * | 2010-06-25 | 2013-03-20 | 可泰克斯有限合伙公司 | Alkali-swellable acrylic emulsions comprising acrylic acid, use thereof in aqueous formulations and formulations containing same |
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Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005220435A (en) * | 2003-10-22 | 2005-08-18 | Mitsuboshi Belting Ltd | Method of producing metal nanoparticle and dispersion of metal nanoparticle |
| JP2006328472A (en) * | 2005-05-26 | 2006-12-07 | Mitsui Chemicals Inc | Production method of silver nanoparticle, silver nanoparticle and application thereof |
| US20080087137A1 (en) * | 2006-07-06 | 2008-04-17 | Samsung Electro-Mecanics Co., Ltd. | Method for manufacturing metal nanoparticles |
| JP2008031518A (en) * | 2006-07-28 | 2008-02-14 | Furukawa Electric Co Ltd:The | Nanorod, and method for producing nanorod |
| WO2009024312A2 (en) * | 2007-08-17 | 2009-02-26 | Albert-Ludwigs-Universität Freiburg | Method for the production and stabilization of functional metal nanoparticles in ionic liquids |
| CN102985452A (en) * | 2010-06-25 | 2013-03-20 | 可泰克斯有限合伙公司 | Alkali-swellable acrylic emulsions comprising acrylic acid, use thereof in aqueous formulations and formulations containing same |
| CN101921443A (en) * | 2010-08-06 | 2010-12-22 | 浙江大学 | Preparation method of high-strength intelligent hydrogel doped with nanoparticles in homogeneous manner |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106219592A (en) * | 2016-07-27 | 2016-12-14 | 常州大学 | The formation of nanoscale silver oxide and process for dispersing |
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