CN103691966B - A kind of method preparing nano silver particles based on poly-(2-acrylamide-2-methylpro panesulfonic acid) - Google Patents
A kind of method preparing nano silver particles based on poly-(2-acrylamide-2-methylpro panesulfonic acid) Download PDFInfo
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- CN103691966B CN103691966B CN201410004754.4A CN201410004754A CN103691966B CN 103691966 B CN103691966 B CN 103691966B CN 201410004754 A CN201410004754 A CN 201410004754A CN 103691966 B CN103691966 B CN 103691966B
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- acrylamide
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- silver particles
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Abstract
The invention discloses a kind of method preparing nano silver particles based on poly-(2-acrylamide-2-methylpro panesulfonic acid), the method poly-(2-acrylamide-2-methylpro panesulfonic acid) is added to the water to be mixed with emulsion, sodium hypophosphite solution is added in described emulsion, after stirring, described emulsion heated up, in described emulsion, drip liquor argenti nitratis ophthalmicus carries out reduction reaction, after reduction reaction completes simultaneously, breakdown of emulsion, centrifugal, washing, dry, obtain nano silver particles; The method is simply effective, and easily-controlled reaction conditions, is applicable to suitability for industrialized production; Obtained nano silver particles pattern and even particle size distribution, not easily reunite, have extensive use potentiality in fields such as medicine, chemical industry, electronic device, conducing composite materials.
Description
Technical field
The present invention relates to a kind of method 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 21 century important new material, 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 a part important in metal nanoparticle research.
The preparation method of nano silver particles has multiple, and thermal decomposition method, Gas condensation method, electrochemical process, biochemical process, chemical reduction method etc. are the several methods adopted at present.Wherein, chemical reduction method is one of the simplest, effective method.In chemical reduction method, mainly use reducing agent, as sodium hypophosphite, sodium borohydride, trisodium citrate etc., the aqueous solution of reduction silver nitrate obtains.The nano silver particles of polymolecularity, small particle diameter can be obtained by surfactant, as polyvinyl alcohol, neopelex etc. in prior art.But obtained nano silver particles is very easily reunited, pattern is irregular, domain size distribution is wide in range.
Summary of the invention
The present invention is directed to the defect that nano silver particles existence is very easily reunited, pattern is irregular, domain size distribution is wide in range prepared by method of the prior art, object there are provided one to prepare pattern rule and even particle size distribution, the method of the nano silver particles of not easily reuniting, the method is simply effective, easy to control, be applicable to suitability for industrialized production.
The invention provides a kind of method preparing nano silver particles based on poly-(2-acrylamide-2-methylpro panesulfonic acid), the method poly-(2-acrylamide-2-methylpro panesulfonic acid) is added to the water preparation to obtain poly-(2-acrylamide-2-methylpro panesulfonic acid) emulsion that mass fraction is 5 ~ 30%, sodium hypophosphite solution is added in described emulsion, the mass concentration of sodium phosphate in described emulsion is made to reach 0.003 ~ 0.009g/mL, after stirring, described emulsion is warming up to 35 ~ 45 DEG C, in described emulsion, drip concentration is that the liquor argenti nitratis ophthalmicus of 0.1 ~ 0.3g/mL carries out reduction reaction simultaneously, 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 by mass percent be the 2-acrylamide-2-methylpro panesulfonic acid aqueous solution of 15 ~ 25% under 60 ~ 70 DEG C of conditions, obtained by polymerisation; 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) as surfactant first by reduction method for preparing nanometer silver particles, obtained nano silver particles pattern rule and even particle size distribution, have the advantages that not easily reunite, as can be seen from the embodiment of the present invention 1 and the obtained nano silver particles of comparative example 1 domain size distribution normal curve figure: the obtained nano silver particles domain size distribution of the embodiment of the present invention 1 is narrower (there is narrower spike in a of Fig. 3, that can find out the nano silver particles near 100nm in Fig. 4 occupies 57.373% of the Nano Silver of whole preparation, particle diameter occupies 82.132% at below 106nm particle, illustrate that particle diameter majority is near 100nm, particle diameter narrow distribution), particle diameter little (can find out in a of Fig. 3 that average grain diameter is at about 100nm), pattern rule (Fig. 2 can see the spherical particle of even particle size), and the nano silver particles domain size distribution wider (occurring wider bimodal in the b of Fig. 3) that comparative example 1 is obtained, particle diameter large (can find out in the b of Fig. 3 that average grain diameter is at about 1000nm), the nano silver particles agglomeration that comparative example 1 obtains is obvious.
Accompanying drawing explanation
XRD figure: a of the nano silver particles that [Fig. 1] obtains for standard crystalline state silver and the embodiment of the present invention 1 is standard crystalline state silver collection of illustrative plates, and b is the XRD figure of the nano silver particles that embodiment 1 obtains.
The scanning electron microscope diagram of the nano silver particles that [Fig. 2] obtains for embodiment 1: a is 30,000 × image, and b is 50,000 × image.
[Fig. 3] the domain size distribution normal curve of nano silver particles for preparing in emulsion: a to be the domain size distribution normal curve figure of nano silver particles prepared by embodiment 1, b be nano silver particles obtained in comparative example 1 domain size distribution normal curve figure.
The histogram of particle size distribution of the nano silver particles that [Fig. 4] is prepared for embodiment 1.
Detailed description of the invention
Following specific embodiment is intended to further illustrate content of the present invention, and unrestricted the scope of protection of the invention.Embodiment 1
Nano silver particles is prepared in 5wt%PAAMPS emulsion
Getting 30.0g2-acrylamide-2-methylpro panesulfonic acid (AAMPS) joins in 120g distilled water, and add 0.015g APS after dissolving, be slowly warming up to 65 DEG C after stirring and dissolving, isothermal reaction 4h, finally obtains PAAMPS.
Get 5.0g PAAMPS to join in 95.0g distilled water and be configured to the PAAMPS emulsion that mass fraction is 5%, 0.44g sodium hypophosphite to be dissolved in 10mL distilled water and to join in the emulsion of the PAAMPS of 100mL mass fraction 5%, subsequently after electric stirring 15 minutes, reaction system is warming up to 40 DEG C, drip the liquor argenti nitratis ophthalmicus 10mL containing 1.42g, rate of addition controls at 15 ~ 20 droplets/point, 90 minutes reaction time; Add acetone breakdown of emulsion, centrifugal, washing subsequently, drying obtains nano silver particles, nano silver particles XRD schemes as shown in Figure 1, and as shown in Figure 2, domain size distribution is as shown in Fig. 3 (a) He Fig. 4, and nano silver particles average grain diameter is about 100nm for scanning electron microscope diagram.
Embodiment 2
Nano silver particles is prepared in 10wt%PAAMPS emulsion
Getting 30.0g2-acrylamide-2-methylpro panesulfonic acid (AAMPS) joins in 120g distilled water, and add 0.015g APS after dissolving, be slowly warming up to 65 DEG C after stirring and dissolving, isothermal reaction 4h, finally obtains PAAMPS.
Get 10.0g PAAMPS to join in 90.0g distilled water and be configured to the PAAMPS emulsion that mass fraction is 10%, 0.44g sodium hypophosphite to be dissolved in 10mL distilled water and to join in the emulsion of the PAAMPS of 100mL mass fraction 10%, subsequently after electric stirring 15 minutes, reaction system is warming up to 40 DEG C, drip the liquor argenti nitratis ophthalmicus 10mL containing 1.42g, rate of addition controls at 15 ~ 20 droplets/point, 70 minutes reaction time; Add acetone breakdown of emulsion, centrifugal, washing subsequently, drying obtains nano silver particles, nano silver particles average grain diameter is about 100nm.
Example 1 is executed in contrast
Nano silver particles is prepared in 5wt% neopelex emulsion
Get 5.0g neopelex and join in 95.0g distilled water that to be configured to mass fraction be emulsion in the neopelex emulsion of 5%, 0.44g sodium hypophosphite to be dissolved in 10mL distilled water and to join 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 DEG C, drip the liquor argenti nitratis ophthalmicus 10mL containing 1.42g, rate of addition controls at 15 ~ 20 droplets/point, 90 minutes reaction time; Add acetone breakdown of emulsion, centrifugal, washing subsequently, drying obtains nano silver particles, domain size distribution as shown in Figure 3 (b).
Claims (6)
1. prepare the method for nano silver particles based on poly-(2-acrylamide-2-methylpro panesulfonic acid) for one kind, it is characterized in that, (2-acrylamide-2-methylpro panesulfonic acid) will be gathered be added to the water preparation and obtain poly-(2-acrylamide-2-methylpro panesulfonic acid) emulsion that mass fraction is 5 ~ 30%, sodium hypophosphite solution is added in described emulsion, the mass concentration of sodium hypophosphite in described emulsion is made to reach 0.003 ~ 0.009g/mL, after stirring, described emulsion is warming up to 35 ~ 45 DEG C, in described emulsion, drip concentration is that the liquor argenti nitratis ophthalmicus of 0.1 ~ 0.3g/mL carries out reduction reaction simultaneously, 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, described poly-(2-acrylamide-2-methylpro panesulfonic acid) be by mass percent be the 2-acrylamide-2-methylpro panesulfonic acid aqueous solution of 15 ~ 25% under 60 ~ 70 DEG C of conditions, obtained by polymerisation.
6. the method as described in any one of Claims 1 to 5, is characterized in that, described nano silver particles average grain diameter is 80 ~ 120nm.
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| 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 |
| 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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| KR100836659B1 (en) * | 2006-07-06 | 2008-06-10 | 삼성전기주식회사 | Method for manufacturing metal nanoparticles |
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| 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 |
| 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 |
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