CN103381485B - A kind of method preparing 3-mercaptopropionic acid parcel silver nano-grain - Google Patents
A kind of method preparing 3-mercaptopropionic acid parcel silver nano-grain Download PDFInfo
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- CN103381485B CN103381485B CN201210509883.XA CN201210509883A CN103381485B CN 103381485 B CN103381485 B CN 103381485B CN 201210509883 A CN201210509883 A CN 201210509883A CN 103381485 B CN103381485 B CN 103381485B
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Abstract
One prepares the method for 3 mercaptopropionic acids (MPA) parcel silver nano-grain, belongs to technical field of nanometer material preparation.The problem such as it is responsible for, cost is high, yield poorly for existing silver nano-grain preparation technology, the invention discloses the method that one prepares 3 mercaptopropionic acids (MPA) parcel silver nano-grain, its technical scheme is: first by toluene and oleyl amine mix homogeneously, adds AgNO3Solid and NaBH4Oil phase silver nano-grain is obtained after aqueous solution, fully reaction；It is subsequently adding methanol/acetone extractant, reacts to a large amount of precipitation of generation, after being centrifuged, take solid product；MPA adds solid product again, and reaction terminates rear centrifugation and obtains solid product；Solid product, after ethanol and ultra-pure water clean, adds ultra-pure water ice-bath ultrasonic and disperses 2 10min, regulates pH 8 12, i.e. obtains MPA and wraps up silver nano-grain.Present invention process is simple, low cost, and yield is high, and granule small particle is more uniform.
Description
Technical field
The present invention relates to the method that one prepares 3-mercaptopropionic acid (MPA) parcel silver nano-grain, belong to
In technical field of nanometer material preparation.
Background technology
The silver nano-grain of MPA parcel is a kind of particle diameter to be accomplished nanoscale and the metal wrapped up by MPA
Pathogenic microorganism escherichia coli are had strong suppression and killing action, and will not produce drug resistance by silver simple substance
Property.Silver nano-grain also has antibacterial, deodorization and absorbs the function of some ultra violet rays, therefore can be applicable to
Pharmaceuticals industry and cosmetic industry.In addition, silver nano material has special optical property, and this makes
The purposes obtaining silver nano material is more extensive, attention in numerous nano materials.And prepare in the past
The shortcoming that the method for silver nano-grain generally exists that cost is high, yields poorly, particle size dispersion is excessive.Therefore,
The new method of silver nano-grain is prepared in exploration, and the preparation method of research silver nano-grain is for following reality
Utilization has great importance.
The synthetic method of silver nano-grain mainly has physical method and chemical method.Physical principle is simple,
Products obtained therefrom impurity is few, quality is high, but requires higher to instrument and equipment, and producing cost is expensive, typically
It is applicable to the size and dimension of nano silver particles requires prepared by the highest industrialization.Chemical method synthesis
Nano silver particles is mainly used in optics, electricity and the biomedicine etc. higher to nanoparticle performance requirement
Field, its key technology is how to control the size of granule, narrower particle size distribution and obtain specific and equal
Even crystalline structure.The present invention uses solution phase chemical reduction, the advantage of this method be apparatus and process simple,
Productivity is high, be easy to industrialized production, and prepared argentum powder granularity is little, favorable reproducibility.
Summary of the invention
It is an object of the invention to prepare a kind of Nanoparticle Size uniform, the water-soluble silver that size is less is received
The method of rice grain, the method technique is simple, low cost, and yield is high, and granule small particle is more uniform.
The present invention provides a kind of method that solution phase chemical reduction prepares silver nano-grain, including following step
Rapid:
1) take 10-30mL toluene and 1-5mL oleyl amine stirs to obtain clear solution, add 1-5mmol
AgNO3, heated and stirred to being completely dissolved, AgNO3It is completely dissolved and obtains clear solution, add 0.5-2
mol L-1 NaBH4Aqueous solution, keeps temperature 40-90 DEG C and carries out magnetic agitation.After reaction terminates,
Obtain oil-soluble silver nano-grain to be scattered in the toluene solution on upper strata, use separatory funnel separatory, obtain
Oil phase silver nano-grain.
2) taking oil phase silver nano-grain and add methanol/acetone extractant, the mixing reaction of vortex vortex mixer is to producing
Raw a large amount of precipitation, at 20 DEG C, centrifugal 10min under 10000g.Collect solid-state and be centrifuged product, add
A small amount of toluene dissolves, and adds the mixing of methanol/acetone solvent extraction vortex vortex mixer and extremely produces a large amount of precipitation,
Under 10000g, centrifugal 10min, abandons supernatant.
3) collect solid-state and be centrifuged product, add a small amount of toluene and dissolve, add MPA, ultrasonic 5-20min,
At 20 DEG C, centrifugal 10min under 10000g.
4) collect solid-state and be centrifuged product and with ethanol purge, 20 DEG C, be centrifuged 10min under 10000g.
Collect solid-state and be centrifuged product, clean with ultra-pure water, 20 DEG C, centrifugal 10min under 10000g, abandon
Clear liquid.
5) collect solid-state and be centrifuged product, add ultra-pure water ice-bath ultrasonic dispersion 2-10min, regulate pH
8-12。
Synthetic route is as follows:
Figure of description
Fig. 1 is the silver nano-grain transmission electron microscope photo according to embodiment 1 preparation: oil-soluble silver is received
Rice grain；
Fig. 2 is the silver nano-grain transmission electron microscope photo according to embodiment 1 preparation: MPA parcel
Water-soluble silver nano-particle；
Fig. 3 is the silver nano-grain transmission electron microscope photo according to embodiment 2 preparation: oil-soluble silver is received
Rice grain；
Fig. 4 is the silver nano-grain transmission electron microscope photo according to embodiment 2 preparation: MPA parcel
Water-soluble silver nano-particle.
Detailed description of the invention
Embodiment 1:
2ml oleyl amine mixes with 20ml toluene, adds 0.169g AgNO3, stirring is to dissolving；Add 1mol
L-1Sodium borohydride solution 15ml, 60 DEG C of stirring in water bath reaction 4h.After reaction terminates, separatory takes upper strata and obtains
Oil phase silver nano-grain (Fig. 1)
Taking oil phase silver nano-grain and add methanol and the mixed liquor of acetone 1:1, the mixing reaction of vortex vortex mixer is extremely
Produce a large amount of precipitation, 20 DEG C, under 10000g, be centrifuged 10min；Collect solid-state and be centrifuged product, add 3mL
Toluene dissolves, and adds methanol and the mixed liquor of acetone 1: 1, and the mixing reaction of vortex vortex mixer is a large amount of heavy to producing
Form sediment, 20 DEG C, centrifugal 10min under 10000g, abandon supernatant, collect solid-state and be centrifuged product, add 3mL
Toluene dissolves, 1ml MPA, ice-bath ultrasonic reaction 10min, then 20 DEG C, centrifugal 10min under 10000g.
Collect solid-state and be centrifuged product, add washes of absolute alcohol, ice-bath ultrasonic 20min, 20 DEG C, under 10000g from
Heart 10min, abandons supernatant, adds ultra-pure water and cleans, ice-bath ultrasonic 20min, 20 DEG C, under 10000 × g
Centrifugal 10min, abandons supernatant, collects solid-state and is centrifuged product, adds the dispersion of ultra-pure water ice-bath ultrasonic, uses NaOH
Adjusting pH is 9.33, obtains MPA parcel silver nano-grain (Fig. 2)
Embodiment 2:
4ml oleyl amine 40ml toluene mixes, and adds 0.341g AgNO3, stirring is to dissolving；Add 1mol L-1
Sodium borohydride solution 30ml, 60 DEG C of stirring in water bath reaction 2h.After reaction terminates, separatory takes upper strata and obtains oil phase
Silver nano-grain (Fig. 3).
Taking oil phase silver nano-grain and add methanol and the mixed liquor of acetone 1: 1, the mixing reaction of vortex vortex mixer is extremely
Produce a large amount of precipitation, 20 DEG C, centrifugal 10min under 10000g；Collect solid-state and be centrifuged product, add 3mL
After toluene dissolves, adding methanol and the mixed liquor of acetone 1: 1, the mixing reaction of vortex vortex mixer is a large amount of to producing
Precipitation, 20 DEG C, centrifugal 10min under 10000 × g, abandon supernatant.Collect solid-state and be centrifuged product, add 3mL
After toluene dissolves, add 1ml MPA, after ultrasonic reaction 10min, 20 DEG C, centrifugal 10min under 10000g.
Collect solid-state and be centrifuged product, add washes of absolute alcohol, after ultrasonic 20min, 20 DEG C, under 10000g from
Heart 10min, abandons supernatant, adds ultra-pure water and cleans, ultrasonic 20min, 20 DEG C, centrifugal under 10000g
10min, abandons supernatant.Collect solid-state and be centrifuged product, add ultra-pure water ultrasonic disperse, adjust by NaOH solution
PH is 9.16, obtains MPA parcel silver nano-grain (Fig. 4).
Claims (4)
1. the method preparing 3-mercaptopropionic acid parcel silver nano-grain, it is characterised in that the method includes as follows
Step:
1. by toluene and oleyl amine mix homogeneously, AgNO is added3Solid and NaBH4After aqueous solution, fully reaction
Obtain oil phase silver nano-grain；
2. in oil phase silver nano-grain, add methanol/acetone extractant, after a large amount of precipitation of reaction to generation, centrifugal
After take solid product；
3. MPA adds solid product, ultrasonic reaction 5-20min, and reaction terminates rear centrifugation and obtains solid-state
Product；
4. solid product is after ethanol and ultra-pure water clean, and adds ultra-pure water ice-bath ultrasonic dispersion 2-10min, adjusts
Joint pH is to alkalescence.
Method the most according to claim 1, it is characterised in that in the preparation of oil phase silver nano-grain toluene and
The volume of oleyl amine is respectively 10-30mL and 1-5mL, AgNO3Amount be 1-5mmol.
Method the most according to claim 1, it is characterised in that in the preparation of oil phase silver nano-grain, constant temperature is adopted
With heating in water bath, temperature is 40-90 DEG C.
Method the most according to claim 1, it is characterised in that step 4. in, regulate its pH to 8-12.
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| CN111838180B (en) * | 2020-07-31 | 2021-06-08 | 武汉大学 | Ag-MPA layered material and preparation method thereof |
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