CN107552810A - A kind of preparation method of Nano Silver isometric particle - Google Patents
A kind of preparation method of Nano Silver isometric particle Download PDFInfo
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- CN107552810A CN107552810A CN201710826441.0A CN201710826441A CN107552810A CN 107552810 A CN107552810 A CN 107552810A CN 201710826441 A CN201710826441 A CN 201710826441A CN 107552810 A CN107552810 A CN 107552810A
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Abstract
The present invention relates to a kind of preparation method of Nano Silver isometric particle, silver salt is scattered in polyalcohol by this method, obtains silver salt dispersion liquid；Polyvinylpyrrolidone is scattered in polyalcohol, obtains polyvinylpyrrolidone dispersion liquid；Hydrochloric acid is scattered in polyalcohol, obtains hydrochloric acid dispersion liquid；The silver nitrate dispersion liquid that will be obtained, polyvinylpyrrolidone dispersion liquid and the mixing of hydrochloric acid dispersion liquid, reaction, product separation of solid and liquid, obtain Nano Silver isometric particle.The preparation method process is simple, yield is high, reaction system is simple, easily controllable, can reliablely and stablely obtain the Nano Silver isometric particle of high-purity.
Description
Technical field
The invention belongs to metal nano material field, is related to a kind of preparation method of Nano Silver isometric particle.
Background technology
Silver nano material is one kind of nano material.In various metal nano materials, silver nano material is excellent due to its
Characteristic electron, optical characteristics, mechanical property and catalysis characteristics, while there is good antibacterial characteristics, bio-compatibility and table
The focus that the advantages that face is easily modified is studied as whole world scientist.Industrially, silver nano material is a kind of very important
Nano material, in bio-medical field, chemical catalysis field, ceramic material field, sewage treatment area, paint field and high property
Energy electrode material field is all widely used.Particularly, the one kind of silver nanoparticle cubic material as silver nano material, compared to
The silver nano material of other patterns, there is the optical signalling enhancing characteristic, catalysis characteristics etc. of highly significant, be widely used as surface etc.
Ion reinforcing material and Raman reinforcing material, it is the focus of recent researches.
The key obstacle that silver nano material is widely applied is that it is difficult to stable synthesize.The preparation method of nano material
Have a lot, be broadly divided into chemical method, physical method and biological reducing method etc..Chemical reduction method have it is simple to operate,
The features such as stable reaction is controllable, particle diameter distribution is uniform, therefore be widely used for preparing nano silver material.The general step of this method
For in dicyandiamide solution, metal ion to be reduced into the process of metal simple-substance in the atmosphere of surfactant with reducing agent.
In the synthesis of nano-Ag particles, polyol process is also its main synthetic method.The master that the preparation of current nano-Ag particles runs into
Problem is wanted to be the stability and reaction yield of its preparation process, the preparative-scale of nano-Ag particles is mostly milligram level at present
Not, and stability can not be guaranteed.
CN104889418A discloses a kind of biological synthesis method of cube shaped nano silver particles, and this method is with sweet orange peel
Extract solution and Lotus Leaf Extracts are reducing agent and protective agent, using silver nitrate as silver-colored source, regulation mixed liquor to suitable pH environment,
It is in relatively regular cube shaped nano silver particles that reaction, which obtains form, at 60 DEG C, this method step complexity, cumbersome, final product by
The influence of mixed liquor pH value and the dosage of extract solution is very big, and reaction product is unstable.
CN106001607A disclose it is a kind of prepare the cubical method of Nano Silver in hydrophobic phase, this method using oleyl amine as
Solvent, silver bromide are silver-colored source, and triphenylphosphine reacts 2h for stabilizer at 250 DEG C and obtains Nano Silver cube product, this method
Synthesis condition requires high, expensive needed for reaction, while final product has more accessory substance, and subsequent purification process is answered
It is miscellaneous, and obtained Nano Silver cube product can only be dissolved in hydrophobic solvent, seriously limit the selection of its dispersant.
The content of the invention
To solve the problems, such as that existing nano-Ag particles synthetic technology is present, the invention provides a kind of Nano Silver isometric particle
Preparation method, the preparation method process is simple, and yield is high, and reaction system is simple, easily controllable, can reliablely and stablely obtain
The Nano Silver isometric particle of high-purity.
In order to realize above-mentioned purpose, the present invention uses following technical scheme：
The invention provides a kind of preparation method of Nano Silver isometric particle, the described method comprises the following steps：
(1) silver salt is scattered in polyalcohol, obtains silver salt dispersion liquid；Polyvinylpyrrolidone is scattered in polyalcohol
In, obtain polyvinylpyrrolidone dispersion liquid；Hydrochloric acid is scattered in polyalcohol, obtains hydrochloric acid dispersion liquid；
(2) silver salt dispersion liquid, polyvinylpyrrolidone dispersion liquid and the mixing of hydrochloric acid dispersion liquid obtained step (1),
Silver ion reduction can be made separation of solid and liquid, to obtain Nano Silver isometric particle to be reacted under conditions of argent.
As the preferable technical scheme of the present invention, the polyalcohol used in step (1) each dispersion liquid each stands alone as second
Any one in glycol, diethylene glycol (DEG), glycerine, 1,2-PD or pentaerythrite or at least two any combination, it is preferably
Ethylene glycol.
As the preferable technical scheme of the present invention, step (1) described silver salt is silver acetate, silver bromide, silver nitrate or chlorine
Change in silver any one or at least two combination, preferably silver nitrate.
As the preferable technical scheme of the present invention, silver-colored concentration is 85~110mM in step (1) the silver-colored dispersion liquid,
Preferably 90mM.
As the present invention preferable technical scheme, step (1) described polyvinylpyrrolidone include PVPK12,
Any one in PVPK15, PVPK30, PVPK45, PVPK60 or PVPK-70 or at least two combination, preferably PVPK30；
Preferably, the concentration of polyvinylpyrrolidone is 90~180mM in step (1) the polyvinylpyrrolidone dispersion liquid, preferably
For 120~150mM.
As the preferable technical scheme of the present invention, in step (1) the hydrochloric acid dispersion liquid concentration of hydrogen chloride for 1~
30mM, preferably 8~18mM.
As the preferable technical scheme of the present invention, when being mixed in step (2), silver, polyvinylpyrrolidone and hydrochloric acid
Molar ratio be 30%~45% silver medal：50%~64% polyvinylpyrrolidone：0.1%~0.9% hydrochloric acid.
As the preferable technical scheme of the present invention, step (2) reaction is carried out under agitation, the rotating speed of the stirring
For 400~1500r/min, preferably 600~1200r/min, preferably 700~1000r/min；Such as 650r/min, 800r/
Min, 1100r/min or 1300r/min etc., it is not limited to cited numerical value, other are unrequited in the number range
Numerical value is equally applicable；
Preferably, the temperature of step (2) described reaction is 120~180 DEG C, preferably 130 DEG C~160 DEG C, is more preferably
140 DEG C~160 DEG C, such as 120 DEG C, 140 DEG C, 150 DEG C or 160 DEG C etc., it is not limited to cited numerical value, the numerical value model
Other unrequited numerical value are equally applicable in enclosing.
Preferably, the time of step (2) described reaction is 12~36h, preferably 10~24h, more preferably 14~20h, such as
12h, 15h, 18h or 20h etc., it is not limited to cited numerical value, other interior unrequited numerical value of the number range are same
It is applicable.
As the preferable technical scheme of the present invention, the method for step (2) described separation of solid and liquid includes filtering, sedimentation, steamed
Hair or centrifugation in any one or at least two combination, preferably centrifuge.
As the preferable technical scheme of the present invention, the preparation method also includes：
(3) the Nano Silver isometric particle obtained after step (2) described separation of solid and liquid is washed and dried；
Preferably, step (3) cleaning solution that uses of washing is deionized water, any one in absolute ethyl alcohol or acetone
Kind or any two kinds of combination, preferably deionized water.
Preferably, the method for step (3) described drying is vacuum drying or constant pressure and dry, is preferably dried in vacuo.
As the preferable technical scheme of the present invention, the preparation method comprises the following steps：
(1) silver salt is scattered in polyalcohol, the silver salt dispersion liquid that concentration is 85~110mM is obtained, by polyvinyl pyrrole
Alkanone is scattered in polyalcohol, obtains the polyvinylpyrrolidone dispersion liquid that concentration is 90~180mM, preferably 120~150mM,
Hydrochloric acid is scattered in polyalcohol, obtains the hydrochloric acid dispersion liquid that concentration is 1~30mM, preferably 8~18mM；
(2) the silver salt dispersion liquid for obtaining step (1), polyvinylpyrrolidone and the mixing of hydrochloric acid dispersion liquid, 400~
15-36h is reacted under 1500r/min rotating speed at 120~160 DEG C, separation of solid and liquid, is washed, dries, obtains Nano Silver cube
Grain.
The Nano Silver isometric particle obtained according to preparation method provided by the invention has cubic structure, its average chi
It is very little generally in more than 40nm, such as 80nm, and in below 400nm, such as 220nm, and standard deviation, within 10nm, purity is at least
It is for example, at least 85% for 70%.
The Nano Silver isometric particle obtained according to preparation method provided by the invention is suitable to a variety of applications, such as being catalyzed
The fields such as material, optical characterisation.
Compared with prior art, preparation method of the invention at least has the advantages that：
(1) present invention provides a kind of preparation method of Nano Silver isometric particle, and raw material used in this method is substantially nontoxic
Pollution-free, reaction is simple to operation, and process is simple, low without special reaction condition requirement, equipment requirement.
(2) the invention provides a kind of preparation method of Nano Silver isometric particle, methods described is single step reaction, is reacted
Cheng Wending is easy to control, and final product purity is higher, needs not move through the purge process of complexity.
(3) the invention provides a kind of preparation method of Nano Silver isometric particle, methods described under optimal conditions, most
End-product size is controllable, can meet different requirements.
(4) present invention provides a kind of preparation method of Nano Silver isometric particle, and methods described primary first-order equation yield is higher, can
To meet the requirement routinely applied.
Embodiment
Of the invention for ease of understanding, illustrative example of the present invention is as follows.It will be understood by those skilled in the art that the embodiment
Only it is to aid in understanding the present invention, is not construed as the concrete restriction to the present invention.
Embodiment 1
A kind of preparation method of Nano Silver isometric particle, this method comprise the following steps：
(1) 0.85mmol silver nitrate is scattered in 10mL ethylene glycol, obtains silver nitrate dispersion liquid, by 0.96mmol's
PVPK30 is scattered in 10ml ethylene glycol, obtains polyvinylpyrrolidone dispersion liquid, and 0.003mmol hydrochloric acid is scattered in into 3ml
Ethylene glycol in, obtain hydrochloric acid dispersion liquid；
(2) silver nitrate dispersion liquid, polyvinylpyrrolidone dispersion liquid and the mixing of hydrochloric acid dispersion liquid obtained step (1),
140 DEG C of reaction 20h, centrifuge, obtain initial Nano Silver isometric particle under 800r/min stirrings；
(3) using deionized water as solvent, the Nano Silver isometric particle that step (2) is obtained centrifuges under 3000rpm rotating speeds
Washing, treat that the boarding of Nano Silver isometric particle to centrifugation bottom of the tube, discards supernatant, to complete once washing operation, and repeats to be somebody's turn to do
Three times, the precipitation for collecting to obtain is placed in air drying 2h in vacuum drying oven to washing operation, obtains final Nano Silver cube
Grain.
Embodiment 2
A kind of preparation method of Nano Silver isometric particle, this method comprise the following steps：
(1) 1.1mmol silver nitrate is scattered in 10mL ethylene glycol, obtains silver nitrate dispersion liquid, by 1.3mmol's
PVPK30 is scattered in 10ml ethylene glycol, obtains polyvinylpyrrolidone dispersion liquid, and 0.018mmol hydrochloric acid is scattered in into 3ml
Ethylene glycol in, obtain hydrochloric acid dispersion liquid；
(2) the silver nitrate dispersion liquid for obtaining step (1), polyvinylpyrrolidone dispersion liquid and the mixing of hydrochloric acid dispersion liquid,
140 DEG C of reaction 20h, centrifuge, obtain initial Nano Silver isometric particle under 800r/min stirrings；
(3) using deionized water as solvent, the Nano Silver isometric particle that step (2) is obtained centrifuges under 3000rpm rotating speeds
Washing, treat that the boarding of Nano Silver isometric particle to centrifugation bottom of the tube, discards supernatant, to complete once washing operation, and repeats to be somebody's turn to do
Three times, the precipitation for collecting to obtain is placed in air drying 2h in vacuum drying oven to washing operation, obtains final Nano Silver cube
Grain.
Embodiment 3
A kind of preparation method of Nano Silver isometric particle, this method comprise the following steps：
(1) 0.85mmol silver nitrate is scattered in 10mL diethylene glycol (DEG)s, obtains silver nitrate dispersion liquid, by 0.96mmol's
PVPK70 is scattered in 10ml diethylene glycol (DEG)s, obtains polyvinylpyrrolidone dispersion liquid, and 0.003mmol hydrochloric acid is scattered in into 3ml
Diethylene glycol (DEG) in, obtain hydrochloric acid dispersion liquid；
(2) the silver nitrate dispersion liquid for obtaining step (1), polyvinylpyrrolidone dispersion liquid and the mixing of hydrochloric acid dispersion liquid,
140 DEG C of reaction 20h, centrifuge, obtain initial Nano Silver isometric particle under 800r/min stirrings；
(3) using deionized water as solvent, the Nano Silver isometric particle that step (2) is obtained centrifuges under 3000rpm rotating speeds
Washing, treat that the boarding of Nano Silver isometric particle to centrifugation bottom of the tube, discards supernatant, to complete once washing operation, and repeats to be somebody's turn to do
Three times, the precipitation for collecting to obtain is placed in air drying 2h in vacuum drying oven to washing operation, obtains final Nano Silver cube
Grain.
Embodiment 4
A kind of preparation method of Nano Silver isometric particle, this method comprise the following steps：
(1) 0.85mmol silver nitrate is scattered in 10mL ethylene glycol, obtains silver nitrate dispersion liquid, by 0.96mmol's
PVPK45 is scattered in 10ml ethylene glycol, obtains polyvinylpyrrolidone dispersion liquid, and 0.003mmol hydrochloric acid is scattered in into 3ml
Ethylene glycol in, obtain hydrochloric acid dispersion liquid；
(2) the silver nitrate dispersion liquid for obtaining step (1), polyvinylpyrrolidone dispersion liquid and the mixing of hydrochloric acid dispersion liquid,
150 DEG C of reaction 24h, centrifuge, obtain initial Nano Silver isometric particle under 1500r/min stirrings；
(3) using deionized water as solvent, the Nano Silver isometric particle that step (2) is obtained centrifuges under 3000rpm rotating speeds
Washing, treat that the boarding of Nano Silver isometric particle to centrifugation bottom of the tube, discards supernatant, to complete once washing operation, repeats this and wash
Wash operation three times, the precipitation for collecting to obtain is placed in air drying 2h in vacuum drying oven, obtains final Nano Silver isometric particle.
Embodiment 5
A kind of preparation method of Nano Silver isometric particle, the described method comprises the following steps：
(1) 0.85mmol silver acetate is scattered in 10mL glycerine, obtains silver acetate dispersion liquid, by 0.96mmol's
PVPK15 (5500) is scattered in 10ml glycerine, obtains polyvinylpyrrolidone dispersion liquid, and 0.003mmol hydrochloric acid is disperseed
In 3ml glycerine, hydrochloric acid dispersion liquid is obtained；
(2) the silver nitrate dispersion liquid for obtaining step (1), polyvinylpyrrolidone dispersion liquid and the mixing of hydrochloric acid dispersion liquid,
120 DEG C of reaction 36h, centrifuge, obtain initial Nano Silver isometric particle under 1000r/min stirrings；
(3) using deionized water as solvent, the Nano Silver isometric particle that step (2) is obtained centrifuges under 3000rpm rotating speeds
Washing, treat that the boarding of Nano Silver isometric particle to centrifugation bottom of the tube, discards supernatant, to complete once washing operation, and repeats to be somebody's turn to do
Three times, the precipitation for collecting to obtain is placed in air drying 2h in vacuum drying oven to washing operation, obtains final Nano Silver cube
Grain.
The average-size and purity for the Nano Silver isometric particle that embodiment 1-5 is prepared are tested, Size Distribution
Carried out with purity test by SEM (SEM) and laser particle analyzer by this area usual manner.As a result see
Shown in table 1.
Table 1
| Project | Size | Purity | Yield |
| Embodiment 1 | 135±7nm | 91% | 95% |
| Embodiment 2 | 153±10nm | 83% | 89% |
| Embodiment 3 | 148±9nm | 85% | 91% |
| Embodiment 4 | 175±12nm | 81% | 85% |
| Embodiment 5 | 240±13nm | 79% | 82% |
Applicant states that the present invention illustrates the detailed process equipment of the present invention and technological process by above-described embodiment,
But the invention is not limited in above-mentioned detailed process equipment and technological process, that is, it is above-mentioned detailed not mean that the present invention has to rely on
Process equipment and technological process could be implemented.Person of ordinary skill in the field it will be clearly understood that any improvement in the present invention,
The addition of equivalence replacement and auxiliary element to each raw material of product of the present invention, selection of concrete mode etc., all fall within the present invention's
Within the scope of protection domain and disclosure.
Claims (10)
1. a kind of preparation method of Nano Silver isometric particle, it is characterised in that the described method comprises the following steps：
(1) silver salt is scattered in polyalcohol, obtains silver salt dispersion liquid；Polyvinylpyrrolidone is scattered in polyalcohol, obtained
To polyvinylpyrrolidone dispersion liquid；Hydrochloric acid is scattered in polyalcohol, obtains hydrochloric acid dispersion liquid；
(2) silver salt dispersion liquid, polyvinylpyrrolidone dispersion liquid and the mixing of hydrochloric acid dispersion liquid obtained step (1), can make
Silver ion reduction separation of solid and liquid, obtains Nano Silver isometric particle to be reacted under conditions of argent.
2. preparation method according to claim 1, it is characterised in that used in step (1) each dispersion liquid polynary
Alcohol each stands alone as any one in ethylene glycol, diethylene glycol (DEG), glycerine, 1,2-PD or pentaerythrite or at least two times
Meaning combination, preferably ethylene glycol.
3. preparation method according to claim 1, it is characterised in that step (1) described silver salt be silver acetate, silver bromide,
In silver nitrate or silver chlorate any one or at least two combination, preferably silver nitrate.
4. preparation method according to claim 1, it is characterised in that silver-colored concentration in step (1) the silver salt dispersion liquid
For 85~110mM, preferably 90mM.
5. preparation method according to claim 1, it is characterised in that step (1) described polyvinylpyrrolidone includes
Any one in PVPK12, PVPK15, PVPK30, PVPK45, PVPK60 or PVPK70 or at least two combination, it is preferably
PVPK30；
Preferably, the concentration of polyvinylpyrrolidone is 90~180mM in step (1) the polyvinylpyrrolidone dispersion liquid,
Preferably 120~150mM.
6. preparation method according to claim 1, it is characterised in that hydrogen chloride in step (1) the hydrochloric acid dispersion liquid
Concentration is 1~30Mm, preferably 8~18Mm.
7. according to the preparation method described in claim 1 to 6 any one, it is characterised in that when being mixed in step (2), silver,
The molar ratio of polyvinylpyrrolidone and hydrochloric acid is 30%~45% silver medal：50%~64% polyvinylpyrrolidone：0.1%~
0.9% hydrochloric acid.
8. according to the preparation method described in claim 1 to 6 any one, it is characterised in that step (2) reaction is being stirred
Lower progress, the rotating speed of the stirring are 400~1500r/min, preferably 600~1200r/min, more preferably 700~
1000r/min；
Preferably, the temperature of step (2) described reaction is 120 DEG C~180 DEG C, preferably 130 DEG C~160 DEG C, more preferably 140
DEG C~160 DEG C；
Preferably, the time of step (2) described reaction is 12~36h, preferably 10~24h, more preferably 14~20h.
9. according to the preparation method described in claim 1 to 6 any one, it is characterised in that step (2) described separation of solid and liquid
Mode include filtering, sedimentation, evaporation or centrifugation in any one or at least two combination, preferably centrifuge.
10. according to the preparation method described in claim 1 to 6 any one, it is characterised in that the preparation method also includes：
(3) the Nano Silver isometric particle obtained after step (2) described separation of solid and liquid is washed and dried；
Preferably, step (3) it is described wash the cleaning solution that uses be in deionized water, absolute ethyl alcohol or acetone any one or
Any two kinds of combination, preferably deionized water；
Preferably, the method for step (3) described drying is vacuum drying or constant pressure and dry, is preferably dried in vacuo.
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| CN113600828A (en) * | 2021-08-19 | 2021-11-05 | 南京工业大学 | Protection method of silver nanoparticles |
| CN113953524A (en) * | 2021-10-12 | 2022-01-21 | 浙江工业大学 | Novel synthesis of nano-silver colloid by polyol solvothermal method |
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