CN107008921B - A method of preparing nano silver - Google Patents
A method of preparing nano silver Download PDFInfo
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- CN107008921B CN107008921B CN201710206932.5A CN201710206932A CN107008921B CN 107008921 B CN107008921 B CN 107008921B CN 201710206932 A CN201710206932 A CN 201710206932A CN 107008921 B CN107008921 B CN 107008921B
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- B82—NANOTECHNOLOGY
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Abstract
The present invention discloses a kind of method for preparing nano silver, prepare the mixed solution of silver ammino solution and polyglycol solution, the mixed solution of soluble starch solution and hydrazine hydrate solution is prepared again, two kinds of mixed solutions are subjected to ultrasonic atomizatio respectively, and two kinds of aerosols is made to contact with each other the raw reaction of hybrid concurrency, gained aaerosol solution obtains nano silver by washing repeatedly；Silver ammino solution and soluble starch solution are carried out ullrasonic spraying by the present invention, mixed solution concentration is improved in the uniformity of part, avoid the generation of the solution selfdecomposition phenomenon and bulky grain monomer silver in conventional nano silvery Preparation Method, prepared nano silver stable structure and it is uniform, Argent grain size is in nanoscale；Integrated artistic is simple, and device is easy, and easy to operate, energy conservation and environmental protection can be realized volume production.
Description
Technical field
The present invention relates to a kind of methods for preparing nano silver, belong to technical field of nano material.
Background technique
Nano particle refers to the particle in the size in the one-dimensional space between 1-100nm.What nano silver particles had receives
Many macroscopic materials such as skin effect, bulk effect, quantum size effect, the macro quanta tunnel effect of rice material are not had
Special nature.Nano silver particles do not have drug resistance as antibacterial agent, more next as antibiotic and sterilizing material using safe natural
More it is valued by people.Nano silver releases silver ion in the solution, and silver ion has very strong bactericidal properties.
Nano silver have excellent thermal conductivity, electric conductivity, surface-active and catalytic performance, optics, catalysis, microelectronics,
The fields such as bio-sensing, antibacterial have very big potentiality.As a kind of emerging functional material, nano silver is widely used as catalysis material
Material, antistatic material, low temperature superconducting material, biosensor material, electric slurry and antibacterial bacteriostatic material.
Chemical Physics ring locating for the performance of nano silver and its structure, pattern, size and size distribution and material itself
Border is closely related, and pattern, size and the size distribution of nano silver can come by using different synthetic technology and reaction condition
Regulation.The preparation of traditional nano silver is divided into physical method and chemical method.Physical method requires relatively high, producing cost to instrument and equipment
It is expensive.Chemical method is used as reducing agent using vitamin, glucose, sucrose, formaldehyde etc., but its reproducibility is limited, and is made
Nano silver is easy to happen reunion.
It is put into a large amount of protective agent to avoid the reunion of nano silver from generalling use currently, preparing in the method for nano silver,
In the most frequently used protective agent have polyvinylpyrrolidone, polyvinyl alcohol, gelatin and chitosan polymer etc., but this kind of protective agent is general
All over toxic, medical product cannot be used.
Summary of the invention
Of the existing technology in order to overcome the problems, such as, the present invention provides a kind of method for preparing nano silver, specifically include with
Lower step:
(1) preparation of silver ammino solution
The silver nitrate suspension that molar concentration is 0.1-0.2mol/L is prepared, adds the ammonium hydroxide that mass fraction is 25% extremely
Suspension clarification, then pH value is adjusted to 10-11 with NaOH solution, obtain silver ammino solution；
(2) preparation of polyglycol solution
Prepare the polyglycol solution that molar concentration is 0.05-0.1mol/L；
(3) preparation of soluble starch solution
Soluble starch is dissolved in the water, concentration is prepared is 5-8g/L soluble starch solution；
(4) preparation of mixed solution
The polyethylene glycol of the ratio of 5-10:1 by volume, the silver ammino solution for taking step (1) to prepare and step (2) preparation is molten
It is stirred 15-30min at 60 DEG C of liquid, is prepared into mixed solution A；The ratio of 1:1 by volume, take step (3) prepare can
Soluble starch solution and mass fraction are ultrasonic mixing 15min at 20 DEG C of hydrazine hydrate solution of 38%, are prepared into mixed solution B；
(5) preparation of nano silver
Isometric mixed solution A and mixed solution B are taken, two kinds of solution are added in reaction unit and carry out ultrasonic mist respectively
Change, two kinds of aerosols contact with each other, and hybrid concurrency is raw to react, and reaction temperature is 60-90 DEG C, reacts 10-15min, and it is anti-to collect product
Rehydration is washed till neutrality, obtains the nano silver suspending liquid of package soluble starch.
Step (5) described reaction unit, including ultrasonic atomizer I 1, ultrasonic nebulizer II 2, carrier gas conveying device 3, quartz
Pipe 4, heating device 5, receiving flask 6, vacuum pump 7, heating device 5 are wrapped in outside quartz ampoule 4,4 one end of quartz ampoule and ultrasonic mist
Change device I 1, ultrasonic nebulizer II 2 and carrier gas conveying device 3 are separately connected, the other end is connect with receiving flask 6, and receiving flask 6 is also and very
7 connection of sky pump.
The carrier gas conveying device 3 is air blower.
4 both ends of quartz ampoule are equipped with end cap, and end cap is equipped with connecting hole or quartz ampoule 4 and is blocked by glass cement, envelope
Connecting hole is left when stifled.
The heating device 4 is water bath with thermostatic control heating device or constant temperature oil bath heating device.
Water of the present invention is deionized water.
The partial size of the nano silver being prepared is 20-100nm, wraps up starch outside nano silver, forms core-shell structure.
The present invention compared with prior art possessed by advantage and positive effect:
(1) the method for the present invention is simple, and securely and reliably, equipment is simple, easy to operate, energy conservation and environmental protection, it is easy to accomplish serialization
Preparation, can be realized volume production.
(2) soluble starch that the present invention uses both can be used as the template in nano silver preparation process, can also be affected
For the shell of core-shell structure.
(3) it is dense to improve mixed solution by the contact between ultrasonic atomizatio solution, the raw reaction of hybrid concurrency for the method for the present invention
The uniformity in part is spent, the life of the solution selfdecomposition phenomenon and bulky grain monomer silver in conventional nano silvery Preparation Method is avoided
At the size of the nano silver of formation is easy to control, and concentration is limited, thus can avoid incident in conventional chemical reduction method
The formation of nano silver selfdecomposition, silver mirror reaction and bulky grain silver simple substance and so on.
(4) stability of nano silver prepared by the present invention is high, and uniform particle sizes, Argent grain size contains in nanoscale, impurity
Measuring extremely low, prepared nano silver can store for a long time；And there are extremely strong bactericidal properties, can be used for medical field.
Detailed description of the invention
Fig. 1 is the structural schematic diagram for the reaction unit that the embodiment of the present invention 1 uses；
Fig. 2 is the XRD diagram for the nano silver that the embodiment of the present invention 1 obtains；
Fig. 3 is the TEM figure for the nano silver that the embodiment of the present invention 1 obtains；
Fig. 4 is the TEM figure for the nano silver that the embodiment of the present invention 2 obtains；
In figure, 1- ultrasonic nebulizer I, 2- ultrasonic nebulizer II, 3- carrier gas conveying device, 4- quartz ampoule, 5- heating device,
6- receiving flask, 7- vacuum pump.
Specific embodiment
The present invention is described in further details in the following with reference to the drawings and specific embodiments.
Embodiment 1
A kind of method for preparing nano silver of the present embodiment, specifically includes the following steps:
(1) preparation of silver ammino solution
Weigh 169.87mg silver nitrate be dissolved in 10mL go it is outstanding from the silver nitrate that concentration is 0.1mol/L is obtained in water
Supernatant liquid adds ammonium hydroxide to the suspension that mass fraction is 25% and clarifies, then the NaOH solution for being 5mol/L with concentration adjusts pH value
To 10, silver ammino solution is obtained；
(2) preparation of polyglycol solution
Prepare the polyglycol solution that molar concentration is 0.05mol/L；
(3) preparation of soluble starch solution
Weigh 0.6g soluble starch be dissolved in 100mL heat go from be prepared in water concentration be 6g/L solubility form sediment
Powder solution；
(4) preparation of mixed solution
The ratio of 5:1 by volume, the polyglycol solution of the silver ammino solution for taking step (1) to prepare and step (2) preparation
It is added to the container, is stirred 15min at 60 DEG C, is prepared into mixed solution A；The ratio of 1:1 by volume takes step (3)
The hydrazine hydrate solution that the soluble starch solution and mass fraction of preparation are 38% is added in another container, and ultrasound is mixed at 20 DEG C
15min is closed, mixed solution B is prepared into；
(5) preparation of nano silver
Reaction unit adopted in this step, as shown in Figure 1, including ultrasonic nebulizer I 1, ultrasonic nebulizer II 2, carrier gas
Conveying device 3, quartz ampoule 4, heating device 5, receiving flask 6, vacuum pump 7, heating device 5 are water bath with thermostatic control heating device, quartz
Pipe 4 is immersed in constant temperature water bath apparatus, is heated by constant temperature water bath apparatus, 4 one end of quartz ampoule and ultrasonic atomizer I 1, ultrasonic mist
Change device II 2 and carrier gas conveying device 3 is separately connected, carrier gas conveying device 3 is air blower, and 4 other end of quartz ampoule and receiving flask 6 connect
It connects, receiving flask 6 is also connect with vacuum pump 7, and the product that completion is reacted in quartz ampoule 4 is extracted into receiving flask 6 by vacuum pump 7, quartz
4 both ends of pipe are equipped with end cap, and end cap is equipped with connecting hole for connecting；
When use, the mixed solution A and mixed solution B for taking isometric step (4) to prepare are added separately to ultrasonic atomizatio
In device I 1 and ultrasonic atomizer II 2, it is powered and carries out ultrasonic atomizatio, using 3 air blower of carrier gas conveying device using air as carrier gas
Atomized drop is sent into quartz ampoule 4, maximum condensation rate is sprayed into and is greater than 3 ml/mins, quartz ampoule 4 is controlled using heating device 5
Interior temperature is 60 DEG C, reacts 15min, and the water mist extraction after reaction is collected into receiving flask 6 by vacuum pump 7, will be collected
Aaerosol solution washed repeatedly with deionized water to after neutral, obtain nano silver suspending liquid.
The XRD diagram for the product that Fig. 2 is shown, the product being prepared as seen from the figure are silver；What Fig. 3 was shown
The TEM of product schemes, it can be seen that obtained product does not reunite and has core-shell structure, it is nanometer by core known to analysis
Silver, having a size of 20-100nm, it be shell is starch that it is external, which to be wrapped in it,.
Embodiment 2
A kind of method for preparing nano silver of the present embodiment, specifically includes the following steps:
(1) preparation of silver ammino solution
Weigh 212.5mg silver nitrate be dissolved in 10mL go it is outstanding from the silver nitrate that concentration is 0.125mol/L is obtained in water
Supernatant liquid adds ammonium hydroxide to the suspension that mass fraction is 25% and clarifies, then the NaOH solution for being 5mol/L with concentration adjusts pH value
To 11, silver ammino solution is obtained；
(2) preparation of polyglycol solution
Preparation molar concentration is 0.06mol/L polyglycol solution；
(3) preparation of soluble starch solution
Weigh 0.7g soluble starch be dissolved in 100mL heat go from be prepared in water concentration be 7g/L solubility form sediment
Powder solution；
(4) preparation of mixed solution
The ratio of 7:1 by volume, the polyglycol solution of the silver ammino solution for taking step (1) to prepare and step (2) preparation
It is added to the container, is stirred 20min at 60 DEG C, is prepared into mixed solution A；The ratio of 1:1 by volume takes step (3)
The hydrazine hydrate solution that the soluble starch solution and mass fraction of preparation are 38% is added in another container, and ultrasound is mixed at 20 DEG C
15min is closed, mixed solution B is prepared into；
(5) preparation of nano silver
Reaction unit adopted in this step is that constant temperature oil bath refueling device, quartz ampoule 4 pass through glass in addition to heating device 5
Glue blocks, when closure leave connecting hole for connect it is outer other are same as Example 1, when use, take isometric step (4)
The mixed solution A and mixed solution B of preparation are added separately in ultrasonic atomizer I 1 and ultrasonic atomizer II 2, are powered and are carried out ultrasound
Atomized drop is sent into quartz ampoule 4 using 3 air blower of carrier gas conveying device using air as carrier gas, sprays into most dense fog by atomization
Rate is greater than 3 ml/mins, uses heating device 5 to control the temperature in quartz ampoule 4 as 70 DEG C, reacts 10min, pass through vacuum
Water mist extraction after reaction is collected into receiving flask 6 by pump 7, and the aaerosol solution of collection is washed repeatedly with deionized water to neutrality
Afterwards, nano silver suspending liquid is obtained.
Fig. 4 show the TEM figure for the product that the present embodiment obtains, it can be seen that obtained product is not reunited and had
There is core-shell structure, be nano silver by core known to analysis, having a size of 20-100nm, it be shell is starch that it is external, which to be wrapped in it,.
Embodiment 3
A kind of method for preparing nano silver of the present embodiment, specifically includes the following steps:
(1) preparation of silver ammino solution
Weigh 255mg silver nitrate be dissolved in 10mL go from obtained in water concentration be 0.15mol/L silver nitrate suspend
Liquid, add mass fraction be 25% ammonium hydroxide to suspension clarify, then with concentration be 5mol/L NaOH solution adjust pH value to
10, obtain silver ammino solution；
(2) preparation of polyglycol solution
Preparation molar concentration is 0.075mol/L polyglycol solution；
(3) preparation of soluble starch solution
Weigh 0.8g soluble starch be dissolved in 100mL heat go from be prepared in water concentration be 8g/L solubility form sediment
Powder solution；
(4) preparation of mixed solution
The ratio of 9:1 by volume, the polyglycol solution of the silver ammino solution for taking step (1) to prepare and step (2) preparation
It is added to the container, is stirred 25min at 60 DEG C, is prepared into mixed solution A；The ratio of 1:1 by volume takes step (3)
The hydrazine hydrate solution that the soluble starch solution and mass fraction of preparation are 38% is added in another container, and ultrasound is mixed at 20 DEG C
15min is closed, mixed solution B is prepared into；
(5) preparation of nano silver
The used reaction unit of this step is same as Example 1, when use, takes isometric step (4) to prepare mixed
It closes solution A and mixed solution B is added separately in ultrasonic atomizer I 1 and ultrasonic atomizer II 2, be powered and carry out ultrasonic atomizatio, use
Atomized drop is sent into quartz ampoule 4 by 3 air blower of carrier gas conveying device using air as carrier gas, is sprayed into maximum condensation rate and is greater than 3
Ml/min uses heating device 5 to control the temperature in quartz ampoule 4 as 80 DEG C, reacts 12min, will be reacted by vacuum pump 7
Water mist extraction afterwards is collected into receiving flask 6, and the aaerosol solution of collection is washed with deionized water to after neutrality repeatedly, is received
The silver-colored suspension of rice.
Embodiment 4
A kind of method for preparing nano silver of the present embodiment, specifically includes the following steps:
(1) preparation of silver ammino solution
Weigh 340mg silver nitrate be dissolved in 10mL go from obtained in water concentration be 0.2mol/L silver nitrate suspend
Liquid, add mass fraction be 25% ammonium hydroxide to suspension clarify, then with concentration be 5mol/L NaOH solution adjust pH value to
11, obtain silver ammino solution；
(2) preparation of polyglycol solution
Preparation molar concentration is 0.1mol/L polyglycol solution；
(3) preparation of soluble starch solution
Weigh 0.5g soluble starch be dissolved in 100mL heat go from be prepared in water concentration be 5g/L solubility form sediment
Powder solution；
(4) preparation of mixed solution
The ratio of 10:1 by volume, the polyglycol solution of the silver ammino solution for taking step (1) to prepare and step (2) preparation
It is added to the container, is stirred 30min at 60 DEG C, is prepared into mixed solution A；The ratio of 1:1 by volume takes step (3)
The hydrazine hydrate solution that the soluble starch solution and mass fraction of preparation are 38% is added in another container, and ultrasound is mixed at 20 DEG C
15min is closed, mixed solution B is prepared into；
(5) preparation of nano silver
Reaction unit adopted in this step is same as Example 2, when use, isometric step (4) is taken to prepare
Mixed solution A and mixed solution B are added separately in ultrasonic atomizer I 1 and ultrasonic atomizer II 2, are powered and are carried out ultrasonic atomizatio, adopt
It uses 3 air blower of carrier gas conveying device that atomized drop is sent into quartz ampoule 4 using air as carrier gas, sprays into maximum condensation rate and be greater than
3 ml/mins use heating device 5 to control the temperature in quartz ampoule 4 as 90 DEG C, react 13min, will be reacted by vacuum pump 7
Water mist extraction afterwards is collected into receiving flask 6, and the aaerosol solution of collection is washed with deionized water to after neutrality repeatedly, is received
The silver-colored suspension of rice.
Embodiment described above is only several embodiments of the invention, and the description thereof is more specific and detailed, but can not
Therefore limitations on the scope of the patent of the present invention are interpreted as, it is noted that for those of ordinary skill in the art,
Without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection model of the invention
It encloses.
Claims (5)
1. a method of prepare nano silver, which is characterized in that specifically includes the following steps:
(1) preparation of silver ammino solution
The silver nitrate suspension that molar concentration is 0.1-0.2mol/L is prepared, the ammonium hydroxide that mass fraction is 25% is added and extremely suspends
Liquid clarification, then pH value is adjusted to 10-11 with NaOH solution, obtain silver ammino solution；
(2) preparation of polyglycol solution
Prepare the polyglycol solution that molar concentration is 0.05-0.1mol/L；
(3) preparation of soluble starch solution
Soluble starch is dissolved in the water, concentration is prepared is 5-8g/L soluble starch solution；
(4) preparation of mixed solution
The ratio of 5-10:1 by volume, the polyglycol solution 60 of the silver ammino solution for taking step (1) to prepare and step (2) preparation
It is stirred 15-30min at DEG C, is prepared into mixed solution A；The ratio of 1:1 by volume, the solubility for taking step (3) to prepare
Starch solution and mass fraction are ultrasonic mixing 15min at 20 DEG C of hydrazine hydrate solution of 38%, are prepared into mixed solution B；
(5) preparation of nano silver
Isometric mixed solution A and mixed solution B are taken, two kinds of solution are added in reaction unit and carry out ultrasonic atomizatio respectively,
Two kinds of aerosols contact with each other, and hybrid concurrency is raw to react, and reaction temperature is 60-90 DEG C, reacts 10-15min, collects product repeatedly
It is washed to neutrality, obtains the nano silver suspending liquid of package soluble starch.
2. preparing the method for nano silver according to claim 1, which is characterized in that step (5) described reaction unit, including it is super
Sound atomizer I (1), ultrasonic nebulizer II (2), carrier gas conveying device (3), quartz ampoule (4), heating device (5), receiving flask (6),
Vacuum pump (7), heating device (5) are wrapped in quartz ampoule (4) outside, and quartz ampoule (4) one end and ultrasonic atomizer I (1), ultrasound are sprayed
Day with fog II (2) and carrier gas conveying device (3) are separately connected, and the other end is connect with receiving flask (6), and receiving flask (6) is gone back and vacuum pump
(7) it connects.
3. preparing the method for nano silver according to claim 2, which is characterized in that the carrier gas conveying device (3) is air blast
Machine.
4. preparing the method for nano silver according to claim 2, which is characterized in that quartz ampoule (4) both ends are equipped with end cap,
End cap is equipped with connecting hole or quartz ampoule (4) by glass cement closure, and when closure leaves connecting hole.
5. preparing the method for nano silver according to claim 2, which is characterized in that heating device (5) is water bath with thermostatic control heating
Device or constant temperature oil bath heating device.
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| CN116196919A (en) * | 2023-03-07 | 2023-06-02 | 广西至善新材料科技有限公司 | Nano silver microsphere catalyst and preparation method and application thereof |
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| CN101941075A (en) * | 2009-07-03 | 2011-01-12 | 北京印刷学院 | Synthetic method of antibacterial agent containing nano-silver |
| CN103691967B (en) * | 2014-01-09 | 2016-01-27 | 三河市京纳环保技术有限公司 | A kind of simple method for preparing of novel extensive nano-silver hydrosol |
| CN105345029B (en) * | 2015-12-11 | 2017-07-11 | 广东工业大学 | The method that one kettle way prepares nano silver gel |
| CN106001608B (en) * | 2016-07-11 | 2017-11-28 | 上海理工大学 | A kind of method that silver nano-grain is prepared using water soluble starch |
| CN106270500B (en) * | 2016-09-30 | 2019-02-19 | 昆明理工大学 | A kind of carbon nano tube surface uniformly coats the method and device of metallic silver |
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