CN108723390A - A kind of short-cut method preparing nano silver composite antibacterial agent - Google Patents
A kind of short-cut method preparing nano silver composite antibacterial agent Download PDFInfo
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- CN108723390A CN108723390A CN201810525376.2A CN201810525376A CN108723390A CN 108723390 A CN108723390 A CN 108723390A CN 201810525376 A CN201810525376 A CN 201810525376A CN 108723390 A CN108723390 A CN 108723390A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The invention discloses a kind of short-cut methods preparing nano silver composite antibacterial agent.Aqueous solution containing gamma-polyglutamic acid, source of silver ions, lithium magnesium silicate is pyrolyzed, the powder after pyrolysis is nano silver composite antibacterial agent.The present invention is a kind of easy smart way of combination Physical and chemical method, has the characteristics that easy, environmental protection, efficiently and with high antibacterial activity, and its nano silver particles grain size of prepared nano silver composite antibacterial agent is small, good dispersion, soilless sticking phenomenon, and can gradually be discharged from matrix and achieve the purpose that long-term antibacterial.
Description
Technical field：
The invention belongs to antiseptic preparation fields, and in particular to a kind of easy, inexpensive, efficient, environmental protection, favorable dispersibility
And the preparation method of the nano silver antimicrobials of agglomeration will not occur.
Background technology：
Nano material is a kind of new material of rapid development, wherein nano silver is that since the advent of the world is deep by people always
Concern, this is not only it with unique characteristic electron, optical characteristics, mechanical property and catalysis characteristics, and with good
Antibiotic property, the advantages that bio-compatibility and surface are easily modified.Therefore nano silver is in bio-medical material, the catalyst of chemical industry, pottery
Ceramic material, electrocondution slurry, sewage disposal, construction material, light absorbing material, coating, sensor, high performance electrode material etc. have
Wide application prospect becomes the important topic of functional material theoretical research and application and development with property.
Nano silver is one of currently used anti-biotic material, it refers to the metal silver particles between 1nm~100nm, is had
Significant skin effect, quantum size effect and quantum tunneling effect, show good antibacterial activity, are widely used in leading
The medical materials such as pipe and holder, surgical apparatus and wound healing gauze.Although silver nano material is in anti-biotic material and antibacterial
It is used widely in medical material, but existing production method cost high pollution is larger, in addition its particle is easy to by air
Oxidation and aggregation, lead to the decline of its anti-microbial property.
There are many preparation method of nano silver, generally speaking res divisibiles logos, chemical method and bioanalysis three categories.Different nanometers
The preparation method of silver respectively has advantage and disadvantage.Using existing method, the ball shaped nano silver particles of a variety of grain sizes and various are synthesized
The nano silver colloidal sol of color also synthesizes nano-silver thread and the dendritic silver nano material etc. with certain space structure.With
The progress of science and technology, nano silver production technology will develop to the direction that at low cost, consumption is low, pollution is low.
Invention content：
The object of the present invention is to provide a kind of easy, environmental protection, efficient and with high antibacterial activity nano silver composite antibacterials
The preparation method of agent, and its nano silver particles grain size of prepared nano silver composite antibacterial agent is small, good dispersion, soilless sticking are existing
As, and can gradually be discharged from matrix and achieve the purpose that long-term antibacterial.
The preparation method of nano silver provided by the invention is different from existing preparation method, on the one hand utilizes lithium magnesium silicate
Expansion energy forms the gel for including a large amount of Water Network structures in water, has preferable dispersibility, suspension, thickening property and thixotroping
Property and the characteristics such as good adsorptivity, large specific surface area adsorption capacity is strong after on the other hand utilizing gamma-polyglutamic acid high temperature cabonization
The characteristics of, the two combination can as the good carrier material of loading nano silvery, the nano silver that is prepared energy it is fully dispersed because
Without reuniting, and silver nitrate is energy formation element silver (2AgNO in high temperature pyrolysis3=2Ag+2NO2↑+O2↑), thus exists
Silver nitrate can also be made directly to be pyrolyzed into nano silver in carrier material carbonisation, be a kind of letter of combination Physical and chemical method
Just smart way has the characteristics that easy, environmentally friendly, efficient and has high antibacterial activity, and prepared nano silver composite antibacterial
Its nano silver particles grain size of agent is small, good dispersion, soilless sticking phenomenon, and can gradually be discharged from matrix and reach long-term antibacterial
Purpose, be a kind of nano silver new preparation technology with unique technology and cost advantage.
The short-cut method for preparing nano silver composite antibacterial agent of the present invention, which is characterized in that include the following steps：
Aqueous solution containing gamma-polyglutamic acid, silver ion, lithium magnesium silicate is pyrolyzed, the powder after pyrolysis is nanometer
Silver-colored complex antimicrobials.
The silver ion can be the various soluble salt for being capable of providing silver ion, preferably silver nitrate.
It is preferred that the gamma-polyglutamic acid aqueous solution of 10~30g/L of preparation mass-volume concentration, mass-volume concentration 10~
The silver nitrate aqueous solution of 30g/L；By mass volume ratio 1g：17-33ml mixes lithium magnesium silicate and water, and it is water-soluble to obtain lithium magnesium silicate
Liquid；
By lithium magnesium silicate：The ratio of gamma-polyglutamic acid aqueous solution=1g ︰ 5-10ml is poly- by lithium magnesium silicate aqueous solution and γ-
Glutamic acid aqueous solution is mixed to get mixed liquor, then presses lithium magnesium silicate：The ratio of silver nitrate aqueous solution=1g ︰ 12-18ml is by nitric acid
Silver-colored aqueous solution is added in mixed liquor, and mixture is made, mixture is placed in crucible, when 380-420 DEG C of heated baking, heating
Between be 10-60 minute, collect the powder after heating, drying, it is cooling after nano silver composite antibacterial agent to obtain the final product.
The gamma-polyglutamic acid can be：CN1932007A, it is entitled：The poly- paddy of γ-
It propylhomoserin producing strains and is prepared using the method for the preparing gamma-polyglutamic acid.
The lithium magnesium silicate can be according to document【Organically-modified and to Cr (VI) the characterization of adsorption of lithium magnesium silicate,
Chemical Journal of Chinese Universities, 38 (2)：173~181】In synthesis method by using hydrothermal method synthesize it, preparation process is:Weigh 1.0g
LiCl is put into beaker, and a certain amount of water is added and is completely dissolved to it.Weigh 13.5g MgCl2·6H2O is put into another beaker
In, the ammonium hydroxide of 2mol/L is slowly added into and fills MgCl2·6H2It in the beaker of O and stirs, makes MgCl2It fully reacts and is formed
Mg(OH)2Precipitation；Supercentrifuge is used to centrifuge 20min to solution under the conditions of rotating speed 16000r/min after reaction, so
Precipitation is washed with deionized by gained Mg (OH) in profit afterwards2It is transferred in LiCl solution, is sufficiently stirred to form mixing slurry
Then 27.8g Na are added in liquid2SiO3·9H2O (waterglass) simultaneously stirs evenly mixed serum is finally placed in hydrothermal reaction kettle
In, hydro-thermal reaction 72h., which waits for that suspension being placed in centrifuge tube after reaction, at 150 DEG C is centrifuged (centrifuge speed
16000r/min, centrifugation time 20min), then centrifugation product is washed using deionized water, and in an oven in 70 DEG C
Lower drying for 24 hours, then utilizes mortar grinder sample, can be by 200 mesh standard sieves to get to lithium magnesium silicate sample.
Nano silver composite antibacterial agent being prepared in situ by what Physical and chemical method were combined the present invention provides a kind of
Method.Nano silver grain size can be prepared in 10-60nm in black powder nano silver composite antibacterial according to above-mentioned preparation method
Agent can reach 90%-100% to the sterilizing rate of Escherichia coli and staphylococcus aureus.Made from the method for the present invention
Nano silver composite antibacterial agent, since lithium magnesium silicate has preferable dispersibility, and polyglutamic acid is after pyrolytic process, degradable
For soft, loose and porous charcoal.This carbonaceous matrix has high load capability, this can support metal nanoparticle
Dispersion, and keep its stability by protecting the aggregation of metal nanoparticle and oxidation.In addition, the baking charcoal obtained
Enough permeability can be shown, so that embedded nano silver (AgNPs) is easily discharged from matrix to kill bacterium.
Compared with chemical reduction method, this pyrolysis strategy of patent of the present invention seems that easy, efficient, cost-effectiveness is high,
Therefore it is more advantageous to applied to industry manufacture.In addition, compared with chemical method, it does not have to generate the pollutants such as solvent substantially.?
To the composite material for being adsorbed with nano silver (AgNPs) be used as antibacterial filler, the nanocomposite of preparation can be with
For multiple industries such as coating, antibacterial material for air purification.And prepared nano silver composite antibacterial agent its nano silver particles grain
Diameter is small, good dispersion, soilless sticking phenomenon, and can gradually be discharged from matrix and achieve the purpose that long-term antibacterial.
Specific implementation mode：
The following examples are further illustrations of the invention, rather than limiting the invention.
Embodiment 1：
The gamma-polyglutamic acid powder for weighing 2g is dissolved in the distilled water of 100ml, and 2% gamma-polyglutamic acid solution is made；
It weighs 2g silver nitrates to be dissolved in the distilled water of 100ml, 2% silver nitrate solution is made；1g lithium magnesium silicates are weighed, porcelain crucible is packed into
In, it is added in the distilled water of 33mL, then 2% gamma-polyglutamic acid that 7ml is made into is added on one side stirring the while of being added inside
Then the silver nitrate solution of above-mentioned 2% be made into of 15ml is added in solution.Then by the porcelain crucible equipped with mixture, it is placed in Muffle
With 400 DEG C of heated bakings in stove, heating time is 40 minutes.After muffle furnace reduces and then collects above-mentioned heating, drying
Powder is gradually cooling to room temperature indoors under environment, that is, the nano silver of lithium magnesium silicate+nano silver+polyglutamic acid charcoal is made
Complex antimicrobials.
After measured, the nano silver composite antibacterial agent of the present embodiment, silver particles grain size are 5~40nm, nano-Ag particles point
It dissipates well, when adding a concentration of 25mg/L, 100% is reached to staphylococcus aureus antibiotic rate, to Escherichia coli antibiotic rate
Reach 99.99%, shows good antibacterial activity.
Embodiment 2：
The gamma-polyglutamic acid powder for weighing 1g is dissolved in the distilled water of 100ml, and 1% gamma-polyglutamic acid solution is made；
It weighs 2g silver nitrates to be dissolved in the distilled water of 100ml, 2% silver nitrate solution is made；1g lithium magnesium silicates are weighed, porcelain crucible is packed into
In, it is added in the distilled water of 17mL, then 1% γ-polyglutamic that 10ml is made into is added on one side stirring the while of being added inside
Then the silver nitrate solution of above-mentioned 2% be made into of 12ml is added in acid solution.Then by the porcelain crucible equipped with mixture, it is placed in horse
Not it is 10 minutes with 380 DEG C of heated bakings, heating time in stove.After muffle furnace reduces and then collects above-mentioned heating, drying
Powder, room temperature is gradually cooling under environment indoors, that is, the nanometer of lithium magnesium silicate+nano silver+polyglutamic acid charcoal is made
Silver-colored complex antimicrobials.
After measured, the nano silver composite antibacterial agent of the present embodiment, silver particles grain size are 5~35nm, nano-Ag particles point
It dissipates well, when adding a concentration of 25mg/L, 94.80% is reached to staphylococcus aureus antibiotic rate, to Escherichia coli antibacterial
Rate reaches 98.70%, shows good antibacterial activity.
Embodiment 3：
The gamma-polyglutamic acid powder for weighing 3g is dissolved in the distilled water of 100ml, and 3% gamma-polyglutamic acid solution is made；
It weighs 3g silver nitrates to be dissolved in the distilled water of 100ml, 3% silver nitrate solution is made；1g lithium magnesium silicates are weighed, porcelain crucible is packed into
In, it is added in the distilled water of 25mL, then 3% gamma-polyglutamic acid that 5ml is made into is added on one side stirring the while of being added inside
Then the silver nitrate solution of above-mentioned 3% be made into of 12ml is added in solution.Then by the porcelain crucible equipped with mixture, it is placed in Muffle
With 420 DEG C of heated bakings in stove, heating time is 60 minutes.After muffle furnace reduces and then collects above-mentioned heating, drying
Powder is gradually cooling to room temperature indoors under environment, that is, the nano silver of lithium magnesium silicate+nano silver+polyglutamic acid charcoal is made
Complex antimicrobials.
After measured, the nano silver composite antibacterial agent of the present embodiment, silver particles grain size are 5~60nm, nano-Ag particles point
It dissipates well, when adding a concentration of 25mg/L, 98.85% is reached to staphylococcus aureus antibiotic rate, to Escherichia coli antibacterial
Rate reaches 99.99%, shows good antibacterial activity.
Embodiment 4：
The gamma-polyglutamic acid powder for weighing 2g is dissolved in the distilled water of 100ml, and 2% gamma-polyglutamic acid solution is made；
It weighs 3g silver nitrates to be dissolved in the distilled water of 100ml, 3% silver nitrate solution is made；1g lithium magnesium silicates are weighed, porcelain crucible is packed into
In, it is added in the distilled water of 25mL, then 2% gamma-polyglutamic acid that 7ml is made into is added on one side stirring the while of being added inside
Then the silver nitrate solution of above-mentioned 3% be made into of 15ml is added in solution.Then by the porcelain crucible equipped with mixture, it is placed in Muffle
With 400 DEG C of heated bakings in stove, heating time is 30 minutes.After muffle furnace reduces and then collects above-mentioned heating, drying
Powder is gradually cooling to room temperature indoors under environment, that is, the nano silver of lithium magnesium silicate+nano silver+polyglutamic acid charcoal is made
Complex antimicrobials.
After measured, the nano silver composite antibacterial agent of the present embodiment, silver particles grain size are 5~40nm, nano-Ag particles point
It dissipates well, when adding a concentration of 25mg/L, 99.99% is reached to staphylococcus aureus antibiotic rate, to Escherichia coli antibacterial
Rate reaches 100.00%, shows good antibacterial activity.
Embodiment 5：
The gamma-polyglutamic acid powder for weighing 3g is dissolved in the distilled water of 100ml, and 3% gamma-polyglutamic acid solution is made；
It weighs 1g silver nitrates to be dissolved in the distilled water of 100ml, 1% silver nitrate solution is made；1g lithium magnesium silicates are weighed, porcelain crucible is packed into
In, it is added in the distilled water of 17mL, then 3% gamma-polyglutamic acid that 5ml is made into is added on one side stirring the while of being added inside
Then the silver nitrate solution of above-mentioned 1% be made into of 18ml is added in solution.Then by the porcelain crucible equipped with mixture, it is placed in Muffle
With 380 DEG C of heated bakings in stove, heating time is 20 minutes.After muffle furnace reduces and then collects above-mentioned heating, drying
Powder is gradually cooling to room temperature indoors under environment, that is, the nano silver of lithium magnesium silicate+nano silver+polyglutamic acid charcoal is made
Complex antimicrobials.
After measured, the nano silver composite antibacterial agent of the present embodiment, silver particles grain size are 5~40nm, nano-Ag particles point
It dissipates well, when adding a concentration of 25mg/L, 95.32% is reached to staphylococcus aureus antibiotic rate, to Escherichia coli antibacterial
Rate reaches 98.35%, shows good antibacterial activity.
Embodiment 6：
The gamma-polyglutamic acid powder for weighing 1g is dissolved in the distilled water of 100ml, and 1% gamma-polyglutamic acid solution is made；
It weighs 1g silver nitrates to be dissolved in the distilled water of 100ml, 1% silver nitrate solution is made；1g lithium magnesium silicates are weighed, porcelain crucible is packed into
In, it is added in the distilled water of 33mL, then 1% γ-polyglutamic that 10ml is made into is added on one side stirring the while of being added inside
Then the silver nitrate solution of above-mentioned 1% be made into of 18ml is added in acid solution.Then by the porcelain crucible equipped with mixture, it is placed in horse
Not it is 50 minutes with 420 DEG C of heated bakings, heating time in stove.After muffle furnace reduces and then collects above-mentioned heating, drying
Powder, room temperature is gradually cooling under environment indoors, that is, the nanometer of lithium magnesium silicate+nano silver+polyglutamic acid charcoal is made
Silver-colored complex antimicrobials.
After measured, the nano silver composite antibacterial agent of the present embodiment, silver particles grain size are 5~50nm, nano-Ag particles point
It dissipates well, when adding a concentration of 25mg/L, 90.63% is reached to staphylococcus aureus antibiotic rate, to Escherichia coli antibacterial
Rate reaches 94.81%, shows good antibacterial activity.
Claims (3)
1. a kind of short-cut method preparing nano silver composite antibacterial agent, which is characterized in that include the following steps：
Aqueous solution containing gamma-polyglutamic acid, source of silver ions, lithium magnesium silicate is pyrolyzed, the powder after pyrolysis is nano silver
Complex antimicrobials.
2. according to the method described in claim 1, it is characterized in that, the source of silver ions is silver nitrate.
3. according to the method described in claim 2, it is characterized in that, preparing γ-polyglutamic of 10~30g/L of mass-volume concentration
The silver nitrate aqueous solution of aqueous acid, 10~30g/L of mass-volume concentration；By mass volume ratio 1g：17-33ml is by lithium magnesium silicate
It is mixed with water, obtains lithium magnesium silicate aqueous solution；
By lithium magnesium silicate：The ratio of gamma-polyglutamic acid aqueous solution=1g ︰ 5-10ml is by lithium magnesium silicate aqueous solution and γ-polyglutamic
Aqueous acid is mixed to get mixed liquor, then presses lithium magnesium silicate：The ratio of silver nitrate aqueous solution=1g ︰ 12-18ml is by silver nitrate water
Solution is added in mixed liquor, and mixture is made, mixture is placed in crucible, in 380-420 DEG C of heated baking, heating time is
10-60 minutes, the powder after heating, drying is collected, up to nano silver composite antibacterial agent after cooling.
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Cited By (2)
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| CN112551596A (en) * | 2020-11-27 | 2021-03-26 | 天长市中德电子有限公司 | Preparation method of nano nickel-zinc ferrite magnetic material |
| CN116285067A (en) * | 2023-04-03 | 2023-06-23 | 安徽康然创氧生物科技有限公司 | Antibacterial plastic master batch and application thereof in antibacterial plastic products |
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