CN109758474A - A kind of Ag/ZIF-8 antibacterial agent and preparation method thereof - Google Patents
A kind of Ag/ZIF-8 antibacterial agent and preparation method thereof Download PDFInfo
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- CN109758474A CN109758474A CN201910168087.6A CN201910168087A CN109758474A CN 109758474 A CN109758474 A CN 109758474A CN 201910168087 A CN201910168087 A CN 201910168087A CN 109758474 A CN109758474 A CN 109758474A
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Abstract
The present invention relates to a kind of Ag/ZIF-8 antibacterial agents and preparation method thereof, belong to technical field of nano material.The present invention provides compound preservatives of a kind of Ag/ZIF-8 and preparation method thereof.Ag nanoparticle is distributed on ZIF-8 by the method for impregnating, restoring, Ag/ZIF-8 compound preservative is prepared.The ZIF-8 material that the present invention uses has hierarchical porous structure and bigger serface, has good stabilization and peptizaiton to Ag nanoparticle.In the Ag/ZIF-8 bacteriostatic agent, the Ag/ZIF-8 nano antibacterial agent particle of offer is small, partial size is 10-200nm spherical shape or polyhedral structure, be conducive to the adhesive force for increasing it to bacterium, Ag nanoparticle and ZIF-8 have collaboration bacteriostasis, and a variety of indicator bacterias are shown with the fungistatic effect of high-efficiency broad spectrum；The process of preparing of heretofore described Ag/ZIF-8 bacteriostatic agent is simple, economically feasible.
Description
Technical field
The invention belongs to technical field of nano material, and in particular to a kind of Ag/ZIF-8 nano antibacterial agent and its preparation side
Method.
Background technique
The infectious disease as caused by pathogen is an important public health problem.With antibiotic and chemical bactericide
Abuse, drug tolerant bacteria become increasingly prevalent, and this considerably increases medical treatment costs and the death rate.Exploitation it is new, it is effective anti-
Bacterium material is the key that control growth of pathogenic bacteria.Metallic silver has has a broad antifungal spectrum as bacteriostatic agent, is not easy that bacterium is made to generate drug resistance
Property and the superiority such as have no toxic side effect, be commonly used by people for control infection very early.And there are silver ions to release for conventional silver system bacteriostatic agent
Excessive velocities are put, the poor disadvantage of antibacterial persistence, with the development that nanosecond science and technology are swift and violent, people start sight turning to nanometer
Silver-colored antibacterial material.By confirming, the fungistatic effect of nano silver particles is 200 times of micro nanometer silver particle or more.But silver nanoparticle
Particle haves the shortcomings that easily aggregation, stability are poor, seriously limit its fungistatic effect in practical applications.
Summary of the invention
To make up the deficiencies in the prior art, the present invention provides a kind of Ag/ZIF-8 antibacterial agents and preparation method thereof.
Inventive concept of the invention is: by solid material with unique properties as supported on carriers high degree of dispersion
Ag nanoparticle, carrier can not only be used to stablize nano silver, while can also generate synergistic effect with nano silver, improve composite wood
The whole fungistatic effect of material.The carrier ZIF-8 that the present invention uses is a kind of metal-organic framework materials, has porosity, high
Specific surface area and biocompatibility.Zn simultaneously2+With certain bacteriostasis property, and metallic nanoparticle may be implemented in its nano-cavity
The determinate growth of sub- Ag, to generate monodispersed metal Ag nano particle.
The present invention specifically adopts the following technical scheme that a kind of Ag/ZIF-8 antibacterial agent, Ag nanoparticle is highly dispersed to
On ZIF-8, Ag Nanoparticle Size is 0.5-10nm, mass content 0.1-20%.Used ZIF-8 pattern be it is spherical or
Person's polyhedron, size is in 10-200nm.
Second purpose of the invention is that the preparation method of above-mentioned Ag/ZIF-8 antibacterial agent is claimed, and is included the following steps:
The synthesis of S1.ZIF-8
By 0.1-100g Zn (NO3)·6H2O and 0.1-400g 2-methylimidazole is dissolved in water or methanol, and 0- is added
400g CTAB, 0-100ml triethylamine, 0-100g histidine, stir 10min-24h at 0-100 DEG C of temperature, after centrifugation, use first
The washing of alcohol deionized water mixed solution, again with methanol reflux, centrifugal drying obtain white powder ZIF-8；
The synthesis of S2.Ag/ZIF-8
Take ZIF-8, AgNO3Concussion reaction 2h adds sodium borohydride, reacts 1-12h；With methanol dehydrated alcohol mixed liquor
Elution 3 times, centrifugal drying obtains Ag/ZIF-8, wherein ZIF-8 and AgNO3, sodium borohydride mass ratio be 100:(0.5-10):
(1-10)。
Further, Zn (NO in the step S13)·6H2O, CTAB and the histidine ultrasonic dissolution in methanol or water, 2- first
Base imidazoles, the triethylamine ultrasonic dissolution in methanol or water.
In the step S1, in methanol deionized water mixed solution, the ratio of methanol and deionized water volume is 1:1.
In the step S2, in methanol dehydrated alcohol mixed liquor, the ratio of methanol and dehydrated alcohol volume is 1:1.
As a preferred embodiment of the invention, Ag/ZIF-8 antibacterial agent the preparation method is as follows:
The synthesis of S1.ZIF-8
By 0.1-100g Zn (NO3)·6H2O and 0.1-400g 2-methylimidazole is dissolved in water or methanol, and 0- is added
400g CTAB, 0-100ml triethylamine, 0-100g histidine, stir 10min-24h at 0-100 DEG C of temperature, after centrifugation, use first
The washing of alcohol deionized water mixed solution, again with methanol reflux, centrifugal drying obtain white powder ZIF-8；
The synthesis of S2.Ag/ZIF-8
Take 0.1-100g ZIF-8,0.01g-100gAgNO3Concussion reaction 2h adds 89mg-100g sodium borohydride, instead
Answer 1-12h；It is eluted 3 times with methanol dehydrated alcohol mixed liquor, centrifugal drying obtains Ag/ZIF-8.
A kind of compound preservative is claimed simultaneously in the present invention, including the Ag/ZIF-8 nanometer using above method preparation
Acceptable auxiliary material in grain and bacteriostatic agent.
Ag nanoparticle is distributed on ZIF-8 nanoparticle by the present invention, utilizes the more of metal-organic framework materials ZIF-8
Grade pore structure and the limit threshold effect of nano pore limit growing up and reuniting for Ag nanoparticle, and the porosity of carrier ZIF-8 is advantageous
In Ag+The diffusion of ion；And ZIF-8 carrier has better stabilization to Ag nanoparticle, to be prepared single point
Scattered Ag nanoparticle, further obtains the compound preservative of efficient Ag/ZIF-8.
Compared with prior art, the invention has the following advantages that
1, Ag/ZIF-8 nano antibacterial agent preparation method provided by the invention, synthesis condition is mild, and process is simple, warp
It helps feasible.
2, in Ag/ZIF-8 nano antibacterial agent provided by the invention, Ag nanoparticle high degree of dispersion has with ZIF-8 to be cooperateed with
Fungistatic effect is conducive to the bacteriostatic agent for preparing high-efficiency broad spectrum.
3, Ag/ZIF-8 nano antibacterial agent particle provided by the invention is small, and partial size is 10-200nm spherical shape or elliposoidal knot
Structure is conducive to the adhesive force for increasing it to bacterium, effectively destroys cell wall and cell membrane, discharges the content of bacterium, have
Extensive antibacterial spectrogram.
Detailed description of the invention
The preparation flow figure of Fig. 1 nano antibacterial agent Ag/ZIF-8；
SEM (A), TEM figure (B) and the SEM-EDX figure (C) of Fig. 2 nano antibacterial agent Ag/ZIF-8
The fungistatic effect of Fig. 3 nano antibacterial agent Ag/ZIF-8, wherein (a), staphylococcus aureus, (b), Escherichia coli；
The plate fungistatic effect figure of Fig. 4 nano antibacterial agent Ag/ZIF-8, wherein (a), Escherichia coli, (b), bacillus subtilis
Bacterium.
Specific embodiment
Technical solution of the present invention is described in further detail below in conjunction with specific embodiment, but is not limited of the invention
Protection scope.
Embodiment 1 prepares the agent of Ag/ZIF-8 nano antibacterial using impregnation-reduction method
The synthesis of S1.ZIF-8
It takes 125mL deionized water to be added in conical flask, adds 1.88g Zn (NO3)·6H2O、1.2665g CTAB、
2.1425g histidine ultrasonic dissolution, obtains A liquid；
It takes 125mL deionized water to be added in another conical flask, 4.074g 2-methylimidazole, tri- second of 6.8565ml is added
Amine ultrasonic dissolution obtains B liquid；
B liquid is poured into A liquid, reaction 7h is stirred at reflux at 20-60 DEG C of temperature.With vol/vol methanol: deionized water=
1:1 centrifuge washing 3 times, again with methanol flows back 3 times, and 40min/ times, centrifugal drying obtains white powder ZIF-8.
The synthesis of S2.Ag/ZIF-8
It takes 4ml methanol to be added in conical flask, 0.5g ZIF-8,0.01gAgNO is added32h is reacted, then is gradually added
89mg sodium borohydride reacts 12h；With vol/vol methanol: dehydrated alcohol=1:1 is eluted twice, then primary with 95% ethanol elution,
Centrifugal drying obtains Ag/ZIF-8.
Embodiment 2
Using the Ag/ZIF-8 for preparing in fask oscillating method evaluation embodiment 1 to staphylococcus aureus (gram-positive bacteria) and
The fungistatic effect of Escherichia coli (Gram-negative bacteria), test results are shown in figure 3.
Staphylococcus aureus and Escherichia coli are cultivated in LB (Luria-Bertani) respectively culture solution in 37 DEG C
12h.0-12mgAg/ZIF-8 is distributed to respectively in 40ml LB liquid medium, being separately added into 400 μ L concentration is 108CFU/
The staphylococcus aureus of ml and E. coli suspension.It is incubated at 37 DEG C, by the optical density at monitoring 600nm, to measure
The growth rate of bacterium.Fig. 3 (a) is staphylococcus aureus fungistatic effect, and Fig. 3 (b) is the fungistatic effect of Escherichia coli；From figure
In it will be evident that in fluid nutrient medium be added Ag/ZIF-8 after, can obviously reduce the growth rate of bacterium.
Embodiment 3
Using the Ag/ZIF-8 nano antibacterial agent prepared in flat band method evaluation embodiment 1 to Escherichia coli (Gram-negative
Bacterium) with the bacteriostasis property of bacillus subtilis (gram-positive bacteria), test results are shown in figure 4.
0-12mgAg/ZIF-8 nano material is distributed in 40ml agar medium, is then by 50 μ L concentration
105The bacterial suspension of CFU/ml is uniformly coated on agar plate, then in 37 DEG C of culture 12h, observes bacterial clump quantity.Figure
4 (a) be E. coli plate fungistatic effect, and Fig. 4 (b) is bacillus subtilis plate fungistatic effect.It can be obviously from Fig. 4
Out, Ag/ZIF-8 either all has significant fungistatic effect to gram-positive bacteria or Gram-negative bacteria, with Ag/
The increase of ZIF-8 concentration, fungistatic effect are more obvious.It follows that Ag/ZIF-8 has broad-spectrum antibacterial.
The preferable specific embodiment of the above, only the invention, but the protection scope of the invention is not
It is confined to this, anyone skilled in the art is in the technical scope that the invention discloses, according to the present invention
The technical solution of creation and its inventive concept are subject to equivalent substitution or change, should all cover the invention protection scope it
It is interior.
Claims (8)
1. a kind of Ag/ZIF-8 antibacterial agent, which is characterized in that Ag nanoparticle is highly dispersed on ZIF-8, and Ag nanoparticle is big
Small is 0.5-10nm, mass content 0.1-20%.
2. Ag/ZIF-8 antibacterial agent according to claim 1, which is characterized in that used ZIF-8 pattern be it is spherical or
Person's polyhedron, size is in 10-200nm.
3. a kind of Ag/ZIF-8 antibacterial agent and preparation method thereof, which is characterized in that preparation method includes the following steps:
The synthesis of S1.ZIF-8
By 0.1-100g Zn (NO3)·6H2O and 0.1-400g 2-methylimidazole is dissolved in water or methanol, and 0-400g is added
CTAB, 0-100ml triethylamine, 0-100g histidine, stir 10min-24h at 0-100 DEG C of temperature, after centrifugation, are gone with methanol
The washing of ion water mixed solution, again with methanol reflux, centrifugal drying obtain white powder ZIF-8；
The synthesis of S2.Ag/ZIF-8
Take ZIF-8, AgNO3Concussion reaction 2h adds sodium borohydride, reacts 1-12h；With methanol dehydrated alcohol mixed liquor elution 3
Secondary, centrifugal drying obtains Ag/ZIF-8, wherein ZIF-8 and AgNO3, sodium borohydride mass ratio be 100:(0.5-10): (1-10).
4. a kind of preparation method of Ag/ZIF-8 antibacterial agent according to claim 3, which is characterized in that in the step S1
Zn(NO3)·6H2O, CTAB and histidine in methanol or water ultrasonic dissolution, 2-methylimidazole and triethylamine in methanol or water
Ultrasonic dissolution.
5. a kind of preparation method of Ag/ZIF-8 antibacterial agent according to claim 3, which is characterized in that the step S1
In, in methanol deionized water mixed solution, the ratio of methanol and deionized water volume is 1:1.
6. a kind of preparation method of Ag/ZIF-8 antibacterial agent according to claim 3, which is characterized in that the step S2
In, in methanol dehydrated alcohol mixed liquor, the ratio of methanol and dehydrated alcohol volume is 1:1.
7. a kind of preparation method of Ag/ZIF-8 antibacterial agent according to claim 3, which is characterized in that specific steps are such as
Under:
S1. by 0.1-100g Zn (NO3)·6H2O and 0.1-400g 2-methylimidazole is dissolved in water or methanol, and 0- is added
400g CTAB, 0-100ml triethylamine, 0-100g histidine, stir 10min-24h at 0-100 DEG C of temperature, after centrifugation, use first
The washing of alcohol deionized water mixed solution, again with methanol reflux, centrifugal drying obtain white powder ZIF-8；
S2. 0.1-100g ZIF-8,0.01g-100gAgNO are taken3Concussion reaction 2h adds 89mg-100g sodium borohydride, reaction
1-12h；It is eluted 3 times with methanol dehydrated alcohol mixed liquor, centrifugal drying obtains Ag/ZIF-8.
8. a kind of compound preservative, which is characterized in that including using Ag/ZIF-8 nano particle described in claim 1 and antibacterial
Acceptable auxiliary material in agent.
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|---|---|---|---|---|
| CN110506741A (en) * | 2019-09-20 | 2019-11-29 | 天津科技大学 | A kind of compound antibacterial material of novel nano and preparation method thereof and purposes |
| CN110522910A (en) * | 2019-08-01 | 2019-12-03 | 山东大学 | Based on metal organic frame administration nano-drug administration system and its preparation method and application |
| CN111109293A (en) * | 2019-12-27 | 2020-05-08 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of silver-metal organic framework composite antibacterial material |
| CN111234245A (en) * | 2020-01-15 | 2020-06-05 | 扬州大学 | Ag nanowire/ZIF ultrathin nanosheet composite material, preparation method and application |
| CN111450806A (en) * | 2020-04-23 | 2020-07-28 | 陕西科技大学 | Preparation method of porous adsorption antibacterial composite material based on waste corncobs |
| CN112206349A (en) * | 2020-10-19 | 2021-01-12 | 吉林大学 | ZIF-8@ antibacterial ion coating prepared on surface of medical metal implant material and preparation method thereof |
| CN112826832A (en) * | 2019-11-25 | 2021-05-25 | 中国科学院大连化学物理研究所 | Nano reactor, preparation method and application thereof |
| CN113069940A (en) * | 2021-04-20 | 2021-07-06 | 江苏理工学院 | Preparation method of anti-pollution membrane |
| CN113181212A (en) * | 2020-01-14 | 2021-07-30 | 南京理工大学 | ZIF-8/carbon dot anti-biofilm composite nano material and preparation method thereof |
| CN113261566A (en) * | 2021-04-14 | 2021-08-17 | 湖南工业大学 | Preparation method of basic magnesium hypochlorite loaded metal organic framework bacteriostatic agent |
| CN113786809A (en) * | 2021-08-31 | 2021-12-14 | 重庆大学 | Method for detecting household garbage odor thiol-containing factor by using SERS platform on paper |
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| CN115779862A (en) * | 2022-12-29 | 2023-03-14 | 宝武水务科技有限公司 | Silver nanoparticle composite material and preparation method and application thereof |
| CN116554495A (en) * | 2023-07-10 | 2023-08-08 | 北京石油化工学院 | Antibacterial and antiseptic dual-function powder, and preparation method and application thereof |
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| CN110522910B (en) * | 2019-08-01 | 2020-11-06 | 山东大学 | Nano drug delivery system based on metal organic framework and preparation method and application thereof |
| CN110506741A (en) * | 2019-09-20 | 2019-11-29 | 天津科技大学 | A kind of compound antibacterial material of novel nano and preparation method thereof and purposes |
| CN110506741B (en) * | 2019-09-20 | 2021-09-21 | 天津科技大学 | Novel nano composite antibacterial material and preparation method and application thereof |
| CN112826832B (en) * | 2019-11-25 | 2022-05-17 | 中国科学院大连化学物理研究所 | Nano reactor, preparation method and application thereof |
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| CN112206349A (en) * | 2020-10-19 | 2021-01-12 | 吉林大学 | ZIF-8@ antibacterial ion coating prepared on surface of medical metal implant material and preparation method thereof |
| CN113261566A (en) * | 2021-04-14 | 2021-08-17 | 湖南工业大学 | Preparation method of basic magnesium hypochlorite loaded metal organic framework bacteriostatic agent |
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| CN115463151A (en) * | 2022-08-18 | 2022-12-13 | 湖北文理学院 | Nano enzyme, preparation method and application thereof, and bacteriostatic agent |
| CN115463151B (en) * | 2022-08-18 | 2023-09-19 | 湖北文理学院 | Nano-enzyme, preparation method and application thereof, and bacteriostat |
| CN115779862A (en) * | 2022-12-29 | 2023-03-14 | 宝武水务科技有限公司 | Silver nanoparticle composite material and preparation method and application thereof |
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Application publication date: 20190517 |