CN109820000A - A kind of MOFs carrying nano silver anti-biotic material and preparation method thereof - Google Patents
A kind of MOFs carrying nano silver anti-biotic material and preparation method thereof Download PDFInfo
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- CN109820000A CN109820000A CN201910121915.0A CN201910121915A CN109820000A CN 109820000 A CN109820000 A CN 109820000A CN 201910121915 A CN201910121915 A CN 201910121915A CN 109820000 A CN109820000 A CN 109820000A
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Abstract
A kind of MOFs carrying nano silver anti-biotic material and preparation method thereof, belong to inorganic antibacterial material technical field, can solve the easy self-assemble of silver nano-grain cannot effectively be dispersed in basis material at bulky grain, the problem of influencing its anti-microbial property, can cut with structure, the porous material MOFs of big specific surface area and various topological structures is template, by nano silver appendix in the surface of MOFs, skeleton and duct, Ag@MOFs efficacious anti-microbial material that is of uniform size, being easily dispersed is synthesized.For the present invention using porous material MOFs as template, hydro-thermal method realizes MOFs appendix nano silver.This method is easy to operate, at low cost, needs the field of antibacterial functions to be with a wide range of applications nano silver-group antibacterial agent etc. is similar.
Description
Technical field
The invention belongs to inorganic antibacterial material technical fields, and in particular to a kind of MOFs carrying nano silver anti-biotic material and its system
Preparation Method.
Background technique
The chemicals such as antibiotic, disinfectant are abused at present, and the microbial variation problem as caused by drug resistance is extremely serious,
The antibacterial agent that pathogenic bacteria can efficiently be killed becomes research hotspot.Not only antibacterial activity is big for silver-based antimicrobial agent, antimicrobial spectrum
Extensively, and Induction of bacterial drug resistance tendency is low.The size of silver is to influence the key factor of its anti-microbial property, and silver nano-grain compares micron
The anti-microbial property of grade silver improves 200 times or more.Although the silver nano-grain of small size has higher anti-microbial property, nanometer
The easy self-assemble of grain cannot be effectively dispersed in basis material at bulky grain, influence its anti-microbial property.Metal is organic
Framework compound (Metal-Organic Frameworks, MOFs) is using metal ion as tie point, and organic ligand is branch
The porous material constituted is supportted, there is good structure can cut, huge specific surface area and diversified topological structure, it will be silver-colored
Nano particle is carried on MOFs it is possible to prevente effectively from its reunion, efficiently plays its anti-microbial property.
Summary of the invention
The present invention, which is easy self-assemble for silver nano-grain, cannot effectively be dispersed in basis material at bulky grain
In, the problem of influencing its anti-microbial property, provides a kind of MOFs carrying nano silver anti-biotic material and preparation method thereof.
The present invention adopts the following technical scheme:
A kind of MOFs carrying nano silver anti-biotic material, can be cut with structure, big specific surface area and several topological structures it is more
Porous materials MOFs is template, and by nano silver appendix in the surface of MOFs, skeleton and duct, synthesis is of uniform size, is easily dispersed
Ag@MOFs efficacious anti-microbial material.
A kind of preparation method of MOFs carrying nano silver anti-biotic material, includes the following steps:
It is anti-to pour into progress hydro-thermal in reaction kettle respectively by the solution of the solution of the metallic of MOFs and organic ligand for the first step
It answers, obtains MOFs crystal grain；
MOFs crystal grain is dispersed in solvent by second step, obtains MOFs solution, silver nitrate is placed in solvent, obtain
To silver nitrate solution, silver nitrate solution is added in MOFs solution, stirring 6h or more is protected from light, supernatant is outwelled, by bottom precipitation
12h is activated in 60 DEG C of vacuum drying ovens, glucose is dissolved in solvent, glucose solution is obtained, by the precipitating Portugal after activation
After grape sugar juice restores 1h, supernatant is outwelled, then will be deposited in 60 DEG C of vacuum drying ovens and catch up with for 24 hours, obtain MOFs carrying nano silver
Anti-biotic material.
Solvent described in second step includes water or ethyl alcohol.
The molar ratio of glucose described in second step and silver ion is 1:2.
The concentration of silver nitrate described in second step is 0.1mol/L.
Beneficial effects of the present invention are as follows:
1. the present invention with good structure can cut, the porous material of huge specific surface area and various topological structures
MOFs is template, using simple hydro-thermal method by nano silver appendix in the surface of MOFs, skeleton and duct, synthesis size it is equal
Ag@MOFs efficacious anti-microbial material that is even, being easily dispersed.
2. 10nm nano-Ag particles appendix below in the surface of MOFs, skeleton and duct, is avoided nanometer by the present invention
High-efficiency antimicrobial effect is realized in the reunion of silver.
3. the present invention is using simple hydro-thermal method in-situ preparation nano-Ag particles appendix in the surface of MOFs, skeleton and hole
In road, the scale and appendix amount of nano-Ag particles can flexibly be adjusted according to type, the concentration of reactant, reaction time of MOFs etc.
Section.
Detailed description of the invention
Fig. 1 is respectively the MOF-5(a of the embodiment of the present invention 1) and Ag@MOF-5(b) SEM figure；
Fig. 2 is the HRTEM pattern of the Ag@MOF-5 of the embodiment of the present invention 1；
Fig. 3 is the elemental analysis figure of the Ag@MOF-5 of the embodiment of the present invention 1；
Fig. 4 is MOF-5 the and Ag@MOF-5 of the embodiment of the present invention 1 respectively to Escherichia coli (a1, a2) and staphylococcus aureus
The inhibition zone of (b1, b2)；
Fig. 5 be the embodiment of the present invention 2 β-CD-MOF(a) and Ag@β-CD-MOF(b) SEM scheme；
Fig. 6 is the HRTEM image of the Ag@β-CD-MOF of the embodiment of the present invention 2；
Fig. 7 is β-CD-MOF and Ag the@β-CD-MOF of the embodiment of the present invention 2 to Escherichia coli (a, c) and staphylococcus aureus
(b, d) inhibition zone.
Specific embodiment
Embodiment 1
2.496g zinc nitrate hexahydrate and 0.528g terephthalic acid (TPA) are dissolved in suitable DMF, solution is poured into hydrothermal reaction kettle
In, react 4h in 130 DEG C of baking ovens, after reaction, cooled to room temperature, gained sample is washed three times with DMF, incline on
Clear liquid, products obtained therefrom is dry for 24 hours in 60 DEG C of vacuum ovens, it can be prepared by MOF-5 crystal grain.Weigh the MOF-5 of 0.2g
It is dispersed in 30mL water, MOF-5 aqueous solution is made, the silver nitrate aqueous solution of 0.1mol/L is added thereto while stirring,
It is protected from light stirring 6h or more, lightpink precipitating is generated, supernatant is inclined to falling, 12h is activated in 60 DEG C of vacuum drying ovens, with the water of glucose
Solution (molar ratio of glucose and silver ion is 1:2) reduction 1h, incline supernatant, and drying for 24 hours, obtains in 60 DEG C of vacuum drying ovens
To nanoscale Ag@MOF-5 antimicrobial particle, scanning nuclear microprobe pattern and elemental analysis the result is shown in Figure 1, Fig. 2 and Fig. 3.Ag@
Uniform a large amount of diameter about 3-5nm of appendix or so rule nanometer ball particle in MOF-5 nanometers of chips, after measured in full resolution pricture
The lattice fringe spacing of nanosphere is d=0.235nm, consistent with the spacing of lattice of (111) crystal face of silver.To the Ag@MOF- in figure
5 nanometer sheet particles carry out energy spectrum analysis, and the content of discovery Zn and Ag element is respectively 18.13% and 38.87%, illustrate a large amount of Ag
Nanometer ball particle is displaced in the duct MOF-5 or on appendix to MOF-5 chip.It disperses 0.005gMOF-5, Ag@MOF-5 in
It is made into the dispersion concentration solution of 500ppm in 10ml water, filter paper is pressed into the sequin of diameter 6mm with punch, is impregnated
In the above solution, it is sterilized with ultraviolet lamp to antimicrobial sample in super-clean bench, carries out anti-microbial property test, as a result see Fig. 4.
MOF-5, Ag@MOF-5 are respectively 11.44mm, 16.05mm to the average diameter of inhibition zone of Escherichia coli； MOF-5,Ag@MOF-5
Average diameter of inhibition zone to staphylococcus aureus is respectively 13.36mm, 14.62mm.Ag nano particle appendix is in MOF-5 bone
Duct, the edge of frame material can be sustained out the cell membrane that nanometer Ag destroys Escherichia coli, to show excellent in the medium
Different anti-microbial property.
Embodiment 2
0.378mmol beta-cyclodextrin (β-CD) is dissolved in 15mL, in the potassium hydroxide solution of 200mmol/L, is stirred evenly simultaneously
Filtering, filtrate are collected in 25mL small beaker.It takes proper amount of methanol in 400mL vial, the beaker equipped with filtrate is placed in glass
In glass bottle, sealing is stored at room temperature preservation one week or more, until having colourless cubic crystal generation in small beaker.Collect colourless cube
Crystal, it is dry in 60 DEG C of vacuum drying ovens after crystal is sufficiently washed with dehydrated alcohol to obtain β-CD-MOF crystal grain for 24 hours,
β-CD-MOF powder is obtained after grinding, scanning electron microscope image is shown in Fig. 5 (a).Configure 4.45g/L β-CD-MOF ethanol solution and
The AgNO of 0.1mol/L3Each 30mL of ethanol solution, by AgNO under conditions of being protected from light stirring3β-CD-MOF second is added in ethanol solution
In alcoholic solution, holding is protected from light stirring 6h or more, outwells supernatant, takes and activate in vacuum drying oven at 60 DEG C of underlayer red deposit
12h.The glucose ethanol solution 30mL for configuring 0.05mol/L, mixes with above-mentioned solution, and supernatant is removed in 1h hypsokinesis, dries in vacuum
Case is dried for 24 hours, obtains Ag@β-CD-MOF antimicrobial particle, scanning electron microscope and high-resolution-ration transmission electric-lens image see Fig. 5 (b),
Fig. 6.The irregular Ag nano particles of uniform a large amount of diameter about 3-10nm of appendix or so in-CD-MOF nanometers of chips of Ag β, through surveying
The lattice fringe spacing for determining nanoparticle in full resolution pricture is d=0.235nm, the spacing of lattice one with (111) crystal face of silver
It causes, illustrates a large amount of Ag nano particles appendix on the surface, duct and skeleton of β-CD-MOF.β-CD-MOF and Ag@β-CD-
The antibacterial experiment result of MOF is shown in Fig. 7.It can be seen that β-CD-MOF itself without antibacterial effect, Ag from inhibition zone method testing result
β-CD-MOF is respectively 11.68mm and 12.39mm to the average diameter of inhibition zone of Escherichia coli and staphylococcus aureus；Explanation
Ag nanoparticle on Ag β-CD-MOF can be sustained out nanometer Ag in the medium and play antibacterial action.
Claims (5)
1. a kind of MOFs carrying nano silver anti-biotic material, it is characterised in that: can be cut with structure, big specific surface area and several
The porous material MOFs of topological structure is template, and by nano silver appendix in the surface of MOFs, skeleton and duct, synthesis size is equal
Ag@MOFs efficacious anti-microbial material that is even, being easily dispersed.
2. a kind of preparation method of MOFs carrying nano silver anti-biotic material as described in claim 1, it is characterised in that: including as follows
Step:
It is anti-to pour into progress hydro-thermal in reaction kettle respectively by the solution of the solution of the metallic of MOFs and organic ligand for the first step
It answers, obtains MOFs crystal grain；
MOFs crystal grain is dispersed in solvent by second step, obtains MOFs solution, silver nitrate is placed in solvent, obtain
To silver nitrate solution, silver nitrate solution is added in MOFs solution, stirring 6h or more is protected from light, supernatant is outwelled, by bottom precipitation
12h is activated in 60 DEG C of vacuum drying ovens, glucose is dissolved in solvent, glucose solution is obtained, by the precipitating Portugal after activation
After grape sugar juice restores 1h, supernatant is outwelled, then will be deposited in 60 DEG C of vacuum drying ovens and catch up with for 24 hours, obtain MOFs carrying nano silver
Anti-biotic material.
3. a kind of preparation method of MOFs carrying nano silver anti-biotic material according to claim 2, it is characterised in that: second step
Described in solvent include water or ethyl alcohol.
4. a kind of preparation method of MOFs carrying nano silver anti-biotic material according to claim 2, it is characterised in that: second step
Described in the molar ratio of glucose and silver ion be 1:2.
5. a kind of preparation method of MOFs carrying nano silver anti-biotic material according to claim 2, it is characterised in that: second step
Described in silver nitrate concentration be 0.1mol/L.
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| CN111234691A (en) * | 2020-04-03 | 2020-06-05 | 朱生寿 | Antibacterial and mildew-proof coating with good weather resistance |
| CN111286046A (en) * | 2020-03-30 | 2020-06-16 | 上海烟草集团有限责任公司 | Composite hydrogel with antibacterial property and preparation method and application thereof |
| CN111296480A (en) * | 2020-02-21 | 2020-06-19 | 衢州学院 | Iron-based metal-organic framework material loaded with silver nanoparticles and preparation method and application thereof |
| CN111955479A (en) * | 2020-08-10 | 2020-11-20 | 东莞东阳光科研发有限公司 | Silver-containing antibacterial liquid and preparation method thereof |
| CN112616834A (en) * | 2020-10-26 | 2021-04-09 | 杭州乐铭科技有限公司 | Preparation process of organic framework material bearing nano virus killing material |
| CN112931530A (en) * | 2021-01-26 | 2021-06-11 | 新乡市华西卫材有限公司 | Nano-silver loaded Cu-MOF antibacterial material and preparation method and application thereof |
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