CN107950570A - A kind of preparation method of graphene/titanium dioxide/nano silver composite material - Google Patents
A kind of preparation method of graphene/titanium dioxide/nano silver composite material Download PDFInfo
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- CN107950570A CN107950570A CN201711162932.6A CN201711162932A CN107950570A CN 107950570 A CN107950570 A CN 107950570A CN 201711162932 A CN201711162932 A CN 201711162932A CN 107950570 A CN107950570 A CN 107950570A
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
Abstract
The invention discloses a kind of preparation method of graphene/titanium dioxide/nano silver composite material, step is：Graphene oxide is scattered in solvent, graphene oxide dispersion is obtained, ammonium hydroxide is added dropwise thereto, obtains graphene oxide aqueous slkali；Butyl titanate is added in organic solvent, organic solvent is ethanol and 1, and the mixed liquor of 3 propane diols, obtains butyl titanate solution；Butyl titanate solution is added in graphene oxide aqueous slkali, is stirred, is separated, dry, annealing, obtains graphene oxide/composite titania material；It is scattered in solvent, adds silver nitrate solution, stirring, obtains graphene/titanium dioxide/nano silver composite material.Graphene/titanium dioxide/nano silver composite material that preparation method using the present invention obtains has excellent anti-microbial property; in addition, preparation process of the present invention have it is easy to operate, cost is low; it is efficient, it is easy to accomplish scale, industrialization production and the advantages that be widely used.
Description
Technical field
The invention belongs to new material and its preparing technical field, is specifically related to a kind of graphene/titanium dioxide/nanometer
The preparation method of silver composite material.
Background technology
The mankind recognize that some metals such as silver, copper, zinc, mercury, bismuth, cadmium have antibacterial effect very early, and to people and move
Thing is safe.Compared with organic antibacterial agent, metal antibacterial agent have high temperature resistant, broad-spectrum antibacterial property, long-acting, safety, without secondary dirt
The features such as dye, be increasingly becoming the new research hotspot in antibacterial field.
Silver-series antibacterial agent commercialization at present, including silver ion, metallic silver and nano-Ag particles, wherein nano-Ag particles by
In nano level small-size effect and larger specific surface area, the anti-microbial property with higher.But nano-Ag particles antiseptic
There are the defects of stability is poor, onset time is slow.
Allotrope of the graphene as carbon, is that carbon atom has honeycomb structure by what sp2 orbital hybridizations were formed
Individual layer two dimensional crystal material, good mechanical performance that graphene has, chemical stability etc., also will be in fields such as composite materials
Have broad application prospects.
Find that graphene has certain anti-microbial property in conventional research, such as《American Chemical Society-nanometer》
(ACS-Nano, 2010 volume 4 page 4317) report a kind of graphene paper by graphene oxide reduction have it is certain anti-
Bacterium property.Then there is a series of graphene with preferable anti-microbial property/silver nanoparticle composite antibacterial material, research finds such
Material has certain limitation in using effect；Since nano silver is in granular form, granularity is Nano grade, can only often be assembled
In the privileged site of graphene, surface can not be evenly distributed on, so that the antibacterial effect influenced；On the other hand, nano silver and stone
Black alkene can not combine closely and (particularly when nano-Ag particles content increase, agglomeration easily occur), in use
Easily come off, so as to influence service life and antibacterial effect.Therefore, how to improve graphene/silver nano material stability and
Antibiotic property becomes current main direction of studying.
Patent of invention such as Application No. 201110434350.5 discloses a kind of Ag/TiO2/ graphene nano complex light
Catalyst and preparation method thereof, is to be assembled into metallic silver, nano-titanium dioxide (P25) powder by photocatalytic redox method
In two-dimensional layer graphene carrier material.It is using the graphene of two-dimensional layer as carrier material that it, which is prepared, and silver nitrate is used as silver-colored source,
Nano-titanium dioxide is catalysis material, and it is empty with photoproduction to produce light induced electron by simulated solar irradiation excitation nano titanium dioxide
Cave, photohole are sacrificed agent capture, and silver ion and graphite oxide are reduced into metal Ag and graphite by light induced electron respectively at the same time
Alkene, obtains Ag/TiO2/ graphene nano composite photo-catalyst.But the patent is directly by TiO2It is dispersed in graphite oxide and nitre
In the mixed liquor of sour silver, the antibacterial effect of obtained composite material is general.
The content of the invention
The defects of present invention is in order to overcome the above-mentioned prior art, technical problems to be solved are to provide a kind of dispersed, anti-
The preparation method of the good graphene/titanium dioxide/nano silver composite material of bacterium property.
Present disclosure includes providing a kind of preparation method of graphene/titanium dioxide/nano silver composite material, including
Following steps：
(1) graphene oxide is scattered in solvent, obtains graphene oxide dispersion, into graphene oxide dispersion
Ammonium hydroxide is added dropwise, obtains graphene oxide aqueous slkali；
(2) butyl titanate is added in organic solvent, organic solvent is ethanol and 1, and the mixed liquor of 3 propane diols, obtains
Butyl titanate solution；
(3) butyl titanate solution is added in graphene oxide aqueous slkali, stirred, separated, it is dry, in air atmosphere
Annealing, obtains graphene oxide/composite titania material；
(4) graphene oxide/composite titania material of step (3) is scattered in solvent, adds silver nitrate solution,
Stirring, obtains intermediate, the silver nitrate, the mass ratio of graphene oxide/composite titania material are (0.08-0.12)：
1；
(5) intermediate is ultrasonically treated, after cleaning, carries out light processing, intensity of illumination 90-120mW/cm2, illumination
Time is 1-4h, obtains graphene/titanium dioxide/nano silver composite material.
The graphene oxide is made using Hummers methods.
The mass ratio of the silver nitrate and ethanol is (0.08-0.12)：98.9.
Solvent is the mixed liquor of second alcohol and water in the graphene oxide dispersion, and wherein the volume ratio of ethanol and water is 1:
3, the concentration of graphene oxide is 0.3-1.2mg/mL in the graphene oxide dispersion.
The pH value of the graphene oxide aqueous slkali is 7.5-9.5.
The volume ratio of ethanol and 1,3 propane diols is 1 in the mixed liquor of the ethanol and 1,3 propane diols:1.
The concentration of the butyl titanate solution is 0.2-0.4g/mL.
The particle diameter of the graphene oxide/composite titania material is 1-10 μm.
The temperature annealed in the air atmosphere of step (3) is 380-410 DEG C.
The cleaning of step (5) is cleaned using nitrogen.
Preferably, the graphene oxide is 1-3 layers.
The invention has the advantages that graphene/titanium dioxide/nano silver composite material antibacterial that the present invention is prepared
Agent, by band engineering, promotes the separation of electric charge, silver ion reduction in situ and deposition improve titanium dioxide/nano silver circle
Face, has collaboration facilitation to the antibacterial of nano-Ag particles, increases substantially the utilization rate and anti-microbial property of silver.Institute of the present invention
The preparation process being related to has easy to operate, and cost is low, efficient, it is easy to accomplish scale, industrialization production and application are wide
The advantages that general.
Brief description of the drawings
Fig. 1 is antibacterial activity test result comparison diagram of the present invention.
Embodiment
Embodiment 1
It is first according to following steps and prepares graphene/titanium dioxide/nano silver composite material：
(1) graphene oxide (GO) is prepared using Hummers methods, the wherein mass ratio of potassium permanganate and graphite is 6：1, will
GO is scattered in mixed liquor (wherein volume ratio=1 of ethanol and water of alcohol-water：3), concentration 0.6mg/mL, is ultrasonically treated 6h,
The alcohol-water dispersion liquid of GO is made；
(2) it is added dropwise concentrated ammonia liquor into the alcohol-water dispersion liquid of above-mentioned GO, control pH is stirred at room temperature 8.0 or so
30min, obtains the first mixed liquor；
(3) butyl titanate is dissolved in ethanol -1,3 mixed with propylene glycol liquid, wherein the volume ratio of ethanol and 1,3-PD
=1：1, obtain ethanol -1,3 propylene glycol solution that concentration is 0.2g/mL butyl titanates, i.e. the second mixed liquor, by titanium atom and
Alcoholic extract hydroxyl group combines, and controls sequential hydrolysis speed；
(4) the first mixed liquor obtained by 10L steps (2) is taken, while being stirred continuously at room temperature, is added dropwise thereto
The second mixed liquor obtained by 90mL steps (3), persistently stirs 24h, centrifuges, cleaning 3~5 times, afterwards 60 DEG C of dry 12h,
Anneal 30min at 400 DEG C, obtains graphene oxide/composite titania material；
(5) graphene oxide/composite titania material obtained by step (4) is scattered in ethanol again, thereto
Silver nitrate ethanol solution is added, the mass ratio for making silver nitrate, graphene oxide/composite titania material and ethanol is 0.1：1：
98.9, stir 10 minutes, obtain intermediate.
(6) storing solution using above-mentioned intermediate as light reaction, is placed in 250ml reaction kettles, is ultrasonically treated 15min, in
Dark place is passed through nitrogen and is cleaned, and reaction kettle, is placed in Photoreactor by scavenging period 15min afterwards, under room temperature into
Row stirring, while using mercury lamp ultraviolet-visible illumination 4h, intensity of illumination 90mW/cm2, obtain final product.
Sample antibiotic property test with reference to minimal inhibitory concentration (Minimal Inhibitory Concentration,
MIC test method), it is Escherichia coli and staphylococcus aureus to select strain, and test result is shown in Table 1.
Test side of the antibacterial activity assessment of sample with reference to Colony Forming Unit (Colony-forming Units, CFU)
Method, selection strain are Escherichia coli, staphylococcus aureus, hay bacillus, Pseudomonas aeruginosa and B.pumilus, are respectively adopted
Different light application time detections is antibacterial as a result, test result is shown in Fig. 1.
Embodiment 2
It is first according to following steps and prepares graphene/titanium dioxide/nano silver composite material：
(1) graphene oxide (GO) is prepared using Hummers methods, the wherein mass ratio of potassium permanganate and graphite is 5：1, will
GO is scattered in mixed liquor (wherein volume ratio=1 of ethanol and water of alcohol-water：3), concentration 0.9mg/mL, is ultrasonically treated 6h,
The alcohol-water dispersion liquid of GO is made；
(2) it is added dropwise concentrated ammonia liquor into the alcohol-water dispersion liquid of above-mentioned GO, control pH is stirred at room temperature 9.0 or so
30min, obtains the first mixed liquor；
(3) butyl titanate is dissolved in ethanol -1,3 mixed with propylene glycol liquid, wherein the volume ratio of ethanol and 1,3-PD
=1：1, obtain ethanol -1,3 propylene glycol solution that concentration is 0.4g/mL butyl titanates, i.e. the second mixed liquor, by titanium atom and
Alcoholic extract hydroxyl group combines, and controls sequential hydrolysis speed；
(4) the first mixed liquor obtained by 10L steps (2) is taken, while being stirred continuously at room temperature, is added dropwise thereto
The second mixed liquor obtained by 90mL steps (3), persistently stirs 24h, centrifuges, cleaning 3~5 times, afterwards 60 DEG C of dry 12h,
Anneal 30min at 410 DEG C, obtains graphene oxide/composite titania material；
(5) graphene oxide/composite titania material obtained by step (4) is scattered in ethanol again, thereto
Silver nitrate ethanol solution is added, the mass ratio for making silver nitrate, graphene oxide/composite titania material and ethanol is 0.08：
1：98.9, stir 10 minutes, obtain intermediate.
(6) storing solution using above-mentioned intermediate as light reaction, is placed in 250ml reaction kettles, is ultrasonically treated 15min, in
Dark place is passed through nitrogen and is cleaned, and reaction kettle, is placed in Photoreactor by scavenging period 15min afterwards, under room temperature into
Row stirring, while using mercury lamp ultraviolet-visible illumination 2h, intensity of illumination 100mW/cm2, obtain final product.
Embodiment 3
It is first according to following steps and prepares graphene/titanium dioxide/nano silver composite material：
(1) graphene oxide (GO) is prepared using Hummers methods, the wherein mass ratio of potassium permanganate and graphite is 8：1, will
GO is scattered in mixed liquor (wherein volume ratio=1 of ethanol and water of alcohol-water：3), concentration 1.2mg/mL, is ultrasonically treated 6h,
The alcohol-water dispersion liquid of GO is made；
(2) concentrated ammonia liquor is added dropwise into the alcohol-water dispersion liquid of above-mentioned GO, it is 9.5 to control pH, and 30min is stirred at room temperature,
Obtain the first mixed liquor；
(3) butyl titanate is dissolved in ethanol -1,3 mixed with propylene glycol liquid, wherein the volume ratio of ethanol and 1,3-PD
=1：1, obtain ethanol -1,3 propylene glycol solution that concentration is 0.3g/mL butyl titanates, i.e. the second mixed liquor, by titanium atom and
Alcoholic extract hydroxyl group combines, and controls sequential hydrolysis speed；
(4) the first mixed liquor obtained by 10L steps (2) is taken, while being stirred continuously at room temperature, is added dropwise thereto
The second mixed liquor obtained by 90mL steps (3), persistently stirs 24h, centrifuges, cleaning 3~5 times, afterwards 60 DEG C of dry 12h,
Anneal 30min at 380 DEG C, obtains graphene oxide/composite titania material；
(5) graphene oxide/composite titania material obtained by step (4) is scattered in ethanol again, thereto
Silver nitrate ethanol solution is added, the mass ratio for making silver nitrate, graphene oxide/composite titania material and ethanol is 0.12：
1：98.9, stir 10 minutes, obtain intermediate.
(6) storing solution using above-mentioned intermediate as light reaction, is placed in 250ml reaction kettles, is ultrasonically treated 15min, in
Dark place is passed through nitrogen and is cleaned, and reaction kettle, is placed in Photoreactor by scavenging period 15min afterwards, under room temperature into
Row stirring, while using mercury lamp ultraviolet-visible illumination 1h, intensity of illumination 110mW/cm2, obtain final product.
Embodiment 4
It is first according to following steps and prepares graphene/titanium dioxide/nano silver composite material：
(1) graphene oxide (GO) is prepared using Hummers methods, the wherein mass ratio of potassium permanganate and graphite is 7：1, will
GO is scattered in mixed liquor (wherein volume ratio=1 of ethanol and water of alcohol-water：3), concentration 0.3mg/mL, is ultrasonically treated 6h,
The alcohol-water dispersion liquid of GO is made；
(2) concentrated ammonia liquor is added dropwise into the alcohol-water dispersion liquid of above-mentioned GO, it is 7.5 to control pH, and 30min is stirred at room temperature,
Obtain the first mixed liquor；
(3) butyl titanate is dissolved in ethanol -1,3 mixed with propylene glycol liquid, wherein the volume ratio of ethanol and 1,3-PD
=1：1, obtain ethanol -1,3 propylene glycol solution that concentration is 0.4g/mL butyl titanates, i.e. the second mixed liquor, by titanium atom and
Alcoholic extract hydroxyl group combines, and controls sequential hydrolysis speed；
(4) the first mixed liquor obtained by 10L steps (2) is taken, while being stirred continuously at room temperature, is added dropwise thereto
The second mixed liquor obtained by 90mL steps (3), persistently stirs 24h, centrifuges, cleaning 3~5 times, afterwards 60 DEG C of dry 12h,
Anneal 30min at 400 DEG C, obtains graphene oxide/composite titania material；
(5) graphene oxide/composite titania material obtained by step (4) is scattered in ethanol again, thereto
Silver nitrate ethanol solution is added, the mass ratio for making silver nitrate, graphene oxide/composite titania material and ethanol is 0.1：1：
98.9, stir 10 minutes, obtain intermediate.
(6) storing solution using above-mentioned intermediate as light reaction, is placed in 250ml reaction kettles, is ultrasonically treated 15min, in
Dark place is passed through nitrogen and is cleaned, and reaction kettle, is placed in Photoreactor by scavenging period 15min afterwards, under room temperature into
Row stirring, while using mercury lamp ultraviolet-visible illumination 0.5h, intensity of illumination 120mW/cm2, obtain final product.
Comparative example 1
Graphene/titanium dioxide/nano silver composite material is prepared in accordance with the following steps：
(1) graphene oxide (GO) is prepared using Hummers methods, the wherein mass ratio of potassium permanganate and graphite is 6：1, will
GO is scattered in mixed liquor (wherein volume ratio=1 of ethanol and water of alcohol-water：3), concentration 0.6mg/mL, is ultrasonically treated 6h,
The alcohol-water dispersion liquid of GO is made；
(2) the alcohol-water dispersion liquid and silver nitrate aqueous solution of above-mentioned GO are mixed, titanium dioxide is dispersed in above-mentioned mixing
In liquid, the mass ratio of silver nitrate, graphene oxide and titanium dioxide is 0.01：0.3：1.
(3) and then by above-mentioned substance add in Photoreactor, in simulated solar light reaction 2h, filter, wash, it is dry, obtain
To graphene/titanium dioxide/nano silver composite material.It is detected, the results are shown in Table 1.
Comparative example 2
According to the embodiment 1 of patent document (Application No. 201610738245.3), antimicrobial composite material is prepared, it is right
It is detected, and the results are shown in Table 1.
1 antibacterial effect contrast table of table
| Escherichia coli (ppm) | Staphylococcus aureus (ppm) | |
| Embodiment 1 | 100 | 50 |
| Comparative example 1 | 220 | 60 |
| Comparative example 2 | 170 | 65 |
Interpretation of result：
With the growth of mercury lamp ultraviolet-visible light application time, final graphene/titanium dioxide/nano silver composite material
Anti-microbial property is more preferable, this is because the surface of composite material film produces defect under illumination condition, hydrophily is improved, and water is excellent
First adsorbed at surface defect, as the increase of light application time, antibacterial effect are better.
Graphene/titanium dioxide/nano silver composite material to the antibacterial effects of Escherichia coli and staphylococcus aureus with
The increase of Ag contents and strengthen；This is because silver ion antimicrobial agent by the interference effect to bacteria cell wall, damages thalline,
Therefore antibacterial effect is more preferable.
During preparing titanium dioxide, the pH value of the reaction solution of concentrated ammonia liquor and butyl titanate is higher, graphene/titanium dioxide
Titanium/nano silver composite material is better to the antibacterial effect of Escherichia coli and staphylococcus aureus, for Escherichia coli and golden yellow
For color staphylococcus, optimal pH is about 7.0-8.0, and bacterial growth is most active within this range, and antibacterial effect is relatively
Difference.
The situ aggregation method that embodiment 1 uses is straight compared to comparative example 1 in surface of graphene oxide uniform deposition titanium dioxide
Connect and add for finished titanium dioxide particle, the antibacterial effect of final composite material is more preferable.
Claims (10)
1. a kind of preparation method of graphene/titanium dioxide/nano silver composite material, it is characterised in that comprise the following steps：
(1) graphene oxide is scattered in solvent, obtains graphene oxide dispersion, be added dropwise into graphene oxide dispersion
Ammonium hydroxide, obtains graphene oxide aqueous slkali；
(2) butyl titanate is added in organic solvent, organic solvent is ethanol and 1, and the mixed liquor of 3 propane diols, obtains metatitanic acid
Butyl acetate solution；
(3) butyl titanate solution is added in graphene oxide aqueous slkali, stirred, separated, it is dry, moved back in air atmosphere
Fire, obtains graphene oxide/composite titania material；
(4) graphene oxide/composite titania material of step (3) is scattered in solvent, adds silver nitrate solution, stir
Mix, obtain intermediate, the mass ratio of the silver nitrate and graphene oxide/composite titania material is (0.08-0.12)：1；
(5) intermediate is ultrasonically treated, after cleaning, carries out light processing, intensity of illumination 90-120mW/cm2, light application time
For 1-4h, graphene/titanium dioxide/nano silver composite material is obtained.
2. the preparation method of graphene/titanium dioxide/nano silver composite material as claimed in claim 1, it is characterised in that institute
Graphene oxide is stated to be made using Hummers methods.
3. the preparation method of graphene/titanium dioxide/nano silver composite material as claimed in claim 1, it is characterised in that institute
The mass ratio for stating silver nitrate and ethanol is (0.08-0.12)：98.9.
4. the preparation method of graphene/titanium dioxide/nano silver composite material as claimed in claim 1, it is characterised in that institute
The mixed liquor that solvent in graphene oxide dispersion is second alcohol and water is stated, the wherein volume ratio of ethanol and water is 1:3, the oxidation
The concentration of graphene oxide is 0.3-1.2mg/mL in graphene dispersing solution.
5. the preparation method of graphene/titanium dioxide/nano silver composite material as claimed in claim 1, it is characterised in that institute
The pH value for stating graphene oxide aqueous slkali is 7.5-9.5.
6. the preparation method of graphene/titanium dioxide/nano silver composite material as claimed in claim 1, it is characterised in that institute
It is 1 to state the volume ratio of ethanol and 1,3 propane diols in the mixed liquor of ethanol and 1,3 propane diols：1.
7. the preparation method of graphene/titanium dioxide/nano silver composite material as described in claim 1 or 6, its feature exist
In the concentration of the butyl titanate solution is 0.2-0.4g/mL.
8. the preparation method of graphene/titanium dioxide/nano silver composite material as claimed in claim 1, it is characterised in that institute
The particle diameter for stating graphene oxide/composite titania material is 1-10 μm.
9. the preparation method of graphene/titanium dioxide/nano silver composite material as claimed in claim 1, it is characterised in that step
Suddenly the temperature annealed in the air atmosphere of (3) is 380-410 DEG C.
10. such as the preparation method of claim 1-6 any one of them graphene/titanium dioxide/nano silver composite material, it is special
Sign is that the cleaning of step (5) is cleaned using nitrogen.
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Cited By (17)
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| CN108868563A (en) * | 2018-05-16 | 2018-11-23 | 董凤良 | A kind of window screening and preparation method thereof to be purified the air of a room based on visible light photocatalysis |
| CN110180542A (en) * | 2019-04-01 | 2019-08-30 | 武汉理工大学 | A kind of titanium dioxide/graphene/metal simple-substance tri compound catalysis material and photo-reduction preparation method |
| CN110214790A (en) * | 2018-09-04 | 2019-09-10 | 莆田学院 | A kind of magnetic bamboo charcoal/nanometer silver/titanium dioxide compound disinfectant and its preparation method and application |
| CN110367279A (en) * | 2019-06-21 | 2019-10-25 | 冉圳 | A kind of preparation method of long-acting type drinking water anti-biotic material |
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| CN110214790A (en) * | 2018-09-04 | 2019-09-10 | 莆田学院 | A kind of magnetic bamboo charcoal/nanometer silver/titanium dioxide compound disinfectant and its preparation method and application |
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