CN109077064A - A kind of GQDs/TiO2/ CuO composite antibacterial material and the preparation method and application thereof - Google Patents
A kind of GQDs/TiO2/ CuO composite antibacterial material and the preparation method and application thereof Download PDFInfo
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- CN109077064A CN109077064A CN201810989006.4A CN201810989006A CN109077064A CN 109077064 A CN109077064 A CN 109077064A CN 201810989006 A CN201810989006 A CN 201810989006A CN 109077064 A CN109077064 A CN 109077064A
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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
- A01N59/20—Copper
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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
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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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Abstract
The invention discloses a kind of GQDs/TiO2/ CuO composite antibacterial material and the preparation method and application thereof, when preparation, prepare nano-TiO first2/ CuO, the preparation of composite antibacterial material is completed in its area load GQDs later, preparation process is simple, material is cheap and easy to get, it is easily industrialized production, composite antibacterial material prepared by the present invention has preferable anti-microbial property, can be widely applied in various antibacterial, sterilization fields, such as environmental protection and antibiotic paint field, it is suitable for promoting the use of.
Description
Technical field
The invention belongs to photocatalysis antibacterial field of composite material preparation more particularly to a kind of GQDs/TiO2/ CuO is compound
Anti-biotic material and the preparation method and application thereof.
Background technique
Photocatalysis antibacterial agent is a kind of antibacterial agent occurred in recent years, due to its is nontoxic, without special odor, non-stimulated
Property, body color be mostly white, colour stability is good, under high temperature it is non-discolouring, do not decompose, cheap and resourceful spy
Property, such antibacterial agent are used widely in recent years, and such antibacterial agent is with TiO2For representative substances.Photocatalysis is strong due to it
Oxidability can destroy the cell wall structure of bacterium and decomposite bacterial body, solidify virus protein, control the activity of virus,
Achieve the purpose that efficient sterilizing, but TiO2Antibacterial ability only can be just shown under the irradiation of ultraviolet light, greatly limited
It is applied.
By in TiO2Middle doping metals or nonmetallic ion and introduce impurity or defect, TiO can not only be improved2Light
It absorbing, inhibits the compound again of photo-generate electron-hole, improve quantum efficiency, range and photocatalysis efficiency can be utilized by improving spectrum,
And the lattice defect of titanium dioxide itself can be improved, increase forbidden band absorption region, enhances photosensitive property.Utilize titanium dioxide
The characteristics of surface polyhydroxy, can load other antibacterial agents, improve anti-microbial property.Expand studies have shown that the metal oxide of incorporation rises
Open up TiO2Spectrum can utilize the effect of range, and nonmetallic, inhibit the compound of photo-generated carrier, the two synergistic effect, Ke Yiti
High anti-microbial property.
Zero dimension graphene-structured of the graphene quantum dot (GQDs) as Nano grade, inherits the antibiotic property of graphene
Matter, also, since its molecular structure is rich in defect, special nature thus is shown in many aspects, and correlative study shows graphite
Alkene quantum dot is likewise supplied with certain antimicrobial effect.
Therefore, present invention contemplates that in TiO2Middle blended metal oxide or nonmetallic materials and introduce impurity or defect is formed
A kind of photocatalysis composite antibacterial material of Cheap highly effective, and can be widely used in environment and antimicrobial product.
Summary of the invention
It is an object of the invention to solve deficiency in the prior art, a kind of GQDs/TiO is provided2/ CuO composite antibacterial material
The preparation method and applications of material, antimicrobial composite material prepared by the present invention improve graphene quantum dot load nano-TiO2/
The anti-microbial property of CuO, enhances nano-TiO2The antibacterial activity of/CuO.
The specific technical solution of the present invention is as described below:
A kind of GQDs/TiO2The preparation method of/CuO composite antibacterial material, specifically comprises the following steps:
1) preparation of GQDs: citric acid heating fusing is taken, then adjusting pH with alkaline solution is 6-8, prepares GQDs aqueous solution；
2) prepared by CuO: NaOH solution is instilled Cu (CH3COO)2·H2It in O solution, is vigorously stirred, acquired solution is placed in
In reaction kettle, hydro-thermal reaction prepares CuO；
3)TiO2The preparation of/CuO: titanium dioxide (99.8%, 40nm, rutile titania is hydrophilic, the production of Mike woods company) is added
In deionized water, and NaOH is added thereto, the copper oxide for later preparing step 2 is dissolved in deionized water, and copper oxide is molten
Drop is added in titania solution, is vigorously stirred, water-bath, and washing obtains TiO in 100 DEG C of dry 1h2/ CuO solid；
4)GQDs/TiO2The preparation of/CuO: TiO is prepared2The aqueous solution of/CuO, is added GQDs thereto, ultrasonic reaction, from
The heart washs, dry, obtains GQDs/TiO2/ CuO composite antibacterial material.
Further, in the step 1) citric acid fusion temperature be 150~250 DEG C, alkaline solution include NaOH and
KOH solution.
Further, NaOH and Cu (CH in the step 2)3COO)2·H2The molar ratio of O is (4~10): 5.
Further, the reaction temperature in the step 2) in reaction kettle is 110~150 DEG C, and the reaction time is in 2~4h.
Further, TiO in the step 3)2, NaOH and CuO molar ratio be (10~1): (1~5): 1.
Further, GQDs and TiO in the step 4)2The mass ratio of/CuO is (10~1): 1.
Further, the time of ultrasonic reaction is 1~3h in the step 4).
GQDs/TiO of the present invention2/ CuO composite antibacterial material can be applicable in antibacterial, sterilization field.
Compared with prior art, the invention has the following advantages:
1. the GQDs/TiO that method disclosed by the invention is prepared2/ CuO composite antibacterial material has preferable antibiotic property
Can, it can be widely applied in various antibacterial, sterilization fields, such as environmental protection and antibiotic paint field.
2. the process of preparation method disclosed by the invention is simple, it is easy to accomplish industrialization is suitable for promoting the use of.
Detailed description of the invention
Fig. 1 is the fluorescence spectra for the graphene quantum dot that the embodiment of the present invention one synthesizes, and wherein a is exciting light spectrogram, b
For launching light spectrogram；
Fig. 2 is GQDs/TiO prepared by the embodiment of the present invention one2Antibiotic rate statistical chart (this of/CuO composite antibacterial material
It is relatively good whether three words of statistical chart are not deleted)；
Fig. 3 A is GQDs/TiO prepared by the embodiment one of various concentration2/ CuO composite antibacterial material is to Escherichia coli (E)
Bacteriostasis rate change with time figure；
Fig. 3 B is GQDs/TiO prepared by the embodiment one of various concentration2/ CuO composite antibacterial material is to Staphylococcus aureus
The bacteriostasis rate of bacterium (S) changes with time figure.
Specific embodiment
Following embodiment further illustrates the contents of the present invention, but should not be construed as limiting the invention.Without departing substantially from
In the case where essence of the present invention, to modification made by the method for the present invention, step or condition and replaces, belong to model of the invention
It encloses.
Embodiment one
(1) preparation of GQDs:
Take 2g citric acid in 5mL beaker, in heating mantle, 195 DEG C of heating；After 5min, lemon acid dissolution then exists
Solution gradually becomes light yellow again to orange from colourless in 30min, shows that GQDs has been formed；Then titrated with the NaOH of 1M,
Ultrasound promotes dispersion, is vigorously stirred, and obtains the GQDs solution that pH is 7, final concentration of 80mg/mL；
(2) preparation of CuO:
The NaOH solution of 40mL, 1mol/L are instilled into 50mL, the Cu (CH of 1mol/L3COO)2·H2In O solution, acutely stir
It mixes, forms uniform blue solution, by acquired solution as in reaction kettle, 110 DEG C, hydro-thermal 2h.
(3)TiO2/ CuO preparation:
0.0125mol titanium dioxide is dissolved in 30mL deionized water, the NaOH of 0.0125mol is added, reaction temperature is protected
80 DEG C are held, then 0.0125mol CuO is dissolved in 30mL deionized water, CuO solution is added drop-wise to TiO2In solution, 80 DEG C are stirred
Mix 2h, centrifugation, washing, 100 DEG C of vacuum drying 1h.
(4)GQDs/TiO2/ CuO preparation:
Prepare TiO2/ CuO aqueous solution, is added GQDs, GQDs and TiO thereto2The mass ratio of/CuO is 1:1, ultrasonic 1h.
Centrifugation, washing, drying, obtain GQDs/TiO2/ CuO composite antibacterial material.
The characterization test of composite antibacterial material:
1. the graphene quantum dot that pair the present embodiment obtains carries out fluorescence detection, the results are shown in attached figure 1:
Figure a and b is the fluorescence spectrum of graphene quantum dot, and figure a is excitation spectrum, as can be seen from the figure wavelength 518nm
Fluorescence have maximum excitation peak at 446nm.Figure b is emission spectrum, as can be seen from the figure in the case where 370nm excites light action,
There is maximum emission peak at 508nm, this also demonstrates the substance with luminescence generated by light effect, is consistent with graphene quantum dot, demonstrate,proves
It is bright using citric acid as predecessor, the graphene quantum dot of pyrolysis is successfully prepared.
2. antibacterial experiment:
The preparation of bacterium mother liquor: the staphylococcus aureus (S.) for taking laboratory to save respectively and Gram-negative bacteria large intestine
For bacillus (E.coli.) in 20mL NA fluid nutrient medium, 37 DEG C of isothermal vibration cultures for 24 hours, obtain bacterium mother liquor.
The preparation of antibacterial mother liquor: TiO2/ CuO and GQDs/TiO2/ CuO respectively takes 10mg, sequentially add two containing 10mL it is ultrapure
In the test tube of water and ultrasonic disperse 10min, in addition use the test tube equipped with 10mL ultrapure water as compareing, three test tube conducts
Antibacterial mother liquor.
Plate count counts antibiotic rate: taking three test tubes, 8mL sterile saline is added thereto respectively, 1mL bacterium is female
Liquid is vortexed concussion uniformly, and 1mL antibacterial mother liquor is then added, and 37 DEG C of isothermal vibration 2h, i.e. antibacterial mother liquid concentration are 100 μ g/mL.
In mixed liquor 1mL injection 9mL sterile saline after taking concussion, this dilution is 10-1, gradient dilution to 10-5, then take
0.1mL 10-5The dilution of gradient is coated on NA plate, and repeats six plates.It is inverted in 37 DEG C of constant incubator cultures
After for 24 hours, counts and count antibiotic rate.
By attached drawing 2 it is found that the TiO of 100 μ g/mL2/ CuO distinguishes the antibiotic rate of Escherichia coli and staphylococcus aureus
For 70% and 60%；100μg/mL GQDs/TiO2/ CuO to the antibiotic rates of Escherichia coli and staphylococcus aureus be 96% with
92%.Composite antibacterial material prepared by the present invention has staphylococcus aureus and gram-positive bacteria Escherichia coli very strong
Antibiotic property.
3. the bacteriostasis rate of various concentration composite antibacterial material
Attached drawing 3A and 3B are the GQDs/TiO of various concentration respectively2/ CuO composite antibacterial material is to Escherichia coli and golden yellow
Staphylococcic bacteriostasis rate statistical chart, it can be seen from the figure that 50mg/L composite antibacterial material is to Gram-negative bacteria large intestine bar
The growth of bacterium has apparent inhibitory effect, and 80mg/L composite antibacterial material has apparent inhibition to the growth of staphylococcus aureus
Effect.
Embodiment two
(1) preparation of GQDs:
Take 2g citric acid in 5mL beaker, in heating mantle, 150 DEG C of heating；After 5min, lemon acid dissolution then exists
Solution gradually becomes light yellow again to orange from colourless in 30min, shows that GQDs has been formed；Then titrated with the NaOH of 1M,
Ultrasound promotes dispersion, is vigorously stirred, and obtains the GQDs solution that pH is 7, final concentration of 80mg/mL；
(2) preparation of CuO:
The NaOH solution of 40mL, 1mol/L are instilled into 50mL, the Cu (CH of 1mol/L3COO)2·H2In O solution, acutely stir
It mixes, forms uniform blue solution, acquired solution is placed in reaction kettle, 130 DEG C, hydro-thermal 3h.
(3)TiO2/ CuO preparation:
0.125mol titanium dioxide is dissolved in 30mL deionized water, the NaOH of 0.0125mol is added, reaction temperature is kept
80 DEG C, then 0.0125mol copper oxide is dissolved in 30mL deionized water, oxidation copper solution is added drop-wise to titania solution
In, 80 DEG C of stirring 2h, centrifugation, washing, 100 DEG C of vacuum drying 1h.
(4)GQDs/TiO2/ CuO preparation:
Prepare TiO2/ CuO aqueous solution, is added GQDs, GQDs and TiO thereto2The mass ratio of/CuO is 5:1, ultrasonic 2h.
Centrifugation, washing, drying, obtain GQDs/TiO2/ CuO composite antibacterial material, is detected composite antibacterial material made from the present embodiment
99% or more is reached to the antibiotic rate of Escherichia coli and staphylococcus aureus.
Embodiment three
(1) preparation of GQDs:
Take 2g citric acid in 5mL beaker, in heating mantle, 250 DEG C of heating；After 5min, lemon acid dissolution then exists
Solution gradually becomes light yellow again to orange from colourless in 30min, shows that GQDs has been formed；It is then titrated, is surpassed with the KOH of 1M
Sound promotes dispersion, is vigorously stirred, and obtains the GQDs solution that pH is 7, final concentration of 80mg/mL；
(2) preparation of CuO:
The NaOH solution of 40mL, 1mol/L are instilled into 50mL, the Cu (CH of 1mol/L3COO)2·H2In O solution, acutely stir
It mixes, forms uniform blue solution, acquired solution is placed in reaction kettle, 150 DEG C, hydro-thermal 4h.
(3)TiO2/ CuO preparation:
0.0625mol titanium dioxide is dissolved in 30mL deionized water, the NaOH of 0.0125mol is added, reaction temperature is protected
80 DEG C are held, then 0.0125mol copper oxide is dissolved in 30mL deionized water, oxidation copper solution is added drop-wise to titania solution
In, 80 DEG C of stirring 2h, centrifugation, washing, 100 DEG C of vacuum drying 1h.
(4)GQDs/TiO2/ CuO preparation:
Prepare TiO2/ CuO aqueous solution, is added GQDs, GQDs and TiO thereto2The mass ratio of/CuO be 10:1, ultrasonic 3h,
Centrifugation, washing, drying, obtain GQDs/TiO2/ CuO composite antibacterial material, is detected composite antibacterial material made from the present embodiment
98% and 99% are respectively reached to the antibiotic rate of Escherichia coli and staphylococcus aureus.
Basic principles and main features and advantage of the invention have been shown and described above.But the foregoing is merely this hairs
Bright specific embodiment, technical characteristic of the invention are not limited thereto, and any those skilled in the art is not departing from this hair
The other embodiments obtained under bright technical solution should all cover within the scope of the patent of the present invention.
Claims (9)
1. a kind of GQDs/TiO2The preparation method of/CuO composite antibacterial material, which is characterized in that specifically comprise the following steps:
1) preparation of GQDs: citric acid heating fusing is taken, then adjusting pH with alkaline solution is 6-8, prepares GQDs aqueous solution；
2) prepared by CuO: NaOH solution is instilled Cu (CH3COO)2·H2It in O solution, is vigorously stirred, acquired solution is placed in reaction
In kettle, hydro-thermal reaction prepares CuO；
3)TiO2The preparation of/CuO: by TiO2It is added in deionized water, and NaOH is added thereto, later by step 2) preparation
CuO is dissolved in deionized water, and CuO solution is added drop-wise to TiO2It in solution, is vigorously stirred, water-bath, washs, it is dry in 100 DEG C
Dry 1h obtains TiO2/ CuO solid；
4)GQDs/TiO2The preparation of/CuO: TiO is prepared2The aqueous solution of/CuO, is added GQDs, ultrasonic reaction thereto, and centrifugation is washed
It washs, it is dry, obtain GQDs/TiO2/ CuO composite antibacterial material.
2. a kind of GQDs/TiO as described in claim 12The preparation method of/CuO composite antibacterial material, which is characterized in that described
The fusion temperature of citric acid is 150~250 DEG C in step 1), and alkaline solution includes NaOH and KOH solution.
3. a kind of GQDs/TiO as described in claim 12The preparation method of/CuO composite antibacterial material, which is characterized in that described
NaOH and Cu (CH in step 2)3COO)2·H2The molar ratio of O is (4~10): 5.
4. a kind of GQDs/TiO as described in claim 12The preparation method of/CuO composite antibacterial material, which is characterized in that described
Reaction temperature in step 2) in reaction kettle is 110~150 DEG C, and the reaction time is in 2~4h.
5. a kind of GQDs/TiO as described in claim 12The preparation method of/CuO composite antibacterial material, which is characterized in that described
TiO in step 3)2, NaOH and CuO molar ratio be (10~1): (1~5): 1.
6. a kind of GQDs/TiO as described in claim 12The preparation method of/CuO composite antibacterial material, which is characterized in that described
GQDs and TiO in step 4)2The mass ratio of/CuO is (10~1): 1.
7. a kind of GQDs/TiO as described in claim 12The preparation method of/CuO composite antibacterial material, which is characterized in that described
The time of ultrasonic reaction is 1~3h in step 4).
8. such as a kind of described in any item GQDs/TiO of claim 1-72The preparation method preparation of/CuO composite antibacterial material
GQDs/TiO2/ CuO composite antibacterial material.
9. a kind of GQDs/TiO as claimed in claim 82/ CuO composite antibacterial material is in application antibacterial, in sterilization field.
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| CN110736770A (en) * | 2019-10-16 | 2020-01-31 | 郑州大学 | N-GQDs modified 3DOM In2O3Composite material and preparation method and application thereof |
| WO2022086315A1 (en) * | 2020-10-23 | 2022-04-28 | Ah Eng Siaw | A resonance antimicrobial coating for disinfecting surface |
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