CN106359373A - Porous graphene zinc-oxide-loaded antibacterial composite material and preparation method thereof - Google Patents
Porous graphene zinc-oxide-loaded antibacterial composite material and preparation method thereof Download PDFInfo
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- CN106359373A CN106359373A CN201610738528.8A CN201610738528A CN106359373A CN 106359373 A CN106359373 A CN 106359373A CN 201610738528 A CN201610738528 A CN 201610738528A CN 106359373 A CN106359373 A CN 106359373A
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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
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
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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
Abstract
The invention discloses a porous graphene zinc-oxide-loaded antibacterial composite material and a preparation method thereof. The preparation method comprises the following steps: (1) preparing graphene quantum dot suspension liquid; (2) preparing zinc-oxide-loaded graphene quantum dots; (3) carrying out surface treatment; (4) preparing a composite material. According to the method, the graphene quantum dots irradiated by laser are taken as carriers of nano-zinc oxide, are then subjected to the surface treatment, and are finally attached to porous graphene, so that the nano-zinc oxide is better loaded and fixed so as to be prevented from agglomerating. After the method is adopted, the stability of the nano-zinc oxide is obviously improved, and the nano-zinc oxide is enabled to have a more long-acting antibacterial activity, so that the porous graphene zinc-oxide-loaded antibacterial composite material has wide prospect in industrial application.
Description
Technical field
The present invention relates to a kind of porous graphene load zinc oxide antimicrobial composite material and preparation method thereof.
Background technology
Nano zine oxide, because its size is between cluster and Macroscopic particulates, has volume (the little chi of nano material
Very little) effect, skin effect and macro quanta tunnel effect, in the aspects such as light, electricity, air-sensitive, antibiotic and sterilizing, ultraviolet screener tool
Standby specific function not available for common zinc oxide product.
Graphene, as the allotrope of carbon, is that carbon atom has alveolate texture by what sp2 orbital hybridization was formed
Monolayer two dimensional crystal material, good mechanical performance that Graphene has, chemical stability etc. also will be in fields such as composites
Have broad application prospects.
Nano zine oxide and Graphene are combined and will improve the anti-microbial property of zinc oxide, but this kind of antibacterial characteristics are still inadequate
Ideal, nano zine oxide is reunited seriously, is difficult to disperse, is gathered in the local of Graphene；And nano zine oxide is with Graphene no
Method is combined closely, and easily comes off in use, thus affecting service life and antibacterial effect.
Content of the invention
The technical problem to be solved there is provided a kind of porous graphene load zinc oxide antimicrobial composite material
And preparation method thereof.
The technical problem to be solved is achieved by the following technical programs:
A kind of porous graphene loads the preparation method of zinc oxide antimicrobial composite material, and it comprises the following steps:
(1) prepare graphene quantum dot suspension: weigh 0.5 ~ 0.8g c60 powder, measuring 50 ~ 100ml mass fraction is 98%
Concentrated sulphuric acid, c60 powder and concentrated sulphuric acid are mixed in beaker, beaker is placed in ice-water bath, simultaneously with the speed of 300 ~ 500rpm
Degree stirring, obtains mixed liquor；Weigh 0.5 ~ 3g potassium permanganate powder, slowly add in above-mentioned mixed liquor；Remove ice-water bath, change
Become water-bath, keep 30 ~ 40 DEG C of bath temperature, react 5 ~ 8h；Rapidly join 100 ~ 200ml pure water, filter, then with retention molecule
Measure the bag filter for 1000 to dialyse 3 days, obtain graphene quantum dot suspension；100rpm speed stirring graphene quantum dot suspends
Liquid, laser irradiation 30 ~ 60min simultaneously, laser irradiation power is 1 ~ 2w.
(2) weigh Zinc oxide quantum dot (particle diameter about 2 ~ 5nm) and be configured to the dispersion liquid that concentration is 0.5 ~ 1mg/ml, solvent is
Water；Ultrasonic agitation (500 ~ 1000w ultrasonic power, 600 ~ 800rpm mixing speed) 80 ~ 100ml zinc oxide fluid dispersion, Deca walks
Suddenly the graphene quantum dot suspension that (1) is obtained, continues ultrasonic agitation 30 ~ 60min；Centrifugation, cleaning, dry, obtain loading oxygen
Change the graphene quantum dot of zinc.
(3) surface treatment of the graphene quantum dot of load zinc oxide: 0.005 ~ 0.01g graphite oxide is added to 5 ~
In the dispersant (dmso) of 10ml, ultrasonic agitation (300 ~ 500w ultrasonic power, 200 ~ 300rpm mixing speed) add 0.1 ~
0.3g loads the graphene quantum dot of zinc oxide, continues ultrasonic agitation 10 ~ 30min, moves to the microwave that liner is politef
In hydrothermal reaction kettle (50 ml), it is placed in after sealing in microwave assisted hydrothermal synthesis apparatus, microwave power is 200 ~ 400w, 200 ~ 240
60 ~ 90min is reacted at DEG C；Cooling, filters, and dries the graphene quantum dot of the load zinc oxide that must be surface-treated.
(4) weigh porous graphene (2 ~ 5 layers, hole size about 3 ~ 6nm) and be configured to the graphite that concentration is 0.2 ~ 0.8mg/ml
Alkene dispersion soln, solvent is water, acetone or dimethyl sulfoxide；(500 ~ 1000w ultrasonic power, 600 ~ 800rpm stirs ultrasonic agitation
Mix speed) 80 ~ 100ml graphene dispersion solution, add the graphene quantum dot loading zinc oxide that step (4) is obtained, ultrasonic
Stirring 10 ~ 30min, then moves in the reactor of politef, is incubated 15 ~ 30min at 80 ~ 120 DEG C；Cooling, centrifugation,
Cleaning, dries to obtain antimicrobial composite material.
The invention has the following beneficial effects:
The inventive method, is then surface-treated as the carrier of nano zine oxide using the graphene quantum dot after laser irradiation,
Finally it is attached on porous graphene, can preferably load and fixing nano zine oxide, prevent its reunion, significantly improve nanometer
The stability of zinc oxide, makes nano zine oxide have more efficient antibacterial activity, has broad prospects in industrial applications.
Specific embodiment
With reference to embodiment, the present invention will be described in detail, and embodiment is only the preferred embodiment of the present invention,
It is not limitation of the invention.
Embodiment 1
A kind of porous graphene loads the preparation method of zinc oxide antimicrobial composite material, and it comprises the following steps:
(1) prepare graphene quantum dot suspension: weigh 0.5g c60 powder, measure the dense sulfur that 50ml mass fraction is 98%
Acid, c60 powder and concentrated sulphuric acid is mixed in beaker, beaker is placed in ice-water bath, is stirred with the speed of 500rpm simultaneously, obtains mixed
Close liquid；Weigh 3g potassium permanganate powder, slowly add in above-mentioned mixed liquor；Remove ice-water bath, change water-bath into, keep water-bath
30 ~ 40 DEG C of temperature, reacts 8h；Rapidly join 200ml pure water, filter, the bag filter dialysis 3 being then 1000 with molecular cut off
My god, obtain graphene quantum dot suspension；100rpm speed stirs graphene quantum dot suspension, laser irradiation 30min simultaneously, swashs
Photoirradiation power is 2w.
(2) weigh Zinc oxide quantum dot (particle diameter about 2 ~ 5nm) and be configured to the dispersion liquid that concentration is 0.5mg/ml, solvent is
Water；Ultrasonic agitation (1000w ultrasonic power, 800rpm mixing speed) 80ml zinc oxide fluid dispersion, the stone that Deca step (1) is obtained
Black alkene quantum dot suspension, continues ultrasonic agitation 60min；Centrifugation, cleaning, dry, obtain loading the Graphene quantum of zinc oxide
Point.
(3) surface treatment of the graphene quantum dot of load zinc oxide: 0.005g graphite oxide is added to the dispersion of 8ml
In agent (dmso), ultrasonic agitation (500w ultrasonic power, 300rpm mixing speed) simultaneously adds 0.2g to load the Graphene of zinc oxide
Quantum dot, continues ultrasonic agitation 20min, moves in the microwave hydrothermal reaction kettle (50 ml) that liner is politef, after sealing
It is placed in microwave assisted hydrothermal synthesis apparatus, microwave power is 200w, at 240 DEG C, react 60min；Cooling, filters, dries to obtain surface
The graphene quantum dot of the load zinc oxide processing.
(4) weigh porous graphene (2 ~ 5 layers, hole size about 3 ~ 6nm) be configured to concentration be 0.8mg/ml Graphene divide
Scattered solution, solvent is water, acetone or dimethyl sulfoxide；Ultrasonic agitation (1000w ultrasonic power, 800rpm mixing speed) 100ml
Graphene dispersion solution, adds the graphene quantum dot loading zinc oxide that step (4) is obtained, ultrasonic agitation 30min, Ran Houyi
To the reactor of politef, it is incubated 30min at 100 DEG C；Cooling, centrifugation, cleaning, dry to obtain antimicrobial composite material.
Embodiment 2
A kind of porous graphene loads the preparation method of zinc oxide antimicrobial composite material, and it comprises the following steps:
(1) prepare graphene quantum dot suspension: weigh 0.7g c60 powder, measure the dense sulfur that 80ml mass fraction is 98%
Acid, c60 powder and concentrated sulphuric acid is mixed in beaker, beaker is placed in ice-water bath, is stirred with the speed of 500rpm simultaneously, obtains mixed
Close liquid；Weigh 2g potassium permanganate powder, slowly add in above-mentioned mixed liquor；Remove ice-water bath, change water-bath into, keep water-bath
30 ~ 40 DEG C of temperature, reacts 6h；Rapidly join 200ml pure water, filter, the bag filter dialysis 3 being then 1000 with molecular cut off
My god, obtain graphene quantum dot suspension；100rpm speed stirs graphene quantum dot suspension, laser irradiation 45min simultaneously, swashs
Photoirradiation power is 1.5w.
(2) weigh Zinc oxide quantum dot (particle diameter about 2 ~ 5nm) and be configured to the dispersion liquid that concentration is 0.8mg/ml, solvent is
Water；Ultrasonic agitation (1000w ultrasonic power, 800rpm mixing speed) 100ml zinc oxide fluid dispersion, Deca step (1) is obtained
Graphene quantum dot suspension, continues ultrasonic agitation 60min；Centrifugation, cleaning, dry, obtain loading the Graphene amount of zinc oxide
Sub- point.
(3) surface treatment of the graphene quantum dot of load zinc oxide: 0.008g graphite oxide is added to dividing of 10ml
In powder (dmso), ultrasonic agitation (500w ultrasonic power, 300rpm mixing speed) simultaneously adds 0.1g to load the graphite of zinc oxide
Alkene quantum dot, continues ultrasonic agitation 20min, moves in the microwave hydrothermal reaction kettle (50 ml) that liner is politef, sealing
After be placed in microwave assisted hydrothermal synthesis apparatus, microwave power be 300w, at 220 DEG C react 60min；Cooling, filters, dries to obtain table
The graphene quantum dot of the load zinc oxide that face is processed.
(4) weigh porous graphene (2 ~ 5 layers, hole size about 3 ~ 6nm) be configured to concentration be 0.5mg/ml Graphene divide
Scattered solution, solvent is water, acetone or dimethyl sulfoxide；Ultrasonic agitation (1000w ultrasonic power, 800rpm mixing speed) 80ml stone
Black alkene dispersion soln, adds the graphene quantum dot loading zinc oxide that step (4) is obtained, ultrasonic agitation 30min, then moves to
In the reactor of politef, it is incubated 30min at 100 DEG C；Cooling, centrifugation, cleaning, dry to obtain antimicrobial composite material.
Embodiment 3
A kind of porous graphene loads the preparation method of zinc oxide antimicrobial composite material, and it comprises the following steps:
(1) prepare graphene quantum dot suspension: weigh 0.8g c60 powder, measure the dense sulfur that 100ml mass fraction is 98%
Acid, c60 powder and concentrated sulphuric acid is mixed in beaker, beaker is placed in ice-water bath, is stirred with the speed of 500rpm simultaneously, obtains mixed
Close liquid；Weigh 1g potassium permanganate powder, slowly add in above-mentioned mixed liquor；Remove ice-water bath, change water-bath into, keep water-bath
30 ~ 40 DEG C of temperature, reacts 5h；Rapidly join 100ml pure water, filter, the bag filter dialysis 3 being then 1000 with molecular cut off
My god, obtain graphene quantum dot suspension；100rpm speed stirs graphene quantum dot suspension, laser irradiation 60min simultaneously, swashs
Photoirradiation power is 1w.
(2) weigh Zinc oxide quantum dot (particle diameter about 2 ~ 5nm) and be configured to the dispersion liquid that concentration is 1mg/ml, solvent is water；
Ultrasonic agitation (1000w ultrasonic power, 800rpm mixing speed) 100ml zinc oxide fluid dispersion, the graphite that Deca step (1) is obtained
Alkene quantum dot suspension, continues ultrasonic agitation 60min；Centrifugation, cleaning, dry, obtain loading the graphene quantum dot of zinc oxide.
(3) surface treatment of the graphene quantum dot of load zinc oxide: 0.01g graphite oxide is added to the dispersion of 5ml
In agent (dmso), ultrasonic agitation (500w ultrasonic power, 300rpm mixing speed) simultaneously adds 0.3g to load the Graphene of zinc oxide
Quantum dot, continues ultrasonic agitation 20min, moves in the microwave hydrothermal reaction kettle (50 ml) that liner is politef, after sealing
It is placed in microwave assisted hydrothermal synthesis apparatus, microwave power is 400w, at 200 DEG C, react 60min；Cooling, filters, dries to obtain surface
The graphene quantum dot of the load zinc oxide processing.
(4) weigh porous graphene (2 ~ 5 layers, hole size about 3 ~ 6nm) be configured to concentration be 0.2mg/ml Graphene divide
Scattered solution, solvent is water, acetone or dimethyl sulfoxide；Ultrasonic agitation (1000w ultrasonic power, 800rpm mixing speed) 100ml
Graphene dispersion solution, adds the graphene quantum dot loading zinc oxide that step (4) is obtained, ultrasonic agitation 30min, Ran Houyi
To the reactor of politef, it is incubated 30min at 100 DEG C；Cooling, centrifugation, cleaning, dry to obtain antimicrobial composite material.
Comparative example 1
A kind of preparation method of porous graphene carried titanium dioxide composite, it comprises the following steps: weighs zinc oxide amount
Sub- point (particle diameter about 2 ~ 5nm) is configured to the dispersion liquid that concentration is 1mg/ml, and solvent is water；Ultrasonic agitation (1000w ultrasonic power,
800rpm mixing speed) 100ml zinc oxide fluid dispersion, Deca 80ml concentration is the porous graphene dispersion soln of 0.2mg/ml,
Ultrasonic agitation 30min, then moves in the reactor of politef, is incubated 30min at 100 DEG C；Cooling, centrifugation, cleaning,
Dry to obtain antimicrobial composite material.
Antimicrobial composite material staphylococcus aureuses, Shewanella and the large intestine bar that each embodiment and comparative example 1 are obtained
Bacterium carries out inhibition zone test, and result is as follows:
Embodiment described above only have expressed embodiments of the present invention, and its description is more concrete and detailed, but can not be therefore
And it is interpreted as the restriction to the scope of the claims of the present invention, as long as the technical side being obtained in the form of equivalent or equivalent transformation
Case, all should fall within the scope and spirit of the invention.
Claims (5)
1. a kind of porous graphene loads the preparation method of zinc oxide antimicrobial composite material, and it comprises the following steps:
(1) weigh Zinc oxide quantum dot and be configured to the dispersion liquid that concentration is 0.5 ~ 1mg/ml, solvent is water；Ultrasonic agitation 80 ~
100ml zinc oxide fluid dispersion, Deca graphene quantum dot suspension, continues ultrasonic agitation 30 ~ 60min；Centrifugation, cleaning, dry,
Obtain loading the graphene quantum dot of zinc oxide；
(2) surface treatment of the graphene quantum dot of load zinc oxide；
(3) weigh porous graphene be configured to concentration be 0.2 ~ 0.8mg/ml graphene dispersion solution, solvent be water, acetone or
Dimethyl sulfoxide；Ultrasonic agitation 80 ~ 100ml graphene dispersion solution, adds the Graphene loading zinc oxide that step (2) is obtained
Quantum dot, ultrasonic agitation 10 ~ 30min, then move in the reactor of politef, at 80 ~ 120 DEG C insulation 15 ~
30min；Cooling, centrifugation, cleaning, dry to obtain antimicrobial composite material.
2. porous graphene according to claim 1 loads the preparation method of zinc oxide antimicrobial composite material, and its feature exists
In described graphene quantum dot suspension manufacturing methods are as follows: weigh 0.5 ~ 0.8g c60 powder, measure 50 ~ 100ml mass and divide
The concentrated sulphuric acids for 98% for the number, c60 powder and concentrated sulphuric acid are mixed in beaker, beaker is placed in ice-water bath, simultaneously with 300 ~
The speed stirring of 500rpm, obtains mixed liquor；Weigh 0.5 ~ 3g potassium permanganate powder, slowly add in above-mentioned mixed liquor；Remove
Ice-water bath, changes water-bath into, keeps 30 ~ 40 DEG C of bath temperature, reacts 5 ~ 8h；Rapidly join 100 ~ 200ml pure water, filter, then
Dialysed 3 days with the bag filter that molecular cut off is 1000, obtain graphene quantum dot suspension；100rpm speed stirs Graphene amount
Son point suspension, laser irradiation 30 ~ 60min simultaneously, laser irradiation power is 1 ~ 2w.
3. porous graphene according to claim 1 loads the preparation method of zinc oxide antimicrobial composite material, and its feature exists
In the surface treatment of the graphene quantum dot of described load zinc oxide: 0.005 ~ 0.01g graphite oxide is added to 5 ~ 10ml's
In dispersant, ultrasonic agitation simultaneously adds 0.1 ~ 0.3g to load the graphene quantum dot of zinc oxide, continues ultrasonic agitation 10 ~ 30min,
Move in the microwave hydrothermal reaction kettle that liner is politef, be placed in after sealing in microwave assisted hydrothermal synthesis apparatus, microwave work(
Rate is 200 ~ 400w, reacts 60 ~ 90min at 200 ~ 240 DEG C；Cooling, filters, and dries the stone of the load zinc oxide that must be surface-treated
Black alkene quantum dot.
4. porous graphene according to claim 1 loads the preparation method of zinc oxide antimicrobial composite material, and its feature exists
In described porous graphene is 2 ~ 5 layers, the porous graphene of hole size about 3 ~ 6nm.
5. a kind of porous graphene load zinc oxide antimicrobial composite material is it is characterised in that arbitrary described by Claims 1-4
Preparation method be obtained.
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Cited By (7)
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| CN107006516A (en) * | 2017-04-14 | 2017-08-04 | 南通强生石墨烯科技有限公司 | Graphene antibiosis liquid and preparation method thereof |
| CN107372600A (en) * | 2017-08-10 | 2017-11-24 | 陕西科技大学 | Optical driving type nano antibacterial agent and preparation method thereof |
| CN108219221A (en) * | 2017-12-23 | 2018-06-29 | 广州双乳胶制品有限公司 | A kind of high isolation, the sheath and preparation method thereof of high heat conduction |
| CN109077062A (en) * | 2018-08-09 | 2018-12-25 | 陕西科技大学 | A kind of preparation method of modified MMT/ZnO/GQDs composite nano germicide |
| CN110204787A (en) * | 2019-06-06 | 2019-09-06 | 江苏通用科技股份有限公司 | A method of zinc oxide is loaded in surface of graphene oxide |
| CN112795108A (en) * | 2021-02-09 | 2021-05-14 | 上海光研化学技术有限公司 | Quantum dot diffusion plate |
| CN114054011A (en) * | 2021-11-08 | 2022-02-18 | 惠州市银嘉环保科技有限公司 | Six-component columnar zinc oxide graphene piezoelectric photocatalytic material and preparation method and application thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107006516A (en) * | 2017-04-14 | 2017-08-04 | 南通强生石墨烯科技有限公司 | Graphene antibiosis liquid and preparation method thereof |
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| CN107372600A (en) * | 2017-08-10 | 2017-11-24 | 陕西科技大学 | Optical driving type nano antibacterial agent and preparation method thereof |
| CN107372600B (en) * | 2017-08-10 | 2019-12-17 | 陕西科技大学 | light-driven nano antibacterial agent and preparation method thereof |
| CN108219221A (en) * | 2017-12-23 | 2018-06-29 | 广州双乳胶制品有限公司 | A kind of high isolation, the sheath and preparation method thereof of high heat conduction |
| CN109077062A (en) * | 2018-08-09 | 2018-12-25 | 陕西科技大学 | A kind of preparation method of modified MMT/ZnO/GQDs composite nano germicide |
| CN109077062B (en) * | 2018-08-09 | 2021-05-18 | 陕西科技大学 | Preparation method of modified MMT/ZnO/GQDs nano composite antibacterial agent |
| CN110204787A (en) * | 2019-06-06 | 2019-09-06 | 江苏通用科技股份有限公司 | A method of zinc oxide is loaded in surface of graphene oxide |
| CN112795108A (en) * | 2021-02-09 | 2021-05-14 | 上海光研化学技术有限公司 | Quantum dot diffusion plate |
| CN114054011A (en) * | 2021-11-08 | 2022-02-18 | 惠州市银嘉环保科技有限公司 | Six-component columnar zinc oxide graphene piezoelectric photocatalytic material and preparation method and application thereof |
| CN114054011B (en) * | 2021-11-08 | 2024-01-02 | 惠州市银嘉环保科技有限公司 | Six-component columnar zinc oxide graphene piezoelectric photocatalytic material and preparation method and application thereof |
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Application publication date: 20170201 |