CN110477012B - GO-PEG/Ag-SD composite material and preparation method and application thereof - Google Patents
GO-PEG/Ag-SD composite material and preparation method and application thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title abstract description 9
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 46
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 39
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 37
- SEEPANYCNGTZFQ-UHFFFAOYSA-N sulfadiazine Chemical compound C1=CC(N)=CC=C1S(=O)(=O)NC1=NC=CC=N1 SEEPANYCNGTZFQ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000000243 solution Substances 0.000 claims abstract description 26
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 22
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229960004306 sulfadiazine Drugs 0.000 claims abstract description 20
- 239000006185 dispersion Substances 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 16
- 239000002243 precursor Substances 0.000 claims abstract description 12
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000013329 compounding Methods 0.000 claims abstract description 7
- 239000007864 aqueous solution Substances 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims abstract description 4
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000001509 sodium citrate Substances 0.000 claims abstract description 4
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims abstract description 4
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims description 12
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- 238000000034 method Methods 0.000 claims description 9
- 238000009777 vacuum freeze-drying Methods 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 5
- 238000000502 dialysis Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 4
- 239000002105 nanoparticle Substances 0.000 claims description 4
- 239000004599 antimicrobial Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 31
- 239000000463 material Substances 0.000 abstract description 17
- 230000001954 sterilising effect Effects 0.000 abstract description 6
- 238000004659 sterilization and disinfection Methods 0.000 abstract description 6
- 230000008901 benefit Effects 0.000 abstract description 5
- 239000003242 anti bacterial agent Substances 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 229960003600 silver sulfadiazine Drugs 0.000 description 7
- 241000894006 Bacteria Species 0.000 description 5
- 241000588724 Escherichia coli Species 0.000 description 5
- 241000191967 Staphylococcus aureus Species 0.000 description 5
- 230000002195 synergetic effect Effects 0.000 description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
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- 206010059866 Drug resistance Diseases 0.000 description 1
- 206010039509 Scab Diseases 0.000 description 1
- 206010053615 Thermal burn Diseases 0.000 description 1
- 206010052428 Wound Diseases 0.000 description 1
- 206010048038 Wound infection Diseases 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
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- 230000008022 sublimation Effects 0.000 description 1
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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
- A01N25/10—Macromolecular 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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/48—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
- A01N43/54—1,3-Diazines; Hydrogenated 1,3-diazines
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Abstract
The invention belongs to the technical field of nano antibacterial materials, and discloses a GO-PEG/Ag-SD composite material, and a preparation method and application thereof. (1) Mixing the aqueous dispersion of the PEGylated graphene oxide with the aqueous solution of silver nitrate under stirring, and then adding the mixture while stirringAlkali liquor, sodium citrate or hydrazine hydrate till the pH of the system is 8-14 to obtain GO-PEG/AgNO3Compounding a precursor solution; (2) GO-PEG/AgNO3Carrying out hydrothermal reaction on the composite precursor solution for 1-2 min under the condition of microwave power of 200-400 w, washing, drying, and adding water to dissolve to obtain a GO-PEG/Ag water dispersion; (3) stirring and mixing the GO-PEG/Ag water dispersion and a sulfadiazine DMSO solution for 12-16 h, and dialyzing for 3 days to obtain the GO-PEG/Ag-SD composite material. The GO-PEG/Ag-SD composite material has large specific surface area, has the characteristics of strong sterilization capability and obvious sterilization effect when being used as an antibacterial agent, is easy to regenerate and recycle, has good economic benefit and environmental benefit, and is suitable for popularization and use.
Description
Technical Field
The invention belongs to the technical field of nano antibacterial materials, and particularly relates to a GO-PEG/Ag-SD composite material and a preparation method and application thereof.
Background
In hospitals, food preparation plants, pharmaceutical processing plants and other places with strict hygiene requirements and household articles with high use frequency, such as furniture, household appliances, fabrics and the like, need to be subjected to antibacterial treatment, but in recent years, due to abuse of antibacterial drugs, the drug resistance of bacteria is gradually improved and gradually threatens the health of people, so that research and development of novel efficient antibacterial materials are very important. At present, antibacterial materials can be classified into inorganic antibacterial materials, natural polymer antibacterial materials and artificially synthesized polymer antibacterial materials, and with the development of science and technology, inorganic nano antibacterial materials are concerned by researchers due to their high-efficiency antibacterial performance. The research and development of antibacterial materials with inorganic materials-high molecular materials cooperating with antibacterial materials become a hot problem of the current research.
Graphene (Graphene), the first time stabilized Graphene was obtained by micromechanical cleaving in 2004 by Geim et al, manchester university, uk. Graphene is receiving attention of researchers due to its excellent physicochemical properties, and exhibits great potential in the biological field due to its high specific surface area, excellent biocompatibility and abundant surface functional groups.
In the prior art, some applications of graphene in antibacterial aspect have been reported. For example, the antibacterial performance of graphene-based materials is reported in the united states of america "american chemical society — nanomaterials" (ACS-Nano, 2011, volume 5, page 6971), which reveals a great potential of graphene materials in terms of antibacterial.
In addition, silver is used as an old and effective inorganic antibacterial material, has a synergistic antibacterial effect with sulfadiazine, and is widely applied to treatment of burn and scald wound infection in clinical aspects, and can promote wound drying, scabbing and healing besides infection control.
Disclosure of Invention
The invention aims to provide a GO-PEG/Ag-SD composite material and a preparation method and application thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the GO-PEG/Ag-SD composite material is composed of PEG graphene oxide and silver nanoparticles and sulfadiazine nanoparticles loaded on the surface of the PEG graphene oxide.
The preparation method comprises the following steps:
(1) according to the mass ratio, according to the PEG graphene oxide and silver nitrate = 1: (34-68), stirring and mixing the PEG graphene oxide water dispersion liquid and a silver nitrate water solution, and then adding alkali liquor, sodium citrate or hydrazine hydrate while stirring until the pH value of the system is 8-14 to obtain GO-PEG/AgNO3Compounding a precursor solution;
(2) GO-PEG/AgNO3Carrying out hydrothermal reaction on the composite precursor solution for 1-2 min under the condition of microwave power of 200-400 w, washing, drying, and adding water to dissolve to obtain a GO-PEG/Ag water dispersion;
(3) according to the mass ratio of GO-PEG/Ag to sulfadiazine =1 to (0.5-2), stirring and mixing the GO-PEG/Ag water dispersion with the DMSO solution of sulfadiazine for 12-16 h, and dialyzing for 3 days to obtain the GO-PEG/Ag-SD composite material.
Preferably, in the step (1), the concentration of the aqueous dispersion of PEGylated graphene oxide is 0.2-0.5 mg/mL, and the concentration of the silver nitrate aqueous solution is 1-5 mmol/mL.
Preferably, in the step (1), the alkali liquor is sodium hydroxide solution, and after the pH of the system is adjusted to 8-14, the mixture is continuously stirred for 30-60 min to obtain GO-PEG/AgNO3And compounding the precursor solution.
Preferably, in the step (2), the drying is vacuum freeze drying; the vacuum freeze drying is to freeze in vacuum for 30-60 min under the conditions of-20 to-40 ℃, and then to dry for 3-4 h after the temperature is raised to 40-60 ℃.
Preferably, in the step (1) and the step (3), the stirring speed is 300-600 rpm.
Preferably, in the step (3), the concentration of the GO-PEG/Ag aqueous dispersion is 0.5-2 mg/mL, and the concentration of the sulfadiazine DMSO solution is 100-300 mg/mL.
Preferably, in the step (3), a dialysis bag with the molecular weight cutoff of 4000-8000 is adopted during dialysis.
The GO-PEG/Ag-SD composite material is applied as an antibacterial agent.
In the invention, the PEGylated graphene oxide (GO-PEG) is prepared according to the prior art, and specifically comprises the following steps: firstly, graphene oxide is prepared by a Hummers method or an improved Hummers method, then the graphene oxide is carboxylated (Carbon, vol.117 page 301 of 2017), and finally PEG is grafted on the carboxylated graphene oxide (ACS Appl Mater Interfaces, vol.5 page 6909 of 2013), so that the PEG graphene oxide is obtained.
The GO-PEG/Ag-SD composite material is a composite material prepared by simultaneously modifying nano silver, sulfadiazine and graphene oxide, modifying graphene oxide, improving the suspension performance of graphene oxide in aqueous solution, generating silver nanoparticles on a graphene oxide sheet layer by adopting a microwave hydrothermal method, connecting abundant functional groups on the surface of graphene oxide with sulfadiazine in the form of intermolecular force, effectively and firmly combining the silver nanoparticles, sulfadiazine and the surface of PEG graphene oxide, fully playing the excellent performances of nano ions, high-molecular drugs and graphene oxide, and realizing the synergistic effect of the three components, so that the large specific surface area can be maintained, but also can effectively prevent the aggregation of silver nano particles and play a role in the synergetic antibacterial effect of the high-molecular antibacterial material and the inorganic antibacterial material.
Has the advantages that: the GO-PEG/Ag-SD composite material has large specific surface area, has the characteristics of strong sterilization capability and obvious sterilization effect when being used as an antibacterial agent, is easy to regenerate and recycle, has good economic benefit and environmental benefit, and is suitable for popularization and use.
Drawings
FIG. 1: SEM images of GO-PEG/Ag obtained by different hydrothermal reaction times.
FIG. 2: TEM image of GO-PEG/Ag obtained by 200W hydrothermal reaction for 1 min.
FIG. 3: an XRD pattern of GO-PEG/Ag obtained by hydrothermal reaction at 200W for 1 min.
FIG. 4: carrying out 200W hydrothermal reaction for 1 min, and obtaining the medicine-loading rate and encapsulation rate of the GO-PEG/Ag-SD composite material with different GO-PEG/Ag/SD mass ratios.
FIG. 5: FT-IR diagram of GO-PEG/Ag-SD composite material obtained by 200W hydrothermal reaction for 1 min and GO-PEG/Ag/SD mass ratio = 1: 2.
FIG. 6: the antibacterial performance results of GO-PEG/Ag-SD, GO-PEG/Ag and SSD on escherichia coli.
FIG. 7: the antibacterial performance results of GO-PEG/Ag-SD, GO-PEG/Ag and SSD on staphylococcus aureus.
Detailed Description
The technical solution of the present invention is further described in detail with reference to the following specific examples, but the scope of the present invention is not limited thereto.
Example 1
A preparation method of a GO-PEG/Ag-SD composite material comprises the following preparation steps:
(1) preparing PEGylated graphene oxide (GO-PEG);
(2) in terms of the mass ratio, according to the PEGylated graphite oxideAlkene/silver nitrate = 1: 34, aqueous dispersion (0.2 mg/mL) of PEGylated graphene oxide and aqueous solution (1 mmol/mL) of silver nitrate are stirred and mixed, then sodium hydroxide solution with the concentration of 1 mol/L is dripped into the mixture while stirring until the pH value of the system is 10, and the mixture is continuously stirred for 30 min to obtain GO-PEG/AgNO3Compounding a precursor solution;
(3) GO-PEG/AgNO3Carrying out hydrothermal reaction on the composite precursor solution for 1 min or 2 min under the condition of microwave power of 200 w respectively, then washing, carrying out vacuum freeze drying to obtain GO-PEG/Ag (PEG oxidized graphene loaded silver nanoparticle composite material), and adding water to dissolve the GO-PEG/Ag to obtain a GO-PEG/Ag water dispersion;
(4) according to the mass ratio, respectively stirring and mixing 1 mg/mL aqueous dispersion of GO-PEG/Ag and 200 mg/mL DMSO solution of sulfadiazine for 16 h according to the ratio of GO-PEG/Ag to SD (sulfadiazine) = 1: 0.5, 1: 1, 1: 2 and 1: 4, and dialyzing for 3 days by a dialysis bag with the cut-off molecular weight of 4000 to obtain the GO-PEG/Ag-SD composite material;
wherein in the step (2) and the step (4), the stirring speed is 300 rpm; in the step (3), the vacuum freeze drying is to freeze in vacuum for 30 min at the temperature of minus 20 ℃, then heat to 40 ℃ and dry for 4 h, and the drying process is completed through sublimation of ice.
SEM images of GO-PEG/Ag obtained in this example at different hydrothermal reaction times are shown in FIG. 1 (a-200W hydrothermal reaction for 2 min, b-200W hydrothermal reaction for 1 min). Therefore, the following steps are carried out: carrying out 200W hydrothermal reaction for 2 min, wherein the silver nanoparticles are about 25 nm; carrying out 200W hydrothermal reaction for 1 min, wherein the silver nanoparticles are about 8 nm; the particle size of the silver nanoparticles can be regulated and controlled by controlling the hydrothermal reaction time; the silver nanoparticles with fine particles and uniform size prepared by the embodiment are uniformly loaded on the surface of the graphene oxide, so that the agglomeration of the silver nanoparticles is effectively prevented, and meanwhile, the composite material has a large comparative area and has a large application potential as an antibacterial material.
The TEM image and the XRD image of GO-PEG/Ag obtained by the 200W hydrothermal reaction for 1 min in the embodiment are respectively shown in FIG. 2 and FIG. 3. And (3) confirming that: the well-crystallized silver nanoparticles are indeed loaded on the graphene oxide.
The drug loading and encapsulation efficiency of the GO-PEG/Ag-SD composite material obtained by the 200W hydrothermal reaction for 1 min and different GO-PEG/Ag/SD mass ratios in the embodiment are shown in FIG. 4. Therefore, the following steps are carried out: SD = 1: 2/GO-PEG/Ag, sulfadiazine has reached maximum drug loading.
In this example, FT-IR chart of GO-PEG/Ag-SD composite material obtained by hydrothermal reaction of 200W for 1 min and GO-PEG/Ag: SD mass ratio = 1: 2 is shown in FIG. 5. Therefore, the following steps are carried out: sulfadiazine is successfully loaded on the surface of GO-PEG/Ag, and the GO-PEG/Ag-SD composite material is successfully prepared.
Antibacterial experiments
The antibacterial performance of the GO-PEG/Ag-SD composite material obtained by the hydrothermal reaction of 200W for 1 min and the mass ratio of GO-PEG/Ag to SD = 1: 2 in the embodiment on Escherichia coli and staphylococcus aureus is tested by a 96-well plate method, and GO-PEG/Ag and Silver Sulfadiazine (SSD) are set as a control group. Adding 100 mu L of physiological saline into each hole, then adding 100 mu L of 100 mu g/mL GO-PEG/Ag-SD composite material into the initial hole, adopting a two-fold dilution method, wherein the antibacterial concentration of GO-PEG/Ag-SD is 50, 25, 12.5, 6.25, 3.125, 1.56 and 0.78 mu g/mL in sequence, and a pure bacteria hole (100 mu L of pure bacteria is arranged in each hole), the concentration of bacteria liquid is 105cfu/mL. Three sets of replicates were performed for each experimental condition.
The antibacterial performance results of GO-PEG/Ag-SD, GO-PEG/Ag and SSD on Escherichia coli and Staphylococcus aureus are shown in the figure 6 and the figure 7 respectively. The test result shows that: the antibacterial performance of GO-PEG/Ag-SD on escherichia coli is obviously superior to that of GO-PEG/Ag and SSD, and GO-PEG, Ag and SD show excellent synergistic antibacterial performance; the antibacterial property of GO-PEG/Ag-SD on staphylococcus aureus is almost the same as that of GO-PEG/Ag, but is obviously higher than that of SSD, and the GO-PEG/Ag-SD antibacterial agent does not show an excellent synergistic antibacterial effect.
Sterilization test
50 μ g/mL and 25 μ g/mL (100 μ L) of aqueous solution of GO-PEG/Ag-SD composite material obtained by hydrothermal reaction of 200W in the embodiment for 1 min and with GO-PEG/Ag: SD mass ratio = 1: 2 were acted on the GO-PEG/Ag-SD composite material with concentration of 105cfu/mL of Escherichia coli and Staphylococcus aureus (100. mu.L) was allowed to act for 1 hour, and Hoechst and PI staining were performed on them, followed by observation under a fluorescence microscope.The experimental results show that: the bacteria are basically killed within 1 hour, and the sterilization rate can reach 100 percent.
Claims (9)
1. A GO-PEG/Ag-SD composite material is characterized in that: the composite material consists of PEG-oxidized graphene, silver nanoparticles and sulfadiazine nanoparticles, wherein the silver nanoparticles and the sulfadiazine nanoparticles are loaded on the surface of the PEG-oxidized graphene; the composite material is prepared by the following steps:
(1) according to the mass ratio, according to the PEG graphene oxide and silver nitrate = 1: (34-68), stirring and mixing the PEG graphene oxide water dispersion liquid and a silver nitrate water solution, and then adding alkali liquor, sodium citrate or hydrazine hydrate while stirring until the pH value of the system is 8-14 to obtain GO-PEG/AgNO3Compounding a precursor solution;
(2) GO-PEG/AgNO3Carrying out hydrothermal reaction on the composite precursor solution for 1-2 min under the condition of microwave power of 200-400 w, washing, drying, and adding water to dissolve to obtain a GO-PEG/Ag water dispersion;
(3) according to the mass ratio of GO-PEG/Ag to sulfadiazine = 1: 2, stirring and mixing the GO-PEG/Ag water dispersion and the DMSO solution of sulfadiazine for 12-16 h, and dialyzing for 3 days to obtain the GO-PEG/Ag-SD composite material.
2. A method of making the GO-PEG/Ag-SD composite of claim 1, comprising the steps of:
(1) according to the mass ratio, according to the PEG graphene oxide and silver nitrate = 1: (34-68), stirring and mixing the PEG graphene oxide water dispersion liquid and a silver nitrate water solution, and then adding alkali liquor, sodium citrate or hydrazine hydrate while stirring until the pH value of the system is 8-14 to obtain GO-PEG/AgNO3Compounding a precursor solution;
(2) GO-PEG/AgNO3Carrying out hydrothermal reaction on the composite precursor solution for 1-2 min under the condition of microwave power of 200-400 w, washing, drying, and adding water to dissolve to obtain a GO-PEG/Ag water dispersion;
(3) according to the mass ratio of GO-PEG/Ag to sulfadiazine = 1: 2, stirring and mixing the GO-PEG/Ag water dispersion and the DMSO solution of sulfadiazine for 12-16 h, and dialyzing for 3 days to obtain the GO-PEG/Ag-SD composite material.
3. The method of preparing a GO-PEG/Ag-SD composite of claim 2, wherein: in the step (1), the concentration of the PEG graphene oxide aqueous dispersion is 0.2-0.5 mg/mL, and the concentration of the silver nitrate aqueous solution is 1-5 mmol/mL.
4. The method of preparing a GO-PEG/Ag-SD composite of claim 2, wherein: in the step (1), the alkali liquor is a sodium hydroxide solution, and after the pH of the system is adjusted to be 8-14, the mixture is continuously stirred for 30-60 min to obtain GO-PEG/AgNO3And compounding the precursor solution.
5. The method of preparing a GO-PEG/Ag-SD composite of claim 2, wherein: in the step (2), the drying is vacuum freeze drying; the vacuum freeze drying is to freeze in vacuum for 30-60 min under the conditions of-20 to-40 ℃, and then to dry for 3-4 h after the temperature is raised to 40-60 ℃.
6. The method of preparing a GO-PEG/Ag-SD composite of claim 2, wherein: in the step (1) and the step (3), the stirring speed is 300-600 rpm.
7. The method of preparing a GO-PEG/Ag-SD composite of claim 2, wherein: in the step (3), the concentration of the GO-PEG/Ag water dispersion is 0.5-2 mg/mL, and the concentration of the sulfadiazine DMSO solution is 100-300 mg/mL.
8. The method of preparing a GO-PEG/Ag-SD composite of claim 2, wherein: in the step (3), a dialysis bag with the molecular weight cutoff of 4000-8000 is adopted during dialysis.
9. Use of the GO-PEG/Ag-SD composite of claim 1 as an antimicrobial agent.
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Citations (14)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US8709394B2 (en) * | 2007-09-28 | 2014-04-29 | Ndsu Research Foundation | Antimicrobial polysiloxane materials containing metal species |
CN104027807A (en) * | 2014-06-04 | 2014-09-10 | 上海师范大学 | Graphene oxide/copper selenide/PEG (Polyethylene Glycol) nanocomposite material, as well as preparation method and application thereof |
CN104472538A (en) * | 2014-11-24 | 2015-04-01 | 暨南大学 | Functional graphene oxide loaded nano-silver antibacterial material as well as preparation method and application thereof |
CN104839210A (en) * | 2015-03-24 | 2015-08-19 | 浙江工商大学 | Preparation method and application for magnetic-nanosilver-graphene nano composite material l |
WO2015142938A1 (en) * | 2014-03-17 | 2015-09-24 | Washington University | Composite nanostructures having a crumpled graphene oxide shell |
CN104971358A (en) * | 2015-04-19 | 2015-10-14 | 奉化市宇创产品设计有限公司 | Functionalized graphene oxide supported nano-silver preparation method |
US9334386B2 (en) * | 2013-09-04 | 2016-05-10 | Alfaisal University | Antimicrobial polymer-graphene-silver nanocomposite |
US9480260B2 (en) * | 2008-12-16 | 2016-11-01 | The Board Of Regents Of The University Of Texas System | Acrylic polymers containing metallic nanoparticles |
CN106312089A (en) * | 2016-08-26 | 2017-01-11 | 太原理工大学 | Preparation method of carbon nanoscroll/nano-silver composite antibacterial material |
CN106391002A (en) * | 2015-08-03 | 2017-02-15 | 北京化工大学 | Nanosilver/graphene oxide composite dispersion fluid, and preparation method and application thereof |
CN106832844A (en) * | 2017-02-10 | 2017-06-13 | 四川大学 | Four arm PEG PCL of one kind, graphene oxide composite material and preparation method thereof |
CN107761081A (en) * | 2017-09-27 | 2018-03-06 | 郴州博太超细石墨股份有限公司 | A kind of graphene/silver composite material of high-compactness and preparation method thereof |
CN108782607A (en) * | 2018-05-17 | 2018-11-13 | 天津宝兴威科技股份有限公司 | A kind of preparation method of graphene/silver nano antibacterial composite material |
CN109400960A (en) * | 2018-08-28 | 2019-03-01 | 江苏理工学院 | A kind of graphene/nano silver polymer composites and preparation method thereof |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106000297B (en) * | 2016-05-10 | 2019-02-05 | 郑州大学 | A kind of graphene-supported zirconium oxide composite material, preparation method and its application as desulfuration adsorbent |
-
2019
- 2019-08-22 CN CN201910780264.6A patent/CN110477012B/en not_active Expired - Fee Related
Patent Citations (14)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US8709394B2 (en) * | 2007-09-28 | 2014-04-29 | Ndsu Research Foundation | Antimicrobial polysiloxane materials containing metal species |
US9480260B2 (en) * | 2008-12-16 | 2016-11-01 | The Board Of Regents Of The University Of Texas System | Acrylic polymers containing metallic nanoparticles |
US9334386B2 (en) * | 2013-09-04 | 2016-05-10 | Alfaisal University | Antimicrobial polymer-graphene-silver nanocomposite |
WO2015142938A1 (en) * | 2014-03-17 | 2015-09-24 | Washington University | Composite nanostructures having a crumpled graphene oxide shell |
CN104027807A (en) * | 2014-06-04 | 2014-09-10 | 上海师范大学 | Graphene oxide/copper selenide/PEG (Polyethylene Glycol) nanocomposite material, as well as preparation method and application thereof |
CN104472538A (en) * | 2014-11-24 | 2015-04-01 | 暨南大学 | Functional graphene oxide loaded nano-silver antibacterial material as well as preparation method and application thereof |
CN104839210A (en) * | 2015-03-24 | 2015-08-19 | 浙江工商大学 | Preparation method and application for magnetic-nanosilver-graphene nano composite material l |
CN104971358A (en) * | 2015-04-19 | 2015-10-14 | 奉化市宇创产品设计有限公司 | Functionalized graphene oxide supported nano-silver preparation method |
CN106391002A (en) * | 2015-08-03 | 2017-02-15 | 北京化工大学 | Nanosilver/graphene oxide composite dispersion fluid, and preparation method and application thereof |
CN106312089A (en) * | 2016-08-26 | 2017-01-11 | 太原理工大学 | Preparation method of carbon nanoscroll/nano-silver composite antibacterial material |
CN106832844A (en) * | 2017-02-10 | 2017-06-13 | 四川大学 | Four arm PEG PCL of one kind, graphene oxide composite material and preparation method thereof |
CN107761081A (en) * | 2017-09-27 | 2018-03-06 | 郴州博太超细石墨股份有限公司 | A kind of graphene/silver composite material of high-compactness and preparation method thereof |
CN108782607A (en) * | 2018-05-17 | 2018-11-13 | 天津宝兴威科技股份有限公司 | A kind of preparation method of graphene/silver nano antibacterial composite material |
CN109400960A (en) * | 2018-08-28 | 2019-03-01 | 江苏理工学院 | A kind of graphene/nano silver polymer composites and preparation method thereof |
Non-Patent Citations (7)
Title |
---|
Galvanic displacement-induced codeposition of reduced-graphene-oxide/silver on alloy fibers for non-destructive SPME@SERS analysis of antibioticsSPME@SERS analysis of antibiotics;Jingcheng Cui et al;《Microchimica Acta》;20181214;第186卷;第19页 * |
PEG化氧化石墨烯/高分子复合膜的结构和性能;钱彭华;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20190715(第7期);第B020-441页 * |
氧化石墨烯PEG化后对L929细胞毒性的影响;徐宏杨等;《华西药学杂志》;20150815;第30卷(第4期);第425-427页 * |
氧化石墨烯纳米银复合材料的制备及其抗菌性;秦静等;《环境化学》;20160315;第35卷(第3期);第445-450页 * |
磁性氧化石墨烯/壳聚糖制备及其对磺胺嘧啶吸附性能研究;丁杰等;《环境科学学报》;20161031;第36卷(第10期);第3691-3700页 * |
纳米抗菌材料及石墨烯复合抗菌材料的研究进展;王秀平等;《河北科技师范学院学报》;20161231;第30卷(第4期);第71-77、84页 * |
纳米银-氧化石墨烯复合材料抗菌性能研究进展;钟涛等;《材料导报》;20140531;第28卷;第64-66、71页 * |
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