CN113173575A - Copper nanoparticle/fullerol nanocomposite and preparation method and application thereof - Google Patents
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Abstract
The invention discloses a copper nanoparticle/fullerol nanocomposite and a preparation method and application thereof, belonging to the technical field of nanomaterials. According to the preparation method, fullerene is used as a matrix, the fullerene is subjected to hydroxylation modification to obtain fullerol, copper ions in copper chloride are reduced into copper nanoparticles through laser photoreduction, and the copper nanoparticles are stably loaded on the surface of the fullerol, so that the copper nanoparticle/fullerol composite material is prepared. The method is simple and efficient, the obtained copper nanoparticle/fullerol composite material is small in particle size and uniform in distribution, can be better applied to the anti-oxidation field, solves the problem that a single fullerene derivative is not strong in anti-oxidation performance, and has a better application prospect.
Description
Technical Field
The invention relates to a copper nanoparticle/fullerol nanocomposite and a preparation method and application thereof, belonging to the technical field of nanomaterials.
Background
In the daily metabolism of people, Reactive Oxygen Species (ROS) are continuously generated, and the excessive existence of the ROS can cause the accelerated aging and the remarkable increase of heart-brain system diseases. Therefore, it is desirable to find a material having good oxidation resistance, so that ROS can be inhibited from slowing down aging.
Fullerene is a hollow molecule composed entirely of carbon, is a unique allotrope among many carbon nanomaterials, and has good photoactivity and chemical reactivity. Based on the special p-pi conjugated structure, fullerene can absorb free radicals through carbon-carbon double bonds, thereby having stronger antioxidant effect. However, fullerene is easy to agglomerate and has strong hydrophobicity, and is only dissolved in limited organic solvents (such as toluene, carbon tetrachloride and the like), thereby severely limiting the application of fullerene in the field of biomedicine. Conventionally, various modification methods such as amination, carboxylation, hydroxylation and the like have been used to provide good water solubility to the resulting fullerene derivative. However, the fullerene derivative has a poor antioxidant effect because the fullerene derivative has a reduced radical absorption effect after functionalization. The copper nanoparticles are widely used as antioxidants in biological systems, and the copper nanoparticles are added to the fullerene water-soluble derivative to form the composite material, so that the composite material has a good synergistic effect in the aspect of oxidation resistance. But the loading and particle size of the copper nanoparticles need to be controlled to reduce the impact of their toxicity on human health.
Therefore, how to prepare copper nanoparticles with small particle size by a simple and effective method and stably coat the copper nanoparticles on the fullerene water-soluble derivative to form the fullerene water-soluble derivative/copper nanoparticle composite material is still a challenge and is one of the key problems for further improving the oxidation resistance of the fullerene water-soluble derivative/copper nanoparticle composite material.
Disclosure of Invention
In order to solve the above problems, the present invention firstly provides a method for preparing a copper nanoparticle/fullerol composite material, the method comprising the steps of:
(1) dispersing fullerene in an organic solvent to prepare fullerene dispersion liquid, and then adding peroxide and tetrabutylammonium hydroxide to carry out solvothermal reaction; after the reaction is finished, standing for layering, collecting a lower-layer liquid phase, then adding a precipitator for solid-liquid separation, collecting solids, and drying to obtain fullerol powder;
(2) and dispersing the obtained fullerol powder and cupric salt in water, uniformly mixing to obtain a mixed solution, then placing under laser for illumination, after illumination is finished, carrying out solid-liquid separation, collecting solids, and drying to obtain the copper nanoparticle/fullerol composite material.
In one embodiment of the present invention, the organic solvent in step (1) is toluene.
In one embodiment of the present invention, the mass-to-volume ratio of the fullerene to the organic solvent in step (1) is (1.5-3): 1 (mg/mL); specifically, 2 can be selected: 1 (mg/mL).
In one embodiment of the present invention, the peroxide in step (1) comprises any one or more of: 30% of hydrogen peroxide, tert-butyl hydroperoxide, dibenzoyl peroxide and potassium permanganate serving as an oxide.
In one embodiment of the invention, the volume ratio of toluene, 30% hydrogen peroxide and tetrabutylammonium hydroxide in step (1) is 100: 20: 1 (mL).
In one embodiment of the present invention, the temperature of the solvothermal reaction in step (1) is in the range of 50 ℃ to 80 ℃; the time is 12-20 h.
In one embodiment of the present invention, the layering in step (1) is an upper transparent liquid phase and a lower dark yellow liquid phase.
In one embodiment of the present invention, the precipitant in step (1) comprises: any one or more of isopropanol, anhydrous ether and n-hexane. When three mixtures are selected, the volume ratio of the isopropanol to the anhydrous ether to the n-hexane is 7: 5: 5.
in one embodiment of the present invention, the solid-liquid separation in step (1) further comprises: after the precipitant is added for separation, the detergent is added for continuous separation, and finally, the solid product is collected.
In one embodiment of the present invention, the detergent in step (1) is anhydrous diethyl ether.
In one embodiment of the present invention, the centrifugation in step (1) is performed at 8000rpm for 8 min.
In one embodiment of the present invention, the drying in step (1) is performed by using a vacuum oven, wherein the vacuum degree is-1 MPa, and the drying temperature is 25 ℃.
In one embodiment of the present invention, the cupric salt in step (2) is selected from: copper chloride, copper chloride dihydrate, copper nitrate hydrate, copper carbonate hydrate, copper sulfate hydrate.
In one embodiment of the present invention, the mass ratio of the fullerol to the cupric salt in the step (2) is 1: 3-1: 4; the preferred mass ratio is 1: 3.3.
In one embodiment of the invention, in the step (2), the mass concentration of the fullerol in the mixed solution is 0.1-0.2 mg/mL; specifically, 0.13mg/mL can be used.
In one embodiment of the present invention, the laser in step (2) has a wavelength of 660nm and an excitation energy of 0.9mW/cm2。
In one embodiment of the present invention, the solid-liquid separation in step (2) is performed by centrifugation at 8000rpm for 6 min.
In one embodiment of the present invention, the drying in step (2) is performed by using a vacuum oven, wherein the vacuum degree is-1 MPa, and the drying temperature is 50 ℃.
In an embodiment of the present invention, the method specifically includes the following processes:
(1) dispersing fullerene into a toluene solvent to form a toluene dispersion liquid, then adding 30% of hydrogen peroxide and tetrabutylammonium hydroxide solution, mixing, stirring and heating;
(2) separating the upper and lower layered mixed liquor obtained in the step (1), taking the lower liquid phase, adding a precipitator and a detergent into the lower liquid phase, centrifuging, decanting and drying to obtain fullerol powder;
(3) preparing the fullerol powder obtained in the step (2) and copper chloride (II) dihydrate into a mixed solution according to a certain proportion, and fully illuminating under laser so as to give certain energy to the mixed solution for carrying out photoelectron conversion to ensure that copper is coated on the surface of the fullerol. Then the copper nano particles/fullerol composite material which ensures that the copper nano particles are better and uniformly coated on the fullerol is obtained by centrifuging, decanting and drying.
The invention also provides a copper nanoparticle/fullerol composite material by utilizing the method.
In one embodiment of the present invention, the particle size of the copper nanoparticle/fullerol composite material is about 2-3 nm.
The invention also provides application of the copper nanoparticle/fullerol composite material in the field of oxidation resistance of non-organic cup diagnosis and treatment.
The invention has the advantages of
According to the invention, the copper nanoparticles can be coated on the surface of the fullerol by a simple means, and the coated copper nanoparticles have a lower particle size and are relatively uniformly distributed. The copper nanoparticle/fullerol composite material prepared by the invention can be applied to the oxidation resistance aspect, and can well adsorb free radicals so as to play a role in oxidation resistance.
Drawings
FIG. 1 shows an infrared spectrum (FT-IR) of Fullerol.
FIG. 2 is a thermogravimetric plot (TGA) of fullerol.
FIG. 3 is an X-ray photoelectron spectroscopy (XPS) plot of a copper nanoparticle/fullerol nanocomposite material, wherein (a) is the XPS plot of the composite material; (b) is Cu 2p XPS spectrum; (c) is a C1 s XPS spectrum; (d) o1 s XPS spectra.
Fig. 4 is an X-ray diffraction (XRD) pattern of fullerol and copper nanoparticle/fullerol composites.
FIG. 5 is a diagram showing particle size analysis, wherein (a) is a fullerol; (b) is a copper nano-particle/fullerol composite material.
Fig. 6 is a Transmission Electron Microscope (TEM) image of the copper nanoparticle/fullerol composite.
Fig. 7 is a particle size distribution histogram of copper nanoparticles counted by TEM.
Fig. 8 is the antioxidant activity of the composite: 2, 2-biphenyl-1-picrylhydrazino (DPPH) inhibition assay.
Fig. 9 is the antioxidant activity of the composite: half Inhibitory Concentration (IC) of DPPH inhibition assay50) Graph is shown.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings. The raw materials mentioned in the invention are not specified in detail and are all commercial products; the process steps or preparation methods not mentioned in detail are all process steps or preparation methods well known to the person skilled in the art.
Example 1 preparation of copper nanoparticle/Fullerol composite
(1) Preparing fullerol:
0.1g of fullerene was dispersed in 50mL of toluene solution, and 10mL of 30% hydrogen peroxide solution and 500. mu.L of tetrabutylammonium hydroxide solution were further added thereto, and stirred in a heated stirrer at 60 ℃ and 400rpm for 16 hours.
After stirring for 16 hours, a supernatant and a lower turbid separated solution were obtained, and the lower turbid solution was separated using a separatory funnel, to which 74.12 mL of isopropanol, 52.94mL of anhydrous ether, and 52.94mL of n-hexane were added. Thereafter, the solution was centrifuged for 8min (8000rpm) to sufficiently separate the fullerol. After decantation, 10mL of anhydrous ether was added to each tube and the above centrifugation-decantation step was repeated two to three times to sufficiently remove impurities. Then the obtained precipitate was dried in a vacuum oven (degree of vacuum: -1 MPa; temperature: 25 ℃ C.).
The infrared spectrum scanning is carried out on the prepared fullerol, and the result is shown in figure 1, so that the spectrum of the prepared fullerol is 3400cm-1A broad O-H band is shown nearby at 1080, 1370 and 1620cm-1Three characteristic bands are shown, which can be designated vC–O，νC–O–HV and vC＝CAbsorbing, thereby further proving that the fullerene is successfully hydroxylated.
Thermogravimetric analysis of the prepared fullerol showed that the prepared fullerol had a loss of bound water at 120 ℃, probably due to hydroxyl group detachment at 120 ℃ to 300 ℃ and probably due to heat loss from the fullerene itself at temperatures >300 ℃, as shown in fig. 2.
(2) Preparing a copper nanoparticle/fullerol composite material:
mixing the obtained fullerol 2mg with copper (II) chloride dihydrate (34.5) of different massmg, 17.5mg, 9.3mg, 6.6 mg) and 15mL of water were put in a glass vial and irradiated with laser light having a wavelength of 660nm (0.9 mW/cm)2) So that the copper oxide obtains corresponding energy to be reduced. Further, it was found that the mixed aqueous solution to which 34.5mg of copper (II) chloride dihydrate was added exhibited a deep blue color and a yellow flocculent precipitate was produced after irradiation with light; adding 17.5mg of mixed solution of copper (II) chloride dihydrate, and generating a light blue colored flocculent precipitate after illumination; adding 9.3mg of mixed solution of copper (II) chloride dihydrate, and after illumination, the mixed solution is light blue and transparent and only trace floccule is separated out; 6.6mg of a mixed solution of copper (II) chloride dihydrate is added, and the mixed solution is transparent and colorless after illumination and almost has no flocculent precipitate; finally, 6.6mg of a mixed aqueous solution of copper (II) chloride dihydrate was selected for use. Then the solution was centrifuged for 6min (8000rpm) to sufficiently separate the copper nanoparticle/fullerol composite, and the obtained precipitate was dried in a vacuum oven (degree of vacuum: -1 MPa; temperature: 50 ℃ C.) to obtain a copper nanoparticle/fullerol composite.
The prepared copper nano-particle/fullerol composite material is subjected to X-ray photoelectron spectroscopy analysis and detection, the result is shown in figure 3, the Cu 2p spectrum shows two peaks at 932.6 and 952.3eV, which are respectively designated as Cu 2p3/2And Cu 2p1/2Showing that Cu2+Is present.
As a result of X-ray diffraction analysis of the copper nanoparticle/fullerol nanocomposite material prepared, as shown in fig. 4, the XRD pattern of fullerol contains diffraction peaks at 2 θ ═ 10.78 °, 17.64 °, 20.74 ° and 21.68 °, corresponding to the planar structures of (111), (022), (113) and (222) in a body-centered cubic, respectively. And the XRD pattern of the copper nanoparticle/fullerol composite shows characteristic peaks and highly crystalline peaks of the copper particles, including diffraction peaks at 2 θ ═ 43.2 °, 50.4 ° and 74.1 °, and corresponding to the planes of the metal cubes located at (111), (200) and (220), respectively.
Both of the above data indicate that copper nanoparticles are indeed present in the composite.
As a result of measuring the particle size of the prepared fullerene-copper nanoparticle/fullerene composite material, as shown in fig. 5(a) and (b), the particle size of the fullerene of the unmodified copper nanoparticle was about 34nm, and the particle size of the composite material coated with the copper nanoparticle was about 37 nm. Indicating that the synthesized coated copper nanoparticles have a smaller particle size.
The Transmission Electron Microscope (TEM) detection of the prepared copper nanoparticle/fullerol composite material showed that the copper nanoparticles are uniformly coated on the surface of the fullerol, as shown in fig. 6. And the lattice spacing obtained by magnified photography of the coated particles was about 0.22nm, further indicating that the coated particles were copper nanoparticles. Meanwhile, as shown in FIG. 7, the particle size of the prepared copper nanoparticles is 2 to 3 nm.
Example 2 Oxidation resistance of copper nanoparticle/Fullerol composites
(1) Selecting copper nano-particle/fullerol composite materials (0.0025mg, 0.005mg, 0.01mg, 0.025mg, 0.05mg, 0.1mg and 0.25mg) with different masses, and adding the copper nano-particle/fullerol composite materials into 1mL of absolute ethyl alcohol to obtain a composite material ethanol solution;
(2) firstly, diluting DPPH in ethanol solution to obtain 0.3mM ethanol solution of DPPH; taking 0.5mL of prepared DPPH ethanol solution into a quartz cuvette, further dropwise adding 0.5mL of ethanol solution to obtain DPPH/ethanol solution, and recording the absorbance of the DPPH/ethanol solution as Ac(ii) a This DPPH/ethanol solution (0.5mL) was then further mixed with 0.5mL of the composite solution of step (1); the mixed solution was incubated in the dark for 30 minutes, and after the incubation, the absorbance was measured at 517nm (A)s). The absorbance of the ethanol solution of the composite sample without DPPH was also measured in the same manner (A)b)；
(3) And (2) passing the corresponding parameters obtained in the step (1) through the following formula: percent inhibition of DPPH ═ 1- (A)s–Ab)/Ac]X 100%, and taking the average value by parallel measurement for three times to obtain the DPPH inhibition degree. Specific results are shown in table 1.
Fig. 8 is the antioxidant activity of the copper nanoparticle/fullerol composite: DPPH inhibition assay graph DPPH inhibition degree is 45.43% at a sample concentration of about 0.01 mg/mL; at a concentration of about 0.025mg/mL, the DPPH inhibition was 76.39%; at a concentration of about 0.05mg/mL, the DPPH inhibition was 85.86%; at a concentration of about 0.1mg/mL, the DPPH inhibition degree is 96.25%; at a concentration of about 0.25mg/mL, the DPPH inhibition was 99.05%.
Fig. 9 is the antioxidant activity of the copper nanoparticle/fullerol composite: half Inhibitory Concentration (IC) of DPPH inhibition assay50) The curve chart shows the equation of the half inhibition concentration curve as follows: y 2975.01x +6.63 (R)20.95). The half inhibitory concentration was about 0.0145 mg/mL.
TABLE 1 DPPH Activity inhibition with different masses of copper nanoparticle/Fullerol composites
Example 3
Referring to example 1, the mass ratio of the fullerol to the cupric salt was changed, and the other conditions were not changed, to obtain the corresponding composite material.
The oxidation resistance of the resulting composite was measured with reference to the oxidation resistance measurement procedure in example 2 to obtain IC of corresponding DPPH free radical scavenging test50The value is obtained.
TABLE 2 IC of DPPH radical scavenging test for different copper nanoparticle/Fullerol composites50Value of
Comparative example 1
Corresponding performance results of several antioxidant materials reported in the prior art are shown in table 3.
TABLE 3 IC for DPPH radical scavenging test of copper nanoparticle/Fullerol composites with other materials50Value comparison
[a]S.Rajeshkumar,G.Rinitha,et al.Nanostructural characterization of antimicrobial and antioxidant copper nanoparticles synthesized using novel Persea americana seeds[J].OpenNano, 2018(3):18-27.
[b]Dilaveez Rehana,D.Mahendirana,R.Senthil Kumar,et al.Evaluation of antioxidant and anticancer activity of copper oxide nanoparticles synthesized using medicinally important plant extracts[J].Biomed.Pharmacother.,2017(89):1067-1077.
[c]F.Liu,F.Xiong,Y.Fan,et al.Facile and scalable fabrication engineering of fullerenol nanoparticles by improved alkaline-oxidation approach and its antioxidant potential in maize[J].J. Nanopart.Res.(2016)18:338.
[d]J.R.Soares,T.C.P.Dins,A.P.Cunha,et al.Antioxidant activities of some extracts of Thymus zygis[J],Free Radic.Res.1997(26):469–478.
Comparing with other materials in table 3, the copper nanoparticle/fullerol composite material of the present invention has excellent oxidation resistance.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. A method of preparing a copper nanoparticle/fullerol composite, the method comprising the steps of:
(1) dispersing fullerene in an organic solvent to prepare fullerene dispersion liquid, and then adding peroxide and tetrabutylammonium hydroxide to carry out solvothermal reaction; after the reaction is finished, standing for layering, collecting a lower-layer liquid phase, then adding a precipitator for solid-liquid separation, collecting solids, and drying to obtain fullerol powder;
(2) and dispersing the obtained fullerol powder and cupric salt in water, uniformly mixing to obtain a mixed solution, then placing under laser for illumination, after illumination is finished, carrying out solid-liquid separation, collecting solids, and drying to obtain the copper nanoparticle/fullerol composite material.
2. The method according to claim 1, wherein the mass-to-volume ratio of fullerene to organic solvent in step (1) is (1.5-3): 1 mg/mL.
3. The method of claim 1, wherein the precipitating agent in step (1) comprises: any one or more of isopropanol, anhydrous ether and n-hexane.
4. The method of claim 1, wherein the solid-liquid separation in step (1) further comprises: after the precipitant is added for separation, the detergent is added for continuous separation, and finally, the solid product is collected.
5. The method according to claim 1, wherein the cupric salt in step (2) comprises: copper chloride dihydrate, copper nitrate, copper carbonate and copper sulfate.
6. The method according to claim 1, wherein the mass ratio of the fullerol to the cupric salt in step (2) is 1: 3-1: 4.
7. the method according to claim 1, wherein in step (2), the mass concentration of the fullerol in the mixed solution is 0.1-0.2 mg/mL.
8. The method according to any one of claims 1 to 7, wherein the laser in step (2) has a wavelength of 660nm and an excitation energy of 0.9mW/cm2。
9. A copper nanoparticle/fullerol composite material produced by the method of any one of claims 1 to 8.
10. Use of the copper nanoparticle/fullerol composite material according to claim 9 in the field of oxidation resistance for non-disease diagnosis and treatment.
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| CN113926487A (en) * | 2021-09-14 | 2022-01-14 | 杭州师范大学 | Fullerol/palladium nano composite photocatalyst and preparation method and application thereof |
| CN114344465A (en) * | 2021-12-29 | 2022-04-15 | 江南大学 | Preparation method and application of copper nanoparticle/size-controllable spherical fullerol composite material |
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| CN114344465B (en) * | 2021-12-29 | 2022-11-04 | 江南大学 | Preparation method and application of copper nanoparticle/size-controllable spherical fullerol composite material |
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