CN113173575B - Copper nanoparticle/fullerol nanocomposite material and preparation method and application thereof - Google Patents
Copper nanoparticle/fullerol nanocomposite material and preparation method and application thereof Download PDFInfo
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/152—Fullerenes
- C01B32/156—After-treatment
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
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- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
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Abstract
The invention discloses a copper nanoparticle/fullerol nanocomposite and a preparation method and application thereof, and belongs to the technical field of nanomaterials. The invention uses fullerene as a matrix, and the fullerene is subjected to hydroxylation modification to obtain fullerol, copper ions in copper chloride are reduced into copper nano particles through laser light reduction and stably loaded on the surface of the fullerol, so that the copper nano particle/fullerol composite material is prepared. The method is simple and efficient, the particle size of the obtained copper nanoparticle/fullerene alcohol composite material is smaller, the distribution is uniform, the copper nanoparticle/fullerene alcohol composite material can be better applied to the field of antioxidation, the problem that the antioxidation performance of a single fullerene derivative is not strong is solved, and the copper nanoparticle/fullerene alcohol composite material has a good application prospect.
Description
Technical Field
The invention relates to a copper nanoparticle/fullerol nanocomposite, a preparation method and application thereof, and belongs to the technical field of nanomaterials.
Background
In the daily metabolism of people, reactive Oxygen Species (ROS) are always produced, and their excessive presence often causes accelerated aging and significant increase of heart brain system diseases. Therefore, a material having good oxidation resistance, so that ROS can be suppressed to slow down aging, is desired.
Fullerene is a hollow molecule completely composed of carbon, is a unique allotrope in a plurality of carbon nano materials, and has good photoactivity and chemical reactivity. Based on the special p-pi conjugated structure, the fullerene can adsorb free radicals through carbon-carbon double bonds, so that the fullerene has a strong antioxidation effect. However, fullerene is easy to agglomerate, has strong hydrophobicity, is only dissolved in limited organic solvents (such as toluene, carbon tetrachloride and the like), and severely limits the application of the fullerene in the field of biological medicine. At present, various modification methods such as amination, carboxylation, hydroxylation and the like of fullerene exist, so that the obtained fullerene derivative has good water-solubility. However, the fullerene derivative has poor antioxidant effect because the radical-absorbing effect of the fullerene is reduced after the functionalization. Copper nano-particles are widely used antioxidants in biological systems, and the addition of copper nano-particles to fullerene water-soluble derivatives to construct composite materials can play a good role in antioxidation. However, the loading and particle size of the copper nanoparticles need to be controlled to reduce the effect of 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, so that the formation of the fullerene water-soluble derivative/copper nanoparticle composite material is still a challenge, and is one of 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, comprising the steps of:
(1) Dispersing fullerene in an organic solvent to prepare fullerene dispersion liquid, and then adding peroxide and tetrabutyl ammonium hydroxide to perform solvothermal reaction; after the reaction is finished, standing for layering, collecting a lower liquid phase, adding a precipitator for solid-liquid separation, collecting solids, and drying to obtain fullerol powder;
(2) Dispersing the obtained fullerol powder and cupric salt in water, uniformly mixing to obtain a mixed solution, then placing under laser to carry out illumination, and after the illumination is finished, carrying out solid-liquid separation, collecting solids and drying to obtain the copper nano particle/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 fullerene to organic solvent in step (1) is (1.5-3): 1 (mg/mL); specifically, the method comprises the following steps of: 1 (mg/mL).
In one embodiment of the present invention, the peroxide in step (1) comprises any one or more of the following: 30% hydrogen peroxide, tert-butyl hydroperoxide, dibenzoyl peroxide and potassium oxide permanganate.
In one embodiment of the present invention, the volume ratio of toluene, 30% hydrogen peroxide, tetrabutylammonium hydroxide in step (1) is 100:20:1 (mL).
In one embodiment of the present invention, the solvothermal reaction in step (1) has a temperature in the range of 50 ℃ to 80 ℃; the time is 12h-20h.
In one embodiment of the invention, the layering in step (1) is an upper clear liquid phase and a lower dark yellow liquid phase.
In one embodiment of the present invention, the precipitating agent in step (1) comprises: any one or more of isopropanol, anhydrous diethyl ether and n-hexane. When three mixtures were selected, the volume ratio of isopropanol, anhydrous diethyl ether and n-hexane was 7:5:5.
in one embodiment of the present invention, the solid-liquid separation in step (1) further comprises: after the precipitation agent is added for separation, the washing agent 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 speed in step (1) is 8000rpm and the centrifugation time is 8min.
In one embodiment of the present invention, the drying in step (1) is performed using a vacuum oven, the vacuum degree is-1 MPa, and the drying temperature is 25 ℃.
In one embodiment of the invention, the divalent copper salt in step (2) is selected from the group consisting of: 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 step (2) is 1: 3-1: 4, a step of; preferably the mass ratio is 1:3.3.
In one embodiment of the present invention, in step (2), the mass concentration of the mixed solution fullerol is 0.1-0.2mg/mL; specifically, 0.13mg/mL may 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/cm 2 。
In one embodiment of the present invention, the solid-liquid separation in step (2) is performed by centrifugation at 8000rpm for 6min.
In one embodiment of the present invention, the drying in step (2) is performed using a vacuum oven, the vacuum degree is-1 MPa, and the drying temperature is 50 ℃.
In one embodiment of the present invention, the method specifically comprises the following steps:
(1) Dispersing fullerene into toluene solvent to form toluene dispersion, then adding 30% hydrogen peroxide and tetrabutylammonium hydroxide solution into the toluene dispersion, mixing and stirring and heating the mixture;
(2) Separating the upper and lower layered mixed liquid obtained in the step (1), taking a lower layer liquid phase, adding a precipitator and a detergent into the lower layer liquid phase, centrifuging, decanting and drying to obtain fullerol powder;
(3) The fullerol powder obtained in the step (2) and copper (II) chloride dihydrate are prepared into a mixed solution according to a certain proportion, and the mixed solution is fully irradiated under laser, so that a certain energy is given to carry out photoelectron conversion to coat copper on the surface of the fullerol. And centrifuging, decanting and drying to obtain the copper nano particle/fullerol composite material which enables the copper nano particles to be better and more uniformly coated on the fullerol.
The invention also provides a copper nanoparticle/fullerol composite material by utilizing the method.
In one embodiment of the invention, the copper nanoparticle/fullerol composite material has a particle size of about 2 to 3nm.
The invention also provides application of the copper nanoparticle/fullerol composite material in the field of antioxidation of diagnosis and treatment of non-cups.
The beneficial effects of the invention are that
According to the invention, the copper nano particles can be coated on the surface of the fullerol by a simple means, and the coated copper nano particles have lower particle size and are relatively uniformly distributed. The copper nanoparticle/fullerol composite material prepared by the invention can be applied to the aspect of antioxidation, and can well adsorb free radicals so as to play a role in antioxidation.
Drawings
FIG. 1 is an infrared (FT-IR) spectrum of fullerols.
FIG. 2 is a thermogravimetric curve (TGA) of fullerols.
FIG. 3 is an X-ray photoelectron spectroscopy (XPS) chart of a copper nanoparticle/fullerol nanocomposite, where (a) is the XPS chart of the composite; (b) is a Cu 2p XPS profile; (C) is a C1 s XPS profile; (d) O1 s XPS spectrum.
Fig. 4 is an X-ray diffraction (XRD) pattern of fullerols and copper nanoparticle/fullerol composites.
FIG. 5 is a graph of particle size analysis, wherein (a) is fullerol; (b) is a copper nanoparticle/fullerol composite material.
Fig. 6 is a Transmission Electron Microscope (TEM) image of a copper nanoparticle/fullerol composite material.
Fig. 7 is a histogram of particle size distribution of copper nanoparticles counted by TEM.
FIG. 8 is an antioxidative activity of a composite material: inhibition profile of 2, 2-biphenyl-1-picrylhydrazyl (DPPH).
FIG. 9 is an antioxidative activity of a composite material: semi-Inhibitory Concentration (IC) of DPPH inhibition assay 50 ) Graph diagram.
Detailed Description
The present invention will be described in detail 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 those familiar 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, while further 10mL of 30% hydrogen peroxide solution and 500. Mu.L of tetrabutylammonium hydroxide solution were added thereto, and stirred in a heated stirrer with parameters set at 60℃and 400rpm for 16 hours.
After stirring for 16 hours, a layered solution of the supernatant was obtained, and the lower layer of the turbid solution was separated by using a separating funnel, and 74.12mL of isopropyl alcohol, 52.94mL of dehydrated ether and 52.94mL of n-hexane were added to the turbid solution. The solution was then centrifuged for 8min (8000 rpm) to allow the fullerols to fully separate. After decantation, 10mL of dehydrated ether was added to each centrifuge tube, and the above centrifugation-decantation steps were repeated two to three times to sufficiently remove impurities. The precipitate obtained is then dried in a vacuum oven (vacuum: -1MPa; temperature: 25 ℃).
The obtained fullerols were scanned by infrared spectrum, and the result is shown in FIG. 1, which shows that the spectrum of the obtained fullerols is 3400cm -1 The vicinity showed a broad O-H band at 1080, 1370 and 1620cm -1 Three characteristic bands are shown, which can be designated as v C–O ，ν C–O–H And v C＝C Absorption, further justifying successful hydroxylation of fullerenes.
The result of thermogravimetric analysis of the prepared fullerols is shown in fig. 2, and it can be seen that the prepared fullerols have a loss of bound water at 120 deg.c, possibly due to the detachment of hydroxyl groups at 120 deg.c to 300 deg.c, and possibly due to the heat loss of the fullerenes themselves at temperatures >300 deg.c.
(2) Preparing a copper nanoparticle/fullerol composite material:
adding 2mg of obtained fullerol, copper (II) chloride dihydrate (34.5 mg, 17.5mg, 9.3mg, 6.6 mg) of different mass, and 15mL of water into a glass bottle, and irradiating with laser light of 660nm wavelength (0.9 mW/cm) 2 ) Thereby the copper oxide obtains corresponding energy for reduction. It was further found that the mixed aqueous solution to which 34.5mg of copper (II) chloride dihydrate was added was dark blue after illumination and had a yellow flocculent precipitate formed; the mixed solution added with 17.5mg of copper (II) chloride dihydrate is light blue after illumination and the colored flocculent precipitate is generated; the mixed solution added with 9.3mg of copper (II) chloride dihydrate is light blue and transparent after illumination, and only trace floccules are separated out; the mixed solution added with 6.6mg of copper (II) chloride dihydrate is transparent and colorless after illumination and almost no flocculent precipitate is generated; finally, a mixed aqueous solution of 6.6mg of copper (II) chloride dihydrate was selected for use. And centrifuging the solution for 6min (8000 rpm) to fully separate the copper nano-particle/fullerol composite material, and then placing the obtained precipitate in a vacuum oven for drying (vacuum degree: 1MPa; temperature: 50 ℃) to obtain the copper nano-particle/fullerol composite material.
The prepared copper nano particle/fullerol composite material is processedAs a result of analysis and detection by X-ray photoelectron spectroscopy, as shown in FIG. 3, cu 2p spectra show two peaks at 932.6 and 952.3eV, respectively designated as Cu 2p 3/2 And Cu 2p 1/2 Indicating Cu 2+ Is present.
The prepared copper nanoparticle/fullerol nanocomposite was subjected to X-ray diffraction analysis, and as a result, as shown in fig. 4, the XRD pattern of fullerol contained diffraction peaks at 2θ=10.78 °, 17.64 °, 20.74 ° and 21.68 °, corresponding to the planar structures of (111), (022), (113) and (222), respectively, in body-centered cubes. Whereas the XRD pattern of the copper nanoparticle/fullerol composite material shows characteristic peaks and highly crystalline peaks of copper particles, including diffraction peaks at 2θ=43.2 °, 50.4 °, 74.1 °, and their diffraction peaks correspond to planes of the metal cubes located at (111), (200) and (220), respectively.
The above data indicate that copper nanoparticles are indeed present in the composite.
As a result of measuring the particle size of the prepared composite material of fullerol and copper nanoparticles/fullerol, the particle size of fullerol of unmodified copper nanoparticles was about 34nm, and the particle size of the composite material after coating copper nanoparticles was about 37nm, as shown in FIGS. 5 (a) and (b). Indicating that the synthesized coated copper nanoparticles have a smaller particle size.
As shown in fig. 6, the result of Transmission Electron Microscope (TEM) detection of the prepared copper nanoparticle/fullerol composite material shows that the prepared copper nanoparticle is coated on the surface of fullerol in a relatively uniform and dispersed manner. And the lattice spacing obtained by enlarging the coated particles is about 0.22nm, further illustrating that the coated particles are copper nanoparticles. Meanwhile, as shown in FIG. 7, the particle size of the prepared copper nanoparticles is mostly 2 to 3nm.
EXAMPLE 2 antioxidant Properties of copper nanoparticle/Fullerene composite
(1) Selecting copper nano-particles/fullerol composite materials (0.0025 mg, 0.005mg, 0.01mg, 0.025mg, 0.05mg, 0.1mg and 0.25 mg) with different masses, and adding the copper nano-particles/fullerol composite materials into 1mL of absolute ethyl alcohol to obtain a composite material ethanol solution;
(2) First dilute in ethanol solutionReleasing DPPH to obtain 0.3mM DPPH ethanol solution; taking 0.5mL of the prepared DPPH ethanol solution, putting the solution into a quartz cuvette, further dripping 0.5mL of the ethanol solution to obtain the DPPH/ethanol solution, and recording the absorbance as A c The method comprises the steps of carrying out a first treatment on the surface of the This DPPH/ethanol solution (0.5 mL) was then further mixed with 0.5mL of the composite solution of step (1); the mixed solution was incubated under dark conditions for 30 minutes, and absorbance was measured at 517nm after incubation (A s ). The absorbance of the ethanol solution of the composite sample without DPPH was also tested in the same manner (a b )；
(3) And (3) passing the corresponding parameters obtained in the step (1) through the following formula: percentage inhibition of dpph= [1- (a) s –A b )/A c ]The average value is obtained by measuring 100% in parallel three times, and the DPPH inhibition degree is obtained. The specific results are shown in Table 1.
FIG. 8 is an illustration of antioxidant activity of copper nanoparticle/fullerol composites: DPPH inhibition assay at a sample concentration of about 0.01mg/mL, the DPPH inhibition level was 45.43%; at a concentration of about 0.025mg/mL, the DPPH inhibition level was 76.39%; at a concentration of about 0.05mg/mL, the DPPH inhibition level was 85.86%; the DPPH inhibition degree is 96.25% at a concentration of about 0.1 mg/mL; the DPPH inhibition level was 99.05% at a concentration of about 0.25 mg/mL.
FIG. 9 is an illustration of antioxidant activity of copper nanoparticle/fullerol composites: semi-Inhibitory Concentration (IC) of DPPH inhibition assay 50 ) The graph, the half-inhibition concentration curve equation is: y=2975.01x+6.63 (R 2 =0.95). The semi-inhibitory concentration was about 0.0145mg/mL.
TABLE 1 DPPH Activity inhibition with copper nanoparticle/Fulleritol composites of different masses
Example 3
Referring to example 1, the mass ratio of fullerol to cupric salt was changed, and other conditions were unchanged, to prepare a corresponding composite material.
The results were measured with reference to the antioxidant assay procedure in example 2The oxidation resistance of the composite material is obtained to obtain the IC of the corresponding DPPH free radical scavenging test 50 Values.
TABLE 2 DPPH radical scavenging test IC for different copper nanoparticle/Fullerol composites 50 Value of
Comparative example 1
Several antioxidant materials reported previously have the corresponding performance results shown in Table 3.
TABLE 3 DPPH radical scavenging test IC of copper nanoparticle/Fullerol composites with other materials 50 Value 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.
The copper nanoparticle/fullerol composites of the present invention have excellent oxidation resistance as compared to other materials in table 3.
While the invention has been described with reference to the preferred embodiments, it is not limited thereto, and 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 material, comprising the steps of:
(1) Dispersing fullerene in an organic solvent to prepare fullerene dispersion liquid, and then adding peroxide and tetrabutyl ammonium hydroxide to perform solvothermal reaction; after the reaction is finished, standing for layering, collecting a lower liquid phase, adding a precipitator for solid-liquid separation, collecting solids, and drying to obtain fullerol powder;
(2) Dispersing the obtained fullerol powder and cupric salt in water, uniformly mixing to obtain a mixed solution, then placing under laser to carry out illumination, and after the illumination is finished, carrying out solid-liquid separation, collecting solids and drying to obtain the copper nano particle/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): 1mg/mL.
3. The method of claim 1, wherein the precipitating agent in step (1) comprises: any one or more of isopropanol, anhydrous diethyl ether and n-hexane.
4. The method of claim 1, wherein the solid-liquid separation in step (1) further comprises: after the precipitation agent is added for separation, the washing agent is added for continuous separation, and finally the solid product is collected.
5. The method according to claim 1, wherein the divalent copper salt in step (2) comprises: copper chloride dihydrate, copper nitrate, copper carbonate, copper sulfate.
6. The method according to claim 1, wherein the mass ratio of fullerol to cupric salt in step (2) is 1: 3-1: 4.
7. the method according to claim 1, wherein in the step (2), the mass concentration of the mixed solution fullerol is 0.1-0.2mg/mL.
8. The method according to any one of claims 1 to 7, wherein the laser light in step (2) has a wavelength of 660nm and excitation energy of 0.9mW/cm 2 。
9. A copper nanoparticle/fullerol composite material prepared by the method of any one of claims 1-8.
10. Use of the copper nanoparticle/fullerol composite material as claimed in claim 9 in the field of antioxidation for diagnosis and treatment of non-disease.
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| CN102849717A (en) * | 2012-09-12 | 2013-01-02 | 深圳市通产丽星股份有限公司 | Fullerol and preparation method thereof |
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