CN111392698A - Nickel ditelluride micron ball and preparation method and application thereof - Google Patents
Nickel ditelluride micron ball and preparation method and application thereof Download PDFInfo
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- CN111392698A CN111392698A CN202010288447.9A CN202010288447A CN111392698A CN 111392698 A CN111392698 A CN 111392698A CN 202010288447 A CN202010288447 A CN 202010288447A CN 111392698 A CN111392698 A CN 111392698A
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 182
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 91
- JPIIVHIVGGOMMV-UHFFFAOYSA-N ditellurium Chemical compound [Te]=[Te] JPIIVHIVGGOMMV-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000004005 microsphere Substances 0.000 claims abstract description 64
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims abstract description 40
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims abstract description 31
- 239000002243 precursor Substances 0.000 claims abstract description 24
- 229910052714 tellurium Inorganic materials 0.000 claims abstract description 24
- WNAHIZMDSQCWRP-UHFFFAOYSA-N dodecane-1-thiol Chemical compound CCCCCCCCCCCCS WNAHIZMDSQCWRP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- 238000002156 mixing Methods 0.000 claims abstract description 19
- CCCMONHAUSKTEQ-UHFFFAOYSA-N octadecene Natural products CCCCCCCCCCCCCCCCC=C CCCMONHAUSKTEQ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000006722 reduction reaction Methods 0.000 claims abstract description 15
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 13
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 12
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 12
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 12
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000005642 Oleic acid Substances 0.000 claims abstract description 12
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 12
- 150000002815 nickel Chemical class 0.000 claims abstract description 12
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 claims abstract description 7
- 239000011941 photocatalyst Substances 0.000 claims description 9
- BMGNSKKZFQMGDH-FDGPNNRMSA-L nickel(2+);(z)-4-oxopent-2-en-2-olate Chemical compound [Ni+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O BMGNSKKZFQMGDH-FDGPNNRMSA-L 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 7
- 238000004090 dissolution Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 239000012298 atmosphere Substances 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 3
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 3
- 229940078494 nickel acetate Drugs 0.000 claims description 3
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 3
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 3
- 229910001873 dinitrogen Inorganic materials 0.000 claims 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 8
- 239000001257 hydrogen Substances 0.000 abstract description 8
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 8
- 229910052724 xenon Inorganic materials 0.000 abstract description 7
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 abstract description 7
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 abstract description 6
- 229960000907 methylthioninium chloride Drugs 0.000 abstract description 6
- 239000013078 crystal Substances 0.000 abstract description 3
- 239000008204 material by function Substances 0.000 abstract description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 8
- 230000001699 photocatalysis Effects 0.000 description 8
- 230000015556 catabolic process Effects 0.000 description 7
- 238000006731 degradation reaction Methods 0.000 description 7
- 238000005406 washing Methods 0.000 description 7
- 238000001035 drying Methods 0.000 description 5
- 239000010453 quartz Substances 0.000 description 5
- 230000035484 reaction time Effects 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- 239000012295 chemical reaction liquid Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 239000013110 organic ligand Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 229910052979 sodium sulfide Inorganic materials 0.000 description 1
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000036962 time dependent Effects 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
Images
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/057—Selenium or tellurium; Compounds thereof
- B01J27/0576—Tellurium; Compounds thereof
-
- B01J35/39—
-
- B01J35/51—
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Abstract
The invention provides a nickel ditelluride microsphere and a preparation method and application thereof, belonging to the field of functional materials. The invention provides a preparation method of nickel ditelluride microspheres, which comprises the following steps: mixing tellurium powder, dodecyl mercaptan and oleylamine, and performing ultrasonic treatment to obtain a precursor solution of tellurium; mixing nickel salt, octadecene, oleylamine and oleic acid, and heating for dissolving to obtain a nickel source solution; and mixing the tellurium precursor solution and the nickel source solution, and carrying out reduction reaction to obtain the nickel ditelluride microspheres. The nickel ditelluride microspheres prepared by the preparation method provided by the invention have excellent photocatalytic degradation performance on methylene blue under xenon lamp irradiation, and after the nickel ditelluride microspheres are recycled for 5 times, the photocatalytic degradation performance is not reduced, the crystal structure is not changed, and meanwhile, the nickel ditelluride microspheres have higher hydrogen production rate under xenon lamp irradiation.
Description
Technical Field
The invention belongs to the field of functional materials, and particularly relates to a nickel ditelluride microsphere as well as a preparation method and application thereof.
Background
The photocatalysis technology is one of important ways for solving the problems of energy shortage and environmental pollution, and has good application prospects in the aspects of light energy conversion, pollution treatment, energy storage and the like. At present, the development of novel high-efficiency, stable and low-toxicity photocatalytic materials is the focus of research in this field. Most semiconductor photocatalysts are limited by self energy band structures and morphological structures, can only absorb and utilize ultraviolet light parts in sunlight, and have low light absorption coefficient, small specific surface area and few active sites, such as ZnO and TiO2Etc.; visible light catalysts with visible light response, e.g. CdS, CdSe, CdxZn1-xS(0<x<1) And the like, although the photocatalyst has a high light energy utilization rate, the photocatalyst has poor photocatalytic stability and contains heavy metal Cd element, so that water body pollution and the like are easily caused, and practical application is difficult to carry out. There is a need to develop a photocatalyst having excellent catalytic performance and good stability.
Disclosure of Invention
In view of the above, the invention provides a nickel ditelluride microsphere and a preparation method and application thereof, and the nickel ditelluride microsphere provided by the invention has the advantages of uniform appearance, stable physical and chemical properties, good photocatalytic performance, simple preparation method, easy implementation and suitability for industrial application.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of nickel ditelluride microspheres, which comprises the following steps:
mixing tellurium powder, dodecyl mercaptan and oleylamine, and performing ultrasonic treatment to obtain a precursor solution of tellurium;
mixing nickel salt, octadecene, oleylamine and oleic acid, and heating for dissolving to obtain a nickel source solution;
and mixing the tellurium precursor solution with a nickel source solution, and carrying out reduction reaction to obtain the nickel ditelluride microspheres.
Preferably, the power of ultrasonic treatment is 50-100W, and the time is 15-25 min.
Preferably, the temperature of the reduction reaction is 175-250 ℃ and the time is 5-30 min.
Preferably, the heating and dissolving temperature is 175-250 ℃.
Preferably, the heating dissolution and reduction reaction are performed in a nitrogen or inert gas atmosphere.
Preferably, the using amount ratio of the tellurium powder to the dodecanethiol is 0.0478g: 0.2-0.4 m L, and the percentage of the dodecanethiol in the total volume of the dodecanethiol and the oleylamine is more than or equal to 15%.
Preferably, the nickel salt is at least one of nickel acetylacetonate, nickel nitrate, nickel chloride and nickel acetate.
Preferably, the volume ratio of the octadecene to the oleylamine is 3: 1.8-2.2, the volume of the oleic acid accounts for 0.08-1.2% of the total volume of the octadecene and the oleylamine, and the using amount ratio of the nickel salt to the total amount of the octadecene and the oleylamine is 0.0642g: 18-22 m L.
The invention also provides a nickel ditelluride microsphere prepared by the preparation method in the technical scheme.
The invention also provides application of the nickel ditelluride microspheres in the technical scheme as a photocatalyst.
The invention provides a preparation method of nickel ditelluride microspheres, which comprises the following steps: mixing tellurium powder, dodecyl mercaptan and oleylamine, and performing ultrasonic treatment to obtain a precursor solution of tellurium; mixing nickel salt, octadecene, oleylamine and oleic acid, and heating for dissolving to obtain a nickel source solution; and mixing the tellurium precursor solution with a nickel source solution, and carrying out reduction reaction to obtain the nickel ditelluride microspheres. Tellurium powder, dodecanethiol and oleylamine are mixed, and subjected to ultrasonic treatment, so that tellurium precursors are formed by the tellurium powder and the dodecanethiol serving as organic ligands, and a tellurium precursor solution is obtained; and dropwise adding the tellurium precursor solution into a nickel source solution, and carrying out reduction reaction under the reduction action of oleylamine and the regulation and control of oleic acid to generate the nickel ditelluride microspheres. The preparation method is simple and easy to implement, and the obtained nickel ditelluride has uniform appearance, stable physical and chemical properties and good photocatalytic performance. The experimental results show that: the nickel ditelluride microspheres prepared by the preparation method provided by the invention have excellent photocatalytic degradation performance on methylene blue under xenon lamp irradiation, and after the nickel ditelluride microspheres are recycled for 5 times, the photocatalytic degradation performance is not reduced, the crystal structure is not changed, and meanwhile, the nickel ditelluride microspheres have higher hydrogen production rate under xenon lamp irradiation.
Drawings
FIG. 1 is an XRD pattern of nickel ditelluride microspheres obtained in examples 1-4;
FIG. 2 is an XRD pattern of nickel ditelluride microspheres obtained in example 1 and examples 5-8;
FIG. 3 is an SEM scanning electron micrograph of nickel ditelluride microspheres obtained in example 1;
FIG. 4 is a TEM transmission electron micrograph of the nickel ditelluride microspheres obtained in example 1;
FIG. 5 is a graph showing the UV-VIS absorption spectrum of the nickel ditelluride microspheres obtained in example 1;
FIG. 6 is a graph showing the degradation curves of methylene blue by photocatalytic degradation of nickel ditelluride microspheres obtained in examples 1-4;
FIG. 7 is a graph showing the degradation of methylene blue by cyclic photocatalytic degradation of nickel ditelluride microspheres obtained in example 1;
FIG. 8 is an XRD pattern of nickel ditelluride obtained in example 1 before and after 5 cycles.
Detailed Description
The invention provides a preparation method of nickel ditelluride microspheres, which comprises the following steps:
mixing tellurium powder, dodecyl mercaptan and oleylamine, and performing ultrasonic treatment to obtain a precursor solution of tellurium;
mixing nickel salt, octadecene, oleylamine and oleic acid, and heating for dissolving to obtain a nickel source solution;
and mixing the tellurium precursor solution with a nickel source solution, and carrying out reduction reaction to obtain the nickel ditelluride microspheres.
Tellurium powder, dodecyl mercaptan and oleylamine are mixed and subjected to ultrasonic treatment to obtain a tellurium precursor solution.
The specification of the tellurium powder is not specially limited, and the tellurium powder is commercially available.
In the invention, the dosage ratio of the tellurium powder to the dodecanethiol is preferably 0.0478g: 0.2-0.4 m L, more preferably 0.0478g:0.3m L, the dodecanethiol accounts for preferably not less than 15% and more preferably 15% of the total volume of the dodecanethiol and the oleylamine, the dodecanethiol is used as an organic ligand to form a tellurium precursor together with the tellurium powder and the dodecanethiol in an ultrasonic treatment process, and the oleylamine is used as a reducing agent and a solvent.
In the invention, the power of ultrasonic treatment is preferably 50-100W, more preferably 80-100W, and the time is preferably 15-25 min, more preferably 20 min.
The method comprises the steps of mixing nickel salt, octadecene, oleylamine and oleic acid, and heating to dissolve to obtain a nickel source solution.
In the present invention, the nickel salt is preferably at least one of nickel acetylacetonate, nickel nitrate, nickel chloride, and nickel acetate, and more preferably nickel acetylacetonate.
In the invention, the volume ratio of octadecene to oleylamine is preferably 3: 1.8-2.2, more preferably 3:2, the volume of oleic acid is preferably 0.08-1.2% and more preferably 1.0% of the total volume of octadecene and oleylamine, the using amount ratio of the nickel salt to the total volume of octadecene and oleylamine is preferably 0.0642g: 18-22 m L, more preferably 0.0642g:20m L.
In the invention, the heating and dissolving temperature is preferably 175-250 ℃; the heating dissolution is preferably performed in a nitrogen or inert gas atmosphere to avoid oxidation of the nickel source. The heating rate of the invention for heating to the temperature required for heating and dissolving is not particularly limited, and any heating rate can be used.
The sequence of the tellurium precursor solution and the nickel source solution is not particularly limited, and can be any sequence.
After obtaining the tellurium precursor solution and the nickel source solution, the invention mixes the tellurium precursor solution and the nickel source solution, and carries out reduction reaction to obtain the nickel ditelluride microspheres.
In the invention, the tellurium precursor solution and the nickel source solution are preferably mixed in a manner that the tellurium precursor solution is dripped into the nickel source solution; the dropping speed is not particularly limited, the uniform dropping is preferably kept, the mixture is dropwise injected, more preferably, the liquid drops continuously fall during the dropping, the liquid drops are not interrupted and do not form strands, and the dropping mode is favorable for ensuring the uniform contact of reaction liquid.
In the invention, the temperature of the reduction reaction is preferably 175-250 ℃, and the time is preferably 5-30 min; the reduction reaction is preferably carried out under a nitrogen or inert gas atmosphere.
After the reduction reaction is completed, the reaction solution is preferably cooled to room temperature, then centrifuged, and the precipitate is taken out, and then chloroform washing, ethanol washing and drying are sequentially performed. The specific modes of the chloroform washing and the ethanol washing are not particularly limited, and the residual solvent on the surface of the product can be removed by adopting a conventional washing mode, such as soaking and centrifugal washing.
The drying mode is not particularly limited, and the product with constant weight can be obtained.
The invention also provides a nickel ditelluride microsphere prepared by the preparation method in the technical scheme.
The invention also provides the application of the nickel ditelluride microspheres in the technical scheme as a photocatalyst; the photocatalyst is preferably a catalyst for photocatalytic degradation of organic matters or a catalyst for photocatalytic hydrogen production.
The nickel ditelluride microspheres and the preparation method and application thereof provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
0.0478g of tellurium powder is mixed with 0.3m L dodecanethiol and 1.7m L oleylamine, and then ultrasonic treatment is carried out for 20min under the power of 80W to obtain a precursor solution of tellurium;
mixing 15m of L octadecene, 10m of L oleylamine, 0.25m of L oleic acid and 0.0642g of nickel acetylacetonate, stirring for 5min under the nitrogen atmosphere to form a suspension, heating to 175 ℃, dissolving by heating, and obtaining a nickel source solution after the nickel acetylacetonate is dissolved;
dropwise adding the tellurium precursor solution into the nickel source solution, reacting at 175 ℃ for 30min, cooling to room temperature, centrifugally cleaning for 3 times by using chloroform and ethanol, and drying to obtain the nickel ditelluride microspheres.
The nickel ditelluride microspheres obtained in this example were measured to have an average particle size of 300 nm.
Example 2
Nickel ditelluride microspheres were prepared as in example 1, except that the temperature for dissolution and reaction was 200 ℃.
Example 3
Nickel ditelluride microspheres were prepared as in example 1, except that the temperature for dissolution and reaction was 225 ℃.
Example 4
Nickel ditelluride microspheres were prepared as in example 1, except that the temperature for dissolution and reaction was 250 ℃.
Example 5
Mixing 0.0478g of tellurium powder, 0.3m L dodecanethiol and 1.7m L oleylamine, and then carrying out ultrasonic treatment for 20min under the power of 100W to obtain a tellurium precursor solution;
mixing 15m of L octadecene, 10m of L oleylamine, 0.25m of L oleic acid and 0.0642g of nickel acetylacetonate, stirring for 5min under the nitrogen atmosphere to form a suspension, heating to 175 ℃, dissolving by heating, and obtaining a nickel source solution after the nickel acetylacetonate is dissolved;
dropwise adding the tellurium precursor solution into the nickel source solution, reacting for 5min at 175 ℃, then cooling to room temperature, centrifugally cleaning for 3 times by using chloroform and ethanol, and drying to obtain the nickel ditelluride microspheres.
Example 6
Nickel ditelluride microspheres were prepared as in example 5, except that the reaction time was 10 min.
Example 7
Nickel ditelluride microspheres were prepared as in example 5, except that the reaction time was 15 min.
Example 8
Nickel ditelluride microspheres were prepared as in example 5, except that the reaction time was 20 min.
The XRD patterns of the nickel ditelluride microspheres obtained in examples 1 to 4 were measured, and as shown in fig. 1, the XRD patterns of the nickel ditelluride microspheres obtained in examples 1 and 5 to 8 were measured, and as shown in fig. 2, it can be seen from fig. 1 and 2 that the nickel ditelluride microspheres obtained in examples 1 to 8 have stronger crystallinity with the increase of the reaction time.
SEM images and TEM images of the nickel ditelluride microspheres obtained in example 1 were measured, and the results are shown in fig. 3 and 4. As can be seen from fig. 3 and 4, the nickel ditelluride microspheres obtained in this example are formed by stacking nanoparticles, and have uniform particle size distribution, and the nanoparticles are stacked to form a three-dimensional hierarchical structure.
Fig. 5 is an ultraviolet-visible absorption spectrum of the nickel ditelluride microspheres obtained in example 1, and as can be seen from fig. 5, the nickel ditelluride microspheres obtained by the preparation method provided by the invention have high absorption intensity for light of 200-1000 nm.
The catalytic degradation performance of the nickel ditelluride microspheres obtained in the examples 1-4 on methylene blue is tested, and specifically:
adding 30mg of nickel ditelluride microspheres into a methylene blue solution with the concentration of 20mg/m L, placing the solution under a 300W xenon lamp for photocatalytic degradation, testing the absorbance of the reaction solution every 20min, converting the absorbance into the concentration, and calculating the reaction timingRatio of time-dependent concentration to initial concentration (C/C)0) The results are shown in FIG. 6. As can be seen from the calculation of FIG. 6, in examples 1 to 4, when the catalytic degradation is carried out for 2 hours, the degradation rates are 97.2%, 94.8% and 92.5% in sequence, and it can be seen that the degradation rates can exceed 93% when the catalytic degradation is carried out for 2 hours.
The cycling stability of the nickel ditelluride microspheres obtained in example 1 was tested according to the above method, the photocatalytic degradation reaction time of each cycle test was 150min, after one cycle was completed, the supernatant of the reaction solution was removed, and after centrifugal washing with distilled water, solid-liquid separation was performed, followed by drying, and the nickel ditelluride catalyst was recovered and used for the next cycle. The photocatalytic degradation process was recorded, and the result is shown in FIG. 7, and the XRD pattern of the nickel ditelluride microspheres recycled for 5 times was measured, and the result is shown in FIG. 8, in which "UsedNiTe" is used2"XRD pattern of nickel ditelluride microsphere after 5 times of recycling," FershNiTe2"is the XRD pattern of the initially obtained nickel ditelluride microspheres. As can be seen from fig. 7, the photocatalytic degradation performance of the nickel ditelluride microspheres obtained in example 1 is not reduced after 5 times of recycling, and as can be seen from fig. 8, the XRD of the nickel ditelluride microspheres after 5 times of recycling is consistent with the XRD curve of the initially obtained nickel ditelluride microspheres, and the crystal structure is not changed, which indicates that the nickel ditelluride microspheres have excellent stability.
With Na2S/Na2SO3Taking the solution as a sacrificial agent and a 300W xenon lamp as a light source, taking 10mg of the nickel ditelluride micro spheres obtained in the example 1 as a photocatalyst to carry out photocatalytic hydrogen production, specifically, adding 10mg of the nickel ditelluride micro spheres obtained in the example 1 and 100m L reaction liquid into a quartz reactor, wherein Na in the reaction liquid2The concentration of S is 0.15 mol/L, Na2SO3The concentration of the hydrogen is 0.35 mol/L, the quartz reactor is vacuumized, the air in the reactor is removed, a 300W xenon lamp is started to irradiate the quartz window of the quartz reactor, the photocatalytic hydrogen production is carried out at 20 ℃, the gas in the quartz reactor is sampled on line every 30min, a gas chromatograph TCD detector is adopted to carry out hydrogen content analysis, the result is calculated, and the hydrogen production rate is 1438.6 mu mol h-1·g-1。
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of nickel ditelluride microspheres is characterized by comprising the following steps:
mixing tellurium powder, dodecyl mercaptan and oleylamine, and performing ultrasonic treatment to obtain a precursor solution of tellurium;
mixing nickel salt, octadecene, oleylamine and oleic acid, and heating for dissolving to obtain a nickel source solution;
and mixing the tellurium precursor solution with a nickel source solution, and carrying out reduction reaction to obtain the nickel ditelluride microspheres.
2. The preparation method according to claim 1, wherein the ultrasonic treatment is performed at a power of 50-100W for 15-25 min.
3. The method according to claim 1, wherein the temperature of the reduction reaction is 175 to 250 ℃ and the time is 5 to 30 min.
4. The method according to claim 1, wherein the temperature for the thermal dissolution is 175 to 250 ℃.
5. The production method according to any one of claims 1, 3 and 4, wherein the heating dissolution and reduction reaction is performed in a nitrogen gas or an inert gas atmosphere.
6. The preparation method of claim 1, wherein the usage ratio of the tellurium powder to the dodecanethiol is 0.0478g: 0.2-0.4 m L, and the percentage of the dodecanethiol in the total volume of the dodecanethiol and the oleylamine is not less than 15%.
7. The method according to claim 1, wherein the nickel salt is at least one of nickel acetylacetonate, nickel nitrate, nickel chloride, and nickel acetate.
8. The preparation method of claim 1 or 7, wherein the volume ratio of the octadecene to the oleylamine is 3: 1.8-2.2, the volume of the oleic acid accounts for 0.08-1.2% of the total volume of the octadecene and the oleylamine, and the using amount ratio of the nickel salt to the total amount of the octadecene and the oleylamine is 0.0642g: 18-22 m L.
9. Nickel ditelluride microspheres prepared by the preparation method of any one of claims 1-8.
10. Use of nickel ditelluride microspheres as claimed in claim 9 as a photocatalyst.
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