CN112808259B - Preparation method and application of hybrid nano-diamond - Google Patents
Preparation method and application of hybrid nano-diamond Download PDFInfo
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- CN112808259B CN112808259B CN202110109817.2A CN202110109817A CN112808259B CN 112808259 B CN112808259 B CN 112808259B CN 202110109817 A CN202110109817 A CN 202110109817A CN 112808259 B CN112808259 B CN 112808259B
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- 239000002113 nanodiamond Substances 0.000 title claims abstract description 70
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229940043267 rhodamine b Drugs 0.000 claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000002253 acid Substances 0.000 claims abstract description 9
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 239000001257 hydrogen Substances 0.000 claims abstract description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 8
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims abstract description 7
- 239000012300 argon atmosphere Substances 0.000 claims abstract description 6
- 239000012298 atmosphere Substances 0.000 claims abstract description 6
- 238000001354 calcination Methods 0.000 claims abstract description 6
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims abstract 2
- 238000004140 cleaning Methods 0.000 claims description 7
- 238000010992 reflux Methods 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 13
- 239000000463 material Substances 0.000 abstract description 9
- 238000005406 washing Methods 0.000 abstract description 5
- 238000011160 research Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 238000005457 optimization Methods 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 5
- 150000002431 hydrogen Chemical class 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 238000001782 photodegradation Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 125000006417 CH Chemical group [H]C* 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
-
- B01J35/23—
-
- B01J35/39—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/06—Washing
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention provides a preparation method and application of hybrid nano-diamond, comprising the following steps: (1) acid washing and purifying the nano-diamond; (2) placing the acid-washed and purified nano-diamond in a tubular furnace, heating and calcining the nano-diamond in an argon atmosphere, and naturally cooling the nano-diamond to room temperature; (3) and (3) changing the atmosphere of the tube furnace in the step (2) into hydrogen, heating and calcining again, and naturally cooling to room temperature to obtain the hybrid nano-diamond. According to the invention, through structure optimization, the novel and efficient hybrid nano diamond material is prepared, so that the hybrid nano diamond material has higher photocatalytic activity and has greater research significance. Sp in the hybrid nanodiamond prepared according to the invention 2 The proportion of carbon increases significantly. Compared with untreated nano-diamond, the activity of photocatalytic degradation of rhodamine B (RhB) of the hybrid nano-diamond is obviously improved under the irradiation of simulated sunlight (AM 1.5). And has better cycle stability.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to a preparation method and application of hybrid nano diamond.
Background
As a novel carbon nanomaterial, nanodiamond receives more and more attention in the field of photocatalysis due to the advantages of excellent chemical stability, easy surface modification, large specific surface area and the like. However, the photocatalytic activity of the single nano-diamond is relatively low, and the single nano-diamond is usually compounded with other semiconductor photocatalytic materials to construct a composite material, so that the high photocatalytic activity is achieved by the advantages of the condensed multi-component material. Research shows that the hydrogen-treated nano-diamond has certain activity of photolyzing water to produce hydrogen under 532nm laser irradiation, but the photocatalytic activity is lower. If the structure is optimized, a method for preparing a novel and efficient hybrid nano-diamond material is developed, so that the material has higher photocatalytic activity and higher research value.
Disclosure of Invention
The invention provides a preparation method and application of hybrid nano-diamond, and solves the problem that the existing single nano-diamond is low in photocatalytic activity.
The technical scheme for realizing the invention is as follows:
a preparation method of hybrid nano-diamond comprises the following steps:
(1) acid washing and purifying the nano-diamond;
(2) placing the acid-washed and purified nano-diamond in a tubular furnace, heating and calcining the nano-diamond in an argon atmosphere, and naturally cooling the nano-diamond to room temperature;
(3) and (3) changing the atmosphere of the tube furnace in the step (2) into hydrogen, heating and calcining again, and naturally cooling to room temperature to obtain the hybrid nano-diamond.
And (2) refluxing and cleaning the nano-diamond with the particle size of 3nm-10nm by using a mixed acid solution in the step (1), and then evaporating to dryness by using a refrigerator.
The mixed acid is prepared from the following components in a molar ratio of 3: 1 HNO 3 And H 2 SO 4 The reflux cleaning time is 12-24h, and the drying time is 12-48 h.
The heating temperature in the step (2) is 1000-.
The heating temperature in the step (3) is 750-.
The hybrid nanodiamond has sp 2 、sp 3 A hybrid carbon.
The hybrid nano-diamond is applied to photocatalytic degradation of rhodamine B.
The invention has the beneficial effects that: according to the invention, through structure optimization, the novel and efficient hybrid nano diamond material is prepared, so that the hybrid nano diamond material has higher photocatalytic activity and has greater research significance. Sp in the hybrid nanodiamond prepared according to the invention 2 The proportion of carbon increases significantly. Compared with untreated nano-diamond, the activity of photocatalytic degradation of rhodamine B (RhB) of the hybrid nano-diamond is obviously improved under the irradiation of simulated sunlight (AM 1.5). And has better cycle stability.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a TEM image of the hybrid nanodiamond of example 1.
FIG. 2 is an X-ray photoelectron spectrum of C1 s of the sample of example 1.
Fig. 3 is a photocatalytic activity test chart of the sample of example 1.
FIG. 4 is the cycle test chart of the hybrid nano-diamond photodegradation RhB in example 1.
Detailed Description
The technical solutions of the present invention will be described clearly and completely below with reference to embodiments of the present invention, and it should be apparent that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art based on the embodiments of the present invention without inventive step, are within the scope of the present invention.
Example 1
The preparation method of the hybrid nano-diamond comprises the following steps:
(1) nano-diamond with a size of 5nm was purchased commercially, purified by acid washing: with HNO 3 /H 2 SO 4 = 3: 1, refluxing and cleaning the solution for 24 hours, and then evaporating the solution to dryness in a refrigerator for 24 hours;
(2) placing the acid-purified nano-diamond into a tube furnace, heating at 1100 ℃ for 3-10min under the argon atmosphere, wherein the heating rate is 2-10 ℃/min, and then naturally cooling to room temperature;
(3) the treated nano-diamond is kept still, the treatment atmosphere is changed into hydrogen, then the nano-diamond is heated to 800 ℃ and is kept warm for 2 hours, and then the nano-diamond is naturally cooled to the room temperature.
As shown in FIG. 1, TEM image of the prepared sample, sp appeared in the hybridized nanodiamond 2 ,sp 3 A hybrid carbon.
FIG. 2 is an x-ray photoelectron spectrum (C1 s spectrum) of a sample. Some diffraction peaks appear in the spectrum, namely 284.6 eV, 285.5 eV and 286.2 eV, which correspond to sp (sp) respectively 2 Hybridized carbon, sp 3 Hybrid carbon, C-H, functional groups. From the intensity of the peaks in the graph, sp in the hybrid nanodiamond compared to nanodiamond 2 The proportion of carbon increases significantly.
Fig. 3 is a photocatalytic activity test chart of the sample. The test result shows that the photocatalytic activity of the hybrid nano-diamond is far higher than that of the nano-diamond. At one hour of solar irradiation RhB was degraded by about 50%.
FIG. 4 is a test chart of a cycle experiment of the hybrid nano-diamond for photodegradation of RhB, and after three cycle experiments, the hybrid nano-diamond still has good photocatalytic activity, which shows that the prepared material has good photostability.
Example 2
The preparation method of the hybrid nano-diamond comprises the following steps:
(1) nano-diamond with a size of 3nm is purchased commercially, purified by acid washing: with HNO 3 /H 2 SO 4 = 3: 1, refluxing and cleaning for 15h, and then evaporating to dryness in a refrigerator for 48 h;
(2) placing the acid-purified nano-diamond into a tube furnace, heating for 1000 to 3 to 10min under the argon atmosphere at the heating rate of 2 to 10 ℃/min, and then naturally cooling to room temperature;
(3) the treated nano-diamond is kept still, the treatment atmosphere is changed into hydrogen, then the nano-diamond is heated to 780 ℃, the temperature is kept for 2.5h, and then the nano-diamond is naturally cooled to the room temperature.
Example 3
The preparation method of the hybrid nano-diamond comprises the following steps:
(1) nano-diamond with a size of 10nm is purchased commercially, purified by acid washing: with HNO 3 /H 2 SO 4 = 3: 1, refluxing and cleaning the solution for 24 hours, and then evaporating the solution to dryness in a refrigerator for 12 hours;
(2) placing the acid-purified nano-diamond into a tube furnace, heating at 1200 ℃ for 3-10min under the argon atmosphere, wherein the heating rate is 2-10 ℃/min, and then naturally cooling to room temperature;
(3) the treated nano-diamond is kept still, the treatment atmosphere is changed into hydrogen, then the nano-diamond is heated to 750 ℃ and is kept warm for 1.5h, and then the nano-diamond is naturally cooled to room temperature.
Control group
Control refers to RhB solution without photocatalyst. The conditions were otherwise identical to those of example 1, except that no photocatalyst was added.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (3)
1. A preparation method of hybrid nano-diamond applied to photocatalytic degradation of organic matters is characterized by comprising the following steps:
(1) refluxing and cleaning 3nm-10nm of nano-diamond by using a mixed acid solution, and evaporating to dryness by using a refrigerating machine;
(2) placing the acid-washed and purified nano-diamond in a tubular furnace, heating and calcining the nano-diamond in an argon atmosphere, and naturally cooling the nano-diamond to room temperature; wherein the heating temperature is 1000-1200 ℃, and the time is 3-10 min;
(3) changing the atmosphere of the tube furnace in the step (2) into hydrogen, heating and calcining again, and naturally cooling to room temperature to obtain the product with sp 2 、sp 3 Hybrid nanodiamonds of hybrid carbon; wherein the heating temperature is 750-800 ℃, and the time is 1.5-2.5 h.
2. The preparation method of the hybrid nano-diamond applied to photocatalytic degradation of organic matters according to claim 1, is characterized in that: the mixed acid is prepared from the following components in a molar ratio of 3: 1 HNO 3 And H 2 SO 4 The reflux cleaning time is 12-24h, and the drying time is 12-48 h.
3. The application of the hybrid nano-diamond prepared by the method of claim 1 or 2 and applied to photocatalytic degradation of organic matters in photocatalytic degradation of rhodamine B.
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CN101029359A (en) * | 2007-04-10 | 2007-09-05 | 天津大学 | Method for producing nano-diamond reinforced copper-base composite material by chemical codeposition |
CN102965666A (en) * | 2012-11-27 | 2013-03-13 | 郑州大学 | Flexible substrate nanometer diamond film and preparation method thereof |
CN110643972A (en) * | 2019-09-29 | 2020-01-03 | 哈尔滨工业大学 | Preparation method and application of gold nanoparticle modified boron-doped diamond electrode |
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WO2007133765A2 (en) * | 2006-05-15 | 2007-11-22 | Drexel University | Process of purifying nanodiamond compositions and applications thereof |
US20090110626A1 (en) * | 2007-10-02 | 2009-04-30 | Hemley Russell J | Low Pressure Method of Annealing Diamonds |
FR3007019B1 (en) * | 2013-06-12 | 2017-03-17 | Commissariat Energie Atomique | NANOMATERIAL GRAPHICS IN THE FORM OF CARBON ONIONS, PROCESS FOR THEIR PREPARATION AND THEIR USE |
WO2016126912A1 (en) * | 2015-02-06 | 2016-08-11 | The Government Of The United States Of America, As Represented By The Secretary Of The Navy | Defects annealing and impurities activation in semiconductors at thermodynamically non-stable conditions |
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CN101029359A (en) * | 2007-04-10 | 2007-09-05 | 天津大学 | Method for producing nano-diamond reinforced copper-base composite material by chemical codeposition |
CN102965666A (en) * | 2012-11-27 | 2013-03-13 | 郑州大学 | Flexible substrate nanometer diamond film and preparation method thereof |
CN110643972A (en) * | 2019-09-29 | 2020-01-03 | 哈尔滨工业大学 | Preparation method and application of gold nanoparticle modified boron-doped diamond electrode |
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