CN113332983A - Porous rod-shaped Fe21.34O32Preparation method of/C nanorod composite material - Google Patents
Porous rod-shaped Fe21.34O32Preparation method of/C nanorod composite material Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 45
- 239000002073 nanorod Substances 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims description 8
- 239000011941 photocatalyst Substances 0.000 claims abstract description 31
- 239000002243 precursor Substances 0.000 claims abstract description 27
- 238000002360 preparation method Methods 0.000 claims abstract description 23
- 238000001354 calcination Methods 0.000 claims abstract description 21
- 229910021577 Iron(II) chloride Inorganic materials 0.000 claims abstract description 16
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- 238000001816 cooling Methods 0.000 claims abstract description 8
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- 230000008569 process Effects 0.000 claims description 2
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- 230000001699 photocatalysis Effects 0.000 abstract description 12
- 239000003054 catalyst Substances 0.000 abstract description 7
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- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 150000003839 salts Chemical class 0.000 abstract description 2
- 238000005245 sintering Methods 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 33
- 239000000203 mixture Substances 0.000 description 19
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical class OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 description 16
- 230000003197 catalytic effect Effects 0.000 description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 9
- 230000004048 modification Effects 0.000 description 8
- 238000012986 modification Methods 0.000 description 8
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- 239000004065 semiconductor Substances 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
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- 229910021641 deionized water Inorganic materials 0.000 description 5
- 239000012467 final product Substances 0.000 description 5
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- 238000002441 X-ray diffraction Methods 0.000 description 2
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- 238000001308 synthesis method Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
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- 230000004075 alteration Effects 0.000 description 1
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical class O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
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- 230000005764 inhibitory process Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
-
- B01J35/39—
-
- B01J35/40—
-
- B01J35/60—
-
- B01J35/61—
-
- 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
- B01J37/082—Decomposition and pyrolysis
-
- 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
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/022—Preparation of aqueous ammonia solutions, i.e. ammonia water
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
Abstract
The invention relates to the technical field of catalysts, and provides porous rod-shaped Fe aiming at the problem of high cost of a noble metal doped modified photocatalyst21.34O32The preparation method of the/C nanorod composite material comprises the following steps: using NTA and FeCl2·4H2Preparing a precursor by an O hydrothermal method, calcining the precursor in inert gas at the temperature of 450-500 ℃ for 2-2.5 hours, and cooling to obtain rod-shaped porous Fe after the calcination21.34O32a/C nano-rod composite photocatalyst. The invention is composed of NTA and metal salt FeCl2·4H2O is prepared by firstly hydrothermal and then sintering in a tube furnace, the condition is mild, the purity is good, and the prepared rod-shaped porous Fe21.34O32the/C nanorod composite photocatalyst has high photocatalytic activity.
Description
Technical Field
The invention relates to the technical field of catalysts, in particular to porous rod-shaped Fe21.34O32A preparation method of a/C nano-rod composite material.
Background
In recent years, the problems of environmental pollution and energy shortage have become increasingly serious, and research and development of various novel energy techniques and equipment have been intensively conducted. The photocatalytic technology has the advantages of environmental friendliness, high chemical energy and the like, and is widely considered as an important way for solving the problems of environmental pollution and energy crisis. With the development of industrialization, the problems of energy shortage and environmental pollution become more serious, which forces people to continuously search clean and sustainable energy to improve the environmental and energy problems. Ammonia is one of the essential raw materials for industrial development and agriculture. The photocatalytic synthesis of ammonia is one of the important approaches with good development prospect and application prospect, can greatly realize the conversion from solar energy to chemical energy, and has the characteristics of environmental friendliness, high stability and the like. Fe is one of the elements that is currently of great interest and promising for the fabrication of photocatalysts. The photocatalyst has the advantages of high photocatalytic performance, high oxidation efficiency, no toxicity, low cost, environmental friendliness and the like, so that the photocatalyst is widely applied to the aspects of photoelectric conversion, hydrogen production by decomposing water to produce oxygen, pollutant degradation and the like.
However, the semiconductor material prepared by a single traditional semiconductor mostly has the defects of large forbidden band width, unobvious adsorption performance and the like, and the utilization efficiency of the semiconductor material to sunlight is extremely low (only about five percent), so that the large-scale application of the semiconductor material in the technical field of photocatalysis is hindered; in addition, the photo-generated electron-hole pairs are very easy to recombine under the irradiation of light, thereby reducing the photocatalytic efficiency thereof, which is one of the major disadvantages of the photo-generated electron-hole pairs as a photocatalyst. Therefore, in order to solve the above problems, a series of strategies are proposed to modify the above photocatalyst, for example, patent CN112058308B discloses an organic-inorganic composite formaldehyde catalytic composition, a preparation method thereof, and an air purification filter element, which comprises the following components in parts by weight: 10-50 parts of modified catalyst, 30-50 parts of modified bentonite and 40-100 parts of high molecular organic polymer. According to the invention, the noble metal-doped composite photocatalyst is carried by the rare earth element modified carrier, and a microenvironment is formed on the surface of the catalyst by the rare earth metal solid ions, so that the inhibition of water vapor on the catalytic activity in the reaction process can be effectively avoided, and the synergistic effect between the two photocatalysts and Pt can be enhanced, so that formaldehyde is completely catalytically converted into carbon dioxide and water at room temperature, the addition of noble metals is remarkably reduced, and the performance of catalytic oxidation of formaldehyde at room temperature is not reduced. The use of precious metals also raises costs. Besides the noble metal loading modification, metal oxide doping modification, semiconductor composite modification, ion doping modification and the like are also available, and in the strategy methods, the photocatalyst can generate synergistic action with the noble metal loading modification, so that the photocatalytic activity is well enhanced, however, the defects of uncontrollable content, destructive conjugated system and the like limit the application of the noble metal loading modification, the semiconductor composite modification, the ion doping modification and the like. Therefore, there is a need to find suitable photocatalysts to improve their photocatalytic performance.
Disclosure of Invention
The invention provides porous rod-shaped Fe in order to solve the problem of high cost of a noble metal doped modified photocatalyst21.34O32The preparation method of the/C nano-rod composite material comprises the following steps of mixing NTA and metal salt FeCl2·4H2The O is prepared by firstly hydrothermal and then sintering in a tube furnace, the condition is mild, the purity is good, the method is suitable for large-scale production, and the prepared rod-shaped porous Fe21.34O32the/C nanorod composite photocatalyst has high photocatalytic activity.
In order to achieve the purpose, the invention adopts the following technical scheme:
porous rod-shaped Fe21.34O32The preparation method of the/C nanorod composite material comprises the following steps: using NTA (nitrilotriacetic acid) and FeCl2·4H2Preparing a precursor by an O hydrothermal method, calcining the precursor in inert gas at the temperature of 450-500 ℃ for 2-2.5 hours, and cooling to obtain rod-shaped porous Fe after the calcination21.34O32a/C nano-rod composite photocatalyst.
Rod-like porous Fe prepared by the synthesis method provided by the invention21.34O32the/C nanorod composite photocatalyst has high photocatalytic activity, particularly under the driving condition of visible light, the porous loose unique structure of the composite photocatalyst enables the composite photocatalyst to have a high specific area and high-density catalytic active centers, and the porous structure enables incident light to be reflected and scattered for multiple times inside a pore channel, so that the light absorption rate is improved, and the utilization efficiency of the visible light is obviously improved. The synthesis method provided by the invention has the characteristics of mild conditions, good purity and the like, and is suitable for industrial large-scale production and application.
Preferably, NTA and FeCl2·4H2The molar ratio of O is (0.5-2)):1。
Preferably, NTA and FeCl2·4H2The mixing process of O is as follows: dispersing NTA in water, adding FeCl2·4H2And O, stirring to dissolve, adding isopropanol, and stirring uniformly.
Preferably, the reaction temperature of the hydrothermal method is 160-200 ℃, and the reaction time is 4-8 h.
Preferably, the reaction product obtained by the hydrothermal method is firstly centrifuged to obtain precipitate, and the precipitate is washed and dried to obtain the precursor.
Preferably, the washing is carried out by washing with water to neutrality and then washing with absolute ethyl alcohol for 1-3 times.
Preferably, the drying condition is drying at 50-70 ℃ for 10-12 hours under vacuum.
Preferably, the calcination of the precursor is carried out in a tube furnace, and the temperature rise rate of the tube furnace is controlled to be 3-5 ℃/min.
Therefore, the beneficial effects of the invention are as follows: porous rod-like Fe prepared by the invention21.34O32The porous material has a high specific area and has high-density catalytic active centers, and the porous structure enables incident light to be reflected and scattered for multiple times inside a pore channel, so that the light absorption rate is improved.
Drawings
FIG. 1 is a schematic view showing rod-shaped porous Fe obtained in examples 1 to 3 of the present invention21.34O32XRD pattern of/C nano-rod composite photocatalyst.
FIG. 2 is a schematic view showing a rod-shaped porous Fe obtained in example 1 of the present invention21.34O32a/C nanorod composite photocatalyst microscopic morphology image by scanning electron microscopy.
FIG. 3 is a schematic view showing a rod-shaped porous Fe obtained in example 1 of the present invention21.34O32A transmission electron microscope microscopic morphology image of the/C nanorod composite photocatalyst.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples.
In the present invention, unless otherwise specified, all the raw materials and equipment used are commercially available or commonly used in the art, and the methods in the examples are conventional in the art unless otherwise specified.
Example 1
Porous rod-shaped Fe21.34O32The preparation method of the/C nanorod composite material comprises the following steps:
(1) preparing a precursor: in a beaker containing 10mL of deionized water, 0.1911g of NTA white powder was added and dispersed, and 0.20g of FeCl was added2·4H2O, NTA and FeCl2·4H2The molar ratio of O is 1:1, the mixture is magnetically stirred for 10 minutes at normal temperature until the mixture is completely dissolved, then 20ml of isopropanol is added, the mixture is magnetically stirred for half an hour at normal temperature until the mixture is uniform, the mixture is moved into a high-pressure reaction kettle, and the mixture is put into an oven to react for 6 hours at 180 ℃; and centrifuging the reaction product by using a high-speed centrifuge at the rotating speed of 4000rpm to obtain a precipitate, washing the precipitate for 3 times to be neutral, then washing the precipitate for 3 times by using absolute ethyl alcohol, and drying the washed precipitate in a vacuum oven at the temperature of 60 ℃ for 12 hours to obtain a precursor.
(2) Preparation of Fe21.34O32C nano rod: calcining the precursor in a tube furnace at a heating rate of 5 ℃/min for 90 minutes to 450 ℃, calcining in argon for 2 hours, and naturally cooling to obtain the final product, namely the rod-shaped porous Fe21.34O32a/C nano-rod composite photocatalyst.
Observation of the obtained porous rod-like Fe21.34O32The microstructure of the/C nanorod composite photocatalyst obtains the structure diagrams shown in figures 2 and 3. As can be seen from FIG. 2, it has a good and stable micro-morphology in which Fe is rod-like21.34O32the/C nano rods have uniform sizes and are better combined; as can be seen from FIG. 3, it has a good micro-morphology, uniform distribution and obvious porosity.
Example 2
Porous rod-shaped Fe21.34O32The preparation method of the/C nanorod composite material comprises the following steps:
(1) preparing a precursor: in a 10mL deionized water beaker was added 0.0994g NTA white powder first and dispersed, then0.21g FeCl was added2·4H2O, NTA and FeCl2·4H2The molar ratio of O is 1:2, the mixture is magnetically stirred for 10 minutes at normal temperature until the mixture is completely dissolved, then 20ml of isopropanol is added, the mixture is magnetically stirred for half an hour at normal temperature until the mixture is uniform, the mixture is moved into a high-pressure reaction kettle, and the mixture is put into an oven to react for 6 hours at 180 ℃; centrifuging the reaction product by using a high-speed centrifuge at the rotating speed of 4000rpm to obtain a precipitate, washing the precipitate for 3 times to be neutral, then washing the precipitate for 3 times by using absolute ethyl alcohol, and drying the washed precipitate in a vacuum oven at the temperature of 60 ℃ for 12 hours to obtain a precursor;
(2) preparation of Fe21.34O32C nano rod: calcining the precursor in a tube furnace at a heating rate of 5 ℃/min for 90 minutes to 450 ℃, calcining in argon for 2 hours, and naturally cooling to obtain the final product, namely the rod-shaped porous Fe21.34O32a/C nano-rod composite photocatalyst.
Example 3
Porous rod-shaped Fe21.34O32The preparation method of the/C nanorod composite material comprises the following steps:
(1) preparing a precursor: in a beaker containing 10mL of deionized water, 0.38g of NTA white powder was added and dispersed, and 0.20g of FeCl was added2·4H2O, NTA and FeCl2·4H2The molar ratio of O is 2:1, the mixture is magnetically stirred for 10 minutes at normal temperature until the mixture is completely dissolved, then 20ml of isopropanol is added, the mixture is magnetically stirred for half an hour at normal temperature until the mixture is uniform, the mixture is moved into a high-pressure reaction kettle, and the mixture is put into an oven to react for 6 hours at 180 ℃; centrifuging the reaction product by using a high-speed centrifuge at the rotating speed of 4000rpm to obtain a precipitate, washing the precipitate for 3 times to be neutral, then washing the precipitate for 3 times by using absolute ethyl alcohol, and drying the washed precipitate in a vacuum oven at the temperature of 60 ℃ for 12 hours to obtain a precursor;
(2) preparation of Fe21.34O32C nano rod: calcining the precursor in a tube furnace at a heating rate of 5 ℃/min for 90 minutes to 450 ℃, calcining in argon for 2 hours, and naturally cooling to obtain the final product, namely the rod-shaped porous Fe21.34O32a/C nano-rod composite photocatalyst.
FIG. 1 shows a rod-shaped polymer obtained in examples 1 to 3 of the present inventionFe pore21.34O32XRD pattern of/C nano-rod composite photocatalyst. As can be seen from FIG. 1, the porous rod-like Fe produced by the present invention21.34O32the/C nanorod composite photocatalysis material has good crystallinity, does not generate other impurities, and has high purity.
Example 4
Porous rod-shaped Fe21.34O32The preparation method of the/C nanorod composite material comprises the following steps:
(1) preparing a precursor: in a beaker containing 10mL of deionized water, 0.1911g of NTA white powder was added and dispersed, and 0.20g of FeCl was added2·4H2O, magnetically stirring for 10 minutes at normal temperature until the solution is completely dissolved, then adding 20ml of isopropanol, magnetically stirring for half an hour at normal temperature until the solution is uniform, transferring the solution to a high-pressure reaction kettle, putting the reaction kettle into an oven, and reacting for 8 hours at 160 ℃; and centrifuging the reaction product by using a high-speed centrifuge at the rotating speed of 4000rpm to obtain a precipitate, washing the precipitate for 3 times to be neutral, then washing the precipitate for 1 time by using absolute ethyl alcohol, and drying the washed precipitate in a vacuum oven at the temperature of 50 ℃ for 12 hours to obtain a precursor.
(2) Preparation of Fe21.34O32C nano rod: calcining the precursor in a tube furnace at a heating rate of 3 ℃/min for 150 minutes to 450 ℃, calcining in argon for 2.5 hours, and naturally cooling to obtain the final product, namely the rod-shaped porous Fe21.34O32a/C nano-rod composite photocatalyst.
Example 5
Porous rod-shaped Fe21.34O32The preparation method of the/C nanorod composite material comprises the following steps:
(1) preparing a precursor: in a beaker containing 10mL of deionized water, 0.1911g of NTA white powder was added and dispersed, and 0.20g of FeCl was added2·4H2O, magnetically stirring for 10 minutes at normal temperature until the solution is completely dissolved, then adding 20ml of isopropanol, magnetically stirring for half an hour at normal temperature until the solution is uniform, transferring the solution to a high-pressure reaction kettle, putting the reaction kettle into an oven, and reacting for 4 hours at 200 ℃; centrifuging the reaction product at 4000rpm with high speed centrifuge to obtain precipitate, washing the precipitate with water for 3 times to neutral, washing with anhydrous ethanol for 2 times, and collecting the precipitateAnd drying in a vacuum oven at 70 ℃ for 10 hours to obtain the precursor.
(2) Preparation of Fe21.34O32C nano rod: calcining the precursor in a tube furnace at a heating rate of 5 ℃/min for 100 minutes to 500 ℃, calcining in argon for 2 hours, and naturally cooling to obtain the final product, namely the rod-shaped porous Fe21.34O32a/C nano-rod composite photocatalyst.
Example 6
The difference from example 1 is NTA and FeCl2·4H2The molar ratio of O is 3: 1.
Example 7
The difference from example 1 is NTA and FeCl2·4H2The molar ratio of O is 1: 3.
Comparative example 1
The difference from example 1 is that the calcination temperature of the precursor was 700 ℃.
Comparative example 2
The difference from example 1 is that the calcination temperature of the precursor was 400 ℃.
Performance testing
The rod-shaped porous Fe obtained in example 1 was used21.34O32the/C nanorod composite photocatalyst is used for the reaction of synthesizing ammonia by photocatalytic nitrogen, the dosage of the catalyst is 40mg, the solvent is 60mL of water, and the trend of the change of the yield of ammonium radicals along with time is shown in the following table, which shows that the catalyst has excellent catalytic performance.
Rod-shaped porous Fe prepared by examples 2-7 and comparative examples 1-221.34O32The same photocatalytic reaction is carried out on the/C nanorod composite photocatalyst, and the catalytic performance is shown in the following table.
From the perspective of catalytic effectiveness, examples 1-7 are catalyzed relative to conventional iron oxideThe catalyst and the catalytic performance are greatly improved. Example 6 FeCl relative to example 12·4H2The amount of O is low, and the catalytic performance is reduced because of Fe2+Acts to increase the specific surface area, but as can be seen from example 7, with Fe2+The addition amount is further increased, and the catalytic performance is not greatly changed, so NTA and FeCl are added2·4H2The molar ratio of O is preferably (0.5-2): 1. It can be seen from comparative examples 1 and 2 that the calcination temperature also has an effect on the catalytic performance, and the catalytic performance of comparative example 1 is reduced compared to example 1, presumably because too high a temperature causes blocking, affecting the porous structure.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (8)
1. Porous rod-shaped Fe21.34O32The preparation method of the/C nanorod composite material is characterized by comprising the following steps of: using NTA and FeCl2·4H2Preparing a precursor by an O hydrothermal method, calcining the precursor in inert gas at the temperature of 450-500 ℃ for 2-2.5 hours, and cooling to obtain rod-shaped porous Fe after the calcination21.34O32a/C nano-rod composite photocatalyst.
2. Porous rod-shaped Fe according to claim 121.34O32The preparation method of the/C nano-rod composite material is characterized in that NTA and FeCl2·4H2The molar ratio of O is (0.5-2) to 1.
3. According to the rightA porous rod-like Fe as claimed in claim 1 or 221.34O32The preparation method of the/C nano-rod composite material is characterized in that NTA and FeCl2·4H2The mixing process of O is as follows: dispersing NTA in water, adding FeCl2·4H2And O, stirring to dissolve, adding isopropanol, and stirring uniformly.
4. Porous rod-shaped Fe according to claim 121.34O32The preparation method of the/C nanorod composite material is characterized in that the reaction temperature of the hydrothermal method is 160-200 ℃, and the reaction time is 4-8 h.
5. Porous rod-shaped Fe according to claim 121.34O32The preparation method of the/C nanorod composite material is characterized in that a reaction product obtained by a hydrothermal method is firstly centrifuged to obtain a precipitate, and the precipitate is washed and dried to obtain a precursor.
6. Porous rod-shaped Fe according to claim 521.34O32The preparation method of the/C nanorod composite material is characterized in that washing is carried out for 1-3 times after water washing is carried out to be neutral.
7. A porous rod-like Fe according to claim 5 or 621.34O32The preparation method of the/C nanorod composite material is characterized in that the drying condition is that the composite material is dried for 10-12 hours at 50-70 ℃ under vacuum.
8. Porous rod-shaped Fe according to claim 121.34O32The preparation method of the/C nanorod composite material is characterized in that the calcination of the precursor is carried out in a tubular furnace, and the temperature rise speed of the tubular furnace is controlled to be 3-5 ℃/min.
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