CN105833882A - Performance enhanced Fenton catalyst and application thereof - Google Patents
Performance enhanced Fenton catalyst and application thereof Download PDFInfo
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- CN105833882A CN105833882A CN201610207074.1A CN201610207074A CN105833882A CN 105833882 A CN105833882 A CN 105833882A CN 201610207074 A CN201610207074 A CN 201610207074A CN 105833882 A CN105833882 A CN 105833882A
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- Prior art keywords
- titanium dioxide
- additive
- fenton
- ferrite
- microsphere
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- 239000003054 catalyst Substances 0.000 title claims abstract description 37
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 82
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 39
- 239000004005 microsphere Substances 0.000 claims abstract description 25
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000010865 sewage Substances 0.000 claims abstract description 4
- 239000000654 additive Substances 0.000 claims description 23
- 230000000996 additive effect Effects 0.000 claims description 23
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 16
- 239000002086 nanomaterial Substances 0.000 claims description 11
- 239000007787 solid Substances 0.000 claims description 8
- 229910052748 manganese Inorganic materials 0.000 claims description 4
- 229910017163 MnFe2O4 Inorganic materials 0.000 claims description 2
- 239000000758 substrate Substances 0.000 claims description 2
- 238000002474 experimental method Methods 0.000 abstract description 4
- 238000006555 catalytic reaction Methods 0.000 abstract 1
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 21
- 239000011572 manganese Substances 0.000 description 20
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 17
- 230000015556 catabolic process Effects 0.000 description 12
- 238000006731 degradation reaction Methods 0.000 description 12
- 238000003756 stirring Methods 0.000 description 9
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 7
- 239000002243 precursor Substances 0.000 description 7
- 230000003197 catalytic effect Effects 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000001354 calcination Methods 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 239000010936 titanium Substances 0.000 description 5
- 229910021577 Iron(II) chloride Inorganic materials 0.000 description 4
- 229910021380 Manganese Chloride Inorganic materials 0.000 description 4
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 description 4
- 238000003837 high-temperature calcination Methods 0.000 description 4
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 4
- 239000011565 manganese chloride Substances 0.000 description 4
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 3
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 3
- 239000001099 ammonium carbonate Substances 0.000 description 3
- 229960000935 dehydrated alcohol Drugs 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 3
- 229940012189 methyl orange Drugs 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- 241000790917 Dioxys <bee> Species 0.000 description 1
- 239000012028 Fenton's reagent Substances 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000007172 homogeneous catalysis Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Classifications
-
- 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
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/889—Manganese, technetium or rhenium
- B01J23/8892—Manganese
-
- 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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- B01J35/33—
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- 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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
-
- 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
- C02F2101/40—Organic compounds containing sulfur
-
- 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
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
Abstract
The invention discloses a performance enhanced Fenton catalyst. The Fenton catalyst is prepared from titanium dioxide/manganese-doped ferrite microspheres. Experiments confirm that the Fenton catalyst prepared from the titanium dioxide/manganese-doped ferrite microspheres has the characteristics of good morphology, excellent Fenton catalysis performance and large cycle use frequency, is hopeful to play a great role in the environmentally-friendly sewage treatment process as an ideal catalyst, and has wide application prospect.
Description
Technical field
The present invention relates to catalyst and the application thereof of a kind of performance enhancement, particularly relate to a kind of micro-by titanium dioxide/additive Mn ferrite
Fenton catalyst prepared by ball and application.
Background technology
Along with the fast development of modern industry, water pollution problem is increasingly serious.Wherein, organic pollutant have kind many,
The features such as toxicity is big, difficult decomposition, are the major pollutants in current waste water.At present, the method processing organic pollution mainly has
Absorption method, biological degradation method, light degradation method and Fenton-catalytic degradation method etc..
Wherein, Fenton-catalytic degradation method because its degradation efficiency is high, equipment requirements is low, simple operation and other advantages and enjoy favor.But
Homogeneous Fenton-reagent (Fe2+/H2O2) when processing organic pollution, there is pH value range narrow, and be attended by ferrum
The drawbacks such as the generation of mud.Based on this, the recent focus of people has turned to heterocatalysis from homogeneous catalysis.It is said that in general, out-phase
Fenton catalyst has not only widened the range of pH value, overcomes the drawback producing ferrum mud in homogeneous Fenton's reaction, simultaneously
Also there is the rear catalyst in reaction end can be recycled, thus the advantage reducing processing cost.
At present, apply additive Mn ferrite nano material to carry the document of high catalytic activity by frequency in all kinds of out-phase fenton catalyst
Numerous report, but to recycle number of times the most limited for the ferrite of additive Mn, still can not meet the industrial requirement of fast development.
Through retrieval, yet there are no report about having the document of fenton catalyst and the application utilizing titanium dioxide/additive Mn ferrite microsphere to prepare
Road.
Summary of the invention
For the deficiencies in the prior art, the problem to be solved in the present invention is to provide fenton catalyst and the application thereof of a kind of performance enhancement
With application.
The technical scheme is that " ferrimanganic carbonate precursor ferrimanganic carbonate precursor microsphere/titanium dioxide is received in utilization
Rice structure binary metal oxide/titanium dioxide heterogeneous structure " thinking, by adjust, optimize preparation technology, overcome
Fe2+Oxidizable problem, synthesizes single dispersing, spherical ferrimanganic carbonate nano material, and then loads dioxy on this basis
Changing titanium nanostructured, and further determine that exploration Technology for Heating Processing, final acquisition is magnetic and can recycle manganese repeatedly
Dopen Nano ferrite/titanium dioxide heterogeneous structure nano material, and thus material prepares fenton catalyst.
The fenton catalyst of performance enhancement of the present invention, is made up of titanium dioxide/additive Mn ferrite microsphere, wherein, described
Titanium dioxide/additive Mn ferrite microsphere, is with single dispersing, spherical ferrimanganic carbonate nano material as substrate, area load one
Layer titanium dioxide nanostructure is constituted;Described ferrimanganic carbonate nano material is that a diameter of 250nm~450nm, solid manganese are mixed
Miscellaneous ferrite microsphere, described titanium dioxide nanostructure is the titanium dioxide being grown on microsphere surface shape floweriness piece shape structure, its
Wall thickness 1nm~3nm, described additive Mn ferrite microsphere is the hollow knot of core and the titanium dioxide layer composition of shape floweriness piece shape structure
Structure is collectively forming the ferrite heterojunction structure of titanium dioxide/additive Mn, in mass, TiO2:MnFe2O4=0.01~1.
The preparation method of the fenton catalyst of above-mentioned performance enhancement, is with NH4HCO3、MnCl2·4H2O、FeCl2·4H2O、
C4H4K2O11Ti, ethylene glycol, diglycol are raw material, use solvent structure ferrimanganic carbonate forerunner's microsphere, then lead to
Cross hydro-thermal method in microsphere surface carried titanium dioxide nanostructured, then the presoma of carried titanium dioxide carried out high-temperature calcination,
Obtain surface configuration floweriness piece shape structure and magnetic titanium dioxide/additive Mn ferrite heterojunction structure microsphere, is performance
The fenton catalyst strengthened.
Wherein: the temperature of the hydro-thermal in two one-step hydrothermals is preferably 120 DEG C~230 DEG C, and the response time is preferably 2h~20h;High temperature
The temperature of calcining is preferably 400 DEG C~1000 DEG C, and calcination time is preferably 2h~10h.
Fenton catalyst of the present invention processes the application in sewage under Fenton-like system.
Monodisperse magnetic titanium dioxide in fenton catalyst disclosed by the invention/additive Mn ferrite microsphere has good pattern,
Excellent Fenton catalytic performance, can recycle the multiple good characteristic such as often, can as the preferable catalyst of process sewage,
It is expected to during environmental protection treatment play a significant role.
The ferritic energy level of additive Mn, by the method for carried titanium dioxide on the ferrite of additive Mn, is adjusted by the present invention
Control, thus further promote Fe3+/Fe2+Conversion, it is thus achieved that the fenton catalyst of performance enhancement.The present invention utilizes structure first
The mode making heterojunction structure significantly improves the degradation property of out-phase fenton catalyst and recycles performance, the additive Mn ferrum obtained
Oxysome/titanium dioxide heterogeneous structure nano material has that magnetic response is strong, pattern good, Fenton catalytic performance is excellent, recycle time
The plurality of advantages such as number is many, industrial applications has a extensive future.
Accompanying drawing explanation
Fig. 1 is the stereoscan photograph of the ferrimanganic carbonate microsphere in fenton catalyst of the present invention.
Fig. 2 is the stereoscan photograph of the ferrimanganic carbonate microsphere having loaded titanium dioxide.
Fig. 3 is the stereoscan photograph of the titanium dioxide in fenton catalyst of the present invention/additive Mn ferrite microsphere.
Fig. 4 is the X ray diffracting spectrum of the titanium dioxide in fenton catalyst of the present invention/additive Mn ferrite microsphere.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the protection content of the present invention is further elaborated.
Embodiment 1
The preparation of the fenton catalyst of performance enhancement of the present invention
1. taking organic solvent ethylene glycol, volume is 156mL, pours in the hydrothermal reaction kettle of 200mL, addition ammonium hydrogencarbonate 7g,
MnCl2·4H2O 0.6590g、FeCl2·4H2O 1.3255g, compactedness controls 50%~80%, and stirs, puts into
In drying baker, making hydrothermal temperature control at 200 ± 10 DEG C, react 12h, reaction naturally cools to room temperature, products therefrom after terminating
Repeatedly rinse to neutrality with dehydrated alcohol, then sucking filtration, be dried, the yellow-brown solid obtained be ferrimanganic carbonate precursor (see
Fig. 1).
2. by 0.7082g C4H4K2O11Ti joins in 20mL deionized water stirring to dissolving, and adds 60mL mono-and contracts two
Ethylene glycol, continues stirring 0.5h, is transferred in 100mL reactor, adds the ferrimanganic carbonate precursor of 0.17g~0.5g.
Being put into by this reactor and be heated to 175 DEG C in baking oven, the response time is 2h, it is thus achieved that the predecessor of carried titanium dioxide.
3. the predecessor of carried titanium dioxide carries out high-temperature calcination, and temperature 700 DEG C, calcination time is 3h, is cooled to room temperature
After the solid that obtains be have Fenton catalytic performance titanium dioxide/additive Mn ferrite microsphere (see Fig. 2,3), be the present invention
The fenton catalyst of described performance enhancement.
It is 0.0049mol/L by above-mentioned fenton catalyst at concentration of hydrogen peroxide, in the methyl orange degradation experiment under conditions of 60 DEG C,
30min degradation rate reaches 98%.
Embodiment 2
The preparation of the fenton catalyst of performance enhancement of the present invention
1. taking organic solvent ethylene glycol, volume is 156mL, pours in the hydrothermal reaction kettle of 200mL, addition ammonium hydrogencarbonate 7g,
MnCl2·4H2O 0.6590g、FeCl2·4H2O 1.3255g, compactedness controls 50%~80%, and stirs,
Putting in drying baker, make hydrothermal temperature control at 200 ± 10 DEG C, react 12h, reaction naturally cools to room temperature after terminating, institute
Product dehydrated alcohol repeatedly rinse to neutrality, then sucking filtration, be dried, the yellow-brown solid obtained is ferrimanganic carbonate forerunner
Body (see Fig. 1).
2. by 0.7082g C4H4K2O11Ti joins in 20mL deionized water stirring to dissolving, and adds 60mL mono-and contracts two
Ethylene glycol, continues stirring 0.5h, is transferred in 100mL reactor, adds the ferrimanganic carbonate precursor of 0.17g~0.5g.
Being put into by this reactor and be heated to 230 DEG C in baking oven, the response time is 2h, it is thus achieved that the predecessor of carried titanium dioxide.
3. the predecessor of carried titanium dioxide carries out high-temperature calcination, and temperature 400 DEG C, calcination time is 3h, is cooled to room temperature
After the solid that obtains be the titanium dioxide/additive Mn ferrite microsphere with Fenton catalytic performance, be performance of the present invention and increase
Strong fenton catalyst.
It is 0.0049mol/L by above-mentioned fenton catalyst at concentration of hydrogen peroxide, in the methyl orange degradation experiment under conditions of 60 DEG C,
30min degradation rate reaches 95%.
Embodiment 3
The preparation of the fenton catalyst of performance enhancement of the present invention
1. taking organic solvent ethylene glycol, volume is 156mL, pours in the hydrothermal reaction kettle of 200mL, addition ammonium hydrogencarbonate 7g,
MnCl2·4H2O 0.6590g、FeCl2·4H2O 1.3255g, compactedness controls 50%~80%, and stirs, puts into
In drying baker, making hydrothermal temperature control at 200 ± 10 DEG C, react 12h, reaction naturally cools to room temperature, products therefrom after terminating
Repeatedly rinse to neutrality with dehydrated alcohol, then sucking filtration, be dried, the yellow-brown solid obtained be ferrimanganic carbonate precursor (see
Fig. 1).
2. by 0.7082g C4H4K2O11Ti joins in 20mL deionized water stirring to dissolving, and adds 60mL mono-and contracts two
Ethylene glycol, continues stirring 0.5h, is transferred in 100mL reactor, adds the ferrimanganic carbonate precursor of 0.17g~0.5g.
Being put into by this reactor and be heated to 120 DEG C in baking oven, the response time is 2h, it is thus achieved that the predecessor of carried titanium dioxide.
3. the predecessor of carried titanium dioxide carries out high-temperature calcination, and temperature 1000 DEG C, calcination time is 3h, after being cooled to room temperature
The solid obtained is the titanium dioxide/additive Mn ferrite microsphere with Fenton catalytic performance, is performance enhancement of the present invention
Fenton catalyst.
It is 0.0049mol/L by above-mentioned fenton catalyst at concentration of hydrogen peroxide, in the methyl orange degradation experiment under conditions of 60 DEG C,
30min degradation rate reaches 90%.
Claims (2)
1. the fenton catalyst of a performance enhancement, it is characterised in that: described catalyst is by titanium dioxide/additive Mn ferrite microsphere
Making, wherein, described titanium dioxide/additive Mn ferrite microsphere, is to be with single dispersing, spherical ferrimanganic carbonate nano material
Substrate, area load layer of titanium dioxide nanostructured is constituted;Described ferrimanganic carbonate nano material is a diameter of
250nm~450nm, solid additive Mn ferrite microsphere, described titanium dioxide nanostructure is to be grown on microsphere surface shape
The titanium dioxide of floweriness piece shape structure, its wall thickness 1nm~3nm, described additive Mn ferrite microsphere is that core is tied with shape floweriness piece shape
The hollow structure that the titanium dioxide layer of structure is constituted is collectively forming the ferrite heterojunction structure of titanium dioxide/additive Mn, in mass,
TiO2:MnFe2O4=0.01~1.
2. the fenton catalyst described in claim 1 processes the application in sewage under Fenton-like system.
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CN105833882A true CN105833882A (en) | 2016-08-10 |
CN105833882B CN105833882B (en) | 2018-08-24 |
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Cited By (2)
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CN109794280A (en) * | 2019-02-28 | 2019-05-24 | 山东大学 | A kind of magnetic Nano g-C3N4/MnFe2O4The preparation method of catalyst |
CN111569899A (en) * | 2020-06-03 | 2020-08-25 | 苏州科技大学 | MnFe2O4-TiO2-preparation method of graphene aerogel |
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CN109794280A (en) * | 2019-02-28 | 2019-05-24 | 山东大学 | A kind of magnetic Nano g-C3N4/MnFe2O4The preparation method of catalyst |
CN111569899A (en) * | 2020-06-03 | 2020-08-25 | 苏州科技大学 | MnFe2O4-TiO2-preparation method of graphene aerogel |
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