CN111167432A - Cerium oxide-hydrotalcite composite catalyst, preparation method and application - Google Patents
Cerium oxide-hydrotalcite composite catalyst, preparation method and application Download PDFInfo
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- CN111167432A CN111167432A CN202010143898.3A CN202010143898A CN111167432A CN 111167432 A CN111167432 A CN 111167432A CN 202010143898 A CN202010143898 A CN 202010143898A CN 111167432 A CN111167432 A CN 111167432A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 58
- 229960001545 hydrotalcite Drugs 0.000 title claims abstract description 55
- 229910001701 hydrotalcite Inorganic materials 0.000 title claims abstract description 55
- 239000002131 composite material Substances 0.000 title claims abstract description 50
- 229910052684 Cerium Inorganic materials 0.000 title claims abstract description 38
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000000243 solution Substances 0.000 claims description 165
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 105
- 239000002243 precursor Substances 0.000 claims description 28
- 238000003756 stirring Methods 0.000 claims description 23
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 22
- 238000001035 drying Methods 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000007864 aqueous solution Substances 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- 230000007935 neutral effect Effects 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- 230000035484 reaction time Effects 0.000 claims description 8
- 238000003760 magnetic stirring Methods 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- JLDSOYXADOWAKB-UHFFFAOYSA-N aluminium nitrate Chemical compound [Al+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O JLDSOYXADOWAKB-UHFFFAOYSA-N 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 230000007613 environmental effect Effects 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 229910052748 manganese Inorganic materials 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 abstract description 18
- 230000003197 catalytic effect Effects 0.000 abstract description 9
- 229910000420 cerium oxide Inorganic materials 0.000 abstract description 8
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 abstract description 7
- 241000446313 Lamella Species 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 5
- 238000011065 in-situ storage Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000002105 nanoparticle Substances 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 230000002195 synergetic effect Effects 0.000 abstract description 3
- 238000005054 agglomeration Methods 0.000 abstract description 2
- 230000002776 aggregation Effects 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000004886 process control Methods 0.000 abstract description 2
- 239000002912 waste gas Substances 0.000 abstract description 2
- 239000002351 wastewater Substances 0.000 abstract description 2
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 15
- 238000001179 sorption measurement Methods 0.000 description 10
- 229910002651 NO3 Inorganic materials 0.000 description 9
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 7
- 229910052799 carbon Inorganic materials 0.000 description 6
- -1 hydrotalcite compound Chemical class 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- 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 5
- 229940012189 methyl orange Drugs 0.000 description 5
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 238000001782 photodegradation Methods 0.000 description 4
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 3
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- AXDJCCTWPBKUKL-UHFFFAOYSA-N 4-[(4-aminophenyl)-(4-imino-3-methylcyclohexa-2,5-dien-1-ylidene)methyl]aniline;hydron;chloride Chemical compound Cl.C1=CC(=N)C(C)=CC1=C(C=1C=CC(N)=CC=1)C1=CC=C(N)C=C1 AXDJCCTWPBKUKL-UHFFFAOYSA-N 0.000 description 2
- JUQPZRLQQYSMEQ-UHFFFAOYSA-N CI Basic red 9 Chemical compound [Cl-].C1=CC(N)=CC=C1C(C=1C=CC(N)=CC=1)=C1C=CC(=[NH2+])C=C1 JUQPZRLQQYSMEQ-UHFFFAOYSA-N 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- 241001480010 Cestrum Species 0.000 description 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229940052223 basic fuchsin Drugs 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 239000004202 carbamide Substances 0.000 description 2
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 2
- 238000002848 electrochemical method Methods 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229940107698 malachite green Drugs 0.000 description 2
- FDZZZRQASAIRJF-UHFFFAOYSA-M malachite green Chemical compound [Cl-].C1=CC(N(C)C)=CC=C1C(C=1C=CC=CC=1)=C1C=CC(=[N+](C)C)C=C1 FDZZZRQASAIRJF-UHFFFAOYSA-M 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 150000003568 thioethers Chemical class 0.000 description 2
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 229940044927 ceric oxide Drugs 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003933 environmental pollution control Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000002638 heterogeneous catalyst Substances 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002048 multi walled nanotube Substances 0.000 description 1
- 238000007709 nanocrystallization Methods 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
- 238000002411 thermogravimetry Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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- 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
- B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
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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
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- 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
- B01J23/83—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 rare earths or actinides
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/00—Nature of the contaminant
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Abstract
The invention belongs to the technical field of materials, and relates to a cerium oxide-hydrotalcite composite catalyst, a preparation method and application thereof. The cerium oxide-hydrotalcite composite catalyst is characterized in that cerium oxide nanoparticles are distributed on hydrotalcite lamella, so that agglomeration of pure cerium oxide nanoparticles is changed, the hydrotalcite lamella is not easy to agglomerate, the cerium oxide catalytic performance is improved, and a synergistic catalytic effect is generated with hydrotalcite, so that the cerium oxide-hydrotalcite composite catalyst is a novel efficient composite catalyst. The cerium oxide-hydrotalcite composite catalyst has excellent catalytic performance, is expected to be used in the environment-friendly fields of treatment of refractory wastewater, treatment of waste gas and the like, and has considerable commercialization prospect. Compared with the prior art, the method adopts a double in-situ one-step hydrothermal synthesis method, has the advantages of simple production process, easy process control, low energy consumption and production cost and the like, and can be used for large-scale industrial production.
Description
Technical Field
The invention belongs to the technical field of materials, and relates to a cerium oxide-hydrotalcite composite catalyst, a preparation method and application thereof.
Background
Hydrotalcite (Hydrotalcite) compounds, also called Layered Double Hydroxides (LDHs), are a class of layered structure materials with anionic intercalation. Because of their special layered structure, they exhibit good performance in catalysis, adsorption, separation, ion exchange, and wastewater treatment. In recent years, hydrotalcite compounds have attracted much attention as a novel catalyst carrier due to the particularity of their layered structure, the exchangeability of anions between layers, the controllability of metal elements in layers, and the intrinsic basicity.
CeO2The rare earth oxide is a cheap and widely-used rare earth oxide, has the forbidden band width of 2.94eV and the light absorption threshold of about 420nm, can be used for catalysts, polishing powder, ultraviolet absorption materials and the like, has a plurality of new properties and uses after nanocrystallization, and has wide application prospects in the aspects of chemical industry and environmental pollution control.
LDHs load CeO2The composite catalyst has the synergistic effect of chemical catalysis and physical catalysis, and is a novel efficient composite catalyst.
Preparation of Cestrum species (Cestrum species, high brilliant. hydrotalcite compound-cerium oxide catalyst) and performance study of photodegradation of methyl orange [ J]Petrochemical, 2012,41(2):204-209) prepared LDHs-CeO by coprecipitation method2(LDHs is hydrotalcite compound) catalyst, and the catalyst is used for photocatalytic degradation of methyl orange solution, and the influence of the raw material ratio, the reaction time, the initial content of methyl orange, the pH of the methyl orange solution and the catalyst dosage of the catalyst on the degradation rate of methyl orange is examined; meanwhile, the catalyst is characterized by methods such as FTIR, XRD, SEM, TEM, EDS, TG and the like. The experimental result shows that the LDHs-CeO of n (Mg), n (Al) and n (Ce) is 2: 1: 0.502The activity of the catalyst is the highest,the suitable conditions for degrading the methyl orange solution by the catalyst through photocatalysis are as follows: 250mL of methyl orange solution, wherein the initial mass concentration of methyl orange is 40mg/L, the pH value is 5, the reaction time is 80min (standing in the dark for 20min, and the illumination time is 60min), and the dosage of the catalyst is 0.3 g; under the condition, the degradation rate of methyl orange reaches 98.69 percent. The characterization result shows that LDHs-CeO2The crystal phase is single, the crystal structure is consistent, the crystallinity is good, the crystal belongs to a hexagonal crystal system, the appearance is a regular sheet structure, and the dispersity is good.
Preparation and environmental application of Xifei et al (Xifei, Li Jing, jin Guanping, ceric oxide/calcium aluminium hydrotalcite/active carbon [ J)]Chemical evolution, 2016,35(1): 182-188; preparation of Xifei functional active carbon composite material and water treatment application [ D]Preparing cerium dioxide/calcium aluminum hydrotalcite/active carbon composite material (CeO) by adopting an ultrasonic-assisted coprecipitation method, namely 2016 and 03 of university of combined fertilizer industry2/CaAl-LDHs/AC). Performing field emission scanning electron microscope, X-ray diffraction, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy and thermogravimetric analysis on CeO2The morphology, composition and structure of the/CaAl-LDHs/AC are characterized. As a result, it was found that: flower-like sheet layered CeO2the/CaAl-LDHs material is uniformly distributed on the activated carbon. Examine CeO2The adsorption performance of/CaAl-LDHs/AC on chromium (VI), lead (II), fluorine and malachite green in an aqueous solution. The adsorption process of the pollutants conforms to a quasi-second order kinetic model and a Langmuir isothermal model; at pH 7, 45 ℃ and adsorption time 2h, CeO2the/CaAl-LDHs/AC can be successfully used for adsorbing and removing chromium (VI), lead (II), fluorine and malachite green, and the maximum adsorption amounts are 83.06mg/g, 131.58mg/g, 61.20mg/g and 420.17mg/g respectively.
Lijing (preparation of Lijing carbon carrier composite material and treatment study of sulfide in aqueous solution [ D ]]Preparation of cerium oxide-nickel aluminum/layered double hydroxide/chelated active carbon composite (CeO) by Urea hydrolysis method using chelated active carbon as carrier2NiAl-LDHs/MFT/AC). And the structure and the performance of the composite material are characterized by adopting a Fourier infrared spectrum (FT-IR), X-ray crystal diffraction (XRD), a field emission scanning electron microscope (FE-SEM) and an electrochemical method. ResultsShows that: petal-shaped CeO2the-NiAl-LDHs are uniformly dispersed on the surface of the chelating activated carbon. Examine CeO2The adsorption behavior of NiAl-LDHs/MFT/AC on sulfides in aqueous solutions. The results show that: the adsorption process is a spontaneous endothermic reaction, and conforms to a quasi-second order kinetic model and a Langmuir adsorption model. The maximum adsorption amount of sulfite ions at room temperature is 483.09mg/g, and the maximum adsorption amount of sulfur ions is 181.15 mg/g. Then, CeO was prepared2-NiAl-LDHs/MFT/AC and carbon nanotube mixture modified wax-filled graphite electrode (MWCNTs/CeO)2NiAl-LDHs/MFT/AC/WGE). The electrochemical catalytic oxidation behavior of the electrode on sulfides in water was studied. The results show that: the modified electrode can successfully oxidize sulfite and sulfide ions in water into sulfate radicals. Preparing cerium dioxide-nickel aluminum/layered double hydroxide/graphene oxide composite material (CeO) by using graphene oxide as carrier and adopting urea hydrolysis method2-NiAl-LDHs/GO). And the structure and the performance of the composite material are characterized by FT-IR, XRD, FE-SEM and electrochemical methods. The results show that: layered CeO2NiAl-LDHs complexes have formed. Prepared CeO by coating method2-NiAl-LDHs/GO modified wax-filled graphite electrode, which is used for detecting sulfite and sulfide ions in water. The results show that: SO (SO)3 2-And S2-The oxidation peak current and the concentration of (2) are respectively 1X 10-6～13×10-6mol/L and 1X 10-6～15×10-6Within the concentration range of mol/L, the linear growth relationship is good, and the detection limit is respectively 7 multiplied by 10-8mol/L and 2X 10-7mol/L(3σ)。
Design synthesis and property study of Wangganskey (Wangganskey. rare earth composite hydrotalcite-based heterogeneous catalyst [ D)]Lanzhou, Lanzhou university, 2019,04) constructs a novel CeO by utilizing a synthesis strategy of a self-sacrifice template2Catalyst with @ NC/LDH core-shell structure. The catalyst shows excellent OER catalytic activity and stability in alkaline electrolyte. This high performance benefits primarily from the rare earth CeO2The introduction of the catalyst effectively regulates and controls the electronic state of the catalyst and forms more defect structures. In addition, the surface in-situ growth strategy can also prevent LDH lamella aggregationIncreasing the number of active sites.
Disclosure of Invention
The invention aims to provide a novel high-efficiency cerium oxide-hydrotalcite composite catalyst, which has a simple preparation process and solves the problems of poor catalytic effect, complex preparation process, high cost and the like of the conventional single catalyst.
The invention is realized by the following technical scheme:
a preparation method of a cerium oxide-hydrotalcite composite catalyst comprises the following steps:
(1) a certain amount of cerium nitrate (Ce (NO)3)2·6H2O) preparing solution A, preparing solution B from a certain amount of NaOH aqueous solution, taking a certain amount of solution B, and controlling NaOH and NO in the solution B and A3-The molar ratio is (1.5-3):1, uniformly dropwise adding the solution B into the solution A, magnetically stirring, and reacting to obtain a precursor C;
(2) with a quantity of Me (II) (NO)3)2·6H2O、Al(NO3)3·9H2O) preparation of solutions D, Me2+With Al3+The molar ratio is (1.5-3):1, a certain amount of solution B is taken, and NaOH and NO in the solution B and D are controlled3-The molar ratio is (1.5-3):1, uniformly dropwise adding the solution B into the solution D, magnetically stirring, and reacting to obtain a precursor E;
(3) pressing the precursor C and the precursor E according to Ce2+And Me2+Mixing the components according to the molar ratio of (0.1-5), adding the mixture into a hydrothermal reaction kettle, reacting at a certain temperature, cooling, washing with water to be neutral, and drying to obtain the cerium oxide-hydrotalcite composite catalyst.
Preferably, the temperature of the magnetic stirring in the step (1) is 60-80 ℃.
Preferably, the reaction time in step (1) is 0.5-2 h.
Preferably, Me in the step (2) is one of divalent metal elements of Fe, Mg, Zn, Ni, Co, Mn and Cu.
Preferably, the temperature of the magnetic stirring in the step (2) is 60-80 ℃.
Preferably, the reaction time in step (2) is 0.5-2 h.
Preferably, the reaction temperature in step (3) is 120-180 ℃.
Preferably, the reaction time in step (3) is 5-24 h.
The invention also protects the cerium oxide-hydrotalcite composite catalyst prepared by the preparation method.
The invention also protects the application of the cerium oxide-hydrotalcite composite catalyst in the fields of chemical industry and environmental protection.
The invention has the beneficial effects that:
the cerium oxide-hydrotalcite composite catalyst is characterized in that cerium oxide nanoparticles are distributed on hydrotalcite lamella, so that agglomeration of pure cerium oxide nanoparticles is changed, the hydrotalcite lamella is not easy to agglomerate, the cerium oxide catalytic performance is improved, and a synergistic catalytic effect is generated with hydrotalcite, so that the cerium oxide-hydrotalcite composite catalyst is a novel efficient composite catalyst. The cerium oxide-hydrotalcite composite catalyst has excellent catalytic performance, is expected to be used in the environment-friendly fields of treatment of refractory wastewater, treatment of waste gas and the like, and has considerable commercialization prospect. Compared with the prior art, the method adopts a double in-situ one-step hydrothermal synthesis method, has the advantages of simple production process, easy process control, low energy consumption and production cost and the like, and can be used for large-scale industrial production.
Drawings
FIG. 1 is an SEM picture of a sample of example 1;
FIG. 2 is an SEM picture of a sample of example 2;
FIG. 3 is an SEM picture of a sample of example 3;
FIG. 4 is an SEM picture of a sample of example 4;
figure 5 is an XRD pattern of the samples of examples 1-4.
Detailed Description
For a better understanding of the present invention, the present invention will be further described with reference to the following examples and the accompanying drawings, which are illustrative of the present invention and are not to be construed as limiting thereof.
Example 1:
(1)0.005ml of cerium nitrate (Ce (NO)3)2·6H2O) preparing solution A, preparing solution B from a certain amount of NaOH aqueous solution, taking a certain amount of solution B, and controlling NaOH and NaOH in the solution B and ANO3-And (3) uniformly dropwise adding the solution B into the solution A at a molar ratio of 2:1, magnetically stirring at 70 ℃, and reacting for 2 hours to obtain a precursor C.
(2) With 0.005molMg (NO)3)2·6H2O and a certain amount of Al (NO)3)3·9H2O) preparation of solution D, Mg2+With Al3+Taking a certain amount of solution B with the molar ratio of 2:1, controlling NaOH and NO in the solution B and the solution D3-And (3) uniformly dropwise adding the solution B into the solution D at a molar ratio of 2:1, magnetically stirring at 70 ℃, and reacting for 2 hours to obtain a precursor E.
(3) And mixing the solution C and the solution E, adding the mixture into a hydrothermal reaction kettle, putting the hydrothermal reaction kettle into a drying oven, reacting for 12 hours at 160 ℃, cooling, washing with water to be neutral, and drying to obtain a cerium oxide-hydrotalcite composite catalyst sample.
Example 2:
(1)0.01mol of cerium nitrate (Ce (NO)3)2·6H2O) preparing solution A, preparing solution B from a certain amount of NaOH aqueous solution, taking a certain amount of solution B, and controlling NaOH and NO in the solution B and A3-The molar ratio is 2: and 1, uniformly dropwise adding the solution B into the solution A, magnetically stirring at 70 ℃, and reacting for 2 hours to obtain a precursor C.
(2)0.005molMg(NO3)2·6H2O and a certain amount of Al (NO)3)3·9H2O) preparation of solution D, Mg2+With Al3+Taking a certain amount of solution B with the molar ratio of 2:1, controlling NaOH and NO in the solution B and the solution D3-And (3) uniformly dropwise adding the solution B into the solution D at a molar ratio of 2:1, magnetically stirring at 70 ℃, and reacting for 2 hours to obtain a precursor E.
(3) And mixing the solution C and the solution E, adding the mixture into a hydrothermal reaction kettle, putting the hydrothermal reaction kettle into a drying oven, reacting for 12 hours at 160 ℃, cooling, washing with water to be neutral, and drying to obtain a cerium oxide-hydrotalcite composite catalyst sample.
Example 3:
(1)0.015mol of cerium nitrate (Ce (NO)3)2·6H2O) preparing solution A, preparing solution B from a certain amount of NaOH aqueous solution, taking a certain amount of solution B, and controlling NaOH and NO in the solution B and A3-The molar ratio is 2:1, the solution B is evenly dripped into the solution A, the solution A is magnetically stirred at the temperature of 70 ℃, and the reaction 2 is carried outh to obtain a precursor C.
(2)0.005molMg(NO3)2·6H2O and a certain amount of Al (NO)3)3·9H2O) preparation of solution D, Mg2+With Al3+Taking a certain amount of solution B with the molar ratio of 2:1, controlling NaOH and NO in the solution B and the solution D3-And (3) uniformly dropwise adding the solution B into the solution D at a molar ratio of 2:1, magnetically stirring at 70 ℃, and reacting for 2 hours to obtain a precursor E.
(3) And mixing the solution C and the solution E, adding the mixture into a hydrothermal reaction kettle, putting the hydrothermal reaction kettle into a drying oven, reacting for 12 hours at 160 ℃, cooling, washing with water to be neutral, and drying to obtain a cerium oxide-hydrotalcite composite catalyst sample.
Example 4:
(1)0.02mol of cerium nitrate (Ce (NO)3)2·6H2O) preparing solution A, preparing solution B from a certain amount of NaOH aqueous solution, taking a certain amount of solution B, and controlling NaOH and NO in the solution B and A3-And (3) uniformly dropwise adding the solution B into the solution A at a molar ratio of 2:1, magnetically stirring at 70 ℃, and reacting for 2 hours to obtain a precursor C.
(2)0.005molMg(NO3)2·6H2O and a certain amount of Al (NO)3)3·9H2O) preparation of solution D, Mg2+With Al3+Taking a certain amount of solution B with the molar ratio of 2:1, controlling NaOH and NO in the solution B and the solution D3-And (3) uniformly dropwise adding the solution B into the solution D at a molar ratio of 2:1, magnetically stirring at 70 ℃, and reacting for 2 hours to obtain a precursor E.
(3) And mixing the solution C and the solution E, adding the mixture into a hydrothermal reaction kettle, putting the hydrothermal reaction kettle into a drying oven, reacting for 12 hours at 160 ℃, cooling, washing with water to be neutral, and drying to obtain a cerium oxide-hydrotalcite composite catalyst sample.
Example 5:
(1)0.005mol of cerium (Ce (NO) acid3)2·6H2O) preparing solution A, preparing solution B from a certain amount of NaOH aqueous solution, taking a certain amount of solution B, and controlling NaOH and NO in the solution B and A3-And (3) uniformly dropwise adding the solution B into the solution A at a molar ratio of 1.5:1, magnetically stirring at 80 ℃, and reacting for 0.5h to obtain a precursor C.
(2)0.01molMn(NO3)2·6H2O and a certain amount of Al (NO)3)3·9H2O) preparation of solution D, where Mn2+With Al3+The molar ratio is 1.5:1, a certain amount of solution B is taken, NaOH and NO in the solution B and D are controlled3-And (3) uniformly dropwise adding the solution B into the solution D at a molar ratio of 1.5:1, magnetically stirring at 80 ℃, and reacting for 0.5h to obtain a precursor E.
(3) And mixing the solution C and the solution E, adding the mixture into a hydrothermal reaction kettle, putting the hydrothermal reaction kettle into a drying oven, reacting for 24 hours at 130 ℃, cooling, washing with water to be neutral, and drying to obtain a cerium oxide-hydrotalcite composite catalyst sample.
Example 6:
(1)0.025mol of cerium nitrate (Ce (NO)3)2·6H2O) preparing solution A, preparing solution B from a certain amount of NaOH aqueous solution, taking a certain amount of solution B, and controlling NaOH and NO in the solution B and A3-The molar ratio is 2.5: and 1, uniformly dropwise adding the solution B into the solution A, magnetically stirring at 60 ℃, and reacting for 2 hours to obtain a precursor C.
(2)0.005molNi(NO3)2·6H2O and a certain amount of Al (NO)3)3·9H2O) preparation of solution D, Ni2+With Al3+The molar ratio is 2.5:1, a certain amount of solution B is taken, NaOH and NO in the solution B and D are controlled3-And uniformly dripping the solution B into the solution D at a molar ratio of 2.5:1, magnetically stirring at 60 ℃, and reacting for 2 hours to obtain a precursor E.
(3) And mixing the solution C and the solution E, adding the mixture into a hydrothermal reaction kettle, putting the hydrothermal reaction kettle into a drying oven, reacting for 10 hours at 150 ℃, cooling, washing with water to be neutral, and drying to obtain a cerium oxide-hydrotalcite composite catalyst sample.
Example 7:
(1)0.002mol of cerium nitrate (Ce (NO)3)2·6H2O) preparing solution A, preparing solution B from a certain amount of NaOH aqueous solution, taking a certain amount of solution B, and controlling NaOH and NO in the solution B and A3-And (3) uniformly dropwise adding the solution B into the solution A at a molar ratio of 3:1, magnetically stirring at 80 ℃, and reacting for 1.5 hours to obtain a precursor C.
(2)0.005molZn(NO3)2·6H2O and a certain amount of Al (NO)3)3·9H2O) preparing a solution D,wherein Zn is2+With Al3+Taking a certain amount of solution B, controlling NaOH and NO in the solution B and D at a molar ratio of 3:13-And (3) uniformly dropwise adding the solution B into the solution D at a molar ratio of 3:1, magnetically stirring at 80 ℃, and reacting for 1.5 hours to obtain a precursor E.
(3) And mixing the solution C and the solution E, adding the mixture into a hydrothermal reaction kettle, putting the hydrothermal reaction kettle into a drying oven, reacting for 6 hours at 170 ℃, cooling, washing with water to be neutral, and drying to obtain a cerium oxide-hydrotalcite composite catalyst sample.
Example 8:
(1)0.0015mol of cerium nitrate (Ce (NO)3)2·6H2O) preparing solution A, preparing solution B from a certain amount of NaOH aqueous solution, taking a certain amount of solution B, and controlling NaOH and NO in the solution B and A3-And (3) uniformly dropwise adding the solution B into the solution A at a molar ratio of 2:1, magnetically stirring at 65 ℃, and reacting for 1.5 hours to obtain a precursor C.
(2)0.005molFe(NO3)2·6H2O and a certain amount of Al (NO)3)3·9H2O) preparation of solution D, where Fe2+With Al3+The molar ratio is 2.5:1, a certain amount of solution B is taken, NaOH and NO in the solution B and D are controlled3-And (3) uniformly dropwise adding the solution B into the solution D at a molar ratio of 2:1, magnetically stirring at 65 ℃, and reacting for 1.5 hours to obtain a precursor E.
(3) And mixing the solution C and the solution E, adding the mixture into a hydrothermal reaction kettle, putting the hydrothermal reaction kettle into a drying oven, reacting for 24 hours at 120 ℃, cooling, washing with water to be neutral, and drying to obtain a cerium oxide-hydrotalcite composite catalyst sample.
Example 9:
(1)0.001mol of cerium nitrate (Ce (NO)3)2·6H2O) preparing solution A, preparing solution B from a certain amount of NaOH aqueous solution, taking a certain amount of solution B, and controlling NaOH and NO in the solution B and A3-And (3) uniformly dropwise adding the solution B into the solution A at a molar ratio of 1.5:1, magnetically stirring at 75 ℃, and reacting for 1h to obtain a precursor C.
(2)0.005molCo(NO3)2·6H2O and a certain amount of Al (NO)3)3·9H2O) preparation of solution D, where Co2+With Al3+Taking a certain amount of solution B, controlling the solution B and the solution D to dissolve at a molar ratio of 3:1NaOH and NO in liquid3-And (3) uniformly dropwise adding the solution B into the solution D at a molar ratio of 1.5:1, magnetically stirring at 75 ℃, and reacting for 1h to obtain a precursor E.
(3) And mixing the solution C and the solution E, adding the mixture into a hydrothermal reaction kettle, putting the hydrothermal reaction kettle into a drying oven, reacting for 5 hours at 180 ℃, cooling, washing with water to be neutral, and drying to obtain a cerium oxide-hydrotalcite composite catalyst sample.
Example 10:
(1)0.0005mol of cerium nitrate (Ce (NO)3)2·6H2O) preparing solution A, preparing solution B from a certain amount of NaOH aqueous solution, taking a certain amount of solution B, and controlling NaOH and NO in the solution B and A3-And (3) uniformly dropwise adding the solution B into the solution A at a molar ratio of 2:1, magnetically stirring at 70 ℃, and reacting for 1.5 hours to obtain a precursor C.
(2)0.005molCu(NO3)2·6H2O and a certain amount of Al (NO)3)3·9H2O) preparation of solution D, in which Cu2+With Al3+The molar ratio is 2.5:1, a certain amount of solution B is taken, NaOH and NO in the solution B and D are controlled3-And (3) uniformly dropwise adding the solution B into the solution D at a molar ratio of 2:1, magnetically stirring at 70 ℃, and reacting for 1.5 hours to obtain a precursor E.
(3) And mixing the solution C and the solution E, adding the mixture into a hydrothermal reaction kettle, putting the hydrothermal reaction kettle into a drying oven, reacting for 20 hours at 140 ℃, cooling, washing with water to be neutral, and drying to obtain a cerium oxide-hydrotalcite composite catalyst sample.
The samples of examples 1-4 were tested for photocatalytic performance by the following methods:
(1) preparing a salt-based fuchsin solution with the concentration of 8.0730 mg/L;
(2) weighing 0.0180g of the sample of example 1-4 into a 100ml conical flask;
(3) transferring 18ml of the salt base fuchsin solution prepared in the step (1) into the conical flask in the step (2);
(4) performing adsorption-desorption balance, namely performing magnetic stirring in a water bath for 2 hours under the constant temperature (25 ℃) and light-proof condition, sucking 9ml of suspension into a 10ml centrifuge tube, marking as ①, and placing in the light-proof condition;
(5) performing photocatalysis, namely performing photodegradation on the residual suspension in the conical flask in the step (3) for 2 hours under the condition of a 365nm ultraviolet lamp, taking out the conical flask, and transferring the residual suspension into a 10ml centrifugal tube, wherein the mark is ②;
(6) centrifuging for 20min at 10000r/min in a high-speed refrigerated centrifuge, taking supernatant into a prepared 10ml centrifuge tube with a sharp end, and marking as (I);
(7) measuring absorbance (A), namely setting the wavelength of an ultraviolet visible spectrophotometer to be 546nm, using distilled water as a standard test solution, and measuring the absorbance of supernatant liquid I and II, wherein the absorbance is marked as A01, A02 and A03, and At1, At2 and At 3;
(8) calculating the concentration of supernatant liquid (C0 and C1), wherein [ A ═ epsilon bc: epsilon 9.5107L/g.cm is absorption coefficient (L/g.cm), b is cuvette thickness (cm), and C is solution concentration (g/L) ];
(9) degradation rate of basic fuchsin solution:
(10) as shown in Table 1, the photodegradation rates of the basic fuchsin solutions of examples 1-4 were all above 90%.
TABLE 1 EXAMPLES 1-4 sample salt-based magenta solution photodegradation ratio List
| Example 1 | Example 2 | Example 3 | Example 4 | |
| Degradation Rate (%) | 92.6 | 90.8 | 93.2 | 91.3 |
The samples of examples 1-4 were examined by SEM and XRD, respectively.
Fig. 1 to 4 are SEM pictures of samples of examples 1 to 4, respectively, and it can be seen from fig. 1 to 4 that hexagonal and other shaped lamellae of the ceria-hydrotalcite composite catalyst sample prepared by the dual in-situ hydrothermal one-step synthesis method are hydrotalcite, the white point of the surface of the lamellae is ceria, and the ceria is distributed on the surface of the lamellae of the hydrotalcite.
FIG. 5 is an XRD pattern of the samples of examples 1-4 with the characteristic diffraction peaks of cerium oxide marked by inverted triangles. From fig. 5 and the standard XRD card of magnesium aluminum hydrotalcite, the characteristic diffraction peaks of (003), (006), (009), (015), (110) and (113) of magnesium aluminum hydrotalcite are all found, and are obvious and sharp, indicating that the cerium oxide-hydrotalcite composite catalyst samples synthesized in examples 1-4 all have the structure of magnesium aluminum hydrotalcite and good crystallinity. The sample still had a diffraction peak for ceria, indicating that the sample still had the magnetic substrate ceria, as compared to the XRD card for ceria.
The above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements made to the technical solution of the present invention by those skilled in the art without departing from the spirit of the present invention should fall within the protection scope defined by the claims of the present invention.
Claims (10)
1. The preparation method of the cerium oxide-hydrotalcite composite catalyst is characterized by comprising the following steps of:
(1) a certain amount of cerium nitrate (Ce (NO)3)2·6H2O) preparing solution A, preparing solution B from a certain amount of NaOH aqueous solution, taking a certain amount of solution B, and controllingNaOH and NO in B and A solutions3-The molar ratio is (1.5-3):1, uniformly dropwise adding the solution B into the solution A, magnetically stirring, and reacting to obtain a precursor C;
(2) with a quantity of Me (II) (NO)3)2·6H2O、Al(NO3)3·9H2O) preparation of solutions D, Me2+With Al3+The molar ratio is (1.5-3):1, a certain amount of solution B is taken, and NaOH and NO in the solution B and D are controlled3-The molar ratio is (1.5-3):1, uniformly dropwise adding the solution B into the solution D, magnetically stirring, and reacting to obtain a precursor E;
(3) pressing the precursor C and the precursor E according to Ce2+And Me2+Mixing the components according to the molar ratio of (0.1-5), adding the mixture into a hydrothermal reaction kettle, reacting at a certain temperature, cooling, washing with water to be neutral, and drying to obtain the cerium oxide-hydrotalcite composite catalyst.
2. The method for preparing a cerium oxide-hydrotalcite composite catalyst according to claim 1, wherein: the magnetic stirring temperature in the step (1) is 60-80 ℃.
3. The method for preparing a cerium oxide-hydrotalcite composite catalyst according to claim 1, wherein: the reaction time in the step (1) is 0.5-2 h.
4. The method for preparing a cerium oxide-hydrotalcite composite catalyst according to claim 1, wherein: me in the step (2) is one of divalent metal elements in Fe, Mg, Zn, Ni, Co, Mn and Cu.
5. The method for preparing a cerium oxide-hydrotalcite composite catalyst according to claim 1, wherein: the magnetic stirring temperature in the step (2) is 60-80 ℃.
6. The method for preparing a cerium oxide-hydrotalcite composite catalyst according to claim 1, wherein: the reaction time in the step (2) is 0.5-2 h.
7. The method for preparing a cerium oxide-hydrotalcite composite catalyst according to claim 1, wherein: the reaction temperature in the step (3) is 120-180 ℃.
8. The method for preparing a cerium oxide-hydrotalcite composite catalyst according to claim 1, wherein: the reaction time in the step (3) is 5-24 h.
9. A cerium oxide-hydrotalcite composite catalyst prepared by the preparation method according to any one of claims 1 to 8.
10. Use of the cerium oxide-hydrotalcite composite catalyst according to claim 9 in the fields of chemical industry and environmental protection.
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