CN111482172B - Composite nano material of CuO/defect titanium dioxide and application thereof - Google Patents

Composite nano material of CuO/defect titanium dioxide and application thereof Download PDF

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CN111482172B
CN111482172B CN201910072248.1A CN201910072248A CN111482172B CN 111482172 B CN111482172 B CN 111482172B CN 201910072248 A CN201910072248 A CN 201910072248A CN 111482172 B CN111482172 B CN 111482172B
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郭彦炳
赵超颖
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Central China Normal University
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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
    • B01J23/72—Copper
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    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
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    • B01D2255/20707—Titanium
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    • Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
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Abstract

The invention discloses a composite nano material of CuO/defective titanium dioxide, which is characterized by comprising CuO and defective titanium dioxide, wherein the CuO is loaded on the defective titanium dioxide, the CuO loading amount is between 2 and 8 mol percent, and the defective titanium dioxide is prepared by adding NaBH into a white titanium dioxide nanosheet 4 And/or KBH 4 And partially reducing the obtained gray or black titanium dioxide nanosheet. The CuO/defect titanium dioxide composite nano material has oxygen vacancy, can effectively activate oxygen molecules, thereby improving the efficiency of catalytic oxidation of CO, and particularly can ensure that the conversion rate of catalytic oxidation of CO is more than 90 percent at the catalytic temperature of 180 ℃. Moreover, the preparation method of the composite nano material is simple, and raw materials needed in the preparation process are cheap and easy to obtain, so that the composite nano material has a good industrial application prospect.

Description

Composite nano material of CuO/defect titanium dioxide and application thereof
Technical Field
The invention belongs to the field of environmental protection, and particularly relates to a CuO/defective titanium dioxide composite nanomaterial for CO catalytic oxidation and application thereof.
Background
With the continuous improvement of national economic level in China, the automobile preservation amount is continuously increased, the harm caused by automobile exhaust emission is more and more serious, carbon monoxide (CO) is one of main pollutants discharged by automobile exhaust, is colorless, odorless and tasteless combustible toxic gas, not only causes huge pollution to the environment, but also has stronger toxicity in a blood nervous system through the CO entering a human body through breathing, and also brings serious threat to the health of human beings. Therefore, the elimination of CO has strong social reality development significance. Current catalytic oxidation of CO converts CO to non-polluting carbon dioxide (CO) 2 ) Is a direct, economic and effective method and receives more and more attention. Although noble metal catalysts such as Pt, Pd, Au, Ru, etc. have good catalytic performance, their wide development and application are limited due to their high price, small reserves, complex preparation process and low yield. Copper oxide (CuO) is considered as one of the best alternatives to noble metal catalysts due to its good catalytic performance, low cost and abundance, and catalysts having CuO as a main active component have been widely used in catalytic reactions such as CO oxidation, hydrogenation and combustion of CO and hydrocarbons. Titanium dioxide (TiO) 2 ) It is often used as a carrier of catalysts due to its low toxicity, low cost, availability, stable physicochemical properties, etc. The study showed that the oxygen vacancy is TiO 2 The most common intrinsic defect, when TiO 2 Surface ofWhen defects exist, the defects can be used as active sites of catalytic reaction, and the transfer of electrons between the carrier and the active component is accelerated, so that the catalytic performance of the catalyst is improved.
The most common research means currently used by researchers to create oxygen vacancies in metal oxides is high temperature calcination in a hydrogen atmosphere. The method has high requirements on equipment and high dangerousness, the CO catalytic oxidation activity of the catalyst needs to be further improved, and the reduction of the temperature for catalyzing CO oxidation is still one of the technical problems to be solved by the technical personnel in the field.
Disclosure of Invention
In view of the above-mentioned problems, an object of the present invention is to provide a catalyst having high catalytic oxidation activity of CO and low catalytic oxidation temperature. In another aspect, the invention also relates to the application and the manufacturing method of the catalyst.
In order to solve the technical problem of the invention, the following technical scheme is adopted:
the invention relates to a composite nano material of CuO/defect titanium dioxide, which is characterized in that the composite nano material comprises CuO and defect titanium dioxide, wherein the CuO is loaded on the defect titanium dioxide, the load of the CuO is between 2 and 8 mol percent, and the defect titanium dioxide is formed by adding NaBH into a white titanium dioxide nanosheet 4 And/or KBH 4 And partially reducing the obtained gray or black titanium dioxide nanosheet.
In a preferred embodiment of the present invention, the nanocomposite exhibits a nano-platelet structure.
In a preferred embodiment of the invention, the nanocomposite has CuO, Cu as detected by HR-TEM 2 O and TiO 2 The lattice fringes of (2).
In a preferred embodiment of the present invention, the nanocomposite has oxygen vacancies.
In a preferred embodiment of the invention, the nanocomposite is prepared by impregnating grey or black titanium dioxide nanoplates with Cu (NO) 3 ) 2 In solution of (2), dried and then calcinedAnd (4) firing to obtain the product.
In a preferred embodiment of the present invention, the drying is performed by removing the solvent water from the solution by rotary evaporation at 50 to 70 ℃. By making Cu (NO) possible under spinning conditions 3 ) 2 With TiO 2 The uniform mixing can also evaporate the water, thereby saving the preparation process.
In a preferred embodiment of the present invention, the calcination is performed at a temperature of 300 to 400 ℃. By carrying out the reaction at such a temperature, a nanocomposite having high catalytic activity can be obtained efficiently.
In a preferred embodiment of the invention, the gray titanium dioxide nanosheets are prepared by adding white titanium dioxide nanosheets to NaBH 4 And/or KBH 4 After partial reduction, heating to 280-320 ℃ in an inert atmosphere and preserving heat for 20-40 minutes to obtain the catalyst.
In a preferred embodiment of the present invention, the black titanium dioxide nanosheets are prepared by adding white titanium dioxide nanosheets to NaBH 4 And/or KBH 4 After partial reduction, heating to 340-370 ℃ in an inert atmosphere and preserving heat for 20-40 minutes to obtain the catalyst.
In another aspect, the invention also relates to the use of the above composite nanomaterial of CuO/defective titania as a catalyst for the catalytic oxidation of CO.
In a preferred embodiment of the invention, the temperature of the catalytic oxidation of CO is 200 ℃ or less.
In a preferred embodiment of the present invention, the conversion of the catalytic oxidation of CO is 90% or more at a catalytic temperature of 180 ℃ or less; preferably 95% or more.
The composite nanomaterial of CuO/deficient titania of the present invention has at least one or all of the following advantages:
(1) the CuO/defect titanium dioxide composite nanomaterial has oxygen vacancy, can effectively activate oxygen molecules, thereby improving the efficiency of catalytic oxidation of CO, and particularly can ensure that the conversion rate of catalytic oxidation of CO is more than 90% at the catalytic temperature of 180 ℃;
(2) the preparation method of the CuO/defective titanium dioxide composite nanomaterial is simple, and the raw materials required in the preparation process are cheap and easy to obtain, so that the CuO/defective titanium dioxide composite nanomaterial has a good industrial application prospect.
Drawings
FIG. 1 shows TiO 2 -w，TiO 2 -g，TiO 2 -b，5％CuO/TiO 2 -w，5％CuO/TiO 2 -g，5％CuO/TiO 2 -XRD spectrum of sample b.
FIG. 2 shows 5% CuO/TiO 2 -g of samples (a) TEM (1), HADDF (2) and HR-TEM (3, 4); the right panel shows the TEM-mapping spectrum.
FIG. 3 shows the left diagram of 5% CuO/TiO 2 -TEM (1), HADDF (2) and HRTEM (3,4) of the b samples; shown on the right is 5% CuO/TiO 2 B TEM-mapping spectrum of the sample.
FIG. 4 shows 5% CuO/TiO 2 -w、5％CuO/TiO 2 G and 5% CuO/TiO 2 B EPR spectrum of the sample.
FIG. 5 shows 5% CuO/TiO 2 -w、5％CuO/TiO 2 G and 5% CuO/TiO 2 B XPS spectrum of Cu2p, Ti2p, O1s orbits of the sample.
FIG. 6 shows the left diagram of 5% CuO/TiO 2 -w、5％CuO/TiO 2 G and 5% CuO/TiO 2 -b conversion of catalytically converted CO; shown on the right is 5% CuO/TiO 2 -w、5％CuO/TiO 2 G and 5% CuO/TiO 2 The activation energy of b.
Detailed Description
In order to further illustrate the technical solution of the present invention, the above technical solution is described in detail below with specific examples, but the present invention is not limited to the following embodiments.
Example 1:
preparation of white titanium dioxide (TiO) 2 -w)：
60mL of deionized water was placed in a 100mL autoclave. 1.65mL of titanium tetrachloride solution was added dropwise to the reaction vessel, cooled in an ice water bath and stirred vigorously for 30 min. Under the condition of vigorous stirring, 5g of urea is added into the solution, and after the urea is fully dissolvedThen, 5mL of sodium lactate solution was added and the reaction was carried out for 30 min. Sealing the high-pressure reaction kettle, putting the high-pressure reaction kettle into an oven, and reacting for 12 hours at 200 ℃. Centrifuging the product after reaction, filtering to remove supernatant, filtering the obtained white sample, washing with ethanol and deionized water respectively, transferring the sample to a 60 ℃ oven, and drying to obtain white TiO 2 -w nanosheets.
Preparation of Gray titanium dioxide (TiO) 2 -g)：
1.0g TiO at room temperature 2 -w nanosheet powder with 0.375g NaBH 4 Mixing the powders, and grinding for 30 min. The mixture was then transferred to a porcelain boat under inert gas N 2 Heating the mixture to 300 ℃ from room temperature in a tube furnace in an atmosphere, and keeping the temperature for 30 min. Naturally cooling to room temperature, washing the calcined product with ethanol and deionized water to remove unreacted NaBH 4 Finally drying at 70 ℃ to obtain TiO 2 -g of powder.
TiO supported CuO 2 -g nanomaterial (CuO/TiO) 2 Preparation of g):
0.5g of TiO prepared above was weighed 2 -g powder dissolved in 40mL deionized water, 6.26mL 0.05mol/L Cu (NO) 3 ) 2 Stirring the solution for 2h, then rotationally evaporating at 60 ℃ until the hydrosolvent is completely removed, transferring to a 60 ℃ oven for drying, and finally calcining the dried product in a muffle furnace at 350 ℃ for 4h to obtain 5 mol% CuO/TiO 2 -g nanomaterial.
Example 2:
preparation of Black titanium dioxide (TiO) 2 -b)：
1.0g of TiO prepared in example 1 was added at room temperature 2 -w nanosheet powder with 0.375g NaBH 4 Mixing the powders, and grinding for 30 min. The mixture was then transferred to a porcelain boat under inert gas N 2 Heating the mixture to 350 ℃ from room temperature in a tube furnace under the atmosphere, and keeping the temperature for 30 min. Naturally cooling to room temperature, washing the calcined product with ethanol and deionized water to remove unreacted NaBH 4 Finally drying at 70 ℃ to obtain TiO 2 -b powder.
TiO supported CuO 2 -b nanomaterial (CuO/TiO) 2 Preparation of (b)Preparing:
0.5g of TiO prepared above was weighed 2 -b powder, dissolved in 40mL deionized water, 6.26mL 0.05mol/L Cu (NO) 3 ) 2 Stirring the solution for 2h, then rotationally evaporating at 60 ℃ until the hydrosolvent is completely removed, transferring to a 60 ℃ oven for drying, and finally calcining the dried product in a muffle furnace at 350 ℃ for 4h to obtain 5 mol% CuO/TiO 2 B nano-materials.
Comparative example 1:
0.5g of TiO prepared as described in example 1 above was weighed 2 -w nanosheet powder, dissolved in 40mL of deionized water, added 6.26mL of 0.05mol/L Cu (NO) 3 ) 2 Stirring the solution for 2h, then rotationally evaporating at 60 ℃ until the hydrosolvent is completely removed, transferring to a 60 ℃ oven for drying, and finally calcining the dried product in a muffle furnace at 350 ℃ for 4h to obtain 5 mol% CuO/TiO 2 -w nanomaterial.
A series of characterization methods are adopted to characterize the composite materials prepared in the embodiments 1 and 2 and the comparative example 1, and characterization results are shown in figures 1-5.
TiO shown in FIG. 1 2 -w，TiO 2 -g，TiO 2 -b，5％CuO/TiO 2 -w，5％CuO/TiO 2 -g，5％CuO/TiO 2 -XRD spectrum of sample b. XRD results show that the TiO is treated by the method 2 -w TiO resulting from sodium borohydride treatment of the sample 2 G and TiO 2 B sample still retains brookite TiO 2 But the diffraction peak intensity is reduced, which is probably due to the effect of oxygen vacancies. When in TiO 2 -w，TiO 2 G and TiO 2 B sample copper oxide loaded 5% CuO/TiO 2 -w，5％CuO/TiO 2 G and 5% CuO/TiO 2 The-b sample has no diffraction peak of Cu species.
FIG. 2 shows 5% CuO/TiO 2 -g of samples (a) TEM (1), HADDF (2) and HR-TEM (3, 4); (b) TEM-mapping spectrum. TEM results show that the catalyst still maintains the nano sheet structure of the carrier, and CuO and TiO appear in HR-TEM 2 The lattice stripes of (A) indicate that Cu exists mainly in the form of CuO, and TEM-mapping results indicate that Cu species all existIs uniformly dispersed in TiO 2 The above.
FIG. 3 shows the left diagram of 5% CuO/TiO 2 -TEM (1), HADDF (2) and HRTEM (3,4) of the b samples; the left panel shows 5% CuO/TiO 2 B TEM-mapping spectrum of the sample. TEM results show that the catalyst still maintains the nano sheet structure of the carrier, and CuO and Cu appear in HR-TEM 2 O and TiO 2 Shows from the TEM-mapping results that Cu species are uniformly dispersed in TiO 2 The above.
FIG. 4 shows 5% CuO/TiO 2 -w、5％CuO/TiO 2 G and 5% CuO/TiO 2 -b EPR spectrum of the sample; 5% CuO/TiO at g 2.002 2 G and 5% CuO/TiO 2 The sample (b) shows a signal peak of oxygen vacancy, and 5% of CuO/TiO 2 B intensity of signal peak of sample greater than 5% CuO/TiO 2 G sample, indicating 5% CuO/TiO 2 -b sample has oxygen vacancy concentration higher than 5% CuO/TiO 2 -g of sample.
FIG. 5 shows 5% CuO/TiO 2 -w、5％CuO/TiO 2 G and 5% CuO/TiO 2 XPS spectra of Cu2p, Ti2p, O1s orbitals of the b sample. From XPS analysis, 5% CuO/TiO 2 B Ti in the sample 3+ Is higher than 5% of CuO/TiO 2 G samples, which is consistent with EPR results. And 5% CuO/TiO 2 The content of adsorbed oxygen in the sample is higher than 5% of CuO/TiO 2 G of sample, more advantageously catalyzing the oxidation reaction of CO.
Example 2:
in order to further evaluate the catalytic activity of the catalyst of the present invention, the present invention was evaluated by a gas phase catalytic oxidation activity evaluation experiment.
The test conditions were:
100mg of catalyst, total gas flow 100mL/min -1 (1％CO，5％O 2 ，N 2 As an equilibrium gas), a test for evaluating catalytic combustion activity of carbon monoxide (CO) was conducted in a quartz tube having a diameter of 8 mm. 100mg of the powder catalyst was packed in a quartz tube, which was placed in a tube furnace and was heated from room temperature to 250 ℃ by temperature programming. The reaction gas composition (volume fraction) was: 1% CO, 5% O 2 ，94％N 2 The total flow rate is 100mL/min, and the mass space velocity is 60000 mL/(g.h). Finally, the components of the reaction tail gas are analyzed on line by a FuliGC-9790 gas chromatograph for CO.
The conversion is calculated as: CO conversion (%) — (area of inlet CO peak-area of outlet CO peak)/area of CO peak × 100%.
The results of the activity test are shown in fig. 6. The test result shows that 5 percent of CuO/TiO 2 Temperature (T) at which the catalytic conversion of w is 50% 50 ) Is 174 ℃, 5% CuO/TiO 2 Temperature (T) at which the catalytic conversion of w is 100% 100 ) Is 188 ℃; 5% CuO/TiO 2 Temperature (T) at which the catalytic conversion of g is 50% 50 ) Is 138.6 ℃ and 5% CuO/TiO 2 Temperature (T) at which the catalytic conversion of g is 100% 100 ) Is 157 ℃; 5% CuO/TiO 2 Temperature (T) at which the catalytic conversion of-b is 50% 50 ) Is 129.6 ℃, 5% CuO/TiO 2 Temperature (T) at which the catalytic conversion of-b is 100% 100 ) Is 147 ℃; the test result shows that: catalytic performance 5% CuO/TiO 2 -w<5％CuO/TiO 2 -g<5％CuO/TiO 2 -b. And 5% CuO/TiO 2 Activation energy of 63.8KJ/mol, 5% CuO/TiO 2 Activation energy of 23.6KJ/mol, 5% CuO/TiO 2 The activation energy of-b was 22.5KJ/mol, so 5% CuO/TiO 2 The activation energy of b is the smallest and most favorable for the catalytic oxidation of CO.
The applicant states that the present invention is described in detail by the above embodiments, but the present invention is not limited to the above embodiments, that is, the present invention is not limited to the above embodiments, and it should be understood by those skilled in the art that any modifications to the present invention, equivalent substitutions and additions to the present invention product, selection of specific modes, etc. are within the scope and disclosure of the present invention.

Claims (9)

1. A CuO/deficient titania composite nanomaterial, characterized in that the composite nanomaterial comprises CuO and deficient titania, wherein CuO is supported on the deficient titania, and the CuO is supported in an amount that is different from the amount of the deficient titaniaBetween 2 mol% and 8 mol%, the defect titanium dioxide is prepared by adding NaBH into white titanium dioxide nanosheet 4 And/or KBH 4 Partially reducing the obtained gray or black titanium dioxide nanosheets; the nano composite material is detected to have CuO and Cu through HR-TEM 2 O and TiO 2 The lattice fringes of (2).
2. The CuO/deficient titania composite nanomaterial of claim 1, said nanocomposite exhibiting a nano-platelet structure.
3. The CuO/deficient titania composite nanomaterial of claim 1, said nanocomposite having oxygen vacancies.
4. The CuO/deficient titanium dioxide composite nanomaterial of claim 1, said nanocomposite being obtained by impregnating a grey or black titanium dioxide nanoplatelet with Cu (NO) 3 ) 2 Dried and then calcined.
5. The CuO/deficient titania composite nanomaterial according to claim 4, wherein said drying is carried out by removing solvent water from the solution by rotary evaporation at 50-70 ℃.
6. The CuO/defective titanium dioxide composite nanomaterial of claim 4, wherein said calcination is carried out at a temperature ranging from 300 ℃ to 400 ℃.
7. The CuO/deficient titania composite nanomaterial of claim 1, said gray titania nanosheets being formed by adding white titania nanosheets to NaBH 4 And/or KBH 4 After partial reduction, heating to 280-320 ℃ under inert atmosphere and preserving heat for 20-40 minutes to obtain the catalyst.
8. The CuO/deficient titania composite nanomaterial of claim 1The black titanium dioxide nanosheet is prepared by adding white titanium dioxide nanosheets into NaBH 4 And/or KBH 4 After partial reduction, heating to 340-370 ℃ under inert atmosphere and preserving heat for 20-40 minutes to obtain the catalyst.
9. Use of the composite nanomaterial of CuO/defective titania of claim 1 as a catalyst for catalytic oxidation of CO at a temperature of 180 ℃ or less.
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Denomination of invention: Composite nanomaterials of CuO/defective titanium dioxide and their applications

Granted publication date: 20220816

License type: Common License

Record date: 20231220

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Application publication date: 20200804

Assignee: Hubei Ouyue Pharmaceutical Co.,Ltd.

Assignor: CENTRAL CHINA NORMAL University

Contract record no.: X2023980054452

Denomination of invention: Composite nanomaterials of CuO/defective titanium dioxide and their applications

Granted publication date: 20220816

License type: Common License

Record date: 20240102

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