CN115999614B - Ultraviolet-visible-near infrared light responsive carbon dioxide reduction photocatalyst - Google Patents
Ultraviolet-visible-near infrared light responsive carbon dioxide reduction photocatalyst Download PDFInfo
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- CN115999614B CN115999614B CN202310121554.6A CN202310121554A CN115999614B CN 115999614 B CN115999614 B CN 115999614B CN 202310121554 A CN202310121554 A CN 202310121554A CN 115999614 B CN115999614 B CN 115999614B
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 23
- 230000009467 reduction Effects 0.000 title claims description 16
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 title abstract description 6
- 229910002092 carbon dioxide Inorganic materials 0.000 title abstract description 3
- 239000001569 carbon dioxide Substances 0.000 title abstract description 3
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims description 56
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 17
- 239000000843 powder Substances 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 11
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 8
- 239000012279 sodium borohydride Substances 0.000 claims description 8
- 239000004408 titanium dioxide Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 238000011068 loading method Methods 0.000 claims description 7
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 239000002243 precursor Substances 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 19
- 238000006243 chemical reaction Methods 0.000 abstract description 14
- 230000004298 light response Effects 0.000 abstract description 5
- 230000004044 response Effects 0.000 abstract description 3
- 230000003595 spectral effect Effects 0.000 abstract description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 abstract description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 abstract description 2
- 229910052707 ruthenium Inorganic materials 0.000 description 20
- 238000006722 reduction reaction Methods 0.000 description 15
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 5
- 239000000446 fuel Substances 0.000 description 5
- 229910052573 porcelain Inorganic materials 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 241001464837 Viridiplantae Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a novel ultraviolet-visible-near infrared light response photocatalyst, a preparation method thereof and application thereof in the field of CO 2 photocatalytic conversion. The photocatalyst has broad spectral response, and can efficiently catalyze the selective conversion of carbon dioxide to generate carbon monoxide under the irradiation of ultraviolet-visible-near infrared light. The photocatalyst has simple preparation process and wide application prospect in the aspects of preparing renewable energy sources by utilizing solar energy and the like.
Description
Technical Field
The invention belongs to the technical field of photocatalytic materials, and particularly relates to a CO 2 reduction photocatalyst with ultraviolet-visible-near infrared light response, a preparation method and application thereof.
Background
The conversion of photocatalytic CO 2 to high value-added fuels is considered one of the effective methods to alleviate energy crisis and environmental problems. The environment-friendly solar energy environment-friendly carbon-based fuel can simulate green plants, and CO 2 and H 2 O are converted into carbon-based fuels (such as CO) and O 2 by utilizing sunlight, so that high-added-value carbon-based chemicals/fuels can be provided when carbon circulation is realized, and the environment-friendly solar energy environment-friendly carbon-based fuel has the advantages of being green, sustainable and the like and has application prospects. However, the photocatalytic CO 2 conversion technology still faces problems such as low overall conversion efficiency. The efficiency of photocatalytic CO 2 reduction can be effectively improved by widening the light capturing range of the photocatalyst, improving the separation efficiency of carriers, strengthening the dynamics of surface interface reaction and the like.
The light response of the traditional inorganic semiconductor photocatalysis materials (such as TiO 2, znO, cdS and the like) is mainly concentrated in ultraviolet light or visible light, and the photocatalysis reaction is difficult to be driven by near infrared light. In recent years, some metal nitrides have been widely used in infrared light-driven photocatalytic research due to their broad spectrum of light absorption, unique electronic properties, and special band structures. According to the invention, the Ru/TiN photocatalyst is prepared by modifying the surface promoter of the titanium nitride material with broad spectral response, and is applied to ultraviolet-visible-near infrared light-driven photocatalytic CO 2 reduction to generate carbon monoxide, and the promoter Ru can effectively improve the separation efficiency of photogenerated carriers, accelerate the dynamic process of surface interface oxidation-reduction reaction, and further remarkably improve the efficiency of photocatalytic reduction of CO 2.
Disclosure of Invention
The invention aims to provide an ultraviolet-visible-near infrared light response photocatalyst, a preparation method and application thereof, aiming at the defects of the existing photocatalytic conversion technology. Compared with the traditional semiconductor photocatalyst, the Ru/TiN photocatalyst has the characteristic of wide spectral response, can utilize near infrared light to drive CO 2 to selectively reduce and generate CO, and has simple preparation process, considerable yield and wide application prospect.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
An ultraviolet-visible-near infrared light responsive CO 2 reduction photocatalyst is prepared by loading a cocatalyst Ru on titanium nitride (TiN), wherein the loading amount of Ru is 0-1 wt% and is not 0.
The preparation method of the CO 2 reduction photocatalyst comprises the steps of taking commercial titanium dioxide (P25) as a precursor, preparing titanium nitride powder through high-temperature nitridation treatment, and preparing Ru-loaded photocatalyst Ru/TiN through a dipping-reduction method; which comprises the following steps:
(1) Calcining the P25 powder in an ammonia atmosphere to obtain titanium nitride powder;
(2) Uniformly dispersing the obtained titanium nitride powder in deionized water, adding a ruthenium chloride aqueous solution, uniformly stirring, adding a sodium borohydride-containing NaOH solution, reacting, centrifuging, and drying to obtain Ru/TiN.
Further, the flow rate of the ammonia gas in the step (1) is 100-200 mL/min.
Further, the calcination temperature in the step (1) is 750-850 ℃ and the time is 6-10 h.
Further, the mass ratio of the sodium borohydride to the titanium nitride powder used in the step (2) is 1:15-1:8.
Further, the concentration of the NaOH solution in the step (2) is 6 g/L-15 g/L.
The photocatalyst can be used for generating CO through CO 2 reduction driven by ultraviolet-visible-near infrared light.
The invention has the remarkable effects that:
(1) According to the invention, the high-temperature nitridation treatment commercial titanium dioxide is utilized to prepare the TiN photocatalyst with ultraviolet-visible-near infrared light response, and then the Ru/TiN composite photocatalyst is prepared by carrying the Ru cocatalyst on the surface, so that the efficiency and selectivity of preparing CO by reducing photocatalytic CO 2 can be remarkably improved.
(2) The method is simple and easy to implement, has considerable yield and is beneficial to popularization and application.
Drawings
FIG. 1 shows XRD spectra of TiN and 0.5% Ru/TiN prepared in examples 1 and 2.
FIG. 2 shows DRS spectra of TiN and 0.5% Ru/TiN prepared in examples 1 and 2.
FIG. 3 is an SEM image of TiN (a) and 0.5% Ru/TiN (b) prepared according to examples 1, 2.
FIG. 4 is a graph comparing the performance of catalysts with different Ru loadings under near infrared (800 nm) conditions.
FIG. 5 is a graph showing the performance of the 0.5% Ru/TiN prepared in example 2 in photocatalytic reduction of CO 2 at different wavelengths.
Detailed Description
An ultraviolet-visible-near infrared light responsive CO 2 reduction photocatalyst, the preparation method comprising the steps of:
(1) Weighing commercial titanium dioxide powder, placing the commercial titanium dioxide powder in a porcelain boat, then placing the porcelain boat in a high-temperature tube furnace, and introducing ammonia gas 30min to remove air in the tube (the flow is 100-200 mL/min); then heating to 750-850 ℃, calcining 6-10 h, cooling to room temperature, closing the gas, taking out the sample, and preparing TiN powder;
(2) Uniformly dispersing 300-500 mg of TiN powder in 16 mL of deionized water, adding ruthenium chloride aqueous solution (with the concentration of 5 g/L), uniformly stirring, adding 4-mL of NaOH solution (with the concentration of 6-15 g/L) containing 20-100 mg sodium borohydride (NaBH 4), centrifuging after reaction, and drying to obtain Ru/TiN, wherein the Ru load is 0-1 wt% and is not 0.
In order to make the contents of the present invention more easily understood, the technical scheme of the present invention will be further described with reference to the specific embodiments, but the present invention is not limited thereto.
Example 1 TiN preparation
Weighing commercial titanium dioxide powder, placing the commercial titanium dioxide powder in a porcelain boat, then placing the porcelain boat in a high-temperature tube furnace, and introducing ammonia gas 30min to remove air in the tube; then heating to 750 ℃, calcining 6h, cooling to room temperature, closing the gas, taking out the sample, and obtaining the TiN photocatalyst.
EXAMPLE 2 preparation of 0.5% Ru/TiN
Dispersing 500 mg of the TiN powder prepared in the example 1 in 16 mL deionized water, adding 0.5 of mL ruthenium chloride solution (with the concentration of 5 g/L), uniformly stirring, adding 4 of mL of NaOH solution (with the concentration of 10 g/L) containing 50 mg sodium borohydride, centrifuging after the reaction is finished, and drying to prepare 0.5% Ru/TiN.
FIG. 1 is an XRD pattern of the prepared TiN and 0.5% Ru/TiN. As shown in FIG. 1, all diffraction peaks in the XRD spectrum of the TiN sample were matched with the standard XRD spectrum of TiN (JCPLS: 38-1420), and no other impurity peaks were detected, indicating that a high crystallinity, pure phase TiN sample was obtained. In the XRD spectrum of the 0.5% Ru/TiN sample, no characteristic peak of Ru species was detected, except for the diffraction peak of TiN.
FIG. 2 is a DRS plot of the prepared TiN and 0.5% Ru/TiN. As shown, tiN and 0.5% Ru/TiN have the ability to absorb ultraviolet-visible-near infrared light. The light absorption of the 0.5% Ru/TiN sample is blue shifted compared to the TiN sample.
FIG. 3 is an SEM image of the prepared TiN (a) and 0.5% Ru/TiN (b). As shown, both TiN and 0.5% Ru/TiN had coralline-like morphology, indicating that the modification of the promoter did not change the morphology of the TiN sample.
EXAMPLE 3 preparation of 0.2% Ru/TiN
Dispersing 500 mg of the TiN powder prepared in the example 1 in 16 mL deionized water, adding 0.2 of mL ruthenium chloride solution (with the concentration of 5 g/L), stirring uniformly, adding 4 of mL of NaOH solution (with the concentration of 10 g/L) containing 50 mg sodium borohydride, centrifuging after the reaction is finished, and drying to prepare 0.8% Ru/TiN.
EXAMPLE 4 preparation of 0.8% Ru/TiN
Dispersing 500 mg of the TiN powder prepared in the example 1 in 16 mL deionized water, adding 0.8 of mL ruthenium chloride solution (with the concentration of 5 g/L), uniformly stirring, adding 4 mL of NaOH solution (with the concentration of 10 g/L) containing 50 mg sodium borohydride, centrifuging after the reaction is finished, and drying to prepare 0.8% Ru/TiN.
Example 5 Ru/TiN photocatalytic reduction of CO 2 to CO
The catalysts with different Ru loadings prepared in the example of 40mg are respectively dispersed in Dan Yingmin, 1mL deionized water is dripped, the uniformly dispersed catalysts are placed in a 100 ℃ oven for drying, then the catalysts are placed in a batch reactor, after the air in the reactor is exhausted, high-purity CO 2 gas is filled, and the reactor is sealed. 40. Mu.L of deionized water (electron sacrificial agent) was added to the batch reactor through a sampling needle, a 300W xenon lamp was used as a lamp source, and cut-off filters of different wavelengths were provided. The product was detected after 1 hour of illumination.
FIG. 4 is a graph comparing the performance of catalysts with different Ru loadings under near infrared (800 nm) conditions. As shown in the figure, under the irradiation of infrared light, 0.5% Ru/TiN has the optimal photocatalytic performance, and the reaction rate of photocatalytic reduction of CO 2 to CO is 69.09 mu mol g -1h-1, which is about 10 times that of a TiN sample.
FIG. 5 is a graph of the performance of 0.5% Ru/TiN in photocatalytic reduction of CO 2 at different wavelengths. As shown, the photocatalytic reduction CO 2 performance of the 0.5% Ru/TiN sample gradually decreases with wavelength extension, but when the wavelength is greater than 800: 800 nm, the sample still has photocatalytic conversion properties.
The foregoing description is only of the preferred embodiments of the invention, and all changes and modifications that come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (6)
1. The application of an ultraviolet-visible-near infrared light responsive photocatalyst in light-driven CO 2 reduction to produce CO is characterized in that: the photocatalyst is prepared by loading a cocatalyst Ru on titanium nitride; the preparation method comprises the steps of taking commercial titanium dioxide as a precursor, preparing titanium nitride powder through high-temperature nitridation treatment, and preparing the Ru-loaded photocatalyst Ru/TiN through a dipping-reduction method
The loading of the promoter Ru on the titanium nitride is 0-1 wt% and is not 0.
2. The use according to claim 1, characterized in that: the specific preparation of the photocatalyst comprises the following steps:
(1) Calcining commercial titanium dioxide powder in an ammonia atmosphere to obtain titanium nitride powder;
(2) Uniformly dispersing the obtained titanium nitride powder in deionized water, adding a ruthenium chloride aqueous solution, uniformly stirring, adding a sodium borohydride-containing NaOH solution, reacting, centrifuging, and drying to obtain Ru/TiN.
3. The use according to claim 2, characterized in that: the flow of the ammonia gas in the step (1) is 100-200 mL/min.
4. The use according to claim 2, characterized in that: the calcining temperature in the step (1) is 750-850 ℃ and the calcining time is 6-10 h.
5. The use according to claim 2, characterized in that: the mass ratio of the sodium borohydride to the titanium nitride powder used in the step (2) is 1:15-1:8.
6. The use according to claim 2, characterized in that: the concentration of the NaOH solution in the step (2) is 6 g/L-15 g/L.
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| CN108144636A (en) * | 2018-01-31 | 2018-06-12 | 成都新柯力化工科技有限公司 | A kind of cobalt titanate doped titanium nitride photochemical catalyst and preparation method for hydrogen manufacturing |
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| 《Plasmonic Titanium Nitride Tubes Decorated with Ru Nanoparticles as Photo-Thermal Catalyst for CO2 Methanation》;Diego Mateo等;《Molecules》;20221231;第27卷(第9期);第1-10页 * |
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