CN113941348B - BP/BBS heterostructure photocatalyst and preparation method and application thereof - Google Patents
BP/BBS heterostructure photocatalyst and preparation method and application thereof Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 238000007540 photo-reduction reaction Methods 0.000 claims abstract description 7
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 66
- 238000001291 vacuum drying Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000007795 chemical reaction product Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 4
- 238000013329 compounding Methods 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 21
- 238000000034 method Methods 0.000 abstract description 8
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 238000007146 photocatalysis Methods 0.000 abstract description 3
- 230000010757 Reduction Activity Effects 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000006722 reduction reaction Methods 0.000 description 17
- 230000009467 reduction Effects 0.000 description 16
- 239000011259 mixed solution Substances 0.000 description 12
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 10
- 239000000243 solution Substances 0.000 description 9
- 238000002474 experimental method Methods 0.000 description 8
- 239000000047 product Substances 0.000 description 6
- 229910002092 carbon dioxide Inorganic materials 0.000 description 5
- 239000001569 carbon dioxide Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000013032 photocatalytic reaction Methods 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 229910052724 xenon Inorganic materials 0.000 description 4
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/186—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/40—Carbon monoxide
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention relates to a preparation method of a BP/BBS heterostructure photocatalyst, which comprises the following steps of dissolving BBS and BP in waterAnd after the reaction is finished, the BP/BBS heterostructure photocatalyst can be obtained. A heterostructure photocatalyst made by the method of preparation. Heterostructure photocatalyst in CO 2 Application in photoreduction. The beneficial effects of the invention are as follows: the preparation method has the advantages of simple operation, safety, low cost and the like; the prepared BP/BBS heterostructure photocatalyst has high junction purity, and the photocatalytic CO of the BP/BBS heterostructure photocatalyst can be controlled by changing the content of BP 2 Reduction activity; the obtained BP/BBS heterostructure photocatalyst of 2D/1D has high catalytic activity and good application prospect in the field of photocatalysis.
Description
Technical Field
The invention relates to the field of photocatalysts, in particular to a BP/BBS heterostructure photocatalyst, and a preparation method and application thereof.
Background
CO 2 Is the most common gas compound, can be used for preparing various high-added-value chemicals and can also cause serious greenhouse effect, so that how to efficiently treat CO under mild conditions 2 Conversion to high value-added chemicals has been one of the hot spots and difficulties in the catalytic field, mainly due to the high c=o activation energy (about 750kJ mol -1 ) Making photocatalytic carbon dioxide conversion difficult. Traditional thermocatalytic conversion of CO 2 Compared with the photocatalysis technology, the method has the advantages of mild condition, environment protection and the like, and is focused by vast researchers.
It is generally believed that three key factors in the photocatalytic carbon dioxide reduction reaction process essentially determine the catalytic efficiency, namely light absorption, charge separation and transport, and surface catalysis. First, a strong light trapping capability is required to provide sufficient electron-hole pairs; second, the generated electron-hole should be effectively separated; then, the surface of the catalyst is favorable for adsorption and reduction of carbon dioxide; CO 2 The photo-reduction is a multiple proton coupling and electron transfer process, and can generate CO and CH according to the difference of the number of transferred electrons 3 OH and CH 4 And the like. It should be noted that in these C1 products, the kinetics are fromFrom the point of view, CO formation requires 2 electrons, less than CH 3 OH and CH 4 The desired 6 electrons and 8 electrons are formed. However, CH 4 Formation ratio of CO and CH 3 OH formation is more thermodynamically advantageous due to CH 4 Can be formed at a lower potential E 0redox = -0.53VvsNHE, whereas CO: e (E) 0redox = -0.24VvsNHE. This suggests that carbon dioxide reduction is limited by kinetics and thermodynamics, which together determine CO 2 The product selectivity and efficiency of the photoreduction. In addition, the pH value of the solution, the added sacrificial agent and other factors are also considered in the carbon dioxide reduction process.
Although photocatalytic materials are various, the existing photocatalyst generally has the problems of limited solar energy utilization efficiency, low photon-generated carrier separation efficiency and the like in view of the overall situation, and aims to obtain CO with high activity, low cost and high selectivity 2 The photoreduction photocatalyst adopts different regulation strategies for the catalyst by scientists, such as constructing defects on the surface of the catalyst, preparing the catalyst into a two-dimensional ultrathin structure, preparing a heterostructure and the like.
Research shows that the construction of the heterostructure is an important factor influencing the photocatalytic reaction activity, and the 2D/2D and 2D/1D heterostructure photocatalysts have the characteristics of large interface area, strong interaction and wide photoresponse range, and are greatly focused by people. Currently, very limited research is done on BP/BBS (2D/1D) heterostructure photocatalysts, especially for use with CO 2 The field of photoreduction has not been reported yet.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a BP/BBS heterostructure photocatalyst, and a preparation method and application thereof, so as to overcome the defects in the prior art.
The technical scheme for solving the technical problems is as follows: a preparation method of a BP/BBS heterostructure photocatalyst comprises the following steps:
and dissolving BBS and BP in water, and ending the reaction to obtain the BP/BBS heterostructure photocatalyst.
On the basis of the technical scheme, the invention can be improved as follows.
Further, BBS and BP were dissolved in water and then combined with stirring at room temperature.
Further, the stirring time at 25.+ -. 5 ℃ was 6.+ -. 1h.
Further, after the reaction is finished, washing and vacuum drying reaction products, and obtaining the BP/BBS heterostructure photocatalyst.
Further, the temperature of the vacuum drying was 75.+ -. 5 ℃ and the time was 10.+ -. 2h.
Further, the BP content is 1wt% to 7wt%.
Further, the BP content was 1wt%, 3wt%, 5wt% or 7wt%.
A BP/BBS heterostructure photocatalyst is prepared by the preparation method.
BP/BBS heterostructure photocatalyst in CO 2 Application in photoreduction.
The beneficial effects of the invention are as follows:
1) The 2D/1D BP/BBS heterostructure photocatalyst is prepared by adopting common stirring, and the preparation method has the advantages of simplicity in operation, safety, low cost and the like;
2) The prepared BP/BBS heterostructure photocatalyst has high junction purity, and the photocatalytic CO of the BP/BBS heterostructure photocatalyst can be controlled by changing the content of BP 2 Reduction activity;
3) The obtained BP/BBS heterostructure photocatalyst of 2D/1D has high catalytic activity and good application prospect in the field of photocatalysis.
Drawings
FIG. 1 is an XRD spectrum of a series of BP/BBS heterostructure photocatalysts prepared by the present invention, wherein curves (b), (c), (d) and (e) are XRD spectra of BP/BBS heterostructure photocatalysts prepared in example 1, example 2, example 3 and example 4, respectively;
FIG. 2 shows the photocatalytic CO of the series BP/BBS heterostructure photocatalyst prepared by the present invention 2 Reduction effect is shown in the figures, wherein graphs (b), (c), (d) and (e) are the light of series BP/BBS heterostructure photocatalysts prepared in example 1, example 2, example 3 and example 4, respectivelyCatalytic reduction of CO 2 Effect diagram.
FIG. 3 is a TEM image of a 5wt% BP/BBS heterostructure photocatalyst prepared according to the present invention.
Detailed Description
The principles and features of the present invention are described below with reference to the drawings, the examples are illustrated for the purpose of illustrating the invention and are not to be construed as limiting the scope of the invention.
Example 1
A BP/BBS heterostructure photocatalyst is prepared by the following method:
1) 50mg BBS (Bi 19 Br 3 S 27 ) Dispersing to 20mL of water to obtain a mixed solution A;
2) Then 100. Mu.l of BP (black phosphorus) solution with the concentration of 5mg/L is added into the reaction solution to obtain a mixed solution B;
3) And (3) mixing the mixed solution B at the temperature of 25+/-5 ℃ for 6+/-1 h, washing and drying a reaction product after the reaction is finished, and performing vacuum drying at the temperature of 75+/-5 ℃ for 10 hours+/-2 h to obtain the BP/BBS heterostructure photocatalyst, wherein the BP/BBS heterostructure photocatalyst is marked as 1wt% BP/BBS photocatalyst.
The XRD spectrum of the 1wt% BP/BBS photocatalyst prepared in this example is shown in FIG. 1 (b), and in FIG. 1 (b), it is shown that the XRD peak of the obtained product is consistent with the characteristic peak of standard BBS, and the characteristic peak of BP is not detected obviously, possibly due to the lower content of BP;
the 1wt% BP/BBS photocatalyst prepared in this example was used for the photocatalytic CO 2 Reduction, in the experiment, a 300W xenon lamp is adopted as a light source, and the photocatalytic reduction experiment shows that the 1wt% BP/BBS photocatalyst prepared in the embodiment after photocatalytic reaction for 6 hours is subjected to photocatalytic CO under the irradiation of visible light 2 The reduction to CO yield was 203.0878. Mu. Mol g -1 ，CH 4 The amount of (C) is 71.7342 mu mol g -1 In addition, H 2 The amount of (C) is 95.7049 mu mol g -1 (fig. 2 (b)).
Example 2
A BP/BBS heterostructure photocatalyst is prepared by the following method:
1) 50mg BBS (Bi 19 Br 3 S 27 ) Dispersing to 20mL of water to obtain a mixed solution A;
2) Then, 300. Mu.l of BP (black phosphorus) solution with a concentration of 5mg/L was added to the above reaction solution to obtain a mixed solution B;
3) And (3) mixing the mixed solution B at the temperature of 25+/-5 ℃ for 6+/-1 h, washing and drying a reaction product after the reaction is finished, and performing vacuum drying at the temperature of 75+/-5 ℃ for 10 hours+/-2 h to obtain the BP/BBS heterostructure photocatalyst, wherein the BP/BBS heterostructure photocatalyst is marked as 3wt% BP/BBS photocatalyst.
The XRD spectrum of the 3wt% BP/BBS photocatalyst prepared in this example is shown in FIG. 1 (c), and in FIG. 1 (c), it is shown that the XRD peak of the obtained product is consistent with the characteristic peak of standard BBS, and the characteristic peak of BP is not detected obviously, possibly due to the lower content of BP;
the 3wt% BP/BBS photocatalyst prepared in this example was used for photocatalytic CO 2 Reduction, in the experiment, a 300W xenon lamp is adopted as a light source, and the photocatalytic reduction experiment shows that after 4 hours of photocatalytic reaction, the 3wt% BP/BBS photocatalyst prepared in the embodiment has photocatalytic CO under the irradiation of visible light 2 The reduction to CO yield was 236.9084. Mu. Mol g -1 ，CH 4 The amount of (C) is 85.4371 mu mol g -1 In addition, H 2 The amount of (C) is 69.6719 mu mol g -1 (in FIG. 2 (c)).
Example 3
A BP/BBS heterostructure photocatalyst is prepared by the following method:
1) 50mg BBS (Bi 19 Br 3 S 27 ) Dispersing to 20mL of water to obtain a mixed solution A;
2) Then, 500. Mu.l of BP (black phosphorus) solution with a concentration of 5mg/L was added to the above reaction solution to obtain a mixed solution B;
3) And (3) mixing the mixed solution B at the temperature of 25+/-5 ℃ for 6+/-1 h, washing and drying a reaction product after the reaction is finished, and performing vacuum drying at the temperature of 75+/-5 ℃ for 10 hours+/-2 h to obtain the BP/BBS heterostructure photocatalyst, wherein the BP/BBS heterostructure photocatalyst is marked as 5wt% BP/BBS photocatalyst.
XRD spectra of the 5wt% BP/BBS photocatalyst prepared in the embodiment are shown in (d) of figure 1, and (d) of figure 1 shows that XRD peaks of the obtained product are consistent with characteristic peaks of standard BBS, and BP can be uniformly distributed on the rod-shaped BBS through TEM (figure 3);
the 5wt% BP/BBS photocatalyst prepared in this example was used to photocatalytic CO 2 Reduction, in the experiment, a 300W xenon lamp is adopted as a light source, and the photocatalytic reduction experiment shows that after 4 hours of photocatalytic reaction, the 5wt% BP/BBS photocatalyst prepared in the embodiment has photocatalytic CO under the irradiation of visible light 2 The reduction to CO yield was 399.1261. Mu. Mol g -1 ，CH 4 The amount of (C) is 64.7614 mu mol g -1 In addition, H 2 The amount of (C) is 212.7888 mu mol g -1 (in FIG. 2 (d)).
Example 4
A BP/BBS heterostructure photocatalyst is prepared by the following method:
1) 50mg BBS (Bi 19 Br 3 S 27 ) Dispersing to 20mL of water to obtain a mixed solution A;
2) Then, 700. Mu.l of BP (black phosphorus) solution with the concentration of 5mg/L was added to the above reaction solution to obtain a mixed solution B;
3) And (3) mixing the mixed solution B at the temperature of 25+/-5 ℃ for 6+/-1 h, washing and drying a reaction product after the reaction is finished, and performing vacuum drying at the temperature of 75+/-5 ℃ for 10 hours+/-2 h to obtain the BP/BBS heterostructure photocatalyst, wherein the BP/BBS heterostructure photocatalyst is marked as 7wt% BP/BBS photocatalyst.
XRD spectra of the 7wt% BP/BBS photocatalyst prepared in the embodiment are shown in (f) of figure 1, and (f) of figure 1 shows that XRD peak of the obtained product is consistent with characteristic peaks of standard BBS, and no characteristic peak of BP is detected obviously;
the 7wt% BP/BBS photocatalyst prepared in this example was used for photocatalytic CO 2 Reduction, in the experiment, a 300W xenon lamp is adopted as a light source, and the photocatalytic reduction experiment shows that after 4 hours of photocatalytic reaction, the 7wt% BP/BBS photocatalyst prepared in the embodiment has photocatalytic CO under the irradiation of visible light 2 The reduction to CO yield was 178.0483. Mu. Mol g -1 ，CH 4 The amount of (C) is 116.3057 mu mol g -1 In addition, H 2 The amount of (C) is 12.1356 mu mol g -1 (in FIG. 2 (e)).
While embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are illustrative and not to be construed as limiting the invention, and that variations, modifications, alternatives and variations may be made to the above embodiments by one of ordinary skill in the art within the scope of the invention.
Claims (5)
1. The application of the BP/BBS heterostructure photocatalyst is characterized in that the BP/BBS heterostructure photocatalyst is applied to CO 2 Photo-reduction;
the preparation method of the BP/BBS heterostructure photocatalyst comprises the following steps:
dissolving BBS and BP in water, stirring and compounding at room temperature, after the reaction is finished, washing the reaction product, and vacuum drying to obtain BP/BBS heterostructure photocatalyst, wherein BBS is Bi 19 Br 3 S 27 BP is black phosphorus.
2. The use according to claim 1, characterized in that: BBS and BP are dissolved in water and then are stirred and compounded at 25+/-5 ℃ for 6+/-1 h.
3. The use according to claim 1, characterized in that: the temperature of vacuum drying is 75+/-5 ℃ and the time is 10+/-2 hours.
4. The use according to claim 1, characterized in that: BP content is 1wt% -7 wt%.
5. The use according to claim 4, characterized in that: BP content was 1wt%, 3wt%, 5wt% or 7wt%.
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| CN109759098A (en) * | 2019-03-07 | 2019-05-17 | 郑州大学 | Novel nano red phosphorus photochemical catalyst, preparation method and the application in degradation water in dyestuff and photocatalysis water hydrogen manufacturing |
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| US10727050B1 (en) * | 2016-06-15 | 2020-07-28 | Northrop Grumman Systems Corporation | Wafer-scale catalytic deposition of black phosphorus |
| CN107447229B (en) * | 2017-07-14 | 2019-01-25 | 中国科学院长春应用化学研究所 | A kind of method that electro-catalysis reduction carbon dioxide generates ethyl alcohol |
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| CN109759097B (en) * | 2019-03-06 | 2021-11-19 | 郑州大学 | Nano red phosphorus photocatalytic material and preparation method and application thereof |
| CN111185210B (en) * | 2020-01-15 | 2020-09-25 | 湖南大隆环境科技有限公司 | Titanium carbide/titanium dioxide/black phosphorus nanosheet composite photocatalyst and preparation method and application thereof |
| CN111871445A (en) * | 2020-08-13 | 2020-11-03 | 郑州大学 | CN/BOS van der Waals heterostructure photocatalyst and preparation method thereof |
| CN112076769A (en) * | 2020-09-15 | 2020-12-15 | 大连民族大学 | Spherical bismuth vanadate/black phosphorus composite photocatalyst and preparation method thereof |
| CN113083367B (en) * | 2021-04-08 | 2022-11-18 | 郑州大学 | Single-atom catalytic material NiPc-MPOP for efficient photocatalytic carbon dioxide reduction and preparation method thereof |
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