CN113941348A - BP/BBS heterostructure photocatalyst and preparation method and application thereof - Google Patents
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000007540 photo-reduction reaction Methods 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 8
- 239000007795 chemical reaction product Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000006722 reduction reaction Methods 0.000 abstract description 19
- 230000001699 photocatalysis Effects 0.000 abstract description 15
- 230000000694 effects Effects 0.000 abstract description 7
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 238000007146 photocatalysis Methods 0.000 abstract description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 58
- 229910002092 carbon dioxide Inorganic materials 0.000 description 14
- 230000009467 reduction Effects 0.000 description 13
- 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 7
- 239000001569 carbon dioxide Substances 0.000 description 5
- 238000013329 compounding Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000013032 photocatalytic reaction Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000001228 spectrum 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
- 239000003054 catalyst Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000008569 process Effects 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
- 230000004075 alteration Effects 0.000 description 1
- 239000000969 carrier Substances 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
- 238000011217 control strategy 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
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental 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
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000006467 substitution reaction 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
-
- 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)
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- 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 water, and obtaining the BP/BBS heterostructure photocatalyst after reaction. A heterostructure photocatalyst is prepared by the preparation method. Heterostructure photocatalyst in CO2Application in photoreduction. The invention has the beneficial effects that: the preparation method has the advantages of simple and safe operation, 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 BP2Reduction activity; the obtained 2D/1D BP/BBS heterostructure photocatalyst 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
CO2Is the most common gas compound, can be used for preparing various high value-added chemicals, and can also cause serious greenhouse effect, so how to efficiently react CO under mild conditions2Into high value-added chemicals, aHas been one of the research hotspots and difficulties in the field of catalysis, and the difficulty is mainly that the high activation energy of C ═ O (about 750kJ mol)-1) Making photocatalytic carbon dioxide conversion difficult. Conventional thermocatalytic conversion of CO2The method has high energy consumption and harsh reaction conditions, and compared with the method, the photocatalysis technology reaction is concerned by extensive research workers due to the advantages of mild conditions, environmental protection and the like.
It is generally believed that there are three key factors that essentially determine the catalytic efficiency during the reaction of photocatalytic carbon dioxide reduction, namely absorption of light, 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 efficiently separated; then, the surface of the catalyst is beneficial to the adsorption and reduction of carbon dioxide; CO 22The photoreduction is a process of coupling multiple protons and transferring electrons, and according to the number of transferred electrons, CO and CH can be generated3OH and CH4And the like. It is noted that in these C1 products, the formation of CO requires 2 electrons, less than CH, from a kinetic point of view3OH and CH4The desired 6 and 8 electrons are formed. However, CH4Formation ratio of CO and CH3The formation of OH is more thermodynamically favored due to CH4Can be formed at a lower potential E0redox-0.53 vvsshe, and CO: e0redox-0.24 vvsshe. This suggests that carbon dioxide reduction is limited by kinetics and thermodynamics, which together determine CO2Product selectivity and efficiency of photoreduction. In addition, the factors such as the pH value of the solution, the added sacrificial agent and the like are also considered in the process of reducing the carbon dioxide.
Although the photocatalytic materials are various, the existing photocatalysts generally have the problems of limited solar energy utilization efficiency, low separation efficiency of photon-generated carriers and the like, and in order to obtain CO with high activity, low cost and high selectivity2The different control strategies adopted by scientists for the photo-reduction photocatalyst, such as constructing defects on the surface of the catalyst, and preparing the catalyst into a two-dimensional ultrathin structure and a heterojunctionPreparation of the structure and the like.
Researches show that the construction of the heterostructure is an important factor influencing the activity of the photocatalytic reaction, and the photocatalyst of the 2D/2D and 2D/1D heterostructures has the characteristics of large interface area, strong interaction and wide photoresponse range and is greatly concerned by people. At present, the research on BP/BBS (2D/1D) heterostructure photocatalysts is very limited, especially for use in CO2The field of photoreduction is not reported at present.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a BP/BBS heterostructure photocatalyst, a preparation method and an 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 (3) dissolving the BBS and the BP in water, and finishing the reaction to obtain the BP/BBS heterostructure photocatalyst.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, BBS and BP were dissolved in water and then compounded by stirring at room temperature.
Further, the stirring time at 25 ℃ plus or minus 5 ℃ is 6 plus or minus 1 h.
And further, after the reaction is finished, washing and vacuum drying the reaction product to obtain the BP/BBS heterostructure photocatalyst.
Further, the temperature of vacuum drying is 75 ℃ plus or minus 5 ℃ and the time is 10 plus or minus 2 hours.
Further, the content of BP is 1 wt% -7 wt%.
Further, the content of BP is 1 wt%, 3 wt%, 5 wt% or 7 wt%.
A BP/BBS heterostructure photocatalyst prepared by the preparation method.
BP/BBS heterostructure photocatalyst in CO2Application in photoreduction.
The invention has the beneficial effects that:
1) the 2D/1D BP/BBS heterostructure photocatalyst is prepared by common stirring, and the preparation method has the advantages of simple 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 BP2Reduction activity;
3) the obtained 2D/1D BP/BBS heterostructure photocatalyst 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 according to the present invention, in which curves (b), (c), (d) and (e) are XRD spectra of BP/BBS heterostructure photocatalysts prepared in examples 1, 2, 3 and 4, respectively;
FIG. 2 shows the photocatalytic CO of the series of BP/BBS heterostructure photocatalysts prepared by the invention2The reduction effect graphs are (b), (c), (d) and (e) are the photocatalytic reduction CO of the series of BP/BBS heterostructure photocatalysts prepared in example 1, example 2, example 3 and example 4 respectively2And (5) effect diagrams.
FIG. 3 is a TEM image of a 5 wt% BP/BBS heterostructure photocatalyst prepared according to the present invention.
Detailed Description
The principles and features of this invention are described below in conjunction with the following drawings, which are set forth by way of illustration only and are not intended to limit the scope of the invention.
Example 1
A BP/BBS heterostructure photocatalyst is prepared by the following method:
1) 50mg of BBS (Bi)19Br3S27) Dispersing the mixture into 20mL of water to obtain a mixed solution A;
2) then 100 mul 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 stirring and compounding the mixed solution B for 6 +/-1 h at the temperature of 25 +/-5 ℃, after the reaction is finished, washing and drying a reaction product, and performing vacuum drying at the temperature of 75 +/-5 ℃ for 10 +/-2 h to obtain the BP/BBS heterostructure photocatalyst which is recorded as 1 wt% of the BP/BBS photocatalyst.
The XRD spectrum of the 1 wt% BP/BBS photocatalyst prepared in the example is shown in figure 1 (b), and figure 1 (b) shows that the XRD peaks of the obtained product are consistent with the characteristic peak of the standard BBS, and the characteristic peak of BP is not obviously detected, possibly caused by the low content of the characteristic peak;
the 1 wt% BP/BBS photocatalyst prepared in this example was used to catalyze CO2Reduction, wherein a 300W xenon lamp is used as a light source in the experiment, and a photocatalytic reduction experiment shows that the 1 wt% BP/BBS photocatalyst prepared in the embodiment catalyzes CO under the irradiation of visible light after the photocatalytic reaction is carried out for 6 hours2The amount of CO produced by the reduction was 203.0878. mu. mol g-1，CH4The amount of (B) is 71.7342. mu. mol. g-1Furthermore, H2The amount of (B) 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 of BBS (Bi)19Br3S27) Dispersing the mixture into 20mL of water to obtain a mixed solution A;
2) then 300 mul 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 stirring and compounding the mixed solution B for 6 +/-1 h at the temperature of 25 +/-5 ℃, after the reaction is finished, washing and drying a reaction product, and performing vacuum drying at the temperature of 75 +/-5 ℃ for 10 +/-2 h to obtain the BP/BBS heterostructure photocatalyst which is recorded as 3 wt% of the BP/BBS photocatalyst.
The XRD spectrum of the 3 wt% BP/BBS photocatalyst prepared in the example is shown in figure 1 (c), and figure 1 (c) shows that the XRD peaks of the obtained product are consistent with the characteristic peak of the standard BBS, and the characteristic peak of BP is not obviously detected, possibly caused by the low content of the characteristic peak;
the 3 wt% BP/BBS photocatalyst prepared in this example was used to catalyze CO2Reduction, wherein a 300W xenon lamp is used as a light source in the experiment, and the photocatalytic reduction experiment shows that the product is obtained after 4 hours of photocatalytic reactionThe 3 wt% BP/BBS photocatalyst prepared in the example can catalyze CO under the irradiation of visible light2The amount of CO produced by the reduction was 236.9084. mu. mol g-1，CH4The amount of (B) is 85.4371. mu. mol. g-1Furthermore, H2The amount of (B) is 69.6719. mu. mol. g-1(2 (c) in the figure).
Example 3
A BP/BBS heterostructure photocatalyst is prepared by the following method:
1) 50mg of BBS (Bi)19Br3S27) Dispersing the mixture into 20mL of water to obtain a mixed solution A;
2) then adding 500 mul of BP (black phosphorus) solution with the concentration of 5mg/L into the reaction solution to obtain a mixed solution B;
3) and stirring and compounding the mixed solution B for 6 +/-1 h at the temperature of 25 +/-5 ℃, after the reaction is finished, washing and drying a reaction product, and performing vacuum drying at the temperature of 75 +/-5 ℃ for 10 +/-2 h to obtain the BP/BBS heterostructure photocatalyst which is recorded as 5 wt% of the BP/BBS photocatalyst.
The XRD pattern of the 5 wt% BP/BBS photocatalyst prepared in this example is shown in FIG. 1 (d), and FIG. 1 (d) shows that the XRD peaks of the obtained product are consistent with the characteristic peaks of the standard BBS, and it can be seen by TEM (FIG. 3) that BP is uniformly distributed on the rod-shaped BBS;
the 5 wt% BP/BBS photocatalyst prepared in this example was used to catalyze CO2Reduction, wherein a 300W xenon lamp is used as a light source in the experiment, and the photocatalytic reduction experiment shows that after the photocatalytic reaction is carried out for 4 hours, the 5 wt% BP/BBS photocatalyst prepared in the embodiment catalyzes CO under the irradiation of visible light2The amount of CO produced by the reduction was 399.1261. mu. mol g-1，CH4The amount of (B) is 64.7614. mu. mol. g-1Furthermore, H2The amount of (B) is 212.7888. mu. mol. g-1(FIG. 2 (d)).
Example 4
A BP/BBS heterostructure photocatalyst is prepared by the following method:
1) 50mg of BBS (Bi)19Br3S27) Dispersing the mixture into 20mL of water to obtain a mixed solution A;
2) then 700 mul 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 stirring and compounding the mixed solution B for 6 +/-1 h at the temperature of 25 +/-5 ℃, after the reaction is finished, washing and drying a reaction product, and performing vacuum drying at the temperature of 75 +/-5 ℃ for 10 +/-2 h to obtain the BP/BBS heterostructure photocatalyst which is recorded as 7 wt% of BP/BBS photocatalyst.
The XRD spectrum of the 7 wt% BP/BBS photocatalyst prepared in the example is shown in (f) in FIG. 1, and (f) in FIG. 1 shows that the XRD peaks of the obtained product are consistent with the characteristic peak of the standard BBS, and the characteristic peak of BP is not obviously detected;
the 7 wt% BP/BBS photocatalyst prepared in this example was used to catalyze CO2Reduction, wherein a 300W xenon lamp is used as a light source in the experiment, and a photocatalytic reduction experiment shows that after the photocatalytic reaction is carried out for 4 hours, the 7 wt% BP/BBS photocatalyst prepared in the embodiment catalyzes CO under the irradiation of visible light2The amount of CO produced by the reduction was 178.0483. mu. mol g-1，CH4The amount of (B) is 116.3057. mu. mol. g-1Furthermore, H2The amount of (B) is 12.1356. mu. mol. g-1(2 (e) in the figure).
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (9)
1. A preparation method of a BP/BBS heterostructure photocatalyst is characterized by comprising the following steps:
and (3) dissolving the BBS and the BP in water, and finishing the reaction to obtain the BP/BBS heterostructure photocatalyst.
2. The method for preparing the BP/BBS heterostructure photocatalyst according to claim 1, wherein the method comprises the following steps: BBS and BP are dissolved in water and then stirred and compounded at room temperature.
3. The method for preparing a BP/BBS heterostructure photocatalyst according to claim 1 or 2, wherein: stirring at 25 +/-5 deg.C for 6 +/-1 hr.
4. A BP/BBS according to claim 1 or 2 or 37The preparation method of the heterostructure photocatalyst is characterized in that: and after the reaction is finished, washing and vacuum drying the reaction product to obtain the BP/BBS heterostructure photocatalyst.
5. The method for preparing the BP/BBS heterostructure photocatalyst according to claim 4, wherein the method comprises the following steps: the temperature of vacuum drying is 75 ℃ plus or minus 5 ℃, and the time is 10h plus or minus 2 h.
6. The method for preparing the BP/BBS heterostructure photocatalyst according to claim 1, wherein the method comprises the following steps: the content of BP is 1 wt% -7 wt%.
7. The method for preparing the BP/BBS heterostructure photocatalyst according to claim 6, wherein the method comprises the following steps: the BP content is 1 wt.%, 3 wt.%, 5 wt.% or 7 wt.%.
8. A BP/BBS heterostructure photocatalyst, prepared by the method of any of claims 1 to 8.
9. The BP/BBS heterostructure photocatalyst of claim 8 in CO2Application in photoreduction.
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