CN113198505A - Sodium bismuth titanate/graphite phase carbon nitride heterojunction piezoelectric photocatalyst and preparation method thereof - Google Patents
Sodium bismuth titanate/graphite phase carbon nitride heterojunction piezoelectric photocatalyst and preparation method thereof Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 85
- FSAJRXGMUISOIW-UHFFFAOYSA-N bismuth sodium Chemical compound [Na].[Bi] FSAJRXGMUISOIW-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 229910002115 bismuth titanate Inorganic materials 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 37
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 26
- 239000010439 graphite Substances 0.000 title claims abstract description 26
- 239000002105 nanoparticle Substances 0.000 claims abstract description 37
- 238000003756 stirring Methods 0.000 claims abstract description 26
- 238000000227 grinding Methods 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- 230000008569 process Effects 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims description 51
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 33
- 239000002243 precursor Substances 0.000 claims description 22
- 238000001816 cooling Methods 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 18
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
- 239000011259 mixed solution Substances 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 18
- 239000002244 precipitate Substances 0.000 claims description 18
- 239000000047 product Substances 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 16
- 239000004570 mortar (masonry) Substances 0.000 claims description 14
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 12
- 239000004202 carbamide Substances 0.000 claims description 12
- 239000004809 Teflon Substances 0.000 claims description 11
- 229920006362 Teflon® Polymers 0.000 claims description 11
- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical compound O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 claims description 11
- 230000015572 biosynthetic process Effects 0.000 claims description 9
- 239000007795 chemical reaction product Substances 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 238000003786 synthesis reaction Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims description 7
- 239000010935 stainless steel Substances 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 230000004044 response Effects 0.000 claims description 2
- 230000035807 sensation Effects 0.000 claims description 2
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 36
- 230000001699 photocatalysis Effects 0.000 abstract description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 8
- 230000003197 catalytic effect Effects 0.000 abstract description 8
- 239000001257 hydrogen Substances 0.000 abstract description 8
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 8
- 230000002194 synthesizing effect Effects 0.000 abstract description 8
- 238000001354 calcination Methods 0.000 abstract description 6
- 230000015556 catabolic process Effects 0.000 abstract description 5
- 238000006731 degradation reaction Methods 0.000 abstract description 5
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 5
- 239000003054 catalyst Substances 0.000 abstract description 4
- 230000005684 electric field Effects 0.000 abstract description 3
- 230000010287 polarization Effects 0.000 abstract description 2
- 238000012719 thermal polymerization Methods 0.000 abstract description 2
- 239000012071 phase Substances 0.000 description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 12
- 239000000243 solution Substances 0.000 description 12
- 239000000969 carrier Substances 0.000 description 7
- 239000010931 gold Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 229910002113 barium titanate Inorganic materials 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 4
- 229940043267 rhodamine b Drugs 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 230000004298 light response Effects 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000002305 electric material Substances 0.000 description 1
- 238000004134 energy conservation 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
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000002198 surface plasmon resonance spectroscopy Methods 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
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- B01J27/24—Nitrogen compounds
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Abstract
The invention discloses a sodium bismuth titanate/graphite phase carbon nitride heterojunction piezoelectric photocatalyst and a preparation method thereof, and solves the problems that the existing heterojunction photocatalyst is complex in preparation and high in cost, and g-C cannot be improved to the maximum extent3N4The catalytic activity of (2). The invention synthesizes graphite by a one-step thermal polymerization methodThe phase carbon nitride photocatalyst is prepared by synthesizing sodium bismuth titanate nano particles in one-step hydrothermal process and then obtaining NBT/g-C through simple grinding, mixing and calcining3N4Heterojunction piezoelectric photocatalyst, g-C3N4The photo-generated carrier can be generated by absorbing part of visible light, the surface of the piezoelectric material NBT generates charges due to external pressure in the stirring process, and meanwhile, the piezoelectric polarization forms a built-in electric field at the interface of the two materials to drive photo-generated electrons and holes to move in opposite directions. The invention controls NBT and g-C3N4The piezoelectric photocatalyst with different photocatalytic performances can be obtained according to the proportion of the components in the catalyst, and can be used for organic dye degradation and hydrogen production.
Description
Technical Field
The invention belongs to the technical field of photocatalytic energy conversion, and particularly relates to a sodium bismuth titanate/graphite phase carbon nitride heterojunction piezoelectric photocatalyst and a preparation method thereof.
Background
The crisis of energy shortage and environmental pollution caused by global industrialization are two major problems in the 21 st century. Photocatalysis is a clean, safe, sustainable technology that can convert endless solar energy into chemical energy.
Graphite phase carbon nitride (g-C) for the last decade3N4) The advantages of absorbing part of visible light, being suitable for band edge positions, high physicochemical thermal stability, economy, environmental protection and the like are widely concerned; however, compared with a theoretical single-component material, the material has a very low specific surface area and few reactive active sites, and low crystallinity results in high photon-generated carrier recombination rate and narrow visible light response, which are three major bottleneck problems limiting the promotion of the photocatalytic activity at present. Therefore, other materials and g-C are currently used3N4In combination with the formation of a heterojunction to improve the transport of photo-generated charge.
For example, document 1 "Rational constraint of plasma Au associated ferroelectric-BaTiO3/Au/g-C3N4 Z-scheme system for efficient photocatalysis[J]Catalysis Today,2020,355,311-31 "discloses a BaTiO3/Au/g-C3N4Z-type heterojunction photocatalyst, in which gold nanoparticles are present as electrons in barium titanate (BaTiO)3) And g-C3N4The medium for conduction between the two elements can also introduce an additional surface plasmon resonance effect, so that the separation of effective photon-generated carriers and high electron reduction capability are realized, and the enhanced activities of photocatalytic hydrogen production and rhodamine B degradation are shown; however, the material uses precious metal gold, which is not beneficial to saving cost and practical application, and the preparation method of the technical scheme is complex and is used for preparing BaTiO3/Au/g-C3N4BaTiO is not considered in the case of Z-type heterojunction photocatalyst3The piezoelectric and ferroelectric properties of (1) cannot fully exert BaTiO considering only that it promotes the separation and transport of photo-generated charges as a heterojunction3The piezoelectric and ferroelectric properties of BaTiO are suppressed3/Au/g-C3N4The development and application of the Z-type heterojunction photocatalyst.
Overview of the presently disclosed compounds with g-C3N4Of more interest in the materials and methods of forming heterojunctions is that the introduction of another material promotes g-C3N4The separation and transmission of photo-generated charges are not fully considered by the characteristics of the introduced material, and therefore, the g-C is not improved to the maximum extent3N4The catalytic activity of (3) inhibits the application development of the photocatalyst; is visible for g-C3N4The study of the base heterojunction piezoelectric photocatalyst still has shortcomings.
In view of the above, it is necessary to combine the piezo-catalysis and the photo-catalysis to deeply research the materials, and introduce a suitable piezo-electric material to improve the g-C3N4The catalytic activity of (3).
Disclosure of Invention
The invention aims to solve the problems that the existing heterojunction photocatalyst is complex in preparation and high in cost, and g-C cannot be improved to the maximum extent3N4The problem of catalytic activity of the bismuth sodium titanate/graphite phase carbon nitride heterojunction piezoelectric photocatalyst and a preparation method thereof are provided.
In order to achieve the purpose, the technical solution provided by the invention is as follows:
a preparation method of a sodium bismuth titanate/graphite phase carbon nitride heterojunction piezoelectric photocatalyst is characterized by comprising the following steps:
1) synthesis of g-C3N4Photocatalyst and process for producing the same
1.1) taking urea as a precursor, heating to 520-550 ℃ at a heating rate of 5 +/-1 ℃/min, preserving heat for 2-4 h, and cooling to room temperature to obtain a blocky product;
1.2) the block product obtained in step 1.1)Grinding into powder to obtain powder with specific surface area of 50-100m2G of/g of3N4A photocatalyst;
2) preparation of sodium bismuth titanate/graphite phase carbon nitride heterojunction piezoelectric photocatalyst
g-C obtained in step 1)3N4Uniformly mixing the photocatalyst and the sodium bismuth titanate nanoparticles, heating to 380-420 ℃ at a heating rate of 5 +/-1 ℃/min, preserving heat for 2-4 h, and cooling to room temperature to obtain the sodium bismuth titanate/graphite phase carbon nitride heterojunction piezoelectric photocatalyst.
Further, in step 2), the g-C3N4The mass ratio of the photocatalyst to the sodium bismuth titanate nano particles is 1: 0.02-0.1.
Further, the preparation method of the sodium bismuth titanate nanoparticles used in the step 2) comprises the following steps:
s1, dispersing tetra-n-butyl titanate, bismuth nitrate pentahydrate and sodium hydroxide in deionized water, and stirring at room temperature to obtain a mixed solution;
s2, carrying out heat treatment on the mixed solution obtained in the step S1, heating to 160-200 ℃ at a heating rate of 3 +/-1 ℃/min, and carrying out heat preservation for 12-24 hours to obtain a reaction product;
s3, cleaning and centrifuging the reaction product obtained in the step S2, and collecting a precipitate;
s4, drying the precipitate obtained in the step S3 to obtain the sodium bismuth titanate nano-particles.
Of course, other methods can be adopted to prepare the sodium bismuth titanate nanoparticles, but the method disclosed by the invention is a one-step hydrothermal synthesis method, is simpler, and has the advantages of lower reaction temperature and higher yield.
Further, the step 1) is specifically as follows:
1.1) putting urea as a precursor into a covered crucible (the covering is used for providing a semi-closed environment, so that the gas in the crucible contains a part of volatilized precursor, thereby being capable of inhibiting the precursor at the bottom of the crucible from volatilizing rapidly. If the cover is not covered, all precursors are volatilized, and a product cannot be obtained after the precursor is cooled to the room temperature), heating to 520-550 ℃ at the heating rate of 5 +/-1 ℃/min in a muffle furnace, preserving the temperature for 2-4 h, and cooling to the room temperature to obtain a blocky product; compared with a slower heating rate (such as 2 ℃/min), the heating rate of 5 +/-1 ℃/min is selected to facilitate rapid heating to the polymerization temperature, and although the specific surface area of the obtained product is smaller than 2 ℃/min, more defects generated in the material due to a long-time heating process are avoided, and the defects can become recombination centers of photo-generated electron hole pairs, so that the utilization rate of carriers is reduced;
1.2) grinding the cake obtained in step 1.1) into a powder without granular sensation with an agate mortar to obtain a specific surface area of 50-100m2G of/g of3N4A photocatalyst. The physical grinding can crush the substance into smaller powder particles, and facilitates the preparation and characterization test of the subsequent heterojunction material. Here, the sense of no grain may vary from person to person, but has no effect on the result.
Further, the step 2) is specifically as follows:
mixing g-C with agate mortar3N4Mixing and grinding the photocatalyst and the sodium bismuth titanate nano particles until the photocatalyst and the sodium bismuth titanate nano particles are uniformly mixed, and basically grinding for 30min to achieve the effect of uniform mixing (uniform color and light yellow white), wherein the grinding method is simple, convenient, time-saving and efficient, and can be used for preparing large-scale composite heterojunctions; placing the materials in a covered crucible (the covering is carried out in order to avoid more contact with air so as to reduce the influence of oxidation of graphite phase carbon nitride by air), heating the materials to 380-420 ℃ in a muffle furnace at a heating rate of 5 +/-1 ℃/min, and keeping the temperature for 2-4 h, wherein the two materials can be in closer contact within the range of the calcining temperature and the heat-keeping time, if the temperature is too high, the surface oxidation and decomposition of the materials can be caused, and if the temperature is too low, the close contact cannot be formed; and cooling to room temperature, wherein the two materials generate a connection effect from the microstructure, so that an additional grinding process is not needed, and the sodium bismuth titanate/graphite phase carbon nitride heterojunction piezoelectric photocatalyst is obtained.
Further, the preparation method of the sodium bismuth titanate nanoparticles used in the step 2) specifically comprises the following steps:
s1, dispersing tetra-n-butyl titanate, bismuth nitrate pentahydrate and sodium hydroxide in deionized water, and stirring at room temperature for 2 hours to obtain a mixed solution;
s2, pouring the mixed solution obtained in the step S1 into a Teflon lining, putting the Teflon lining into a matched stainless steel outer lining, integrally putting the Teflon lining into a shaft furnace, heating to 160-200 ℃ at a heating rate of 3 +/-1 ℃/min, and preserving heat for 12-24 hours to obtain a reaction product; the slow heating rate and the longer heat preservation time are beneficial to the sufficient nucleation growth of the sodium bismuth titanate nano particles, and the hydrothermal method for preparing the material has the advantages of low temperature, energy conservation, special spherical shape and good product crystallinity; if a high-temperature calcination method is adopted, high temperature close to 1000 ℃ is required, so that high energy consumption is caused, the material appearance is not uniform, and the internal defects are more, so that low crystallinity is caused;
s3, washing the reaction product obtained in the step S2 with deionized water and absolute ethyl alcohol for 3 times respectively, centrifuging for 5min at the rotating speed of 10000r/min, and collecting precipitates; the purpose of cleaning is to remove unreacted water-soluble precursors and impurities so as to ensure the purity of the product, and the solid-liquid separation is realized in the centrifugal process;
s4, drying the precipitate obtained in the step S3 in an oven at 80 +/-5 ℃ for 12 hours to obtain the sodium bismuth titanate nanoparticles.
Further, in S1, the mass ratio of tetra-n-butyl titanate, bismuth nitrate pentahydrate, sodium hydroxide and deionized water is 5.6: 3.88: 14.4: 80.
Meanwhile, the invention also provides a sodium bismuth titanate/graphite phase carbon nitride heterojunction piezoelectric photocatalyst, which is characterized in that: is obtained by the preparation method.
Further, response to visible light in the range of 450-500 nm.
The invention provides a sodium bismuth titanate/graphite phase carbon nitride heterojunction piezoelectric photocatalyst and a preparation method thereof for the first time; meanwhile, the piezoelectric catalytic property and the photocatalytic property of the material are considered, and the influence of visible light irradiation and external pressure conditions on the catalytic property is further researched. The method adopts urea as a precursor, and g-C is prepared by a simple one-step thermal polymerization method3N4Has a large specific surface area and thus can make more contact with other materials. Synthesizing NBT nano-particles by a one-step hydrothermal process, and then synthesizing the NBT nano-particles by a simple processGrinding, mixing and calcining to obtain NBT/g-C3N4A heterojunction piezoelectric photocatalyst. Simple grinding can enable the two materials to be fully and uniformly mixed without long-time stirring under the liquid phase condition, and the subsequent low-temperature calcination process can enable a compact interface to be formed between the two materials, so that the respective advantages of the two materials can be combined, the transmission of photon-generated carriers is promoted, and the catalytic performance is finally improved. Compared with the prior art, the invention has the following beneficial effects:
1. the preparation method of the heterojunction formed by compounding the two materials is very simple and only needs solid-phase grinding and calcination. In the preparation of g-C3N4The urea is used as a precursor of the photocatalyst, the source of raw materials is wide, the preparation cost is low, and meanwhile, as the urea generates gas in the reaction process, a porous structure can be formed, the specific surface area of the product can be improved, and the product obtained by polymerization can have more catalytic active sites and excellent photocatalytic performance; the synthesis process of NBT is also a one-step hydrothermal method, and three economical and cheap precursors are selected; therefore, the cost of product preparation is lower.
2. In the bismuth sodium titanate/graphite phase carbon nitride heterojunction piezoelectric photocatalyst prepared by the invention, g-C3N4The photo-generated carrier can be generated by absorbing part of visible light, the surface of the piezoelectric material NBT generates charges due to external pressure in the stirring process, and meanwhile, the piezoelectric polarization forms a built-in electric field at the interface of the two materials to drive photo-generated electrons and holes to move in opposite directions.
3. The invention controls NBT and g-C3N4The proportion of the components can obtain the piezoelectric photocatalyst with different photocatalytic performances, and can be used for organic dye degradation and hydrogen production (namely obtaining the piezoelectric photocatalyst with different photocatalytic performances for organic light degradation and hydrogen production); NBT was compared to g-C for the first time with some of the disclosed piezo-catalytic and heterojunction materials3N4The heterojunction is formed by combination for piezoelectric photocatalytic reaction, fills the blank of the two materials in the field of piezoelectric photocatalysis, provides insight for the preparation of other piezoelectric photocatalytic composite materials, and has the advantages of both academic research and practical applicationHas great significance.
4. The vibration caused by the external stirring condition has the promotion effect on the photocatalytic degradation of the dye and the photocatalytic hydrogen production of the composite catalyst prepared by the invention, the rhodamine B solution (with the concentration of 5mg/L) can be completely degraded in simulated sunlight within 70min, and the material has faster charge transmission, and has very wide application prospect.
Drawings
FIG. 1 shows NBT/g-C prepared in the first embodiment of the present invention3N4Scanning electron microscope pictures of heterojunction piezoelectric photocatalysts.
FIG. 2 shows NBT/g-C prepared in the first embodiment of the present invention3N4Ultraviolet-visible absorption spectrum curve of the heterojunction piezoelectric photocatalyst.
FIG. 3 shows NBT/g-C prepared according to example one of the present invention3N4And (3) measuring electrochemical impedance curves of the heterojunction piezoelectric photocatalyst under the conditions of no external stirring and stirring at the rotating speed of 1000 r/min.
FIG. 4 shows NBT/g-C prepared according to example one of the present invention3N4The heterojunction piezoelectric photocatalyst respectively degrades a 50ml photocatalytic activity curve with 5mg/L rhodamine B concentration under the conditions of no external stirring and stirring at the rotating speed of 1000r/min under the irradiation of visible light.
FIG. 5 shows NBT/g-C prepared according to example one of the present invention3N4And (3) comparing hydrogen production with time of the heterojunction piezoelectric photocatalyst under the conditions of no external stirring and stirring at the rotating speed of 1000r/min under the irradiation of visible light.
Detailed Description
The invention is described in further detail below with reference to the following figures and specific examples:
example 1
A preparation method of a sodium bismuth titanate/graphite phase carbon nitride heterojunction piezoelectric photocatalyst comprises the following steps:
5.6ml of tetra-n-butyl titanate, 3.88g of bismuth nitrate pentahydrate and 14.4g of sodium hydroxide were dispersed in 80ml of deionized water, and stirred at room temperature for 2 hours to obtain a mixed solution. 60ml of the obtained mixed solution is measured by using a measuring cylinder, poured into 100ml of Teflon lining, put into a matched stainless steel outer lining, integrally placed in a shaft furnace, heated to 160 ℃ at a uniform heating rate of 3 ℃/min and kept at the temperature for 24 hours. And pouring the finally obtained solution and the precipitate into a centrifugal tube, washing for 3 times by using deionized water and absolute ethyl alcohol respectively, centrifuging for 5min at the rotating speed of 10000r/min, pouring out unreacted precursor solution, and drying the precipitate in an oven at the temperature of 80 ℃ for 12h to obtain the NBT nano-particles.
10g of urea as precursor was placed in a covered crucible, heated to 520 ℃ in a muffle furnace at a uniform heating rate of 5 ℃/min and held at this temperature for 4 h. Cooling to room temperature, grinding the block product with agate mortar to obtain powder without granular feeling3N4A photocatalyst.
Taking 200mg g-C3N4Putting the photocatalyst and 4mg of NBT nano-particles into an agate mortar for fully grinding for 30min, then putting the mixture into a crucible, heating the mixture to 380 ℃ in a muffle furnace at a uniform heating rate of 5 ℃/min, preserving the heat for 4h at the temperature, cooling the mixture to room temperature, and collecting the powder, namely NBT/g-C3N4A heterojunction piezoelectric photocatalyst.
FIG. 1 shows NBT/g-C prepared according to the present invention3N4Scanning electron microscope pictures of heterojunction piezoelectric photocatalysts. It can be shown that simple attrition mixing allows for contact between the two materials, which can be more intimate during the subsequent low temperature calcination at 380 ℃. In which the black dotted circles come out NBT nanoparticles of a size of a few microns, and g-C3N4The morphology of the sheet is smaller, and the successful combination of the two materials to form a heterojunction is proved.
In FIG. 3, curves 2 and 3 are NBT/g-C prepared according to the present invention3N4And (3) measuring electrochemical impedance curves of the heterojunction piezoelectric photocatalyst under the conditions of no external stirring and stirring at the rotating speed of 1000 r/min. After external stirring conditions are added, the material is equivalently pressurized, so that extra photo-generated electron hole pairs can be generated on the NBT surface, a built-in electric field is formed at the interface of the two materials due to the piezoelectric property, the photo-generated electrons and holes can move along opposite directions, and therefore effective separation of photo-generated carriers is achieved, and the semi-circle with impedance after stirring is smaller in the drawing.
In FIG. 4, curves 4 and 5 are NBT/g-C prepared according to the present invention3N4The heterojunction piezoelectric photocatalyst respectively degrades a 50ml photocatalytic activity curve with 5mg/L rhodamine B concentration under the conditions of no external stirring and stirring at the rotating speed of 1000r/min under the irradiation of visible light. It can be seen that the degradation rate of the catalyst is obviously improved after the stirring condition is added, and the dye can be degraded into colorless in 70min, because more photon-generated carriers are generated to participate in the reaction. It took 130min to degrade the dye to colorless without stirring.
In FIG. 5, curves 6 and 7 are NBT/g-C prepared according to the present invention3N4And (3) respectively carrying out hydrogen production quantity curve with time under the conditions of no external stirring and stirring at the rotating speed of 1000r/min under the irradiation of visible light by the heterojunction piezoelectric photocatalyst. It can be seen that the hydrogen production rate of the catalyst is improved after the stirring condition is added, and the vibration generated by stirring promotes the NBT material to generate more photon-generated carriers to participate in the reaction.
Example 2:
a preparation method of a sodium bismuth titanate/graphite phase carbon nitride heterojunction piezoelectric photocatalyst comprises the following steps:
5.6ml of tetra-n-butyl titanate, 3.88g of bismuth nitrate pentahydrate and 14.4g of sodium hydroxide were dispersed in 80ml of deionized water, and stirred at room temperature for 2 hours to obtain a mixed solution. 60ml of the obtained mixed solution is measured by using a measuring cylinder, poured into 100ml of Teflon lining, put into a matched stainless steel outer lining, integrally placed in a shaft furnace, heated to 180 ℃ at a uniform heating rate of 3 ℃/min and kept at the temperature for 18 h. And pouring the finally obtained solution and the precipitate into a centrifugal tube, washing for 3 times by using deionized water and absolute ethyl alcohol respectively, centrifuging for 5min at the rotating speed of 10000r/min, pouring out unreacted precursor solution, and drying the precipitate in an oven at the temperature of 80 ℃ for 12h to obtain the NBT nano-particles.
10g of urea as precursor was placed in a covered crucible, heated to 535 ℃ in a muffle furnace at a uniform heating rate of 5 ℃/min and held at this temperature for 3 h. Cooling to room temperature, grinding the block product with agate mortar to obtain powder without granular feeling3N4A photocatalyst.
taking 200mg g-C3N4Putting the photocatalyst and 12mg of NBT nano-particles into an agate mortar for fully grinding for 30min, then putting the mixture into a crucible, heating the mixture to 400 ℃ in a muffle furnace at a uniform heating rate of 5 ℃/min, preserving the heat for 3h at the temperature, cooling the mixture to room temperature, and collecting powder, namely NBT/g-C3N4A heterojunction piezoelectric photocatalyst.
Example 3:
a preparation method of a sodium bismuth titanate/graphite phase carbon nitride heterojunction piezoelectric photocatalyst comprises the following steps:
5.6ml of tetra-n-butyl titanate, 3.88g of bismuth nitrate pentahydrate and 14.4g of sodium hydroxide were dispersed in 80ml of deionized water, and stirred at room temperature for 2 hours to obtain a mixed solution. 60ml of the obtained mixed solution is measured by using a measuring cylinder, poured into 100ml of Teflon lining, put into a matched stainless steel outer lining, integrally placed in a shaft furnace, heated to 200 ℃ at a uniform heating rate of 3 ℃/min and kept at the temperature for 12 h. And pouring the finally obtained solution and the precipitate into a centrifugal tube, washing for 3 times by using deionized water and absolute ethyl alcohol respectively, centrifuging for 5min at the rotating speed of 10000r/min, pouring out unreacted precursor solution, and drying the precipitate in an oven at the temperature of 80 ℃ for 12h to obtain the NBT nano-particles.
10g of urea as precursor was placed in a covered crucible, heated to 550 ℃ in a muffle furnace at a uniform heating rate of 5 ℃/min and held at this temperature for 2 h. Cooling to room temperature, grinding the block product with agate mortar to obtain powder without granular feeling3N4A photocatalyst.
taking 200mg g-C3N4Putting the photocatalyst and 20mg of NBT nano-particles into an agate mortar for fully grinding for 30min, then putting the mixture into a crucible, heating the mixture to 420 ℃ in a muffle furnace at a uniform heating rate of 5 ℃/min, preserving the heat at the temperature for 2h, cooling the mixture to room temperature, and collecting powder, namely NBT/g-C3N4A heterojunction piezoelectric photocatalyst.
Example 4:
a preparation method of a sodium bismuth titanate/graphite phase carbon nitride heterojunction piezoelectric photocatalyst comprises the following steps:
5.6ml of tetra-n-butyl titanate, 3.88g of bismuth nitrate pentahydrate and 14.4g of sodium hydroxide were dispersed in 80ml of deionized water, and stirred at room temperature for 2 hours to obtain a mixed solution. 60ml of the obtained mixed solution is measured by using a measuring cylinder, poured into 100ml of Teflon lining, put into a matched stainless steel outer lining, integrally placed in a shaft furnace, heated to 190 ℃ at a uniform heating rate of 2 ℃/min and kept at the temperature for 22 h. And pouring the finally obtained solution and the precipitate into a centrifugal tube, washing for 3 times by using deionized water and absolute ethyl alcohol respectively, centrifuging for 4min at the rotating speed of 10000r/min, pouring out unreacted precursor solution, and drying the precipitate in an oven at 85 ℃ for 10h to obtain the NBT nano-particles.
10g of urea as precursor was placed in a covered crucible, heated to 540 ℃ in a muffle furnace at a uniform heating rate of 4 ℃/min and held at this temperature for 3 h. Cooling to room temperature, grinding the block product with agate mortar to obtain powder without granular feeling3N4A photocatalyst.
taking 200mg g-C3N4Putting the photocatalyst and 20mg of NBT nano-particles into an agate mortar for fully grinding for 30min, then putting the mixture into a crucible, heating the mixture to 400 ℃ in a muffle furnace at a uniform heating rate of 6 ℃/min, preserving the heat for 3h at the temperature, cooling the mixture to room temperature, and collecting powder, namely NBT/g-C3N4A heterojunction piezoelectric photocatalyst.
Example 5:
a preparation method of a sodium bismuth titanate/graphite phase carbon nitride heterojunction piezoelectric photocatalyst comprises the following steps:
5.6ml of tetra-n-butyl titanate, 3.88g of bismuth nitrate pentahydrate and 14.4g of sodium hydroxide were dispersed in 80ml of deionized water, and stirred at room temperature for 2 hours to obtain a mixed solution. 60ml of the obtained mixed solution is measured by using a measuring cylinder, poured into 100ml of Teflon lining, put into a matched stainless steel outer lining, integrally placed in a shaft furnace, heated to 170 ℃ at a uniform heating rate of 4 ℃/min and kept at the temperature for 20 hours. And pouring the finally obtained solution and the precipitate into a centrifugal tube, washing for 3 times by using deionized water and absolute ethyl alcohol respectively, centrifuging for 6min at the rotating speed of 10000r/min, pouring out unreacted precursor solution, and drying the precipitate in an oven at 75 ℃ for 14h to obtain the NBT nano-particles.
10g of urea as precursor was placed in a covered crucible, heated to 530 ℃ in a muffle furnace at a uniform heating rate of 6 ℃/min and held at this temperature for 4 h. Cooling to room temperature, grinding the block product with agate mortar to obtain powder without granular feeling3N4A photocatalyst.
taking 200mg g-C3N4Putting the photocatalyst and 20mg of NBT nano-particles into an agate mortar for fully grinding for 30min, then putting the mixture into a crucible, heating the mixture to 390 ℃ in a muffle furnace at a uniform heating rate of 4 ℃/min, preserving the heat for 4h at the temperature, cooling the mixture to room temperature, and collecting powder, namely NBT/g-C3N4A heterojunction piezoelectric photocatalyst.
While the invention has been described with reference to specific embodiments, the invention is not limited thereto, and various equivalent modifications or substitutions can be easily made by those skilled in the art within the technical scope of the present disclosure.
Claims (9)
1. A preparation method of a sodium bismuth titanate/graphite phase carbon nitride heterojunction piezoelectric photocatalyst is characterized by comprising the following steps:
1) synthesis of g-C3N4Photocatalyst and process for producing the same
1.1) taking urea as a precursor, heating to 520-550 ℃ at a heating rate of 5 +/-1 ℃/min, preserving heat for 2-4 h, and cooling to room temperature to obtain a blocky product;
1.2) grinding the lumpy product obtained in step 1.1) into a powder, resulting in a specific surface area of 50-100m2G of/g of3N4A photocatalyst;
2) preparation of sodium bismuth titanate/graphite phase carbon nitride heterojunction piezoelectric photocatalyst
g-C obtained in step 1)3N4Uniformly mixing the photocatalyst and the sodium bismuth titanate nanoparticles, heating to 380-420 ℃ at a heating rate of 5 +/-1 ℃/min, preserving heat for 2-4 h, and cooling to room temperature to obtain the sodium bismuth titanate/graphite phase carbon nitride heterojunction piezoelectric photocatalyst.
2. The production method according to claim 1,
in step 2), the g-C3N4The mass ratio of the photocatalyst to the sodium bismuth titanate nano particles is 1: 0.02-0.1.
3. The method of claim 2, wherein:
the preparation method of the sodium bismuth titanate nano-particles used in the step 2) comprises the following steps:
s1, dispersing tetra-n-butyl titanate, bismuth nitrate pentahydrate and sodium hydroxide in deionized water, and stirring at room temperature to obtain a mixed solution;
s2, carrying out heat treatment on the mixed solution obtained in the step S1, heating to 160-200 ℃ at a heating rate of 3 +/-1 ℃/min, and carrying out heat preservation for 12-24 hours to obtain a reaction product;
s3, cleaning and centrifuging the reaction product obtained in the step S2, and collecting a precipitate;
s4, drying the precipitate obtained in the step S3 to obtain the sodium bismuth titanate nano-particles.
4. The preparation method according to any one of claims 1 to 3, wherein the step 1) is specifically:
1.1) putting urea serving as a precursor into a covered crucible, heating to 520-550 ℃ in a muffle furnace at a heating rate of 5 +/-1 ℃/min, preserving heat for 2-4 h, and cooling to room temperature to obtain a blocky product;
1.2) grinding the cake obtained in step 1.1) into a powder without granular sensation with a mortar to obtain a specific surface area of 50-100m2G of/g of3N4A photocatalyst.
5. The preparation method according to claim 4, wherein the step 2) is specifically:
mixing g-C with mortar3N4Uniformly mixing the photocatalyst and the sodium bismuth titanate nanoparticles, placing the mixture in a covered crucible, heating the mixture to 380-420 ℃ in a muffle furnace at a heating rate of 5 +/-1 ℃/min, preserving the temperature for 2-4 h, and cooling the mixture to room temperature to obtain the sodium bismuth titanate/graphite phase carbon nitride heterojunction piezoelectric photocatalyst.
6. The method according to claim 3, wherein:
the preparation method of the sodium bismuth titanate nano-particles used in the step 2) comprises the following steps:
s1, dispersing tetra-n-butyl titanate, bismuth nitrate pentahydrate and sodium hydroxide in deionized water, and stirring at room temperature for 2 hours to obtain a mixed solution;
s2, pouring the mixed solution obtained in the step S1 into a Teflon lining, putting the Teflon lining into a matched stainless steel outer lining, integrally putting the Teflon lining into a well type furnace, heating to 160-200 ℃ at a heating rate of 3 +/-1 ℃/min, and preserving heat for 12-24 hours to obtain a reaction product;
s3, washing the reaction product obtained in the step S2 with deionized water and absolute ethyl alcohol for 3 times respectively, centrifuging for 5 +/-1 min at the rotating speed of 10000r/min, and collecting precipitates;
s4, placing the precipitate obtained in the step S3 in an oven to be dried for 12 +/-2 hours at the temperature of 80 +/-5 ℃ to obtain the sodium bismuth titanate nano-particles.
7. The method according to claim 6, wherein:
in S1, the mass ratio of tetrabutyl titanate, bismuth nitrate pentahydrate, sodium hydroxide and deionized water is 5.6: 3.88: 14.4: 80.
8. A sodium bismuth titanate/graphite phase carbon nitride heterojunction piezoelectric photocatalyst is characterized in that: obtained by the preparation method of any one of claims 1 to 7.
9. The sodium bismuth titanate/graphite phase carbon nitride heterojunction piezoelectric photocatalyst of claim 8, wherein: response to visible light in the range of 450-500 nm.
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