CN111151278A - A kind of preparation method of carbon dot composite bismuth oxycarbonate visible light catalyst - Google Patents
A kind of preparation method of carbon dot composite bismuth oxycarbonate visible light catalyst Download PDFInfo
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- 229910000014 Bismuth subcarbonate Inorganic materials 0.000 title claims abstract description 53
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 40
- 239000002131 composite material Substances 0.000 title claims abstract description 34
- FWIZHMQARNODNX-UHFFFAOYSA-L dibismuth;oxygen(2-);carbonate Chemical compound [O-2].[O-2].[Bi+3].[Bi+3].[O-]C([O-])=O FWIZHMQARNODNX-UHFFFAOYSA-L 0.000 title claims abstract description 26
- 239000003054 catalyst Substances 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000011941 photocatalyst Substances 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 8
- JBANFLSTOJPTFW-UHFFFAOYSA-N azane;boron Chemical compound [B].N JBANFLSTOJPTFW-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 5
- 239000012279 sodium borohydride Substances 0.000 claims abstract description 5
- 239000000725 suspension Substances 0.000 claims description 45
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 24
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 24
- 239000002245 particle Substances 0.000 claims description 23
- 239000007787 solid Substances 0.000 claims description 20
- 239000000243 solution Substances 0.000 claims description 20
- 230000005291 magnetic effect Effects 0.000 claims description 19
- 239000000843 powder Substances 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 235000019253 formic acid Nutrition 0.000 claims description 12
- 229910052797 bismuth Inorganic materials 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 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 4
- 239000011294 coal tar pitch Substances 0.000 claims description 4
- 239000006228 supernatant Substances 0.000 claims description 4
- 238000006555 catalytic reaction Methods 0.000 abstract description 8
- 230000000593 degrading effect Effects 0.000 abstract description 7
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract description 5
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 5
- 230000027756 respiratory electron transport chain Effects 0.000 abstract description 5
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 2
- 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 12
- 229940043267 rhodamine b Drugs 0.000 description 12
- 238000012360 testing method Methods 0.000 description 8
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 238000000804 electron spin resonance spectroscopy Methods 0.000 description 6
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 5
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 5
- 229940012189 methyl orange Drugs 0.000 description 5
- 229960000907 methylthioninium chloride Drugs 0.000 description 5
- 230000001699 photocatalysis Effects 0.000 description 5
- 229940036358 bismuth subcarbonate Drugs 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- OUUQCZGPVNCOIJ-UHFFFAOYSA-M Superoxide Chemical compound [O-][O] OUUQCZGPVNCOIJ-UHFFFAOYSA-M 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- TUJKJAMUKRIRHC-UHFFFAOYSA-N hydroxyl Chemical compound [OH] TUJKJAMUKRIRHC-UHFFFAOYSA-N 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011300 coal pitch Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 231100000701 toxic element Toxicity 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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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
- B01J27/20—Carbon compounds
- B01J27/232—Carbonates
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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Abstract
为提高催化反应过程中的电子转移能力，进而提高可见光催化剂降解有机污染物的性能，本发明公开了一种室温环境下制备碳点复合碳酸氧铋可见光催化剂的方法，采用碳点、硝酸铋、硼氢化钠或氨硼烷通过6个步骤合成碳点复合碳酸氧铋可见光催化剂。采用本专利公开的碳点复合碳酸氧铋可见光催化剂制备方法制备的碳点复合碳酸氧铋可见光催化剂有强的可见光催化性能，且具有可以在常温下反应，制备工艺简单，有利于大规模工业化生产等优点。
In order to improve the electron transfer ability in the catalytic reaction process and further improve the performance of visible light catalyst for degrading organic pollutants, the invention discloses a method for preparing carbon dot composite bismuth oxycarbonate visible light catalyst under room temperature environment. Sodium borohydride or ammonia borane was used to synthesize carbon dots composite bismuth oxycarbonate visible photocatalyst in six steps. The carbon dot composite bismuth oxycarbonate visible light catalyst prepared by the carbon dot composite bismuth oxycarbonate visible light catalyst preparation method disclosed in this patent has strong visible light catalytic performance, and can react at room temperature, the preparation process is simple, and it is conducive to large-scale industrial production Etc.
Description
Technical Field
The invention belongs to the field of nano composite materials, and particularly relates to a preparation method of a carbon dot composite bismuthyl carbonate visible-light-driven photocatalyst.
Background
Nowadays, the environmental pollution problem is more and more serious, and the human health is seriously threatened, so that the environmental pollution problem becomes the first problem to be solved at home and abroad. Solar energy is a clean and renewable natural resource, organic pollutants can be degraded into micromolecular water, carbon dioxide and the like by using a photocatalyst, and the application prospect is good. Bismuth (Bi) -based photocatalysts have been developed, the oxides of bismuth having (BiO)2 2+The layered structure can be self-assembled to form different shapes, and effectively degrade organic pollutants in the wastewater. Bismuth oxycarbonate ((BiO)2CO3) Is a photocatalyst only responding to ultraviolet light, does not contain toxic elements such as halogen and the like, (BiO)2 2+Layer and CO3 2-The layers are alternately stacked in the C-axis direction to form a layered structure. However, the regular layered structure provides bismuth oxycarbonate with a small specific surface area, which greatly limits its photocatalytic performance, and at the same time, its performance is also affected by the limited electron transfer capacity and photoinduced redox capacity. Therefore, bismuth subcarbonate is compounded with a plurality of suitable semiconductor photocatalysts, the morphology of the bismuth subcarbonate is controlled to increase the specific surface area of the photocatalyst to create more catalytic reaction active sites, and a heterojunction is formed to improve the electron transfer capacity in the catalytic reaction process, so that the performance of the visible light photocatalyst for degrading organic pollutants is improved, and the bismuth subcarbonate is an important and urgent problem to be solved.
The Carbon Dots (CDs) are used as a zero-dimensional carbon-based material with wide source, simple preparation and environmental friendliness, and have a wider photoresponse range, stronger electron transfer capability and better photoinduced redox capability. Thus, the coal pitch carbon dots react with bismuth oxycarbonate in situ to form carbon dots and bismuth oxycarbonate heterostructures (CDs @ (BiO)2CO3)，The specific surface area of the catalyst can be increased, more catalytic reaction active sites are created, and the heterojunction is formed, so that the electron transfer capability and the photoinduced redox capability in the catalytic reaction process can be improved, and the catalytic performance of the visible-light-driven photocatalyst for degrading organic pollutants is improved. At present, the performance of the visible-light-driven photocatalyst is improved by utilizing the above mode, and particularly, the carbon-point composite bismuth oxycarbonate visible-light-driven photocatalyst (CDs @ (BiO) is prepared under the room temperature environment2CO3) The method (2) has not been reported.
Disclosure of Invention
The invention aims to provide a method for preparing a carbon-point composite bismuthyl carbonate visible-light-driven photocatalyst at room temperature so as to improve the visible-light-driven catalytic performance of the catalyst.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a carbon-point composite bismuthyl carbonate visible light photocatalyst adopts the following steps:
step 1: preparing a mL of 88% formic acid and b mL of 30% hydrogen peroxide into a mixed solution of the formic acid and the hydrogen peroxide, wherein: b is 9.5-10.5, c mL of mixed solution of formic acid and hydrogen peroxide is poured into a beaker, d mg of coal tar pitch powder is added into the beaker, and suspension is prepared, wherein: d, putting the suspension on a magnetic stirrer, stirring at normal temperature for 18-20 hours, putting the suspension into a centrifugal machine, centrifuging to remove large particles, and taking supernatant to obtain carbon dot solution, wherein c is 5.5-6.5 mg/mL;
step 2: taking e mL of the carbon dot solution prepared in the step 1, adding f mg of pentahydrate bismuth nitrate powder, and preparing the carbon dot-bismuth nitrate solution, wherein: e is 12.5-17.5 mg/mL, then the carbon dot-bismuth nitrate solution is placed on a magnetic stirrer, and is stirred and reacted for 10-12 hours at normal temperature at the rotating speed of 600-800 r/min to obtain a suspension A;
and step 3: placing the suspension A prepared in the step 2 into a centrifuge, centrifuging for 20-30 min at the rotating speed of 8000-10000 r/min, taking solid particles, washing with deionized water for 3-5 times, then placing the solid particles into a vacuum drying oven, and drying at the temperature of 40-50 ℃ to obtain carbon dot-bismuth oxyformate composite powder;
and 4, step 4: and (3) adding g mg of the carbon dot-bismuth oxyformate composite powder prepared in the step (3) into a beaker, pouring h mL of deionized water into the beaker, and preparing a suspension B, wherein: g, h is 25-35 mg/mL, then the suspension B is placed on a magnetic stirrer, and the suspension B is stirred at the normal temperature for 30-40 min at the rotating speed of 600-800 r/min;
and 5: putting i mL of the stirred suspension B prepared in the step 4 on a magnetic stirrer, and adding j mL of sodium borohydride or ammonia borane solution with the concentration of 0.5-1.5 g/L into the magnetic stirrer at the rotating speed of 600-800 r/min, wherein: j is 4.5-7.5, and stirring and reacting for 30-40 min at normal temperature to obtain suspension C;
step 6: and (5) centrifuging the suspension C prepared in the step (5) in a centrifuge at the rotating speed of 8000-10000 r/min for 20-30 min, taking solid particles, washing the solid particles with deionized water for 3-5 times, then putting the solid particles into a vacuum drying oven, and drying at the temperature of 40-50 ℃ to finally obtain the carbon-point composite bismuth oxycarbonate visible light catalyst.
Compared with the prior art, the invention has the advantages of reaction at normal temperature, simple preparation process, contribution to large-scale industrial production and the like; the carbon-point composite bismuthyl carbonate visible-light-induced photocatalyst prepared by the invention has strong visible-light-induced catalytic performance.
Drawings
FIG. 1 is a process flow diagram for preparing a carbon-point composite bismuth oxycarbonate visible-light-induced photocatalyst;
FIG. 2 shows a carbon dot composite bismuthyl carbonate visible-light-induced photocatalyst sample and (BiO)2CO3XRD pattern of standard card;
FIG. 3 is a UV-VISIBLE absorption spectrum of a sample of carbon dot bismuth oxycarbonate visible light photocatalyst;
FIG. 4 is a graph showing pore volume and pore size distribution of a carbon dot composite bismuth oxycarbonate visible light photocatalyst sample;
FIG. 5 is a graph showing the effect of visible light-catalyzed degradation of rhodamine B (RhB) by a carbon dot composite bismuthyl carbonate visible light-catalyzed photocatalyst sample;
FIG. 6 is a graph showing the effect of visible-light photocatalytic degradation of Methylene Blue (MB) for a carbon-point composite bismuthyl carbonate visible-light photocatalyst sample;
FIG. 7 is CDs @ (BiO)2CO3A graph of the effect of photocatalytic degradation of Methyl Orange (MO) on a sample;
FIG. 8 is a graph showing the results of an electron paramagnetic resonance spectroscopy (ESR) test of whether a sample of carbon-point bismuth oxycarbonate photocatalyst produced hydroxyl radical actives;
FIG. 9 shows the results of ESR testing whether a sample of carbon point bismuth subcarbonate visible photocatalyst produces superoxide radical actives;
FIG. 10 shows the photocurrent test results of carbon dot composite bismuth oxycarbonate visible light catalyst samples;
FIG. 11 is a repeatability test of photocatalytic degradation of RhB by a carbon dot composite bismuth oxycarbonate visible-light-induced photocatalyst sample;
FIG. 12 is a graph showing the effect of photocatalytic degradation of RhB by a carbon dot composite bismuth oxycarbonate visible-light-induced photocatalyst sample under different light intensities.
Detailed Description
The detailed technical scheme of the invention is described in the following with the accompanying drawings:
a preparation method of a carbon-point composite bismuthyl carbonate visible light photocatalyst adopts the following steps:
step 1: preparing a mL of 88% formic acid and b mL of 30% hydrogen peroxide into a mixed solution of the formic acid and the hydrogen peroxide, wherein: b is 9.5-10.5, c mL of mixed solution of formic acid and hydrogen peroxide is poured into a beaker, d mg of coal tar pitch powder is added into the beaker, and suspension is prepared, wherein: d, putting the suspension on a magnetic stirrer, stirring at normal temperature for 18-20 hours, putting the suspension into a centrifugal machine, centrifuging to remove large particles, and taking supernatant to obtain carbon dot solution, wherein c is 5.5-6.5 mg/mL;
step 2: taking e mL of the carbon dot solution prepared in the step 1, adding f mg of pentahydrate bismuth nitrate powder, and preparing the carbon dot-bismuth nitrate solution, wherein: e is 12.5-17.5 mg/mL, then the carbon dot-bismuth nitrate solution is placed on a magnetic stirrer, and is stirred and reacted for 10-12 hours at normal temperature at the rotating speed of 600-800 r/min to obtain a suspension A;
and step 3: placing the suspension A prepared in the step 2 into a centrifuge, centrifuging for 20-30 min at the rotating speed of 8000-10000 r/min, taking solid particles, washing with deionized water for 3-5 times, then placing the solid particles into a vacuum drying oven, and drying at the temperature of 40-50 ℃ to obtain carbon dot-bismuth oxyformate composite powder;
and 4, step 4: and (3) adding g mg of the carbon dot-bismuth oxyformate composite powder prepared in the step (3) into a beaker, pouring h mL of deionized water into the beaker, and preparing a suspension B, wherein: g, h is 25-35 mg/mL, then the suspension B is placed on a magnetic stirrer, and the suspension B is stirred at the normal temperature for 30-40 min at the rotating speed of 600-800 r/min;
and 5: putting i mL of the stirred suspension B prepared in the step 4 on a magnetic stirrer, and adding j mL of sodium borohydride or ammonia borane solution with the concentration of 0.5-1.5 g/L into the magnetic stirrer at the rotating speed of 600-800 r/min, wherein: j is 4.5-7.5, and stirring and reacting for 30-40 min at normal temperature to obtain suspension C;
step 6: and (5) centrifuging the suspension C prepared in the step (5) in a centrifuge at the rotating speed of 8000-10000 r/min for 20-30 min, taking solid particles, washing the solid particles with deionized water for 3-5 times, then putting the solid particles into a vacuum drying oven, and drying at the temperature of 40-50 ℃ to finally obtain the carbon-point composite bismuth oxycarbonate visible light catalyst.
Example 1
A preparation method of a carbon dot composite bismuthyl carbonate visible light photocatalyst is shown in figure 1 and comprises the following steps:
step 1: preparing a mL of 88% formic acid and b mL of 30% hydrogen peroxide into a mixed solution of the formic acid and the hydrogen peroxide, wherein: b is 10, c mL of mixed solution of formic acid and hydrogen peroxide is poured into a beaker, d mg of coal tar pitch powder is added into the beaker, and suspension is prepared, wherein: d, putting the suspension on a magnetic stirrer, stirring at normal temperature for 19 hours, putting the suspension into a centrifuge, centrifuging to remove large particles, and taking supernatant to obtain carbon dot solution;
step 2: taking e mL of the carbon dot solution prepared in the step 1, adding f mg of pentahydrate bismuth nitrate powder, and preparing the carbon dot-bismuth nitrate solution, wherein: e is 15mg/mL, then the carbon dot-bismuth nitrate solution is placed on a magnetic stirrer, and is stirred and reacted for 11 hours at normal temperature at the rotating speed of 700r/min to obtain a suspension A;
and step 3: placing the suspension A prepared in the step 2 into a centrifuge, centrifuging for 25min at the rotating speed of 9000r/min, taking solid particles, washing for 5 times by using deionized water, then placing the solid particles into a vacuum drying oven, and drying at the temperature of 45 ℃ to obtain carbon dot-bismuth oxyformate composite powder;
and 4, step 4: and (3) adding g mg of the carbon dot-bismuth oxyformate composite powder prepared in the step (3) into a beaker, pouring h mL of deionized water into the beaker, and preparing a suspension B, wherein: g, h is 30mg/mL, then the suspension B is placed on a magnetic stirrer, and the suspension B is stirred for 40min at the normal temperature at the rotating speed of 700 r/min;
and 5: i mL of the stirred suspension B prepared in the step 4 is put on a magnetic stirrer, and j mL of sodium borohydride or ammonia borane solution with the concentration of 1g/L is added into the suspension B at the rotating speed of 700r/min, wherein: i, j is 6, stirring and reacting for 40min at normal temperature to obtain suspension C;
step 6: placing the suspension C prepared in step 5 into a centrifuge, centrifuging at 9000r/min for 25min, taking solid particles, washing with deionized water for 5 times, placing the solid particles into a vacuum drying oven, and drying at 50 deg.C to obtain carbon point composite bismuth oxycarbonate visible light catalyst (CDs @ (BiO)2CO3)。
FIG. 2 is CDs @ (BiO)2CO3Sample and (BiO)2CO3The XRD spectrum of the standard card shows that the carbon point and the bismuth oxycarbonate realize heterogeneous combination.
FIG. 3 is CDs @ (BiO)2CO3The uv-vis absorption spectrum of the solid sample shows that the sample has strong absorption over the entire visible range.
FIG. 4 is CDs @ (BiO)2CO3The pore volume and pore diameter distribution curve chart of the sample shows that the sample has abundant mesopores and micropores, which is beneficial to increasing reactive sites.
FIG. 5 is CDs @ (BiO)2CO3The sample degraded rhodamine B (RhB) under visible light catalysis, and the degradation is about 60 percent in 10 minutesThe sample has better capacity of degrading RhB by photocatalysis.
FIG. 6 is CDs @ (BiO)2CO3The sample can be degraded by visible light catalysis to Methylene Blue (MB), and the degradation is about 70% in 10 minutes, which shows that the sample has better photocatalytic MB degradation capability.
FIG. 7 is CDs @ (BiO)2CO3The sample degrades Methyl Orange (MO) in 10 minutes by about 75%, which shows that the sample has better capability of degrading MO by photocatalysis.
FIG. 8 is the electron paramagnetic resonance spectroscopy (ESR) test CDs @ (BiO)2CO3Whether the sample produced hydroxyl radical activity indicates that the sample produced hydroxyl radicals in aqueous solution only in the presence of light and not in the absence of light.
FIG. 9 is a test of ESR for CDs @ (BiO)2CO3Whether the sample produced superoxide radical actives indicates that superoxide radicals were generated in the sample in aqueous solution only when illuminated and not when not illuminated.
FIG. 10 is CDs @ (BiO)2CO3The photocurrent test of the sample shows that the photo-generated electron-hole pair can be well separated and can realize high-efficiency migration, which is beneficial to promoting surface catalytic reaction.
FIG. 11 is CDs @ (BiO)2CO3The repeatability test of the sample photocatalytic degradation RhB shows that the activity of the sample photocatalytic degradation RhB is not reduced after the sample photocatalytic degradation RhB is repeatedly used for four times under visible light, which indicates that the sample has high photocatalytic stability.
FIG. 12 is CDs @ (BiO) under different light intensities2CO3The sample photocatalytically degrades RhB, and it can be seen that the rate of photocatalytically degrading RhB of the sample is increased along with the increase of the illumination intensity, which shows that the performance of photocatalytically degrading organic matters can be improved by increasing the number of input photons.
Claims (1)
1. A preparation method of a carbon-point composite bismuthyl carbonate visible light photocatalyst is characterized by comprising the following steps: the method comprises the following steps:
step 1: preparing a mL of 88% formic acid and b mL of 30% hydrogen peroxide into a mixed solution of the formic acid and the hydrogen peroxide, wherein: b is 9.5-10.5, c mL of mixed solution of formic acid and hydrogen peroxide is poured into a beaker, d mg of coal tar pitch powder is added into the beaker, and suspension is prepared, wherein: d, putting the suspension on a magnetic stirrer, stirring at normal temperature for 18-20 hours, putting the suspension into a centrifugal machine, centrifuging to remove large particles, and taking supernatant to obtain carbon dot solution, wherein c is 5.5-6.5 mg/mL;
step 2: taking e mL of the carbon dot solution prepared in the step 1, adding f mg of pentahydrate bismuth nitrate powder, and preparing the carbon dot-bismuth nitrate solution, wherein: e is 12.5-17.5 mg/mL, then the carbon dot-bismuth nitrate solution is placed on a magnetic stirrer, and is stirred and reacted for 10-12 hours at normal temperature at the rotating speed of 600-800 r/min to obtain a suspension A;
and step 3: placing the suspension A prepared in the step 2 into a centrifuge, centrifuging for 20-30 min at the rotating speed of 8000-10000 r/min, taking solid particles, washing with deionized water for 3-5 times, then placing the solid particles into a vacuum drying oven, and drying at the temperature of 40-50 ℃ to obtain carbon dot-bismuth oxyformate composite powder;
and 4, step 4: and (3) adding g mg of the carbon dot-bismuth oxyformate composite powder prepared in the step (3) into a beaker, pouring h mL of deionized water into the beaker, and preparing a suspension B, wherein: g, h is 25-35 mg/mL, then the suspension B is placed on a magnetic stirrer, and the suspension B is stirred at the normal temperature for 30-40 min at the rotating speed of 600-800 r/min;
and 5: putting i mL of the stirred suspension B prepared in the step 4 on a magnetic stirrer, and adding j mL of sodium borohydride or ammonia borane solution with the concentration of 0.5-1.5 g/L into the magnetic stirrer at the rotating speed of 600-800 r/min, wherein: j is 4.5-7.5, and stirring and reacting for 30-40 min at normal temperature to obtain suspension C;
step 6: and (5) centrifuging the suspension C prepared in the step (5) in a centrifuge at the rotating speed of 8000-10000 r/min for 20-30 min, taking solid particles, washing the solid particles with deionized water for 3-5 times, then putting the solid particles into a vacuum drying oven, and drying at the temperature of 40-50 ℃ to finally obtain the carbon-point composite bismuth oxycarbonate visible light catalyst.
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