CN110465285A - A kind of BiVO4The preparation method and application of@carbon nano dot composite photocatalyst material - Google Patents
A kind of BiVO4The preparation method and application of@carbon nano dot composite photocatalyst material Download PDFInfo
- Publication number
- CN110465285A CN110465285A CN201910688738.4A CN201910688738A CN110465285A CN 110465285 A CN110465285 A CN 110465285A CN 201910688738 A CN201910688738 A CN 201910688738A CN 110465285 A CN110465285 A CN 110465285A
- Authority
- CN
- China
- Prior art keywords
- bivo
- preparation
- carbon nano
- nano dot
- composite material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 55
- 239000002096 quantum dot Substances 0.000 title claims abstract description 54
- 239000002131 composite material Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000000463 material Substances 0.000 title abstract description 40
- 239000011941 photocatalyst Substances 0.000 title abstract description 9
- 229910002915 BiVO4 Inorganic materials 0.000 claims abstract description 39
- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical class [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 45
- 239000011259 mixed solution Substances 0.000 claims description 28
- 239000000243 solution Substances 0.000 claims description 20
- 238000001354 calcination Methods 0.000 claims description 11
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims 1
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- MZSDGDXXBZSFTG-UHFFFAOYSA-M sodium;benzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=CC=C1 MZSDGDXXBZSFTG-UHFFFAOYSA-M 0.000 claims 1
- 230000015556 catabolic process Effects 0.000 abstract description 20
- 238000006731 degradation reaction Methods 0.000 abstract description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 11
- 239000012620 biological material Substances 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 5
- 238000011161 development Methods 0.000 abstract description 4
- 239000002351 wastewater Substances 0.000 abstract description 4
- 230000000593 degrading effect Effects 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 230000003115 biocidal effect Effects 0.000 abstract description 2
- 239000005447 environmental material Substances 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 238000010586 diagram Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 239000003054 catalyst Substances 0.000 description 6
- 230000003197 catalytic effect Effects 0.000 description 5
- 230000001699 photocatalysis Effects 0.000 description 5
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 4
- 229920005610 lignin Polymers 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000002023 wood Substances 0.000 description 4
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000008033 biological extinction Effects 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- UBDNTYUBJLXUNN-IFLJXUKPSA-N Oxytetracycline hydrochloride Chemical compound Cl.C1=CC=C2[C@](O)(C)[C@H]3[C@H](O)[C@H]4[C@H](N(C)C)C(O)=C(C(N)=O)C(=O)[C@@]4(O)C(O)=C3C(=O)C2=C1O UBDNTYUBJLXUNN-IFLJXUKPSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003738 black carbon Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000004020 conductor Substances 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
- 239000013078 crystal Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000006552 photochemical reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 229940126680 traditional chinese medicines Drugs 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/20—Vanadium, niobium or tantalum
- B01J23/22—Vanadium
-
- B01J35/39—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- 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
-
- 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
- C02F2101/34—Organic compounds containing oxygen
-
- 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
- C02F2101/36—Organic compounds containing halogen
-
- 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
-
- 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
Abstract
The invention belongs to environmental material fields, and in particular to a kind of BiVO4The preparation method and application of@carbon nano dot composite photocatalyst material.The present invention is using sodium lignin sulfonate, five water bismuth nitrates and ammonium metavanadate as raw material, by hydrothermal synthesis BiVO4During sodium lignin sulfonate is added, sodium lignin sulfonate controls BiVO during the reaction4Pattern growth, itself is carbonized into nano dot at high temperature under high pressure, to obtain a kind of BiVO of carbon nano dot package4The BiVO of nutty structure4@carbon nano dot composite material.Preparation process of the present invention is simple and convenient, with pure phase BiVO4Material, which is compared, has more excellent degradation occrycetin effect, has great application prospect in terms of antibiotic waste water of degrading.Meanwhile the present invention is rich using biomaterial as carbon source, enriches the development and utilization of biomaterial.
Description
Technical field
The invention belongs to environmental material fields, and in particular to a kind of BiVO4The preparation of@carbon nano dot composite photocatalyst material
Method and application.
Background technique
Long-term industrial development, although improving the level of human society, various resources are also largely consumed.The energy
As the foundation stone of social development, global environmental pollution is also gradually aggravated during the utilization of the energy, and ecological disruption is serious.How
Pollution remission and the harm of ecological disruption bring, are always a scientific research significant problem urgently to be solved, as a result, a kind of light
Catalysis technique is widely studied.Photocatalysis refers to the photochemical reaction carried out under the action of some catalyst, utilizes catalyst
With photochemical combination, accelerate chemical reaction under the synergistic effect of light by catalysis material.
In recent years, pucherite semiconductor material due to the characteristics such as easily prepared, stability is good, visible UV Absorption is strong by
Applied to photocatalysis field, but in practical degradation experiment, electron-hole is easily compound, and hardly possible separates and adsorption is indifferent,
Cause its catalytic activity limited.Existing research surface, it is modified to pucherite semiconductor material, as noble metal loading, element doping,
The technologies such as semiconductor coupling can be effectively improved the activity of catalyst.Carbon nano dot is as a kind of zero dimension carbon material, surface tool
There is oxygen-containing functional group abundant, be easy to modify, preferable light property of converting shows carbon nano dot also in photocatalysis field
Good application prospect.However, using the derivative or extract of biomaterial or biomaterial as the report of carbon source and research
Still less.
Summary of the invention
In view of this, it is an object of the invention to a kind of BiVO4The preparation method of@carbon nano dot composite photocatalyst material with
Lignin sulfonic acid sodium raw materials are probed into as formation mechenism of the carbon source in terms of preparing catalysis material and right using, the present invention
The advantage of conductor photocatalysis aspect of performance, BiVO provided by the invention4@carbon nano dot composite photocatalyst material is applied to processing
The processing of occrycetin in Wastewater Pollutant.
The present invention provides a kind of BiVO4The preparation method of@carbon nano dot composite photocatalyst material, comprising the following steps:
Ammonium metavanadate, which is dissolved in sodium hydroxide solution, is made mixed solution A, and five water bismuth nitrates and neopelex are total
Mixed solution B is made with being dissolved in nitric acid solution, mixed solution A and mixed solution B are mixed evenly, adjusts pH value and obtains
To BiVO4Presoma；Take suitable sodium lignin sulfonate that the BiVO of preparation is added4In presoma, reaction is moved to after mixing evenly
Kettle, the solid centrifuge washing that will be obtained after calcining are obtained by drying to arrive BiVO4@carbon nano dot composite material.
Preferably, the mass ratio of the ammonium metavanadate and sodium hydroxide is 3:20.
Preferably, the mass ratio of the five water bismuth nitrate, neopelex and nitric acid is 0.49:0.25:2.52.
Preferably, it is 6 ~ 8 that the adjusting pH value, which is with sodium hydroxide solution adjusting pH value,.
Preferably, the mass ratio of the quality of the sodium lignin sulfonate and ammonium metavanadate is 1 ~ 20g:11.70 g.
Preferably, 160 ~ 200 DEG C of the calcination temperature, 8 ~ 16h of calcination time.
The present invention is prepared for a kind of BiVO4@carbon nano dot composite photocatalyst material, preparation method as described above obtain
The composite photo-catalyst arrived, the degradation applied to occrycetin.
Compared with prior art, beneficial effects of the present invention embody as follows:
The present invention is using sodium lignin sulfonate, five water bismuth nitrates and ammonium metavanadate as raw material, by hydrothermal synthesis BiVO4Mistake
Sodium lignin sulfonate is added in journey, sodium lignin sulfonate controls BiVO during the reaction4Pattern growth, from high temperature height
Pressure carbonization is at nano dot, to obtain a kind of BiVO of carbon nano dot package4The BiVO of nutty structure4@carbon nano dot is compound
Material.Preparation process of the present invention is simple and convenient, with pure phase BiVO4Material, which is compared, has more excellent degradation occrycetin effect
Fruit has great application prospect in terms of antibiotic waste water of degrading.Meanwhile the present invention is enriched using biomaterial as carbon source
The development and utilization of biomaterial prepares carbon nano dot and has established research base for the byproduct of biomaterial or biomaterial
Plinth.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
The embodiment of invention for those of ordinary skill in the art without creative efforts, can also basis
The attached drawing of offer obtains other attached drawings.
Fig. 1 is the pure phase BiVO prepared in embodiment 54The BiVO prepared in material and embodiment 34@carbon nano dot composite wood
The SEM comparison diagram of material；
Fig. 2 is BiVO prepared by embodiment 34The TEM of@carbon nano dot composite material schemes；
Fig. 3 is the pure phase BiVO prepared in embodiment 54The BiVO prepared in material and embodiment 1-44@carbon nano dot composite wood
Expect the degradation curve comparison diagram of degradation OXYTETRACYCLINE HCL respectively；
Fig. 4 is BiVO prepared by embodiment 34The pure phase BiVO prepared in@carbon nano dot composite material and embodiment 54Material
XRD comparison diagram.
Specific embodiment
Below with reference to specific implementation example, the present invention will be further described.
It is limited that reagent alcohol used in the present invention, sodium hydroxide, neopelex are purchased from traditional Chinese medicines chemical reagent
Company；Ammonium metavanadate, five water bismuth nitrates, occrycetin, sodium lignin sulfonate purchase are in Shanghai Aladdin reagent Co., Ltd.
Prepared BiVO in the present invention4The photocatalytic activity evaluation of@carbon nano dot composite material is in photochemical reactor
Middle progress, 300 W xenon lamps irradiation, 100 mL occrycetin simulated wastewaters are added in reactor and measure its initial value, so
20 mg composite catalysts obtained are added afterwards, magnetic agitation maintains the catalyst in suspension or afloat, and first dark absorption half is small
When, it is then spaced 15 min sampling analyses in During Illumination, supernatant liquor spectrophotometric determination extinction is taken after centrifuge separation
Degree calculates degradation rate.Degradation rate formula :=[(1-Ct/C0)] x100%, wherein C0The extinction of solution when to reach adsorption equilibrium
Degree, CtFor the absorbance of the solution of timing sampling measurement.
Embodiment 1
0.1170 g ammonium metavanadate is dissolved in the sodium hydroxide solution of 10 mL, 2 mol/L, mixed solution A is made, it will
0.4851 g, five water bismuth nitrate and 0.25 g neopelex co-dissolve are in the nitric acid solution of 10 mL, 4 mol/L
Mixed solution B is made, mixed solution A and mixed solution B are mixed evenly, adjusts pH with the sodium hydroxide solution of 2mol/L
=6, obtain BiVO4Presoma；Take the sodium lignin sulfonate of 0.01 g that the BiVO of preparation is added4In presoma, stirring makes lignin
Sodium sulfonate is completely dissolved, and obtained mixed solution is transferred in reaction kettle 200 DEG C after calcination reaction 8 hours and is consolidated what is obtained
Body centrifuge washing, it is obtained by drying to arrive BiVO4@carbon nano dot composite material.
Photocatalytic degradation test: the BiVO that will be obtained4@carbon nano dot composite material carries out light in photochemical reactor and urges
Change Degrading experiment, measures the BiVO4@carbon nano dot composite material reaches 35 in 90 min to the degradation rate of occrycetin
%。
Embodiment 2:
0.1170 g ammonium metavanadate is dissolved in the sodium hydroxide solution of 10 mL, 2 mol/L, mixed solution A is made, it will
0.4851 g, five water bismuth nitrate and 0.25 g neopelex co-dissolve are in the nitric acid solution of 10 mL 4mol/L
Mixed solution B is made, mixed solution A and mixed solution B are mixed evenly, 2mol/L sodium hydroxide solution adjusts pH=8,
Obtain BiVO4Presoma；Take the sodium lignin sulfonate of 0.05 g that the BiVO of preparation is added4In presoma, stirring makes lignin sulfonic acid
Sodium is completely dissolved, by obtained mixed solution be transferred in reaction kettle 160 DEG C after calcination reaction 16 hours by obtained solid from
Heart washing, it is obtained by drying to arrive BiVO4@carbon nano dot composite material.
Photocatalytic degradation test: the BiVO that will be obtained4@carbon nano dot composite material, which is placed in photochemical reactor, carries out light
Catalytic degradation test, measures the BiVO4@carbon nano dot composite material reaches 46 in 90 min to the degradation rate of occrycetin
%。
Embodiment 3:
0.1170 g ammonium metavanadate is dissolved in the sodium hydroxide solution of 10 mL, 2 mol/L, mixed solution A is made, it will
0.4851 g, five water bismuth nitrate and 0.25 g neopelex co-dissolve are in the nitric acid solution of 10 mL, 4 mol/L
Mixed solution B is made, mixed solution A and mixed solution B are mixed evenly, 2mol/L sodium hydroxide solution adjusts pH=7,
Obtain BiVO4Presoma；Take the sodium lignin sulfonate of 0. 10 g that the BiVO of preparation is added4In presoma, stirring makes sulfomethylated lignin
Sour sodium is completely dissolved, and obtained mixed solution is transferred in reaction kettle 160 DEG C of solids that will be obtained after calcination reaction 16 hours
Centrifuge washing, it is obtained by drying to arrive BiVO4@carbon nano dot composite material.
Photocatalytic degradation test: by the BiVO of preparation4@carbon nano dot composite material, which is placed in photochemical reactor, carries out light
Catalytic degradation test, measures the BiVO4@carbon nano dot composite material reaches 51 in 90 min to the degradation rate of occrycetin
%。
Embodiment 4:
0.1170 g ammonium metavanadate is dissolved in the sodium hydroxide solution of 10 mL, 2 mol/L, mixed solution A is made, it will
0.4851 g, five water bismuth nitrate and 0.25 g neopelex co-dissolve are in the nitric acid solution of 10 mL, 4 mol/L
Mixed solution B is made, mixed solution A and mixed solution B are mixed evenly, 2mol/L sodium hydroxide solution adjusts pH=7,
Obtain BiVO4Presoma；Take the sodium lignin sulfonate of 0. 20g that the BiVO of preparation is added4In presoma, stirring makes lignin sulfonic acid
Sodium is completely dissolved, by obtained mixed solution be transferred in reaction kettle 160 DEG C after calcination reaction 16 hours by obtained solid from
Heart washing, it is obtained by drying to arrive BiVO4@carbon nano dot composite material.
Photocatalytic degradation test: by the BiVO of preparation4@carbon nano dot composite material, which is placed in photochemical reactor, carries out light
Catalytic degradation test, measures the BiVO4@carbon nano dot composite material reaches 39 in 90 min to the degradation rate of occrycetin
%。
Embodiment 5: pure phase BiVO4The preparation of material
The BiVO that will be prepared in embodiment 34Presoma be directly placed into reaction kettle 160 DEG C after calcination reaction 16 hours from
Heart washing, obtains pure phase BiVO after drying4Material.The pure phase BiVO that will be prepared4Material carries out in photochemical reactor
Photocatalytic degradation test, measures and reaches 22% in 90 min to the degradation rate of occrycetin.
Fig. 1 is the pure phase BiVO prepared in embodiment 54The BiVO prepared in material and embodiment 34@carbon nano dot composite wood
The SEM comparison diagram of material；In figure, a is pure phase BiVO4Material, b BiVO4@carbon nano dot composite material；It can be seen from figure 1 that pure phase
BiVO4Material is a kind of laminated structure, and material surface is smooth；And the BiVO prepared4@carbon nano dot composite material surface is size
The grain structure of very little illustrates the addition of sodium lignin sulfonate to BiVO4Size and shape have significant effect.
Fig. 2 is BiVO prepared by embodiment 34The TEM of@carbon nano dot composite material schemes；It is clear that from Fig. 3
A kind of black color dots that size is minimum are coated on a kind of biggish material periphery of particle, form carbon nano dot enwrapped granule structure,
In, minimum stain is that sodium lignin sulfonate carbonization is formed by black carbon nano dot, and the biggish material of particle is BiVO4
Grain, the sodium lignin sulfonate known to TEM photo not only limit BiVO during the reaction4Growth, and be carbonized at nanometer
Point is wrapped in BiVO4Around particle.
Fig. 3 is the pure phase BiVO prepared in embodiment 54The BiVO prepared in material and embodiment 1-44@carbon nano dot is compound
Material is degraded the degradation curve comparison diagram of occrycetin respectively；In figure, the 1 pure phase BiVO to be prepared in embodiment 54Material, 2
For the BiVO prepared in embodiment 14@carbon nano dot composite material, 3 BiVO to be prepared in embodiment 24@carbon nano dot composite wood
Material, 4 BiVO to be prepared in embodiment 34@carbon nano dot composite material, 5 BiVO to be prepared in embodiment 44@carbon nano dot is multiple
Condensation material.As can be seen from Figure 3, pure phase BiVO4Catalyst degradation rate is about 22 %, is prepared in the embodiment of the present application 1-4
BiVO4@carbon nano dot composite degradation rate improves 1.6 times or more, and the degradation effect of 3 products therefrom of embodiment is best, reaches
To 2.3 times, catalytic performance is more excellent.
Fig. 4 is BiVO prepared by embodiment 34Pure phase BiVO prepared by@carbon nano dot composite material and embodiment 54Material
The XRD comparison diagram of material.In figure, a is pure phase BiVO4The XRD diagram of material, b are BiVO prepared by embodiment 34@carbon nano dot is multiple
The XRD diagram of condensation material；It can be found that pure phase BiVO4The characteristic diffraction peak and standard card BiVO of material4(PDF#44-0081) complete
It is complete corresponding, and without any miscellaneous peak.BiVO4The characteristic diffraction peak and pure phase BiVO of@carbon nano dot composite material4The diffraction of material
Peak exact matching, the position of diffraction maximum also do not shift, illustrate that sodium lignin sulfonate is carbonized the carbon nano dot to be formed to BiVO4
Crystal form do not impact.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, without conflicting with each other, those skilled in the art can say this
The feature of different embodiments or examples described in bright book and different embodiments or examples is combined.
Claims (7)
1. a kind of BiVO4The preparation method of@carbon nano dot composite material, which comprises the following steps: ammonium metavanadate is molten
Mixed solution A is made in solution in sodium hydroxide solution, and five water bismuth nitrates and neopelex co-dissolve are molten in nitric acid
Mixed solution B is made in liquid, mixed solution A and mixed solution B are mixed evenly, adjusts pH value and obtains BiVO4Presoma；
Take suitable sodium lignin sulfonate that the BiVO of preparation is added4In presoma, reaction kettle is moved to after mixing evenly, will be obtained after calcining
Solid centrifuge washing, it is obtained by drying arrive BiVO4@carbon nano dot composite material.
2. the preparation method of composite material according to claim 1, which is characterized in that the ammonium metavanadate and sodium hydroxide
Mass ratio is 3:20.
3. the preparation method of composite material according to claim 1, which is characterized in that the five water bismuth nitrate, dodecyl
The mass ratio of benzene sulfonic acid sodium salt and nitric acid is 0.49:0.25:2.52.
4. the preparation method of composite material according to claim 1, which is characterized in that adjusting pH value is to use sodium hydroxide solution
Adjusting pH value is 6 ~ 8.
5. the preparation method of composite material according to claim 1, which is characterized in that the quality of the sodium lignin sulfonate with
The mass ratio of ammonium metavanadate is 1 ~ 20g:11.70 g.
6. the preparation method of composite material according to claim 2, which is characterized in that 160 ~ 200 DEG C of the calcination temperature,
8 ~ 16h of calcination time.
7. the BiVO of preparation method preparation as claimed in any one of claims 1 to 64@carbon nano dot composite material is for being catalyzed drop
Solve the purposes of occrycetin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910688738.4A CN110465285B (en) | 2019-07-29 | 2019-07-29 | BiVO4Preparation method and application of @ carbon nano-dot composite photocatalytic material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910688738.4A CN110465285B (en) | 2019-07-29 | 2019-07-29 | BiVO4Preparation method and application of @ carbon nano-dot composite photocatalytic material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110465285A true CN110465285A (en) | 2019-11-19 |
| CN110465285B CN110465285B (en) | 2022-05-17 |
Family
ID=68509644
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910688738.4A Active CN110465285B (en) | 2019-07-29 | 2019-07-29 | BiVO4Preparation method and application of @ carbon nano-dot composite photocatalytic material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110465285B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114784256A (en) * | 2022-06-21 | 2022-07-22 | 暨南大学 | Preparation method of bismuth-based composite negative electrode material of ultrahigh-rate potassium ion battery |
| CN116237037A (en) * | 2023-03-01 | 2023-06-09 | 西南科技大学 | Preparation method and application of bismuth vanadate nanosheet composite material |
| CN116328843A (en) * | 2022-12-29 | 2023-06-27 | 广西民族大学 | Heterogeneous photocatalyst and preparation method and application thereof |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102951682A (en) * | 2012-11-14 | 2013-03-06 | 陕西科技大学 | Preparation method of cellular spherical bismuth vanadate microcrystalline |
| CN103007921A (en) * | 2012-12-24 | 2013-04-03 | 陕西科技大学 | Method for synthesizing carbon-doped BiVO4 photocatalyst by using microwave hydrothermal method |
| CN103408063A (en) * | 2013-08-07 | 2013-11-27 | 江苏大学 | Hydrothermal method for preparation of nano-zinc oxide by taking lignosulphonate as surfactant |
| WO2014096544A1 (en) * | 2012-12-19 | 2014-06-26 | Teknologian Tutkimuskeskus Vtt | Process for the hydrothermal treatment of high molar mass biomaterials |
| WO2015094888A1 (en) * | 2013-12-17 | 2015-06-25 | Polyad Services, Llc | Pre-exfoliated layered materials |
| CN105080534A (en) * | 2015-08-10 | 2015-11-25 | 广西大学 | Microwave hydrothermal synthesis method for photocatalyst BiVO4 |
| CN108390043A (en) * | 2018-03-07 | 2018-08-10 | 齐鲁工业大学 | A kind of sodium-ion battery positive material Na3V2(PO4)3/ C and preparation method thereof |
| CN110052263A (en) * | 2019-04-30 | 2019-07-26 | 广东工业大学 | A kind of photocatalytic nanometer fibrous material and its preparation method and application |
-
2019
- 2019-07-29 CN CN201910688738.4A patent/CN110465285B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102951682A (en) * | 2012-11-14 | 2013-03-06 | 陕西科技大学 | Preparation method of cellular spherical bismuth vanadate microcrystalline |
| WO2014096544A1 (en) * | 2012-12-19 | 2014-06-26 | Teknologian Tutkimuskeskus Vtt | Process for the hydrothermal treatment of high molar mass biomaterials |
| CN103007921A (en) * | 2012-12-24 | 2013-04-03 | 陕西科技大学 | Method for synthesizing carbon-doped BiVO4 photocatalyst by using microwave hydrothermal method |
| CN103408063A (en) * | 2013-08-07 | 2013-11-27 | 江苏大学 | Hydrothermal method for preparation of nano-zinc oxide by taking lignosulphonate as surfactant |
| WO2015094888A1 (en) * | 2013-12-17 | 2015-06-25 | Polyad Services, Llc | Pre-exfoliated layered materials |
| CN105080534A (en) * | 2015-08-10 | 2015-11-25 | 广西大学 | Microwave hydrothermal synthesis method for photocatalyst BiVO4 |
| CN108390043A (en) * | 2018-03-07 | 2018-08-10 | 齐鲁工业大学 | A kind of sodium-ion battery positive material Na3V2(PO4)3/ C and preparation method thereof |
| CN110052263A (en) * | 2019-04-30 | 2019-07-26 | 广东工业大学 | A kind of photocatalytic nanometer fibrous material and its preparation method and application |
Non-Patent Citations (2)
| Title |
|---|
| JIANTING TANG等: "Facile hydrothermal-carbonization approach to carbon-modified BiVO4 composites with enhanced photocatalytic activity", 《MATERIALS SCIENCE IN SEMICONDUCTOR PROCESSING》 * |
| SHENGJUN YE 等: "Photocatalytic performance of multi-walled carbon nanotube/BiVO4 synthesized by electro-spinning process and its degradation mechanisms on oxytetracycline", 《CHEMICAL ENGINEERING JOURNAL》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114784256A (en) * | 2022-06-21 | 2022-07-22 | 暨南大学 | Preparation method of bismuth-based composite negative electrode material of ultrahigh-rate potassium ion battery |
| CN114784256B (en) * | 2022-06-21 | 2022-09-09 | 暨南大学 | Preparation method of bismuth-based composite negative electrode material of ultrahigh-rate potassium ion battery |
| CN116328843A (en) * | 2022-12-29 | 2023-06-27 | 广西民族大学 | Heterogeneous photocatalyst and preparation method and application thereof |
| CN116237037A (en) * | 2023-03-01 | 2023-06-09 | 西南科技大学 | Preparation method and application of bismuth vanadate nanosheet composite material |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110465285B (en) | 2022-05-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110465285A (en) | A kind of BiVO4The preparation method and application of@carbon nano dot composite photocatalyst material | |
| CN107376968B (en) | Tungstic acid/double Z shaped photochemical catalyst of carbonitride/bismuth oxide and its preparation method and application | |
| CN105032464B (en) | Carbonitride metatitanic acid nickel composite material and preparation method and application | |
| CN101972645B (en) | Method for preparing bismuth titanate as visible light response semiconductor photochemical catalyst | |
| Sun et al. | The effect of pH on the photocatalytic performance of BiVO4 for phenol mine sewage degradation under visible light | |
| CN110465315A (en) | Supermolecule polymerize carbon nitride photocatalyst and its preparation method and application | |
| CN109364958A (en) | A kind of Bi4O5BrxI2-xThe preparation method of mischcrystal photocatalyst | |
| CN105664988B (en) | A kind of (BiO)2CO3/ C composite photo-catalysts and its application | |
| CN109482219A (en) | Activate the CoFe of persulfate advanced treatment on coking wastewater2O4/ N doping sludge-based activated carbon catalyst and preparation method | |
| CN108671951B (en) | Carbon nitride composite photocatalyst and preparation method and application thereof | |
| CN105833887B (en) | A kind of BiOCl/ β FeOOH composite nano materials and preparation method thereof | |
| CN109317184A (en) | Difunctional β-FeOOH/eg-C3N4Composite nano materials and its preparation method and application | |
| CN110354895A (en) | A kind of oxide porous photochemical catalyst of molecular screen base Ce-Mn and its preparation method and application | |
| CN107670683A (en) | A kind of FeVO4@g‑C3N4Core shell structure heterojunction photocatalyst and preparation method thereof | |
| CN102836719A (en) | Preparation method of perovskite type photocatalyst and product thereof | |
| CN105709744B (en) | The preparation method of catalytic wet oxidation catalyst | |
| CN108940349A (en) | The method of carbonitride Z-type photochemical catalyst removal dyestuff contaminant is mixed using siliver chromate/sulphur | |
| CN103950978A (en) | Biomimetic synthesis method of bismuth vanadate visible-light photocatalyst having hierarchical structure | |
| CN109806881A (en) | A kind of iron-molybdic catalyst and preparation method thereof for prepn. of formaldehyde by oxidation of methanol | |
| CN113893855B (en) | Resin fibrous mesoporous SiO 2 Loaded with Fe 2 O 3 Catalyst, preparation method and application thereof | |
| CN1159098C (en) | Fe-base catalyst for Fischer-Tropsch syuthesis and its preparing process | |
| CN108440576B (en) | A kind of application of hydridization copper iodine cluster and its photocatalytic degradation of dye | |
| CN107983385B (en) | Nickel-based magnetic composite material and synthesis method and application thereof | |
| Othman et al. | Preparation, Characterization and Photocatalytic Activity of sulphated V2O5-ZrO2 Catalysts for the Degradation of Direct Blue-1 dye | |
| CN111054422B (en) | Composite photocatalyst and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |