CN107930625A - A kind of BiVO of ruthenium load4The preparation method of@C composite material of core-shell structure - Google Patents
A kind of BiVO of ruthenium load4The preparation method of@C composite material of core-shell structure Download PDFInfo
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- CN107930625A CN107930625A CN201711137025.6A CN201711137025A CN107930625A CN 107930625 A CN107930625 A CN 107930625A CN 201711137025 A CN201711137025 A CN 201711137025A CN 107930625 A CN107930625 A CN 107930625A
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- bivo
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- shell structure
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- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 229910052707 ruthenium Inorganic materials 0.000 title claims abstract description 30
- 239000002131 composite material Substances 0.000 title claims abstract description 26
- 239000011258 core-shell material Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 229910002915 BiVO4 Inorganic materials 0.000 claims abstract description 41
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 20
- 239000008103 glucose Substances 0.000 claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 16
- 229910019891 RuCl3 Inorganic materials 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 claims abstract description 10
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 20
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 20
- 239000000243 solution Substances 0.000 claims description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- -1 polytetrafluoroethylene Polymers 0.000 claims description 10
- 229910001220 stainless steel Inorganic materials 0.000 claims description 10
- 239000010935 stainless steel Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 9
- 238000000926 separation method Methods 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000013019 agitation Methods 0.000 claims description 7
- 239000003643 water by type Substances 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 150000001621 bismuth Chemical class 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 229910052720 vanadium Inorganic materials 0.000 claims description 6
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 229910003206 NH4VO3 Inorganic materials 0.000 claims description 3
- 229910020700 Na3VO4 Inorganic materials 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical class O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- JHXKRIRFYBPWGE-UHFFFAOYSA-K bismuth chloride Chemical compound Cl[Bi](Cl)Cl JHXKRIRFYBPWGE-UHFFFAOYSA-K 0.000 claims description 3
- 239000012456 homogeneous solution Substances 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 3
- IHIXIJGXTJIKRB-UHFFFAOYSA-N trisodium vanadate Chemical compound [Na+].[Na+].[Na+].[O-][V]([O-])([O-])=O IHIXIJGXTJIKRB-UHFFFAOYSA-N 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 230000008859 change Effects 0.000 claims description 2
- 238000009413 insulation Methods 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 1
- UXAMZEYKWGPDBI-UHFFFAOYSA-N C(CCCCCCCCCCCCCCC)Br(C)(C)C Chemical class C(CCCCCCCCCCCCCCC)Br(C)(C)C UXAMZEYKWGPDBI-UHFFFAOYSA-N 0.000 claims 1
- 230000015556 catabolic process Effects 0.000 abstract description 13
- 238000006731 degradation reaction Methods 0.000 abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 12
- 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 abstract description 10
- 229940043267 rhodamine b Drugs 0.000 abstract description 10
- 229910052799 carbon Inorganic materials 0.000 abstract description 9
- 239000002114 nanocomposite Substances 0.000 abstract description 8
- 238000005516 engineering process Methods 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 3
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 150000004676 glycans Chemical class 0.000 abstract 1
- 229910001385 heavy metal Inorganic materials 0.000 abstract 1
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- 150000002500 ions Chemical class 0.000 abstract 1
- 239000004005 microsphere Substances 0.000 abstract 1
- 229920001282 polysaccharide Polymers 0.000 abstract 1
- 239000005017 polysaccharide Substances 0.000 abstract 1
- 239000011257 shell material Substances 0.000 description 17
- 238000005253 cladding Methods 0.000 description 7
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 6
- 230000003760 hair shine Effects 0.000 description 5
- 238000005286 illumination Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 229910021389 graphene Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- SWLVFNYSXGMGBS-UHFFFAOYSA-N ammonium bromide Chemical compound [NH4+].[Br-] SWLVFNYSXGMGBS-UHFFFAOYSA-N 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000000921 elemental analysis Methods 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 125000000913 palmityl group Chemical group [H]C([*])([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])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910014033 C-OH Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910014570 C—OH Inorganic materials 0.000 description 1
- 241001062009 Indigofera Species 0.000 description 1
- 238000002083 X-ray spectrum Methods 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 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
- 230000007812 deficiency Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000005036 potential barrier Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
- B01J23/64—Platinum group metals with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/648—Vanadium, niobium or tantalum or polonium
- B01J23/6482—Vanadium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
-
- 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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Toxicology (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Carbon And Carbon Compounds (AREA)
- Catalysts (AREA)
Abstract
The invention belongs to inorganic nano composite material preparation field, is related to a kind of BiVO of ruthenium load4The preparation method of@C composite material of core-shell structure, by combining RuCl3、BiVO4And glucose, the monodispersity for the carbon containing polysaccharide microsphere being carbonized using glucose hydro-thermal method is good and outer layer contains the BiVO that substantial amounts of hydroxyl hydrophilic group structure New Ruthenium loads4@C composite material of core-shell structure, and have very high absorption degradation rate to rhodamine B, substantially increase BiVO4Application range.The technology has the advantages that method is simple, energy saving green non-pollution.The fields such as the material synthesized can be widely used for being catalyzed, useless Organic substance in water, heavy metal ion reduction.
Description
Technical field
The invention belongs to inorganic nano composite material preparation field, is related to a kind of BiVO of ruthenium load4@C core shell structures are answered
The preparation method of condensation material.
Background technology
Polynary metal oxide BiVO4Due to abundant structure and pattern, it is considered to be have a extensive future
One of novel visible catalyst.Being reported first from 1998 under visible light can be since photodissociation aquatic products oxygen, this ten
Between several years significant progress has been obtained in visible light catalytic field.But still suffer from present quantum efficiency is low, solar energy utilization ratio is low,
The shortcomings of photocatalytic mechanism is still not very clear, it is difficult to realize the efficient degradation to organic pollution, this will become BiVO4Light is urged
The key of agent design.
Another material cladding is got up and the nucleocapsid knot formed by chemical bond or other interactions by a kind of material
Structure nanocomposite, it can not only retain the substance characteristics of one-component, but also can the ingenious coupling using between multi-stage interface
Cooperation is used, and obtains more effective active units and more preferable stability, has huge application prospect.Wherein, amorphous carbon by
Contain abundant functional group (C=O, C-OH etc.) in surface to be often used as supporting and protecting BiVO4Shell Materials.Separately
On the one hand, by depositing noble metal, Schottky potential barriers are formed on metal-semiconductor interface, so as to change the table of semiconductor
Surface properties, improve photodegradative quantum efficiency.It is contemplated that the high efficiency charge separation rate of integrated application noble metal and with abundant
The shell of activity hydroxy makes BiVO4With many new characteristics.Patent CN102600857A discloses a kind of carbon ball load
CuO-BiVO4The preparation method of heterojunction composite photocatalyst, photochemical catalyst made from the technology are degraded methylene under visible light
Base indigo plant shows preferable activity.Patent CN104437466A and patent CN104383910A disclose a kind of carbon nanotubes respectively
Pucherite/graphene complex light that the preparation method and a kind of granular size of compound pucherite green deep water treatment agent are controllable is urged
The preparation method of agent, is modified pucherite using graphene.Although these modified pucherites have carried in performance
Height, but the degrading activity in practical application is still undesirable, and also the carbon material such as graphene used, carbon nanotubes is costly.
Therefore, in order to overcome deficiency of the prior art, the present invention provide it is a kind of can efficient degradation rhodamine B ruthenium load BiVO4@C
The preparation method of composite material of core-shell structure, substantially increases BiVO4Application range.The technology is simple, energy saving with method
The advantages that green non-pollution, there is presently no the report on such technology, this is that the development exploration of new material goes out one newly
Road.
The content of the invention
Method it is an object of the invention to provide a kind of simple, the energy saving green non-pollution of method prepares ruthenium load
BiVO4@C composite material of core-shell structure.
What the object of the invention was realized in：A kind of BiVO of ruthenium load4The preparation method of@C composite material of core-shell structure,
It is it is critical that by BiVO4Sample and glucose are according to molar ratio：BiVO4:Glucose=1:1~16 is added to reaction vessel
In, and add RuCl3, and deionized water is added, RuCl3With BiVO4The molar ratio of sample is 0.5~2.5:25, stir at room temperature
It is uniformly mixed, then adds 140~200 DEG C of insulation reactions in reaction kettle, obtains the BiVO of target product ruthenium load4@C nucleocapsid knots
Structure composite material.
More particularly, comprise the following steps that：
Step 1：Weigh 2.5mmol BiVO4(0.81g) sample, according to n (BiVO4:Glucose)=1:1~16 adds 2.5
~40mmol glucose (0.45~7.2g), adds 25mL deionized waters and 0.05~0.25mmol RuCl3(0.01~
0.052g), 24~48h of magnetic agitation at room temperature；
Step 2：By step 1 resulting solution add 50mL liner for polytetrafluoroethylene (PTFE) stainless steel cauldron in, 140~
4h, products obtained therefrom separation, washing and dry, the BiVO loaded up to target product ruthenium are kept at 200 DEG C4@C core shell structures are compound
Material.
More particularly, BiVO4The preparation process of sample is as follows：
Step A：Take the bismuth salt of 0.02mol to be dissolved in 20mL concentrated nitric acids and obtain homogeneous solution, stir 2h；
Step B：The vanadium-containing compound of 0.02mol is dissolved in the NaOH aqueous solutions of the 6M of 20mL；
Step C：Step B resulting solutions are added in step A resulting solutions, then by 0.1~0.5g cetyl front threes
Base ammonium bromide (CTAB) is added in resulting solution, stirs 2h, is then slowly added into the NaOH aqueous solutions of 30mL 6M, is obtained uniformly
Suspension, stirs 2h；
Step D：It is in the stainless steel cauldron of polytetrafluoroethylene (PTFE) 180 by the liner that step C resulting solutions add 100mL
48h is kept at DEG C, products therefrom is centrifuged with deionized water multiple, then dry 8h at 60 DEG C, obtains BiVO4Sample.
Bismuth salt described in above-mentioned steps A is Bi (NO3)3·5H2O or BiCl3。
Vanadium-containing compound described in above-mentioned steps A is NH4VO3Or Na3VO4。
The purity of medicine used is pure not less than analyzing in above-mentioned steps D.
In above-mentioned steps 2 after solid matter separation, alternately washed using deionized water, absolute ethyl alcohol, up to ruthenium after drying
The BiVO of load4@C composite material of core-shell structure.
In above-mentioned steps 2, deionized water washing times are used as 4~6 times；The drying temperature is 60~80 DEG C, dry
Time is 6~12h.
The beneficial effects of the present invention are：
1st, the present invention is realized the ruthenium formed based on ruthenium and carbon-coating " one-step method " cladding and loads BiVO4@C core shell structures are compound
Material, the composite material surface contain abundant hydroxyl group, have preferably dispersiveness and stability, compared to pure phase BiVO4
There is very high absorption degradation rate to rhodamine B.
2nd, synthetic method provided by the invention need not add auxiliary agent, and material has environmental-friendly, degradable harmful dirt in itself
The advantages that contaminating thing.
3rd, products therefrom post processing of the present invention is simple, and recycling is convenient, reusable edible, and accessory substance is few.
Brief description of the drawings
Fig. 1 show the high-resolution-ration transmission electric-lens figure (HRTEM) of various embodiments of the present invention products therefrom.
Fig. 2 show the energy dispersion X-ray spectrum (EDX elemental analyses) of 4 products therefrom of the embodiment of the present invention.
Fig. 3 show various embodiments of the present invention products therefrom and degrades under visible light to waste water from dyestuff rhodamine B (RhB)
Figure.
Embodiment
The present invention is further clarified with reference to embodiment.
Embodiment 1
BiVO4The preparation process of sample is as follows：
Step A：Take the bismuth salt of 0.02mol to be dissolved in 20mL concentrated nitric acids and obtain homogeneous solution, stir 2h；The bismuth salt is Bi
(NO3)3·5H2O or BiCl3；The vanadium-containing compound is NH4VO3Or Na3VO4；
Step B：The vanadium-containing compound of 0.02mol is dissolved in the NaOH aqueous solutions of the 6M of 20mL；
Step C：Step B resulting solutions are added in step A resulting solutions, then by 0.1~0.5g cetyl front threes
Base ammonium bromide (CTAB) is added in resulting solution, stirs 2h, is then slowly added into the NaOH aqueous solutions of 30mL 6M, is obtained uniformly
Suspension, stirs 2h；
Step D：It is in the stainless steel cauldron of polytetrafluoroethylene (PTFE) 180 by the liner that step 3 resulting solution adds 100mL
48h is kept at DEG C, products therefrom is centrifuged with deionized water multiple, then dry 8h at 60 DEG C, obtains BiVO4Sample.Step D
In medicine used purity not less than analyze it is pure, ensure cleaning separation process in does not bring impurity into.
Embodiment 2：
Weigh the 2.5mmol BiVO that embodiment 1 obtains4(0.81g) sample, according to n (BiVO4:Glucose)=1:1 adds
2.5mmol glucose (0.45g), adds 25mL deionized waters and 0.05mmol RuCl3(0.01g), at room temperature magnetic agitation
24h.It is in the stainless steel cauldron of polytetrafluoroethylene (PTFE) by the liner that resulting solution adds 50mL, 4h, gained production is kept at 140 DEG C
Product separation, washing and dry, the BiVO loaded up to target product ruthenium4@C composite material of core-shell structure.
Fig. 1 b show the embodiment of the present invention 2 and ruthenium load BiVO are made4The HRTEM of/C nuclear-shell structured nano-composite materials shines
Piece, Fig. 1 a photos show that interplanar distance d=0.31nm corresponds to BiVO4(- 121) crystal face (JCPDS No.14-0688).Compared to
Sample obtained by Fig. 1 a is shown as BiVO4Outer cladding one layer of non-uniform agraphitic carbon shell, C shell thicknesses are 2~4nm, such as
Shown in Fig. 3, illumination 4h is 76.8% to the degradation efficiency of RhB to the present embodiment product under visible light, is pure phase BiVO4Degraded effect
1.4 times of rate.
Embodiment 3
Weigh the 2.5mmol BiVO that embodiment 1 obtains4(0.81g) sample, according to n (BiVO4:Glucose)=1:4 add
10mmol glucose (1.8g), adds 25mL deionized waters and 0.2mmol RuCl3(0.041g), at room temperature magnetic agitation 24h.
It is in the stainless steel cauldron of polytetrafluoroethylene (PTFE) by the liner that resulting solution adds 50mL, 4h, products obtained therefrom point is kept at 160 DEG C
From, washing and dry, up to the BiVO of target product ruthenium load4@C composite material of core-shell structure.
Fig. 1 c show the embodiment of the present invention 3 and ruthenium load BiVO are made4The HRTEM of/C nuclear-shell structured nano-composite materials shines
Piece, BiVO is shown as compared to sample obtained by Fig. 1 a4One layer of non-uniform agraphitic carbon shell of outer cladding, C shell thicknesses are 6
~8nm, as shown in figure 3, illumination 4h is 80% to the degradation efficiency of RhB to the present embodiment product under visible light, it is pure phase BiVO4
1.6 times of degradation efficiency.
Embodiment 4
Weigh the 2.5mmol BiVO that embodiment 1 obtains4(0.81g) sample, according to n (BiVO4:Glucose)=1:8 add
20mmol glucose (3.6g), adds 25mL deionized waters and 0.2mmol RuCl3(0.041g), at room temperature magnetic agitation 24h.
It is in the stainless steel cauldron of polytetrafluoroethylene (PTFE) by the liner that resulting solution adds 50mL, 4h, products obtained therefrom point is kept at 180 DEG C
From, washing and dry, up to the BiVO of target product ruthenium load4@C composite material of core-shell structure.
Fig. 1 d show the embodiment of the present invention and ruthenium load BiVO are made4The HRTEM of/C nuclear-shell structured nano-composite materials shines
Piece, BiVO is shown as compared to sample obtained by Fig. 1 a4Outer cladding one layer of non-uniform agraphitic carbon shell, C shell thicknesses are
13~16nm, as shown in figure 3, illumination 4h is 90% to the degradation efficiency of RhB to the present embodiment product under visible light, it is pure phase
BiVO41.64 times of degradation efficiency.Fig. 2 show the EDX elemental analysis photos of the present embodiment product, and photo shows products therefrom
Containing Bi, V, O, Ru, Cl, C and Cu element, wherein Cu and C element come from copper mesh substrate.
Embodiment 5
Weigh the 2.5mmol BiVO that embodiment 1 obtains4(0.81g) sample, according to n (BiVO4:Glucose)=1:12 add
Enter 30mmol glucose (5.4g), add 25mL deionized waters and 0.2mmol RuCl3(0.041g), at room temperature magnetic agitation
24h.It is in the stainless steel cauldron of polytetrafluoroethylene (PTFE) by the liner that resulting solution adds 50mL, 4h, gained production is kept at 200 DEG C
Product separation, washing and dry, the BiVO loaded up to target product ruthenium4@C composite material of core-shell structure.
Fig. 1 e show the embodiment of the present invention and ruthenium load BiVO are made4The HRTEM of/C nuclear-shell structured nano-composite materials shines
Piece, BiVO is shown as compared to sample obtained by Fig. 1 a4Outer cladding one layer of non-uniform agraphitic carbon shell, C shell thicknesses are
20~26nm, as shown in figure 3, illumination 4h is 89.7% to the degradation efficiency of RhB to the present embodiment product under visible light, it is pure phase
BiVO41.63 times of degradation efficiency.
Embodiment 6
Weigh the 2.5mmol BiVO that embodiment 1 obtains4(0.81g) sample, according to n (BiVO4:Glucose)=1:16 add
Enter 40mmol glucose (7.2g), add 25mL deionized waters and 0.25mmol RuCl3(0.052g), at room temperature magnetic agitation
24h.It is in the stainless steel cauldron of polytetrafluoroethylene (PTFE) by the liner that resulting solution adds 50mL, 4h, gained production is kept at 180 DEG C
Product separation, washing and dry, the BiVO loaded up to target product ruthenium4@C composite material of core-shell structure.
Fig. 1 f show the embodiment of the present invention and ruthenium load BiVO are made4The HRTEM of/C nuclear-shell structured nano-composite materials shines
Piece, BiVO is shown as compared to sample obtained by Fig. 1 a4Outer cladding one layer of non-uniform agraphitic carbon shell, C shell thicknesses are
28~33nm, as shown in figure 3, illumination 4h is 82% to the degradation efficiency of RhB to the present embodiment product under visible light, it is pure phase
BiVO41.5 times of degradation efficiency.
Although the embodiment of the present invention is had been presented for herein, it will be appreciated by those of skill in the art that not taking off
In the case of from spirit of the invention, the embodiments herein can be changed.Above-described embodiment is only exemplary, should not be with
Restriction of the embodiments herein as interest field of the present invention.
Claims (7)
- A kind of 1. BiVO of ruthenium load4The preparation method of@C composite material of core-shell structure, it is characterised in that by BiVO4Sample and Portugal Grape sugar is according to molar ratio：BiVO4:Glucose=1:1~16 is added in reaction vessel, and adds RuCl3, and add go from Sub- water, RuCl3With BiVO4The molar ratio of sample is 0.5~2.5:25, it is uniformly mixed, then adds in reaction kettle at room temperature 140~200 DEG C of insulation reactions, obtain the BiVO of target product ruthenium load4@C composite material of core-shell structure.
- A kind of 2. BiVO of ruthenium load according to claim 14The preparation method of@C composite material of core-shell structure, its feature It is, comprises the following steps that：Step 1：Weigh 2.5mmol BiVO4Sample, according to molar ratio n (BiVO4:Glucose)=1:1~16 add 2.5~ 40mmol glucose, adds 25mL deionized waters and 0.05~0.25mmol RuCl3, 24~48h of magnetic agitation at room temperature；Step 2：It is in the stainless steel cauldron of polytetrafluoroethylene (PTFE) 140~200 by the liner that step 1 resulting solution adds 50mL 4h, products obtained therefrom separation, washing and dry, the BiVO loaded up to target product ruthenium are kept at DEG C4@C core shell structure composite woods Material.
- A kind of 3. BiVO of ruthenium load according to claim 1 or 24The preparation method of@C composite material of core-shell structure, it is special Sign is, BiVO4The preparation process of sample is as follows：Step A：Take the bismuth salt of 0.02mol to be dissolved in 20mL concentrated nitric acids and obtain homogeneous solution, stir 2h；Step B：The vanadium-containing compound of 0.02mol is dissolved in the NaOH aqueous solutions of the 6M of 20mL；Step C：Step B resulting solutions are added in step A resulting solutions, then by 0.1~0.5g cetyl trimethyl bromines Change ammonium to add in resulting solution, stir 2h, be then slowly added into the NaOH aqueous solutions of 30mL 6M, obtain unit for uniform suspension, stir 2h；Step D：It is in the stainless steel cauldron of polytetrafluoroethylene (PTFE), at 180 DEG C by the liner that step C resulting solutions add 100mL 48h is kept, products therefrom is centrifuged with deionized water multiple, then dry 8h at 60 DEG C, obtains BiVO4Sample.
- A kind of 4. BiVO of ruthenium load according to claim 34The preparation method of@C composite material of core-shell structure, its feature It is, bismuth salt described in step A is Bi (NO3)3·5H2O or BiCl3。
- A kind of 5. BiVO of ruthenium load according to claim 34The preparation method of@C composite material of core-shell structure, its feature It is, vanadium-containing compound described in step A is NH4VO3Or Na3VO4。
- A kind of 6. BiVO of ruthenium load according to claim 24The preparation method of@C composite material of core-shell structure, its feature It is, in step 2 after solid matter separation, is alternately washed using deionized water, absolute ethyl alcohol, up to ruthenium load after drying BiVO4@C composite material of core-shell structure.
- A kind of 7. BiVO of ruthenium load according to claim 24The preparation method of@C composite material of core-shell structure, its feature It is, in step 2, uses deionized water washing times as 4~6 times；The drying temperature is 60~80 DEG C, drying time 6 ~12h.
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| CN103933972A (en) * | 2014-04-21 | 2014-07-23 | 国家纳米科学中心 | Method for preparing precious metal titanium dioxide core-shell structure |
| CN105332050A (en) * | 2015-11-30 | 2016-02-17 | 中国科学技术大学 | Palladium nanocrystals and synthesis method thereof |
| CN105879857A (en) * | 2016-06-08 | 2016-08-24 | 南昌航空大学 | Titanium dioxide rod catalyst doped with bismuth molybdate nanosheets |
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| CN103933972A (en) * | 2014-04-21 | 2014-07-23 | 国家纳米科学中心 | Method for preparing precious metal titanium dioxide core-shell structure |
| CN105332050A (en) * | 2015-11-30 | 2016-02-17 | 中国科学技术大学 | Palladium nanocrystals and synthesis method thereof |
| CN105879857A (en) * | 2016-06-08 | 2016-08-24 | 南昌航空大学 | Titanium dioxide rod catalyst doped with bismuth molybdate nanosheets |
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