CN108970629A - A kind of preparation method of carbon doping BiOCl visible light responsible photocatalytic material - Google Patents
A kind of preparation method of carbon doping BiOCl visible light responsible photocatalytic material Download PDFInfo
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- CN108970629A CN108970629A CN201810799983.8A CN201810799983A CN108970629A CN 108970629 A CN108970629 A CN 108970629A CN 201810799983 A CN201810799983 A CN 201810799983A CN 108970629 A CN108970629 A CN 108970629A
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- biocl
- visible light
- carbon doping
- dusty material
- white
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- 239000000463 material Substances 0.000 title claims abstract description 65
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 title claims abstract description 62
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 32
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000000137 annealing Methods 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 7
- ZDYUUBIMAGBMPY-UHFFFAOYSA-N oxalic acid;hydrate Chemical compound O.OC(=O)C(O)=O ZDYUUBIMAGBMPY-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 238000010792 warming Methods 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 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
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 230000001376 precipitating effect Effects 0.000 claims abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 5
- 238000007146 photocatalysis Methods 0.000 abstract description 5
- 238000003786 synthesis reaction Methods 0.000 abstract description 5
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 229910052797 bismuth Inorganic materials 0.000 description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- RLXDCJUIXHSXQD-UHFFFAOYSA-N oxalic acid;hydrate Chemical compound O.OC(=O)C(O)=O.OC(=O)C(O)=O RLXDCJUIXHSXQD-UHFFFAOYSA-N 0.000 description 3
- 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 3
- 229940043267 rhodamine b Drugs 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 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 description 2
- 238000005297 material degradation process Methods 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- -1 bismuthino Chemical group 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- CREMABGTGYGIQB-UHFFFAOYSA-N carbon carbon Chemical compound C.C CREMABGTGYGIQB-UHFFFAOYSA-N 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 239000002305 electric material Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 230000004044 response Effects 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
- B01J27/22—Carbides
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Glass Compositions (AREA)
Abstract
The invention discloses a kind of preparation methods of carbon doping BiOCl visible light responsible photocatalytic material, five water bismuth nitrates and deionized water are placed in reaction vessel, concentrated nitric acid is added after being uniformly mixed, hydrochloric acid solution is added after continuing stirring to solution clear and continues to stir, it repeatedly rinses again to neutrality, takes precipitating to be placed in drying box and be dried to obtain white BiOCl dusty material；Obtained white BiOCl dusty material is placed in crucible and two oxalic acid hydrate powder are added, 280 DEG C of annealing 100min grey sheet-like morphology target product carbon doping BiOCl visible light responsible photocatalytic material produced above is warming up to the heating rate of 5 DEG C/min after mixing.Preparation process simple possible of the present invention, synthesis cycle is shorter, carbon doping BiOCl dusty material obtained is much larger than white BiOCl dusty material in the utilization rate of visible wavelength range interior focusing wave, and photocatalysis performance is further promoted, and has potential using value in terms of photoelectric material.
Description
Technical field
The invention belongs to the synthesis technical fields of visible light responsible photocatalytic material, and in particular to a kind of carbon doping BiOCl
The preparation method of visible light responsible photocatalytic material.
Background technique
China's bismuth is resourceful, and for annual output up to more than 6000 tons, bismuthino material has the crystal structure of stratiform, and bismuth atom
With special electronic structure, higher catalytic activity is often shown in light-catalyzed reaction, is become a kind of important light and is urged
Change material.BiOCl is white as a kind of important bismuth system base optic catalytic material, appearance, cannot absorb visible light, and not having can
Light-exposed response characteristic.Therefore, it is necessary to design a kind of new conjunction with visible light-responded BiOCl high efficiency photocatalysis dusty material
At method.
Summary of the invention
The technical problem to be solved by the present invention is to provide a kind of carbon that synthesis technology is simple and the period is shorter doping BiOCl can
The preparation method of light-exposed responsible photocatalytic material.
The present invention adopts the following technical scheme that solve above-mentioned technical problem, and a kind of carbon adulterates the visible light-responded light of BiOCl
The preparation method of catalysis material, it is characterised in that specific steps are as follows:
Step S1: five water bismuth nitrates and deionized water are placed in reaction vessel, and concentrated nitric acid is added after being uniformly mixed, and are continued
Hydrochloric acid solution is added after stirring to solution clear and continues to stir, then repeatedly rinses to neutrality, precipitating is taken to be placed in drying box
In be dried to obtain white BiOCl dusty material；
Step S2: the white BiOCl dusty material that step S1 is obtained is placed in crucible and is added two oxalic acid hydrate powder, mixing
280 DEG C of annealing 100min grey sheet-like morphology target product carbon produced above are warming up to the heating rate of 5 DEG C/min after uniformly
Adulterate BiOCl visible light responsible photocatalytic material.
Preferably, the molar concentration of hydrochloric acid solution described in step S1 is 6mol/L, and drying condition is 100 DEG C of dryings
150min。
Preferably, the charge ratio of five water bismuth nitrates described in step S1, deionized water, concentrated nitric acid and hydrochloric acid solution is
4.85g:186.5mL:13.5mL:10mL。
Preferably, the mass ratio that feeds intake of white BiOCl dusty material described in step S2 and two oxalic acid hydrate powder is 0.3
~0.5:1~1.5.
Preferably, the mass ratio that feeds intake of white BiOCl dusty material described in step S2 and two oxalic acid hydrate powder is
0.5:1.4。
Preparation process simple possible of the present invention, synthesis cycle is shorter, and carbon doping BiOCl dusty material obtained is in visible light
The utilization rate of wave-length coverage interior focusing wave is much larger than white BiOCl dusty material, and photocatalysis performance is further promoted, in light
There is potential using value in terms of electric material.
Detailed description of the invention
Fig. 1 is white BiOCl dusty material made from the embodiment of the present invention 1, carbon doping BiOCl dusty material and implementation
Carbon carbon made from example 2 adulterates the abosrption spectrogram of BiOCl dusty material, and as seen from the figure, carbon made from embodiment 1 adulterates BiOCl
The absorption that absorption intensity of the dusty material within the scope of 400~800nm visible light wave is apparently higher than white BiOCl dusty material is strong
Degree；
Fig. 2 is white BiOCl dusty material made from the embodiment of the present invention 1, carbon doping BiOCl dusty material and embodiment 2
The XRD diffracting spectrum of carbon obtained doping BiOCl dusty material, as seen from the figure, the XRD diffraction maximum of three kinds of materials all with standard card
Piece JCPDS No.73-2060 matches, it was demonstrated that three kinds of materials are pure phase BiOCl material；
Fig. 3 is to weigh white BiOCl dusty material made from the embodiment of the present invention 1 of 0.08g, carbon doping BiOCl powder respectively
Carbon made from material and embodiment 2 adulterates BiOCl dusty material, and (300W xenon lamp adds 420nm optical filter under visible light illumination
Simulated visible light) degradation 80mL molar concentration be 0.02mmol/L rhodamine B effect picture, as seen from the figure, made from embodiment 1
Carbon doping BiOCl dusty material degradation effect is significant, and after photocatalysis 75min, which adulterates BiOCl dusty material degradation rhodamine
B reaches 90% or so, and untreated white BiOCl dusty material rhodamine B degradation can only achieve 30% or so, and embodiment 2 is made
The carbon doping BiOCl dusty material obtained is equally than white BiOCl dusty material good degrading effect；
Fig. 4 is the SEM spectrum of the doping BiOCl dusty material of carbon made from the embodiment of the present invention 1, as seen from the figure carbon doping obtained
BiOCl dusty material is sheet-like morphology；
Fig. 5 is the SEM spectrum of the doping BiOCl dusty material of carbon made from the embodiment of the present invention 2, as seen from the figure carbon doping obtained
BiOCl dusty material is sheet-like morphology.
Specific embodiment
Above content of the invention is described in further details by the following examples, but this should not be interpreted as to this
The range for inventing above-mentioned theme is only limitted to embodiment below, and all technologies realized based on above content of the present invention belong to this hair
Bright range.
Embodiment 1
Step S1: five water bismuth nitrate of 4.85g and 186.5mL deionized water are placed in reaction vessel, are added after being uniformly mixed
Enter 13.5mL concentrated nitric acid, the hydrochloric acid solution that 10mL molar concentration is 6mol/L is added after continuing to stir to solution clear and holds
Continuous stirring, then repeatedly rinse to neutrality, it takes precipitating to be placed in drying box and obtains white BiOCl powder in 100 DEG C of dry 150min
Material；
Step S2: the white BiOCl dusty material that 0.5g step S1 is obtained is placed in crucible and bis- oxalic acid hydrate of 1.4g is added
Powder is warming up to 280 DEG C of annealing 100min after mixing with the heating rate of 5 DEG C/min and the doping of gray object product carbon is made
BiOCl dusty material.
Embodiment 2
Step S1: five water bismuth nitrate of 4.85g and 186.5mL deionized water are placed in reaction vessel, are added after being uniformly mixed
Enter 13.5mL concentrated nitric acid, the hydrochloric acid solution that 10mL molar concentration is 6mol/L is added after continuing to stir to solution clear and holds
Continuous stirring, then repeatedly rinse to neutrality, it takes precipitating to be placed in drying box and obtains white BiOCl powder in 100 DEG C of dry 150min
Material；
Step S2: the white BiOCl dusty material that 0.5g step S1 is obtained is placed in crucible and bis- oxalic acid hydrate of 1.4g is added
Powder is warming up to 280 DEG C of annealing 50min after mixing with the heating rate of 5 DEG C/min and the doping of gray object product carbon is made
BiOCl dusty material.
Embodiment 3
Bis- oxalic acid hydrate powder of 1.4g is placed in crucible, using the heating rate of 5 DEG C/min be warming up to 280 DEG C of annealing 50min as
Control, same method anneal 100min as control.It is all evaporated in crucible without powder after annealing.Prove embodiment 1 and reality
Applying BiOCl powder color in example 2 becomes grey, and not being decomposed into carbon black by oxalic acid causes, and BiOCl material itself has occurred
Variation, carbon doping cause to enter in BiOCl lattice.
Preparation process simple possible of the present invention, synthesis cycle is shorter, and carbon obtained adulterates BiOCl dusty material appearance color
Larger in the utilization rate of 400~800nm visible wavelength range interior focusing wave for grey, photocatalysis performance is better than white BiOCl
Dusty material has potential using value in terms of photoelectric material.
Embodiment above describes basic principles and main features of the invention and advantage, the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, and the above embodiments and description only describe originals of the invention
Reason, under the range for not departing from the principle of the invention, various changes and improvements may be made to the invention, these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (5)
1. a kind of preparation method of carbon doping BiOCl visible light responsible photocatalytic material, it is characterised in that specific steps are as follows:
Step S1: five water bismuth nitrates and deionized water are placed in reaction vessel, and concentrated nitric acid is added after being uniformly mixed, and are continued
Hydrochloric acid solution is added after stirring to solution clear and continues to stir, then repeatedly rinses to neutrality, precipitating is taken to be placed in drying box
In be dried to obtain white BiOCl dusty material；
Step S2: the white BiOCl dusty material that step S1 is obtained is placed in crucible and is added two oxalic acid hydrate powder, mixing
280 DEG C of annealing 100min grey sheet-like morphology target product carbon produced above are warming up to the heating rate of 5 DEG C/min after uniformly
Adulterate BiOCl visible light responsible photocatalytic material.
2. the preparation method of carbon doping BiOCl visible light responsible photocatalytic material according to claim 1, feature exist
In: the molar concentration of hydrochloric acid solution described in step S1 is 6mol/L, and drying condition is 100 DEG C of dry 150min.
3. the preparation method of carbon doping BiOCl visible light responsible photocatalytic material according to claim 1, feature exist
In the charge ratio of: five water bismuth nitrates described in step S1, deionized water, concentrated nitric acid and hydrochloric acid solution be 4.85g:186.5mL:
13.5mL:10mL。
4. the preparation method of carbon doping BiOCl visible light responsible photocatalytic material according to claim 1, feature exist
In the mass ratio that feeds intake of: white BiOCl dusty material described in step S2 and two oxalic acid hydrate powder be 0.3~0.5:1~
1.5。
5. the preparation method of carbon doping BiOCl visible light responsible photocatalytic material according to claim 1, feature exist
In: the mass ratio that feeds intake of white BiOCl dusty material described in step S2 and two oxalic acid hydrate powder is 0.5:1.4.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109550511A (en) * | 2018-12-14 | 2019-04-02 | 西安理工大学 | A kind of preparation method at carbon doping perite nanometer pollen end |
| CN109607671A (en) * | 2018-12-17 | 2019-04-12 | 河南师范大学 | A kind of preparation method of C/Bi/BiOCl tri compound catalysis material |
| CN109999783A (en) * | 2019-04-18 | 2019-07-12 | 河南师范大学 | A kind of preparation method of the grey BiOCl photocatalytic material of visible absorption enhancing |
| CN114225951A (en) * | 2021-12-09 | 2022-03-25 | 四川轻化工大学 | Surface photovoltage signal enhanced BiOCl processing method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109550511A (en) * | 2018-12-14 | 2019-04-02 | 西安理工大学 | A kind of preparation method at carbon doping perite nanometer pollen end |
| CN109607671A (en) * | 2018-12-17 | 2019-04-12 | 河南师范大学 | A kind of preparation method of C/Bi/BiOCl tri compound catalysis material |
| CN109607671B (en) * | 2018-12-17 | 2021-10-26 | 河南师范大学 | Preparation method of C/Bi/BiOCl ternary composite photocatalytic material |
| CN109999783A (en) * | 2019-04-18 | 2019-07-12 | 河南师范大学 | A kind of preparation method of the grey BiOCl photocatalytic material of visible absorption enhancing |
| CN114225951A (en) * | 2021-12-09 | 2022-03-25 | 四川轻化工大学 | Surface photovoltage signal enhanced BiOCl processing method |
| CN114225951B (en) * | 2021-12-09 | 2023-11-17 | 四川轻化工大学 | Processing method of surface photovoltage signal enhanced BiOCl |
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