CN107952480A - A kind of Bi/BiOCOOH composite photo-catalysts and preparation method thereof - Google Patents
A kind of Bi/BiOCOOH composite photo-catalysts and preparation method thereof Download PDFInfo
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- CN107952480A CN107952480A CN201711264456.9A CN201711264456A CN107952480A CN 107952480 A CN107952480 A CN 107952480A CN 201711264456 A CN201711264456 A CN 201711264456A CN 107952480 A CN107952480 A CN 107952480A
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 41
- 239000002131 composite material Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical class CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 22
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- 229910001868 water Inorganic materials 0.000 claims abstract description 14
- 235000011187 glycerol Nutrition 0.000 claims abstract description 8
- 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 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 6
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000012046 mixed solvent Substances 0.000 claims description 13
- 239000003054 catalyst Substances 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000000839 emulsion Substances 0.000 claims description 6
- 238000002347 injection Methods 0.000 claims description 6
- 239000007924 injection Substances 0.000 claims description 6
- 238000003760 magnetic stirring Methods 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 230000001699 photocatalysis Effects 0.000 abstract description 12
- 238000000034 method Methods 0.000 abstract description 10
- 238000007146 photocatalysis Methods 0.000 abstract description 10
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 238000006555 catalytic reaction Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 4
- 239000011259 mixed solution Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 4
- 239000005864 Sulphur Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 229910052797 bismuth Inorganic materials 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- XUCNUKMRBVNAPB-UHFFFAOYSA-N fluoroethene Chemical compound FC=C XUCNUKMRBVNAPB-UHFFFAOYSA-N 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 150000001621 bismuth Chemical class 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 229910001410 inorganic ion Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 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 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/04—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing carboxylic acids or their salts
-
- 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
- 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
- B01J37/16—Reducing
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of preparation method of Bi/BiOCOOH composite photo-catalysts, belong to photocatalysis field.It is mainly characterized by by controlling thioacetamide addition, one kettle way causes BiOCOOH to realize to Bi original positions Partial Conversion, it may finally obtain Bi/BiOCOOH composite photo-catalysts, compared to pure BiOCOOH, the visible light catalysis activity of prepared Bi/BiOCOOH composite photo-catalysts, which has, to be obviously improved.Preparation process is：With special ratios configuration glycerine, deionized water and N, the mixed solution of N dimethylformamides, successively add five water bismuth nitrates and thioacetamide, after reacting a period of time at a certain temperature, products therefrom is centrifuged, collected after washing is dry, you can obtain Bi/BiOCOOH composite photo-catalysts.This method simple process and low cost is honest and clean, and a step realizes the preparation of Bi/BiOCOOH, which has higher visible light catalysis activity.
Description
Technical field
The invention belongs to the photocatalysis technology in environment functional material, relates to the use of the preparation of one step of high-temperature high-pressure reaction kettle
Bi/BiOCOOH composite photo-catalysts, by varying the amount as sulphur source, control BiOCOOH to Bi Partial Conversions, final to obtain
The Bi/BiOCOOH composite photo-catalysts with compared with high visible light catalytic activity are arrived.
Background technology
At present, environmental pollution is on the rise, and energy crisis is increasingly serious, current scientific technological advance is proposed huge
Challenge.Photocatalysis technology progressively grows up from the middle and later periods in last century, is a kind of green technology, is led in the energy and environment
There is important application prospect in domain.Photocatalysis technology can occur organic pollution present in environment and toxic heavy metal ion
Redox decomposition reaction, is finally degraded to the small-molecule substances such as carbon dioxide, water and inorganic ions, is not deposited due to environmentally protective
Secondary pollution, the palliating degradation degree that has a wide range of application is high the advantages that be considered as great exploitation potential environmental pollution treatment method.
Bismuth based semiconductor photochemical catalyst has good photocatalytic activity, can effectively degradable organic pollutant, development
Have a extensive future.Most of bismuth based semiconductor photochemical catalyst can have visible light catalysis activity by excited by visible light.BiOCOOH is
Typical bismuth series photocatalyst, has visible light photocatalysis performance, but there are particle size is big, specific surface area is small, visible ray is inhaled
The problems such as receipts are less, photo-generate electron-hole separative efficiency is relatively low, electron-hole recombination rate is high.Light can be effectively improved using metal
Raw electron-hole separative efficiency, therefore select one step of solvent-thermal method to prepare Bi/BiOCOOH composite photo-catalysts, effectively accelerate electricity
Son-hole separation, so as to improve photocatalytic activity.
The content of the invention
It is an object of the invention to provide a kind of preparation method of Bi/BiOCOOH composite photo-catalysts, the letter of this method technique
Single, of low cost, the photochemical catalyst photocatalytic degradation effect of synthesis is preferable.
The present invention is provided to the Bi/BiOCOOH composite photo-catalysts of degradable organic pollutant, it is characterised in that：With molten
Hot one step of method of agent prepares Bi/BiOCOOH composite photo-catalysts, controls reaction condition, BiOCOOH is partially converted into Bi, finally
Bi/BiOCOOH composite photo-catalysts are obtained, which gets a promotion compared with BiOCOOH visible light catalytic performances, including
Following steps：
Glycerine, deionized water and n,N-Dimethylformamide are configured to mixed solvent with certain proportion, then weighed
Five water bismuth nitrates of 2mmol are dissolved in above-mentioned in the mixed solvent, under magnetic stirring to clear, then weigh and add 0~
The sulphur source of 3mmol, is mixed 30min, forms homogeneous black emulsion, be then transferred to 50mL containing polytetrafluoroethyllining lining
In stainless steel autoclave, 10~15h is reacted at 140~160 DEG C, product is centrifuged, first with hot water injection 3 times,
After washing 5 times with deionized water and absolute ethyl alcohol respectively, dry 6~12h, obtains Bi/BiOCOOH complex lights at 60~80 DEG C
Catalyst.
Compared with prior art, the present invention there is remarkable advantage：
(1) present invention use solvent-thermal method one-step synthesis Bi/BiOCOOH composite photo-catalysts, by control BiOCOOH to
Bi Partial Conversions, in-situ reducing obtain Bi/BiOCOOH composite photo-catalysts, and this method technique is simple, and energy consumption is relatively low, easily behaviour
Make.
(2) the Bi/BiOCOOH composite photo-catalysts prepared by the present invention are separated using Bi beneficial to electron-hole, can be effective
Control electron-hole in conjunction with the composite photo-catalyst is significantly improved compared to pure BiOCOOH photocatalysis performances.
Brief description of the drawings
The X-ray diffraction style of Fig. 1 BiOCOOH and Bi/BiOCOOH composite photo-catalysts
The transmission electron micrograph of Fig. 2 Bi/BiOCOOH composite photo-catalysts
The UV-vis DRS spectrogram of Fig. 3 BiOCOOH and Bi/BiOCOOH composite photo-catalysts
The photocatalysis performance test of Fig. 4 BiOCOOH and Bi/BiOCOOH composite photo-catalysts
Embodiment
A kind of Bi/BiOCOOH composite photo-catalysts of the present invention, were reduction BiOCOOH originally by controlling the sulphur source amount of addition
To Bi Partial Conversions, the visible light catalytic performance of obtained Bi/BiOCOOH composite photo-catalysts greatly promotes.
A kind of preparation method of Bi/BiOCOOH composite photo-catalysts of the present invention, includes the following steps：
Glycerine, deionized water and n,N-Dimethylformamide are configured to mixed solvent with certain proportion, then weighed
Five water bismuth nitrates of 2mmol are dissolved in above-mentioned in the mixed solvent, under magnetic stirring to clear, then weigh and add 0~
The sulphur source of 3mmol, is mixed 30min, forms homogeneous black emulsion, be then transferred to 50mL containing polytetrafluoroethyllining lining
In stainless steel autoclave, 10~15h is reacted at 140~160 DEG C, product is centrifuged, first with hot water injection 3 times,
After washing 5 times with deionized water and absolute ethyl alcohol respectively, dry 6~12h, obtains Bi/BiOCOOH complex lights at 60~80 DEG C
Catalyst.
In order to be better understood from the present invention, with reference to the example content that the present invention is furture elucidated, but the present invention's is interior
Appearance is not limited to example given below.
Embodiment 1：A kind of preparation method of Bi/BiOCOOH composite photo-catalysts, comprises the following steps：
By glycerine, deionized water and N,N-dimethylformamide with 12:3:5 ratio is configured to mixed solvent, then
Weigh five water bismuth nitrates of 2mmol and be dissolved in above-mentioned in the mixed solvent, under magnetic stirring to clear, then weigh and add
The thioacetamide of 0.5208mmol, is mixed 30min, forms homogeneous black emulsion, is then transferred to 50mL containing poly- four
In the stainless steel autoclave of vinyl fluoride liner, 12h is reacted at 150 DEG C, product is centrifuged, first with hot water injection 3 times,
After washing 5 times with deionized water and absolute ethyl alcohol respectively, dry 12h, obtains Bi/BiOCOOH composite photocatalysts at 80 DEG C
Agent.
X-ray diffraction characterization is carried out to BiOCOOH and Bi/BiOCOOH composite photo-catalysts, diffraction maximum corresponds to respectively
In the characteristic peak of the standard card of BiOCOOH and Bi, as shown in Figure 1, the results showed that using synthetic method of the present invention into
Work(has obtained Bi/BiOCOOH composite photo-catalysts.Pattern with transmission electron microscope to Bi/BiOCOOH composite photo-catalysts
Characterized, wherein sheet is BiOCOOH photochemical catalysts, and graininess Bi, is evenly distributed on schistose surface, as shown in Figure 2.
The optical property of BiOCOOH and Bi/BiOCOOH composite photo-catalysts is tested using UV-vis DRS spectrum,
As shown in Figure 3, the results showed that the Bi/BiOCOOH composite photo-catalysts prepared using synthetic method of the present invention are to visible
The absorption of light greatly enhances.The photocatalysis performance of photochemical catalyst is the Luo Dan that degrades under the radiation of visible light provided by 300W xenon lamps
For bright B (Rhodamine B, RhB) solution come what is weighed, specific experimentation is as follows：Weighing 5mg photochemical catalysts addition concentration is
10-5In the 100mL RhB solution of mol/L, the solution prepared is placed in dark place it is dispersed with stirring 30min and reach adsorption equilibrium,
Then opening xenon source makes solution carry out light-catalyzed reaction, takes the solution of about 4mL every 10min, utilizes centrifuge point
Photochemical catalyst is separated out, takes supernatant with ultraviolet specrophotometer to measure remaining RhB absorbances in solution.Bi/BiOCOOH
The photocatalysis performance of composite photo-catalyst is as shown in figure 4, its photocatalysis performance is substantially better than the light of BiOCOOH under visible light urges
Change performance.
Embodiment 2：A kind of preparation method of Bi/BiOCOOH composite photo-catalysts, comprises the following steps：
By glycerine, deionized water and N,N-dimethylformamide with 12:3:5 ratio is configured to mixed solvent, then
Weigh five water bismuth nitrates of 2mmol and be dissolved in above-mentioned in the mixed solvent, under magnetic stirring to clear, then weigh and add
The thioacetamide of 0.7188mmol, is mixed 30min, forms homogeneous black emulsion, is then transferred to 50mL containing poly- four
In the stainless steel autoclave of vinyl fluoride liner, 15h is reacted at 140 DEG C, product is centrifuged, first with hot water injection 3 times,
After washing 5 times with deionized water and absolute ethyl alcohol respectively, dry 12h, obtains Bi/BiOCOOH composite photocatalysts at 80 DEG C
Agent.
Embodiment 3：A kind of preparation method of Bi/BiOCOOH composite photo-catalysts, comprises the following steps：
By glycerine, deionized water and N,N-dimethylformamide with 12:3:5 ratio is configured to mixed solvent, then
Weigh five water bismuth nitrates of 2mmol and be dissolved in above-mentioned in the mixed solvent, under magnetic stirring to clear, then weigh and add
The thioacetamide of 1.5369mmol, is mixed 30min, forms homogeneous black emulsion, is then transferred to 50mL containing poly- four
In the stainless steel autoclave of vinyl fluoride liner, 10h is reacted at 160 DEG C, product is centrifuged, first with hot water injection 3 times,
After washing 5 times with deionized water and absolute ethyl alcohol respectively, dry 12h, obtains Bi/BiOCOOH composite photocatalysts at 80 DEG C
Agent.
Claims (3)
1. a kind of preparation method of Bi/BiOCOOH composite photo-catalysts, it is characterised in that include the following steps：
Glycerine, deionized water and n,N-Dimethylformamide are configured to mixed solvent with certain proportion, then weigh 2mmol
Five water bismuth nitrates are dissolved in above-mentioned in the mixed solvent, under magnetic stirring to clear, then weigh and add 0~3mmol's
Thioacetamide, is mixed 30min, forms homogeneous black emulsion, be then transferred to 50mL containing polytetrafluoroethyllining lining
In stainless steel autoclave, 10~15h is reacted at 140~160 DEG C, product is centrifuged, first with hot water injection 3 times,
After washing 5 times with deionized water and absolute ethyl alcohol respectively, dry 6~12h, obtains Bi/BiOCOOH complex lights at 60~80 DEG C
Catalyst.
A kind of 2. preparation method of Bi/BiOCOOH composite photo-catalysts according to claim 1, it is characterised in that right
It is required that glycerine described in 1, deionized water and N,N-dimethylformamide are with 12:3:5 ratios are configured to mixed solvent.
3. a kind of Bi/BiOCOOH composite photo-catalysts, it is characterised in that Bi/BiOCOOH composite photo-catalysts are according to claim
Preparation method in 1~2 described in any one is made.
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| CN201711264456.9A CN107952480A (en) | 2017-12-05 | 2017-12-05 | A kind of Bi/BiOCOOH composite photo-catalysts and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110586181A (en) * | 2018-06-13 | 2019-12-20 | 南京理工大学 | HCOOBiO photocatalyst prepared by room-temperature solid-phase grinding method and method thereof |
| CN110586067A (en) * | 2019-09-20 | 2019-12-20 | 太原理工大学 | Bi/Bi2SiO5Preparation method and application of photocatalyst |
| CN114471469A (en) * | 2022-01-06 | 2022-05-13 | 河南师范大学 | Dye recovery material without secondary pollution, preparation method thereof and dye recovery method |
| CN115430462A (en) * | 2022-08-31 | 2022-12-06 | 西安建筑科技大学 | PVDF (polyvinylidene fluoride) membrane loaded Bi-based photocatalytic material as well as preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110586067A (en) * | 2019-09-20 | 2019-12-20 | 太原理工大学 | Bi/Bi2SiO5Preparation method and application of photocatalyst |
| CN110586067B (en) * | 2019-09-20 | 2022-08-05 | 太原理工大学 | Bi/Bi 2 SiO 5 Preparation method and application of photocatalyst |
| CN114471469A (en) * | 2022-01-06 | 2022-05-13 | 河南师范大学 | Dye recovery material without secondary pollution, preparation method thereof and dye recovery method |
| CN115430462A (en) * | 2022-08-31 | 2022-12-06 | 西安建筑科技大学 | PVDF (polyvinylidene fluoride) membrane loaded Bi-based photocatalytic material as well as preparation method and application thereof |
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Application publication date: 20180424 |