CN106423286B - A kind of BiOCOOH-Bi2O2CO3Composite photo-catalyst and preparation method thereof - Google Patents
A kind of BiOCOOH-Bi2O2CO3Composite photo-catalyst and preparation method thereof Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000002131 composite material Substances 0.000 claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances 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 24
- 239000008367 deionised water Substances 0.000 claims abstract description 19
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-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 6
- 239000000725 suspension Substances 0.000 claims abstract description 6
- 239000000543 intermediate Substances 0.000 claims description 24
- 238000005406 washing Methods 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 3
- 238000003760 magnetic stirring Methods 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 abstract description 15
- 238000000034 method Methods 0.000 abstract description 13
- 230000001699 photocatalysis Effects 0.000 abstract description 13
- 238000007146 photocatalysis Methods 0.000 abstract description 11
- 238000006555 catalytic reaction Methods 0.000 abstract description 7
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 238000003756 stirring Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 8
- 229910052797 bismuth Inorganic materials 0.000 description 6
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 238000011065 in-situ storage Methods 0.000 description 4
- 230000031700 light absorption Effects 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 150000001621 bismuth Chemical class 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical group [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 2
- 229940043267 rhodamine b Drugs 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000003643 water by type Substances 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
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- -1 and illumination 6h Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001875 compounds Chemical class 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
- 238000002242 deionisation method Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000006864 oxidative decomposition reaction Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000000985 reflectance spectrum 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
- 239000006228 supernatant Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
-
- B01J35/39—
-
- 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 discloses a kind of BiOCOOH Bi2O2CO3Composite photo-catalyst and preparation method thereof belongs to photocatalysis field.It is mainly characterized by using prepared BiOCOOH photochemical catalysts being raw material, under ultraviolet light, controls light application time, can obtain the BiOCOOH Bi with high efficiency photocatalysis activity2O2CO3Composite photo-catalyst.Preparation process is：1. the preparation of BiOCOOH：Five water bismuth nitrates are first dissolved in N, in N dimethylformamides (DMF) solution, stirring is to transparent, a certain amount of deionized water is added to mix to form white suspension, it is fitted into reaction kettle and is reacted, products therefrom is centrifuged, and wash drying.2. a certain amount of prepared BiOCOOH is taken to irradiate 3~8h under ultraviolet light, product is washed several times with water and absolute ethyl alcohol, and dry, obtains BiOCOOH Bi2O2CO3Composite photo-catalyst.This method simple process and low cost is honest and clean, prepared BiOCOOH Bi2O2CO3Composite photo-catalyst has efficient visible light catalysis activity.
Description
Technical field
The invention belongs to photocatalysis technology, it is related to preparing intermediate B iOCOOH using solvent-thermal method, passes through ultraviolet lighting
It penetrates, controls light application time, converted in-situ part BiOCOOH is prepared for BiOCOOH-Bi2O2CO3Composite photo-catalyst, the photocatalysis
Agent has efficient visible light catalysis activity.
Background technology
Currently, environmental pollution is on the rise, it has also become one directly threatens human survival, the focal issue of urgent need to resolve.
Photocatalysis technology be gradually grow up the seventies from twentieth century have important application foreground in the energy and environmental area
Green technology.The technology can make the organic pollution in environment that oxidative decomposition occur, and finally be degraded to CO2, water and inorganic
The small-molecule substances such as ion, since there is no secondary pollution, palliating degradation degree is high the advantages that be considered as most potentiality to be exploited at present
Environmental pollution treatment method.
Bismuth series photocatalyst is that research hotspot, bismuth based semiconductor photochemical catalyst were lived with good photocatalysis in recent years
Property, can effectively degradable organic pollutant, development prospect be wide.Most of bismuth series photocatalyst can carry out under visible light
Light-catalyzed reaction, but a small number of bismuth series photocatalyst such as BiOCOOH greater band gaps, it is poor to visible light absorption capacity, thus can
Light-exposed lower photocatalysis performance is poor, therefore also limits the application of the bismuth system catalysis material.It is urged therefore, it is necessary to widen light bismuth system
Change the light abstraction width of material, reduce the recombination rate of bismuth system catalysis material photo-generate electron-hole, improves bismuth based semiconductor material
Catalytic activity.Wherein, semiconductors coupling is the effective means that bismuth based semiconductor catalysis material performance improves.Traditional partly leads
Bluk recombination method is compound substance will to be wanted to be mixed, deposited or in-situ preparation etc., and process is complex.The present invention utilizes
BiOCOOH's is unstable, under ultraviolet light, by controlling light application time, is by BiOCOOH converted in-situs
BiOCOOH-Bi2O2CO3Composite photo-catalyst, obtained photochemical catalyst enhance visible light absorption capacity, and photocatalytic activity is notable
It improves.Meanwhile this method is to prepare high-efficiency photocatalysis material to improve a kind of new method.
Invention content
The purpose of the present invention is to provide a kind of BiOCOOH-Bi2O2CO3Composite photo-catalyst and preparation method thereof, the party
Method is simple for process, of low cost, and the photochemical catalyst photocatalytic degradation effect of synthesis is preferable.
The present invention is provided to the BiOCOOH-Bi of degradable organic pollutant2O2CO3Composite photo-catalyst, it is characterised in that：
BiOCOOH intermediates are first prepared with solvent-thermal method, under ultraviolet light, control light application time, BiOCOOH intermediates is in situ
Partial Conversion obtains BiOCOOH-Bi2O2CO3Composite photo-catalyst includes the following steps：
(1) BiOCOOH is prepared：1~2mmol, five water bismuth nitrates are dissolved in the N,N-dimethylformamide (DMF) of 5mL
In, under magnetic stirring to clear, a certain amount of deionized water is added, 10min is mixed, forms uniform white suspension
Then liquid is transferred in stainless steel autoclaves of the 50mL containing polytetrafluoroethyllining lining, 8~16h is reacted at 100~140 DEG C, will
Products therefrom centrifuges, and after washing 3 times with deionized water and absolute ethyl alcohol respectively, and 6~12h is dried at 60 DEG C, is obtained
BiOCOOH intermediates；
(2)BiOCOOH-Bi2O2CO3Preparation：BiOCOOH intermediates prepared by step (1) are taken to be added to deionized water
In, 3~8h is irradiated under ultraviolet light, and products therefrom is centrifuged, and is washed 3 times with deionized water and absolute ethyl alcohol respectively
Afterwards, dry 6~12h at 60 DEG C, obtains BiOCOOH-Bi2O2CO3Composite photo-catalyst.
Compared with prior art, the present invention having remarkable advantage：
(1) present invention first synthesizes BiOCOOH photochemical catalyst intermediates using solvent-thermal method, under ultraviolet light, control
BiOCOOH intermediates original position Partial Conversion is obtained BiOCOOH-Bi by light application time2O2CO3Composite photo-catalyst, this method work
Skill is simple, easy to operate.
(2) BiOCOOH-Bi prepared by the present invention2O2CO3Composite photo-catalyst, compared with pure BiOCOOH, to visible light
Absorption significantly increase, it is seen that photocatalytic activity is obviously improved.
Description of the drawings
Figure 1B iOCOOH-Bi2O2CO3Composite photo-catalyst, Bi2O2CO3The X- of photochemical catalyst and intermediate B iOCOOH are penetrated
Line diffraction pattern；
Fig. 2 BiOCOOH-Bi2O2CO3Composite photo-catalyst, Bi2O2CO3The purple of photochemical catalyst and intermediate B iOCOOH
Outside-visible diffusing reflection spectrum；
Fig. 3 BiOCOOH-Bi2O2CO3Composite photo-catalyst, Bi2O2CO3The light of photochemical catalyst and intermediate B iOCOOH
Catalytic performance compares
Specific implementation mode
BiOCOOH-Bi of the present invention2O2CO3Composite photo-catalyst, using BiOCOOH as intermediate, under ultraviolet light, control
BiOCOOH intermediates original position Partial Conversion is obtained BiOCOOH-Bi by light application time processed2O2CO3Composite photo-catalyst, to visible
Light absorption enhances, and has efficient visible light catalytic performance.
A kind of BiOCOOH-Bi of the present invention2O2CO3The preparation method of composite photo-catalyst, includes the following steps：
(1) BiOCOOH is prepared：1~2mmol, five water bismuth nitrates are dissolved in the N,N-dimethylformamide (DMF) of 5mL
In, under magnetic stirring to clear, a certain amount of deionized water is added, 10min is mixed, forms uniform white suspension
Then liquid is transferred in stainless steel autoclaves of the 50mL containing polytetrafluoroethyllining lining, 8~16h is reacted at 100~140 DEG C, will
Products therefrom centrifuges, and after washing 3 times with deionized water and absolute ethyl alcohol respectively, and 6~12h is dried at 60 DEG C, is obtained
BiOCOOH intermediates；
(2)BiOCOOH-Bi2O2CO3Preparation：BiOCOOH intermediates prepared by step (1) are taken to be added to deionized water
In, 3~8h is irradiated under ultraviolet light, and products therefrom is centrifuged, and is washed 3 times with deionized water and absolute ethyl alcohol respectively
Afterwards, dry 6~12h at 60 DEG C, obtains BiOCOOH-Bi2O2CO3Composite photo-catalyst.
In order to better understand 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 party's example 1：A kind of BiOCOOH-Bi of the present invention2O2CO3The preparation method of composite photo-catalyst, including it is following
Step：
(1) BiOCOOH is prepared：Five water bismuth nitrates of 1mmol are dissolved in the n,N-Dimethylformamide of 5mL, in magnetic force
Deionized water 30mL is added down toward clear in stirring, and 10min is mixed, forms uniform white suspension, is then transferred to
In stainless steel autoclaves of the 50mL containing polytetrafluoroethyllining lining, 10h is reacted at 120 DEG C, products therefrom is centrifuged, and
After washing 3 times with deionized water and absolute ethyl alcohol respectively, dry 12h, obtains BiOCOOH intermediates at 60 DEG C；
(2)BiOCOOH-Bi2O2CO3The preparation of composite photo-catalyst：The BiOCOOH intermediates for taking step (1) to prepare
0.1g is added in 40mL deionized waters, and illumination 6h, products therefrom is centrifuged under ultraviolet lamp, and uses deionization respectively
After water and absolute ethyl alcohol wash 3 times, dry 10h, obtains BiOCOOH-Bi at 60 DEG C2O2CO3Composite photo-catalyst.
To BiOCOOH-Bi2O2CO3Composite photo-catalyst, Bi2O2CO3Photochemical catalyst and BiOCOOH intermediates carry out
X-ray diffraction characterizes, and diffraction maximum corresponds respectively to corresponding standard card, as shown in Figure 1, the results showed that utilizes institute of the present invention
The synthetic method stated successfully has obtained BiOCOOH-Bi2O2CO3Composite photo-catalyst.Utilize ultraviolet-visible diffuse reflectance spectrum pair
BiOCOOH-Bi2O2CO3Composite photo-catalyst, Bi2O2CO3The absorption feelings of photochemical catalyst and BiOCOOH intermediates to visible light
Condition is characterized, as shown in Fig. 2, BiOCOOH-Bi2O2CO3Composite photo-catalyst to the absorptance BiOCOOH of visible light among
Body significantly increases.The photocatalysis performance of photochemical catalyst is rhodamine B degradation under the radiation of visible light provided by 300W xenon lamps
For (Rhodamine B, RhB) solution come what is weighed, specific experimentation is as follows：It is a concentration of to weigh the addition of 100mg photochemical catalysts
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.BiOCOOH-
Bi2O2CO3Composite photo-catalyst, Bi2O2CO3The photocatalysis performance of photochemical catalyst and BiOCOOH intermediates as shown in figure 3,
BiOCOOH-Bi2O2CO3The photocatalysis performance of composite photo-catalyst is substantially better than Bi2O2CO3Among photochemical catalyst and BiOCOOH
Body.
Embodiment 2：A kind of BiOCOOH-Bi of the present invention2O2CO3The preparation method of composite photo-catalyst, including following step
Suddenly：
(1) BiOCOOH is prepared：Five water bismuth nitrates of 1mmol are dissolved in the n,N-Dimethylformamide of 5mL, in magnetic force
Deionized water 35mL is added down toward clear in stirring, and 10min is mixed, forms uniform white suspension, is then transferred to
In stainless steel autoclaves of the 50mL containing polytetrafluoroethyllining lining, 12h is reacted at 100 DEG C, products therefrom is centrifuged, and
After washing 3 times with deionized water and absolute ethyl alcohol respectively, dry 12h, obtains BiOCOOH intermediates at 60 DEG C；
(2)BiOCOOH-Bi2O2CO3The preparation of composite photo-catalyst：The BiOCOOH intermediates for taking step (1) to prepare
0.1g is added in 40mL deionized waters, under ultraviolet light illumination 4h, and products therefrom is centrifuged, and uses deionized water respectively
After being washed 3 times with absolute ethyl alcohol, dry 10h, obtains BiOCOOH-Bi at 60 DEG C2O2CO3Composite photo-catalyst.
Claims (3)
1. a kind of BiOCOOH-Bi2O2CO3The preparation method of composite photo-catalyst, which is characterized in that include the following steps：
(1) BiOCOOH intermediates are prepared：1~2mmol, five water bismuth nitrates are dissolved in the N,N-dimethylformamide (DMF) of 5mL
In, under magnetic stirring to clear, a certain amount of deionized water is added, 10min is mixed, forms uniform white suspension
Then liquid is transferred in stainless steel autoclaves of the 50mL containing polytetrafluoroethyllining lining, 8~16h is reacted at 100~140 DEG C, will
Products therefrom centrifuges, and after washing 3 times with deionized water and absolute ethyl alcohol respectively, and 6~12h is dried at 60 DEG C, is obtained
BiOCOOH intermediates；
(2)BiOCOOH-Bi2O2CO3Preparation：BiOCOOH intermediates prepared by step (1) are taken to be add to deionized water,
3~8h is irradiated under ultraviolet light, products therefrom is centrifuged, and after washing 3 times with deionized water and absolute ethyl alcohol respectively, 60
Dry 6~12h, obtains BiOCOOH-Bi at DEG C2O2CO3Composite photo-catalyst.
2. BiOCOOH-Bi according to claim 12O2CO3The preparation method of composite photo-catalyst, it is characterised in that step
(1) volume ratio of DMF and the deionized water of addition is 1 in:6 or 1:7.
3. a kind of BiOCOOH-Bi2O2CO3Composite photo-catalyst, it is characterised in that：The BiOCOOH-Bi2O2CO3Complex light is urged
Agent preparation method according to claim 1 or 2 is made.
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| CN107952480A (en) * | 2017-12-05 | 2018-04-24 | 江南大学 | A kind of Bi/BiOCOOH composite photo-catalysts and preparation method thereof |
| 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 |
| CN108786895B (en) * | 2018-07-06 | 2020-12-22 | 兰州大学 | BiOCOOH/g-C3N4Composite photocatalyst and preparation method and application thereof |
| CN110075892A (en) * | 2019-04-24 | 2019-08-02 | 莆田学院 | A kind of photochemical catalyst and its preparation method and application |
| CN112121866A (en) * | 2020-10-09 | 2020-12-25 | 广州大学 | Photocatalyst and preparation method thereof |
| 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 |
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| CN101817555A (en) * | 2010-03-25 | 2010-09-01 | 山东大学 | Bismuthyl carbonate micro flowery material with graded structure and preparation method thereof |
| CN102527420A (en) * | 2012-02-17 | 2012-07-04 | 重庆工商大学 | Bismuth subcarbonate photocatalyst and preparation method thereof |
| CN105481009A (en) * | 2015-12-14 | 2016-04-13 | 长沙理工大学 | Preparation method of bismuth subcarbonate nanoribbon |
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| CN101817555A (en) * | 2010-03-25 | 2010-09-01 | 山东大学 | Bismuthyl carbonate micro flowery material with graded structure and preparation method thereof |
| CN102527420A (en) * | 2012-02-17 | 2012-07-04 | 重庆工商大学 | Bismuth subcarbonate photocatalyst and preparation method thereof |
| CN105481009A (en) * | 2015-12-14 | 2016-04-13 | 长沙理工大学 | Preparation method of bismuth subcarbonate nanoribbon |
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