CN105797760A - Bi2O2CO3-WO3 composite photocatalyst and preparation method thereof - Google Patents
Bi2O2CO3-WO3 composite photocatalyst and preparation method thereof Download PDFInfo
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- CN105797760A CN105797760A CN201610235977.0A CN201610235977A CN105797760A CN 105797760 A CN105797760 A CN 105797760A CN 201610235977 A CN201610235977 A CN 201610235977A CN 105797760 A CN105797760 A CN 105797760A
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- mixed solution
- bismuth nitrate
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- catalyst
- microwave
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 30
- 239000002131 composite material Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000011259 mixed solution Substances 0.000 claims abstract description 27
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 22
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 22
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims abstract description 21
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims abstract description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000011780 sodium chloride Substances 0.000 claims abstract description 11
- 239000004202 carbamide Substances 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims description 20
- 230000004044 response Effects 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 12
- 235000013877 carbamide Nutrition 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 5
- 238000001035 drying Methods 0.000 abstract 2
- 239000007864 aqueous solution Substances 0.000 abstract 1
- 238000005119 centrifugation Methods 0.000 abstract 1
- 238000006555 catalytic reaction Methods 0.000 description 5
- 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 5
- 229940043267 rhodamine b Drugs 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000969 carrier Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 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
- B01J27/232—Carbonates
-
- B01J35/39—
Abstract
The invention discloses a Bi2O2CO3-WO3 composite photocatalyst and a preparation method thereof, and belongs to the technical field of inorganic environment-friendly photocatalytic materials. According to the technical scheme, the preparation method is characterized by comprising the steps that 1, sodium tungstate and sodium chloride are added to deionized water to be prepared into a mixed solution, the pH value of the mixed solution is adjusted to range from 0.5 to 1 with hydrochloric acid, the mixed solution is transferred to a hydrothermal reaction still and placed in a microwave digester to be subjected to a microwave reaction for 10 min to 30 min at the temperature of 180 DEG C, and cooling, washing and drying are carried out to obtain WO3 powder; 2, a bismuth nitrate aqueous solution is prepared, urea and the WO3 powder are added, and a mixed solution is formed; 3, the mixed solution is stirred for 1 h at room temperature, then transferred to the hydrothermal reaction still, placed in the microwave digester to be subjected to a microwave reaction for 10 min to 30 min at the temperature of 180 DEG C to 200 DEG C, after the reaction is finished, the product is cooled to normal temperature, centrifugation, washing and drying are carried out, and the Bi2O2CO3-WO3 composite photocatalyst is prepared. By means of the prepared composite photocatalyst, the utilization rate of sunlight is effectively increased, and the photocatalytic activity of sunlight is effectively improved.
Description
Technical field
The invention belongs to inorganic environment-friendly catalysis material technical field, be specifically related to a kind of Bi2O2CO3-WO3Composite photo-catalyst and preparation method thereof.
Background technology
In recent years, utilizing the Organic substance in semi-conducting material photocatalytic oxidation degradation sewage to have become as an active research direction, people have carried out more in-depth study to the photocatalysis performance of some conductor oxidates.In numerous conductor photocatalysis materials, Bi2O2CO3Photocatalyst has catalysis activity height, good stability, low price and the premium properties such as nontoxic it is considered to be have most the catalysis material of potential using value.
But Bi2O2CO3Energy gap is 3.4eV, the most just can excite its catalysis activity.In the solar energy arriving ground, the energy of this wave band is still less than 5%, and the ratio of visible light part accounts for about the 45% of solar energy.Additionally, Bi2O2CO3Photocatalyst light induced electron and hole in photocatalytic process are easily combined, and catalytic efficiency is low.Therefore, how Bi is widened2O2CO3Photocatalyst spectral response range, improve its photo-quantum efficiency and become emphasis and the difficult point of photocatalysis disciplinary study.Research shows, WO3Energy gap be 2.77eV, be a kind of catalysis material with visible light-responded ability.But, the most still there is no pertinent literature about Bi2O2CO3-WO3The report of composite photo-catalyst.
Summary of the invention
Present invention solves the technical problem that and there is provided the Bi that a kind of Solar use efficiency rate is high and photocatalytic activity is good2O2CO3-WO3Composite photo-catalyst.
Another technical problem that the present invention solves there is provided Bi that is a kind of simple to operate and that be easily achieved2O2CO3-WO3The preparation method of composite photo-catalyst.
The present invention solves that above-mentioned technical problem adopts the following technical scheme that, a kind of Bi2O2CO3-WO3The preparation method of composite photo-catalyst, it is characterized in that comprising the following steps: sodium tungstate and sodium chloride are joined the mixed solution being made into sodium tungstate in deionized water with sodium chloride by (1) in molar ratio for 1:1, after stirring 30min, the pH value with hydrochloric acid regulation mixed solution is 0.5-1, it is transferred to hydrothermal reaction kettle after continuing stirring 30min, then hydrothermal reaction kettle is put in 180 DEG C of microwave reaction 10-30min in microwave dissolver, question response terminate after through cooling down, wash, being dried to obtain WO3Powder；(2) with bismuth nitrate and deionized water for preparation of raw material aqueous bismuth nitrate solution, under conditions of stirring, in aqueous bismuth nitrate solution, carbamide is added and WO that step (1) obtains3Powder forms mixed solution, and wherein added carbamide is 3:1 with the mol ratio of bismuth nitrate, added WO3Powder is 0.25-1:1 with the mol ratio of bismuth nitrate；(3) it is transferred to hydrothermal reaction kettle after mixed solution stirring 1h step (2) obtained under conditions of room temperature, then hydrothermal reaction kettle is put in 180-200 DEG C of microwave reaction 10-30min in microwave dissolver, question response terminate to be cooled to room temperature after through being centrifuged, washing, be dried prepare Bi2O2CO3-WO3Composite photo-catalyst.
Further preferably, in the mixed solution of step (1), the molar concentration of sodium tungstate is 0.05-0.2mol/L.
Further preferably, in the aqueous bismuth nitrate solution of step (2), the molar concentration of bismuth nitrate is 0.5-1mol/L.
Bi of the present invention2O2CO3-WO3Composite photo-catalyst, prepares according to the method described above.
The present invention compared with prior art has the advantages that
1, the present invention is in order to widen Bi2O2CO3Spectrum ring scope, by itself and the WO with ideal bandgap3It is combined mutually, utilizes the energy level difference between two kinds of quasiconductors that photogenerated carriers can be made to be injected on the energy level of another kind of quasiconductor by the energy level of a kind of semiconductive particles, thus improve the separation efficiency of photogenerated charge；
2、Bi2O2CO3Conduction band potential E of photocatalystCB=0.16eV, valence band electromotive force EVB=3.56eV, and WO3Conduction band potential E of photocatalystCB=0.41eV, valence band electromotive force EVB=3.18eV, at Bi2O2CO3-WO3In composite semiconductor, Bi2O2CO3Conduction band potential more negative, light induced electron is easily from the Bi that energy level is low2O2CO3Move to the WO that energy level is high3On conduction band, WO simultaneously3Valence band electromotive force corrigendum, photohole is easily from the WO that energy level is high3Valence band moves to the Bi that energy level is low2O2CO3In valence band, thus improve the separation efficiency of photogenerated charge, extend Bi2O2CO3Spectral response range；
3、WO3Forbidden band is narrower, can effectively expand Bi2O2CO3-WO3The composite photo-catalyst utilization rate to visible ray, and then it is effectively improved utilization rate and the photocatalytic activity of sunlight.
Accompanying drawing explanation
Fig. 1 is under the high voltage mercury lamp radiation of 300W, the Bi that the embodiment of the present invention 2 prepares2O2CO3-WO3Composite photo-catalyst and pure Bi2O2CO3Light urges the agent degraded correlation curve figure (operating condition: the amount of catalyst: 0.1g to rhodamine B；The mass concentration of rhodamine B: 5mg/L).
Detailed description of the invention
Being described in further details the foregoing of the present invention by the following examples, but this should not being interpreted as, the scope of the above-mentioned theme of the present invention is only limitted to below example, all technology realized based on foregoing of the present invention belong to the scope of the present invention.
Embodiment 1
(1) sodium tungstate of 0.005mol and the sodium chloride of 0.005mol are joined constant volume in deionized water and forms the mixed solution of sodium tungstate and sodium chloride to 100mL, after stirring 30min, the pH value with hydrochloric acid regulation mixed solution is 0.5, it is transferred to hydrothermal reaction kettle after continuing stirring 30min, then hydrothermal reaction kettle is put in 180 DEG C of microwave reaction 10min in microwave dissolver, question response terminate after through cooling down, wash, being dried to obtain WO3Powder；
(2) preparation molar concentration is the aqueous bismuth nitrate solution 100mL of 0.5mol/L, the WO that addition 0.15mol carbamide and 0.05mol step (1) obtain in aqueous bismuth nitrate solution under conditions of stirring3Powder body forms mixed solution；
(3) it is transferred to hydrothermal reaction kettle after mixed solution stirring 1h step (2) obtained under conditions of room temperature, then being put into by hydrothermal reaction kettle in 180 DEG C of microwave reaction 30min in microwave dissolver, question response has the Bi of high catalytic activity through being centrifuged, wash, be dried to obtain after terminating to be cooled to room temperature2O2CO3-WO3Composite photo-catalyst.
Embodiment 2
(1) sodium tungstate of 0.01mol and the sodium chloride of 0.01mol are joined constant volume in deionized water and forms sodium tungstate and the mixed solution of sodium chloride to 100mL, after stirring 30min, the pH value with hydrochloric acid regulation mixed solution is 0.5, it is transferred to hydrothermal reaction kettle after continuing stirring 30min, then hydrothermal reaction kettle is put in 180 DEG C of microwave reaction 20min in microwave dissolver, question response terminate after through cooling down, wash, being dried to obtain WO3Powder；
(2) preparation molar concentration is the aqueous bismuth nitrate solution 100mL of 0.75mol/L, the WO that addition 0.225mol carbamide and 0.0375mol step (1) obtain in aqueous bismuth nitrate solution under conditions of stirring3Powder body forms mixed solution；
(3) it is transferred to hydrothermal reaction kettle after mixed solution stirring 1h step (2) obtained under conditions of room temperature, then being put into by hydrothermal reaction kettle in 190 DEG C of microwave reaction 20min in microwave dissolver, question response has the Bi of high catalytic activity through being centrifuged, wash, be dried to obtain after terminating to be cooled to room temperature2O2CO3-WO3Composite photo-catalyst.
Fig. 1 is under the high voltage mercury lamp radiation of 300W, the Bi that the present embodiment prepares2O2CO3-WO3Composite photo-catalyst and pure Bi2O2CO3Light urges the agent degraded correlation curve figure to rhodamine B, as seen from the figure, at identical conditions, after illumination 80min, pure Bi2O2CO3Photocatalyst is about 82% to the degradation rate of rhodamine B, and Bi2O2CO3-WO3Composite photo-catalyst can reach about 89% to the degradation rate of rhodamine B, shows the photocatalytic activity being remarkably reinforced.
Embodiment 3
(1) sodium tungstate of 0.02mol and the sodium chloride of 0.02mol are joined constant volume in deionized water and forms sodium tungstate and the mixed solution of sodium chloride to 100mL, after stirring 30min, the pH value with hydrochloric acid regulation mixed solution is 1, it is transferred to hydrothermal reaction kettle after continuing stirring 30min, then hydrothermal reaction kettle is put in 180 DEG C of microwave reaction 30min in microwave dissolver, question response terminate after through cooling down, wash, being dried to obtain WO3Powder；
(2) preparation molar concentration is the aqueous bismuth nitrate solution 100mL of 1mol/L, the WO that addition 0.3mol carbamide and 0.025mol step (1) obtain in aqueous bismuth nitrate solution under conditions of stirring3Powder body forms mixed solution；
(3) it is transferred to hydrothermal reaction kettle after mixed solution stirring 1h step (2) obtained under conditions of room temperature, then being put into by hydrothermal reaction kettle in 200 DEG C of microwave reaction 10min in microwave dissolver, question response has the Bi of high catalytic activity through being centrifuged, wash, be dried to obtain after terminating to be cooled to room temperature2O2CO3-WO3Composite photo-catalyst.
Embodiment above describes the ultimate principle of the present invention, principal character and advantage; skilled person will appreciate that of the industry; the present invention is not restricted to the described embodiments; the principle that the present invention is simply described described in above-described embodiment and description; under the scope without departing from the principle of the invention; the present invention also has various changes and modifications, and these changes and improvements each fall within the scope of protection of the invention.
Claims (4)
1. a Bi2O2CO3-WO3The preparation method of composite photo-catalyst, it is characterized in that comprising the following steps: sodium tungstate and sodium chloride are joined the mixed solution being made into sodium tungstate in deionized water with sodium chloride by (1) in molar ratio for 1:1, after stirring 30min, the pH value with hydrochloric acid regulation mixed solution is 0.5-1, it is transferred to hydrothermal reaction kettle after continuing stirring 30min, then hydrothermal reaction kettle is put in 180 DEG C of microwave reaction 10-30min in microwave dissolver, question response terminate after through cooling down, wash, being dried to obtain WO3Powder；(2) with bismuth nitrate and deionized water for preparation of raw material aqueous bismuth nitrate solution, under conditions of stirring, in aqueous bismuth nitrate solution, carbamide is added and WO that step (1) obtains3Powder forms mixed solution, and wherein added carbamide is 3:1 with the mol ratio of bismuth nitrate, added WO3Powder is 0.25-1:1 with the mol ratio of bismuth nitrate；(3) it is transferred to hydrothermal reaction kettle after mixed solution stirring 1h step (2) obtained under conditions of room temperature, then hydrothermal reaction kettle is put in 180-200 DEG C of microwave reaction 10-30min in microwave dissolver, question response terminate to be cooled to room temperature after through being centrifuged, washing, be dried prepare Bi2O2CO3-WO3Composite photo-catalyst.
Bi the most according to claim 12O2CO3-WO3The preparation method of composite photo-catalyst, it is characterised in that: in the mixed solution of step (1), the molar concentration of sodium tungstate is 0.05-0.2mol/L.
Bi the most according to claim 12O2CO3-WO3The preparation method of composite photo-catalyst, it is characterised in that: in the aqueous bismuth nitrate solution of step (2), the molar concentration of bismuth nitrate is 0.5-1mol/L.
4. a Bi2O2CO3-WO3Composite photo-catalyst, it is characterised in that be to prepare according to the method described in any one in claim 1-3.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610235977.0A CN105797760A (en) | 2016-04-18 | 2016-04-18 | Bi2O2CO3-WO3 composite photocatalyst and preparation method thereof |
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| CN201610235977.0A CN105797760A (en) | 2016-04-18 | 2016-04-18 | Bi2O2CO3-WO3 composite photocatalyst and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108786872A (en) * | 2018-07-05 | 2018-11-13 | 河南师范大学 | A kind of flower-shaped WS2/Bi2O2CO3The synthetic method of heterojunction photocatalysis material and its application |
| CN110756206A (en) * | 2019-10-14 | 2020-02-07 | 东北大学秦皇岛分校 | WO3Modified Bi2O2CO3Preparation method and application of photocatalyst |
| CN111804295A (en) * | 2019-04-12 | 2020-10-23 | 中国科学技术大学 | Method for preparing oxygen vacancy-containing bismuth tungstate ultrathin slice, oxygen vacancy-containing bismuth tungstate ultrathin slice and application thereof |
| CN114392734A (en) * | 2021-12-29 | 2022-04-26 | 北京工业大学 | Tungsten oxide composite material and preparation method and application thereof |
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| CN103011293A (en) * | 2013-01-05 | 2013-04-03 | 吉林大学 | Synthesis method of tungsten trioxide |
| CN104772158A (en) * | 2015-03-23 | 2015-07-15 | 上海应用技术学院 | Preparation method of WO3/C3N4 mixed photocatalyst |
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2016
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| CN103011293A (en) * | 2013-01-05 | 2013-04-03 | 吉林大学 | Synthesis method of tungsten trioxide |
| CN104772158A (en) * | 2015-03-23 | 2015-07-15 | 上海应用技术学院 | Preparation method of WO3/C3N4 mixed photocatalyst |
| CN104998671A (en) * | 2015-06-03 | 2015-10-28 | 河南师范大学 | Supported Bi2O2CO3 photocatalyst and preparation method thereof |
Non-Patent Citations (1)
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| DANDAN HU等: "Super-high photocatalytic activity of Fe2O3 nanoparticles anchored on Bi2O2CO3 nanosheets with exposed {001} active facets", 《APPLIED SURFACE SCIENCE》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108786872A (en) * | 2018-07-05 | 2018-11-13 | 河南师范大学 | A kind of flower-shaped WS2/Bi2O2CO3The synthetic method of heterojunction photocatalysis material and its application |
| CN111804295A (en) * | 2019-04-12 | 2020-10-23 | 中国科学技术大学 | Method for preparing oxygen vacancy-containing bismuth tungstate ultrathin slice, oxygen vacancy-containing bismuth tungstate ultrathin slice and application thereof |
| CN110756206A (en) * | 2019-10-14 | 2020-02-07 | 东北大学秦皇岛分校 | WO3Modified Bi2O2CO3Preparation method and application of photocatalyst |
| CN110756206B (en) * | 2019-10-14 | 2022-03-11 | 东北大学秦皇岛分校 | WO3Modified Bi2O2CO3Preparation method and application of photocatalyst |
| CN114392734A (en) * | 2021-12-29 | 2022-04-26 | 北京工业大学 | Tungsten oxide composite material and preparation method and application thereof |
| CN114392734B (en) * | 2021-12-29 | 2024-01-30 | 北京工业大学 | Tungsten oxide composite material and preparation method and application thereof |
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