CN107262120A - The preparation method that a kind of BiOCl surface photovoltages signal is significantly increased - Google Patents
The preparation method that a kind of BiOCl surface photovoltages signal is significantly increased Download PDFInfo
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- CN107262120A CN107262120A CN201710562338.XA CN201710562338A CN107262120A CN 107262120 A CN107262120 A CN 107262120A CN 201710562338 A CN201710562338 A CN 201710562338A CN 107262120 A CN107262120 A CN 107262120A
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- biocl
- bismuth nitrate
- glacial acetic
- significantly increased
- acetic acid
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- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 44
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 39
- 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 35
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229920002307 Dextran Polymers 0.000 claims abstract description 27
- 229960000583 acetic acid Drugs 0.000 claims abstract description 27
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 27
- 239000000843 powder Substances 0.000 claims abstract description 13
- 238000001556 precipitation Methods 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 9
- 229920001503 Glucan Polymers 0.000 claims description 25
- 229910052797 bismuth Inorganic materials 0.000 claims description 24
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 24
- 235000011054 acetic acid Nutrition 0.000 claims description 12
- 150000001243 acetic acids Chemical class 0.000 claims description 12
- 230000001699 photocatalysis Effects 0.000 abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 14
- 239000008367 deionised water Substances 0.000 abstract description 12
- 229910021641 deionized water Inorganic materials 0.000 abstract description 12
- 238000001035 drying Methods 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 32
- 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 description 11
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 10
- 229910017604 nitric acid Inorganic materials 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- 238000005406 washing Methods 0.000 description 10
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 9
- 230000000694 effects Effects 0.000 description 9
- 150000004676 glycans Chemical class 0.000 description 8
- 238000006555 catalytic reaction Methods 0.000 description 6
- 229910000014 Bismuth subcarbonate Inorganic materials 0.000 description 5
- HFQQZARZPUDIFP-UHFFFAOYSA-M sodium;2-dodecylbenzenesulfonate Chemical compound [Na+].CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O HFQQZARZPUDIFP-UHFFFAOYSA-M 0.000 description 5
- 229910002900 Bi2MoO6 Inorganic materials 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 230000002708 enhancing effect Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 230000005284 excitation Effects 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000005685 electric field effect Effects 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000008107 benzenesulfonic acids Chemical class 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 239000002355 dual-layer Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 1
- 229940012189 methyl orange Drugs 0.000 description 1
- 238000005580 one pot reaction Methods 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 230000005855 radiation 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
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 239000003643 water by type 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
- B01J27/06—Halogens; Compounds thereof
-
- 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
- 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
Abstract
The present invention relates to technical field of material chemistry, especially field of photocatalytic material, the preparation method that specially a kind of BiOCl surface photovoltages signal is significantly increased.This method is：Bismuth nitrate is dissolved in glacial acetic acid, Dextran 200 00 is added, 10 mL KCl solution are added dropwise into bismuth nitrate glacial acetic acid dextran solution（KCl molal quantity is equal to the molal quantity of bismuth nitrate）.The precipitation of generation is transferred to hydrothermal reaction kettle hydro-thermal process, room temperature is naturally cooled to.By powder deionized water and ethanol wash, taking-up is dispersed in alcohol, and sample is obtained after drying.Prepared BiOCl sample surfaces photoelectric signal is significantly increased in 300 500 intervals after being aided in through Dextran 200 00.The present invention is easy to operate, and raw material is easy to get, is easily achieved and be safe and reliable.
Description
Technical field
The present invention relates to technical field of material chemistry, especially field of photocatalytic material, specially a kind of BiOCl surface photovoltages
The preparation method that signal is significantly increased.
Background technology
BiOCl crystal structure is PbFCl types, symmetry: D4h, space group:P4/nmm, belongs to tetragonal crystal system.BiOCl
With layer structure, combined between the BiOCl atomic layers of dual layer arrangement by Cl atoms by non-bonding force (Van der Waals force).BiOCl
Valence band is mainly that O 2p and Cl 3p are occupied, and conduction band is mainly the contribution of Bi 6p tracks.Because BiOCl belongs to indirect transition band gap,
Therefore excite electronics to have to pass through some K layers and get to valence band, this reduces the probability for exciting electronics and hole-recombination.
The open crystal structures of BiOCl and indirect transition pattern and have efficiently separating and electric charge transfer beneficial to hole-electron pair,
These features make it have relatively high photocatalytic activity.Research shows that BiOCl, which is shown, in some cases compares TiO2More preferably
Photocatalytic activity and Geng Gao stability.BiOCl relies primarily on ultraviolet excitation with a width of 3.22 eV, but visible
(nm of λ ＞ 420) BiOCl shows certain visible light catalysis activity under light irradiation, and this is mainly due to Sensitized Photo-degradation.It is full
Sufficient practical application, BiOCl photogenerated charge separation effect and photocatalytic activity await further raising.Therefore, people are to it
Do and adulterated, construct the study on the modification such as hetero-junctions.It is to improve photogenerated charge separation effect that hetero-junctions is constructed in numerous means
Should be one of with the very effective method of photocatalytic activity.
People have carried out research to BiOCl base heterojunction photocatalytic activities.Mushtaq is prepared original position with partner
Bi2O3/ BiOCl hetero-junctions, they speculate to the photogenerated charge transfer under radiation of visible light：Under visible light illumination
Bi2O3Be excited, electron transition to conduction band produces hole in valence band, due to Interface electric field effect, electronics in BiOCl valence band to
Bi2O3Valence band is shifted, so that hole is accumulated in BiOCl valence band, in Bi2O3Conduction band accumulates electronics, effectively realizes point of photogenerated charge
From.Photogenerated charge after separation induces light-catalyzed reaction, so as to improve its photocatalytic activity.Guerrero seminars are using molten
BiOCl is carried on porous TiO by glue-gel method2Surface, experimental result shows photocatalytic activity of the catalyst to rhodamine B
Enhancing.Under ultraviolet-visible light irradiation, because of the difference of its position of energy band, TiO2Electronics on conduction band is shifted to BiOCl conduction bands,
Hole in BiOCl valence band is to TiO2Valence band is shifted, and effectively realizes that photogenerated charge is separated, its photocatalytic activity is significantly improved.Good fortune
State university professor Wang Xuxu etc. is prepared for Bi using " one pot of hydro-thermal method "3O4Cl/BiOCl hetero-junctions, as a result shows Bi3O4Cl/
BiOCl hetero-junctions is than pure Bi3O4Cl and BiOCl photocatalytic activities are high, after by excited by visible light, Bi3O4Cl is excited production
Raw hole and electronics.Due to Interface electric field effect, the electronics in BiOCl valence band can move to Bi3O4Cl valence band, so as to realize
Electric charge is efficiently separated.Tsing-Hua University professor Zhu Yongfa etc. is prepared for Bi using hydro-thermal method2MoO6- BiOCl hetero-junctions, this is heterogeneous
Knot is shown than BiOCl, Bi2MoO6More excellent visible light catalysis activity.Under visible light illumination, Bi2MoO6Produce electricity
Son-hole pair, due to Bi2MoO6Conduction band of the conduction band positions than BiOCl it is more negative, Bi2MoO6Conduction band on light induced electron can be to
BiOCl conduction band transfer, so that photo-generate electron-hole is efficiently separated, the enhancing of its visible light catalysis activity.Zhejiang is pedagogical big
Learn brave wait recklessly and be prepared for flower-shaped BiOCl/ (BiO) using ion exchange and 400 DEG C of mode of heatings2CO3/Bi2O3Hetero-junctions, this three
First heterojunction photocatalysis activity is higher than BiOCl/ (BiO)2CO3 And Bi2O3/(BiO)2CO3.Under visible light illumination, absorption exists
The methyl orange on BiOCl surfaces is changed into excitation state, and the excitation state injects electronics to BiOCl conduction bands, due to BiOCl and (BiO)2CO3The difference of conduction band positions, BiOCl conduction band electrons are to (BiO)2CO3Conduction band is migrated.Work as Bi2O3After excited by visible light, conduction band
Electronics is to (BiO)2CO3Conduction band is migrated, and hole is then stayed in valence band.By the way that with upper type, electron-hole pair is effectively divided
From photocatalytic activity is significantly improved.But above method haves the shortcomings that cumbersome, poor controllability, it is badly in need of using letter
Just means improve BiOCl photogenerated charge separation effects, further to improve photocatalysis performance, to realize that industrial applications are established
Solid foundation.
The content of the invention
There is provided the preparation method that a kind of BiOCl surface photovoltages signal is significantly increased based on above technical problem by the present invention.
This method is easy to operate, and raw material is easy to get, is easily achieved and be safe and reliable；The present invention is under the auxiliary of Dextran 200 00 through hydro-thermal method
The BiOCl of preparation is compared with the BiOCl for being not added with the preparation of the assisting alcohol-hydrothermal method of Dextran 200 00, in the interval surface photoelectricity of 300-500 nm
Pressure signal is significantly increased, or even also has obvious surface photovoltage signal in visible region.
The concrete technical scheme of the present invention is as follows：
The preparation method that a kind of BiOCl surface photovoltages signal is significantly increased, is prepared from using the method comprised the following steps：
The first step：5g bismuth nitrates are dissolved in 40-60 mL glacial acetic acids, Dextran 200 00 is then added, obtains bismuth nitrate-ice second
The mol ratio of acid-dextran solution, wherein glucan and bismuth nitrate is 1-11%.
Second step：KCl solution is added dropwise into bismuth nitrate-glacial acetic acid-dextran solution, the precipitation of generation is transferred to water
Thermal response kettle, 160-180 DEG C of hydro-thermal process 24 hours, naturally cools to room temperature.
3rd step：Ethanol wash is used after sample is washed with a large amount of deionized waters again 1-2 times, powder is taken out and is dispersed in wine
In essence, 60-80 DEG C is dried to obtain sample.
Preferably, glucan selects Dextran 200 00.
The sample of hydro-thermal reaction, it is scattered with ethanol after being washed with deionized water and ethanol, then it is dried to obtain sample.Its
In, the mass concentration of ethanol is 95% or so.
The positive effect of the present invention is embodied in：
（One）This method is easy to operate, and raw material is easy to get, is easily achieved and be safe and reliable；The present invention is under glucan auxiliary through hydro-thermal
BiOCl prepared by method is compared with the BiOCl for being not added with the preparation of glucan assisting alcohol-hydrothermal method, in the interval surface photovoltages of 300-500 nm
Signal is significantly increased, or even also has obvious surface photovoltage signal in visible region.
（Two）The present invention is aided in using Dextran 200 00, and being prepared for surface photovoltage signal using hydro-thermal method significantly increases
BiOCl, prepared BiOCl shows higher photocatalytic activity.
Brief description of the drawings
Fig. 1 schemes for the XRD of the products obtained therefrom of comparative example 1
Fig. 2 is the surface photovoltage signal contrast curve map of comparative example 1 and the products obtained therefrom of embodiment 1
Fig. 3 is the surface photovoltage signal contrast curve map of comparative example 1 and the products obtained therefrom of embodiment 2
Fig. 4 is the surface photovoltage signal contrast curve map of comparative example 1 and the products obtained therefrom of embodiment 3
Fig. 5 is the surface photovoltage signal contrast curve map of comparative example 1 and the products obtained therefrom of embodiment 4
Fig. 6 is the surface photovoltage signal contrast curve map of comparative example 1 and the products obtained therefrom of embodiment 5
Fig. 7 is the surface photovoltage signal contrast curve map of comparative example 1 and the products obtained therefrom of embodiment 6
Fig. 8 is the surface photovoltage signal contrast curve map of comparative example 1 and the products obtained therefrom of embodiment 7
Fig. 9 is the surface photovoltage signal contrast curve map of comparative example 1 and the products obtained therefrom of embodiment 8
Figure 10 is the surface photovoltage signal contrast curve map of comparative example 1 and the products obtained therefrom of embodiment 9
Embodiment
The present invention is expanded on further with reference to specific embodiment and comparative example.It will be appreciated that these embodiments are only used for
Illustrate the present invention rather than limitation the scope of the present invention.It should also be understood that be, after the content of the invention lectured has been read,
Those skilled in the art can make various changes or modifications to the present invention, and these equivalent form of values equally fall within right appended by the application
Claim limited range.
Comparative example 1：
The first step, bismuth nitrate is dissolved in glacial acetic acid.Specially 5g bismuth nitrates are dissolved in 40 mL glacial acetic acids.
Second step, 10 mLKCl solution are added dropwise into bismuth nitrate-glacial acetic acid solution, and KCl molal quantity is equal to nitric acid
The molal quantity of bismuth.The precipitation of generation is transferred to 100mL hydrothermal reaction kettles, 180 DEG C of hydro-thermal process 24 hours naturally cool to room
Temperature.
3rd step, uses ethanol wash 1-2 times again after deionized water washing, powder is taken out and is dispersed in alcohol, 80 DEG C are done
It is dry to obtain sample, test surfaces photovoltage.
Fig. 1 is the XRD spectrograms that comparative example 1 obtains sample, as seen from the figure, prepared sample diffraction peak and standard card
Piece (No.06-0249) is completely the same, and this shows that sample is BiOCl, and purity is higher.
Embodiment 1：
The first step, bismuth nitrate is dissolved in glacial acetic acid.Specially 5g bismuth nitrates are dissolved in 40 mL glacial acetic acids, Portugal is added
Glycan 20000, glucan molal quantity is the 1% of bismuth nitrate.
Second step, 10 mL KCl solution are added dropwise into bismuth nitrate-glacial acetic acid solution, and KCl molal quantity is equal to nitric acid
The molal quantity of bismuth.The precipitation of generation is transferred to hydrothermal reaction kettle, 180 DEG C of hydro-thermal process 24 hours naturally cool to room temperature.
3rd step, uses ethanol wash 1-2 times again after deionized water washing, powder is taken out and is dispersed in alcohol, 80 DEG C are done
It is dry to obtain sample, test surfaces photovoltage.
Contrasted with comparative example 1, embodiment 2 adds Dextran 200 00, and glucan molal quantity is the 1% of bismuth nitrate.
Fig. 2 compares figure for the surface photovoltage signal of comparative example 1 and the products obtained therefrom of embodiment 1.As can be seen that glucan
After 20000 auxiliary hydro-thermal reactions, significantly increased in 300-400 nm interval B iOCl surface photovoltage signals.And in 400-450
Nm is interval, surface photovoltage signal enhancing, shows that visible ray can excite prepared photochemical catalyst, produces surface photovoltage letter
Number, this is conducive to improving visible light catalysis activity.
Embodiment 2：
The first step, bismuth nitrate is dissolved in glacial acetic acid.Specially 5g bismuth nitrates are dissolved in 50 mL glacial acetic acids, Portugal is added
Glycan 20000, glucan molal quantity is the 3% of bismuth nitrate.
Second step, 10 mL KCl solution are added dropwise into bismuth nitrate-glacial acetic acid solution, and KCl molal quantity is equal to nitric acid
The molal quantity of bismuth.The precipitation of generation is transferred to hydrothermal reaction kettle, 160 DEG C of hydro-thermal process 24 hours naturally cool to room temperature.
3rd step, uses ethanol wash 1-2 times again after deionized water washing, powder is taken out and is dispersed in alcohol, 60 DEG C are done
It is dry to obtain sample, test surfaces photovoltage.
Contrasted with comparative example 1, embodiment 2 adds Dextran 200 00, and glucan molal quantity is the 3% of bismuth nitrate, hydro-thermal temperature
Spend for 160 DEG C, glacial acetic acid volume is 50 mL, drying temperature is 60 DEG C.
Fig. 3 compares figure for the surface photovoltage signal of comparative example 1 and the products obtained therefrom of embodiment 2.The auxiliary water of Dextran 200 00
After thermal response, significantly increased in 300-400 nm interval B iOCl surface photovoltage signals.And, surface interval in 425-475 nm
Photoelectric signal strengthens, and shows that visible ray can excite prepared photochemical catalyst, produces surface photovoltage signal, this is conducive to
Improve visible light catalysis activity.
Embodiment 3：
The first step, bismuth nitrate is dissolved in glacial acetic acid.Specially 5g bismuth nitrates are dissolved in 60 mL glacial acetic acids, Portugal is added
Glycan 20000, glucan molal quantity is the 4% of bismuth nitrate.
Second step, 10 mLKCl solution are added dropwise into bismuth nitrate-glacial acetic acid solution, and KCl molal quantity is equal to nitric acid
The molal quantity of bismuth.The precipitation of generation is transferred to hydrothermal reaction kettle, 170 DEG C of hydro-thermal process 24 hours naturally cool to room temperature.
3rd step, uses ethanol wash 1-2 times again after deionized water washing, powder is taken out and is dispersed in alcohol, 70 DEG C are done
It is dry to obtain sample, test surfaces photovoltage.
Contrasted with comparative example 1, embodiment 3 adds Dextran 200 00, and glucan molal quantity is the 4% of bismuth nitrate, hydro-thermal temperature
Spend for 170 DEG C, glacial acetic acid volume is 60 mL, drying temperature is 70 DEG C.
Fig. 4 compares figure for the surface photovoltage signal of comparative example 1 and the products obtained therefrom of embodiment 2.Add Dextran 200 00 auxiliary
Help after hydro-thermal reaction, significantly increased in 300-400 nm interval B iOCl surface photovoltage signals.And it is interval in 425-475 nm,
Surface photovoltage signal enhancing, shows that visible ray can excite prepared photochemical catalyst, produces surface photovoltage signal.
Embodiment 4：
The first step, bismuth nitrate is dissolved in glacial acetic acid.Specially 5g bismuth nitrates are dissolved in 45 mL glacial acetic acids, Portugal is added
Glycan 20000, glucan molal quantity is the 7% of bismuth nitrate.
Second step, 10 mLKCl solution are added dropwise into bismuth nitrate-glacial acetic acid solution, and KCl molal quantity is equal to nitric acid
The molal quantity of bismuth.The precipitation of generation is transferred to hydrothermal reaction kettle, 165 DEG C of hydro-thermal process 24 hours naturally cool to room temperature.
3rd step, uses ethanol wash 1-2 times again after deionized water washing, powder is taken out and is dispersed in alcohol, 65 DEG C are done
It is dry to obtain sample, test surfaces photovoltage.
Contrasted with embodiment 1, comparative example 2 adds Dextran 200 00, and glucan molal quantity is the 7% of bismuth nitrate, hydro-thermal temperature
Spend for 165 DEG C, glacial acetic acid volume is 45 mL, drying temperature is 65 DEG C.
Fig. 5 compares figure for the surface photovoltage signal of comparative example 1 and the products obtained therefrom of embodiment 4.Add Dextran 200 00 auxiliary
Help after hydro-thermal reaction, significantly increased in 300-375 nm interval B iOCl surface photovoltage signals.
Embodiment 5
The first step, bismuth nitrate is dissolved in glacial acetic acid.Specially 5g bismuth nitrates are dissolved in 55 mL glacial acetic acids, Portugal is added
Glycan 20000, glucan molal quantity is the 9% of bismuth nitrate.
Second step, 10 mLKCl solution are added dropwise into bismuth nitrate-glacial acetic acid solution, and KCl molal quantity is equal to nitric acid
The molal quantity of bismuth.The precipitation of generation is transferred to 100 mL hydrothermal reaction kettles, 175 DEG C of hydro-thermal process 24 hours naturally cool to room
Temperature.
3rd step, uses ethanol wash 1-2 times again after deionized water washing, powder is taken out and is dispersed in alcohol, 75 DEG C are done
It is dry to obtain sample, test surfaces photovoltage.
Contrasted with comparative example 1, embodiment 5 adds Dextran 200 00, and glucan molal quantity is the 9% of bismuth nitrate, hydro-thermal temperature
Spend for 175 DEG C, glacial acetic acid volume is 55 mL, drying temperature is 75 DEG C.
Fig. 6 compares figure for the surface photovoltage signal of comparative example 1 and the products obtained therefrom of embodiment 5.Add Dextran 200 00 auxiliary
Help after hydro-thermal reaction, significantly increased in 300-375 nm interval B iOCl surface photovoltage signals.
Embodiment 6
The first step, bismuth nitrate is dissolved in glacial acetic acid.Specially 5g bismuth nitrates are dissolved in 60 mL glacial acetic acids, Portugal is added
Glycan 20000, glucan molal quantity is the 11% of bismuth nitrate.
Second step, 10 mLKCl solution are added dropwise into bismuth nitrate-glacial acetic acid solution, and KCl molal quantity is equal to nitric acid
The molal quantity of bismuth.The precipitation of generation is transferred to hydrothermal reaction kettle, 180 DEG C of hydro-thermal process 24 hours naturally cool to room temperature.
3rd step, uses ethanol wash 1-2 times again after deionized water washing, powder is taken out and is dispersed in alcohol, 80 DEG C are done
It is dry to obtain sample, test surfaces photovoltage.
Contrasted with comparative example 1, embodiment 6 adds Dextran 200 00, and glucan molal quantity is the 11% of bismuth nitrate.
Fig. 7 compares figure for the surface photovoltage signal of comparative example 1 and the products obtained therefrom of comparative example 6.Add Dextran 200 00 auxiliary
Help after hydro-thermal reaction, significantly increased in 300-450 nm interval B iOCl surface photovoltage signals, enhanced surface photovoltage has
Beneficial to raising photocatalytic activity.
Embodiment 7：
The first step, bismuth nitrate is dissolved in glacial acetic acid.Specially 5g bismuth nitrates are dissolved in 60 mL glacial acetic acids, Portugal is added
Glycan 20000, glucan molal quantity is the 13% of bismuth nitrate.
Second step, 10 mL KCl solution are added dropwise into bismuth nitrate-glacial acetic acid solution, and KCl molal quantity is equal to nitric acid
The molal quantity of bismuth.The precipitation of generation is transferred to hydrothermal reaction kettle, 180 DEG C of hydro-thermal process 24 hours naturally cool to room temperature.
3rd step, uses ethanol wash 1-2 times again after deionized water washing, powder is taken out and is dispersed in alcohol, 80 DEG C are done
It is dry to obtain sample, test surfaces photovoltage.
Contrasted with comparative example 1, embodiment 7 adds Dextran 200 00, and glucan molal quantity is the 13% of bismuth nitrate.
Fig. 8 compares figure for the surface photovoltage signal of comparative example 1 and the products obtained therefrom of embodiment 7.As can be seen that glucan
It is not bright in 300-400 nm interval B iOCl surface photovoltages signals after 20000 auxiliary hydro-thermal reactions, it is contemplated that measurement error
Significant difference is different.
Embodiment 8：
The first step, bismuth nitrate is dissolved in glacial acetic acid.Specially 5g bismuth nitrates are dissolved in 50 mL glacial acetic acids, Portugal is added
Glycan 20000, glucan molal quantity is the 0.5% of bismuth nitrate.
Second step, 10 mL KCl solution are added dropwise into bismuth nitrate-glacial acetic acid solution, and KCl molal quantity is equal to nitric acid
The molal quantity of bismuth.The precipitation of generation is transferred to hydrothermal reaction kettle, 180 DEG C of hydro-thermal process 24 hours naturally cool to room temperature.
3rd step, uses ethanol wash 1-2 times again after deionized water washing, powder is taken out and is dispersed in alcohol, 80 DEG C are done
It is dry to obtain sample, test surfaces photovoltage.
Contrasted with comparative example 1, embodiment 8 adds Dextran 200 00, and glucan molal quantity is the 0.5% of bismuth nitrate.
Fig. 9 compares figure for the surface photovoltage signal of comparative example 1 and the products obtained therefrom of embodiment 8.It can be seen that, it is contemplated that survey
Measure after error, the auxiliary hydro-thermal reaction of Dextran 200 00, it is unobvious in 300-400 nm interval B iOCl surface photovoltages signals
Difference.
Embodiment 9：
The first step, bismuth nitrate is dissolved in glacial acetic acid.Specially 5g bismuth nitrates are dissolved in 55 mL glacial acetic acids, ten are added
Dialkyl benzene sulfonic acids sodium (SDBS), SDBS molal quantitys are the 5% of bismuth nitrate.
Second step, 10 mL KCl solution are added dropwise into bismuth nitrate-glacial acetic acid solution, and KCl molal quantity is equal to nitric acid
The molal quantity of bismuth.The precipitation of generation is transferred to hydrothermal reaction kettle, 180 DEG C of hydro-thermal process 24 hours naturally cool to room temperature.
3rd step, uses ethanol wash 1-2 times again after deionized water washing, powder is taken out and is dispersed in alcohol, 80 DEG C are done
It is dry to obtain sample, test surfaces photovoltage.
Contrasted with comparative example 1, embodiment 9 adds SDBS, and SDBS molal quantitys are the 5% of bismuth nitrate.
Figure 10 compares figure for the surface photovoltage signal of comparative example 1 and the products obtained therefrom of embodiment 9.As can be seen that adding
After SDBS auxiliary hydro-thermal reactions, do not strengthen in 300-400 nm interval B iOCl surface photovoltages signals.
Example described above is only the preferred embodiment of this patent, but the protection domain of this patent is not limited thereto.
It should be pointed out that for those skilled in the art, on the premise of this patent principle is not departed from, according to this specially
The technical scheme and its inventional idea of profit, can also make some improvements and modifications, and these improvements and modifications also should be regarded as this specially
The protection domain of profit.
Claims (3)
1. the preparation method that a kind of BiOCl surface photovoltages signal is significantly increased, it is characterised in that comprise the following steps preparation and
Into：
The first step：Bismuth nitrate is dissolved in 40-60 mL glacial acetic acids, bismuth nitrate quality/glacial acetic acid volume=5g/40mL-5g/60
ML, then adds glucan, obtains bismuth nitrate-glacial acetic acid-dextran solution, and glucan is 1-11% with bismuth nitrate mol ratio；
Second step：KCl solution is added dropwise into bismuth nitrate-glacial acetic acid-dextran solution, it is anti-that the precipitation of generation is transferred into hydro-thermal
Answer kettle, 160-180 DEG C of hydro-thermal process 24 hours naturally cools to room temperature；
3rd step：Ethanol wash is used after sample is washed with deionized again 1-2 times, powder is taken out and is dispersed in alcohol, 60-
80 DEG C are dried to obtain sample.
2. the BiOCl preparation methods that surface photovoltage signal is significantly increased according to claim 1, it is characterised in that：It is described
Glucan be selected from Dextran 200 00.
3. the BiOCl preparation methods that surface photovoltage signal is significantly increased according to claim 1, it is characterised in that：Using
The BiOCl that this method is prepared is significantly increased in the interval surface photoelectric signals of 300-500 nm.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108408773A (en) * | 2018-04-04 | 2018-08-17 | 湘潭大学 | A kind of preparation method and applications of BiOCl materials |
| CN108502925A (en) * | 2018-04-11 | 2018-09-07 | 湘潭大学 | A kind of preparation method and applications of { 110 } high energy crystal face exposure BiOCl materials |
| CN108816260A (en) * | 2018-05-16 | 2018-11-16 | 四川理工学院 | Surface photovoltage signal enhancing type (BiO)2CO3Preparation method |
| CN113457698A (en) * | 2021-06-16 | 2021-10-01 | 四川轻化工大学 | Method for improving BiOCl surface photovoltage signal |
| CN114225951A (en) * | 2021-12-09 | 2022-03-25 | 四川轻化工大学 | Surface photovoltage signal enhanced BiOCl processing method |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103101974A (en) * | 2011-11-09 | 2013-05-15 | 上海纳米技术及应用国家工程研究中心有限公司 | Bismuth oxychloride powder and preparation method thereof |
| CN104069876A (en) * | 2014-06-24 | 2014-10-01 | 华中师范大学 | Ag-BiOCl compound photocatalyst prepared by depositing nanometer silver on [001] crystal face of BiOCl nanometer sheet and method |
| CN104190448A (en) * | 2014-07-29 | 2014-12-10 | 南开大学 | Preparation method and application of visible light photocatalyst, namely BiOCl nanosheets |
| CN105289680A (en) * | 2015-11-26 | 2016-02-03 | 常州大学 | Preparation method for visible-light-driven photocatalyst compositing bismuth oxychloride/silver carbonate |
| CN105396603A (en) * | 2015-12-08 | 2016-03-16 | 辽宁石油化工大学 | Bismuth oxychloride catalyst with visible light response core-shell structure and preparation method thereof |
| CN106492849A (en) * | 2016-11-03 | 2017-03-15 | 江苏大学 | A kind of preparation method of BiOCl ultrathin nanometers piece photochemical catalyst |
-
2017
- 2017-07-11 CN CN201710562338.XA patent/CN107262120B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103101974A (en) * | 2011-11-09 | 2013-05-15 | 上海纳米技术及应用国家工程研究中心有限公司 | Bismuth oxychloride powder and preparation method thereof |
| CN104069876A (en) * | 2014-06-24 | 2014-10-01 | 华中师范大学 | Ag-BiOCl compound photocatalyst prepared by depositing nanometer silver on [001] crystal face of BiOCl nanometer sheet and method |
| CN104190448A (en) * | 2014-07-29 | 2014-12-10 | 南开大学 | Preparation method and application of visible light photocatalyst, namely BiOCl nanosheets |
| CN105289680A (en) * | 2015-11-26 | 2016-02-03 | 常州大学 | Preparation method for visible-light-driven photocatalyst compositing bismuth oxychloride/silver carbonate |
| CN105396603A (en) * | 2015-12-08 | 2016-03-16 | 辽宁石油化工大学 | Bismuth oxychloride catalyst with visible light response core-shell structure and preparation method thereof |
| CN106492849A (en) * | 2016-11-03 | 2017-03-15 | 江苏大学 | A kind of preparation method of BiOCl ultrathin nanometers piece photochemical catalyst |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108408773A (en) * | 2018-04-04 | 2018-08-17 | 湘潭大学 | A kind of preparation method and applications of BiOCl materials |
| CN108408773B (en) * | 2018-04-04 | 2020-04-07 | 湘潭大学 | Preparation method and application of BiOCl material |
| CN108502925A (en) * | 2018-04-11 | 2018-09-07 | 湘潭大学 | A kind of preparation method and applications of { 110 } high energy crystal face exposure BiOCl materials |
| CN108816260A (en) * | 2018-05-16 | 2018-11-16 | 四川理工学院 | Surface photovoltage signal enhancing type (BiO)2CO3Preparation method |
| CN113457698A (en) * | 2021-06-16 | 2021-10-01 | 四川轻化工大学 | Method for improving BiOCl surface photovoltage signal |
| CN113457698B (en) * | 2021-06-16 | 2023-04-25 | 四川轻化工大学 | Method for improving BiOCl surface photovoltage signal |
| 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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