CN110227502A - A kind of method that one step of room temperature prepares the colored hetero-junctions of bismuthyl chloride/bismuth sulfide nano - Google Patents
A kind of method that one step of room temperature prepares the colored hetero-junctions of bismuthyl chloride/bismuth sulfide nano Download PDFInfo
- Publication number
- CN110227502A CN110227502A CN201910501138.2A CN201910501138A CN110227502A CN 110227502 A CN110227502 A CN 110227502A CN 201910501138 A CN201910501138 A CN 201910501138A CN 110227502 A CN110227502 A CN 110227502A
- Authority
- CN
- China
- Prior art keywords
- room temperature
- bismuth
- hetero
- nano flower
- biocl
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims abstract description 31
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 title claims abstract description 25
- NNLOHLDVJGPUFR-UHFFFAOYSA-L calcium;3,4,5,6-tetrahydroxy-2-oxohexanoate Chemical compound [Ca+2].OCC(O)C(O)C(O)C(=O)C([O-])=O.OCC(O)C(O)C(O)C(=O)C([O-])=O NNLOHLDVJGPUFR-UHFFFAOYSA-L 0.000 title claims abstract description 25
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 claims abstract description 68
- 239000000463 material Substances 0.000 claims abstract description 45
- 239000002057 nanoflower Substances 0.000 claims abstract description 37
- 230000001699 photocatalysis Effects 0.000 claims abstract description 29
- 238000007146 photocatalysis Methods 0.000 claims abstract description 25
- 239000002904 solvent Substances 0.000 claims abstract description 15
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 70
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 62
- 239000008367 deionised water Substances 0.000 claims description 57
- 229910021641 deionized water Inorganic materials 0.000 claims description 57
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 56
- 239000000203 mixture Substances 0.000 claims description 43
- 239000000725 suspension Substances 0.000 claims description 36
- 239000001103 potassium chloride Substances 0.000 claims description 28
- 235000011164 potassium chloride Nutrition 0.000 claims description 28
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 26
- 150000001621 bismuth Chemical class 0.000 claims description 24
- 239000000460 chlorine Substances 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 229910052797 bismuth Inorganic materials 0.000 claims description 20
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 19
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 19
- 238000013019 agitation Methods 0.000 claims description 18
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 18
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 18
- 239000006210 lotion Substances 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 18
- 239000007787 solid Substances 0.000 claims description 18
- 239000011780 sodium chloride Substances 0.000 claims description 13
- 230000015556 catabolic process Effects 0.000 claims description 9
- 238000006731 degradation reaction Methods 0.000 claims description 9
- JHXKRIRFYBPWGE-UHFFFAOYSA-K bismuth chloride Chemical compound Cl[Bi](Cl)Cl JHXKRIRFYBPWGE-UHFFFAOYSA-K 0.000 claims description 7
- 229910000380 bismuth sulfate Inorganic materials 0.000 claims description 7
- BEQZMQXCOWIHRY-UHFFFAOYSA-H dibismuth;trisulfate Chemical compound [Bi+3].[Bi+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O BEQZMQXCOWIHRY-UHFFFAOYSA-H 0.000 claims description 7
- 150000001804 chlorine Chemical class 0.000 claims description 6
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 claims description 4
- 230000003197 catalytic effect Effects 0.000 claims description 4
- 238000002604 ultrasonography Methods 0.000 claims description 3
- 239000002957 persistent organic pollutant Substances 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 16
- 238000006243 chemical reaction Methods 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 229930013930 alkaloid Natural products 0.000 abstract description 2
- 238000007086 side reaction Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 103
- 239000000047 product Substances 0.000 description 18
- 238000006555 catalytic reaction Methods 0.000 description 17
- 238000005406 washing Methods 0.000 description 17
- -1 halide salt Chemical class 0.000 description 16
- BDJYZEWQEALFKK-UHFFFAOYSA-N bismuth;hydrate Chemical compound O.[Bi] BDJYZEWQEALFKK-UHFFFAOYSA-N 0.000 description 12
- 239000002086 nanomaterial Substances 0.000 description 12
- 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 8
- 229940043267 rhodamine b Drugs 0.000 description 7
- 239000011259 mixed solution Substances 0.000 description 6
- 238000001878 scanning electron micrograph Methods 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 238000009415 formwork Methods 0.000 description 3
- 238000011031 large-scale manufacturing process Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- CJJMLLCUQDSZIZ-UHFFFAOYSA-N oxobismuth Chemical compound [Bi]=O CJJMLLCUQDSZIZ-UHFFFAOYSA-N 0.000 description 3
- 238000007704 wet chemistry method Methods 0.000 description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000007210 heterogeneous catalysis Methods 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 125000000446 sulfanediyl group Chemical group *S* 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 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—
-
- 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
-
- 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 one steps of room temperature to prepare bismuthyl chloride/bismuth sulfide nano flower hetero-junctions method.BiOCl/Bi disclosed in this invention2S3The preparation process of nano flower heterojunction photocatalysis material has following good effect: 1. prepare BiOCl/Bi with simple one-step method2S3Nano flower hetero-junctions, preparation process are simple；2. preparation process carries out at 20~35 DEG C of room temperature, it is not necessarily to high-temperature solvent thermal process, mild condition is low for equipment requirements；3. not adding the disagreeableness alkaloids of environment in reaction system and using expensive template, economy is high；4. reaction process is substantially without side reaction, BiOCl/Bi2S3Production rate be maintained at 95% or more；5. the BiOCl/Bi of preparation2S3Nano flower heterojunction material photocatalytic activity with higher, potential is larger in terms of administering or repairing ecological environment.
Description
Technical field
The present invention relates to nano material preparation and solar energy photocatalytics and catalytic organism degradation field, and in particular to one
Kind prepares novel bismuthyl chloride/bismuth sulfide nano flower heterojunction photocatalysis material method in 20~35 DEG C of conditions of room temperature in next step
And its application.
Background technique
In recent years, hetero-junctions causes the interest of relevant industries with its excellent physical property and chemical activity.Wherein, chlorine
Change oxygen bismuth/bismuth sulfide hetero-junctions since its excellent visible light catalytic performance receives everybody common concern.According to research reports, chlorine
Change oxygen bismuth/bismuth sulfide hetero-junctions visible light activity is related to its pattern, and wherein 3D structure nano is flower-shaped can more easily separated photoproduction
Its combined efficiency is effectively reduced in carrier, is greatly improved its effect in terms of photocatalysis reduces pollutant.But current chlorine
Change oxygen bismuth/bismuth sulfide nano flower heterojunction photocatalyst to mostly use through the two-step method preparation in situ for etching BiOCl nano flower.And
And the BiOCl nano flower prepared in advance, mostly use organic formwork method synthesize, template is expensive, high production cost without
Conducive to large-scale production (Catalysis Communications, 2012,23,54-57；CrystEngComm,2010,12,
3875-3881).In addition, prepare bismuthyl chloride/bismuth sulfide nano flower hetero-junctions process is related to solvent-thermal method, reaction temperature more
Height, process flow is long and complex, and the requirement to equipment is also higher, greatly limits bismuthyl chloride/bismuth sulfide nano flower hetero-junctions
The application (Applied Surface Science, 2014,290,313-319) of photochemical catalyst.Secondly, to improve hetero-junctions
Prepare yield, Many researchers during preparing bismuthyl chloride/bismuth sulfide nano and using up catalyst, using addition NaOH,
KOH、K2CO3、NH3·H2The alkaline matters such as O adjust pH, but alkali is not environment friendly type substance, have strong corrosion to equipment
Effect brings security risk (Catalysis Communications, 2012,26,204-208) to production.Therefore, ring is researched and developed
Cleaning is protected, novel bismuthyl chloride/bismuth sulfide nano of good economy performance uses up the hot spot that catalyst preparation technology has become the field.
The present invention uses a kind of simple wet chemistry method, thio with soluble bismuth salt, sodium chloride or potassium chloride and five hydrations
Sodium sulphate has prepared BiOCl/Bi as raw material, in 20~35 DEG C of conditions of room temperature in next step2S3Nano flower heterojunction structure.This
Kind one step of room temperature prepares BiOCl/Bi2S3The method of nano flower hetero-junctions has not been reported both at home and abroad.And these BiOCl/Bi2S3It receives
Popped rice hetero-junctions has preferable photocatalytic activity under visible light, and potential is huge in terms of administering or repairing ecological environment.This
The BiOCl/Bi of kind method preparation2S3Nano flower heterojunction material is at low cost, synthesis condition is mild, easy to operate, technique is simple
Single, instrument and equipment requires the features such as low, is conducive to large-scale production, has huge application value.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of simple normal temperature conditions to prepare in next step
BiOCl/Bi2S3The method of nano flower heterojunction photocatalysis material.By using soluble bismuth salt, sodium chloride or potassium chloride and five
Sodium thiosulfate is hydrated as raw material, under normal temperature conditions, a step has prepared BiOCl/Bi2S3Nano flower heterojunction photocatalysis
Material, the reaction system are neither related to hot conditions, be not related to yet complicated reaction unit and valuableness organic formwork agent and
Alkaline matter effectively reduces environmental pollution, has saved production cost, is a kind of preparation process of complete green, while again can
Maintain high product yield.The preparation method has that at low cost, reaction condition is mild, instrument and equipment requires that low, yield is high, and easily
In large-scale production many advantages, such as, have wide prospects for commercial application.
The specific technical solution of the present invention is as follows:
It is an object of the invention to overcome deficiency in the prior art, a kind of 20~35 DEG C of conditions next step of room temperature are provided
Prepare BiOCl/Bi2S3The method of nano flower heterojunction photocatalysis material, its step are as follows:
Step (1) at 20~35 DEG C of room temperature, soluble bismuth salt is dissolved in solvent a, the concentration of bismuth element is made
80mM, 5~10min of ultrasound are completely dissolved to soluble bismuth salt, obtain clear solution A；
The soluble bismuth salt is one of five nitric hydrate bismuths, bismuth sulfate or bismuth chloride or a variety of arbitrary proportions
Mixture, preferably five nitric hydrate bismuths；
The solvent a is the arbitrary proportion mixture of one or both of deionized water or ethylene glycol, preferably second
Glycol；
Step (2) at 20~35 DEG C of room temperature, soluble chlorine salt dissolving is dissolved in solvent b, the concentration of chlorate is made
400mM, 5~10min of ultrasound to soluble chlorine salt dissolving are completely dissolved, and obtain clear solution B；
The soluble chlorine salt dissolving is one of KCl or NaCl or a variety of arbitrary proportion mixtures, preferably chlorination
Potassium；
The solvent b is the arbitrary proportion mixture of one or both of deionized water or ethylene glycol, is preferably gone
Ionized water；
At 20~35 DEG C of room temperature, under agitation, B solution is added drop-wise in solution A dropwise for step (3), is formed suspended
Liquid C, wherein the atomic ratio of Cl element and Bi element is 1:1 in suspension；
Step (4) at 20~35 DEG C of room temperature, soluble hypo is dissolved in solvent c, is obtained transparent molten
Liquid D, wherein the concentration of sodium thiosulfate is 0.25~1.0mol/L；
The solvent c is the arbitrary proportion mixture of one or both of deionized water or ethylene glycol, preferably go from
Sub- water；
Step (5) after mixture C is stirred 0.5h, solution D is added dropwise thereto, obtains suspended lotion E, wherein outstanding
The atomic ratio of Bi and S is 2:1~2:4 in turbid E.
Step (6) after said mixture E is stirred 0.5h, is centrifuged, is successively washed with deionized water and dehydrated alcohol, respectively
After washing 3~4 times, products therefrom is placed in 18 in 80~100 DEG C of baking ovens~for 24 hours, obtain dry solid powder.
Compared with prior art, the advantages of the present invention are as follows:
(1) BiOCl/Bi is prepared with simple one-step method2S3Nano flower hetero-junctions, preparation process are simple；
(2) preparation process can be completed at 20~35 DEG C of room temperature, be not necessarily to solvent thermal process, reaction condition is mild, to anti-
It answers device requirement low and high income, industrially there is higher application prospect；
(3)BiOCl/Bi2S3Preparation process is simple, cleaning, pollution-free.Without expensive organic formwork agent and
Organic solvent, reaction process extremely safe green；
The present invention passes through one step of wet chemistry method under normal temperature conditions and has prepared BiOCl/Bi2S3Nano flower hetero-junctions light is urged
Change material.It can achieve following good effect: 1.BiOCl/Bi using the present invention2S3Nano flower heterojunction photocatalyst passes through one
Footwork preparation, operating procedure are simple；2. preparation process carries out at 20~35 DEG C of room temperature, it is not necessarily to high-temperature solvent thermal process, condition
Mildly, low for equipment requirements；3. the template of the disagreeableness alkaloids of environment and valuableness is not added in reaction system, it is economical
Property it is high；4. reaction process is substantially without side reaction, BiOCl/Bi2S3Production rate be maintained at 95% or more；5. the BiOCl/ of preparation
Bi2S3Nano flower heterojunction material photocatalytic activity with higher, potential is larger in terms of administering or repairing ecological environment.
Detailed description of the invention
Fig. 1 is the XRD spectrum of the flower hetero-junctions catalysis material of bismuthyl chloride/bismuth sulfide nano prepared by embodiment 1, in figure
Show that bismuthyl chloride obtained/bismuth sulfide nano flower crystallinity is preferable, the not presence of miscellaneous peak substantially mainly shows BiOCl
Diffracted signal.
Fig. 2 is BiOCl/Bi prepared by embodiment 12S3The common SEM image of catalysis material shows BiOCl/ in figure
Bi2S3The microstructure of nano material is the nano flower-like of rule, a series of and nanometer sheets that it is about 13nm that nano flower, which is by thickness,
Assemble.
Fig. 3 is BiOCl/Bi prepared by embodiment 12S3Catalysis material is under visible light to the degradation curve of rhodamine B.
It can be seen from the figure that under visible light, BiOCl/Bi2S3Obvious to the degradation effect of rhodamine B, degradation rate connects in 15min
Nearly 100%.
The BiOCl/Bi prepared with embodiment 2-122S3The degradation effect and embodiment 1 of nano flower heterojunction photocatalysis material
It is essentially identical, the degradation rate in 50min is above 90%.
Fig. 4 is BiOCl/Bi prepared by embodiment 32S3XRD spectrum in catalysis material shows BiOCl/ obtained in figure
Bi2S3Nano material crystallinity is preferable, substantially the not presence of miscellaneous peak, mainly shows the diffracted signal of BiOCl.
Fig. 5 is BiOCl/Bi prepared by embodiment 32S3The common SEM image of catalysis material shows BiOCl/ in figure
Bi2S3The microstructure of nano material is the nano flower that the nanometer sheet of rule assembles.
Fig. 6 is BiOCl/Bi prepared by embodiment 52S3The XRD spectra of catalysis material shows BiOCl/ obtained in figure
Bi2S3Nano material crystallinity is preferable, substantially the not presence of miscellaneous peak, mainly shows the diffracted signal of BiOCl.
Fig. 7 is BiOCl/Bi prepared by embodiment 52S3The common SEM image of catalysis material shows BiOCl/ in figure
Bi2S3The microstructure of nano material is the nano flower that the nanometer sheet of rule assembles.
Fig. 8 is BiOCl/Bi prepared by embodiment 72S3The XRD spectrum of catalysis material shows BiOCl/ obtained in figure
Bi2S3Nano material crystallinity is preferable, substantially the not presence of miscellaneous peak, mainly shows the diffracted signal of BiOCl.
Fig. 9 is BiOCl/Bi prepared by embodiment 72S3The common SEM image of catalysis material shows BiOCl/ in figure
Bi2S3The microstructure of nano material is the nano flower-like that the nanometer sheet of rule assembles.
Figure 10 is BiOCl/Bi prepared by embodiment 92S3The XRD spectrum of catalysis material shows BiOCl/ obtained in figure
Bi2S3Nano material crystallinity is preferable, substantially the not presence of miscellaneous peak, mainly shows the diffracted signal of BiOCl.
Figure 11 is BiOCl/Bi prepared by embodiment 92S3The common SEM image of catalysis material shows BiOCl/ in figure
Bi2S3The microstructure of nano material is the nano flower-like that the nanometer sheet of rule assembles.
Figure 12 is BiOCl/Bi prepared by embodiment 112S3The XRD spectrum of catalysis material, in figure made from display
BiOCl/Bi2S3Nano material crystallinity is preferable, substantially the not presence of miscellaneous peak, mainly shows the diffracted signal of BiOCl.
Figure 13 is BiOCl/Bi prepared by embodiment 112S3The XRD spectrum of catalysis material, in figure made from display
BiOCl/Bi2S3The common SEM image of catalysis material shows BiOCl/Bi in figure2S3The microstructure of nano material is regular
The nano flower-like that nanometer sheet assembles.
Specific embodiment
In order to make those skilled in the art better understand technical solution of the present invention, below applicant will be in conjunction with specific real
Applying example and attached drawing, the present invention is described in further detail.It should be understood that these embodiments be merely to illustrate the present invention without
For limiting the scope of the invention.In addition, it should also be understood that, after reading the content lectured of the present invention, those skilled in the art can be with
The present invention is made various changes or modifications, such equivalent forms equally fall within model defined by the application the appended claims
It encloses.
Embodiment 1
Step (1) at 20 DEG C of room temperature, five nitric hydrate bismuth of 0.97g is dissolved in ethylene glycol, the concentration of bismuth element is made
80mM, ultrasonic 5min to soluble bismuth salt are completely dissolved, and obtain clear solution A；
Step (2) at 20 DEG C of room temperature, 0.15g potassium chloride is dissolved in deionized water, the concentration of potassium chloride is made
400mM, ultrasonic 5min are completely dissolved to soluble halide salt, obtain clear solution B；
At 20 DEG C of room temperature, under agitation, B solution is added drop-wise in solution A dropwise for step (3), forms suspension C,
Wherein, the atomic ratio of Cl element and Bi element is 1:1 in suspension；
Step (4) at 20 DEG C of room temperature, 0.123g solubility hypo is dissolved in deionized water, is obtained
Clear solution D, wherein the concentration of sodium thiosulfate is 0.25mol/L；
Step (5) after mixture C is stirred 0.5h, solution D is added dropwise thereto, obtains suspended lotion E.
Step (6) after said mixture E is stirred 0.5h, is centrifuged, is successively washed with deionized water and dehydrated alcohol, respectively
After washing 3 times, products therefrom is placed in 18h in 100 DEG C of baking ovens, obtains dry solid powder.Up to BiOCl/Bi2S3Nanometer
Flower heterojunction photocatalysis material, as shown in Figure 1, Figure 2, Figure 3 shows.
Embodiment 2
Step (1) at 20 DEG C of room temperature, 0.706g bismuth sulfate is dissolved in ethylene glycol, the concentration 80mM of bismuth element is made,
Ultrasonic 5min is completely dissolved to soluble bismuth salt, obtains clear solution A；
Step (2) at 20 DEG C of room temperature, 0.15g potassium chloride is dissolved in deionized water, the concentration of potassium chloride is made
400mM, ultrasonic 7min are completely dissolved to soluble halide salt, obtain clear solution B；
At 20 DEG C of room temperature, under agitation, B solution is added drop-wise in solution A dropwise for step (3), forms suspension C,
Wherein, the atomic ratio of Cl element and Bi element is 1:1 in suspension；
Step (4) at 20 DEG C of room temperature, 0.123g solubility hypo is dissolved in deionized water, is obtained
Clear solution D, wherein the concentration of sodium thiosulfate is 0.25mol/L；
Step (5) after mixture C is stirred 0.5h, solution D is added dropwise thereto, obtains suspended lotion E.
Step (6) after said mixture E is stirred 0.5h, is centrifuged, is successively washed with deionized water and dehydrated alcohol, respectively
After washing 4 times, products therefrom is placed in 100 DEG C of baking ovens for 24 hours, dry solid powder is obtained.Up to BiOCl/Bi2S3Nanometer
Flower heterojunction photocatalysis material.
Embodiment 3
Step (1) at 20 DEG C of room temperature, 0.631g bismuth chloride is dissolved in ethylene glycol, the concentration 80mM of bismuth element is made,
Ultrasonic 5min is completely dissolved to soluble bismuth salt, obtains clear solution A；
Step (2) at 20 DEG C of room temperature, 0.15g potassium chloride is dissolved in deionized water, the concentration of potassium chloride is made
400mM, ultrasonic 8min are completely dissolved to soluble halide salt, obtain clear solution B；
At 20 DEG C of room temperature, under agitation, B solution is added drop-wise in solution A dropwise for step (3), forms suspension C,
Wherein, the atomic ratio of Cl element and Bi element is 1:1 in suspension；
Step (4) at 20 DEG C of room temperature, 0.123g solubility hypo is dissolved in deionized water, is obtained
Clear solution D, wherein the concentration of sodium thiosulfate is 0.25mol/L；
Step (5) after mixture C is stirred 0.5h, solution D is added dropwise thereto, obtains suspended lotion E.
Step (6) after said mixture E is stirred 0.5h, is centrifuged, is successively washed with deionized water and dehydrated alcohol, respectively
After washing 4 times, products therefrom is placed in 20h in 100 DEG C of baking ovens, obtains dry solid powder.Up to BiOCl/Bi2S3Nanometer
Flower heterojunction photocatalysis material, as shown in Figure 4, Figure 5.
Embodiment 4
Step (1) at 20 DEG C of room temperature, five nitric hydrate bismuth of 0.97g is dissolved in ethylene glycol, the concentration of bismuth element is made
80mM, ultrasonic 5min to soluble bismuth salt are completely dissolved, and obtain clear solution A；
Step (2) at 20 DEG C of room temperature, 0.15g potassium chloride is dissolved in deionized water, the concentration of potassium chloride is made
400mM, ultrasonic 5min are completely dissolved to soluble halide salt, obtain clear solution B；
At 20 DEG C of room temperature, under agitation, B solution is added drop-wise in solution A dropwise for step (3), forms suspension C,
Wherein, the atomic ratio of Cl element and Bi element is 1:1 in suspension；
Step (4) at 20 DEG C of room temperature, 0.492g solubility hypo is dissolved in deionized water, is obtained
Clear solution D, wherein the concentration of sodium thiosulfate is 1.0mol/L；
Step (5) after mixture C is stirred 0.5h, solution D is added dropwise thereto, obtains suspended lotion E.
Step (6) after said mixture E is stirred 0.5h, is centrifuged, is successively washed with deionized water and dehydrated alcohol, respectively
After washing 3 times, products therefrom is placed in 100 DEG C of baking ovens for 24 hours, dry solid powder is obtained.Up to BiOCl/Bi2S3Nanometer
Flower heterojunction photocatalysis material.
Embodiment 5
Step (1) at 35 DEG C of room temperature, five nitric hydrate bismuth of 0.97g is dissolved in ethylene glycol, the concentration of bismuth element is made
80mM, ultrasonic 5min to soluble bismuth salt are completely dissolved, and obtain clear solution A；
Step (2) at 35 DEG C of room temperature, 0.15g potassium chloride is dissolved in deionized water, the concentration of potassium chloride is made
400mM, ultrasonic 5min are completely dissolved to soluble halide salt, obtain clear solution B；
At 35 DEG C of room temperature, under agitation, B solution is added drop-wise in solution A dropwise for step (3), forms suspension C,
Wherein, the atomic ratio of Cl element and Bi element is 1:1 in suspension；
Step (4) at 35 DEG C of room temperature, 0.492g solubility hypo is dissolved in deionized water, is obtained
Clear solution D, wherein the concentration of sodium thiosulfate is 1.0mol/L；
Step (5) after mixture C is stirred 0.5h, solution D is added dropwise thereto, obtains suspended lotion E.
Step (6) after said mixture E is stirred 0.5h, is centrifuged, is successively washed with deionized water and dehydrated alcohol, respectively
After washing 3 times, products therefrom is placed in 18h in 100 DEG C of baking ovens, obtains dry solid powder.Up to BiOCl/Bi2S3Nanometer
Flower heterojunction photocatalysis material, as shown in Figure 6, Figure 7.
Embodiment 6
Step (1) at 35 DEG C of room temperature, five nitric hydrate bismuth of 0.97g is dissolved in ethylene glycol, the concentration of bismuth element is made
80mM, ultrasonic 5min to soluble bismuth salt are completely dissolved, and obtain clear solution A；
Step (2) at 35 DEG C of room temperature, 0.15g potassium chloride is dissolved in deionized water, the concentration of potassium chloride is made
400mM, ultrasonic 5min are completely dissolved to soluble halide salt, obtain clear solution B；
At 35 DEG C of room temperature, under agitation, B solution is added drop-wise in solution A dropwise for step (3), forms suspension C,
Wherein, the atomic ratio of Cl element and Bi element is 1:1 in suspension；
Step (4) at 35 DEG C of room temperature, 0.123g solubility hypo is dissolved in deionized water, is obtained
Clear solution D, wherein the concentration of sodium thiosulfate is 0.25mol/L；
Step (5) after mixture C is stirred 0.5h, solution D is added dropwise thereto, obtains suspended lotion E.
Step (6) after said mixture E is stirred 0.5h, is centrifuged, is successively washed with deionized water and dehydrated alcohol, respectively
After washing 3 times, products therefrom is placed in 18h in 100 DEG C of baking ovens, obtains dry solid powder.Up to BiOCl/Bi2S3Nanometer
Flower heterojunction photocatalysis material.
Embodiment 7
Step (1) at 20 DEG C of room temperature, five nitric hydrate bismuth of 0.97g is dissolved in ethylene glycol, the concentration of bismuth element is made
80mM, ultrasonic 5min to soluble bismuth salt are completely dissolved, and obtain clear solution A；
Step (2) at 20 DEG C of room temperature, 0.117g sodium chloride is dissolved in deionized water, the concentration of potassium chloride is made
400mM, ultrasonic 10min are completely dissolved to soluble halide salt, obtain clear solution B；
At 20 DEG C of room temperature, under agitation, B solution is added drop-wise in solution A dropwise for step (3), forms suspension C,
Wherein, the atomic ratio of Cl element and Bi element is 1:1 in suspension；
Step (4) at 20 DEG C of room temperature, 0.123g solubility hypo is dissolved in deionized water, is obtained
Clear solution D, wherein the concentration of sodium thiosulfate is 0.25mol/L；
Step (5) after mixture C is stirred 0.5h, solution D is added dropwise thereto, obtains suspended lotion E.
Step (6) after said mixture E is stirred 0.5h, is centrifuged, is successively washed with deionized water and dehydrated alcohol, respectively
After washing 4 times, products therefrom is placed in 100 DEG C of baking ovens for 24 hours, dry solid powder is obtained.Up to BiOCl/Bi2S3Nanometer
Flower heterojunction photocatalysis material, as shown in Figure 8, Figure 9.
Embodiment 8
Step (1) at 20 DEG C of room temperature, 706g bismuth sulfate is dissolved in ethylene glycol, the concentration 80mM of bismuth element is made, and is surpassed
Sound 5min is completely dissolved to soluble bismuth salt, obtains clear solution A；
Step (2) at 20 DEG C of room temperature, 0.117g sodium chloride is dissolved in deionized water, the concentration of potassium chloride is made
400mM, ultrasonic 10min are completely dissolved to soluble halide salt, obtain clear solution B；
At 20 DEG C of room temperature, under agitation, B solution is added drop-wise in solution A dropwise for step (3), forms suspension C,
Wherein, the atomic ratio of Cl element and Bi element is 1:1 in suspension；
Step (4) at 20 DEG C of room temperature, 0.123g solubility hypo is dissolved in deionized water, is obtained
Clear solution D, wherein the concentration of sodium thiosulfate is 0.25mol/L；
Step (5) after mixture C is stirred 0.5h, solution D is added dropwise thereto, obtains suspended lotion E.
Step (6) after said mixture E is stirred 0.5h, is centrifuged, is successively washed with deionized water and dehydrated alcohol, respectively
After washing 4 times, products therefrom is placed in 100 DEG C of baking ovens for 24 hours, dry solid powder is obtained.Up to BiOCl/Bi2S3Nanometer
Flower heterojunction photocatalysis material.
Embodiment 9
Step (1) at 20 DEG C of room temperature, 0.631g bismuth chloride is dissolved in ethylene glycol, the concentration 80mM of bismuth element is made,
Ultrasonic 5min is completely dissolved to soluble bismuth salt, obtains clear solution A；
Step (2) at 20 DEG C of room temperature, 0.117g sodium chloride is dissolved in deionized water, the concentration of potassium chloride is made
400mM, ultrasonic 10min are completely dissolved to soluble halide salt, obtain clear solution B；
At 20 DEG C of room temperature, under agitation, B solution is added drop-wise in solution A dropwise for step (3), forms suspension C,
Wherein, the atomic ratio of Cl element and Bi element is 1:1 in suspension；
Step (4) at 20 DEG C of room temperature, 0.123g solubility hypo is dissolved in deionized water, is obtained
Clear solution D, wherein the concentration of sodium thiosulfate is 0.25mol/L；
Step (5) after mixture C is stirred 0.5h, solution D is added dropwise thereto, obtains suspended lotion E.
Step (6) after said mixture E is stirred 0.5h, is centrifuged, is successively washed with deionized water and dehydrated alcohol, respectively
After washing 3 times, products therefrom is placed in 18h in 100 DEG C of baking ovens, obtains dry solid powder.Up to BiOCl/Bi2S3Nanometer
Flower heterojunction photocatalysis material, as shown in Figure 10, Figure 11.
Embodiment 10
Step (1) at 20 DEG C of room temperature, five nitric hydrate bismuth of 0.97g is dissolved in ethylene glycol, the concentration of bismuth element is made
80mM, ultrasonic 5min to soluble bismuth salt are completely dissolved, and obtain clear solution A；
Step (2) at 20 DEG C of room temperature, 0.117g sodium chloride is dissolved in deionized water, the concentration of potassium chloride is made
400mM, ultrasonic 5min are completely dissolved to soluble halide salt, obtain clear solution B；
At 20 DEG C of room temperature, under agitation, B solution is added drop-wise in solution A dropwise for step (3), forms suspension C,
Wherein, the atomic ratio of Cl element and Bi element is 1:1 in suspension；
Step (4) at 20 DEG C of room temperature, 0.492g solubility hypo is dissolved in deionized water, is obtained
Clear solution D, wherein the concentration of sodium thiosulfate is 1.0mol/L；
Step (5) after mixture C is stirred 0.5h, solution D is added dropwise thereto, obtains suspended lotion E.
Step (6) after said mixture E is stirred 0.5h, is centrifuged, is successively washed with deionized water and dehydrated alcohol, respectively
After washing 3 times, products therefrom is placed in 18h in 100 DEG C of baking ovens, obtains dry solid powder.Up to BiOCl/Bi2S3Nanometer
Flower heterojunction photocatalysis material.
Embodiment 11
Step (1) at 35 DEG C of room temperature, five nitric hydrate bismuth of 0.97g is dissolved in ethylene glycol, the concentration of bismuth element is made
80mM, ultrasonic 5min to soluble bismuth salt are completely dissolved, and obtain clear solution A；
Step (2) at 35 DEG C of room temperature, 0.117g sodium chloride is dissolved in deionized water, the concentration of potassium chloride is made
400mM, ultrasonic 10min are completely dissolved to soluble halide salt, obtain clear solution B；
At 35 DEG C of room temperature, under agitation, B solution is added drop-wise in solution A dropwise for step (3), forms suspension C,
Wherein, the atomic ratio of Cl element and Bi element is 1:1 in suspension；
Step (4) at 35 DEG C of room temperature, 0.123g solubility hypo is dissolved in deionized water, is obtained
Clear solution D, wherein the concentration of sodium thiosulfate is 0.25mol/L；
Step (5) after mixture C is stirred 0.5h, solution D is added dropwise thereto, obtains suspended lotion E.
Step (6) after said mixture E is stirred 0.5h, is centrifuged, is successively washed with deionized water and dehydrated alcohol, respectively
After washing 4 times, products therefrom is placed in 18h in 100 DEG C of baking ovens, obtains dry solid powder.Up to BiOCl/Bi2S3Nanometer
Flower heterojunction photocatalysis material, as shown in Figure 12 and Figure 13.
Embodiment 12
Step (1) at 35 DEG C of room temperature, five nitric hydrate bismuth of 0.97g is dissolved in ethylene glycol, the concentration of bismuth element is made
80mM, ultrasonic 5min to soluble bismuth salt are completely dissolved, and obtain clear solution A；
Step (2) at 35 DEG C of room temperature, 0.117g sodium chloride is dissolved in deionized water, the concentration of potassium chloride is made
400mM, ultrasonic 5min are completely dissolved to soluble halide salt, obtain clear solution B；
At 35 DEG C of room temperature, under agitation, B solution is added drop-wise in solution A dropwise for step (3), forms suspension C,
Wherein, the atomic ratio of Cl element and Bi element is 1:1 in suspension；
Step (4) at 35 DEG C of room temperature, 0.492g solubility hypo is dissolved in deionized water, is obtained
Clear solution D, wherein the concentration of sodium thiosulfate is 1.0mol/L；
Step (5) after mixture C is stirred 0.5h, solution D is added dropwise thereto, obtains suspended lotion E.
Step (6) after said mixture E is stirred 0.5h, is centrifuged, is successively washed with deionized water and dehydrated alcohol, respectively
After washing 3 times, products therefrom is placed in 20h in 100 DEG C of baking ovens, obtains dry solid powder.Up to BiOCl/Bi2S3Nanometer
Flower heterojunction photocatalysis material.
Embodiment 13
Step (1) at 20 DEG C of room temperature, five nitric hydrate bismuth of 0.97g is dissolved in ethylene glycol, the concentration of bismuth element is made
80mM, ultrasonic 5min to soluble bismuth salt are completely dissolved, and obtain clear solution A；
Step (2) at 20 DEG C of room temperature, 0.15g potassium chloride is dissolved in deionized water, the concentration of potassium chloride is made
400mM, ultrasonic 10min are completely dissolved to soluble halide salt, obtain clear solution B；
At 20 DEG C of room temperature, under agitation, B solution is added drop-wise in solution A dropwise for step (3), forms suspension C,
Wherein, the atomic ratio of Cl element and Bi element is 1:1 in suspension；
Step (4) at 20 DEG C of room temperature, 0.123g solubility hypo is dissolved in deionized water, is obtained
Clear solution D, wherein the concentration of sodium thiosulfate is 0.25mol/L；
Step (5) after mixture C is stirred 0.5h, solution D is added dropwise thereto, obtains suspended lotion E.
Step (6) after said mixture E is stirred 0.5h, is centrifuged, is successively washed with deionized water and dehydrated alcohol, respectively
After washing 4 times, products therefrom is placed in 18h in 100 DEG C of baking ovens, obtains dry solid powder.Up to BiOCl/Bi2S3Nanometer
Flower heterojunction photocatalysis material.
Embodiment 14
Step (1), at 25 DEG C of room temperature, by five nitric hydrate bismuth of 0.485g, 0.1765g bismuth sulfate, 0.15775g bismuth chloride
It is dissolved in the mixed solution of water and ethylene glycol 1:1, keeps the concentration 80mM, ultrasonic 5min of bismuth element complete to soluble bismuth salt
Dissolution, obtains clear solution A；
0.075g potassium chloride and 0.0585g sodium chloride at 25 DEG C of room temperature, are dissolved in deionized water and second two by step (2)
In the mixed solution of alcohol 1:1, it is completely dissolved the concentration 400mM, ultrasonic 5min of chloride ion to soluble halide salt, obtains transparent
Solution B；
At 25 DEG C of room temperature, under agitation, B solution is added drop-wise in solution A dropwise for step (3), forms suspension C,
Wherein, the atomic ratio of Cl element and Bi element is 1:1 in suspension；
Step (4) at 25 DEG C of room temperature, 0.123g solubility hypo is dissolved in deionized water, is obtained
Clear solution D, wherein the concentration of sodium thiosulfate is 0.25mol/L；
Step (5) after mixture C is stirred 0.5h, solution D is added dropwise thereto, obtains suspended lotion E.
Step (6) after said mixture E is stirred 0.5h, is centrifuged, is successively washed with deionized water and dehydrated alcohol, respectively
After washing 4 times, products therefrom is placed in 100 DEG C of baking ovens for 24 hours, dry solid powder is obtained.Up to BiOCl/Bi2S3Nanometer
Flower heterojunction photocatalysis material.
Embodiment 15
Step (1), at 25 DEG C of room temperature, by five nitric hydrate bismuth of 0.2425g, 0.353g bismuth sulfate, 0.15775g bismuth chloride
It is dissolved in the mixed solution of water and ethylene glycol 1:1, keeps the concentration 80mM, ultrasonic 5min of bismuth element complete to soluble bismuth salt
Dissolution, obtains clear solution A；
0.075g potassium chloride and 0.0585g sodium chloride at 25 DEG C of room temperature, are dissolved in deionized water and second two by step (2)
In the mixed solution of alcohol 2:1, it is completely dissolved the concentration 400mM, ultrasonic 5min of chloride ion to soluble halide salt, obtains transparent
Solution B；
At 25 DEG C of room temperature, under agitation, B solution is added drop-wise in solution A dropwise for step (3), forms suspension C,
Wherein, the atomic ratio of Cl element and Bi element is 1:1 in suspension；
Step (4) at 25 DEG C of room temperature, 0.123g solubility hypo is dissolved in deionized water, is obtained
Clear solution D, wherein the concentration of sodium thiosulfate is 0.25mol/L；
Step (5) after mixture C is stirred 0.5h, solution D is added dropwise thereto, obtains suspended lotion E.
Step (6) after said mixture E is stirred 0.5h, is centrifuged, is successively washed with deionized water and dehydrated alcohol, respectively
After washing 3 times, products therefrom is placed in 100 DEG C of baking ovens for 24 hours, dry solid powder is obtained.Up to BiOCl/Bi2S3Nanometer
Flower heterojunction photocatalysis material.
Embodiment 16
Step (1), at 25 DEG C of room temperature, by five nitric hydrate bismuth of 0.2425g, 0.353g bismuth sulfate, 0.15775g bismuth chloride
It is dissolved in the mixed solution of water and ethylene glycol 1:1, keeps the concentration 80mM, ultrasonic 5min of bismuth element complete to soluble bismuth salt
Dissolution, obtains clear solution A；
0.0375g potassium chloride and 0.08775g sodium chloride at 25 DEG C of room temperature, are dissolved in deionized water and second by step (2)
In the mixed solution of glycol 1:1, it is completely dissolved the concentration 400mM, ultrasonic 10min of chloride ion to soluble halide salt, obtains
Clear solution B；
At 25 DEG C of room temperature, under agitation, B solution is added drop-wise in solution A dropwise for step (3), forms suspension C,
Wherein, the atomic ratio of Cl element and Bi element is 1:1 in suspension；
Step (4) at 25 DEG C of room temperature, 0.123g solubility hypo is dissolved in deionized water, is obtained
Clear solution D, wherein the concentration of sodium thiosulfate is 0.25mol/L；
Step (5) after mixture C is stirred 0.5h, solution D is added dropwise thereto, obtains suspended lotion E.
Step (6) after said mixture E is stirred 0.5h, is centrifuged, is successively washed with deionized water and dehydrated alcohol, respectively
After washing 4 times, products therefrom is placed in 100 DEG C of baking ovens for 24 hours, dry solid powder is obtained.Up to BiOCl/Bi2S3Nanometer
Flower heterojunction photocatalysis material.
Embodiment 17:
Under the conditions of 20~35 DEG C of room temperature a kind of, by one step of wet chemistry method prepare bismuthyl chloride/bismuth sulfide nano spend it is heterogeneous
Catalysis material is tied, catalytic degradation rhodamine B is used for:
Bismuthyl chloride prepared by 15mg embodiment 1-12/bismuth sulfide nano flower heterojunction photocatalysis material is accurately weighed respectively
Material is added in the aqueous solution for the rhodamine B that 50mL concentration is 15mg/L, stirring 1h is protected from light after ultrasonic 10min, so as to rhodamine B
Reach adsorption-desorption balance on the surface of catalysis material, is then simulated after the optical filtering of 400nm optical filter with 300W mercury lamp visible
Light irradiation, carries out photocatalytic degradation experiment, the 2mL of interval sampling at regular intervals, be centrifugated out after catalyst upper layer is clear
Liquid is analyzed at 553nm with concentration of the ultraviolet-uisible spectrophotometer to supernatant liquor.Luo Dan in photocatalytic degradation experiment
The degradation rate of bright B=(concentration of initial rhodamine B-residual rhodamine B concentration) × 100%/initial rhodamine B concentration.
As a result see Fig. 3 and its Detailed description of the invention.
Above-described embodiment is not for limitation of the invention, and the present invention is not limited only to above-described embodiment, as long as meeting
The present invention claims all belong to the scope of protection of the present invention.
Claims (10)
1. a kind of one step of room temperature prepares bismuthyl chloride/bismuth sulfide nano flower hetero-junctions method, it is characterised in that: this method is specific
Steps are as follows:
Step (1) at 20~35 DEG C of room temperature, soluble bismuth salt is dissolved in solvent a, the concentration 80mM of bismuth element is made, and is surpassed
5~10min of sound is completely dissolved to soluble bismuth salt, obtains clear solution A；
Step (2) at 20~35 DEG C of room temperature, soluble chlorine salt dissolving is dissolved in solvent b, the concentration 400mM of chlorate is made,
5~10min of ultrasound is completely dissolved to soluble chlorine salt dissolving, obtains clear solution B；
At 20~35 DEG C of room temperature, under agitation, B solution is added drop-wise in solution A dropwise for step (3), forms suspension C；
Step (4) at 20~35 DEG C of room temperature, soluble hypo is dissolved in solvent c, clear solution D is obtained；
Step (5) after mixture C is stirred 0.5h, solution D is added dropwise thereto, obtains suspended lotion E；
Step (6) after said mixture E is stirred 0.5h, is centrifuged, is successively washed with deionized water and dehydrated alcohol, respectively wash 3
After~4 times, products therefrom is placed in 18 in 80~100 DEG C of baking ovens~for 24 hours, obtain dry solid powder.
2. a kind of one step of room temperature as described in claim 1 prepares bismuthyl chloride/bismuth sulfide nano flower hetero-junctions method, special
Sign is: soluble bismuth salt described in step (1) is one of five nitric hydrate bismuths, bismuth sulfate and bismuth chloride or a variety of timess
Meaning scalemic thereof.
3. a kind of one step of room temperature as described in claim 1 prepares bismuthyl chloride/bismuth sulfide nano flower hetero-junctions method, special
Sign is that solvent a described in step (1) is deionized water and/or ethylene glycol.
4. a kind of one step of room temperature as described in claim 1 prepares bismuthyl chloride/bismuth sulfide nano flower hetero-junctions method, special
Sign be soluble chlorine salt dissolving described in step (2) be one of KCl or NaCl or a variety of arbitrary proportion mixtures, preferably
Potassium chloride；
5. a kind of one step of room temperature as described in claim 1 prepares bismuthyl chloride/bismuth sulfide nano flower hetero-junctions method, special
Sign is that solvent b described in step (2) is deionized water and/or ethylene glycol.
6. a kind of one step of room temperature as described in claim 1 prepares bismuthyl chloride/bismuth sulfide nano flower hetero-junctions method, special
Sign is step (3), wherein the atomic ratio of Cl element and Bi element is 1:1 in suspension C.
7. a kind of one step of room temperature as described in claim 1 prepares bismuthyl chloride/bismuth sulfide nano flower hetero-junctions method, special
Sign is step (4), wherein the concentration of sodium thiosulfate is 0.25~1.0mol/L.
8. a kind of one step of room temperature as described in claim 1 prepares bismuthyl chloride/bismuth sulfide nano flower hetero-junctions method, special
Sign is that solvent c described in step (4) is the arbitrary proportion mixture of one or both of deionized water or ethylene glycol, excellent
Select deionized water；
9. a kind of one step of room temperature as described in claim 1 prepares bismuthyl chloride/bismuth sulfide nano flower hetero-junctions method, special
Sign is step (5), wherein the atomic ratio of Bi and S is 2:1~2:4 in suspension E.
10. one step of a kind of room temperature as described in any in claim 1-10 prepares bismuthyl chloride/bismuth sulfide nano flower hetero-junctions
Method, it is characterised in that: BiOCl/Bi obtained2S3Nano flower heterojunction photocatalysis material is under visible light source or sunlight
The application of catalytic degradation organic pollutant.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910501138.2A CN110227502A (en) | 2019-06-11 | 2019-06-11 | A kind of method that one step of room temperature prepares the colored hetero-junctions of bismuthyl chloride/bismuth sulfide nano |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910501138.2A CN110227502A (en) | 2019-06-11 | 2019-06-11 | A kind of method that one step of room temperature prepares the colored hetero-junctions of bismuthyl chloride/bismuth sulfide nano |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110227502A true CN110227502A (en) | 2019-09-13 |
Family
ID=67858796
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910501138.2A Pending CN110227502A (en) | 2019-06-11 | 2019-06-11 | A kind of method that one step of room temperature prepares the colored hetero-junctions of bismuthyl chloride/bismuth sulfide nano |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110227502A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110882705A (en) * | 2019-12-10 | 2020-03-17 | 武汉纺织大学 | Microwave synthesis oxygen vacancy BiOCl/Bi2S3Catalyst and preparation method and application thereof |
| CN111533168A (en) * | 2020-04-26 | 2020-08-14 | 昆明理工大学 | Preparation method of bismuth sulfur chlorine particles |
| CN112891536A (en) * | 2021-02-04 | 2021-06-04 | 中国科学院宁波材料技术与工程研究所 | Bismuth-based nano heterojunction material and preparation method and application thereof |
| CN113772725A (en) * | 2020-06-10 | 2021-12-10 | 中国科学院宁波工业技术研究院慈溪生物医学工程研究所 | Bismuth-based semiconductor nano composite material, preparation method and application |
| CN114400263A (en) * | 2021-12-16 | 2022-04-26 | 内蒙古鄂尔多斯电力冶金集团股份有限公司 | Preparation method and application of substrate-loaded bismuth oxyhalide/bismuth sulfide nanosheet heterojunction device |
| CN115006546A (en) * | 2022-03-16 | 2022-09-06 | 四川大学 | Disulfide heterojunction material for promoting wound healing and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107803210A (en) * | 2016-09-08 | 2018-03-16 | 南京理工大学 | One-step method prepares the excellent Bi of photocatalysis performance2S3The method of/BiOCl hetero-junctions |
| CN110882705A (en) * | 2019-12-10 | 2020-03-17 | 武汉纺织大学 | Microwave synthesis oxygen vacancy BiOCl/Bi2S3Catalyst and preparation method and application thereof |
-
2019
- 2019-06-11 CN CN201910501138.2A patent/CN110227502A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107803210A (en) * | 2016-09-08 | 2018-03-16 | 南京理工大学 | One-step method prepares the excellent Bi of photocatalysis performance2S3The method of/BiOCl hetero-junctions |
| CN110882705A (en) * | 2019-12-10 | 2020-03-17 | 武汉纺织大学 | Microwave synthesis oxygen vacancy BiOCl/Bi2S3Catalyst and preparation method and application thereof |
Non-Patent Citations (4)
| Title |
|---|
| HAILI LIN等: "Ethylene glycol-assisted synthesis, photoelectrochemical and photocatalytic properties of BiOI microflowers", 《CHIN. SCI. BULL.》 * |
| XI ZHANG等: "Generalized One-Pot Synthesis, Characterization, and Photocatalytic Activity of Hierarchical BiOX (X = Cl, Br, I) Nanoplate Microspheres", 《J. PHYS. CHEM. C》 * |
| 王立斌: "Bi2S3/BiOX(X=Cl、Br、I)复合材料的制备及其光催化性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
| 褚伟等: "纳米碘氧铋／硫化铋／偕胺肟纤维光催化剂的合成、表征及其性能研究", 《化工新型材料》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110882705A (en) * | 2019-12-10 | 2020-03-17 | 武汉纺织大学 | Microwave synthesis oxygen vacancy BiOCl/Bi2S3Catalyst and preparation method and application thereof |
| CN110882705B (en) * | 2019-12-10 | 2022-10-21 | 武汉纺织大学 | Microwave synthesis oxygen vacancy BiOCl/Bi 2 S 3 Catalyst and preparation method and application thereof |
| CN111533168A (en) * | 2020-04-26 | 2020-08-14 | 昆明理工大学 | Preparation method of bismuth sulfur chlorine particles |
| CN113772725A (en) * | 2020-06-10 | 2021-12-10 | 中国科学院宁波工业技术研究院慈溪生物医学工程研究所 | Bismuth-based semiconductor nano composite material, preparation method and application |
| CN113772725B (en) * | 2020-06-10 | 2023-06-06 | 中国科学院宁波工业技术研究院慈溪生物医学工程研究所 | Bismuth semiconductor nanocomposite, preparation method and application |
| CN112891536A (en) * | 2021-02-04 | 2021-06-04 | 中国科学院宁波材料技术与工程研究所 | Bismuth-based nano heterojunction material and preparation method and application thereof |
| CN114400263A (en) * | 2021-12-16 | 2022-04-26 | 内蒙古鄂尔多斯电力冶金集团股份有限公司 | Preparation method and application of substrate-loaded bismuth oxyhalide/bismuth sulfide nanosheet heterojunction device |
| CN114400263B (en) * | 2021-12-16 | 2023-12-05 | 内蒙古鄂尔多斯电力冶金集团股份有限公司 | Preparation method and application of substrate-supported bismuth halide/bismuth sulfide nanosheet heterojunction device |
| CN115006546A (en) * | 2022-03-16 | 2022-09-06 | 四川大学 | Disulfide heterojunction material for promoting wound healing and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110227502A (en) | A kind of method that one step of room temperature prepares the colored hetero-junctions of bismuthyl chloride/bismuth sulfide nano | |
| CN107866234B (en) | High-activity ZnIn2S4/TiO2Preparation method of Z-system catalyst material | |
| CN106076421B (en) | A kind of MIL-53 (Fe)/g-C3N4The preparation method of nanometer sheet composite photocatalyst material | |
| CN110227503A (en) | A kind of method of one step of room temperature preparation halogenation oxygen bismuth nanometer sheet | |
| CN107349961B (en) | NH (hydrogen sulfide)2Preparation of-UIO-66 @ TpPa-1 composite material and hydrogen production by photolysis of water | |
| CN104841461A (en) | Preparation method and application of novel hexagonal-prism BiOCl nanometer photocatalytic materials | |
| CN103539097B (en) | Preparation method of multi-shape alkaline manganese phosphate microcrystal | |
| CN106179318A (en) | A kind of preparation method of pucherite nano wire graphene photo-catalyst | |
| CN103285894B (en) | Photochemical catalyst of a kind of organic matter halogenation and preparation method thereof | |
| CN108690072A (en) | A kind of Phenylphosphine hydrochlorate and its preparation method and application with photocatalytic activity | |
| CN105271319A (en) | Method for preparing nanometer MgO | |
| CN105771948A (en) | Double-shell titanium dioxide catalyst with high photocatalytic hydrogen generation performance and preparation method thereof | |
| CN105396603A (en) | Bismuth oxychloride catalyst with visible light response core-shell structure and preparation method thereof | |
| CN106824279A (en) | A kind of metal-organic framework material of energy photocatalytic cleavage water and preparation method thereof | |
| CN102553620B (en) | Visible light photocatalyst Bi12O17Cl2 and preparation method thereof | |
| CN106629840B (en) | A kind of truncated cylinder shape octahedron Detitanium-ore-type TiO2Preparation method | |
| Zou et al. | Oxalic acid modified hexagonal ZnIn2S4 combined with bismuth oxychloride to fabricate a hierarchical dual Z-scheme heterojunction: Accelerating charge transfer to improve photocatalytic activity | |
| CN102806078B (en) | Method for preparing one-dimensional hollow superstructure photocatalytic material of Bi system composite oxide | |
| CN110639616A (en) | Preparation of amino modified MIL-68(Ga) novel photocatalyst and method for reducing Cr (VI) by using same | |
| CN103785425A (en) | Preparation method and application of flower-like Bi2O(OH)2SO4 photocatalyst | |
| CN109911936A (en) | A kind of sheet basic bismuth nitrate and preparation method thereof | |
| CN111468094B (en) | CaTiO 3 CaO composite material and preparation method and application thereof | |
| CN111408377B (en) | NiTi nano-flower hydrotalcite photocatalyst and preparation method and application thereof | |
| CN106179431B (en) | A kind of zinc titanium metal composite oxide and its preparation and application | |
| CN110003248B (en) | Polycarboxylic acid uranyl complex photocatalyst and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190913 |
|
| RJ01 | Rejection of invention patent application after publication |