CN109603867A - A kind of loess particulate load bismuth sulfide cadmium sulfide nano heterojunction composite photocatalyst and preparation method thereof - Google Patents
A kind of loess particulate load bismuth sulfide cadmium sulfide nano heterojunction composite photocatalyst and preparation method thereof Download PDFInfo
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- CN109603867A CN109603867A CN201910106466.2A CN201910106466A CN109603867A CN 109603867 A CN109603867 A CN 109603867A CN 201910106466 A CN201910106466 A CN 201910106466A CN 109603867 A CN109603867 A CN 109603867A
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- AFMHYDVGYSYYMF-UHFFFAOYSA-N cadmium(2+) sulfanylidenebismuthanylium sulfide Chemical compound [Bi+]=S.[S-2].[Cd+2] AFMHYDVGYSYYMF-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 36
- 239000002131 composite material Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000002245 particle Substances 0.000 claims abstract description 32
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 28
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 16
- JHXKRIRFYBPWGE-UHFFFAOYSA-K bismuth chloride Chemical compound Cl[Bi](Cl)Cl JHXKRIRFYBPWGE-UHFFFAOYSA-K 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 claims abstract description 14
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002270 dispersing agent Substances 0.000 claims abstract description 8
- 239000012153 distilled water Substances 0.000 claims abstract description 8
- 238000007789 sealing Methods 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 239000002904 solvent Substances 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical group OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 27
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 10
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 7
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 7
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 7
- 239000012736 aqueous medium Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 18
- 239000000463 material Substances 0.000 abstract description 6
- 239000002351 wastewater Substances 0.000 abstract description 5
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 4
- 239000010919 dye waste Substances 0.000 abstract description 2
- 238000006555 catalytic reaction Methods 0.000 abstract 1
- 229920002521 macromolecule Polymers 0.000 abstract 1
- 238000007146 photocatalysis Methods 0.000 description 13
- 239000013078 crystal Substances 0.000 description 12
- 238000006731 degradation reaction Methods 0.000 description 9
- 230000015556 catabolic process Effects 0.000 description 8
- 238000005286 illumination Methods 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- 238000001291 vacuum drying Methods 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000012876 carrier material Substances 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- IRUDKOHJSBEQFA-UHFFFAOYSA-N bismuth cadmium(2+) sulfide Chemical compound [Bi+3].[S-2].[Cd+2] IRUDKOHJSBEQFA-UHFFFAOYSA-N 0.000 description 1
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 1
- 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 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000012916 structural analysis Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000002459 sustained effect Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J27/138—Halogens; Compounds thereof with alkaline earth metals, magnesium, beryllium, zinc, cadmium or mercury
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of preparation methods of loess particulate load bismuth sulfide cadmium sulfide nano heterojunction composite photocatalyst, it is in the presence of dispersants, bismuth chloride, cadmium nitrate, thiocarbamide and macromolecule dispersing agent are dispersed with stirring in organic alcohol solvent, loess particle is added portionwise under stiring again, makes loess particle fully dispersed at room temperature；Then mixed liquor is moved into reaction kettle, reacts 2 ~ 10 h at 120 DEG C ~ 160 DEG C under sealing；Product centrifuge separation, obtains black particle shape product；It dries after successively being washed with acetone, distilled water to get graininess loess particulate load bismuth sulfide cadmium sulfide nano heterojunction photocatalyst.Photocatalytic degradation organic wastewater the experimental results showed that, loess particulate load bismuth sulfide cadmium sulfide nano heterojunction photocatalyst prepared by the present invention has very high photocatalytic activity under simulated solar irradiation irradiation, it is a kind of efficient, easily separated and lower-cost catalysis material, is had a good application prospect in photocatalytic degradation of dye waste water field.
Description
Technical field
The present invention relates to a kind of bismuth sulfide cadmium sulfide nano heterojunction photocatalyst more particularly to a kind of loess particulate loads
The preparation method of bismuth sulfide cadmium sulfide nano heterojunction composite photocatalyst, the organic dirt being mainly used in wastewater by photocatalysis
Object is contaminated, technical field of composite materials and technical field of waste water processing are belonged to.
Background technique
Water plays important role in the normal operation of terrestrial ecosystem.In recent decades, in industrialization degree
Problem of environmental pollution, especially water pollution problem day aobvious protrusion are caused while raising.The processing of dyeing wastewater because
This becomes waste water industry and gives more sustained attention simultaneously urgent problem.In recent years, the development of Photocatalitic Technique of Semiconductor, mentions for us
For a kind of approach that high efficient energy sources use.
For bismuth sulfide cadmium sulfide as a kind of novel semiconductor material, they can either be such that fluorescent emission and absorbing wavelength generates
Blue-shifted phenomenon, while the redox ability of nanoparticle also can be enhanced, stronger photocatalysis performance is shown, it can be in difference
Efficient degradation effect is played to organic pollutant difficult to degrade in environment.However, bismuth sulfide cadmium sulfide has certain biology poison
Property, the defects of particle is too thin, difficult recycling, keep its application limited.Therefore, how to be kept away while using its high efficiency photocatalysis performance
Exempting from its defect is to need the direction of innovation and development.By high efficiency photocatalyst and with adsorption activity and cheap environmental-friendly carrier
Material combines, and can not only reduce catalyst amount, and its easy recycling and reusing can be made to improve utilization efficiency.
Clay class inorganic mineral can be used for loaded optic catalyst.However, exploring more efficient and cheap photocatalysis carrier
Material is the effective way for solving problem of environmental pollution.Graininess loess is nature largely existing natural inorganic mineral, tool
Have the advantages that environmental-friendly and cheap and easy to get, loose and nutty structure makes it have certain adsorption capacity and load capacity.
Bismuth sulfide cadmium sulfide nano hetero-junctions with high efficiency photocatalysis performance is carried on loess particle surface, makes the performance association of the two
Same-action, to obtain very high photocatalytic activity.
Summary of the invention
Object of the present invention is to the structure and characteristics using loess particle, provide a kind of loess particulate load bismuth sulfide cadmium sulfide
The preparation method of nano heterojunction photocatalysis agent.
One, the preparation of loess particulate load bismuth sulfide cadmium sulfide nano heterojunction composite photocatalyst
First anhydrous bismuth chloride, cadmium nitrate, thiocarbamide and dispersing agent are well-dispersed in organic alcohol solvent, then loess is added portionwise
Grain, stirring keep loess particle fully dispersed；Then mixed liquor is moved into reaction kettle, reacts 2 at 120 DEG C ~ 160 DEG C under sealing
~10 h；Product is removed, centrifuge separation obtains black particle shape product；It is successively washed 3 ~ 5 times with acetone, distilled water, vacuum is dry
It is dry to get loess particulate load bismuth sulfide cadmium sulfide nano heterojunction photocatalyst.
The mass ratio of anhydrous bismuth chloride and cadmium nitrate is 1:1 ~ 2:1；The mass ratio of anhydrous bismuth chloride and thiocarbamide is 1:1 ~ 3:
1；Anhydrous bismuth chloride, cadmium nitrate, thiocarbamide gross mass be loess particle 5% ~ 30%.
The dispersing agent uses polyvinylpyrrolidone, and average molecular weight is 20 ~ 50 kDa.The additional amount of dispersing agent is nothing
Water bismuth chloride, cadmium nitrate, 1 ~ 2 times of thiocarbamide gross mass.
The loess particle is using natural loess as raw material, and using it, differential settling velocity is isolated in an aqueous medium
The tiny loess of granularity, partial size are 1 ~ 10 μm.
The organic alcohol solvent is ethylene glycol or/and propylene glycol；When for ethylene glycol and propylene glycol, the volume ratio of the two is
1:1~1:3。
Two, the pattern of loess particulate load bismuth sulfide cadmium sulfide nano heterojunction composite photocatalyst and structural analysis
1, microscopic appearance
Using the microscopic appearance of scanning electron microscopic observation loess particulate load bismuth sulfide cadmium sulfide heterojunction photocatalyst.Fig. 1 is
Its scanning electron microscope (SEM) photograph.It will be seen from figure 1 that loess particulate load bismuth sulfide cadmium sulfide heterojunction photocatalyst substrate is typical
Loess granule-morphology, the loess particle surface in loose and more gaps have loaded bismuth sulfide cadmium sulfide hetero-junctions.It is this loose
And heterojunction structure is loaded on more gaps, both there is absorption property, should also have photocatalysis performance.
2, infrared spectrum analysis
Fig. 2 is the infrared spectrum of loess particulate load bismuth sulfide cadmium sulfide heterojunction photocatalyst, wherein 1300 ~ 1400cm-1Place
It is the stretching vibration of Bi-S key, 1084cm-1It is nearby the stretching vibration absworption peak of Si-O-Si, 1600cm-1Nearby for Cd-S's
Stretching vibration absworption peak, 3300 ~ 3600cm-1Nearby there is the stretching vibration that wide absorption peak is loess surface hydroxyl O-H to absorb
Peak.As shown in Figure 2, the structure of loess particle is kept substantially, may also detect that the characteristic peak of bismuth sulfide cadmium sulfide, is illustrated compound
Material is made of loess particle and bismuth sulfide cadmium sulfide, this is consistent with SEM result.
3, X-ray diffraction analysis
Fig. 3 is the X-ray diffractogram of loess particulate load bismuth sulfide cadmium sulfide hetero-junctions, wherein the diffraction of the appearance at 25 °, 27 °
Peak belongs to the characteristic diffraction peak of bismuth sulfide, and very strong diffraction maximum occur at 26 ° is characteristic diffraction peak quartzy in loess, and 45 ° attached
Closely there is the characteristic diffraction peak of cadmium sulfide, 28 ° of diffraction maximums nearby occurred are amorphous silicate or alumino-silicate in loess
Characteristic diffraction peak, these all illustrate what composite material was made of loess and bismuth sulfide cadmium sulfide, and bismuth sulfide cadmium sulfide
Molecular structure of the addition of hetero-junctions without destruction Loess Yuan.
Three, the light degradation property test of loess particulate load bismuth sulfide cadmium sulfide heterojunction composite photocatalyst
In order to test the photocatalytic activity of loess particulate load bismuth sulfide cadmium sulfide hetero-junctions, crystal violet is chosen as representative difficult
Photocatalytic activity test is carried out with the organic pollutant of degradation.The photochemical catalyst for weighing 0.05g is distributed to the crystallization of 50mL
In purple solution (concentration 20mg/L), dark reaction 20min reaches adsorption/desorption balance.Then, the photocatalysis in photo catalysis reactor
70min takes 5mL sample to be centrifuged at regular intervals, and upper liquid passes through 0.22 μm of filter membrane, is surveyed using ultraviolet-visible spectrophotometry
The concentration of fixed remnants crystal violet, calculates percent of decolourization.
Fig. 4 is light degradation curve graph of the catalyst different time to crystal violet.From fig. 4, it can be seen that loess particulate load
Bismuth sulfide cadmium sulfide hetero-junctions reaches 60.45% to the removal rate of crystal violet after dark reaction 20min, removes after 60 min of illumination
Rate reaches 96.38%, illustrates that loess particulate load bismuth sulfide cadmium sulfide hetero-junctions has certain adsorption capacity to crystal violet, opens
Mainly photocatalytic degradation plays main function after opening light source.These results suggest that loess particulate load bismuth sulfide cadmium sulfide is heterogeneous
Tying composite photo-catalyst has good catalytic degradation performance to crystal violet under simulated solar irradiation, and degradation reaction is loess
The result of the absorption of grain and bismuth sulfide cadmium sulfide heterojunction photocatalysis degradation synergistic effect.
In conclusion the present invention is using loess particle as carrier, it is by one kettle way that bismuth sulfide cadmium sulfide hetero-junctions is in situ
It is carried on loess particle surface, the absorption of loess particle and the collaboration of bismuth sulfide cadmium sulfide heterojunction photocatalysis degradation, into one
Step improves the photocatalytic activity of composite catalyst, to obtain a kind of efficient, easily separated and lower-cost photocatalysis material
Material.The material has a good application prospect in photocatalytic degradation of dye waste water field.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of loess particulate load bismuth sulfide cadmium sulfide nano heterojunction photocatalyst.
Fig. 2 is the infrared absorpting light spectra of loess particulate load bismuth sulfide cadmium sulfide nano heterojunction photocatalyst.
Fig. 3 is the X-ray diffractogram of loess particulate load bismuth sulfide cadmium sulfide nano heterojunction photocatalyst.
Fig. 4 is light degradation curve of the loess particulate load bismuth sulfide cadmium sulfide nano heterojunction photocatalyst to crystal violet
Figure.
Specific embodiment
Below by specific embodiment to loess particulate load bismuth sulfide cadmium sulfide nano heterojunction photocatalyst of the present invention
Preparation and photocatalysis performance be described further.
Embodiment 1
The anhydrous bismuth chloride of 0.13g, 0.13g cadmium nitrate, 0.12g thiocarbamide and 3g polyvinylpyrrolidone (average molecular weight 30kDa),
It is well-dispersed in 25mL ethylene glycol under stiring；3g loess particle is taken, is stirred at room temperature down and is added portionwise in mixed liquor and divides
It dissipates uniform；Then mixed liquor is moved into reaction kettle, reacts 10 h at 120 DEG C under sealing；Product is removed, centrifuge separation obtains
To black particle shape product；Product acetone, distilled water successively wash 3 ~ 5 times, and vacuum drying is to get the vulcanization of loess particulate load
Bismuth cadmium sulfide nano heterojunction photocatalyst.
The loess particulate load bismuth sulfide cadmium sulfide hetero-junctions reaches the removal rate of crystal violet after dark reaction 20min
Removal rate reaches 95.34% after 58.23%, illumination 70min.
Embodiment 2
Take the anhydrous bismuth chloride of 0.14g, 0.13g cadmium nitrate, 0.12g thiocarbamide and 4g polyvinylpyrrolidone (average molecular weight
38kDa), it is well-dispersed in 30mL propylene glycol under stiring；4g loess particle is taken, is stirred at room temperature down and mixed liquor is added portionwise
In and be uniformly dispersed；Then mixed liquor is moved into reaction kettle, reacts 8 h at 140 DEG C under sealing；Remove product, centrifugation point
From obtaining black particle shape product；Product acetone, distilled water successively wash 3 ~ 5 times, and vacuum drying is negative to get loess particle
Carry bismuth sulfide cadmium sulfide nano heterojunction photocatalyst.
The loess particulate load bismuth sulfide cadmium sulfide hetero-junctions reaches the removal rate of crystal violet after dark reaction 20min
Removal rate reaches 96.17% after 59.52%, illumination 70min.
Embodiment 3
Take the anhydrous bismuth chloride of 0.16g, 0.15g cadmium nitrate, 0.14g thiocarbamide and 5g polyvinylpyrrolidone (average molecular weight
42kDa), it is well-dispersed in 30mL ethylene glycol under stiring；5g loess particle is taken, is stirred at room temperature down and mixed liquor is added portionwise
In and be uniformly dispersed；Then mixed liquor is moved into reaction kettle, reacts 4 h at 160 DEG C under sealing；Remove product, centrifugation point
From obtaining black particle shape product；Product acetone, distilled water successively wash 3 ~ 5 times, and vacuum drying is negative to get loess particle
Carry bismuth sulfide cadmium sulfide nano heterojunction photocatalyst.
The loess particulate load bismuth sulfide cadmium sulfide hetero-junctions reaches the removal rate of crystal violet after dark reaction 20min
Removal rate reaches 96.23% after 60.01%, illumination 70min.
Embodiment 4
Take the anhydrous bismuth chloride of 0.17g, 0.13 g cadmium nitrate, 0.15g thiocarbamide and 6g polyvinylpyrrolidone (average molecular weight
32kDa), it is well-dispersed in 40 mL ethylene glycol and 1,2-propylene glycol in the mixed solvents under stiring；6g loess particle is taken, is stirred at room temperature down
It is added portionwise in mixed liquor and is uniformly dispersed；Then mixed liquor is moved into reaction kettle, reacts 2 h at 160 DEG C under sealing；
Product is removed, centrifuge separation obtains black particle shape product；Product acetone, distilled water successively wash 3 ~ 5 times, vacuum drying,
Up to loess particulate load bismuth sulfide cadmium sulfide nano heterojunction photocatalyst.
The loess particulate load bismuth sulfide cadmium sulfide hetero-junctions reaches the removal rate of crystal violet after dark reaction 20min
Removal rate reaches 98.59% after 59.76%, illumination 70min.
Embodiment 5
Take the anhydrous bismuth chloride of 0.15g, (average molecular weight is for 0.12g cadmium nitrate, 0.11g thiocarbamide and 2g polyvinylpyrrolidone
32Kda), it is well-dispersed in 15 mL ethylene glycol and 1,2-propylene glycol in the mixed solvents under stiring；2g loess particle is taken, is stirred at room temperature down
It is added portionwise in mixed liquor and is uniformly dispersed；Then mixed liquor is moved into reaction kettle, reacts 6 h at 130 DEG C under sealing；
Product is removed, centrifuge separation obtains black particle shape product；Product acetone, distilled water successively wash 3 ~ 5 times, vacuum drying,
Up to loess particulate load bismuth sulfide cadmium sulfide nano heterojunction photocatalyst.
The loess particulate load bismuth sulfide cadmium sulfide hetero-junctions reaches the removal rate of crystal violet after dark reaction 20min
Removal rate reaches 92.78% after 57.25%, illumination 70min.
Claims (9)
1. a kind of preparation method of loess particulate load bismuth sulfide cadmium sulfide nano heterojunction composite photocatalyst, being first will be anhydrous
Bismuth chloride, cadmium nitrate, thiocarbamide and dispersing agent are well-dispersed in organic alcohol solvent, then be added portionwise loess particle and stir make it
It is fully dispersed；Then mixed liquor is moved into reaction kettle, reacts 2 ~ 10 h at 120 DEG C ~ 160 DEG C under sealing；Product is removed, from
Heart separation, obtains black particle shape product；It is successively washed 3 ~ 5 times, is dried in vacuo to get graininess loess with acetone, distilled water
Particulate load bismuth sulfide cadmium sulfide nano heterojunction photocatalyst.
2. the preparation side of loess particulate load bismuth sulfide cadmium sulfide nano heterojunction composite photocatalyst as described in claim 1
Method, it is characterised in that: the mass ratio of anhydrous bismuth chloride and cadmium nitrate is 1:1 ~ 2:1.
3. the preparation side of loess particulate load bismuth sulfide cadmium sulfide nano heterojunction composite photocatalyst as described in claim 1
Method, it is characterised in that: the mass ratio of anhydrous bismuth chloride and thiocarbamide is 1:1 ~ 3:1.
4. the preparation side of loess particulate load bismuth sulfide cadmium sulfide nano heterojunction composite photocatalyst as described in claim 1
Method, it is characterised in that: the loess particle is using natural loess as raw material, and differential settling velocity separates in an aqueous medium using it
The tiny loess of granularity out, partial size are 1 ~ 10 μm.
5. the preparation side of loess particulate load bismuth sulfide cadmium sulfide nano heterojunction composite photocatalyst as claimed in claim 4
Method, it is characterised in that: anhydrous bismuth chloride, cadmium nitrate, thiocarbamide gross mass be loess particle 5% ~ 30%.
6. the preparation side of loess particulate load bismuth sulfide cadmium sulfide nano heterojunction composite photocatalyst as described in claim 1
Method, it is characterised in that: the dispersing agent uses polyvinylpyrrolidone, and average molecular weight is 20 ~ 50 kDa.
7. the preparation side of loess particulate load bismuth sulfide cadmium sulfide nano heterojunction composite photocatalyst as claimed in claim 6
Method, it is characterised in that: the additional amount of dispersing agent is anhydrous bismuth chloride, cadmium nitrate, 1 ~ 2 times of thiocarbamide gross mass.
8. the preparation side of loess particulate load bismuth sulfide cadmium sulfide nano heterojunction composite photocatalyst as described in claim 1
Method, it is characterised in that: organic alcohol solvent is ethylene glycol or/and propylene glycol.
9. the preparation side of loess particulate load bismuth sulfide cadmium sulfide nano heterojunction composite photocatalyst as claimed in claim 8
Method, it is characterised in that: when organic alcohol solvent is ethylene glycol and propylene glycol, the volume ratio of ethylene glycol and propylene glycol is 1:1 ~ 1:3.
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| CN201910106466.2A CN109603867A (en) | 2019-02-02 | 2019-02-02 | A kind of loess particulate load bismuth sulfide cadmium sulfide nano heterojunction composite photocatalyst and preparation method thereof |
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