CN108187740A - A kind of APTES-Sb that can be applied to photo-catalytic degradation of methyl-orange2WO6The preparation method of-RGO composite materials - Google Patents
A kind of APTES-Sb that can be applied to photo-catalytic degradation of methyl-orange2WO6The preparation method of-RGO composite materials Download PDFInfo
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- CN108187740A CN108187740A CN201810057482.2A CN201810057482A CN108187740A CN 108187740 A CN108187740 A CN 108187740A CN 201810057482 A CN201810057482 A CN 201810057482A CN 108187740 A CN108187740 A CN 108187740A
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- 239000002131 composite material Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000013033 photocatalytic degradation reaction Methods 0.000 title claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 27
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 claims abstract description 23
- 229940012189 methyl orange Drugs 0.000 claims abstract description 23
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 230000015556 catabolic process Effects 0.000 claims abstract description 13
- 238000006731 degradation reaction Methods 0.000 claims abstract description 13
- 230000003197 catalytic effect Effects 0.000 claims abstract description 11
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims abstract description 9
- 150000001875 compounds Chemical class 0.000 claims abstract description 8
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 4
- 239000010439 graphite Substances 0.000 claims abstract description 4
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 16
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 15
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 12
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 10
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 10
- 239000012498 ultrapure water Substances 0.000 claims description 10
- 238000010521 absorption reaction Methods 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 239000012286 potassium permanganate Substances 0.000 claims description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 5
- 238000002604 ultrasonography Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 230000002378 acidificating effect Effects 0.000 claims description 3
- FAPDDOBMIUGHIN-UHFFFAOYSA-K antimony trichloride Chemical compound Cl[Sb](Cl)Cl FAPDDOBMIUGHIN-UHFFFAOYSA-K 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 3
- 238000001514 detection method Methods 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000000643 oven drying Methods 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 239000003643 water by type Substances 0.000 claims description 3
- -1 Methyl Chemical group 0.000 claims description 2
- 229910020350 Na2WO4 Inorganic materials 0.000 claims description 2
- 238000004108 freeze drying Methods 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims description 2
- 238000005297 material degradation process Methods 0.000 claims 1
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000000356 contaminant Substances 0.000 abstract description 2
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical group CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 abstract 1
- 238000000034 method Methods 0.000 description 10
- 230000001699 photocatalysis Effects 0.000 description 10
- 238000007146 photocatalysis Methods 0.000 description 8
- 238000004042 decolorization Methods 0.000 description 4
- 239000002957 persistent organic pollutant Substances 0.000 description 4
- 239000010865 sewage Substances 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000002688 persistence Effects 0.000 description 3
- 150000003254 radicals Chemical class 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 2
- 241001465754 Metazoa Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000000987 azo dye Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 125000005909 ethyl alcohol group Chemical group 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/0272—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing elements other than those covered by B01J31/0201 - B01J31/0255
- B01J31/0275—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing elements other than those covered by B01J31/0201 - B01J31/0255 also containing elements or functional groups covered by B01J31/0201 - B01J31/0269
-
- 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
-
- 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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- 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)
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Abstract
The present invention relates to a kind of APTES Sb that can be applied to photo-catalytic degradation of methyl-orange2WO6The preparation method of RGO composite materials.Include the following steps：Prepare Sb2WO6Catalysis material modifies Sb using 3 aminopropyl triethoxysilanes (APTES)2WO6Catalysis material prepares graphite oxide (GO), is reduced to GO to make itself and APTES Sb while redox graphene (RGO)2WO6Occur compound so as to prepare APTES Sb2WO6RGO optic catalytic composite materials, by APTES Sb2WO6RGO optic catalytic composite materials are applied to the degradation of water body common contaminant methyl orange.The beneficial effects of the invention are as follows：APTES‑Sb2WO6RGO optic catalytic composite materials are very fast to the degradation rate of the organic molecules such as methyl orange and are easy to reuse.
Description
Technical field
The present invention relates to a kind of APTES-Sb that can be applied to photo-catalytic degradation of methyl-orange2WO6The preparation of-RGO composite materials
Method belongs to wastewater treatment and materials synthesis field.
Technical background
China's shortage of water resources situation is more serious.According to 2008 annual data of the United Nations, China possesses the whole world 21%
Population, but only occupy the 6% of gross amount of water resources, water resource of per capita is only a quarter of world's per capita share, is global people
One of equal poorest country of water resource.However, with the rapid development of industrial or agricultural, agricultural effluent, industrial wastewater and life are dirty
Water discharge capacity increases year by year, and the handling rate of sewage is relatively low in addition, and the water pollution problems in China is just on the rise.In each pollutant
In, persistence organic pollutant is very big to environmental hazard as a kind of typical environmental contaminants.This pollutant has high poison
Property, fat-solubility, the feature of extended residual, and currently used water process means as filter, absorption the methods of be difficult by it
It removes.Due to that can be enriched with transmission in food chain, persistence organic pollutant has more health and ecological environment
Serious harm.Methyl orange is a kind of typical persistence organic pollutant, is widely used in industries such as printing and dyeing, weavings.This
Invention chooses methyl orange as application, has certain representativeness.
Methyl orange is a kind of azo dyes, and aqueous solution is in orange, if untreated in industrial production be just discharged into water body,
On the one hand coloured water body can be made to hinder aquatic plant that sunlight is absorbed and utilized, another aspect methyl orange itself is toxic, this is to contaminated
The existence of water body periphery animals and plants causes serious threat.
Photocatalytic method is a kind of Novel sewage treatment method.Its principle is：Under the conditions of certain wavelength light photograph, semiconductor light
Electronics in catalysis material valence band transits to conduction band, and hole is left in valence band by luminous energy excitation.Subsequent light induced electron and sky
Cave is combined with lewis' acid, living radical of the generation with oxidisability or reproducibility.This living radical can be by water
Unconditionally mineralising is water and carbon dioxide to organic macromolecule in body, so as to achieve the purpose that degradable organic pollutant.Light is urged
Change method has many advantages compared to traditional sewage water treatment method.First, when photocatalysis is carried out in water body, hole is easily and moisture
Son reacts, and forms the extremely strong hydroxyl radical free radical of oxidisability.The free radical can with all organic substances of the mineralising of non-selectivity,
The organic principle being extremely suitble in treated sewage.Secondly, photocatalytic method using luminous energy as energy source, by seek can absorb can
See the catalysis material of light, solar energy can be effectively utilized, it is economic and environment-friendly.Finally, in catalytic reaction process, photochemical catalyst sheet
Body does not change, therefore can recycle, and has certain practicability.
Sb2WO6Have the characteristics that chemical property is stable, cheap and production is easy, be light-catalysed ideal material.But
It is Sb2WO6Photocatalysis efficiency itself is not high.This is because Sb2WO6The electrons and holes generated in photocatalytic process are easily
It is compound, cause the two that cannot play a role.It is of the invention by redox graphene (RGO) and Sb in order to cope with this problem2WO6
It is compound, using RGO to the conductive performance of electronics, promote the separation in light induced electron and hole.Zeta potential shows Sb2WO6And RGO
Surface is negatively charged.With 3- aminopropyl triethoxysilanes (ATPES) to Sb2WO6It is surface modified, its surface is presented
Positive charge is conducive to Sb2WO6It is compound with RGO.The purpose of the present invention is to provide a kind of APTES-Sb2WO6- RGO photocatalysis
The preparation method of composite material.
Invention content
The purpose of the present invention is to provide a kind of APTES-Sb that can be applied to photo-catalytic degradation of methyl-orange2WO6- RGO materials
Preparation method.
A kind of APTES-Sb that can be applied to photo-catalytic degradation of methyl-orange of the present invention2WO6The preparation of-RGO materials, packet
Include following steps：
A, Sb is prepared2WO6Catalysis material：Na is added in the mixed solution of ethylene glycol and water2WO4, stir evenly subsequent
Continuous addition SbCl3；Mixed liquor is transferred in 100mL hydrothermal reaction kettles, 180 DEG C of reaction 12h；By the yellow solid precipitate of precipitation
It centrifuges and is alternately washed each 3 times with absolute ethyl alcohol and ultra-pure water, be put into baking oven drying, obtain Sb2WO6Catalysis material；
B, Sb is modified using APTES2WO6Catalysis material：By Sb2WO6Catalysis material is dissolved in absolute ethyl alcohol, ultrasound
Disperse and APTES is added dropwise；Water-bath heat preservation 4h, suction filtration, drying, obtain APTES-Sb under the conditions of 70 DEG C2WO6；
C, graphite oxide (GO) is prepared：Weigh KMnO4And graphite powder, it is placed in beaker and stirs evenly, it is spare；In three mouthfuls of burnings
The concentrated sulfuric acid, phosphoric acid are sequentially added in bottle, is added slowly with stirring KMnO4With the mixture of graphite powder；48 DEG C of set temperature, water
Bath reaction 12h；After reaction, prepare 1000mL beakers, add in ice cube and H2O2, reaction solution is poured into 1000mL beakers, it is quiet
12h is put, solution layering is removed a layer yellow filtrate, centrifuged；Ultra-pure water, stirring, centrifugation, until solution is in weakly acidic pH are added in repeatedly；
Solution is poured into culture dish, standing 48h makes solvent volatilize, and obtains GO；
D, APTES-Sb is prepared2WO6- RGO optic catalytic composite materials：Weigh APTES-Sb made from step b2WO6And step
GO made from c, is scattered in ultra-pure water, and ultrasound makes it be uniformly dispersed；Dispersion liquid is transferred in 100mL hydrothermal reaction kettles, 180
DEG C reaction 12h；After reaction, product is taken out, is freeze-dried at -45 DEG C for 24 hours, obtains APTES-Sb2WO6- RGO photocatalysis
Composite material；
e、APTES-Sb2WO6- RGO optic catalytic composite materials are applied to the methyl orange in light degradation water：Prepare a certain concentration
Methyl orange solution, use APTES-Sb made from step d2WO6- RGO optic catalytic composite materials decline in ultraviolet light irradiation condition
Methyl orange in Xie Shui, while use the characteristic absorption peak intensity of ultraviolet-uisible spectrophotometer detection methyl orange solution；Work as spy
When levying absorption peak disappearance, that is, illustrate that the methyl orange degradation in solution is complete, record the time used in degradation.
Further, ethylene glycol proportion in mixed solution is 0.1~0.9 in step a, and mixed solution total amount is 50
~80mL, SbCl3Dosage is 0.1~10g, Na2WO4Dosage is 0.05~5g.
Further, Sb in step b2WO6Dosage be 0.1~1g, absolute ethyl alcohol dosage be 100~500mL, ATPES dosages
For 0.1~5mL.
Further, KMnO in step c4Dosage is 1~10g, and graphite powder dosage is 0.1~2g, and concentrated sulfuric acid dosage is 80
~180mL, phosphoric acid dosage are 1~20mL, H2O2Dosage is 5~15mL.
Further, APTES-Sb in step d2WO6Dosage is 0.1~1g, and GO dosages are 0.001~0.1g, and ultra-pure water is used
It measures as 50~70mL.
Further, in step e methyl orange solution a concentration of 1~100mg/L, APTES-Sb2WO6- RGO photocatalysis materials
Expect a concentration of 0.01~1g/L in methyl orange solution, the characteristic absorption peak of methyl orange is at 465nm.
The beneficial effects of the invention are as follows：APTES-Sb2WO6The preparation method of-RGO catalysis materials is simple and to methyl orange
Degradation rate it is very fast.
Description of the drawings
This experiment is further illustrated below in conjunction with the accompanying drawings.
Fig. 1 is APTES-Sb in embodiment one2WO6The X-ray powder diffraction figure of-RGO catalysis materials；
Fig. 2 is APTES-Sb in embodiment one2WO6The uv drs figure of-RGO catalysis materials；
Fig. 3 is APTES-Sb in embodiment one2WO6The transmission electron microscope figure of-RGO catalysis materials；
Fig. 4 is APTES-Sb in embodiment two2WO6- RGO catalysis materials are applied to the design sketch of methyl orange degradation；
Fig. 5 is influence of the raw material proportioning to catalyst photocatalysis effect in embodiment three.
Specific embodiment
Presently in connection with specific embodiment, the present invention will be further described, following embodiment be intended to illustrate invention rather than
Limitation of the invention further.
The percent of decolourization of methyl orange solution shown in narration in detail of the invention and examples of implementation is to calculate as follows
's：Certain density methyl orange solution is prepared, the absorbance at 465nm is measured using ultraviolet-visible spectrophotometer, is denoted as
a0.It is sampled during UV degradation, measures the absorbance at 465nm using ultraviolet-visible spectrophotometer, be denoted as an(n
To sample number).Percent of decolourization bnIt is calculated by the following formula：
bn=1-an/a0(n=0,1,2 ...)
Embodiment one：
It is 3 in ethylene glycol and water ratio:0.91g Na are added in 1 80mL mixed solutions2WO4, continue to add after stirring evenly
Add 0.66g SbCl3.Mixed liquor is transferred in 100mL hydrothermal reaction kettles, 180 DEG C of reaction 12h.The yellow solid of precipitation is sunk
It forms sediment and centrifuges and alternately washed each 3 times with absolute ethyl alcohol and ultra-pure water, be put into baking oven drying, obtain Sb2WO6Catalysis material.
By 0.6g Sb2WO6Catalysis material is dissolved in 300mL absolute ethyl alcohols, and simultaneously 2mL APTES are added dropwise in ultrasonic disperse.At 70 DEG C
Under the conditions of water-bath heat preservation 4h.It filters, drying, obtains APTES-Sb2WO6.Weigh 6g KMnO4With 1g graphite powders, it is placed in beaker
It stirs evenly, it is spare.The 120mL concentrated sulfuric acids, 13.3mL phosphoric acid are sequentially added in three-necked flask, is added slowly with stirring
KMnO4With the mixture of graphite powder.48 DEG C of set temperature, water-bath 12h.After reaction, prepare 1000mL beakers, add in
Ice cube and 10mL H2O2, reaction solution is poured into 1000mL beakers, stands 12h.Solution is layered, and removes a layer yellow filtrate, is centrifuged.
Ultra-pure water, stirring, centrifugation, until solution is in weakly acidic pH are added in repeatedly.Solution is poured into culture dish, standing 48h waves solvent
Hair, obtains GO.Weigh 0.2g APTES-Sb2WO6It with 0.002g GO, is scattered in 70mL ultra-pure waters, ultrasound makes its dispersion equal
It is even.Dispersion liquid is transferred in 100mL hydrothermal reaction kettles, 180 DEG C of reaction 12h.After reaction, product is taken out, at -45 DEG C
Freeze-drying for 24 hours, obtains APTES-Sb2WO6- RGO optic catalytic composite materials.X-ray powder diffraction pattern as shown in Figure 1, table
The bright made sample of the present invention is APTES-Sb2WO6-RGO.Solid uv drs collection of illustrative plates as shown in Figure 2, shows APTES-
Sb2WO6- RGO catalysis materials have good absorbability to ultraviolet light.Transmission electron microscope image as shown in Figure 3,
Show Sb2WO6It can be preferable compound with RGO.
Embodiment two：
Compound concentration is the methyl orange solution 500mL of 6mg/L, weighs the APTES-Sb of the preparation of embodiment one2WO6- RGO light
Catalysis material 0.05g, the methyl orange under 11W ultra violet lamps in degradation water, every two hours sampling is primary, uses UV, visible light
Spectrophotometer detects the characteristic absorption peak intensity of methyl orange solution, calculates solution percent of decolourization.As a result as shown in Figure 4, it is ultraviolet
It is 100% to irradiate 6h rear decolorings rate.
Embodiment three：
Raw material proportioning is investigated to APTES-Sb2WO6The influence of-RGO photocatalysis effects.Weigh respectively 0.001g, 0.002g,
0.004g, 0.01g GO are scattered in 70mL ultra-pure waters, each to add in 0.2g APTES-Sb2WO6, ultrasound makes it be uniformly dispersed.It will
Dispersion liquid is transferred in 100mL hydrothermal reaction kettles, 180 DEG C of reaction 12h.After reaction, product is taken out, is freezed at -45 DEG C
Drying for 24 hours, obtains the APTES-Sb of different ratios of raw materials2WO6- RGO samples, wherein GO and APTES-Sb2WO6Quality score
It Wei 1:200,1:100,1:50 and 1:20.Compound concentration is 6mg/L methyl orange solution 500mL, and it is above-mentioned not to weigh 0.05g respectively
With the APTES-Sb of proportioning2WO6- RGO samples, the methyl orange under 11W ultra violet lamps in degradation water, every two hours sample one
It is secondary, using the characteristic absorption peak intensity of ultraviolet-uisible spectrophotometer detection methyl orange solution, calculate solution percent of decolourization.As a result such as
Shown in attached drawing 5, as GO and APTES-Sb2WO6Ratio be 1:When 100, photocatalysis effect is best.
Claims (6)
1. a kind of APTES-Sb that can be applied to photo-catalytic degradation of methyl-orange2WO6The preparation method of-RGO composite materials, step is such as
Under：
A, Sb is prepared2WO6Catalysis material：Na is added in the mixed solution of ethylene glycol and water2WO4, continue to add after stirring evenly
Add SbCl3；Mixed liquor is transferred in 100mL hydrothermal reaction kettles, 180 DEG C of reaction 12h；The yellow solid precipitate of precipitation is centrifuged
It detaches and is alternately washed each 3 times with absolute ethyl alcohol and ultra-pure water, be put into baking oven drying, obtain Sb2WO6Catalysis material；
B, APTES-Sb is prepared2WO6Composite material：By Sb2WO6Catalysis material is dissolved in absolute ethyl alcohol, ultrasonic disperse and dropwise
Add in 3- aminopropyl triethoxysilanes (APTES)；Water-bath heat preservation 4h, suction filtration, drying, obtain APTES- under the conditions of 70 DEG C
Sb2WO6Composite material；
C, graphite oxide (GO) is prepared：Weigh KMnO4And graphite powder, it is placed in beaker and stirs evenly, it is spare；In three-necked flask
The concentrated sulfuric acid, phosphoric acid are sequentially added, is added slowly with stirring KMnO4With the mixture of graphite powder；48 DEG C of set temperature, water-bath is anti-
Answer 12h；After reaction, prepare 1000mL beakers, add in ice cube and H2O2, reaction solution is poured into 1000mL beakers, is stood
12h；Solution is layered, and removes a layer yellow filtrate, is centrifuged；Ultra-pure water, stirring, centrifugation, until solution is in weakly acidic pH are added in repeatedly；It will
Solution is poured into culture dish, and standing 48h makes solvent volatilize, and obtains GO；
D, APTES-Sb is prepared2WO6- RGO optic catalytic composite materials：Weigh APTES-Sb made from step b2WO6It is made with step c
GO, be scattered in ultra-pure water, ultrasound makes it be uniformly dispersed；Dispersion liquid is transferred in 100mL hydrothermal reaction kettles, 180 DEG C anti-
12h is answered to make APTES-Sb2WO6Occur with redox graphene (RGO) compound；After reaction, product is taken out, at -45 DEG C
Freeze-drying for 24 hours, obtains APTES-Sb2WO6- RGO optic catalytic composite materials；
e、APTES-Sb2WO6- RGO optic catalytic composite materials are applied to the methyl orange in degradation water：Prepare certain density methyl
Orange solution, the APTES-Sb made from step d2WO6Methyl orange in-RGO optic catalytic composite material degradation waters, while using purple
The characteristic absorption peak intensity of outer visible spectrophotometer detection methyl orange solution；When characteristic absorption peak disappears, that is, illustrate solution
In methyl orange degradation it is complete, record degradation used in the time.
2. a kind of APTES-Sb that can be applied to photo-catalytic degradation of methyl-orange according to claim 12WO6- RGO composite materials
Preparation method, it is characterized in that：Ethylene glycol proportion in mixed solution is 0.1~0.9 in the step a, mixed solution
Total amount is 50~80mL, SbCl3Dosage is 0.1~10g, Na2WO4Dosage is 0.05~5g.
3. a kind of APTES-Sb that can be applied to photo-catalytic degradation of methyl-orange according to claim 12WO6- RGO composite materials
Preparation method, it is characterized in that：Sb in the step b2WO6Dosage is 0.1~1g, and absolute ethyl alcohol dosage is 100~500mL,
ATPES dosages are 0.1~5mL.
4. a kind of APTES-Sb that can be applied to photo-catalytic degradation of methyl-orange according to claim 12WO6- RGO composite materials
Preparation method, it is characterized in that：KMnO in the step c4Dosage is 1~10g, and graphite powder dosage is 0.1~2g, and the concentrated sulfuric acid is used
It measures as 80~180mL, phosphoric acid dosage is 1~20mL, H2O2Dosage is 5~15mL.
5. a kind of APTES-Sb that can be applied to photo-catalytic degradation of methyl-orange according to claim 12WO6- RGO composite materials
Preparation method, it is characterized in that：APTES-Sb in the step d2WO6Dosage is 0.1~1g, and GO dosages are 0.001~0.1g,
Ultrapure water consumption is 50~70mL.
6. a kind of APTES-Sb that can be applied to photo-catalytic degradation of methyl-orange according to claim 12WO6- RGO composite materials
Preparation method, it is characterized in that：A concentration of 1~the 100mg/L, APTES-Sb of methyl orange solution in the step e2WO6- RGO light
A concentration of 0.01~1g/L of the catalysis material in methyl orange solution.The characteristic absorption peak of methyl orange is at 465nm.
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| CN110787792A (en) * | 2019-11-19 | 2020-02-14 | 常州大学 | Bi with visible light response2Ti2O7-TiO2Preparation method of/RGO nano composite material |
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| CN104667929A (en) * | 2015-02-10 | 2015-06-03 | 湖南大学 | Magnetic nanometer photocatalyst |
| CN104971720A (en) * | 2015-06-11 | 2015-10-14 | 西北师范大学 | Bismuth tungstate nanocomposite, and preparation method and application thereof |
| CN105879885A (en) * | 2016-05-04 | 2016-08-24 | 上海大学 | Catalyst for photocatalytic decomposition of water into hydrogen by visible light and method for preparing catalyst |
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| CN110787792B (en) * | 2019-11-19 | 2023-08-29 | 常州大学 | Bi with visible light response 2 Ti 2 O 7 -TiO 2 Preparation method of RGO nanocomposite |
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