CN108187740B - A kind of APTES-Sb can be applied to photo-catalytic degradation of methyl-orange2WO6The preparation method of-RGO composite material - Google Patents
A kind of APTES-Sb can be applied to photo-catalytic degradation of methyl-orange2WO6The preparation method of-RGO composite material Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000013033 photocatalytic degradation reaction Methods 0.000 title claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 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 21
- 229940012189 methyl orange Drugs 0.000 claims abstract description 21
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 230000003197 catalytic effect Effects 0.000 claims abstract description 12
- 230000015556 catabolic process Effects 0.000 claims abstract description 11
- 238000006731 degradation reaction Methods 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 8
- 150000001875 compounds Chemical class 0.000 claims abstract description 8
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 3
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 3
- 239000010439 graphite Substances 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 18
- 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
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 12
- 239000012498 ultrapure water Substances 0.000 claims description 12
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 10
- 238000003756 stirring Methods 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 8
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 5
- 239000012286 potassium permanganate 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
- 238000001556 precipitation Methods 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 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
- 239000002904 solvent Substances 0.000 claims description 3
- -1 Methyl Chemical group 0.000 claims description 2
- 229910020350 Na2WO4 Inorganic materials 0.000 claims description 2
- 230000002378 acidificating effect Effects 0.000 claims description 2
- 238000004108 freeze drying Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims description 2
- 238000005303 weighing 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
- 230000001699 photocatalysis Effects 0.000 description 11
- 238000000034 method Methods 0.000 description 10
- 238000007146 photocatalysis Methods 0.000 description 9
- 238000004042 decolorization Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000002957 persistent organic pollutant Substances 0.000 description 4
- 239000010865 sewage Substances 0.000 description 4
- 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
- 230000005540 biological transmission Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 238000000926 separation method 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
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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
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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
- 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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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 material.The following steps are included: preparation Sb2WO6Catalysis material modifies Sb using 3- aminopropyl triethoxysilane (APTES)2WO6Catalysis material prepares graphite oxide (GO), is reduced to GO to make itself and APTES-Sb while redox graphene (RGO)2WO6Occur compound to prepare APTES-Sb2WO6- RGO optic catalytic composite material, by APTES-Sb2WO6- RGO optic catalytic composite material is applied to the degradation of water body common contaminant methyl orange.The beneficial effects of the present invention are: APTES-Sb2WO6- RGO optic catalytic composite material is very fast to the degradation rate of the organic molecules such as methyl orange and is 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 material
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
Equal poorest one of the country of water resource.However, agricultural effluent, industrial wastewater and life are dirty with the rapid development of industrial or agricultural
Water discharge amount increases year by year, and the handling rate of sewage is lower 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 filtering, absorption the methods of be difficult it
It removes.Due to that can be enriched with transmitting in food chain, persistence organic pollutant has more human 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 sewage water treatment method.Its principle is: under the conditions of certain wavelength light is shone, conductor photocatalysis
Electronics in material valence band transits to conduction band by luminous energy excitation, and hole is left in valence band.Subsequent light induced electron and hole with
Lewis' acid combines, and generates the living radical with oxidisability or reproducibility.This living radical can will be in water body
Organic macromolecule unconditionally mineralising be water and carbon dioxide, to achieve the purpose that degradable organic pollutant.Photocatalytic method
It is had many advantages compared to traditional sewage water treatment method.Firstly, hole is easily sent out with hydrone when carrying out photocatalysis in water body
Raw reaction, forms the extremely strong hydroxyl radical free radical of oxidisability.The free radical can be with all organic substances of the mineralising of non-selectivity, extremely
The organic principle being suitble in processing sewage.Secondly, photocatalytic method is using luminous energy as energy source, by seeking visible light absorbing
Catalysis material, solar energy can be effectively utilized, it is economic and environment-friendly.Finally, photochemical catalyst itself is no in catalytic reaction process
It changes, therefore can recycle, there is certain practicability.
Sb2WO6Have the characteristics that chemical property is stable, cheap and production is easy, is light-catalysed ideal material.But
It is Sb2WO6Photocatalysis efficiency itself is not high.This is because Sb2WO6The electrons and holes pole generated in the photocatalytic process
It is easily compound, cause the two that cannot play a role.In order to cope with this problem, the present invention by redox graphene (RGO) with
Sb2WO6It is compound, using RGO to the conductive performance of electronics, promote the separation of light induced electron and hole.Zeta potential shows Sb2WO6
It is negatively charged with the surface RGO.With 3- aminopropyl triethoxysilane (ATPES) to Sb2WO6It is surface modified, makes its surface
Positive charge is presented, is conducive to Sb2WO6It is compound with RGO.The purpose of the present invention is to provide a kind of APTES-Sb2WO6- RGO light
The preparation method of catalytic composite materials.
Summary of the invention
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 material
Preparation method.
A kind of APTES-Sb can be applied to photo-catalytic degradation of methyl-orange of the present invention2WO6The preparation of-RGO material, 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 kettle, 180 DEG C of reaction 12h；By the yellow solid precipitate of precipitation
It is centrifugated and is alternately washed each 3 times with dehydrated alcohol and ultrapure water, be put into baking oven drying, obtain Sb2WO6Catalysis material；
B, Sb is modified using APTES2WO6Catalysis material: by Sb2WO6Catalysis material is dissolved in dehydrated alcohol, ultrasound
Disperse and APTES is added dropwise；Water-bath keeps the temperature 4h, suction filtration, drying under the conditions of 70 DEG C, obtains APTES-Sb2WO6；
C, it prepares graphite oxide (GO): weighing KMnO4And graphite powder, it is placed in a beaker and stirs evenly, it is spare；It is burnt at three mouthfuls
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 beaker, ice cube and H is added2O2, reaction solution is poured into 1000mL beaker,
12h is stood, solution layering takes lower layer's yellow filtrate, is centrifuged；Ultrapure water, stirring, centrifugation, until solution is in close are added repeatedly
Property；Solution is poured into culture dish, standing 48h makes solvent volatilize, and obtains GO；
D, APTES-Sb is prepared2WO6- RGO optic catalytic composite material: APTES-Sb made from step b is weighed2WO6And step
GO made from c, is scattered in ultrapure water, and ultrasound makes it be uniformly dispersed；Dispersion liquid is transferred in 100mL hydrothermal reaction kettle, 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 material is applied to the methyl orange in light degradation water: preparing a certain concentration
Methyl orange solution, use APTES-Sb made from step d2WO6- RGO optic catalytic composite material declines in ultraviolet light irradiation condition
The methyl orange of Xie Shuizhong, while using 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, records the degradation time used.
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 is 0.1~1g, and dehydrated alcohol dosage is 100~500mL, ATPES dosage
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 dosage is 0.001~0.1g, and ultrapure water is used
Amount is 50~70mL.
Further, the concentration of methyl orange solution is 1~100mg/L, APTES-Sb in step e2WO6- RGO photocatalysis material
Expect that the concentration in methyl orange solution is 0.01~1g/L, the characteristic absorption peak of methyl orange is at 465nm.
The beneficial effects of the present invention are: APTES-Sb2WO6The preparation method of-RGO catalysis material is simple and to methyl orange
Degradation rate it is very fast.
Detailed description of the invention
This experiment is further illustrated with reference to the accompanying drawing.
Fig. 1 is APTES-Sb in embodiment one2WO6The X-ray powder diffraction figure of-RGO catalysis material；
Fig. 2 is APTES-Sb in embodiment one2WO6The uv drs figure of-RGO catalysis material；
Fig. 3 is APTES-Sb in embodiment one2WO6The transmission electron microscope figure of-RGO catalysis material；
Fig. 4 is APTES-Sb in embodiment two2WO6- RGO catalysis material is applied to the effect picture 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 the methyl orange solution shown in narration in detail of the invention and examples of implementation is to calculate as follows
: certain density methyl orange solution is prepared, using the absorbance at ultraviolet-visible spectrophotometer measurement 465nm, is denoted as
a0.It is sampled during UV degradation, using the absorbance at ultraviolet-visible spectrophotometer measurement 465nm, is denoted as an(n
To sample number).Percent of decolourization bnIt is calculated by following formula:
bn=1-an/a0(n=0,1,2 ...)
Embodiment one:
0.91g Na is added in the 80mL mixed solution that ethylene glycol and water ratio are 3:12WO4, continue to add after mixing evenly
Add 0.66g SbCl3.Mixed liquor is transferred in 100mL hydrothermal reaction kettle, 180 DEG C of reaction 12h.By the yellow solid of precipitation
Precipitation and centrifugal separation is simultaneously alternately washed each 3 times with dehydrated alcohol and ultrapure water, is put into baking oven drying, is obtained Sb2WO6Photocatalysis material
Material.By 0.6g Sb2WO6Catalysis material is dissolved in 300mL dehydrated alcohol, and simultaneously 2mL APTES is added dropwise in ultrasonic disperse.70
Water-bath keeps the temperature 4h under the conditions of DEG C.It filters, drying, obtains APTES-Sb2WO6.Weigh 6g KMnO4With 1g graphite powder, it is placed in beaker
In stir evenly, it is spare.The 120mL concentrated sulfuric acid, 13.3mL phosphoric acid are sequentially added in three-necked flask, are added slowly with stirring
KMnO4With the mixture of graphite powder.48 DEG C of set temperature, water-bath 12h.After reaction, prepare 1000mL beaker, be added
Ice cube and 10mL H2O2, reaction solution is poured into 1000mL beaker, 12h is stood.Solution layering, takes lower layer's yellow filtrate, is centrifuged.
Ultrapure water, stirring, centrifugation, until solution is in weakly acidic pH are added 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 ultrapure water, ultrasound keeps its dispersion equal
It is even.Dispersion liquid is transferred in 100mL hydrothermal reaction kettle, 180 DEG C of reaction 12h.After reaction, product is taken out, at -45 DEG C
Lower freeze-drying for 24 hours, obtains APTES-Sb2WO6- RGO optic catalytic composite material.X-ray powder diffraction pattern is as shown in Fig. 1,
Show that the made sample of the present invention is APTES-Sb2WO6-RGO.Solid uv drs map is as shown in Fig. 2, shows APTES-
Sb2WO6- RGO catalysis material has good absorbability to ultraviolet light.Transmission electron microscope image is as shown in Fig. 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, in the methyl orange of the ultraviolet light irradiation decline Xie Shuizhong of 11W, 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 Fig. 4, ultraviolet
Irradiating 6h rear decoloring rate is 100%.
Embodiment three:
Raw material proportioning is investigated to APTES-Sb2WO6The influence of-RGO photocatalysis effect.Weigh respectively 0.001g, 0.002g,
0.004g, 0.01g GO are scattered in 70mL ultrapure water, each that 0.2g APTES-Sb is added2WO6, ultrasound makes it be uniformly dispersed.It will
Dispersion liquid is transferred in 100mL hydrothermal reaction kettle, 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 sample, wherein GO and APTES-Sb2WO6Quality score
It Wei not 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 proportion2WO6- RGO sample every two hours samples one in the methyl orange of the ultraviolet light irradiation decline Xie Shuizhong of 11W
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 1:100 when, photocatalysis effect is best.
Claims (4)
1. a kind of APTES-Sb that can be applied to photo-catalytic degradation of methyl-orange2WO6The preparation method of-RGO composite material, 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 mixing evenly
Add SbCl3；Mixed liquor is transferred in 100mL hydrothermal reaction kettle, 180 DEG C of reaction 12h；The yellow solid precipitate of precipitation is centrifuged
It separates and is alternately washed each 3 times with dehydrated alcohol and ultrapure water, be put into baking oven drying, obtain Sb2WO6Catalysis material；
B, APTES-Sb is prepared2WO6Composite material: by Sb2WO6Catalysis material is dissolved in dehydrated alcohol, ultrasonic disperse and dropwise
It is added 3- aminopropyl triethoxysilane (APTES)；Water-bath keeps the temperature 4h, suction filtration, drying under the conditions of 70 DEG C, obtains APTES-
Sb2WO6Composite material；
C, it prepares graphite oxide (GO): weighing KMnO4And graphite powder, it is placed in a beaker and stirs evenly, it is spare；In three-necked flask
The concentrated sulfuric acid, phosphoric acid are sequentially added, KMnO is added slowly with stirring4With the mixture of graphite powder；48 DEG C of set temperature, water-bath is anti-
Answer 12h；After reaction, prepare 1000mL beaker, ice cube and H is added2O2, reaction solution is poured into 1000mL beaker, is stood
12h；Solution layering, takes lower layer's yellow filtrate, is centrifuged；Ultrapure water, stirring, centrifugation, until solution is in weakly acidic pH are added repeatedly；It will
Solution pours into culture dish, and standing 48h makes solvent volatilize, and obtains GO；
D, APTES-Sb is prepared2WO6- RGO optic catalytic composite material: APTES-Sb made from step b is weighed2WO6It is made with step c
GO, be scattered in ultrapure water, ultrasound makes it be uniformly dispersed；Dispersion liquid is transferred in 100mL hydrothermal reaction kettle, 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 material；
e、APTES-Sb2WO6- RGO optic catalytic composite material is applied to the methyl orange in degradation water: preparing certain density methyl
Orange solution, the APTES-Sb made from step d2WO6Methyl orange in-RGO optic catalytic composite material degradation water, 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 the degradation time used；Sb in step b2WO6Dosage is 0.1~1g, dehydrated alcohol dosage
For 100~500mL, APTES dosage is 0.1~5mL；APTES-Sb in step d2WO6Dosage is 0.1~1g, and GO dosage is
0.001~0.1g, ultrapure water consumption are 50~70mL.
2. a kind of APTES-Sb that can be applied to photo-catalytic degradation of methyl-orange according to claim 12WO6- RGO composite material
Preparation method, it is characterized in that: in the step a ethylene glycol in mixed solution proportion be 0.1~0.9, 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 material
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
Amount is 80~180mL, and phosphoric acid dosage is 1~20mL, H2O2Dosage is 5~15mL.
4. a kind of APTES-Sb that can be applied to photo-catalytic degradation of methyl-orange according to claim 12WO6- RGO composite material
Preparation method, it is characterized in that: in the step e methyl orange solution concentration be 1~100mg/L, APTES-Sb2WO6- RGO light
Concentration of the catalysis material in methyl orange solution is 0.01~1g/L, and the characteristic absorption peak of methyl orange is at 465nm.
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| 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 |
| CN106693908A (en) * | 2017-01-17 | 2017-05-24 | 河南理工大学 | Preparation method and application of nano composite material capable of simultaneously recognizing and efficient degrading tetracycline |
| CN107200361A (en) * | 2017-06-29 | 2017-09-26 | 济南大学 | A kind of rGO/Fe2O3The preparation method of nano composite material |
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| 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 |
| CN106693908A (en) * | 2017-01-17 | 2017-05-24 | 河南理工大学 | Preparation method and application of nano composite material capable of simultaneously recognizing and efficient degrading tetracycline |
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