CN109569681A - Silver nanoparticles loaded and the sodium tantalate composite photo-catalyst of graphite phase carbon nitride nanometer sheet and its preparation method and application - Google Patents
Silver nanoparticles loaded and the sodium tantalate composite photo-catalyst of graphite phase carbon nitride nanometer sheet and its preparation method and application Download PDFInfo
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- CN109569681A CN109569681A CN201710894327.1A CN201710894327A CN109569681A CN 109569681 A CN109569681 A CN 109569681A CN 201710894327 A CN201710894327 A CN 201710894327A CN 109569681 A CN109569681 A CN 109569681A
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- carbon nitride
- nanometer sheet
- phase carbon
- graphite phase
- sodium tantalate
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- 239000011734 sodium Substances 0.000 title claims abstract description 154
- 229910052708 sodium Inorganic materials 0.000 title claims abstract description 154
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 title claims abstract description 153
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 137
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 130
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 126
- 239000010439 graphite Substances 0.000 title claims abstract description 126
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 239000002131 composite material Substances 0.000 title claims abstract description 70
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052709 silver Inorganic materials 0.000 claims abstract description 14
- 239000004332 silver Substances 0.000 claims abstract description 14
- 238000007540 photo-reduction reaction Methods 0.000 claims abstract description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 33
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 239000000843 powder Substances 0.000 claims description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- 238000006555 catalytic reaction Methods 0.000 claims description 15
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Substances OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 229910052799 carbon Inorganic materials 0.000 claims description 12
- 239000002105 nanoparticle Substances 0.000 claims description 12
- 238000012545 processing Methods 0.000 claims description 12
- 239000003054 catalyst Substances 0.000 claims description 10
- 239000002135 nanosheet Substances 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims description 9
- 230000008859 change Effects 0.000 claims description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 6
- 239000004575 stone Substances 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 4
- 229920000877 Melamine resin Polymers 0.000 claims description 3
- 239000000654 additive Substances 0.000 claims description 3
- 230000000996 additive effect Effects 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 3
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 229910052715 tantalum Inorganic materials 0.000 claims description 3
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- -1 melamine Amine Chemical class 0.000 claims description 2
- 238000006722 reduction reaction Methods 0.000 claims 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 1
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 19
- 230000001699 photocatalysis Effects 0.000 abstract description 10
- 238000007146 photocatalysis Methods 0.000 abstract description 4
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- 238000005265 energy consumption Methods 0.000 abstract description 3
- 231100000614 poison Toxicity 0.000 abstract description 2
- 230000007096 poisonous effect Effects 0.000 abstract description 2
- 229910003256 NaTaO3 Inorganic materials 0.000 description 37
- YCIHPQHVWDULOY-FMZCEJRJSA-N (4s,4as,5as,6s,12ar)-4-(dimethylamino)-1,6,10,11,12a-pentahydroxy-6-methyl-3,12-dioxo-4,4a,5,5a-tetrahydrotetracene-2-carboxamide;hydrochloride Chemical group Cl.C1=CC=C2[C@](O)(C)[C@H]3C[C@H]4[C@H](N(C)C)C(=O)C(C(N)=O)=C(O)[C@@]4(O)C(=O)C3=C(O)C2=C1O YCIHPQHVWDULOY-FMZCEJRJSA-N 0.000 description 17
- 238000006731 degradation reaction Methods 0.000 description 12
- 230000015556 catabolic process Effects 0.000 description 10
- 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 9
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- 239000000463 material Substances 0.000 description 8
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- 229910052724 xenon Inorganic materials 0.000 description 4
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 4
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- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 2
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- 229930182555 Penicillin Natural products 0.000 description 1
- JGSARLDLIJGVTE-MBNYWOFBSA-N Penicillin G Chemical compound N([C@H]1[C@H]2SC([C@@H](N2C1=O)C(O)=O)(C)C)C(=O)CC1=CC=CC=C1 JGSARLDLIJGVTE-MBNYWOFBSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
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- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
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- 150000003385 sodium Chemical class 0.000 description 1
- 150000003388 sodium compounds Chemical class 0.000 description 1
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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
- B01J27/24—Nitrogen compounds
-
- 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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
-
- 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
- C02F2101/36—Organic compounds containing halogen
-
- 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
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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 silver nanoparticles loadeds and the sodium tantalate composite photo-catalyst of graphite phase carbon nitride nanometer sheet and its preparation method and application, the composite photo-catalyst is using sodium tantalate as carrier, load has graphite phase carbon nitride nanometer sheet on sodium tantalate, and sodium tantalate and graphite phase carbon nitride nanometer sheet surface are deposited with silver nano-grain.Preparation method includes preparation graphite phase carbon nitride nanometer sheet/sodium tantalate compound and deposits silver nano-grain on graphite phase carbon nitride nanometer sheet/sodium tantalate compound by photoreduction.Composite photo-catalyst of the invention has many advantages, such as that visible light-responded range is big, photocatalytic activity is high, stability is good, and preparation method has simple, easy to operate, at low cost, less energy consumption, do not generate poisonous and harmful substance, advantages of environment protection.The composite photo-catalyst can be used for handling antibiotic waste water and waste water from dyestuff, and antibiotic and dyestuff that can effectively in wastewater by photocatalysis have many advantages, such as that application method is simple, removal rate is high.
Description
Technical field
The invention belongs to function and service photochemical catalyst field, it is related to a kind of sodium tantalate composite photo-catalyst and preparation method thereof
And application, and in particular to the sodium tantalate composite photo-catalyst of a kind of silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet and its
Preparation method and application.
Background technique
Since nineteen eighty-two finds penicillin, all kinds of antibiotic are constantly found and are widely used in human production life
In.The use of antibiotic greatly strengthens the ability that the mankind resist bacterial infection, has saved the life of countless people.But closely
The excessive use of all kinds of antibiotic causes bacterial drug resistance to enhance over year, and comes as sanitary sewage, medical waste water and cultivation
Antibiotic in waste water is largely accumulated, and causes a series of problems to environment, as the antibiotic in environment can be tired by food chain
Human body is accumulated and reentered, great adverse effect is caused to the ecological balance, human health.Therefore, how water is effectively removed
Antibiotic in body be at this stage urgent need to resolve the technical issues of.
Currently, the method for antibiotic has photocatalytic degradation method, absorption method, chemical oxidization method and membrane separation process in processing water body
Deng.Wherein, photocatalytic method is because its is environmental-friendly, low energy consumption, at low cost, material is reusable and higher treatment effeciency etc. is excellent
Point is more and more valued by people.
Tantalates because its valence band with higher and due to lower conduction band positions in photocatalytic cleavage water and degradation water it is organic
There is preferable application prospect in the fields such as pollutant.Wherein, sodium tantalate (NaTaO3) because preparation method it is simple, it is nontoxic, and more
It degrades suitable for organic pollutants in water body.However, NaTaO3Biggish band gap width causes it that can only make to ultraviolet light response
Its photocatalysis performance is very limited, therefore obtains that a kind of visible light-responded range is big, photocatalytic activity is high, stability is good
Sodium tantalate composite photocatalyst material is of great significance for the organic pollutant in degradation water body.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the deficiencies in the prior art, provide a kind of visible light-responded range it is big,
The sodium tantalate composite photo-catalyst of photocatalytic activity is high, stability is good silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet
And its preparation method and application.
In order to solve the above technical problems, the invention adopts the following technical scheme:
A kind of sodium tantalate composite photo-catalyst of silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet is to carry with sodium tantalate
Body, load has graphite phase carbon nitride nanometer sheet, the sodium tantalate and the graphite phase carbon nitride nanometer sheet table on the sodium tantalate
Face is deposited with silver nano-grain.
In the sodium tantalate composite photo-catalyst of above-mentioned silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet, further
It is improved, sodium tantalate described in the sodium tantalate composite photo-catalyst of the silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet
Mass ratio with the graphite phase carbon nitride nanometer sheet is 1: 0.05~0.1；The silver nanoparticles loaded and graphite-phase nitridation
The mass percent of silver nano-grain described in the sodium tantalate composite photo-catalyst of carbon nanosheet is 0.5%~1%.
In the sodium tantalate composite photo-catalyst of above-mentioned silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet, further
Improved, the sodium tantalate is the positive six faces nanocube of monocrystalline.
As a general technical idea, the present invention also provides a kind of above-mentioned silver nanoparticles loadeds and graphite-phase nitrogen
Change the preparation method of the sodium tantalate composite photo-catalyst of carbon nanosheet, comprising the following steps:
S1, it disperses sodium tantalate and graphite phase carbon nitride nanometer sheet in solvent, ultrasonic disperse obtains sodium tantalate and graphite-phase nitrogen
Change the suspension of carbon nanosheet；
Solvent in the suspension of S2, the removal sodium tantalate and graphite phase carbon nitride nanometer sheet, obtained solid is heated,
Obtain graphite phase carbon nitride nanometer sheet/sodium tantalate compound；
S3, it disperses the graphite phase carbon nitride nanometer sheet/sodium tantalate compound in methanol solution, Ag is added+Solution carries out
Photoreduction obtains the sodium tantalate composite photo-catalyst of silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet.
Further improved in above-mentioned preparation method, the sodium tantalate is by Ta2O5Ethylene glycol mixture and hydrogen-oxygen
It is made after changing sodium solution mixing through hydro-thermal reaction；The Ta2O5Ethylene glycol mixture in Ta2O5It is molten with the sodium hydroxide
The mass ratio of the sodium hydroxide of liquid is 0.4~0.5: 0.8~1.6；The temperature of the hydro-thermal reaction is 140 DEG C~150 DEG C；It is described
The time of hydro-thermal reaction is the h of 12 h~15.
Further improved in above-mentioned preparation method, the graphite phase carbon nitride nanometer sheet is by graphite phase carbon nitride
Powder is heat-treated the h of 1 h~2 at 520 DEG C~550 DEG C and is made；The graphite phase carbon nitride powder is by melamine 500
DEG C~520 DEG C at be heat-treated the h of 2 h~4 be made.
Further improved in above-mentioned preparation method, in step S1, the solvent is methanol；The ultrasonic disperse
Time is the min of 30 min~60；
And/or in step S2, the heating carries out in a nitrogen atmosphere；The temperature of the heating is 500 DEG C~550 DEG C；It is described
The time of heating is the h of 3 h~5；
And/or in step S3, the volume ratio of methanol and water is 1: 1~5 in the methanol solution；The Ag+Ag in solution+'s
Concentration is the g/L of 1 g/L~3；The Ag+Solution is AgNO3Solution；The photoreduction carries out under agitation；It is described
The time of photoreduction is 30min~60min.
As a general technical idea, the present invention also provides a kind of above-mentioned silver nanoparticles loadeds and graphite-phase nitrogen
Change application of the sodium tantalate composite photo-catalyst of carbon nanosheet in processing antibiotic waste water.
It is further improved, comprising the following steps: by silver nanoparticles loaded and graphite phase carbon nitride in above-mentioned application
The sodium tantalate composite photo-catalyst of nanometer sheet mixes under light protected environment with antibiotic waste water, gained mixed liquor under visible light into
The processing to antibiotic waste water is completed in row light-catalyzed reaction；The silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet
The additive amount of sodium tantalate composite photo-catalyst is that silver nanoparticles loaded and graphite-phase nitrogen are added in every liter of antibiotic waste water
Change sodium tantalate composite photo-catalyst 0.5 g~1.0 g of carbon nanosheet.
Further improved in above-mentioned application, the antibiotic in the antibiotic waste water is quadracycline；It is described anti-
The concentration of antibiotic is the mg/L of 20 mg/L~50 in raw element waste water；
And/or the light-catalyzed reaction carries out under the visible light of wavelength > 420nm；
And/or the time of the light-catalyzed reaction is the min of 30 min~60.
As a general technical idea, the present invention also provides a kind of above-mentioned silver nanoparticles loadeds and graphite-phase nitrogen
Change application of the sodium tantalate composite photo-catalyst of carbon nanosheet in processing waste water from dyestuff.
It is further improved, comprising the following steps: by silver nanoparticles loaded and graphite phase carbon nitride in above-mentioned application
The sodium tantalate composite photo-catalyst of nanometer sheet mixes under light protected environment with waste water from dyestuff, and gained mixed liquor carries out under visible light
The processing to waste water from dyestuff is completed in light-catalyzed reaction；The tantalic acid of the silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet
The additive amount of sodium composite photo-catalyst is that addition silver nanoparticles loaded and graphite phase carbon nitride are received in every liter of waste water from dyestuff
Sodium tantalate composite photo-catalyst 0.5 g~1.0 g of rice piece.
Further improved in above-mentioned application, dyestuff is rhodamine B in the waste water from dyestuff；In the waste water from dyestuff
The concentration of dyestuff is the mg/L of 20 mg/L~50；
And/or the light-catalyzed reaction carries out under the visible light of wavelength > 420nm；
And/or the time of the light-catalyzed reaction is the min of 30 min~60.
Compared with the prior art, the advantages of the present invention are as follows:
1, the present invention provides the sodium tantalate composite photo-catalyst of a kind of silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet,
With sodium tantalate (NaTaO3) it is carrier, graphite phase carbon nitride (g-C3N4) nanometer sheet is supported on sodium tantalate, stone sodium tantalate and described
The surface of graphite phase carbon nitride nanometer sheet is deposited with silver nano-grain.In the present invention, graphite phase carbon nitride nanometer sheet is supported on
On sodium tantalate, due to g-C3N4There is preferable response to visible light, composite material can be enhanced to the utilization rate of visible light, pass through g-
C3N4And NaTaO3Hetero-junctions is formed, light induced electron and hole concentrate on g-C respectively3N4Conduction band and NaTaO3Valence band, favorably
In the separation of photo-generate electron-hole, while surface A g nano particle can not only be acted on by SPR and further enhance catalyst to can
Light-exposed is absorbed and utilized performance, moreover it is possible to serve as the bridge of light induced electron transhipment in the composite, promote photo-generate electron-hole point
From.
2, the present invention also provides the sodium tantalate complex lights of a kind of silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet
The preparation method of catalyst has simple, easy to operate, at low cost, less energy consumption, does not generate poisonous and harmful substance, is environmental-friendly
The advantages that.
3, in preparation method of the invention, graphite phase carbon nitride nanometer sheet is supported on sodium tantalate by infusion process and is formed
Graphite phase carbon nitride nanometer sheet/sodium tantalate compound, wherein by graphite phase carbon nitride nanometer sheet in conjunction with sodium tantalate after in nitrogen
High-temperature process is carried out under atmosphere, so that the combination of the two is even closer, while silver nano-grain is raw by photo-reduction sedimentation
The surface in graphite phase carbon nitride nanometer sheet and sodium tantalate is grown, so that stability of material is good.
4, the present invention also provides a kind of method for handling antibiotic waste water, using silver nanoparticles loaded of the invention and
The sodium tantalate composite photo-catalyst of graphite phase carbon nitride nanometer sheet handles antibiotic waste water, being capable of effective photocatalytic degradation
Antibiotic in waste water has many advantages, such as that application method is simple, removal rate is high.
5, the present invention also provides a kind of methods for handling waste water from dyestuff, using silver nanoparticles loaded and stone of the invention
The sodium tantalate composite photo-catalyst of black phase carbon nitride nanometer sheet handles waste water from dyestuff, being capable of effective wastewater by photocatalysis
In dyestuff, have many advantages, such as that application method is simple, removal rate is high.
Detailed description of the invention
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, the technical scheme in the embodiment of the invention is clearly and completely described.
Fig. 1 is the scanning electron microscope (SEM) photograph of sodium tantalate powder in the embodiment of the present invention 1.
Fig. 2 is the sodium tantalate complex light of silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet in the embodiment of the present invention 1
The transmission electron microscope picture of catalyst.
Fig. 3 is sodium tantalate (NaTaO in the embodiment of the present invention 13) powder, graphite phase carbon nitride (g-C3N4) nanometer sheet, graphite
Phase carbon nitride nanometer sheet/sodium tantalate compound (g-C3N4/NaTaO3) and silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet
Sodium tantalate composite photo-catalyst (Ag/g-C3N4/NaTaO3) XRD diagram.
Fig. 4 is sodium tantalate (NaTaO in the embodiment of the present invention 13) powder, graphite phase carbon nitride (g-C3N4) nanometer sheet, graphite
Phase carbon nitride nanometer sheet/sodium tantalate compound (g-C3N4/NaTaO3) and silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet
Sodium tantalate composite photo-catalyst (Ag/g-C3N4/NaTaO3) ultraviolet-visible diffuse reflectance spectrum figure.
Fig. 5 is sodium tantalate (NaTaO in the embodiment of the present invention 23) powder, graphite phase carbon nitride (g-C3N4) nanometer sheet, graphite
Phase carbon nitride nanometer sheet/sodium tantalate compound (g-C3N4/NaTaO3) and silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet
Sodium tantalate composite photo-catalyst (Ag/g-C3N4/NaTaO3) quadracycline concentration changes with time during catalytic degradation
Relation schematic diagram.
Fig. 6 is the sodium tantalate complex light of silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet in the embodiment of the present invention 3
The relation schematic diagram of rhodamine B concentration changes with time in catalyst degradation process.
Fig. 7 is the sodium tantalate complex light of silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet in the embodiment of the present invention 4
Catalyst degradation quadracycline recycles figure.
Specific embodiment
Below in conjunction with Figure of description and specific preferred embodiment, the invention will be further described, but not therefore and
It limits the scope of the invention.
Raw material employed in following embodiment and instrument are commercially available；Wherein light-source system is PLS-SXE 300C xenon
Lamp is purchased from Beijing Bo Feilai Science and Technology Ltd..In following embodiment, unless otherwise noted, the data obtained is more than three times
Repeat the average value of experiment.
Embodiment 1
A kind of sodium tantalate composite photo-catalyst of silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet is to carry with sodium tantalate
Body, load has graphite phase carbon nitride nanometer sheet on sodium tantalate, and sodium tantalate and graphite phase carbon nitride nanometer sheet surface are deposited with Yin Na
Rice grain.
In the present embodiment, tantalum in the sodium tantalate composite photo-catalyst of silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet
Sour sodium and the mass ratio of graphite phase carbon nitride nanometer sheet are 1: 0.05.
It is silver-colored in the sodium tantalate composite photo-catalyst of silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet in the present embodiment
The mass percent of nano particle is 1%.
In the present embodiment, sodium tantalate is the positive six faces nanocube of monocrystalline.
In the present embodiment, graphite phase carbon nitride nanometer sheet is supported on sodium tantalate by infusion process forms graphite phase carbon nitride
Nanometer sheet/sodium tantalate compound；It is compound that silver nano-grain by photoreduction met hod is deposited on graphite phase carbon nitride nanometer sheet/sodium tantalate
Graphite phase carbon nitride nanometer sheet in object and sodium tantalate surface form silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet
Sodium tantalate composite photo-catalyst.
A kind of sodium tantalate complex light of silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet in above-mentioned the present embodiment
The preparation method of catalyst, comprising the following steps:
(1) 1 g sodium tantalate (NaTaO is taken3) powder ultrasonic is scattered in 50 mL methanol, 50 mg graphite phase carbon nitrides are added
(g-C3N4) nanometer sheet, 30 min of ultrasonic disperse obtains the suspension of sodium tantalate Yu graphite phase carbon nitride nanometer sheet.
(2) under room temperature (20 DEG C~30 DEG C), by sodium tantalate obtained in step (1) and graphite phase carbon nitride nanometer sheet
Suspension lasts stirring, until methanol volatilization is complete.Obtained solid is placed in tube furnace, in a nitrogen atmosphere with 2 DEG C/
The heating rate of min rises to 500 DEG C from room temperature, keeps 3 h, is cooled to room temperature, obtains powdered graphite phase carbon nitride nanometer
Piece/sodium tantalate compound (g-C3N4/NaTaO3).
(3) 1.0 g g-C obtained in step (2) is taken3N4/NaTaO3Powder ultrasonic is scattered in 50 mL methanol solution (first
The volume ratio of methanol and water is 1: 4 in alcoholic solution, i.e., volumetric concentration be 20%) in, 7.8 mL, dense are added dropwise into gained mixed liquor
Degree is the AgNO of 2 g/L3Solution, the after mixing evenly illumination under 300W xenon lamp carry out photoreduction 30 under agitation
Min, sodium tantalate and graphite phase carbon nitride nanometer sheet surface deposition silver in graphite phase carbon nitride nanometer sheet/sodium tantalate compound
Nano particle, suction filtration are isolated solid product, are washed three times with deionized water and dehydrated alcohol respectively, dry 12 at 80 DEG C
H obtains the sodium tantalate composite photo-catalyst (Ag/g-C of silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet3N4/
NaTaO3).
In the step of the present embodiment preparation method (1), sodium tantalate powder used is prepared by following methods: by 1.20 g
NaOH is dissolved in 30 mL deionized waters, obtains sodium hydroxide solution.By 0.442 g Ta2O510 mL ethylene glycol are scattered in, are obtained
Ta2O5Ethylene glycol mixture.By sodium hydroxide solution and Ta2O5Ethylene glycol mixture be uniformly mixed, be added 50 mL reaction
In kettle, 12 h of hydro-thermal reaction is carried out at 140 DEG C.It is cooled to room temperature to reaction kettle, isolates solid product by filtering, respectively
It is washed three times with deionized water and dehydrated alcohol, dry 12 h at 80 DEG C, obtain sodium tantalate powder in baking oven.The sodium tantalate
Powder is a kind of nanocube material.
In the step of the present embodiment preparation method (1), graphite phase carbon nitride nanometer sheet used is prepared by following methods:
By g-C3N4Powder is placed in ceramic crucible, is put into Muffle furnace, is risen to 550 DEG C from room temperature with the heating rate of 2 DEG C/min, is protected
Hold 2 h(and be heat-treated 2h at 550 DEG C), it is cooled to room temperature, obtains graphite phase carbon nitride nanometer sheet.Wherein, g-C3N4Powder by
Following methods are prepared: take melamine to be laid in square ceramic crucible, close the lid, be put into Muffle furnace, with 2 DEG C/
The heating rate of min rises to 500 DEG C from room temperature, and 3 h(is kept to be heat-treated 3h at 500 DEG C), it is cooled to room temperature, is ground,
Obtain g-C3N4Powder.
Electron microscope analysis is scanned to sodium tantalate powder obtained in embodiment 1, as a result as shown in Figure 1.Fig. 1 is the present invention
The scanning electron microscope (SEM) photograph of sodium tantalate powder in embodiment 1.As shown in Figure 1, the NaTaO of preparation3Shape is regular, receives for positive six face of monocrystalline
Rice cube.
To the sodium tantalate composite photocatalyst of silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet obtained in embodiment 1
Agent carries out transmission electron microscope analysis, as a result as shown in Figure 2.Fig. 2 is silver nanoparticles loaded and graphite-phase nitrogen in the embodiment of the present invention 1
Change the transmission electron microscope picture of the sodium tantalate composite photo-catalyst of carbon nanosheet.As shown in Figure 2, graphite phase carbon nitride nanometer sheet is supported on
On sodium tantalate, silver nano-grain is deposited on the graphite phase carbon nitride nanometer in graphite phase carbon nitride nanometer sheet/sodium tantalate compound
Piece and sodium tantalate surface, this explanation have successfully loaded g-C in sodium tantalate nanocube3N4Nanometer sheet and Ag nano particle, i.e.,
The sodium tantalate composite photo-catalyst of success obtained silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet.
To the sodium tantalate (NaTaO being prepared in embodiment 13) powder, graphite phase carbon nitride (g-C3N4) nanometer sheet, stone
Black phase carbon nitride nanometer sheet/sodium tantalate compound (g-C3N4/NaTaO3) and silver nanoparticles loaded and graphite phase carbon nitride nanometer
Sodium tantalate composite photo-catalyst (the Ag/g-C of piece3N4/NaTaO3) XRD analysis is carried out, as a result as shown in Figure 3.Fig. 3 is the present invention
Sodium tantalate (NaTaO in embodiment 13) powder, graphite phase carbon nitride (g-C3N4) nanometer sheet, graphite phase carbon nitride nanometer sheet/tantalic acid
Sodium compound (g-C3N4/NaTaO3) and silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet sodium tantalate composite photocatalyst
Agent (Ag/g-C3N4/NaTaO3) XRD diagram.From the figure 3, it may be seen that NaTaO3And g-C3N4Respective characteristic peak only all is shown, and
g-C3N4/NaTaO3And Ag/g-C3N4/NaTaO3Then contain NaTaO3And g-C3N4The characteristic peak of two kinds of substances, this also indicates that this
Two kinds of composite materials are successfully prepared.Ag nano particle can not see apparent characteristic peak because of content very little.
To the sodium tantalate (NaTaO being prepared in embodiment 13) powder, graphite phase carbon nitride (g-C3N4) nanometer sheet, stone
Black phase carbon nitride nanometer sheet/sodium tantalate compound (g-C3N4/NaTaO3) and silver nanoparticles loaded and graphite phase carbon nitride nanometer
Sodium tantalate composite photo-catalyst (the Ag/g-C of piece3N4/NaTaO3) UV-Vis DRS analysis is carried out, as a result as shown in Figure 4.
Fig. 4 is sodium tantalate (NaTaO in the embodiment of the present invention 13) powder, graphite phase carbon nitride (g-C3N4) nanometer sheet, graphite phase carbon nitride
Nanometer sheet/sodium tantalate compound (g-C3N4/NaTaO3) and silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet sodium tantalate
Composite photo-catalyst (Ag/g-C3N4/NaTaO3) ultraviolet-visible diffuse reflectance spectrum figure.As shown in Figure 4, in NaTaO3Upper load
G-C3N4Obvious red shift occurs for the visible absorption side of material after nanometer sheet, and material is 470 after having modified Ag nano particle
Nm nearby has the absorption peak of apparent SPR effect, this illustrates g-C3N4Introducing with Ag nano particle can effectively improve the present invention
The optical response range of composite photo-catalyst, to improve the photocatalysis performance and the efficiency of light energy utilization of material, this equally also illustrates Ag
Nano particle is successfully introduced into composite material.
Embodiment 2
The sodium tantalate composite photo-catalyst of a kind of silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet is at processing hydrochloric acid Fourth Ring
Application in plain waste water, comprising the following steps:
The sodium tantalate complex light for weighing silver nanoparticles loaded made from 50 mg embodiments 1 and graphite phase carbon nitride nanometer sheet is urged
Agent is added in the quadracycline waste water that 50 mL initial concentrations are 20 mg/L under the conditions of being protected from light, stirs 30 min, reach
Mixed liquor is placed in photocatalytic reaction device after to adsorption equilibrium, using the 300W xenon for having 420 nm ultraviolet cut-off filters
Lamp is that light source carries out 60 min of light-catalyzed reaction, completes the processing to quadracycline waste water.
During light-catalyzed reaction, every 10 minutes sample, sample is centrifuged, supernatant is taken, with it is ultraviolet-
Visible spectrophotometer measures its concentration, as a result as shown in Figure 5.
Meanwhile with sodium tantalate (NaTaO obtained in embodiment 13) powder, graphite phase carbon nitride (g-C3N4) nanometer sheet, stone
Black phase carbon nitride nanometer sheet/sodium tantalate compound (g-C3N4/NaTaO3) above-mentioned silver nanoparticles loaded and graphite-phase is replaced to nitrogenize
The sodium tantalate composite photo-catalyst of carbon nanosheet handles quadracycline waste water under the same conditions.In light-catalyzed reaction process
In, it was sampled every 10 minutes, sample is centrifuged, supernatant is taken, it is dense to measure its with ultraviolet-visible spectrophotometer
Degree, as a result as shown in Figure 5.
Fig. 5 is sodium tantalate (NaTaO in the embodiment of the present invention 23) powder, graphite phase carbon nitride (g-C3N4) nanometer sheet, graphite
Phase carbon nitride nanometer sheet/sodium tantalate compound (g-C3N4/NaTaO3) and silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet
Sodium tantalate composite photo-catalyst (Ag/g-C3N4/NaTaO3) quadracycline concentration changes with time during catalytic degradation
Relation schematic diagram.As shown in Figure 5, under visible light illumination, NaTaO3There is no degradation, three kinds of materials to quadracycline
Quadracycline content is substantially reduced in the waste water of processing, wherein Ag/g-C3N4/NaTaO3To the degradation efficiency of quadracycline
It is apparently higher than g-C3N4And g-C3N4/NaTaO3.After 60 min of illumination, Ag/g-C3N4/NaTaO3Removal to quadracycline
Rate reaches 91.48%, and g-C3N4And g-C3N4/NaTaO3Removal rate to quadracycline is only 51.74% and 82.46%.Thus
It is found that the sodium tantalate composite photo-catalyst of silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet of the invention can effectively drop
The quadracycline in waste water is solved, realizes and antibiotic in waste water is effectively removed, this is because composite photocatalyst of the present invention
It is compound using sodium tantalate and graphite phase carbon nitride nanometer sheet by the way that graphite phase carbon nitride nanometer sheet to be supported on sodium tantalate in agent
The hetero-junctions of formation, can be improved the hollow separative efficiency of light induced electron, at the same by by Ag nanoparticle deposition in graphite-phase
Azotized carbon nano piece and sodium tantalate surface, further enhance composite photo-catalyst to visible light be absorbed and utilized and photocatalytic
Can, so as to which the light degradation ability to quadracycline is greatly improved.
Embodiment 3
The sodium tantalate composite photo-catalyst of a kind of silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet is useless in processing rhodamine B
Application in water, comprising the following steps:
The sodium tantalate complex light for weighing silver nanoparticles loaded made from 50 mg embodiments 1 and graphite phase carbon nitride nanometer sheet is urged
Agent is added in the rhodamine B that 50 mL initial concentrations are 20 mg/L under the conditions of being protected from light, stirs 30 min, reach
After adsorption equilibrium, gained mixed liquor is placed in photocatalytic reaction device, using with 420 nm ultraviolet cut-off filters
300W xenon lamp is that light source carries out 60 min of light-catalyzed reaction, completes the processing to rhodamine B.
During light-catalyzed reaction, every 10 minutes sample, sample is centrifuged, supernatant is taken, with it is ultraviolet-
Visible spectrophotometer measures its concentration, as a result as shown in Figure 6.
Fig. 6 is the sodium tantalate complex light of silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet in the embodiment of the present invention 3
The relation schematic diagram of rhodamine B concentration changes with time in catalyst degradation process.It will be appreciated from fig. 6 that under visible light, this
Sodium tantalate composite photo-catalyst (the Ag/g-C of invention silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet3N4/NaTaO3) right
Rhodamine B has preferable degradation, after 60 min of illumination, Ag/g-C3N4/NaTaO3The removal rate of rhodamine B is reached
95.49%.It follows that the sodium tantalate composite photocatalyst of silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet of the invention
Agent can effectively in degrading waste water rhodamine B, realize and Wastewater Dyes effectively removed.
Embodiment 4
The stability of the sodium tantalate composite photo-catalyst of silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet of the present invention is investigated,
The following steps are included:
(1) the remaining reaction solution after light-catalyzed reaction in embodiment 2 is centrifuged, collects silver nanoparticles loaded and graphite
The sodium tantalate composite photo-catalyst of phase carbon nitride nanometer sheet is washed three times with deionized water and dehydrated alcohol respectively, is then placed
Dry 12 h in 60 DEG C of baking ovens.
(2) processing method in the same manner as in Example 2 is used, the load silver obtained after drying in step (1) is reused
Nano particle and the sodium tantalate composite photo-catalyst of graphite phase carbon nitride nanometer sheet handle quadracycline waste water, altogether into
5 repetitions of row are tested.
Fig. 7 is the sodium tantalate complex light of silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet in the embodiment of the present invention 4
Catalyst degradation quadracycline recycles figure.As shown in Figure 7, after 5 times are recycled, the present invention loads silver nanoparticle
Particle and the sodium tantalate composite photo-catalyst of graphite phase carbon nitride nanometer sheet in 60 min to the removal rate of quadracycline still
It is so up to 80% or more, this illustrates that the sodium tantalate complex light of silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet of the present invention is urged
Agent is with good stability and reusing.
Above embodiments are only the preferred embodiment of the present invention, and protection scope of the present invention is not limited merely to above-mentioned reality
Apply example.All technical solutions belonged under thinking of the present invention all belong to the scope of protection of the present invention.It is noted that being led for this technology
For the those of ordinary skill in domain, improvements and modifications without departing from the principle of the present invention, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (10)
1. the sodium tantalate composite photo-catalyst of a kind of silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet, which is characterized in that
Using sodium tantalate as carrier, load has graphite phase carbon nitride nanometer sheet, the sodium tantalate and the graphite-phase nitrogen on the sodium tantalate
Change carbon nanosheet surface and is deposited with silver nano-grain.
2. the sodium tantalate complex light of silver nanoparticles loaded according to claim 1 and graphite phase carbon nitride nanometer sheet is urged
Agent, which is characterized in that in the sodium tantalate composite photo-catalyst of the silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet
The sodium tantalate and the mass ratio of the graphite phase carbon nitride nanometer sheet are 1: 0.05~0.1；The silver nanoparticles loaded and
The mass percent of silver nano-grain described in the sodium tantalate composite photo-catalyst of graphite phase carbon nitride nanometer sheet is 0.5%~1%.
3. according to claim 1 or the sodium tantalate of silver nanoparticles loaded described in 2 and graphite phase carbon nitride nanometer sheet is compound
Photochemical catalyst, which is characterized in that the sodium tantalate is the positive six faces nanocube of monocrystalline.
4. a kind of tantalum of silver nanoparticles loaded according to any one of claims 1 to 3 and graphite phase carbon nitride nanometer sheet
The preparation method of sour sodium composite photo-catalyst, which comprises the following steps:
S1, it disperses sodium tantalate and graphite phase carbon nitride nanometer sheet in solvent, ultrasonic disperse obtains sodium tantalate and graphite-phase nitrogen
Change the suspension of carbon nanosheet；
Solvent in the suspension of S2, the removal sodium tantalate and graphite phase carbon nitride nanometer sheet, obtained solid is heated,
Obtain graphite phase carbon nitride nanometer sheet/sodium tantalate compound；
S3, it disperses the graphite phase carbon nitride nanometer sheet/sodium tantalate compound in methanol solution, Ag is added+Solution carries out light
Reduction reaction obtains the sodium tantalate composite photo-catalyst of silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet.
5. preparation method according to claim 4, which is characterized in that the sodium tantalate is by Ta2O5Ethylene glycol mixing
Liquid is made after mixing with sodium hydroxide solution through hydro-thermal reaction；The Ta2O5Ethylene glycol mixture in Ta2O5With the hydrogen
The mass ratio of the sodium hydroxide of sodium hydroxide solution is 0.4~0.5: 0.8~1.6；The temperature of the hydro-thermal reaction be 140 DEG C~
150℃；The time of the hydro-thermal reaction is the h of 12 h~15.
6. preparation method according to claim 5, which is characterized in that the graphite phase carbon nitride nanometer sheet is by graphite
Phase carbon nitride powder is heat-treated the h of 1 h~2 at 520 DEG C~550 DEG C and is made；The graphite phase carbon nitride powder is by melamine
Amine is heat-treated the h of 2 h~4 at 500 DEG C~520 DEG C and is made.
7. the preparation method according to any one of claim 4~6, which is characterized in that in step S1, the solvent is first
Alcohol；The time of the ultrasonic disperse is the min of 30 min~60；
And/or in step S2, the heating carries out in a nitrogen atmosphere；The temperature of the heating is 500 DEG C~550 DEG C；It is described
The time of heating is the h of 3 h~5；
And/or in step S3, the volume ratio of methanol and water is 1: 1~5 in the methanol solution；The Ag+Ag in solution+It is dense
Degree is the g/L of 1 g/L~3；The Ag+Solution is AgNO3Solution；The photoreduction carries out under agitation；The light
The time of reduction reaction is 30min~60min.
8. a kind of tantalum of silver nanoparticles loaded according to any one of claims 1 to 3 and graphite phase carbon nitride nanometer sheet
Application of the sour sodium composite photo-catalyst in processing antibiotic waste water or waste water from dyestuff.
9. application according to claim 8, which comprises the following steps: by silver nanoparticles loaded and stone
The sodium tantalate composite photo-catalyst of black phase carbon nitride nanometer sheet mixes under light protected environment with antibiotic waste water or waste water from dyestuff, institute
It obtains mixed liquor and carries out light-catalyzed reaction under visible light, complete the processing to antibiotic waste water or waste water from dyestuff；The load silver
The additive amount of nano particle and the sodium tantalate composite photo-catalyst of graphite phase carbon nitride nanometer sheet is every liter of antibiotic waste water
Or added in waste water from dyestuff 0.5 g of sodium tantalate composite photo-catalyst of silver nanoparticles loaded and graphite phase carbon nitride nanometer sheet~
1.0 g。
10. application according to claim 9, which is characterized in that the antibiotic in the antibiotic waste water is hydrochloric acid four
Ring element；The concentration of antibiotic is the mg/L of 20 mg/L~50 in the antibiotic waste water；Dyestuff is Luo Dan in the waste water from dyestuff
Bright B；The concentration of dyestuff is the mg/L of 20 mg/L~50 in the waste water from dyestuff；
And/or the light-catalyzed reaction carries out under the visible light of wavelength > 420nm；
And/or the time of the light-catalyzed reaction is the min of 30 min~60.
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