CN106732661B - Bismuth sulfide-application of the fullerene hybrid material in photocatalysis denitrogenation - Google Patents
Bismuth sulfide-application of the fullerene hybrid material in photocatalysis denitrogenation Download PDFInfo
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- CN106732661B CN106732661B CN201611242599.5A CN201611242599A CN106732661B CN 106732661 B CN106732661 B CN 106732661B CN 201611242599 A CN201611242599 A CN 201611242599A CN 106732661 B CN106732661 B CN 106732661B
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- ammonia nitrogen
- fullerene
- based material
- bismuth sulfide
- bismuth
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- 229910003472 fullerene Inorganic materials 0.000 title claims abstract description 43
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 239000000463 material Substances 0.000 title claims abstract description 34
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 5
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 5
- 230000001699 photocatalysis Effects 0.000 title abstract description 7
- 238000007146 photocatalysis Methods 0.000 title abstract description 7
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 claims abstract description 54
- NNLOHLDVJGPUFR-UHFFFAOYSA-L calcium;3,4,5,6-tetrahydroxy-2-oxohexanoate Chemical compound [Ca+2].OCC(O)C(O)C(O)C(=O)C([O-])=O.OCC(O)C(O)C(O)C(=O)C([O-])=O NNLOHLDVJGPUFR-UHFFFAOYSA-L 0.000 claims abstract description 35
- 150000001875 compounds Chemical class 0.000 claims abstract description 30
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 12
- 238000005286 illumination Methods 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000007791 liquid phase Substances 0.000 claims description 9
- 229910001868 water Inorganic materials 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 6
- 230000003287 optical effect Effects 0.000 claims description 6
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 4
- 229910000069 nitrogen hydride Inorganic materials 0.000 claims description 4
- 238000003672 processing method Methods 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims 2
- 239000007788 liquid Substances 0.000 claims 1
- 238000004073 vulcanization Methods 0.000 claims 1
- 230000015556 catabolic process Effects 0.000 abstract description 21
- 238000006731 degradation reaction Methods 0.000 abstract description 21
- 239000003054 catalyst Substances 0.000 abstract description 10
- 230000003197 catalytic effect Effects 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 5
- 238000002835 absorbance Methods 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- NXMWOOVRJPJOSH-UHFFFAOYSA-N C1(=CC=CC=C1)O.C1(=CC=CC=C1)O.[Cl] Chemical compound C1(=CC=CC=C1)O.C1(=CC=CC=C1)O.[Cl] NXMWOOVRJPJOSH-UHFFFAOYSA-N 0.000 description 1
- 241001125671 Eretmochelys imbricata Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000000873 masking effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- LJCNRYVRMXRIQR-OLXYHTOASA-L potassium sodium L-tartrate Chemical compound [Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O LJCNRYVRMXRIQR-OLXYHTOASA-L 0.000 description 1
- 229940074439 potassium sodium tartrate Drugs 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 235000011006 sodium potassium tartrate Nutrition 0.000 description 1
- 238000002560 therapeutic procedure Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- WCTAGTRAWPDFQO-UHFFFAOYSA-K trisodium;hydrogen carbonate;carbonate Chemical compound [Na+].[Na+].[Na+].OC([O-])=O.[O-]C([O-])=O WCTAGTRAWPDFQO-UHFFFAOYSA-K 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
-
- 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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Toxicology (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of bismuth sulfide-application of the fullerene hybrid material in photocatalysis denitrogenation, comprising: is N by ammonia nitrogen degradation using the compound fullerene-based material of bismuth sulfide as photochemical catalyst under the conditions of near infrared light2And H2O.The method of the compound fullerene-based material catalytic degradation ammonia nitrogen of bismuth sulfide of the invention, has the function of molecular recognition and infrared photocatalytic degradation to ammonia nitrogen, ammonia nitrogen can be degraded to N under near infrared light2And H2O can still make degradation rate > 90% of ammonia nitrogen after the catalyst repeats catalytic degradation ammonia nitrogen 5~10 times.
Description
Technical field
The present invention relates to a kind of compound fullerene-based material of bismuth sulfide and its using near infrared light in catalytic degradation ammonia nitrogen
Using.
Background technique
It can solve environmental energy problem using the sun, utilize TiO originating from Fujishima in 19722Optoelectronic pole electrolysis water
Hydrogen manufacturing, subsequent Carey were reported in 1976 and are utilized TiO2The toxicity of more chlorine diphenol is eliminated in photochemical catalytic oxidation, from this, using too
Sun can degrade environmental contaminants research rapidly become people research hot spot.But TiO2It can only be left using solar energy 4% is accounted for
Right ultraviolet light, to TiO2It is doped and develops Fe2O3、WO3、Bi2WO6Equal new catalysts, although part is solved to can
Light-exposed Utilizing question, but account for the infrared light of solar energy nearly 50% it is still necessary to develop and use.
Summary of the invention
The main purpose of the present invention is to provide a kind of bismuth sulfide-fullerene hybrid material answering in photocatalysis denitrogenation
With to overcome deficiency in the prior art.
For realization aforementioned invention purpose, the technical solution adopted by the present invention includes:
The embodiment of the present invention provides a kind of compound fullerene-based material of bismuth sulfide photocatalysis drop under near infrared light illumination condition
Solve the purposes in ammonia nitrogen.
Further, the compound fullerene-based material of the bismuth sulfide includes fullerene and 1wt%~10wt% bismuth sulfide particle,
The bismuth sulfide is distributed in the chondritic of the fullerene surface and/or the fullerene.
Further, the specific surface area of the compound fullerene-based material of the bismuth sulfide is 10-80m2/g。
Further, the partial size of the compound fullerene-based material of the bismuth sulfide is 1.0-20nm, and adjacent bismuth sulfide interlamellar spacing is
0.54-0.84nm。
In some embodiments, the ammonia nitrogen includes NH3And/or NH4 +, but not limited to this.
In some embodiments, the wave-length coverage of the near infrared light is 780-2500nm.
The embodiment of the present invention also provides a kind of ammonia nitrogen purification method comprising: the compound fullerene-based material of bismuth sulfide is added
Liquid-phase system containing ammonia nitrogen, and with liquid-phase system described near infrared light illumination, make the ammonia nitrogen by photocatalytic degradation N2With
H2O。
In a little embodiments, the mass ratio of the compound fullerene-based material of the bismuth sulfide and ammonia nitrogen is 100mg:5-50mg.
Further, the liquid phase sample to be tested containing ammonia nitrogen and the compound fullerene-based material of bismuth sulfide are mixed into and are protected from light instead
It answers in device, and the optical filter that only near infrared light can be made to pass through is set at the illumination window for being protected from light device, later with light
It is protected from light device described in the irradiation of source, makes ammonia nitrogen therein by photocatalytic degradation N2And H2O。
Compared with prior art, the invention has the advantages that the compound fullerene-based material catalytic degradation of bismuth sulfide of the invention
The method of ammonia nitrogen, using near infrared light light by ammonia nitrogen degradation be N2And H2O, without adding extra oxidant, to reduce into
This, and after the catalyst repetition catalytic degradation ammonia nitrogen 5-10 times, the degradation rate of the ammonia nitrogen is still > 90%.
Detailed description of the invention
Fig. 1 is the compound fullerene-based material (C of bismuth sulfide obtained in the embodiment of the present invention 160-Bi2S3) ammonia nitrogen degradation rate with
The change curve of time；
Fig. 2 is the compound fullerene-based material (C of bismuth sulfide obtained in the embodiment of the present invention 160-Bi2S3) it is repeated 7 times rear ammonia nitrogen
The curve graph of degradation rate.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, with reference to the accompanying drawing to specific reality of the invention
The mode of applying is described in detail.The example of these preferred embodiments is illustrated in the accompanying drawings.Shown in attached drawing and according to
The embodiments of the present invention of attached drawing description are only exemplary, and the present invention is not limited to these embodiments.
Here, it should also be noted that, in order to avoid having obscured the present invention because of unnecessary details, in the accompanying drawings only
Show with closely related structure and/or processing step according to the solution of the present invention, and be omitted little with relationship of the present invention
Other details.
The embodiment of the present invention provides a kind of compound fullerene-based material of bismuth sulfide photocatalysis drop under near infrared light illumination condition
Solve the purposes in ammonia nitrogen.
Further, the compound fullerene-based material of the bismuth sulfide includes fullerene and 1wt%~10wt% bismuth sulfide particle,
The bismuth sulfide is distributed in the chondritic of the fullerene surface and/or the fullerene.
Further, the specific surface area of the compound fullerene-based material of the bismuth sulfide is 10-80m2/g。
Further, the partial size of the compound fullerene-based material of the bismuth sulfide is 1.0-20nm, and adjacent bismuth sulfide interlamellar spacing is
0.54-0.84nm。
In some embodiments, the ammonia nitrogen includes NH3And/or NH4 +, but not limited to this.
In some embodiments, the wave-length coverage of the near infrared light is 780-2500nm.
The embodiment of the present invention also provides a kind of processing method of ammonia nitrogen comprising: the compound fullerene-based material of bismuth sulfide is added
Enter the liquid-phase system containing ammonia nitrogen, and with liquid-phase system described near infrared light illumination, makes the ammonia nitrogen by photocatalytic degradation N2
And H2O。
In a little embodiments, the mass ratio of the compound fullerene-based material of the bismuth sulfide and ammonia nitrogen is 100mg:5-50mg.
Further, the liquid phase sample to be tested containing ammonia nitrogen and the compound fullerene-based material of bismuth sulfide are mixed into and are protected from light instead
It answers in device, and the optical filter that only near infrared light can be made to pass through is set at the illumination window for being protected from light device, later with light
It is protected from light device described in the irradiation of source, makes ammonia nitrogen therein by photocatalytic degradation N2And H2O。
In one more preferred embodiment, a kind of ammonia nitrogen purification method is specifically included:
(1) Photoreactor and optical filter are provided, to guarantee to only have near infrared radiation to enter Photoreactor；
(2) sample to be tested and the compound fullerene-based material of bismuth sulfide are added in the Photoreactor in step (1), covers optical filtering
Piece, then it is placed in illumination under light source, sample to be tested described in different time sections is measured in the light absorption value of visible light wave range；
(3) according to formula: ammonia nitrogen degradation rate=(1-Ci/C0) × 100%=(1-Ai/A0) × 100% calculates ammonia nitrogen
Degradation rate.
Further, light absorption value of the sample to be tested at 554nm is measured.
Further, after the compound fullerene-based material of the bismuth sulfide repeats catalytic degradation ammonia nitrogen 5-10 times, the degradation of ammonia nitrogen
Rate is still > 90%.
Technology of the invention is further explained below in conjunction with drawings and examples.
Embodiment 1
(1)C60-Bi2S3Preparation: weigh 0.6g bismuth nitrate and be dissolved in 20mL deionized water, it is molten to weigh 0.2g thiocarbamide later
It is uniformly mixed in 20mL deionized water and with bismuth nitrate solution, adjusts the pH of mixed liquor using the NaOH solution of 1mol/L later
Value is 10.0, adds 0.01g fullerene, mixed solution is transferred in autoclave, react 8h under the conditions of 150 DEG C,
It is cooled to room temperature, the C is made after filtration washing60-Bi2S3
(2) photocatalysis is tested: being encased the wall of cup of a 100ml beaker with masking foil, to avoid ultraviolet light and visible light
It into reaction system, is covered on beaker mouth with λ > 780nm cut-off type optical filter, to guarantee to only have near infrared radiation to enter light
300W ultraviolet-visible light lamp is placed in above reactor by reactor.Certain density ammonia nitrogen solution is added in beaker, uses
NaHCO3-Na2CO3(0.1mol/L) buffer solution adjusts pH value, and a certain amount of catalyst is added into beaker, is placed under light source,
Magnetic stirrer, per the absorbance for measuring remaining ammonia nitrogen solution every other hour.1ml ammonia nitrogen solution is taken, 1.5ml Na Shi is added to try
Agent, 1ml potassium sodium tartrate solution are diluted to 50ml, measure the absorbance at 388nm with T1901 ultraviolet-uisible spectrophotometer,
The degradation rate of ammonia nitrogen is calculated with this.
Ammonia nitrogen degradation rate=(1-Ci/C0) × 100%=(1-Ai/A0) × 100%
In formula, C0For the initial concentration of ammonia nitrogen, A0For the absorbance of initial soln, CiFor the concentration of remaining ammonia nitrogen, AiIt is surplus
The absorbance of remaining ammonia nitrogen.
Referring to Fig. 1, after photocatalytic degradation 8h, the degradation rate of ammonia nitrogen is 90%.
(4) stability of hybrid catalyst catalyst stability: is evaluated by multiple circulation experiment.C60-Bi2S=is urged
The degradation rate of agent continuous 7 catalytic degradation ammonia nitrogens under near infrared radiation.Therapy lasted 8h each time degrades each time
After, it washs to obtain catalyst by centrifuge separation, deionized water, is then further continued for that the catalyst is recycled.Referring to fig. 2
It is shown, in C60-Bi2S3After the 7 circulation degradations of catalyst photocatalytic degradation ammonia nitrogen, ammonia nitrogen removal frank is still 90% or more.
It should be appreciated that the technical concepts and features of above-described embodiment only to illustrate the invention, its object is to allow be familiar with this
The personage of item technology cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all
Equivalent change or modification made by Spirit Essence according to the present invention, should be covered by the protection scope of the present invention.
Claims (4)
1. purposes of the compound fullerene-based material of bismuth sulfide under near infrared light illumination condition in photocatalytic degradation ammonia nitrogen, feature exist
In, the compound fullerene-based material of bismuth sulfide is dissolved in 20mL deionized water the preparation method is as follows: weighing 0.6g bismuth nitrate, it
After weigh 0.2g thiocarbamide and be dissolved in 20mL deionized water and be uniformly mixed with bismuth nitrate solution, it is molten using the NaOH of 1mol/L later
The pH value that liquid adjusts mixed liquor is 10.0, adds 0.01g fullerene, mixed solution is transferred in autoclave, 150
8h is reacted under the conditions of DEG C, is cooled to room temperature, and the compound fullerene-based material of the bismuth sulfide is made after filtration washing；The ammonia nitrogen is
NH3And/or NH4 +；The wave-length coverage of the near infrared light is 780-2500nm.
2. a kind of processing method of ammonia nitrogen, characterized by comprising: the compound fullerene-based material addition of bismuth sulfide is contained ammonia nitrogen
Liquid-phase system, and with liquid-phase system described near infrared light illumination, make the ammonia nitrogen by photocatalytic degradation N2And H2O；
The compound fullerene-based material of bismuth sulfide is dissolved in 20mL deionized water the preparation method is as follows: weighing 0.6g bismuth nitrate,
0.2g thiocarbamide is weighed later to be dissolved in 20mL deionized water and be uniformly mixed with bismuth nitrate solution, uses the NaOH of 1mol/L later
The pH value that solution adjusts mixed liquor is 10.0, adds 0.01g fullerene, mixed solution is transferred in autoclave,
8h is reacted under the conditions of 150 DEG C, is cooled to room temperature, the compound fullerene-based material of the bismuth sulfide is made after filtration washing；The ammonia nitrogen
For NH3And/or NH4 +；The wave-length coverage of the near infrared light is 780-2500nm.
3. processing method as claimed in claim 2, it is characterised in that: the matter of the bismuth sulfide compound fullerene-based material and ammonia nitrogen
Amount is than being 100mg:5-50mg.
4. processing method as claimed in claim 2, characterized by comprising: by the liquid phase sample to be tested containing ammonia nitrogen and vulcanization
The compound fullerene-based material of bismuth, which is mixed into, to be protected from light in device, and is arranged at the illumination window for being protected from light device and can only be made
The optical filter that near infrared light passes through, later with light source irradiate described in be protected from light device, make ammonia nitrogen therein by photocatalytic degradation
N2And H2O。
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103086429A (en) * | 2013-01-28 | 2013-05-08 | 中南林业科技大学 | Preparation method of novel bismuth sulfide nanorods |
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| CN103086429A (en) * | 2013-01-28 | 2013-05-08 | 中南林业科技大学 | Preparation method of novel bismuth sulfide nanorods |
Non-Patent Citations (1)
| Title |
|---|
| "Bi2S3纳米材料的制备及性能研究";张小敏;《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》;20131115(第11期);第76页 |
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