CN106179304A - A kind of CeO possessing photo catalytic reduction performance2tiO2the preparation method of nano composite material - Google Patents
A kind of CeO possessing photo catalytic reduction performance2tiO2the preparation method of nano composite material Download PDFInfo
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- CN106179304A CN106179304A CN201610599195.5A CN201610599195A CN106179304A CN 106179304 A CN106179304 A CN 106179304A CN 201610599195 A CN201610599195 A CN 201610599195A CN 106179304 A CN106179304 A CN 106179304A
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- 239000000463 material Substances 0.000 title claims abstract description 32
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 18
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 18
- 238000010531 catalytic reduction reaction Methods 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 38
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- 229910004631 Ce(NO3)3.6H2O Inorganic materials 0.000 claims abstract description 8
- 238000005119 centrifugation Methods 0.000 claims abstract description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 239000000376 reactant Substances 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims abstract description 3
- 238000001354 calcination Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000012065 filter cake Substances 0.000 claims description 2
- 239000000047 product Substances 0.000 claims description 2
- 238000007146 photocatalysis Methods 0.000 abstract description 7
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 3
- 239000003643 water by type Substances 0.000 abstract description 3
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 2
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 244000309464 bull Species 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000010041 electrostatic spinning Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
- 150000002602 lanthanoids Chemical class 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 238000006053 organic reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 230000001603 reducing effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
-
- 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
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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)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention discloses a kind of CeO possessing photo catalytic reduction performance2‑TiO2The preparation method of nano composite material.The method is specifically by Ce (NO3)3.6H2O dissolves in ethanol, is dissolved in by tetrabutyl titanate in the mixed liquor of ethanol and deionized water, is uniformly dispersed mixing under conditions of ultrasonic in above two solution；Gained reactant mixture is put into hydrothermal reaction kettle, 120 DEG C of reaction 48h；Then carry out centrifugation after product being cooled to room temperature, wash, dry and calcine, obtain CeO2‑TiO2Nano composite material.Preparation method of the present invention is simple, easily operates, the CeO prepared2‑TiO2Nano composite material can be effectively applied to the photocatalysis improvement that Heavy Metals in Waters pollutes.
Description
Technical field
The present invention relates to a kind of CeO possessing photo catalytic reduction performance2-TiO2The preparation method of nano composite material, specifically
Belong to catalysis material technical field.
Background technology
Photocatalysis technology has economy, efficiently, does not easily cause the advantages such as secondary pollution, obtains in processing environment pollutant
It is widely applied.The most the most frequently used catalysis material is TiO2, because it is nontoxic, stable chemical nature and with low cost.But
It can only mainly utilize ultraviolet light and relatively low photocatalysis efficiency to constrain its application, and therefore, many methods grow up use
In modified TiO2To improve its efficiency.Wherein, metal-oxide composite algorithm is widely used.Face here, CeO2Compound
TiO2Nano material cause numerous concerns.Ce is a kind of lanthanide series rare-earth elements nontoxic and with low cost.CeO2Special
F and d electron orbit structure, unique UV absorbent properties, high electron conductivity, high thermal stability and big Oxygen storage capacity all can show
Write ground and improve TiO2Photocatalysis efficiency.Numerous CeO2-TiO2 nano composite materials has been had to be in the news.Such as: Hu Mingjiang
Report coaxial electrostatic spinning method is prepared for CeO2-TiO2 composite nano fiber, and available effectiveness is in aldoketones organic pollution
Photocatalytic oxidation degradation [ACTA Scientiae Circumstantiae, 2015,35(01): 215-221]；The report such as Xi Lihe uses liquid phase synthesis legal system
Standby CeO2-TiO2 nano composite material, available effectiveness in formaldehyde photochemical catalytic oxidation [functional material, 2007,38(11): 1762-
1765].However, it is noteworthy that current CeO2-TiO2The application of the photocatalysis performance of nano composite material is mainly limited to
The organic reaction of photochemical catalytic oxidation.This is because, Ce has the strongest affinity to the functional group of many organic compound, because of
This it Organic substance can be enriched in photocatalyst surface, thus improve photocatalysis efficiency.Therefore, CeO2-TiO2Nano combined material
Material is used for the performance of photochemical catalytic oxidation organic pollution by wide coverage [Mater. Res. Bull. 45 (2010) 1406-
1412; Appl. Surf. Sci. 255 (2009) 5975-5978].But, possess the CeO of photo catalytic reduction performance2-
TiO2Nano-complex is almost without report, and this greatly constrains CeO2-TiO2The application of this outstanding catalysis material.Open up
Exhibition CeO2-TiO2The visible ray reducing property of nano-complex a, it has also become focus of this area research.It is contemplated that visit
The method seeking the meaning certainly this key issue.
Method and the ratio of compounding ingredients that the performance of catalyst is prepared with it are closely related, explore in terms of these
Be conducive to the preparation method that development catalyst is new.The inventive method prepares CeO with the method for hydro-thermal, calcining2-TiO2Nano combined
Material, the CeO obtained with the ratio of preparation method of the present invention and compounding ingredients2-TiO2Nano composite material, possesses in the past
CeO2-TiO2The performance do not reported, possesses and excites lower photo catalytic reduction Heavy Metals in Waters pollutant Cr (VI) can see below
Performance.The inventive method, can widen CeO effectively2-TiO2The range of application of nano composite material.
Summary of the invention
It is an object of the invention to provide a kind of CeO possessing photo catalytic reduction performance2-TiO2The system of nano composite material
Preparation Method, comprises the steps:
By Ce (NO3)3.6H2O dissolves in ethanol, obtains cerous nitrate solution；Tetrabutyl titanate is dissolved in ethanol with go from
In the mixed liquor of sub-water, obtain tetrabutyl titanate solution；It is uniformly dispersed above two solution mixes under conditions of ultrasonic,
Obtain reactant mixture.
By stepReactant mixture put in hydrothermal reaction kettle, maintain 120 DEG C reaction 48h.
By stepProduct be cooled to room temperature after carry out centrifugation, gained filter cake is scrubbed, drying and processing
After calcine, obtain CeO2-TiO2Nano composite material.
Described Ce (NO3)3.6H2O is 1:0.5～5 with the mol ratio of the Ce/Ti of tetrabutyl titanate.
Described tetrabutyl titanate is dissolved in the mixed liquor of ethanol and deionized water, ethanol and the volume ratio of deionized water
For 2:1.
The condition of described calcining is for maintaining 450 DEG C of calcining 5h, and heating rate is 5 DEG C of min−1。
The invention have the advantage that described method is simple, easily operate.The CeO prepared by this method2-TiO2Nano combined material
Material can carry out photo catalytic reduction to the Cr (VI) in aqueous phase under excited by visible light effectively, and this material can be effectively applied to
The photocatalysis that Heavy Metals in Waters pollutes is administered so that material is suitable for popularization and application on a large scale.
Accompanying drawing explanation
Fig. 1 is CeO of the present invention2-TiO2The scanning electron microscope (SEM) photograph of nano composite material；
Fig. 2 is CeO of the present invention2-TiO2Nano composite material photo catalytic reduction Cr (VI) performance.
Detailed description of the invention
Hereinafter embodiments of the invention are described in further detail, but the present embodiment is not limited to the present invention, all
It is to use the analog structure of the present invention and similar change thereof, protection scope of the present invention all should be listed in.
Embodiment 1
0.1498g Ce(NO3)3.6H2O is dissolved in 20mL ethanol, and 352uL tetrabutyl titanate is dissolved in 20mL ethanol and 10mL
In the mixed liquor of deionized water.Above two solution mixed under conditions of ultrasonic and is uniformly dispersed, then mixed liquor being filled
Enter 100 mL hydrothermal reaction kettles, at 120 DEG C, react 48h.React after terminating after system drops to room temperature, the solid of gained will be reacted
By centrifugation and collect, then alternately clean up with deionized water and ethanol, dry overnight in 60 DEG C.Finally, by institute
Obtaining material and calcine 5h at 450 DEG C, heating rate is 5 DEG C/min-1.
Embodiment 2
0.1498g Ce(NO3)3.6H2O is dissolved in 20mL ethanol, and 117uL tetrabutyl titanate is dissolved in 20mL ethanol and 10mL
In the mixed liquor of deionized water.Above two solution mixed under conditions of ultrasonic and is uniformly dispersed, then mixed liquor being filled
Enter 100 mL hydrothermal reaction kettles, at 120 DEG C, react 48h.React after terminating after system drops to room temperature, the solid of gained will be reacted
By centrifugation and collect, then alternately clean up with deionized water and ethanol, dry overnight in 60 DEG C.Finally, by institute
Obtaining material and calcine 5h at 450 DEG C, heating rate is 5 DEG C/min-1.
Embodiment 3
0.1498g Ce(NO3)3.6H2O is dissolved in 20mL ethanol, and 587uL tetrabutyl titanate is dissolved in 20mL ethanol and 10mL
In the mixed liquor of deionized water.Above two solution mixed under conditions of ultrasonic and is uniformly dispersed, then mixed liquor being filled
Enter 100 mL hydrothermal reaction kettles, at 120 DEG C, react 48h.React after terminating after system drops to room temperature, the solid of gained will be reacted
By centrifugation and collect, then alternately clean up with deionized water and ethanol, dry overnight in 60 DEG C.Finally, by institute
Obtaining material and calcine 5h at 450 DEG C, heating rate is 5 DEG C/min-1.
Claims (2)
1. the CeO possessing photo catalytic reduction performance2-TiO2The preparation method of nano composite material, it is characterised in that: described
Preparation method comprise the steps:
(1) by Ce (NO3)3.6H2O dissolves in ethanol, obtains cerous nitrate solution；Tetrabutyl titanate is dissolved in ethanol with go from
In the mixed liquor of sub-water, obtain tetrabutyl titanate solution；It is uniformly dispersed above two solution mixes under conditions of ultrasonic,
Obtain reactant mixture；
(2) reactant mixture of step (1) is put in hydrothermal reaction kettle, maintain 120 DEG C of reaction 48h；
(3) carrying out centrifugation after the product of step (2) being cooled to room temperature, gained filter cake is scrubbed, after drying and processing
Calcine, obtain CeO2-TiO2Nano composite material；
Described Ce (NO3)3.6H2O is 1:0.5～5 with the mol ratio of the Ce/Ti of tetrabutyl titanate；
Described tetrabutyl titanate is dissolved in the mixed liquor of ethanol and deionized water, and ethanol is 2 with the volume ratio of deionized water:
1。
A kind of CeO possessing photo catalytic reduction performance the most according to claim 12-TiO2The preparation side of nano composite material
Method, it is characterised in that: the condition of described calcining is for maintaining 450 DEG C of calcining 5h, and heating rate is 5 DEG C of min−1。
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107243340A (en) * | 2017-06-22 | 2017-10-13 | 南昌航空大学 | A kind of preparation method of ceric oxide nanorod doping titanium dioxide nano particle photochemical catalyst |
| CN108993374A (en) * | 2018-07-25 | 2018-12-14 | 沈阳理工大学 | A kind of preparation method of one-dimensional mesoporous catalysis material |
| CN109772367A (en) * | 2019-01-15 | 2019-05-21 | 天津大学 | A kind of preparation method of fabricated in situ transition metal oxide-Ni-based sulfide composite material |
| CN110605111A (en) * | 2019-09-26 | 2019-12-24 | 宿迁学院 | Cerium dioxide/titanium dioxide heterojunction micro-nano material and preparation method and application thereof |
| CN111085185A (en) * | 2019-12-11 | 2020-05-01 | 扬州大学 | CeO2:CDs/TiO2Nano material and application thereof in photocatalysis |
| CN111592079A (en) * | 2020-06-02 | 2020-08-28 | 无锡市伙伴日化科技有限公司 | Preparation method of acidic potential water |
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| CN104907060A (en) * | 2015-04-24 | 2015-09-16 | 宿州学院 | CeO2 / TiO2 heterojunction nano flower preparation method |
| CN105170130A (en) * | 2015-09-02 | 2015-12-23 | 中国科学院新疆理化技术研究所 | Preparation method and application of high-dispersion CeO2 modified TiO2 meso-porous photocatalyst |
-
2016
- 2016-07-28 CN CN201610599195.5A patent/CN106179304A/en active Pending
Patent Citations (4)
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| CN104128172A (en) * | 2014-07-29 | 2014-11-05 | 南昌航空大学 | Method for regulating and controlling morphology of nano TiO2-CeO2 into ball shape, dumbbell shape or sheet shape |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107243340A (en) * | 2017-06-22 | 2017-10-13 | 南昌航空大学 | A kind of preparation method of ceric oxide nanorod doping titanium dioxide nano particle photochemical catalyst |
| CN107243340B (en) * | 2017-06-22 | 2020-04-03 | 南昌航空大学 | Preparation method of cerium dioxide nanorod doped titanium dioxide nanoparticle photocatalyst |
| CN108993374A (en) * | 2018-07-25 | 2018-12-14 | 沈阳理工大学 | A kind of preparation method of one-dimensional mesoporous catalysis material |
| CN108993374B (en) * | 2018-07-25 | 2020-12-15 | 沈阳理工大学 | Preparation method of one-dimensional mesoporous photocatalytic material |
| CN109772367A (en) * | 2019-01-15 | 2019-05-21 | 天津大学 | A kind of preparation method of fabricated in situ transition metal oxide-Ni-based sulfide composite material |
| CN110605111A (en) * | 2019-09-26 | 2019-12-24 | 宿迁学院 | Cerium dioxide/titanium dioxide heterojunction micro-nano material and preparation method and application thereof |
| CN111085185A (en) * | 2019-12-11 | 2020-05-01 | 扬州大学 | CeO2:CDs/TiO2Nano material and application thereof in photocatalysis |
| CN111085185B (en) * | 2019-12-11 | 2023-02-28 | 扬州大学 | CeO 2 :CDs/TiO 2 Nano material and application thereof in photocatalysis |
| CN111592079A (en) * | 2020-06-02 | 2020-08-28 | 无锡市伙伴日化科技有限公司 | Preparation method of acidic potential water |
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