CN107335434B - A kind of nano-TiO of double pentagonal pyramid cylindricality looks of Fe doping2Photochemical catalyst preparation method - Google Patents

A kind of nano-TiO of double pentagonal pyramid cylindricality looks of Fe doping2Photochemical catalyst preparation method Download PDF

Info

Publication number
CN107335434B
CN107335434B CN201710453001.5A CN201710453001A CN107335434B CN 107335434 B CN107335434 B CN 107335434B CN 201710453001 A CN201710453001 A CN 201710453001A CN 107335434 B CN107335434 B CN 107335434B
Authority
CN
China
Prior art keywords
tio
photochemical catalyst
liquid
doping
pentagonal pyramid
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201710453001.5A
Other languages
Chinese (zh)
Other versions
CN107335434A (en
Inventor
周凌云
杜玉良
黄文�
单龙龙
周云浩
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Henan Institute of Science and Technology
Original Assignee
Henan Institute of Science and Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Henan Institute of Science and Technology filed Critical Henan Institute of Science and Technology
Priority to CN201710453001.5A priority Critical patent/CN107335434B/en
Publication of CN107335434A publication Critical patent/CN107335434A/en
Application granted granted Critical
Publication of CN107335434B publication Critical patent/CN107335434B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/30Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39Photocatalytic properties
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/06Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
    • B01J21/063Titanium; Oxides or hydroxides thereof
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/74Iron group metals
    • B01J23/745Iron
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/20Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
    • B01J35/23Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/30Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/391Physical properties of the active metal ingredient
    • B01J35/393Metal or metal oxide crystallite size

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Catalysts (AREA)

Abstract

The invention belongs to a kind of nano-TiOs of double pentagonal pyramid cylindricality looks of Fe doping2Photochemical catalyst preparation method, comprising the following steps: 1. butyl titanate is dissolved in dehydrated alcohol, oleyl amine and PVP is then added, stirs evenly to obtain A liquid;2. nine water ferric nitrates, EDTA-2Na, DMF are uniformly mixed, B liquid is obtained;3. B drop is added in A liquid, it is transferred in hydrothermal reaction kettle after mixing evenly, 12 ~ 18h is reacted at 160 ~ 200 DEG C, up to the TiO of double pentagonal pyramid cylindricality looks of Fe doping after is filtered, washed, drying2Photochemical catalyst.The present invention has prepared the nano-TiO for double pentagonal pyramid cylindricality looks that surface exposure has the Fe of high miller index surface to adulterate in conjunction with dehydrated alcohol and DMF as reaction dissolvent used as dispersing agent and Morphological control agent in proportion by using oleyl amine, PVP and EDTA-2Na2Photochemical catalyst, average grain diameter 10nm, greatly improves TiO2The catalytic activity of photochemical catalyst, and good catalytic activity is shown to the degradation rate of rhodamine B under ultraviolet source, it is with a wide range of applications.

Description

A kind of nano-TiO of double pentagonal pyramid cylindricality looks of Fe doping2Photochemical catalyst preparation method
Technical field
The invention belongs to double pentagonal pyramid cylindricality looks that organic pollutant degradation technique field more particularly to a kind of Fe are adulterated TiO2Photochemical catalyst preparation method.
Background technique
TiO2Material because can organic and inorganic pollution effectively in catalytic degradation air and water, and do not generate secondary dirt It contaminates and reusable, gradually attracts people's attention in recent years, scientific worker has carried out many to TiO2Material light catalysis Oxidation, reduction or degradation treatment contain the research of the toxic wastes such as DDT, dinitroaniline, trichloro ethylene, NO, Cr (VI).But it is existing Some TiO2Photochemical catalyst or preparation method are complicated, and expensive or product catalytic performance is not high, therefore provides one kind Preparation method is simple, the TiO high to organic pollutant degradation efficiency2Photochemical catalyst is very important.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods simply, pair of the Fe doping high to organic pollutant degradation efficiency The nano-TiO of pentagonal pyramid cylindricality looks2Photochemical catalyst preparation method.
To achieve the above object, the technical solution adopted by the present invention is that, a kind of double pentagonal pyramid cylindricality looks of Fe doping are received Rice TiO2Photochemical catalyst preparation method, comprising the following steps: 1. butyl titanate is dissolved in dehydrated alcohol, oleyl amine is then added And PVP, stir evenly to obtain A liquid;2. by nine water ferric nitrates, EDTA-2Na, DMF(dimethylformamide) it is uniformly mixed, obtain B liquid; 3. B drop is added in A liquid, it is transferred in hydrothermal reaction kettle after mixing evenly, 12 ~ 18h is reacted at 160 ~ 200 DEG C, filters, wash Up to the TiO of double pentagonal pyramid cylindricality looks of Fe doping after washing, drying2Photochemical catalyst.
Preferably, the nano-TiO of double pentagonal pyramid cylindricality looks of Fe doping2Photochemical catalyst preparation method includes following 6g butyl titanate: being 1. dissolved in 30mL dehydrated alcohol by step, and 20mL oleyl amine and 100mg PVP is then added, stirs evenly Obtain A liquid;2. nine water ferric nitrate of 51mg, 150mg EDTA-2Na, 25mL DMF are uniformly mixed, B liquid is obtained;3. B drop is added to A In liquid, be transferred in hydrothermal reaction kettle after mixing evenly, hydro-thermal reaction 16h at 200 DEG C, be filtered, washed, dry after mixed up to Fe The TiO of miscellaneous double pentagonal pyramid cylindricality looks2Photochemical catalyst.
The beneficial effect comprise that: the present invention by using oleyl amine, PVP and EDTA-2Na in proportion used as Dispersing agent and Morphological control agent, in conjunction with dehydrated alcohol and DMF as reaction dissolvent, having prepared surface exposure has high miller index surface Fe doping double pentagonal pyramid cylindricality looks nano-TiO2Photochemical catalyst, average grain diameter 10nm, greatly improves TiO2Photocatalysis The catalytic activity of agent, and good catalytic activity is shown to the degradation rate of rhodamine B under ultraviolet source, have extensive Application prospect.
Detailed description of the invention
Fig. 1 is the TiO of the double pentagonal pyramid cylindricality looks for the Fe doping that embodiment 1 is prepared2The transmission electron microscope of photochemical catalyst Photo;
Fig. 2 is the TiO of the double pentagonal pyramid cylindricality looks for the Fe doping that embodiment 1 is prepared2The XRD diagram of photochemical catalyst;
Fig. 3 is the TiO of the double pentagonal pyramid cylindricality looks for the Fe doping that reference examples 1 are prepared2The transmission electron microscope of photochemical catalyst Photo;
Fig. 4 is the TiO of the double pentagonal pyramid cylindricality looks for the Fe doping that reference examples 2 are prepared2The transmission electron microscope of photochemical catalyst Photo;
Fig. 5 is double pentagonal pyramid rod structure model schematics.
Specific embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.It is not specified in embodiment specific Condition person carries out according to conventional conditions or manufacturer's recommended conditions.Reagents or instruments used without specified manufacturer is The conventional products that can be obtained by commercially available purchase.
Embodiment 1
A kind of nano-TiO of double pentagonal pyramid cylindricality looks of Fe doping21. photochemical catalyst preparation method will be the following steps are included: will 6g butyl titanate is dissolved in 30mL dehydrated alcohol, and 20mL oleyl amine and 100mg PVP(polyvinylpyrrolidone is then added), Stir evenly to obtain A liquid;2. nine water ferric nitrate of 51mg, 150mg EDTA-2Na, 25mL DMF are uniformly mixed, B liquid is obtained;3. by B Drop is added in A liquid, is transferred in hydrothermal reaction kettle after mixing evenly, and hydro-thermal reaction 16h at 200 DEG C is filtered, washed, dries Afterwards up to the TiO of double pentagonal pyramid cylindricality looks of Fe doping2Photochemical catalyst.
Fig. 2 is the TiO of double pentagonal pyramid cylindricality looks of the Fe doping prepared in embodiment 12The XRD diagram of photochemical catalyst, with The angle that the characteristic peak of the titanium dioxide of Detitanium-ore-type in standard graph card (PDF01-0562) occurs is almost the same, does not see The characteristic peak for observing doping Fe atom, illustrates under the doping ratio of embodiment 1, the Fe atom of doping is present in a dispersed form TiO in catalyst, with Detitanium-ore-type2Crystal is compounded to form photocatalytic activity position, can not be in TiO2It is formed in crystal and contains Fe Crystallite, so not observing the XRD characteristic peak in relation to Fe.
Reference examples 1
Be except reference examples 1 and the difference of embodiment 1: 1 step of reference examples 1. in be added without EDTA-2Na.
Reference examples 2
Be except reference examples 2 and the difference of embodiment 1: 2 step of reference examples 1. in be added without oleyl amine.
Fig. 1 is the TiO of the double pentagonal pyramid cylindricality looks for the Fe doping that embodiment 1 is prepared2The transmission electron microscope of photochemical catalyst Photo;Fig. 3 is the TiO for the Fe doping that reference examples 1 are prepared2The transmission electron microscope photo of photochemical catalyst;Fig. 4 is the system of reference examples 2 The TiO of standby obtained Fe doping2The transmission electron microscope photo of photochemical catalyst.By oleyl amine in embodiment 1 it can be seen from Fig. 1,3-4, PVP and EDTA-2Na has prepared double the five of Fe doping in conjunction with solvent thermal reaction condition used as Morphological control agent in proportion The nano-TiO of pyramid column pattern2Photochemical catalyst;The TiO that Fe is adulterated is prepared from reference examples 1 and reference examples 22Photochemical catalyst pattern From the point of view of, in the case where having lacked EDTA-2Na or oleyl amine, the nano-titanium dioxide pattern of formation is irregular and particle size not Uniformly.
Application test
Take four photocatalysis instrument reaction tubes, be separately added into 100mL concentration be 10mg/L rhodamine B solution, then to The nanometer of Fe doping prepared by embodiment 1, reference examples 1 and reference examples 2 is wherein separately added into three photocatalysis instrument reaction tubes TiO2Photochemical catalyst 0.01g, another photocatalysis instrument reaction tube are blank control group (being added without photochemical catalyst), ultrasonic disperse 4min reaches reaction adsorption equilibrium in darkroom after Static Adsorption 30min, open ultraviolet source and magnetic stirring apparatus, illumination It is sampled in the process at interval of 10min, takes supernatant liquor at rhodamine B maximum absorption wavelength l=554nm after centrifuge separation, used 722N visible spectrophotometer measures sample absorbance, and passes through formula: DC=[(A0-Ai )/A0 ] * 100% completion degradation rate Calculating, wherein for A0For the absorbance of the rhodamine B solution of 10mg/L, AiFor the rhodamine B solution that is measured when timing sampling Absorbance.
The TiO of Fe doping prepared by embodiment 1, reference examples 1 and reference examples 22Photochemical catalyst degrades to rhodamine B, After irradiating 60min under 254nm length ultraviolet light, the degradation rate of rhodamine B is respectively 99.1%, 86% and 81%.
Although illustrate and describing the present invention with specific embodiment, it will be appreciated that without departing substantially from of the invention Many other change and modification can be made in the case where spirit and scope.It is, therefore, intended that in the following claims Including belonging to all such changes and modifications in the scope of the invention.

Claims (2)

1. a kind of nano-TiO of double pentagonal pyramid cylindricality looks of Fe doping2Photochemical catalyst preparation method, which is characterized in that including following Butyl titanate: being 1. dissolved in dehydrated alcohol by step, and oleyl amine and PVP is then added, stirs evenly to obtain A liquid;2. by nine water nitre Sour iron, EDTA-2Na, DMF are uniformly mixed, and obtain B liquid;3. B drop is added in A liquid, it is transferred to hydrothermal reaction kettle after mixing evenly In, 12 ~ 18h is reacted at 160 ~ 200 DEG C, up to the TiO of double pentagonal pyramid cylindricality looks of Fe doping after being filtered, washed, drying2Light is urged Agent.
2. the nano-TiO of double pentagonal pyramid cylindricality looks of Fe doping as described in claim 12Photochemical catalyst preparation method, feature exist In, comprising the following steps: 1. 6g butyl titanate is dissolved in 30mL dehydrated alcohol, 20mL oleyl amine and 100mg is then added PVP stirs evenly to obtain A liquid;2. nine water ferric nitrate of 51mg, 150mg EDTA-2Na, 25mL DMF are uniformly mixed, B liquid is obtained;③ B drop is added in A liquid, is transferred in hydrothermal reaction kettle after mixing evenly, hydro-thermal reaction 16h at 200 DEG C is filtered, washed, does Up to the TiO of double pentagonal pyramid cylindricality looks of Fe doping after dry2Photochemical catalyst.
CN201710453001.5A 2017-06-15 2017-06-15 A kind of nano-TiO of double pentagonal pyramid cylindricality looks of Fe doping2Photochemical catalyst preparation method Active CN107335434B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710453001.5A CN107335434B (en) 2017-06-15 2017-06-15 A kind of nano-TiO of double pentagonal pyramid cylindricality looks of Fe doping2Photochemical catalyst preparation method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710453001.5A CN107335434B (en) 2017-06-15 2017-06-15 A kind of nano-TiO of double pentagonal pyramid cylindricality looks of Fe doping2Photochemical catalyst preparation method

Publications (2)

Publication Number Publication Date
CN107335434A CN107335434A (en) 2017-11-10
CN107335434B true CN107335434B (en) 2019-07-09

Family

ID=60220563

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710453001.5A Active CN107335434B (en) 2017-06-15 2017-06-15 A kind of nano-TiO of double pentagonal pyramid cylindricality looks of Fe doping2Photochemical catalyst preparation method

Country Status (1)

Country Link
CN (1) CN107335434B (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108837833A (en) * 2018-06-29 2018-11-20 烟台智本知识产权运营管理有限公司 Fe adulterates TiO2The preparation of catalyst

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103599810A (en) * 2013-10-28 2014-02-26 江苏大学 Preparation and application of Sr<2+>-doped TiO2 composite hollow sphere photocatalyst
CN103861593A (en) * 2014-03-25 2014-06-18 陕西科技大学 Chromium-silver co-doped nano TiO2 photo-catalyst, and preparation method and use thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103599810A (en) * 2013-10-28 2014-02-26 江苏大学 Preparation and application of Sr<2+>-doped TiO2 composite hollow sphere photocatalyst
CN103861593A (en) * 2014-03-25 2014-06-18 陕西科技大学 Chromium-silver co-doped nano TiO2 photo-catalyst, and preparation method and use thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
Hydrothermal synthesis of different TiO2 nanostructures: structure, growth and gas sensor properties;Long Huang et al.;《J Mater Sci: Mater Electron》;20120403;第1911-1915页
Synthesis of Metal Ion-Doped TiO2 Nanoparticles Using Two-Phase Method and Their Photocatalytic Activity Under Visible Light Irradiation;Journal of Nanoscience and Nanotechnology;《 Journal of Nanoscience and Nanotechnology》;20161231;第2024–2029页

Also Published As

Publication number Publication date
CN107335434A (en) 2017-11-10

Similar Documents

Publication Publication Date Title
Xing et al. Preparation of TiO2/activated carbon composites for photocatalytic degradation of RhB under UV light irradiation
Guan et al. Fabrication of a magnetic nanocomposite photocatalysts Fe3O4@ ZIF-67 for degradation of dyes in water under visible light irradiation
CN108940338A (en) Potassium element adulterates nitride porous carbon photochemical catalyst and its preparation method and application
CN109603880A (en) Hollow tubular carbon nitride photocatalyst and its preparation method and application
CN109603882A (en) Utilize the method for modified carbon quantum dot load hollow tubular carbon nitride photocatalyst processing organic pollutant and photo-catalyst
CN106423153B (en) Mix the preparation method and oxygen indicator of silver-colored titania nanotube
Zhai et al. Effective sonocatalytic degradation of organic dyes by using Er3+: YAlO3/TiO2–SnO2 under ultrasonic irradiation
CN106881111A (en) Composite bismuth vanadium photocatalyst of cuprous oxide and silver-colored mutual load and its preparation method and application
CN106381682A (en) Nano-TiO2/activated carbon fibrofelt three-dimensional porous material high in adsorption and photocatalytic performance, and preparation method thereof
Hernández-Gordillo et al. Mesoporous TiO 2 monoliths impregnated with CdS and CuO nanoparticles for airborne bacteria inactivation under visible light
CN107335434B (en) A kind of nano-TiO of double pentagonal pyramid cylindricality looks of Fe doping2Photochemical catalyst preparation method
CN110252334A (en) A kind of doped nano manganese dioxide composite material, preparation method and applications
CN108772053B (en) Bismuth titanate/bismuth oxide photocatalyst and preparation method and application thereof
CN110368990A (en) A kind of preparation method and applications of Cu system polyoxometallate-functional graphene oxide nano material
CN109759139A (en) A kind of environment-friendly sewage processing photoactivation material and preparation method thereof
CN109046433A (en) g-C3N4The method of/BiOBr photocatalytic degradation carbamazepine
CN108940324A (en) A kind of multi-walled carbon nanotube-Ag@AgCl composite nano materials and preparation method thereof with photocatalytic
CN107008258A (en) TiO2Application of the nanometer Ag photochemical catalyst of load in degradation of phenol
CN101125683A (en) Preparation method for photocatalysis water-purifying material MoO3 and application thereof
Saygi et al. Photocatalytic degradation kinetics of Reactive Black 5 (RB5) dyestuff on TiO 2 modified by pretreatment with ultrasound energy
CN106882855A (en) Cu2MoS4Application of the nanotube in photocatalysis
CN107008245A (en) TiO for the processing of high slat-containing wastewater organic pollution2Carbon fiber composite photo-catalyst and its preparation
CN107552051B (en) The nano-TiO of Fe doping2Application of the photochemical catalyst in degradation p-nitrophenol
CN105833865B (en) A kind of preparation method of the graphene-supported Ag photochemical catalysts with concave surface cube pattern
CN106582500B (en) Adsorbable degradation Cr (VI) diatomite composite material of one kind and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant