CN107335434A - 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

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CN107335434A
CN107335434A CN201710453001.5A CN201710453001A CN107335434A CN 107335434 A CN107335434 A CN 107335434A CN 201710453001 A CN201710453001 A CN 201710453001A CN 107335434 A CN107335434 A CN 107335434A
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tio
liquid
photochemical catalyst
doping
pentagonal pyramid
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CN201710453001.5A
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CN107335434B (en
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周凌云
杜玉良
黄文�
单龙龙
周云浩
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Henan Institute of Science and Technology
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Henan Institute of Science and Technology
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    • 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

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  • 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-TiO of double pentagonal pyramid cylindricality looks of Fe doping2Photochemical catalyst preparation method, comprises the following steps:1. butyl titanate is dissolved in absolute ethyl alcohol, oleyl amine and PVP are then added, stir to obtain A liquid;2. nine water ferric nitrates, EDTA 2Na, DMF are well mixed, B liquid is obtained;3. B drops are added in A liquid, be transferred to after stirring in hydrothermal reaction kettle, at 160 ~ 200 DEG C react 12 ~ 18h, filtering, washing, dry after produce Fe doping double pentagonal pyramid cylindricality looks TiO2Photochemical catalyst.The present invention uses in proportion by using oleyl amine, PVP and EDTA 2Na is used as dispersant and Morphological control agent, with reference to the nano-TiO of absolute ethyl alcohol and the DMF double pentagonal pyramid cylindricality looks adulterated as reaction dissolvent, the Fe that having prepared surface exposure has high miller index surface2Photochemical 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 organic pollutant degradation technique field, more particularly to a kind of double pentagonal pyramid cylindricality looks of Fe doping TiO2Photochemical catalyst preparation method.
Background technology
TiO2Material and does not produce secondary dirt because of organic and inorganic pollution that can be effectively in catalytic degradation air and water Contaminate and reusable, gradually attract people's attention in recent years, scientific worker has carried out many to TiO2Material light catalysis The research of oxidation, reduction or degradation treatment containing the toxic waste such as DDT, dinitroaniline, trichloro ethylene, NO, Cr (VI).It is but existing Some TiO2Or photochemical catalyst preparation method is complicated, costly, or the catalytic performance of product is not high, therefore provide a kind of Preparation method is simple, the TiO high to organic pollutant degradation efficiency2Photochemical catalyst is very important.
The content of the invention
Adulterated it is an object of the invention to provide a kind of simple, high to the organic pollutant degradation efficiency Fe of preparation method double 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, comprises the following steps:1. butyl titanate is dissolved in absolute ethyl alcohol, oleyl amine is then added And PVP, stir to obtain A liquid;2. by nine water ferric nitrates, EDTA-2Na, DMF(Dimethylformamide)It is well mixed, obtain B liquid; 3. B drops are added in A liquid, it is transferred to after stirring in hydrothermal reaction kettle, 12 ~ 18h is reacted at 160 ~ 200 DEG C, filters, wash Wash, dry after produce Fe doping double pentagonal pyramid cylindricality looks TiO2Photochemical catalyst.
Preferably, the nano-TiO of double pentagonal pyramid cylindricality looks of described Fe doping2Photochemical catalyst preparation method includes following Step:1. 6g butyl titanates are dissolved in 30mL absolute ethyl alcohols, 20mL oleyl amines and 100mg PVP are then added, is stirred Obtain A liquid;2. the water ferric nitrates of 51mg nine, 150mg EDTA-2Na, 25mL DMF are well mixed, B liquid is obtained;3. B drops are added to A In liquid, it is transferred to after stirring in hydrothermal reaction kettle, hydro-thermal reaction 16h at 200 DEG C, producing Fe after filtering, washing, drying mixes The TiO of miscellaneous double pentagonal pyramid cylindricality looks2Photochemical catalyst.
The beneficial effect comprise that:The present invention uses conduct in proportion by using oleyl amine, PVP and EDTA-2Na Dispersant and Morphological control agent, with reference to absolute ethyl 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.
Brief description of the drawings
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 of photochemical catalyst;
Fig. 3 is the TiO of the double pentagonal pyramid cylindricality looks for the Fe doping that embodiment 1 and reference examples 1 and 2 are prepared2Photochemical catalyst Degradation effect figure;
Fig. 4 is the TiO of the double pentagonal pyramid cylindricality looks for the Fe doping that reference examples 1 are prepared2The transmission electron microscope photo of photochemical catalyst;
Fig. 5 is the TiO of the double pentagonal pyramid cylindricality looks for the Fe doping that reference examples 2 are prepared2The transmission electron microscope photo of photochemical catalyst;
Fig. 6 is double pentagonal pyramid rod structure model schematics.
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 present invention.It is unreceipted specific in embodiment Condition person, the condition suggested according to normal condition or manufacturer are carried out.Agents useful for same or the unreceipted production firm person of instrument, it 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 doping2Photochemical catalyst preparation method comprises the following steps:1. by 6g titaniums Sour four butyl esters are dissolved in 30mL absolute ethyl alcohols, then add 20mL oleyl amines and 100mg PVP(Polyvinylpyrrolidone), stirring It is uniform to obtain A liquid;2. the water ferric nitrates of 51mg nine, 150mg EDTA-2Na, 25mL DMF are well mixed, B liquid is obtained;3. by B drops It is added in A liquid, is transferred to after stirring in hydrothermal reaction kettle, hydro-thermal reaction 16h at 200 DEG C, filtering, washing, is after drying Obtain 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 of photochemical catalyst, its with Standard graph card(PDF01-0562)In Detitanium-ore-type titanium dioxide characteristic peak occur angle it is basically identical, do not see The characteristic peak of doping Fe atoms is observed, is illustrated under the doping ratio of embodiment 1, the Fe atoms of doping are present in a dispersed form In catalyst, the TiO with Detitanium-ore-type2Crystal is compounded to form photocatalytic activity position, can not be in TiO2Formed in crystal and contain Fe Crystallite, so not observing the XRD characteristic peaks about Fe.
Reference examples 1
Reference examples 1 outside the difference of embodiment 1 with being:The step of reference examples 1 1. in be added without EDTA-2Na.
Reference examples 2
Reference examples 2 outside the difference of embodiment 1 with being:The step of reference examples 2 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. 4 is the TiO for the Fe doping that reference examples 1 are prepared2The transmission electron microscope photo of photochemical catalyst;Fig. 5 is that reference examples 2 are made The TiO of standby obtained Fe doping2The transmission electron microscope photo of photochemical catalyst.In embodiment it can be seen from Fig. 1,4-5 1 oleyl amine, PVP and EDTA-2Na is used in proportion is used as Morphological control agent, with reference to solvent thermal reaction condition, has prepared double the five of Fe doping The nano-TiO of pyramid column pattern2Photochemical catalyst;The TiO of Fe doping 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 oxide pattern of formation is irregular and particle size not Uniformly.
Application test
Four photocatalysis instrument reaction tubes are taken, are separately added into the rhodamine B solution that 100mL concentration is 10mg/L, then thereto The nano-TiO of Fe doping prepared by embodiment 1, reference examples 1 and reference examples 2 is separately added into three photocatalysis instrument reaction tubes2 Photochemical catalyst 0.01g, another photocatalysis instrument reaction tube are blank control group(It is added without photochemical catalyst), ultrasonic disperse 4min, reach reaction adsorption equilibrium after Static Adsorption 30min in darkroom, open ultraviolet source and magnetic stirring apparatus, illumination During at interval of 10min sample, supernatant liquor is taken after centrifugation rhodamine B maximum absorption wavelength l=554nm at, use 722N visible spectrophotometer determination sample absorbances, and pass through formula:DC=[( A0-Ai )/A0 ] * 100% completion degradation rate Calculating, wherein being A0For the absorbance of 10mg/L rhodamine B solution, AiFor the rhodamine B solution that is determined during timing sampling Absorbance.
The TiO of Fe doping prepared by embodiment 1, reference examples 1 and reference examples 22Photochemical catalyst to rhodamine B degradation effect such as Shown in Fig. 3, 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, but will be appreciated that without departing substantially from the present invention's Many other change and modification can be made in the case of 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 1. nano-TiO of double pentagonal pyramid cylindricality looks of Fe doping2Photochemical catalyst preparation method, it is characterised in that including following Step:1. butyl titanate is dissolved in absolute ethyl alcohol, oleyl amine and PVP are then added, stir to obtain A liquid;2. by nine water nitre Sour iron, EDTA-2Na, DMF are well mixed, and obtain B liquid;3. B drops are added in A liquid, hydrothermal reaction kettle is transferred to after stirring In, at 160 ~ 200 DEG C react 12 ~ 18h, filtering, washing, dry after produce Fe doping double pentagonal pyramid cylindricality looks TiO2Light is urged Agent.
  2. 2. the nano-TiO of double pentagonal pyramid cylindricality looks of Fe doping as claimed in claim 22Photochemical catalyst, it is characterised in that bag Include following steps:1. 6g butyl titanates are dissolved in 30mL absolute ethyl alcohols, 20mL oleyl amines and 100mg PVP are then added, is stirred Mix uniform A liquid;2. the water ferric nitrates of 51mg nine, 150mg EDTA-2Na, 25mL DMF are well mixed, B liquid is obtained;3. by B liquid It is added drop-wise in A liquid, is transferred to after stirring in hydrothermal reaction kettle, hydro-thermal reaction 16h at 200 DEG C, after filtering, washing, drying Produce the TiO of double pentagonal pyramid cylindricality looks of Fe doping2Photochemical 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)

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Cited By (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
JOURNAL OF NANOSCIENCE AND NANOTECHNOLOGY: "Synthesis of Metal Ion-Doped TiO2 Nanoparticles Using Two-Phase Method and Their Photocatalytic Activity Under Visible Light Irradiation", 《 JOURNAL OF NANOSCIENCE AND NANOTECHNOLOGY》 *
LONG HUANG ET AL.: "Hydrothermal synthesis of different TiO2 nanostructures: structure, growth and gas sensor properties", 《J MATER SCI: MATER ELECTRON》 *

Cited By (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

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