CN102716747A - (001) surface exposure Fe (ferrum) doping TiO2 (titanium dioxide) multi-stage catalyst and preparation method of Fe doping TiO2 multi-stage catalyst - Google Patents
(001) surface exposure Fe (ferrum) doping TiO2 (titanium dioxide) multi-stage catalyst and preparation method of Fe doping TiO2 multi-stage catalyst Download PDFInfo
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Abstract
The invention relates to a (001) surface exposure Fe (ferrum) doping TiO2 (titanium dioxide) multi-stage catalyst and a preparation method of the Fe doping TiO2 multi-stage catalyst and belongs to the technical field of multi-stage structure nanometer material catalysis. The catalyst consists of the following ingredients in percentage by mass: 35.5 percent to 45.5 percent of titanium, 55.5 percent to 65.5 percent of oxygen and 0.1 percent to 1 percent of Fe. A one-step in-situ solvent terminal method is adopted in the catalyst synthesis process, amorphous Fe doping TiO2 nanometer sheet layer multi-stage microspheres are adopted as precursors, a Fe-doping anatase type TiO2 multi-stage microsphere catalyst with the exposed (001) surface is obtained through the roasting, and the catalyst is applicable to visible light degradation organic matter catalysis reaction. The catalyst and the preparation method have the advantages that the catalyst has higher visible light degradation organic matter catalysis activity, the catalyst is maintained at the higher specific surface area of the nanometer materials, and the advantages of easy separation and high recovery and reutilization rate of the micrometer dimension materials are realized.
Description
Technical field
The invention belongs to multilevel hierarchy nano material catalysis technical field, the iron that particularly provides a kind of (001) face to expose is mixed multistage catalyst of titanium dioxide and preparation method.
Technical background
In the face of the global crisis of energy shortage and ecological deterioration, photocatalysis technology is prone to the solution of row as a kind of green and is extensively paid close attention to.Photocatalysis technology typically refers to semiconductor nano material under ultraviolet light or visible light radiation, utilizes luminous energy to be converted into chemical energy, thereby promotes the technology that organic matter is synthetic or degrade.TiO
2As the semi-conducting material of finding to have photocatalytic activity the earliest, because of its cheapness, nontoxic, chemical property stable and unique characteristics such as photoelectric effect are considered to the photochemical catalyst of tool application potential.Yet, about TiO
2The research of photochemical catalyst, people still are faced with some problems: how (1) suppresses the compound of light induced electron and hole, thereby improves TiO
2Photocatalysis efficiency (2) how to reduce energy gap, widen its light abstraction width, thereby improve the utilization ratio of solar energy.At present to TiO
2The effective ways of modification are doping, surperficial noble metal loading, semiconductor is compound and material surface control etc.
TiO
2Have three kinds of crystalline phases, wherein Detitanium-ore-type TiO
2Show best photocatalysis performance because of having more surface state activated centre.Follow people to Detitanium-ore-type TiO
2Photochemical catalyst deep research comprehensively, more and more researchers find that the crystal face that catalyst surface exposed is a key factor of decision photocatalytic activity and efficient.2008, it was 47% that Yang etc. time have synthesized (001) face exposure in Nature the 453rd volume 638 beginnings of the page, be of a size of the nanoscale anatase TiO of 1.5 μ m
2Monocrystalline.Anatase TiO
2(001) surface free energy of face is 0.9 J/m
2, be higher than 0.44 J/m of (101) face of anatase
2, and the Ti atom has lower Atomic coordinate number and bigger Ti-O-Ti bond angle on (001) face, makes the anatase TiO of exposure (001) face
2What in heterogeneous reaction, show is more active.Afterwards, people such as Kuang Qin is TiO in the 131st volume 3152-3153 page or leaf at Journal of the American Chemical Society in 2009 through butyl titanate
2Precursor, hydrofluoric acid are that to prepare (001) face exposure be 89% to solvent, be of a size of the Detitanium-ore-type TiO of 40nm
2The nanometer sheet catalyst is than commercial Degussa P25 TiO
2, it is active that this catalyst shows higher ultraviolet degradation methyl orange.It is thus clear that the exposure of high activity face (001) face is to improve one of effective way of photocatalytic activity.Meanwhile, it is the Ti source that Liu Min adopts titanium valve, and hydrofluoric acid is solvent, delivers in nearly 2 years about exposing the Detitanium-ore-type TiO of (001) face
23 of the patents of invention of monocrystalline and nanometer sheet layer material (200910092873.9,201010231407.7,201010231429.3).But, in above-mentioned work, all use hydrofluoric acid to obtain the TiO that (001) face exposes
2, and hydrofluoric acid has severe corrosive and excitant, in the preparation process, exists certain dangerous.
Yet the catalyst that provides in the above document only shows photocatalysis performance under ultraviolet light, in order to improve the effective utilization to solar energy resources, widens this Detitanium-ore-type TiO with (001) face
2The photoresponse scope of nano material catalyst is significant.Mix through transition-metal Fe and to modify TiO
2The research report that catalyst is widened light abstraction width is a lot.2010, S.A.Giraldo etc. are report in the 119th page to the 124th page of the 157th volume of Catalysis Today, adopts Hydrothermal Preparation Fe-TiO
2Beaded catalyst helps Fe
3+The stable TiO that is present in
2In the structure, thus the activity of raising photocatalytic degradation ice color.In addition, 2012, Lei Jianfei etc. in the 625th page to the 632nd page of the 16th volume of Journal of Solid State Electrochemistry through adopting Prepared by Sol Gel Method Fe-doped TiO
2Photochemical catalyst, wherein Fe
3+The instrumentality that plays the electric charge transmission improves photocatalytic activity.It is thus clear that the doping through the Fe element is to TiO
2It is the effective way that improves visible light catalysis activity that photochemical catalyst carries out modification.Yet, also do not see the Detitanium-ore-type TiO with (001) face of relevant Fe element doping so far
2The report of nano material catalyst, particularly Fe doped Ti O
2The microspheroidal multilevel hierarchy catalyst of nanometer lamella self assembly.
Therefore, the present invention intends and proposes a kind of simple and effective synthetic method, the Detitanium-ore-type Fe doped Ti O that exposes through the hot method preparation of a step situ solvent (001) face first
2The multistage microspherical catalyst of nanometer lamella provides a kind of novel visible light response catalyst.
Summary of the invention
The iron that the object of the present invention is to provide a kind of (001) face to expose is mixed multistage catalyst of titanium dioxide and preparation method.Detitanium-ore-type Fe doped Ti O through the exposure of the hot method preparation of a step situ solvent (001) face
2The multistage microspherical catalyst of nanometer lamella is a kind of visible light response catalyst, has higher visible light degradation of organic substances catalytic activity.
A large amount of exposures of this catalyst (001) crystal face give catalyst higher catalytic activity, and through the doping of transition-metal Fe element, the absorption spectrum generation red shift phenomenon of catalyst has higher visible light degradation of organic substances catalytic activity.Gained Fe doped Ti O
2The multilevel hierarchy microspherical catalyst has been given the advantage of the easily separated and high recycling of micron-scale material again when keeping the nano material high-specific surface area.
Catalyst of the present invention is made up of titanium, oxygen, iron, and the quality percentage composition of each component is: titanium: 35.5% ~ 45.5%; Oxygen: 55.5% ~ 65.5%; Iron: 0.1% ~ 1%; The building-up process of catalyst adopts the hot method of a step situ solvent, with unformed Fe doped Ti O
2The multistage microballoon of nanometer lamella is a presoma, after roasting, obtains the Detitanium-ore-type Fe doped Ti O that (001) face exposes
2The multistage microspherical catalyst of nanometer lamella is applicable to visible light degradation of organic substances catalytic reaction.
Multistage microballoon of the present invention is of a size of 500nm ~ 700nm, and the specific area of catalyst is 143m
2/ g ~ 160m
2/ g, (001) face exposure is 85% ~ 95%; Fe doped Ti O by the exposure of (001) face
2The self assembly of nanometer lamella forms TiO
2Crystal formation be Detitanium-ore-type, the thickness of nanometer lamella is that 8nm ~ 12nm, nanometer sheet size is 100nm ~ 300nm.
Catalyst provided by the present invention is to adopt isopropyl titanate (TIP) to be the Ti source, and isopropyl alcohol (IPA) is a solvent, and diethylenetriamine (DETA) is as block agent, FeCl
36H
2O is the Fe source of adulterant, is equipped with catalyst precursor through the hot legal system of a step situ solvent, obtains the Fe doped Ti O that (001) face exposes after 2 hours through 400 ℃ of calcinings
2Multistage microspherical catalyst.Concrete preparation process is:
1, the preparation of catalyst precursor
Accurately measure the solvent isopropyl alcohol (IPA) of certain volume; Add a certain amount of block agent diethylenetriamine (DETA); After stirring 3 ~ 5 minutes, a certain amount of isopropyl titanate (TIP) joined obtain mixed solution in the solvent, accurately the FeCl of weighing certain mass
36H
2O is dissolved in the mixed liquor, ultrasonic dispersion 3 ~ 5 minutes, and wherein the volume ratio of IPA:TIP:DETA is 71:0.05:3.35 ~ 71:1:3.35; Mixed liquor is gone in the spontaneous pressure agitated reactor of 100 ml; In 200 ℃ of following crystallization 20 ~ 28 hours, reaction finished to naturally cool to room temperature, uses absolute ethanol washing reaction precipitation thing 3 ~ 5 times then; Washing finishes back following dry 12 hours in 60 ℃; Obtain faint yellow powder, be catalyst precursor, be designated as x ~ Fe-TiO
2NSHS-as, x are metal cations Fe
3+With Ti
4+Mol ratio, x is 0.1% ~ 1%.
2, Preparation of catalysts
With the catalyst precursor x ~ Fe-TiO that obtains
2NSHS-as, the heating rate with 1 ℃/min is warming up to 400 ~ 500 ℃ under air atmosphere in tube furnace, and roasting 2 ~ 4 hours obtains corresponding catalyst and is designated as x ~ Fe-TiO
2NSHS, x are metal cations Fe
3+With Ti
4+Mol ratio, x is 0.1% ~ 1%.
Advantage of the present invention and characteristics are:
1, the present invention is through adopting the hot method of a step situ solvent, the Fe doped Ti O that provides a kind of novel (001) face to expose
2Multistage microspherical catalyst, this preparation method's step is simple, and diethylenetriamine replaces the use of hydrofluoric acid as the growth of block agent control (001) face in the Experiment Preparation process, and the danger of having avoided hydrofluoric acid to exist reaches the pollution that environment is produced.
2, the Fe doped Ti O of (001) provided by the present invention face exposure
2Multistage microspherical catalyst pattern is TiO
2The multilevel hierarchy microballoon that the self assembly of nanometer lamella forms, the average-size of microballoon are about 500nm ~ 700nm, and specific area is 143m
2/ g ~ 160m
2/ g had both kept the high-specific surface area of nano material, had easily separated, the high characteristics of recycling of micron-scale material again, therefore, had potential application prospect in fields such as catalysis, absorption.
3, catalyst provided by the present invention is Detitanium-ore-type TiO
2Semi-conducting material, Detitanium-ore-type TiO
2(001) face expose and to make catalyst have higher catalytic activity.In addition,, make the absorption spectrum generation red shift phenomenon of catalyst, give the light degradation catalytic capability of catalyst under visible light, new thinking is provided for efficiently utilizing solar energy resources through the doping of Fe.
Description of drawings
Fig. 1 is embodiment 1 prepared 0.1% ~ Fe-TiO
2The ESEM spectrogram of NSHS catalyst under low multiplication factor.
Fig. 2 is embodiment 1 prepared 0.1% ~ Fe-TiO
2The ESEM spectrogram of NSHS catalyst under high-amplification-factor.
Fig. 3 is embodiment 1 prepared 0.1% ~ Fe-TiO
2The high-resolution-ration transmission electric-lens spectrogram of NSHS catalyst.
The specific embodiment
Below in conjunction with the accompanying drawing and the specific embodiment the present invention is described further.
Embodiment 1
1, the preparation of catalyst precursor:
Accurately measure the isopropyl alcohol that volume is 71 ml (IPA) and place beaker; Adding 0.05 ml diethylenetriamine (DETA) leniently stirred 3 minutes; After stirring, be that the isopropyl titanate (TIP) of 3.35 ml joins in the above-mentioned solvent and obtains mixed solution with volume.Accurate weighing 0.0027 g FeCl
36H
2O is dissolved in the mixed liquor, ultrasonic dispersion 3 minutes.Mixed liquor is gone in the spontaneous pressure agitated reactor of 100 ml, and in 200 ℃ of following crystallization 24 hours, reaction finished to naturally cool to room temperature; Use absolute ethanol washing reaction precipitation thing 3 times then; Washing finish the back in 60 ℃ dry 12 hours down, obtain faint yellow powder, be designated as 0.1% ~ Fe-TiO
2NSHS-as, 0.1% is metal cations Fe
3+With Ti
4+Mol ratio.
2, Preparation of catalysts:
With the catalyst precursor 0.1% ~ Fe-TiO that obtains
2NSHS-as, the heating rate with 1 ℃/min is warming up to 400 ℃ under air atmosphere in tube furnace, and roasting 2 hours obtains corresponding catalyst and is designated as 0.1% ~ Fe-TiO
2NSHS, 0.1% is metal cations Fe
3+With Ti
4+Mol ratio.
The Fe doped Ti O that (001) face that Fig. 1 and Fig. 2 make for present embodiment exposes
2Multistage microspherical catalyst can see that micro-spherical catalyst is of a size of about 600nm, is by Fe doped Ti O
2The nanometer sheet self assembly forms, and lamellar spacing is about 10nm, can know that in conjunction with Fig. 3 the size of lamella is about 200nm, and the spacing that can see lattice fringe is 0.19nm, corresponding Detitanium-ore-type TiO
2(001) face.
Embodiment 2
1, the preparation of catalyst precursor:
Accurately measure the isopropyl alcohol that volume is 71 ml (IPA) and place beaker; Adding 0.05 ml diethylenetriamine (DETA) leniently stirred 3 minutes; After stirring, be that the isopropyl titanate (TIP) of 3.35 ml joins in the above-mentioned solvent and obtains mixed solution with volume.Accurate weighing 0.0054 g FeCl
36H
2O is dissolved in the mixed liquor, ultrasonic dispersion 3 minutes.Mixed liquor is gone in the spontaneous pressure agitated reactor of 100 ml, and in 200 ℃ of following crystallization 24 hours, reaction finished to naturally cool to room temperature; Use absolute ethanol washing reaction precipitation thing 3 times then; Washing finish the back in 60 ℃ dry 12 hours down, obtain faint yellow powder, be designated as 0.2% ~ Fe-TiO
2NSHS-as, 0.2% is metal cations Fe
3+With Ti
4+Mol ratio.
2, Preparation of catalysts:
With the catalyst precursor 0.2% ~ Fe-TiO that obtains
2NSHS-as, the heating rate with 1 ℃/min is warming up to 400 ℃ under air atmosphere in tube furnace, and roasting 2 hours obtains corresponding catalyst and is designated as 0.2% ~ Fe-TiO
2NSHS, 0.2% is metal cations Fe
3+With Ti
4+Mol ratio.
Embodiment 3
1, the preparation of catalyst precursor
Accurately measure the isopropyl alcohol that volume is 71 ml (IPA) and place beaker; Adding 0.05 ml diethylenetriamine (DETA) leniently stirred 3 minutes; After stirring, be that the isopropyl titanate (TIP) of 3.35 ml joins in the above-mentioned solvent and obtains mixed solution with volume.Accurate weighing 0.0135g FeCl
36H
2O is dissolved in the mixed liquor, ultrasonic dispersion 3 minutes.Mixed liquor is gone in the spontaneous pressure agitated reactor of 100 ml, and in 200 ℃ of following crystallization 24 hours, reaction finished to naturally cool to room temperature; Use absolute ethanol washing reaction precipitation thing 3 times then; Washing finish the back in 60 ℃ dry 12 hours down, obtain faint yellow powder, be designated as 0.5% ~ Fe-TiO
2NSHS-as, 0.5% is metal cations Fe
3+With Ti
4+Mol ratio.
2, Preparation of catalysts:
With the catalyst precursor 0.5% ~ Fe-TiO that obtains
2NSHS-as, the heating rate with 1 ℃/min is warming up to 400 ℃ under air atmosphere in tube furnace, and roasting 2 hours obtains corresponding catalyst and is designated as 0.5% ~ Fe-TiO
2NSHS, 0.5% is metal cations Fe
3+With Ti
4+Mol ratio.
Embodiment 4
1, the preparation of catalyst precursor
Accurately measure the isopropyl alcohol that volume is 71 ml (IPA) and place beaker; Adding 0.5 ml diethylenetriamine (DETA) leniently stirred 3 minutes; After stirring, be that the isopropyl titanate (TIP) of 3.35 ml joins in the above-mentioned solvent and obtains mixed solution with volume.Accurate weighing 0.027 g FeCl
36H
2O is dissolved in the mixed liquor, ultrasonic dispersion 3 minutes.Mixed liquor is gone in the spontaneous pressure agitated reactor of 100 ml, and in 200 ℃ of following crystallization 24 hours, reaction finished to naturally cool to room temperature; Use absolute ethanol washing reaction precipitation thing 3 times then; Washing finish the back in 60 ℃ dry 12 hours down, obtain faint yellow powder, be designated as 1% ~ Fe-TiO
2NSHS-as, 1% is metal cations Fe
3+With Ti
4+Mol ratio.
2, Preparation of catalysts:
With the catalyst precursor 1% ~ Fe-TiO that obtains
2NSHS-as, the heating rate with 1 ℃/min is warming up to 400 ℃ under air atmosphere in tube furnace, and roasting 2 hours obtains corresponding catalyst and is designated as 1% ~ Fe-TiO
2NSHS, 1% is metal cations Fe
3+With Ti
4+Mol ratio.
Embodiment 5
1, the preparation of catalyst precursor:
Accurately measure the isopropyl alcohol that volume is 71 ml (IPA) and place beaker; Adding 1 ml diethylenetriamine (DETA) leniently stirred 3 minutes; After stirring, be that the isopropyl titanate (TIP) of 3.35 ml joins in the above-mentioned solvent and obtains mixed solution with volume.Accurate weighing 0.0027 g FeCl
36H
2O is dissolved in the mixed liquor, ultrasonic dispersion 3 minutes.Mixed liquor is gone in the spontaneous pressure agitated reactor of 100 ml, and in 200 ℃ of following crystallization 24 hours, reaction finished to naturally cool to room temperature; Use absolute ethanol washing reaction precipitation thing 3 times then; Washing finish the back in 60 ℃ dry 12 hours down, obtain faint yellow powder, be designated as 0.1% ~ Fe-TiO
2NSHS-as, 0.1% is metal cations Fe
3+With Ti
4+Mol ratio.
2, Preparation of catalysts:
With the catalyst precursor 0.1% ~ Fe-TiO that obtains
2NSHS-as, the heating rate with 1 ℃/min is warming up to 400 ℃ under air atmosphere in tube furnace, and roasting 2 hours obtains corresponding catalyst and is designated as 0.1% ~ Fe-TiO
2NSHS, 0.1% is metal cations Fe
3+With Ti
4+Mol ratio.
Claims (4)
1. the iron of (001) face exposure is mixed the multistage catalyst of titanium dioxide, it is characterized in that this catalyst is made up of titanium, oxygen, iron, and the quality percentage composition of each component is: titanium: 35.5% ~ 45.5%; Oxygen: 55.5% ~ 65.5%; Iron: 0.1% ~ 1%; The building-up process of catalyst adopts the hot method of a step situ solvent, with unformed Fe doped Ti O
2The multistage microballoon of nanometer lamella is a presoma, after roasting, obtains the Detitanium-ore-type Fe doped Ti O that (001) face exposes
2The multistage microspherical catalyst of nanometer lamella is applicable to visible light degradation of organic substances catalytic reaction.
2. multistage catalyst according to claim 1 is characterized in that, described multistage microballoon is of a size of 500nm ~ 700nm, and the specific area of catalyst is 143m
2/ g ~ 160m
2/ g, (001) face exposure is 85% ~ 95%; Fe doped Ti O by the exposure of (001) face
2The self assembly of nanometer lamella forms TiO
2Crystal formation be Detitanium-ore-type, the thickness of nanometer lamella is that 8nm ~ 12nm, nanometer sheet size is 100nm ~ 300nm.
3. claim 1 or 2 described Preparation of catalysts methods is characterized in that preparation process is following:
(1) preparation of catalyst precursor
Accurately measure the solvent isopropyl alcohol IPA of certain volume, add a certain amount of block agent diethylenetriamine DETA, after stirring 3 ~ 5 minutes, a certain amount of isopropyl titanate TIP joined obtain mixed solution in the solvent, accurately the FeCl of weighing certain mass
36H
2O is dissolved in the mixed liquor, ultrasonic dispersion 3 ~ 5 minutes, and wherein the volume ratio of IPA:TIP:DETA is 71:0.05:3.35 ~ 71:1:3.35; Mixed liquor is gone in the spontaneous pressure agitated reactor of 100 ml; In 200 ℃ of following crystallization 20 ~ 28 hours, reaction finished to naturally cool to room temperature, uses absolute ethanol washing reaction precipitation thing 3 ~ 5 times then; Washing finishes back following dry 12 hours in 60 ℃; Obtain faint yellow powder, be catalyst precursor, be designated as x ~ Fe-TiO
2NSHS-as, x are metal cations Fe
3+With Ti
4+Mol ratio, x is 0.1% ~ 1%;
(2) Preparation of catalysts
With the catalyst precursor x ~ Fe-TiO that obtains
2NSHS-as, the heating rate with 1 ℃/min is warming up to 400 ~ 500 ℃ under air atmosphere in tube furnace, and roasting 2 ~ 4 hours obtains corresponding catalyst and is designated as x ~ Fe-TiO
2NSHS.
4. preparation method according to claim 3 is characterized in that, adopts diethylenetriamine DETA as the growth of block agent with control (001) face.
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CN103991902A (en) * | 2014-05-19 | 2014-08-20 | 中国矿业大学 | Preparation method of iron-doped anatase titanium dioxide microspheres with exposed surfaces {001} |
CN104078244A (en) * | 2013-03-26 | 2014-10-01 | 中国科学院大连化学物理研究所 | Metallic-niobium-doping titanium dioxide nanometer sheet, and preparing method and application of metallic-niobium-doping titanium dioxide nanometer sheet |
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CN103316678A (en) * | 2013-06-20 | 2013-09-25 | 北京化工大学 | Multilevel-structure supported nano gold catalyst and preparation method thereof |
CN103316678B (en) * | 2013-06-20 | 2015-10-14 | 北京化工大学 | A kind of multilevel hierarchy load type nano gold catalyst and preparation method thereof |
CN103991902A (en) * | 2014-05-19 | 2014-08-20 | 中国矿业大学 | Preparation method of iron-doped anatase titanium dioxide microspheres with exposed surfaces {001} |
CN103991902B (en) * | 2014-05-19 | 2015-04-22 | 中国矿业大学 | Preparation method of iron-doped anatase titanium dioxide microspheres with exposed surfaces {001} |
CN104772159A (en) * | 2015-04-07 | 2015-07-15 | 北京化工大学 | Nitrogen-doped anatase TiO2 nano-sheet multilevel ball and preparation method thereof |
CN110465294A (en) * | 2019-08-28 | 2019-11-19 | 青岛理工大学 | Nanoscale Iron/mesoporous (001) face is compound-flower pattern crystal cladded type TiO2The preparation method of monocrystalline |
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