CN107253737A - It is a kind of available for environment protecting nano material of nitrogen oxide in automobile exhaust catalytic purification and preparation method thereof - Google Patents

It is a kind of available for environment protecting nano material of nitrogen oxide in automobile exhaust catalytic purification and preparation method thereof Download PDF

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Publication number
CN107253737A
CN107253737A CN201710604339.6A CN201710604339A CN107253737A CN 107253737 A CN107253737 A CN 107253737A CN 201710604339 A CN201710604339 A CN 201710604339A CN 107253737 A CN107253737 A CN 107253737A
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nano material
environment protecting
iron wire
nitrogen oxide
automobile exhaust
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CN201710604339.6A
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CN107253737B (en
Inventor
王兴利
吴家欢
唐闻雄
王晶博
刘阳生
唐海武
李清贵
吴晓晨
陈表娟
符式锦
符瞰
薛易育
陈峻峰
颜为军
王晨野
莫凌
黄春
张翠萍
穆晓东
钱益斌
王海妹
黄薇
徐诗琴
杨晓姝
盛广能
梁焱
李腾崖
姜佳
符金州
刘贤
蒋林林
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HAINAN RESEARCH ACADEMY OF ENVIRONMENTAL SCIENCES
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HAINAN RESEARCH ACADEMY OF ENVIRONMENTAL SCIENCES
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00Compounds of iron
    • C01G49/02Oxides; Hydroxides
    • C01G49/06Ferric oxide (Fe2O3)
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/92Chemical or biological purification of waste gases of engine exhaust gases
    • B01D53/94Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
    • B01D53/9404Removing only nitrogen compounds
    • B01D53/9409Nitrogen oxides
    • 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
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/62Submicrometer sized, i.e. from 0.1-1 micrometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/64Nanometer sized, i.e. from 1-100 nanometer

Abstract

A kind of environment protecting nano material γ Fe available for nitrogen oxide in automobile exhaust catalytic purification2O3And preparation method thereof, belong to environmental purification technical field of material.The environment protecting nano material by γ phases Fe2O3Particle is constituted, and the size range of the particle is 23~228nm.It is, using the smooth clean iron wire in surface as raw material, to be put into 80mL mixed solutions, the composition of the mixed solution is 5~15mL absolute ethyl alcohols and 33.6g~44.8g KOH, and remaining is deionized water;Then 24~48h of hydro-thermal reaction under the conditions of 270~290 DEG C, then 9~20h of ultrasound, first soaking and stirring 2~5 hours in the ammonia spirit of mass fraction 10%~25%, then soaking and stirring 1~6 minute in the aqueous hydrochloric acid solution of mass fraction 2~6% after filtering;Environment protecting nano material is obtained after deionized water washing, dry, calcining.The preparation cost of the nano material is low, and raw material is cheap, processing procedure green, it is not necessary to complex instrument equipment, in nitrogen oxide in automobile exhaust NOxHaving in terms of catalysis preferably has market prospects.

Description

A kind of environment protecting nano material available for nitrogen oxide in automobile exhaust catalytic purification and its Preparation method
Technical field
The invention belongs to environmental purification technical field of material, and in particular to one kind can be used for nitrogen oxide in automobile exhaust Environment protecting nano material γ-the Fe of catalytic purification2O3And preparation method thereof.
Background technology
Existing more nano material is used for the catalytic purification field of vehicle exhaust at present, makes NO in tail gasxPass through catalysis Conversion, so that harmless discharge.Nano-sized iron oxide has higher specific surface area, and good weatherability can be used for catalyst, life Thing medical material and field of magnetic material.After ferric oxide nano powder is by sintering, catalytic performance is necessarily lifted, and can be used for Cleaning catalyst for tail gases of automobiles field.
Nanometer γ-Fe2O3Preparation method mainly have vapour deposition process, low-temperature plasma chemical deposition, mechanical crushing method, Solid state reaction method, thermal decomposition method, oxidation-precipitation method, hydro-thermal method, colloid chemistry methods etc..The above preparation method is gone back at present There are problems that, such as preparation cost is higher, yield is relatively low or particle is easily reunited.Preparation method of the present invention is with iron wire For reaction raw materials, prepared in alkaline solution by hydro-thermal reaction, reactions steps are simple and convenient, cheap, easily extensive system It is standby, with larger promotion prospect.Nanometer γ-Fe after treatment2O3Nano material is to the NO in vehicle exhaustxHave preferably Catalyticing purifying effect, the NO at 400 DEG CXConversion ratio highest close to 92%.
The content of the invention
It can be used for nitrogen oxide in automobile exhaust NO it is an object of the invention to provide one kindxThe environment protecting nano material of catalytic purification γ-Fe2O3And preparation method thereof.γ-Fe of the present invention2O3Made under hydro-thermal reaction of the iron wire at 270~290 DEG C It is standby, adjust the particle diameter of nanoparticle by adjusting reaction temperature, reaction time, solvent ratios, post processing calcination process, and then Modulation catalytic performance.The composition of above nanoparticle is the Fe of γ phases2O3
Environment protecting nano material of the present invention has following features:Prepare simply, without expensive device, raw material is cheap, Processing procedure environmental protection, it is very promising, and can be applied to nitrogen oxides NO in vehicle exhaustxCatalytic purification processing.
Described iron wire is commercial goods, is superfine pure iron (Taiyuan steel plant pure iron DT4C), by mass percentage, contains Fe:99.9%, 0<P (phosphorus)<0.02%, 0<Si (silicon)<0.02%, 0<C (carbon)<0.03%, 0<S (sulphur)<0.01%, 0<Cu (copper)<0.01%, the impurity such as remaining cobalt (Co), nickel (Ni), zinc (Zn), manganese (Mn) due in iron wire content it is too low, it is low In the detection limit of general instrument, therefore it can omit;
It is of the present invention to can be used for nitrogen oxide in automobile exhaust NOxThe ring of (x span is 1 or 2) catalytic purification Protect nano material γ-Fe2O3Preparation method, its step is as follows:
(1) iron wire (0.5~2.8mm of diameter, 4~9 grams of quality) surface is wiped with emery paper and alcohol swab, removed The oxide on surface is removed, makes surface smooth clean;
(2) iron wire for obtaining step (1) processing, which is cut into after segment, is put into 80mL mixed solutions, the group of the mixed solution As 5mL~15mL absolute ethyl alcohols, 33.6g~44.8g KOH, remaining is deionized water;
(3) iron wire and mixed solution obtained step (2) 24~48h of hydro-thermal reaction under the conditions of 270~290 DEG C;
(4) reaction solution for obtaining step (3) is cooled to room temperature, then 9~20h of ultrasound, then carried out to ultrasonic product Filter, removes the iron wire that unreacted is finished;Particulate obtained by filtering first soaks in the ammonia spirit of mass fraction 10%~25% Bubble stirring 2~5 hours, then soaking and stirring 1~6 minute in the aqueous hydrochloric acid solution of mass fraction 2~6%;
(5) product for obtaining step (4) is washed with deionized, and is finally done washed product at 30~90 DEG C Dry 24~72 hours;
(6) desciccate for obtaining step (5) is calcined 4~8 hours at 350~450 DEG C, Temperature fall to room temperature, from And obtain of the present invention available for nitrogen oxide in automobile exhaust NOxEnvironment protecting nano material γ-the Fe of catalytic purification2O3
The environment protecting nano material can by adjust reaction temperature, the reaction time, solvent ratios, post processing calcination process come The particle diameter (23~228nm) of nanoparticle is adjusted, and then obtains the γ-Fe to nitrogen oxides with different catalytic performances2O3Nanometer Material.
Described can be used for vehicle exhaust NOxEnvironment protecting nano material γ-the Fe of catalysis2O3It is at 270~290 DEG C by iron wire Hydro-thermal reaction under prepared, the catalysis of the material comes from the γ-Fe2O3The more rich pore structure of nanoparticle, compared with Big specific surface area, abundant lattice surface oxygen.
Environment protecting nano material γ-the Fe of the present invention2O3There is following advantage:
The preparation cost of the environment protecting nano material is low, and raw material is cheap, processing procedure green, it is not necessary to complex instrument equipment, In nitrogen oxide in automobile exhaust NOxThere are preferable market prospects in terms of catalysis.
Brief description of the drawings
Fig. 1:Environment protecting nano material γ-Fe2O3Energy spectrum diagram.The Fe elements and O elements of the nano material are can be seen that from energy spectrum diagram Atomic molar number ratio be respectively 39.3% and 59.1%, γ-Fe are met in error range2O3Middle Fe elements and O elements Atomic molar number ratio.The energy spectrum diagram of Fig. 1 correspondence embodiments 1, energy spectrum diagram and the embodiment 1 of the product nano material of other embodiment It is similar.
Fig. 2:Environment protecting nano material γ-Fe2O3XRD.The XRD of the nano material of gained peak and powder diffraction standard γ-Fe in joint committee (JCPDS)2O3Card match, six in institute's test sample product spectrogram at main lattice diffraction maximum with γ-Fe2O3Characteristic peak is consistent, it was demonstrated that prepared material is the Fe of γ phases2O3.The XRD of Fig. 2 correspondence embodiments 1, other The XRD and embodiment 1 of the product nano material of embodiment are similar.
Fig. 3:Product of the raw material under different mixing solution ratios and reaction temperature obtained by hydro-thermal reaction, then forged through 400 DEG C Burn the environment protecting nano material γ-Fe finally obtained2O3SEM scheme (see embodiment 1-4).Sample a (figure a):270 DEG C, KOH (44.8g), ethanol (5mL);Sample b (figure b):270 DEG C, KOH (44.8g), ethanol (10mL);Sample c (figure c):280 DEG C, KOH (44.8g), ethanol (5mL);Sample d (figure d):280 DEG C, KOH (44.8g), ethanol (10mL).The environmental protection as seen from Figure 3 Nano material γ-Fe2O3Size is mainly distributed between 23~228nm.
Fig. 4~7:Product of the raw material under different mixing solution ratios and reaction temperature obtained by hydro-thermal reaction, then through 400 DEG C Calcine the environment protecting nano material γ-Fe finally obtained2O3NOx catalytic conversion break figures (see embodiment 1-4).Sample a (Fig. 4):270 DEG C, KOH (44.8g), ethanol (5mL);Sample b (Fig. 5):270 DEG C, KOH (44.8g), ethanol (10mL);Sample c (Fig. 6):280 DEG C, KOH (44.8g), ethanol (5mL);Sample d (Fig. 7):280 DEG C, KOH (44.8g), ethanol (10mL).Sample a To the NOx catalytic conversion (amount/reaction-ure mixture *s of the reactant of catalytic conversion=converted of the sample d at 400 DEG C 100%) it is respectively 88%, 85%, 92% and 91%.
Embodiment
Embodiment 1:Environment protecting nano material γ-Fe2O3Preparation:
(1) iron wire (diameter 0.5mm, 4.5 grams of quality) surface is wiped with emery paper and alcohol swab, removes surface Oxide, make surface smooth clean;
(2) iron wire (being cut into the long segments of 2cm) is put into 80mL mixed solutions, the composition of the mixed solution is anhydrous for 5mL Ethanol and 44.8g KOH, remaining is deionized water;
(3) iron wire and mixed solution are fitted into the reactor of polytetrafluoroethyllining lining together, reacted under the conditions of 270 DEG C 36h;
(4) room temperature is cooled to after reactor is taken out, then by reaction system ultrasound 9h, then ultrasonic product was carried out Filter, removes the iron wire that unreacted is finished;The first soaking and stirring 2 in the ammonia spirit of mass fraction 10% of particulate obtained by filtering Hour, after in the aqueous hydrochloric acid solution of mass fraction 5% soaking and stirring 1 minute;
(5) above-mentioned product is washed with deionized, 48h is dried at 80 DEG C in last washed product.
(6) by desciccate carry out 400 DEG C calcine 8 hours, Temperature fall to room temperature so that obtain it is of the present invention can For nitrogen oxide in automobile exhaust NOxEnvironment protecting nano material γ-the Fe of catalytic purification2O3, products therefrom quality is about 4.5g.
Gained environment protecting nano material γ-Fe2O3There is part agglomeration, the size of particle is mainly distributed on 228~35nm, It is 88% in 400 DEG C of NOx catalytic conversions after tested.
Embodiment 2:Environment protecting nano material γ-Fe2O3Preparation:
(1) iron wire (diameter 2.8mm, 5 grams of quality) surface is wiped with emery paper and alcohol swab, removes surface Oxide, makes surface smooth clean;
(2) iron wire (being cut into the long segments of 2cm) is put into 80mL mixed solutions, the composition of the mixed solution is anhydrous for 10mL Ethanol and 44.8g KOH, remaining is deionized water;
(3) iron wire and mixed solution are fitted into the reactor of polytetrafluoroethyllining lining together, reacted under the conditions of 270 DEG C 24h;
(4) room temperature is cooled to after reactor is taken out, then by reaction system ultrasound 10h, then ultrasonic product is carried out Filtering, removes the iron wire that unreacted is finished;Particulate obtained by filtering first soaks in the ammonia spirit of mass fraction 10% to be stirred Mix 2 hours, after in the aqueous hydrochloric acid solution of mass fraction 4% soaking and stirring 1 minute;
(5) above-mentioned product is washed with deionized, last washed product is dried 36 hours at 80 DEG C.
(6) by desciccate carry out 400 DEG C calcine 7 hours, Temperature fall to room temperature so that obtain it is of the present invention can For nitrogen oxide in automobile exhaust NOxEnvironment protecting nano material γ-the Fe of catalytic purification2O3, products therefrom quality is about 4.6g.
Gained environment protecting nano material γ-Fe2O3There is part agglomeration, the size of particle is mainly distributed on 220~24nm, It is 85% in 400 DEG C of NOx catalytic conversions after tested.
Embodiment 3:Environment protecting nano material γ-Fe2O3Preparation:
(1) iron wire (diameter 0.5mm, 6 grams of quality) surface is wiped with emery paper and alcohol swab, removes surface Oxide, makes surface smooth clean;
(2) iron wire (being cut into the long segments of 2cm) is put into 80mL mixed solutions, the composition of the mixed solution is anhydrous for 5mL Ethanol and 44.8g KOH, remaining is deionized water;
(3) iron wire and mixed solution are fitted into the reactor of polytetrafluoroethyllining lining together, reacted under the conditions of 280 DEG C 36h;
(4) room temperature is cooled to after reactor is taken out, then by reaction system ultrasound 15h, then ultrasonic product is carried out Filtering, removes the iron wire that unreacted is finished;Particulate obtained by filtering first soaks in the ammonia spirit of mass fraction 15% to be stirred Mix 2 hours, after in the aqueous hydrochloric acid solution of mass fraction 5% soaking and stirring 2 minutes;
(5) above-mentioned product is washed with deionized, last washed product is dried 36 hours at 80 DEG C.
(6) by desciccate carry out 400 DEG C calcine 6 hours, Temperature fall to room temperature so that obtain it is of the present invention can For nitrogen oxide in automobile exhaust NOxEnvironment protecting nano material γ-the Fe of catalytic purification2O3, products therefrom quality is about 5.1g.
Gained environment protecting nano material γ-Fe2O3There is part agglomeration, the size of particle is mainly distributed on 206~28nm, It is 92% in 400 DEG C of NOx catalytic conversions after tested.
Embodiment 4:Environment protecting nano material γ-Fe2O3Preparation:
(1) iron wire (diameter 2.8mm, 6 grams of quality) surface is wiped with emery paper and alcohol swab, removes surface Oxide, makes surface smooth clean;
(2) iron wire (being cut into the long segments of 2cm) is put into 80mL mixed solutions, the composition of the mixed solution is anhydrous for 10mL Ethanol and 44.8g KOH, remaining is deionized water;
(3) iron wire and mixed solution are fitted into the reactor of polytetrafluoroethyllining lining together, reacted under the conditions of 280 DEG C 24h;
(4) room temperature is cooled to after reactor is taken out, then by reaction system ultrasound 15h, then ultrasonic product is carried out Filtering, removes the iron wire that unreacted is finished;Particulate obtained by filtering first soaks in the ammonia spirit of mass fraction 15% to be stirred Mix 2 hours, after in the aqueous hydrochloric acid solution of mass fraction 4% soaking and stirring 2 minutes;
(5) above-mentioned product is washed with deionized, last washed product is dried 24 hours at 80 DEG C.
(6) by desciccate carry out 400 DEG C calcine 5 hours, Temperature fall to room temperature so that obtain it is of the present invention can For nitrogen oxide in automobile exhaust NOxEnvironment protecting nano material γ-the Fe of catalytic purification2O3, products therefrom quality is about 5.0g.
Gained environment protecting nano material γ-Fe2O3There is part agglomeration, the size of particle is mainly distributed on 202~23nm, It is 91% in 400 DEG C of NOx catalytic conversions after tested.
Embodiment 5:Environment protecting nano material γ-Fe2O3Preparation:
(1) iron wire (diameter 1.3mm, 6 grams of quality) surface is wiped with emery paper and alcohol swab, removes surface Oxide, makes surface smooth clean;
(2) iron wire (being cut into the long segments of 2cm) is put into 80mL mixed solutions, the composition of the mixed solution is anhydrous for 15mL Ethanol and 44.8g KOH, remaining is deionized water;
(3) iron wire and mixed solution are fitted into the reactor of polytetrafluoroethyllining lining together, reacted under the conditions of 275 DEG C 24h;
(4) room temperature is cooled to after reactor is taken out, then by reaction system ultrasound 20h, then ultrasonic product is carried out Filtering, removes the iron wire that unreacted is finished;Particulate obtained by filtering first soaks in the ammonia spirit of mass fraction 20% to be stirred Mix 2 hours, after in the aqueous hydrochloric acid solution of mass fraction 5% soaking and stirring 3 minutes;
(5) above-mentioned product is washed with deionized, last washed product is dried 36 hours at 70 DEG C.
(6) by desciccate carry out 400 DEG C calcine 4 hours, Temperature fall to room temperature so that obtain it is of the present invention can For nitrogen oxide in automobile exhaust NOxEnvironment protecting nano material γ-the Fe of catalytic purification2O3, products therefrom quality is about 4.8g.
Gained environment protecting nano material γ-Fe2O3There is part agglomeration, the size of particle is mainly distributed on 217~36nm, It is 86% in 400 DEG C of NOx catalytic conversions after tested.
Embodiment 6:Environment protecting nano material γ-Fe2O3Preparation:
(1) iron wire (diameter 1.6mm, 6 grams of quality) surface is wiped with emery paper and alcohol swab, removes surface Oxide, makes surface smooth clean;
(2) iron wire (being cut into the long segments of 2cm) is put into 80mL mixed solutions, the composition of the mixed solution is anhydrous for 15mL Ethanol and 44.8g KOH, remaining is deionized water;
(3) iron wire and mixed solution are fitted into the reactor of polytetrafluoroethyllining lining together, reacted under the conditions of 275 DEG C 36h;
(4) room temperature is cooled to after reactor is taken out, then by reaction system ultrasound 12h, then ultrasonic product is carried out Filtering, removes the iron wire that unreacted is finished;Particulate obtained by filtering first soaks in the ammonia spirit of mass fraction 25% to be stirred Mix 2 hours, after in 4% aqueous hydrochloric acid solution soaking and stirring 3 minutes;
(5) above-mentioned product is washed with deionized, last washed product is dried 48 hours at 60 DEG C.
(6) by desciccate carry out 400 DEG C calcine 4 hours, Temperature fall to room temperature so that obtain it is of the present invention can For nitrogen oxide in automobile exhaust NOxEnvironment protecting nano material γ-the Fe of catalytic purification2O3, products therefrom quality is about 5.3g.
Gained environment protecting nano material γ-Fe2O3There is part agglomeration, the size of particle is mainly distributed on 212~34nm, It is 89% in 400 DEG C of NOx catalytic conversions after tested.
Embodiment 7:Environment protecting nano material γ-Fe2O3Preparation:
(1) iron wire (diameter 1.6mm, 4 grams of quality) surface is wiped with emery paper and alcohol swab, removes surface Oxide, makes surface smooth clean;
(2) iron wire (being cut into the long segments of 2cm) is put into 80mL mixed solutions, the composition of the mixed solution is anhydrous for 15mL Ethanol and 33.6g KOH, remaining is deionized water;
(3) iron wire and mixed solution are fitted into the reactor of polytetrafluoroethyllining lining together, reacted under the conditions of 290 DEG C 48h;
(4) room temperature is cooled to after reactor is taken out, then by reaction system ultrasound 12h, then ultrasonic product is carried out Filtering, removes the iron wire that unreacted is finished;Particulate obtained by filtering first soaks in the ammonia spirit of mass fraction 25% to be stirred Mix 5 hours, after in 6% aqueous hydrochloric acid solution soaking and stirring 1 minute;
(5) above-mentioned product is washed with deionized, last washed product is dried 24 hours at 90 DEG C.
(6) by desciccate carry out 400 DEG C calcine 8 hours, Temperature fall to room temperature so that obtain it is of the present invention can For nitrogen oxide in automobile exhaust NOxEnvironment protecting nano material γ-the Fe of catalytic purification2O3, products therefrom quality is about 4.3g.
Gained environment protecting nano material γ-Fe2O3There is part agglomeration, the size of particle is mainly distributed on 262~32nm, It is 81% in 400 DEG C of NOx catalytic conversions after tested.
Embodiment 8:Environment protecting nano material γ-Fe2O3Preparation:
(1) iron wire (diameter 2.8mm, 9 grams of quality) surface is wiped with emery paper and alcohol swab, removes surface Oxide, makes surface smooth clean;
(2) iron wire (being cut into the long segments of 2cm) is put into 80mL mixed solutions, the composition of the mixed solution is anhydrous for 15mL Ethanol and 33.6g KOH, remaining is deionized water;
(3) iron wire and mixed solution are fitted into the reactor of polytetrafluoroethyllining lining together, reacted under the conditions of 290 DEG C 48h;
(4) room temperature is cooled to after reactor is taken out, then by reaction system ultrasound 12h, then ultrasonic product is carried out Filtering, removes the iron wire that unreacted is finished;Particulate obtained by filtering first soaks in the ammonia spirit of mass fraction 25% to be stirred Mix 5 hours, after in 2% aqueous hydrochloric acid solution soaking and stirring 6 minutes;
(5) above-mentioned product is washed with deionized, last washed product is dried 72 hours at 30 DEG C.
(6) by desciccate carry out 400 DEG C calcine 8 hours, Temperature fall to room temperature so that obtain it is of the present invention can For nitrogen oxide in automobile exhaust NOxEnvironment protecting nano material γ-the Fe of catalytic purification2O3, products therefrom quality is about 5.7g.
Gained environment protecting nano material γ-Fe2O3There is part agglomeration, the size of particle is mainly distributed on 252~30nm, It is 83% in 400 DEG C of NOx catalytic conversions after tested.

Claims (2)

1. a kind of environment protecting nano material γ-Fe available for nitrogen oxide in automobile exhaust catalytic purification2O3Preparation method, its walk It is rapid as follows:
(1) by 0.5~2.8mm of diameter, the iron wire surface of 4~9 grams of quality is wiped with emery paper and alcohol swab, removes table The oxide in face, makes surface smooth clean;
(2) iron wire for obtaining step (1) processing, which is cut into after segment, is put into 80mL mixed solutions, and the composition of the mixed solution is 5mL~15mL absolute ethyl alcohols, 33.6g~44.8g KOH, remaining is deionized water;
(3) iron wire and mixed solution obtained step (2) 24~48h of hydro-thermal reaction under the conditions of 270~290 DEG C;
(4) reaction solution for obtaining step (3) is cooled to room temperature, then 9~20h of ultrasound, then filtered to ultrasonic product, goes The iron wire finished except unreacted;The first soaking and stirring in the ammonia spirit of mass fraction 10%~25% of particulate obtained by filtering 2~5 hours, then soaking and stirring 1~6 minute in the aqueous hydrochloric acid solution of mass fraction 2~6%;
(5) product for obtaining step (4) is washed with deionized, and washed product finally is dried into 24 at 30~90 DEG C ~72 hours;
(6) desciccate for obtaining step (5) is calcined 4~8 hours at 350~450 DEG C, and Temperature fall is to room temperature, so as to obtain It can be used for nitrogen oxide in automobile exhaust NO to of the present inventionxEnvironment protecting nano material γ-the Fe of catalytic purification2O3
2. a kind of environment protecting nano material γ-Fe available for nitrogen oxide in automobile exhaust catalytic purification2O3, it is characterised in that:Be by Method described in claim 1 is prepared.
CN201710604339.6A 2017-07-24 2017-07-24 A kind of environment protecting nano material and preparation method thereof can be used for nitrogen oxide in automobile exhaust catalytic purification Active CN107253737B (en)

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CN1108425A (en) * 1994-03-07 1995-09-13 中国科学院山西煤炭化学研究所 Super-fine magnetic powder and its prepn. method
CN101898749A (en) * 2010-08-02 2010-12-01 武汉理工大学 Method for preparing metal oxide hollow particles or fibers
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