CN107459067A - A kind of γ Fe available for the conversion of NOx efficient catalytics2O3Nanometer powder and preparation method thereof - Google Patents
A kind of γ Fe available for the conversion of NOx efficient catalytics2O3Nanometer powder and preparation method thereof Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 53
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 96
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 57
- 229910052742 iron Inorganic materials 0.000 claims abstract description 41
- 230000003197 catalytic effect Effects 0.000 claims abstract description 29
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000012535 impurity Substances 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 17
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 16
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 40
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 claims description 18
- 229910001566 austenite Inorganic materials 0.000 claims description 14
- 238000000746 purification Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 8
- 239000002994 raw material Substances 0.000 abstract description 7
- 238000006555 catalytic reaction Methods 0.000 abstract description 6
- 238000004140 cleaning Methods 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 3
- 238000012545 processing Methods 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- CWPOINBYXIYTHX-UHFFFAOYSA-N ethanol;iron Chemical compound [Fe].CCO CWPOINBYXIYTHX-UHFFFAOYSA-N 0.000 abstract 1
- 230000002000 scavenging effect Effects 0.000 abstract 1
- 238000002604 ultrasonography Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 25
- 239000000047 product Substances 0.000 description 22
- 229910006297 γ-Fe2O3 Inorganic materials 0.000 description 16
- 239000002105 nanoparticle Substances 0.000 description 12
- 239000011259 mixed solution Substances 0.000 description 6
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 239000002086 nanomaterial Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 238000001354 calcination Methods 0.000 description 3
- 239000011858 nanopowder Substances 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- 238000012805 post-processing Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical class ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide (Fe2O3)
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation 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
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
- B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
- B01D53/9404—Removing only nitrogen compounds
- B01D53/9409—Nitrogen oxides
- B01D53/9413—Processes characterised by a specific catalyst
- B01D53/9418—Processes characterised by a specific catalyst for removing nitrogen oxides by selective catalytic reduction [SCR] using a reducing agent in a lean exhaust gas
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
-
- B01J35/23—
-
- B01J35/393—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/01—Engine exhaust gases
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
One kind can be used for NOxThe γ Fe of efficient catalytic2O3Nanometer powder and preparation method thereof, belong to the preparing technical field of environment-friendly type environmental catalysis scavenging material.The nanometer powder by γ phases Fe2O3Particle forms, and the size range of the particle is 23 98nm.Preparation process is as follows：Using pure iron silk as raw material, remove pure iron silk surface impurity, after washed respectively with acetone, ethanol；Iron wire is cut into after segment afterwards and is put into 80mL solution (containing 40 60g NaOH)；Then the 36h of hydro-thermal reaction 20 at 230 265 DEG C；Reaction solution is cooled to room temperature, and rear toward being slowly added to deionized water in system and stir ultrasound, with attraction powder product, auxiliary is separated off other impurities, rear filtering, washing, dry；Calcined 48 hours at 400 DEG C again, rear Temperature fall to room temperature.Nanometer powder preparation cost is low, and processing procedure is pollution-free, expensive instrument and equipment is not required to, in NOxEspecially catalytic cleaning of car tail gas aspect has preferable prospect in terms of efficient catalytic.
Description
Technical field
The invention belongs to nano catalytic material field preparing technical field, and in particular to one kind can be used for NOx especially vapour
Nanometer powder of nitrogen oxides efficient catalytic and preparation method thereof in tail gas.
Background technology
Existing more nano material is used for the catalytic purification field of vehicle exhaust at present, NOx in tail gas is passed through catalysis
Conversion, so as to harmless discharge.Nano-sized iron oxide has higher specific surface area, 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.
Oxide-based nanomaterial of the existing more nanometer powder applied to NOx catalyzed conversion, especially noble metal at present.
But often technology of preparing is complicated, condition is harsh, expensive starting materials for such material, so needing to develop a kind of new preparation method.
γ-Fe2O3Nano-sized iron oxide powder has high-specific surface area, more surface reaction site, be widely used to biologic medical,
Environmental catalysis, field of magnetic material, γ-Fe2O3Nanometer powder preparation is easy, cost is low, can be applied to NOx catalyzed conversion,
The catalytic purification field of vehicle exhaust is expected to play immense value.
Nanometer powder γ-Fe2O3Preparation method mainly has colloid chemistry methods, vapour deposition process, hydro-thermal method, solid state chemistry anti-
Ying Fa, thermal decomposition method, oxidation-precipitation method etc..Above γ-Fe2O3Also be present many deficiencies in the preparation method of nanometer powder, such as prepare
The problems such as complex steps, cost are higher, raw material availability is low.This preparation method is using iron wire as reaction raw materials, in NaOH solution
It is prepared by hydro-thermal reaction, reactions steps are easy, do not need that complex device, cost be cheap, easy batch production, in car tail
By with larger market value in terms of the catalytic purification of nitroxide of gas.γ-the Fe prepared by this method2O3Nanometer powder
There is efficient catalytic conversion performance to NOx, in 400 DEG C of catalytic conversion highests close to 95%.
The content of the invention
It is an object of the invention to provide it is a kind of available for nitrogen oxide in automobile exhaust NOx catalysis environment protecting nano material γ-
Fe2O3Powder and preparation method thereof.γ-Fe of the present invention2O3Powder is by iron wire under 230 ~ 265 DEG C of hydro-thermal reaction
Prepared, by adjusting reaction temperature, reaction time, solvent ratios, post processing calcination process adjust the grain of nanoparticle
Footpath, and then modulation catalytic performance.The composition of above nanoparticle is the Fe of γ phases2O3。
It is an object of the invention to provide it is a kind of available for nitrogen oxide in automobile exhaust NOx catalysis environment protecting nano material and its
Preparation method.
Environment protecting nano material of the present invention has following features：Prepare simply, without expensive device, raw material is cheap,
Processing procedure is green, very promising, and can be applied to nitrogen oxide NOx catalytic treatment in vehicle exhaust.
The iron wire, it is pure iron, by mass percentage, containing Fe：99.95%, 0<P<0.01%, 0<Si<0.01%, 0<C
<0.01%, 0<Cu<0.01%；
A kind of γ-Fe available for the conversion of NOx efficient catalytics of the present invention2O3The preparation method of nano-powder, its step
It is as follows：
（1）Remove pure iron silk（0.5 ~ 2.8mm of diameter, 4 ~ 9 grams of quality）Surface iron rust and impurity, after washed respectively with acetone, ethanol
Wash；
（2）By step（1）Handling after obtained iron wire is cut into the segment of 2cm length and be put into 80mL solution, the solution contains 40-
60g NaOH；
（3）By step（2）Obtained iron wire and mixed solution-36h of hydro-thermal reaction 20 under the conditions of 230-265 DEG C；
（4）By step（3）Obtained reaction solution is cooled to room temperature, rear toward being slowly added to deionized water and stirring 2-5 in system
Hour, ultrasonic 10-15h, with attraction powder product, auxiliary is separated off other a small amount of impurity, rear filtering；
（5）By step（4）Obtained product is washed with absolute alcohol and deionized water respectively, and last washed product is 50-80
24-48 hours are dried at DEG C.
（6）By step（5）Obtained desciccate is calcined 4-8 hours at 400 DEG C again, rear Temperature fall to room temperature.
γ-the Fe2O3Powder can by adjust reaction temperature, the reaction time, solution concentration, post processing calcination process come
The particle diameter of nanoparticle is adjusted, and then obtains the γ-Fe to NOx with efficient catalytic performance2O3Nanometer powder.
Described γ-the Fe to NOx with efficient catalytic performance2O3Nanometer powder is at 230 ~ 265 DEG C by pure iron silk
Prepared under hydro-thermal reaction, the catalysis of the material comes from the γ-Fe2O3The small-size effect and table that nanoparticle has
Face effect, make the dusty material that there is abundant pore structure, larger specific surface area, abundant lattice surface oxygen.
γ-the Fe of the present invention2O3Nanometer powder has following advantage：
The preparation cost of the nanometer powder is cheap, and raw material sources are extensive, processing procedure green non-pollution, it is not necessary to expensive instrument
Equipment, especially there are preferable market prospects in terms of catalytic cleaning of car tail gas in terms of the NOx efficient catalytics.
Brief description of the drawings
Fig. 1：γ-Fe available for the conversion of NOx efficient catalytics2O3Powder energy spectrum diagram.The nano-powder can be learnt from energy spectrum diagram
The mole ratio of Fe elements and O elements be respectively 39.1% and 59.4%, the ratio can illustrate gained nanometer in error range
Powder body material is γ-Fe2O3.Fig. 1 corresponds to the energy spectrum diagram of embodiment 1, the energy spectrum diagram and embodiment of the nanometer powder of other embodiment
1 is similar.
Fig. 2：XRD available for the γ-Fe2O3 powders of NOx efficient catalytics conversion.γ-the Fe of gained2O3Nanometer powder
XRD peaks and Joint Committee on Powder Diffraction Standards（JCPDS）Middle γ-Fe2O3Card coincide, it is main in institute's test sample product spectrogram
Lattice diffraction maximum with standard gamma-Fe2O3Characteristic peak is consistent, it was demonstrated that prepared material is the Fe of γ phases2O3.Fig. 2 is corresponding
The XRD of embodiment 1, the XRD and embodiment 1 of the nanometer powder of other embodiment are similar.
Fig. 3：Raw material hydro-thermal reaction products therefrom under differential responses solution concentration, reaction temperature, then through 400 DEG C of calcinings
Nanometer powder γ-the Fe finally obtained2O3SEM figure（See embodiment 1-4）.Sample a（Scheme a, embodiment 1）：250 DEG C,
NaOH（40g）, 24h；Sample b（Scheme b, embodiment 2）：250 DEG C, NaOH（48g）, 36h；Sample c（Scheme c, embodiment 3）：260
DEG C, NaOH（40g）, 24h；Sample d（Scheme d, embodiment 4）：260 DEG C, NaOH（48g）, 36h.This nanometer of material as seen from Figure 3
Feed powder end γ-Fe2O3Size be mainly distributed between 23 ~ 98nm.
Fig. 4~7：Raw material hydro-thermal reaction products therefrom under differential responses solution concentration, reaction temperature, then forged through 400 DEG C
Burn the nanometer powder γ-Fe finally obtained2O3NOx catalytic conversion break figures (see embodiment 1-4).Sample a (Fig. 4, it is real
Apply example 1)：250 DEG C, NaOH (40g), 24h；Sample b (Fig. 5,
Embodiment 2)：250 DEG C, NaOH (48g), 36h；Sample c (Fig. 6, embodiment 3)：260 DEG C, NaOH (40g), 24h；Sample
D (Fig. 7, embodiment 4)：260 DEG C, NaOH (48g), 36h.Sample a to sample d is respectively in 400 DEG C of NOx catalytic conversions
91.8%th, 92.6%, 93.9% and 94.3%.
Embodiment
Embodiment 1：γ-Fe available for the conversion of NOx efficient catalytics2O3The preparation of powder：
Remove pure iron silk（Diameter 0.5mm, 4 grams of quality）Surface iron rust and impurity, after washed respectively with acetone, ethanol；
（2）By step（1）Handle after obtained iron wire is cut into the segment of 2cm length and be put into 80mL solution, the solution contains 40g
NaOH；
（3）By step（2）Obtained iron wire and mixed solution hydro-thermal reaction 24h under the conditions of 250 DEG C；
（4）By step（3）Obtained reaction solution is cooled to room temperature, rear toward being slowly added to deionized water and stirring 2 hours in system,
Ultrasonic 15h, with attraction powder product, auxiliary is separated off other a small amount of impurity, rear filtering；
（5）By step（4）Obtained product is washed with absolute alcohol and deionized water respectively, and last washed product is entered at 80 DEG C
Row is dried 24 hours.
（6）By step（5）Obtained desciccate is calcined 8 hours at 400 DEG C again, rear Temperature fall to room temperature.
Gained γ-Fe2O3Powder has part reunion, and the size of nano-particle is mainly distributed on 85-25nm, after tested its
It is 91.8% in 400 DEG C of NOx catalytic conversions.
Embodiment 2：γ-Fe available for the conversion of NOx efficient catalytics2O3The preparation of powder：
（1）Remove pure iron silk（Diameter 1.3mm, 4.4 grams of quality）Surface iron rust and impurity, after washed respectively with acetone, ethanol；
（2）By step（1）Handle after obtained iron wire is cut into the segment of 2cm length and be put into 80mL solution, the solution contains 48g
NaOH；
（3）By step（2）Obtained iron wire and mixed solution hydro-thermal reaction 36h under the conditions of 250 DEG C；
（4）By step（3）Obtained reaction solution is cooled to room temperature, rear toward being slowly added to deionized water and stirring 5 hours in system,
Ultrasonic 10h, with attraction powder product, auxiliary is separated off other a small amount of impurity, rear filtering；
（5）By step（4）Obtained product is washed with absolute alcohol and deionized water respectively, and last washed product is entered at 50 DEG C
Row is dried 48 hours.
（6）By step（5）Obtained desciccate is calcined 4 hours at 400 DEG C again, rear Temperature fall to room temperature.
Gained γ-Fe2O3Powder has part reunion, and the size of nano-particle is mainly distributed on 55-27nm, after tested its
It is 92.6% in 400 DEG C of NOx catalytic conversions.
Embodiment 3：γ-Fe available for the conversion of NOx efficient catalytics2O3The preparation of powder：
（1）Remove pure iron silk（Diameter 2.8mm, 4.6 grams of quality）Surface iron rust and impurity, after washed respectively with acetone, ethanol；
（2）By step（1）Handle after obtained iron wire is cut into the segment of 2cm length and be put into 80mL solution, the solution contains 40g
NaOH；
（3）By step（2）Obtained iron wire and mixed solution hydro-thermal reaction 24h under the conditions of 260 DEG C；
（4）By step（3）Obtained reaction solution is cooled to room temperature, rear toward being slowly added to deionized water and stirring 5 hours in system,
Ultrasonic 10h, with attraction powder product, auxiliary is separated off other a small amount of impurity, rear filtering；
（5）By step（4）Obtained product is washed with absolute alcohol and deionized water respectively, and last washed product is entered at 80 DEG C
Row is dried 24 hours.
（6）By step（5）Obtained desciccate is calcined 8 hours at 400 DEG C again, rear Temperature fall to room temperature.
Gained γ-Fe2O3Powder has part reunion, and the size of nano-particle is mainly distributed on 62-33nm, after tested its
It is 93.9% in 400 DEG C of NOx catalytic conversions.
Embodiment 4：γ-Fe available for the conversion of NOx efficient catalytics2O3The preparation of powder：
（1）Remove pure iron silk（Diameter 1.6mm, 4.7 grams of quality）Surface iron rust and impurity, after washed respectively with acetone, ethanol；
（2）By step（1）Handle after obtained iron wire is cut into the segment of 2cm length and be put into 80mL solution, the solution contains 48g
NaOH；
（3）By step（2）Obtained iron wire and mixed solution hydro-thermal reaction 36h under the conditions of 260 DEG C；
（4）By step（3）Obtained reaction solution is cooled to room temperature, rear toward being slowly added to deionized water and stirring 5 hours in system,
Ultrasonic 15h, with attraction powder product, auxiliary is separated off other a small amount of impurity, rear filtering；
（5）By step（4）Obtained product is washed with absolute alcohol and deionized water respectively, and last washed product is entered at 50 DEG C
Row is dried 48 hours.
（6）By step（5）Obtained desciccate is calcined 5 hours at 400 DEG C again, rear Temperature fall to room temperature.
Gained γ-Fe2O3Powder has part reunion, and the size of nano-particle is mainly distributed on 51-30nm, after tested its
It is 94.3% in 400 DEG C of NOx catalytic conversions.
Embodiment 5：γ-Fe available for the conversion of NOx efficient catalytics2O3The preparation of powder：
（1）Remove pure iron silk（Diameter 0.5mm, 9 grams of quality）Surface iron rust and impurity, after washed respectively with acetone, ethanol；
（2）By step（1）Handle after obtained iron wire is cut into the segment of 2cm length and be put into 80mL solution, the solution contains 60g
NaOH；
（3）By step（2）Obtained iron wire and mixed solution hydro-thermal reaction 20h under the conditions of 230 DEG C；
（4）By step（3）Obtained reaction solution is cooled to room temperature, rear toward being slowly added to deionized water and stirring 2 hours in system,
Ultrasonic 10h, with attraction powder product, auxiliary is separated off other a small amount of impurity, rear filtering；
（5）By step（4）Obtained product is washed with absolute alcohol and deionized water respectively, and last washed product is entered at 50 DEG C
Row is dried 24 hours.
（6）By step（5）Obtained desciccate is calcined 8 hours at 400 DEG C again, rear Temperature fall to room temperature.
Gained γ-Fe2O3Powder has part reunion, and the size of nano-particle is mainly distributed on 98-45nm, after tested its
It is 88.1% in 400 DEG C of NOx catalytic conversions.
Embodiment 6：γ-Fe available for the conversion of NOx efficient catalytics2O3The preparation of powder：
（1）Remove pure iron silk（Diameter 2.8mm, 9 grams of quality）Surface iron rust and impurity, after washed respectively with acetone, ethanol；
（2）By step（1）Handle after obtained iron wire is cut into the segment of 2cm length and be put into 80mL solution, the solution contains 60g
NaOH；
（3）By step（2）Obtained iron wire and mixed solution hydro-thermal reaction 36h under the conditions of 265 DEG C；
（4）By step（3）Obtained reaction solution is cooled to room temperature, rear toward being slowly added to deionized water and stirring 2 hours in system,
Ultrasonic 15h, with attraction powder product, auxiliary is separated off other a small amount of impurity, rear filtering；
（5）By step（4）Obtained product is washed with absolute alcohol and deionized water respectively, and last washed product is entered at 80 DEG C
Row is dried 24 hours.
（6）By step（5）Obtained desciccate is calcined 4 hours at 400 DEG C again, rear Temperature fall to room temperature.
Gained γ-Fe2O3Powder has part reunion, and the size of nano-particle is mainly distributed on 49-23nm, after tested its
It is 94.9% in 400 DEG C of NOx catalytic conversions.
Claims (5)
1. one kind can be used for NOxγ-the Fe that nitrogen oxides efficient catalytic purifies especially in vehicle exhaust2O3Nanometer powder, it is special
Sign is：By pure iron silk, hydro-thermal reaction is prepared under NaOH aqueous environments, is formed as the Fe of γ phases2O3。
2. γ-Fe as claimed in claim 12O3Nanometer powder, it is characterised in that：Iron wire is commercial goods, by weight percent
Meter, containing Fe：99.95%, 0<P<0.01%, 0<Si<0.01%, 0<C<0.01%, 0<Cu<0.01%.
A kind of 3. γ-Fe described in claim 12O3The preparation method of nanometer powder, it is characterised in that：
Remove pure iron silk（0.5 ~ 2.8mm of diameter, 4 ~ 9 grams of quality）Surface iron rust and impurity, after washed respectively with acetone, ethanol；
By step（1）Handle after obtained iron wire is cut into the segment of 2cm length and be put into 80mL solution, the solution contains 40-60g
NaOH；
By step（2）Obtained iron wire and mixed solution-36h of hydro-thermal reaction 20 under the conditions of 230-265 DEG C；
By step（3）Obtained reaction solution is cooled to room temperature, rear toward being slowly added to deionized water in system and stirring 2-5 is small
When, ultrasonic 10-15h, with attraction powder product, auxiliary is separated off other a small amount of impurity, rear filtering；
By step（4）Obtained product is washed with absolute alcohol and deionized water respectively, and last washed product is at 50-80 DEG C
24-48 hours are dried.
4. by step（5）Obtained desciccate is calcined 4-8 hours at 400 DEG C again, rear Temperature fall to room temperature.
5. can obtain gained can be used for NOxγ-the Fe of efficient catalytic especially nitrogen oxide in automobile exhaust catalytic purification2O3
Nanometer powder.
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| CN107253737A (en) * | 2017-07-24 | 2017-10-17 | 海南省环境科学研究院 | It is a kind of available for environment protecting nano material of nitrogen oxide in automobile exhaust catalytic purification and preparation method thereof |
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| CN103466717A (en) * | 2013-08-28 | 2013-12-25 | 西北工业大学 | Preparation method for micro-nano jackfruit-like gamma-Fe2O3 powder |
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| CN103466717A (en) * | 2013-08-28 | 2013-12-25 | 西北工业大学 | Preparation method for micro-nano jackfruit-like gamma-Fe2O3 powder |
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| SATOSHI UCHIDA ET AL.: "Synthesis of Monodispersed Micaceous Iron Oxide by the Oxidation of Iron with Oxygen under Hydrothermal Conditions", 《J.CHEM.TECH.BIOTECHNOL》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107253737A (en) * | 2017-07-24 | 2017-10-17 | 海南省环境科学研究院 | It is a kind of available for environment protecting nano material of nitrogen oxide in automobile exhaust catalytic purification and preparation method thereof |
| CN107253737B (en) * | 2017-07-24 | 2018-10-19 | 海南省环境科学研究院 | A kind of environment protecting nano material and preparation method thereof can be used for nitrogen oxide in automobile exhaust catalytic purification |
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