CN107253737B - A kind of environment protecting nano material and preparation method thereof can be used for nitrogen oxide in automobile exhaust catalytic purification - Google Patents
A kind of environment protecting nano material and preparation method thereof can be used for nitrogen oxide in automobile exhaust catalytic purification Download PDFInfo
- Publication number
- CN107253737B CN107253737B CN201710604339.6A CN201710604339A CN107253737B CN 107253737 B CN107253737 B CN 107253737B CN 201710604339 A CN201710604339 A CN 201710604339A CN 107253737 B CN107253737 B CN 107253737B
- Authority
- CN
- China
- Prior art keywords
- nano material
- environment protecting
- iron wire
- nitrogen oxide
- automobile exhaust
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 52
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 32
- 238000000746 purification Methods 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 116
- 229910052742 iron Inorganic materials 0.000 claims abstract description 48
- 239000011259 mixed solution Substances 0.000 claims abstract description 34
- 235000019441 ethanol Nutrition 0.000 claims abstract description 29
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 22
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 22
- 239000002245 particle Substances 0.000 claims abstract description 21
- 238000002791 soaking Methods 0.000 claims abstract description 14
- 239000000243 solution Substances 0.000 claims abstract description 13
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 11
- 238000002604 ultrasonography Methods 0.000 claims abstract description 11
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 9
- 238000012545 processing Methods 0.000 claims abstract description 6
- 125000005909 ethyl alcohol group Chemical group 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 45
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 42
- 229910001651 emery Inorganic materials 0.000 claims description 10
- 238000000034 method Methods 0.000 abstract description 9
- 238000001914 filtration Methods 0.000 abstract description 8
- 239000002994 raw material Substances 0.000 abstract description 7
- 238000006555 catalytic reaction Methods 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 5
- 238000001354 calcination Methods 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 229910006297 γ-Fe2O3 Inorganic materials 0.000 description 24
- 238000005054 agglomeration Methods 0.000 description 8
- 230000002776 aggregation Effects 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 229910001566 austenite Inorganic materials 0.000 description 7
- 238000010586 diagram Methods 0.000 description 7
- 239000002105 nanoparticle Substances 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- 238000012805 post-processing Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 229910052759 nickel 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
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 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
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- 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
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Nanotechnology (AREA)
- Crystallography & Structural Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Combustion & Propulsion (AREA)
- Composite Materials (AREA)
- Biomedical Technology (AREA)
- Environmental & Geological Engineering (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Catalysts (AREA)
- Exhaust Gas Treatment By Means Of Catalyst (AREA)
Abstract
A kind of environment protecting nano material γ Fe can be used 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 forms, and the size range of the particle is 23~228nm.It is to be put into 80mL mixed solutions using the smooth clean iron wire in surface as raw material, the group of the mixed solution becomes 5~15mL absolute ethyl alcohols and 33.6g~44.8g KOH, 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 manufacturing cost of the nano material is low, and raw material is cheap, and processing procedure green does not need complex instrument equipment, in nitrogen oxide in automobile exhaust NOxWith preferable with market prospects in terms of catalysis.
Description
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
Have the catalytic purification field that more nano material is used for vehicle exhaust at present, makes NO in tail gasxPass through catalysis
Conversion, to harmless discharge.There is nano-sized iron oxide higher specific surface area, good weatherability can be used for catalyst, life
Object medical material and field of magnetic material.After ferric oxide nano powder is by sintering, catalytic performance is centainly promoted, 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 manufacturing cost is higher, yield is relatively low or particle is easy to reunite.Preparation method of the present invention is with iron wire
It for reaction raw materials, is prepared by hydro-thermal reaction in alkaline solution, simple and convenient, cheap, the easily extensive system of reaction step
It is standby, there is 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%.
Invention content
The object of the present invention is to provide one kind can be used for nitrogen oxide in automobile exhaust NOxThe environment protecting nano material of catalytic purification
γ-Fe2O3And preparation method thereof.γ-Fe of the present invention2O3It is made under 270~290 DEG C of hydro-thermal reaction by iron wire
It is standby, the grain size of nanoparticle is adjusted by adjusting reaction temperature, reaction time, solvent ratios, post-processing calcination process, in turn
Modulation catalytic performance.The group of the above nanoparticle becomes the Fe of γ phases2O3。
Environment protecting nano material of the present invention has following features：It preparing simply, is not necessarily to expensive device, raw material is cheap,
Processing procedure is environmentally protective, very promising, and can be applied to nitrogen oxides NO in vehicle exhaustxCatalytic purification processing.
The iron wire is commercial goods, for superfine pure iron (Taiyuan steel plant pure iron DT4C), by mass percentage, is contained
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 can omit；
It is of the present invention to can be used for nitrogen oxide in automobile exhaust NOxThe ring of (value range of x is 1 or 2) catalytic purification
Protect nano material γ-Fe2O3Preparation method, its step are 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, is removed
The oxide for going to surface keeps surface smooth clean；
(2) iron wire that step (1) processing obtains is cut into after segment and 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 that step (3) obtains is cooled to room temperature, then 9~20h of ultrasound, then ultrasonic product was carried out
Filter, the iron wire that removal unreacted finishes；Obtained particle is filtered first to soak 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 that step (4) obtains is washed with deionized, finally does 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 it obtains of the present invention can be used 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 grain size (23~228nm) of nanoparticle is adjusted, and then obtains the γ-Fe that there are different catalytic performances to nitrogen oxides2O3Nanometer
Material.
Described can be used for vehicle exhaust NOxEnvironment protecting nano material γ-the Fe of catalysis2O3It is by iron wire at 270~290 DEG C
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 manufacturing cost of the environment protecting nano material is low, and raw material is cheap, and processing procedure green does not need complex instrument equipment,
In nitrogen oxide in automobile exhaust NOxThere are preferable market prospects in terms of catalysis.
Description of the drawings
Fig. 1：Environment protecting nano material γ-Fe2O3Energy spectrum diagram.It can be seen that the Fe elements and O elements of the nano material from energy spectrum diagram
Atomic molar number ratio be respectively 39.3% and 59.1%, meet γ-Fe in error range2O3Middle Fe elements and O elements
Atomic molar number ratio.The energy spectrum diagram of Fig. 1 corresponding 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 diagram.The peak of the XRD of the nano material of gained and powder diffraction standard
γ-Fe in joint committee (JCPDS)2O3Card match, six in institute's sample 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 diagram of Fig. 2 corresponding embodiments 1, other
The XRD diagram of the product nano material of embodiment is similar with embodiment 1.
Fig. 3：Product of the raw material under different mixed solutions proportioning and reaction temperature obtained by hydro-thermal reaction, then forged through 400 DEG C
Burn the environment protecting nano material γ-Fe finally obtained2O3SEM figure (see embodiment 1-4).Sample a (figure a)：270 DEG C, KOH
(44.8g), ethyl alcohol (5mL)；Sample b (figure b)：270 DEG C, KOH (44.8g), ethyl alcohol (10mL)；Sample c (figure c)：280 DEG C, KOH
(44.8g), ethyl alcohol (5mL)；Sample d (figure d)：280 DEG C, KOH (44.8g), ethyl alcohol (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 mixed solutions proportioning 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), ethyl alcohol (5mL)；Sample b (Fig. 5)：270 DEG C, KOH (44.8g), ethyl alcohol (10mL)；Sample c
(Fig. 6)：280 DEG C, KOH (44.8g), ethyl alcohol (5mL)；Sample d (Fig. 7)：280 DEG C, KOH (44.8g), ethyl alcohol (10mL).Sample a
NOx catalytic conversions (amount/reaction-ure mixture * of the reactant for catalytic conversion=converted to sample d at 400 DEG C
100%) it is respectively 88%, 85%, 92% and 91%.
Specific implementation mode
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, keep surface smooth clean；
(2) iron wire (being cut into 2cm long segments) is put into 80mL mixed solutions, the group of the mixed solution is anhydrous as 5mL
Ethyl alcohol and 44.8g KOH, remaining is deionized water；
(3) iron wire and mixed solution are fitted into the reaction kettle of polytetrafluoroethyllining lining together, are reacted under the conditions of 270 DEG C
36h；
(4) reaction kettle is taken out into postcooling to room temperature, then by reaction system ultrasound 9h, then ultrasonic product was carried out
Filter, the iron wire that removal unreacted finishes；Filter the obtained particle first soaking and stirring 2 in the ammonia spirit of mass fraction 10%
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, to 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 are part agglomeration, the size of particle to be 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 keeps surface smooth clean；
(2) iron wire (being cut into 2cm long segments) is put into 80mL mixed solutions, the group of the mixed solution is anhydrous as 10mL
Ethyl alcohol and 44.8g KOH, remaining is deionized water；
(3) iron wire and mixed solution are fitted into the reaction kettle of polytetrafluoroethyllining lining together, are reacted under the conditions of 270 DEG C
24h；
(4) reaction kettle is taken out into postcooling to room temperature, then by reaction system ultrasound 10h, then ultrasonic product is carried out
Filtering, the iron wire that removal unreacted finishes；First impregnate in the ammonia spirit of mass fraction 10% of obtained particle is filtered to stir
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, to 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 are part agglomeration, the size of particle to be 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 keeps surface smooth clean；
(2) iron wire (being cut into 2cm long segments) is put into 80mL mixed solutions, the group of the mixed solution is anhydrous as 5mL
Ethyl alcohol and 44.8g KOH, remaining is deionized water；
(3) iron wire and mixed solution are fitted into the reaction kettle of polytetrafluoroethyllining lining together, are reacted under the conditions of 280 DEG C
36h；
(4) reaction kettle is taken out into postcooling to room temperature, then by reaction system ultrasound 15h, then ultrasonic product is carried out
Filtering, the iron wire that removal unreacted finishes；First impregnate in the ammonia spirit of mass fraction 15% of obtained particle is filtered to stir
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, to 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 are part agglomeration, the size of particle to be 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 keeps surface smooth clean；
(2) iron wire (being cut into 2cm long segments) is put into 80mL mixed solutions, the group of the mixed solution is anhydrous as 10mL
Ethyl alcohol and 44.8g KOH, remaining is deionized water；
(3) iron wire and mixed solution are fitted into the reaction kettle of polytetrafluoroethyllining lining together, are reacted under the conditions of 280 DEG C
24h；
(4) reaction kettle is taken out into postcooling to room temperature, then by reaction system ultrasound 15h, then ultrasonic product is carried out
Filtering, the iron wire that removal unreacted finishes；First impregnate in the ammonia spirit of mass fraction 15% of obtained particle is filtered to stir
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, to 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 are part agglomeration, the size of particle to be 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 keeps surface smooth clean；
(2) iron wire (being cut into 2cm long segments) is put into 80mL mixed solutions, the group of the mixed solution is anhydrous as 15mL
Ethyl alcohol and 44.8g KOH, remaining is deionized water；
(3) iron wire and mixed solution are fitted into the reaction kettle of polytetrafluoroethyllining lining together, are reacted under the conditions of 275 DEG C
24h；
(4) reaction kettle is taken out into postcooling to room temperature, then by reaction system ultrasound 20h, then ultrasonic product is carried out
Filtering, the iron wire that removal unreacted finishes；First impregnate in the ammonia spirit of mass fraction 20% of obtained particle is filtered to stir
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, to 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 are part agglomeration, the size of particle to be 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 keeps surface smooth clean；
(2) iron wire (being cut into 2cm long segments) is put into 80mL mixed solutions, the group of the mixed solution is anhydrous as 15mL
Ethyl alcohol and 44.8g KOH, remaining is deionized water；
(3) iron wire and mixed solution are fitted into the reaction kettle of polytetrafluoroethyllining lining together, are reacted under the conditions of 275 DEG C
36h；
(4) reaction kettle is taken out into postcooling to room temperature, then by reaction system ultrasound 12h, then ultrasonic product is carried out
Filtering, the iron wire that removal unreacted finishes；First impregnate in the ammonia spirit of mass fraction 25% of obtained particle is filtered to stir
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, to 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 are part agglomeration, the size of particle to be 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 keeps surface smooth clean；
(2) iron wire (being cut into 2cm long segments) is put into 80mL mixed solutions, the group of the mixed solution is anhydrous as 15mL
Ethyl alcohol and 33.6g KOH, remaining is deionized water；
(3) iron wire and mixed solution are fitted into the reaction kettle of polytetrafluoroethyllining lining together, are reacted under the conditions of 290 DEG C
48h；
(4) reaction kettle is taken out into postcooling to room temperature, then by reaction system ultrasound 12h, then ultrasonic product is carried out
Filtering, the iron wire that removal unreacted finishes；First impregnate in the ammonia spirit of mass fraction 25% of obtained particle is filtered to stir
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, to 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 are part agglomeration, the size of particle to be 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 keeps surface smooth clean；
(2) iron wire (being cut into 2cm long segments) is put into 80mL mixed solutions, the group of the mixed solution is anhydrous as 15mL
Ethyl alcohol and 33.6g KOH, remaining is deionized water；
(3) iron wire and mixed solution are fitted into the reaction kettle of polytetrafluoroethyllining lining together, are reacted under the conditions of 290 DEG C
48h；
(4) reaction kettle is taken out into postcooling to room temperature, then by reaction system ultrasound 12h, then ultrasonic product is carried out
Filtering, the iron wire that removal unreacted finishes；First impregnate in the ammonia spirit of mass fraction 25% of obtained particle is filtered to stir
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, to 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 are part agglomeration, the size of particle to be mainly distributed on 252~30nm,
It is 83% in 400 DEG C of NOx catalytic conversions after tested.
Claims (1)
1. one kind can be used for nitrogen oxide in automobile exhaust NOxEnvironment protecting nano material γ-the Fe of catalytic purification2O3Preparation method,
Steps are 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 keeps surface smooth clean；
(2) iron wire that step (1) processing obtains is cut into after segment and is put into 80mL mixed solutions, the group of the mixed solution becomes
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 that step (3) obtains is cooled to room temperature, then 9~20h of ultrasound, then ultrasonic product is filtered, gone
The iron wire finished except unreacted；Filter the obtained particle first soaking and stirring in the ammonia spirit of mass fraction 10%~25%
2~5 hours, then soaking and stirring 1~6 minute in the aqueous hydrochloric acid solution of mass fraction 2~6%；
(5) product that step (4) obtains is washed with deionized, washed product is finally dried 24 at 30~90 DEG C
~72 hours；
(6) desciccate for obtaining step (5) is calcined 4~8 hours at 350~450 DEG C, Temperature fall to room temperature, to
It can be used for nitrogen oxide in automobile exhaust NO to describedxEnvironment protecting nano material γ-the Fe of catalytic purification2O3。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710604339.6A CN107253737B (en) | 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 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710604339.6A CN107253737B (en) | 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 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107253737A CN107253737A (en) | 2017-10-17 |
| CN107253737B true CN107253737B (en) | 2018-10-19 |
Family
ID=60025106
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710604339.6A Expired - Fee Related CN107253737B (en) | 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 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107253737B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN101993113A (en) * | 2010-09-20 | 2011-03-30 | 烟台大学 | Low-temperature industrial preparation method of monodisperse superparamagnetic gamma-Fe2O3 nanoparticles |
| CN107459067A (en) * | 2017-07-08 | 2017-12-12 | 王兴利 | A kind of γ Fe available for the conversion of NOx efficient catalytics2O3Nanometer powder and preparation method thereof |
-
2017
- 2017-07-24 CN CN201710604339.6A patent/CN107253737B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN101993113A (en) * | 2010-09-20 | 2011-03-30 | 烟台大学 | Low-temperature industrial preparation method of monodisperse superparamagnetic gamma-Fe2O3 nanoparticles |
| CN107459067A (en) * | 2017-07-08 | 2017-12-12 | 王兴利 | A kind of γ Fe available for the conversion of NOx efficient catalytics2O3Nanometer powder and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107253737A (en) | 2017-10-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108554439B (en) | Photo-reduction of CO2Ultrathin Ti-based LDHs composite photocatalyst and preparation method thereof | |
| EP1894620B2 (en) | Method to produce a porous zirconia powder | |
| CN112619648B (en) | Copper-cobalt-based catalyst for organic sulfur hydrolysis removal and preparation method thereof | |
| CN109482175B (en) | Manganese-potassium ore type manganese dioxide catalyst with yolk-shell structure and preparation method and application thereof | |
| CN102315433A (en) | Graphene loaded Cu-CuxO composite material and preparation method thereof | |
| CN106975479B (en) | Sea urchin-shaped CeO2-MnO2Process for producing composite oxide catalyst | |
| CN101879439A (en) | Preparation method of composite oxide | |
| JP5459322B2 (en) | Redox material for thermochemical water splitting and hydrogen production method | |
| JP5110868B2 (en) | Method for producing perovskite complex oxide precursor and method for producing perovskite complex oxide | |
| CN110586094B (en) | Copper-based nanoflower catalyst for producing methanol and ethylene glycol by ethylene carbonate hydrogenation and preparation method thereof | |
| CN111377475A (en) | Method for manufacturing oxygen vacancy-containing CuO nanosheet | |
| CN103357394A (en) | Catalyst for synthesizing glycerol carbonate from glycerol, method for producing the catalyst and method for synthesizing glycerol carbonate from glycerol using the catalyst | |
| Fu et al. | Highly dispersed rhodium atoms supported on defect-rich Co (OH) 2 for the chemoselective hydrogenation of nitroarenes | |
| CN102275974B (en) | Preparation method of ultra-micrometer copper oxide powdery material | |
| CN110745862A (en) | Method for producing nano lead oxide by cleaning transformation-microwave pyrolysis of lead sulfate paste | |
| CN107253737B (en) | A kind of environment protecting nano material and preparation method thereof can be used for nitrogen oxide in automobile exhaust catalytic purification | |
| CN113134352B (en) | Composite metal oxide catalyst for catalyzing direct decomposition of nitrogen oxide and preparation method thereof | |
| JP2007083197A (en) | Method for producing copper-zinc-aluminum based catalyst | |
| CN101565208A (en) | Method for preparing manganic manganous oxide nano-material | |
| CN114849789B (en) | Preparation method and application of MIL-125 supported 1T-phase molybdenum sulfide composite photocatalyst | |
| CN107459067B (en) | A kind of γ-Fe can be used for the conversion of NOx efficient catalytic2O3Nanometer powder and preparation method thereof | |
| CN117019214A (en) | Preparation method of catalyst for improving denitration performance of metal modified SSZ-13 | |
| JPH0535017B2 (en) | ||
| CN114377709A (en) | Hydrothermal method for preparing CeO2/Ce(OH)CO3Method of heterojunction | |
| CN115245820A (en) | Spinel catalyst, preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20181019 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |