CN106315657B - A kind of preparation method of nano-metal-oxide - Google Patents
A kind of preparation method of nano-metal-oxide Download PDFInfo
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- CN106315657B CN106315657B CN201610644179.3A CN201610644179A CN106315657B CN 106315657 B CN106315657 B CN 106315657B CN 201610644179 A CN201610644179 A CN 201610644179A CN 106315657 B CN106315657 B CN 106315657B
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- 229910044991 metal oxide Inorganic materials 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229910002651 NO3 Inorganic materials 0.000 claims abstract description 48
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000000203 mixture Substances 0.000 claims abstract description 42
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 14
- 230000001007 puffing effect Effects 0.000 claims abstract description 11
- 239000007864 aqueous solution Substances 0.000 claims abstract description 3
- 239000003921 oil Substances 0.000 claims description 20
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- UPHWVVKYDQHTCF-UHFFFAOYSA-N octadecylazanium;acetate Chemical compound CC(O)=O.CCCCCCCCCCCCCCCCCCN UPHWVVKYDQHTCF-UHFFFAOYSA-N 0.000 claims description 12
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 claims description 4
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 4
- 229910001960 metal nitrate Inorganic materials 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 3
- 229910052684 Cerium Inorganic materials 0.000 claims description 2
- 239000012075 bio-oil Substances 0.000 claims description 2
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 2
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 2
- 239000010687 lubricating oil Substances 0.000 claims description 2
- 239000004200 microcrystalline wax Substances 0.000 claims description 2
- 239000012188 paraffin wax Substances 0.000 claims description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical group [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 2
- 239000001993 wax Substances 0.000 claims description 2
- -1 Naina this 810 Substances 0.000 claims 1
- LSHFIWNMHGCYRS-UHFFFAOYSA-N [O-][N+]([O-])=O.[O-][N+]([O-])=O.[OH4+2] Chemical compound [O-][N+]([O-])=O.[O-][N+]([O-])=O.[OH4+2] LSHFIWNMHGCYRS-UHFFFAOYSA-N 0.000 claims 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims 1
- 230000035699 permeability Effects 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 16
- 230000000694 effects Effects 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 229910003455 mixed metal oxide Inorganic materials 0.000 abstract 1
- 238000001354 calcination Methods 0.000 description 18
- 230000005540 biological transmission Effects 0.000 description 15
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 12
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 11
- 239000012071 phase Substances 0.000 description 11
- 239000013078 crystal Substances 0.000 description 10
- 238000001228 spectrum Methods 0.000 description 8
- 229960004643 cupric oxide Drugs 0.000 description 7
- 238000004090 dissolution Methods 0.000 description 7
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 6
- 238000002485 combustion reaction Methods 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 6
- 239000002086 nanomaterial Substances 0.000 description 6
- 238000000746 purification Methods 0.000 description 6
- 239000000470 constituent Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 239000002105 nanoparticle Substances 0.000 description 5
- 238000012876 topography Methods 0.000 description 5
- 229910000420 cerium oxide Inorganic materials 0.000 description 4
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(2+);cobalt(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 description 4
- 239000005751 Copper oxide Substances 0.000 description 3
- ODPUKHWKHYKMRK-UHFFFAOYSA-N cerium;nitric acid Chemical compound [Ce].O[N+]([O-])=O ODPUKHWKHYKMRK-UHFFFAOYSA-N 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 229910000431 copper oxide Inorganic materials 0.000 description 3
- 239000002283 diesel fuel Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000011787 zinc oxide Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 239000004202 carbamide Substances 0.000 description 2
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 2
- 229940044927 ceric oxide Drugs 0.000 description 2
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 2
- 238000009841 combustion method Methods 0.000 description 2
- 238000004945 emulsification Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 2
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- OERNJTNJEZOPIA-UHFFFAOYSA-N zirconium nitrate Chemical compound [Zr+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O OERNJTNJEZOPIA-UHFFFAOYSA-N 0.000 description 2
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003245 coal Substances 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
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- WXYNCCWBUXKSBG-UHFFFAOYSA-N copper;nitric acid Chemical compound [Cu].O[N+]([O-])=O WXYNCCWBUXKSBG-UHFFFAOYSA-N 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000007734 materials engineering Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000012184 mineral wax Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- IJRVLVIFMRWJRQ-UHFFFAOYSA-N nitric acid zinc Chemical compound [Zn].O[N+]([O-])=O IJRVLVIFMRWJRQ-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 239000011775 sodium fluoride Substances 0.000 description 1
- 235000013024 sodium fluoride Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/02—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
-
- 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]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/04—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
-
- 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
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- 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
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of preparation methods of nano-metal-oxide, include the following steps, by nitrate aqueous solution under emulsifier effect puffing is formationed porosity nitrate mixture, be then uniformly mixed with oil phase and be placed in Muffle furnace the corresponding nano-metal-oxide of roasting acquisition.The nano-metal-oxide that the present invention prepares can be the oxide of single metallic element, can also be the mixed-metal oxides of several elements.The method of the present invention is simple for process, easy to operate, helps to improve nano-metal-oxide stability and size tunable, while simplifying preparation section and improving efficiency, more conducively industrialized production.
Description
Technical field
The present invention relates to field of nano material preparation, and in particular to the preparation side of one or more nano-metal-oxides
Method.
Background technology
Due to influences such as skin effect, quantum size effect, small-size effect and macroscopic quantum effects, a nanometer ruler is resulted in
Very little material has the special performance that raw material do not have, to keep nano material living in thermodynamics, optics, catalysis, biology
Many aspects such as property show unusual physics and chemical characteristic so that nano material is obtained as functional material in many fields
Extensive research and application.
Although many aspects of nano material have superior performance, then material itself prepares relative complex, it is full
Sufficient nanoscale materials engineering demand, so many people propose that many methods prepare nano material.In nano-metal-oxide such as
CN101342486A prepares nano-oxide using the method for microwave heating, and CN102616748A is obtained by dissolving recrystallization method
Nano-oxide is obtained, CN1403375A hydro-thermal methods obtain nano-oxide, and CN1613772A combustion methods obtain nano-oxide etc.,
In general, it prepares nano-metal-oxide and is broadly divided into vapor phase method, liquid phase method and solid phase method.Nitrate shape is utilized in solid phase method
At self-propagating combustion due to preparation method it is simple, product preparation amount is relatively large, and the features such as being convenient for industrialization obtains
Extensive attention has been arrived, research hotspot is also become.CN103420341A obtains nano oxygen using ammonium nitrate and triethanolamine combustion method
Compound, CN102583256A be added sodium fluoride control nitrate combustion mode realize nano-oxide, CN103935961A with
Nitrate aerosol spray method on heat source obtains nano-metal-oxide, and CN101462722A urea and ammonium nitrate are fuel
Prepare nano-oxide etc..
Take a broad view of the nano-metal-oxide that current self-propagating combustion obtains have the shortcomings that it is notable, since ammonium nitrate is normal
Self-sustaining burning is can not achieve under normal temperature and pressure, once extraneous heat supply burning i.e. stopping, the mixture based on ammonium nitrate that stop also being deposited
In this phenomenon so that slow in ammonium nitrate mixture reaction speed, combustion reaction is incomplete, therefore the nano-metal-oxide obtained
Stability there are some problems.Another aspect citric acid or urea etc. need to prepare first to prepare nano-metal-oxide
Presoma causes to need to consume a large amount of energy when preparing nano-particle, be unfavorable for due to containing a large amount of water in presoma
Industrialized production.
Another aspect preparation section is relatively cumbersome, improves efficiency to simplify preparation section, while improving metal nano oxidation
Object stability and size tunable, therefore carry out the present invention.
Invention content
The object of the present invention is to provide one kind, low energy consumption, preparation section is simple, efficient, while can improve nano metal
Oxide stability and the single nano-metal-oxide of size tunable or the preparation method of nano composite metal oxide.
Realize that the technical solution of the object of the invention is：
A kind of preparation method of nano-metal-oxide, includes the following steps：It is first that ammonium nitrate and metal nitrate is molten
Yu Shuizhong is added emulsifier, porosity nitrate mixture is obtained through puffing after；Secondly by porosity nitrate mixture with
Oil phase is calcined 1-3 hours at 600-1000 DEG C obtain nano-metal-oxide after mixing.
In above-mentioned steps, the metal nitrate be cerous nitrate, zinc nitrate, zirconium nitrate and aluminum nitrate in any one or
Person is several.
In above-mentioned steps, the emulsifier is octadecylamine or octadecylamine acetate salt.
In above-mentioned steps, the puffing process is that emulsifier is added in nitrate aqueous solution, and heating for dissolving forms water
After the emulsification system for wrapping oil, vacuumize to obtain porosity nitrate mixture under the conditions of -0.08~-0.09MPa, wherein institute
It is 110-120 DEG C to state solution temperature.
In above-mentioned steps, in the porosity nitrate mixture, the mass fraction of nitrate is 90%~95%, emulsification
The mass fraction of agent is 0.15%-0.2%, remaining is water.
In above-mentioned steps, the oil phase be diesel oil, lubricating oil, bio-oil, coal derived oil, Naina this 801 and 810,
It is one or more in paraffin, microwax, complex wax etc., and oil phase needs to be heated to fusing point to form uniform liquid.
In above-mentioned steps, oxygen balance is positive oxygen balance after porosity nitrate mixture is mixed with oil phase.
In above-mentioned steps, the combustion product solvent for use of acquisition is absolute ethyl alcohol.
Compared with prior art, the present invention its remarkable advantage is：Nitrate swelling and watering is prepared into cavernous nitrate,
While reducing nano material preparation energy consumption, increase nitrate specific surface, enhancing nitrate improves the adsorption capacity of oil phase
The activity of nitrate and oil phase improves nitrate combustion characteristic, helps to improve nano-metal-oxide stability and grain size can
Control property, while simplifying preparation section and improving efficiency, more conducively industrialized production.
Description of the drawings
Fig. 1 is the XRD diagram of nano ceric oxide of the present invention.
Fig. 2 is the transmission electron microscope picture of nano ceric oxide of the present invention.
Fig. 3 is the XRD diagram of nano-cobaltic-cobaltous oxide of the present invention.
Fig. 4 is the transmission electron microscope picture of nano-cobaltic-cobaltous oxide of the present invention.
Fig. 5 is the XRD diagram of nano cupric oxide of the present invention.
Fig. 6 is the transmission electron microscope picture of nano cupric oxide of the present invention.
Fig. 7 is the XRD diagram of nano zine oxide of the present invention.
Fig. 8 is the transmission electron microscope picture of nano zine oxide of the present invention.
Fig. 9 is the XRD diagram of nano-sized iron oxide of the present invention.
Figure 10 is the transmission electron microscope picture of nano-sized iron oxide of the present invention.
Specific implementation mode
Technical scheme of the present invention is further described with reference to embodiment, but should not be as the limitation present invention
Protection domain.
Embodiment 1
Nano-cerium oxide is prepared according to the method for the present invention, this experiment is divided into three steps, and the first step is to prepare nitrate mixture,
Constituent mass score is ammonium nitrate：Cerous nitrate：Water：Octadecylamine acetate salt=60:30:9.85:0.15, by ammonium nitrate and nitric acid
Cerium is dissolved in water, and separately plus after emulsifier octadecylamine acetate salt 110-120 DEG C of uniform dissolution of heating is poured into vacuum tank ,-
It is vacuumized under the pressure of 0.085MPa, obtains uniform puffing porosity nitrate mixture；Second step prepares nitrate and oil
Nitrate mixture and diesel oil according to mass ratio are 94 by phase mixture：6 ratio uniform mixing；Third walks, and mixture is forged
It burns, which is placed in Muffle furnace and is calcined, calcination temperature is set as 600 DEG C, calcination time 1h.By calcined product from horse
It is not taken out in stove, up to nano-cerium oxide finished product after washed and purification.With D8ADVANCE types X-ray diffractometer to sample into
Row detection.The XRD diffracting spectrums of sample are as shown in Figure 1.(111) of the appearance of 10~80 ° of 2 angles θ, (200), (220), (311),
(222), the diffraction crystal face such as (400) is all the feature diffraction crystal face of cubic system cerium oxide, it was demonstrated that success sintetics cerium oxide.
With transmission electron microscope observing sample topography, appearance is spherical shape；By testing proof above, product is purer ball shaped nano oxygen
Change cerium, the purity of product is 99.9% or more.The transmission electron microscope of sample is as shown in Figure 2.
Embodiment 2
Nano-cobaltic-cobaltous oxide is prepared according to the method for the present invention, this experiment is divided into three steps, and the first step is to prepare nitrate to mix
Object is closed, constituent mass score is ammonium nitrate：Cobalt nitrate：Water：Octadecylamine acetate salt=60:35:4.8:0.2, by ammonium nitrate and nitre
Sour cobalt is dissolved in water, and separately plus after emulsifier octadecylamine acetate salt 110-120 DEG C of uniform dissolution of heating is poured into vacuum tank ,-
It is vacuumized under the pressure of 0.08MPa, obtains uniform puffing porosity nitrate mixture；Second step prepares nitrate and oil phase
Mixture, by nitrate mixture and diesel oil according to mass ratio 94：6 ratio uniform mixing；Third walks, mixture calcining, will
The mixture, which is placed in Muffle furnace, to be calcined, and calcination temperature is set as 700 DEG C, calcination time 1.5h.By calcined product from Muffle
It is taken out in stove, up to nano-cobaltic-cobaltous oxide finished product after washed and purification.With D8ADVANCE type X-ray diffractometers to sample
It is detected.The XRD diffracting spectrums of sample as shown in figure 3, (111) of 2 angles θ, 10~80 ° of appearance, (220), (311),
(400), the diffraction crystal face such as (442) is all the feature diffraction crystal face of cobaltosic oxide, it was demonstrated that the product of generation is cobaltosic oxide.
With transmission electron microscope observing sample topography, appearance is spherical shape；By testing proof above, product is purer ball shaped nano four
Co 3 O.Diffracting spectrum and transmission electron microscope such as Fig. 3 of sample, shown in 4.
Embodiment 3
Nano cupric oxide is prepared according to the method for the present invention, this experiment is divided into three steps, and the first step is to prepare nitrate mixture,
Constituent mass score is ammonium nitrate：Copper nitrate：Water：Octadecylamine=30.85:60:9:0.15, by ammonium nitrate and nitric acid copper dissolution
In water, it separately plus after emulsifier octadecylamine 110-120 DEG C of uniform dissolution of heating pours into vacuum tank, under the pressure of -0.09MPa
It vacuumizes, obtains uniform puffing porosity nitrate mixture；Second step prepares nitrate and oil mixture, by nitrate
Mixture is 93 according to mass ratio with oil phase：7 ratio uniform mixing；Third walks, and mixture calcining, wherein oil phase are mass ratio
1：1 Naina this 801 and mineral wax mixture, which is placed in Muffle furnace and is calcined, calcination temperature is set as 1000 DEG C, forges
The burning time is 1.5h.Calcined product is taken out from Muffle furnace, up to nano cupric oxide finished product after washed and purification.With
D8ADVANCE type X-ray diffractometers are detected sample.The XRD diffracting spectrums of sample are as shown in figure 5,10~80 ° of 2 angles θ
(111) that occur, (002), (111), (20-2), (020), the diffraction crystal face such as (202) are all the feature diffraction crystal face of copper oxide,
Prove that the product generated is copper oxide.With transmission electron microscope observing sample topography, appearance is spherical shape；By testing proof above,
Product is purer ball shaped nano copper oxide particle.Diffracting spectrum and transmission electron microscope such as Fig. 5 of sample, shown in 6.
Embodiment 4
Nano zine oxide is prepared according to the method for the present invention, this experiment is divided into three steps, and the first step is to prepare nitrate mixture,
Constituent mass score is ammonium nitrate：Zinc nitrate：Water：Octadecylamine acetate salt=60:30:9.85:0.15, by ammonium nitrate and nitric acid
Zinc is dissolved in water, and separately plus after emulsifier octadecylamine acetate salt 110-120 DEG C of uniform dissolution of heating is poured into vacuum tank ,-
It is vacuumized under the pressure of 0.09MPa, obtains uniform puffing porosity nitrate mixture；Second step prepares nitrate and oil phase
Mixture, by nitrate mixture and Naina, this 810 according to mass ratio is 94.5：5.5 ratio uniform mixing；Third walks, and mixes
Object calcining is closed, which is placed in Muffle furnace and is calcined, calcination temperature is set as 800 DEG C, calcination time 3h.Calcining is produced
Object takes out from Muffle furnace, up to nano zine oxide finished product after washed and purification.With D8ADVANCE type X-ray diffractometers pair
Sample is detected.The XRD diffracting spectrums of sample as shown in fig. 7, (100) of 2 angles θ, 10~80 ° of appearance, (002), (101),
(102), the diffraction crystal face such as (110), (103) is all the feature diffraction crystal face of zinc oxide, it was demonstrated that the product of generation is zinc oxide.With
Transmission electron microscope observing sample topography；By testing proof above, product is purer ball shaped nano zinc oxide.The diffraction of sample
Collection of illustrative plates and transmission electron microscope such as Fig. 7, shown in 8.
Embodiment 5
Nano-sized iron oxide is prepared according to the method for the present invention, this experiment is divided into three steps, and the first step is to prepare nitrate mixture,
Constituent mass score is ammonium nitrate：Ferric nitrate：Water：Octadecylamine acetate salt=67.5:22.5:9.85:0.15, by ammonium nitrate and
Ferric nitrate is dissolved in water, and separately plus after emulsifier octadecylamine acetate salt 110-120 DEG C of uniform dissolution of heating is poured into vacuum tank,
It is vacuumized under the pressure of -0.09MPa, obtains uniform puffing porosity nitrate mixture；Second step prepare nitrate and
Oil mixture, by nitrate mixture and Naina, this 801 according to mass ratio is 94：6 ratio uniform mixing；Third walks, and mixes
Object calcining is closed, which is placed in Muffle furnace and is calcined, calcination temperature is set as 600 DEG C, calcination time 2h.Calcining is produced
Object takes out from Muffle furnace, up to nano-sized iron oxide finished product after washed and purification.With D8ADVANCE type X-ray diffractometers pair
Sample is detected.The XRD diffracting spectrums of sample as shown in fig. 7, (012) of 2 angles θ, 10~80 ° of appearance, (104), (110),
(113), the diffraction crystal face such as (024), (116) is all the feature diffraction crystal face of iron oxide, it was demonstrated that the product of generation is iron oxide.With
Transmission electron microscope observing sample topography, appearance are spherical shape；By testing proof above, product is that purer ball shaped nano aoxidizes
Iron.Diffracting spectrum and transmission electron microscope such as Fig. 9 of sample, shown in 10.
Embodiment 6
Nano ferrous acid copper is prepared according to the method for the present invention, this experiment is divided into three steps, and the first step is to prepare nitrate mixture,
Quality proportioning is ammonium nitrate：(ferric nitrate+copper nitrate)：Water：Octadecylamine acetate salt=50：(30.81+9.19)：9.85：0.15.
Ammonium nitrate, copper nitrate and ferric nitrate are dissolved in water, separately plus emulsifier octadecylamine acetate salt heats 110-120 DEG C of uniform dissolution
After pour into vacuum tank, vacuumized under the pressure of -0.09MPa, obtain uniform puffing porosity nitrate mixture；Second
Step prepares nitrate and oil mixture, and by nitrate mixture and Naina, this 801 according to mass ratio is 94：6 ratio uniform
Mixing；Third walks, which is placed in Muffle furnace and calcines by mixture calcining, and calcination temperature is set as 600 DEG C, when calcining
Between be 2h.Calcined product is taken out from Muffle furnace, up to ball shaped nano coppe ferrite finished product after washed and purification.
Claims (3)
1. a kind of preparation method of nano-metal-oxide, which is characterized in that include the following steps：First by ammonium nitrate and metal
Nitrate is soluble in water, and emulsifier is added, porosity nitrate mixture is obtained through puffing after；Secondly by porosity nitrate
Mixture is calcined 1-3 hours after mixing at 600-1000 DEG C with oil phase and obtains nano-metal-oxide；The puffing mistake
Journey is that emulsifier is added in nitrate aqueous solution, after heating for dissolving, vacuumizes to obtain under the conditions of -0.08~-0.09MPa more
Permeability nitrate mixture；The solution temperature is 110-120 DEG C；In the porosity nitrate mixture, the matter of nitrate
It is 90%~95% to measure score, and the mass fraction of emulsifier is 0.15%-0.2%, remaining is water；The metal nitrate is nitre
In sour cerium, zinc nitrate, cobalt nitrate, copper nitrate and ferric nitrate any one or it is several；The emulsifier be octadecylamine or
Person's octadecylamine acetate salt.
2. the preparation method of nano-metal-oxide according to claim 1, it is characterised in that：The oil phase is bavin
One or more of this 801, Naina of oil, lubricating oil, bio-oil, Naina this 810, paraffin, microwax, complex wax.
3. the preparation method of nano-metal-oxide according to claim 1, it is characterised in that：The porosity nitrate
Oxygen balance is positive oxygen balance after mixture is mixed with oil phase.
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| EP0304369A3 (en) * | 1987-08-19 | 1990-08-16 | Rhone-Poulenc Chimie | Process for the preparation of colloidal dispersions of ceric dioxide in an alcoholic medium |
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| CN103011279A (en) * | 2012-11-20 | 2013-04-03 | 南京理工大学 | Method for synthesizing spherical nano-zirconia by using detonation method in grain diameter controllable manner |
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