CN106588964B - A kind of rare earth compounding nano material and its preparation method and application - Google Patents
A kind of rare earth compounding nano material and its preparation method and application Download PDFInfo
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- CN106588964B CN106588964B CN201611094713.4A CN201611094713A CN106588964B CN 106588964 B CN106588964 B CN 106588964B CN 201611094713 A CN201611094713 A CN 201611094713A CN 106588964 B CN106588964 B CN 106588964B
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 50
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 48
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 41
- 238000013329 compounding Methods 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- CYIDZMCFTVVTJO-UHFFFAOYSA-N pyromellitic acid Chemical compound OC(=O)C1=CC(C(O)=O)=C(C(O)=O)C=C1C(O)=O CYIDZMCFTVVTJO-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 22
- 150000003839 salts Chemical class 0.000 claims abstract description 15
- 235000019441 ethanol Nutrition 0.000 claims abstract description 14
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 238000001354 calcination Methods 0.000 claims description 6
- 150000000921 Gadolinium Chemical class 0.000 claims description 5
- 239000012046 mixed solvent Substances 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 230000000536 complexating effect Effects 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 18
- 239000002243 precursor Substances 0.000 abstract description 6
- 150000001875 compounds Chemical class 0.000 abstract description 4
- 238000003837 high-temperature calcination Methods 0.000 abstract description 2
- 239000011259 mixed solution Substances 0.000 abstract 1
- 239000012429 reaction media Substances 0.000 abstract 1
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 9
- 229910017053 inorganic salt Inorganic materials 0.000 description 7
- 239000002245 particle Substances 0.000 description 7
- -1 polyethylene pyrrolidones Polymers 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 239000002131 composite material Substances 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 4
- 206010013786 Dry skin Diseases 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- GXCUBNRUECGTSC-UHFFFAOYSA-K gadolinium(3+);triacetate;hydrate Chemical compound O.[Gd+3].CC([O-])=O.CC([O-])=O.CC([O-])=O GXCUBNRUECGTSC-UHFFFAOYSA-K 0.000 description 3
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 description 3
- 150000000000 tetracarboxylic acids Chemical class 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052723 transition metal Inorganic materials 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 229910000420 cerium oxide Inorganic materials 0.000 description 2
- 229960004643 cupric oxide Drugs 0.000 description 2
- 229910001938 gadolinium oxide Inorganic materials 0.000 description 2
- 229940075613 gadolinium oxide Drugs 0.000 description 2
- 238000009396 hybridization Methods 0.000 description 2
- 239000002135 nanosheet Substances 0.000 description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- 150000000703 Cerium Chemical class 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 150000000914 Dysprosium Chemical class 0.000 description 1
- 150000000917 Erbium Chemical class 0.000 description 1
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 150000000922 Holmium Chemical class 0.000 description 1
- 150000001169 Lutetium Chemical class 0.000 description 1
- 150000001206 Neodymium Chemical class 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 229910002637 Pr6O11 Inorganic materials 0.000 description 1
- 150000001213 Praseodymium Chemical class 0.000 description 1
- 150000001215 Promethium Chemical class 0.000 description 1
- 150000001216 Samarium Chemical class 0.000 description 1
- 150000001217 Terbium Chemical class 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 150000001225 Ytterbium Chemical class 0.000 description 1
- QFWBEIWGYSUWSI-UHFFFAOYSA-N acetic acid;copper;hydrate Chemical compound O.[Cu].CC(O)=O QFWBEIWGYSUWSI-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- VGBWDOLBWVJTRZ-UHFFFAOYSA-K cerium(3+);triacetate Chemical compound [Ce+3].CC([O-])=O.CC([O-])=O.CC([O-])=O VGBWDOLBWVJTRZ-UHFFFAOYSA-K 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 150000001868 cobalt Chemical class 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
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(III) oxide Inorganic materials O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 description 1
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 1
- RSEIMSPAXMNYFJ-UHFFFAOYSA-N europium(III) oxide Inorganic materials O=[Eu]O[Eu]=O RSEIMSPAXMNYFJ-UHFFFAOYSA-N 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- JYTUFVYWTIKZGR-UHFFFAOYSA-N holmium oxide Inorganic materials [O][Ho]O[Ho][O] JYTUFVYWTIKZGR-UHFFFAOYSA-N 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 150000002603 lanthanum Chemical class 0.000 description 1
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 1
- 229910003443 lutetium oxide Inorganic materials 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 150000002696 manganese Chemical class 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- LPUQAYUQRXPFSQ-DFWYDOINSA-M monosodium L-glutamate Chemical compound [Na+].[O-]C(=O)[C@@H](N)CCC(O)=O LPUQAYUQRXPFSQ-DFWYDOINSA-M 0.000 description 1
- 235000013923 monosodium glutamate Nutrition 0.000 description 1
- 239000004223 monosodium glutamate Substances 0.000 description 1
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 description 1
- 150000002815 nickel Chemical class 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 description 1
- 238000005120 petroleum cracking Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 description 1
- 150000003325 scandium Chemical class 0.000 description 1
- HYXGAEYDKFCVMU-UHFFFAOYSA-N scandium(III) oxide Inorganic materials O=[Sc]O[Sc]=O HYXGAEYDKFCVMU-UHFFFAOYSA-N 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- ZIKATJAYWZUJPY-UHFFFAOYSA-N thulium (III) oxide Inorganic materials [O-2].[O-2].[O-2].[Tm+3].[Tm+3] ZIKATJAYWZUJPY-UHFFFAOYSA-N 0.000 description 1
- FRNOGLGSGLTDKL-UHFFFAOYSA-N thulium atom Chemical class [Tm] FRNOGLGSGLTDKL-UHFFFAOYSA-N 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- FIXNOXLJNSSSLJ-UHFFFAOYSA-N ytterbium(III) oxide Inorganic materials O=[Yb]O[Yb]=O FIXNOXLJNSSSLJ-UHFFFAOYSA-N 0.000 description 1
- 150000003746 yttrium Chemical class 0.000 description 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
- C07F5/003—Compounds containing elements of Groups 3 or 13 of the Periodic Table without C-Metal linkages
-
- 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
- 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
- C01F17/30—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6
- C01F17/32—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6 oxide or hydroxide being the only anion, e.g. NaCeO2 or MgxCayEuO
-
- 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
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of rare earth compounding nano materials and its preparation method and application, the rare earth compounding nano material the preparation method is as follows: using ethyl alcohol and water mixed solution as reaction medium, Pyromellitic Acid and inorganic salts are raw material, triethylamine is regulator, and a variety of rare earth compounding nano materials have been made.The appearance of nano material is uniform, and size and shape can be adjusted by different demands, is easy to disperse in water, ethyl alcohol, DMF etc., solves the problems, such as that nano material is not easy to disperse.Preparation method simple and the characteristics of be easily dispersed, makes it have the potential quality of industrial application.Using rare earth and doping type rare earth compounding as presoma, by air high-temperature calcination, it is prepared for that there is the nanometer rare earth oxide material similar with presoma.The method can control the morphology and size of rare earth oxide by complex precursors, realize the uniform compound of oxide, and preparation process is simple, be not necessarily to expensive device, and raw material is cheap and easy to get.
Description
Technical field
The preparation for the organic inorganic hybridization rare earth compounding nano material with good dispersion that the present invention relates to a kind of with
And rare earth, the preparation of composite rare-earth oxide nano material, belong to nano material synthesis field.
Background technique
Rare earth usually enjoys the laudatory title of " industrial monosodium glutamate ", and new material and high-technology field have pole to rare earth in recent years
Big demand.There are more strict requirements in different applications to the particle size distribution of rare earth powder, and this requires me
Be dedicated to the synthesis technology of exploratory development rare earth material.
The special excellent properties that there are nano material many traditional materials not have, such as small-size effect, surface effect
It answers, macro quanta tunnel effect etc., thus the study on the synthesis of nano material is concerned.Preparation method has very much, and total comes
It says and is divided into two major classes, is i.e. physical method and chemical method, wherein physical method includes comminuting method, vacuum deposition method, sputtering method, gas
Evacuator body method etc., chemical method include gas-phase decomposition method, the precipitation method, spray-on process, sol-gal process, hydro-thermal method etc..
2010, related application (102531022 A of Chinese patent CN), which is reported, prepared list by precipitating reagent of urea
Disperse nanometer rare earth oxide ball, needs to be added exhibiting high surface activated polyethylene pyrrolidones in synthesis process.2012, have
Patent (102730738 A of Chinese patent CN), which is reported, to be smelted into alloy as raw material using rare earth metal and prepares binary or polynary dilute
The method of native oxide nano particles.This method complex process needs higher reaction temperature, and energy consumption is high, and equipment cost is high.
2010, there is patent application (101857192 A of Chinese patent CN) to report sol-gel method and prepare titanium/rare earth hybrid nanometer
Material.This method is needed using a large amount of organic gel agent, and entire sol-gel process needs the long period, and technique is multiple
It is miscellaneous.
The present invention is prepared for the uniform rare earth compounding nano material of appearance and size by easy complexed-precipitation method.Nanometer
One of key problem in technology of the material application i.e. dispersion of material.Due to high specific surface area and high surface energy, nano material is held very much
It is easy to reunite, to lose its due property.Thus have to that nano particle is allowed to be uniformly dispersed in practical applications
In system, the phenomenon that overcoming nanoparticle agglomerates.Direct precipitation method is to prepare nano material method the easiest, but this method
Nano material obtained cannot obtain evenly dispersed material due to agglomeration.
Summary of the invention
The present invention provides a kind of simple preparation method of organic inorganic hybridization rare earth compounding nano material, the preparation sides
Method simple process, it is high-efficient;Obtained product has good dispersion performance in water, ethyl alcohol, DMF equal solvent.
The present invention also provides a kind of using rare earth compounding as the method for precursor preparation nanometer rare earth oxide material, obtains
The uniform doping of the oxide arrived, granularity are uniform.
A kind of preparation method of rare earth compounding nano material, comprising the following steps:
In the in the mixed solvent of second alcohol and water, using triethylamine as regulator, using Pyromellitic Acid and inorganic salts as raw material into
Row complex reaction, after reaction by being centrifuged and being dried to obtain the rare earth compounding nano material.
Rare earth compounding appearance of nano material made from complexed-precipitation method through the invention is uniform, and (nanometer is to micro- for size
Rice) and pattern (particle, rodlike, sheet material) be adjusted on demand.Also, granular material obtained is easy in water, ethyl alcohol, DMF
Disperse in equal solvent.The preparation method of the rare earth compounding nano material has many advantages, such as that such as product particle degree obtained is uniform,
Preparation process is simple, high-efficient, is not necessarily to high temperature and pressure, the equipment for not needing valuableness, and required raw material is cheap and easy to get etc..
Preferably, the inorganic salts are the one or more or inorganic salt of rare earth of inorganic salt of rare earth and transition gold
Belong to the combination of inorganic salts.
Preferably, the inorganic salt of rare earth is scandium salts, yttrium salt, lanthanum salt, cerium salt, praseodymium salt, neodymium salt, promethium salt, samarium salt, europium
One or more of salt, gadolinium salt, terbium salt, dysprosium salt, holmium salt, erbium salt, thulium salt, ytterbium salt, lutetium salt.
Other than the inorganic salt of rare earth of one-component, the rare earth that inorganic salt raw material is also possible to hybrid transition metal salt is inorganic
Salt or two kinds and two or more inorganic salt of rare earth mixtures.Preferably, the transition metal inorganic salts are titanium
One or more of salt, vanadic salts, chromic salts, manganese salt, molysite, cobalt salt, nickel salt, mantoquita.
Preferably, the volume ratio of the second alcohol and water is 1:0.9~1.1;
The mole dosage ratio of the Pyromellitic Acid and inorganic salts is 1:0.9~1.1.
Preferably, the temperature of the complex reaction is 70~90 DEG C.
The present invention also provides the rare earth compounding nano materials that the preparation method described in one kind obtains.
Meanwhile using rare earth compounding of the invention as presoma, by the simple process of air high-temperature calcination, can prepare
Rare earth compounding presoma has the rare earth oxide and composite rare-earth oxide nano material of similar pattern.
The present invention also provides a kind of preparation method of rare earth oxide, the rare earth compounding nano material is in air
In calcined, obtain affiliated rare earth oxide.
The advantages of the method is the morphology and size that rare earth oxide can be adjusted by rare earth compounding presoma, can
To realize the Uniform Doped of oxide, product particle degree obtained is uniform, and simple process is efficient, is not necessarily to expensive device.
Preferably, the temperature of calcining is 600~700 DEG C, calcination time is 1~5h.
The present invention also provides a kind of rare earth oxides, are obtained by the preparation method;
The rare earth oxide is single rare earth oxide or composite rare-earth oxide.Obtained single rare earth oxidation
Object includes Sc2O3, Y2O3, La2O3, CeO2, Pr6O11, Nd2O3, Pm2O3, Sm2O3, Eu2O3, Gd2O3, Tb4O7, Dy2O3, Ho2O3,
Er2O3, Tm2O3, Yb2O3, Lu2O3;Composite rare-earth oxide includes that titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper are transient metal doped
Rare earth oxide, and two kinds and the compound oxide-based nanomaterial of two or more rare earths.
Compared with existing nano material synthetic technology, synthetic method of this invention has that process flow is simple, condition
Mildly, at low cost, the advantages that pattern of nano material is uniform, and size can regulate and control on demand.The invention achievement is for rare earth in industry
Exhaust gas and vehicle maintenance service, petroleum cracking, battery electrode material, luminescent material, electromagnetic shielding, ultraviolet radiation preventing, rare earth
The application of the industries such as filling-modified polymer is significantly.
Detailed description of the invention
Fig. 1 is the cupric oxide doped cerium oxide nano sheet material that embodiment 6 obtains.
Specific embodiment
Embodiment 1
A method of organic-inorganic hybrid nano material is synthesized with Pyromellitic Acid and gadolinium salt.Weigh the equal benzene of 0.1272g
Tetracarboxylic acid and 0.1762g gadolinium acetate hydrate dissolve in 10mL second alcohol and water respectively, and 80 DEG C of reaction 1h after mixing finally will be anti-
Object centrifuge dripping is answered, 50 DEG C of convection ovens dryings is placed in, obtains about 5 microns of length of rod-like nano material, yield 72%.
Embodiment 2
A method of organic-inorganic hybrid nano material is synthesized with Pyromellitic Acid and gadolinium salt.Weigh the equal benzene of 0.1272g
Tetracarboxylic acid and 0.1762g gadolinium acetate hydrate dissolve in 10mL second alcohol and water respectively, and the three of 40 microlitres are added in ethanol solution
Ethamine, 80 DEG C of reaction 1h after mixing are placed in 50 DEG C of convection ovens dryings, obtain partial size 300 finally by reactant centrifuge dripping
~400 nanometers of rare earth Gd coordination compound particle, yield 74%.
Embodiment 3
A method of organic-inorganic hybrid nano material is synthesized with Pyromellitic Acid and gadolinium salt.Weigh the equal benzene of 0.1272g
Tetracarboxylic acid and 0.1762g gadolinium acetate hydrate dissolve in 10mL second alcohol and water respectively, and 100 microlitres are added in ethanol solution
Triethylamine, 80 DEG C of reaction 1h after mixing are placed in 50 DEG C of convection ovens dryings, obtain partial size and exist finally by reactant centrifuge dripping
200~300 nanometers of rare earth Gd coordination compound particle, yield 75%.Nano particle easily disperses in water, ethyl alcohol, DMF, about
4mg/mL suspension, which is placed three days, does not occur obvious sediment.
Embodiment 4
For one kind with Pyromellitic Acid, the rare earth cerium salt for mixing transition metal mantoquita is Material synthesis organic-inorganic hybrid nanometer
The method of material.Weigh three kinds of 0.3180g Pyromellitic Acid, 0.3770g cerous acetate hydrate and 0.0250g acetic acid copper hydrate
Inorganic salts, Pyromellitic Acid and inorganic salts are dissolved in respectively in 25mL second alcohol and water, 80 DEG C of reaction 1h after mixing, then will reaction
Object centrifuge dripping is placed in 50 DEG C of convection ovens dryings, obtains thickness in the Nano sheet material of 100 rans, yield is 71%.
Embodiment 5
A method of using rare earth compounding as precursor preparation pure rare earth oxide-based nanomaterial.What embodiment 3 obtained
Gadolinium rare earth compounding in air 650 DEG C of calcining 2h up to gadolinium oxide nano material, yield: 87%.Nanometer rare earth oxide material
Material has similar pattern with rare earth compounding presoma, is gadolinium oxide particle of the partial size at 200~300 nanometers.
Embodiment 6
A method of using rare earth compounding as precursor preparation composite rare-earth oxide nano material.Embodiment 4 obtains
Complex precursors in air 650 DEG C of calcining 2h up to cupric oxide doped cerium oxide nano materials, yield: 89%.It is multiple
Closing nanometer rare earth oxide material has similar pattern with its complex precursors, and specific structure is shown in Fig. 1.
Claims (5)
1. a kind of preparation method of rare earth compounding nano material, which comprises the following steps:
In the in the mixed solvent of second alcohol and water, using triethylamine as regulator, network is carried out using Pyromellitic Acid and inorganic salts as raw material
Reaction is closed, after reaction by being centrifuged and being dried to obtain the rare earth compounding nano material;
The inorganic salts are gadolinium salt.
2. the preparation method of rare earth compounding nano material according to claim 1, which is characterized in that the ethyl alcohol and
The volume ratio of water is 1:0.9~1.1;
The mole dosage ratio of the Pyromellitic Acid and inorganic salts is 1:0.9~1.1.
3. the preparation method of rare earth compounding nano material according to claim 1, which is characterized in that the complexing is anti-
The temperature answered is 70~90 DEG C.
4. a kind of preparation method of rare earth oxide characterized by comprising
(1) rare earth compounding nano material is obtained according to the described in any item methods of claims 1 to 3;
(2) the rare earth compounding nano material that step (1) obtains is calcined in air, obtains the rare-earth oxidation
Object.
5. the preparation method of rare earth oxide according to claim 4, which is characterized in that the temperature of calcining is 600~700
DEG C, calcination time is 1~5h.
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