CN1296282C

CN1296282C - Technology for preparing nanometer rare-earth oxide

Info

Publication number: CN1296282C
Application number: CNB2003101003776A
Authority: CN
Inventors: 叶祖光; 马永茂
Original assignee: BAOTOU HUAMEI RE PRODUCTS Co Ltd
Current assignee: BAOTOU HUAMEI RE PRODUCTS Co Ltd
Priority date: 2003-10-14
Filing date: 2003-10-14
Publication date: 2007-01-24
Anticipated expiration: 2023-10-14
Also published as: CN1607180A

Abstract

The present invention relates to a process method for preparing nanometer rare earth oxide, which belongs to the preparation field of rare earth new materials. Rare earth carbonate used as a raw material is dissolved by nitric acid, and is filtered; a slow-release deposition agent and a dispersing agent are added in the filtered solution, a precursor is obtained by micro-emulsion homogeneous deposition, and then the dispersing agent is added in; the mixed solution is washed through micro-emulsion ultrasonic by ultrasonic shock, is filtered, is dried and is calcined; and the nanometer rare earth oxide is obtained. By adopting a micro-emulsion homogeneous deposition method, the process method is beneficial to deposition granule core generation, is not beneficial to granule core growth, and ensures small and uniform product granules under the function of the slow-release deposition agent and the dispersing agent. The obtained precursor is washed through micro-emulsion ultrasonic with the process method, and the dispersing agent is added in once again; when a large granule is changed into a small granule, a micro-emulsion net is formed on the surface of the small granule, the agglomeration phenomenon is eliminated once again, and the granules of the product can be further guaranteed to be small and uniform.

Description

A kind of method for preparing oxide nano rare earth

One, technical field

The present invention relates to a kind of preparation oxide nano rare earth method, belong to the rare earth material preparation field.

Two, background technology

At present the technology of preparation oxide nano rare earth is a lot, but it is more serious to have a product agglomeration, and granularity is inhomogeneous, long flow path, and complicated operation, the equipment requirements height, output is little, shortcomings such as cost height.(CN1230582) discloses a kind of fluorescent nanometer rare earth oxide powder and preparation method thereof as Chinese patent, adopted homogeneous precipitation method, the precipitation from homogeneous solution (PFHS) manufacturing presoma that combines with sonochemical method, its shortcoming is that presoma and nano rareearth oxidate powder body easily produce reunion, particle is inhomogeneous, influences quality product.

Three, summary of the invention

The object of the present invention is to provide a kind of good product quality, be difficult for producing reunion, evengranular a kind of oxide nano rare earth.

The present invention realizes in the following manner:

The present invention is to be raw material with the carbonated rare earth, through nitric acid dissolve, filter, add the slowly-releasing precipitation agent in the solution after filtration, dilution adds dispersion agent in the solution after dilution, wherein: the slowly-releasing precipitation agent is a urea, dispersion agent is Pentyl alcohol or n-hexyl alcohol, and the dispersion agent add-on is 5 of dilution back liquor capacity---10%, and temperature is 50---90 ℃, through the micro emulsion precipitation from homogeneous solution (PFHS), be incubated 1-2 hour, clear liquid is taken out in sedimentation, in precipitation, add dispersion agent again, the dispersion agent add-on is 1 of a precipitation solution volume---2%, and temperature is 50---90 ℃, utilize ultrasonic oscillation, carry out the micro emulsion supersound washing, time is filtration in 0.5-2 hour, and presoma is 50---dry under 90 ℃ of temperature, the time is 1---2 hours,---calcination 1.5 under the temperature of 800 ℃ of degree---3.5 hours, obtain nano-oxide 300.

Carbonated rare earth raw material of the present invention can be a kind of in cerous carbonate, Phosbloc, praseodymium carbonate, the neodymium carbonate.

The present invention under the effect of slowly-releasing precipitation agent and dispersion agent, helps the generation of deposit seeds nuclear owing to adopted the micro emulsion homogeneous precipitation method, and what be unfavorable for examining grows up, and has guaranteed that the particle of product is little and even; Owing to add dispersion agent, when particle generates, form the micro emulsion net at particle surface, reduced intergranular contact, eliminated agglomeration, guaranteed the particulate homogeneity.The present invention is owing to also adopted the micro emulsion supersound washing, utilize ultrasonic concussion, make some reunion macrobead of presoma obtain disperseing, owing to also added dispersion agent in this process, become the short grained while at macrobead, short grained surface has formed the micro emulsion net, has eliminated agglomeration once more, has guaranteed that further the particle of product is little and even.

Four, description of drawings

Accompanying drawing is a process flow sheet of the present invention

Five, embodiment

Embodiment 1: get 44 gram cerous carbonate (CeO ₂45%),, transfers to PH 4 with 1: 1 nitric acid dissolve, filter, in solution, add 330 gram urea, be diluted to 1 liter with deionized water, add 5% (V/V) Pentyl alcohol, mix, transfer to PH 7, kept 2 hours at 82 ± 2 ℃, clear liquid is taken out in sedimentation 4 hours, adds 1% (V/V) Pentyl alcohol in precipitation, connect ultrasonic generator, wash 50 ± 5 ℃ of temperature, 2 hours time, filter, filter cake was dried 2 hours under 80 ℃, calcined 2 hours down at 500 ℃ then, obtain nano-cerium oxide, medium particle diameter D ₅₀30nm..

Embodiment 2: get 88 gram cerous carbonate (CeO ₂45%),, transfers to PH 4 with 1: 1 nitric acid dissolve, filter, add 660 gram urea in the solution, be diluted to 2 liters with deionized water, add 10% (V/V) Pentyl alcohol, mix, transfer to PH 7, kept 1.5 hours at 85 ± 2 ℃, clear liquid is taken out in sedimentation 4 hours, adds 2% (V/V) Pentyl alcohol in precipitation, connect ultrasonic generator, wash 40 ± 5 ℃ of temperature, 1 hour time, filter, filter cake was dried 2 hours under 80 ℃, calcined 2 hours down at 500 ℃ then, obtain nano-cerium oxide, medium particle diameter D ₅₀29nm..

Embodiment 3: get 44 gram Phosbloc (La ₂O ₃43%),, transfers to PH 4 with 1: 1 nitric acid dissolve, filter, in solution, add 330 gram urea, be diluted to 1 liter with deionized water, add 5% (V/V) Pentyl alcohol, mix, transfer to PH 7, kept 2 hours at 82 ± 2 ℃, clear liquid is taken out in sedimentation 4 hours, adds 1% (V/V) Pentyl alcohol in precipitation, connect ultrasonic generator, wash 50 ± 5 ℃ of temperature, 2 hours time, filter, filter cake was dried 2 hours under 80 ℃, calcined 2 hours down at 500 ℃ then, obtain nano lanthanum oxide, medium particle diameter D ₅₀28nm..

Embodiment 4: get 44 gram praseodymium carbonate (Pr ₆O ₁₁45%),, transfers to PH4 with 1: 1 nitric acid dissolve, filter, in solution, add 330 gram urea, be diluted to 1 liter with deionized water, add 5% (V/V) Pentyl alcohol, mix, transfer to PH7, kept 2 hours at 82 ± 2 ℃, clear liquid is taken out in sedimentation 4 hours, adds 1% (V/V) Pentyl alcohol in precipitation, connect ultrasonic generator, wash 50 ± 5 ℃ of temperature, 2 hours time, filter, filter cake was dried 2 hours below 80 ℃, calcined 2 hours down at 500 ℃ then, obtain nano oxidized praseodymium, medium particle diameter D ₅₀27nm.

Embodiment 5: get 44 gram neodymium carbonate (Nd ₂O ₃45%),, transfers to PH4 with 1: 1 nitric acid dissolve, filter, in solution, add 330 gram urea, be diluted to 1 liter with deionized water, add 5% (V/V) Pentyl alcohol, mix, transfer to PH7, kept 2 hours at 82 ± 2 ℃, clear liquid is taken out in sedimentation 4 hours, adds 1% (V/V) Pentyl alcohol in precipitation, connect ultrasonic generator, wash 50 ± 5 ℃ of temperature, 2 hours time, filter, filter cake was dried 2 hours below 80 ℃, calcined 2 hours down at 500 ℃ then, obtain nano oxidized neodymium, medium particle diameter D ₅₀28nm.

Claims

1, a kind of method for preparing oxide nano rare earth is characterized in that: with the carbonated rare earth is raw material, through nitric acid dissolve, filter, add the slowly-releasing precipitation agent in the solution after filtration, dilution adds dispersion agent in the solution after dilution, and wherein: the slowly-releasing precipitation agent is a urea, dispersion agent is Pentyl alcohol or n-hexyl alcohol, the dispersion agent add-on is the 5-10% of dilution back liquor capacity, and temperature is 50-90 ℃, through the micro emulsion precipitation from homogeneous solution (PFHS), be incubated 1-2 hour, clear liquid is taken out in sedimentation, adds dispersion agent again in precipitation, the dispersion agent add-on is the 1-2% of precipitation solution volume, temperature is 50-90 ℃, utilizes ultrasonic oscillation, carries out the micro emulsion supersound washing, time is 0.5-2 hour, filter, presoma is dried under 50-90 ℃ of temperature, and the time is 1-2 hour, under 300-800 ℃ temperature calcination 1.5-3.5 hour, obtain nano-oxide.

2, the method for preparing oxide nano rare earth according to claim 1 is characterized in that: carbonated rare earth is a kind of of cerous carbonate, Phosbloc, praseodymium carbonate, neodymium carbonate.