CN104003432A - Method for preparing low apparent density rare earth oxide - Google Patents
Method for preparing low apparent density rare earth oxide Download PDFInfo
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- CN104003432A CN104003432A CN201410260046.7A CN201410260046A CN104003432A CN 104003432 A CN104003432 A CN 104003432A CN 201410260046 A CN201410260046 A CN 201410260046A CN 104003432 A CN104003432 A CN 104003432A
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- rare earth
- earth oxide
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Abstract
The invention belongs to the technical field of preparation of rear earth oxide powder materials with the special physical performance, and particularly relates to a method for preparing a low apparent density rare earth oxide. According to the method, a chlorination solution obtained by rear earth extraction separation is used as raw materials, microwave external field is adopted for assistance, and the defects that an existing method for preparing the low apparent density rare earth oxide is high in cost, and the purity of the rare earth oxide is easily polluted are overcome. The method for preparing the low apparent density rare earth oxide comprises the following steps of (1) using the rear earth chlorination solution as the raw materials, (2) conducting microwave assistance and liquid phase crystallization to obtain a precursor sediment, (3) conducting a reaction at the sediment temperature for 1 h to 3 h, (4) conducting hot filtration, washing and drying on the sediment, and (5) conducting thermal decomposition to obtain the low apparent density rare earth oxide. The method for preparing the low apparent density rare earth oxide has the advantages that the cost is low, the purity is high, the technology is simple, operation is convenient, the preparation process and the product quality are easy to control, and no additives are added.
Description
Technical field
The invention belongs to the preparing technical field of specific physical performance RE oxide powder material, being specifically related to a kind of chlorated liquid of take rare earth extraction separation is raw material, and adopts microwave outfield auxiliary, prepares the method for low-apparent-density rare earth oxide.
Background technology
" rare earth element " refers to 17 kinds of element summations such as the lanthanon of periodic table of elements ZhongⅢ B family and scandium, yttrium in general, because promethium is artificial radioelement, therefore be not included in wherein.
RE in this rare earth oxide REO comprises single or more than one the rare earth element of La, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Sc or Y.
In industrial production, often adopt rare-earth oxalate or carbonate thermal degradation to transform into corresponding oxide, its D50 is 3-5 μ m, specific surface area is generally difficult to surpass 10m
2/ g, its loose density is generally all at 1.0～1.5g/cm
3, its pattern is irregular flaky powder.And the rare earth oxide pattern of generally preparing low-apparent-density is cotton-shaped or coralliform, its preparation process need be added the coating materialss such as promoting agent, dispersion agent, template for preventing from reuniting in rare earth oxide presoma precipitation process, not only raise the cost, the more important thing is that presoma is difficult to guarantee to remove above-mentioned coating materials completely in thermal decomposition process, existence may be polluted the possibility of final earth oxide product purity.
Summary of the invention
(1) technical problem that will solve
The present invention is in order to overcome the existing shortcoming that the cost that low-apparent-density rare earth oxide method exists is high, easily pollute earth oxide product purity of preparing, and the technical problem to be solved in the present invention is to provide that a kind of cost is low, purity is high, technique is simple, easy to operate, preparation process and quality product are easy to the method for preparing low-apparent-density rare earth oxide of controlling.
(2) technical scheme
In order to solve the problems of the technologies described above, the invention provides a kind of like this method of preparing low-apparent-density rare earth oxide.
(1) take rare-earth mineral through full extracting and separating and rare-earth chloride solution be raw material, concentration is 0.2 ~ 1.0 mol/L;
(2) chloride soln of rare earth extraction separation being placed in to microwave reactor, is under 60 ~ 85 ° of C conditions in temperature, evenly drips ammonium bicarbonate soln, the bicarbonate of ammonia (NH of interpolation
4hCO
3) concentration be 0.5 ~ 1.5 mol/L, in the process of adding, constantly stir, obtain REO presoma throw out;
(3) under precipitation temperature, reaction 1 ~ 3 h;
(4) throw out is carried out to heat filtering, washing, dry under 80 ~ 120 ° of C;
(5) dried presoma is carried out to thermolysis in 600 ~ 900 ° of C of temperature, obtain product.
Preferably, in described step (2), NH
4hCO
3solution addition is 200 ~ 300% of theoretical amount, i.e. NH
4hCO
3(mol)/RE
3+(mol)=6 ~ 9;
Preferably, in described step (2), the microwave power using is 400 ~ 800 W;
Preferably, in described step (4), the described heat filtering that is filtered into, filters no longer ageing immediately after having reacted.
Principle of work: nothing.
(3) beneficial effect
1. the present invention prepares and in rare earth oxide presoma process, adopts microwave outfield radiation heating, make full use of heating and molecule whipping characteristic in microwave, liquid-phase precipitation process is except necessary precipitation agent, without adding the coating materialss such as any promoting agent, dispersion agent, template, make presoma both avoid agglomeration, avoided again adding coating materials and had the possibility of polluting earth oxide product.
2. rare earth oxide fine size, the pattern that prepared by the present invention are regular, and not only loose density is low, and purity is high owing to having alleviated the impurity of mechanical entrainment.
3. method technique of the present invention is simple, easy to operate, and preparation process and quality product are easy to control.
4. directly to take the rare earth strip liquor of rare earth extraction separation be raw material in the present invention, and without adding coating materials, cost is low.
Accompanying drawing explanation
Fig. 1 is techniqueflow chart of the present invention.
Fig. 2 is that the pattern of the low-apparent-density yttrium oxide prepared of method of the present invention adopts high power electronic scanning Electronic Speculum to analyze the photo of demonstration.
Fig. 3 is that the pattern of the low-apparent-density cerium oxide prepared of method of the present invention adopts high power electronic scanning Electronic Speculum to analyze the photo of demonstration.
Fig. 4 is that the pattern of the low-apparent-density lanthanum trioxide prepared of method of the present invention adopts high power electronic scanning Electronic Speculum to analyze the photo of demonstration.
Embodiment
Below in conjunction with drawings and Examples, the present invention is further illustrated.
embodiment 1
Yttrium chloride solution 40 ml that get 0.2 mol/L pour in 200ml reaction vessel, are then put in microwave radiation device and open magnetic agitation; In question response container, reach after 70 ° of C of design temperature, separately get 1.5 mol/L ammonium bicarbonate soln 30 ml, agitation and dropping precipitates in yttrium chloride solution, and the reaction times is 90 min.After filtering, with pure water and absolute ethanol washing filter cake, throw out is dry under 80 ° of C conditions.Then thermolysis 2 h under 800 ° of C conditions in retort furnace, are cooled to room temperature, obtain yttrium oxide powder, and its loose density is 0.18 g/cm3, and specific surface area is 30.69 m
2/ g.The pattern of prepared low-apparent-density yttrium oxide adopts photo that high power electronic scanning Electronic Speculum analyzes demonstration as shown in Figure 2, and the yttrium oxide obtaining is the needle-like submicron particles that median size is about 0.2 μ m, and pattern is regular.
embodiment 2:
Solution of cerium chloride by oxidation 30 ml that get 0.5 mol/L pour in 200 ml reaction vessels, are then put in microwave radiation device, and open magnetic agitation; In question response container, reach after 60 ° of C of design temperature, bicarbonate of ammonia 60 ml that separately get 0.3 mol/L pour in reaction vessel, and agitation and dropping precipitates in solution of cerium chloride by oxidation, and the reaction times is 60 min.After filtering, with pure water and absolute ethanol washing filter cake, throw out is dry under 80 ° of C conditions.Then thermolysis 3h under 600 ° of C conditions in retort furnace, is cooled to room temperature, obtains ceria oxide powder, and its loose density is 0.31 g/cm3, and specific surface area is 26.73 m
2/ g.The pattern of prepared low-apparent-density cerium oxide adopts photo that high power electronic scanning Electronic Speculum analyzes demonstration as shown in Figure 3, and the cerium oxide obtaining is the needle-like submicron particles that median size is about 0.3 μ m, and pattern is regular.
embodiment 3:
Lanthanum chloride solution 20 ml that get 0.9 mol/L pour in 200 ml reaction vessels, are then put in microwave radiation device, and carry out magnetic agitation; In question response container, reach after 85 ° of C of design temperature, separately get ammonium bicarbonate soln 40 ml of 1.0 mol/L, agitation and dropping precipitates in lanthanum chloride solution, thereby obtains presoma throw out, and the reaction times is 180 min.Then presoma is carried out to suction filtration, and use successively distilled water and absolute ethanol washing, the filter cake obtaining is dry in baking oven.Dried presoma precipitated product is placed in to retort furnace, and calcination 1h under 900 ° of C, is cooled to room temperature, obtains ultra-fine, lanthanum trioxide that median size is about 0.4 μ m (Fig. 4), and its loose density is 0.21 g/cm3, and specific surface area is 16.50 m
2/ g.
In sum, the method applied in the present invention is: the strip liquor of rare earth extraction separation (re chloride) is placed in to reaction vessel, under the booster action of microwave outfield, certain temperature of reaction is set, at the uniform velocity drip ammonium bicarbonate soln, and uniform stirring, the precipitation of salts of rare-earth alkali formula obtained, after filtration, washing, dry, thermolysis, obtain low-apparent-density rare earth oxide.To utilizing the pattern of rare earth oxide prepared by aforesaid method to adopt high power electronic scanning Electronic Speculum to analyze demonstration (as Figure of description 2, Fig. 3, Fig. 4): the oxide compound of gained is needle-like submicron particles, particle diameter is 0.2 ~ 0.5 μ m, its pattern is regular, be different from completely and adopt heating in water bath to using oxalic acid or bicarbonate of ammonia as the resulting rare earth oxide of precipitation agent, without adding any promoting agent, dispersion agent, template etc., therefore both there is low-apparent-density, exempted interpolation promoting agent simultaneously, dispersion agent, the modifiers such as template may pollute the possibility of rare earth oxide.
The above embodiment has only expressed the preferred embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion, improvement and substitute, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (4)
1. a method of preparing low-apparent-density rare earth oxide, is characterized in that:
(1) take rare-earth mineral through full extracting and separating and rare-earth chloride solution be raw material, concentration is 0.2 ~ 1.0 mol/L;
(2) chloride soln of rare earth extraction separation being placed in to microwave reactor, is under 60 ~ 85 ° of C conditions in temperature, evenly drips ammonium bicarbonate soln, the bicarbonate of ammonia (NH of interpolation
4hCO
3) concentration be 0.5 ~ 1.5 mol/L, in the process of adding, constantly stir, obtain REO presoma throw out;
(3) under precipitation temperature, reaction 1 ~ 3 h;
(4) throw out is carried out to heat filtering, washing, dry under 80 ~ 120 ° of C;
(5) dried presoma is carried out to thermolysis in 600 ~ 900 ° of C of temperature, obtain product.
2. a kind of method of preparing low-apparent-density rare earth oxide according to claim 1, is characterized in that: in described step (2), and NH
4hCO
3solution addition is 200 ~ 300% of theoretical amount, i.e. NH
4hCO
3(mol)/RE
3+(mol)=6 ~ 9.
3. a kind of method of preparing low-apparent-density rare earth oxide according to claim 1, is characterized in that: in described step (2), the microwave power using is 400 ~ 800 W.
4. a kind of method of preparing low-apparent-density rare earth oxide according to claim 1, is characterized in that: in described step (4), the described heat filtering that is filtered into, filters no longer ageing immediately after having reacted.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115010163A (en) * | 2022-05-20 | 2022-09-06 | 全南县新资源稀土有限责任公司 | Rare earth oxide with low apparent density and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1749169A (en) * | 2004-09-15 | 2006-03-22 | 北京有色金属研究总院 | Low bulk specific weight and large specific surface rare-earth oxide REO and its preparing method |
| CN101698609A (en) * | 2009-11-04 | 2010-04-28 | 中国科学院上海硅酸盐研究所 | Method for preparing spherical, monodisperse and single-size yttrium oxide nano-powder |
| CN102583492A (en) * | 2012-02-20 | 2012-07-18 | 甘肃稀土新材料股份有限公司 | Production process of neodymium oxide with small bulk density |
| WO2012155931A1 (en) * | 2011-05-17 | 2012-11-22 | King Saud University | Method for preparing metal oxide nanoparticles |
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2014
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1749169A (en) * | 2004-09-15 | 2006-03-22 | 北京有色金属研究总院 | Low bulk specific weight and large specific surface rare-earth oxide REO and its preparing method |
| CN101698609A (en) * | 2009-11-04 | 2010-04-28 | 中国科学院上海硅酸盐研究所 | Method for preparing spherical, monodisperse and single-size yttrium oxide nano-powder |
| WO2012155931A1 (en) * | 2011-05-17 | 2012-11-22 | King Saud University | Method for preparing metal oxide nanoparticles |
| CN102583492A (en) * | 2012-02-20 | 2012-07-18 | 甘肃稀土新材料股份有限公司 | Production process of neodymium oxide with small bulk density |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115010163A (en) * | 2022-05-20 | 2022-09-06 | 全南县新资源稀土有限责任公司 | Rare earth oxide with low apparent density and preparation method thereof |
| CN115010163B (en) * | 2022-05-20 | 2024-04-09 | 全南县新资源稀土有限责任公司 | Rare earth oxide with low apparent density and preparation method thereof |
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