CN100348496C - Low bulk specific weight and large specific surface rare-earth oxide REO and its preparing method - Google Patents
Low bulk specific weight and large specific surface rare-earth oxide REO and its preparing method Download PDFInfo
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- CN100348496C CN100348496C CNB2004100778300A CN200410077830A CN100348496C CN 100348496 C CN100348496 C CN 100348496C CN B2004100778300 A CNB2004100778300 A CN B2004100778300A CN 200410077830 A CN200410077830 A CN 200410077830A CN 100348496 C CN100348496 C CN 100348496C
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Abstract
The present invention relates to a rare-earth oxide REO with low bulk specific weight and large specific surface area and a preparation method thereof. Large specific surface area rare-earth oxide REO, wherein RE is one or more than one kind of rare-earth elements in La, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Sc and Y. The rare-earth oxide REO is one or more than one kind of rare earth oxygenize complex in the rare earth elements, the specific surface area of the rare-earth oxide REO is 10 to 100 m<2>/g, and the bulk specific gravity is 0.25 to 1.0 g/cm<3>. In the preparation method, rare earth precipitate can be obtained by quantificationally adding ammonia water, mixed solution of ammonia water and ammonium hydrogen carbonate, and sodium hydroxide solution or potassium hydroxide solution into soluble salt solution of rare earth with surfactant; products can be obtained through settling, filtering, washing, drying and calcining. The obtained oxide is a macroaggregate which is composed of fine particles of 50 nm to 100 nm, and the surface shape of the aggregate is similar to honeycombs or the surface of a coral. The present invention is widely used in condensers, ceramics, soft magnets and catalytic materials.
Description
Technical field
The present invention relates to a kind of low bulk proportion, large specific surface rare earth oxide REO and preparation method thereof.
Background technology
" rare earth element " refers to 17 kinds of element summations such as the lanthanon of IIIB family in the periodic table of elements and scandium, yttrium in general, because of promethium is artificial emissivity element, so be not included in wherein.
RE among 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 specific surface area generally is difficult to surpass 10m
2/ g (with the BET determination of nitrogen adsorption, down together), its loose specific weight is generally all at 1.0～1.5g/m
3
Summary of the invention
The purpose of this invention is to provide a kind of specific surface area at 10～200m
2The bigger serface of/g, loose specific weight are 0.25～1.0g/cm
3The rare earth oxide and the manufacture method of low bulk specific gravity.The oxide compound of this specific physical performance can be widely used in electrical condenser, pottery, soft magnetic bodies and catalytic material.
For achieving the above object, the present invention takes following technical scheme:
A kind of large specific surface rare earth oxide REO, wherein, RE is single rare earth element among La, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Sc and the Y or more than one rare earth element, this rare earth oxide REO is the single rare earth oxide compound or above-mentioned more than one the composite oxides of rare earth element of above-mentioned rare earth element, and the specific surface area of this rare earth oxide REO is 10～200m
2/ g, its loose specific weight is 0.25～1.0g/cm
3
In large specific surface rare earth oxide REO of the present invention, described rare earth oxide REO is La
2O
3, Pr
6O
11, Nd
2O
3, Sm
2O
3, Eu
2O
3, Gd
2O
3, Tb
4O
7, Dy
2O
3, Ho
2O
3, Er
2O
3, Tm
2O
3, Yb
2O
3, Lu
2O
3, Y
2O
3And Sc
2O
3In one or more mixture.
A kind of method for preparing large specific surface rare earth oxide REO of the present invention, this method comprises the steps:
(1) nitrate or the chloride soln with rare earth is raw material, and concentration is 0.1～2.5mol/L;
(2) add tensio-active agents such as polyoxyethylene glycol, polyoxyethylene, poly-third ethene or ammonium stearate in the nitrate of rare earth or chloride soln, its addition is strength of solution 1～2000ppm;
(3) in the solution that obtains in step (2), be under 15～80 ℃ of conditions in temperature, add mixing solutions, sodium hydroxide solution or the potassium hydroxide solution of ammoniacal liquor, ammoniacal liquor and bicarbonate of ammonia, its concentration is pressed positively charged ion M
+(M
+Be NH
4 +, K
+, Na
+) be calculated as 0.2～3.0mol/L, in the interpolation process, constantly stir, obtain the rare-earth precipitation thing;
(4) precipitation temperature ageing 1～8 hour;
(5) throw out sedimentation, filtration, washing, in 50～220 ℃ of dryings;
(6) with dry thing in 500～1000 ℃ of calcinings, obtain product.
In the method for the invention, the nitrate of the rare earth in the described step (1) or the concentration of chloride soln are preferably 0.3～1.2mol/L.
In the method for the invention, the interpolation ammoniacal liquor in the described step (3) and the mixing solutions of bicarbonate of ammonia, wherein the molar ratio of bicarbonate of ammonia and ammoniacal liquor is 1: 20～1: 2;
In the method for the invention, the addition of the mixing solutions of ammoniacal liquor, ammoniacal liquor and bicarbonate of ammonia, sodium hydroxide solution, potassium hydroxide solution is 100%～300% of theoretical consumption, i.e. M in the described step (3)
-(mol)/RE
3-(mol)=3～9.
In the method for the invention, the preferred addition of mixing solutions, sodium hydroxide solution or the potassium hydroxide solution of ammoniacal liquor, ammoniacal liquor and bicarbonate of ammonia is 110～150% of theoretical consumption, i.e. M in the described step (3)
+(mol)/RE
3+(mol)=3.3～4.5.
In the method for the invention, the mixing solutions of ammoniacal liquor, ammoniacal liquor and the bicarbonate of ammonia of the interpolation in the described step (3), the preferred concentration of sodium hydroxide solution or potassium hydroxide solution is with [M
+] be calculated as 0.5～1.5mol/L.
In the method for the invention, in the described step (3), the preferred temperature of described precipitin reaction is 20～50 ℃.
In the method for the invention, in the described step (4), after described precipitation was finished, the preferred time of ageing was 1～5 hour under precipitation reaction temperature.
In the method for the invention, in the described step (5), the preferred temperature of described exsiccant is 120 ℃～200 ℃.
In the method for the invention, in the described step (6), the preferred temperature of described incinerating is 600～900 ℃.
The present invention has following advantage:
1. rare earth oxide yield height loses little.
2. the rare-earth precipitation thing of the present invention's preparation is easy to sedimentation and filtration.
3. the large specific surface that method of the present invention is produced, that low bulk proportion oxide compound has production lot is big, the simple characteristics of technology.
4. the specific surface area of rare earth oxide of the present invention is 10～200m
2/ g, its loose specific weight is 0.25～1.0g/cm
3Can be widely used in electrical condenser, pottery, soft magnetic bodies and catalytic material.
To help to understand the present invention by following embodiment, but not limit content of the present invention.
Description of drawings
Fig. 1 adopts high power electronic scanning Electronic Speculum to analyze the photo of demonstration for the low bulk proportion of method preparation of the present invention, the pattern of bigger serface yttrium oxide
Fig. 2 adopts high power electronic scanning Electronic Speculum to analyze the photo of demonstration for the low bulk proportion of method preparation of the present invention, the pattern of bigger serface lanthanum trioxide
Fig. 3 adopts high power electronic scanning Electronic Speculum to analyze the photo of demonstration for the low bulk proportion of method preparation of the present invention, the pattern of bigger serface Samarium trioxide
Embodiment
Embodiment 1:
Get 0.5M yttrium nitrate solution 200ml and put into the 1000ml beaker, add 2ml, the polyoxyethylene glycol of 1wt% stirs; Other gets 200ml ammoniacal liquor 1.0mol/L, stirs to join in the yttrium nitrate solution to precipitate.Through the ageing of a few hours, filter back pure water washing leaching cake, throw out was calcined 2 hours for 800 ℃ in retort furnace 140 ℃ of dryings, was cooled to room temperature, obtained yttrium oxide powder, and its specific surface area is 60m
2/ g, loose specific weight is 0.45g/cm
3Prepared low bulk proportion, the pattern of bigger serface yttrium oxide adopt photo that high power electronic scanning Electronic Speculum analyzes demonstration as shown in Figure 1, the yttrium oxide of gained is the macro aggregate that 50～100nm fine particle is formed, the coacervate surface shape is similar to honeycomb or coral surface, therefore has higher specific surface area.
Embodiment 2:
The lanthanum chloride solution 200ml that gets 0.45mol/L puts into the 500ml beaker, adds 1ml, and the polyoxyethylene glycol of 5wt% stirs; Other gets the mixed solution 2.0mol/L of 150ml bicarbonate of ammonia and ammoniacal liquor (mixing molar ratio is 1: 20), stirring joins in the lanthanum chloride solution and precipitates, ageing, after the filtration, use the pure water washing leaching cake, throw out is 140 ℃ of dryings, in retort furnace, calcined 2 hours for 800 ℃, be cooled to room temperature, obtain lanthanum oxide powder, its specific surface area is 28m
2/ g, loose specific weight is 0.49g/cm
3Prepared low bulk proportion, the pattern of bigger serface lanthanum trioxide adopt photo that high power electronic scanning Electronic Speculum analyzes demonstration as shown in Figure 2, the lanthanum trioxide of gained is the macro aggregate that 50～100nm fine particle is formed, the coacervate surface shape is similar to honeycomb or coral surface, therefore has higher specific surface area.
Embodiment 3:
Get 0.25mol/L samarium trichloride solution 200ml and put into the 1000ml beaker, add 2.0ml, the polyoxyethylene of 0.1wt% stirs; Other gets the mixed solution 1.0mol/L (mixing molar ratio is 1: 10) of 300ml bicarbonate of ammonia and ammoniacal liquor, stirring joins in the samarium trichloride solution and precipitates, ageing, after the filtration, use the pure water washing leaching cake, throw out is 140 ℃ of dryings, in retort furnace, calcined 2 hours for 800 ℃, be cooled to room temperature, obtain yttrium oxide powder, its specific surface area is 36m
2/ g, loose specific weight is 0.50g/cm
3Prepared low bulk proportion, the pattern of bigger serface Samarium trioxide adopt photo that high power electronic scanning Electronic Speculum analyzes demonstration as shown in Figure 3, the Samarium trioxide of gained is the macro aggregate that 50～100nm fine particle is formed, the coacervate surface shape is similar to honeycomb or coral surface, therefore has higher specific surface area.
Embodiment 4:
Get 0.5mol/L Holmium trichloride solution 200ml and put into the 500ml beaker, add 5ml, the ammonium stearate of 4wt% stirs; Other gets 2mol/L ammoniacal liquor 200ml, stirs to join in the Holmium trichloride solution to precipitate, and ageing is after the filtration, use the pure water washing leaching cake, throw out was calcined 2 hours for 800 ℃ in retort furnace 120～140 ℃ of dryings, be cooled to room temperature, obtain the Holmium trioxide powder, specific surface area is 75m
2/ g, loose specific weight is 0.35g/cm
3
Embodiment 5:
The preparation of large specific surface area earth-rare oxides (samarium, gadolinium, europium), by weight samarium: gadolinium: europium=0.4: 0.4: 0.2 is made into 0.35mol/L rare earth nitrate solution 200ml and puts into the 1000ml beaker, adds 5ml simultaneously, and the polyacrylic acid of 1wt% stirs; Other gets 1.0mol/L sodium hydroxide solution 500ml; Stirring joins in the rare earth nitrate solution and precipitates; Ageing 1 hour, filtration, washing, vacuum filtration, 140 ℃ of dryings were calcined 2 hours for 800 ℃ in retort furnace, were cooled to room temperature, obtained above-mentioned RE oxide powder, and its specific surface area is 36m
2/ g, loose specific weight is 0.25g/cm
3
In sum, the method that order of the present invention adopted is: to the soluble salt of rare earth, as adding tensio-active agent in nitrate, the chloride soln quantitatively, after evenly stirring, under certain temperature of reaction, to add mixing solutions, sodium hydroxide solution or the potassium hydroxide solution of ammoniacal liquor, ammoniacal liquor and bicarbonate of ammonia, obtain rare-earth hydroxide or the precipitation of salts of rare-earth alkali formula again, through ageing, filtration, washing, drying, calcining obtains low bulk proportion, large specific surface area earth-rare oxides.Pattern to the rare earth oxide that utilizes method for preparing adopts high power electronic scanning Electronic Speculum to analyze demonstrations (as Figure of description 1, Fig. 2, Fig. 3): the oxide compound of gained is the macro aggregate of 50～100nm fine particle composition, the coacervate surface shape is similar to honeycomb or coral surface, be different from fully and adopt oxalic acid precipitation or bicarbonate of ammonia, therefore have higher specific surface area as the good rare earth oxide of the resulting crystalline condition of precipitation agent.
Claims (12)
1, a kind of method for preparing large specific surface rare earth oxide REO, it is characterized in that: this method comprises the steps:
(1) nitrate or the chloride soln with rare earth is raw material, and concentration is 0.1～2.5mol/L;
(2) add polyoxyethylene glycol, polyoxyethylene, poly-third ethene or ammonium stearate tensio-active agent in the nitrate of rare earth or chloride soln, its addition is strength of solution 1～2000ppm;
(3) in the solution that step (2) obtains, be under 15～80 ℃ of conditions in temperature, add mixing solutions, sodium hydroxide solution or the potassium hydroxide solution of ammoniacal liquor, ammoniacal liquor and bicarbonate of ammonia, the concentration of interpolation is with M
+Be calculated as 0.2～3.0mol/L, wherein, M
+Be NH
4 +, K
+Or Na
+, in the interpolation process, constantly stir, obtain the rare-earth precipitation thing;
(4) precipitation temperature ageing 1～8 hour;
(5) throw out sedimentation, filtration, washing, in 50～220 ℃ of dryings;
(6) with dry thing in 500～1000 ℃ of calcinings, obtain product.
2, method according to claim 1 is characterized in that: the nitrate of the rare earth in the described step (1) or the concentration of chloride soln are 0.3～1.2mol/L.
3, method according to claim 1 is characterized in that: the ammoniacal liquor of the interpolation in the described step (3) and the mixing solutions of bicarbonate of ammonia, wherein the molar ratio of bicarbonate of ammonia and ammoniacal liquor is 1: 20～1: 2.
4, method according to claim 1 is characterized in that: mixing solutions, sodium hydroxide solution or the potassium hydroxide solution of ammoniacal liquor, ammoniacal liquor and the bicarbonate of ammonia of the interpolation in the described step (3), its addition are 100%～300% of theoretical consumption, i.e. M
+(mol)/RE
3+(mol)=3～9.
5, method according to claim 4 is characterized in that: mixing solutions, sodium hydroxide solution or the potassium hydroxide solution of described interpolation ammoniacal liquor, ammoniacal liquor and bicarbonate of ammonia, its addition are 110～150% of theoretical consumption, i.e. M
+(mol)/RE
3+(mol)=3.3～4.5.
6, method according to claim 1 is characterized in that: mixing solutions, sodium hydroxide solution or the potassium hydroxide solution of ammoniacal liquor, ammoniacal liquor and the bicarbonate of ammonia of the interpolation in the described step (3), the concentration of interpolation is with [M
+] be calculated as 0.5～1.5mol/L.
7, method according to claim 1 is characterized in that: in the described step (3), the temperature of described precipitin reaction is 20～50 ℃.
8, method according to claim 1 is characterized in that: in the described step (4), after described precipitation was finished, ageing was 1～5 hour under precipitation reaction temperature.
9, method according to claim 1 is characterized in that: in the described step (5), described exsiccant temperature is 120 ℃～200 ℃.
10, method according to claim 1 is characterized in that: in the described step (6), described incinerating temperature is 600～900 ℃.
11, the prepared large specific surface rare earth oxide REO of a kind of method of claim 1, wherein, RE is list-rare earth element among La, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Sc and the Y or more than one rare earth element, this rare earth oxide REO is the single rare earth oxide compound or above-mentioned more than one the rare-earth oxidation mixture of rare earth element of above-mentioned rare earth element, and it is characterized in that: the specific surface area of this rare earth oxide REO is 10～200m
2/ g, its loose specific weight is 0.25～1.0g/cm
3
12, large specific surface rare earth oxide REO according to claim 11, it is characterized in that: described rare earth oxide REO is La
2O
3, Pr
6O
11, Nd
2O
3, Sm
2O
3, Eu
2O
3, Gd
2O
3, Tb
4O
7, Dy
2O
3, Ho
2O
3, Er
2O
3, Tm
2O
3, Yb
2O
3, Lu
2O
3, Y
2O
3And Sc
2O
3In one or more mixture.
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Application publication date: 20060322 Assignee: Qunan New Resources Rare Earth Co., Ltd. Assignor: Beijing Nonferrous Metals Research Institute | Rare Earth New Materials Co., Ltd. Contract record no.: 2010990000192 Denomination of invention: Low bulk specific weight and large specific surface rare-earth oxide REO and its preparing method Granted publication date: 20071114 License type: Exclusive License Record date: 20100412 |
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Effective date of registration: 20130802 Address after: 100088, 2, Xinjie street, Beijing Patentee after: Grirem Advanced Materials Co., Ltd. Address before: 100088, 2, Xinjie street, Beijing Patentee before: General Research Institute for Nonferrous Metals Patentee before: Grirem Advanced Materials Co., Ltd. |