CN103011240A - Bulky-grain rare earth carbonate and preparation method and application of carbonate - Google Patents
Bulky-grain rare earth carbonate and preparation method and application of carbonate Download PDFInfo
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Abstract
The invention relates to bulky-grain rare earth carbonate and a preparation method and application of carbonate, and belongs to the technical field of powdered material preparation. The method comprises the steps of taking sodium carbonate as a precipitant, adding sodium carbonate to rare earth material liquid containing a high-polymer dispersing agent, ageing, washing, filtering, drying, and obtaining rare earth carbonate with a central gain size D50 of 50-202 micrometers, wherein grains are spherical and distributed uniformly. According to the bulky-grain rare earth carbonate and the preparation method and the application of carbonate, the technology is simple and easy to control, the dispersity and filtering performance of sediment in a technology process are good, the technological production is facilitated, the cost is low, no pollution is caused, rare earth carbonate can be further prepared to bulky-grain rare earth oxide with a central grain size D50 of 30-103 micrometers, and the grains are spherical and distributed uniformly.
Description
Technical field
The present invention relates to a kind of large particle rare-earth carbonate and preparation method thereof and application, belong to rare earth powder body material and preparing technical field thereof with specific physical character.
Background technology
Rare earth element has special chemical property, plays very important effect as additive in industrial application, have the title of " industrial monosodium glutamate ".Along with the development of science and technology, more current high-tech areas have also proposed some special character requirements to rare earth material, also show some physical properties aspects except the purity height, such as size, particle shape, dispersiveness, flowability etc.Such as fields such as stupalith, fluorescent material, polishing material, electronic material, opticglass, magneticsubstance, catalyzer, all respectively rare earth material there is different physical property requirements.For example, the polishing powder used of glass and ornament needs that particle diameter is large, density is large, the uniform RE oxide powder of particle shape; During the electrolytic preparation rare earth metal, the oxide compound of large particle diameter, high-density low specific surface area is conducive to electrolytic reaction to carry out, and reduces the workshop dust; In the glass industry, for improving specific refractory power, reduce dispersion, improve the resistance to chemical corrosion of glass, also used the macrobead lanthanum oxide powder of medium particle diameter D50 more than 50 μ m.In recent years, the application of rare earth carbonate is also more and more extensive, is used for medicine such as Phosbloc, and the macrobead cerous carbonate is applied to polishing powder and catalyst technical field etc.
Yet the rare earth carbonate of general wet method preparation is amorphous precipitated, and particle is tiny, is difficult for filtering and washing, causes foreign matter content high, and impact is used, and can not satisfy the occasion that some needs are used large particle rare-earth carbonate.Chinese patent CN1070166 discloses a kind of novel method for preparing carbonated rare earth, rare earth feed liquid joins in the solid ammonium bicarbonate, by changing the mode of operations and controlling temperature and the pH value of reaction soln, reach prepared carbonated rare earth deposit seeds large, the purpose that impurity is few, unexposed granular size.Chinese patent CN1094380 discloses a kind of processing method for preparing carbonated rare earth, take the sulfuric acid rare earth aqueous solution as stock liquid, precipitate take bicarbonate of ammonia as precipitation agent, need to add the solid carbonic acid rare earth as crystal seed, deposit seeds is easy to greatly filter, also unexposed granular size.Chinese patent CN102583493A discloses the preparation method of the rich Ce rare earth oxide of a kind of macrobead, adds rich Ce carbonate crystal seed in the earth solution of low acidity, uses ammonium bicarbonate precipitation again, obtains the rich Ce rare earth oxide of macrobead, and D50 is at 30～40 μ m.Chinese patent CN101381092 discloses the preparation method of a kind of volume particle size, large specific surface spherical yttrium oxide, its preparation process is with the inorganic salt solution of yttrium and ammonium bicarbonate aqueous solution direct reaction, generation contains the slurries of yttrium carbonate, then add a certain amount of solubility ammonium salt, after again slurries are still aging, filter, wash and calcining, can make granularity D50 between 20-100 μ m, specific surface area is at 10-100m
2Controlled spherical yttrium oxide between the/g adds the solubility ammonium salt and reaches the granularity of the synthetic yttrium oxide powder of regulation and control and the purpose of specific surface area size.Chinese patent CN101049952A discloses high apparent density, low specific surface area RE oxide powder and preparation method thereof, contain in the salts solution of rare earth and add additive, add the precipitation agent that contains carbanion, the loose density that obtains at last rare earth oxide is 1.8～2.2g/cm again
3, specific surface area is less than 3g/m
2, volume center particle diameter D50 is greater than 20 μ m.
These disclosed methods most of use bicarbonate of ammonia to be precipitation agent, and what have also needs to add other materials such as crystal seed or ammonium salt.Bicarbonate of ammonia and ammonium salt can produce a large amount of ammonia nitrogen waste waters, process to environment protection standard and bring very big difficulty, have more increased production cost; And add the method for crystal seed, at first will obtain preferably crystal seed of crystal formation, but the crystal seed of carbonated rare earth is also and be not easy to make, and precipitation process is wayward.The carbonate deposition crystal formation is bad, easily carries impurity secretly, causes the product foreign matter content higher, and particularly non-rare earth impurity such as calcium, chlorion equal size are higher.
Summary of the invention
The purpose of this invention is to provide a kind of large particle rare-earth carbonate and preparation method thereof and application.Large particle rare-earth carbonate of the present invention is spheroidal particle, and medium particle diameter D50 is 60～202 μ m, and even particle distribution is mobile good.Large particle rare-earth manufacture of carbonates method of the present invention easy control simple to operate, non-environmental-pollution; Large and be spherical because of particle, precipitation is easily filtered, is washed, and is difficult for carrying secretly impurity, so foreign matter content is low, can be used for being prepared into high-purity large particle rare-earth carbonate products more than the 4N, and carbonate can further be processed and prepare large particle rare-earth oxide; And cost is low, is easy to realize suitability for industrialized production.
The technical solution used in the present invention comprises as follows:
A kind of large particle rare-earth carbonate provided by the invention, medium particle diameter D50 are 60～202 μ m, and particle is spherical, even particle size distribution, good fluidity.
Rare earth carbonate of the present invention refers to the carbonate of one or two or more kinds rare earth element among rare earth element La and Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, the Y.
The preparation method of large particle rare-earth carbonate of the present invention, be included under the whipped state, the carbonate deposition agent is joined in the rare earth feed liquid, control precipitation endpoint pH, obtain the rare earth carbonate precipitation, through ageing, obtain spherical large particle rare-earth carbonate after filtration, washing, the drying, its key is to have added macromolecule dispersing agent PAA and/or PVA before the precipitation in rare earth feed liquid.These two kinds of macromolecule dispersing agents generally are applied to prepare superfine powder and play dissemination, and the present invention have been prepared large particle rare-earth carbonate with it, has played unexpected effect.
One of preferred version of the present invention, described macromolecule dispersing agent quality consumption is for pressing rare earth feed liquid volumeter 0.01～1g/L.
One of preferred version of the present invention, described carbonate deposition agent be sodium bicarbonate and or the aqueous solution of yellow soda ash, precipitant solution concentration is counted 0.1～2mol/L with carbonate.
One of preferred version of the present invention, described rare earth feed liquid are to contain solution at least a in nitrate, muriate and the vitriol, and rare earth ion concentration is 0.1～2mol/L.
One of preferred version of the present invention, control precipitation endpoint pH is 5～6.5.PH is excessively low, and the rare earth ion precipitation is incomplete, and pH is too high, can not get spherical macrobead.
One of preferred version of the present invention, 20～250 rev/mins of stirring velocitys.
One of preferred version of the present invention, temperature of reaction are room temperature～55 ℃, and digestion time is 6～12 hours.
The method that further prepares large particle rare-earth oxide with large particle rare-earth carbonate of the present invention is decomposed the calcination under high temperature of gained rare earth carbonate fully, can prepare corresponding large particle rare-earth oxide; Gained large particle rare-earth oxide, granule-morphology are spherical, and particle diameter D50 is 30～103 μ m, and even particle size distribution is mobile good.
The present invention has the following advantages
1, large particle rare-earth carbonate of the present invention, pattern is spheroidal particle, medium particle diameter D50 is 60～202 μ m, even particle size distribution, good fluidity.
2, large particle rare-earth manufacture of carbonates of the present invention, technique is simple and easy to control, and without ammonia and nitrogen pollution, cost is low, does not need to add crystal seed, and preparation cycle shortens, and is easy to realize suitability for industrialized production.
3, large particle rare-earth manufacture of carbonates of the present invention, because deposit seeds is large and be sphere, thus easily filter and wash, and be difficult between particle being mingled with, non-rare earth impurity content is low, can prepare the above high-purity rare-earth carbonate products of 4N.
4, use large particle rare-earth manufacture of carbonates method of the present invention, further be applied to prepare corresponding large particle rare-earth oxide, granule-morphology also is spherical, and medium particle diameter D50 is 30～103 μ m, and even particle size distribution is without reuniting, mobile good.
Description of drawings
Fig. 1 is the product yttrium carbonate SEM picture of Comparative Examples 1.
Fig. 2 is the product yttrium carbonate SEM picture of embodiment 1.
Fig. 3 is the product yttrium oxide SEM picture of embodiment 1.
Fig. 4 is the product samaric carbonate SEM picture of embodiment 5.
Fig. 5 is the product yttrium carbonate europium gadolinium SEM picture of embodiment 6.
Fig. 6 is the product terbium sesquioxide SEM picture of embodiment 7.
Fig. 7 is the product carbonic acid erbium SEM picture of embodiment 8.
Fig. 8 is the product carbonic acid lutetium SEM picture of embodiment 10.
Embodiment
Comparative Examples 1
Referring to Fig. 1.Under the room temperature, getting concentration is 0.5mol/L yttrium chloride solution 1.0L, regulates 100 rev/mins of mixing speed, adding concentration in the feed liquid is the 0.5mol/L sodium hydrogen carbonate solution, reaches end in 6.0 o'clock to the pH value, obtains the carbonated rare earth throw out, stop to stir, ageing 48h filters throw out, washing gets yttrium carbonate after dehydrating, detecting granularity D50 is 10.4 μ m, the indivedual subglobulars of electron microscopic observation pattern, major part is irregularly shaped, porous, be mingled with many irregular particles, not of uniform size; This yttrium carbonate is calcined 3h in 900 ℃ retort furnace, the yttrium oxide that obtains, the electron microscopic observation pattern does not change, and detecting granularity D50 is 3.6 μ m.
Comparative Examples 2
Getting concentration is 1.0mol/L praseodymium nitrate neodymium solution 1.0L, be heated to 40 ℃, regulate 150 rev/mins of mixing speed, adding concentration in the feed liquid is the 1.0mol/L sodium carbonate solution, reach end in 5.5 o'clock to the pH value, obtain the carbonated rare earth throw out, stop to stir ageing 24h, throw out is filtered, washing gets the praseodymium carbonate neodymium after dehydrating, detecting granularity D50 is 12.1 μ m; The electron microscopic observation pattern is sheet, and size is more even; This praseodymium carbonate neodymium is calcined 5h in 1000 ℃ retort furnace, the Praseodymium trioxide neodymium that obtains, the electron microscopic observation pattern is sheet, and size is more even, and detecting granularity D50 is 5.3 μ m.
Embodiment 1
Referring to Fig. 2, Fig. 3.Under the room temperature, getting concentration is 0.5mol/L yttrium chloride solution 1.0L, adds 1%PAA solution 10ml, regulate 100 rev/mins of mixing speed, adding concentration in the feed liquid is the 0.5mol/L sodium carbonate solution, reaches end in 6.0 o'clock to the pH value, obtain the carbonated rare earth throw out, stop to stir ageing 12h, throw out is filtered, washing gets yttrium carbonate after dehydrating, detecting granularity D50 is 201.9 μ m, the whole granule-morphologies of electron microscopic observation are spherical (as shown in Figure 2), and size evenly; This yttrium carbonate is calcined 3h in 900 ℃ retort furnace, the yttrium oxide that obtains, electron microscopic observation still are that whole granule-morphologies are spherical (as shown in Figure 3), and size is even, and detecting granularity D50 is 102.8 μ m.
Embodiment 2
Getting concentration is 1.0mol/L praseodymium nitrate neodymium solution 1.0L, is heated to 40 ℃, adds 1%PAA solution 5ml, regulating 150 rev/mins of mixing speed, to add concentration in the feed liquid be the 1.0mol/L sodium hydrogen carbonate solution, reaches end in 5.5 o'clock to the pH value, obtains the carbonated rare earth throw out, stop to stir, ageing 6h filters throw out, washing, get the praseodymium carbonate neodymium after dehydrating, detecting granularity D50 is 92.8 μ m, and the whole granule-morphologies of electron microscopic observation are spherical, and size evenly; This praseodymium carbonate neodymium is calcined 5h in 1000 ℃ retort furnace, the Praseodymium trioxide neodymium that obtains, electron microscopic observation granule-morphology all are spherical, and size is even, and detecting granularity D50 is 55.6 μ m.
Embodiment 3
Getting concentration is 2.0mol/L lanthanum chloride solution 1.0L, is heated to 50 ℃, adds 1%PVA solution 1ml, regulate 250 rev/mins of mixing speed, entering to add concentration in the feed liquid is the 2.0mol/L sodium carbonate solution, reaches end in 6.5 o'clock to the pH value, obtain the carbonated rare earth throw out, stop to stir ageing 6h, throw out is filtered, washing gets Phosbloc after dehydrating, detecting granularity D50 is 60.2 μ m, the whole granule-morphologies of electron microscopic observation are spherical, and size evenly; This Phosbloc is calcined 2h in 1000 ℃ retort furnace, the lanthanum trioxide that obtains, electron microscopic observation granule-morphology all are spherical, and size is even, and detecting granularity D50 is 30.5 μ m.
Embodiment 4
Getting concentration is 1.5mol/L solution of cerium chloride by oxidation 1.0L, is heated to 40 ℃, adds 1%PAA solution 1ml, regulate 200 rev/mins of mixing speed, adding concentration in the feed liquid is the 1.5mol/L sodium hydrogen carbonate solution, reaches end in 6.2 o'clock to the pH value, obtain the carbonated rare earth throw out, stop to stir ageing 6h, throw out is filtered, washing gets cerous carbonate after dehydrating, detecting granularity D50 is 110.2 μ m, the whole granule-morphologies of electron microscopic observation are spherical, and size evenly; This cerous carbonate is calcined 3h in 800 ℃ retort furnace, the cerium oxide that obtains, electron microscopic observation granule-morphology all are spherical, and size is even, and detecting granularity D50 is 65.8 μ m.
Embodiment 5
Referring to Fig. 4.Under the room temperature, getting concentration is 0.1mol/L samaric sulfate solution 1.0L, adds 10%PAA and each 5ml of 10%PVA solution, regulate 250 rev/mins of mixing speed, adding concentration in the feed liquid is the 0.1mol/L sodium hydrogen carbonate solution, reaches end in 5.8 o'clock to the pH value, obtain the carbonated rare earth throw out, stop to stir ageing 10h, throw out is filtered, washing gets samaric carbonate after dehydrating, detecting granularity D50 is 88.6 μ m, the whole granule-morphologies of electron microscopic observation are spherical (as shown in Figure 4), and size evenly; This samaric carbonate is calcined 5h in 800 ℃ retort furnace, the Samarium trioxide that obtains, electron microscopic observation granule-morphology all are spherical, and size is even, and detecting granularity D50 is 45.8 μ m.
Embodiment 6
Referring to Fig. 5.Under the room temperature, get respectively Yttrium trichloride, europium sulfate and each 0.3L of Gadolinium trinitrate solution, 0.4L, 0.3L that concentration is 0.2mol/L, add 10%PVA solution 10ml, regulate 250 rev/mins of mixing speed, adding concentration in the feed liquid is the 0.2mol/L sodium carbonate solution, reach end in 5.5 o'clock to the pH value, obtain the carbonated rare earth throw out, stop to stir ageing 8h, throw out is filtered, washing gets yttrium carbonate europium gadolinium after dehydrating, detecting granularity D50 is 114.2 μ m, the whole granule-morphologies of electron microscopic observation are spherical (as shown in Figure 5), and size evenly; This yttrium carbonate europium gadolinium is calcined 3h in 900 ℃ retort furnace, the yttrium europium oxide gadolinium that obtains, electron microscopic observation granule-morphology all are spherical, and size is even, and detecting granularity D50 is 76.4 μ m.
Embodiment 7
Referring to Fig. 6.Under the room temperature, getting concentration is 0.5mol/L terbium chloride and each 0.5L of sulfuric acid terbium solution, adds 1%PVA solution 10ml, regulate 150 rev/mins of mixing speed, adding concentration in the feed liquid is the 0.5mol/L sodium hydrogen carbonate solution, reaches end in 5 o'clock to the pH value, obtain the carbonated rare earth throw out, stop to stir ageing 10h, throw out is filtered, washing gets terbium carbonate after dehydrating, detecting granularity D50 is 78.5 μ m, the whole granule-morphologies of electron microscopic observation are spherical, and size evenly; This terbium carbonate is calcined 2h in 1000 ℃ retort furnace, the terbium sesquioxide that obtains, electron microscopic observation granule-morphology all are spherical (as shown in Figure 6), and size is even, and detecting granularity D50 is 31.2 μ m.
Embodiment 8
Referring to Fig. 7.Under the room temperature, getting concentration is 0.8mol/L Erbium trichloride solution 1.0L, adds 1%PVA solution 5ml, regulate 150 rev/mins of mixing speed, adding concentration in the feed liquid is the 0.8mol/L sodium carbonate solution, reaches end in 5.8 o'clock to the pH value, obtain the carbonated rare earth throw out, stop to stir ageing 12h, throw out is filtered, washing gets the carbonic acid erbium after dehydrating, detecting granularity D50 is 160.8 μ m, the whole granule-morphologies of electron microscopic observation are spherical (as shown in Figure 7), and size evenly; This carbonic acid erbium is calcined 4h in 900 ℃ retort furnace, the Erbium trioxide that obtains, electron microscopic observation granule-morphology all are spherical, and size is even, and detecting granularity D50 is 100.3 μ m.
Embodiment 9
Under the room temperature, getting concentration is 0.25mol/L Ytterbium trichloride solution and each 0.5L of ytterbium nitrate, adds 5%PVA solution 10ml, regulate 150 rev/mins of mixing speed, adding concentration in the feed liquid is the 0.5mol/L sodium carbonate solution, reaches end in 6.5 o'clock to the pH value, obtain the carbonated rare earth throw out, stop to stir ageing 12h, throw out is filtered, washing gets ytterbium carbonate after dehydrating, detecting granularity D50 is 143.6 μ m, the whole granule-morphologies of electron microscopic observation are spherical, and size evenly; This ytterbium carbonate is calcined 4h in 900 ℃ retort furnace, the ytterbium oxide that obtains, electron microscopic observation granule-morphology all are spherical, and size is even, and detecting granularity D50 is 98.2 μ m.
Embodiment 10
Referring to Fig. 8.Under the room temperature, getting concentration is 1.0mol/L lutecium nitrate solution 1.0L, add 1%PVA solution 2ml, regulate 200 rev/mins of mixing speed, add concentration in the feed liquid and be 1.0mol/L yellow soda ash and sodium bicarbonate mixing solutions (mass ratio each 50%), reach end in 6.0 o'clock to the pH value, obtain the carbonated rare earth throw out, stop to stir ageing 10h, throw out is filtered, washing gets the carbonic acid lutetium after dehydrating, detecting granularity D50 is 125.1 μ m, the whole granule-morphologies of electron microscopic observation are spherical (as shown in Figure 8), and size evenly; This carbonic acid lutetium is calcined 4h in 900 ℃ retort furnace, the lutecium oxide that obtains, electron microscopic observation granule-morphology all are spherical, and size is even, and detecting granularity D50 is 76.5 μ m.
Explanation is that above embodiment is only unrestricted in order to technical scheme of the present invention to be described at last.Although with reference to preferred embodiment the present invention is had been described in detail, those of ordinary skill in the art is to be understood that, technical scheme of the present invention made amendment or be equal to replace and do not break away from aim and the scope of technical solution of the present invention, all should be encompassed in the middle of the claim scope of the present invention.
Claims (10)
1. a large particle rare-earth carbonate is characterized in that, medium particle diameter D50 is 60～202 μ m.
2. large particle rare-earth carbonate according to claim 1, it is characterized in that, described rare earth carbonate refers to the carbonate of one or two or more kinds rare earth element among rare earth element La and Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, the Y.
3. method for preparing the described large particle rare-earth carbonate of claim 1, be included under the whipped state, the carbonate deposition agent is joined in the rare earth feed liquid, control precipitation endpoint pH, obtain the rare earth carbonate precipitation, through ageing, obtain spherical large particle rare-earth carbonate after filtration, washing, the drying, it is characterized in that, in rare earth feed liquid, added macromolecule dispersing agent PAA and/or PVA before the precipitation.
4. the preparation method of described large particle rare-earth carbonate according to claim 3 is characterized in that, described macromolecule dispersing agent quality consumption is counted 0.01～1g/L by the rare earth feed liquid volume.
5. according to claim 3 or the preparation method of 4 described large particle rare-earth carbonate, it is characterized in that, described carbonate deposition agent be sodium bicarbonate and or yellow soda ash, the concentration of precipitation agent is counted 0.1～2mol/L with carbonate.
6. the preparation method of described large particle rare-earth carbonate according to claim 3 is characterized in that, rare earth feed liquid is to contain solution at least a in nitrate, muriate, the vitriol, counts 0.1～2mol/L with rare earth ion concentration.
7. the preparation method of described large particle rare-earth carbonate according to claim 3 is characterized in that, the precipitation endpoint pH is 5～6.5.
8. the preparation method of described large particle rare-earth carbonate according to claim 3 is characterized in that 20～250 rev/mins of stirring velocitys.
9. the preparation method of described large particle rare-earth carbonate according to claim 3 is characterized in that, temperature of reaction is room temperature～55 ℃, and digestion time is 6～12 hours.
10. the method that further prepares large particle rare-earth oxide with the large particle rare-earth carbonate of claim 3 method preparation, it is characterized in that, the calcination of gained rare earth carbonate is namely got large particle rare-earth oxide, and described rare earth oxide particle diameter D50 is 30～103 μ m.
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Application publication date: 20130403 |