CN103011241A - Rare-earth praseodymium lamellar crystal and preparation method for same - Google Patents
Rare-earth praseodymium lamellar crystal and preparation method for same Download PDFInfo
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- CN103011241A CN103011241A CN2012105907891A CN201210590789A CN103011241A CN 103011241 A CN103011241 A CN 103011241A CN 2012105907891 A CN2012105907891 A CN 2012105907891A CN 201210590789 A CN201210590789 A CN 201210590789A CN 103011241 A CN103011241 A CN 103011241A
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Abstract
The invention relates to a rare-earth praseodymium lamellar crystal and a preparation method for the same. The praseodymium content in the praseodymium lamellar crystal is 68-85% (mass fraction), the particle diameter of the praseodymium lamellar crystal is 15-40 mu m, the thickness is less than 1 mu m, and the aspect ratio, namely, the particle diameter/thickness ratio is greater than 20. During preparation, praseodymium saline solution containing a mineralizer and a phosphorus compound is mixed with a precipitator aqueous solution to obtain a suspensoid or a gel, and the suspensoid or the gel is dried via evaporation, the dried suspensoid or gel is treated for 2-6 hours at 850-1400 DEG C via a molten-salt method to obtain a solid product, and then the solid product is washed by water, filtered and dried to obtain the rare-earth praseodymium lamellar crystal. The praseodymium lamellar crystal is high in aspect ratio, good in dispersity and smooth in surface; the praseodymium lamellar crystal is a black lamellar crystal, and presents a red gloss after being added with a small amount of cerium, thus being suitable for being used as a matrix for a pearlescent pigment, and capable of being widely used for plastics, coatings, inks, cosmetics and glazes.
Description
Technical field
The invention belongs to the inorganic powder material preparation field, relate to a kind of praseodymium tabular crystal and preparation method thereof.
Background technology
Pearly pigment is the pigment that a class has pearlescent soft color and luster, and it is to apply laminar matrix (such as sheet mica) by the metal oxide with high refractive index (such as ferric oxide, titanium oxide) to form.Surrogate as mica, several flake oxide powders have been synthesized at present, such as laminar titanium oxide, flake aluminum oxide, platelet shaped iron oxide, with flake ferric oxide of mixing aluminium etc., yet, the matrix kind that can be used for pearly pigment of synthetic is also few at present, rare earth element is introduced in the matrix just still less, only have Chinese patent ZL200810003686.4 to propose to prepare the Neodymium trioxide substrate with molten-salt growth method, the Neodymium trioxide sheet of preparation presents distinct colors under different light, being observed red-purple under natural light, is light blue under luminescent lamp, is pink under incandescent light.
Summary of the invention
The object of the invention provides a kind of praseodymium tabular crystal and preparation method thereof, increases the matrix kind that is used for pearly pigment, expands the application of rare earths field; It has larger radius-thickness ratio than conventional Praseodymium trioxide, and smooth surface is not easy to form twin and crystal is reunited, and has good acidproof, alkaline-resisting and weathering resistance.
Technical scheme of the present invention: a kind of praseodymium tabular crystal, wherein the quality percentage composition of praseodymium is 68%～85%, and the quality percentage composition of oxygen is 15%～23.5%, and the quality percentage composition of sulphur is 0～8.5%.
Praseodymium platelet particle diameter is 15 μ m～40 μ m, and thickness is less than 1 μ m, aspect ratio, and namely particle diameter/Thickness Ratio is greater than 20.
The praseodymium platelet is black, has nacreous lustre, and smooth surface is difficult for forming twin and crystal is reunited, and is fit to do the matrix of pearly pigment.
After adding mass ratio and being 0～10% Cerium II Chloride, the praseodymium platelet gloss that takes on a red color.
A kind of praseodymium tabular crystal preparation method, the precipitation agent aqueous solution is added drop-wise in the mixed solution of praseodymium salt, mineralizer, phosphorus compound, obtain a kind of suspensoid or gel, by this suspensoid of evaporation drying or gel, then with dried product as in the resistance furnace 850-1400 ℃ of lower thermal treatments 2～6 hours, wash again, filter and the dry praseodymium tabular crystal that obtains.
Water-soluble praseodymium salt can be various water-soluble praseodymium salt among the present invention, and the aqueous precipitation agent can be alkali or alkaline carbonate, and the amount of its consumption and water-soluble praseodymium salt is suitable.
Mineralizer and phosphorus compound can join the praseodymium salt brine solution together among the present invention, also can join together in the precipitation agent aqueous solution.Mineralizer is one or more in alkali metal chloride and the alkali metal sulfates.Consumption be water-soluble praseodymium salt molar weight 2-6 doubly.Phosphorus compound is one or more in the water-soluble cpds of phosphoric acid, phosphoric acid salt, condensed phosphoric acid and condensed phosphate, and consumption is counted 1～5% of praseodymium compound quality with Vanadium Pentoxide in FLAKES.
In order to obtain more excellent praseodymium tabular crystal, the present invention adopts presoma and fused salt Hybrid Heating, and at high temperature melting treatment prepares the praseodymium tabular crystal.
The prepared praseodymium tabular crystal of the present invention is compared with conventional Praseodymium trioxide, and it has larger particle diameter, even and little thickness, and larger radius-thickness ratio.Praseodymium tabular crystal particle diameter is 15 μ m-45 μ m, and thickness is less than 1 μ m, aspect ratio, and namely particle diameter/Thickness Ratio is greater than 20 laminar particle.This praseodymium tabular crystal color is black, and smooth surface is difficult for forming twin and crystal is reunited, and is fit to do the matrix of pearly pigment.Can be made after the metal oxide-coated of high refractive index and be had better nacreous pearly pigment.This pearly pigment is suitable for plastics, coating, printing ink, makeup and glaze.
Embodiment
Embodiment 1
Heating in water bath to 80 ℃ is dissolved in 0.5 mole of praseodymium chloride and 2 mole nacls in the 250ml deionized water, obtains the praseodymium chloride solution of sodium chloride-containing.Dissolving 1.5 molar sodium hydroxides and 1.5 restrain ten phosphate dihydrate trisodiums in the 200ml deionized water, obtain the aqueous sodium hydroxide solution of P contained compound.In situation about stirring, mix above-mentioned two kinds of aqueous solution, mix complete continuation and stirred 30 minutes, get a suspensoid or colloidal sol, be evaporated to drying regime, the gained solid was heated 4 hours under 1100 ℃.Add deionized water in the product that heat treated is crossed to dissolve free sodium-chlor.Leach insoluble solid, use deionized water wash again, final drying obtains desired praseodymium tabular crystal thus.
Praseodymium tabular crystal with the X-ray diffractometer test obtains only has a kind of peak of composing compound in the diffraction pattern.Result with opticmicroscope and electron microscope observation shows that praseodymium tabular crystal particle diameter is 15～35 μ m, and thickness is 0.5 μ m, does not produce twin.When by dispersed with stirring in water the time, the praseodymium tabular crystal produces smooth streamline.
Embodiment 2
Heating in water bath to 80 ℃ is dissolved in 0.5 mole of praseodymium chloride in the 250ml deionized water, gets the praseodymium chloride aqueous solution.Dissolving 1.5 molar sodium hydroxides obtain aqueous sodium hydroxide solution in the 200ml deionized water.In situation about stirring, mix above-mentioned two kinds of aqueous solution, mixing complete continuation stirred 30 minutes, get a suspensoid, be evaporated to drying regime, the powder that drying is good and 142 gram sodium sulfate, 174 gram vitriolate of tartar, 2 grams, ten phosphate dihydrate trisodiums place ball grinder, and ball milling is 4 hours in planetary ball mill, make to mix, the gained solid was heated 4 hours under 1100 ℃.Add deionized water in the product that heat treated is crossed to dissolve free sodium-chlor.Leach insoluble solid, use deionized water wash again, final drying obtains desired praseodymium tabular crystal thus.
The result shows that the praseodymium tabular crystal particle diameter of preparation is 15～25 μ m in this way, and thickness is 0.3 μ m, favorable dispersity.Compare with enforcement experiment 1, the sulfuric acid composite fused salt has better dissolving power, makes rule of tabular crystal shape, and size distribution is more even.
Embodiment 3
Heating in water bath to 80 ℃ is dissolved in 0.5 mole of praseodymium chloride, 1 mole nacl and 1 mole of Repone K in the 250ml deionized water, obtains containing the praseodymium chloride solution of villaumite.0.75 mole of yellow soda ash of dissolving and 2 restrains ten phosphate dihydrate trisodiums in the 200ml deionized water, obtains the aqueous sodium hydroxide solution of P contained compound.In situation about stirring, mix above-mentioned two kinds of aqueous solution, mix complete continuation and stirred 30 minutes, get a suspensoid or colloidal sol, be evaporated to drying regime, the gained solid was heated 4 hours under 1100 ℃.Add deionized water in the product that heat treated is crossed to dissolve free sodium-chlor.Leach insoluble solid, use deionized water wash again, final drying obtains desired praseodymium tabular crystal thus.
The result shows that praseodymium tabular crystal particle diameter is 15～25 μ m, and thickness is about 0.4 μ m, regular shape, favorable dispersity.
Embodiment 4
Change the thermal treatment temp among the embodiment 2 into 1200 ℃, all the other compositions, prescription and preparation technology are identical.
The result shows that because the rising of firing temperature, praseodymium tabular crystal size distribution broadens, and particle diameter is 15～45 μ m, and shape is not very regular.
Embodiment 5
Change the soaking time among the embodiment 2 into 6 hours, all the other compositions, prescription and preparation technology are identical.
The result shows that because the prolongation of soaking time, praseodymium tabular crystal thickness increases to some extent, is 0.9 μ m, and shape is rule, favorable dispersity.
Embodiment 6
Change respectively the quality of the sodium sulfate among the embodiment 2 and vitriolate of tartar into 284 grams and 348 grams, all the other compositions, prescription and preparation technology are identical.
The result shows that because the increase of fused salt amount, praseodymium tabular crystal particle diameter reduces, and it is also inhomogeneous to distribute,
Embodiment 7
Be heated to 80 ℃, 0.45 mole of praseodymium chloride, 0.05 mole of Cerium II Chloride and 2 mole nacls are dissolved in the 250ml deionized water, obtain the praseodymium chloride solution of sodium chloride-containing.Dissolving 1.5 molar sodium hydroxides and 1.5 restrain ten phosphate dihydrate trisodiums in the 200ml deionized water, obtain the aqueous sodium hydroxide solution of P contained compound.In situation about stirring, mix above-mentioned two kinds of aqueous solution, mix complete continuation and stirred 30 minutes, get a suspensoid or colloidal sol, be evaporated to drying regime, the gained solid was heated 4 hours under 1100 ℃.Add deionized water in the product that heat treated is crossed to dissolve free sodium-chlor.Leach insoluble solid, use again deionized water wash, final drying.
Gained praseodymium tabular crystal color becomes redness, and the praseodymium tabular crystal with the X-ray diffractometer test obtains also only has a kind of peak of composing compound in the diffraction pattern.Result with opticmicroscope and electron microscope observation shows that praseodymium tabular crystal particle diameter is 15～40 μ m, and thickness is 0.6 μ m, is evenly distributed.
Claims (9)
1. praseodymium tabular crystal, it is characterized in that: wherein the quality percentage composition of praseodymium is 68%～85%, and the quality percentage composition of oxygen is 15%～23.5%, and the quality percentage composition of sulphur is 0～8.5%.
2. described a kind of praseodymium tabular crystal according to claim 1, it is characterized in that: praseodymium platelet particle diameter is 15 μ m～40 μ m, thickness is less than 1 μ m, aspect ratio, namely particle diameter/Thickness Ratio is greater than 20.
3. described a kind of praseodymium tabular crystal according to claim 1, it is characterized in that: the praseodymium platelet is black, has nacreous lustre, and smooth surface is difficult for forming twin and crystal is reunited, and is fit to do the matrix of pearly pigment.
4. described a kind of praseodymium tabular crystal according to claim 1 is characterized in that: after adding mass ratio and being 0～10% Cerium II Chloride, and the praseodymium platelet gloss that takes on a red color.
5. the preparation method of a praseodymium tabular crystal, it is characterized in that: the precipitation agent aqueous solution is added drop-wise in the mixed solution of praseodymium salt, mineralizer, phosphorus compound, obtain a kind of suspensoid or gel, by this suspensoid of evaporation drying or gel, with molten-salt growth method 850-1400 ℃ lower after processing cooling in 2-6 hour a solid product, after wash again, filter and the dry praseodymium tabular crystal that obtains.
6. the preparation method of described a kind of praseodymium tabular crystal according to claim 5, it is characterized in that: the described precipitation agent aqueous solution is the aqueous solution a kind of in alkali, alkaline carbonate, the oxalate, the amount of its consumption and water-soluble praseodymium salt is suitable.
7. the preparation method of described a kind of praseodymium tabular crystal according to claim 5, it is characterized in that: mineralizer is one or more in alkali metal chloride and the alkali metal sulfates in the mixed solution of described praseodymium salt, mineralizer, phosphorus compound, the mineralizer consumption be water-soluble praseodymium salt molar weight 2-6 doubly.
8. the preparation method of described a kind of praseodymium tabular crystal according to claim 5, it is characterized in that: phosphorus compound is one or more in the water-soluble cpds of phosphoric acid, phosphoric acid salt, condensed phosphoric acid and condensed phosphate in the mixed solution of described praseodymium salt, mineralizer, phosphorus compound, and the phosphorus compound consumption is counted 1～5% of praseodymium compound quality with Vanadium Pentoxide in FLAKES.
9. the preparation method of described a kind of praseodymium tabular crystal according to claim 5, it is characterized in that: better implementation condition is: heating in water bath to 80 ℃, 0.5 mole of praseodymium chloride and 2 mole nacls are dissolved in the 250ml deionized water, obtain the praseodymium chloride solution of sodium chloride-containing; Dissolving 1.5 molar sodium hydroxides and 1.5 restrain ten phosphate dihydrate trisodiums in the 200ml deionized water, obtain the aqueous sodium hydroxide solution of P contained compound; In situation about stirring, mix above-mentioned two kinds of aqueous solution, mix complete continuation and stirred 30 minutes, get a suspensoid or colloidal sol, be evaporated to drying regime, the gained solid was heated 4 hours under 1100 ℃; Add deionized water in the product that heat treated is crossed to dissolve free sodium-chlor, leach insoluble solid, use again deionized water wash, final drying obtains desired praseodymium tabular crystal thus, and praseodymium tabular crystal particle diameter is 15～35 μ m, thickness is 0.5 μ m, do not produce twin, in water the time, the praseodymium tabular crystal produces smooth streamline by dispersed with stirring.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103613112A (en) * | 2013-11-26 | 2014-03-05 | 内蒙古大学 | Simple preparation method of rare earth carbonate pearlescent pigment |
| CN103613113A (en) * | 2013-11-26 | 2014-03-05 | 内蒙古大学 | Preparation method of rare earth oxides or carbonic acid oxidized rare earth pearl pigments |
| CN106517295A (en) * | 2016-10-18 | 2017-03-22 | 西北工业大学 | Method for synthesizing high-stability gamma-Pr2S3 powder |
| CN112028105A (en) * | 2020-08-06 | 2020-12-04 | 常州市卓群纳米新材料有限公司 | Method for preparing nanometer praseodymium oxide by fused salt coprecipitation method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103613112A (en) * | 2013-11-26 | 2014-03-05 | 内蒙古大学 | Simple preparation method of rare earth carbonate pearlescent pigment |
| CN103613113A (en) * | 2013-11-26 | 2014-03-05 | 内蒙古大学 | Preparation method of rare earth oxides or carbonic acid oxidized rare earth pearl pigments |
| CN106517295A (en) * | 2016-10-18 | 2017-03-22 | 西北工业大学 | Method for synthesizing high-stability gamma-Pr2S3 powder |
| CN112028105A (en) * | 2020-08-06 | 2020-12-04 | 常州市卓群纳米新材料有限公司 | Method for preparing nanometer praseodymium oxide by fused salt coprecipitation method |
| CN112028105B (en) * | 2020-08-06 | 2023-09-05 | 常州市卓群纳米新材料有限公司 | Method for preparing nano praseodymium oxide by fused salt coprecipitation method |
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