CN103011241B - 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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- CN103011241B CN103011241B CN201210590789.1A CN201210590789A CN103011241B CN 103011241 B CN103011241 B CN 103011241B CN 201210590789 A CN201210590789 A CN 201210590789A CN 103011241 B CN103011241 B CN 103011241B
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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 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 that metal oxide (as ferric oxide, titanium oxide) by having high refractive index applies laminar matrix (as sheet mica) and formed.As the surrogate of mica, synthesize several flake oxide powder at present, as laminar titanium oxide, flake aluminum oxide, platelet shaped iron oxide, with the flake ferric oxide etc. mixing aluminium, but, the matrix kind that can be used for pearly pigment of current synthetic is also few, rare earth element is introduced in matrix just less, only have Chinese patent ZL200810003686.4 to propose and prepare Neodymium trioxide substrate by molten-salt growth method, the Neodymium trioxide sheet of preparation presents distinct colors under different light, red-purple is observed under natural light, be light blue under fluorescent light, it is pink under incandescent light.
Summary of the invention
The object of the invention is to provide a kind of praseodymium tabular crystal and preparation method thereof, increases the matrix kind being used for pearly pigment, expands the Application Areas of rare earth; It has larger radius-thickness ratio than regular oxidation praseodymium, and smooth surface is not easy to form twin and crystal reunion, has good acidproof, alkaline-resisting and weathering resistance.
Technical scheme of the present invention: a kind of praseodymium tabular crystal, wherein the mass percentage of praseodymium is 68% ~ 85%, and the mass percentage of oxygen is 15% ~ 23.5%, and the mass percentage of sulphur is 0 ~ 8.5%.
Praseodymium platelet particle diameter is 15 μm ~ 40 μm, and thickness is less than 1 μm, aspect ratio, and namely particle diameter/Thickness Ratio is greater than 20.
Praseodymium platelet is black, has nacreous lustre, smooth surface, not easily forms twin and crystal reunion, is applicable to the matrix doing pearly pigment.
Adding mass ratio is after 0 ~ 10% Cerium II Chloride, and praseodymium platelet takes on a red color gloss.
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 by dried product as thermal treatment 2 ~ 6 hours at 850-1400 DEG C in resistance furnace, then wash, filter and dryly obtain praseodymium tabular crystal.
In the present invention, water-soluble praseodymium salt can be various water-soluble praseodymium salt, and aqueous precipitation agent can be alkali or alkaline carbonate, and the amount of its consumption and water-soluble praseodymium salt is suitable.
In the present invention mineralizer and phosphorus compound can together with join praseodymium salt brine solution, also can join in the precipitation agent aqueous solution together.Mineralizer is one or more in alkali metal chloride and alkali metal sulfates.Consumption is 2-6 times of the molar weight of water-soluble praseodymium salt.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 counts 1 ~ 5% of praseodymium compound quality with Vanadium Pentoxide in FLAKES.
In order to obtain preferably praseodymium tabular crystal, the present invention adopts presoma and fused salt Hybrid Heating, and at high temperature melting treatment prepares praseodymium tabular crystal.
Praseodymium tabular crystal prepared by the present invention is compared with regular oxidation praseodymium, and it has larger particle diameter, even and little thickness, and larger radius-thickness ratio.Praseodymium tabular crystal particle diameter is 15 μm-45 μm, and thickness is less than 1 μm, aspect ratio, i.e. particle diameter/Thickness Ratio flake-shaped particles of being greater than 20.This praseodymium tabular crystal color is black, smooth surface, not easily forms twin and crystal reunion, is applicable to the matrix doing pearly pigment.Can be obtained after the metal oxide-coated of high refractive index and be there is better nacreous pearly pigment.This pearly pigment is suitable for plastics, coating, ink, makeup and glaze.
Embodiment
Embodiment 1
Heating in water bath to 80 DEG C, is dissolved in 0.5 mole of praseodymium chloride and 2 mole nacls in 250ml deionized water, obtains the praseodymium chloride solution of sodium chloride-containing.In 200ml deionized water, dissolve 1.5 molar sodium hydroxides and 1.5 gram of ten phosphate dihydrate trisodium, obtain the aqueous sodium hydroxide solution of P contained compound.When stirring, mixing above-mentioned two kinds of aqueous solution, mixing complete continuation stirring 30 minutes, obtain a suspensoid or colloidal sol, be evaporated to drying regime, gained solid is heated 4 hours at 1100 DEG C.Deionized water is added to dissolve free sodium-chlor in the product that heat treated is crossed.Leach insoluble solid, then use deionized water wash, final drying, obtain desired praseodymium tabular crystal thus.
With the praseodymium tabular crystal that X-ray diffractometer test obtains, in diffraction pattern, only has a kind of peak composing compound.Show by the result of opticmicroscope and electron microscope observation, praseodymium tabular crystal particle diameter is 15 ~ 35 μm, and thickness is 0.5 μm, does not produce twin.When by dispersed with stirring in water time, praseodymium tabular crystal produces smooth streamline.
Embodiment 2
Heating in water bath to 80 DEG C, is dissolved in 0.5 mole of praseodymium chloride in 250ml deionized water, obtains the praseodymium chloride aqueous solution.In 200ml deionized water, dissolve 1.5 molar sodium hydroxides, obtain aqueous sodium hydroxide solution.When stirring, mix above-mentioned two kinds of aqueous solution, mix complete continuation stirring 30 minutes, obtain a suspensoid, be evaporated to drying regime, dried powder and 142 grams of sodium sulfate, 174 grams of potassium sulfate, 2 gram of ten phosphate dihydrate trisodium are placed in ball grinder, ball milling 4 hours in planetary ball mill, make to mix, gained solid is heated 4 hours at 1100 DEG C.Deionized water is added to dissolve free sodium-chlor in the product that heat treated is crossed.Leach insoluble solid, then use deionized water wash, final drying, obtain desired praseodymium tabular crystal thus.
Result shows, the praseodymium tabular crystal particle diameter prepared in this way is 15 ~ 25 μm, and thickness is 0.3 μm, favorable dispersity.With enforcement experiment 1 compare, sulfuric acid composite fused salt has better dissolving power, makes tabular crystal shape more regular, size distribution evenly.
Embodiment 3
Heating in water bath to 80 DEG C, is dissolved in 0.5 mole of praseodymium chloride, 1 mole nacl and 1 M KCl in 250ml deionized water, obtains the praseodymium chloride solution containing villaumite.In 200ml deionized water, dissolve 0.75 mole of either sodium carbonate and 2 gram of ten phosphate dihydrate trisodium, obtain the aqueous sodium hydroxide solution of P contained compound.When stirring, mixing above-mentioned two kinds of aqueous solution, mixing complete continuation stirring 30 minutes, obtain a suspensoid or colloidal sol, be evaporated to drying regime, gained solid is heated 4 hours at 1100 DEG C.Deionized water is added to dissolve free sodium-chlor in the product that heat treated is crossed.Leach insoluble solid, then use deionized water wash, final drying, obtain desired praseodymium tabular crystal thus.
Result shows, praseodymium tabular crystal particle diameter is 15 ~ 25 μm, and thickness is about 0.4 μm, regular shape, favorable dispersity.
Embodiment 4
Change the thermal treatment temp in embodiment 2 into 1200 DEG C, all the other compositions, formula are identical with preparation technology.
Result shows, due to the rising of firing temperature, praseodymium tabular crystal size distribution broadens, and particle diameter is 15 ~ 45 μm, and shape is not very regular.
Embodiment 5
Change the soaking time in embodiment 2 into 6 hours, all the other compositions, formula are identical with preparation technology.
Result shows, due to the prolongation of soaking time, praseodymium tabular crystal thickness increases to some extent, and be 0.9 μm, shape is more regular, favorable dispersity.
Embodiment 6
Change the quality of the sodium sulfate in embodiment 2 and potassium sulfate into 284 grams and 348 grams respectively, all the other compositions, formula are identical with preparation technology.
Result shows, due to the increase of fused salt amount, praseodymium tabular crystal particle diameter reduces, and distributes also uneven,
Embodiment 7
Be heated to 80 DEG C, 0.45 mole of praseodymium chloride, 0.05 mole of Cerium II Chloride and 2 mole nacls be dissolved in 250ml deionized water, obtain the praseodymium chloride solution of sodium chloride-containing.In 200ml deionized water, dissolve 1.5 molar sodium hydroxides and 1.5 gram of ten phosphate dihydrate trisodium, obtain the aqueous sodium hydroxide solution of P contained compound.When stirring, mixing above-mentioned two kinds of aqueous solution, mixing complete continuation stirring 30 minutes, obtain a suspensoid or colloidal sol, be evaporated to drying regime, gained solid is heated 4 hours at 1100 DEG C.Deionized water is added to dissolve free sodium-chlor in the product that heat treated is crossed.Leach insoluble solid, then use deionized water wash, final drying.
Gained praseodymium tabular crystal color becomes red, and the praseodymium tabular crystal obtained with X-ray diffractometer test, also only has a kind of peak composing compound in diffraction pattern.Show by the result of opticmicroscope and electron microscope observation, praseodymium tabular crystal particle diameter is 15 ~ 40 μm, and thickness is 0.6 μm, is evenly distributed.
Claims (7)
1. a praseodymium tabular crystal, it is characterized in that: wherein the mass percentage of praseodymium is 68% ~ 80.5%, the mass percentage of oxygen is 15% ~ 20%, the mass percentage of sulphur is 0.1 ~ 8.5%, the mass percentage of phosphorus is 0.01 ~ 2.8%, and praseodymium platelet particle diameter is 15 μm ~ 40 μm, and thickness is less than 1 μm, aspect ratio, namely particle diameter/Thickness Ratio is greater than 20.
2. a kind of praseodymium tabular crystal according to claim 1, is characterized in that: praseodymium platelet is black, has nacreous lustre, smooth surface, not easily forms twin and crystal is reunited, and is applicable to the matrix doing pearly pigment.
3. a kind of praseodymium tabular crystal according to claim 1, is characterized in that: adding mass ratio is after 0 ~ 10% Cerium II Chloride, and praseodymium platelet takes on a red color gloss.
4. the preparation method of a praseodymium tabular crystal according to claim 1, it is characterized in that: the precipitation agent aqueous solution is added drop-wise in the mixed solution of water-soluble praseodymium salt, mineralizer, phosphorus compound, obtain a kind of suspensoid or gel, by this suspensoid of evaporation drying or gel, at 850-1400 DEG C, to process after cooling in 2-6 hour to obtain a solid product by molten-salt growth method, after wash again, filter and dry obtain praseodymium tabular crystal.
5. the preparation method of a kind of praseodymium tabular crystal according to claim 4, is characterized in that: the described precipitation agent aqueous solution is a kind of aqueous solution in alkali, alkaline carbonate, oxalate, and the amount of its consumption and water-soluble praseodymium salt is suitable.
6. the preparation method of a kind of praseodymium tabular crystal according to claim 4, it is characterized in that: the mineralizer in the mixed solution of described water-soluble praseodymium salt, mineralizer, phosphorus compound is one or more in alkali metal chloride and alkali metal sulfates, mineralizer consumption be the 2-6 of the molar weight of water-soluble praseodymium salt doubly.
7. the preparation method of a kind of praseodymium tabular crystal according to claim 4, it is characterized in that: in the mixed solution of described water-soluble praseodymium salt, mineralizer, phosphorus compound, phosphorus compound is one or more in the water-soluble cpds of phosphoric acid, phosphoric acid salt, condensed phosphoric acid and condensed phosphate, and phosphorus compound consumption counts 1 ~ 5% of praseodymium compound quality with Vanadium Pentoxide in FLAKES.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN106517295B (en) * | 2016-10-18 | 2018-02-23 | 西北工业大学 | A kind of synthesizing high-stability γ Pr2S3The method of powder |
| 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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| CN1241987A (en) * | 1996-11-19 | 2000-01-19 | 罗狄亚化学公司 | Use of a beta rare earth sulphide as colouring pigment and method for preparing same |
| CN101024506A (en) * | 2007-02-05 | 2007-08-29 | 金坛市西南化工研究所 | Process for preparing superfine, high-purity praseodymium oxide by using Pr-Nd riched materials |
| CN101225244A (en) * | 2008-01-11 | 2008-07-23 | 江西理工大学 | Sheet-like neodymium oxide and method for manufacturing same |
| CN101583567A (en) * | 2007-01-12 | 2009-11-18 | 巴斯夫欧洲公司 | Pigments containing tin and rare earth elements |
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Patent Citations (4)
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|---|---|---|---|---|
| CN1241987A (en) * | 1996-11-19 | 2000-01-19 | 罗狄亚化学公司 | Use of a beta rare earth sulphide as colouring pigment and method for preparing same |
| CN101583567A (en) * | 2007-01-12 | 2009-11-18 | 巴斯夫欧洲公司 | Pigments containing tin and rare earth elements |
| CN101024506A (en) * | 2007-02-05 | 2007-08-29 | 金坛市西南化工研究所 | Process for preparing superfine, high-purity praseodymium oxide by using Pr-Nd riched materials |
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| "几种稀土纳米材料的合成及性能研究";尹小斌;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20110115;B020-371，正文第33-34页 * |
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