CN103011242B - Flaky lanthanum compound and preparation method thereof - Google Patents
Flaky lanthanum compound and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a new flaky lanthanum compound and a preparation method thereof. The preparation method comprises the following steps: adding proportional water into a reactor, starting stirring while slowly adding proportional lanthanum salt, mineralizer and phosphorous compound into the reactor, gradually heating while stirring to completely dissolve the lanthanum salt, mineralizer and phosphorous compound to a moderate degree, slowly and dropwisely adding a precipitating agent water solution while stirring to obtain a suspension or gel, drying the suspension or gel by evaporation, and drying the product at 800-1400 DEG C by a molten salt method to obtain the flaky lanthanum compound. The particle size of the flaky lanthanum compound is 15-45 mu m, the thickness is less than 1 mu m, and the aspect ratio (particle size/thickness ratio) is greater than 20. The new flaky lanthanum compound has the advantages of favorable dispersity and smooth surface, is almost completely colorless, can be widely used in plastics, paints, inks, cosmetics and glaze, and can also be used as a base material of pearlescent pigments.
Description
Technical field
The invention belongs to inorganic powder material preparation field, relate to a kind of new Flaky lanthanum compound 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, synthesized several flake oxide powder at present, as laminar titanium oxide, flake aluminum oxide, platelet shaped iron oxide, and mix the flake ferric oxide of aluminium, they have all developed and have put on market successively.
For reaching better pearl effect, requiring that matrix is uniform thin slice, having large aspect ratio simultaneously, and the thermotolerance had at wafer state and high physical strength.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, under natural light, be observed red-purple, be light blue under fluorescent light, is pink under incandescent light.
Summary of the invention
The object of the invention is to provide a kind of Flaky lanthanum compound and preparation method thereof, increase the matrix kind being used for pearly pigment, expand the Application Areas of rare earth, it has larger radius-thickness ratio than regular oxidation lanthanum, smooth surface, almost completely free look, is not easy to form twin and crystal reunion, have good acidproof, alkaline-resisting and weathering resistance, preparation technology is fairly simple.
Technical solution of the present invention: a kind of Flaky lanthanum compound, wherein lanthanum element mass percentage is 66% ~ 85.36%, and oxygen mass percentage is 14.64% ~ 24.2%, and sulphur mass percentage is 0 ~ 9.8%.
Flaky lanthanum compound particle diameter is 15 μm-45 μm, and thickness is less than 1 μm, aspect ratio, and namely particle diameter/Thickness Ratio is greater than 20.
A kind of preparation method's (first method) of Flaky lanthanum compound, comprise the following steps: the water of proportional quantity is added in reactor, start stir and by the lanthanum salt of proportional quantity, mineralizer, phosphorus compound adds in reactor slowly, stir and heat up gradually, lanthanum salt can be made, mineralizer, phosphorus compound is dissolved as appropriateness completely, continue again stir and slowly add the precipitation agent aqueous solution, drip until complete while stirring, obtain suspensoid or gel, by this suspensoid of evaporation drying and gel, then molten-salt growth method is used to process dried product at 800-1400 DEG C, thus obtain a kind of solid product, again it is washed, filter and drying.
The step that above-mentioned preparation method comprises is more specifically:
The water of proportional quantity is added in reactor, start stir and the lanthanum salt of proportional quantity, mineralizer, phosphorus compound are added in reactor slowly, stir and heat up gradually, lanthanum salt, mineralizer, phosphorus compound can be made to be dissolved as appropriateness completely, continue again stir and slowly add the precipitation agent aqueous solution, drip until complete while stirring, obtain suspensoid or gel, by this suspensoid of evaporation drying and gel, then by the thermal treatment 2 ~ 7 hours at 800-1400 DEG C of dried product, thus obtain a kind of solid product, then it is washed, filter and drying.
Described lanthanum salt can be various lanthanum salt, and wherein Lanthanum trichloride and lanthanum nitrate are preferred.The precipitation agent aqueous solution is obtained by alkali or alkaline carbonate, and its amount is roughly suitable with the amount of above-mentioned water soluble lanthanum salt.Preferred alkali is sodium hydroxide and potassium hydroxide, and alkaline carbonate is sodium carbonate, salt of wormwood, sodium bicarbonate.
Described mineralizer is one or both in sodium-chlor, Repone K, the molar weight of mineralizer should be the 2-6 of water soluble lanthanum doubly.Phosphorus compound can be one or more in the water-soluble cpds of phosphoric acid, phosphoric acid salt, condensed phosphoric acid and condensed phosphate, example comprises phosphoric acid, Sodium phosphate dibasic, SODIUM PHOSPHATE, MONOBASIC, dipotassium hydrogen phosphate, potassium primary phosphate, ammonium phosphate, the quality (in Vanadium Pentoxide in FLAKES) of phosphorus compound is 0.5 ~ 2% of lanthanum compound, and phosphorus compound makes crystal form thin slice during the process of heating fused salt.
Described suspensoid or colloidal sol, it contains hydrous zirconia gel, mineralizer and phosphorus compound, and they are dispersed in water medium, and suspensoid or colloidal sol are then also dry by dehydration by evaporation.Add heat in order to save for drying, should heat (60-90 DEG C) when preparing the aqueous solution, and by the least possible water dissolution, as long as ensure to dissolve solute completely.The product dewatered completely thermal treatment 2 ~ 7 hours at 800-1400 DEG C.The products in water washing obtained is to remove sticky free cpds thereon.Finally refilter drying.The Flaky lanthanum compound of expection can be obtained by this way.
The second preparation method of Flaky lanthanum compound, comprise the following steps: the water of proportional quantity is added in reactor, start stir and in water, drip water soluble lanthanum salts solution and the precipitation agent aqueous solution simultaneously, form suspensoid thus, continuation is stirred and is added the aqueous solution of mineralizer and phosphorus compound, obtain suspensoid or the gel of mixed hydrolysis product, by this suspensoid of evaporation drying or gel, and at 800-1400 DEG C, process dried product by molten-salt growth method, thus obtain a kind of solid product, again it is washed, filter and drying.
The step that the second preparation method comprises is more specifically: add in reactor by the water of proportional quantity, start stir and in water, drip water soluble lanthanum salts solution and the precipitation agent aqueous solution simultaneously, form suspensoid thus, continuation is stirred and is added the aqueous solution of mineralizer and phosphorus compound, obtain suspensoid or the gel of mixed hydrolysis product, by this suspensoid of evaporation drying or gel, then by the thermal treatment 2 ~ 7 hours at 800-1400 DEG C of dried product, thus obtain a kind of solid product, again it is washed, filter and drying.
In the second preparation method using suspensoid obtained in advance or gel as raw material, adding mineralizer and phosphorous compound aqueous solution wherein, by evaporating, the suspended substance obtained being dewatered completely by the mode identical with above-mentioned first method.Dewatered product was 800-1400 DEG C of thermal treatment 2 ~ 7 hours, then the product obtained is washed with water, to remove adhesion free cpds thereon, better by hot wash effect, final drying, through the product of washing, in this way can obtain expection Flaky lanthanum compound.Preparing in the process of Flaky lanthanum compound in this way, mineralizer can select alkali metal sulfates, because by this method, is lanthanum hydroxide and alkali metal sulfates mixing, can not forms the double sulphate of lanthanum.In the second preparation method, unaccounted technical qualification are identical with the first preparation method.
The third preparation method of Flaky lanthanum compound, comprise the following steps: the water of proportional quantity is added in reactor, start stir and the lanthanum salt of proportional quantity is added in reactor slowly, stir and heat up gradually, lanthanum salt can be made to be dissolved as appropriateness completely, continue again stir and slowly add mineralizer, phosphorus compound, the mixing solutions of precipitation agent, drip until complete while stirring, obtain suspensoid or gel, by this suspensoid of evaporation drying and gel, then molten-salt growth method is used to process dried product at 800-1400 DEG C, thus obtain a kind of solid product, again it is washed, filter and drying.In the third preparation method, unaccounted technical qualification are identical with the second preparation method.
The present invention is embodied in prepared Flaky lanthanum compound compared with regular oxidation lanthanum, and it has larger particle diameter, even and little thickness, and larger radius-thickness ratio.In addition, it has smooth surface, and not easily forms twin and crystal reunion, and these are all the outstanding character needed for matrix, and it can be obtained the nacreous pearly pigment had by the metal oxide-coated with high refractive index.This Flaky lanthanum compound sample disperses and stirs the obvious streamline of rear formation in water, and prove that it has good dispersiveness thus, streamline is the stratiform candy strip formed by the reflection ray on the surface of the flake-shaped particles suspended in a liquid and flow.With the Flaky lanthanum compound sample more than scanning electron microscopic observation prepared, find its particle diameter 15-45 μm, its thickness is less than 1 μm, and aspect ratio is greater than 20, and does not have twin and gathering.It possesses the prominent feature needed for the matrix making pearly pigment, can be used as the raw material of coating, plastics, ink, makeup and glaze with pearly pigment prepared by this substrate.
Embodiment
In order to further illustrate the present invention, provide example but be not any limitation of the invention below.
Embodiment 1
The water of 250ml is added in reactor, start by magnetic stirrer and 1mol Lanthanum trichloride, 3mol sodium-chlor, 3g ten phosphate dihydrate trisodium are added in reactor slowly, continue stir and be heated to 70 DEG C with water-bath, continue again to stir the aqueous sodium hydroxide solution also slowly adding 300ml10mol/L, drip until complete while stirring, obtain suspensoid or gel, by evaporation gained solution to drying regime.Gained solid heats 5h at being placed in resistance furnace about 1000 DEG C.Solid matter to fused salt process adds deionized water to dissolve soluble salt.Leach insoluble solid, then wash with water, last filtration drying.Obtain required Flaky lanthanum compound thus.
The Flaky lanthanum compound obtained is detected with x diffraction analysis instrument.The peak of lanthanum compound is only had in diffraction pattern.Shown by the result of electron microscope observation, Flaky lanthanum compound particle diameter is 15-25 μm, and thickness about 0.1 μm, does not produce twin.When by dispersed with stirring in water time, Flaky lanthanum compound produces smooth streamline, and this is the mark of good dispersion.
Embodiment 2:
The water of 250ml is added in reactor, start stir and 1mol Lanthanum trichloride, 1.5mol sodium-chlor, 1.5mol Repone K, 3g ten phosphate dihydrate trisodium are added in reactor slowly, stir and be warming up to 70 DEG C gradually, continue again to stir the aqueous sodium hydroxide solution also slowly adding 300ml10mol/L, drip until complete while stirring, obtain suspensoid or gel, by evaporation gained solution to drying regime.Gained solid heats 5h at about 1000 DEG C.Solid matter to fused salt process adds deionized water to dissolve soluble salt.Leach insoluble solid, then wash with water, last filtration drying.Obtain required Flaky lanthanum compound thus.
The Flaky lanthanum compound obtained is detected with x diffraction analysis instrument.The peak of lanthanum compound is only had in diffraction pattern.Shown by the result of electron microscope observation, this Flaky lanthanum compound particle diameter is 15-30 μm, and thickness about 0.1 μm, does not produce twin.When by dispersed with stirring in water time, this Flaky lanthanum compound has good dispersion.
Embodiment 3:
By being heated above 60 DEG C, be dissolved in the deionized water of 250m1 by 1mol Lanthanum trichloride, 1.5mol sodium-chlor and 1.5mol Repone K, obtained solution is called the aqueous solution (a).
In 250m1 deionized water, dissolve 3g tertiary sodium phosphate and 3mol sodium hydroxide, obtained solution is called the aqueous solution (b).
Under agitation the aqueous solution (a) is evenly joined in the aqueous solution (b) being heated to about 70 DEG C.Continue stirring 15 minutes, the two kinds of solution mixtures obtained are a kind of thick throw outs.Evaporation gained throw out is to drying regime.Gained solid heats 5 hours at about 1100 DEG C.Water is added to dissolve soluble salt in the product that heat treated is crossed.Leach insoluble solid, then wash with water, final drying.Laminar lanthanum trioxide needed for obtaining thus.
The Flaky lanthanum compound obtained is detected with x diffraction analysis instrument.The peak of lanthanum compound is only had in diffraction pattern.Shown by the result of electron microscope observation, this Flaky lanthanum compound particle diameter is 20-45 μm, and thickness about 0.1 μm, does not produce twin.When by dispersed with stirring in water time, this Flaky lanthanum compound has good dispersion.
Embodiment 4:
By being heated above 60 DEG C, by 1mol Lanthanum trichloride, 1.5mol sodium-chlor and 1.5mol Repone K are dissolved in the deionized water of 250m1, and obtained solution is called the aqueous solution (a).
In 250m1 deionized water, dissolve 3g tertiary sodium phosphate and 3mol sodium hydroxide, obtained solution is called the aqueous solution (b).
Under agitation the aqueous solution (a) is evenly joined in the aqueous solution (b) being heated to about 70 DEG C.Continue stirring 15 minutes, the two kinds of solution mixtures obtained are a kind of thick throw outs.Evaporation gained throw out is to drying regime.Gained solid heats 3 hours at about 1100 DEG C.Water is added to dissolve soluble salt in the product that heat treated is crossed.Leach insoluble solid, then wash with water, final drying.Obtain required Flaky lanthanum compound thus.
The Flaky lanthanum compound obtained is detected with x diffraction analysis instrument.The peak of lanthanum compound is only had in diffraction pattern.Shown by the result of electron microscope observation, this Flaky lanthanum compound particle diameter is 20-40 μm, and thickness about 0.1 μm, does not produce twin.When by dispersed with stirring in water time, this Flaky lanthanum compound has good dispersion.
Embodiment 5:
By being heated above 60 DEG C, by 1mol Lanthanum trichloride, 1.5mol sodium-chlor and 1.5mol Repone K are dissolved in the deionized water of 250m1, and obtained solution is called the aqueous solution (a).
In 250m1 deionized water, dissolve 6g tertiary sodium phosphate and 3mol sodium hydroxide, obtained solution is called the aqueous solution (b).
Under agitation the aqueous solution (a) is evenly joined in the aqueous solution (b) being heated to about 70 DEG C.Continue stirring 15 minutes, the two kinds of solution mixtures obtained are a kind of thick throw outs.Evaporation gained throw out is to drying regime.Gained solid heats 5 hours at about 1100 DEG C.Water is added to dissolve soluble salt in the product that heat treated is crossed.Leach insoluble solid, then wash with water, final drying.Laminar lanthanum trioxide needed for obtaining thus.
The Flaky lanthanum compound obtained is detected with x diffraction analysis instrument.The peak of lanthanum compound is only had in diffraction pattern.Shown by the result of electron microscope observation, this Flaky lanthanum compound particle diameter is 15-32 μm, and thickness about 0.1 μm, does not produce twin.When by dispersed with stirring in water time, this Flaky lanthanum compound has good dispersion.
Embodiment 6:
By being heated above 60 DEG C, by 1mol Lanthanum trichloride, 2mol sodium-chlor and 2mol Repone K are dissolved in the deionized water of 250m1, and obtained solution is called the aqueous solution (a).
In 250m1 deionized water, dissolve 6g tertiary sodium phosphate and 3mol sodium hydroxide, obtained solution is called the aqueous solution (b).
Under agitation the aqueous solution (a) is evenly joined in the aqueous solution (b) being heated to about 70 DEG C.Continue stirring 15 minutes, the two kinds of solution mixtures obtained are a kind of thick throw outs.Evaporation gained throw out is to drying regime.Gained solid heats 5 hours at about 1100 DEG C.Water is added to dissolve soluble salt in the product that heat treated is crossed.Leach insoluble solid, then wash with water, final drying.Obtain required Flaky lanthanum compound thus.
Shown by the result of electron microscope observation, this Flaky lanthanum compound particle diameter is 15-30 μm, and thickness about 0.1 μm, does not produce twin.When by dispersed with stirring in water time, this Flaky lanthanum compound has good dispersion.
Embodiment 7:
By being heated to 70 DEG C, 0.5mol Lanthanum trichloride is dissolved in the deionized water of 250ml.1.5mol sodium hydroxide is dissolved in 300ml deionized water.Under agitation, in 15 minutes, with uniform rate, two kinds of aqueous solution are joined in 200ml deionized water simultaneously, make the solute in the first solution always suitable with the solute in the second solution.Continue stirring 15 minutes, obtain a kind of throw out, filter and obtain hydrous zirconia gel.
By heating, in 400ml deionized water, dissolve 3mol anhydrous sodium sulphate, in gained solution, add above-mentioned hydrous zirconia gel, and add 1.5g ten phosphate dihydrate trisodium.Solution made by stirring 10 minutes, evaporating solns is to dry state.The solid that obtains is heated again 5 hours at 1100 DEG C.Add water to dissolve free sulfate in the product that heat treated is crossed again, leach insoluble solid, then wash with water, final drying.Obtain required Flaky lanthanum compound thus.
The Flaky lanthanum compound obtained is detected with x diffraction analysis instrument.The peak of lanthanum compound is only had in diffraction pattern.Shown by the result of electron microscope observation, this Flaky lanthanum compound particle diameter is 16-35 μm, and thickness about 0.1 μm, does not produce twin.When by dispersed with stirring in water time, this Flaky lanthanum compound has good dispersion.
Claims (8)
1. a Flaky lanthanum compound, is characterized in that: wherein lanthanum element mass percentage is 66% ~ 85.36%, and oxygen mass percentage is 14.64% ~ 24.2%, and sulphur mass percentage is 0 ~ 9.8%;
Described Flaky lanthanum compound particle diameter is 15 μm-45 μm, and thickness is less than 1 μm, aspect ratio, and namely particle diameter/Thickness Ratio is greater than 20.
2. prepare the method for Flaky lanthanum compound according to claim 1 for one kind, it is characterized in that: the water of proportional quantity is added in reactor, start stir and by the water soluble lanthanum salt of proportional quantity, mineralizer, phosphorus compound adds in reactor slowly, heat up gradually, water soluble lanthanum salt can be made, mineralizer, phosphorus compound is dissolved as appropriateness completely, continue again stir and slowly add the precipitation agent aqueous solution, drip until complete while stirring, obtain suspensoid or gel, by this suspensoid of evaporation drying and gel, then molten-salt growth method is used to process dried product at 800-1400 DEG C, wash with the product after molten-salt growth method process, filter and drying, thus obtain solid product Flaky lanthanum compound.
3. prepare the method for Flaky lanthanum compound according to claim 1 for one kind, it is characterized in that: the water of proportional quantity is added in reactor, start stir and in water, drip water soluble lanthanum salts solution and the precipitation agent aqueous solution simultaneously, form suspensoid thus, continuation is stirred and is added the aqueous solution of mineralizer and phosphorus compound, obtain suspensoid or the gel of mixed hydrolysis product, by this suspensoid of evaporation drying or gel, and at 800-1400 DEG C, process dried product by molten-salt growth method, wash with the product after molten-salt growth method process, filter and drying, thus obtain solid product Flaky lanthanum compound.
4. a kind of method preparing Flaky lanthanum compound according to claim 1 according to Claims 2 or 3, is characterized in that: described water soluble lanthanum salt is Lanthanum trichloride, lanthanum sulfat, the one in lanthanum nitrate.
5. a kind of method preparing Flaky lanthanum compound according to claim 1 according to claim 2, it is characterized in that: described mineralizer be selected from alkali metal chloride one or more, the molar weight of mineralizer should be the 2-6 of water soluble lanthanum salt molar weight doubly.
6. a kind of method preparing Flaky lanthanum compound according to claim 1 according to claim 3, it is characterized in that: described mineralizer be selected from alkali metal chloride, vitriol one or more, the molar weight of mineralizer should be the 2-6 of water soluble lanthanum salt molar weight doubly.
7. a kind of method preparing Flaky lanthanum compound according to claim 1 according to Claims 2 or 3, it is characterized in that: the described precipitation agent aqueous solution is the aqueous solution a kind of in alkali, alkaline carbonate, oxalate, the amount of precipitation agent is suitable with water soluble lanthanum salt amount.
8. a kind of method preparing Flaky lanthanum compound according to claim 1 according to Claims 2 or 3, it is characterized in that: described phosphorus compound be selected from the water-soluble cpds of phosphoric acid, phosphoric acid salt, condensed phosphoric acid, condensed phosphate one or more, be lanthanum compound in the quality of Vanadium Pentoxide in FLAKES phosphorus compound 0.5 ~ 2%.
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| CN103803629B (en) * | 2013-12-27 | 2016-03-16 | 江西理工大学 | A kind of preparation method of compound sheet rare earth compound |
| CN103803628B (en) * | 2013-12-27 | 2015-11-25 | 江西理工大学 | A kind of flakey yttrium compound and preparation method thereof |
| AU2021446295A1 (en) * | 2021-05-21 | 2024-01-18 | China Petroleum & Chemical Corporation | Lanthanum oxycarbonate catalyst, and preparation method therefor and application thereof |
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| US3340006A (en) * | 1963-05-01 | 1967-09-05 | Corning Glass Works | Method of producing thin flakes of metal oxide |
| CN1150165A (en) * | 1995-09-14 | 1997-05-21 | 默克专利股份有限公司 | Flaky aluminium oxide and pearlescent pigment, and production thereof |
| CN101225244A (en) * | 2008-01-11 | 2008-07-23 | 江西理工大学 | Sheet-like neodymium oxide and method for manufacturing same |
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Patent Citations (3)
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| US3340006A (en) * | 1963-05-01 | 1967-09-05 | Corning Glass Works | Method of producing thin flakes of metal oxide |
| CN1150165A (en) * | 1995-09-14 | 1997-05-21 | 默克专利股份有限公司 | Flaky aluminium oxide and pearlescent pigment, and production thereof |
| CN101225244A (en) * | 2008-01-11 | 2008-07-23 | 江西理工大学 | Sheet-like neodymium oxide and method for manufacturing same |
Non-Patent Citations (3)
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| Controlled synthesis of rare earth nanostructures;Zheng-Guang Yan et al.;《J. Mater. Chem.》;20080929;第18卷;第5046-5059页 * |
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