CN103011242A - 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 the inorganic powder material preparation field, relate to a kind of new laminar 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 to apply laminar matrix (such as sheet mica) by the metal oxide with high refractive index (such as ferric oxide, titanium oxide) to form.As the surrogate of mica, synthesized at present several flake oxide powders, such as laminar titanium oxide, flake aluminum oxide, platelet shaped iron oxide, and mix the flake ferric oxide of aluminium, they all develop and put on market successively.
For reaching better pearl effect, requiring matrix is uniform thin slice, and large aspect ratio is arranged simultaneously, and at the thin slice state good thermotolerance and high physical strength is arranged.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 laminar lanthanum compound and preparation method thereof, increase the matrix kind that is used for pearly pigment, expand the application of rare earths field, it has larger radius-thickness ratio than conventional lanthanum trioxide, smooth surface, almost completely colourless, be not easy to form twin and crystal and reunite, have good acidproof, alkaline-resisting and weathering resistance, preparation technology is fairly simple.
Technical solution of the present invention: a kind of laminar lanthanum compound, wherein lanthanum element quality percentage composition is 66%～85.36%, and oxygen quality percentage composition is 14.64%～24.2%, and sulphur quality percentage composition is 0～9.8%.
Laminar lanthanum compound 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.
A kind of preparation method of laminar lanthanum compound (first method), may further comprise the steps: the water of proportional quantity is added in the reactor, begin to stir and with the lanthanum salt of proportional quantity, mineralizer, phosphorus compound adds in the reactor slowly, stir and gradually intensification, can make lanthanum salt, mineralizer, phosphorus compound is dissolved as appropriateness fully, continue again to stir and slowly add the precipitation agent aqueous solution, drip until finish while stirring, obtain suspensoid or gel, by this suspensoid of evaporation drying and gel, then use molten-salt growth method at 800-1400 ℃ of dried products of lower processing, thereby obtain a kind of solid product, again it is washed, filter and drying.
The step that comprises among the above-mentioned preparation method is more specifically:
The water of proportional quantity is added in the reactor, begin to stir and slowly add lanthanum salt, mineralizer, the phosphorus compound of proportional quantity in the reactor, stir and gradually intensification, can make lanthanum salt, mineralizer, phosphorus compound be dissolved as appropriateness fully, continue again to stir and slowly add the precipitation agent aqueous solution, drip until finish while stirring, obtain suspensoid or gel, by this suspensoid of evaporation drying and gel, then with dried product 800-1400 ℃ of lower thermal treatments 2～7 hours, thereby obtain a kind of solid product, again 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 made by alkali or alkaline carbonate, and roughly the amount with above-mentioned water-soluble lanthanum salt is suitable for its amount.Preferred alkali is sodium hydroxide and potassium hydroxide, and alkaline carbonate is yellow soda ash, salt of wormwood, sodium bicarbonate.
Described mineralizer is one or both in sodium-chlor, the Repone K, and the molar weight of mineralizer should be 2-6 times of water-soluble lanthanum.Phosphorus compound can be one or more in the water-soluble cpds of phosphoric acid, phosphoric acid salt, condensed phosphoric acid and condensed phosphate, comprise phosphoric acid, Sodium phosphate dibasic, SODIUM PHOSPHATE, MONOBASIC, dipotassium hydrogen phosphate, potassium primary phosphate, ammonium phosphate in the example, the quality of phosphorus compound (take Vanadium Pentoxide in FLAKES) is 0.5～2% of lanthanum compound, and phosphorus compound makes crystal form thin slice during the heating fused salt is processed.
Described suspensoid or colloidal sol, it contains aqua oxidation lanthanum, mineralizer and phosphorus compound, and they are dispersed in the water medium, and suspensoid or colloidal sol are then by dehydration by evaporation and dry.In order to save the heat that adds for drying, should heat (60-90 ℃) during the preparation aqueous solution, and with the least possible water dissolution, can dissolve solute fully as long as guarantee.The product of dehydration was 800-1400 ℃ of lower thermal treatment 2～7 hours fully.The product that obtains washes to remove sticking free cpds thereon with water.Refilter at last drying.The laminar lanthanum compound that can obtain to expect by this way.
The second preparation method of laminar lanthanum compound, may further comprise the steps: the water of proportional quantity is added in the reactor, begin to stir and in water, drip simultaneously water-soluble lanthanum salts solution and the precipitation agent aqueous solution, form thus suspensoid, continue to stir and add 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 lower process dried products with molten-salt growth method at 800-1400 ℃, thereby obtain a kind of solid product, again it is washed, filter and drying.
The step that comprises among the second preparation method is more specifically: the water of proportional quantity is added in the reactor, begin to stir and in water, drip simultaneously water-soluble lanthanum salts solution and the precipitation agent aqueous solution, form thus suspensoid, continue to stir and add 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 with dried product 800-1400 ℃ of lower thermal treatments 2～7 hours, thereby obtain a kind of solid product, again it is washed, filter and drying.
The suspensoid that will make in advance among the second preparation method or gel to wherein adding mineralizer and phosphorous compound aqueous solution, use the mode identical with above-mentioned first method by evaporation the suspended substance that obtains to be dewatered fully as raw material.Dewatered product was 800-1400 ℃ of thermal treatment 2～7 hours, then wash the product that obtains with water, to remove adhesion free cpds thereon, better with the hot wash effect, final drying in this way can obtain to expect laminar lanthanum compound through the product of washing.In the process for preparing in this way laminar lanthanum compound, mineralizer can be selected alkali metal sulfates, because by this method, is that lanthanum hydroxide and alkali metal sulfates mix, and can not form the double sulphate of lanthanum.Unaccounted technical qualification are identical with the first preparation method among the second preparation method.
The third preparation method of laminar lanthanum compound, may further comprise the steps: the water of proportional quantity is added in the reactor, begin to stir and slowly add the lanthanum salt of proportional quantity in the reactor, stir and gradually intensification, can make lanthanum salt be dissolved as appropriateness fully, continue again to stir and slowly add mineralizer, phosphorus compound, the mixing solutions of precipitation agent, drip until finish while stirring, obtain suspensoid or gel, by this suspensoid of evaporation drying and gel, then use molten-salt growth method at 800-1400 ℃ of dried products of lower processing, thereby obtain a kind of solid product, again it is washed, filter and drying.Unaccounted technical qualification are identical with the second preparation method among the third preparation method.
The present invention is embodied in prepared laminar lanthanum compound and compares with conventional lanthanum trioxide, and it has larger particle diameter, even and little thickness, and larger radius-thickness ratio.In addition, it has smooth surface, and be difficult for to form twin and crystal is reunited, and these all are the required outstanding character of matrix, and the metal oxide-coated that it can be had a high refractive index makes has good nacreous pearly pigment.This laminar lanthanum compound sample in water, disperse and stir after form obvious streamline, prove that thus it has good dispersiveness, streamline is the stratiform candy strip that the reflection ray by the surface of the laminar particle that suspends in liquid and flow forms.With the laminar lanthanum compound sample for preparing more than the scanning electron microscopic observation, find its particle diameter 15-45 μ m, its thickness is less than 1 μ m, and aspect ratio is greater than 20, and do not have twin and gathering.It possesses the required prominent feature of matrix of making pearly pigment, can be used as the raw material of coating, plastics, printing ink, makeup and glaze with the pearly pigment of this substrate preparation.
Embodiment
In order to further specify the present invention, provide following example but be not any limitation of the invention.
Embodiment 1
The water of 250ml is added in the reactor, begin with magnetic stirrer and slowly add 1mol Lanthanum trichloride, 3mol sodium-chlor, 3g ten phosphate dihydrate trisodiums in the reactor, continue to stir and be heated to 70 ℃ with water-bath, continue to stir and slowly add again the aqueous sodium hydroxide solution of 300ml10mol/L, drip until finish while stirring, obtain suspensoid or gel, by evaporating gained solution to drying regime.The gained solid places the about 1000 ℃ of lower heating 5h of resistance furnace.The solid matter of processing to fused salt adds deionized water with the dissolving soluble salt.Leach insoluble solid, wash with water again, last filtration drying.Obtain thus required laminar lanthanum compound.
Detect the laminar lanthanum compound that obtains with x diffraction analysis instrument.The peak that only has lanthanum compound in the diffraction pattern.Result by electron microscope observation shows that laminar lanthanum compound particle diameter is 15-25 μ m, and the about 0.1 μ m of thickness does not produce twin.When by dispersed with stirring in water the time, laminar lanthanum compound produces smooth streamline, and this is the sign of good dispersion.
Embodiment 2:
The water of 250ml is added in the reactor, begin to stir and slowly add 1mol Lanthanum trichloride, 1.5mol sodium-chlor, 1.5mol Repone K, 3g ten phosphate dihydrate trisodiums in the reactor, stir also and be warming up to gradually 70 ℃, continue to stir and slowly add again the aqueous sodium hydroxide solution of 300ml10mol/L, drip until finish while stirring, obtain suspensoid or gel, by evaporating gained solution to drying regime.The gained solid is at about 1000 ℃ of lower heating 5h.The solid matter of processing to fused salt adds deionized water with the dissolving soluble salt.Leach insoluble solid, wash with water again, last filtration drying.Obtain thus required laminar lanthanum compound.
Detect the laminar lanthanum compound that obtains with x diffraction analysis instrument.The peak that only has lanthanum compound in the diffraction pattern.Result by electron microscope observation shows that this laminar lanthanum compound particle diameter is 15-30 μ m, and the about 0.1 μ m of thickness does not produce twin.When by dispersed with stirring in water the time, this laminar lanthanum compound has good dispersion.
Embodiment 3:
By being heated above 60 ℃, 1mol Lanthanum trichloride, 1.5mol sodium-chlor and 1.5mol Repone K are dissolved in the deionized water of 250m1, the solution that makes is called the aqueous solution (a).
Dissolving 3g tertiary sodium phosphate and 3mol sodium hydroxide in the 250m1 deionized water, the solution that makes is called the aqueous solution (b).
Under agitation condition, the aqueous solution (a) evenly joined and be heated in about 70 ℃ aqueous solution (b).Continue to stir 15 minutes, two kinds of solution mixtures that obtain are a kind of thick throw outs.Evaporation gained throw out is to drying regime.The gained solid was about 1100 ℃ of lower heating 5 hours.Add entry in the product that heat treated is crossed with the dissolving soluble salt.Leach insoluble solid, wash with water again, final drying.Obtain thus required laminar lanthanum trioxide.
Detect the laminar lanthanum compound that obtains with x diffraction analysis instrument.The peak that only has lanthanum compound in the diffraction pattern.Result by electron microscope observation shows that this laminar lanthanum compound particle diameter is 20-45 μ m, and the about 0.1 μ m of thickness does not produce twin.When by dispersed with stirring in water the time, this laminar lanthanum compound has good dispersion.
Embodiment 4:
By being heated above 60 ℃, with the 1mol Lanthanum trichloride, 1.5mol sodium-chlor and 1.5mol Repone K are dissolved in the deionized water of 250m1, and the solution that makes is called the aqueous solution (a).
Dissolving 3g tertiary sodium phosphate and 3mol sodium hydroxide in the 250m1 deionized water, the solution that makes is called the aqueous solution (b).
Under agitation condition, the aqueous solution (a) evenly joined and be heated in about 70 ℃ aqueous solution (b).Continue to stir 15 minutes, two kinds of solution mixtures that obtain are a kind of thick throw outs.Evaporation gained throw out is to drying regime.The gained solid was about 1100 ℃ of lower heating 3 hours.Add entry in the product that heat treated is crossed with the dissolving soluble salt.Leach insoluble solid, wash with water again, final drying.Obtain thus required laminar lanthanum compound.
Detect the laminar lanthanum compound that obtains with x diffraction analysis instrument.The peak that only has lanthanum compound in the diffraction pattern.Result by electron microscope observation shows that this laminar lanthanum compound particle diameter is 20-40 μ m, and the about 0.1 μ m of thickness does not produce twin.When by dispersed with stirring in water the time, this laminar lanthanum compound has good dispersion.
Embodiment 5:
By being heated above 60 ℃, with the 1mol Lanthanum trichloride, 1.5mol sodium-chlor and 1.5mol Repone K are dissolved in the deionized water of 250m1, and the solution that makes is called the aqueous solution (a).
Dissolving 6g tertiary sodium phosphate and 3mol sodium hydroxide in the 250m1 deionized water, the solution that makes is called the aqueous solution (b).
Under agitation condition, the aqueous solution (a) evenly joined and be heated in about 70 ℃ aqueous solution (b).Continue to stir 15 minutes, two kinds of solution mixtures that obtain are a kind of thick throw outs.Evaporation gained throw out is to drying regime.The gained solid was about 1100 ℃ of lower heating 5 hours.Add entry in the product that heat treated is crossed with the dissolving soluble salt.Leach insoluble solid, wash with water again, final drying.Obtain thus required laminar lanthanum trioxide.
Detect the laminar lanthanum compound that obtains with x diffraction analysis instrument.The peak that only has lanthanum compound in the diffraction pattern.Result by electron microscope observation shows that this laminar lanthanum compound particle diameter is 15-32 μ m, and the about 0.1 μ m of thickness does not produce twin.When by dispersed with stirring in water the time, this laminar lanthanum compound has good dispersion.
Embodiment 6:
By being heated above 60 ℃, with the 1mol Lanthanum trichloride, 2mol sodium-chlor and 2mol Repone K are dissolved in the deionized water of 250m1, and the solution that makes is called the aqueous solution (a).
Dissolving 6g tertiary sodium phosphate and 3mol sodium hydroxide in the 250m1 deionized water, the solution that makes is called the aqueous solution (b).
Under agitation condition, the aqueous solution (a) evenly joined and be heated in about 70 ℃ aqueous solution (b).Continue to stir 15 minutes, two kinds of solution mixtures that obtain are a kind of thick throw outs.Evaporation gained throw out is to drying regime.The gained solid was about 1100 ℃ of lower heating 5 hours.Add entry in the product that heat treated is crossed with the dissolving soluble salt.Leach insoluble solid, wash with water again, final drying.Obtain thus required laminar lanthanum compound.
Result by electron microscope observation shows that this laminar lanthanum compound particle diameter is 15-30 μ m, and the about 0.1 μ m of thickness does not produce twin.When by dispersed with stirring in water the time, this laminar lanthanum compound has good dispersion.
Embodiment 7:
By being heated to 70 ℃, the 0.5mol Lanthanum trichloride is dissolved in the deionized water of 250ml.1.5mol sodium hydroxide is dissolved in the 300ml deionized water.Under agitation condition, in 15 minutes, with uniform rate two kinds of aqueous solution are joined in the 200ml deionized water simultaneously, make in the first solution solute always with the second solution in solute suitable.Continue to stir 15 minutes, obtain a kind of throw out, filter and obtain the aqua oxidation lanthanum.
By heating, dissolving 3mol anhydrous sodium sulphate adds above-mentioned aqua oxidation lanthanum in gained solution in the 400ml deionized water, and adds 1.5g ten phosphate dihydrate trisodiums.Stirred made solution 10 minutes, evaporating solns is to dry state.The solid that heating obtains under 1100 ℃ again 5 hours.Add water in the product that heat treated is crossed again with the dissolving free sulfate, leach insoluble solid, wash again final drying with water.Obtain thus required laminar lanthanum compound.
Detect the laminar lanthanum compound that obtains with x diffraction analysis instrument.The peak that only has lanthanum compound in the diffraction pattern.Result by electron microscope observation shows that this laminar lanthanum compound particle diameter is 16-35 μ m, and the about 0.1 μ m of thickness does not produce twin.When by dispersed with stirring in water the time, this laminar lanthanum compound has good dispersion.
Claims (10)
1. laminar lanthanum compound, it is characterized in that: wherein lanthanum element quality percentage composition is 66%～85.36%, and oxygen quality percentage composition is 14.64%～24.2%, and sulphur quality percentage composition is 0～9.8%.
2. a kind of laminar lanthanum compound according to claim 1, it is characterized in that: laminar lanthanum compound particle diameter is 15 μ m-45 μ m, thickness is less than 1 μ m, aspect ratio, namely particle diameter/Thickness Ratio is greater than 20.
3. the preparation method of a laminar lanthanum compound, it is characterized in that: the water of proportional quantity is added in the reactor, begin to stir and with the lanthanum salt of proportional quantity, mineralizer, phosphorus compound adds in the reactor slowly, heat up gradually, can make lanthanum salt, mineralizer, phosphorus compound is dissolved as appropriateness fully, continue again to stir and slowly add the precipitation agent aqueous solution, drip until finish while stirring, obtain suspensoid or gel, by this suspensoid of evaporation drying and gel, then use molten-salt growth method at 800-1400 ℃ of dried products of lower processing, dried product is washed, filter and drying, thereby obtain the laminar lanthanum compound of solid product.
4. the preparation method of a laminar lanthanum compound, it is characterized in that: the water of proportional quantity is added in the reactor, begin to stir and in water, drip simultaneously water-soluble lanthanum salts solution and the precipitation agent aqueous solution, form thus suspensoid, continue to stir and add 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 lower process dried products with molten-salt growth method at 800-1400 ℃, dried product is washed, filter and drying, thereby obtain the laminar lanthanum compound of solid product.
5. according to claim 3 or the preparation method of 4 described a kind of laminar lanthanum compounds, it is characterized in that: described water-soluble lanthanum salt is Lanthanum trichloride, lanthanum sulfat, a kind of in the lanthanum nitrate.
6. the preparation method of a kind of laminar lanthanum compound according to claim 3, it is characterized in that: described mineralizer is selected from one or more in the alkali metal chloride, the molar weight of mineralizer should be water-soluble lanthanum 2-6 doubly.
7. the preparation method of a kind of laminar lanthanum compound according to claim 4, it is characterized in that: described mineralizer is selected from one or more in alkali metal chloride, the vitriol, the molar weight of mineralizer should be water-soluble lanthanum 2-6 doubly.
8. according to claim 3 or the preparation method of 4 described a kind of laminar lanthanum compounds, it is characterized in that: the described precipitation agent aqueous solution is the aqueous solution a kind of in alkali, alkaline carbonate, the oxalate, and the amount of precipitation agent is suitable with lanthanum salt amount.
9. according to claim 3 or the preparation method of 4 described a kind of laminar lanthanum compounds, it is characterized in that: described phosphorus compound is selected from one or more in the water-soluble cpds of phosphoric acid, phosphoric acid salt, condensed phosphoric acid and condensed phosphate, take the quality of Vanadium Pentoxide in FLAKES phosphorus compound as 0.5～2% of lanthanum compound.
10. the preparation method of a kind of laminar lanthanum compound according to claim 4, it is characterized in that: by being heated above 60 ℃, 1mol Lanthanum trichloride, 1.5mol sodium-chlor and 1.5mol Repone K are dissolved in the deionized water of 250m1, and the solution that makes is called aqueous solution a;
Dissolving 3g tertiary sodium phosphate and 3mol sodium hydroxide in the 250m1 deionized water, the solution that makes is called aqueous solution b;
Under agitation condition aqueous solution a evenly joined and be heated among about 70 ℃ aqueous solution b, continue to stir 15 minutes, two kinds of solution mixtures that obtain are a kind of thick throw outs, and evaporation gained throw out is to drying regime; The gained solid was about 1100 ℃ of lower heating 5 hours, add entry in the product that heat treated is crossed with the dissolving soluble salt, leach insoluble solid, wash with water again, final drying, obtain thus required laminar lanthanum trioxide, this laminar lanthanum compound particle diameter is 20-45 μ m, and the about 0.1 μ m of thickness does not produce twin, in water the time, this laminar lanthanum compound has good dispersion by dispersed with stirring.
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Cited By (4)
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| CN103803629A (en) * | 2013-12-27 | 2014-05-21 | 江西理工大学 | Method for preparing composite flake rare earth compound |
| CN103803628A (en) * | 2013-12-27 | 2014-05-21 | 江西理工大学 | Scaly yttrium compound and preparation method thereof |
| CN115382562A (en) * | 2021-05-21 | 2022-11-25 | 中国石油化工股份有限公司 | Lanthanum oxycarbonate catalyst, preparation method and application thereof |
| CN115382562B (en) * | 2021-05-21 | 2024-05-10 | 中国石油化工股份有限公司 | Lanthanum oxide carbonate catalyst and preparation method 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 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103803629A (en) * | 2013-12-27 | 2014-05-21 | 江西理工大学 | Method for preparing composite flake rare earth compound |
| CN103803628A (en) * | 2013-12-27 | 2014-05-21 | 江西理工大学 | Scaly yttrium compound and preparation method thereof |
| CN103803628B (en) * | 2013-12-27 | 2015-11-25 | 江西理工大学 | A kind of flakey yttrium compound and preparation method thereof |
| 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 |
| CN115382562A (en) * | 2021-05-21 | 2022-11-25 | 中国石油化工股份有限公司 | Lanthanum oxycarbonate catalyst, preparation method and application thereof |
| CN115382562B (en) * | 2021-05-21 | 2024-05-10 | 中国石油化工股份有限公司 | Lanthanum oxide carbonate catalyst and preparation method and application thereof |
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| CN103011242B (en) | 2015-03-18 |
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