CN103803629A - Method for preparing composite flake rare earth compound - Google Patents
Method for preparing composite flake rare earth compound Download PDFInfo
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- CN103803629A CN103803629A CN201310736893.1A CN201310736893A CN103803629A CN 103803629 A CN103803629 A CN 103803629A CN 201310736893 A CN201310736893 A CN 201310736893A CN 103803629 A CN103803629 A CN 103803629A
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Abstract
The invention discloses a method for preparing a composite flake rare earth compound. The method comprises specific steps of dissolving rare earth soluble salt, mineralizer and phosphorus compound into deionized water so as to obtain a mixed solution, heating the mixed solution up to 80DEG C, dropwise adding precipitator water solution into the solution, then continuously stirring for half an hour so as to obtain a suspensoid or gel, drying the suspensoid or gel through evaporating; then putting the dried product into a resistance furnace, treating for 2-7 hours at 800DEG C-1400DEG C; washing with water, filtering and drying so as to obtain the composite flake rare earth compound. The method for preparing the composite flake rare earth compound is simple to operate, has mild technological conditions, and does no pollute the environment, and the prepared composite flake rare earth compound has no phenomena of agglomeration and twinning, has good dispersibility and is more uniform in diameter distribution.
Description
Technical field
The present invention relates to inorganic powder material technical field, relate in particular to a kind of preparation method of compound sheet rare earth compound.
Background technology
The principal character of flaky compound is to have less thickness and larger particle diameter.Due to its special two-dimension plane structure, make flakey compound have good sticking power, shield significantly the ability of effectiveness and reflection ray, there is good application performance in fields such as pigment, coating, plastics, automobile finish and makeup.Lamellar titanium oxide, flake aluminum oxide, platelet shaped iron oxide at present, all develop and put on market successively with the flake ferric oxide of mixing aluminium, but few to the report of rare earth flaky compound, patent only has 3, and kind and the color of rare earth flaky compound are less.Patent ZL200810003686.4 has proposed to prepare sheet-like neodymium oxide by molten-salt growth method, this sheet Neodymium trioxide has discoloration effect, under different light, presents distinct colors, under natural light, is observed red-purple, under luminescent lamp, be light blue, be pink under incandescent light.Patent ZL201210590789.1 has proposed to prepare a kind of praseodymium tabular crystal by molten-salt growth method.This praseodymium tabular crystal is black.Patent ZL201210590886.0 has proposed to prepare a kind of laminar lanthanum compound by molten-salt growth method.The almost completely free look of this laminar lanthanum compound.
Summary of the invention
The object of the invention is to provide several compound flaky rare earth compounds, increases the kind of flaky rare earth compound, changes color and the less situation of kind of rare earth flaky compound, expands the Application Areas of rare earth.
Another object of the present invention is to provide the preparation method of above-mentioned several compound flaky rare earth compounds, and the method technique is fairly simple.
The first compound sheet rare earth compound provided by the invention, it is characterized in that: lanthanum quality percentage composition is 0%～85.36%, praseodymium element quality percentage composition is 0%～85.92%, and oxygen quality percentage composition is 13.84%～24.28%, and sulphur quality percentage composition is 0～9.84%.
The first compound sheet rare earth compound is colourless to khaki color, and along with the increase of praseodymium content, color is deepened gradually, has nacreous lustre, smooth surface, is difficult for forming twin and crystal is reunited, and particle diameter is 15 μ m～50 μ m, thickness is less than 1 μ m, aspect ratio, and particle diameter/Thickness Ratio is greater than 20.
The second compound sheet rare earth compound provided by the invention, it is characterized in that: lanthanum quality percentage composition is 0%～85.36%, neodymium element quality percentage composition is 0%～86.12%, and oxygen quality percentage composition is 13.64%～24.13%, and sulphur quality percentage composition is 0～9.89%.
The second compound sheet rare earth compound is colourless to lilac, and along with the increase of neodymium content, color is deepened gradually, has nacreous lustre, smooth surface, is difficult for forming twin and crystal is reunited, and particle diameter is 10 μ m～50 μ m, thickness is less than 1 μ m, aspect ratio, and particle diameter/Thickness Ratio is greater than 20.
The third compound sheet rare earth compound provided by the invention, it is characterized in that: praseodymium quality percentage composition is 0%～85.45%, neodymium element quality percentage composition is 0%～86.16%, and oxygen quality percentage composition is 13.68%～25.02%, and sulphur quality percentage composition is 0～9.92%.
The third compound sheet rare earth compound is colourless to golden yellow, and along with the increase of praseodymium content, color is deepened gradually, has nacreous lustre, smooth surface, is difficult for forming twin and crystal is reunited, and particle diameter is 15 μ m～60 μ m, thickness is less than 1 μ m, aspect ratio, and particle diameter/Thickness Ratio is greater than 20.
The preparation method of above-mentioned several compound sheet rare earth compounds, comprise the following steps: by proportioning, rare earth soluble salt, mineralizer, phosphorus compound are dissolved in and in deionized water, obtain mixing solutions, solution is heated to 80 ℃, drip wherein the precipitation agent aqueous solution, dropwise and continue to stir half an hour, obtain a kind of suspensoid or gel, this suspensoid of evaporation drying or gel, then dried product is placed in to resistance furnace and processes 2～7 hours at 800 ℃～1400 ℃, then through washing, filtration and the dry compound sheet rare earth compound that obtains.
In the present invention, water-solubility rare-earth salt can be one or more in various water-soluble lanthanum salt, praseodymium salt, neodymium salt, and wherein, rare earth chloride and rare earth nitrate salt are first-selected.The precipitation agent aqueous solution is made by alkali, alkaline carbonate or oxalate, and its amount equates with the amount of above-mentioned water-solubility rare-earth 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 more in sodium-chlor, Repone K, potassium sulfate, sodium sulfate, ammonium sulfate, monoammonium sulfate, sodium pyrosulfate, sal enixum, and the molar weight of mineralizer should be 2-7 times of water-solubility rare-earth salt.In the present invention mineralizer and phosphorus compound can together with join rare earth salt aqueous solution, also can join together in the precipitation agent aqueous solution.
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 etc., the quality (take Vanadium Pentoxide in FLAKES) of phosphorus compound is 0～5% of rare earth compound, and phosphorus compound makes crystal form thin slice during heating fused salt is processed.
Positively effect of the present invention is as follows:
That the preparation method of compound sheet rare earth compound of the present invention has is simple, processing condition are gentle, environment is not polluted, and compound sheet rare earth compound prepared by the present invention do not reunite and twinning, favorable dispersity, and footpath is more evenly distributed.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the compound sheet rare earth compound prepared of embodiment 1.
Fig. 2 is the XRD diffractogram of the compound sheet rare earth compound prepared of embodiment 3.
Embodiment
The following examples are to describe in further detail of the present invention.
Embodiment 1
0.25mol praseodymium chloride, 0.25mol Lanthanum trichloride, 1.5mol sodium-chlor, 0.5mol sodium sulfate, 3g ten phosphate dihydrate trisodiums are dissolved in 300ml deionized water, obtain mixing solutions, heating in water bath to 80 ℃, in the situation that stirring, drip 300ml5mol/L aqueous sodium hydroxide solution, dropwise and continue to stir 30 minutes, obtain a suspensoid or colloidal sol, be evaporated to drying regime, gained solid is heated 4 hours at 1000 ℃.In the product that heat treated is crossed, add deionized water to dissolve free sodium-chlor, sodium sulfate.Leach insoluble solid, then use deionized water wash, final drying, obtains compound sheet rare earth compound thus.
Prepared compound sheet rare earth compound is khaki color, presents good pearliness, with opticmicroscope and electron microscope observation, result shows, the particle diameter of this compound sheet rare earth compound is 15～50 μ m, and thickness is about 0.4 μ m, does not reunite and twinning.When by dispersed with stirring in water time, this powder produces smooth streamline, shows favorable dispersity.
Embodiment 2:
Heating in water bath to 80 ℃, is dissolved in 0.25 mole of praseodymium chloride, 0.25 mole of Neodymium trichloride, 1 mole nacl and 1mol sodium sulfate in 300ml deionized water, obtains the mixed rare earth solution containing mineralizer.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.In the situation that stirring, mix above-mentioned two kinds of aqueous solution, mix complete continuation and stir 30 minutes, obtain a suspensoid or colloidal sol, be evaporated to drying regime, gained solid is heated 5 hours at 1100 ℃.In the product of processing to fused salt, add deionized water to dissolve free sodium-chlor, sodium sulfate.Leach insoluble solid, then use deionized water wash, final drying, obtains compound sheet rare earth compound thus.
This compound sheet rare earth compound is golden yellow, presents good nacreous lustre, with opticmicroscope and electron microscope observation, result shows, this compound sheet rare earth compound crystal particle diameter is 15～55 μ m, and thickness is 0.5 μ m, do not produce twin, there is no agglomeration yet.When by dispersed with stirring in water time, this powder produces smooth streamline.
Embodiment 3
Heating in water bath to 80 ℃, is dissolved in 0.25 mole of Lanthanum trichloride, 0.25 mole of Neodymium trichloride in 300ml deionized water, obtains mixed rare earth solution.In 200ml deionized water, dissolve 1.5 molar sodium hydroxides.In the situation that stirring, mix above-mentioned two kinds of aqueous solution, obtain a suspensoid or colloidal sol.The aqueous solution containing 1 mole nacl, 1mol sodium sulfate and 1.5 gram of ten phosphate dihydrate trisodium is joined to this suspensoid or colloidal sol, continues to stir 30 minutes,, be evaporated to drying regime, gained solid is heated 4 hours at 1200 ℃.In the product of processing to fused salt, add deionized water to dissolve free sodium-chlor, sodium sulfate.Leach insoluble solid, then use deionized water wash, final drying, obtains compound sheet rare earth compound thus.
This compound sheet rare earth compound is lilac, has good nacreous lustre, with opticmicroscope and electron microscope observation, result shows, this compound sheet rare earth compound particle diameter is 20～60 μ m, and thickness is 0.5 μ m, do not produce twin, there is no agglomeration yet.When by dispersed with stirring in water time, this powder produces smooth streamline, dispersed fine.
Embodiment 4
Heating in water bath to 85 ℃, is dissolved in 0.25 mole of praseodymium chloride and 0.25 mole of Lanthanum trichloride in 250ml deionized water, obtains the mishmetal aqueous solution.In 200ml deionized water, dissolve 1.5 molar sodium hydroxides, in the situation that stirring, mix above-mentioned two kinds of aqueous solution, mix complete continuation and stir 30 minutes, obtain a suspensoid, filtration drying, dried powder and 142 grams of sodium sulfate, 174 grams of potassium sulfate, 3 gram of ten phosphate dihydrate trisodium are placed in to ball grinder, in planetary ball mill, ball milling 4 hours, makes to mix, and gained solid is heated 5 hours at 1150 ℃.In the product that heat treated is crossed, add deionized water to dissolve free sodium-chlor.Leach insoluble solid, then use deionized water wash, final drying, obtains compound sheet rare earth compound
Result shows, the compound sheet rare earth compound particle diameter of preparation is 20～45 μ m in this way, and thickness is 0.3 μ m, favorable dispersity.Compare with enforcement experiment 1, sulfuric acid composite fused salt has better dissolving power, makes flaky compound shape more regular, and size distribution is more even.
Although illustrated and described embodiments of the invention, for the ordinary skill in the art, be appreciated that without departing from the principles and spirit of the present invention and can carry out multiple variation, modification, replacement and modification to these embodiment, scope of the present invention is limited by claims and equivalent thereof.
Claims (10)
1. the preparation method of a compound sheet rare earth compound, it is characterized in that: the concrete steps of the method are as follows: by proportioning by rare earth soluble salt, mineralizer, phosphorus compound is dissolved in and in deionized water, obtains mixing solutions, solution is heated to 80 ℃, drip wherein the precipitation agent aqueous solution, dropwise and continue to stir half an hour, obtain a kind of suspensoid or gel, this suspensoid of evaporation drying or gel, then dried product is placed in to resistance furnace processes 2～7 hours at 800 ℃～1400 ℃, again through washing, filter and the dry compound sheet rare earth compound that obtains.
2. preparation method as claimed in claim 1, is characterized in that: water-solubility rare-earth salt is one or more in various water-soluble lanthanum salt, praseodymium salt, neodymium salt.
3. preparation method as claimed in claim 1, it is characterized in that: described mineralizer is one or more in sodium-chlor, Repone K, potassium sulfate, sodium sulfate, ammonium sulfate, monoammonium sulfate, sodium pyrosulfate, sal enixum, the molar weight of mineralizer should be 2-7 times of water-solubility rare-earth salt.
4. preparation method as claimed in claim 1, is characterized in that: the described precipitation agent aqueous solution is the aqueous solution a kind of in alkali, alkaline carbonate, oxalate, and precipitation agent equates with the molar weight of rare-earth salts.
5. preparation method as claimed in claim 1, 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, and the quality of phosphorus compound is 0～5% of flaky rare earth compound.
6. preparation method as claimed in claim 1, is characterized in that: dried product is placed in resistance furnace and at 1000 ℃, processes 5 hours.
7. preparation method as claimed in claim 1, is characterized in that: dried product is placed in resistance furnace and at 1200 ℃, processes 4 hours.
8. preparation method as claimed in claim 1, it is characterized in that: prepared compound sheet rare earth compound elementary composition as follows: lanthanum element quality percentage composition is 0%～85.36%, praseodymium element quality percentage composition is 0%～85.92%, oxygen quality percentage composition is 13.84%～24.28%, and sulphur quality percentage composition is 0～9.84%; Color is colourless to khaki color, and along with the increase of praseodymium content, color is deepened gradually, and particle diameter is 15 μ m～50 μ m, and thickness is less than 1 μ m, aspect ratio, and particle diameter/Thickness Ratio is greater than 20.
9. preparation method as claimed in claim 1, it is characterized in that: prepared compound sheet rare earth compound elementary composition as follows: lanthanum element quality percentage composition is 0%～85.36%, neodymium element quality percentage composition is 0%～86.12%, oxygen quality percentage composition is 13.64%～24.13%, and sulphur quality percentage composition is 0～9.89%; Color is colourless to lilac, and along with the increase of neodymium content, color is deepened gradually, and particle diameter is 10 μ m～50 μ m, and thickness is less than 1 μ m, aspect ratio, and particle diameter/Thickness Ratio is greater than 20.
10. preparation method as claimed in claim 1, it is characterized in that: prepared compound sheet rare earth compound elementary composition as follows: praseodymium element quality percentage composition is 0%～85.45%, neodymium element quality percentage composition is 0%～86.16%, oxygen quality percentage composition is 13.68%～25.02%, and sulphur quality percentage composition is 0～9.92%; Color is colourless extremely golden yellow, and along with the increase of praseodymium content, color is deepened gradually, and particle diameter is 15 μ m～60 μ m, and thickness is less than 1 μ m, aspect ratio, and particle diameter/Thickness Ratio is greater than 20.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113800550A (en) * | 2021-10-08 | 2021-12-17 | 江西理工大学 | Flaky Gd2O2SO4And method for preparing the same |
| CN115975453A (en) * | 2023-03-07 | 2023-04-18 | 诺斯科技(天津)有限公司 | Flaky rare earth-based high-radiation heat-dissipation coating and preparation method and application thereof |
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| CN103011242A (en) * | 2012-12-31 | 2013-04-03 | 江西理工大学 | Flaky lanthanum compound and preparation method thereof |
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| CN103011242A (en) * | 2012-12-31 | 2013-04-03 | 江西理工大学 | Flaky lanthanum compound and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113800550A (en) * | 2021-10-08 | 2021-12-17 | 江西理工大学 | Flaky Gd2O2SO4And method for preparing the same |
| CN115975453A (en) * | 2023-03-07 | 2023-04-18 | 诺斯科技(天津)有限公司 | Flaky rare earth-based high-radiation heat-dissipation coating and preparation method and application thereof |
| CN115975453B (en) * | 2023-03-07 | 2023-09-08 | 诺斯科技(天津)有限公司 | Flaky rare earth-based high-radiation heat dissipation coating and preparation method and application thereof |
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