CN103803629B - A kind of preparation method of compound sheet rare earth compound - Google Patents
A kind of preparation method of compound sheet rare earth compound Download PDFInfo
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- CN103803629B CN103803629B CN201310736893.1A CN201310736893A CN103803629B CN 103803629 B CN103803629 B CN 103803629B CN 201310736893 A CN201310736893 A CN 201310736893A CN 103803629 B CN103803629 B CN 103803629B
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Abstract
The invention discloses a kind of preparation method of compound sheet rare earth compound, the concrete steps of the method are as follows: by proportioning by rare earth soluble salt, mineralizer, phosphorus compound is dissolved in deionized water and obtains mixing solutions, solution is heated to 80 DEG C, drip the precipitation agent aqueous solution wherein, 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 resistance furnace and processes 2 ~ 7 hours at 800 DEG C ~ 1400 DEG C, again through washing, filtration and drying obtain compound sheet rare earth compound.The preparation method of compound sheet rare earth compound of the present invention have simple, processing condition are gentle, do not pollute environment, and compound sheet rare earth compound prepared by the present invention is not reunited and twinning, and favorable dispersity, footpath is more evenly distributed.
Description
Technical field
The present invention relates to inorganic powder material technical field, particularly relate to a kind of preparation method of compound sheet rare earth compound.
Background technology
The principal character of flaky compound has less thickness and larger particle diameter.Due to the two-dimension plane structure that it is special, make flakey compound have the ability of good sticking power, significant shielding effectiveness and reflection ray, have good application performance in fields such as pigment, coating, plastics, automobile finish and makeup.Current lamellar titanium oxide, flake aluminum oxide, platelet shaped iron oxide, all develop with the flake ferric oxide mixing aluminium and put on market successively, 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 proposes and prepares sheet-like neodymium oxide by molten-salt growth method, this sheet Neodymium trioxide has discoloration effect, presents distinct colors under different light, under natural light, be observed red-purple, be light blue under fluorescent light, be pink under incandescent light.Patent ZL201210590789.1 proposes and prepares a kind of praseodymium tabular crystal by molten-salt growth method.This praseodymium tabular crystal is black.Patent ZL201210590886.0 proposes and prepares a kind of Flaky lanthanum compound by molten-salt growth method.The almost completely free look of this Flaky lanthanum compound.
Summary of the invention
The object of the invention is to provide several compound flaky rare earth compound, increases the kind of flaky rare earth compound, changes the color of rare earth flaky compound and the less situation of kind, 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 compound, and the method technics comparing is simple.
The first compound sheet rare earth compound provided by the invention, it is characterized in that: lanthanum mass percentage is 0% ~ 85.36%, praseodymium element mass percentage is 0% ~ 85.92%, and oxygen mass percentage is 13.84% ~ 24.28%, and sulphur mass percentage 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, not easily forms twin and crystal is reunited, and particle diameter is 15 μm ~ 50 μm, thickness is less than 1 μm, aspect ratio, and namely 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 mass percentage is 0% ~ 85.36%, neodymium element mass percentage is 0% ~ 86.12%, and oxygen mass percentage is 13.64% ~ 24.13%, and sulphur mass percentage 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, not easily forms twin and crystal is reunited, and particle diameter is 10 μm ~ 50 μm, thickness is less than 1 μm, aspect ratio, and namely 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 mass percentage is 0% ~ 85.45%, neodymium element mass percentage is 0% ~ 86.16%, and oxygen mass percentage is 13.68% ~ 25.02%, and sulphur mass percentage 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, not easily forms twin and crystal is reunited, and particle diameter is 15 μm ~ 60 μm, thickness is less than 1 μm, aspect ratio, and namely particle diameter/Thickness Ratio is greater than 20.
The preparation method of above-mentioned several compound sheet rare earth compound, comprise the following steps: by proportioning, rare earth soluble salt, mineralizer, phosphorus compound are dissolved in deionized water and obtain mixing solutions, solution is heated to 80 DEG C, drip the precipitation agent aqueous solution wherein, 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 resistance furnace and processes 2 ~ 7 hours at 800 DEG C ~ 1400 DEG C, then obtain compound sheet rare earth compound through washing, filtration and drying.
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 obtained by alkali, alkaline carbonate or oxalate, and its amount is equal 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 in the precipitation agent aqueous solution together.
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 (in Vanadium Pentoxide in FLAKES) of phosphorus compound is 0 ~ 5% of rare earth compound, and phosphorus compound makes crystal form thin slice during the process of heating fused salt.
Positively effect of the present invention is as follows:
The preparation method of compound sheet rare earth compound of the present invention have simple, processing condition are gentle, do not pollute environment, and compound sheet rare earth compound prepared by the present invention is not reunited and twinning, and favorable dispersity, footpath is more evenly distributed.
Accompanying drawing explanation
Fig. 1 is the SEM figure of compound sheet rare earth compound prepared by embodiment 1.
Fig. 2 is the XRD diffractogram of compound sheet rare earth compound prepared by embodiment 3.
Embodiment
The following examples 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 trisodium are dissolved in 300ml deionized water, obtain mixing solutions, heating in water bath to 80 DEG C, 300ml5mol/L aqueous sodium hydroxide solution is dripped when stirring, dropwise and continue stirring 30 minutes, obtain a suspensoid or colloidal sol, be evaporated to drying regime, gained solid is heated 4 hours at 1000 DEG C.Deionized water is added to dissolve free sodium-chlor, sodium sulfate in the product that heat treated is crossed.Leach insoluble solid, then use deionized water wash, final drying, obtain 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 μm, and thickness is about 0.4 μm, 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 DEG C, 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.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 5 hours at 1100 DEG C.Deionized water is added to dissolve free sodium-chlor, sodium sulfate in the product of fused salt process.Leach insoluble solid, then use deionized water wash, final drying, obtain 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 μm, and thickness is 0.5 μm, do not produce twin, also there is no agglomeration.When by dispersed with stirring in water time, this powder produces smooth streamline.
Embodiment 3
Heating in water bath to 80 DEG C, is dissolved in 0.25 mole of Lanthanum trichloride, 0.25 mole of Neodymium trichloride in 300ml deionized water, obtains mixed rare earth solution.1.5 molar sodium hydroxides are dissolved in 200ml deionized water.When stirring, mixing above-mentioned two kinds of aqueous solution, obtaining 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 this suspensoid or colloidal sol, continues stirring 30 minutes, be evaporated to drying regime, gained solid is heated 4 hours at 1200 DEG C.Deionized water is added to dissolve free sodium-chlor, sodium sulfate in the product of fused salt process.Leach insoluble solid, then use deionized water wash, final drying, obtain 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 μm, and thickness is 0.5 μm, do not produce twin, also there is no agglomeration.When by dispersed with stirring in water time, this powder produces smooth streamline, very well dispersed.
Embodiment 4
Heating in water bath to 85 DEG C, 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.1.5 molar sodium hydroxides are dissolved in 200ml deionized water, when stirring, mix above-mentioned two kinds of aqueous solution, mix complete continuation stirring 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 ball grinder, in planetary ball mill, ball milling 4 hours, makes to mix, and is heated 5 hours by gained solid at 1150 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 compound sheet rare earth compound
Result shows, the compound sheet rare earth compound particle diameter prepared in this way is 20 ~ 45 μm, and thickness is 0.3 μm, favorable dispersity.With enforcement experiment 1 compare, sulfuric acid composite fused salt has better dissolving power, makes flaky compound shape more regular, size distribution evenly.
Although illustrate and describe embodiments of the invention, for the ordinary skill in the art, be appreciated that and can carry out multiple change, amendment, replacement and modification to these embodiments without departing from the principles and spirit of the present invention, scope of the present invention is by claims and equivalents thereof.
Claims (1)
1. a preparation method for compound sheet rare earth compound, is characterized in that: the concrete steps of the method are as follows:
Heating in water bath to 85 DEG C, 0.25 mole of praseodymium chloride and 0.25 mole of Lanthanum trichloride are dissolved in 250ml deionized water, obtain the mishmetal aqueous solution, 1.5 molar sodium hydroxides are dissolved in 200ml deionized water, when stirring, mix above-mentioned two kinds of aqueous solution, mix complete continuation stirring 30 minutes, obtain a suspensoid, filtration drying, by dried powder and 142 grams of sodium sulfate, 174 grams of potassium sulfate, 3 gram of ten phosphate dihydrate trisodium is placed in ball grinder, ball milling 4 hours in planetary ball mill, make to mix, gained solid is heated 5 hours at 1150 DEG C, deionized water is added to dissolve free sodium-chlor in the product that heat treated is crossed, leach insoluble solid, use deionized water wash again, final drying, obtain compound sheet rare earth compound.
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