CN1907858A - Process for preparing rare earth phosphate - Google Patents
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- CN1907858A CN1907858A CNA2005100889558A CN200510088955A CN1907858A CN 1907858 A CN1907858 A CN 1907858A CN A2005100889558 A CNA2005100889558 A CN A2005100889558A CN 200510088955 A CN200510088955 A CN 200510088955A CN 1907858 A CN1907858 A CN 1907858A
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Abstract
A preparation method for rare earth phosphate comprises stirring raw materials at a ammonium hydrogen phosphate/rare earth ion ratio of 1.0-4.0, adding rare earth inorganic solution (containing rare earth oxide 5 g/L-300 g/L) and 0.1 mol/L-2 mol/L phospahte into 0.01 mol/L-2 mol/L phosphoric acid respectively and controlling the concentration of phosphoric acid to obtain rare earth phosphate with uniform particle size which would increase with increasing of phosphoric acid concentration, aging, filtering the obtained rare earth phosphate, washing and drying, and torrefying at 200-1300DEG C for 1-15 h. This invention can prepare rare earth phosphate with good dispersity and no need for pulverization, and can accurately control the granularity of products in a certain range.
Description
Technical field
The present invention relates to a kind of process for preparing rare earth phosphate, relate in particular to a kind of RE phosphate preparation method that can in technological process, control product granularity simply.
Background technology
RE phosphate, general formula are REPO
4It is a kind of additive of widespread use in the industrial production, for example, RE phosphate can directly be situated between as halogenated aromatic gas phase water and make the catalyzer of phenol, or as the new and effective solidifying agent of building coating, splendid especially for effect in the inorganic composite serial building coating of water glass, the lanthanum orthophosphate particulate can be used in the lithium soap grease, can improve its lubricity greatly; Cerium monophosphate then can be used as the effective additive that improves the oxide ceramics processing characteristics, and is widely used in electronic industry.And some compound rare-earth phosphoric acid salt are fluorescence luminescent materials of widespread use, and wherein most representative is lanthanum-cerium-terbium phosphate green emitting phosphor, and its molecular formula is (La, Ce, Tb) PO
4Be a kind of efficient green fluorescent material that is widely used in purposes such as rare-earth trichromatic luminescent lamp, be called for short LAP, compare with aluminate green powder (CAT) commonly used, have advantages such as luminosity height, synthesis temperature is moderate, chromaticity coordinates X value is bigger, be the qualified product that replace CAT, become the focus of rare earth material chemical field research at present.
Usually, adopt the high temperature solid-state synthesis technique to make RE phosphate, it is characterized in that, with corresponding rare earth oxide and Secondary ammonium phosphate is raw material, synthetic under the high temperature more than 1000 ℃, the defective of this technology is: at high temperature easily produce phosphorus oxide evaporation, make the rare earth element in the product and the ratio of phosphate radical accurately to control; The calcination temperature height, energy consumption is big; Synthetic product is mixed with dephasign and granularity is bigger than normal.Therefore, present research work mainly concentrates on the exploitation of wet method synthesizing rare-earth phosphating processes.But the synthetic problem that often runs into of wet method is that the rare-earth phosphorate that generates often is gel state, and sedimentation function and strainability are poor, very easily harden behind the sintering, are difficult to handle.In addition, in the actual production, also wish to prepare as required the RE phosphate of different-grain diameter, therefore, wish to obtain a kind of preparation method that can control the rare-earth phosphorate powder size, and make good dispersity, easy-to-handle RE phosphate.
In the flat 6-247711 of Japanese Patent TOHKEMY, at first the rare earth nitrate solution for preparing is heated to 80 ℃, under stirring, intensive directly adds solid phosphoric acid hydrogen two ammoniums then, continue to stir and add ammoniacal liquor down, regulate pH to neutral, gained lanthanum-cerium-terbium phosphate particle is a spherical particle, and size distribution is sharp normal distribution.
In the flat 9-296168 of Japanese Patent TOHKEMY, adopt the cocurrent adding material method, rare earth nitrate solution is added drop-wise in the acidic solution with ammonium dibasic phosphate solution, and in reaction process, all the time the pH value is controlled at less than in 3 the scope, obtain the lanthanum-cerium-terbium phosphate powder of small grain size.
In Chinese patent CN1487050, the rare earth nitrate solution and the ammonium dibasic phosphate solution that configure are added drop-wise in the citric acid solution, behind reinforced the end, at 40～60 ℃ of following ageing 1-24 hours, add polyvinyl alcohol or polyglycol solution again, filter collecting precipitation, gained particle median particle (D50) is 3～6 microns, is evenly distributed.
The defective of above method need to be the high temperature ageing process of long period, complex process, and can't make things convenient for as required and accurately control the granularity of product.
Summary of the invention
The object of the present invention is to provide a kind of process for preparing rare earth phosphate,, can control the granularity of RE phosphate product simply by this preparation method, and good product dispersibility, can directly use, need not milled processed.
For achieving the above object, the present invention is by the following technical solutions: a kind of process for preparing rare earth phosphate, it comprises: under agitation, the mol ratio of pressing Secondary ammonium phosphate/rare earth ion is between 1.0 to 4.0, with total amount of the rare earth oxide 5 grams per liters to the inorganic salt of rare earth solution between 300 grams per liters and concentration 0.1 mol to the ammonium dibasic phosphate solution between 2 mol join simultaneously respectively phosphoric acid concentration in 0.01 mol in the phosphate aqueous solution between 2 mol, and the method for passing through control phosphate aqueous solution concentration is controlled the median size of the RE phosphate that generates, improve phosphate aqueous solution concentration, its corresponding RE phosphate median size strengthens; Behind reinforced the end, ageing; With RE phosphate filtration, washing, the drying that generates; And the roasting temperature between 200 ℃ to 1300 ℃ 1 to 15 hour.
Among the present invention, continuing to join a certain proportion of inorganic salt of rare earth solution and ammonium dibasic phosphate solution in the aqueous solution of phosphoric acid respectively simultaneously under the state that stirs; Behind reinforced the finishing, throw out is filtered, and washing, drying; Dried filter cake 200 to 1300 ℃ roasting temperature 1 to 15 hour, is cooled to room temperature, RE phosphate that can certain particle size; By changing the concentration of phosphate aqueous solution, measure the RE phosphate granularity of gained, and the graph of a relation of curve of grain size and phosphoric acid concentration, according to graph of a relation, phosphoric acid concentration when determining the RE phosphate of preparation desired particle size, prepare phosphate aqueous solution according to this concentration conditions, and prepare the RE phosphate of desired particle size according to abovementioned steps.
In the present invention, RE phosphate is preferably lanthanum orthophosphate, Cerium monophosphate and phosphoric acid terbium, and the compound rare-earth phosphoric acid salt that contains any two or more rare earth element in lanthanum, cerium, the terbium, and the compound rare-earth phosphoric acid salt that contains lanthanum, cerium, three kinds of rare earth elements of terbium simultaneously.Wherein, lanthanum cerium terbium composite phosphate is the fluorescent material in a kind of manufacturing that is widely used in three-color fluorescent lamp, and the ratio between lanthanum, cerium and the terbium is that those skilled in the art are known.
In the present invention, the aqueous solution of phosphoric acid (end water), its concentration at 0.01M between the 2M, preferably in 0.02 mol between 0.5 mol, more preferably in 0.05 mol between 0.1 mol.The volume of end water is between 0.2 to 10 times of rare earth nitrate solution, preferably between 2 to 5 times.
The present inventor finds, under the constant situation of other processing condition, the granularity of gained RE phosphate increases and increases gradually along with concentration of phosphoric acid in the end water, therefore, can be by adjusting phosphate aqueous solution concentration as end water, the granularity of RE phosphate product is controlled in the desired scope.For example, in actual production, those skilled in the art can be by the serial experiment of simplicity of design, promptly change phosphate aqueous solution concentration, and the granularity of product measured, concentration of phosphoric acid in the end water as the x value, as the y value, is drawn the graph of a relation of product granularity to phosphoric acid concentration with the particle size results measured.When the granularity to product proposes necessarily to require, on the x of this graph of a relation axle, find this granularity, and find corresponding phosphoric acid concentration value according to graph of a relation, according to this phosphoric acid concentration configuration end water, the granularity of RE phosphate product can be controlled in the desirable scope.In addition, in the present invention, the concentration of other processing condition such as rare earth nitrate and Secondary ammonium phosphate, feed rate etc. also have certain influence to the granularity of reaction product, and this it is known to those skilled in the art that.Therefore, carry out serial experiment or when producing, other processing condition should be determined constantly, thus can be simply control the granularity of phosphate product by regulating concentration of phosphoric acid in the end water, this is especially favourable in industrial production.In addition, have excessive phosphate anion or phosphoric acid in reaction system, can assist to improve the rate that settles out of rare earth, in the present invention, the yield of RE phosphate is all more than 99%.Can be by method of the present invention, in the granularity of 0.5 micron to 30 microns scope inner control RE phosphate product.
Employed inorganic salt of rare earth solution is preferably the nitrate or the chloride soln of rare earth, more preferably rare earth nitrate solution among the present invention.The concentration of inorganic salt of rare earth solution is that every liter of solution contains the rare earth oxide of 5 grams to 300 grams, preferably contains the rare earth oxide of 25 grams to 100 grams.The metering method of this concentration is as well known to those skilled in the art.
Adopt Secondary ammonium phosphate as precipitation agent among the present invention, Secondary ammonium phosphate is soluble in water, make ammonium dibasic phosphate aqueous solution, its concentration is between 0.5 to 1.5 mol, the amount of used Secondary ammonium phosphate, the mol ratio that should control Secondary ammonium phosphate and rare earth ion is between 1.0 to 4.0, preferably between 1.5 to 2.5.
Above-mentioned inorganic salt of rare earth solution and ammonium dibasic phosphate solution are fed to respectively at the bottom of the phosphoric acid that is under the whipped state in the water simultaneously, generate white precipitate, reinforced finishing, preferably under suitable temperature with slurry ageing for some time, wherein, the ageing temperature is between 30 ℃ to 100 ℃, preferably between 70 ℃ to 90 ℃, digestion time is between 1 to 10 hour, preferably between 2 to 8 hours.
After aging step finishes, throw out is filtered, washing, drying was placed on dried filter cake in the crucible, 200 to 1300 ℃ roasting temperatures 1 to 15 hour.Preferably between 700-1000 ℃, calcination time is preferably between 2-8 hour for maturing temperature.Can make the RE phosphate powder of desired particle size after the cooling.Can adopt in the present invention that the known routine techniques of those skilled in the art feeds in raw material, filters, washs, drying and roasting.
The invention has the advantages that, technology and equipment are simple, be easy to realize, reaction conditions gentleness, sedimentation and filtration good dispersion property, product need not to grind broken and screening, can directly use, can control the granularity of product as requested, and particle size distribution is narrow, wherein the composite phosphate of lanthanum, cerium, terbium has good fluorescence property.
Description of drawings
The graph of a relation (embodiment 1) of phosphoric acid concentration and lanthanum orthophosphate granularity in the water at the bottom of Fig. 1
The graph of a relation (embodiment 2) of phosphoric acid concentration and lanthanum orthophosphate granularity in the water at the bottom of Fig. 2
The graph of a relation (embodiment 3) of phosphoric acid concentration and Cerium monophosphate granularity in the water at the bottom of Fig. 3
The graph of a relation (embodiment 4) of phosphoric acid concentration and phosphoric acid terbium granularity in the water at the bottom of Fig. 4
The graph of a relation (embodiment 5) of phosphoric acid concentration and samaric orthophosphate granularity in the water at the bottom of Fig. 5
The graph of a relation (embodiment 6) of phosphoric acid concentration and lanthanum-cerium-terbium phosphate granularity in the water at the bottom of Fig. 6
Among Fig. 1, X-coordinate is a concentration of phosphoric acid in the end water, and unit is a mol, and ordinate zou is the median particle D of lanthanum orthophosphate
50, unit is a micron.Among Fig. 2, X-coordinate is a concentration of phosphoric acid in the end water, and unit is a mol, and ordinate zou is the median particle D of lanthanum orthophosphate
50, unit is a micron.Among Fig. 3, X-coordinate is a concentration of phosphoric acid in the end water, and unit is a mol, and ordinate zou is the median particle D of Cerium monophosphate
50, unit is a micron., among Fig. 4, X-coordinate is a concentration of phosphoric acid in the end water, and unit is a mol, and ordinate zou is the median particle D of phosphoric acid terbium
50, unit is a micron.
Among Fig. 5, X-coordinate is a concentration of phosphoric acid in the end water, and unit is a mol, and ordinate zou is the D of samaric orthophosphate
50Granularity, unit is a micron.Among Fig. 6, X-coordinate is a concentration of phosphoric acid in the end water, and unit is a mol, and ordinate zou is the median particle D of lanthanum-cerium-terbium phosphate
50, unit is a micron.
Embodiment
Following embodiment only is used to elaborate the present invention, rather than scope of the present invention is done any qualification.
Embodiment 1
200 milliliters of the lanthanum nitrate hexahydrates of preparation rare earth oxide content 50 grams per liters, and 200 milliliters of the ammonium dibasic phosphate solutions of 0.5 mol, under agitation with two kinds of solution cocurrent adding materials to end water, end water is respectively 1000 milliliters of the phosphate aqueous solutions of 0.04,0.08,0.16,0.32 and 0.64 mol, and the feed rate of lanthanum nitrate hexahydrate and ammonium dibasic phosphate solution is 20 ml/min.Behind reinforced the end, 80 ℃ of following ageings 2 hours, the white precipitate that generates is filtered, and filter cake is placed on filter cake in the crucible with 20 milliliters deionized water drip washing 3 times, in retort furnace, be heated to 600 ℃, be incubated 4 hours, be cooled to room temperature, obtain white lanthanum orthophosphate powder, test its granularity with laser particle analyzer, the result is shown in the table 1.
Table 1
| Phosphoric acid concentration mol/L in the end water | Product median particle D 50(μm) |
| 0.04 | 2.5 |
| 0.08 | 4.6 |
| 0.16 | 8.4 |
| 0.32 | 12.6 |
| 0.64 | 18.3 |
The graph of a relation of phosphoric acid solution concentration and lanthanum orthophosphate granularity is seen accompanying drawing 1, and as seen from Figure 1, with the raising of phosphoric acid concentration in the end water, the lanthanum orthophosphate granularity improves thereupon.
According to Fig. 1, desire prepares the lanthanum orthophosphate of median size about 5 microns, checks in Fig. 1, and corresponding phosphoric acid concentration is about 0.09 mol.Experimentize according to aforementioned condition, but end water is 1000 milliliters of the phosphate aqueous solutions of 0.09 mol, makes white lanthanum orthophosphate powder that measuring its median size is 5.1 microns.
100 milliliters of the lanthanum nitrate hexahydrates of preparation rare earth oxide content 50 grams per liters, and 100 milliliters of the ammonium dibasic phosphate solutions of 0.5 mol, under agitation with two kinds of solution cocurrent adding materials to end water, end water is respectively 50 milliliters of the phosphate aqueous solutions of 0.01,0.02,0.04,0.08 and 0.16 mol, and the feed rate of lanthanum nitrate hexahydrate and ammonium dibasic phosphate solution is 10 ml/min.Behind reinforced the end, 30 ℃ of following ageings 6 hours, the white precipitate that generates is filtered, and filter cake is placed on filter cake in the crucible with 20 milliliters deionized water drip washing 3 times, in retort furnace, be heated to 400 ℃, be incubated 4 hours, be cooled to room temperature, obtain white lanthanum orthophosphate powder, test its granularity with laser particle analyzer, the result is shown in the table 2.
Table 2
| Phosphoric acid concentration mol/L in the end water | Lanthanum orthophosphate median particle D 50(μm) |
| 0.01 | 0.53 |
| 0.02 | 0.94 |
| 0.04 | 1.9 |
| 0.08 | 4.4 |
| 0.16 | 8.0 |
The graph of a relation of phosphoric acid solution concentration and lanthanum orthophosphate granularity is seen accompanying drawing 2, and as seen from Figure 2, with the raising of phosphoric acid concentration in the end water, the lanthanum orthophosphate granularity improves thereupon.
According to Fig. 2, desire prepares the lanthanum orthophosphate of median particle about 1 micron, obtains corresponding phosphoric acid concentration and be about 0.022M in Fig. 2.Experimentize according to aforementioned condition, but end water is 50 milliliters of the phosphate aqueous solutions of 0.022M, makes the lanthanum orthophosphate powder that measuring its granularity is 1.04 microns.
Embodiment 3
400 milliliters of the cerous nitrate solutions of preparation rare earth oxide content 80 grams per liters, and 400 milliliters of the ammonium dibasic phosphate solutions of 1.2 mol, under agitation with two kinds of solution cocurrent adding materials to end water, end water is respectively 100 milliliters of the phosphate aqueous solutions of 0.12,0.24,0.5,1.0 and 2.0 mol, and the feed rate of cerous nitrate solution and ammonium dibasic phosphate solution is 50 ml/min.Behind reinforced the end, 80 ℃ of following ageings 10 hours, the white precipitate that generates is filtered, and filter cake is placed on filter cake in the crucible with 50 milliliters deionized water drip washing 3 times, in retort furnace, be heated to 700 ℃, be incubated 4 hours, be cooled to room temperature, obtain the Cerium monophosphate powder of white light yellow complexion, test its granularity with laser particle analyzer, the result is shown in the table 3.
Table 3
| Phosphoric acid concentration mol/L in the end water | Cerium monophosphate median particle D 50(μm) |
| 0.12 | 5.5 |
| 0.24 | 9.9 |
| 0.5 | 14.8 |
| 1.0 | 20.8 |
| 2.0 | 29.3 |
The graph of a relation of phosphoric acid solution concentration and Cerium monophosphate granularity is seen accompanying drawing 3, and as seen from Figure 3, with the raising of phosphoric acid concentration in the end water, the Cerium monophosphate granularity improves thereupon.
According to Fig. 3, desire prepares the Cerium monophosphate of median particle about 25 microns, obtains corresponding phosphoric acid concentration and be about 1.5M in Fig. 3.Experimentize according to aforementioned condition, but end water is 100 milliliters of the phosphate aqueous solutions of 1.5M, makes the Cerium monophosphate powder that measuring its granularity is 26.1 microns.
2000 milliliters of the Terbium trinitrate solution of preparation rare earth oxide content 50 grams per liters, and 1000 milliliters of the ammonium dibasic phosphate solutions of 1 mol, under agitation with two kinds of solution cocurrent adding materials to end water, end water is respectively 5000 milliliters of the phosphate aqueous solutions of 0.05,0.10,0.20,0.50 and 1.0 mol, and the feed rate of Terbium trinitrate solution and ammonium dibasic phosphate solution is 200 ml/min.Behind reinforced the end, 90 ℃ of following ageings 5 hours, the white precipitate that generates is filtered, and filter cake is placed on filter cake in the crucible with 50 milliliters deionized water drip washing 3 times, in retort furnace, be heated to 500 ℃, be incubated 8 hours, be cooled to room temperature, obtain the phosphoric acid terbium powder of white, test its granularity with laser particle analyzer, the result is shown in the table 4.
Table 4
| Phosphoric acid concentration mol/L in the end water | Phosphoric acid terbium median particle D 50(μm) |
| 0.05 | 2.7 |
| 0.10 | 4.6 |
| 0.20 | 7.7 |
| 0.50 | 17.8 |
| 1.0 | 24.3 |
The graph of a relation of phosphoric acid solution concentration and phosphoric acid terbium granularity is seen accompanying drawing 4, and as seen from Figure 4, with the raising of phosphoric acid concentration in the end water, phosphoric acid terbium granularity improves thereupon.
Embodiment 5
1000 milliliters of the samarium nitrate solutions of preparation rare earth oxide content 75 grams per liters, and 1000 milliliters of the ammonium dibasic phosphate solutions of 1 mol, under agitation with two kinds of solution cocurrent adding materials to end water, end water is respectively 1000 milliliters of the phosphate aqueous solutions of 0.01,0.02,0.05,0.10 and 0.20 mol, and the feed rate of samarium nitrate solution and ammonium dibasic phosphate solution is 100 ml/min.Behind reinforced the end, 30 ℃ of following ageings 10 hours, the white precipitate that generates is filtered, and filter cake is placed on filter cake in the crucible with 20 milliliters deionized water drip washing 3 times, in retort furnace, be heated to 900 ℃, be incubated 4 hours, be cooled to room temperature, obtain the samaric orthophosphate powder of white, test its granularity with laser particle analyzer, the result is shown in the table 5.
Table 5
| Phosphoric acid concentration mol/L in the end water | Samaric orthophosphate median particle D 50(μm) |
| 0.01 | 0.73 |
| 0.02 | 1.7 |
| 0.05 | 3.5 |
| 0.10 | 5.6 |
| 0.20 | 8.4 |
The graph of a relation of phosphoric acid solution concentration and samaric orthophosphate granularity is seen accompanying drawing 5, and as seen from Figure 5, with the raising of phosphoric acid concentration in the end water, the samaric orthophosphate granularity improves thereupon.
According to stoichiometric ratio configuration rare earth oxide total concn is 200 milliliters of lanthanum, cerium, the terbium nitrate mixed solutions of 100 grams per liters, concentration is 200 milliliters of the ammonium dibasic phosphate aqueous solutions of 1.5 mol, under agitation two kinds of solution and stream being added to concentration is respectively in 1000 milliliters of the phosphate aqueous solutions of 0.10,0.20,0.30,0.40,0.50 and 0.60 mol, the control feed rate can add two kinds of solution simultaneously at 10 minutes.After dropwising,, the white precipitate that generates is filtered 70 ℃ of following ageings 4 hours, with 50 ml water drip washing 3 times, filter cake is placed in the crucible, is warming up to 1000 ℃, and be incubated 2 hours down at 1000 ℃, be cooled to room temperature, obtain the lanthanum-cerium-terbium phosphate powder of white, measure its granularity, test result sees Table 6, draw the graph of a relation of phosphoric acid concentration and lanthanum-cerium-terbium phosphate granularity according to test result, see accompanying drawing 6.
Table 6
| Phosphoric acid concentration mol/L in the end water | Lanthanum-cerium-terbium phosphate median particle D 50(μm) |
| 0.05 | 3.2 |
| 0.1 | 5.1 |
| 0.2 | 9.2 |
| 0.35 | 13.1 |
| 0.5 | 16.4 |
As seen from Figure 6, with the raising of phosphoric acid concentration in the end water, the granularity of lanthanum-cerium-terbium phosphate improves thereupon.
According to Fig. 6, desire prepares the lanthanum-cerium-terbium phosphate of median particle about 8 microns, obtains corresponding phosphoric acid concentration and be about 0.17M in Fig. 6.Experimentize according to aforementioned condition, but end water is 1000 milliliters of the phosphate aqueous solutions of 0.17M, makes the lanthanum-cerium-terbium phosphate powder that measuring its granularity is 8.2 microns.
Claims (12)
1, a kind of process for preparing rare earth phosphate, it is characterized in that: under agitation, the mol ratio of pressing Secondary ammonium phosphate/rare earth ion is between 1.0 to 4.0, with total amount of the rare earth oxide 5 grams per liters to the inorganic salt of rare earth solution between 300 grams per liters and concentration 0.1 mol to the ammonium dibasic phosphate solution between 2 mol join simultaneously respectively phosphoric acid concentration in 0.01 mol in the phosphate aqueous solution between 2 mol, and the method for passing through control phosphate aqueous solution concentration is controlled the median size of the RE phosphate that generates, improve phosphate aqueous solution concentration, its corresponding RE phosphate median size strengthens; Behind reinforced the end, ageing; With RE phosphate filtration, washing, the drying that generates; And the roasting temperature between 200 ℃ to 1300 ℃ 1 to 15 hour.
2, process for preparing rare earth phosphate according to claim 1 is characterized in that: inorganic salt of rare earth solution is single rare earth element or two or more rare earth element blended nitrate solution or rare-earth chloride solution.
3, process for preparing rare earth phosphate according to claim 1, it is characterized in that the method for controlling the phosphate product granularity more specifically is: under the situation that all the other processing condition remain unchanged, regulate the concentration of phosphate aqueous solution, and the granularity of the RE phosphate of measurement generation, corresponding relation according to concentration and granularity is drawn concentration-granulometry curve, and try to achieve the phosphoric acid solution concentration value corresponding with desired particle size according to typical curve, adopt the phosphate aqueous solution of this concentration value, control the granularity of RE phosphate product thus.
4, process for preparing rare earth phosphate according to claim 1 and 2 is characterized in that: described method, the median particle of the RE phosphate that control generates by control phosphate aqueous solution concentration at 0.5 micron in 30 micrometer ranges.
5, process for preparing rare earth phosphate according to claim 1 and 2, it is characterized in that: the total amount of inorganic salt of rare earth solution middle-weight rare earths oxide compound at 25 grams per liters between 100 grams per liters, the concentration of ammonium dibasic phosphate aqueous solution in 0.5 mol between 1.5 mol.
6, according to claim 1 or 2 described process for preparing rare earth phosphate, it is characterized in that: the mol ratio of described Secondary ammonium phosphate/rare earth ion is between 1.5 to 2.5.
7, process for preparing rare earth phosphate according to claim 1 and 2 is characterized in that: the concentration of described phosphate aqueous solution preferably in 0.02 mol between 0.5 mol.
8, process for preparing rare earth phosphate according to claim 7 is characterized in that: the concentration of described phosphate aqueous solution preferably in 0.05 mol between 0.1 mol.
9, process for preparing rare earth phosphate according to claim 1 and 2 is characterized in that: behind reinforced finishing, with reaction mixture ageing 1 to 10 hour under 30 ℃ to 100 ℃ temperature.
10, process for preparing rare earth phosphate according to claim 9 is characterized in that: behind reinforced finishing, with reaction mixture ageing 2 to 8 hours under 70 ℃ to 90 ℃ temperature.
11, process for preparing rare earth phosphate according to claim 1 and 2 is characterized in that: preferably between 700 ℃ to 1000 ℃, roasting time is preferably between 2 to 8 hours for described sedimentary maturing temperature.
12, process for preparing rare earth phosphate according to claim 1 and 2 is characterized in that: described rare earth oxide is lanthanum trioxide or cerium oxide or terbium sesquioxide or by the composite oxides of lanthanum trioxide, cerium oxide, terbium sesquioxide combination.
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|---|---|---|---|---|
| JPH06247711A (en) * | 1993-02-22 | 1994-09-06 | Shin Etsu Chem Co Ltd | Spherical particles of phosphate of rare earth element and their production |
| JP4219514B2 (en) * | 1999-12-16 | 2009-02-04 | 化成オプトニクス株式会社 | Rare earth phosphate manufacturing method, rare earth phosphate phosphor, and rare earth phosphate phosphor manufacturing method |
| CN1487050A (en) * | 2003-08-13 | 2004-04-07 | 华东理工大学 | Green phosphor of spherical RE phosphate and its prepn |
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| CN101402854B (en) * | 2008-11-05 | 2012-05-23 | 江门市科恒实业股份有限公司 | Method of producing coating material applied to improve thermostability of lanthanum-cerium-terbium phosphate green emitting phosphor |
| CN101781563B (en) * | 2009-01-16 | 2012-10-24 | 北京林业大学 | Nanometer fluorescence material with nuclear shell structure and preparation method thereof |
| CN101899305A (en) * | 2009-05-26 | 2010-12-01 | 北京化工大学 | Method for preparing rare earth ion-doped CePO4 microspheres |
| CN101575514B (en) * | 2009-05-26 | 2012-10-24 | 上海应用技术学院 | Mesoporous rare earth phosphate fluophor and preparation method thereof |
| CN101899305B (en) * | 2009-05-26 | 2014-07-23 | 北京化工大学 | Method for preparing rare earth ion-doped CePO4 microspheres |
| CN106315536A (en) * | 2016-11-24 | 2017-01-11 | 淄博包钢灵芝稀土高科技股份有限公司 | Method for preparing rare-earth phosphorate |
| CN107663423A (en) * | 2017-09-28 | 2018-02-06 | 东莞市赛亚稀土实业有限公司 | A kind of preparation method of cerium rouge |
| CN111683749A (en) * | 2018-02-21 | 2020-09-18 | 萨索尔德国有限公司 | Rare earth phosphate alumina composite material for emission control catalyst and preparation method thereof |
| CN111573645A (en) * | 2020-06-18 | 2020-08-25 | 南昌航空大学 | Method for preparing lanthanum phosphate three-dimensional nanoparticles |
| CN112624078A (en) * | 2020-12-24 | 2021-04-09 | 益阳鸿源稀土有限责任公司 | Preparation method of high-purity nano lanthanum phosphate powder |
| CN112624078B (en) * | 2020-12-24 | 2023-05-16 | 益阳鸿源稀土有限责任公司 | Preparation method of high-purity nano lanthanum phosphate powder |
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