CN103626195B - Method for preparing Na3YSi2O7 - Google Patents
Method for preparing Na3YSi2O7 Download PDFInfo
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- CN103626195B CN103626195B CN201310615662.5A CN201310615662A CN103626195B CN 103626195 B CN103626195 B CN 103626195B CN 201310615662 A CN201310615662 A CN 201310615662A CN 103626195 B CN103626195 B CN 103626195B
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- silicate minerals
- natural silicate
- lipid acid
- deionized water
- dissolved
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Abstract
The invention relates to a method for preparing Na3YSi2O7, and particularly relates to a method for preparing Na3YSi2O7 by using natural silicate minerals as a raw material. According to the method, the natural silicate minerals are firstly taken as the raw material for preparing Na3YSi2O7 and are cheap and easily available; the method is simple and consumes less energy. The method adopts a precipitation method and comprises steps of firstly dissolving soluble yttrium salt into aqueous solution containing fatty acid, introducing sodium carbonate so as to generate precipitate, then adding the natural silicate minerals dispersed in fatty acid-absolute ethyl alcohol through ultrasonic, after stirring in water bath, centrifuging and washing so as to obtain a precursor, drying in an oven for one night, finally calcining in air atmosphere so as to obtain the product.
Description
Technical field
The invention discloses one and prepare Na
3ySi
2o
7method, particularly relating to a kind of is that Na prepared by raw material with natural silicate minerals
3ySi
2o
7method, belong to technical field of inorganic material.
Background technology
Na
3ySi
2o
7substrate material as the ion-activated fluorescent material of novel rare-earth has been widely used in the field such as luminescent lamp, white light-emitting diode.Current synthesis Na
3ySi
2o
7method have two kinds.One first makes colloidal sol with yttrium nitrate, saliter hydrochlorate, tetraethoxy for raw material, and colloidal sol is at room temperature placed and become gel in 2 ~ 3 days, gel prior to 500 DEG C of calcining 4h again in reducing atmosphere 950 DEG C of calcining 8h to obtain product.Another kind method is with yttrium oxide, silicon-dioxide, sodium carbonate for raw material, through mechanically mixing again in air atmosphere more than 1200 DEG C calcine 6-10h.First method is prepared gelation process and is needed regulator solution pH, and calcination process needs reducing atmosphere, and not only complicated operation requires also high to calcination condition.Second method uses mechanically mixing, needs to reach presoma melt temperature and just can react, thus need high temperature and longer calcination time.Not only energy consumption is high for above-mentioned two kinds of methods, and the raw material used is all chemical reagent, and cost is relatively high.
Summary of the invention
The object of the present invention is to provide a kind of completely newly, be better than prior art with natural silicate minerals be raw material, the simple Na of preparation technology
3ySi
2o
7preparation method.
Concrete technical scheme:
One prepares Na
3ySi
2o
7method, first soluble yttrium salt is dissolved in the deionized water of fatty acids, then drips sodium carbonate solution wherein, obtain mixed system; Then being dispersed in by natural silicate minerals after in the dehydrated alcohol being dissolved with lipid acid joins in above-mentioned mixed system, and through stirring, centrifuge washing, dries, obtain Na after calcining
3ySi
2o
7.
In the deionized water of fatty acids, the volume ratio of lipid acid and deionized water is 1:20-1:100.
Described natural silicate minerals is preferably the silicate minerals that dioxide-containing silica is greater than 50%.
One prepares Na
3ySi
2o
7method, specifically comprise the steps:
The first step: get soluble yttrium salt and be dissolved in the deionized water of fatty acids, preparation yttrium concentration be 10-50mmol/L containing ruthenium ion solution, wherein the volume ratio of lipid acid and deionized water is 1:20-1:100;
Wherein, lipid acid and deionized water volume ratio, too high, be unfavorable for the dissolving of soluble salt, too low, do not have the effect of dispersion;
Second step: the sodium carbonate solution prepared is dropped to the first step gained containing in ruthenium ion solution, obtain mixed system, wherein the mol ratio of sodium and yttrium is 10:1-20:1;
3rd step: by natural silicate minerals ultrasonic disperse in the dehydrated alcohol being dissolved with lipid acid, wherein dehydrated alcohol and lipid acid volume ratio are 20:1-40:1, and natural silicate minerals is 1:50-1:100 with the mass ratio of the dehydrated alcohol being dissolved with lipid acid;
4th step: natural silicate minerals scattered for the 3rd step is joined in second step gained mixed system, centrifuge washing after stirring under the constant temperature of 20-60 DEG C, at 40-80 DEG C, dry in baking oven, then calcine in the temperature range of 600-800 DEG C under air atmosphere, obtain Na
3ySi
2o
7, the mass ratio containing ruthenium ion solution in described natural silicate minerals and the first step is 1:100-1:400.
Any one preferably in nitrate, chlorate or soluble organic salts of soluble yttrium salt.
Any one preferably in oleic acid, linolic acid, linolenic acid of described lipid acid.
Described concentration of sodium carbonate is preferably 0.2-1.5mol/L.
In 4th step, the time of stirring under the constant temperature of 20-60 DEG C is 6-12h, and during centrifuge washing, rotating speed is 9000-12000rpm, and the time dry in baking oven is 6-12h.
The rate of heating of calcination process is preferably 5-10 DEG C/min, and calcination time is preferably 1-3 hour.
Wherein, natural silicate minerals be natural, without the silicate minerals of any modification, described natural silicate minerals comprises attapulgite, sepiolite, diatomite etc.
In the first step of the present invention, lipid acid dispersion can be formed water-oil systems in deionized water, be beneficial to the dispersion of various ion, also be beneficial to the more complete crystal formation of product formation simultaneously.
In the present invention the 3rd step, planar water is generally all contained in natural silicate minerals surface, these water can be taken away mineral surface by dissolving each other by ethanol effectively, and then lipid acid can be made to be coated on mineral surface, and so such as the positively charged ion such as Y, Na just adheres to each other by lipid acid and mineral.
Principal reaction equation has:
SiO
2+Na
2CO
3→Na
2SiO
3
Y(NO
3)
3+Na
2CO
3→NaY(CO
3)
2
SiO
2+Na
2SiO
3+NaY(CO
3)
2→Na
3YSi
2O
7
Beneficial effect of the present invention
The present invention uses natural silicate minerals to prepare Na as silicon source first
3ySi
2o
7, cheaper starting materials is easy to get and without the need to carrying out any pre-treatment, from having saved cost to a great extent, improves the added value of silicate minerals simultaneously.And in preparation process of the present invention, whole reaction system is liquid-phase system, make each component mix precursor that is more even, that generate and be easy to decompose and temperature of reaction is reduced greatly, energy consumption greatly reduces.Concrete, in preparation process, first choose natural silicate minerals as silicon source, it not only saves the cost of raw material, and natural silicate minerals has abundant pore passage structure and large specific surface area, and more easily discharge silicon by alkaline environment process of the present invention, and then be Na
3ySi
2o
7synthesis silicon source is provided, the present invention further advantage treatment step is also, in the first step, lipid acid dispersion can be formed water-oil systems in deionized water, particularly pass through the volume ratio of conservative control lipid acid and deionized water, be beneficial to dissolving and the dispersion of soluble yttrium salt, be also beneficial to subsequent product simultaneously and form more complete crystal formation; In second step, what sodium carbonate played is dual function, and it, not only as the precipitation agent of ruthenium ion, also serves the effect of dissolve silicates mineral; In 3rd step, planar water is generally all contained in natural silicate minerals surface, these water effectively can be taken away mineral surface by dissolving each other by ethanol, and then lipid acid can be made to be coated on mineral surface, and so such as the positively charged ion such as Y, Na just adheres to each other by lipid acid and mineral.Just because of the appropriate design of first three step, make the 4th step carry out calcining at a lower temperature and just can obtain Na
3ySi
2o
7.Make the present invention not only with low cost by the ingehious design of above-mentioned four steps and perfect adaptation, and technique is simple, is suitable for suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the XRD figure of embodiment 1 products obtained therefrom;
Fig. 2 is the XRD figure of embodiment 2 products obtained therefrom;
Fig. 3 is the XRD figure of embodiment 3 products obtained therefrom;
As can be seen from Fig. 1, Fig. 2, Fig. 3, embodiment 1,2,3 products obtained therefrom is Na
3ySi
2o
7.
Embodiment
Embodiment 1
Take 0.70g six nitric hydrate yttrium and be dissolved in 50ml containing in oleic acid deionized water, wherein, oleic acid and deionized water volume ratio are 1:50, drip the sodium carbonate solution 150mL of 0.2mol/L wherein, obtain mixed system.Take 0.35g attapulgite (SiO
2content 57%), ultrasonic disperse is in 30mL oleic acid-ethanol solution, and wherein, dehydrated alcohol and oleic acid volume ratio are 20:1, are added by scattered attapulgite in above-mentioned mixed system, under the constant temperature of 20 DEG C, stir 12h.Centrifuge washing 3 times under the rotating speed of 9000rpm, dry 12h in 60 DEG C of baking ovens, then 5 DEG C/min calcines 1h and namely obtains Na at 800 DEG C
3ySi
2o
7powder.
Embodiment 2
Take 0.36g anhydrous chlorides of rase yttrium and be dissolved in 50ml containing in linolic acid deionized water, wherein, linolic acid and deionized water volume ratio are 1:30, drip the sodium carbonate solution 50mL of 0.5mol/L wherein, obtain mixed system.Take 0.37g sepiolite (SiO
2content 54%), ultrasonic disperse is in 35mL linolic acid-ethanol solution, and wherein, dehydrated alcohol and linolic acid volume ratio are 30:1, are added by scattered sepiolite in above-mentioned mixed system, under the constant temperature of 40 DEG C, stir 8h.Centrifuge washing 3 times under the rotating speed of 10000rpm, dry 9h in 70 DEG C of baking ovens, then 8 DEG C/min calcines 3h and namely obtains Na at 600 DEG C
3ySi
2o
7powder.
Embodiment 3
Take 0.27g tetra-acetate hydrate yttrium and be dissolved in 50ml containing in linolenic acid deionized water, wherein, linolenic acid and deionized water volume ratio are 1:70, drip the sodium carbonate solution 25mL of 1.0mol/L wherein, obtain mixed system.Take 0.21g diatomite (SiO
2content 95%), ultrasonic disperse is in 25mL linolenic acid-ethanol solution, and wherein, dehydrated alcohol and linolenic acid volume ratio are 40:1, are added by scattered diatomite in above-mentioned mixed system, under 60 DEG C of constant temperature, stir 6h.Centrifuge washing 3 times under the rotating speed of 12000rpm, dry 6h in 80 DEG C of baking ovens, then 10 DEG C/min calcines 2h and namely obtains Na at 700 DEG C
3ySi
2o
7powder.
Claims (9)
1. prepare Na for one kind
3ySi
2o
7method, it is characterized in that, first soluble yttrium salt is dissolved in the deionized water of fatty acids, then drips sodium carbonate solution wherein, obtain mixed system; Then being dispersed in by natural silicate minerals after in the dehydrated alcohol being dissolved with lipid acid joins in above-mentioned mixed system, and through stirring, centrifuge washing, dries, obtain Na after calcining
3ySi
2o
7;
Described natural silicate minerals is selected from the one in attapulgite, sepiolite or diatomite.
2. method according to claim 1, is characterized in that, in the deionized water of fatty acids, the volume ratio of lipid acid and deionized water is 1:20-1:100.
3. method according to claim 1, is characterized in that, described natural silicate minerals is the silicate minerals that dioxide-containing silica is greater than 50%.
4. method according to claim 1, specifically comprises the steps:
The first step: get soluble yttrium salt and be dissolved in the deionized water of fatty acids, preparation yttrium concentration be 10-50mmol/L containing ruthenium ion solution, wherein the volume ratio of lipid acid and deionized water is 1:20-1:100;
Second step: the sodium carbonate solution prepared is dropped to the first step gained containing in ruthenium ion solution, obtain mixed system, wherein the mol ratio of sodium and yttrium is 10:1-20:1;
3rd step: by natural silicate minerals ultrasonic disperse in the dehydrated alcohol being dissolved with lipid acid, wherein dehydrated alcohol and lipid acid volume ratio are 20:1-40:1, and natural silicate minerals is 1:50-1:100 with the mass ratio of the dehydrated alcohol being dissolved with lipid acid;
4th step: natural silicate minerals scattered for the 3rd step is joined in second step gained mixed system, centrifuge washing after stirring under the constant temperature of 20-60 DEG C, at 40-80 DEG C, dry in baking oven, then calcine in the temperature range of 600-800 DEG C under air atmosphere, obtain Na
3ySi
2o
7, the mass ratio containing ruthenium ion solution in described natural silicate minerals and the first step is 1:100-1:400.
5. the method according to claim 1 or 4, is characterized in that, soluble yttrium salt be selected from nitrate, chlorate or soluble organic salts any one.
6. the method according to claim 1 or 4, is characterized in that, lipid acid is the one in oleic acid, linolic acid, linolenic acid.
7. the method according to claim 1 or 4, is characterized in that, described sodium carbonate solution concentration is 0.2-1.5mol/L.
8. method according to claim 4, is characterized in that, in the 4th step, the time of stirring under the constant temperature of 20-60 DEG C is 6-12h, and during centrifuge washing, rotating speed is 9000-12000rpm, and the time dry in baking oven is 6-12h.
9. the method according to claim 1 or 4, is characterized in that, the rate of heating of calcination process is 5-10 DEG C/min, calcination time 1-3 hour.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102391859A (en) * | 2011-12-02 | 2012-03-28 | 福州大学 | Green fluorescent powder for white LED (light-emitting diode) use, its preparation method and application |
| CN102817109A (en) * | 2012-08-10 | 2012-12-12 | 长春理工大学 | Preparation method for europium doped yttrium disilicate red luminescence nano-belts |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102391859A (en) * | 2011-12-02 | 2012-03-28 | 福州大学 | Green fluorescent powder for white LED (light-emitting diode) use, its preparation method and application |
| CN102817109A (en) * | 2012-08-10 | 2012-12-12 | 长春理工大学 | Preparation method for europium doped yttrium disilicate red luminescence nano-belts |
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