CN103626195A - Method for preparing Na3YSi2O7 - Google Patents
Method for preparing Na3YSi2O7 Download PDFInfo
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- CN103626195A CN103626195A CN201310615662.5A CN201310615662A CN103626195A CN 103626195 A CN103626195 A CN 103626195A CN 201310615662 A CN201310615662 A CN 201310615662A CN 103626195 A CN103626195 A CN 103626195A
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- natural silicate
- silicate mineral
- lipid acid
- deionized water
- acid
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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 a kind of Na of preparation
3ySi
2o
7method, relate in particular to and a kind ofly take natural silicate mineral and prepare Na as raw material
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 fields such as luminescent lamp, white light-emitting diode.Current synthetic Na
3ySi
2o
7method have two kinds.Be to take yttrium nitrate, saliter hydrochlorate, tetraethoxy first to make a colloidal sol as raw material, colloidal sol is at room temperature placed and within 2～3 days, is become gel, gel prior to 500 ℃ of calcining 4h again in reducing atmosphere 950 ℃ of calcining 8h to obtain product.Another kind method is that to take yttrium oxide, silicon-dioxide, sodium carbonate be raw material, through mechanically mixing 1200 ℃ of above calcining 6-10h in air atmosphere again.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 is used mechanically mixing, need to reach presoma melt temperature and just can react, thereby need high temperature and longer calcination time.Not only energy consumption is high for above-mentioned two kinds of methods, and the raw material using 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 brand-new, be better than prior art take natural silicate mineral are raw material, the simple Na of preparation technology
3ySi
2o
7preparation method.
Concrete technical scheme:
A kind of Na for preparing
3ySi
2o
7method, first soluble yttrium salt is dissolved in the deionized water of fatty acids, then drips wherein sodium carbonate solution, obtain mixed system; Then after natural silicate mineral being dispersed in the dehydrated alcohol that is dissolved with lipid acid, join in above-mentioned mixed system, through stirring, centrifuge washing, dries, and obtains 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 mineral are preferably the silicate minerals that dioxide-containing silica is greater than 50%.
A kind of Na for preparing
3ySi
2o
7method, specifically comprise the steps:
The first step: get in the deionized water that soluble yttrium salt is dissolved in fatty acids, preparation yttrium concentration is 10-50mmol/L containing ruthenium ion solution, and wherein the volume ratio of lipid acid and deionized water is 1:20-1:100;
Wherein, lipid acid and deionized water volume ratio, the too high dissolving that is unfavorable for soluble salt, the too low effect that does not have dispersion;
Second step: the sodium carbonate solution preparing 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;
The 3rd step: be dispersed in the dehydrated alcohol that is dissolved with lipid acid natural silicate mineral are ultrasonic, wherein dehydrated alcohol and lipid acid volume ratio are 20:1-40:1, natural silicate mineral are 1:50-1:100 with the mass ratio that is dissolved with the dehydrated alcohol of lipid acid;
The 4th step: the scattered natural silicate mineral of the 3rd step are joined in second step gained mixed system, centrifuge washing after stirring under the constant temperature of 20-60 ℃, at 40-80 ℃, dry in baking oven, then under air atmosphere, in the temperature range of 600-800 ℃, calcine, obtain Na
3ySi
2o
7, the mass ratio containing ruthenium ion solution in described natural silicate mineral and the first step is 1:100-1:400.
Soluble yttrium salt is any one in nitrate, chlorate or solubility organic salt preferably.
Described lipid acid is any one in oleic acid, linolic acid, linolenic acid preferably.
Described concentration of sodium carbonate is preferably 0.2-1.5mol/L.
In the 4th step, the time of stirring under the constant temperature of 20-60 ℃ is 6-12h, and during centrifuge washing, rotating speed is 9000-12000rpm, and in baking oven, the dry time is 6-12h.
The rate of heating of calcination process is preferably 5-10 ℃/min, and calcination time is preferably 1-3 hour.
Wherein, natural silicate mineral be natural, without the silicate minerals of any modification, described natural silicate mineral comprise attapulgite, sepiolite, diatomite etc.
In the first step of the present invention, lipid acid is dispersed in deionized water and can forms water-oil systems, be beneficial to the dispersion of various ions, be also beneficial to the crystal formation that product formation is more complete simultaneously.
In the present invention's the 3rd step, natural silicate mineral surface generally all contains planar water, ethanol can take away these water mineral surface effectively by dissolving each other, and then can make lipid acid be coated on mineral surface, and positively charged ions such as Y, Na just can adhere to each other by lipid acid and mineral like this.
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 mineral to prepare Na as silicon source first
3ySi
2o
7, raw material is cheap and easy to get and without carrying out any pre-treatment, from having saved to a great extent cost, has improved 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 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 mineral as silicon source, it has not only saved the cost of raw material, and natural silicate mineral have abundant pore passage structure and large specific surface area, and process and more easily discharge silicon by alkaline environment of the present invention, and then be Na
3ySi
2o
7the synthetic silicon source that provides, the present invention further advantage treatment step is also, in the first step, lipid acid is dispersed in deionized water and can forms water-oil systems, particularly by rationally controlling the volume ratio of 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, has also played the effect of dissolve silicates mineral; In the 3rd step, natural silicate mineral surface generally all contains planar water, ethanol can effectively take away these water mineral surface by dissolving each other, and then can make lipid acid be coated on mineral surface, and positively charged ions such as Y, Na just can adhere to each other by lipid acid and mineral like this.Just because of the appropriate design of first three step, make the 4th step just calcine and can obtain Na at lower temperature
3ySi
2o
7.Ingehious design and perfect adaptation by above-mentioned four steps make the present invention not only with low cost, 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 therefroms;
Fig. 3 is the XRD figure of embodiment 3 products obtained therefroms;
From Fig. 1, Fig. 2, Fig. 3, can find out, embodiment 1,2,3 products obtained therefroms are Na
3ySi
2o
7.
Embodiment
Embodiment 1
Take 0.70g six nitric hydrate yttriums and be dissolved in 50ml containing in oleic acid deionized water, wherein, oleic acid and deionized water volume ratio are 1:50, drip wherein the sodium carbonate solution 150mL of 0.2mol/L, obtain mixed system.Take 0.35g attapulgite (SiO
2content 57%), ultrasonic being scattered in 30mL oleic acid-ethanol solution, wherein, dehydrated alcohol and oleic acid volume ratio are 20:1, and scattered attapulgite is added in above-mentioned mixed system, under the constant temperature of 20 ℃, stir 12h.Under the rotating speed of 9000rpm, centrifuge washing is 3 times, dry 12h in 60 ℃ of baking ovens, and then 5 ℃/min calcines 1h and obtains Na at 800 ℃
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 wherein the sodium carbonate solution 50mL of 0.5mol/L, obtain mixed system.Take 0.37g sepiolite (SiO
2content 54%), ultrasonic being scattered in 35mL linolic acid-ethanol solution, wherein, dehydrated alcohol and linolic acid volume ratio are 30:1, and scattered sepiolite is added in above-mentioned mixed system, under the constant temperature of 40 ℃, stir 8h.Under the rotating speed of 10000rpm, centrifuge washing is 3 times, dry 9h in 70 ℃ of baking ovens, and then 8 ℃/min calcines 3h and obtains Na at 600 ℃
3ySi
2o
7powder.
Embodiment 3
Take 0.27g tetra-hydration yttium acetates and be dissolved in 50ml containing in linolenic acid deionized water, wherein, linolenic acid and deionized water volume ratio are 1:70, drip wherein the sodium carbonate solution 25mL of 1.0mol/L, obtain mixed system.Take 0.21g diatomite (SiO
2content 95%), the ultrasonic 25mL linolenic acid-ethanol solution that is scattered in, wherein, dehydrated alcohol and linolenic acid volume ratio are 40:1, and scattered diatomite is added in above-mentioned mixed system, under 60 ℃ of constant temperature, stir 6h.Under the rotating speed of 12000rpm, centrifuge washing is 3 times, dry 6h in 80 ℃ of baking ovens, and then 10 ℃/min calcines 2h and obtains Na at 700 ℃
3ySi
2o
7powder.
Claims (10)
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 wherein sodium carbonate solution, obtain mixed system; Then after natural silicate mineral being dispersed in the dehydrated alcohol that is dissolved with lipid acid acid, join in above-mentioned mixed system, through stirring, centrifuge washing, dries, and obtains Na after calcining
3ySi
2o
7.
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 mineral are 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 in the deionized water that soluble yttrium salt is dissolved in fatty acids, preparation yttrium concentration is 10-50mmol/L containing ruthenium ion solution, and wherein the volume ratio of lipid acid and deionized water is 1:20-1:100;
Second step: the sodium carbonate solution preparing 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;
The 3rd step: be dispersed in the dehydrated alcohol that is dissolved with lipid acid natural silicate mineral are ultrasonic, wherein dehydrated alcohol and lipid acid volume ratio are 20:1-40:1, natural silicate mineral are 1:50-1:100 with the mass ratio that is dissolved with the dehydrated alcohol of lipid acid;
The 4th step: the scattered natural silicate mineral of the 3rd step are joined in second step gained mixed system, centrifuge washing after stirring under the constant temperature of 20-60 ℃, at 40-80 ℃, dry in baking oven, then under air atmosphere, in the temperature range of 600-800 ℃, calcine, obtain Na
3ySi
2o
7, the mass ratio containing ruthenium ion solution in described natural silicate mineral and the first step is 1:100-1:400.
5. according to the method described in claim 1 or 4, it is characterized in that, soluble yttrium salt is selected from any one in nitrate, chlorate or solubility organic salt.
6. according to the method described in claim 1 or 4, it is characterized in that, lipid acid is a kind of in oleic acid, linolic acid, linolenic acid.
7. according to the method described in claim 1 or 4, it is characterized in that, described natural silicate mineral are selected from a kind of in attapulgite, sepiolite or diatomite.
8. according to the method described in claim 1 or 4, it is characterized in that, described sodium carbonate solution concentration is 0.2-1.5mol/L.
9. according to the method described in claim 1 or 4, it is characterized in that, in the 4th step, the time of stirring under the constant temperature of 20-60 ℃ is 6-12h, and during centrifuge washing, rotating speed is 9000-12000rpm, and in baking oven, the dry time is 6-12h.
10. according to the method described in claim 1 or 4, it is characterized in that, the rate of heating of calcination process is 5-10 ℃/min, calcination time 1-3 hour.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110285863A (en) * | 2019-07-08 | 2019-09-27 | 中国科学院武汉岩土力学研究所 | A kind of salt cave can utilize the measurement method of volume |
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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Patent 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 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110285863A (en) * | 2019-07-08 | 2019-09-27 | 中国科学院武汉岩土力学研究所 | A kind of salt cave can utilize the measurement method of volume |
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