CN104386748B - A kind of scandium tantalic acid strontium raw powder's production technology - Google Patents
A kind of scandium tantalic acid strontium raw powder's production technology Download PDFInfo
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- CN104386748B CN104386748B CN201410599665.9A CN201410599665A CN104386748B CN 104386748 B CN104386748 B CN 104386748B CN 201410599665 A CN201410599665 A CN 201410599665A CN 104386748 B CN104386748 B CN 104386748B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G35/00—Compounds of tantalum
- C01G35/006—Compounds containing, besides tantalum, two or more other elements, with the exception of oxygen or hydrogen
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Abstract
The invention discloses a kind of scandium tantalic acid strontium raw powder's production technology, its with strontium salt, tantalum salt, scandium salts and different linking agent for raw material, fully dissolve in methanol-water mixing solutions, then crosslinking reaction post-crosslinking reaction at a certain temperature, mixing with fused salt and grind makes it fully mix, after pyroreaction, temperature carries out washing and drying after dropping to room temperature again, namely obtains scandium tantalic acid strontium powder.Strontium salt is one in strontium chloride and strontium nitrate or its mixture.Tantalum salt is one in tantalum pentachloride or five ethoxy-tantalum or its mixture.Scandium salts is one in Scium trichloride or Scium trinitrate or its mixture.Linking agent is one in urea or citric acid or its mixture.Fused salt is the mixture of sodium-chlor and strontium chloride.Present invention process is simple and easy to do, and purity is high, and preparation cost is low, is applicable to batch production, and prepared product may be used for the fields such as ferroelectric, photoelectricity, photocatalysis hydrogen production and fuel cell.
Description
Technical field
The invention belongs to the preparing technical field of ceramic, specifically relate to a kind of scandium tantalic acid strontium raw powder's production technology.
Background technology
The general molecular formula of the compound of uhligite (Perovskite) type is ABO
3, this compounds is found to be the calcium titanate (CaTiO be present in uhligite stone the earliest
3) compound, therefore gain the name.Because perovskite compound crystal structure has numerous characteristics, apply in Condensed Matter Physics and chemical industry catalysis and study very extensive.Especially rare earth complex perovskite structure material is a kind of important environmental catalysis material, because the advantages such as the thermally-stabilised and cheap cost that it is good are regarded as the first-selection of alternative noble metal catalyst always.As a kind of important functional materials, in the field such as environment protection and Industrial Catalysis, there is very large potentiality to be exploited.Scandium tantalic acid strontium (SrSc
1/2ta
1/2o
3) be that (A position is Sr to a kind of important compound rare-earth perovskite-type material; B position is Sc
1/2ta
1/2).Be mainly used in the fields such as photochemical catalysis, ion sensor, magnetoresistance material, fuel cell.Traditional solid state reaction technology preparing scandium tantalic acid strontium powder is consuming time longer and need hot conditions, and reaction is normally carried out under 1100 ~ 1300 ° of C, thus limits production and the use of scandium tantalic acid strontium powder.
Summary of the invention
The present invention is intended to overcome the deficiencies in the prior art part and provides a kind of technique simple, and object product yield is high, and preparation cost is low, and operating procedure is simple, and energy consumption is low, the scandium tantalic acid strontium raw powder's production technology of good dispersity.The present invention, by utilizing linking agent, achieves the technological process that pure phase scandium tantalic acid strontium powder is produced in Low Temperature Solid-Phase calcining.By organizing simultaneous test, finding that linking agent plays an important role in the reaction more, having utilized its fusing in the reaction and combustion heat release successfully to generate the scandium tantalic acid strontium powder with good crystallinity.Preparation method of the present invention can be applied to the chemosynthesis research of other functional materials similar with scandium tantalic acid strontium equally, and has broad application prospects.
For achieving the above object, the present invention realizes like this.
A kind of scandium tantalic acid strontium raw powder's production technology, strontium salt, tantalum salt, scandium salts and linking agent fully dissolve by system in methanol-water mixing solutions, carry out crosslinking reaction at a certain temperature, continue mixed with fused salt and grind and make it fully mix, after pyroreaction, temperature drops to room temperature, then carries out washing and drying, namely obtains scandium tantalic acid strontium powder.
As a kind of preferred version, the mol ratio of strontium salt of the present invention, tantalum salt, scandium salts, fused salt and linking agent is 2: 1: 1: 4: 40 ~ 200.
As another kind of preferred version, strontium salt of the present invention is one in strontium chloride and strontium nitrate or its mixture.
Further, tantalum salt of the present invention is one in tantalum pentachloride or five ethoxy-tantalum or its mixture.
Further, scandium salts of the present invention is one in Scium trichloride or Scium trinitrate or its mixture.
Further, linking agent of the present invention is one in urea or citric acid or its mixture.
Again further, described crosslinking reaction temperature is at 150 ~ 500 ° of C, and cross-linking reaction time is 2 ~ 10h.
Thirdly, the temperature of reaction of described high temperature is at 700 ~ 1000 ° of C, and the reaction times is 6 ~ 24h.
Fused salt of the present invention is the mixture of sodium-chlor and strontium chloride; The mol ratio of sodium-chlor and strontium chloride is 1:1.
Compared with prior art, the present invention has following features.
(1) present invention process route is simple, and preparation cost is low, easy to control, has higher production efficiency.
(2) the object product scandium tantalic acid strontium powder prepared of the present invention, its purity is high, and foreign matter content is low, good dispersity, can meet the requirement of modern industry to scandium tantalic acid strontium powder product.
(3) the present invention can react under 700 ~ 1000 ° of C environment, and the reaction times is 6 ~ 24h, and energy-saving effect is obvious.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the invention will be further described.Protection scope of the present invention is not only confined to the statement of following content.
The X-ray diffractogram of the scandium tantalic acid strontium powder of Fig. 1 prepared by the present invention.
The SEM figure of the scandium tantalic acid strontium powder of Fig. 2 prepared by the present invention.
The SEM figure of the scandium tantalic acid strontium powder of Fig. 3 prepared by the present invention.
The SEM figure of the scandium tantalic acid strontium powder of Fig. 4 prepared by the present invention.
The infrared spectrogram of the scandium tantalic acid strontium powder of Fig. 5 prepared by the present invention.
The ultraviolet-visible spectrogram of the scandium tantalic acid strontium powder of Fig. 6 prepared by the present invention.
The energy gap figure of the scandium tantalic acid strontium powder of Fig. 7 prepared by the present invention.
The scandium tantalic acid strontium powder of Fig. 8 prepared by the present invention is as the catalytic activity phenogram of photocatalyst.
Embodiment
The present invention with strontium salt, tantalum salt, scandium salts and different linking agent for raw material.Raw material is according to certain mol ratio, fully dissolve in methanol-water mixing solutions (volume ratio 1:1), then at a certain temperature after crosslinking reaction, mixing with fused salt (mixture of sodium-chlor and strontium chloride mol ratio 1:1) and grind makes it fully mix, after pyroreaction, temperature carries out washing and drying after dropping to room temperature again, and namely obtain scandium tantalic acid strontium powder, its preparation process is.
(1) by strontium salt, tantalum salt, scandium salts and different linking agent according to after certain molar ratio weighing, be placed in alcohol water mixed solution and fully dissolve.
(2) by above-mentioned solution, at 150 ~ 500 ° of C, crosslinking reaction 2 ~ 10h.
(3) naturally cool to room temperature, and after fused salt (mixture of sodium-chlor and strontium chloride mol ratio 1:1) mixing, put into mortar and grind and carefully make it mix, milling time 30 minutes.
(4) after in above-mentioned mixture loading crucible, put into chamber type electric resistance furnace, calcination reaction, temperature of reaction 700 ~ 1000 ° of C, the reaction times is 6 ~ 24h, and naturally cooling, also after washing and drying, namely obtains scandium tantalic acid strontium powder.
See shown in Fig. 1 to 8, the scandium tantalic acid strontium powder preparing gained is carried out XRD and ultraviolet-visible spectrum analysis by the present invention, and consequently, products obtained therefrom scandium tantalic acid strontium powder XRD diffraction pattern is consistent with standard spectrogram, and degree of crystallinity very strong (Fig. 1).As can be seen from the SEM figure of products obtained therefrom scandium tantalic acid strontium powder, scandium tantalic acid strontium powder is uniformly dispersed, and size is between 50 ~ 100nm, and the dispersiveness of product and homogeneity are all very well (Fig. 2 ~ 4).The infrared spectrogram of the scandium tantalic acid strontium powder of Fig. 5 prepared by the present invention.The ABSORPTION EDGE of products obtained therefrom scandium tantalic acid strontium powder is at about 270nm (Fig. 6), and energy gap is about 4.50eV(Fig. 7).And under ultraviolet light conditions (predominant wavelength 254nm), in certain catalysis auxiliary and the aqueous solution of finite concentration sacrifice agent, in the reaction model of photochemical catalysis aquatic products hydrogen, have very high catalytic activity (Fig. 8).
Embodiment 1.
Methanol aqueous solution (volume ratio 1:1) stirring and dissolving is put into by after strontium nitrate, tantalum pentachloride, Scium trinitrate and citric acid precise.By this solution, at 450 ° of C, crosslinking reaction 4h, after reaction, naturally cool to room temperature, and after fused salt (fused salt is the mixture of sodium-chlor and strontium chloride, sodium-chlor and strontium chloride mol ratio 1:1) mixes, put into mortar grind careful, milling time 30 minutes.The mol ratio of above-mentioned strontium nitrate, tantalum pentachloride, Scium trinitrate, fused salt and citric acid is 2: 1: 1: 4: 50.Loaded by above-mentioned mixture after in crucible and put into chamber type electric resistance furnace, calcination reaction, temperature of reaction 800 ° of C, the reaction times is 6h, and cooling after washing is dry, i.e. scandium tantalic acid strontium powder processed.Its product purity is not less than 99.80%, foreign matter content: carbon is less than 0.11%; Chlorine is less than 0.09%.Under ultraviolet light conditions (predominant wavelength 254nm), supporting Pt, as after auxiliary agent, is in the aqueous solution of sacrifice agent at methyl alcohol, and the efficiency of Photocatalyzed Hydrogen Production is 20.9mmol/h.
Embodiment 2.
Methanol aqueous solution (volume ratio 1:1) stirring and dissolving is put into by after strontium nitrate, five ethoxy-tantalum, Scium trinitrate and urea precise.By this solution, at 150 ° of C, crosslinking reaction 10h, after reaction, naturally cool to room temperature, and after fused salt (fused salt is the mixture of sodium-chlor and strontium chloride, sodium-chlor and strontium chloride mol ratio 1:1) mixes, put into mortar grind careful, milling time 30 minutes.The mol ratio of above-mentioned strontium nitrate, five ethoxy-tantalum, Scium trinitrate, fused salt and urea is 2: 1: 1: 4: 200.Loaded by above-mentioned mixture after in crucible and put into chamber type electric resistance furnace, calcination reaction, temperature of reaction 900 ° of C, the reaction times is 12h, and cooling after washing is dry, i.e. scandium tantalic acid strontium powder processed.Its product purity is not less than 99.88%, foreign matter content: carbon is less than 0.07%; Chlorine is less than 0.05%.Under ultraviolet light conditions (predominant wavelength 254nm), supporting Pt, as after auxiliary agent, is in the aqueous solution of sacrifice agent at methyl alcohol, and the efficiency of Photocatalyzed Hydrogen Production is 35.1mmol/h.
Embodiment 3.
Methanol aqueous solution (volume ratio 1:1) stirring and dissolving is put into by after strontium nitrate, tantalum pentachloride, Scium trinitrate and citric acid precise.By this solution, at 450 ° of C, crosslinking reaction 6h, after reaction, naturally cool to room temperature, and after fused salt (fused salt is the mixture of sodium-chlor and strontium chloride, sodium-chlor and strontium chloride mol ratio 1:1) mixes, put into mortar grind careful, milling time 30 minutes.The mol ratio of above-mentioned strontium nitrate, tantalum pentachloride, Scium trinitrate, fused salt and citric acid is 2: 1: 1: 4: 80.Loaded by above-mentioned mixture after in crucible and put into chamber type electric resistance furnace, calcination reaction, temperature of reaction 1000 ° of C, the reaction times is 6h, and cooling after washing is dry, i.e. scandium tantalic acid strontium powder processed.Its product purity is not less than 99.92%, foreign matter content: carbon is less than 0.04%; Chlorine is less than 0.03%.Under ultraviolet light conditions (predominant wavelength 254nm), supporting Pt, as after auxiliary agent, is in the aqueous solution of sacrifice agent at methyl alcohol, and the efficiency of Photocatalyzed Hydrogen Production is 29.3mmol/h(Fig. 8).
Embodiment 4.
Methanol aqueous solution (volume ratio 1:1) stirring and dissolving is put into by after strontium nitrate, tantalum pentachloride, Scium trinitrate and citric acid precise.By this solution, at 500 ° of C, crosslinking reaction 10h, after reaction, naturally cool to room temperature, and after fused salt (fused salt is the mixture of sodium-chlor and strontium chloride, sodium-chlor and strontium chloride mol ratio 1:1) mixes, put into mortar grind careful, milling time 30 minutes.The mol ratio of above-mentioned strontium nitrate, tantalum pentachloride, Scium trinitrate, fused salt and citric acid is 2: 1: 1: 4: 80.Loaded by above-mentioned mixture after in crucible and put into chamber type electric resistance furnace, calcination reaction, temperature of reaction 1000 ° of C, the reaction times is 6h, and cooling after washing is dry, i.e. scandium tantalic acid strontium powder processed.Its product purity is not less than 99.95%, foreign matter content: carbon is less than 0.03%; Chlorine is less than 0.02%.Under ultraviolet light conditions (predominant wavelength 254nm), supporting Pt is as after auxiliary agent, and in pure water, the efficiency of Photocatalyzed Hydrogen Production is 15.1mmol/h; Without auxiliary agent, the efficiency of the Photocatalyzed Hydrogen Production in pure water is 8.1mmol/h.
Embodiment 5.
Methanol aqueous solution (volume ratio 1:1) stirring and dissolving is put into by after strontium nitrate, tantalum pentachloride, Scium trinitrate and citric acid precise.By this solution, at 150 ° of C, crosslinking reaction 10h, after reaction, naturally cool to room temperature, and after fused salt (fused salt is the mixture of sodium-chlor and strontium chloride, sodium-chlor and strontium chloride mol ratio 1:1) mixes, put into mortar grind careful, milling time 30 minutes.The mol ratio of above-mentioned strontium nitrate, tantalum pentachloride, Scium trinitrate, fused salt and citric acid is 2: 1: 1: 4: 80.Loaded by above-mentioned mixture after in crucible and put into chamber type electric resistance furnace, calcination reaction, temperature of reaction 1000 ° of C, the reaction times is 24h, and cooling after washing is dry, i.e. scandium tantalic acid strontium powder processed.Its product purity is not less than 99.98%, foreign matter content: carbon is less than 0.01%; Chlorine is less than 0.01%.Under ultraviolet light conditions (predominant wavelength 254nm), supporting Pt is as after auxiliary agent, and in pure water, the efficiency of Photocatalyzed Hydrogen Production is 18.2mmol/h; Without auxiliary agent, the efficiency of the Photocatalyzed Hydrogen Production in pure water is 9.1mmol/h.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. a scandium tantalic acid strontium raw powder's production technology, is characterized in that, will put into the methanol aqueous solution stirring and dissolving of volume ratio 1:1 after strontium nitrate, tantalum pentachloride, Scium trinitrate and citric acid precise; By this solution at 450 DEG C, crosslinking reaction 4h, after reaction, naturally cools to room temperature, and fused salt mixing after, put into mortar grind careful, milling time 30 minutes; Fused salt is the mixture of sodium-chlor and strontium chloride, sodium-chlor and strontium chloride mol ratio 1:1; The mol ratio of above-mentioned strontium nitrate, tantalum pentachloride, Scium trinitrate, fused salt and citric acid is 2: 1: 1: 4: 50; Loaded by above-mentioned mixture after in crucible and put into chamber type electric resistance furnace, calcination reaction, temperature of reaction 800 DEG C, the reaction times is 6h, and cooling after washing is dry, i.e. scandium tantalic acid strontium powder processed; Its product purity is not less than 99.80%, foreign matter content: carbon is less than 0.11%; Chlorine is less than 0.09%; Under predominant wavelength 254nm ultraviolet light conditions, supporting Pt, as after auxiliary agent, is in the aqueous solution of sacrifice agent at methyl alcohol, and the efficiency of Photocatalyzed Hydrogen Production is 20.9mmol/h.
2. a scandium tantalic acid strontium raw powder's production technology, is characterized in that, will put into the methanol aqueous solution stirring and dissolving of volume ratio 1:1 after strontium nitrate, five ethoxy-tantalum, Scium trinitrate and urea precise; By this solution at 150 DEG C, crosslinking reaction 10h, after reaction, naturally cools to room temperature, and fused salt mixing after, put into mortar grind careful, milling time 30 minutes; Fused salt is the mixture of sodium-chlor and strontium chloride, sodium-chlor and strontium chloride mol ratio 1:1; The mol ratio of above-mentioned strontium nitrate, five ethoxy-tantalum, Scium trinitrate, fused salt and urea is 2: 1: 1: 4: 200; Loaded by above-mentioned mixture after in crucible and put into chamber type electric resistance furnace, calcination reaction, temperature of reaction 900 DEG C, the reaction times is 12h, and cooling after washing is dry, i.e. scandium tantalic acid strontium powder processed; Its product purity is not less than 99.88%, foreign matter content: carbon is less than 0.07%; Chlorine is less than 0.05%; Under predominant wavelength 254nm ultraviolet light conditions, supporting Pt, as after auxiliary agent, is in the aqueous solution of sacrifice agent at methyl alcohol, and the efficiency of Photocatalyzed Hydrogen Production is 35.1mmol/h.
3. a scandium tantalic acid strontium raw powder's production technology, is characterized in that, will put into the methanol aqueous solution stirring and dissolving of volume ratio 1:1 after strontium nitrate, tantalum pentachloride, Scium trinitrate and citric acid precise; By this solution at 450 DEG C, crosslinking reaction 6h, after reaction, naturally cools to room temperature, and fused salt mixing after, put into mortar grind careful, milling time 30 minutes; Fused salt is the mixture of sodium-chlor and strontium chloride, sodium-chlor and strontium chloride mol ratio 1:1; The mol ratio of above-mentioned strontium nitrate, tantalum pentachloride, Scium trinitrate, fused salt and citric acid is 2: 1: 1: 4: 80; Loaded by above-mentioned mixture after in crucible and put into chamber type electric resistance furnace, calcination reaction, temperature of reaction 1000 DEG C, the reaction times is 6h, and cooling after washing is dry, i.e. scandium tantalic acid strontium powder processed; Its product purity is not less than 99.92%, foreign matter content: carbon is less than 0.04%; Chlorine is less than 0.03%; Under predominant wavelength 254nm ultraviolet light conditions, supporting Pt, as after auxiliary agent, is in the aqueous solution of sacrifice agent at methyl alcohol, and the efficiency of Photocatalyzed Hydrogen Production is 29.3mmol/h.
4. a scandium tantalic acid strontium raw powder's production technology, is characterized in that, will put into the methanol aqueous solution stirring and dissolving of volume ratio 1:1 after strontium nitrate, tantalum pentachloride, Scium trinitrate and citric acid precise; By this solution at 500 DEG C, crosslinking reaction 10h, after reaction, naturally cools to room temperature, and fused salt mixing after, put into mortar grind careful, milling time 30 minutes; Fused salt is the mixture of sodium-chlor and strontium chloride, sodium-chlor and strontium chloride mol ratio 1:1; The mol ratio of above-mentioned strontium nitrate, tantalum pentachloride, Scium trinitrate, fused salt and citric acid is 2: 1: 1: 4: 80; Loaded by above-mentioned mixture after in crucible and put into chamber type electric resistance furnace, calcination reaction, temperature of reaction 1000 DEG C, the reaction times is 6h, and cooling after washing is dry, i.e. scandium tantalic acid strontium powder processed; Its product purity is not less than 99.95%, foreign matter content: carbon is less than 0.03%; Chlorine is less than 0.02%; Under predominant wavelength 254nm ultraviolet light conditions, supporting Pt is as after auxiliary agent, and in pure water, the efficiency of Photocatalyzed Hydrogen Production is 15.1mmol/h; Without auxiliary agent, the efficiency of the Photocatalyzed Hydrogen Production in pure water is 8.1mmol/h.
5. a scandium tantalic acid strontium raw powder's production technology, is characterized in that, will put into the methanol aqueous solution stirring and dissolving of volume ratio 1:1 after strontium nitrate, tantalum pentachloride, Scium trinitrate and citric acid precise; By this solution at 150 DEG C, crosslinking reaction 10h, after reaction, naturally cools to room temperature, and fused salt mixing after, put into mortar grind careful, milling time 30 minutes; Fused salt is the mixture of sodium-chlor and strontium chloride, sodium-chlor and strontium chloride mol ratio 1:1; The mol ratio of above-mentioned strontium nitrate, tantalum pentachloride, Scium trinitrate, fused salt and citric acid is 2: 1: 1: 4: 80; Loaded by above-mentioned mixture after in crucible and put into chamber type electric resistance furnace, calcination reaction, temperature of reaction 1000 DEG C, the reaction times is 24h, and cooling after washing is dry, i.e. scandium tantalic acid strontium powder processed; Its product purity is not less than 99.98%, foreign matter content: carbon is less than 0.01%; Chlorine is less than 0.01%; Under predominant wavelength 254nm ultraviolet light conditions, supporting Pt is as after auxiliary agent, and in pure water, the efficiency of Photocatalyzed Hydrogen Production is 18.2mmol/h; Without auxiliary agent, the efficiency of the Photocatalyzed Hydrogen Production in pure water is 9.1mmol/h.
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2014
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| CN1189422C (en) * | 2002-12-06 | 2005-02-16 | 清华大学 | Method of synthesizing nano grade calcium titanium ceramic powder |
| CN1470478A (en) * | 2003-06-20 | 2004-01-28 | 上海大学 | Rare earth-doped srstrontium cerate nano crystal ceramic preparing method |
| CN104108749A (en) * | 2014-06-11 | 2014-10-22 | 华中科技大学 | Preparing method of doped strontium titanate |
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