CN101696030A - Method for preparing stabilizing aluminum titanate at low temperature by non-hydrolytic sol-gel process - Google Patents
Method for preparing stabilizing aluminum titanate at low temperature by non-hydrolytic sol-gel process Download PDFInfo
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Abstract
The invention discloses a method for preparing stabilizing aluminum titanate at low temperature by a non-hydrolytic sol-gel process. In the method, anhydrous aluminum choride and titanium tetrachloride are used as precursors, anhydrous low-carbon alcohol is used as an oxygen donor, and ferric salt or magnesium salt or a compound of the ferric salt and the magnesium salt is used as a stabilizing agent, dry aluminum titanate gel is prepared through the non-hydrolytic sol-gel process, and finally the stabilizing aluminum titanate is obtained through calcining at 750 DEG C. The method for preparing the stabilizing aluminum titanate at low temperature has the prominent advantages of low synthesis temperature, short period, low cost, easy control, and the like.
Description
Technical field
The invention belongs to inorganic material-modified technical field, be specifically related to the method for a kind of non-hydrolytic sol-gel process preparing stabilizing aluminum titanate at low temperature.
Background technology
Aluminium titanates not only has high-melting-point (1860 ℃) and low bulk (α＜1.5 * 10
-6/ ℃) advantage, but also have characteristics such as thermal conductivity low (1.5W/mK), good thermal shock and erosion resistance are strong, have broad application prospects.But aluminium titanates easily is decomposed into rutile and corundum mutually in 800～1280 ℃ of intervals, cause its premium properties to exhaust, so aluminium titanates must stabilization just can obtain practical application.
Just begun the research of aluminium titanates stabilization both at home and abroad in the seventies in last century, usually utilize solid phase method to mix and realize the aluminium titanates stabilization, as stablize the lattice of aluminium titanates by introducing oxide additions such as ferric oxide, magnesium oxide, silicon-dioxide, yttrium oxide, lanthanum trioxide, thus the thermostability of raising aluminium titanates.But, the thermal treatment temp of solid phase method doping vario-property is up to more than 1500 ℃, and for reducing thermal treatment temp, ZL200610005315.0 discloses a kind of preparation method of modified aluminium titanate material, this method adopts traditional hydrolysis sol-gel technology, by introducing Mg (NO
3)
26H
2O, Fe (NO
3)
39H
2O, ZrOCl
28H
2O and Y (NO
3)
39H
2Inorganic additives such as O are stablized the lattice of aluminium titanates, have significantly improved the heat resistanceheat resistant capacity of decomposition of aluminium titanates, and its thermal treatment temp is 1380～1450 ℃.ZL200610005316.5 discloses a kind of method of the non-hydrolytic sol-gel process synthesizing composite oxide powder with alcohol as oxygen donor, and the temperature of its synthetic aluminium titanates is 750 ℃.Though this patent has realized that the low temperature of aluminium titanates is synthetic, do not relate to and suppress aluminium titanates pyrolysated problem, the aluminium titanates that adopts the described method preparation of this patent promptly all is decomposed into rutile and corundum mutually at 1050 ℃ of insulation 15min.Therefore, though ZL200610005316.5 has successfully realized the target with the synthetic aluminium titanates of non-hydrolytic sol-gel process low temperature, fail to solve the problem of synthetic aluminium titanates poor stability.Yet, use non-hydrolytic sol-gel process with the used oxide compound of above-mentioned solid phase method and hydrolytic sol-gel process doping vario-property and inorganic salt as stablizer, can not the synthetic desired stable aluminium titanates of low temperature.This is because metal ions such as the iron in the oxide compound, magnesium, yttrium can not enter the lattice of aluminium titanates under 750 ℃ of low temperature, therefore can't utilize solid solution to mix and improve the stability of aluminium titanates.The crystal water that exists in the inorganic salt then can destroy the polycondensation process of non-hydrolytic sol-gel, and causing can not the synthetic aluminium titanates of low temperature.The common precursor material of non-hydrolytic sol-gel process---anhydrous metal halide also can't make 750 ℃ of lattices that enter aluminium titanates of metal ion such as iron, magnesium as stablizer even use.At present, do not see the bibliographical information that adopts the non-hydrolytic sol-gel process preparing stabilizing aluminum titanate at low temperature both at home and abroad as yet.
Summary of the invention
The object of the present invention is to provide the stabilizing aluminum titanate preparation method that a kind of temperature is low, the cycle short, technology is simple, be easy to control.
The present invention proposes a kind of method that adopts non-hydrolytic sol-gel process preparing stabilizing aluminum titanate at low temperature, it is characterized in that with anhydrous TiCl
4And AlCl
3Being presoma, is oxygen donor with the anhydrous low-carbon alcohol, with molysite or magnesium salts, or compound as stablizer with molysite and magnesium salts, with the synthetic aluminium titanates of non-hydrolytic sol-gel process low temperature.
Described molysite and magnesium salts are meant the anhydrous organic acid salt of iron, magnesium alkoxide and iron, magnesium.
Described low-carbon alcohol is meant the alcohol (except the trimethyl carbinol) that contains 2～4 carbon atoms.
The doping of described stablizer is all with TiCl
4Amount of substance be benchmark, the doping of molysite and magnesium salts is respectively: 5～10mol% and 8～20mol%.Wherein, TiCl
4: AlCl
3: anhydrous low-carbon alcohol=be 1: 2: 5 (mol ratio).
The processing step of above-mentioned preparation stabilizing aluminum titanate is as follows:
(1) be that stablizer prepares stabilizing aluminum titanate with the molysite: under the ice-water bath condition, measure an amount of TiCl with valinche
4, it is slowly joined in the low-carbon alcohol that is dissolved with molysite in advance, add required AlCl again
3, then 75 ℃ of reactions to forming homogeneous phase presoma mixed solution, by just directly forming xerogel after 110 ℃ of gelations, xerogel grinds after 750 ℃ of calcinings obtain stabilizing aluminum titanate;
(2) be that stablizer prepares stabilizing aluminum titanate with the magnesium salts: the Erlenmeyer flask that an amount of low-carbon alcohol will be housed places ice-water bath, measures required TiCl with valinche
4, and slowly join in the low-carbon alcohol, add required AlCl again
3Then 75 ℃ of reactions to forming homogeneous presoma mixed solution, form wet gel through 110 ℃ of ageings, after wet gel dissolves with methylene dichloride, add a certain amount of magnesium salts, carry out back flow reaction at 50 ℃, form thousand gels again after 50 ℃ of dryings, xerogel just obtains stable aluminium titanates through grinding and 750 ℃ of thermal treatments.
(3) be that one package stabilizer prepares stabilizing aluminum titanate with molysite and magnesium salts: processing step is with (2), and different is earlier molysite to be dissolved in the low-carbon alcohol, and then adds TiCl
4
Described ferrite particular methanol iron, ethanol iron, Virahol iron and propyl carbinol iron, preferred anhydrous formic acid iron of anhydrous organic acid iron and Glacial acetic acid iron; Magnesium alkoxide particular methanol magnesium, magnesium ethylate, magnesium isopropoxide, propyl carbinol magnesium and tert-butyl alcohol magnesium, preferred anhydrous formic acid magnesium of anhydrous organic acid magnesium and Glacial acetic acid magnesium.
The present invention proves by a large amount of investigative tests in early stage and theoretical investigation: the oxide compound and the inorganic salt that are used for solid phase method and hydrolytic sol-gel process doping vario-property all can not be applied to non-hydrolytic sol-gel process, this is because the metal ion of these doping agents can not enter the lattice of aluminium titanates under 750 ℃ of low temperature, therefore can't mix by solid solution and improve the stability of aluminium titanates.The present invention is in conjunction with the characteristics of non-hydrolytic sol-gel process, the oxide compound and the inorganic salt that are used for solid phase method and hydrolytic sol-gel process doping vario-property have been abandoned, innovation ground adopts iron, magnesium alkoxide and their anhydrous organic acid salt as stablizer, these stablizers can form heteropolymerizations such as Ti-O-Fe or Ti-O-Mg with the presoma reaction in gel, make magnesium ion and iron ion can under 750 ℃ of low temperature, enter the lattice of aluminium titanates, thereby realize the target of preparing stabilizing aluminum titanate at low temperature.The magnesium stablizer must be introduced after aluminium, the polycondensation of titanium precursor body could obtain best effect.Otherwise then its stabilising effect is undesirable to add magnesium salts before aluminium, titanium precursor body generation polycondensation.For example, when in not producing the aluminium of polycondensation, titanium precursor body mixed solution, adding magnesium acetate, because alcoholic acid polarity and specific inductivity are bigger, Dichlorodiphenyl Acetate magnesium has certain disassociation, the result forms magnesium ion in the presoma mixed solution, and magnesium ion is a kind of strong lewis acid, and it can play the effect of the non-hydrolysis homogeneity of catalysis polymeric, cause the Ti-O-Mg heteropolymerization to reduce, it is not good finally to show as institute's synthetic aluminium titanates stability.Therefore, the formation of Ti-O-Mg bonding is that magnesium ion can enter the aluminium titanates lattice at low temperatures, stablize the key of aluminium titanates in the aluminium titanates gel.
The present invention at home and abroad takes the lead in adopting non-hydrolytic sol-gel process to prepare stabilizing aluminum titanate, has significantly improved the ability that the aluminium titanates heat resistanceheat resistant is decomposed by preferred stabilizer kind and optimization technological process, has realized the target of low temperature synthesizing stable aluminium titanates.
Embodiment
Embodiment 1
With TiCl
4Amount of substance be benchmark, iron mixes and to measure 10mol%.Take by weighing 0.697g ethanol iron (analytical pure) and place Erlenmeyer flask, measuring 10.5ml dehydrated alcohol (analytical pure) pours in the Erlenmeyer flask, be stirred to the ethanol dissolved ferric iron, again Erlenmeyer flask is placed the frozen water mixed solution, measuring 4ml titanium tetrachloride (chemical pure) with valinche inserts rapidly below the ethanolic soln liquid level, slowly add titanium tetrachloride, add 9.707g aluminum trichloride (anhydrous) (analytical pure) then, 75 ℃ of oil baths are heated to and form transparent salmon solution, by just directly forming the black xerogel after 110 ℃ of gelations, gel is through grinding, obtain the stabilizing aluminum titanate powder after 750 ℃ of thermal treatments.
Embodiment 2
With TiCl
4Amount of substance be benchmark, iron mixes and to measure 5mol%.Take by weighing 0.348g iron acetate (analytical pure) and place Erlenmeyer flask, measuring 10.5ml dehydrated alcohol (analytical pure) pours in the Erlenmeyer flask, be stirred to the iron acetate dissolving, then Erlenmeyer flask is placed the frozen water mixed solution, measuring 4ml titanium tetrachloride (chemical pure) with valinche inserts rapidly below the ethanolic soln liquid level, slowly add titanium tetrachloride, add 9.707g aluminum trichloride (anhydrous) (analytical pure) then, 75 ℃ of oil baths are heated to and form transparent salmon solution, by just directly forming the black xerogel after 110 ℃ of gelations, gel is through grinding, obtain stabilizing aluminum titanate after 750 ℃ of thermal treatments.
Embodiment 3
With TiCl
4Amount of substance be benchmark, magnesium mixes and to measure 20mol%.Measure 10.5ml dehydrated alcohol (analytical pure) and place Erlenmeyer flask, and Erlenmeyer flask is placed mixture of ice and water, measure 4.0mlTiCl with valinche
4(chemical pure) places the low-carbon alcohol liquid level to form orange-yellow clear solution following and slow the adding rapidly, add 9.707g aluminum trichloride (anhydrous) (analytical pure) then, 75 ℃ of oil baths are heated to and form the yellow-green colour clear solution, 110 ℃ are back to the translucent wet gel of formation light red again, the cooling back adds 15ml methylene dichloride (analytical pure), be stirred to gel and dissolve formation glassy yellow clear solution fully, add 0.835g magnesium ethylate (analytical pure) again, 50 ℃ of backflows are dried to gelation, and gel obtains the stabilizing aluminum titanate powder through grinding, 750 ℃ of thermal treatments.
Embodiment 4
With TiCl
4Amount of substance be benchmark, magnesium mixes and to measure 8mol%.Measure 10.5ml dehydrated alcohol (analytical pure) and place Erlenmeyer flask, and Erlenmeyer flask is placed mixture of ice and water, measure 4.0mlTiCl with valinche
4(chemical pure) places the dehydrated alcohol liquid level to form orange-yellow clear solution following and slow the adding rapidly, add 9.707g aluminum trichloride (anhydrous) (analytical pure) then, 75 ℃ of oil baths are heated to and form the yellow-green colour clear solution, 110 ℃ are back to the translucent wet gel of formation light red again, the cooling back adds 15ml methylene dichloride (analytical pure), be stirred to gel and dissolve formation glassy yellow clear solution fully, add 0.416g magnesium acetate (analytical pure) again, 50 ℃ of backflows are dried to gelation, and gel obtains the stabilizing aluminum titanate powder through grinding, 750 ℃ of thermal treatments.
Embodiment 5
With TiCl
4Amount of substance be benchmark, iron mixes and to measure 5mol%, magnesium mixes and measures 20mol%.Take by weighing 0.348g ethanol iron (analytical pure) and place Erlenmeyer flask, measure 10.5ml dehydrated alcohol (analytical pure) and place Erlenmeyer flask, and Erlenmeyer flask is placed mixture of ice and water, measure 4.0mlTiCl with valinche
4(chemical pure) places the ethanol liquid level to form orange-yellow clear solution following and slow the adding rapidly, add 9.707g aluminum trichloride (anhydrous) (analytical pure) then, 75 ℃ of oil baths are heated to and form the light red clear solution, 110 ℃ are back to the translucent wet gel of formation light red again, the cooling back adds 15ml methylene dichloride (analytical pure), be stirred to gel and dissolve formation glassy yellow clear solution fully, add 0.835g magnesium ethylate (analytical pure) again, 50 ℃ of backflows are dried to gelation, and gel obtains stable aluminium titanates powder through grinding, 750 ℃ of thermal treatments.
Embodiment 6
With TiCl
4Amount of substance be benchmark, iron mixes and to measure 10mol%, magnesium mixes and measures 8mol%.Take by weighing 0.697g ethanol iron (analytical pure) and place Erlenmeyer flask, measure 10.5ml dehydrated alcohol (analytical pure) and place Erlenmeyer flask, and Erlenmeyer flask is placed mixture of ice and water, measure 4.0mlTiCl with valinche
4(chemical pure) places the ethanol liquid level to form orange-yellow clear solution following and slow the adding rapidly, add 9.707g aluminum trichloride (anhydrous) (analytical pure) then, 75 ℃ of oil baths are heated to and form the light red clear solution, 110 ℃ are back to the translucent wet gel of formation light red again, the cooling back adds 15ml methylene dichloride (analytical pure), be stirred to gel and dissolve formation glassy yellow clear solution fully, add 0.334g magnesium ethylate (analytical pure) again, 50 ℃ of backflows are dried to gelation, and gel obtains the stabilizing aluminum titanate powder through grinding, 750 ℃ of thermal treatments.
Embodiment 7
With TiCl
4Amount of substance be benchmark, iron mixes and to measure 10mol%, magnesium mixes and measures 10mol%.Take by weighing 0.635g iron acetate (analytical pure) and place Erlenmeyer flask, measure 10.5ml dehydrated alcohol (analytical pure) and place Erlenmeyer flask, and Erlenmeyer flask is placed mixture of ice and water, measure 4.0mlTiCl with valinche
4(chemical pure) places the ethanol liquid level to form orange-yellow clear solution following and slow the adding rapidly, add 9.707g aluminum trichloride (anhydrous) (analytical pure) then, 75 ℃ of oil baths are heated to and form the light red clear solution, 110 ℃ are back to the translucent wet gel of formation light red again, the cooling back adds 15ml methylene dichloride (analytical pure), be stirred to gel and dissolve formation glassy yellow clear solution fully, add 0.519g magnesium acetate (analytical pure) again, 50 ℃ of backflows are dried to gelation, and gel obtains the stabilizing aluminum titanate powder through grinding, 750 ℃ of thermal treatments.
Claims (7)
1. the method for non-hydrolytic sol-gel process preparing stabilizing aluminum titanate at low temperature, it is characterized in that: with anhydrous AlCl3 and TiCl4 is presoma, with the anhydrous low-carbon alcohol is oxygen donor, with molysite or magnesium salts, or compound with molysite and magnesium salts as stablizer, method with the synthetic aluminium titanates of non-hydrolytic sol-gel process low temperature, described molysite is ferrite or anhydrous organic acid molysite, described magnesium salts is magnesium alkoxide or anhydrous organic acid magnesium salts, and described anhydrous low-carbon alcohol is the alcohol that contains 2～4 carbon atoms except that the trimethyl carbinol.
2. according to the method for the described non-hydrolytic sol of claim 1-gel process preparing stabilizing aluminum titanate at low temperature, the doping that it is characterized in that described stablizer is a benchmark with the amount of substance of TiCl4 all, the doping of molysite and magnesium salts is respectively 5～10mol% and 8～20mol%, and the mol ratio of anhydrous AlCl3, TiCl4 and anhydrous low-carbon alcohol is TiCl4: AlCl3: anhydrous low-carbon alcohol=1: 2: 5.
3. according to the method for the described non-hydrolytic sol of claim 2-gel process preparing stabilizing aluminum titanate at low temperature, it is characterized in that with the molysite being that the processing step that stablizer prepares stabilizing aluminum titanate is: under the ice-water bath condition, measure TiCl4 with valinche, it is slowly joined in the anhydrous low-carbon alcohol that is dissolved with molysite in advance, add AlCl3 again, then 75 ℃ of reactions to forming homogeneous phase presoma mixed solution, by just directly forming xerogel after 110 ℃ of gelations, xerogel grinds after 750 ℃ of calcinings obtain stablizing aluminium titanates.
4. according to the method for the described non-hydrolytic sol of claim 2-gel process preparing stabilizing aluminum titanate at low temperature, it is characterized in that with the magnesium salts being that the processing step that stablizer prepares stabilizing aluminum titanate is: the Erlenmeyer flask that low-carbon alcohol will be housed places ice-water bath, measures TiCl with valinche
4, and slowly join in the low-carbon alcohol, add AlCl again
3Then 75 ℃ of reactions to forming homogeneous presoma mixed solution, form wet gel through 110 ℃ of ageings, after wet gel dissolves with methylene dichloride, add magnesium salts, pass through 50 ℃ of back flow reaction again to gelation, 110 ℃ of dry backs form xerogel, the grinding of xerogel process and 750 ℃ of thermal treatments and just obtain stable aluminium titanates;
5. according to the method for the described non-hydrolytic sol of claim 2-gel process preparing stabilizing aluminum titanate at low temperature, it is characterized in that with molysite and magnesium salts compound being that the processing step that stablizer prepares stabilizing aluminum titanate is: processing step is described with claim 3, different is earlier molysite to be dissolved in the anhydrous low-carbon alcohol, and then adds TiCl
4
6. according to the method for claim 3 or 5 described non-hydrolytic sol-gel process preparing stabilizing aluminum titanate at low temperature, it is characterized in that wherein ferrite is wherein a kind of of methyl alcohol iron, ethanol iron, Virahol iron or propyl carbinol iron, anhydrous organic acid iron is anhydrous formic acid iron or Glacial acetic acid iron.
7. according to the method for claim 4 or 5 described non-hydrolytic sol-gel process preparing stabilizing aluminum titanate at low temperature, it is characterized in that wherein magnesium alkoxide is wherein a kind of of magnesium methylate, magnesium ethylate, magnesium isopropoxide, propyl carbinol magnesium and tert-butyl alcohol magnesium, anhydrous organic acid magnesium is anhydrous formic acid magnesium or Glacial acetic acid magnesium.
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Cited By (5)
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|---|---|---|---|---|
| CN102424417A (en) * | 2011-09-02 | 2012-04-25 | 景德镇陶瓷学院 | Method for preparing stabilized aluminium titanate superfine powder by sol-gel technology under low temperature and product prepared therefrom |
| CN102432286A (en) * | 2011-09-02 | 2012-05-02 | 景德镇陶瓷学院 | Aluminum titanate powder prepared by taking metal aluminum as aluminum source through non-hydrolytic sol-gel process at low temperature and preparation method thereof |
| CN109663594A (en) * | 2019-01-23 | 2019-04-23 | 景德镇陶瓷大学 | It is a kind of that MgFe is prepared using non-hydrolytic sol-gel process2O4The method of/C-material and its material obtained |
| CN111892083A (en) * | 2020-08-21 | 2020-11-06 | 景德镇陶瓷大学 | Preparation method of novel high-temperature-resistant stable aluminum titanate-based ceramic pigment and product prepared by preparation method |
| CN112044368A (en) * | 2020-08-21 | 2020-12-08 | 航天特种材料及工艺技术研究所 | Low-density blocky alumina composite aerogel based on non-hydrolytic sol-gel technology and preparation method thereof |
Family Cites Families (3)
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| US4915887A (en) * | 1988-04-04 | 1990-04-10 | Corning Incorporated | Method of preparing high temperature low thermal expansion ceramic |
| CN100430321C (en) * | 2006-01-12 | 2008-11-05 | 景德镇陶瓷学院 | Method for preparing modified aluminium titanate material |
| CN100371246C (en) * | 2006-01-27 | 2008-02-27 | 王洪增 | High melt polymeric material |
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| CN102424417A (en) * | 2011-09-02 | 2012-04-25 | 景德镇陶瓷学院 | Method for preparing stabilized aluminium titanate superfine powder by sol-gel technology under low temperature and product prepared therefrom |
| CN102432286A (en) * | 2011-09-02 | 2012-05-02 | 景德镇陶瓷学院 | Aluminum titanate powder prepared by taking metal aluminum as aluminum source through non-hydrolytic sol-gel process at low temperature and preparation method thereof |
| CN102432286B (en) * | 2011-09-02 | 2013-07-17 | 景德镇陶瓷学院 | Preparation method of aluminum titanate powder by taking metal aluminum as aluminum source through non-hydrolytic sol-gel process at low temperature |
| CN109663594A (en) * | 2019-01-23 | 2019-04-23 | 景德镇陶瓷大学 | It is a kind of that MgFe is prepared using non-hydrolytic sol-gel process2O4The method of/C-material and its material obtained |
| CN111892083A (en) * | 2020-08-21 | 2020-11-06 | 景德镇陶瓷大学 | Preparation method of novel high-temperature-resistant stable aluminum titanate-based ceramic pigment and product prepared by preparation method |
| CN112044368A (en) * | 2020-08-21 | 2020-12-08 | 航天特种材料及工艺技术研究所 | Low-density blocky alumina composite aerogel based on non-hydrolytic sol-gel technology and preparation method thereof |
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