A kind of is the aluminium titanates powder and preparation method thereof of the non-hydrolytic sol-gel process low temperature preparation in aluminium source with the metallic aluminium
Technical field
The present invention relates to the ceramic powder preparing technical field, being specifically related to a kind of is the aluminium titanates powder and preparation method thereof of the non-hydrolytic sol-gel process low temperature preparation in aluminium source with the metallic aluminium.
Background technology
Aluminium titanates integrates low bulk and high temperature resistant premium properties; Also have the fusing point height simultaneously, thermal conductivity is low, the coefficient of expansion is little, good thermal shock, erosion resistance be by force and to characteristics such as multiple metal and glass melt do not soak into, have a extensive future in fields such as iron and steel, non-ferrous metal, glass, chemical industry, automobile, war industrys.The aluminium titanates powder is the important starting material of preparation aluminum titanate ceramic material.Selecting cheap reaction raw materials for use, reduce the synthesis temperature of aluminium titanates powder, thereby reach the purpose that reduces production costs, is that aluminum titanate ceramic material can realize industrialization and the key of being used widely.The method for preparing at present the aluminium titanates powder mainly contains solid phase method, combustion method, coprecipitation method, hydrolytic sol-gel process, non-hydrolytic sol-gel process etc.It is raw material that solid phase method directly adopts solid alumina and titanium oxide, generally needs after the mechanically mixing could synthesize the aluminium titanates powder through 1400~1500 ℃ of calcinings; Combustion method need add a large amount of fuel and synthesize aluminium titanates institute energy requirement to provide, and synthesis temperature is more than 1300 ℃; Coprecipitation method need make aluminium, titanium ion precipitation from homogeneous solution through regulating pH value, and CONTROL PROCESS is complicacy, and synthesis temperature generally (is seen Y.X.Huang, Materials Research Bulletin, 2002, Vol.37, P99~111) about 1300 ℃; It is tiny that sol-gel method has a particle, is uniformly dispersed, advantage such as stoichiometry is easy to control; But its used precursor material is expensive metal alkoxide mostly; For this reason, it is the method for the synthetic aluminium titanates of aluminium source hydrolysed sol-gel technology with the inorganic salt aluminum nitrate that this seminar discloses a kind of in ZL200610005317.X, and it compares to uses aluminium-alcohol salt to do the aluminium source; Raw materials cost obviously reduces, but synthesis temperature is up to 1350 ℃; It is the non-hydrolytic sol-gel process of precursor material with inorganic salt aluminum chloride and titanium tetrachloride that this seminar discloses a kind of in ZL200610005316.5; Make the synthesis temperature of aluminium titanates be reduced to 750 ℃; But must use Aluminum chloride anhydrous as the aluminium source; And Aluminum chloride anhydrous suction easily itself, it both had been difficult for preservation and also had been not easy to weighing.The present invention directly utilizes metallic aluminium to do the aluminium source, causes non-hydrolytic sol-gel reaction through adding catalyzer, prepares the aluminium titanates powder at 750 ℃ of low temperature, and this is an innovation research achievement of not seeing domestic and international any bibliographical information so far.
Summary of the invention
It is the aluminium source with cheap metal aluminium that the technical problem that the present invention will solve provides a kind of, aluminium titanates powder that preparation technology is simple, synthesis temperature is low and preparation method thereof.
For solving above technical problem; Technical scheme of the present invention is: a kind of is the aluminium titanates powder of the non-hydrolytic sol-gel process low temperature preparation in aluminium source with the metallic aluminium; With metallic aluminium and titanium tetrachloride is presoma; With the anhydrous low-carbon alcohol is oxygen donor, is catalyzer with in Anhydrous Ferric Chloride, Aluminum chloride anhydrous, anhydrous chlorides of rase zirconium, Magnesium Chloride Anhydrous and the iodine one or more, said metallic aluminium, titanium tetrachloride, low-carbon alcohol and catalyzer; Pressed mole per-cent 2: 1: (8~38): (0.01~0.25), adopt the synthetic aluminium titanates powder that obtains of non-hydrolytic sol-gel process low temperature.
Said metallic aluminium is aluminium powder, aluminium bits or aluminium flake.
The preferred absolute ethyl alcohol of described low-carbon alcohol, propyl carbinol or Virahol.
The preparation method of above-mentioned aluminium titanates powder may further comprise the steps:
(1) in stink cupboard, measure a certain amount of low-carbon alcohol and put into dry wide-necked bottle, wide-necked bottle is placed cooling bath, add amount of metallic aluminum then therein;
(2) measure a certain amount of titanium tetrachloride by the stoichiometric ratio of aluminium titanates with transfer pipet, slowly it is splashed in the wide-necked bottle that fills low-carbon alcohol and metallic aluminium, the back that stirs adds a certain amount of catalyzer, finally forms the presoma mixed solution;
(3) precursor mixed solution is formed wet gel at the condition refluxed certain hour of oil bath heating, after super-dry, obtain xerogel;
(4) the aluminium titanates xerogel obtains the aluminium titanates powder through grinding, calcining.
Said reflux temperature is 70~130 ℃, and return time is 7~24 hours.
The calcining temperature of said dry gel powder is 750 ℃, is incubated 30~60 minutes.
The present invention adopts metallic aluminium as the aluminium source in the world first; Ingenious hydrogen chloride emission and the catalyzer that utilizes titanium tetrachloride and low-carbon alcohol reaction to form; Impel the activation of metallic aluminium, make it be converted into aluminum chloride, successfully prepare the aluminium titanates powder at 750 ℃ through non-hydrolytic sol-gel process.Compare with using aluminium-alcohol salt or inorganic aluminate, the metallic aluminium cost is lower, and more is prone to preserve and weighing, improves the synthetic effect of aluminium titanates.
Description of drawings
Fig. 1 is a process flow sheet of the present invention
Embodiment
Below in conjunction with accompanying drawing 1 and embodiment the present invention is done further detailed explanation.
Embodiment 1
Take by weighing the 1.9683g aluminium powder and put into the dry Erlenmeyer flask that the 22ml absolute ethyl alcohol is housed; Measure the 4ml titanium tetrachloride with transfer pipet by the stoichiometric ratio of aluminium titanates and slowly splash into this Erlenmeyer flask; Add 0.59g iron(ic)chloride again, after the vigorous stirring this Erlenmeyer flask is put into 80 ℃ of oil baths, condensing reflux 7h; Obtain the aluminium titanates precursor mixture, obtain the aluminium titanates dry gel powder through 3 hours infrared dryings.Dry gel powder is ground,, promptly obtain aluminium titanates powder of the present invention through 750 ℃ of insulations thermal treatment in 30 minutes.
Embodiment 2
Take by weighing the 1.9683g aluminium powder and put into the dry Erlenmeyer flask that the 22ml absolute ethyl alcohol is housed; Measure the 4ml titanium tetrachloride with transfer pipet by the stoichiometric ratio of aluminium titanates and slowly splash into this Erlenmeyer flask; Add 0.95g aluminum chloride again, after the vigorous stirring this Erlenmeyer flask is put into 110 ℃ of oil baths, condensing reflux 15h; Obtain the aluminium titanates precursor mixture, obtain the aluminium titanates dry gel powder through 3 hours infrared dryings.Dry gel powder is ground,, promptly obtain aluminium titanates powder of the present invention through 750 ℃ of insulations thermal treatment in 60 minutes.
Embodiment 3
Take by weighing the 1.9683g aluminium powder and put into the dry Erlenmeyer flask that the 24ml anhydrous isopropyl alcohol is housed; Measure the 4ml titanium tetrachloride with transfer pipet by the stoichiometric ratio of aluminium titanates and slowly splash into this Erlenmeyer flask; Add 0.1g iodine again, after the vigorous stirring this Erlenmeyer flask is put into 130 ℃ of oil baths, condensing reflux 24h; Obtain the aluminium titanates precursor mixture, obtain the aluminium titanates dry gel powder through 3 hours infrared dryings.Dry gel powder is ground,, promptly obtain aluminium titanates powder of the present invention through 750 ℃ of insulations thermal treatment in 60 minutes.
Embodiment 4
Take by weighing the 2.948g aluminium powder and put into the dry Erlenmeyer flask that the 40ml absolute ethyl alcohol is housed; Measure the 6ml titanium tetrachloride with transfer pipet by the stoichiometric ratio of aluminium titanates and slowly splash into this Erlenmeyer flask; Add 1.2g aluminum chloride again, after the vigorous stirring this Erlenmeyer flask is put into 80 ℃ of oil baths, condensing reflux 15h; Obtain the aluminium titanates precursor mixture, obtain the aluminium titanates dry gel powder through 3 hours infrared dryings.Dry gel powder is ground, promptly obtain aluminium titanates powder of the present invention.
Embodiment 5
Take by weighing the 2.948g aluminium powder and put into the dry Erlenmeyer flask that the 80ml propyl carbinol is housed; Measure the 6ml titanium tetrachloride with transfer pipet by the stoichiometric ratio of aluminium titanates and slowly splash into this Erlenmeyer flask; Add 0.18g iodine again, after the vigorous stirring this Erlenmeyer flask is put into 80 ℃ of oil baths, condensing reflux 15h; Obtain the aluminium titanates precursor mixture, obtain the aluminium titanates dry gel powder through 3 hours infrared dryings.Dry gel powder is ground,, promptly obtain aluminium titanates powder of the present invention through 750 ℃ of insulations thermal treatment in 30 minutes.
Embodiment 6
Take by weighing the 2.948g aluminium powder and put into the dry Erlenmeyer flask that the 80ml absolute ethyl alcohol is housed; Measure the 6ml titanium tetrachloride with transfer pipet by the stoichiometric ratio of aluminium titanates and slowly splash into this Erlenmeyer flask; Add 0.3g iodine and 0.4g zirconium chloride again, after the vigorous stirring this Erlenmeyer flask is put into 110 ℃ of oil baths, condensing reflux 15h; Obtain the aluminium titanates precursor mixture, obtain the aluminium titanates dry gel powder through 3 hours infrared dryings.Dry gel powder is ground,, promptly obtain aluminium titanates powder of the present invention through 750 ℃ of insulations thermal treatment in 30 minutes.
Embodiment 7
Take by weighing the 2.948g aluminium powder and put into the dry Erlenmeyer flask that the 80ml absolute ethyl alcohol is housed; Measure the 6ml titanium tetrachloride with transfer pipet by the stoichiometric ratio of aluminium titanates and slowly splash into this Erlenmeyer flask; Add 1.7g aluminum chloride and 0.65g magnesium chloride again, after the vigorous stirring this Erlenmeyer flask is put into 80 ℃ of oil baths, condensing reflux 15h; Obtain the aluminium titanates precursor mixture, obtain the aluminium titanates dry gel powder through 3 hours infrared dryings.Dry gel powder is ground,, promptly obtain aluminium titanates powder of the present invention through 750 ℃ of insulations thermal treatment in 30 minutes.