A kind of is that the non-hydrolytic sol-gel process low temperature in aluminium source prepares the method for aluminium titanates powder 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 that the non-hydrolytic sol-gel process low temperature in aluminium source prepares the method for aluminium titanates powder 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 by regulating pH value, and control technology is complexity, and synthesis temperature is about 1300 ℃ (see Y. X. Huang, Materials Research Bulletin, 2002, Vol. 37, P99~111) generally; It is tiny that sol-gel method has a particle, be uniformly dispersed, advantages such as stoichiometry is easy to control, but its used precursor material mostly is expensive metal alkoxide greatly, for this reason, it is the method that the synthetic aluminium titanates of hydrolyzed collosol-gelatin technology is used in the aluminium source 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 by 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 that the non-hydrolytic sol-gel process low temperature in aluminium source prepares the method for aluminium titanates powder with the metallic aluminium that the technical problem to be solved in the present invention provides a kind of.
For solving above technical problem, technical scheme of the present invention is: a kind of is that the non-hydrolytic sol-gel process low temperature in aluminium source prepares the method for aluminium titanates powder with the metallic aluminium, be presoma with metallic aluminium and titanium tetrachloride, be oxygen donor with the anhydrous low-carbon alcohol, with Anhydrous Ferric Chloride, Aluminum chloride anhydrous, the anhydrous chlorides of rase zirconium, in Magnesium Chloride Anhydrous and the iodine one or more are catalyzer, described metallic aluminium, titanium tetrachloride, low-carbon alcohol and catalyzer, by 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;
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 backflow certain hour under the condition of oil bath heating is formed wet gel, after super-dry, obtain xerogel;
(4) the aluminium titanates xerogel obtains the aluminium titanates powder through grinding, calcining;
The preferred dehydrated alcohol of described low-carbon alcohol, propyl carbinol or Virahol.
Described metallic aluminium is aluminium powder, aluminium bits or aluminium flake.
Described reflux temperature is 70~130 ℃, and return time is 7~24 hours.
The calcining temperature of described 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 by non-hydrolytic sol-gel process at 750 ℃.Compare with using aluminium-alcohol salt or inorganic aluminate, the metallic aluminium cost is lower, and easier preservation and weighing, improves the synthetic effect of aluminium titanates.
Description of drawings
Fig. 1 is process flow sheet of the present invention.
Embodiment
The present invention is further detailed explanation below in conjunction with accompanying drawing 1 and embodiment.
Embodiment 1
Take by weighing the 1.9683g aluminium powder and put into the dry Erlenmeyer flask that the 22ml dehydrated 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 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, through 750 ℃ of insulations thermal treatment in 30 minutes, namely obtain aluminium titanates powder of the present invention.
Embodiment 2
Take by weighing the 1.9683g aluminium powder and put into the dry Erlenmeyer flask that the 22ml dehydrated 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 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, through 750 ℃ of insulations thermal treatment in 60 minutes, namely obtain aluminium titanates powder of the present invention.
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 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, through 750 ℃ of insulations thermal treatment in 60 minutes, namely obtain aluminium titanates powder of the present invention.
Embodiment 4
Take by weighing the 2.948g aluminium powder and put into the dry Erlenmeyer flask that the 40ml dehydrated 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 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, namely 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 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, through 750 ℃ of insulations thermal treatment in 30 minutes, namely obtain aluminium titanates powder of the present invention.
Embodiment 6
Take by weighing the 2.948g aluminium powder and put into the dry Erlenmeyer flask that the 80ml dehydrated 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 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, through 750 ℃ of insulations thermal treatment in 30 minutes, namely obtain aluminium titanates powder of the present invention.
Embodiment 7
Take by weighing the 2.948g aluminium powder and put into the dry Erlenmeyer flask that the 80ml dehydrated 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 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, through 750 ℃ of insulations thermal treatment in 30 minutes, namely obtain aluminium titanates powder of the present invention.