CN102432286B - Preparation method of aluminum titanate powder by taking metal aluminum as aluminum source through non-hydrolytic sol-gel process at low temperature - Google Patents

Preparation method of aluminum titanate powder by taking metal aluminum as aluminum source through non-hydrolytic sol-gel process at low temperature Download PDF

Info

Publication number
CN102432286B
CN102432286B CN 201110259047 CN201110259047A CN102432286B CN 102432286 B CN102432286 B CN 102432286B CN 201110259047 CN201110259047 CN 201110259047 CN 201110259047 A CN201110259047 A CN 201110259047A CN 102432286 B CN102432286 B CN 102432286B
Authority
CN
China
Prior art keywords
aluminium
aluminum
powder
aluminium titanates
low
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CN 201110259047
Other languages
Chinese (zh)
Other versions
CN102432286A (en
Inventor
江伟辉
张权
刘健敏
朱庆霞
谭训彦
包镇红
苗立锋
虞澎澎
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jingdezhen Ceramic Institute
Original Assignee
Jingdezhen Ceramic Institute
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jingdezhen Ceramic Institute filed Critical Jingdezhen Ceramic Institute
Priority to CN 201110259047 priority Critical patent/CN102432286B/en
Publication of CN102432286A publication Critical patent/CN102432286A/en
Application granted granted Critical
Publication of CN102432286B publication Critical patent/CN102432286B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Landscapes

  • Inorganic Compounds Of Heavy Metals (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

The invention discloses aluminum titanate powder prepared by taking metal aluminum as an aluminum source through a non-hydrolytic sol-gel process at a low temperature and a preparation method thereof. The metal aluminum and titanium tetrachloride are used as precursor raw materials, anhydrous low-carbon alcohol is used as an oxygen donor, and a proper catalyst is selected to prepare the aluminum titanate powder at the low temperature of 750 DEG C. According to the invention, the metal aluminum is utilized to replace aluminum alkoxide and inorganic aluminum salt as the aluminum source, so the preparation method disclosed by the invention has the outstanding advantages of cheap reaction raw material, simple process, low synthesis temperature and the like, and is suitable for industrial mass production.

Description

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.

Claims (2)

1. one kind is that the non-hydrolytic sol-gel process low temperature in aluminium source prepares the method for aluminium titanates powder with the metallic aluminium, it is characterized in that: be presoma with metallic aluminium and titanium tetrachloride, anhydrous low-carbon alcohol is oxygen donor, in Anhydrous Ferric Chloride, Aluminum chloride anhydrous, anhydrous chlorides of rase zirconium, 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.
2. the method for preparing the aluminium titanates powder according to claim 1 is characterized in that: described metallic aluminium is aluminium powder, aluminium bits or aluminium flake.
3, the method for preparing the aluminium titanates powder according to claim 1 is characterized in that: described reflux temperature is 70~130 ℃, and return time is 7~24 hours.
4, the method for preparing the aluminium titanates powder according to claim 1 is characterized in that: the calcining temperature of described dry gel powder is 750 ℃, is incubated 30 ~ 60 minutes.
CN 201110259047 2011-09-02 2011-09-02 Preparation method of aluminum titanate powder by taking metal aluminum as aluminum source through non-hydrolytic sol-gel process at low temperature Expired - Fee Related CN102432286B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 201110259047 CN102432286B (en) 2011-09-02 2011-09-02 Preparation method of aluminum titanate powder by taking metal aluminum as aluminum source through non-hydrolytic sol-gel process at low temperature

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 201110259047 CN102432286B (en) 2011-09-02 2011-09-02 Preparation method of aluminum titanate powder by taking metal aluminum as aluminum source through non-hydrolytic sol-gel process at low temperature

Publications (2)

Publication Number Publication Date
CN102432286A CN102432286A (en) 2012-05-02
CN102432286B true CN102432286B (en) 2013-07-17

Family

ID=45980682

Family Applications (1)

Application Number Title Priority Date Filing Date
CN 201110259047 Expired - Fee Related CN102432286B (en) 2011-09-02 2011-09-02 Preparation method of aluminum titanate powder by taking metal aluminum as aluminum source through non-hydrolytic sol-gel process at low temperature

Country Status (1)

Country Link
CN (1) CN102432286B (en)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104556216B (en) * 2014-12-29 2016-05-04 景德镇陶瓷学院 A kind of method that adopts non-hydrolytic sol-gel process to prepare Barium Titanate nano-powder
CN105271337B (en) * 2015-10-21 2017-03-08 景德镇陶瓷大学 A kind of method that alumina ultrafine powder body is prepared using non-aqueous depositing technology
CN106045523B (en) * 2016-07-29 2018-07-06 张宁 A kind of method based on Bayer process production aluminum nitride ceramic powder
CN115231904B (en) * 2022-08-03 2023-11-17 景德镇陶瓷大学 Method for preparing ceramic powder by non-solvent replacement non-aqueous precipitation process

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1803718A (en) * 2006-01-12 2006-07-19 景德镇陶瓷学院 Method for synthesizing composite oxide powder by non-hydrolytic sol-gel process with alcohol as oxygen donor
CN101696030A (en) * 2009-08-18 2010-04-21 景德镇陶瓷学院 Method for preparing stabilizing aluminum titanate at low temperature by non-hydrolytic sol-gel process

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1803718A (en) * 2006-01-12 2006-07-19 景德镇陶瓷学院 Method for synthesizing composite oxide powder by non-hydrolytic sol-gel process with alcohol as oxygen donor
CN101696030A (en) * 2009-08-18 2010-04-21 景德镇陶瓷学院 Method for preparing stabilizing aluminum titanate at low temperature by non-hydrolytic sol-gel process

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
江伟辉等.非水解溶胶-凝胶法低温制备铁稳定钛酸铝粉体.《人工晶体学报》.2011,第40卷(第2期),455-469.
非水解溶胶-凝胶法低温制备铁稳定钛酸铝粉体;江伟辉等;《人工晶体学报》;20110430;第40卷(第2期);455-469 *

Also Published As

Publication number Publication date
CN102432286A (en) 2012-05-02

Similar Documents

Publication Publication Date Title
CN102432286B (en) Preparation method of aluminum titanate powder by taking metal aluminum as aluminum source through non-hydrolytic sol-gel process at low temperature
Yang et al. Synthesis of ZrO2/ZrW2O8 composites with low thermal expansion
CN102775141B (en) Method for finely synthesizing ternary ZnO-Nb2O5-TiO2 microwave dielectric ceramics by wet chemical process
CN102626785B (en) Preparation method for rare earth oxide doped tungsten powder
CN108946787A (en) A kind of preparation method of the high entropy oxide powder material of Property of Rare earth based Fluorite Type
Vives et al. Influence of the synthesis route on sol–gel SiO2–TiO2 (1: 1) xerogels and powders
CN100463715C (en) Core-shell structure magnetic microsphere aluminum oxide and method for preparing the same
CN102775985A (en) One method for synthesizing Sr2MgSi2O7nanowire with long afterglow luminescence (Eu2+, dy3+)
CN103864075A (en) Method for catalytically synthesizing calcium carbide
CN102260084A (en) Corundum refractory castable
CN101925538A (en) Process for producing aluminum magnesium titanate
CN101746834B (en) Preparation method of perovskite composite oxide La1-xCaxFeO3 superfines
CN101941731B (en) Preparation method of void type nano-sheet zinc oxide and activated carbon load complex
CN101172661A (en) Method of producing ultra-fine perovskite type LaFeO*, LaMnO*, LaNiO*
CN101508437A (en) Process for producing medium-temperature solid-oxide fuel battery electrolyte material lanthanum silicate powder
CN1285511C (en) Direct synthesis of Y by citric acid combustion method2O3Method for preparing nano material
CN102964128B (en) Sol-gel preparation method of Yb2Si2O7 powder
CN109553315A (en) A method of with high-calcium fly ass and sa clay and/or solid waste preparation ground polymers
CN100355702C (en) Method for synthesizing composite oxide powder by non-hydrolytic sol-gel process with alcohol as oxygen donor
CN101323463B (en) Production process of high pure superfine tin oxide
CN102153144B (en) Method for preparing calcium ferroaluminates
CN101585711A (en) Utilize useless mud of ceramics factory and commercial alumina to prepare the method for high alumina mullite aggregate
CN101696030B (en) Method for preparing stabilizing aluminum titanate at low temperature by non-hydrolytic sol-gel process
CN101967005A (en) Method for preparing neodymium praseodymium fluoride with large granules and large specific surface area
CN101811677B (en) Method for preparing hollow porous quadruped titanium nitride

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
EE01 Entry into force of recordation of patent licensing contract

Application publication date: 20120502

Assignee: JIANGXI SAICI MATERIALS Co.,Ltd.

Assignor: Jingdezhen Ceramic Institute

Contract record no.: 2014360000099

Denomination of invention: Preparation method of aluminum titanate powder by taking metal aluminum as aluminum source through non-hydrolytic sol-gel process at low temperature

Granted publication date: 20130717

License type: Exclusive License

Record date: 20140605

LICC Enforcement, change and cancellation of record of contracts on the licence for exploitation of a patent or utility model
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20130717

CF01 Termination of patent right due to non-payment of annual fee