CN102924080B

CN102924080B - Technology for producing aluminium titanate material

Info

Publication number: CN102924080B
Application number: CN201210529809.4A
Authority: CN
Inventors: 袁三平
Original assignee: Qingdao Samuels Industrial & Commercial Co Ltd
Current assignee: Qingdao Samuels Industrial & Commercial Co Ltd
Priority date: 2012-12-11
Filing date: 2012-12-11
Publication date: 2015-01-21
Anticipated expiration: 2032-12-11
Also published as: CN102924080A

Abstract

A technology for producing an aluminium titanate material comprises the following steps that: (1) raw materials of TiO2 and Al2O3 and additives of Fe2O3 and SiO2 powders are prepared, and the molar ratio of all the components is that TiO2 to Al2O3 to Fe2O3 to SiO2 is (42.5-49.5%): (42.5-49.5%): (0.5-6%): (0.5-9%), and the molar ratio of TiO2 to Al2O3 is 1:1; (2) the weighed raw materials and additives are mixed with each other, 5-10% of polyvinyl alcohol is added into a mashed mixture; (3) the mixture of the step (2) is dried until the humidity is 3%-6%, a compression molding method is adopted to produce the mashed mixture into a cylindrical compression blank with the diameter of phi 20mm and the height of 5-30mm, and the compression blank is put in a drying oven of 100 DEG C to be thermally insulated for 4-6 hours or is dried for 24 hours in the room temperature environment; and (4) the compression blank of the step (3) is put in a high temperature resistance furnace to be heated to 400 DEG C and 1450 DEG C, so that the aluminium titanate material is synthesized.

Description

A kind of technique preparing material of aluminum titanate

Technical field

The present invention relates to a kind of low-thermal-expansion, resistant to elevated temperatures aluminium titanates (Al ₂tiO ₅) preparation method of material, belong to materials synthesis and processing ceramic field.

Background technology

Material of aluminum titanate is the type material integrating low-expansion coefficient and high-melting-point, it is the one that in current low-expansion material, resistance to elevated temperatures is best, in addition, it also has that thermal conductivity is low, anti-slag, anti-corrosion, alkaline-resisting and not wetting property to various metals and glass, the environment of the conditional request harshnesses such as anti-thermal shock, high temperature resistant, wear-resistant, anticorrosive, alkali resistant can be widely used in, particularly require the occasion of highly heatproof and shockproof.

No. WO2005/018776, world patent discloses a kind of alkali feldspar by interpolation 1 ~ 10 massfraction, containing the oxide compound of Mg spinel structure or MgO or the al titanate sintering body that undertaken sintering by the raw mixture containing Mg compound that sintering transforms MgO and formed.

No. 2005-519834, Japanese Patent discloses by adjustment at TiO ₂source power and Al ₂o ₃the kind of additive, composition and addition in source power, obtain while the original thermotolerance of maintenance and low-expansion coefficient advantage, and the problem of its thermolysis, low mechanical strength obtains the aluminium titanates technology improved.

Above patent is all improve the thermolysis of aluminium titanates own and the low performance of physical strength by different methods, but but exists following not enough:

(1) innovative approach of just single aspect, effect is also not obvious.

(2) select additive aspect, additive is more single and be not optimum additive, and additive is too complicated, will certainly affect the low expansion of aluminium titanates like this.

(3) additives ratio does not well control within the scope not affecting aluminium titanates excellent properties.

Summary of the invention

The present invention is directed to the above-mentioned deficiency of prior art, propose a kind of preparation method of aluminium titanates, be included in and keep suitable TiO ₂source power and Al ₂o ₃while source power particle diameter, add the Fe that molar fraction is appropriate ₂o ₃and SiO ₂as additive.Fe ₂o ₃significantly can suppress the thermolysis of aluminium titanates, improve the stability of aluminium titanates.This is owing to adding Fe ³⁺the Fe formed ₂tiO ₅and Al ₂tiO ₅belong to pseudobrookite compound together, continuous solid solution Al can be formed _{2 (1-x)}fe _2xtiO ₅, the thermolysis of aluminium titanates can be suppressed preferably.And do not affect the thermal expansivity of aluminium titanates.Add SiO ₂the stability that can not only improve aluminium titanates suppresses the thermolysis of aluminium titanates, and can improve its physical strength, but add-on is too high, the Al that will produce with aluminium titanate decomposes ₂o ₃form mullite and thermal expansivity is increased, thus will keep certain proportional range.Especially, both employings compound can play better effect, thus better can reduce crackle, improves the intensity of aluminium titanates and can be good at suppressing the thermolysis of aluminium titanates.The aluminium titanates obtained is suitable for being used as stupalith.

The invention provides a kind of by TiO ₂powder and Al ₂o ₃the additional a certain amount of oxide addition (Fe of powder ₂o ₃, SiO ₂, MgO etc.) material of aluminum titanate that synthesizes.

Aluminium titanates of the present invention is with TiO ₂powder and Al ₂o ₃powder is main raw material, oxide addition be auxiliary material for improving the high-temperature behavior of aluminium titanates, as suppressed its thermolysis, reduce crackle and improve intensity etc.; Under the prerequisite ensureing its lower thermal expansivity, physical strength obtains corresponding raising.

Material of aluminum titanate of the present invention is prepared by following steps:

(1) TiO is got ready ₂and Al ₂o ₃raw material and additive Fe ₂o ₃and SiO ₂powder, wherein: described TiO ₂raw material is chemical pure level, Al ₂o ₃raw material is technical pure level, and the molar percentage of each component is:

TiO ₂：42.5－49.5%：

Al ₂O ₃：42.5－49.5%：

Fe ₂o ₃: 0.5-6%: preferably 3% ~ 4%

SiO ₂: 0.5-9%: preferably 3% ~ 5%

And TiO ₂and Al ₂o ₃mol ratio be 1:1;

(2) adopt wet-mixed, in said components, namely add the PVA of 5 ~ 10%, wet-mixed becomes pureed mixture;

(3) mixture of step (2) is dried to humidity 3% ~ 6%, adopt compression-moulding methods, above-mentioned pureed mixture is made the cylindrical pressure embryo of Φ 20mm, high 5 ~ 30mm, 4 ~ 6 hours are incubated in the loft drier of 100 DEG C, control to be 50 DEG C/h from room temperature to the temperature rise rate of 100 DEG C, or drying at room temperature 24 hours;

(4) the pressure embryo of step (3) being put into high temperature resistance furnace, is 20 ~ 50 DEG C/h from room temperature to 400 DEG C of stage temperature rise rates, and 400 DEG C ~ 1450 DEG C temperature rise rates are 150 DEG C ~ 250 DEG C/h, and is incubated 3 ~ 5 hours at 1450 DEG C, synthesis material of aluminum titanate.

Embodiment

The present invention can be understood further below by specific embodiment.

Embodiment 1:

(1) chemical pure TiO is got ready ₂and industrial pure Al ₂o ₃and oxide addition (Fe ₂o ₃, SiO ₂) powder, wherein: the mol ratio of each feed composition is: TiO ₂: Al ₂o ₃: Fe ₂o ₃: SiO ₂=49:49:1:1.

(2) adopt wet-mixed, the PVA wet-mixed adding 10% by load weighted mixed powder becomes pureed mixture.

Etc. (3) mixture of (2) gained is dried to humidity when being 5%, adopt compression-moulding methods, above-mentioned pureed mixture is made the cylindrical pressure embryo of Φ 20mm, high 25mm, then pressure embryo is incubated 5 hours in the loft drier of 100 DEG C, wherein room temperature is 50 DEG C/h to the temperature rise rate of 100 DEG C.

(4) pressure embryo dried in (3) is put into high temperature resistance furnace, set heating schedule: room temperature is 50 DEG C/h to 400 DEG C of stage temperature rise rates, 400 DEG C ~ 1450 DEG C temperature rise rates are 200 DEG C/h, and at 1450 DEG C, are incubated 3 hours, to ensure to synthesize material of aluminum titanate completely.Product performance are as table 1.

Table 1

Embodiment 2

Be TiO by the proportioning of raw material and oxide addition ₂: Al ₂o ₃: Fe ₂o ₃: SiO ₂=42.5%:42.5%:6%:9%.Other processes are with embodiment 1.Obtained product performance are as table 2.

Table 2

Embodiment 3

TiO is changed into by the proportioning of raw material and oxide addition ₂: Al ₂o ₃: Fe ₂o ₃: SiO ₂=46%:46%:3%:5%.Other processes are with embodiment 1.Obtained product performance are as table 3.

Table 3

Claims

1. a preparation method for material of aluminum titanate, comprises the following steps:

(1) TiO is got ready ₂and Al ₂o ₃raw material and additive Fe ₂o ₃and SiO ₂powder, wherein: the molar percentage of each component is,

TiO ₂?：48%?；

Al ₂O ₃?：48%?；

Fe ₂O ₃?：1%?；

SiO ₂?：?3%?；

(2) by load weighted raw material and additive mixing, the PVA adding 5 ~ 10% makes pureed mixture;

(3) mixture of step (2) being dried to humidity is 3% ~ 6%, adopt compression-moulding methods, described pureed mixture is made the cylindrical pressure embryo of Φ 20mm, high 5 ~ 30mm, in the loft drier of 100 DEG C, be incubated 4 ~ 6 hours, or under room temperature environment dry 24 hours;

(4) the pressure embryo of step (3) is put into high temperature resistance furnace, be warming up to 400 DEG C ~ 1450 DEG C, synthesis material of aluminum titanate, described temperature-rise period is first from room temperature to 400 DEG C, temperature rise rate is 20 ~ 50 DEG C/h, be warming up to 1450 DEG C from 400 DEG C again, temperature rise rate is 150 DEG C ~ 250 DEG C/h, and is incubated 3 ~ 5 hours at 1450 DEG C.

2. according to the preparation method of material of aluminum titanate described in claim 1, it is characterized in that, described TiO ₂raw material is chemical pure level, Al ₂o ₃raw material is technical pure level.

3., according to the preparation method of material of aluminum titanate described in claim 1, it is characterized in that, in described step (3) from room temperature to the temperature rise rate of 100 DEG C be 50 DEG C/h.