CN106747414B - Microporous calcium titanium aluminate raw material and preparation method thereof - Google Patents

Microporous calcium titanium aluminate raw material and preparation method thereof Download PDF

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CN106747414B
CN106747414B CN201611160685.1A CN201611160685A CN106747414B CN 106747414 B CN106747414 B CN 106747414B CN 201611160685 A CN201611160685 A CN 201611160685A CN 106747414 B CN106747414 B CN 106747414B
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raw material
microporous calcium
calcium titanium
mixture
titanium aluminate
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CN106747414A (en
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张寒
陈建威
赵惠忠
李静捷
赵鹏达
易萍
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JINZHOU GUOTAI INDUSTRIAL Co.,Ltd.
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Wuhan University of Science and Engineering WUSE
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
    • C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
    • C04B35/465—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
    • C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
    • C04B35/478—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on aluminium titanates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
    • C—CHEMISTRY; METALLURGY
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    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
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    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/78—Grain sizes and shapes, product microstructures, e.g. acicular grains, equiaxed grains, platelet-structures
    • C04B2235/786—Micrometer sized grains, i.e. from 1 to 100 micron

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Abstract

The invention relates to a microporous calcium titanium aluminate raw material and a preparation method thereof. The technical scheme is as follows: adding bauxite and rutile into a stirrer according to the mass ratio of the bauxite to the rutile of (1-1.05) to 1, and stirring for 0.3-0.5 hours to obtain a mixture; adding the mixture into an electric arc furnace, heating to 1500-1600 ℃, and preserving heat for 20-30 minutes; then adding limestone into the electric arc furnace, heating to 1630-1650 ℃, and preserving heat for 20-30 minutes; removing the upper layer scum, cooling to room temperature along with the furnace, and crushing to obtain the microporous calcium titanium aluminate raw material. The addition amount of the limestone is 20-25 wt% of the mixture. The preparation process is simple and the production cost is low; the prepared microporous calcium titanium aluminate raw material has the characteristics of high purity and good crystallization.

Description

Microporous calcium titanium aluminate raw material and preparation method thereof
Technical Field
The invention belongs to the technical field of calcium titanium aluminate. In particular to a microporous calcium titanium aluminate raw material and a preparation method thereof.
Background
The calcium titanium aluminate being Al2O3、TiO2And CaO under high temperature conditions, has the characteristics of high temperature resistance, corrosion resistance, low heat conduction and the like, and is widely applied to the field of refractory materials. Such as ' a ladle bottom castable and a preparation method thereof ' (201510311418.9) ' a titanium calcium aluminate-high bauxite modified refractory material and a preparation method and application thereof ' (201510013589.3) ' a titanium calcium aluminate prefabricated part for vanadium-smelting reverberatory furnace lining and a preparation method thereof ' (201510469732. X) ', and other technologies, the titanium calcium aluminate and a binding agent are mainly mixed, molded and sintered to obtain a finished refractory material.
At present, the preparation of high-purity, large-crystal and single-phase calcium titanium aluminate raw materials, especially the preparation of microporous calcium titanium aluminate raw materials, mostly adopts an additive loss-by-ignition method, i.e. air holes are formed by escaping loss-by-ignition materials under the condition of high temperature. Although the additive loss-by-ignition method has the advantages, in the high-temperature sintering process, the diffusion between solid phases is slow, so that the growth and development of crystal grains are incomplete, and the purity and the grain size of the microporous raw material are reduced.
Disclosure of Invention
The invention aims to provide a preparation method of a microporous calcium titanium aluminate raw material, which has simple process and low production cost. The microporous calcium titanium aluminate prepared by the method has high purity and good crystallization.
In order to achieve the purpose, the invention adopts the technical scheme that: adding bauxite and rutile into a stirrer according to the mass ratio of the bauxite to the rutile of (1-1.05) to 1, and stirring for 0.3-0.5 hours to obtain a mixture; adding the mixture into an electric arc furnace, heating to 1500-1600 ℃, and preserving heat for 20-30 minutes; then adding limestone into the electric arc furnace, heating to 1630-1650 ℃, and preserving heat for 20-30 minutes; removing the upper layer scum, cooling to room temperature along with the furnace, and crushing to obtain the microporous calcium titanium aluminate raw material.
The addition amount of the limestone is 20-25 wt% of the mixture.
The bauxite comprises the following chemical components: al (Al)2O3The content is more than or equal to 90 wt%; SiO 22The content is 5-8 wt%; the MgO content is less than or equal to 0.5wt percent.
TiO of the rutile2The content is more than or equal to 95 wt%.
CaCO of said limestone3The content is more than or equal to 95 wt%.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following positive effects:
1. the invention adopts bauxite, limestone and other minerals as raw materials, has rich mineral reserves and low cost, and reduces the production cost of the microporous calcium titanium aluminate raw material.
2. The method improves the purity of the microporous calcium titanium aluminate raw material through the solid solution reaction of the raw material components, and remarkably improves the grain size and the content of the microporous calcium titanium aluminate raw material by combining the liquid phase mass transfer process of an electric melting method.
The microporous calcium titanium aluminate raw material prepared by the invention is detected as follows: the content of the calcium titanium aluminate is 85-90 wt%; the grain size is 6 to 11 μm.
Therefore, the preparation process is simple and the production cost is low; the prepared microporous calcium titanium aluminate raw material has the characteristics of high purity and good crystallization.
Detailed Description
The invention will be further described with reference to specific embodiments without limiting the scope of the invention:
in order to avoid repetition, the materials related to this specific embodiment are described in a unified manner, which is not described in the embodiments again:
the bauxite comprises the following chemical components: al (Al)2O3The content is more than or equal to 90 wt%; SiO 22The content is 5-8 wt%; the MgO content is less than or equal to 0.5wt percent.
TiO of the rutile2The content is more than or equal to 95 wt%.
CaCO of said limestone3The content is more than or equal to 95 wt%.
Example 1
A microporous calcium titanium aluminate raw material and a preparation method thereof. Adding bauxite and rutile into a stirrer according to the mass ratio of the bauxite to the rutile of (1-1.02) to 1, and stirring for 0.3-0.5 hours to obtain a mixture; adding the mixture into an electric arc furnace, heating to 1500-1560 ℃, and preserving heat for 20-30 minutes; adding limestone into the electric arc furnace, heating to 1630-1645 ℃, and preserving heat for 20-30 minutes; removing the upper layer scum, cooling to room temperature along with the furnace, and crushing to obtain the microporous calcium titanium aluminate raw material.
The addition amount of the limestone is 20-22 wt% of the mixture.
The microporous calcium titanoaluminate raw material prepared in the embodiment is detected as follows: the content of the calcium titanium aluminate is 85-87 wt%; the grain size is 6-8 μm.
Example 2
A microporous calcium titanium aluminate raw material and a preparation method thereof. Adding bauxite and rutile into a stirrer according to the mass ratio of the bauxite to the rutile of 1.01-1.03: 1, and stirring for 0.3-0.5 hours to obtain a mixture; adding the mixture into an electric arc furnace, heating to 1500-1560 ℃, and preserving heat for 20-30 minutes; adding limestone into the electric arc furnace, heating to 1630-1645 ℃, and preserving heat for 20-30 minutes; removing the upper layer scum, cooling to room temperature along with the furnace, and crushing to obtain the microporous calcium titanium aluminate raw material.
The addition amount of the limestone is 21-23 wt% of the mixture.
The microporous calcium titanoaluminate raw material prepared in the embodiment is detected as follows: the content of the calcium titanium aluminate is 86-88 wt%; the grain size is 7 to 9 μm.
Example 3
A microporous calcium titanium aluminate raw material and a preparation method thereof. Adding bauxite and rutile into a stirrer according to the mass ratio of the bauxite to the rutile of 1.02-1.04 to 1, and stirring for 0.3-0.5 hours to obtain a mixture; adding the mixture into an electric arc furnace, heating to 1540-1600 ℃, and preserving heat for 20-30 minutes; then adding limestone into the electric arc furnace, heating to 1635-1650 ℃, and preserving heat for 20-30 minutes; removing the upper layer scum, cooling to room temperature along with the furnace, and crushing to obtain the microporous calcium titanium aluminate raw material.
The addition amount of the limestone is 22-24 wt% of the mixture.
The microporous calcium titanoaluminate raw material prepared in the embodiment is detected as follows: the content of the calcium titanium aluminate is 87-89 wt%; the grain size is 8-10 μm.
Example 4
A microporous calcium titanium aluminate raw material and a preparation method thereof. Adding bauxite and rutile into a stirrer according to the mass ratio of the bauxite to the rutile of 1.03-1.05: 1, and stirring for 0.3-0.5 hours to obtain a mixture; adding the mixture into an electric arc furnace, heating to 1540-1600 ℃, and preserving heat for 20-30 minutes; then adding limestone into the electric arc furnace, heating to 1635-1650 ℃, and preserving heat for 20-30 minutes; removing the upper layer scum, cooling to room temperature along with the furnace, and crushing to obtain the microporous calcium titanium aluminate raw material.
The addition amount of the limestone is 23-25 wt% of the mixture.
The microporous calcium titanoaluminate raw material prepared in the embodiment is detected as follows: the content of the calcium titanium aluminate is 88-90 wt%; the grain size is 9-11 μm.
Compared with the prior art, the specific implementation mode has the following positive effects:
1. the specific embodiment adopts bauxite, limestone and other minerals as raw materials, so that the mineral reserves are rich, the cost is low, and the production cost of the microporous calcium titanium aluminate raw material is reduced.
2. According to the specific embodiment, the purity of the microporous calcium titanium aluminate raw material is improved through the solid solution reaction of the raw material components, and the grain size and the content of the microporous calcium titanium aluminate raw material are obviously improved by combining the liquid phase mass transfer process of an electric melting method.
The detection of the microporous calcium titanium aluminate raw material prepared by the embodiment is as follows: the content of the calcium titanium aluminate is 85-90 wt%; the grain size is 6 to 11 μm.
Therefore, the preparation process of the embodiment is simple and the production cost is low; the prepared microporous calcium titanium aluminate raw material has the characteristics of high purity and good crystallization.

Claims (4)

1. A preparation method of a microporous calcium titanium aluminate raw material is characterized by comprising the following specific steps:
adding bauxite and rutile into a stirrer according to the mass ratio of the bauxite to the rutile of (1-1.05) to 1, and stirring for 0.3-0.5 hours to obtain a mixture; adding the mixture into an electric arc furnace, heating to 1500-1600 ℃, and preserving heat for 20-30 minutes; then adding limestone into the electric arc furnace, heating to 1630-1650 ℃, and preserving heat for 20-30 minutes; removing the upper layer floating slag, cooling to room temperature along with the furnace, and crushing to obtain the microporous calcium titanium aluminate raw material;
the addition amount of the limestone is 20-25 wt% of the mixture;
TiO of the rutile2The content is more than or equal to 95 wt%.
2. The method for preparing a microporous calcium titanoaluminate raw material according to claim 1, wherein the chemical composition of the bauxite is: al (Al)2O3The content is more than or equal to 90 wt%; SiO 22The content is 5-8 wt%; the MgO content is less than or equal to 0.5wt percent.
3. The method for preparing a microporous calcium titanoaluminate feedstock as claimed in claim 1, wherein said limestone is CaCO3The content is more than or equal to 95 wt%.
4. A microporous calcium titanoaluminate raw material, characterized in that the microporous calcium titanoaluminate raw material is the microporous calcium titanoaluminate raw material prepared by the method for preparing a microporous calcium titanoaluminate raw material according to any one of claims 1 to 3.
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CN107266052B (en) * 2017-07-10 2020-03-24 武汉科技大学 Alumina-titanium calcium aluminate-silicon carbide complex phase refractory material and preparation method thereof
CN111377727B (en) * 2020-03-13 2022-05-27 宜兴摩根热陶瓷有限公司 Titanium-containing calcium hexaluminate material and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN1554778A (en) * 2003-12-26 2004-12-15 张延大 Low-titanium calcium aluminate and its preparing method
CN104861969A (en) * 2015-05-20 2015-08-26 中国科学院新疆理化技术研究所 Aluminum calcium titanate solid-solution type red phosphor and preparation method thereof
CN105859165A (en) * 2016-04-06 2016-08-17 同济大学 Method for preparing high-purity monocalcium aluminate by solid-phase reaction

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1554778A (en) * 2003-12-26 2004-12-15 张延大 Low-titanium calcium aluminate and its preparing method
CN104861969A (en) * 2015-05-20 2015-08-26 中国科学院新疆理化技术研究所 Aluminum calcium titanate solid-solution type red phosphor and preparation method thereof
CN105859165A (en) * 2016-04-06 2016-08-17 同济大学 Method for preparing high-purity monocalcium aluminate by solid-phase reaction

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