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CN106495714B - A kind of honeycomb calcium aluminate titanate hollow sphere and preparation method thereof - Google Patents

A kind of honeycomb calcium aluminate titanate hollow sphere and preparation method thereof Download PDF

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CN106495714B
CN106495714B CN201610931554.2A CN201610931554A CN106495714B CN 106495714 B CN106495714 B CN 106495714B CN 201610931554 A CN201610931554 A CN 201610931554A CN 106495714 B CN106495714 B CN 106495714B
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calcium aluminate
powder
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preparation
hollow sphere
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CN106495714A (en
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张寒
赵惠忠
李静捷
余俊
梁永和
聂建华
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Jinzhou Guotai Industrial Co ltd
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Wuhan University of Science and Engineering WUSE
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    • 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
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    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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Abstract

The present invention relates to a kind of honeycomb titanium calcium aluminate hollow spheres and preparation method thereof.Its technical solution is: by ilmenite: rutile: the mass ratio of magnetic iron ore is 100: (3 ~ 13): (5 ~ 15), ilmenite, rutile and magnetic iron ore are mixed, mixed mixed powder is added in electromagnetic induction furnace again, is warming up to 1300 ~ 1400 DEG C, heat preservation；Then press mixed powder: the mass ratio of aluminium powder is 100: (25 ~ 30) aluminium powder is added into electromagnetic induction furnace, is warming up to 1550 ~ 1600 DEG C, heat preservation；Finally press mixed powder: the mass ratio of lime stone powder is 100: (8 ~ 10) lime stone powder is added into electromagnetic induction furnace, is warming up to 1950 ~ 2000 DEG C, heat preservation；Slag is separated from slag-drip opening, it is cooling to get honeycomb titanium calcium aluminate hollow sphere with the compressed air spraying slag of 0.4 ~ 0.8MPa.Present invention process is simple, production cost is low and balling ratio is high；Prepared honeycomb titanium calcium aluminate hollow sphere bulk density is small, thermal conductivity is low and cold conditions compressive resistance is big.

Description

A kind of honeycomb titanium calcium aluminate hollow sphere and preparation method thereof
Technical field
The invention belongs to titanium calcium aluminate hollow sphere technical fields.More particularly to a kind of honeycomb titanium calcium aluminate hollow sphere and its Preparation method.
Background technique
Hollow sphere refractory material is a kind of excellent fireclay insulating refractory, can be used for producing hollow sphere refractory product or direct It is used for high temperature kiln with bulk material, appearance to be (or elliposoidal) spherical in shape, and inner hollow is held one's breath hole, thus hollow sphere fire proofed wood The thermal coefficient of material is smaller.
Currently, the preparation method of hollow sphere refractory material mainly includes foaming, template and electric smelting blowing process.
Hollow sphere refractory material is prepared using foaming, such as a kind of " preparation side of light aluminum oxide hollow sphere insulating product Method " (201410434384.8) patented technology, mainly by the effect of getting angry of foaming agent in liquid medium, through slurry curing, It is formed after standing.Hollow sphere refractory material is prepared using foaming, foaming agent selects and the stability of bubble is to material property shadow Ring it is significant, and foaming prepare hollow sphere refractory material technical process it is complex.
Hollow sphere refractory material is prepared using template, such as " a kind of ball non-sticky to aluminum alumina hollow ball and preparation method thereof " (201210007134.7) patented technology mainly carries out " cladding " (granulation process) according to the size of template, characteristic, then passes through The techniques such as surface modification, heat treatment prepare hollow sphere refractory material.Hollow sphere refractory material is prepared using template, to template Select more demanding, and hollow ball inside pore shape is single (be not suitable for prepare honeycomb hollow sphere refractory material).
Hollow sphere refractory material is prepared using electric smelting blowing process, such as " a kind of preparation method of high-strength alumina hollow sphere " (201010120320.2) patented technology, the technology are that high-temperature fusant is blowed into droplet under the action of high pressure draught, In the cooling procedure of whereabouts, droplet surface is cooled and solidified rapidly, and drop internal is still in molten condition, further cooling procedure In, inner melt solidification generates biggish volume contraction, forms hollow ball.The contraction generated in process of setting is bigger, formation Spherical shell is thinner.Due to characteristic (surface tension, the viscosity of such as melt) significant difference of variety classes melt, and then influence hollow sphere The intensity and thermal conductivity of refractory material.
Summary of the invention
The present invention is directed to overcome prior art defect, it is therefore an objective to provide that a kind of simple process, production cost be low and balling ratio The preparation method of high honeycomb titanium calcium aluminate hollow sphere.The volume of honeycomb titanium calcium aluminate hollow sphere prepared by this method Density is small, thermal conductivity is low and cold conditions compressive resistance is big.
To achieve the above object, the technical solution adopted by the present invention is that: press ilmenite: rutile: the mass ratio of magnetic iron ore Be 100: (3 ~ 13): ilmenite, rutile and magnetic iron ore are added in blender, mix 0.3 ~ 0.5 hour, obtain by (5 ~ 15) Mixed powder.The mixed powder is added in electromagnetic induction furnace, is warming up to 1300 ~ 1400 DEG C with the rate of 8 ~ 10 DEG C/min, Heat preservation 5 ~ 10 minutes.Press the mixed powder again: the mass ratio of aluminium powder is 100: (25 ~ 30) aluminium is added into electromagnetic induction furnace Powder is warming up to 1550 ~ 1600 DEG C with the rate of 5 ~ 8 DEG C/min, keeps the temperature 5 ~ 10 minutes.Then the mixed powder: lime stone is pressed The mass ratio of powder is 100: (8 ~ 10) lime stone powder is added into electromagnetic induction furnace, is warming up to the rate of 3 ~ 5 DEG C/min 1950 ~ 2000 DEG C, keep the temperature 5 ~ 10 minutes；Slag from slag-drip opening separation electromagnetic induction furnace, finally using 0.4 ~ 0.8MPa's Compressed air spraying slag, it is cooling to get honeycomb titanium calcium aluminate hollow sphere.
The main chemical compositions of the ilmenite are: TiO2Content >=55wt%, Fe2O3Content >=30wt%；The grain of ilmenite Degree≤0.2mm.
The TiO of the rutile2Content >=95wt%；Granularity≤0.2mm of rutile.
The main chemical compositions of the magnetic iron ore are: Fe2O3Content >=70wt%, SiO2Content≤5wt%, content of MgO≤ 5wt%, CaO content≤5wt%, MnO2Content≤8wt%；Granularity≤0.2mm of magnetic iron ore.
Al content >=97wt% of the aluminium powder；Granularity≤30 μm of aluminium powder.
The CaCO of the lime stone powder3Content >=95wt%；Granularity≤0.5mm of lime stone powder.
Due to the adoption of the above technical scheme, the present invention has the positive effect that compared with prior art:
(1) present invention is directly blown obtained honeycomb titanium calcium aluminate hollow sphere to smelt slag caused by ferro-titanium, Technical process is simple, greatly reduces preparation cost；
(2) present invention is sufficiently stirred slag by the magnetic effect of metal bath, improves the uniform of slag component Property, and then increase the balling ratio and cold conditions compressive resistance of honeycomb titanium calcium aluminate hollow sphere；Utilize that " blowing-oxidation is anti-simultaneously Answer " hole of holding one's breath is formed, reduce the bulk density and thermal conductivity of honeycomb titanium calcium aluminate hollow sphere.
The hollow ball warp detection of honeycomb titanium calcium aluminate prepared by the present invention: balling ratio is 99.2 ~ 99.7%, bulk density For 0.6 ~ 1.1g/cm3, thermal coefficient is 0.40 ~ 0.65Wm-1·K-1, cold conditions compressive resistance is 7.5 ~ 8.0MPa.
Therefore, simple process of the invention, production cost are low and balling ratio is high；Prepared honeycomb titanium calcium aluminate is hollow Ball has the characteristics that bulk density is small, thermal conductivity is low and cold conditions compressive resistance is big.
Specific embodiment
The invention will be further described With reference to embodiment, not to the limitation of its protection scope.
It is first that material Unify legislation involved in present embodiment is as follows to avoid repeating, in specific embodiment not It repeats again:
The main chemical compositions of the ilmenite are: TiO2Content >=55wt%, Fe2O3Content >=30wt%；The grain of ilmenite Degree≤0.2mm.
The TiO of the rutile2Content >=95wt%；Granularity≤0.2mm of rutile.
The main chemical compositions of the magnetic iron ore are: Fe2O3Content >=70wt%, SiO2Content≤5wt%, content of MgO≤ 5wt%, CaO content≤5wt%, MnO2Content≤8wt%；Granularity≤0.2mm of magnetic iron ore.
Al content >=97wt% of the aluminium powder；Granularity≤30 μm of aluminium powder.
The CaCO of the lime stone powder3Content >=95wt%；Granularity≤0.5mm of lime stone powder.
Embodiment 1
A kind of honeycomb titanium calcium aluminate hollow sphere and preparation method thereof.Preparation method is: by ilmenite: rutile: magnetic The mass ratio of iron ore is 100: (3 ~ 7): (5 ~ 9) ilmenite, rutile and magnetic iron ore are added in blender, mixing 0.3 ~ 0.5 Hour, obtain mixed powder.The mixed powder is added in electromagnetic induction furnace, is warming up to 1300 with the rate of 8 ~ 10 DEG C/min ~ 1400 DEG C, keep the temperature 5 ~ 10 minutes.Press the mixed powder again: the mass ratio of aluminium powder is 100: (25 ~ 27), to electromagnetic induction furnace Middle addition aluminium powder is warming up to 1550 ~ 1600 DEG C with the rate of 5 ~ 8 DEG C/min, keeps the temperature 5 ~ 10 minutes.Then the mixed powder is pressed : the mass ratio of lime stone powder is 100: lime stone powder is added, into electromagnetic induction furnace with the rate of 3 ~ 5 DEG C/min in (8 ~ 9) 1950 ~ 2000 DEG C are warming up to, keeps the temperature 5 ~ 10 minutes；Slag from slag-drip opening separation electromagnetic induction furnace, finally using 0.4 ~ The compressed air spraying slag of 0.7MPa, it is cooling to get honeycomb titanium calcium aluminate hollow sphere.
The hollow ball warp detection of honeycomb titanium calcium aluminate manufactured in the present embodiment: balling ratio is 99.2 ~ 99.4%, bulk density For 0.6 ~ 0.8g/cm3, thermal coefficient is 0.40 ~ 0.50Wm-1·K-1, cold conditions compressive resistance is 7.5 ~ 7.7MPa.
Embodiment 2
A kind of honeycomb titanium calcium aluminate hollow sphere and preparation method thereof.Preparation method is: by ilmenite: rutile: magnetic The mass ratio of iron ore is 100: (5 ~ 9): (7 ~ 11) ilmenite, rutile and magnetic iron ore are added in blender, and mixing 0.3 ~ 0.5 hour, obtain mixed powder.The mixed powder is added in electromagnetic induction furnace, is warming up to the rate of 8 ~ 10 DEG C/min 1300 ~ 1400 DEG C, keep the temperature 5 ~ 10 minutes.Press the mixed powder again: the mass ratio of aluminium powder is 100: (26 ~ 28), to electromagnetism sense It answers and aluminium powder is added in furnace, be warming up to 1550 ~ 1600 DEG C with the rate of 5 ~ 8 DEG C/min, keep the temperature 5 ~ 10 minutes.Then the mixing is pressed Powder: the mass ratio of lime stone powder is 100: lime stone powder is added, into electromagnetic induction furnace with 3 ~ 5 DEG C/min's in (8 ~ 9) Rate is warming up to 1950 ~ 2000 DEG C, keeps the temperature 5 ~ 10 minutes；Slag from slag-drip opening separation electromagnetic induction furnace, finally uses 0.4 The compressed air spraying slag of ~ 0.7MPa, it is cooling to get honeycomb titanium calcium aluminate hollow sphere.
The hollow ball warp detection of honeycomb titanium calcium aluminate manufactured in the present embodiment: balling ratio is 99.3 ~ 99.5%, bulk density For 0.7 ~ 0.9g/cm3, thermal coefficient is 0.45 ~ 0.55Wm-1·K-1, cold conditions compressive resistance is 7.6 ~ 7.8MPa.
Embodiment 3
A kind of honeycomb titanium calcium aluminate hollow sphere and preparation method thereof.Preparation method is: by ilmenite: rutile: magnetic The mass ratio of iron ore is 100: (7 ~ 11): (9 ~ 13) ilmenite, rutile and magnetic iron ore are added in blender, and mixing 0.3 ~ 0.5 hour, obtain mixed powder.The mixed powder is added in electromagnetic induction furnace, is warming up to the rate of 8 ~ 10 DEG C/min 1300 ~ 1400 DEG C, keep the temperature 5 ~ 10 minutes.Press the mixed powder again: the mass ratio of aluminium powder is 100: (27 ~ 29), to electromagnetism sense It answers and aluminium powder is added in furnace, be warming up to 1550 ~ 1600 DEG C with the rate of 5 ~ 8 DEG C/min, keep the temperature 5 ~ 10 minutes.Then the mixing is pressed Powder: the mass ratio of lime stone powder is 100: lime stone powder is added, into electromagnetic induction furnace with 3 ~ 5 DEG C/min in (9 ~ 10) Rate be warming up to 1950 ~ 2000 DEG C, keep the temperature 5 ~ 10 minutes；Slag from slag-drip opening separation electromagnetic induction furnace, finally uses The compressed air spraying slag of 0.5 ~ 0.8MPa, it is cooling to get honeycomb titanium calcium aluminate hollow sphere.
The hollow ball warp detection of honeycomb titanium calcium aluminate manufactured in the present embodiment: balling ratio is 99.4 ~ 99.6%, bulk density For 0.8 ~ 1.0g/cm3, thermal coefficient is 0.50 ~ 0.60Wm-1·K-1, cold conditions compressive resistance is 7.7 ~ 7.9MPa.
Embodiment 4
A kind of honeycomb titanium calcium aluminate hollow sphere and preparation method thereof.Preparation method is: by ilmenite: rutile: magnetic The mass ratio of iron ore is 100: (9 ~ 13): (11 ~ 15) ilmenite, rutile and magnetic iron ore are added in blender, and mixing 0.3 ~ 0.5 hour, obtain mixed powder.The mixed powder is added in electromagnetic induction furnace, is warming up to the rate of 8 ~ 10 DEG C/min 1300 ~ 1400 DEG C, keep the temperature 5 ~ 10 minutes.Press the mixed powder again: the mass ratio of aluminium powder is 100: (28 ~ 30), to electromagnetism sense It answers and aluminium powder is added in furnace, be warming up to 1550 ~ 1600 DEG C with the rate of 5 ~ 8 DEG C/min, keep the temperature 5 ~ 10 minutes.Then the mixing is pressed Powder: the mass ratio of lime stone powder is 100: lime stone powder is added, into electromagnetic induction furnace with 3 ~ 5 DEG C/min in (9 ~ 10) Rate be warming up to 1950 ~ 2000 DEG C, keep the temperature 5 ~ 10 minutes；Slag from slag-drip opening separation electromagnetic induction furnace, finally uses The compressed air spraying slag of 0.5 ~ 0.8MPa, it is cooling to get honeycomb titanium calcium aluminate hollow sphere.
The hollow ball warp detection of honeycomb titanium calcium aluminate manufactured in the present embodiment: balling ratio is 99.5 ~ 99.7%, bulk density For 0.9 ~ 1.1g/cm3, thermal coefficient is 0.55 ~ 0.65Wm-1·K-1, cold conditions compressive resistance is 7.8 ~ 8.0MPa.
Present embodiment has the positive effect that compared with prior art:
(1) present embodiment is directly blown obtained honeycomb titanium calcium aluminate to smelt slag caused by ferro-titanium Hollow sphere, technical process is simple, greatly reduces preparation cost；
(2) present embodiment is sufficiently stirred slag by the magnetic effect of metal bath, improves slag group The uniformity divided, and then increase the balling ratio and cold conditions compressive resistance of honeycomb titanium calcium aluminate hollow sphere；" spray is utilized simultaneously Blow-oxidation reaction " hole of holding one's breath is formed, reduce the bulk density and thermal conductivity of honeycomb titanium calcium aluminate hollow sphere.
The hollow ball warp detection of honeycomb titanium calcium aluminate prepared by present embodiment: balling ratio is 99.2 ~ 99.7%, Bulk density is 0.6 ~ 1.1g/cm3, thermal coefficient is 0.40 ~ 0.65Wm-1·K-1, cold conditions compressive resistance is 7.5 ~ 8.0MPa.
Therefore, the simple process of present embodiment, production cost are low and balling ratio is high；Prepared honeycomb titanium aluminium Sour calcium hollow sphere has the characteristics that bulk density is small, thermal conductivity is low and cold conditions compressive resistance is big.

Claims (6)

1.一种蜂窝状钛铝酸钙空心球的制备方法，其特征在于所述制备方法的具体步骤是：1. a preparation method of honeycomb calcium aluminate titanate hollow sphere is characterized in that the concrete steps of described preparation method are: 按钛铁矿∶金红石∶磁铁矿的质量比为100∶(3～13)∶(5～15)，将钛铁矿、金红石和磁铁矿加入搅拌机中，混合0.3～0.5小时，得到混合粉体；将所述混合粉体加入电磁感应炉中，以8～10℃/min的速率升温至1300～1400℃，保温5～10分钟；再按所述混合粉体∶铝粉的质量比为100∶(25～30)，向电磁感应炉中加入铝粉，以5～8℃/min的速率升温至1550～1600℃，保温5～10分钟；然后按所述混合粉体∶石灰石粉体的质量比为100∶(8～10)，向电磁感应炉中加入石灰石粉体，以3～5℃/min的速率升温至1950～2000℃，保温5～10分钟；从排渣口分离电磁感应炉中的熔渣，最后采用0.4～0.8MPa的压缩空气喷吹熔渣，冷却，即得蜂窝状钛铝酸钙空心球；According to the mass ratio of ilmenite: rutile: magnetite to be 100: (3-13): (5-15), add ilmenite, rutile and magnetite into the mixer, and mix for 0.3-0.5 hours to obtain Mixing powders; adding the mixed powders into an electromagnetic induction furnace, heating up to 1300-1400°C at a rate of 8-10°C/min, and keeping the temperature for 5-10 minutes; then according to the mixed powder: the quality of the aluminum powder The ratio is 100: (25～30), add aluminum powder to the electromagnetic induction furnace, heat up to 1550～1600 ℃ at the rate of 5～8 ℃/min, keep warm for 5～10 minutes; Then press the mixed powder body: limestone The mass ratio of the powder is 100:(8-10), add limestone powder into the electromagnetic induction furnace, heat up to 1950-2000 ℃ at a rate of 3-5 ℃/min, and keep the temperature for 5-10 minutes; The slag in the electromagnetic induction furnace is separated, and finally, the slag is sprayed with a compressed air of 0.4-0.8 MPa and cooled to obtain honeycomb calcium titanoaluminate hollow spheres; 所述石灰石粉体的CaCO3含量≥95wt％；石灰石粉体的粒度≤0.5mm。The CaCO 3 content of the limestone powder is greater than or equal to 95wt%; the particle size of the limestone powder is less than or equal to 0.5mm. 2.根据权利要求1所述的蜂窝状钛铝酸钙空心球的制备方法，其特征在于所述钛铁矿的主要化学成分是：TiO2含量≥55wt％，Fe2O3含量≥30wt％；钛铁矿的粒度≤0.2mm。2. The preparation method of honeycomb calcium aluminate titanate hollow spheres according to claim 1, wherein the main chemical components of the ilmenite are: TiO 2 content ≥ 55wt%, Fe 2 O 3 content ≥ 30wt% ; The particle size of ilmenite is less than or equal to 0.2mm. 3.根据权利要求1所述的蜂窝状钛铝酸钙空心球的制备方法，其特征在于所述金红石的TiO2含量≥95wt％；金红石的粒度≤0.2mm。3 . The preparation method of honeycomb calcium aluminate titanate hollow spheres according to claim 1 , wherein the TiO 2 content of the rutile is greater than or equal to 95 wt %; the particle size of the rutile is less than or equal to 0.2 mm. 4 . 4.根据权利要求1所述的蜂窝状钛铝酸钙空心球的制备方法，其特征在于所述磁铁矿的主要化学成分是：Fe2O3含量≥70wt％，SiO2含量≤5wt％，MgO含量≤5wt％，CaO含量≤5wt％，MnO2含量≤8wt％；磁铁矿的粒度≤0.2mm。4. The preparation method of honeycomb calcium aluminate titanate hollow spheres according to claim 1, wherein the main chemical components of the magnetite are: Fe 2 O 3 content≥70wt%, SiO 2 content≤5wt% , MgO content≤5wt%, CaO content≤5wt%, MnO 2 content≤8wt%; the particle size of magnetite≤0.2mm. 5.根据权利要求1所述的蜂窝状钛铝酸钙空心球的制备方法，其特征在于所述铝粉的Al含量≥97wt％；铝粉的粒度≤30μm。5 . The preparation method of honeycomb calcium aluminate titanate hollow spheres according to claim 1 , wherein the Al content of the aluminum powder is greater than or equal to 97 wt %; the particle size of the aluminum powder is less than or equal to 30 μm. 6 . 6.一种蜂窝状钛铝酸钙空心球，其特征在于所述蜂窝状钛铝酸钙空心球是根据权利要求1～5项中任一项所述的蜂窝状钛铝酸钙空心球的制备方法所制备的蜂窝状钛铝酸钙空心球。6. A honeycomb calcium aluminate titanate hollow sphere, characterized in that the honeycomb calcium aluminate titanate hollow sphere is a The honeycomb calcium aluminate titanate hollow sphere prepared by the preparation method.
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