CN105837229B - A kind of preparation method of Mg-Al spinel brick - Google Patents

A kind of preparation method of Mg-Al spinel brick Download PDF

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CN105837229B
CN105837229B CN201610163524.1A CN201610163524A CN105837229B CN 105837229 B CN105837229 B CN 105837229B CN 201610163524 A CN201610163524 A CN 201610163524A CN 105837229 B CN105837229 B CN 105837229B
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materials
fine powder
magnesia
granularity
spinel
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CN105837229A (en
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钱志明
刘成强
蒋菊芳
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JIANGSU NUOMING HIGH TEMPERTURE MATERIALS CO Ltd
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JIANGSU NUOMING HIGH TEMPERTURE MATERIALS CO Ltd
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/66Monolithic refractories or refractory mortars, including those whether or not containing clay
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/44Shaped 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 aluminates
    • C04B35/443Magnesium aluminate spinel
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/6303Inorganic additives
    • C04B35/6306Binders based on phosphoric acids or phosphates
    • C04B35/6309Aluminium phosphates
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/6303Inorganic additives
    • C04B35/6316Binders based on silicon compounds
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54Particle size related information
    • C04B2235/5418Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5427Particle size related information expressed by the size of the particles or aggregates thereof millimeter or submillimeter sized, i.e. larger than 0,1 mm

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

The present invention provides a kind of preparation method of Mg-Al spinel brick, concretely comprises the following steps:A, magnesia particle, corundum fine powder and bonding agent are granulated after mixing, after heat treatment screening obtains A materials and B materials;B, magnesia powder, corundum fine powder, magnesium aluminate spinel fine powder and bonding agent are heat-treated after mixing, then crushing and screening obtains C materials and D materials;C, by the lower heat treatment after mixing of A materials, B materials, C materials, D materials, magnesium aluminate spinel fine powder, magnesia powder, corundum fine powder and bonding agent, that is, the Mg-Al spinel brick is obtained;The method of the present invention not only improves the close contact between various feed particles, also the architectural feature of material under different temperatures is taken full advantage of, prepared Mg-Al spinel brick has the good characteristic that cold crushing strength is big, thermal shock resistance is high, refractoriness under load is high, reheating linear change rate on reheating is low.

Description

A kind of preparation method of Mg-Al spinel brick
Technical field
The present invention relates to fire resisting material field, particularly a kind of preparation method of Mg-Al spinel brick.
Background technology
Mg-Al spinel brick is widely used in Industrial Stoves due to having the advantages that anti-erosion, anti scuffing, slag resistance are good In, but the Mg-Al spinel brick prepared by existing technical method, often there are high temperature hot strength is low, thermal shock resistance is poor The defects of.Although by technique improvement, some performance deficiencies of the material can be made up:Such as promote to burn by introducing additive Knot densification, can improve the strength of materials, but the introducing of additive causes the generation of material at high temperature liquid phase again, weakens magnesium on the contrary The refractoriness under load and thermal shock resistance of Alumina spinel brick;For example draw again by carbon containing or other non-oxidized substance additives Enter, then promote densification, improve the thermal shock resistance and intensity of product, but the Mg-Al spinel brick prepared in this way is not Used suitable for neutrality/oxidizing atmosphere condition, and the presence of its non-oxide composition so that the structure and performance for the facings that works, Fail rapidly with the extension of working time.
The content of the invention
In view of the above-mentioned problems, a kind of production cost of present invention offer is low, the simple high-performance magnesium aluminate spinel of production method The preparation method of brick, what the present invention was realized in:
A kind of preparation method of Mg-Al spinel brick, it is comprised the following steps that:
A, it is calculated in mass percent, the magnesia particle of 20-50wt%, the corundum fine powder of 40-70wt% and bonding agent is mixed Close uniform(100% is complemented to bonding agent)After be granulated, then in 1500-1700 DEG C be heat-treated 1-5 it is small when after, screening obtains Granularity is the A materials of 5-3 mm(Include 5mm and 3mm)It is 3-1 mm with granularity(Comprising 1mm, not comprising 3mm)B materials;
B, it is calculated in mass percent, the magnesia powder of 10-30wt%, the corundum fine powder of 30-50 wt%, the magnesium of 10-30 wt% Aluminate fine powder and bonding agent(100% is complemented to bonding agent)It is uniformly mixed, is placed in the pushing of 100-150 MPa environment After type is made, when heat treatment 1-5 is small at a temperature of being placed in 1300-1600 DEG C, it is 1- that then broken, grinding, screening, which obtain granularity, The C materials of 0.088 mm(Include 1mm and 0.088mm)It is less than the D materials of 0.088 mm with granularity(Do not protect 0.088mm);
C, be calculated in mass percent, by the A materials of 5-10 wt%, the B materials of 5-10 wt%, 10-20 wt% C materials, D materials, the magnesium aluminate spinel fine powder of 10-20 wt%, the magnesia powder of 1-10 wt%, the corundum of 1-10 wt% of 10-30 wt% Fine powder and bonding agent are uniformly mixed(100% is complemented to bonding agent), after compressing under the conditions of the 100-150 MPa, put When heat treatment 1-5 is small under the conditions of 1500-1800 DEG C, that is, obtain the Mg-Al spinel brick;
Wherein, the magnesia particle granularity is 1-3mm(Including 1mm and 3mm), magnesia powder granularity is less than 0.088mm, just The granularity of beautiful fine powder is less than 0.088mm;The granularity of magnesium aluminate spinel fine powder is less than 0.088mm.
Preferably, magnesia of the present invention is one kind in magnesite clinker, reheating magnesia or fused magnesite.
Preferably, corundum of the present invention is one kind in plate diamond spar, Brown Alundum or white fused alumina;
Preferably, bonding agent of the present invention is Ludox or aluminium dihydrogen phosphate.
In the present invention, the granularity of the particle is 1-3mm(Including 1mm and 3mm), the granularity of the fine powder is respectively less than 0.088mm。
The present invention is not only improved each by processes such as stringent control each step raw material type, granularity and heat treating regimes Close contact between kind feed particles, also takes full advantage of the architectural feature of material under different temperatures, and varigrained Raw material(And synthesis material)Between grain composition advantage, be the formation of material spinelle crystal, distribution and microstructural excellent Change and provide necessary condition with control, the Mg-Al spinel brick prepared in the process of the present invention is big with cold crushing strength(It is more than 70MPa), thermal shock resistance it is high(1100 DEG C/water cooling, more than 12 times), refractoriness under load it is high(More than 1700 DEG C), reheating line become Rate is low(1600 DEG C/3h, less than+0.6%)Good characteristic.The raw material sources that preparation method of the present invention uses are extensive, are produced into This is low, the stringent control of process system, it is ensured that the structure of product and performance in use continue development and optimization, fit Preferably promote and apply.
Embodiment
To help understanding to technical solution of the present invention, present invention is described in a manner of specific embodiment below and Illustrate, in following embodiments, if not specified otherwise, used raw material is commercial product, used production method(Such as make Grain etc.)It is this area conventional method.
The granularity of particle in following embodiments is 1-3mm;The granularity < 0.088mm of fine powder.
Embodiment 1
The first step, is calculated by percentage to the quality, by the magnesia particle of 20wt%(Granularity is 1-3mm), 70 wt% corundum it is thin Powder(Granularity < 0.088mm), after surplus is supplied with bonding agent aluminium dihydrogen phosphate, mix in proportion, be granulated, in 1500- After when 1700 DEG C of heat treatments 1 are small, by obtained material by sizing, granularity 3-5mm(Comprising 3mm and 5mm, similarly hereinafter)For A Material, granularity are that 1-3 mm are B materials(Comprising 1mm, not comprising 3mm, similarly hereinafter).
Second step, by the magnesia powder of 10wt%(Granularity < 0.088mm), 50 wt% corundum fine powder(Granularity < 0.088mm), 30 wt% magnesium aluminate spinel fine powder(Granularity < 0.088mm), after surplus is supplied with bonding agent Ludox, mixing Uniformly, it is compressing under the conditions of 100-120 MPa, be heat-treated under the conditions of being subsequently placed in 1300-1500 DEG C 5 it is small when, then by thing Material is broken, grinding, and it is 1-0.088mm that screening, which obtains granularity,(Comprising 1mm and 0.088mm, similarly hereinafter)C materials and granularity be less than 0.088 mm(Not comprising 0.088mm)D materials.
3rd step, by percentage to the quality, by the A materials of 10wt%, the B materials of 10wt%, the C materials of 10wt%, 20 wt% D materials, the magnesium aluminate spinel fine powder of 20wt%(Granularity < 0.088mm), 5wt% magnesia powder(Granularity < 0.088mm)、 The corundum fine powder of 5wt%(Granularity < 0.088mm), surplus complements to 100% with Ludox, is then uniformly mixed, in 100-130 Under the conditions of MPa it is compressing after, under the conditions of being placed in 1500-1700 DEG C be heat-treated 5 it is small when, obtain the Mg-Al spinel brick.
The magnesia that the present embodiment uses(Particle/fine powder)For magnesite clinker(Particle/fine powder), corundum(Fine powder)It is firm for tabular It is beautiful(Fine powder).
By detection, Mg-Al spinel brick cold crushing strength prepared by present embodiment is more than 75MPa, thermal shock resistance (1100 DEG C/water cooling)It is more than 1700 DEG C, reheating linear change rate on reheating more than 12 times, refractoriness under load(1600℃/3h)Less than+ 0.5%。
Embodiment 2
The first step, the corundum fine powder of the magnesia particle of 35wt%, 64wt% after surplus is supplied with Ludox, is uniformly mixed, Be granulated, in 1500-1600 DEG C heat treatment 5 it is small when after, screening obtain the A materials that granularity is 5-3 mm and the B that granularity is 3-1 mm Material.
Second step, the magnalium point of the magnesia powder of 20-30 wt%, the corundum fine powder of 40-50 wt%, 10-20 wt% is brilliant Stone fine powder, the aluminium dihydrogen phosphate of 5-10 wt% mix in proportion, and after compressing under the conditions of the 100-150 MPa, are placed in When heat treatment 1-5 is small under the conditions of 1400-1600 DEG C, broken, grinding, screening obtain the C materials and grain that granularity is 1-0.088 mm D material of the degree less than 0.088 mm.
3rd step, by the A materials of 5-10 wt%, the B materials of 5-10 wt%, the C materials of 10-20 wt%, 20-30 wt% D materials, the magnesium aluminate spinel fine powder of 10-20 wt%, the magnesia powder of 1-5 wt%, the corundum fine powder of 1-5 wt%, 5-10 wt% Aluminium dihydrogen phosphate mix in proportion, after compressing under the conditions of the 100-150 MPa, be placed in 1600-1800 DEG C of condition When lower heat treatment 1-5 is small, the magnesia-alumina spinel refractory is obtained.
The magnesia used in the present embodiment(Particle/fine powder)For fused magnesite(Particle/fine powder), used corundum(Carefully Powder)For white fused alumina(Fine powder).
By detection, Mg-Al spinel brick cold crushing strength manufactured in the present embodiment is more than 80MPa, thermal shock resistance (1100 DEG C/water cooling)It is more than 1700 DEG C, reheating linear change rate on reheating more than 14 times, refractoriness under load(1600℃/3h)Less than+ 0.5%。
Embodiment 3
The first step, is calculated in mass percent, and the magnesia particle of 40wt%, the corundum fine powder of 55wt%, surplus are with biphosphate After aluminium is supplied, example is uniformly mixed, is granulated, in 1600-1700 DEG C heat treatment 3 it is small when after, screening obtain granularity be 5-3 mm A things Material and the B materials that granularity is 3-1 mm.
Second step, the magnalium point of the magnesia powder of 25-30 wt%, the corundum fine powder of 30-40 wt%, 20-30 wt% is brilliant Stone fine powder, the Ludox of 5-10 wt% mix in proportion, and after compressing under the conditions of the 100-150 MPa, are placed in 1300- When heat treatment 1-5 is small under the conditions of 1500 DEG C, broken, grinding, screening obtain the C materials that granularity is 1-0.088 mm and granularity is less than The D materials of 0.088 mm.
3rd step, by the A materials of 5-10 wt%, the B materials of 5-10 wt%, the C materials of 10-20 wt%, 20-30 wt% D materials, the magnesium aluminate spinel fine powder of 10-20 wt%, the magnesia powder of 1-5 wt%, the corundum fine powder of 5-10 wt%, 1-5 wt% Aluminium dihydrogen phosphate mix in proportion, after compressing under the conditions of the 100-150 MPa, be placed in 1500-1700 DEG C of condition When lower heat treatment 1-5 is small, the magnesia-alumina spinel refractory is obtained.
Magnesia used in the present embodiment(Particle/fine powder)For reheating magnesia(Particle/fine powder), corundum(Fine powder)For palm fibre Corundum(Fine powder).
By detection, Mg-Al spinel brick cold crushing strength manufactured in the present embodiment is more than 70MPa, thermal shock resistance (1100 DEG C/water cooling)It is more than 1700 DEG C, reheating linear change rate on reheating more than 12 times, refractoriness under load(1600℃/3h)Less than+ 0.6%。
Embodiment 4
The first step, is calculated in mass percent, and the magnesia particle of 50 wt%, the corundum fine powder of 40 wt%, surplus is with Ludox After supplying, be uniformly mixed, be granulated, in 1500-1700 DEG C heat treatment 3 it is small when after, screening obtain granularity be 5-3 mm A materials and Granularity is the B materials of 3-1 mm.
Second step, the magnalium point of the magnesia powder of 20-30 wt%, the corundum fine powder of 40-50 wt%, 20-30 wt% is brilliant Stone fine powder, the aluminium dihydrogen phosphate of 1-5 wt% mix in proportion, and after compressing under the conditions of the 100-150 MPa, are placed in When heat treatment 1-5 is small under the conditions of 1300-1500 DEG C, broken, grinding, screening obtain the C materials and grain that granularity is 1-0.088 mm D material of the degree less than 0.088 mm.
3rd step, by the A materials of 5-10 wt%, the B materials of 5-10 wt%, the C materials of 10-20 wt%, 10-20 wt% D materials, the magnesium aluminate spinel fine powder of 10-20 wt%, the magnesia powder of 5-10 wt%, the corundum fine powder of 5-10 wt%, 5-10 The Ludox of wt% mixes in proportion, and after compressing under the conditions of the 100-150 MPa, is placed under the conditions of 1500-1700 DEG C When heat treatment 1-5 is small, the magnesia-alumina spinel refractory is obtained.
Magnesia used in the present embodiment(Particle/fine powder)For magnesite clinker(Particle/fine powder), corundum(Fine powder)To be white Corundum(Fine powder).
By detection, the standby Mg-Al spinel brick cold crushing strength of the present embodiment is more than 90MPa, thermal shock resistance (1100 DEG C/water cooling)It is more than 1700 DEG C, reheating linear change rate on reheating more than 12 times, refractoriness under load(1600℃/3h)Less than+ 0.6%。

Claims (4)

1. a kind of preparation method of Mg-Al spinel brick, it is characterised in that comprise the following steps that:
A, it is calculated in mass percent, is complemented to by the magnesia particle of 20-50wt%, the corundum fine powder of 40-70wt%, with bonding agent 100%, be granulated after mixing, then in 1500-1700 DEG C be heat-treated 1-5 it is small when after, screening obtain granularity be 3-5 mm A Material and granularity are the B materials more than or equal to 1mm and less than 3mm;
B, it is calculated in mass percent, the magnesia powder of 10-30wt%, the corundum fine powder of 30-50 wt%, the magnalium point of 10-30 wt% Spar fine powder, with bonding agent complement to 100%, is uniformly mixed, be placed in it is compressing under 100-150 MPa environment after, be placed in When heat treatment 1-5 is small at a temperature of 1300-1600 DEG C, then crushes, grind, screening obtains the C materials that granularity is 1-0.088 mm It is less than the D materials of 0.088 mm with granularity;
C, be calculated in mass percent, by the A materials of 5-10 wt%, the B materials of 5-10 wt%, 10-20 wt% C materials, 10-30 The D materials of wt%, the magnesium aluminate spinel fine powder of 10-20 wt%, the magnesia powder of 1-10 wt%, 1-10 wt% corundum fine powder, with Bonding agent complements to 100%, is uniformly mixed, and after compressing under the conditions of the 100-150 MPa, is placed under the conditions of 1500-1800 DEG C When heat treatment 1-5 is small, that is, obtain the Mg-Al spinel brick;
Wherein, the magnesia particle granularity is 1-3mm, and magnesia powder granularity is less than 0.088mm, and the granularity of corundum fine powder is less than 0.088mm;The granularity of magnesium aluminate spinel fine powder is less than 0.088mm.
2. the preparation method of Mg-Al spinel brick according to claim 1, it is characterised in that the magnesia particle is sintering magnesium One kind in sand, reheating magnesia or fused magnesite;The magnesia powder is one in magnesite clinker, reheating magnesia or fused magnesite Kind.
3. the preparation method of Mg-Al spinel brick according to claim 2, it is characterised in that the corundum for plate diamond spar, One kind in Brown Alundum or white fused alumina.
4. according to the preparation method of one of the claim 1-3 Mg-Al spinel bricks, it is characterised in that the bonding agent is silicon Colloidal sol or aluminium dihydrogen phosphate.
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CN109133987B (en) * 2018-10-29 2021-09-24 成都府天高温材料科技有限公司 Corundum-spinel breathable material and preparation method thereof
CN112010659A (en) * 2020-08-05 2020-12-01 武汉重远炉窑工程技术服务有限公司 Magnesia-alumina spinel refractory material and preparation method thereof
CN112010537A (en) * 2020-08-05 2020-12-01 武汉重远炉窑工程技术服务有限公司 Refractory material suitable for glass kiln and preparation method thereof
CN113213956A (en) * 2021-05-28 2021-08-06 海城利尔麦格西塔材料有限公司 Magnesium aluminate spinel brick with excellent comprehensive performance and moderate price and preparation method thereof

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US4954463A (en) * 1988-12-12 1990-09-04 Dresser Industries, Inc. Magnesium aluminate spinel refractory
CN102633511B (en) * 2012-04-09 2014-07-02 江苏诺明高温材料股份有限公司 Aluminum-spinel-magnesia composite refractory as well as preparation method and application thereof
CN103102166B (en) * 2013-03-05 2014-06-04 江苏诺明高温材料股份有限公司 Preparation method of magnesium spinet zirconium brick
CN104944986B (en) * 2015-06-23 2017-03-22 武汉科技大学 High-infrared reflectivity spinel light fire-resistant thermal insulating material and preparation method thereof
CN104961485B (en) * 2015-06-26 2017-03-22 海城市中兴高档镁质砖有限公司 Magnesium spinel refractory material high in thermal shock resistance and manufacturing method thereof

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