CN105837229A - Preparation method of magnesium aluminate spinel brick - Google Patents

Preparation method of magnesium aluminate spinel brick Download PDF

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Publication number
CN105837229A
CN105837229A CN201610163524.1A CN201610163524A CN105837229A CN 105837229 A CN105837229 A CN 105837229A CN 201610163524 A CN201610163524 A CN 201610163524A CN 105837229 A CN105837229 A CN 105837229A
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fine powder
granularity
magnesia
magnesium aluminate
aluminate spinel
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CN105837229B (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

Abstract

The invention provides a preparation method of a magnesium aluminate spinel brick, wherein the preparation method comprises the specific steps: A, mixing evenly magnesia particles, a corundum fine powder and a binder, then granulating, carrying out heat treatment, and screening to obtain a material A and a material B; B, mixing a magnesia fine powder, a corundum fine powder, a magnesium aluminate spinel fine powder and a binder evenly, carrying out heat treatment, then crushing and screening to obtain a material C and a material D; C, mixing evenly the material A, the material B, the material C, the material D, a magnesium aluminate spinel fine powder, a magnesia fine powder, a corundum fine powder and a binder, and then carrying out heat treatment, to obtain the magnesium aluminate spinel brick. The method is beneficial for close contact of all kinds of raw material particles, but also makes full use of structural characteristics of materials at different temperatures; the prepared magnesium aluminate spinel brick has excellent characteristics of high room-temperature compressive strength, high thermal shock stability, high load softening temperature, and low reburning line change rate.

Description

A kind of preparation method of Mg-Al spinel brick
Technical field
The present invention relates to fire resisting material field, the preparation method of a kind of Mg-Al spinel brick.
Background technology
Mg-Al spinel brick, owing to having anti-erosion, anti scuffing, advantage that slag resistance is good, is widely used in Industrial Stoves, but the Mg-Al spinel brick prepared by existing technical method, often there is the defects such as high temperature hot strength is low, thermal shock resistance is poor.Although passing through technique improvement, some performance deficiencies of this material can be made up: such as by introducing additive acceleration of sintering densification, the strength of materials can be improved, but the introducing of additive causes again the generation of material at high temperature liquid phase, weaken refractoriness under load and the thermal shock resistance of Mg-Al spinel brick on the contrary;The most such as by carbon containing or the introducing of other non-oxidized substance additives, then promote densification, the thermal shock resistance improving product and intensity, but the Mg-Al spinel brick prepared in this way is unsuitable for neutrality/oxidizing atmosphere condition to be used, and the existence of its non-oxide composition, make structure and the performance of work facings, fail rapidly along with the prolongation of working time.
Summary of the invention
For the problems referred to above, the present invention provides that a kind of production cost is low, the preparation method of production method simple high-performance Mg-Al spinel brick, and the present invention is achieved in that
The preparation method of a kind of Mg-Al spinel brick, it specifically comprises the following steps that
A, it is calculated in mass percent, by the magnesia particle of 20-50wt%, the corundum fine powder of 40-70wt% and bonding agent mix homogeneously (i.e. complementing to 100% with bonding agent) pelletize afterwards, then after 1500-1700 DEG C of heat treatment 1-5 hour, screening obtains A material (comprising 5mm and 3mm) that granularity is 5-3 mm and granularity is that 3-1 mm(comprises 1mm, does not comprise 3mm) B material;
B, it is calculated in mass percent; the magnesia powder of 10-30wt%, the corundum fine powder of 30-50 wt%, the magnesium aluminate spinel fine powder of 10-30 wt% and bonding agent (i.e. complementing to 100% with bonding agent) mix homogeneously; be placed in compressing under 100-150 MPa environment after; heat treatment 1-5 hour at a temperature of being placed in 1300-1600 DEG C, then crushes, grinds, sieves the D material (not protecting 0.088mm) obtaining C material (comprising 1mm and 0.088mm) that granularity is 1-0.088 mm and granularity less than 0.088 mm;
C, it is calculated in mass percent, by the A material of 5-10 wt%, the B material of 5-10 wt%, the C material of 10-20 wt%, the D material of 10-30 wt%, the magnesium aluminate spinel fine powder of 10-20 wt%, the magnesia powder of 1-10 wt%, the corundum fine powder of 1-10 wt% and bonding agent mix homogeneously (i.e. complementing to 100% with bonding agent), under the conditions of 100-150 MPa compressing after, heat treatment 1-5 hour under the conditions of being placed in 1500-1800 DEG C, i.e. obtains described Mg-Al spinel brick;
Wherein, described magnesia particle granularity is that 1-3mm(includes 1mm and 3mm), 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.
Preferably, the one during magnesia of the present invention is magnesite clinker, reheating magnesia or fused magnesite.
Preferably, the one during corundum of the present invention is 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 described granule is that 1-3mm(includes 1mm and 3mm), the granularity of described fine powder is respectively less than 0.088mm.
The present invention is by strict control each step raw material type, the operation such as granularity and heat treating regime, not only improve the close contact between various feed particles, also the architectural feature of material under different temperatures is taken full advantage of, and the grain composition advantage between varigrained raw material (and synthesis material), formation for material spinelle crystal, distribution and microstructural optimization provide essential condition with control, it is big (more than 70MPa) that the Mg-Al spinel brick prepared in the process of the present invention has cold crushing strength, high (1100 DEG C/water-cooled of thermal shock resistance, more than 12 times), refractoriness under load is high (more than 1700 DEG C), reheating linear change rate on reheating is low (1600 DEG C/3h, less than+0.6%) good characteristic.The raw material sources of preparation method of the present invention employing are extensive, and production cost is low, the strict control of process system, it is ensured that the continuation in use of the structure of product and performance develops and optimizes, suitable popularization and application.
Detailed description of the invention
For helping the understanding to technical solution of the present invention, in the way of specific embodiment, present invention is described below and explanation, in following example, if not specified otherwise, the raw material used is commercially available prod, and the production method (such as pelletize etc.) used is this area conventional method.
The granularity of the granule in following embodiment is 1-3mm;The granularity < 0.088mm of fine powder.
Embodiment 1
The first step, calculate by percentage to the quality, by the magnesia particle (granularity is 1-3mm) of 20wt%, the corundum fine powder (granularity < 0.088mm) of 70 wt%, after surplus is supplied with bonding agent aluminium dihydrogen phosphate, mix in proportion, pelletize, after 1500-1700 DEG C of heat treatment 1 hour, by the material that obtains by sizing, granularity is that 3-5mm(comprises 3mm and 5mm, lower same) it is A material, granularity be 1-3 mm be B material (comprise 1mm, do not comprise 3mm, lower with).
Second step, by the magnesia powder (granularity < 0.088mm) of 10wt%, the corundum fine powder (granularity < 0.088mm) of 50 wt%, the magnesium aluminate spinel fine powder (granularity < 0.088mm) of 30 wt%, after surplus is supplied with bonding agent Ludox, mix homogeneously, under the conditions of 100-120 MPa compressing, heat treatment 5 hours under the conditions of being subsequently placed in 1300-1500 DEG C, again material is crushed, grind, it is that 1-0.088mm(comprises 1mm and 0.088mm that screening obtains granularity, lower with) C material and granularity do not comprise 0.088mm less than 0.088 mm() D material.
3rd step, by percentage to the quality, by the A material of 10wt%, the B material of 10wt%, the C material of 10wt%, the D material of 20 wt%, the magnesium aluminate spinel fine powder (granularity < 0.088mm) of 20wt%, the magnesia powder (granularity < 0.088mm) of 5wt%, the corundum fine powder (granularity < 0.088mm) of 5wt%, surplus complements to 100% with Ludox, then mix homogeneously, under the conditions of 100-130 MPa compressing after, heat treatment 5 hours under the conditions of being placed in 1500-1700 DEG C, obtain described Mg-Al spinel brick.
The magnesia (granule/fine powder) that the present embodiment uses is magnesite clinker (granule/fine powder), and corundum (fine powder) is plate diamond spar (fine powder).
Through detection, Mg-Al spinel brick cold crushing strength prepared by present embodiment more than 75MPa, thermal shock resistance (1100 DEG C/water-cooled) more than 12 times, refractoriness under load more than 1700 DEG C, reheating linear change rate on reheating (1600 DEG C/3h) is less than+0.5%.
Embodiment 2
The first step, by the magnesia particle of 35wt%, the corundum fine powder of 64wt%, after surplus is supplied with Ludox, mix homogeneously, pelletize, after 1500-1600 DEG C of heat treatment 5 hours, screening obtains the A material that granularity is 5-3 mm and the B material that granularity is 3-1 mm.
Second step, the magnesia powder of 20-30 wt%, the corundum fine powder of 40-50 wt%, the magnesium aluminate spinel fine powder of 10-20 wt%, the aluminium dihydrogen phosphate of 5-10 wt% are mixed in proportion, under the conditions of 100-150 MPa compressing after, heat treatment 1-5 hour under the conditions of being placed in 1400-1600 DEG C, crushes, grinds, sieves the D material obtaining C material that granularity is 1-0.088 mm and granularity less than 0.088 mm.
3rd step, the A material of 5-10 wt%, the B material of 5-10 wt%, the C material of 10-20 wt%, the D material of 20-30 wt%, 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%, the aluminium dihydrogen phosphate of 5-10 wt% are mixed in proportion, under the conditions of 100-150 MPa compressing after, heat treatment 1-5 hour under the conditions of being placed in 1600-1800 DEG C, obtains described magnesia-alumina spinel refractory.
The magnesia (granule/fine powder) used in the present embodiment is fused magnesite (granule/fine powder), and the corundum (fine powder) used is white fused alumina (fine powder).
Through detection, Mg-Al spinel brick cold crushing strength prepared by the present embodiment more than 80MPa, thermal shock resistance (1100 DEG C/water-cooled) more than 14 times, refractoriness under load more than 1700 DEG C, reheating linear change rate on reheating (1600 DEG C/3h) is less than+0.5%.
Embodiment 3
The first step, it is calculated in mass percent, after the magnesia particle of 40wt%, the corundum fine powder of 55wt%, surplus are supplied with aluminium dihydrogen phosphate, example mix homogeneously, pelletize, after 1600-1700 DEG C of heat treatment 3 hours, screening obtains the A material that granularity is 5-3 mm and the B material that granularity is 3-1 mm.
Second step, the magnesia powder of 25-30 wt%, the corundum fine powder of 30-40 wt%, the magnesium aluminate spinel fine powder of 20-30 wt%, the Ludox of 5-10 wt% are mixed in proportion, under the conditions of 100-150 MPa compressing after, heat treatment 1-5 hour under the conditions of being placed in 1300-1500 DEG C, crushes, grinds, sieves the D material obtaining C material that granularity is 1-0.088 mm and granularity less than 0.088 mm.
3rd step, the A material of 5-10 wt%, the B material of 5-10 wt%, the C material of 10-20 wt%, the D material of 20-30 wt%, 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%, the aluminium dihydrogen phosphate of 1-5 wt% are mixed in proportion, under the conditions of 100-150 MPa compressing after, heat treatment 1-5 hour under the conditions of being placed in 1500-1700 DEG C, obtains described magnesia-alumina spinel refractory.
Magnesia (granule/fine powder) used in the present embodiment is reheating magnesia (granule/fine powder), and corundum (fine powder) is Brown Alundum (fine powder).
Through detection, Mg-Al spinel brick cold crushing strength prepared by the present embodiment more than 70MPa, thermal shock resistance (1100 DEG C/water-cooled) more than 12 times, refractoriness under load more than 1700 DEG C, reheating linear change rate on reheating (1600 DEG C/3h) is less than+0.6%.
Embodiment 4
The first step, is calculated in mass percent, the magnesia particle of 50 wt%, the corundum fine powder of 40 wt%, after surplus is supplied with Ludox, mix homogeneously, pelletize, after 1500-1700 DEG C of heat treatment 3 hours, screening obtains the A material that granularity is 5-3 mm and the B material that granularity is 3-1 mm.
Second step, the magnesia powder of 20-30 wt%, the corundum fine powder of 40-50 wt%, the magnesium aluminate spinel fine powder of 20-30 wt%, the aluminium dihydrogen phosphate of 1-5 wt% are mixed in proportion, under the conditions of 100-150 MPa compressing after, heat treatment 1-5 hour under the conditions of being placed in 1300-1500 DEG C, crushes, grinds, sieves the D material obtaining C material that granularity is 1-0.088 mm and granularity less than 0.088 mm.
3rd step, the A material of 5-10 wt%, the B material of 5-10 wt%, the C material of 10-20 wt%, the D material of 10-20 wt%, 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%, the Ludox of 5-10 wt% are mixed in proportion, under the conditions of 100-150 MPa compressing after, heat treatment 1-5 hour under the conditions of being placed in 1500-1700 DEG C, obtains described magnesia-alumina spinel refractory.
Magnesia (granule/fine powder) used in the present embodiment is magnesite clinker (granule/fine powder), and corundum (fine powder) is white fused alumina (fine powder).
Through detection, the standby Mg-Al spinel brick cold crushing strength of the present embodiment more than 90MPa, thermal shock resistance (1100 DEG C/water-cooled) more than 12 times, refractoriness under load more than 1700 DEG C, reheating linear change rate on reheating (1600 DEG C/3h) is less than+0.6%.

Claims (4)

1. the preparation method of a Mg-Al spinel brick, it is characterised in that specifically comprise the following steps that
A, it is calculated in mass percent, by pelletize after the magnesia particle of 20-50wt%, the corundum fine powder of 40-70wt% and bonding agent mix homogeneously, then, after 1500-1700 DEG C of heat treatment 1-5 hour, screening obtains the A material that granularity is 3-5 mm and the B material that granularity is 1-3mm;
B, it is calculated in mass percent, the magnesia powder of 10-30wt%, the corundum fine powder of 30-50 wt%, 10-30 The magnesium aluminate spinel fine powder of wt% and bonding agent mix homogeneously, be placed in 100-150 Under MPa environment compressing after, heat treatment 1-5 hour at a temperature of being placed in 1300-1600 DEG C, then crush, grind, sieve and obtain C material that granularity is 1-0.088 mm and granularity less than 0.088 The D material of mm;
C, it is calculated in mass percent, by the A material of 5-10 wt%, 5-10 The B material of wt%, the C material of 10-20 wt%, the D material of 10-30 wt%, the magnesium aluminate spinel fine powder of 10-20 wt%, 1-10 The magnesia powder of wt%, the corundum fine powder of 1-10 wt% and bonding agent mix homogeneously, compressing under the conditions of 100-150 MPa after, heat treatment 1-5 hour under the conditions of being placed in 1500-1800 DEG C, i.e. obtain described Mg-Al spinel brick;
Wherein, described 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.
The preparation method of Mg-Al spinel brick the most according to claim 1, it is characterised in that described magnesia is the one in magnesite clinker, reheating magnesia or fused magnesite.
The preparation method of Mg-Al spinel brick the most according to claim 2, it is characterised in that described corundum is the one in plate diamond spar, Brown Alundum or white fused alumina.
4. according to the preparation method of the described Mg-Al spinel brick of one of claim 1-3, it is characterised in that described bonding agent is Ludox or aluminium dihydrogen phosphate.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109133987A (en) * 2018-10-29 2019-01-04 成都府天高温材料科技有限公司 A kind of corundum-spinel gas permeable 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
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
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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Publication number Priority date Publication date Assignee Title
US4954463A (en) * 1988-12-12 1990-09-04 Dresser Industries, Inc. Magnesium aluminate spinel refractory
CN102633511A (en) * 2012-04-09 2012-08-15 宜兴市诺明高温耐火材料有限公司 Aluminum-spinel-magnesia composite refractory as well as preparation method and application thereof
CN103102166A (en) * 2013-03-05 2013-05-15 江苏诺明高温材料股份有限公司 Preparation method of magnesium spinet zirconium brick
CN104944986A (en) * 2015-06-23 2015-09-30 武汉科技大学 High-infrared reflectivity spinel light fire-resistant thermal insulating material and preparation method thereof
CN104961485A (en) * 2015-06-26 2015-10-07 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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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4954463A (en) * 1988-12-12 1990-09-04 Dresser Industries, Inc. Magnesium aluminate spinel refractory
CN102633511A (en) * 2012-04-09 2012-08-15 宜兴市诺明高温耐火材料有限公司 Aluminum-spinel-magnesia composite refractory as well as preparation method and application thereof
CN103102166A (en) * 2013-03-05 2013-05-15 江苏诺明高温材料股份有限公司 Preparation method of magnesium spinet zirconium brick
CN104944986A (en) * 2015-06-23 2015-09-30 武汉科技大学 High-infrared reflectivity spinel light fire-resistant thermal insulating material and preparation method thereof
CN104961485A (en) * 2015-06-26 2015-10-07 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

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109133987A (en) * 2018-10-29 2019-01-04 成都府天高温材料科技有限公司 A kind of corundum-spinel gas permeable 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
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
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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