CN110451994B - Magnesium-based sintered castable prefabricated member reinforced by magnesium aluminate spinel whiskers - Google Patents

Magnesium-based sintered castable prefabricated member reinforced by magnesium aluminate spinel whiskers Download PDF

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CN110451994B
CN110451994B CN201910705021.6A CN201910705021A CN110451994B CN 110451994 B CN110451994 B CN 110451994B CN 201910705021 A CN201910705021 A CN 201910705021A CN 110451994 B CN110451994 B CN 110451994B
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magnesium
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CN110451994A (en
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罗旭东
陈娜
李季佳
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University of Science and Technology Liaoning USTL
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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
    • C04B35/03—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 magnesium oxide, calcium oxide or oxide mixtures derived from dolomite
    • C04B35/04—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 magnesium oxide, calcium oxide or oxide mixtures derived from dolomite based on magnesium oxide
    • C04B35/043—Refractories from grain sized mixtures
    • 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
    • C04B35/62204—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products using waste materials or refuse
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • 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
    • C04B2235/444—Halide containing anions, e.g. bromide, iodate, chlorite
    • C04B2235/445—Fluoride containing anions, e.g. fluosilicate
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52—Constituents or additives characterised by their shapes
    • C04B2235/5276—Whiskers, spindles, needles or pins

Abstract

The invention relates to a magnesium-based sintered castable prefabricated member reinforced by magnesium aluminate spinel whiskers, which is prepared by taking fused magnesia as an aggregate, fused magnesia fine powder, high-purity magnesia fine powder, silica fume micro powder and alumina micro powder as matrixes and aluminum fluoride fine powder as a catalyst through premixing, mixing, molding, drying and sintering. The method effectively utilizes the magnesium aluminate spinel whiskers generated in the magnesium-sintered castable prefabricated member, and improves the high-temperature mechanical property and the thermal shock resistance stability of the magnesium castable prefabricated member.

Description

Magnesium-based sintered castable prefabricated member reinforced by magnesium aluminate spinel whiskers
Technical Field
The invention relates to the technical field of inorganic chemical industry, in particular to a magnesium-based sintered castable prefabricated member reinforced by magnesium aluminate spinel whiskers.
Background
The magnesia burnt castable has the advantages of good fire resistance, good alkaline slag corrosion resistance, no molten steel pollution and the like, has wide application prospect in the high-temperature fields of steel smelting, cement, glass, ceramics and the like, but the problems of poor normal-temperature mechanical property and poor thermal shock resistance stability of the castable prefabricated material always restrict the further wide application of the castable. At home and abroad researchers make a great deal of basic research on application, for example, the refractory fiber is applied to the castable to improve the normal temperature strength and the thermal shock stability of the material. The technological process includes crushing magnesia-alumina spinel whisker, mixing with refractory bulk material, mixing, forming, drying, sintering and other steps. The dispersion degree of the broken magnesia-alumina spinel whiskers is poor, and the broken magnesia-alumina spinel whiskers mostly exist in a cloud-shaped or cluster-shaped form with uneven size. Although the strength and the thermal stability of the material are improved to a certain extent by the magnesium aluminate spinel whisker reinforced castable, the overall strength and the thermal shock effect of the product are affected by poor dispersion degree of the magnesium aluminate spinel whiskers, so that a sample is cracked or even exploded due to overhigh local temperature in the sintering process. The magnesia-alumina spinel whisker has excellent high temperature resistance, corrosion resistance, excellent thermal shock stability and excellent mechanical property. The introduction of the magnesia-alumina spinel whisker can improve the toughness of the castable precast block and increase the impact strength, and is often the first choice for the development of heat-resistant composite materials. Therefore, the method effectively utilizes the in-situ generation of the magnesia-alumina spinel whiskers in the magnesium-based sintered castable prefabricated member, thereby improving the high-temperature mechanical property and the thermal shock resistance stability of the magnesium-based sintered castable.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and aims to provide a magnesium-based sintered castable prefabricated member reinforced by magnesium aluminate spinel whiskers.
In order to realize the purpose, the invention is realized by the following technical scheme:
the magnesium-based sintered castable prefabricated member reinforced by the magnesium aluminate spinel whisker is characterized in that fused magnesia with the particle size of 8-0.074mm is used as aggregate, fused magnesia fine powder with the particle size of less than 0.074mm, high-purity magnesia fine powder with the particle size of less than 0.074mm, silica fume micro powder with the particle size of less than 0.045mm and alumina micro powder with the particle size of less than 0.045mm are used as matrix, and aluminum fluoride fine powder with the particle size of less than 0.074mm is used as catalyst, and the magnesium-based sintered castable prefabricated member reinforced by the magnesium aluminate spinel whisker is obtained through premixing, mixing, molding, drying and sintering, and the concrete operation steps are as follows:
step one, premixing, namely putting 60-70% of fused magnesia aggregate with the particle size of 8-0.074mm into a stirrer, and then pouring 5-15% of fused magnesia fine powder with the particle size of less than 0.074mm, 5-15% of high-purity magnesia fine powder with the particle size of less than 0.074mm, 5-15% of silica fume micro powder with the particle size of less than 0.045mm, 5-15% of alumina micro powder with the particle size of less than 0.045mm and 1-5% of aluminum fluoride fine powder with the particle size of less than 0.074mm into the stirrer, and mixing for 10-20 minutes to obtain a premixed material;
step two, mixing, adding water accounting for 5-10% of the total mass of the premixed material obtained in the step one, adding the water into the premixed material obtained in the step one, placing the premixed material into a mixing roll, and continuously mixing for 10-20 minutes to obtain a mixed castable;
step three, molding, namely placing the mixed castable into a mold for molding and casting, and demolding after the sample is maintained in the mold at room temperature for 24-48 hours to form a magnesium castable prefabricated part blank;
drying, namely drying the demolded magnesium castable prefabricated part blank for 24-48 hours at the temperature of 100-150 ℃;
step five, sintering, namely heating the dried magnesium castable prefabricated member blank to 950-.
In the fifth step, the temperature rise rate of the first stage is 1-3 ℃/min, and the temperature rise rate of the second stage is 10-20 ℃/min.
Compared with the prior art, the invention has the beneficial effects that: the magnesium-based sintered castable prefabricated member reinforced by the magnesium aluminate spinel whisker, prepared by the invention, can bear larger external force under the common cooperation effect of various raw materials, and meanwhile, the magnesium aluminate spinel whisker growing in situ avoids the explosion of a sample caused by overhigh local temperature, so that the application range of the refractory castable is greatly improved, the popularization of the refractory castable is facilitated, the whisker can play a toughening role on a brick body, the toughening effect is poor when the length-diameter ratio of the whisker is overlarge, and the product cannot become the whisker when the length-diameter ratio is too small, so that the whisker is called as a crystal grain, and the reinforcing effect is the best when the length-diameter ratio is 15.5-22.5.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention.
Detailed Description
The preparation process of the present invention is further illustrated by the following examples:
example 1:
the magnesium-based sintered castable preform reinforced by the magnesium aluminate spinel whisker provided by the embodiment comprises the following raw materials: 65kg of fused magnesia aggregate with the grain diameter of 8-0.074mm, 8kg of fused magnesia fine powder with the grain diameter of less than 0.074mm, 8kg of high-purity magnesia fine powder with the grain diameter of less than 0.074mm, 8kg of silica fume micro powder with the grain diameter of less than 0.045mm, 8kg of alumina micro powder with the grain diameter of less than 0.045mm and 3kg of aluminum fluoride fine powder with the grain diameter of less than 0.074 mm. The specific operation steps for preparing the magnesium-based sintered castable prefabricated member reinforced by the magnesium aluminate spinel whisker are as follows:
firstly, placing the fused magnesia aggregate in a stirrer, pouring the fused magnesia fine powder, high-purity magnesia fine powder, silica fume micro powder, alumina micro powder and aluminum fluoride fine powder into the stirrer, and mixing for 10 minutes to obtain a premixed material;
step two, mixing, adding 5kg of water, adding the water into the premixed material obtained in the step one, and placing the premixed material into a mixing roll to continue mixing for 20 minutes to obtain a mixed castable;
step three, molding, namely placing the mixed castable into a mold for molding and casting, and demolding after the sample is cured in the mold at room temperature for 24 hours to form a magnesium castable prefabricated part blank;
drying, namely drying the demoulded precast magnesium castable blank for 24 hours at the temperature of 100 ℃;
and fifthly, firing, namely heating the dried magnesium castable preform blank to 1200 ℃ at the heating rate of 1 ℃/min, preserving the heat for 3 hours, continuously heating to 1400 ℃ at the heating rate of 10 ℃/min, preserving the heat for 3 hours, naturally cooling along with the furnace, and taking out to obtain the magnesium castable preform reinforced by the magnesium aluminate spinel crystal whisker.
The length-diameter ratio of the magnesium aluminate spinel whisker in the magnesium-based sintered castable preform reinforced by the magnesium aluminate spinel whisker prepared in the embodiment is 15.5. The high-temperature breaking strength is 14.4MPa, and the thermal shock resistance stability is 15 times.
Example 2:
the magnesium-based sintered castable preform reinforced by the magnesium aluminate spinel whisker provided by the embodiment comprises the following raw materials: 62kg of fused magnesia aggregate with the grain diameter of 8-0.074mm, 9kg of fused magnesia fine powder with the grain diameter of less than 0.074mm, 9kg of high-purity magnesia fine powder with the grain diameter of less than 0.074mm, 9kg of silica fume micro powder with the grain diameter of less than 0.045mm, 8kg of alumina micro powder with the grain diameter of less than 0.045mm and 3kg of aluminum fluoride fine powder with the grain diameter of less than 0.074 mm. The specific operation steps for preparing the magnesium-based sintered castable prefabricated part reinforced by the magnesium aluminate spinel whisker are as follows:
firstly, placing the fused magnesia aggregate in a stirrer, pouring the fused magnesia fine powder, high-purity magnesia fine powder, silica fume micro powder, alumina micro powder and aluminum fluoride fine powder into the stirrer, and mixing for 15 minutes to obtain a premixed material;
step two, mixing, adding 10kg of water, adding the water into the premixed material obtained in the step one, and placing the premixed material into a mixing roll to continue mixing for 10 minutes to obtain a mixed castable;
step three, molding, namely placing the mixed castable into a mold for molding and casting, and demolding after the sample is cured in the mold at room temperature for 36 hours to form the mixed castable;
drying, namely drying the mixed castable after demolding at 120 ℃ for 36 hours;
and fifthly, firing, namely heating the dried magnesium castable prefabricated part blank to 1100 ℃ at the heating rate of 2 ℃/min, preserving heat for 3.5 hours, continuously heating to 1500 ℃ at the heating rate of 15 ℃/min, preserving heat for 3.5 hours, naturally cooling along with the furnace, and taking out to obtain the magnesium spinel whisker reinforced magnesium castable prefabricated part.
The length-diameter ratio of the magnesium aluminate spinel whiskers in the magnesium-based sintered castable preform prepared in the embodiment is 22.5, the high-temperature breaking strength is 16.8MPa, and the thermal shock resistance is 18 times.
Example 3:
the magnesium-based sintered castable prefabricated member reinforced by magnesium aluminate spinel whisker provided by the embodiment comprises the following raw materials: 68kg of fused magnesia aggregate with the grain diameter of 8-0.074mm, 7kg of fused magnesia fine powder with the grain diameter of less than 0.074mm, 7kg of high-purity magnesia fine powder with the grain diameter of less than 0.074mm, 7kg of silica fume micro powder with the grain diameter of less than 0.045mm, 6kg of alumina micro powder with the grain diameter of less than 0.045mm and 5kg of aluminum fluoride fine powder with the grain diameter of less than 0.074 mm. The specific operation steps for preparing the magnesium-based sintered castable prefabricated member reinforced by the magnesium aluminate spinel whisker are as follows:
firstly, placing the fused magnesia aggregate in a stirrer, pouring the fused magnesia fine powder, high-purity magnesia fine powder, silica fume micro powder, alumina micro powder and aluminum fluoride fine powder into the stirrer, and mixing for 20 minutes to obtain a premixed material;
step two, mixing, adding 15kg of water, adding the water into the premixed material obtained in the step one, and placing the premixed material into a mixing mill to continuously mix for 10 minutes to obtain a mixed castable;
step three, molding, namely placing the mixed castable into a mold for molding and casting, and demolding after the sample is cured in the mold at room temperature for 48 hours to form a magnesium castable prefabricated part blank;
drying, namely drying the demoulded magnesium castable prefabricated part blank for 48 hours at the temperature of 140 ℃;
and fifthly, firing, namely heating the dried magnesium castable preform blank to 1000 ℃ at the heating rate of 3 ℃/min, preserving the heat for 4 hours, continuously heating to 1600 ℃ at the heating rate of 20 ℃/min, preserving the heat for 4 hours, naturally cooling along with the furnace, and taking out to obtain the magnesium castable preform reinforced by the magnesium aluminate spinel crystal whisker.
The length-diameter ratio of the magnesium aluminate spinel whiskers in the magnesium-based sintered castable preform prepared in the embodiment is 17.8, the high-temperature breaking strength is 15.2MPa, and the thermal shock resistance is 17 times.

Claims (2)

1. A magnesium-based sintered castable prefabricated member reinforced by magnesium aluminate spinel whiskers is characterized by comprising the following steps: (1) putting 60-70% of fused magnesia aggregate with the particle size of 8-0.074mm into a stirrer, then pouring 5-15% of fused magnesia fine powder with the particle size of less than 0.074mm, 5-15% of high-purity magnesia fine powder with the particle size of less than 0.074mm, 5-15% of silica fume micro powder with the particle size of less than 0.045mm, 5-15% of alumina micro powder with the particle size of less than 0.045mm and 1-5% of aluminum fluoride fine powder with the particle size of less than 0.074mm into the stirrer, and mixing for 10-20 minutes to obtain a premixed material; (2) mixing, adding water accounting for 5-10% of the total mass of the premixed material obtained in the step (1), adding the water into the premixed material obtained in the step (1), and placing the premixed material into a mixing roll to continue mixing for 10-20 minutes to obtain a mixed castable; (3) molding, namely placing the mixed castable into a mold for molding and pouring, and demolding after the sample is cured in the mold at room temperature for 24-48 hours to form a magnesium castable prefabricated part blank; (4) drying, namely drying the demoulded magnesium castable prefabricated part blank for 24-48 hours at the temperature of 100-150 ℃; (5) and (3) sintering, namely heating the dried magnesium castable prefabricated part blank to 950-.
2. The magnesium-based sintered castable preform reinforced by magnesium aluminate spinel whiskers according to claim 1, wherein in the step (5), the temperature rise rate in the first stage is 1-3 ℃/min, and the temperature rise rate in the second stage is 10-20 ℃/min.
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CN111153708B (en) * 2020-02-14 2022-07-08 辽宁科技大学 Corundum-mullite multiphase gradient material for heat recovery coke oven door
CN111217591A (en) * 2020-02-27 2020-06-02 鞍山腾泰耐火材料有限公司 Prefabricated part for inner lining of assembled electric melting furnace and preparation method thereof

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