CN111892387A - Preparation method of large-size thin high-temperature corundum-mullite slab - Google Patents

Preparation method of large-size thin high-temperature corundum-mullite slab Download PDF

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Publication number
CN111892387A
CN111892387A CN202010800341.2A CN202010800341A CN111892387A CN 111892387 A CN111892387 A CN 111892387A CN 202010800341 A CN202010800341 A CN 202010800341A CN 111892387 A CN111892387 A CN 111892387A
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parts
mullite
corundum
temperature
slab
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Chinese (zh)
Inventor
王刚
梁鹏鹏
韩建燊
李红霞
袁波
陈政龙
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Sinosteel Luoyang Institute of Refractories Research Co Ltd
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Sinosteel Nanjing Environmental Engineering Technology Research Institute Co ltd
Sinosteel Luoyang Institute of Refractories Research Co Ltd
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Priority to CN202010800341.2A priority Critical patent/CN111892387A/en
Publication of CN111892387A publication Critical patent/CN111892387A/en
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    • 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
    • C04B35/10Shaped 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 aluminium oxide
    • C04B35/101Refractories from grain sized mixtures
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    • 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
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3418Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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    • 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
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3427Silicates other than clay, e.g. water glass
    • C04B2235/3463Alumino-silicates other than clay, e.g. mullite
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    • 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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    • 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
    • C04B2235/5436Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
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    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/602Making the green bodies or pre-forms by moulding
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    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/606Drying
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    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6567Treatment time

Abstract

The invention relates to the technical field of refractory kiln furniture, in particular to a preparation method of a large-size thin high-temperature corundum-mullite slab. The preparation method of the large-size thin high-temperature corundum-mullite slab comprises the following raw materials in parts by weight: 55-75 parts of aggregate, 5-15 parts of fine powder, 15-35 parts of micro powder, and 0.3-1 part of self-initiated coagulant Isobam and 3-15 parts of water are additionally added; weighing the components according to the proportion, uniformly mixing the components in a forced stirrer, pouring the mixture into a mold, curing the mixture at room temperature for 3 days, preserving the heat at 110 ℃ for 24 hours, and preserving the heat at 1550-1650 ℃ for 3-5 hours in an air atmosphere after demolding. The process solves the problems of high equipment requirement, low green body strength, difficult demoulding, easy cracking and warping in the drying process, uneven products and the like in the preparation process of the large-size thin (the thickness is less than 10 mm) high-temperature corundum-mullite shed plate, and the prepared shed plate has high yield, almost no impurities, high temperature resistance, thermal shock resistance and excellent mechanical property.

Description

Preparation method of large-size thin high-temperature corundum-mullite slab
Technical Field
The invention relates to the technical field of refractory kiln furniture, in particular to a preparation method of a large-size (the length and width are more than 500 mm) thin high-temperature corundum-mullite slab.
Background
The shed plate is used as a special kiln furniture for supporting porcelain pieces in firing, and is always an important auxiliary material in the ceramic industry. In order to meet the generation requirement, the shed plate is required to have the properties of good thermal shock property, excellent high-temperature performance and the like. Most of the traditional shed plate materials are cordierite-mullite composite materials with good thermal shock resistance and excellent high-temperature performance, and shed plates made of materials such as silicon carbide, corundum-mullite and the like are widely used in later development.
Along with the development of functional ceramics in the society, such as soft magnetic (ferrite) materials, electronic insulating ceramics and other high-temperature industries, the corundum-mullite shed plate is widely used, has excellent high-temperature strength, thermal shock resistance and higher use temperature (1700 ℃), has good chemical stability and is not easy to react with fired products.
The shape of the corundum-mullite shed plate is simpler, but the corundum-mullite shed plate is generally prepared by a vibration press semi-dry method, which requires high material purity (impurities can influence the high-temperature service performance of the material), uniform density, good high-temperature mechanical property, larger forming area and thinner thickness. The large-scale corundum-mullite slab prepared by the method has the following problems: the production equipment requirement, high green body strength and low demoulding difficulty, and the problems of easy cracking and warping in the drying process, uneven product density and the like.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a preparation method of a large-size thin high-temperature corundum-mullite slab.
The invention adopts the following technical scheme for achieving the purpose:
a preparation method of a large-size thin high-temperature corundum-mullite slab comprises the following raw materials in parts by weight: 55-75 parts of aggregate5-15 parts of fine powder, 15-35 parts of micro powder and 0.3-1 part of self-initiated coagulant Isobam and 3-15 parts of water; the aggregate comprises corundum coarse aggregate and mullite fine aggregate; the fine powder is corundum fine powder and mullite fine powder; the micro powder is active Al2O3Micropowder and SiO2Micro-powder; weighing the components according to the proportion, uniformly mixing the components in a forced stirrer, pouring the mixture into a mold, curing the mixture at room temperature for 3 days, preserving the heat at 110 ℃ for 24 hours, and preserving the heat at 1550-1650 ℃ for 3-5 hours in an air atmosphere after demolding.
55-75 parts of corundum coarse aggregate and 35-45 parts of mullite fine aggregate in the aggregate; wherein the grain diameter of the corundum coarse aggregate is 1-3 mm, and the grain diameter of the mullite fine aggregate is more than 0 and less than 1 mm.
55-75 parts of corundum fine powder and 35-45 parts of mullite fine powder.
Active Al in the micro powder2O385-92 parts of micro powder and SiO28-15 parts of micro powder.
The grain size of the corundum fine powder is more than 0 mm and less than 0.1mm, and the grain size of the mullite fine powder is 325 meshes; active Al2O3The particle diameter of the micro powder is more than 0 and less than 10 mu m, SiO2The particle size of the micro powder is more than 0 and less than 2 mu m.
The self-initiating coagulant is one or more of Isobam-104, Isobam-600, Isobam-104, Isobam-600-AF or Isobam-104-WS.
The invention provides a preparation method of a large-size thin high-temperature corundum-mullite slab, which adopts a novel solidification forming agent Isobam as a bonding agent and prepares the large-size thin high-temperature corundum-mullite slab through wet forming; the molding process of the method is similar to the casting molding of concrete, and the binding agent Isobam is a high molecular compound which can play the roles of water reducing agent and dispersion in the mixing process; the solidification forming process is a process similar to flocculation of Isobam, micro powder particles and water, the addition amount of the Isobam in the blank is small (less than or equal to 1 percent), and after drying, the blank has high strength and is easy to demould. The method has the advantages of simple process and high yield, and the prepared large-size high-temperature corundum-mullite material has the characteristics of almost no impurities, high temperature resistance, thermal shock resistance, excellent mechanical property and the like.
Detailed description of the preferred embodiments
The first embodiment is as follows:
the large-size thin high-temperature corundum-mullite slab comprises the following raw materials in parts by weight: 65 parts of aggregate, 12 parts of fine powder, 23 parts of micro powder, 5 parts of external water and 0.5 part of Isobam-104.
In the aggregate, 60 parts of corundum coarse aggregate with the thickness of 1-3 mm and 40 parts of mullite fine aggregate with the thickness of 0-1 mm.
60 parts of corundum fine powder with the particle size of 0-0.1mm and 40 parts of 325-mesh mullite fine powder; fine powder of 0 to 10 μm Al2O390 parts of micro powder and 0-2 mu m SiO210 parts of micro powder. Weighing the components according to the proportion, uniformly mixing in a forced stirrer, pouring into a mould, curing at room temperature for 3 d, preserving heat at 110 ℃ for 24 h, and preserving heat at 1550 ℃ for 4h after demoulding.
Example two:
the large-size thin high-temperature corundum-mullite slab comprises the following raw materials in parts by weight: 70 parts of aggregate, 10 parts of fine powder, 20 parts of micro powder, 4 parts of additional water and 0.4 part of Isobam-600-AF additional water.
The aggregate comprises 65 parts of corundum coarse aggregate with the thickness of 1-3 mm and 35 parts of mullite fine aggregate with the thickness of 0-1 mm.
The fine powder comprises 65 parts of corundum fine powder with the particle size of 0-0.1mm and 35 parts of mullite fine powder with the particle size of 325 meshes.
Fine powder of 0 to 10 μm Al2O392 parts of micro powder, 0-2 mu m SiO28 parts of micro powder.
Weighing the components according to the proportion and uniformly mixing in a forced stirrer, weighing the components according to the proportion and uniformly mixing in the forced stirrer, pouring into a mould, curing at room temperature for 3 d, preserving heat at 110 ℃ for 24 h, and preserving heat at 1600 ℃ for 4h after demoulding.
Example three:
the large-size thin high-temperature corundum-mullite slab comprises the following raw materials in parts by weight: 65 parts of aggregate, 10 parts of fine powder, 25 parts of micro powder, 6 parts of additional water and 0.4 part of Isobam-600 additional water.
63 parts of corundum coarse aggregate with the thickness of 1-3 mm and 37 parts of mullite fine aggregate with the thickness of 0-1 mm.
The fine powder comprises 63 parts of corundum fine powder with the particle size of 0-0.1mm and 37 parts of mullite fine powder with the particle size of 325 meshes.
Fine powder of 0 to 10 μm Al2O391 parts of micro powder, 0-2 mu m SiO29 parts of micro powder.
Weighing the components according to the proportion and uniformly mixing in a forced stirrer, weighing the components according to the proportion and uniformly mixing in the forced stirrer, pouring into a mould, curing at room temperature for 3 d, preserving heat at 110 ℃ for 24 h, and preserving heat at 1550 ℃ for 4h after demoulding.
Example four:
the large-size thin high-temperature corundum-mullite slab comprises the following raw materials in parts by weight:
60 parts of aggregate, 10 parts of fine powder, 30 parts of micro powder, 8 parts of external water, and 0.3 part of each of Isobam-104 and Isobam-600.
In the aggregate, 70 parts of corundum coarse aggregate with the thickness of 1-3 mm and 30 parts of mullite fine aggregate with the thickness of 0-1 mm.
The fine powder comprises 70 parts of corundum fine powder with the particle size of 0-0.1mm and 30 parts of mullite fine powder with the particle size of 325 meshes.
Fine powder of 0 to 10 μm Al2O392 parts of micro powder, 0-2 mu m SiO28 parts of micro powder.
Weighing the components according to the proportion and uniformly mixing in a forced stirrer, weighing the components according to the proportion and uniformly mixing in the forced stirrer, pouring into a mould, curing at room temperature for 3 d, preserving heat at 110 ℃ for 24 h, and preserving heat at 1580 ℃ for 4h after demoulding.
Example five:
the large-size thin high-temperature corundum-mullite slab comprises the following raw materials in parts by weight: 58 parts of aggregate, 14 parts of fine powder, 28 parts of micro powder, 6 parts of additional water and 0.5 part of additional Isobam-104-WS.
In the aggregate, 68 parts of corundum coarse aggregate with the thickness of 1-3 mm and 38 parts of mullite fine aggregate with the thickness of 0-1 mm.
The fine powder comprises 68 parts of corundum fine powder with the particle size of 0-0.1mm and 38 parts of 325-mesh mullite fine powder.
Fine powder of 0 to 10 μm Al2O387 parts of micro powder, 0-2 mu mSiO213 parts of micro powder.
Weighing the components according to the proportion and uniformly mixing in a forced stirrer, weighing the components according to the proportion and uniformly mixing in the forced stirrer, pouring into a mould, curing at room temperature for 3 d, preserving heat at 110 ℃ for 24 h, and preserving heat at 1620 ℃ for 4h after demoulding.
According to the preparation scheme of the example I, a sample strip of 40 mm multiplied by 150 mm is poured, the sample strip is demoulded after being cured for 3 days at room temperature, the sample strip is placed into an oven and is kept at 110 ℃ for 24 hours, the dried sample strip is kept at 1550 ℃ for 4 hours to obtain a sintered sample block, and the sample block is subjected to air cooling and thermal shock for 20 times at 1400 ℃. The samples treated at different temperatures were tested for apparent porosity, bulk density, room temperature flexural strength and compressive strength (the treatment temperature is varied with respect to the length after demolding), and the test values are shown in Table 1.
Table 1.
Figure DEST_PATH_IMAGE001

Claims (6)

1. A preparation method of a large-size thin high-temperature corundum-mullite slab is characterized by comprising the following steps: the thin and large-size high-temperature corundum-mullite slab comprises the following raw materials in parts by weight: 55-75 parts of aggregate, 5-15 parts of fine powder, 15-35 parts of micro powder, and 0.3-1 part of self-initiated coagulant Isobam and 3-15 parts of water are additionally added; the aggregate comprises corundum coarse aggregate and mullite fine aggregate; the fine powder is corundum fine powder and mullite fine powder; the micro powder is active Al2O3Micropowder and SiO2Micro-powder; weighing the components according to the proportion, uniformly mixing the components in a forced stirrer, pouring the mixture into a mold, curing the mixture at room temperature for 3 days, preserving the heat at 110 ℃ for 24 hours, and preserving the heat at 1550-1650 ℃ for 3-5 hours in an air atmosphere after demolding.
2. The method for preparing a large-size thin high-temperature corundum-mullite slab as claimed in claim 1, wherein the method comprises the following steps: 55-75 parts of corundum coarse aggregate and 35-45 parts of mullite fine aggregate in the aggregate; wherein the grain diameter of the corundum coarse aggregate is 1-3 mm, and the grain diameter of the mullite fine aggregate is more than 0 and less than 1 mm.
3. The method for preparing a large-size thin high-temperature corundum-mullite slab as claimed in claim 1, wherein the method comprises the following steps: 55-75 parts of corundum fine powder and 35-45 parts of mullite fine powder.
4. The method for preparing a large-size thin high-temperature corundum-mullite slab as claimed in claim 1, wherein the method comprises the following steps: active Al in the micro powder2O385-92 parts of micro powder and SiO28-15 parts of micro powder.
5. The method for preparing a large-size thin high-temperature corundum-mullite slab as claimed in claim 1, wherein the method comprises the following steps: the grain size of the corundum fine powder is more than 0 mm and less than 0.1mm, and the grain size of the mullite fine powder is 325 meshes; active Al2O3The particle diameter of the micro powder is more than 0 and less than 10 mu m, SiO2The particle size of the micro powder is more than 0 and less than 2 mu m.
6. The method for preparing a large-size thin high-temperature corundum-mullite slab as claimed in claim 1, wherein the method comprises the following steps: the self-initiating coagulant Isobam is one or more of Isobam-104, Isobam-600, Isobam-104, Isobam-600-AF or Isobam-104-WS.
CN202010800341.2A 2020-08-11 2020-08-11 Preparation method of large-size thin high-temperature corundum-mullite slab Pending CN111892387A (en)

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