CN113149620A - Light mullite-spinel hollow sphere sagger pressurization forming process - Google Patents
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- 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
- C04B35/10—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 aluminium oxide
- C04B35/101—Refractories from grain sized mixtures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B11/00—Apparatus or processes for treating or working the shaped or preshaped articles
- B28B11/24—Apparatus or processes for treating or working the shaped or preshaped articles for curing, setting or hardening
- B28B11/243—Setting, e.g. drying, dehydrating or firing ceramic articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B3/00—Producing shaped articles from the material by using presses; Presses specially adapted therefor
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- 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
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/08—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding porous substances
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- 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
- C04B2235/3222—Aluminates other than alumino-silicates, e.g. spinel (MgAl2O4)
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- 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
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3427—Silicates other than clay, e.g. water glass
- C04B2235/3463—Alumino-silicates other than clay, e.g. mullite
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- 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
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/349—Clays, e.g. bentonites, smectites such as montmorillonite, vermiculites or kaolines, e.g. illite, talc or sepiolite
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- 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
- C04B2235/528—Spheres
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient
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Abstract
A sagger pressure forming process for light mullite-spinel hollow spheres relates to the field of refractory materials, and comprises the following steps of putting 8-12 parts by weight of Suzhou second mud, 8-12 parts by weight of alpha-alumina powder, 4-6 parts by weight of alpha-alumina micropowder, 6-8 parts by weight of fused corundum powder, 13-21 parts by weight of fused mullite powder, 0.2-1mm15-25 parts by weight of fused spinel hollow spheres, 1-2mm 4-6 parts by weight of fused spinel hollow spheres, 0-1mm5-15 parts by weight of light mullite particles and 1-2mm10-20 parts by weight of light mullite particles into a stirrer for full mixing, adding a binding agent pulp waste liquid, fully stirring to form a mixture with certain cohesiveness, pouring the mixture into a mold, pressure forming and sintering in a kiln, wherein the prepared sagger has the advantages of light weight and long service life of products, high cost performance.
Description
Technical Field
The invention relates to the field of refractory materials, in particular to a pressure forming process of a light mullite-spinel hollow sphere sagger.
Background
Currently, high temperature saggers suitable for temperatures above 1500 ℃ are all made from electrically fused mullite and corundum, for example, chinese patent application CN201810903009.1 discloses a "sagger for high temperature firing" made from alumina powder, kaolin powder, clay powder, white corundum, quartz, mullite, etc. as raw materials, and then fired at high temperature after mixing and molding. Compared with the quartz, mullite and saggar which is synthesized in advance on the market and then is formed by mixing, the produced finished product phase is more uniform, the color and the thermal shock stability are better, and the thermal expansion coefficient of the produced phase is small, so that the thermal shock resistance is extremely high, the quartz is added, the thermal shock performance can be improved, the crack resistance, the uniformity and the quality stability of the product can be kept during batch production, and the saggar is suitable for the environment with larger temperature difference. The method has the defects of short service life and instability, and takes sintering of the fluorescent powder as an example, the service life is 10-30 times at present.
Disclosure of Invention
In order to further prolong the service life of the sagger for sintering the product with the sintering temperature higher than 1500 ℃, the invention overcomes the defects and provides the pressure forming process of the light mullite-spinel hollow sphere sagger with light weight, high cost performance and long service life. The main innovation lies in that high-purity light high-strength mullite grains are used for replacing electric melting mullite, spinel hollow balls are used for replacing corundum grains, the high-purity light high-strength mullite is formed through a pressing process and is sintered at high temperature for use, and the service life of the product can be greatly prolonged.
The method is implemented specifically as follows: the light mullite-spinel hollow sphere sagger pressure forming process is characterized by comprising the following steps of putting 8-12 parts of Suzhou second mud, 8-12 parts of alpha-alumina powder, 4-6 parts of alpha-alumina micro powder, 6-8 parts of fused corundum powder, 13-21 parts of fused mullite powder, 0.2-1mm15-25 parts of fused spinel hollow spheres, 1-2mm 4-6 parts of fused spinel hollow spheres, 0-1mm5-15 parts of light mullite particles and 1-2mm10-20 parts of light mullite particles into a stirrer for full mixing, adding a binding agent pulp waste liquid, fully stirring to form a mixture with certain cohesiveness, pouring the mixture into a mold, pressure forming and sintering in a kiln.
Al of the Suzhou No. two mud2O333-35% of Fe2O3≤0.80% ，K2O+ Na2O is less than or equal to 0.80 percent, and the fineness is less than 10 percent after 320 meshes.
Al of the alpha-alumina powder2O3The content is more than 95 percent, and the fineness is less than 10 percent after 320 meshes.
Al of the alpha-alumina micropowder2O3The content is more than 95 percent, and the median diameter D50 of the particle size is less than 2 mu m.
Al of the fused corundum powder2O3Content greater than 98.5%, finenessThe 320-mesh sieve residue is less than 10 percent.
Al of the electrically fused mullite powder2O3The content is 68-73%, the fineness is 320 meshes, and the residue is less than 10%.
The electric melting spinel hollow ball adopts an electric melting spinel hollow ball with a crystal bond mark.
The volume density of the light mullite grains is less than or equal to 2g/cm3，Al2O3%≥60，SiO2%≤37，Al2O3+SiO2%≥97，Fe2O3+TiO2%≤2。
The mass percentage concentration of solid matters in the waste paper pulp liquid serving as the binding agent is 20-25%.
During preparation, the waste paper pulp liquid as the binding agent is added into the powder and the aggregate to form a mixture with the weight content of the waste paper pulp liquid being 6-8%, the mixture is fully stirred for later use, the mixture is poured into a mould, pressed and molded, demoulded, then dried in a drying kiln and sent into the kiln for sintering, the sintering temperature is controlled between 1350 ℃ and 1550 ℃, and the heat preservation time is 4-8 hours.
The light mullite particles are prepared by introducing saw dust into high-purity clay and alumina powder as pore-forming agents, and crushing the high-temperature sintered light mullite particles after high-temperature sintering, the high-temperature sintered light mullite particles contain rich holes, stress generated by rapid cooling and rapid heating can be effectively released in practical application, and generated micro cracks and macro cracks can be effectively released. The spinel hollow sphere has a smaller expansion coefficient than an alumina hollow sphere, the melting point of the product is 2100 ℃, and the spinel hollow sphere also has good thermal shock resistance, and the introduction of the spinel hollow sphere can effectively improve the service temperature of the product, thereby laying a foundation for the production of a long-life sagger with the service temperature of more than 1500 ℃.
Compared with the traditional product, the sagger has the advantages of light weight, long service life and high cost performance.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The raw material standards involved in the examples are:
al of Suzhou mud II2O333-35% of Fe2O3≤0.80% ，K2O+ Na2O is less than or equal to 0.80 percent, and the fineness is less than 10 percent after 320 meshes.
Al of alpha-alumina powder2O3The content is more than 95 percent, and the fineness is less than 10 percent after 320 meshes.
Al of alpha-alumina micropowder2O3The content is more than 95 percent, and the median diameter D50 of the particle size is less than 2 mu m.
Al of fused corundum powder2O3The content is more than 98.5 percent, and the screen residue with the fineness of 320 meshes is less than 10 percent.
Al of electrically fused mullite powder2O3The content is 68-73%, the fineness is 320 meshes, and the residue is less than 10%.
The electric melting spinel hollow ball adopts an electric melting spinel hollow ball which is named as Jingbang, and the indexes are as follows:
the light mullite particles are prepared by introducing saw dust into high-purity clay and alumina powder as pore-forming agents, sintering at high temperature and crushing, and the volume density is less than or equal to 2g/cm3，Al2O3%≥60，SiO2%≤37，Al2O3+SiO2%≥97，Fe2O3+TiO2%≤2。
The mass percentage concentration of the solid matters of the paper waste liquid used as the binding agent is 20-25%.
Example 1, a lightweight mullite-spinel hollow sphere sagger pressure forming process includes weighing 12 parts by weight of suzhou second mud, 8 parts by weight of alpha-alumina powder, 4 parts by weight of alpha-alumina micropowder, 8 parts by weight of fused corundum powder, 13 parts by weight of fused mullite powder, 0.2-1mm25 parts by weight of fused spinel hollow spheres, 1-2mm6 parts by weight of fused spinel hollow spheres, 0-1mm5 parts by weight of lightweight mullite particles, and 1-2mm19 parts by weight of lightweight mullite particles, placing the materials in a stirrer for full mixing, adding a binding agent pulp waste liquid to form a mixture with the weight content of the pulp waste liquid being 6%, fully stirring the mixture for later use, pouring the mixture into a mold, pressure forming, demolding, drying in a drying kiln, feeding the mixture into a kiln for firing, wherein the firing kiln can be a shuttle kiln, a tunnel kiln, a down-flame kiln or a roller path kiln, the firing temperature is controlled at 1450 ℃, the holding time was 6 hours and the performance index of the finished product is shown in table 1.
Examples 2 to 7, reference example 1, the raw material compatibility and the finished product performance index of each example are shown in table 1.
TABLE 1
In examples 8 to 10, the raw material compatibility was the same as in example 3, the heat retention time after firing was 6 hours, and the firing temperature and the performance index of the finished product are shown in Table 2.
TABLE 2
Therefore, the optimal sintering temperature in the preparation method is 1450 +/-50 ℃.
In examples 11 to 13, the raw material formulation was the same as in example 3, the firing temperature was 1450 ℃, and the holding time and the performance index of the final product were as shown in Table 3.
TABLE 3
The sagger prepared in the above examples 1 to 13 has no crack, no drop, no damage in the surface state after 30 times of use, and as can be seen from tables 1 to 3, the service life is at least more than 40 times, and as high as 60 times, which is far longer than the service life of the current high temperature sagger in the market by 10 to 30 times, and the sagger is light in weight and has higher cost performance.
Claims (7)
1. The light mullite-spinel hollow sphere sagger pressure forming process is characterized by comprising the following steps of putting 8-12 parts of Suzhou second mud, 8-12 parts of alpha-alumina powder, 4-6 parts of alpha-alumina micro powder, 6-8 parts of fused corundum powder, 13-21 parts of fused mullite powder, 0.2-1mm15-25 parts of fused spinel hollow spheres, 1-2mm 4-6 parts of fused spinel hollow spheres, 0-1mm5-15 parts of light mullite particles and 1-2mm10-20 parts of light mullite particles into a stirrer for full mixing, adding a binding agent pulp waste liquid, fully stirring to form a mixture with certain cohesiveness, pouring the mixture into a mold, pressure forming and sintering in a kiln.
2. The process of claim 1, wherein the Al of suzhou mud is a spinel hollow ball sagger2O333-35% of Fe2O3≤0.80% ，K2O+ Na2O is less than or equal to 0.80 percent, and the fineness is less than 10 percent after 320 meshes; al of the alpha-alumina powder2O3The content is more than 95 percent, and the fineness is less than 10 percent after 320 meshes; al of the alpha-alumina micropowder2O3The content is more than 95 percent, and the median diameter D50 of the particle size is less than 2 mu m; al of the fused corundum powder2O3The content is more than 98.5 percent, the fineness is less than 10 percent after 320 meshes; al of the electrically fused mullite powder2O3The content is 68-73%, the fineness is 320 meshes, and the residue is less than 10%; the electric melting spinel hollow ball adopts an electric melting spinel hollow ball with a crystal bond mark; the volume density of the light mullite grains is less than or equal to 2g/cm3，Al2O3%≥60，SiO2%≤37，Al2O3+SiO2%≥97，Fe2O3+TiO2The percentage is less than or equal to 2; the mass percentage concentration of solid matters of the pulp waste liquid is 20-25%.
3. The lightweight mullite-spinel hollow sphere sagger pressure forming process as claimed in claim 1 or 2, wherein the lightweight mullite grains are prepared by introducing saw dust as a pore forming agent into high-purity clay and alumina powder, sintering at high temperature and then crushing.
4. The pressure forming process of the light mullite-spinel hollow sphere sagger as claimed in claim 1, wherein the pulp waste liquid of the binding agent is added into each powder and aggregate to form a mixture with the weight content of the pulp waste liquid of 6-8%, the mixture is fully stirred for later use, and the mixture is poured into a mold, is subjected to pressure forming, is demoulded, is put into a drying kiln for drying, and is sent into the kiln for sintering.
5. The pressure forming process of the lightweight mullite-spinel hollow sphere sagger as claimed in claim 1 or 4, wherein the firing temperature is controlled between 1350 ℃ and 1550 ℃ and the holding time is 4-8 hours.
6. The pressure forming process of the light mullite-spinel hollow sphere sagger as claimed in claim 5, wherein the firing temperature is 1450 ± 50 ℃.
7. The lightweight mullite-spinel hollow sphere sagger pressure forming process of claim 1 is characterized in that the raw materials comprise the following components in parts by weight: 10 parts of Suzhou second mud, 10 parts of alpha-alumina powder, 5 parts of alpha-alumina micro powder, 7 parts of fused corundum powder, 18 parts of fused mullite powder, 0.2-1mm20 parts of fused spinel hollow spheres, 1-2mm5 parts of fused spinel hollow spheres, 0-1mm10 parts of light mullite particles and 1-2mm15 parts of light mullite particles.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113548884A (en) * | 2021-08-04 | 2021-10-26 | 浙江吉昌新材料有限公司 | Sagger containing cordierite and composite spinel mullite and preparation method thereof |
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| CN103482993A (en) * | 2013-09-13 | 2014-01-01 | 湖南仁海科技材料发展有限公司 | Adamantine spar and mullite composite material sagger and method for manufacturing sagger |
| CN108033798A (en) * | 2017-12-12 | 2018-05-15 | 浙江大学 | Light cordierite-spinel hollow ball saggar, preparation method and applications |
| CN108341666A (en) * | 2018-04-03 | 2018-07-31 | 郑州大学 | A kind of saggar and preparation method thereof |
| CN110818398A (en) * | 2018-08-09 | 2020-02-21 | 山东莱科陶瓷材料有限公司 | Sagger for high-temperature firing and preparation method thereof |
| CN111056834A (en) * | 2019-12-17 | 2020-04-24 | 洛阳索莱特材料科技有限公司 | Preparation method of spinel-mullite ceramic sagger |
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2021
- 2021-03-24 CN CN202110311806.2A patent/CN113149620A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101508588A (en) * | 2009-02-19 | 2009-08-19 | 浙江大学 | Composite high-temperature deck of high-performance mullite and spinel, and method of producing the same |
| CN103396141A (en) * | 2013-08-07 | 2013-11-20 | 武汉钢铁(集团)公司 | Lightweight high-strength heat-insulation refractory castable |
| CN103482993A (en) * | 2013-09-13 | 2014-01-01 | 湖南仁海科技材料发展有限公司 | Adamantine spar and mullite composite material sagger and method for manufacturing sagger |
| CN108033798A (en) * | 2017-12-12 | 2018-05-15 | 浙江大学 | Light cordierite-spinel hollow ball saggar, preparation method and applications |
| CN108341666A (en) * | 2018-04-03 | 2018-07-31 | 郑州大学 | A kind of saggar and preparation method thereof |
| CN110818398A (en) * | 2018-08-09 | 2020-02-21 | 山东莱科陶瓷材料有限公司 | Sagger for high-temperature firing and preparation method thereof |
| CN111056834A (en) * | 2019-12-17 | 2020-04-24 | 洛阳索莱特材料科技有限公司 | Preparation method of spinel-mullite ceramic sagger |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113548884A (en) * | 2021-08-04 | 2021-10-26 | 浙江吉昌新材料有限公司 | Sagger containing cordierite and composite spinel mullite and preparation method thereof |
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