CN105669241A - Preparation method of closed-pore-structure light fireproof corundum - Google Patents
Preparation method of closed-pore-structure light fireproof corundum Download PDFInfo
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- CN105669241A CN105669241A CN201511018434.5A CN201511018434A CN105669241A CN 105669241 A CN105669241 A CN 105669241A CN 201511018434 A CN201511018434 A CN 201511018434A CN 105669241 A CN105669241 A CN 105669241A
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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
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
- C04B38/0635—Compounding ingredients
- C04B38/0645—Burnable, meltable, sublimable materials
- C04B38/067—Macromolecular compounds
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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
- C04B35/10—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
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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
- 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
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
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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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
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- Porous Artificial Stone Or Porous Ceramic Products (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a preparation method of closed-pore-structure light fireproof corundum and aims to solve a technical problem of low closed pore ratio of the closed-pore fireproof corundum prepared in the prior art. In the technical scheme, raw materials include, by mass, 70-98.5% of alumina powder and 0.5-10% of magnesium oxide powder, and polymer-based microspheres being 1-20% by mass is employed as a pore-forming agent, wherein the components are mixed and are ball-milled for 10-50 h, and then are moulded under 30-250 MPa. A moulded green body is subjected to temperature maintenance at 600 DEG C in air atmosphere for 1-2 h and then at 1500-1800 for 1-5 h to prepare the closed-pore-structure light fireproof corundum. By adding the polymer-based microspheres to alumina slurry with adjustment on addition quantity of the polymer-based microspheres, the fireproof corundum is 1-25% in closed pore ratio and 1-5% in exposed pore ratio and is 1-100 [mu]m in pore diameter range.
Description
Technical field
The preparation method that the present invention relates to the fire-resistant corundum of a kind of closed pore, particularly to the preparation method of a kind of hole-closing structure light-weight refractory corundum.
Background technology
Alumina-based refractory is widely used in the heat-insulation and heat-preservation such as heat insulating coat, high temperature furnace lining field. Along with the raising day by day that environmental protection and energy saving are required, and refractory material uses the increasingly sophisticated of environment, and traditional corundum refractory cannot meet technology requirement. The performance requirement of current refractory material mainly has following several respects: (1) thermal shock resistance and high-temperature anti-corrosion performance need further raising badly, increases service life; (2) design of lighting, to reduce cost, improves energy-saving effect. Therefore, low-density, high intensity, low heat conduction are the main development directions of heat-barrier material both at home and abroad at present.
Realizing holding one's breath pore structure and reducing its open pore rate in aluminium oxide ceramics is a kind of effective means simultaneously realizing lightweight, low heat conduction and good corrosion resistance. The method of report mainly has interpolation pore creating material method and foaming at present. Document 1 " Yuan Lei, Yu Jingkun, Yan Zheng state etc. the corundum of a kind of hole-closing structure-magnesium aluminate spinel matter refractory aggregate and preparation method, China, CN103833383B [P], 2015 " disclose a kind of have good thermal shock resistance can the preparation method of closed pore corundum. The method uses carborundum, silicon nitride or aluminium nitride as high-temperature foaming agent, after 100～500MPa forming under the pressure, is sintered by molding blank at 1600～1800 DEG C of temperature. The weak point of the method is the purity that the introducing of high-temperature foaming agent reduces corundum, has slackened its corrosion resistance in high temperature environments, additionally requires too high to the condition of molding of material, substantially increases production cost. Document 2 " Gu Huazhi, Fu Lvping, Huang Ao etc. a kind of micro-closed pore of lightweight containing magnesium corundum fireproof aggregate and preparation method thereof, China, CN104446543A [P], 2015 " disclose the aperture fire-resistant corundum preparation method of micro-closed pore little, resistance to erosion. The method is with γ-Al2O3Fine powder, nano alumina powder and fine magnesium oxide micro-powder are raw material, are incubated 1-8 hour at 1750-1900 DEG C of temperature. Its shortcoming is that sintering temperature is too high, and it is big to burn till energy consumption, and closes air vent aperture and cannot adjust.
In sum, although hole-closing structure corundum prepared at present possesses certain performance requirement, but there is preparation technology and require height, closed pore porosity difficulty controls, the defects such as aperture is single, it is difficult to meet actual industrial production requirement.
Summary of the invention
In order to overcome the fire-resistant corundum of closed pore prepared by existing method to hold one's breath the low deficiency of porosity, the preparation method that the present invention provides a kind of hole-closing structure light-weight refractory corundum. The method with mass fraction be 70-98.5% alumina powder jointed, with mass fraction be 0.5-10% magnesia powder for raw material, with mass fraction be 1-20% polymer-matrix microsphere for pore creating material, ball milling 10-50 hour after mixing, then in the forming under the pressure of 30-250MPa, by the base substrate after molding in air atmosphere 600 DEG C be incubated 1-2 hour, then it is incubated 1-5 hour in 1500-1800 DEG C, obtains hole-closing structure light-weight refractory corundum. The inventive method by adding polymer-matrix microsphere in alumina slurry, and by adjusting the addition of polymer microballoon, the porosity of holding one's breath of the fire-resistant corundum of preparation is 1-25%, and apparent porosity is 1-5%, and bulk density is 2.8-3.8g/cm3, pore diameter range 1-100 μm; The fire-resistant corundum of preparation is with α-Al2O3For principal crystalline phase, and containing magnesium aluminate spinel phase, without other impurity phases; Fire-resistant corundum after sintering has the erosiveness of the media such as good thermal shock resistance and anti-slag.
The technical solution adopted for the present invention to solve the technical problems: the preparation method of a kind of hole-closing structure light-weight refractory corundum, is characterized in comprising the following steps:
Step one, with mass fraction be 70-98.5% the magnesia powder of alumina powder jointed and 0.5-10% mix for raw material, add the polymer-matrix microsphere of 1-20wt%;
Or, it is placed in aluminum nitrate solution by polymer-matrix microsphere mechanical agitation 2h, 80 DEG C dry, and obtain mixing microsphere. According to mixing microsphere: alumina powder: magnesia powder=10:89:1 mixing.
After step 2, compound step one obtained are dispersed in dehydrated alcohol, it are placed in planetary ball mill ball milling 10-50h, ball milling disposed slurry is obtained premix material after drying in 80 DEG C.
Step 3, premix material step 2 prepared are placed in mould in the forming under the pressure of 30-250MPa, obtain hole-closing structure light-weight refractory corundum base substrate.
Step 4, hole-closing structure light-weight refractory corundum base substrate is placed in Muffle furnace, is warming up to 600 DEG C, be incubated 1-2h, remove polymer-matrix microsphere, then heat to 1500-1800 DEG C, be incubated 1-5h, insulation naturally cools to room temperature after terminating, and obtains hole-closing structure light-weight refractory corundum.
Described polymer-matrix microsphere is any one of polymethyl methacrylate or polystyrene.
The invention has the beneficial effects as follows: the method with mass fraction be 70-98.5% alumina powder jointed, with mass fraction be 0.5-10% magnesia powder for raw material, with mass fraction be 1-20% polymer-matrix microsphere for pore creating material, ball milling 10-50 hour after mixing, then in the forming under the pressure of 30-250MPa, by the base substrate after molding in air atmosphere 600 DEG C be incubated 1-2 hour, then it is incubated 1-5 hour in 1500-1800 DEG C, obtains hole-closing structure light-weight refractory corundum. The inventive method by adding polymer-matrix microsphere in alumina slurry, and by adjusting the addition of polymer microballoon, the porosity of holding one's breath of the fire-resistant corundum of preparation is 1-25%, and apparent porosity is 1-5%, and bulk density is 2.8-3.8g/cm3, pore diameter range 1-100 μm; The fire-resistant corundum of preparation is with α-Al2O3For principal crystalline phase, and containing magnesium aluminate spinel phase, without other impurity phases; Fire-resistant corundum after sintering has the erosiveness of the media such as good thermal shock resistance and anti-slag.
Below in conjunction with the drawings and specific embodiments, the present invention is elaborated.
Accompanying drawing explanation
Fig. 1 is the flow chart of the preparation method of hole-closing structure light-weight refractory corundum of the present invention.
Fig. 2 is the stereoscan photograph of the hole-closing structure light-weight refractory corundum of the inventive method embodiment 1 preparation.
Detailed description of the invention
Following example are with reference to Fig. 1-2.
Embodiment 1:
(1) alumina powder, magnesia powder 99:1 in mass ratio is mixed, the addition of polymethyl methacrylate (hereinafter referred to as PMMA) microsphere is 1-20wt%, dispersed in dehydrated alcohol it is placed on planetary ball mill ball milling 10h, by ball milling disposed slurry in 80 DEG C of dried premix material.
(2) gained premix material is placed in mould axially embosses, 30MPa pressurize 3 minutes, obtain hole-closing structure light-weight refractory corundum base substrate.
(3) being placed in Muffle furnace by hole-closing structure light-weight refractory corundum base substrate, be warming up to 600 DEG C, be incubated 1h, remove PMMA microsphere, then heat to 1650 DEG C, be incubated 3h, insulation naturally cools to room temperature after terminating, and obtains hole-closing structure light-weight refractory corundum.
Hole-closing structure light-weight refractory corundum prepared by the present embodiment, its porosity of holding one's breath is 1-25%, and open pore rate is 1-4%, and bulk density is 2.8-3.8g/cm3. Figure it is seen that containing hole of holding one's breath in a large number inside the hole-closing structure light-weight refractory corundum prepared of the present embodiment, and base densities.
Embodiment 2:
(1) being mixed by alumina powder, magnesia powder 99.5:0.5 in mass ratio, the addition of PMMA microsphere is 5-20wt%, dispersed in dehydrated alcohol is placed on planetary ball mill ball milling 10h, by ball milling disposed slurry in 80 DEG C of dried premix material.
(2) gained premix material is placed in mould axially embosses, 30MPa pressurize 3 minutes, isostatic cool pressing 250MPa pressurize 1 minute, obtain hole-closing structure light-weight refractory corundum base substrate.
(3) being placed in Muffle furnace by hole-closing structure light-weight refractory corundum base substrate, be warming up to 600 DEG C, be incubated 2h, remove PMMA microsphere, then heat to 1500 DEG C, be incubated 5h, insulation naturally cools to room temperature after terminating, and obtains hole-closing structure light-weight refractory corundum.
The closed pore corundum prepared by the present embodiment method, its porosity of holding one's breath is 5-25%, and open pore rate is 1-5%, and bulk density is 2.9-3.8g/cm3。
Embodiment 3:
(1) being mixed by alumina powder, magnesia powder 9:1 in mass ratio, the addition of PMMA microsphere is 5-20wt%, dispersed in dehydrated alcohol is placed on planetary ball mill ball milling 50h, by ball milling disposed slurry in 80 DEG C of dried premix material.
(2) gained premix material is placed in mould axially embosses, 30MPa pressurize 3 minutes, obtain hole-closing structure light-weight refractory corundum base substrate.
(3) being placed in Muffle furnace by hole-closing structure light-weight refractory corundum base substrate, be warming up to 600 DEG C, be incubated 2h, remove PMMA microsphere, then heat to 1800 DEG C, be incubated 1h, insulation naturally cools to room temperature after terminating, and obtains hole-closing structure light-weight refractory corundum.
Embodiment 4:
(1) being placed in aluminum nitrate solution by PMMA microsphere mechanical agitation 2h, 80 DEG C dry.
(2) above-mentioned dry microsphere is mixed with alumina powder, magnesia powder 10:89:1 in mass ratio, dispersed in dehydrated alcohol be placed on planetary ball mill ball milling 20h, by ball milling disposed slurry in 80 DEG C of dried premix material.
(3) gained premix material is placed in mould axially embosses, 30MPa pressurize 3 minutes, obtain hole-closing structure light-weight refractory corundum base substrate.
(4) being placed in Muffle furnace by hole-closing structure light-weight refractory corundum base substrate, be warming up to 600 DEG C, be incubated 2h, remove PMMA microsphere, then heat to 1600 DEG C, be incubated 2h, insulation naturally cools to room temperature after terminating, and obtains hole-closing structure light-weight refractory corundum.
Embodiment 5:
(1) being placed in aluminum nitrate solution by PMMA microsphere mechanical agitation 2h, 80 DEG C dry, in the lower 500 DEG C of insulation 2h of argon gas atmosphere.
(2) above-mentioned dry microsphere is mixed with alumina powder, magnesia powder 20:79:1 in mass ratio, dispersed in dehydrated alcohol be placed on planetary ball mill ball milling 30h, by ball milling disposed slurry in 80 DEG C of dried premix material.
(3) gained premix material is placed in mould axially embosses, 30MPa pressurize 3 minutes, isostatic cool pressing 100MPa pressurize 3 minutes, obtain hole-closing structure light-weight refractory corundum base substrate.
(4) being placed in Muffle furnace by hole-closing structure light-weight refractory corundum base substrate, be warming up to 600 DEG C, be incubated 2h, remove PMMA microsphere, then heat to 1650 DEG C, be incubated 4h, insulation naturally cools to room temperature after terminating, and obtains hole-closing structure light-weight refractory corundum.
Embodiment 6:
The present embodiment uses polystyrene (PS) microsphere to replace PMMA microsphere as pore creating material, and all the other steps are with above-described embodiment 1-5.
The present invention uses the microsphere of polymer-matrix as pore creating material, utilizes the feature of its low-temperature oxidation, the hole-closing structure corundum of preparation pure phase. It is low that prepared closed pore corundum has open pore rate, and porosity of holding one's breath is adjustable, the feature that closed pore aperture is controlled, intensity is high, thermal conductivity is low, thermal shock resistance is good and corrosion resistance is strong, it is adaptable to uses under hot environment.
Claims (2)
1. the preparation method of a hole-closing structure light-weight refractory corundum, it is characterised in that comprise the following steps:
Step one, with mass fraction be 70-98.5% the magnesia powder of alumina powder jointed and 0.5-10% mix for raw material, add the polymer-matrix microsphere of 1-20wt%;
Or, it is placed in aluminum nitrate solution by polymer-matrix microsphere mechanical agitation 2h, 80 DEG C dry, and obtain mixing microsphere; According to mixing microsphere: alumina powder: magnesia powder=10:89:1 mixing;
After step 2, compound step one obtained are dispersed in dehydrated alcohol, it are placed in planetary ball mill ball milling 10-50h, ball milling disposed slurry is obtained premix material after drying in 80 DEG C;
Step 3, premix material step 2 prepared are placed in mould in the forming under the pressure of 30-250MPa, obtain hole-closing structure light-weight refractory corundum base substrate;
Step 4, hole-closing structure light-weight refractory corundum base substrate is placed in Muffle furnace, is warming up to 600 DEG C, be incubated 1-2h, remove polymer-matrix microsphere, then heat to 1500-1800 DEG C, be incubated 1-5h, insulation naturally cools to room temperature after terminating, and obtains hole-closing structure light-weight refractory corundum.
2. the preparation method of hole-closing structure light-weight refractory corundum according to claim 1, it is characterised in that: described polymer-matrix microsphere is any one of polymethyl methacrylate or polystyrene.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114195548A (en) * | 2021-12-30 | 2022-03-18 | 中国工程物理研究院电子工程研究所 | Preparation method of light electric porcelain and light electric porcelain |
| CN114315410A (en) * | 2021-12-31 | 2022-04-12 | 八龙应用材料科技(海南)有限公司 | Porous heat-insulating ceramic material with closed pore structure and preparation method thereof |
| CN116120045A (en) * | 2022-12-30 | 2023-05-16 | 新化县顺达电子陶瓷有限公司 | Ceramic material for light low-heat-conduction 5G signal base station |
| CN116496101A (en) * | 2023-04-24 | 2023-07-28 | 武汉科技大学 | Low-heat-conductivity micro-closed cell aluminum-rich spinel material and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103467072A (en) * | 2013-08-27 | 2013-12-25 | 中国科学院宁波材料技术与工程研究所 | Preparation method for light microporous corundum ceramic |
| CN104446635A (en) * | 2014-11-10 | 2015-03-25 | 西北工业大学 | Method for preparing closed-pore porous heat-insulating alumina ceramic |
-
2015
- 2015-12-29 CN CN201511018434.5A patent/CN105669241A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103467072A (en) * | 2013-08-27 | 2013-12-25 | 中国科学院宁波材料技术与工程研究所 | Preparation method for light microporous corundum ceramic |
| CN104446635A (en) * | 2014-11-10 | 2015-03-25 | 西北工业大学 | Method for preparing closed-pore porous heat-insulating alumina ceramic |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114195548A (en) * | 2021-12-30 | 2022-03-18 | 中国工程物理研究院电子工程研究所 | Preparation method of light electric porcelain and light electric porcelain |
| CN114195548B (en) * | 2021-12-30 | 2023-06-09 | 中国工程物理研究院电子工程研究所 | Preparation method of light electroceramics and light electroceramics |
| CN114315410A (en) * | 2021-12-31 | 2022-04-12 | 八龙应用材料科技(海南)有限公司 | Porous heat-insulating ceramic material with closed pore structure and preparation method thereof |
| CN116120045A (en) * | 2022-12-30 | 2023-05-16 | 新化县顺达电子陶瓷有限公司 | Ceramic material for light low-heat-conduction 5G signal base station |
| CN116120045B (en) * | 2022-12-30 | 2023-12-08 | 新化县顺达电子陶瓷有限公司 | Ceramic material for light low-heat-conduction 5G signal base station |
| CN116496101A (en) * | 2023-04-24 | 2023-07-28 | 武汉科技大学 | Low-heat-conductivity micro-closed cell aluminum-rich spinel material and preparation method thereof |
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