CN101671046B - Method for manufacturing high-purity magnesium-aluminum spinel - Google Patents
Method for manufacturing high-purity magnesium-aluminum spinel Download PDFInfo
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- CN101671046B CN101671046B CN2008101956708A CN200810195670A CN101671046B CN 101671046 B CN101671046 B CN 101671046B CN 2008101956708 A CN2008101956708 A CN 2008101956708A CN 200810195670 A CN200810195670 A CN 200810195670A CN 101671046 B CN101671046 B CN 101671046B
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- Prior art keywords
- mgo
- aluminum spinel
- manufacturing
- purity magnesium
- magnesium
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- 229910052596 spinel Inorganic materials 0.000 title claims abstract description 22
- 239000011029 spinel Substances 0.000 title claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 title abstract description 12
- 238000000227 grinding Methods 0.000 claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000007493 shaping process Methods 0.000 claims abstract description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 15
- 238000003303 reheating Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000002131 composite material Substances 0.000 claims description 10
- 239000011812 mixed powder Substances 0.000 claims description 10
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 235000019830 sodium polyphosphate Nutrition 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 3
- 238000001354 calcination Methods 0.000 abstract description 3
- 238000005272 metallurgy Methods 0.000 abstract description 3
- 239000004568 cement Substances 0.000 abstract description 2
- 239000011521 glass Substances 0.000 abstract description 2
- 238000002844 melting Methods 0.000 abstract description 2
- 230000008018 melting Effects 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000000919 ceramic Substances 0.000 abstract 1
- 238000005260 corrosion Methods 0.000 abstract 1
- 230000007797 corrosion Effects 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000005453 pelletization Methods 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 59
- 239000000395 magnesium oxide Substances 0.000 description 29
- 239000002994 raw material Substances 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 6
- 239000011777 magnesium Substances 0.000 description 6
- GANNOFFDYMSBSZ-UHFFFAOYSA-N [AlH3].[Mg] Chemical compound [AlH3].[Mg] GANNOFFDYMSBSZ-UHFFFAOYSA-N 0.000 description 5
- 229910052749 magnesium Inorganic materials 0.000 description 4
- -1 magnesium aluminate Chemical class 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 229960004418 trolamine Drugs 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 238000004880 explosion Methods 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910020068 MgAl Inorganic materials 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 239000011819 refractory material Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 239000011010 synthetic spinel Substances 0.000 description 2
- 241001149900 Fusconaia subrotunda Species 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- HIGRAKVNKLCVCA-UHFFFAOYSA-N alumine Chemical compound C1=CC=[Al]C=C1 HIGRAKVNKLCVCA-UHFFFAOYSA-N 0.000 description 1
- 229910001570 bauxite Inorganic materials 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 238000009749 continuous casting Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000005445 natural material Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention provides a method for manufacturing high-purity magnesium-aluminum spinel, and relates to a method for manufacturing a high-quality fireproof material used in all kinds of thermal equipment widely applied in industries such as metallurgy, cement, glass and ceramics. The method comprises the following steps: mixing 50 to 95 weight percent of Gamma-Al2O3 and 50 to 5 weight percent of dead burnt MgO evenly; carrying out ultrafine grinding and mechanical classification; carrying out pelletizing, shaping and drying; and finally, obtaining finished products by calcining for 8 to 20 hours inside an ultrahigh temperature vertical kiln at a temperature of between 1,820 and 1,930 DEG C. The manufacturing method solves the problems in the prior art of low material density and low production capacity. The magnesium-aluminum spinel obtained by the manufacturing method has the characteristics of high melting point, low coefficient of heat expansion, excellent thermal conductivity, strong chemical corrosion resistance, and the like.
Description
Technical field
The present invention relates to the production method of the high-quality refractory material on a kind of various Thermal Equipments that are widely used in industries such as metallurgy, cement, glass, pottery, relate in particular to a kind of production method of magnesium-aluminium spinel.
Background technology
Along with the development of continuous casting of iron and steel and furnace outer refining technology, the part refining process is transferred to the ladle from steel melting furnace and is carried out, and this just makes ladle be not only the elevated temperature vessel that stores molten steel, and becomes a kind of special metallurgy equipment.At present lining material in the ladle mainly is a magnesium-aluminium spinel, and magnesium-aluminium spinel is big because of fusing point height, hardness, heat-shock resistance and the excellent refractories industry that is widely used in of anti-scouring.But the content of magnesium aluminate spinel in natural minerals is especially few, so magnesium aluminate spinel all is by containing Al
2O
3Natural mineral raw or high-purity α-Al with MgO
2O
3(or γ-Al
2O
3) and MgO manually synthetic.Owing to be subjected to the limitation of the technology of sintering equipment, the product firing temperature generally about 1600-1800 ℃, needs the long solid phase reaction time usually, thus bring the energy consumption height, yield poorly, the problems such as labor productivity is low, quality stability difference.Produce one of raw materials used α-Al for high-purity magnesium-aluminum spinel
2O
3, because α-Al
2O
3Need to be 1400 ℃ of left and right sides pre-burnings, so that α-Al
2O
3Activity be starkly lower than γ-Al
2O
3If, can be with γ-Al
2O
3(commercial alumina), reheating magnesia are raw material, and the introducing by grinding aid improves the Raw material processing fineness, adopt superhigh temperature, firing process fast again, and not only quality is good for the product of producing, cost is low, and more meet national energy-saving and reduce discharging policy.
In recent years, people are doing a lot of research work aspect the exploitation of magnesium-aluminium spinel, as application number is 01115504.3, and name is called the patented technology of " synthetic MgAl spinal and preparation method thereof ", adopts alumine and light-burning magnesium powder 1430-1600 ℃ of calcining 100-130 hour.The patent No. be ZL88106918.3's " method of synthetic MgAl spinal ", adopting high grade bauxite raw material and light calcined magnesia is raw material, high temperature burns till.But because above two kinds of methods are all synthetic with natural material, the magnesium aluminate spinel impurity content that is synthesized is higher, affects the high-temperature behavior of material.
Application number is 200510018154.4 " a kind of fireproof magnesia alumina spinel materials and production method thereof ", adopts γ-Al
2O
3With light-burned MgO be raw material, under 1600-1800 ℃ of temperature, burn till because light-burned MgO very easily is hydrolyzed, generate Mg (OH) after the hydrolysis
2, need to slowly heat, just can burn till for a long time, in sintering process, temperature is grasped bad a little, and is slightly fast such as temperature rise, will explosion.Therefore, adopt light-burned MgO to be only applicable to burn till at a slow speed, production capacity is difficult to improve; In addition, the γ-Al in the raw material
2O
3With light-burned MgO interim Mg (OH) that generates in sintering process
2, in material structure, can take certain space, make volumetric expansion, after the crystallization water decomposed fully, the space of expansion was irrecoverable, caused residual clearance between tissue, lowered the compactness of material.The heat resistanceheat resistant that finally can the have influence on finished product indexs such as performance, thermal expansivity of shaking.
Summary of the invention
The present invention is directed to above problem, provide a kind of, thereby the space in the tissue of back is burnt till in minimizing, makes the principal crystalline phase of material even, compactness is good, and then increase substantially the production method of the high-purity magnesium-aluminum spinel of product quality by the change material prescription.
Technical scheme of the present invention is: by weight percentage with γ-Al of 50～95%
2O
3Mix with 50～5% reheating MgO; Through extra-fine grinding, mechanical classification; Again through balling-up, shaping, oven dry; At last, by ultra-high temperature shaft kiln, in 1820～1930 ℃ temperature range, calcine and formed in 8～20 hours.
Described γ-Al
2O
3In Al
2O
3Content is more than or equal to 98%, and the MgO among the reheating MgO is more than or equal to 97%.
Described γ-Al
2O
3When mixing with reheating MgO, input includes triethanolamine, ethylene glycol, sodium polyphosphate, stearic composite grinding aids, the addition of composite grinding aids is 0.02～1% of mixed material weight, stir, again through extra-fine grinding, by mechanical classification, making fineness is 0.1～10 μ m mixed powder.
Be that 0.1～10 μ m mixed powder is inserted in the nodulizer with the fineness that makes, add bond, water, the water addition is 12～25%, and being processed into diameter is the ball base of 15～35mm, and ball base density is 1.5～2.5g/cm
3
The present invention has changed in the prior art with γ-Al
2O
3With light-burned MgO high-pressure molding, " fast " calcining, make relative density and be the technology of 94～96% magnesium aluminate spinel; Adopt reheating MgO to replace light-burned MgO, it is not high to have overcome in the prior art material density, the problem that production capacity is low.The difference of reheating MgO and light-burned MgO maximum is the active big facile hydrolysis of light-burned MgO, the easy explosion of base substrate in sintering procedure, and material density is not high, the problem that process reliability is bad.In order to improve the density of product, the existing technology that contains light-burned MgO need adopt high-pressure molding, makes that difficulty of processing increases, working (machining) efficiency reduces; Even adopted high-pressure molding,, also be difficult to obtain the product of high-compactness owing to the hydrolysis properties of light-burned MgO.Make about 1800 ℃ and heavily burn MgO, the density of therefore heavily burning the MgO raw material is higher, foreign matter content is relatively low, utilizes its synthetic spinel just not to be prone to the problem of base substrate explosion.In order to adapt to the temperature profile of heavily burning MgO, the present invention is set in the processing temperature of synthetic spinel in 1820～1930 ℃ the temperature range, has satisfied the synthetic processing condition, has guaranteed the synthetic effect.The magnesium-aluminium spinel that the present invention makes has the fusing point height, and thermal expansivity is low, good heat conductivity, characteristics such as chemical resistance of concrete is strong.
Embodiment
Embodiment one
Select Al
2O
3Content is more than or equal to γ-Al of 98%
2O
3, MgO content is raw material more than or equal to 97% reheating MgO.The two was mixed in 1: 1 by weight percentage; During mixing, drop into and include trolamine, ethylene glycol, sodium polyphosphate, stearic composite grinding aids, the add-on of composite grinding aids is 0.5% of a mixture weight, stir, through extra-fine grinding, by air classification, making fineness is 0.1～2 μ m mixed powder again.Be that 0.1～2 μ m mixed powder is inserted in the nodulizer with the fineness that makes, add bond, water, the addition of water is 18%, and being processed into diameter is the ball base of 28mm, and ball base density is 2g/cm
3After shaping, the oven dry,, under 1880 ℃ temperature range, calcined 12 hours, make relative density and be 97% spherical high-purity magnesium-aluminum spinel by ultra-high temperature shaft kiln.
Embodiment two
Select Al
2O
3Content is more than or equal to γ-Al of 98%
2O
3, MgO content is raw material more than or equal to 97% reheating MgO.The two was mixed in 19: 1 by weight percentage; During mixing, drop into and include trolamine, ethylene glycol, sodium polyphosphate, stearic composite grinding aids, the add-on of composite grinding aids is 0.02% of a mixture weight, stir, through extra-fine grinding, by air classification, making fineness is 0.2～10 μ m mixed powder again.Be that 0.2～10 μ m mixed powder is inserted in the nodulizer with the fineness that makes, add bond, water, the addition of water is 25%, and being processed into diameter is the ball base of 35mm, and ball base density is 2.5g/cm
3After shaping, the oven dry,, under 1930 ℃ temperature range, calcined 20 hours, make relative density and be 98% spherical high-purity magnesium-aluminum spinel by ultra-high temperature shaft kiln.
Embodiment three
Select Al
2O
3Content is more than or equal to γ-Al of 98%
2O
3, MgO content is raw material more than or equal to 97% reheating MgO.The two was mixed in 2: 1 by weight percentage; During mixing, drop into and include trolamine, ethylene glycol, sodium polyphosphate, stearic composite grinding aids, the add-on of composite grinding aids is 1% of a mixture weight, stir, through extra-fine grinding, by air classification, making fineness is 0.1～5 μ m mixed powder again.Be that 0.1～5 μ m mixed powder is inserted in the nodulizer with the fineness that makes, add bond, water, the addition of water is 12%, and being processed into diameter is the ball base of 15mm, and ball base density is 1.5g/cm
3After shaping, the oven dry,, under 1820 ℃ temperature range, calcined 8 hours, make relative density and be 99% spherical high-purity magnesium-aluminum spinel by ultra-high temperature shaft kiln.
Claims (3)
1. the production method of a high-purity magnesium-aluminum spinel is by weight percentage with γ-Al of 50～95%
2O
3Mix with 50～5% reheating MgO; Through extra-fine grinding, mechanical classification; Again through balling-up, shaping, oven dry; At last, by ultra-high temperature shaft kiln, in 1820～1930 ℃ temperature range, calcine and formed in 8～20 hours; It is characterized in that described γ-Al
2O
3When mixing with reheating MgO, input includes triethanolamine, ethylene glycol, sodium polyphosphate, stearic composite grinding aids, the addition of composite grinding aids is 0.02～1% of mixed material weight, stir, again through extra-fine grinding, by mechanical classification, making fineness is 0.1～10 μ m mixed powder.
2. the production method of a kind of high-purity magnesium-aluminum spinel according to claim 1 is characterized in that, described γ-Al
2O
3In Al
2O
3Content is more than or equal to 98%, and the MgO among the reheating MgO is more than or equal to 97%.
3. the production method of a kind of high-purity magnesium-aluminum spinel according to claim 1, it is characterized in that, be that 0.1～10 μ m mixed powder is inserted in the nodulizer with the fineness that makes, add bond, water, the water addition is 12～25%, being processed into diameter is the ball base of 15～35mm, and ball base density is 1.5～2.5g/cm
3
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|---|---|---|---|
| CN2008101956708A CN101671046B (en) | 2008-09-09 | 2008-09-09 | Method for manufacturing high-purity magnesium-aluminum spinel |
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|---|---|---|---|
| CN2008101956708A CN101671046B (en) | 2008-09-09 | 2008-09-09 | Method for manufacturing high-purity magnesium-aluminum spinel |
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|---|---|
| CN101671046A CN101671046A (en) | 2010-03-17 |
| CN101671046B true CN101671046B (en) | 2011-06-15 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102863247B (en) * | 2012-10-16 | 2015-06-24 | 中国地质大学（北京） | Preparation method of compact magnesia-alumina spinel refractory aggregate |
| CN102936022B (en) * | 2012-10-17 | 2015-03-11 | 河南科技大学 | High purity nano-scale magnesium-aluminum spinel synthesis method |
| WO2015137468A1 (en) | 2014-03-14 | 2015-09-17 | 大日精化工業株式会社 | Thermally conductive complex oxide, production method therefor, thermally conductive complex oxide-containing composition, and use therefor |
| CN108329016A (en) * | 2018-03-09 | 2018-07-27 | 海城市祥程矿业有限公司 | A kind of technique that shaft furnace burns magnesium iron spinel sand |
| CN110655412A (en) * | 2019-11-13 | 2020-01-07 | 山东恒嘉高纯铝业科技股份有限公司 | Preparation method of high-purity sintered spinel |
| TWI769013B (en) * | 2020-07-13 | 2022-06-21 | 美商賀利氏科納米北美有限責任公司 | Ceramic sintered body comprising magnesium aluminate spinel |
| CN112250448A (en) * | 2020-09-15 | 2021-01-22 | 辽宁东和新材料股份有限公司 | Synthetic method for producing light-burned magnesia-alumina spinel by one-step method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0531130A2 (en) * | 1991-09-04 | 1993-03-10 | Dresser Industries Inc. | Improved magnesite-spinel refractory product and method for making same |
| CN1654418A (en) * | 2005-01-17 | 2005-08-17 | 武汉科技大学 | Fireproof magnesia alumina spinel materials and method for preparing same |
-
2008
- 2008-09-09 CN CN2008101956708A patent/CN101671046B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0531130A2 (en) * | 1991-09-04 | 1993-03-10 | Dresser Industries Inc. | Improved magnesite-spinel refractory product and method for making same |
| CN1654418A (en) * | 2005-01-17 | 2005-08-17 | 武汉科技大学 | Fireproof magnesia alumina spinel materials and method for preparing same |
Non-Patent Citations (1)
| Title |
|---|
| 孙丽枫等.添加轻烧氧化镁对镁铝尖晶石轻质耐火材料烧结性能的影响.《材料与冶金学报》.2004,第3卷(第2期),121-122. * |
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| CN101671046A (en) | 2010-03-17 |
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Effective date of registration: 20141223 Address after: Yang Zhuang Industrial Park Zhenwu town of Jiangdu District of Jiangsu Province in 225200 in Yangzhou City Patentee after: JIANGSU JINGXIN NEW MATERIAL CO., LTD. Address before: 225265 Jiangsu Province Jiangdu Zhenwu Zhen Yang Zhuang Industrial Park Yangzhou Jinghui Refractories Co. Ltd. Patentee before: Li Zhengkun |