CN102863247A - Preparation method of compact magnesia-alumina spinel refractory aggregate - Google Patents
Preparation method of compact magnesia-alumina spinel refractory aggregate Download PDFInfo
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- CN102863247A CN102863247A CN201210391219XA CN201210391219A CN102863247A CN 102863247 A CN102863247 A CN 102863247A CN 201210391219X A CN201210391219X A CN 201210391219XA CN 201210391219 A CN201210391219 A CN 201210391219A CN 102863247 A CN102863247 A CN 102863247A
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Abstract
The invention relates to a preparation method of compact magnesia-alumina spinel refractory aggregate and belongs to the technical field of refractory materials. According to the preparation method, light burned magnesite powders and aluminum oxide powders are used as raw materials and blended according to a certain proportion, the raw materials are subjected to mixing, ball milling, forming, pre-burning and breaking, saturated lime water or a saturated solution of calcium acetate is sprayed on surfaces of bulk materials, or the bulk materials are immersed into the saturated lime water or the saturated solution of the calcium acetate, and then the bulk materials are taken out for natural drying and then sintered at high temperatures. The compact magnesia-alumina spinel refractory aggregate is large in density, high in compactness, good in thermal shock resistant performances and highly stable in reducing atmosphere and alkaline environment, and the compact magnesia-alumina spinel refractory aggregate has wide application prospects in fields of refractory material products, refractory castables and the like.
Description
Technical field:
The present invention relates to a kind of fine and close fireproof magnesia alumina spinel aggregate processing method, belong to fire resisting material field.
Background technology:
Magnesium-aluminium spinel is a kind of very important refractory materials, and it has many superior performances, such as high-melting-point (2135 ℃), low heat expansion property, high heat resistance and erosion resistance.Therefore, magnesium-aluminium spinel matter refractory product is widely used in the industries such as cement, glass, nonferrous smelting and iron and steel, even a lot of external experts of quilt regard 21 century " mullite " as.That the fireproof magnesia alumina spinel aggregate belongs to is novel, efficient, cleaning, environment-friendly product, is the important refractory raw material that substitutes magnesium chromium goods (strong carcinogenesis is arranged) at wide spectrum.Along with the day different increasing of national environmental protection dynamics, along with progressively eliminating of magnesium chromium goods, the Application Areas of fireproof magnesia alumina spinel aggregate can be more and more wider, and demand can be increasing.
The used for refractory material magnesium-aluminum spinel raw material is usually take commercial alumina powder or bauxite chamotte, caustic-calcined magnesite as raw material, and is synthetic through electric smelting method or sintering process.Synthetic spinel reaction has larger volumetric expansion (approximately 5%), be difficult to densified sintering product, and the hot strength of magnesium-aluminium spinel, thermal shock resistance, corrosion resistance, abrasion resistance is all relevant with its density with the anti-ability of degrading, want to prepare the magnesium aluminate spinel product of excellent property, certainly will will improve its density.
It is representational periodical operation that the electric smelting method is produced spinel, large castable need to prolong cooling time, the cooling of castable causes microstructural inhomogeneous, because cooling is very fast, outside spinel crystal is less than the inside, and low melting point impurity concentrates on the center, need to carry out the sorting homogenizing to electric smelting spinel raw material, therefore, electric smelting method produces that spinel exists that energy consumption is large, complex process and the high shortcoming of equipment requirements.The advantage that sintering process is produced spinel is that this technique is a continuous ceramic process, and by delivery rate and balanced temperature distribution in the control kiln, can producing very uniformly, crystalline size is the product of 30-80 μ m and low porosity (＜3%).At present sintering process is produced spinel and is divided into a step and burns till with two steps and burn till.Document (CHEN YONGQIANG, Chen Jiageng, Li Ruchun. the experimental study of dense magnesia alumina spinel synthesized by sintering [J], refractory materials, 2005,39 (2): 116～118,122.) adopting granularity≤0.058mm, MgO massfraction is 96.28% caustic-calcined magnesite and α-Al of granularity≤0.043mm
2O
3Be raw material, through 100MPa moulding and 1750 ℃ calcining one-step synthesis spinel.But this technique is higher for the requirement of raw material, and sintering temperature is also higher.Document (Huang Gang etc. research and the industrial application of a step sintering process synthetic MgAl spinal, refractory materials, 2007,41 (6): 451～453.) take superfine bauxitic clay raw material, light-magnesite powder etc. as raw material, spent pulping liquor is wedding agent, at 1600 ℃ of calcining 3h, has studied active A l
2O
3Micro mist, magnesium aluminium spinel powder, boric acid (H
3BO
3), MgCl
26H
2O etc. are on the impact of synthetic MgAl spinal volume density.Find that the interpolation of boric acid can improve the volume density of synthetic MgAl spinal, but improve limitedly, volume density is lower than 3.03gcm
-3The two step synthesis spinel be approximately 1400 ℃ the time calcining raw materials form spinel, mechanical pressing after then the spinel that obtains being pulverized is again at densified sintering product more than 1700 ℃.Although two-step approach can be prepared the more satisfactory magnesium-aluminium spinel of density, energy consumption is to limit the key reason of its development greatly always.
A kind of fine and close fireproof magnesia alumina spinel aggregate processing method of the present invention is introduced micro-CaO acceleration of sintering after low temperature presintering, reduced the temperature of two step synthesis magnesium-aluminium spinel, reduce the energy consumption of two step synthesis magnesium-aluminium spinel, synthesized the high magnesium-aluminium spinel aggregate of density.Have cost low, be appropriate to the scale of chemical production, adopt its goods as raw material to have the remarkable advantages such as stable high-temperature strength, corrosion-resistant property and thermal shock resistance be good.
Summary of the invention:
The present invention seeks to for the synthetic magnesium-aluminium spinel density of present single stage method not high, the problems such as two step method synthetic MgAl spinal energy consumption is higher are utilized and introduce micro-CaO acceleration of sintering (CaO and the MgO in the synthetic material and Al that the calcium hydroxide pyrolytic decomposition in calcium acetate and the liming generates after low temperature presinterings
2O
3Form intrusion type and substitutional sosoloid, although solid solution capacity is very little, see Figure of description 2, concentrated at crystal surface and crystal grain boundary place, affected interfacial property, reduce the activation energy of ion diffusion, thereby promoted the sintering of spinel; Adopt after the low temperature presintering infiltration to introduce micro-CaO more even with respect to directly introducing micro-CaO in the initial feed batching calcium ion being distributed, crucially simultaneously a bit is, directly introduce micro-CaO in the initial feed batching, CaO can be preferentially and Al
2O
3Reaction generates calcium aluminate, and the calcium aluminate major part all can be hydrolyzed, and affects result of use and the life-span of refractory aggregate, and after the pre-burning, and MgO and Al
2O
3Reaction generates magnesium-aluminium spinel, main and MgO and Al after CaO introduces
2O
3Form intrusion type and substitutional sosoloid, play the effect of acceleration of sintering, reduced the generation of calcium aluminate), reduced the temperature of two step synthesis magnesium-aluminium spinel, reduced the energy consumption of two step synthesis magnesium-aluminium spinel, synthesize the high magnesium-aluminium spinel aggregate of density, propose a kind of fine and close fireproof magnesia alumina spinel aggregate processing method.
For achieving the above object, technical scheme of the present invention is as follows:
A kind of fine and close fireproof magnesia alumina spinel aggregate processing method that the present invention proposes, it is characterized in that take light-calcined magnesite powder and alumina powder as raw material, prepare burden by a certain percentage, take corundum ball or agate ball as ball-milling medium, with ball mill mixing machine mixing and ball milling 5～15 hours, after dry-pressing formed, tie (so that base substrate can obtain certain intensity at low temperature presintering, in ensuing infiltration process, be unlikely to destroy, also be beneficial to simultaneously and be crushed to required particle diameter, reduce energy consumption; Can keep certain porosity again, be convenient to the introducing of micro-CaO), be crushed to required particle diameter, at the saturated solution of block material surface sprinkling saturated limewater or calcium acetate or block material is immersed in the saturated solution of saturated limewater or calcium acetate (time of the amount of saturated solution that can be by spraying saturated limewater or calcium acetate and the saturated solution of infiltration saturated limewater or calcium acetate is controlled the amount of introducing micro-CaO), take out and burn till after nature dries.
MgO content is greater than 98% in the light-calcined magnesite of the present invention, and add-on is 10～28.33wt.%, Al in the alumina powder
2O
3Content is greater than 99%, and add-on is 71.67～90wt.%; Alumina powder is alpha-alumina powder or gama-alumina powder; Forming method is that hydropress is dry-pressing formed, and typed pressure is 70～150MPa; Calcined temperature is 800～1400 ℃, is incubated 0.5-5 hour; The time of the saturated solution of block material surface sprinkling saturated limewater or calcium acetate is 2～6 hours; The time of naturally drying is 12～48 hours; Final firing temperature is 1500～1650 ℃, is incubated 0.5-8 hour.
The present invention have cost low, be appropriate to the scale of chemical production, adopt its goods as raw material to have the remarkable advantages such as stable high-temperature strength, corrosion-resistant property and thermal shock resistance be good.
Description of drawings:
Fig. 1 is the XRD figure spectrum of the fine and close fireproof magnesia alumina spinel aggregate of preparation among the embodiment 1;
Fig. 2 is SEM photo and the EDS data thereof of the fine and close fireproof magnesia alumina spinel aggregate of preparation among the embodiment 1.
Embodiment:
Below in conjunction with embodiment technical scheme of the present invention is described further:
Embodiment 1
Take light-calcined magnesite and alpha-alumina powder as raw material, (the light-calcined magnesite add-on is 28.33wt.% to batching by a certain percentage, the alpha-alumina powder add-on is 71.67wt.%), mixing and ball milling, dry-pressing formed through hydropress is the base substrate of 200mm * 80mm * 110mm, forming pressure is 100MPa, then 1200 ℃ of pre-burnings are 2 hours, after taking-up is crushed to particle diameter and is approximately 15mm with jaw crusher, block material is immersed in the saturated solution of calcium acetate, the time of infiltration is 1h, and the taking-up nature dries after 24 hours and burns till in 1650 ℃.
The fine and close fireproof magnesia alumina spinel aggregate density for preparing is 3.6gcm
-3, apparent porosity is 1.0%.
Embodiment 2
Take light-calcined magnesite and gama-alumina powder as raw material, (the light-calcined magnesite add-on is 27wt.% to batching by a certain percentage, gama-alumina powder add-on is 73wt.%), mixing and ball milling, dry-pressing formed through hydropress is the base substrate of 200mm * 80mm * 110mm, forming pressure is 80MPa, then 1200 ℃ of pre-burnings are 2 hours, after taking-up is crushed to particle diameter and is approximately 15mm with jaw crusher, block material is immersed in the saturated limewater solution, the time of infiltration is 2h, and the taking-up nature dries after 24 hours and burns till in 1600 ℃.
The fine and close fireproof magnesia alumina spinel aggregate density for preparing is 3.5gcm
-3, apparent porosity is 1.2%.
Embodiment 3
Take light-calcined magnesite and alpha-alumina powder as raw material, (the light-calcined magnesite add-on is 28.33wt.% to batching by a certain percentage, the alpha-alumina powder add-on is 71.67wt.%), mixing and ball milling, dry-pressing formed through hydropress is the base substrate of 200mm * 80mm * 110mm, forming pressure is 100MPa, then 1000 ℃ of pre-burnings are 2 hours, after taking-up is crushed to particle diameter and is approximately 10mm with jaw crusher, block material is immersed in the saturated solution of calcium acetate, the time of infiltration is 2h, and the taking-up nature dries after 24 hours and burns till in 1600 ℃.
The fine and close fireproof magnesia alumina spinel aggregate density for preparing is 3.55gcm
-3, apparent porosity is 1.5%.
Embodiment 4
Take light-calcined magnesite and gama-alumina powder as raw material, (the light-calcined magnesite add-on is 15wt.% to batching by a certain percentage, gama-alumina powder add-on is 85wt.%), mixing and ball milling, dry-pressing formed through hydropress is the base substrate of 200mm * 80mm * 110mm, forming pressure is 70MPa, then 1100 ℃ of pre-burnings are 2 hours, after taking-up is crushed to particle diameter and is approximately 15mm with jaw crusher, the saturated solution of block material surface sprinkling calcium acetate, the taking-up nature dries after 16 hours and burns till in 1550 ℃.
The fine and close fireproof magnesia alumina spinel aggregate density for preparing is 3.4gcm
-3, apparent porosity is 1.7%.
Claims (7)
1. fine and close fireproof magnesia alumina spinel aggregate processing method, it is characterized in that: take light-calcined magnesite powder and alumina powder as raw material, prepare burden by a certain percentage, mixing and ball milling, through moulding, pre-burning is after the fragmentation, at the saturated solution of block material surface sprinkling saturated limewater or calcium acetate or block material is immersed in the saturated solution of saturated limewater or calcium acetate, take out nature and dry rear high temperature and burn till.
2. fine and close fireproof magnesia alumina spinel aggregate processing method according to claim 1, it is characterized in that: described light-calcined magnesite powder requires particle diameter less than 74 μ m, and wherein MgO content is greater than 98%, and add-on is 10～28.33wt.%, alumina powder requires particle diameter less than 74 μ m, wherein Al
2O
3Content is greater than 99%, and add-on is 71.67～90wt.%; Alumina powder is alpha-alumina powder or gama-alumina powder.
3. fine and close fireproof magnesia alumina spinel aggregate processing method according to claim 1, it is characterized in that: described forming method is that hydropress is dry-pressing formed, typed pressure is 70～150MPa.
4. fine and close fireproof magnesia alumina spinel aggregate processing method according to claim 1, it is characterized in that: described calcined temperature is 800～1400 ℃, soaking time is 0.5-5 hour.
5. fine and close fireproof magnesia alumina spinel aggregate processing method according to claim 1, it is characterized in that: the time of the saturated solution of described block material surface sprinkling saturated limewater or calcium acetate is 2～6 hours.
6. fine and close fireproof magnesia alumina spinel aggregate processing method according to claim 1, it is characterized in that: the described time of naturally drying is 12～48 hours.
7. fine and close fireproof magnesia alumina spinel aggregate processing method according to claim 1, it is characterized in that: described firing temperature is 1500～1650 ℃, is incubated 0.5-8 hour.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104230222A (en) * | 2014-08-08 | 2014-12-24 | 宿州市汇利新型建材有限责任公司 | Impermeable concrete and preparation method thereof |
| CN106187108A (en) * | 2016-07-22 | 2016-12-07 | 武汉科技大学 | A kind of high temperature kiln magnesia refractories and preparation method thereof |
Citations (2)
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|---|---|---|---|---|
| CN101671046A (en) * | 2008-09-09 | 2010-03-17 | 李正坤 | Production method of high-purity magnesium aluminate spinel |
| CN101712554A (en) * | 2009-10-28 | 2010-05-26 | 郑州真金耐火材料有限责任公司 | Production method of magnesium-aluminum spinel bricks |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101671046A (en) * | 2008-09-09 | 2010-03-17 | 李正坤 | Production method of high-purity magnesium aluminate spinel |
| CN101712554A (en) * | 2009-10-28 | 2010-05-26 | 郑州真金耐火材料有限责任公司 | Production method of magnesium-aluminum spinel bricks |
Non-Patent Citations (1)
| Title |
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| 易帅等: "六铝酸钙/镁铝尖晶石复相梯度材料的制备", 《第十七届全国高技术陶瓷学术年会摘要集》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104230222A (en) * | 2014-08-08 | 2014-12-24 | 宿州市汇利新型建材有限责任公司 | Impermeable concrete and preparation method thereof |
| CN104230222B (en) * | 2014-08-08 | 2016-07-06 | 宿州市汇利新型建材有限责任公司 | A kind of water-tight concrete and preparation method thereof |
| CN106187108A (en) * | 2016-07-22 | 2016-12-07 | 武汉科技大学 | A kind of high temperature kiln magnesia refractories and preparation method thereof |
| CN106187108B (en) * | 2016-07-22 | 2018-11-13 | 武汉科技大学 | A kind of high temperature kiln magnesia refractories and preparation method thereof |
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