CN104591565B - A kind of aluminate cement containing nano magnalium spinelle and preparation method thereof - Google Patents
A kind of aluminate cement containing nano magnalium spinelle and preparation method thereof Download PDFInfo
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- CN104591565B CN104591565B CN201510010803.XA CN201510010803A CN104591565B CN 104591565 B CN104591565 B CN 104591565B CN 201510010803 A CN201510010803 A CN 201510010803A CN 104591565 B CN104591565 B CN 104591565B
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Abstract
The present invention relates to a kind of aluminate cement containing nano magnalium spinelle and preparation method thereof.Its technical scheme is: first by the commercial alumina ball milling 0.5 ~ 3h of the natural dolomite of 15 ~ 85wt% and 15 ~ 85wt%, machine is pressed into block；Again described block is inserted in high temperature sintering furnace, be warming up to 1000 ~ 1600 DEG C with the heating rate of 1 ~ 25 DEG C/min, be incubated 0.1 ~ 5h, furnace cooling, swing crushing, prepare the aluminate cement containing nano magnalium spinelle.The particle diameter of described natural dolomite is 5 ~ 50 μm, and CaO content is 20 ~ 40wt%, and content of MgO is 20 ~ 40wt%.The particle diameter of described commercial alumina is 5 ~ 44 μm；The purity of described commercial alumina is more than 95.0wt%.The present invention has that technique is simple, cost is low, size tunable and be applicable to the feature of industrialized production；The prepared particle diameter containing the aluminate cement of nano magnalium spinelle is only 50 ~ 500nm.
Description
Technical field
The invention belongs to aluminate cement technical field.It is specifically related to a kind of aluminate cement containing nano magnalium spinelle and preparation method thereof.
Background technology
Aluminate cement is a kind of hydraulic cement with calcium aluminate for essential mineral phase, and its main chemical compositions is CaO and Al2O3.Owing to aluminate cement firm time is short, early strength is high, and condenses very fast under low temperature, is referred to as " concrete on the one ", is widely used in the promptly construction such as military engineering, bridge, road, airfield runway and salvaging；Simultaneously because aluminate cement has the ability that excellent high temperature resistant, anti-weak bronsted lowry acids and bases bronsted lowry corrodes, aluminate cement obtains a wide range of applications in the field such as castable refractory, refractory concrete.
CaO in conventional aluminum acid salt cement can with the SiO in slag2、FeO/Fe2O3React with MnO etc. and form low melt-phase, cause the slag resistance of refractory material and the reduction of applied at elevated temperature performance.Result of study shows, in preparing aluminate cement process, when being substituted with a certain amount of MgO by CaO, can generate a certain amount of magnesium aluminate spinel in aluminate cement, to improve use temperature and the service life of aluminate cement.
It is uniformly distributed in aluminate cement owing to magnesium aluminate spinel can be realized at the process situ synthetic MgAl spinal preparing aluminate cement, its preparation cost is relatively low simultaneously, therefore, receive publicity preparing aluminate cement process this method of situ synthetic MgAl spinal.Such as ［ M.A.Khalil such as Khalil, A.S.El-Hemaly, L.G.Girgis.Aluminouscementscontainingmagnesiumaluminates pinelfromEgyptiandolomite.CeramicsInternational, 2001,27:865-873 ］ adopt India's dolomite and the activated alumina fabricated in situ aluminate cement containing magnesium aluminate spinel, and find that the castable adopting the aluminic acid cement containing magnesium aluminate spinel has higher intensity and refractoriness；［ the Duan Feng such as Xiao Guoqing, Xiao Guoqing, Jing Guihua, Mr. Zhang wins, high cloud qin. the preparation and application of the aluminate cement containing magnesium aluminate spinel. refractory material, 2007,4:41-44 ］ having synthesized the aluminate cement containing magnesium aluminate spinel with dolomite and commercial alumina, wherein the particle diameter of magnesium aluminate spinel is more than 10 μm.Along with the low cementization of aluminate cement combined corundum castable develops, in order to reduce aluminate cement consumption be maintained with castable high-temperature behavior and slag resistance, should by the Task-size Controlling of magnesium aluminate spinel at nanoscale, so its volume content will be effectively improved, and can obtain better combination property.nullThe main method preparing nano magnalium spinelle at present is to adopt magnesium salt and aluminium salt to carry out chemolysis，Such as [J.Li such as Li,L.Tong,W.Zhou.PhaseComposition,MicrostructureandMechanicalPropertiesofAluminousCementsContainingMagnesiumAluminateSpinel.KeyEngineeringMaterials.2011,492:467-471] and ［ P.Orosco such as Orosco,L.Barbosa,M.Ruiz,Synthesisofmagnesiumaluminatespinelbypericlaseandaluminachlorination.MaterialsResearchBulletin.2014,59:337-340 ］ to adopt magnesium salt and two kinds of slaines of aluminium salt be precursor，The particle diameter magnesium aluminate spinel at 20 ~ 100nm is obtained by chemolysis." preparation method of a kind of magnesia-alumina spinel " (CN103204528A) patented technology, after adopting the compound containing aluminum and the compound containing magnesium to mix in acid solution, by filtering, washing, dry, roasting etc. obtain magnesia-alumina spinel, this operational process of craft is complicated, it is difficult to realize the commercial Application of magnesium aluminate spinel；" preparation method of a kind of aluminate cement containing magnesium aluminate spinel " (CN101891408A) patented technology, adopting light dolomite and aluminium oxide is raw material, at 1550 ~ 1600 DEG C of temperature, it is incubated 4 ~ 6h is prepared for the aluminous cement containing magnesium aluminate spinel, but operational process of craft is loaded down with trivial details, magnesium aluminate spinel particle diameter in the cement generated is at micron order, and can not control effectively；" a kind of aluminate cement containing magnesium aluminate spinel and preparation method thereof " (ZL201310059691.8) patented technology, with commercial alumina, ground calcium carbonate and caustic-calcined magnesite for raw material, it is incubated 120 ~ 240min when 1200 ~ 1550 DEG C and is prepared for the aluminate cement containing magnesium aluminate spinel, the magnesium aluminate spinel particle diameter that this technique obtains is at 0.2 ~ 5 μm, and crystallite dimension is bigger.
Summary of the invention
It is contemplated that overcome the deficiencies in the prior art, it is therefore an objective to provide a kind of method that technique simply prepares the aluminate cement containing nano magnalium spinelle, controlled and be suitable for industrialized production with the nano magnalium spinel particle size prepared by the method.
For achieving the above object, the present invention adopts following technical scheme: first by the commercial alumina ball milling 0.5 ~ 3h of the natural dolomite of 15 ~ 85wt% and 15 ~ 85wt%, machine is pressed into block；Again described block is inserted in high temperature sintering furnace, be warming up to 1000 ~ 1600 DEG C with the heating rate of 1 ~ 25 DEG C/min, be incubated 0.1 ~ 5h, furnace cooling, swing crushing, prepare the aluminate cement containing nano magnalium spinelle.
The particle diameter of described natural dolomite is 5 ~ 50 μm；CaO content in described natural dolomite is 20 ~ 40wt%, and content of MgO is 20 ~ 40wt%.
The particle diameter of described commercial alumina is 5 ~ 44 μm；The purity of described commercial alumina is more than 95.0wt%.
Owing to adopting technique scheme, the present invention compared with prior art has the positive effect that:
The present invention utilizes high temperature solid state reaction mechanism, in air atmosphere, carries out dispensing according to the weight/mass percentage composition of given natural dolomite and commercial alumina, through ball milling, sintering and crushing process, can obtain the aluminate cement containing nano magnalium spinelle.This preparation technology is simple, sintering temperature is low, it is thus achieved that magnesium aluminate spinel size tunable.Owing to natural dolomite resources enriches, less costly, adopt the less costly of this preparation method preparation aluminate cement containing nano magnalium spinelle, be suitable for industrialized production.
In aluminate cement prepared by the present invention, magnesium aluminate spinel is nanoscale, be conducive to erosion-resisting characteristics and the thermal shock resistance of use temperature and the refractory material improving in aluminate cement combining corundum based refractory materials further, extend the service life of corundum based refractory materials.
The present invention adopts natural dolomite and commercial alumina to be raw material, by controlling synthesis technique system, namely being warming up to 1000 ~ 1600 DEG C with the heating rate of 1 ~ 25 DEG C/min, be incubated 0.1 ~ 5h, prepared particle diameter is the aluminate cement containing nano magnalium spinelle of 50 ~ 500nm.
The particle diameter of magnesium aluminate spinel prepared by the present invention is less compared with the particle diameter of magnesium aluminate spinel prepared by prior art, it is only 50 ~ 500nm, and adopt the easy raw material realized of industry and synthesis mode, therefore have the advantages that technique is simple, cost is low and is applicable to industrialized production.
Accompanying drawing explanation
Fig. 1 is the material phase analysis figure of a kind of aluminate cement containing nano magnalium spinelle prepared by the present invention；
Fig. 2 is the microstructure picture of the aluminate cement shown in Fig. 1 containing nano magnalium spinelle；
Fig. 3 is the another kind prepared of the present invention microstructure picture containing the aluminate cement of nano magnalium spinelle.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the invention will be further described, not the restriction to its protection domain:
For avoiding repeating, first by as follows for the technical parameter Unify legislation involved by this detailed description of the invention, following embodiment repeats no more:
The particle diameter of described natural dolomite is 5 ~ 50 μm；CaO content in described natural dolomite is 20 ~ 40wt%, and content of MgO is 20 ~ 40wt%.
The particle diameter of described commercial alumina is 5 ~ 44 μm；The purity of described commercial alumina is more than 95.0wt%.
Embodiment 1
A kind of aluminate cement containing nano magnalium spinelle and preparation method thereof.Described in the present embodiment, preparation method is: first by the commercial alumina ball milling 0.5 ~ 3h of the natural dolomite of 15 ~ 30wt% and 70 ~ 85wt%, machine is pressed into block；Again described block is inserted in high temperature sintering furnace, be warming up to 1000 ~ 1200 DEG C with the heating rate of 1 ~ 5 DEG C/min, be incubated 3 ~ 5h, furnace cooling, swing crushing, prepare the aluminate cement containing nano magnalium spinelle.
The principal phase of the aluminate cement containing nano magnalium spinelle prepared by the present embodiment is magnesium aluminate spinel and a calcium aluminate magnesium aluminate spinel, and particle diameter is 50nm ~ 100nm.
Embodiment 2
A kind of aluminate cement containing nano magnalium spinelle and preparation method thereof.Described in the present embodiment, preparation method is: first by the commercial alumina ball milling 0.5 ~ 3h of the natural dolomite of 25 ~ 40wt% and 60 ~ 75wt%, machine is pressed into block；Again described block is inserted in high temperature sintering furnace, be warming up to 1100 ~ 1300 DEG C with the heating rate of 5 ~ 10 DEG C/min, be incubated 2 ~ 3h, furnace cooling, swing crushing, prepare the aluminate cement containing nano magnalium spinelle.
The principal phase of the aluminate cement containing nano magnalium spinelle prepared by the present embodiment is the particle diameter of magnesium aluminate spinel and a calcium aluminate magnesium aluminate spinel is 80nm ~ 150nm.
Embodiment 3
A kind of aluminate cement containing nano magnalium spinelle and preparation method thereof.Described in the present embodiment, preparation method is: first by the commercial alumina ball milling 0.5 ~ 3h of the natural dolomite of 40 ~ 55wt% and 45 ~ 60wt%, machine is pressed into block；Again described block is inserted in high temperature sintering furnace, be warming up to 1200 ~ 1400 DEG C with the heating rate of 10 ~ 15 DEG C/min, be incubated 1 ~ 2h, furnace cooling, swing crushing, prepare the aluminate cement containing nano magnalium spinelle.
The principal phase of the aluminate cement containing nano magnalium spinelle prepared by the present embodiment is the particle diameter of magnesium aluminate spinel and a calcium aluminate magnesium aluminate spinel is 100nm ~ 300nm.
Embodiment 4
A kind of aluminate cement containing nano magnalium spinelle and preparation method thereof.Described in the present embodiment, preparation method is: first by the commercial alumina ball milling 0.5 ~ 3h of the natural dolomite of 55 ~ 70wt% and 30 ~ 45wt%, machine is pressed into block；Again described block is inserted in high temperature sintering furnace, be warming up to 1300 ~ 1500 DEG C with the heating rate of 15 ~ 20 DEG C/min, be incubated 0.1 ~ 5h, furnace cooling, swing crushing, prepare the aluminate cement containing nano magnalium spinelle.
The principal phase of the aluminate cement containing nano magnalium spinelle prepared by the present embodiment is the particle diameter of magnesium aluminate spinel and a calcium aluminate magnesium aluminate spinel is 200nm ~ 400nm.
Embodiment 5
A kind of aluminate cement containing nano magnalium spinelle and preparation method thereof.Described in the present embodiment, preparation method is: first by the commercial alumina ball milling 0.5 ~ 3h of the natural dolomite of 70 ~ 85wt% and 15 ~ 30wt%, machine is pressed into block；Again described block is inserted in high temperature sintering furnace, be warming up to 1400 ~ 1600 DEG C with the heating rate of 20 ~ 25 DEG C/min, be incubated 0.1 ~ 0.5h, furnace cooling, swing crushing, prepare the aluminate cement containing nano magnalium spinelle.
The principal phase of the aluminate cement containing nano magnalium spinelle prepared by the present embodiment is the particle diameter of magnesium aluminate spinel and a calcium aluminate magnesium aluminate spinel is 350nm ~ 500nm.
The present invention compared with prior art has the positive effect that:
The present invention utilizes high temperature solid state reaction mechanism, in air atmosphere, carries out dispensing according to the weight/mass percentage composition of given natural dolomite and commercial alumina, through ball milling, sintering and crushing process, can obtain the aluminate cement containing nano magnalium spinelle.This preparation technology is simple, sintering temperature is low, it is thus achieved that magnesium aluminate spinel size tunable.Owing to natural dolomite resources enriches, less costly, adopt the less costly of this preparation method preparation aluminate cement containing nano magnalium spinelle, it is adaptable to industrialized production.
In aluminate cement prepared by the present invention, magnesium aluminate spinel is nanoscale, be conducive to erosion-resisting characteristics and the thermal shock resistance of use temperature and the refractory material improving in aluminate cement combining corundum based refractory materials further, extend the service life of corundum based refractory materials.
The present invention adopts natural dolomite and commercial alumina to be raw material, by controlling synthesis technique system, namely being warming up to 1000 ~ 1600 DEG C with the heating rate of 1 ~ 25 DEG C/min, be incubated 0.1 ~ 5h, prepared particle diameter is the aluminate cement containing nano magnalium spinelle of 50 ~ 500nm.Its thing phasor and micro-structure diagram be as shown in drawings: Fig. 1 is the material phase analysis figure of a kind of aluminate cement containing nano magnalium spinelle prepared by the present invention；Fig. 2 is the microstructure picture of the aluminate cement containing nano magnalium spinelle shown in Fig. 1；Fig. 3 is the microstructure picture that the present invention prepares the another kind of aluminate cement containing nano magnalium spinelle.From Fig. 1 ~ Fig. 3 it can be seen that with magnesium aluminate spinel and calcium aluminate for principal phase the aluminate cement containing nano magnalium spinelle of preparation, the particle diameter of magnesium aluminate spinel is at 50 ~ 500nm.
The particle diameter of magnesium aluminate spinel prepared by the present invention is less compared with the particle diameter of magnesium aluminate spinel prepared by prior art, it is only 50 ~ 500nm, and adopt the easy raw material realized of industry and synthesis mode, therefore have the advantages that technique is simple, cost is low and is applicable to industrialized production.
Claims (3)
1. the preparation method containing the aluminate cement of nano magnalium spinelle, it is characterised in that described preparation method is: first by the commercial alumina ball milling 0.5～3h of the natural dolomite of 15～30wt% and 70～85wt%, machine is pressed into block；Again described block is inserted in high temperature sintering furnace, be warming up to 1000～1200 DEG C with the heating rate of 1～5 DEG C/min, be incubated 3～5h, furnace cooling, swing crushing, prepare the aluminate cement containing nano magnalium spinelle；
The particle diameter of described natural dolomite is 5～50 μm；CaO content in described natural dolomite is 20～40wt%, and content of MgO is 20～40wt%；
The particle diameter of described commercial alumina is 5～44 μm；The purity of described commercial alumina is more than 95.0wt%.
2. the preparation method containing the aluminate cement of nano magnalium spinelle, it is characterised in that described preparation method is: first by the commercial alumina ball milling 0.5～3h of the natural dolomite of 25～40wt% and 60～75wt%, machine is pressed into block；Again described block is inserted in high temperature sintering furnace, be warming up to 1100～1300 DEG C with the heating rate of 5～10 DEG C/min, be incubated 2～3h, furnace cooling, swing crushing, prepare the aluminate cement containing nano magnalium spinelle；
The particle diameter of described natural dolomite is 5～50 μm；CaO content in described natural dolomite is 20～40wt%, and content of MgO is 20～40wt%；
The particle diameter of described commercial alumina is 5～44 μm；The purity of described commercial alumina is more than 95.0wt%.
3. the aluminate cement containing nano magnalium spinelle, it is characterised in that the described aluminate cement containing nano magnalium spinelle is the aluminate cement containing nano magnalium spinelle prepared by the preparation method of the aluminate cement according to any one of claim 1～2 containing nano magnalium spinelle.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101475327A (en) * | 2009-02-19 | 2009-07-08 | 武汉科技大学 | Aluminate cement and preparation thereof |
| RU2383505C1 (en) * | 2008-07-21 | 2010-03-10 | ООО "Ключевская обогатительная фабрика" | Heat-resistant binder |
| CN101891408A (en) * | 2010-08-06 | 2010-11-24 | 西安建筑科技大学 | Method for preparing magnesia-alumina spinel-containing aluminate cement |
| CN103073206A (en) * | 2013-02-26 | 2013-05-01 | 武汉科技大学 | Aluminate cement containing magnesium-aluminate spinel and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2383505C1 (en) * | 2008-07-21 | 2010-03-10 | ООО "Ключевская обогатительная фабрика" | Heat-resistant binder |
| CN101475327A (en) * | 2009-02-19 | 2009-07-08 | 武汉科技大学 | Aluminate cement and preparation thereof |
| CN101891408A (en) * | 2010-08-06 | 2010-11-24 | 西安建筑科技大学 | Method for preparing magnesia-alumina spinel-containing aluminate cement |
| CN103073206A (en) * | 2013-02-26 | 2013-05-01 | 武汉科技大学 | Aluminate cement containing magnesium-aluminate spinel and preparation method thereof |
Non-Patent Citations (2)
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| 含镁铝尖晶石的铝酸盐水泥的制备与应用;段锋，肖国庆，荆桂花，张君博，高云琴;《耐火材料》;20070228(第4期);全文 * |
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