CN105692661A - Magnesium oxide material and preparing method thereof - Google Patents

Magnesium oxide material and preparing method thereof Download PDF

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Publication number
CN105692661A
CN105692661A CN201610152314.2A CN201610152314A CN105692661A CN 105692661 A CN105692661 A CN 105692661A CN 201610152314 A CN201610152314 A CN 201610152314A CN 105692661 A CN105692661 A CN 105692661A
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China
Prior art keywords
magnesium oxide
oxide material
preparation
mixed
oxalic acid
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CN201610152314.2A
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CN105692661B (en
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魏耀武
张涛
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Wuhan University of Science and Engineering WUSE
Wuhan University of Science and Technology WHUST
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Wuhan University of Science and Engineering WUSE
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F5/00—Compounds of magnesium
    • C01F5/02—Magnesia
    • 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
    • C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

The invention relates to a magnesium oxide material and a preparing method thereof. According to the technical scheme, magnesium oxide fine powder and mixed solution are blended according to the mass ratio of 1:2 and placed in a mixing machine to be mixed for 0.5-8 h, so that mixed pulp is obtained; the mixed pulp is filtered and dried for 24 h at 110 DEG C, so that a mixture block is obtained; heat insulation is conducted on the mixture block for 1-6 h at 1000-1300 DEG C, cooling is conducted, and ball milling is conducted to 1-200 microns, so that the magnesium oxide material is obtained. The mixed solution is prepared from 5-30 wt% of beryllium hydroxide and 70-95 wt% of oxalic acid solution. The prepared magnesium oxide material has the advantages of being high in hydration resistance, stable in high temperature performance, high in high-temperature strength and excellent in erosion resistance, and is a novel raw material for preparing a high-temperature industrial high-grade refractory material.

Description

A kind of magnesium oxide material and preparation method thereof
Technical field
The invention belongs to technical field of refractory materials。Particularly relate to a kind of magnesium oxide material and preparation method thereof。
Background technology
Magnesian is current most widely used refractory material kind, and its essential mineral raw material is magnesia (chemical composition is magnesium oxide)。Magnesia is broadly divided into magnesite clinker, seawater magnesia and fused magnesite three kinds。Magnesite clinker mainly by magnesite, water magnesium ore deposit or from sea water extract magnesium hydroxide form through high-temperature calcination。Being called magnesite clinker with the magnesia of burning to death that magnisite is fired for raw material, be called fused magnesite for raw material through what arc melting reached to be formed after molten condition cooling with magnesite etc., that extracts from sea water that magnesium oxide makes is called seawater magnesia。Along with the development of the progress of technology of hot industry and refractory technology, the grade of magnesia is proposed multiple requirement。Wherein, highly-purity magnesite is to select natural superfine giobertite purification by floatation to form through light-burned, fine grinding, pressure ball, ultra-high temperature shaft kiln calcining, is brickmaking and indefinite refractory material quality raw materials；Medium-grade magnesite is with light calcined magnesia for raw material, forming through explained hereafter such as pressure ball, high temperature vertical kiln calcinings, product sintering degree is good, compact crystallization, it is the quality raw materials producing middle-grade magnesia fireproof goods, it is also possible in manufacturing various magnesia bricks, magnesia-alumina brick, ramming mass, mending material etc.。Magnesia refractories containing magnesia has after burning that line change is less, intensity is high, the ability of alkali resistance scouring is strong and the advantage such as the fused mass of resistance to sodium salt erosiveness is strong, and manufacturing cost is moderate, thus have a wide range of applications in hot industry, both can make approved product and can also make the use of unsetting product, such as magnesia carbon brick, magnesia-alumina-carbon brick, magnesia-calcium brick, magnesia coating and castable etc.。
But, unsetting and carbon-free magnesia refractories has general shortcoming, that is: slag penetration resistance is poor, the problems such as easy peeling, easy aquation and dry run easily crack have had influence on the result of use of magnesia product, which results in when castable has become main unshape refractory kind both at home and abroad at present, and the situation that the proportion that castable is wherein is very low。Its reason mainly has two aspects: 1) the easy aquation of magnesia and castable easily crack in dry run；2) chemical composition of magnesia is MgO, and under high temperature, MgO is easily and other oxide impurity such as CaO, SiO2、Fe2O3And Al2O3Deng occurring chemical reaction to form low-melting compound, namely reduce the refractoriness under load of magnesian, reduce again the anti-slag penetrating power of magnesian。Therefore, magnesia or magnesium oxide material are modified, it has also become improve the important channel of magnesian especially castable performance。
Summary of the invention
It is contemplated that overcome prior art not enough, the preparation method that purpose is to provide a kind of magnesium oxide material, the magnesium oxide material hydration resistance prepared by the method is good, have stable high-temperature performance, elevated temperature strength is big and erosion resisting is excellent, is the novel material of hot industry high grade refractory。
For achieving the above object, the technical solution adopted in the present invention is: is first 1: 2 dispensing by the mass ratio of magnesium oxide powder and mixed solution, is placed in mixer blended 0.5～8 hour, obtains mixed slurry；Again mixed slurry is filtered dry, dries 24 hours under 110 DEG C of conditions, obtain mixture block；Then mixture block is incubated 1～6 hour under 1000～1300 DEG C of conditions, cooling, it is milled to 1～200 μm, obtains alumina material。
Described mixed solution is the mixed solution of beryllium hydroxide and oxalic acid solution, and wherein: beryllium hydroxide is 5～30wt%, oxalic acid solution is 70～95wt%。
Content of MgO >=95wt% in described magnesium oxide powder；Particle diameter is 1～200 μm。
Be (OH) in described beryllium hydroxide2Content >=97wt%；Particle diameter is 1～500 μm。
The molar concentration of described oxalic acid solution is 0.2～1mol/L。
Owing to adopting technique scheme, the present invention compared with prior art has following good effect:
The present invention, in time prepared by high temperature, wraps up the Be (OH) with magnesium oxide particle surface in Blending Processes2Being decomposed to form BeO, namely MgO particle surface will parcel a thin layer BeO。BeO high-temperature stability is better than MgO, even better than ZrO2, high-temperature stability is fabulous。The existence of BeO layer, it is possible to bring effect good as follows:
1) when preparing castable, BeO layer, by magnesium oxide material and water segregation, can protect magnesium oxide particle to avoid aquation, it is to avoid because of the Mg (OH) formed on its surface after magnesium oxide particle aquation2The phenomenon of material cracks is caused in warm；
2) BeO layer is by magnesium oxide material and the isolation of other oxide impurity, it is to avoid produce too much low-melting-point material phase under high temperature, is conducive to improving the refractoriness under load of magnesian。
Magnesium oxide material prepared by the present invention is after testing: content of MgO >=94wt%；Apparent porosity≤4%。
Therefore, the feature that the magnesium oxide material prepared by the present invention has that hydration resistance is good, has stable high-temperature performance, elevated temperature strength is big and resistant to corrosion shape is excellent, is the novel material preparing hot industry high grade refractory。
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention will be further described, not the restriction to its protection domain。
For avoiding repeating, existing by as follows for the technical parameter Unify legislation involved by this detailed description of the invention, embodiment repeats no more:
Content of MgO >=95wt% in described magnesium oxide powder；Particle diameter is 1～200 μm。
Be (OH) in described beryllium hydroxide2Content >=97wt%；Particle diameter is 1～500 μm。
The molar concentration of described oxalic acid solution is 0.2～1mol/L。
Embodiment 1
A kind of magnesium oxide material and preparation method thereof。It is first 1: 2 dispensing by the mass ratio of magnesium oxide powder and mixed solution, is placed in mixer blended 0.5～3 hour, obtains mixed slurry；Again mixed slurry is filtered dry, dries 24 hours under 110 DEG C of conditions, obtain mixture block；Then mixture block is incubated 1～3 hour under 1100～1300 DEG C of conditions, cooling, it is milled to 1～100 μm, obtains alumina material。
Described mixed solution is the mixed solution of beryllium hydroxide and oxalic acid solution, and wherein: beryllium hydroxide is 5～10wt%, oxalic acid solution is 90～95wt%。
Magnesium oxide material prepared by the present embodiment is after testing: content of MgO >=94wt%；Apparent porosity≤4%。
Embodiment 2
A kind of magnesium oxide material and preparation method thereof。It is first 1: 2 dispensing by the mass ratio of magnesium oxide powder and mixed solution, is placed in mixer blended 3～6 hours, obtains mixed slurry；Again mixed slurry is filtered dry, dries 24 hours under 110 DEG C of conditions, obtain mixture block；Then mixture block is incubated 3～5 hours under 1100～1200 DEG C of conditions, cooling, it is milled to 100～150 μm, obtains alumina material。
Described mixed solution is the mixed solution of beryllium hydroxide and oxalic acid solution, and wherein: beryllium hydroxide is 10～20wt%, oxalic acid solution is 80～90wt%。
Magnesium oxide material prepared by the present embodiment is after testing: content of MgO >=95wt%；Apparent porosity≤3%。
Embodiment 3
A kind of magnesium oxide material and preparation method thereof。It is first 1: 2 dispensing by the mass ratio of magnesium oxide powder and mixed solution, is placed in mixer blended 6～8 hours, obtains mixed slurry；Again mixed slurry is filtered dry, dries 24 hours under 110 DEG C of conditions, obtain mixture block；Then mixture block is incubated 5～6 hours under 1200～1300 DEG C of conditions, cooling, it is milled to 1～200 μm, obtains alumina material。
Described mixed solution is the mixed solution of beryllium hydroxide and oxalic acid solution, and wherein: beryllium hydroxide is 20～30wt%, oxalic acid solution is 70～80wt%。
Magnesium oxide material prepared by the present embodiment is after testing: content of MgO >=98wt%；Apparent porosity≤2%。
This detailed description of the invention compared with prior art has following good effect:
Magnesium oxide material prepared by this detailed description of the invention, in Blending Processes, wraps up the Be (OH) with magnesium oxide particle surface2Being decomposed to form BeO, namely MgO particle surface will parcel a thin layer BeO。BeO high-temperature stability is better than MgO, even better than ZrO2, high-temperature stability is fabulous。The existence of BeO layer, it is possible to bring effect good as follows:
1) when preparing castable, BeO layer, by magnesium oxide material and water segregation, can protect magnesium oxide particle to avoid aquation, it is to avoid because of the Mg (OH) formed on its surface after magnesium oxide particle aquation2The phenomenon of material cracks is caused in warm；
2) BeO layer is by magnesium oxide material and the isolation of other oxide impurity, it is to avoid produce too much low-melting-point material phase under high temperature, is conducive to improving the refractoriness under load of magnesian。
Magnesium oxide material prepared by this detailed description of the invention is after testing: content of MgO >=94wt%；Apparent porosity≤4%。
Therefore, the feature that the magnesium oxide material prepared by this detailed description of the invention has that hydration resistance is good, has stable high-temperature performance, elevated temperature strength is big and resistant to corrosion shape is excellent, is the novel material preparing hot industry high grade refractory。

Claims (5)

1. the preparation method of a magnesium oxide material, it is characterised in that: it is first 1: 2 dispensing by the mass ratio of magnesium oxide powder and mixed solution, is placed in mixer blended 0.5～8 hour, obtains mixed slurry；Again mixed slurry is filtered dry, dries 24 hours under 110 DEG C of conditions, obtain mixture block；Then mixture block is incubated 1～6 hour under 1000～1300 DEG C of conditions, cooling, it is milled to 1～200 μm, obtains alumina material；
Described mixed solution is the mixed solution of beryllium hydroxide and oxalic acid solution, and wherein: beryllium hydroxide is 5～30wt%, oxalic acid solution is 70～95wt%。
2. the preparation method of magnesium oxide material according to claim 1, it is characterised in that content of MgO >=95wt% in described magnesium oxide powder；Particle diameter is 1～200 μm。
3. the preparation method of magnesium oxide material according to claim 1, it is characterised in that Be (OH) in described beryllium hydroxide2Content >=97wt%；Particle diameter is 1～500 μm。
4. the preparation method of magnesium oxide material according to claim 1, it is characterised in that the molar concentration of described oxalic acid solution is 0.2～1mol/L。
5. a magnesium oxide material, it is characterised in that described magnesium oxide material is the magnesium oxide material prepared by the preparation method of the magnesium oxide material according to any one of Claims 1 to 4 item。
CN201610152314.2A 2016-03-17 2016-03-17 A kind of magnesium oxide material and preparation method thereof Expired - Fee Related CN105692661B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN115959890A (en) * 2023-01-09 2023-04-14 营口鼎盛实业有限公司 Preparation method of modified magnesia refractory material

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1570162A (en) * 2004-05-13 2005-01-26 上海交通大学 Magnesium and magnesium alloy composite protection fire-proof covering flux and its production method
CN101182189A (en) * 2007-11-15 2008-05-21 电子科技大学 Multi-component doping high-performance beryllium oxide ceramic material and preparation method
CN101774826A (en) * 2010-01-15 2010-07-14 电子科技大学 99BeO ceramic metallizing slurry and preparation method thereof
US20140305346A1 (en) * 2013-04-15 2014-10-16 Indra Neelameggham Alkaline Earth Oxides For Green Processes For metals and other Material

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1570162A (en) * 2004-05-13 2005-01-26 上海交通大学 Magnesium and magnesium alloy composite protection fire-proof covering flux and its production method
CN101182189A (en) * 2007-11-15 2008-05-21 电子科技大学 Multi-component doping high-performance beryllium oxide ceramic material and preparation method
CN101774826A (en) * 2010-01-15 2010-07-14 电子科技大学 99BeO ceramic metallizing slurry and preparation method thereof
US20140305346A1 (en) * 2013-04-15 2014-10-16 Indra Neelameggham Alkaline Earth Oxides For Green Processes For metals and other Material

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
曾小勤等: "阻燃镁合金研究", 《铸造》 *
韩富银等: "阻燃镁合金AZ91D-0.3% Be-Sr的研究", 《铸造》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN115959890A (en) * 2023-01-09 2023-04-14 营口鼎盛实业有限公司 Preparation method of modified magnesia refractory material
CN115959890B (en) * 2023-01-09 2023-08-25 营口鼎盛实业有限公司 Preparation method of modified magnesia refractory material

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