CN100335435C - Process for producing high quality high purity magnesite by two-step calcining natural cryptocrystalline magnesite - Google Patents

Process for producing high quality high purity magnesite by two-step calcining natural cryptocrystalline magnesite Download PDF

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CN100335435C
CN100335435C CNB2006100460570A CN200610046057A CN100335435C CN 100335435 C CN100335435 C CN 100335435C CN B2006100460570 A CNB2006100460570 A CN B2006100460570A CN 200610046057 A CN200610046057 A CN 200610046057A CN 100335435 C CN100335435 C CN 100335435C
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magnesite
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roasting
calcining
cryptocrystal
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CN1821137A (en
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杨庆广
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Abstract

The present invention relates to a technique for producing magnesite sand with high quality and high purity using through the two-step calcination of natural cryptocrystal magnesite. Cryptocrystal magnesite is washed by water, dried, crushed to the particle size of 0 to 5mm and roasted in a fluidized bed furnace; then, materials enter a grading and fine grinding working procedure, materials less than 10 mu m in materials of 325 meshes are separated, materials more than 10 mu m in the materials of 325 meshes are added into a fine grinding system and ground into the materials less than 10 mum, and the throughput rate is 97%; the materials and the separated materials are uniformly mixed, an anion activating agent after is added, and then, the mixture is added into a dry process ball pressing system; in the dry process ball pressing system, the materials are crushed into 0 to 3mm after being made into blanks, mixed with new powder which is not made into blanks according to the volume ratio of 6 to 4, made into balls by the dry process, maintained for 48 hours, put into a high temperature oil vertical kiln and calcined at the temperature of 1950 DEG C to 2050 DEG C and discharged from the kiln of the calcining and holding time of 18 to 20 hours. The MgO content of the product is from 98 to 99%, and the volume density is from 3.40 to 3.45 g/cm<3>. Compared with the sea water magnesia, the product has the advantages of low production cost and high fireproof strength.

Description

Natural cryptocrystal type magnesite by two-step calcining is produced the technology of highly-purity magnesite
Technical field
The present invention relates to the production technical field of ferrous metallurgy, the technology of natural cryptocrystal type magnesite by two-step calcining production high-quality highly-purity magnesite with refractory materials.
Background technology
Along with the smelting iron and steel continuous advancement in technology, refractory materials is had higher requirement.China is refractory materials big producing country, all occupy first place in the world from the resource to the product, but more still there is suitable gap in the class and the international most advanced level of all kinds of refractory products, and the refractory products of China is substantially also low and middle-grade.Haicheng and area, Dashiqiao are the production bases of magnesium resource and magnesia industry, but traditional production technique is produced low and middle-grade times product, its MgO purity, and volume density does not still reach the ideal index, has caused the huge waste of magnesium resource.With common highly-purity magnesite is example, compares with seawater magnesia, and its price only is 1/5th of a seawater magnesia.Enter seawater magnesia market through the high-quality highly-purity magnesite of researching and developing out for many years, its MgO content is 97.7%, volume density 3.35-3.40g/cm 3, its price also is 2/3rds of a seawater magnesia price.So with existing magnesite resource, producing that high purity, highdensity high-quality highly-purity magnesite and seawater magnesia contend with is industry technician urgent problem.
The applicant has applied for patent of invention " a kind of magnesia and production method thereof " in 1999, the patent No. is 99113210.6, this patent disclosure be the method for producing magnesia with magnisite, this method is that the magnesite with weight percent MgO>47.5% places fluidizing furnace (or shower furnace), roasting under 950 ℃ of (870 ℃) conditions, get the activated magnesia powder, wear into ultrafine powder then, add anion active agent magnesium chloride and mineralizer boron trioxide again, mix mill altogether, obtain the preceding activated magnesia powder of base, with the balling-up of high pressure ball press, place calcining in the high temperature oil shaft furnace then, obtain MgO 〉=98%, SiO 2≤ 0.5%, CaO≤1.0%, igloss<0.12%, volume density>3.40g/cm 3Magnesia.The magnesia of producing with this method still can not reach the technical requirements of seawater magnesia.And existing raw material all is to use natural phanerocrystalline texture type magnesite, uses natural cryptocrystal type magnesite as also not having in the raw material production highly-purity magnesite prior art.
Summary of the invention
The inventor is at the demand of existing market of fire resisting material, according to for many years to the research and development and the practice of high-quality highly-purity magnesite, working out a kind of is raw material with natural cryptocrystal type magnesite, and producing MgO content through the calcining of two steps is 98%-99% volume density 3.40-3.45g/cm 3The technology of high-quality highly-purity magnesite, because the natural cryptocrystal type of the raw material magnesite purity height of this process choice, not siliceous, iron, aluminium, and when heavily burning, added activator, the highly-purity magnesite that this explained hereafter goes out can meet or exceed the technical requirement of seawater magnesia.
Natural cryptocrystal type magnesite by two-step calcining is produced the technology of highly-purity magnesite, it is characterized in that this technology comprises the steps:
1) with the cryptocrystal type magnesite of exploitation, wash with water, remove impurity, dry then, make moisture less than 8%;
2) adopt Hubei Province to break the granularity that is crushed to 0-5mm with pair roller, roasting in fluidizing furnace, temperature is 870 ℃;
Or adopt ball milling to be milled to 200 purpose granularities and go into the shower furnace roasting, temperature is 820 ℃; The granularity of material outlet is 325 orders, and percent of pass is at 92%-93%, and the activity of material is 35 seconds after the roasting in fluidizing furnace, and the activity of material is 25 seconds after the roasting in shower furnace;
3) material enters classification fine grinding operation, with in the 325 order materials<material of 10 μ m tells, with in the material>material of 10 μ m enters the fine grinding system and is milled to<10 μ m, percent of pass 97%, behind the described material uniform mixing of telling, specific surface area reaches 8-10m 2/ g adds anion active agent magnesium fluoride or Calcium Fluoride (Fluorspan), and magnesium fluoride or Calcium Fluoride (Fluorspan) add-on are 2% of material gross weight, mix once more, enter dry method pressure ball system then;
4) in dry method pressure ball system, will be broken into 0-3mm behind the first base of above-mentioned material, mix back dry method balling-up with the material that does not have base at 6: 4 with volume ratio again, the blank density after the balling-up is 2.10g/cm 3, through maintenance in 48 hours, the volume density after the maintenance can reach 2.15g/cm 3, enter the calcining of high temperature oil shaft furnace, adopting cracked oil or heavy oil is fuel, and calorific value is 11000 kcal/kg, and temperature is 1950 ℃-2050 ℃, and calcining and soaking time are kiln discharge after 18-20 hour, check LOI<0.10%, SiO 2: 0-0.06%, CaO:0.45-0.72%, MgO:99-99.15%, Fe 2O 3: 0-0.01%, Al 2O 3: 0-0.06%, B.D.3.43-3.45g/cm 3
The present invention compared with prior art, its beneficial effect is:
1) selecting cryptocrystal type magnesite for use is raw material, substitutes traditional phanerocrystalline texture type magnesite and produces highly-purity magnesite, material purity height, impurity such as not siliceous, iron, aluminium.
2) by the ultra-fine mill means of classification, make the light burnt powder fineness at<10 μ m, specific surface area reaches 8-10m 2/ g, and have higher activation energy, be that the calcining of two steps creates conditions.
3) use anion active agent, when high-temperature calcination, anion transport, the room appears in lattice, and MgO fills the room, makes material obtain higher volume density.
4) base process makes blank obtain initial high-density, is about to be broken into 0-3mm behind the first base of above-mentioned material, again with 6: 4 ratio of volume ratio and the balling-up of mixing of materials dry method, makes material obtain 2.10g/cm 3Initial density, with the maintenance 48 hours in environment of ball base, the aqueous vapor in its surperficial absorbing environmental is hardened more then, can improve density 0.05g/cm 3, there is Mg (OH) in surperficial material simultaneously 2Reaction is more conducive to sintering than MgO.
5) product is high purity, high-density, and MgO content is 98%-99% in its product, volume density 3.40-3.45g/cm 3Compare with seawater magnesia, production cost is low, fire-resistant intensity height.
Embodiment
Natural cryptocrystal type magnesite by two-step calcining is produced the technology of highly-purity magnesite, and this technology comprises the steps:
1) with the cryptocrystal type magnesite of exploitation, wash with water, remove impurity, dry then, make moisture less than 8%;
2) adopt Hubei Province to break the granularity that is crushed to 0-5mm with pair roller, roasting in fluidizing furnace, temperature is 870 ℃;
Or adopt ball milling to be milled to 200 purpose granularities and go into the shower furnace roasting, temperature is 820 ℃; The granularity of material outlet is 325 orders, and percent of pass is at 92%-93%, and the activity of material is 35 seconds after the roasting in fluidizing furnace, and the activity of material is 25 seconds after the roasting in shower furnace;
3) material enters classification fine grinding operation, with in the 325 order materials<material of 10 μ m tells, with in the material>material of 10 μ m enters the fine grinding system and is milled to<10 μ m, percent of pass 97%, behind the described material uniform mixing of telling, specific surface area reaches 8-10m 2/ g adds anion active agent magnesium fluoride or Calcium Fluoride (Fluorspan), and magnesium fluoride or Calcium Fluoride (Fluorspan) add-on are 2% of material gross weight, mix once more, enter dry method pressure ball system then;
4) in dry method pressure ball system, will be broken into 0-3mm behind the first base of above-mentioned material, mix back dry method balling-up with the material that does not have base at 6: 4 with volume ratio again, the blank density after the balling-up is 2.10g/cm 3, through maintenance in 48 hours, the volume density after the maintenance can reach 2.15g/cm 3, enter the calcining of high temperature oil shaft furnace, adopting cracked oil or heavy oil is fuel, and calorific value is 11000 kcal/kg, and temperature is 1950 ℃-2050 ℃, and calcining and soaking time are kiln discharge after 18-20 hour, check LOI<0.10%, SiO 2: 0-0.06%, CaO:0.45-0.72%, MgO:99-99.15%, Fe 2O 3: 0-0.01%, Al 2O 3: 0-0.06%, B.D.3.43-3.45g/cm 3

Claims (1)

1, natural cryptocrystal type magnesite by two-step calcining is produced the technology of highly-purity magnesite, it is characterized in that this technology comprises the steps:
1) with the cryptocrystal type magnesite of exploitation, wash with water, remove impurity, dry then, make moisture less than 8%;
2) adopt Hubei Province to break the granularity that is crushed to 0-5mm with pair roller, roasting in fluidizing furnace, temperature is 870 ℃;
Or adopt ball milling to be milled to 200 purpose granularities and go into the shower furnace roasting, temperature is 820 ℃; The granularity of material outlet is 325 orders, and percent of pass is at 92%-93%, and the activity of material is 35 seconds after the roasting in fluidizing furnace, and the activity of material is 25 seconds after the roasting in shower furnace;
3) material enters classification fine grinding operation, with in the 325 order materials<material of 10 μ m tells, with in the material>material of 10 μ m enters the fine grinding system and is milled to<10 μ m, percent of pass 97%, behind the described material uniform mixing of telling, specific surface area reaches 8-10m 2/ g adds anion active agent magnesium fluoride or Calcium Fluoride (Fluorspan), and magnesium fluoride or Calcium Fluoride (Fluorspan) add-on are 2% of material gross weight, mix once more, enter dry method pressure ball system then;
4) in dry method pressure ball system, will be broken into 0-3mm behind the first base of above-mentioned material, mix back dry method balling-up with the material that does not have base at 6: 4 with volume ratio again, the blank density after the balling-up is 2.10g/cm 3, through maintenance in 48 hours, the volume density after the maintenance reached 2.15g/cm 3, enter the calcining of high temperature oil shaft furnace, adopting cracked oil or heavy oil is fuel, and calorific value is 11000 kcal/kg, and temperature is 1950 ℃-2050 ℃, and calcining and soaking time are kiln discharge after 18-20 hour, check LOI<0.10%, SiO 2: 0-0.06%, CaO:0.45-0.72%, MgO:99-99.15%, Fe 2O 3: 0-0.01%, Al 2O 3: 0-0.06%, B.D.3.43-3.45g/cm 3
CNB2006100460570A 2006-03-16 2006-03-16 Process for producing high quality high purity magnesite by two-step calcining natural cryptocrystalline magnesite Expired - Fee Related CN100335435C (en)

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Publication number Priority date Publication date Assignee Title
CN102774861A (en) * 2012-08-17 2012-11-14 海城三星矿业有限公司 Purification process of high-purity magnesia
CN103922615A (en) * 2014-03-27 2014-07-16 沈阳化工大学 Method for preparing high-grade electrical-grade magnesium oxide from low-grade fused magnesium oxide
CN109437607B (en) * 2019-01-11 2021-06-22 于景坤 Preparation method of high-density sintered magnesia
CN109809716B (en) * 2019-03-29 2020-05-12 东北大学 Method for preparing high-purity light-burned magnesia by calcining low-grade magnesite, decalcifying and desiliconizing
CN111348845B (en) * 2020-03-13 2021-12-31 海城市光大高纯镁砂有限责任公司 Preparation method for preparing high-grade high-purity magnesite by using magnesium sulfate as binding agent
CN111925191A (en) * 2020-07-13 2020-11-13 辽宁东和新材料股份有限公司 Method for producing high-density high-purity sintered magnesia by using low-grade magnesite

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1070156C (en) * 1996-09-05 2001-08-29 辽宁镁矿耐火材料公司 Method for producing high-purity dense macrocrystalline sintered magnesia
CN1114567C (en) * 1999-08-30 2003-07-16 杨庆广 High-purity magnesite with volume density higher than 3.40 g/cu.cm prepared from magnesite and its preparing process
CN1709827A (en) * 2005-07-06 2005-12-21 东北大学 Sintered magnesium sand preparing method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1070156C (en) * 1996-09-05 2001-08-29 辽宁镁矿耐火材料公司 Method for producing high-purity dense macrocrystalline sintered magnesia
CN1114567C (en) * 1999-08-30 2003-07-16 杨庆广 High-purity magnesite with volume density higher than 3.40 g/cu.cm prepared from magnesite and its preparing process
CN1709827A (en) * 2005-07-06 2005-12-21 东北大学 Sintered magnesium sand preparing method

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