CN106630968A - A compact periclase chondrule and a preparing method thereof - Google Patents

A compact periclase chondrule and a preparing method thereof Download PDF

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Publication number
CN106630968A
CN106630968A CN201610849627.3A CN201610849627A CN106630968A CN 106630968 A CN106630968 A CN 106630968A CN 201610849627 A CN201610849627 A CN 201610849627A CN 106630968 A CN106630968 A CN 106630968A
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Prior art keywords
periclase
fine
close
spherolite
magnesium
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CN201610849627.3A
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CN106630968B (en
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魏耀武
张奇
李楠
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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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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/03Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite
    • C04B35/04Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite based on magnesium oxide
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605Treating the starting powders individually or as mixtures
    • C04B35/62645Thermal treatment of powders or mixtures thereof other than sintering
    • C04B35/6267Pyrolysis, carbonisation or auto-combustion reactions
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605Treating the starting powders individually or as mixtures
    • C04B35/62695Granulation or pelletising
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/66Monolithic refractories or refractory mortars, including those whether or not containing clay

Abstract

The invention relates to a compact periclase chondrule and a preparing method thereof. According to a technical scheme, magnesium hydroxide powder is put into a material barrel of a granulating device; water accounting for 5-30 wt% of the magnesium hydroxide powder is added into the material barrel with the speed being 1000-3000 r/min; when a spherical particle is generated, the rotating speed is adjusted to 500-1000 r/min, and granulation is stopped after 1-10 min of running to obtain a magnesium hydroxide spherical particle; the magnesium hydroxide spherical particle is taken out and dried at 110 DEG C for 24 h; and then the dried magnesium hydroxide spherical particle is put into a heating kiln, the temperature is maintained at 1400-1700 DEG C for 1-6 h, and the spherical particle is cooled to obtain the compact periclase chondrule. The compact periclase chondrule and the method have characteristics of a simple process and a low cost. The using temperature of the prepared compact periclase chondrule is high, the high-temperature performance stability and hydration resistance of the prepared compact periclase chondrule are good, and the compact periclase chondrule is an excellent raw material for preparing magnesium refractory materials and high-temperature ceramics, particularly magnesium unshaped refractory materials.

Description

A kind of fine and close periclase spherolite and preparation method thereof
Technical field
The invention belongs to refractory material and high-temperature ceramic techniques field.Specifically related to a kind of fine and close periclase spherolite and its system Preparation Method.
Background technology
Magnesia refractories refers to content of MgO more than 80wt% and the basic refractory with periclase as principal crystalline phase.It is magnesia Not only refractoriness is high for refractory material, the good and anti-high ferro scouring of alkali resistance slag by force, and the pollution very little to molten steel and has The ability of standby certain purifying of steel, this kind of refractory material be mainly used in converter, electric furnace, ladle, external refining, tundish and Coloured smelting furnace etc..Magnesia refractories is mainly used for each high-temperature field in the form of shaped product, such as:Magnesia brick, magnesia carbon brick, Mg-Al spinel brick etc..In terms of the preparation of unshape refractory, the aquation of the primary raw material-magnesia of magnesian is given Using certain difficulty is brought, the application advantage of castable is weakened.Unshape refractory is referred to by refractory aggregate It is being collectively constituted with certain proportion with powder, bonding agent, additive, not shaped and burn till and directly use or add appropriate liquid (Generally water)Use after allotment, also referred to as loose refractory or monolithic refractory(Can be made into jointless overall fire proofed wood Material).
The main chemical compositions of the raw material magnesia of production magnesia refractories are magnesia, and mineral are periclase.Magnesia root It is divided into the kinds such as magnesite clinker, fused magnesite and seawater magnesia according to preparation technology.Wherein, the preparation technology of magnesite clinker is divided into one Step and two steps annealing method.One-step calcination method be will after magnesite powder briquetting in high temperature calcine, the magnesia bulk density for obtaining compared with It is low.Two step calcination methods are referred to again Jing high-temperature calcinations are obtained after light calcined magnesia fine grinding and pressed compact.By a step or two step calcination methods Prepared magnesia carries out crushing and magnesia particle is obtained.Electric smelting method be by magnesite, shepardite etc. electric furnace high temperature melt and The method for obtaining magnesia.Seawater method is that the magnesium chloride after chemical reaction in seawater is prepared into magnesium hydroxide, then pressed compact(Pressure Block or balling-up)Jing after high-temperature calcination.The size of finished product magnesia block is all in more than 50mm obtained in above method.
As can be seen that in the technical scheme of existing magnesia preparation, resulting magnesia granularity is larger, in magnesia block input It will be crushed using before and be crushed, and magnesia surface Jing after high-temperature process (no matter semi-finished product before high-temperature process Pressed compact or balling-up) sinter layer be seriously damaged in shattering process, it is broken after expose new surface, so as to cause magnesium Sand particle especially magnesia powder easy aquation after contacting with water, brings certain tired to unshaped magnesium refractory material application It is difficult.For example:After the drying, billet surface has a large amount of cracking even larger crackles to be formed to castable.Unshape refractory It is the development trend of refractory material, and the preparation technology of existing magnesia constrains the application of unshaped magnesium refractory material and pushes away Extensively.
The content of the invention
It is contemplated that overcoming prior art not enough, it is therefore an objective to provide a kind of process is simple and lower-cost densification side's magnesium The preparation method of stone spherolite, the fine and close periclase spherolite prepared with the method using temperature it is high, have stable high-temperature performance and hydration-resisting Performance is good;Can be used as the quality raw materials for preparing magnesia refractories and refractory ceramics, especially unshape refractory.
For achieving the above object, the technical solution adopted in the present invention is:Magnesium hydrate powder is placed in into Granulation Equipments In charging basket, under conditions of 1000 ~ 3000 revs/min, the water for accounting for 5 ~ 30wt% of magnesium hydrate powder is added in the charging basket; When there is spheric granules to be formed, rotating speed is adjusted into 500 ~ 1000 revs/min, is operated 1 ~ 10 minute, stop granulation, hydroxide is obtained Magnesium spheric granules.
The magnesium hydroxide spheric granules is taken out, is dried 24 hours under the conditions of 110 DEG C.Then by dried hydrogen-oxygen Change magnesium granules to be placed in heating kiln, under the conditions of 1400 ~ 1700 DEG C 1 ~ 6 hour is incubated, cooling obtains final product fine and close periclase ball Grain.
Content of MgO >=the 60wt% of the magnesium hydrate powder;The particle diameter of the magnesium hydrate powder is 1 ~ 500 μm.
There is compared with prior art following good effect due to adopting above-mentioned technical proposal, the present invention:
1)The present invention is directly granulated to magnesium hydrate powder, and varigrained fine and close periclase spherolite is obtained final product after high-temperature process, can Directly to use, without the need for broken and crushing.And the magnesia product that prior art is obtained will be through being crushed to specification granularity ability Use.
2)The present invention is little due to the granularity of particle prepared by Granulation Equipments, and in high-temperature process, magnesium hydroxide decomposes thorough Bottom simultaneously reaches sintering, and the sintering degree and bulk density of the fine and close periclase spherolite for finally giving is higher.
3)The present invention will not be destroyed without the need for being crushed processing again to the fine and close periclase spherolite obtained after high-temperature process The sinter layer that spherome surface is formed in high-temperature process, thus, the hydration resistance of resulting fine and close periclase spherolite It is good, it is easy to use, the raw material that can be prepared directly as magnesia refractories and refractory ceramics especially magnesia unsetting fire proofed wood The raw material of material is used.
4)The use temperature of fine and close periclase spherolite prepared by the present invention is more than 1600 DEG C, is had stable high-temperature performance, volume Density is big and hydration resistance is good, is that to prepare the advanced materials such as magnesia refractory material and ceramics especially magnesia unsetting resistance to The novel material of fiery material.
Fine and close periclase spherolite prepared by the present invention is after testing:Content of MgO >=90wt%, granularity be 0.02 ~ 10mm, volume Density >=3.0g/cm3;10h is kept under 50 DEG C and 90% damp condition, aquation rate of body weight gain≤1% after 110 DEG C of drying.
Therefore, the characteristics of present invention has process is simple and low cost;Prepared fine and close periclase spherolite uses temperature It is high, have stable high-temperature performance good with hydration resistance, be to prepare magnesia refractories and refractory ceramics, especially magnesia unsetting resistance to The quality raw materials of fiery material.
Specific embodiment
With reference to specific embodiment, the present invention will be further described, not to the restriction of its protection domain.
It is now that the magnesium hydrate powder Unify legislation in this specific embodiment is as follows to avoid repeating, in embodiment not Repeat again:
Content of MgO >=the 60wt% of the magnesium hydrate powder;The particle diameter of the magnesium hydrate powder is 1 ~ 500 μm.
Embodiment 1
A kind of fine and close periclase spherolite and preparation method thereof.Magnesium hydrate powder is placed in the charging basket of Granulation Equipments, 1000 ~ Under conditions of 1500 revs/min, the water for accounting for 5 ~ 15wt% of magnesium hydrate powder is added in the charging basket;When there is spheric granules shape Cheng Shi, by rotating speed 500 ~ 600 revs/min are adjusted to, and are operated 1 ~ 4 minute, stop granulation, and magnesium hydroxide spheric granules is obtained.
The magnesium hydroxide spheric granules is taken out, is dried 24 hours under the conditions of 110 DEG C.Then by dried hydrogen-oxygen Change magnesium granules to be placed in heating kiln, under the conditions of 1400 ~ 1500 DEG C 4 ~ 6 hours are incubated, cooling obtains final product fine and close periclase ball Grain.
Fine and close periclase spherolite manufactured in the present embodiment is after testing:Content of MgO >=90wt%, granularity be 0.02 ~ 3mm, volume Density >=3.0g/cm3;10h is kept under 50 DEG C and 90% damp condition, aquation rate of body weight gain≤1% after 110 DEG C of drying.
Embodiment 2
A kind of fine and close periclase spherolite and preparation method thereof.Magnesium hydrate powder is placed in the charging basket of Granulation Equipments, 1500 ~ Under conditions of 2000 revs/min, the water for accounting for 15 ~ 20wt% of magnesium hydrate powder is added in the charging basket;When there is spheric granules shape Cheng Shi, by rotating speed 600 ~ 800 revs/min are adjusted to, and are operated 4 ~ 8 minutes, stop granulation, and magnesium hydroxide spheric granules is obtained.
The magnesium hydroxide spheric granules is taken out, is dried 24 hours under the conditions of 110 DEG C.Then by dried hydrogen-oxygen Change magnesium granules to be placed in heating kiln, under the conditions of 1500 ~ 1600 DEG C 2 ~ 4 hours are incubated, cooling obtains final product fine and close periclase ball Grain.
Fine and close periclase spherolite manufactured in the present embodiment is after testing:Content of MgO >=94wt%;3 ~ 5mm of granularity, bulk density ≥3.1g/cm3.Under 50 DEG C and 90% damp condition, 10h is kept, after 110 DEG C of drying, the aquation rate of body weight gain of periclase spherolite ≤0.6%。
Embodiment 3
A kind of fine and close periclase spherolite and preparation method thereof.Magnesium hydrate powder is placed in the charging basket of Granulation Equipments, 2000 ~ Under conditions of 3000 revs/min, the water for accounting for 20 ~ 30wt% of magnesium hydrate powder is added in the charging basket;When there is spheric granules shape Cheng Shi, by rotating speed 800 ~ 1000 revs/min are adjusted to, and are operated 8 ~ 10 minutes, stop granulation, and magnesium hydroxide spheric granules is obtained.
The magnesium hydroxide spheric granules is taken out, is dried 24 hours under the conditions of 110 DEG C.Then by dried hydrogen-oxygen Change magnesium granules to be placed in heating kiln, under the conditions of 1600 ~ 1700 DEG C 1 ~ 3 hour is incubated, cooling obtains final product fine and close periclase ball Grain.
Fine and close periclase spherolite manufactured in the present embodiment is after testing:Content of MgO >=97wt%, granularity is 5 ~ 10mm, and volume is close Degree >=3.2g/cm3.10h is kept under 50 DEG C and 90% damp condition, aquation rate of body weight gain≤0.3% after 110 DEG C of drying.
This specific embodiment has compared with prior art following good effect:
1)The present invention is directly granulated to magnesium hydrate powder, and varigrained fine and close periclase spherolite is obtained final product after high-temperature process, can Directly to use, without the need for broken and crushing.
2)The present invention is little due to the granularity of particle prepared by Granulation Equipments, and in high-temperature process, magnesium hydroxide decomposes thorough Bottom simultaneously reaches sintering, and the sintering degree and bulk density of the fine and close periclase spherolite for finally giving is higher.
3)The present invention will not be destroyed without the need for being crushed processing again to the fine and close periclase spherolite obtained after high-temperature process The sinter layer that spherome surface is formed in high-temperature process, thus, the hydration resistance of resulting fine and close periclase spherolite It is good, it is easy to use, the raw material that can be prepared directly as magnesia refractories and refractory ceramics especially magnesia unsetting fire proofed wood The raw material of material is used.
4)More than 1600 DEG C of the use temperature of fine and close periclase spherolite prepared by the present invention, have stable high-temperature performance, volume it is close Degree is big and hydration resistance is good, is to prepare the especially magnesia unsetting fire resisting of the advanced materials such as magnesia refractory material and ceramics The novel material of material.
Fine and close periclase spherolite prepared by the present invention is after testing:Content of MgO >=90wt%, granularity be 0.02 ~ 10mm, volume Density >=3.0g/cm3;10h is kept under 50 DEG C and 90% damp condition, aquation rate of body weight gain≤1% after 110 DEG C of drying.
Therefore, the characteristics of present invention has process is simple, low cost;Prepared fine and close periclase spherolite uses temperature It is high, have stable high-temperature performance good with hydration resistance, be to prepare magnesia refractories and refractory ceramics, especially unsetting fire proofed wood The quality raw materials of material.

Claims (3)

1. a kind of preparation method of fine and close periclase spherolite, it is characterised in that:Magnesium hydrate powder is placed in into the material of Granulation Equipments In bucket, under conditions of 1000 ~ 3000 revs/min, the water for accounting for 5 ~ 30wt% of magnesium hydrate powder is added in the charging basket;When When having spheric granules to be formed, rotating speed is adjusted into 500 ~ 1000 revs/min, is operated 1 ~ 10 minute, stop granulation, magnesium hydroxide is obtained Spheric granules;
The magnesium hydroxide spheric granules is taken out, is dried 24 hours under the conditions of 110 DEG C;Then by dried magnesium hydroxide Particle is placed in heating kiln, and under the conditions of 1400 ~ 1700 DEG C 1 ~ 6 hour is incubated, and cooling obtains final product fine and close periclase spherolite.
2. the preparation method of fine and close periclase spherolite according to claim 1, it is characterised in that the magnesium hydrate powder Content of MgO >=60wt%;The particle diameter of the magnesium hydrate powder is 1 ~ 500 μm.
3. a kind of fine and close periclase spherolite, it is characterised in that the fine and close periclase spherolite is appointed according in claim 1 ~ 2 Fine and close periclase spherolite prepared by the preparation method of the fine and close periclase spherolite described in.
CN201610849627.3A 2016-09-26 2016-09-26 A kind of densification periclase spherolite and preparation method thereof Active CN106630968B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111170749A (en) * 2020-01-16 2020-05-19 海城市中昊镁业有限公司 Method for preparing fused forsterite by utilizing magnesite tailings through electric melting

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1413940A (en) * 2001-10-23 2003-04-30 刘绪庆 Technology for preparing high purity magnesia by high concentration magnesium oxide solution
CN1903769A (en) * 2006-08-01 2007-01-31 东北大学 Preparation method of magnesium calcium clinker
CN103896618A (en) * 2014-01-28 2014-07-02 浙江自立氧化铝材料科技有限公司 Light weight microporous corundum aggregate and preparation method thereof
CN105439577A (en) * 2015-11-25 2016-03-30 武汉科技大学 Magnesia-calcium clinker adopting core-shell coated structure and preparation method of magnesia-calcium clinker

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1413940A (en) * 2001-10-23 2003-04-30 刘绪庆 Technology for preparing high purity magnesia by high concentration magnesium oxide solution
CN1903769A (en) * 2006-08-01 2007-01-31 东北大学 Preparation method of magnesium calcium clinker
CN103896618A (en) * 2014-01-28 2014-07-02 浙江自立氧化铝材料科技有限公司 Light weight microporous corundum aggregate and preparation method thereof
CN105439577A (en) * 2015-11-25 2016-03-30 武汉科技大学 Magnesia-calcium clinker adopting core-shell coated structure and preparation method of magnesia-calcium clinker

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李环等: "菱镁矿轻烧水化对MgO烧结的影响", 《耐火材料》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111170749A (en) * 2020-01-16 2020-05-19 海城市中昊镁业有限公司 Method for preparing fused forsterite by utilizing magnesite tailings through electric melting

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