CN105837242B - A kind of square magnesium stone-spinel light weight refractory material and preparation method thereof - Google Patents
A kind of square magnesium stone-spinel light weight refractory material and preparation method thereof Download PDFInfo
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- CN105837242B CN105837242B CN201610172527.1A CN201610172527A CN105837242B CN 105837242 B CN105837242 B CN 105837242B CN 201610172527 A CN201610172527 A CN 201610172527A CN 105837242 B CN105837242 B CN 105837242B
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- 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
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/0022—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof obtained by a chemical conversion or reaction other than those relating to the setting or hardening of cement-like material or to the formation of a sol or a gel, e.g. by carbonising or pyrolysing preformed cellular materials based on polymers, organo-metallic or organo-silicon precursors
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- 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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- 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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Abstract
The invention discloses a kind of periclase spinelle light weight refractory material and preparation methods, the periclase spinelle light weight refractory material of preparation has density gradient from outside to inside, outside is dense outer layer, and internal porous, dense outer layer assigns material anti-working media infiltration performance, and internal porous assigns material thermal and insulating performance.Preparation method is to choose magnesia and carbon as reaction raw materials, and the sample suppressed, to controlled atmosphere stove evacuation, is then charged with Ar as protection, furnace body is heated certain temperature and is passed through O as in atmosphere sintering furnace2, magnesia and carbon occur carbothermic reduction reaction, generate Mg steam, the O that Mg steam spreads and is passed through2The spinelle of reaction generation magnesia, oxidation generation magnesia or reaction generation makes sample base portion generate combination.With firing temperature is relatively low, the sample porosity, bulk density is adjustable, the characteristics of compressive resistance and higher refractoriness under load.
Description
Technical field
The present invention relates to technical field of fire resistant material production, and in particular to a kind of square magnesium stone-spinel light weight refractory material
And preparation method thereof.
Background technology
Square magnesium stone-spinel fire resistant materials are since its temperature in use is high, resistance performance of slag corrosion is good, anti-thermal shock, raw material are easy to get
Etc. advantages had a wide range of applications in terms of the Thermal Equipments such as RH refining furnaces, cement rotary kiln and glass furnace checker.With
Energy crisis becomes one of the problem of whole world is the most deeply concerned, the energy-saving finger for having become government and corporate boss will control and examine
Mark.As what refractory material was studied gos deep into, scientific worker proposes the concept of light weight refractory material, such refractory body
Product density is between lightweight refracrory and heavy refractory material, by introducing light weight aggregate (hole of holding one's breath in refractory material
Rate is higher, the comparatively dense particle in surface), it can accomplish under the premise of refractory material applied at elevated temperature performance is not significantly reduced,
Reduce refractory material volume density.Already research shows that fireclay insulating refractory is closer to hot working face, heat-insulating and energy-saving effect
Better.Replace heavy refractory material as high temperature kiln working lining by the use of the light weight refractory material for introducing light weight aggregate thus, especially
It is the hot operation lining for being contacted with working media, it is expected to obtain preferably energy conservation and consumption reduction effects.About square magnesium stone-spinel
Existing report is prepared by introducing light weight spinelle aggregate in square magnesium stone-spinel castable to light weight refractory material at present
Go out periclase-spinelle light weight castable refractory.Research confirms that the introducing of light weight aggregate causes the pouring fireproof material volume
Density reduces, and heat-proof quality improves, but also results in the infiltration ability reduction of castable slag-resistant, influences its service life.
Invention content
The defects of for present in above-mentioned background technology or deficiency, it is an object of the present invention to develop a kind of periclase-point
Spar light weight refractory material.Transporting oxidation bonding reaction sintering by magnesia carbon thermal reduction, to prepare square magnesium stone-spinel light
Measure refractory material.To solve the contradiction between high erosion-resisting characteristics and low heat conductivity.The square magnesium stone-spinel light weight for making preparation is resistance to
Fiery material improves its erosion-resisting characteristics and applied at elevated temperature performance in the case where keeping low heat conductivity.
In order to realize above-mentioned task, the present invention takes following technical solution：
A kind of preparation method of square magnesium stone-spinel light weight refractory material, which is characterized in that including following preparation steps：
Step 1 chooses magnesia and carbon as reaction raw materials, raw material is milled down to 180 mesh and hereinafter, is rubbed according to MgO and C
That ratio 1:1 is uniformly mixed, as the pore-creating in fine powder in refractory material dispensing and reaction component；
Raw material for refractory is carried out dispensing by step 2 according to certain grain composition, aggregate fraction and fine fraction
Ratio is 50~80:Between 20~50, wherein fine fraction is spinelle fine powder and step 1 mixes MgO and C powders, root
It is required according to product, MgO the and C powders account for the 20%~70% of fine fraction；Fine fraction needs blending 30 minutes to 90
Minute, so that each component is uniformly mixed；
Step 3 mixes 2~5 minutes according to aggregate fraction is first added in, and adds phenolic resin dilution and mixes 3~5 points
Clock adds fine fraction, mixes 5~20 minutes, and incorporation time was amounted at 20~30 minutes in mixing machine；Mixed object
Material is placed in ageing mixture 2 hours to 6 hours in closed container or polybag；
Step 4, the material after ageing mixture are pressed into definite shape using semi-dry pressing；
Step 5 by sample nature air dry half a day of forming to 1 day, then in drying equipment, is heated up using the stage
It is dried with heat preserving mode, finally keeps the temperature 6 hours to 24 hours at 110 DEG C；
Step 6, dry aftershaping sample firing carry out in controlled atmosphere generator, first to controlled atmosphere stove evacuation, so
After be filled with Ar as protective gas, furnace body is heated to 1450 DEG C~1650 DEG C, reaches and is kept the temperature in the temperature range, and
It is passed through O2, control and be passed through O2Flow velocity ensures that the Mg steam reactions of carbothermic reduction reaction generation are complete, and molding sample is burnt by reacting
Knot is obtained with the square magnesium stone-spinel light weight refractory material compared with low bulk density and higher-strength.
The square magnesium stone-spinel light weight refractory material prepared using the present invention has density gradient from outside to inside, external
For dense outer layer, and internal porous, dense outer layer assign material anti-working media infiltration performance, and internal porous assigns material heat preservation
Heat-proof quality.
Its advantage is mainly manifested in the following aspects：
(1) pore-creating and the reaction-sintered of realizing sample are aoxidized due to being transported using magnesia carbon thermal reduction, can led to thus
It crosses the addition of adjustment magnesia and carbonaceous material, add in granularity and proportion scale, be conveniently adjusted bulk density, the gas of product
Porosity and gas cell distribution, so as to regulate and control thermal and insulating performance.
(2) due to transporting oxidation bonding reaction-sintered using magnesia carbon thermal reduction so that sample base portion has very well
Combination so that square magnesium stone-spinel light weight refractory material intensity is higher, even higher than other preparation methods of same material obtain
Heavy refractory material.
(3) magnesia and the progress of chemical vapour infiltration basic theories are prepared since magnesia carbon thermal reduction is transported oxidizing process
Grafting, when magnesium steam and oxygen react in porous matrix, there are between mass transfer and Chemical Kinetics
Contradiction so that sample external reaction product is more, and internal product is less, so as to form the density gradient of base portion and combination
Intensity gradient.It can make material that there is higher-strength and applied at elevated temperature in the case where keeping light weight refractory material low heat conductivity
Performance.
(4) since magnesium steam oxidation is a strong exothermal reaction, the reduction of product firing temperature can be made by reaction-sintered.
(5) it can be selected according to different use occasions using light weight spinelle aggregate, light weight magnesite clinker or fine and close point
Spar aggregate, the controllable range of properties of product are big.
Specific embodiment
Magnesia carbon thermal reduction transport oxidation bonding reaction sintering prepare light weight refractory material basic principle be：Resistance to
During fiery material dispensing, magnesium oxide powder and graphite fine powder (carbonaceous materials such as carbon black, coke fine powder) are introduced in fine powder, it is high
With graphite carbothermic reduction reaction generation magnesium steam Mg (g) and carbon monoxide CO (g) occur for magnesia in the lower sample of temperature, in sample
Portion forms stomata, and to the oxygen that external diffusion and sample are spread outside to inside exothermic reaction generation magnesia occurs for magnesium steam, newly-generated
Magnesia spinelle light weight aggregate and matrix are combined, the strongly exothermic and reaction bonded by means of magnesium vapor oxidation to try
Sample has higher intensity.When magnesium steam and oxygen react in porous matrix, there are mass transfers and chemical reaction
Contradiction between dynamics so that sample external reaction product is more, and internal product is less, so as to form the close of base portion
Spend gradient and bond strength gradient.Consistency is high outside sample, is conducive to anti-medium under high temperature and infiltrates, improves corrosion resistance, interior
Portion's porosity is higher, is conducive to insulation.It should be noted that be the optimum embodiment that inventor provides below, the present invention
Be not limited to these embodiments, through applicant's it is demonstrated experimentally that in the range of the present invention provides, can prepare periclase-
Spinelle light weight refractory material.
The present embodiment provides a kind of preparation method of square magnesium stone-spinel light weight refractory material, and preparation process includes following
Step：
Step 1 chooses magnesia and carbon as reaction raw materials, hereinafter, rubs raw material is levigate to 180 mesh and according to MgO and C
That ratio 1:1 is uniformly mixed, as the pore-creating in fine powder in refractory material dispensing and reaction component.
Raw material for refractory is carried out dispensing by step 2 according to certain grain composition.Aggregate fraction and fine fraction
Ratio is 50~80:Between 20~50, wherein fine fraction is spinelle fine powder and step 1 mixes MgO and C powders, root
It is required according to product, MgO the and C powders account for the 20%~70% of fine fraction；In order to improve uniform in quality and steady
Qualitative, fine fraction needs blending 30 minutes to 90 minutes, so that each component is uniformly mixed.
Step 3 mixes 2~5 minutes according to aggregate fraction is first added in, and adds phenolic resin ethylene glycol dilution mixing 3
~5 minutes, fine powder is added, is mixed 5~20 minutes, incorporation time was amounted at 20~30 minutes in mixing machine.It is mixed
Material is placed in ageing mixture 2 hours to 6 hours in closed container or polybag, makes bonding agent (phenolic resin ethylene glycol) distribution more
Uniformly, it is easy to be molded.
Step 4, the material after ageing mixture are pressed into the sample base of definite shape and size, root using semi-dry pressing
According to the size of sample base, using the press of different tonnages.
Step 5 by sample nature air dry half a day of forming to 1 day, then in drying equipment, is heated up using the stage
It is dried with heat preserving mode, finally keeps the temperature 6 hours to 24 hours at 110 DEG C.
Step 6, dry aftershaping sample firing carry out in controlled atmosphere generator, first to controlled atmosphere stove evacuation, so
After be filled with Ar as protective gas, furnace body is heated to 1450 DEG C~1600 DEG C, reaching in the temperature range can be kept the temperature,
And it is passed through O2, control and be passed through O2Flow velocity ensures that the Mg steam reactions of carbothermic reduction reaction generation are complete, and molding sample passes through reaction
Sintering is obtained with the square magnesium stone-spinel light weight refractory material compared with low bulk density and higher-strength.
Square magnesium stone-spinel light weight refractory material prepared by the present invention, relatively low with bulk density, compressive resistance is higher
Feature, it is expected to while thermal and insulating performance is ensured, there is preferable anti-medium erosion performance.
According to the present invention, the magnesia is magnesite clinker or fused magnesite；
The carbon is not available thin coke in carbon black, graphite, coke, coal dust, barren rock electrode ink or metallurgical process
Charcoal particle.
The aggregate is light weight magnesia particle, light weight spinel particle, fine and close spinel particle, magnesite clinker, electric-melting magnesium
Sand or their mixture.
It is specific embodiment below.
Embodiment 1：
By 180 mesh fused magnesites and 180 mesh graphite, by MgO and C molar ratios 1:1 is uniformly mixed.Respectively with 1~3mm and
The spinel particle of 0.1~1mm is coarse granule and middle particle.Using magnesia powder, graphite fine powder and spinelle fine powder as matrix portion
Distribution material, coarse granule:Middle particle:Fine powder ratio is 40:20:40.Wherein fine fraction spinelle fine powder and magnesia and graphite
The ratio of mixed powder is 2:1.Using phenolic resin ethylene glycol solution as bonding agent, addition be dispensing total weight 8%, dispensing
It is adequately mixed and is placed on ageing mixture 2 hours in closed container or polybag；Material after ageing mixture is using semidry method in hydraulic pressure
Be molded sample on machine, briquetting pressure 150MPa, molding sample nature air dry half a day to 1 day, then in drying equipment, using rank
Duan Shengwen and heat preserving mode are dried, and finally keep the temperature 6 hours at 110 DEG C；Dry aftershaping sample is put into controlled atmosphere generator
It is interior, Ar protections are filled after vacuumizing, are heated to starting to keep the temperature, and be passed through O at 1450 DEG C2, O2(oxygen gas flow rate can for 250L/h for flow velocity
According to sample how much and size adjustment), heat preservation 4 hours, obtain square magnesium stone-spinel light weight refractory material.Its performance is shown in
Table 1.
Table 1：The performance of 1 square magnesium stone-spinel light weight refractory material of example
Embodiment 2：
By 180 mesh magnesite clinkers and 180 mesh graphite, by MgO and C molar ratios 1:1 is uniformly mixed.Respectively with 1mm~3mm and
The light weight spinelle of 0.1~1mm is coarse granule and middle particle.Using magnesia powder, graphite fine powder and alumina powder as matrix portion
Distribution material, coarse granule:Middle particle:Fine powder ratio is 40:20:40.Wherein fine fraction alumina powder and magnesia and graphite
The ratio of mixed powder is 2:1.Using phenolic resin ethylene glycol solution as bonding agent, addition be dispensing total weight 8%, dispensing
It is adequately mixed and is placed on ageing mixture 2 hours in closed container or polybag；Material after ageing mixture is molded on a hydraulic press, into
Type pressure 150MPa, sample nature air dry half a day of forming then in drying equipment, were heated up and were protected using the stage to 1 day
Warm mode is dried, and finally keeps the temperature 6 hours at 110 DEG C；Dry aftershaping sample is put into controlled atmosphere generator, after vacuumizing
Ar protections are filled, are heated to starting to keep the temperature, and be passed through O at 1550 DEG C2, O2Flow velocity for 250L/h (oxygen gas flow rate can according to sample how much
Adjusted with size), 4 hours are kept the temperature, obtains square magnesium stone-spinel light weight refractory material.Its performance is shown in Table 2.
Table 2：The performance of 2 square magnesium stone-spinel light weight refractory material of example
Embodiment 3：
By 180 mesh fused magnesites and 180 mesh graphite, by MgO and C molar ratios 1:1 is uniformly mixed.Respectively with the light of 1~3mm
Amount magnesia particle is coarse granule, and 0.1~1mm light weights spinelle is middle particle, with magnesia powder, graphite fine powder and alumina powder
For base portion dispensing, coarse granule:Middle particle:Fine powder ratio is 40:20:40.Wherein fine fraction alumina powder and oxidation
The ratio of magnesium and graphite mixed powder is 3:1.Using phenolic resin ethylene glycol solution as bonding agent, addition is dispensing total weight
8%, dispensing after sufficiently mixing, is placed in ageing mixture 4 hours in closed container or polybag；Material after ageing mixture is using half
Dry method is molded on a hydraulic press, briquetting pressure 150MPa, sample after drying, sample nature air dry half a day of forming to 1 day,
Then it in drying equipment, is dried using stage heating and heat preserving mode, finally keeps the temperature 24 hours at 110 DEG C；After drying
Molding sample is put into controlled atmosphere generator, and Ar protections are filled after vacuumizing, are heated to starting to keep the temperature, and be passed through O at 1600 DEG C2, O2Stream
Speed is 250L/h (oxygen gas flow rate can how many according to sample and size adjusts), keeps the temperature 4 hours, it is brilliant to obtain periclase-point
Stone light weight refractory material.Sample performance is shown in Table 3.
Table 3：The performance of 3 square magnesium stone-spinel light weight refractory material of example
Embodiment 4：
By 180 mesh fused magnesites and 180 mesh graphite, by MgO and C molar ratios 1:1 is uniformly mixed.Respectively with 0.1~3mm
Light weight spinel particle be aggregate.Using magnesia powder, graphite fine powder and alumina powder as base portion dispensing, aggregate:Carefully
Powder ratio is 50:50.Wherein the ratio of fine fraction alumina powder and magnesia and graphite mixed powder is 3:1.With phenolic aldehyde tree
Fat ethylene glycol solution is the 10% of dispensing total weight as bonding agent, addition, and dispensing after sufficiently mixing, is placed in closed container
Or ageing mixture 4 hours in polybag；Material after ageing mixture is molded on a hydraulic press using semidry method, briquetting pressure 150MPa,
Sample nature air dry half a day of forming to 1 day, then in drying equipment, is done using stage heating and heat preserving mode
It is dry, finally 24 hours are kept the temperature at 110 DEG C；Dry aftershaping sample firing is filled Ar protections, is heated in atmosphere furnace after vacuumizing
Start to keep the temperature at 1600 DEG C, and be passed through O2, O2Flow velocity is that (oxygen gas flow rate can and size tune how many according to sample by 250L/h
It is whole), 4 hours are kept the temperature, obtains square magnesium stone-spinel light weight refractory material.Sample performance is shown in Table 4.
Table 4：4 square magnesium stone-spinel light weight capabilities of refractory materials of example
Claims (5)
1. a kind of preparation method of square magnesium stone-spinel light weight refractory material, which is characterized in that including following preparation steps：
Step 1 chooses magnesia and carbon as reaction raw materials, raw material is milled down to 180 mesh hereinafter, according to MgO and C molar ratios 1:1
It is uniformly mixed, as the pore-creating in fine powder in refractory material dispensing and reaction component；
Raw material for refractory is carried out the ratio of dispensing, aggregate fraction and fine fraction by step 2 according to certain grain composition
It is 50~80:Between 20~50, wherein fine fraction is spinelle fine powder and step 1 mixes MgO and C powders, according to system
Product requirement, MgO the and C powders account for the 20%~70% of fine fraction；Fine fraction needs blending 30 minutes to 90 minutes,
So that each component is uniformly mixed；
Step 3 mixes 2~5 minutes according to aggregate fraction is first added in, and adds phenolic resin dilution and mixes 3~5 minutes, then
Fine fraction is added in, is mixed 5~20 minutes, incorporation time was amounted at 20~30 minutes in mixing machine；Mixed material is put
Ageing mixture 2 hours to 6 hours in closed container or polybag；
Step 4, the material after ageing mixture are pressed into definite shape using semi-dry pressing；
Step 5 by sample nature air dry half a day of forming to 1 day, then in drying equipment, is heated up and is protected using the stage
Warm mode is dried, and finally keeps the temperature 6 hours to 24 hours at 110 DEG C；
Step 6, dry aftershaping sample firing carries out in controlled atmosphere generator, first to controlled atmosphere stove evacuation, Ran Houchong
Enter Ar as protective gas, furnace body is heated to 1450 DEG C~1650 DEG C, reaches and is kept the temperature, and be passed through in the temperature range
O2, control and be passed through O2Flow velocity ensures that the Mg steam reactions of carbothermic reduction reaction generation are complete, and molding sample is obtained by reaction-sintered
It obtains with the square magnesium stone-spinel light weight refractory material compared with low bulk density and higher-strength；
The aggregate be light weight magnesia particle, light weight spinel particle, fine and close spinel particle, magnesite clinker, fused magnesite or
Their mixture of person.
2. the method as described in claim 1, which is characterized in that the magnesia is magnesite clinker or fused magnesite.
3. the method as described in claim 1, which is characterized in that the carbon is carbon black, graphite, coke or coal dust.
4. square magnesium stone-spinel light weight refractory material prepared by one of claims 1 to 3 the method.
5. square magnesium stone-spinel light weight refractory material as claimed in claim 4, which is characterized in that the square magnesium stone-spinel is light
Refractory material is measured with density gradient from outside to inside, outside is dense outer layer, and internal porous, dense outer layer assign material and resist
Working media infiltrates, and internal porous assigns material insulation.
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| CN114933473A (en) * | 2022-06-20 | 2022-08-23 | 西安建筑科技大学 | Spinel-corundum light-weight refractory material and preparation method thereof |
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| CN101747068A (en) * | 2009-12-24 | 2010-06-23 | 中钢集团洛阳耐火材料研究院有限公司 | Self-bonding SiC product with content of SiC more than 92 percent and preparation method thereof |
| CN103864434A (en) * | 2014-02-21 | 2014-06-18 | 武汉科技大学 | Lightweight periclase-magnesium aluminate spinel refractory material for rotary cement kiln and preparation method thereof |
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2016
- 2016-03-24 CN CN201610172527.1A patent/CN105837242B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1704383A (en) * | 2004-06-02 | 2005-12-07 | 武汉科技大学 | Mg-Al light thermal-insulated fireproof materials and method for preparing same |
| CN101066877A (en) * | 2007-06-07 | 2007-11-07 | 武汉科技大学 | Periclase-ferroalumina spinal brick and its making process |
| CN101423412A (en) * | 2008-11-27 | 2009-05-06 | 中钢集团洛阳耐火材料研究院有限公司 | Method for preparing high performance silicon oxide combining silicon carbide refractory by low-temperature sintering |
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| CN103864434A (en) * | 2014-02-21 | 2014-06-18 | 武汉科技大学 | Lightweight periclase-magnesium aluminate spinel refractory material for rotary cement kiln and preparation method thereof |
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