CN101921113A - Composite material of silicon carbide mullite heat accumulator and preparation method thereof - Google Patents
Composite material of silicon carbide mullite heat accumulator and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a composite material of a silicon carbide mullite heat accumulator and a preparation method thereof. The composite material is prepared from the following raw materials with the total amount of 100%: 75%-85% of black silicon carbide powder, 14%-20% of mullite powder, 1%-3% of metallic silicon powder, 1%-4% of andalusite powder and 1%-4% of kaolin with the addition of hydroxy propyl cellulose, tung oil, glycerol and water. The preparation method comprises the following steps: firstly, ball-milling the black silicon carbide powder and adding and dry-mixing auxiliary materials; then, adding the hydroxy propyl cellulose, tung oil, glycerol and water, wet-mixing, staling and pugging; and extrusion-molding, drying the blank until the water content thereof is lower than or equal to 2%, charging and sintering at 1,350 DEG C. The composite material of the invention has the advantages of high material density and low unit weight, increases the heat accumulation capacity and reduces the size of the heat accumulation chamber; the composite material, owing to the high strength thereof, can meet the requirements of larger heat accumulation chambers for loading at high temperature; the composite material has the advantages of even expansion, good thermal-shock stability and high softening point under load when being heated; and the composite material further has the advantages of low high-temperature creep value, high rigidity, good resistance to chemical corrosion, high heat conductivity and good anti-oxidation effect. Therefore, the composite material is particularly suitable for the occasions with harsh environment and severe oxidation corrosion in the heat accumulation chamber.
Description
One, technical field:
The present invention relates to a kind of heat-storage type burner parts, particularly relate to a kind of composite material of silicon carbide mullite heat accumulator and preparation method thereof.
Two, background technology:
Heat accumulating type high-temperature air burning (being called for short HTAC) is one and has energy-conservation and the novel combustion technology environmental protection double effects, heat storage is the key part of heat-storage type burner, be widely used in iron and steel, machinery, building materials, the various process furnace of industry such as petrochemical industry and non-ferrous metal metallurgy, hotblast stove, heat treatment furnace, pyrolyzer, roaster, thawing furnace, in the kilns such as homogenizing furnace and oil gas boiler, this technology is passed through reversing system, make the heat release of alternately absorbing heat of two regenerator, reclaim the heat in the flue gas to greatest extent, again combustion air and coal gas are heated to more than 1000 ℃, even low-calorie inferior fuel (as blast furnace gas) also can be realized stable ignition and efficient burning, but fuel saving 40-70%, output improves more than 15%, billet oxidization burning loss descends more than 40%, oxynitride (NO
X) quantity discharged is less than 100ppm, smog discharge temperature is lower than 160 ℃, helps reducing the Greenhouse effect of the earth greatly.If national most of Industrial Stoves all adopt the HTAC technology, its economic benefit and social benefit are inestimable, will greatly alleviate the energy scarcity situation, effectively improve existent environment of people.
The HTAC technology needs the main the following aspects of considering: the heat storage capacity of heat storage, heat transfer rate, thermal shock resistance, oxidation-resistance, corrodibility, the pressure-losses and economy etc.The work-ing life of present domestic honeycomb is lower, and the honeycomb of process furnace was generally 3～6 months work-ing life, even occurs using once a large amount of cracked situations of week, and the heat storage that is used on the ladle baking facility increases because of flue-gas temperature low work-ing life to some extent.The problem that heat storage in use often occurs mainly contains: melt, soften, break, obstruction and corrosion etc., wherein the anti-thermal shock poor stability of heat storage material is the problem of the most normal appearance.Cause the reason of above problem to mainly contain following 3 points:
(1) problem of materials: the honeycomb long term operation be at rapid heat cycle, also may have in the severe environment of corrosive gases, often bears high temperature and inside and outside difference variation and the stress that causes.This Working environment has proposed harsh requirement to the heat storage material.In order to increase heat storage capacity, reduce the volume of regenerator, need to increase the density of heat storage.But anti-thermal shock stability is mutually exclusive to a certain extent with density, and promptly density is high more, and anti-thermal shock stability is poor more.In use, heat storage and air-flow carry out heat exchange, and some have corrosive gas and particle has a negative impact to honeycomb.Such as, ferric oxide particles can reduce the reflowing temperature of aluminium silicon material, makes honeycomb fusing and blocks pore; Sour gas is known from experience honeycomb generation corrosive nature; Molecule can stop up gas passage etc. attached to the honeycomb surface.
(2) bias current problem: heat exchanging process is roughly as follows in the regenerator: in the smoke evacuation stage, flue gas flow is stored in sensible heat in the honeycomb when honeycomb, the heating honeycomb; At combustion phases, air (or coal gas) is heated when flowing through honeycomb, and waste heat is taken back in the stove again.In above arbitrary stage,, after several times commutations, cause honeycomb localized hyperthermia easily and produce thermal stresses if bias current appears in gas in regenerator.When the thermal stress that produces exceeded it and bears the limit, honeycomb will break.
(3) " secondary combustion " problem: the air jet of regenerative combustion system and gas port generally all are separate, help forming hypoxic atmosphere in the stove like this, expand flame edge, form the uniform temperature field, improve the discharging of heating quality and minimizing oxynitride.But the optimum value of air and coal gas two bursts of effusive speed, the angle of cut and distances is difficult to hold, and deal with improperly and then cause the interior local gas-fired of stove insufficient easily, and other local oxygen also has residue.These flue gases are when being inhaled into regenerator, and air can contact generation " secondary combustion " again with coal gas, and liberated heat can be absorbed by honeycomb fully, although do not cause power loss, localized hyperthermia is easy to make the honeycomb fusing and lost efficacy.
Three, summary of the invention:
The technical problem to be solved in the present invention: a kind of heat storage capacity height, intensity height, thermal shock resistance height, composite material of silicon carbide mullite heat accumulator that resistance to chemical corrosion is good are provided;
The preparation method of this composite material of silicon carbide mullite heat accumulator also is provided.
Technical scheme of the present invention:
A kind of composite material of silicon carbide mullite heat accumulator, form by following weight percentages: black silicon carbide powder 75-85%, mullite powder 14-20%, metallic silicon power 1-3%, andaluzite powder 1-4%, kaolin 1-4%, the above-mentioned raw materials total amount is 100%; Add the hydroxypropylcellulose that accounts for above-mentioned raw materials 3-5%, the tung oil of 4-6%, the glycerine 1-3% of 1-3% and the water of 15-18%.
Described black silicon carbide powder comprises 150 purpose black silicon carbide powder 22-27%, 250 purpose black silicon carbide powder 37-42%, 325 purpose black silicon carbide powder 12-17%; Described mullite powder is 14-18%, granularity 180-240 order; Described metallic silicon power is 1-1.5%, granularity 250 orders; Described andaluzite powder is 1-2%, granularity 180 orders; Described kaolin is 1-2%, granularity 200-220 order.
Described hydroxypropylcellulose is 3-4%, tung oil 4-5%, glycerine 1-1.5%, water 15-16%.
Described metallic silicon power requires: silicone content 〉=97%, calcium contents≤0.30%, iron level≤0.70%.
Described black silicon carbide is a refinery coke silicon carbide, wherein contains SiC 95-97%, and density is 3.2-3.25g/cm
3
The preparation method of described composite material of silicon carbide mullite heat accumulator may further comprise the steps,
Take by weighing raw material by prescription,, add auxiliary material mullite powder, metallic silicon power, andaluzite powder and kaolin major ingredient black silicon carbide sphere of powder mill 2-3h, do and mix 30-60min, add hydroxypropylcellulose, tung oil, G ﹠ W, wet mixing 1-1.5h, old 8-10h slightly refines mud at vacuum deairing machine; The mud bar that slightly refines behind the mud is cut into sheet, and old 4-5h carries out refining mud, and extrusion moulding dries blank to water content≤2%, and shove charge is burnt till at 1350 ℃.
Pressure is 14-16MPa during described moulding.
Described blank oven dry is carried out at twice, earlier with blank with microwave drying to water content≤10%, dry to water content≤2% under 300-350 ℃ with baking oven again.
Described firing temperature is designed to: be warming up to 400 ℃ by room temperature through 1h, be warming up to 600 ℃ through 1.5h, be warming up to 950 ℃ through 3h, be warming up to 1200 ℃ through 5h, be warming up to 1350 ℃ through 3h again, at 1350 ℃ of insulation 2h; Naturally cool to 200 ℃ then.
Positive beneficial effect of the present invention:
(1) products material compatibility of the present invention is reasonable, and consumption is fastidious, and product performance are good.Product material density is big, unit weight is little, can increase heat storage capacity, reduces the regenerator volume; The product strength height can adapt under the high temperature carriage requirement of big regenerator; Even, the good thermal shock stability of expansion when product is heated, the load softening point height; Product high temperature creep value is little, creep rate≤0.5% behind 1450 ℃, loading 0.2MPa, 48h; Product hardness is big, and resistance to chemical corrosion is good, and the thermal conductivity height has good antioxygenation simultaneously, is specially adapted to abominable, the comparatively serious occasion of regenerator oxidation corrosion of environment, and its long service life is than long 2～4 times of common mullite heat accumulator.
The Performance Detection index of product of the present invention is as following table 1.
(2) the inventive method adopts secondary drying technology, and microwave is adopted in oven dry for the first time, and baking oven is adopted in oven dry for the second time, can prevent the product distortion, helps again reducing cost; Adopt special firing temperature curve to burn till product, can effectively guarantee the quality and the stable performance of product.
(3) product of the present invention can effectively solve fusing that existing honeycomb heat accumulation body in use often occurs, soften, breaks and problem such as corrosion, product anti-thermal shock stability improves greatly, help the application of HTAC technology in Industrial Stoves, the situation of energy scarcity will be alleviated greatly, help improving environment for human survival, will produce better economic and social benefit.
Four, embodiment:
Embodiment 1: a kind of composite material of silicon carbide mullite heat accumulator, form by following weight percentages: 150 order black silicon carbide powder 22%, 250 order black silicon carbide powder 42%, 325 order black silicon carbide powder 12%, 180-240 order mullite powder 15%, 250 order metallic silicon powers 1%, 180 order andaluzite powder 4%, 200-220 order kaolin 4%, above-mentioned raw materials gross weight are 100%; Add the hydroxypropylcellulose that accounts for above-mentioned raw materials 3%, 4% tung oil, 3% glycerine, 15% water.
Wherein metallic silicon power requires: silicone content 〉=97%, calcium contents≤0.30%, iron level≤0.70%; Black silicon carbide is a refinery coke silicon carbide, wherein contains SiC 95-97%, Fe
2O
31-1.2%, density is 3.2-3.25g/cm
3
The preparation method of described composite material of silicon carbide mullite heat accumulator may further comprise the steps:
Take by weighing raw material by prescription and granularity requirements, with major ingredient black silicon carbide sphere of powder mill 2-3h, add auxiliary material mullite powder, metallic silicon power, andaluzite powder and kaolin, do and mix 30-60min, add hydroxypropylcellulose, tung oil, G ﹠ W, wet mixing 1-1.5h, old 8-10h slightly refines mud at vacuum deairing machine; Then the mud bar is cut into the old again 4-5h of sheet, carry out refining mud, extrusion moulding, forming pressure 14-16MPa is that the steel wire of 0.2-0.3mm cuts into blank with diameter, with blank with microwave drying to moisture mass content below 7%, dry to moisture mass content below 2% at 300-350 ℃ with baking oven again, with the diamond saw blade cutting, the floating powder of cleaning, shove charge is burnt till at 1350 ℃.
Temperature design is when burning till: be warming up to 400 ℃ by room temperature through 1h, be warming up to 600 ℃ through 1.5h again, be warming up to 950 ℃ through 3h again; Be warming up to 1200 ℃ through 5h, be warming up to 1350 ℃ through 3h, at 1350 ℃ of insulation 2h, naturally cool to 200 ℃ then, kiln discharge obtains product.
Embodiment 2: the composite material of silicon carbide mullite heat accumulator raw material is formed: 150 purpose black silicon carbide powder 27%, 250 purpose black silicon carbide powder 37%, 325 purpose black silicon carbide powder 17%, 180-240 purpose mullite powder 14%, 250 purpose metallic silicon powers 3%, 180 purpose andaluzite powder 1%, 200-220 purpose kaolin 1%, above-mentioned raw materials gross weight are 100%; Add the hydroxypropylcellulose that accounts for above-mentioned raw materials 5%, 4% tung oil, 2% glycerine, 16% water.The performance requriements of described metallic silicon power and refinery coke silicon carbide is with embodiment 1.
Preparation method: take by weighing raw material by prescription and granularity requirements,, add mullite powder, metallic silicon power, andaluzite powder and kaolin with black silicon carbide sphere of powder mill 2h, do and mix 40min, add hydroxypropylcellulose, tung oil, G ﹠ W, wet mixing 1h, old 10h slightly refines mud at vacuum deairing machine; After thick white silk finishes the mud bar is cut into the old again 4-5h of sheet, carry out refining mud then, extrusion moulding, forming pressure 13-16MPa is that the steel wire of 0.2-0.3mm cuts into blank with diameter, with the blank microwave drying to water content below 9%, under 300 ℃, dry to water content below 2% with baking oven again, with the diamond saw blade cutting, the floating powder of cleaning, shove charge is burnt till at 1350 ℃.Temperature design is with embodiment 1 when burning till.
Embodiment 3: the composite material of silicon carbide mullite heat accumulator raw material is formed: 150 purpose black silicon carbide powder 25%, 250 purpose black silicon carbide powder 37%, 325 purpose black silicon carbide powder 13%, 180-240 purpose mullite powder 18%, 250 purpose metallic silicon powers 2%, 180 purpose andaluzite powder 3%, 200-220 purpose kaolin 2%, above-mentioned raw materials gross weight are 100%; Add the hydroxypropylcellulose that accounts for above-mentioned raw materials 4%, 5% tung oil, 2% glycerine, 16% water.The performance requriements of described metallic silicon power and refinery coke silicon carbide is with embodiment 1.
Preparation method: take by weighing raw material by prescription and granularity requirements, with black silicon carbide sphere of powder mill 2.5h, add mullite powder, metallic silicon power, andaluzite powder and kaolin, do and mix 30min, add hydroxypropylcellulose, tung oil, G ﹠ W, wet mixing 1.5h, old 8h slightly refines mud at vacuum deairing machine; After thick white silk finishes the mud bar is cut into the old again 4-5h of sheet, carry out refining mud then, extrusion moulding, forming pressure 12-15MPa is that the steel wire of 0.2-0.3mm cuts into blank with diameter, with the blank microwave drying to water content below 8%, under 320 ℃, dry to water content below 2% with baking oven again, with the diamond saw blade cutting, the floating powder of cleaning, shove charge is burnt till at 1350 ℃.Temperature design is with embodiment 1 when burning till.
Embodiment 4: the composite material of silicon carbide mullite heat accumulator raw material is formed: 150 purpose black silicon carbide powder 23%, 250 purpose black silicon carbide powder 39%, 325 purpose black silicon carbide powder 13%, 180-240 purpose mullite powder 20%, 250 purpose metallic silicon powers 1%, 180 purpose andaluzite powder 2%, 200-220 purpose kaolin 2%, above-mentioned raw materials gross weight are 100%; Add the hydroxypropylcellulose that accounts for above-mentioned raw materials 4%, 4% tung oil, 1% glycerine, 18% water.The performance requriements of described metallic silicon power and refinery coke silicon carbide is with embodiment 1.
Preparation method: take by weighing raw material by prescription and granularity requirements,, add mullite powder, metallic silicon power, andaluzite powder and kaolin with black silicon carbide sphere of powder mill 3h, do and mix 40min, add hydroxypropylcellulose, tung oil, G ﹠ W, wet mixing 1.2h, old 9h slightly refines mud at vacuum deairing machine; After thick white silk finishes the mud bar is cut into the old again 4-5h of sheet, carry out refining mud then, extrusion moulding, forming pressure 15-17MPa is that the steel wire of 0.2-0.3mm cuts into blank with diameter, with the blank microwave drying to water content below 8%, under 350 ℃, dry to water content below 2% with baking oven again, with the diamond saw blade cutting, the floating powder of cleaning, shove charge is burnt till at 1350 ℃.Temperature design is with embodiment 1 when burning till.
Embodiment 5: the composite material of silicon carbide mullite heat accumulator raw material is formed: 150 purpose black silicon carbide powder 26%, 250 purpose black silicon carbide powder 40%, 325 purpose black silicon carbide powder 15%, 180-240 purpose mullite powder 16%, 250 purpose metallic silicon powers 1%, 180 purpose andaluzite powder 1%, 200-220 purpose kaolin 1%, above-mentioned raw materials gross weight are 100%; Add the hydroxypropylcellulose that accounts for above-mentioned raw materials 3%, 4% tung oil, 3% glycerine, 17% water.The performance requriements of described metallic silicon power and refinery coke silicon carbide is with embodiment 1.
Preparation method: take by weighing raw material by prescription and granularity requirements, with major ingredient black silicon carbide sphere of powder mill 2h, add auxiliary material mullite powder, metallic silicon power, andaluzite powder and kaolin, do and mix 50min, add hydroxypropylcellulose, tung oil, G ﹠ W, wet mixing 1h, old 9h slightly refines mud at vacuum deairing machine; After thick white silk finishes the mud bar is cut into the old again 4-5h of sheet, carry out refining mud then, extrusion moulding, forming pressure 15-16MPa is that the steel wire of 0.2-0.3mm cuts into blank with diameter, with the blank microwave drying to water content below 10%, under 340 ℃, dry to water content below 2% with baking oven again, with the diamond saw blade cutting, the floating powder of cleaning, shove charge is burnt till at 1350 ℃.Temperature design is with embodiment 1 when burning till.
Embodiment 6: the raw material of composite material of silicon carbide mullite heat accumulator is formed: 150 purpose black silicon carbide powder 24%, 250 purpose black silicon carbide powder 38%, 325 purpose black silicon carbide powder 14%, 180-240 purpose mullite powder 19%, 250 purpose metallic silicon powers 2%, 180 purpose andaluzite powder 1%, 200-220 purpose kaolin 2%, above-mentioned raw materials gross weight are 100%; Add the hydroxypropylcellulose that accounts for above-mentioned raw materials 4%, 4% tung oil, 3% glycerine, 15% water.The performance requriements of described metallic silicon power and refinery coke silicon carbide is with embodiment 1.
Preparation method: take by weighing raw material by prescription and granularity requirements, with major ingredient black silicon carbide sphere of powder mill 3h, add auxiliary material mullite powder, metallic silicon power, andaluzite powder and kaolin, do and mix 60min, add hydroxypropylcellulose, tung oil, G ﹠ W, wet mixing 1h, old 8.5h slightly refines mud at vacuum deairing machine; After thick white silk finishes the mud bar is cut into the old again 4-5h of sheet, carry out refining mud then, extrusion moulding, forming pressure 14-16MPa is that the steel wire of 0.2-0.3mm cuts into blank with diameter, with the blank microwave drying to water content below 7%, under 300-350 ℃, dry to water content below 2% with baking oven again, with the diamond saw blade cutting, the floating powder of cleaning, shove charge is burnt till at 1350 ℃.Temperature design is with embodiment 1 when burning till.
Product in the foregoing description after testing, performance index all meet the parameter in the table 1.
Claims (9)
1. a composite material of silicon carbide mullite heat accumulator is characterized in that: be made up of following weight percentages: black silicon carbide powder 75-85%, mullite powder 14-20%, metallic silicon power 1-3%, andaluzite powder 1-4%, kaolin 1-4%, the above-mentioned raw materials total amount is 100%; Add the hydroxypropylcellulose that accounts for above-mentioned raw materials 3-5%, the tung oil of 4-6%, the glycerine 1-3% of 1-3% and the water of 15-18%.
2. composite material of silicon carbide mullite heat accumulator according to claim 1 is characterized in that: described black silicon carbide powder comprises 150 purpose black silicon carbide powder 22-27%, 250 purpose black silicon carbide powder 37-42%, 325 purpose black silicon carbide powder 12-17%; Described mullite powder is 14-18%, granularity 180-240 order; Described metallic silicon power is 1-1.5%, granularity 250 orders; Described andaluzite powder is 1-2%, granularity 180 orders; Described kaolin is 1-2%, granularity 200-220 order.
3. composite material of silicon carbide mullite heat accumulator according to claim 1 is characterized in that: described hydroxypropylcellulose is 3-4%, tung oil 4-5%, glycerine 1-1.5%, water 15-16%.
4. composite material of silicon carbide mullite heat accumulator according to claim 1 is characterized in that: described metallic silicon power requires: silicone content 〉=97%, calcium contents≤0.30%, iron level≤0.70%.
5. composite material of silicon carbide mullite heat accumulator according to claim 1 is characterized in that: described black silicon carbide is a refinery coke silicon carbide, wherein contains SiC 95-97%, and density is 3.2-3.25g/cm
3
6. the preparation method of the described composite material of silicon carbide mullite heat accumulator of claim 1, it is characterized in that: this method may further comprise the steps,
Take by weighing raw material by prescription,, add auxiliary material mullite powder, metallic silicon power, andaluzite powder and kaolin major ingredient black silicon carbide sphere of powder mill 2-3h, do and mix 30-60min, add hydroxypropylcellulose, tung oil, G ﹠ W, wet mixing 1-1.5h, old 8-10h slightly refines mud at vacuum deairing machine; The mud bar that slightly refines behind the mud is cut into sheet, and old 4-5h carries out refining mud, and extrusion moulding dries blank to water content≤2%, and shove charge is burnt till at 1350 ℃.
7. preparation method according to claim 6 is characterized in that: pressure is 14-16MPa during described moulding.
8. preparation method according to claim 6 is characterized in that: described blank oven dry is carried out at twice, earlier with blank with microwave drying to water content≤10%, dry to water content≤2% under 300-350 ℃ with baking oven again.
9. according to each described preparation method of claim 6-8, it is characterized in that: described firing temperature is designed to: be warming up to 400 ℃ by room temperature through 1h, be warming up to 600 ℃ through 1.5h, be warming up to 950 ℃ through 3h, be warming up to 1200 ℃ through 5h, be warming up to 1350 ℃ through 3h again, at 1350 ℃ of insulation 2h; Naturally cool to 200 ℃ then.
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| CN101798212A (en) * | 2010-01-29 | 2010-08-11 | 王献忠 | Honeycomb heat accumulator made of silicon carbide-corundum composite materials |
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2010
- 2010-08-17 CN CN2010102553792A patent/CN101921113B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US4993481A (en) * | 1988-10-03 | 1991-02-19 | The Agency Of Industrial Science And Technology | Thermal storage unit |
| US5281462A (en) * | 1989-11-01 | 1994-01-25 | Corning Incorporated | Material, structure, filter and catalytic converter |
| CN101125751A (en) * | 2007-05-23 | 2008-02-20 | 萍乡市中天化工填料有限公司 | Zirconium chromium corundum honeycomb ceramic heat accumulator |
| CN101628823A (en) * | 2009-07-24 | 2010-01-20 | 姚光纯 | Preparation method of corundum honeycomb ceramic with slag resistance |
| CN101798212A (en) * | 2010-01-29 | 2010-08-11 | 王献忠 | Honeycomb heat accumulator made of silicon carbide-corundum composite materials |
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