CN103011884B - Preparation method of corundum/mullite light-weight heat insulating material - Google Patents
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Abstract
The invention belongs to the technical field of heat insulating material preparation, and particularly relates to a preparation method of a corundum/mullite light-weight heat insulating material, which comprises the following steps: by using ceramic powder, silica sol, deionized water, ammonia water and dryness-control chemical additive as initial raw materials, carrying out ball milling to prepare a ceramic slurry; adding a foaming agent into the ceramic slurry, and foaming in a mechanical stirring mode to obtain a foam slurry; adding an NH4Cl solution into the foam slurry while stirring, injecting the uniformly stirred foam slurry into a mold, and quickly curing to form the foam slurry; and drying the demolded blank, and firing to obtain the corundum/mullite light-weight heat insulating material. The invention is characterized in that the gelation reaction of the silica sol is utilized to implement curing and formation of the foam slurry; meanwhile, the volume expansion generated by mullitization in the firing process is utilized to avoid sample cracking due to excessive sintering shrinkage; and in addition, the raw materials are nontoxic and cheap, and the preparation process is simple to control and suitable for industrial production.
Description
Technical field
The invention belongs to light heat-insulating material preparing technical field, be specifically related to a kind of preparation method of corundum-mullite light heat-insulating material.
Background technology
Day by day exhausted along with the energy, there are higher requirement in country and enterprise to energy-saving and cost-reducing in production process.In the Thermal Equipment such as Industrial Stoves, high-temperature electric resistance furnace, use light heat-insulating material to be a kind of simple and effective method that can significantly save energy and reduce the cost.Wherein with the corundum-mullite complex phase light heat-insulating material that corundum and mullite are principal crystalline phase, have the good characteristic of two kinds of materials concurrently, having that void content is high, thermal conductivity is low, thermal shock resistance is excellent, resistance to elevated temperatures is good and the advantage such as thermal expansivity is little, is one of more satisfactory middle high-temperature energy-conservation material.As the corundum-mullite series light heat-insulation brick of J. P. Morgan & Co. of Britain exploitation, maximum operation (service) temperature is from 1650 DEG C to 1760 DEG C.
The typical pore forming method preparing light heat-insulating material at present has interpolation pore-forming material method and foaming.Adding pore-forming material method is by adding pore-forming material (as graphite, starch, sawdust, polystyrene spheres etc.) in ceramic batch, utilize pore-forming material in base substrate, occupy certain space, after oversintering, pore-forming material leaves matrix and forms pore to obtain light heat-insulating material.A kind of preparation method of light high-alumina insulating firebrick of the patent disclosure of publication number CN 101768005A, with bauxite chamotte and kaolin for raw material, with poly-light ball and sawdust for pore-forming material, has prepared light fire brick.The preparation method that patent discloses a kind of corundum-mullite light brick of publication number CN 102381880A, with alumine, α-Al
2o
3micro mist, aluminium dihydrogen phosphate are raw material, be pore-forming material, prepared light heat-insulation brick with polystyrene spheres.The shortcoming of this technique is that goods inner air vent size is uneven, gas cell distribution is uneven and void content is on the low side, and then causes that product strength is lower, thermal conductivity is higher.Foaming is in ceramic composition, add organic or Inorganic chemical substance and whipping agent, during processing, form volatile gases, produces foam, drying and burn till obtained light porous ceramic.Foaming more easily controls shape and the density of goods, and article construction is evenly distributed, to close porosity high, is particularly suitable for preparing light heat-insulating material.
Simple and one of foam process of practicality by whipping agent mechanical foaming in ceramic size.But because bubble is thermodynamics unsteady state, in ceramic size, the floating of meeting bubbling is discharged, is combined the phenomenon becoming the instability such as large and Ostwald ripening, therefore the key of foaming is to realize solidifying the quick in situ of bubble in conjunction with in-situ consolidation forming technology.Document " Gel-casting process prepares mullite foamed ceramics " (" University Of Tianjin's journal ", 41st volume, 12nd phase) and patent CN 101591175A employing Gel-casting process, on the basis of ceramic size foaming, prepare the light ceramics of high porosity by the in-situ polymerization solidification of organic monomer.Applied widely to raw material of Gel-casting process, the blank strength of preparation is high.But its use organic monomer there is certain toxicity, to HUMAN HEALTH and environmental protection unfavorable; And base substrate binder removal is complicated, sintering shrinkage large, easily causes the cracking of goods.
Sol-gel moulding process is as a kind of novel colloidal formation technique, and it utilizes colloidal sol to the transformation of gel to realize the consolidation in-situ forming of slurry.In inorganic sol, silicon sol mature preparation process, cost are low; Gelation reaction is more easy to control; More stable, good with the matching of ceramic size (iso-electric point is partial to acidity) in the basic conditions, be most widely used.The people (J.Am.Ceram.Soc.73 (1): 85-90 such as Takamitsu Fujiu, 1990) foamed by freonll-11 in silicon sol, dodecyl sulphonic acid sodium stabilise bubbles, the gelation reaction of silicon sol is utilized to fix foam, obtained fumed silica after foams drying, sintering.The people (Journal of Porous Materials 11:107-115,2004) such as Takahiro Tomita take silicon sol as raw material, and sodium laurate sulfuric ester is whipping agent, by sol gel reaction in conjunction with the standby foam silicon-dioxide of mechanical foaming legal system.The shortcoming of the method described in above document foams in silicon sol, only relies on nano-silicon dioxide particle to enclose hole, its drying cycle long (more than 30 days) and dry difficulty, easy to crack, and be difficult to prepare the sample with standard brick size, actual application value is not high.
Summary of the invention
The object of the invention is to the preparation method proposing a kind of corundum-mullite light heat-insulating material, what adopt is the mode that sol-gel moulding process is combined with foaming, and its principle utilizes the gelation reaction of silicon sol to realize the fast curing-formed of foamed slurry.
For reaching goal of the invention the technical solution used in the present invention be: first ceramic powder, silicon sol, deionized water and drying control chemical additive are prepared burden, prepare slurry by the mode of ball milling; In ceramic size, add whipping agent again, adopt churned mechanically mode to carry out foaming and obtain foamed slurry; NH is added in the most backward foamed slurry
4cl solution, as setting accelerator, injects mould after stirring, foamed slurry curing molding; Base substrate drying after the demoulding, burn till after obtain corundum-mullite light heat-insulating material, the method comprises following steps successively:
(1) silicon sol of the deionized water of ceramic powder, ceramic powder quality 0 ~ 15%, ceramic powder quality 35 ~ 50%, the drying control chemical additive of ceramic powder quality 0.2 ~ 0.6% are prepared burden, regulated the pH value of slurry by ball milling mixing and ammoniacal liquor, obtain the slurry of pH=9 ~ 10;
(2) slurry that step (1) obtains is moved in agitation vat, add the whipping agent of free-water quality 5 ~ 10% in slurry, obtain foamed slurry by mechanical stirring foaming, then in foamed slurry, add NH while stirring
4cl solution, controls the NH in foamed slurry
4the concentration of Cl is 0.08 ~ 0.12mol/L, and the foamed slurry after stirring injects mould, and foamed slurry is fast curing-formed;
(3) by successively dry in climatic chamber and electric drying oven with forced convection for the green compact obtained after step (2) foamed slurry curing molding; Dried base substrate obtains corundum/mullite porous ceramic after high temperature burns till.
The median size of described ceramic powder is not more than 20 μm.
Described ceramic powder is the one in following ceramic powder or composite ceramic material; 1. alumina powder, 2. mass ratio are the alumina powder of 5:1 and the alumina powder of the composite ceramic material of fine silica powder, 3. mass ratio 5:1 and the composite ceramic material of sillimanite powder, 4. mass ratio is the alumina powder of 5:1 and the composite ceramic material of andaluzite powder.
Described silicon sol is ammonium ion stable form or sodium ion stable form, and its silica concentration is 20 ~ 30wt%.
Described drying control chemical additive is any one in methane amide, ethylene glycol, Glacial acetic acid.
Described whipping agent be in sodium lauryl sulphate, Sodium dodecylbenzene sulfonate, dodecyl sulphate amine, dodecyltriethanolamine sulfate in a kind of or several with the mixture of any mass ratio arbitrarily.
The curing molding of described foamed slurry is realized by the gelation reaction of silicon sol.
Described drying system is: base substrate carries out dry temperature in climatic chamber and relative humidity controls at 40 ~ 60 DEG C, 60 ~ 80% respectively, and the time length is 24 ~ 60h; In electric drying oven with forced convection, carry out dry temperature controls at 60 ~ 100 DEG C, and the time length is 18 ~ 48h.
Described firing temperature is 1500 DEG C ~ 1700 DEG C, and soaking time is 3 ~ 5 hours.
Advantage of the present invention
(1) quick in situ utilizing the gelation reaction of inorganic sol to realize foamed ceramics slurry solidifies, and the slurry curing time is by NH
4the concentration of Cl controls, and technological process is simple and easy to control.
(2) technological process is introduced without toxic substance, to HUMAN HEALTH and environmental protection favourable.
(3) utilize technique of the present invention, shaping base substrate inner homogeneous is good, dry shrinkage is little, without the need to the volumetric expansion that binder removal utilizes mullitization to produce simultaneously in sintering process, avoids the excessive sample cracking caused of sintering shrinkage.
(4) the Nano particles of silicon dioxide activity introduced by silicon sol is high, can produce liquid phase acceleration of sintering at sintering process, improves the compactness extent of hole wall, reduces sintering temperature.
Accompanying drawing explanation
Fig. 1 and Fig. 2 is respectively photomacrograph and the microstructure photograph of corundum/mullite light heat-insulating material that embodiment 1 obtains.
Embodiment
Below in conjunction with specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in this:
Embodiment 1
Be the alumina powder of 5.0 μm, the deionized water of alumina powder quality 15%, the sodium ion stabilized silica sol (SiO of alumina powder quality 35% by median size
2mass concentration is 30wt.%, and Shangyu, Zhejiang Yu Da Chemical Co., Ltd. produces), the methane amide of alumina powder quality 0.4% is prepared burden, and is regulated the pH value of slurry, obtain the slurry of pH=9 ~ 10 by ball milling mixing and ammoniacal liquor.The slurry be mixed to get by ball milling is transferred in agitation vat, adds the sodium lauryl sulphate of free-water quality 5% in slurry, obtains foamed slurry, then in foamed slurry, add NH while stirring by mechanical stirring foaming
4cl solution, controls the NH in foamed slurry
4the concentration of Cl is 0.10mol/L, and the foamed slurry after stirring injects mould, and foamed slurry is fast curing-formed; Base substrate first dry 36h in climatic chamber after the demoulding, temperature and relative humidity control at 60 DEG C and 80% respectively; 100 DEG C of insulation 18h in rear immigration electric drying oven with forced convection.Dried base substrate is put into electric furnace and is risen to 1600 DEG C with the temperature rise rate of 2 DEG C/min and be incubated 5h, is fired into corundum/mullite porous ceramic.The porosity of gained porous ceramics is 75%, and ultimate compression strength is 40MPa, and the thermal conductivity 1000 DEG C time is 0.598W/ (mK).The photomacrograph of gained sample and microstructure photograph are respectively as depicted in figs. 1 and 2.
Embodiment 2
Be the alumina powder of 1.5 μm, the deionized water of alumina powder quality 15%, the sodium ion stabilized silica sol (SiO of alumina powder quality 50% by median size
2mass concentration is 30wt.%, and Shangyu, Zhejiang Yu Da Chemical Co., Ltd. produces), the methane amide of alumina powder quality 0.6% is prepared burden, and is regulated the pH value of slurry, obtain the slurry of pH=9 ~ 10 by ball milling mixing and ammoniacal liquor.The slurry be mixed to get by ball milling is transferred in agitation vat, adds the Sodium dodecylbenzene sulfonate of free-water quality 10% in slurry, obtains foamed slurry, then in foamed slurry, add NH while stirring by mechanical stirring foaming
4cl solution, controls the NH in foamed slurry
4the concentration of Cl is 0.08mol/L, and the foamed slurry after stirring injects mould, and foamed slurry is fast curing-formed; Base substrate first dry 60h in climatic chamber after the demoulding, temperature and relative humidity control at 40 DEG C and 60% respectively; After to be moved in electric drying oven with forced convection 60 DEG C of insulation 48h.Dried base substrate is put into electric furnace and is risen to 1500 DEG C with the temperature rise rate of 2 DEG C/min and be incubated 5h, is fired into corundum/mullite porous ceramic.
Embodiment 3
Be the alumina powder of 5.0 μm, the deionized water of alumina powder quality 10%, the ammonium ion stabilized silica sol (SiO of alumina powder quality 40% by median size
2mass concentration is 20wt.%, and Shangyu, Zhejiang Yu Da Chemical Co., Ltd. produces), the ethylene glycol of alumina powder quality 0.2% is prepared burden, and is regulated the pH value of slurry, obtain the slurry of pH=9 ~ 10 by ball milling mixing and ammoniacal liquor.The slurry be mixed to get by ball milling is transferred in agitation vat, adds the ammonium lauryl sulfate of free-water quality 8% in slurry, obtains foamed slurry, then in foamed slurry, add NH while stirring by mechanical stirring foaming
4cl solution, controls the NH in foamed slurry
4the concentration of Cl is 0.12mol/L, and the foamed slurry after stirring injects mould, and foamed slurry is fast curing-formed; Base substrate first dry 24h in climatic chamber after the demoulding, temperature and relative humidity control at 50 DEG C and 70% respectively; After to be moved in electric drying oven with forced convection 80 DEG C of insulation 36h.Dried base substrate is put into electric furnace and is risen to 1650 DEG C with the temperature rise rate of 2 DEG C/min and be incubated 3h, is fired into corundum/mullite porous ceramic.
Embodiment 4
Composite ceramic material, the deionized water of ceramic powder quality 5%, the ammonium ion stabilized silica sol (SiO of ceramic powder quality 45% of to be the alumina powder of 19.3 μm and median size by median size the be fine silica powder of 3.5 μm
2mass concentration is 30wt.%), the ethylene glycol of ceramic powder quality 0.5% is prepared burden, and is regulated the pH value of slurry, obtain the slurry of pH=9 ~ 10 by ball milling mixing and ammoniacal liquor.The slurry be mixed to get by ball milling is transferred in agitation vat, add the mixture of the sodium lauryl sulphate of free-water quality 5% in slurry, dodecyl sulphate amine and Sodium dodecylbenzene sulfonate, obtain foamed slurry by mechanical stirring foaming, then in foamed slurry, add NH while stirring
4cl solution, controls the NH in slurry
4the concentration of Cl is 0.10mol/L, and the foamed slurry after stirring injects mould, and foamed slurry is fast curing-formed; Base substrate first dry 24h in climatic chamber after the demoulding, temperature and relative humidity control at 50 DEG C and 70% respectively; After to be moved in electric drying oven with forced convection 80 DEG C of insulation 36h.Dried base substrate is put into electric furnace and is risen to 1700 DEG C with the temperature rise rate of 2 DEG C/min and be incubated 3h, is fired into corundum/mullite porous ceramic.
Embodiment 5
Be alumina powder and the median size of 19.3 μm by median size be the composite ceramic material of the sillimanite powder of 4.9 μm, the ammonium ion stabilized silica sol (SiO of ceramic powder quality 50%
2mass concentration is 25wt.%, and Shangyu, Zhejiang Yu Da Chemical Co., Ltd. produces), the Glacial acetic acid of ceramic powder quality 0.5% is prepared burden, and is regulated the pH value of slurry, obtain the slurry of pH=9 ~ 10 by ball milling mixing and ammoniacal liquor.The slurry be mixed to get by ball milling is transferred in agitation vat, adds the dodecyl trolamine of free-water quality 10% in slurry, obtains foamed slurry, then in foamed slurry, add NH while stirring by mechanical stirring foaming
4cl solution, controls the NH in slurry
4the concentration of Cl is 0.10mol/L, and the foamed slurry after stirring injects mould, and foamed slurry is fast curing-formed; Base substrate first dry 24h in climatic chamber after the demoulding, temperature and relative humidity control at 50 DEG C and 70% respectively; After to be moved in electric drying oven with forced convection 80 DEG C of insulation 36h.Dried base substrate is put into electric furnace and is risen to 1700 DEG C with the temperature rise rate of 2 DEG C/min and be incubated 3h, is fired into corundum/mullite porous ceramic.
Embodiment 6
Be alumina powder and the median size of 10.6 μm by median size be the composite ceramic material of the andaluzite powder of 18.9 μm, the ammonium ion stabilized silica sol (SiO of ceramic powder quality 50%
2mass concentration is 25wt.%, and Shangyu, Zhejiang Yu Da Chemical Co., Ltd. produces), the Glacial acetic acid of ceramic powder quality 0.5% is prepared burden, and is regulated the pH value of slurry, obtain the slurry of pH=9 ~ 10 by ball milling mixing and ammoniacal liquor.The slurry be mixed to get by ball milling is transferred in agitation vat, add the dodecyltriethanolamine sulfate of free-water quality 5% in slurry and the mixture of dodecyl sulphate amine, obtain foamed slurry by mechanical stirring foaming, then in foamed slurry, add NH while stirring
4cl solution, controls the NH in slurry
4the concentration of Cl is 0.10mol/L, and the foamed slurry after stirring injects mould, and foamed slurry is fast curing-formed; Base substrate first dry 24h in climatic chamber after the demoulding, temperature and relative humidity control at 50 DEG C and 70% respectively; After to be moved in electric drying oven with forced convection 80 DEG C of insulation 36h.Dried base substrate is put into electric furnace and is risen to 1700 DEG C with the temperature rise rate of 2 DEG C/min and be incubated 3h, is fired into corundum/mullite porous ceramic.
Claims (3)
1. a preparation method for corundum-mullite light heat-insulating material, is characterized in that: ceramic powder, silicon sol and drying control chemical additive are prepared burden by described preparation method, prepare slurry by the mode of ball milling; In ceramic size, add whipping agent again, adopt churned mechanically mode to carry out foaming and obtain foamed slurry; NH is added in the most backward foamed slurry
4cl solution, as setting accelerator, injects mould after stirring, foamed slurry curing molding, and the curing molding of described foamed slurry is realized by the gelation reaction of silicon sol; Base substrate drying after the demoulding, burn till after obtain corundum/mullite light heat-insulating material, the method comprises following steps successively:
(1) silicon sol of the deionized water of ceramic powder, ceramic powder quality 0 ~ 15%, ceramic powder quality 35 ~ 50%, the drying control chemical additive of ceramic powder quality 0.2 ~ 0.6% are prepared burden, regulated the pH value of slurry by ball milling mixing and ammoniacal liquor, obtain the slurry of pH=9 ~ 10;
(2) slurry that step (1) obtains is moved in agitation vat, add the whipping agent of free-water quality 5 ~ 10% in slurry, obtain foamed slurry by mechanical stirring foaming, then in foamed slurry, add NH while stirring
4cl solution, controls the NH in foamed slurry
4the concentration of Cl is 0.08 ~ 0.12mol/L, and the foamed slurry after stirring injects mould, and foamed slurry is fast curing-formed;
(3) by successively dry in climatic chamber and electric drying oven with forced convection for the green compact obtained after step (2) foamed slurry curing molding; Dried base obtains corundum/mullite porous ceramic after high temperature burns till;
Wherein, described silicon sol is ammonium ion stable form or sodium ion stable form, SiO in silicon sol
2content is 20 ~ 30wt.%; Described whipping agent is a kind of or several with the mixture of any mass ratio arbitrarily in sodium lauryl sulphate, Sodium dodecylbenzene sulfonate, ammonium lauryl sulfate, dodecyltriethanolamine sulfate; Described drying control chemical additive is any one in methane amide, ethylene glycol, Glacial acetic acid; Base substrate carries out dry temperature in climatic chamber and relative humidity controls at 40 ~ 60 DEG C, 60 ~ 80% respectively, and the time length is 24 ~ 60h; In electric drying oven with forced convection, carry out dry temperature controls at 60 ~ 100 DEG C, and the time length is 18 ~ 48h; Firing temperature is 1500 DEG C ~ 1730 DEG C, and soaking time is 3 ~ 5 hours.
2., by the preparation method of a kind of corundum-mullite light heat-insulating material according to claim 1, it is characterized in that: the median size of described ceramic powder is not more than 20 μm.
3. by the preparation method of a kind of corundum-mullite light heat-insulating material described in claim 1 or 2, it is characterized in that: described ceramic powder is the one in following ceramic powder or composite ceramic material; 1. alumina powder, 2. mass ratio are the alumina powder of 5:1 and the alumina powder of the composite ceramic material of fine silica powder, 3. mass ratio 5:1 and the composite ceramic material of sillimanite powder, 4. mass ratio is the alumina powder of 5:1 and the composite ceramic material of andaluzite powder.
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| CN1318348C (en) * | 2005-11-14 | 2007-05-30 | 浙江大学 | Tech. for degassing-free gel injecting moulding shaping of mullite-base precision ceramic component |
| CN102659427A (en) * | 2012-04-25 | 2012-09-12 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method for light refractory raw material |
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Inventor after: Li Hongxia Inventor after: Wang Gang Inventor after: Cao Hehui Inventor after: Yuan Bo Inventor after: Wu Haibo Inventor after: Han Jianshen Inventor before: Wang Gang Inventor before: Cao Hehui Inventor before: Li Hongxia Inventor before: Yuan Bo Inventor before: Wu Haibo Inventor before: Han Jianshen |