CN101913889B - Method for preparing mullite refractory material from aluminum plant sludge and pyrophyllite - Google Patents

Method for preparing mullite refractory material from aluminum plant sludge and pyrophyllite Download PDF

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CN101913889B
CN101913889B CN 201010265607 CN201010265607A CN101913889B CN 101913889 B CN101913889 B CN 101913889B CN 201010265607 CN201010265607 CN 201010265607 CN 201010265607 A CN201010265607 A CN 201010265607A CN 101913889 B CN101913889 B CN 101913889B
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agalmatolite
aluminum manufacturer
sludge
manufacturer sludge
aluminum
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CN101913889A (en
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罗学涛
傅翠梨
许庆水
李锦堂
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Xiamen University
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Abstract

The invention discloses a method for preparing a mullite refractory material from aluminum plant sludge and pyrophyllite, which relates to a refractory material. The method has a simple process and low cost and comprehensively uses solid wastes. The method comprises the following steps of: dryly milling the aluminum plant sludge and the pyrophyllite in a ball mill respectively; adding water into the ball mill and wetly milling the aluminum plant sludge and the pyrophyllite in the ball mill to obtain aluminum plant sludge-pyrophyllite mixed slurry; spraying the aluminum plant sludge-pyrophyllite mixed slurry into a prilling tower by using a sprayer for pulverization and drying to obtain aluminum plant sludge-pyrophyllite aggregates; molding the aluminum plant sludge-pyrophyllite aggregates in a hydraulic molding machine to obtain an aluminum plant sludge-pyrophyllite blank; drying the aluminum plant sludge-pyrophyllite blank to reduce sintering shrinkage and prevent sample cracking; and sintering the aluminum plant sludge-pyrophyllite blank and then cooling the sintered product to room temperature to obtain the mullite refractory material.

Description

A kind of method of utilizing aluminum manufacturer sludge and agalmatolite to prepare mullite refractory
Technical field
The present invention relates to a kind of refractory materials, especially relate to a kind of method of utilizing aluminum manufacturer sludge and agalmatolite to prepare mullite refractory.
Background technology
Along with developing rapidly of Alminum Project material, a large amount of aluminum alloy materials are put into the every field of production, life.For satisfying client's needs, alloy product generally need to pass through surface treatment, to improve rotproofness, the wear resistance of aluminium section bar, finally reaches the purpose of the surface quality that improves aluminium section bar.In each operations such as the degreasing of carrying out the aluminium shape surface processing, alkali cleaning, neutralization, anodic oxidation, all produce a large amount of ageing failure waste liquids, discharging causes environmental pollution in order to avoid directly, producer filters after with the waste liquid flocculation sediment, filtrate meets environmental requirement and discharges, and remaining filter cake is solid mud.
At present, be to store up to the general method of disposal of mud both at home and abroad, comprise that ditch, grain mass are deposited or store up on the level land, this will particularly cause severe contamination in the waters to environment on every side.Because the effluxing, store up and to be accompanied by the discharging of a large amount of pollutent alkali of these mud, and bank up for a long time in the middle of being attached to mud.How store up the seepage control measure in place and recovery measure, be directly connected to the water quality condition of local ground watering.
According to statistics, the aluminium section bar output in China whole nation in 2004 is 280~3,000,000 tons, and this numeral constantly increases with the development in domestic construction market.1~November in 2009, its output is increased to 3,500,000 tons.2010, under the drive of real estate, automobile industry and derived product, aluminium section bar continued to keep steady-state growth.A heat-tinting aluminium section bar plant of producing 10000 tons per year, the annual Aluminiferous waste slag that produces is about 1000 tons, and quantity is huge, has a strong impact on the comprehensive regulation and normal production of aluminium section bar plant waste liquid.The quantity of whole nation aluminum manufacturer sludge is surprising especially, a large amount of wastes such as untimely processing, and pile up like a mountain, not only takies a large amount of vacant soils, caused secondary pollution, and make many useful chemical compositions run off and waste.If can reasonably recycle this part solid waste, turn waste into wealth, can not only help aluminium manufacturer to solve the offal treatment object, and further solve the pollution destruction problem of waste discharge to surrounding enviroment.Therefore, the comprehensive utilization of aluminum manufacturer sludge is essential, has important environmental protection and economic implications.
At present domestic have reclaiming the main approach of mud: 1. utilize waste residue to produce Tai-Ace S 150; 2. purifying industrial aluminium hydroxide; 3. production Aluminum Chloride Hexahydrate.But because mud component is complicated, foreign matter content is high makes its recycling that certain difficulty be arranged, and reclaimer is complicated, and added value of product is low, and promotional value is little.By analysis, filtering the aluminium-containing sludge main component that obtains is Al (OH) 3And AlOOH, contain high temperature resistant composition α-Al 2O 3, and because it has that fine size, specific surface area are large, the surface is can be large, active high, solid state reaction and the characteristics such as the sintering impellent is large, not only can be used as mullite synthesizing Al 2O 3Main source, and can promote solid state reaction, be conducive to the formation of mullite.
Agalmatolite (Al 2O 34SiO 2H 2O) be a kind of clay mineral of three-decker, it not only provides SiO for the mullite preparation 2And Al 2O 3Composition, and it can expand when high-temperature calcination in order to offsetting base substrate in the contraction that sintering process produces, has avoided base substrate to ftracture in the contraction of sintering process, so agalmatolite is the desirable feedstock of synthesizing mullite material.According to statistics, the U.S. and Japan account for respectively national overall consumption 50% and 60% for the pyrophyllite deposit of refractory materials production.And China's pyrophyllite deposit industrial application with compared sizable gap abroad, be mainly manifested in two aspects: the one, Application Areas is narrower; The 2nd, use class lower.China's agalmatolite mineral products aboundresources, annual have a large amount of pyrophyllite deposit outlets, and be nearly all former mineral products, consumes in large quantities the resource of China.Therefore, actively developing the applied research of pyrophyllite deposit in fields such as refractory materialss is significant.
China's agalmatolite is cheap, and reserve is abundant, and the aluminum manufacturer sludge wide material sources can reduce costs, and therefore select aluminum manufacturer sludge and agalmatolite as the raw material mullite synthesizing, and its environment protection significance, Social benefit and economic benefit are all very remarkable.
The Ruan Yuzhong of University of Fuzhou, Wu Renping, Yu Yan etc. have carried out correlative study to the comprehensive utilization of waste aluminum sludge, have obtained many achievements.Chinese patent CN1448367A discloses a kind of method of making mullite refractory with waste aluminum sludge.The method is controlled Al take aluminium section bar plant sludge, clay and quartz as main raw material 2O 3With SiO 2The ratio of weight percentage be 1.50~3.5.Synthesis temperature is 1200~1450 ℃, and the mullite content of synthetic material is 50%~98%.Refractory materials and kiln furniture material with this synthetic material makes have good thermal property and mechanical property.Its folding strength is 15~20MPa, and volume density is 1.9~2.0g/cm 3, apparent porosity is 25%~30%, and water-intake rate is 12%~15%, and maximum operation (service) temperature is 1400 ℃.
Chinese patent CN1557762A discloses a kind of method with waste aluminum sludge development light-weight mullite heat insulating refractory material.The method adopts and mixes flammable admixture or foaming agent, and in the product of producing, mullite content is 50-95%, and volume density is 0.6~1.0g/cm 3, folding strength is 0.7~3.0MPa, refractoriness 〉=1600 ℃.
Chinese patent CN1609040A discloses a kind of synthetic method of mullite material.The fine silicon powder that the method reclaims take aluminium section bar plant sludge and ferroalloy works is as the raw material synthesizing mullite material, and wherein mullite content is 85%~98%.
Chinese patent CN1609058A discloses a kind of New type of light refractory material and manufacture method thereof.The method is take aluminium section bar plant sludge, clay and add waste polystyrene plastic as the synthetic light thermal insulation fire-resistant material of raw material, and wherein mullite content is 30%~80%.Density is 0.79~1.00g/cm 3, folding strength is 2.1~5.2MPa, refractoriness 〉=1600 ℃.
The Chen Ruiwen of Dehua County mineral substance analytic centre utilizes aluminium section bar plant sludge and agalmatolite to prepare mullite material, and as main raw material, add 12% trichroite and make wedding agent, make cordierite-mullite kiln furniture materials (Chen Ruiwen. the development of dichroite-mullite kiln furnitures and performance variation research [J]. ceramic science with the art, 2008,07.).But have a large amount of pores in this kiln furniture material, its void content is all higher than 25%, and the void content of external quality matetrial all is controlled at below 20%.Therefore the production technique of this kiln furniture material also has larger room for improvement.
In the production technique of the described mullite refractory of above-mentioned each patent, base substrate all adopts the plastic molding technology to make.Because solvent and wedding agent that plastic molding adopts are more, base substrate shrinks larger when burning till, and performance is affected.Therefore need to select other blank forming method, improvement of production process is to improve the performance of mullite refractory.
Summary of the invention
The object of the present invention is to provide a kind of method of utilizing aluminum manufacturer sludge and agalmatolite to prepare mullite refractory, the method is that a kind of technological process is simple, and is with low cost, the method for comprehensive utilization solid waste.
The present invention includes following steps:
1) aluminum manufacturer sludge and agalmatolite are sent into respectively ball mill for dry grinding;
2) with step 1) aluminum manufacturer sludge of gained and agalmatolite send into and add the water wet-milling in ball mill, gets aluminum manufacturer sludge-agalmatolite mixed slurry;
3) with step 2) aluminum manufacturer sludge of gained-agalmatolite mixed slurry, spray into atomizer that prilling tower atomizes, drying, get aluminum manufacturer sludge-agalmatolite granule;
4) aluminum manufacturer sludge-agalmatolite granule is delivered to moulding in hydraulic forming machine, get aluminum manufacturer sludge-agalmatolite base substrate;
5) with aluminum manufacturer sludge-agalmatolite body drying, burn till contraction with minimizing, prevent sample cracking;
6) with step 5) aluminum manufacturer sludge of gained-agalmatolite blank sintering, be cooled to room temperature after sintering, get mullite refractory.
In step 1) in, described aluminum manufacturer sludge and agalmatolite, in mass ratio, can be according to Al in aluminum manufacturer sludge and agalmatolite 2O 3With SiO 2The quality percentage composition, calculate Al in aluminum manufacturer sludge-agalmatolite mixture 2O 3With SiO 2The quality percentage composition is controlled Al 2O 3With SiO 2The ratio of quality percentage composition be 2.35~2.75; The material size of described aluminum manufacturer sludge preferably is controlled in 1mm, and the discharging-material size of the aluminum manufacturer sludge after dry grinding preferably is controlled in 3 μ m; The material size of described agalmatolite preferably is controlled in 10mm, and the discharging-material size of the agalmatolite after dry grinding preferably is controlled in 5 μ m.
In step 4) in, described moulding can be adopted the hydraulic forming machine of different model and different die trials, molds the base substrate of different shapes size; Forming pressure can be 120~180MPa, is preferably 135~165MPa, and optimum value is 150MPa; Pressing speed and dwell time need to adjust according to size, thickness and the shape of base substrate.If the large-scale base substrate of moulding, beginning pressurization should be slow, and the centre can be fast, and the later stage should be slow, and certain dwell time is arranged; If the base substrate of moulding is of a size of 300mm * 300mm * 100mm, when pressing speed is controlled to be 0~50MPa, 2MPa/s; During 50~100MPa, 5MPa/s; During 100~180MPa, 2MPa/s, the dwell time is 60s.If the small-sized base substrate of moulding, pressing speed can suitably be accelerated; If the base substrate of moulding is of a size of 5mm * 4mm * 50mm, when pressing speed is controlled to be 0~50MPa, 5MPa/s; During 50~100MPa, 10MPa/s; During 100~180MPa, 5MPa/s, the dwell time is 10s.
In step 5) in, described drying can be put into aluminum manufacturer sludge-agalmatolite base substrate thermostatic drying chamber dry, and dry temperature can be 100~110 ℃, is preferably 102~108 ℃, and optimum value is 105 ℃; The dry time can be 1~3h, is preferably 1.5~2.5h, and optimum value is 2h.
In step 6) in, the temperature of described sintering can be 1400~1600 ℃, is preferably 1450~1600 ℃, and optimum value is 1550 ℃; The temperature rise rate of described sintering process is controlled to be: during room temperature-900 ℃, and 10 ℃/min; In the time of 900~1200 ℃, 5 ℃/min; In the time of 1200~1600 ℃, 3 ℃/min; The time of described sintering can be 2~10h, is preferably 2~6h, and optimum value is 4h; Described cooling being preferably in is cooled to room temperature in air.
The present invention is take aluminum manufacturer sludge and agalmatolite as raw material, by the synthetic a kind of type material of solid state reaction sintering.This material is through XRD analysis, and its mullite content is 85-95%, so the material that this invention makes is a kind of mullite refractory.Its outstanding advantages is: be main raw material owing to adopting agalmatolite, therefore not only provide SiO for the mullite preparation 2And Al 2O 3Composition, and it can expand when high-temperature calcination in order to offsetting base substrate in the contraction that sintering process produces, has avoided base substrate to ftracture in the contraction of sintering process.Owing to adopting mist projection granulating and compression molding technology, the blank density of therefore not only making is large, size accurate, it is little to shrink, and this moulding process is simple, easy to operate, the cycle is short, efficient is high, be convenient to realize automatic production.Owing to accurately controlling Al 2O 3With SiO 2The ratio of quality percentage composition, therefore the mullite content of resulting materials is improved greatly.
Technological process of the present invention is simple, and is with low cost, belongs to multipurpose use of solid waste, has great environment protection meaning.The products obtained therefrom mullite content is high, and excellent property is a kind of very promising mullite refractory.Through XRD analysis, in the mullite refractory that makes, mullite content is 85%~95%, and folding strength is 20~25MPa, and one time the thermal shock conservation rate is 75~90%, refractoriness 〉=1600 ℃, and volume density is 2.00~2.15g/cm 3, apparent porosity is 15~20%, reaches the level of external quality matetrial.Product has competitive power, is convenient to Industry Promotion, has very considerable market outlook.
Description of drawings
Fig. 1 is the XRD figure spectrum of the embodiment of the present invention 1 prepared mullite refractory.
Fig. 2 is the XRD figure spectrum of the embodiment of the present invention 2 prepared mullite refractories.
Fig. 3 is the XRD figure spectrum of the embodiment of the present invention 3 prepared mullite refractories.
Fig. 4 is the XRD figure spectrum of the embodiment of the present invention 4 prepared mullite refractories.
Fig. 5 is the XRD figure spectrum of the embodiment of the present invention 5 prepared mullite refractories.
In Fig. 1~5, X-coordinate be diffraction angle 2-Theta (°), ordinate zou is diffracted intensity Intensity (Counts); M is mullite, and A is aluminum oxide, and S is quartzy.
Embodiment
The present invention adopts aluminum manufacturer sludge and agalmatolite as raw material, and aluminum manufacturer sludge is the waste liquid that produces in the aluminium shape surface treating processes, obtains through coagulative precipitation.Al wherein 2O 3Content is 60%~62%, SiO 2Content is 2%~4%, and loss on ignition is 34%~35%.Agalmatolite is siliceous agalmatolite, Al 2O 3Content is 16%~18%, SiO 2Content is 77%~79%, and essential mineral consists of agalmatolite and a small amount of quartz and kaolinite.
Embodiment 1
1. the dewatered sludge that provides take Fujian Nanping Aluminium Factory and the agalmatolite in Minhou, Foochow are as example.Al in aluminum manufacturer sludge 2O 3Content is 6116%, SiO 2Content is 2.34%, and loss on ignition is 34.26%, Al in agalmatolite 2O 3Content is 16.93%, SiO 2Content is 78.41%, and essential mineral consists of agalmatolite and a small amount of quartz and kaolinite.
2. aluminum manufacturer sludge and agalmatolite are sent into respectively ball mill for dry grinding.The material size of aluminum manufacturer sludge is controlled in 1mm, and discharging-material size is controlled in 3 μ m; The material size of agalmatolite is controlled in 10mm, and discharging-material size is controlled in 5 μ m.
3. aluminum manufacturer sludge and agalmatolite after dry grinding are sent in ball mill, add the water wet-milling, obtain aluminum manufacturer sludge-agalmatolite mixed slurry.In mass ratio, aluminum manufacturer sludge: agalmatolite is 3: 1.At this moment, Al 2O 3With SiO 2The ratio of quality percentage composition be 2.35.
4. aluminum manufacturer sludge-agalmatolite mixed slurry sprays into atomizer that prilling tower atomizes, drying, obtains aluminum manufacturer sludge-agalmatolite granule.
5. aluminum manufacturer sludge-agalmatolite granule is delivered to moulding in hydraulic forming machine, be pressed into the strip base substrate of 5mm * 4mm * 50mm.Forming pressure is 150MPa; Pressing speed is controlled to be: during 0~50MPa, and 5MPa/s; During 50~100MPa, 10MPa/s; During 100~150MPa, 5MPa/s; Dwell time is 10s.
6. base substrate is put into thermostatic drying chamber and dry, the temperature of thermostatic drying chamber is made as 105 ℃, and be 2h time of drying.
7. the base substrate after drying is put into High Temperature Furnaces Heating Apparatus, reaction sintering.Sintering temperature is 1500 ℃; The temperature rise rate of sintering process is controlled to be: during room temperature~900 ℃, and 10 ℃/min; In the time of 900~1200 ℃, 5 ℃/min; In the time of 1200~1500 ℃, 3 ℃/min; Sintering time is 4h.With its taking-up, be cooled to room temperature in air after sintering.
8. show through XRD analysis: sample forms 3 crystalline phases, is respectively mullite, Al 2O 3, SiO 2Wherein mullite content is 87.3%, Al 2O 3Content is 9.8%, SiO 2Content is 2.9%.The folding strength of sample is 22.28MPa, and one time the thermal shock conservation rate is 87.2%, and refractoriness is 1600 ℃, and volume density is 2.05g/cm 3, apparent porosity is 18.7%.
Embodiment 2
Raw material and technological process are with embodiment 1.Aluminum manufacturer sludge: agalmatolite is 3: 1, at this moment Al 2O 3With SiO 2The ratio of quality percentage composition be 2.35.The base substrate that is pressed into is of a size of 5mm * 4mm * 50mm, and forming pressure is 135MPa; Pressing speed is controlled to be: during 0~50MPa, and 5MPa/s; During 50~100MPa, 10MPa/s; During 100~135MPa, 5MPa/s; Dwell time is 10s.Sintering temperature is 1550 ℃; The temperature rise rate of sintering process is controlled to be: during room temperature~900 ℃, and 10 ℃/min; In the time of 900~1200 ℃, 5 ℃/min; In the time of 1200~1550 ℃, 3 ℃/min; Sintering time is 4h.The gained sample forms 3 crystalline phases, is respectively mullite, Al 2O 3, SiO 2Wherein mullite content is 93.3%, Al 2O 3Content is 6.1%, SiO 2Content is 0.6%.The folding strength of sample is 22.17MPa, and one time the thermal shock conservation rate is 77.9%, and refractoriness is 1650 ℃, and volume density is 2.12g/cm 3, apparent porosity is 16.9%.
Embodiment 3
Raw material and technological process are with embodiment 1.Aluminum manufacturer sludge: agalmatolite is 3.55: 1, at this moment Al 2O 3With SiO 2The ratio of quality percentage composition be 2.70.The base substrate that is pressed into is of a size of 300mm * 300mm * 30mm, and forming pressure is 150MPa; Pressing speed is controlled to be: during 0~50MPa, and 3MPa/s; During 50~100MPa, 5MPa/s; During 100~150MPa, 3MPa/s; Dwell time is 45s.Sintering temperature is 1500 ℃; The temperature rise rate of sintering process is controlled to be: during room temperature~900 ℃, and 10 ℃/min; In the time of 900~1200 ℃, 5 ℃/min; In the time of 1200~1500 ℃, 3 ℃/min; Sintering time is 6h.The gained sample forms 3 crystalline phases, is respectively mullite, Al 2O 3, SiO 2Wherein mullite content is 94.2%, Al 2O 3Content is 5.2%, SiO 2Content is 0.6%.The folding strength of sample is 21.53MPa, and one time the thermal shock conservation rate is 82.6%, and refractoriness is 1600 ℃, and volume density is 2.08g/cm 3, apparent porosity is 17.2%.
Embodiment 4
Raw material and technological process are with embodiment 1.Aluminum manufacturer sludge: agalmatolite is 3.76: 1, at this moment Al 2O 3With SiO 2The ratio of quality percentage composition be 2.73.The base substrate that is pressed into is of a size of 300mm * 300mm * 50mm, and forming pressure is 165MPa; Pressing speed is controlled to be: during 0~50MPa, and 3MPa/s; During 50~100MPa, 5MPa/s; During 100~165MPa, 2MPa/s; Dwell time is 50s.Sintering temperature is 1550 ℃; The temperature rise rate of sintering process is controlled to be: during room temperature~900 ℃, and 10 ℃/min; In the time of 900~1200 ℃, 5 ℃/min; In the time of 1200~1550 ℃, 3 ℃/min; Sintering time is 4h.The gained sample forms 3 crystalline phases, is respectively mullite, Al 2O 3, SiO 2Wherein mullite content is 92.9%, Al 2O 3Content is 6.3%, SiO 2Content is 0.8%.The folding strength of sample is 24.12MPa, and one time the thermal shock conservation rate is 86.3%, and refractoriness is 1650 ℃, and volume density is 2.15g/cm 3, apparent porosity is 15.7%.
Embodiment 5
Raw material and technological process are with embodiment 1.Aluminum manufacturer sludge: agalmatolite is 3.35: 1, at this moment Al 2O 3With SiO 2The ratio of quality percentage composition be 2.58.The base substrate that is pressed into is of a size of 300mm * 300mm * 100mm, and forming pressure is 180MPa; Pressing speed is controlled to be: during 0~50MPa, and 2MPa/s; During 50~100MPa, 5MPa/s; During 100~180MPa, 2MPa/s; Dwell time is 60s.Sintering temperature is 1550 ℃; The temperature rise rate of sintering process is controlled to be: during room temperature~900 ℃, and 10 ℃/min; In the time of 900~1200 ℃, 5 ℃/min; In the time of 1200~1550 ℃, 3 ℃/min; Sintering time is 4h.The gained sample forms 3 crystalline phases, is respectively mullite, Al 2O 3, SiO 2Wherein mullite content is 91.8%, Al 2O 3Content is 7.2%, SiO 2Content is 1.0%.The folding strength of sample is 21.35MPa, and one time the thermal shock conservation rate is 81.8%, and refractoriness is 1600 ℃, and volume density is 2.02g/cm 3, apparent porosity is 19.1%.

Claims (5)

1. method of utilizing aluminum manufacturer sludge and agalmatolite to prepare mullite refractory is characterized in that comprising the following steps:
1) aluminum manufacturer sludge and agalmatolite are sent into respectively ball mill for dry grinding; Described aluminum manufacturer sludge and agalmatolite, in mass ratio, according to A1 in aluminum manufacturer sludge and agalmatolite 2O 3With SiO 2The quality percentage composition, calculate A1 in aluminum manufacturer sludge-agalmatolite mixture 2O 3With SiO 2The quality percentage composition is controlled A1 2O 3With SiO 2The ratio of quality percentage composition be 2.35~2.75; The material size of described aluminum manufacturer sludge is controlled in 1mm, and the material size of described agalmatolite is controlled in 10mm; The discharging-material size of the aluminum manufacturer sludge after described dry grinding is controlled in 3 μ m; The discharging-material size of the agalmatolite after dry grinding is controlled in 5 μ m;
2) aluminum manufacturer sludge of step 1) gained and agalmatolite are sent into added the water wet-milling in ball mill, get aluminum manufacturer sludge-agalmatolite mixed slurry;
3) with step 2) aluminum manufacturer sludge of gained-agalmatolite mixed slurry, spray into atomizer that prilling tower atomizes, drying, get aluminum manufacturer sludge-agalmatolite granule;
4) aluminum manufacturer sludge-agalmatolite granule is delivered to moulding in hydraulic forming machine, get aluminum manufacturer sludge-agalmatolite base substrate; The pressure of described moulding is 120~180MPa; The base substrate of described moulding is of a size of 300mm * 300mm * 100mm, when pressing speed is controlled to be 0~50MPa, and 2MPa/s; During 50~100MPa, 5MPa/s; During 100~180MPa, 2MPa/s, the dwell time is 60s; The base substrate of moulding is of a size of 5mm * 4mm * 50mm, when pressing speed is controlled to be 0~50MPa, and 5MPa/s; During 50~100MPa, 10MPa/s; During 100~180MPa, 5MPa/s, the dwell time is 10s;
5) with aluminum manufacturer sludge-agalmatolite body drying, burn till contraction with minimizing, prevent sample cracking;
6) with the aluminum manufacturer sludge of step 5) gained-agalmatolite blank sintering, be cooled to room temperature after sintering, get mullite refractory; The temperature of described sintering is 1400~1600 ℃; The temperature rise rate of described sintering process is controlled to be: during room temperature-900 ℃, and 10 ℃/min; In the time of 900~1200 ℃, 5 ℃/min; In the time of 1200~1600 ℃, 3 ℃/min; The time of described sintering is 2~10h.
2. a kind of method of utilizing aluminum manufacturer sludge and agalmatolite to prepare mullite refractory as claimed in claim 1, the pressure that it is characterized in that described moulding is 135~165MPa.
3. a kind of method of utilizing aluminum manufacturer sludge and agalmatolite to prepare mullite refractory as claimed in claim 1, it is characterized in that in step 5), described drying is that aluminum manufacturer sludge-agalmatolite base substrate is put into the thermostatic drying chamber drying, and dry temperature is 100~110 ℃; The dry time is 1~3h.
4. a kind of method of utilizing aluminum manufacturer sludge and agalmatolite to prepare mullite refractory as claimed in claim 3, the temperature that it is characterized in that described drying is 102~108 ℃; The dry time is 1.5~2.5h.
5. a kind of method of utilizing aluminum manufacturer sludge and agalmatolite to prepare mullite refractory as claimed in claim 1, the temperature that it is characterized in that described sintering is 1450~1600 ℃; The time of described sintering is 2~6h.
CN 201010265607 2010-08-27 2010-08-27 Method for preparing mullite refractory material from aluminum plant sludge and pyrophyllite Expired - Fee Related CN101913889B (en)

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CN105130394B (en) * 2015-08-19 2017-08-04 深圳市正源清环境科技有限公司 Glazed ceramic wall tile and preparation method thereof
CN106800405B (en) * 2017-01-19 2020-06-16 佛山东鹏洁具股份有限公司 High-mullite crystal phase ceramic slurry
CN114180944B (en) * 2021-11-18 2023-04-11 新化柏盛陶瓷科技有限公司 Large-size industrial ceramic hot-pressing manufacturing method
CN115259846B (en) * 2022-07-13 2023-05-09 合肥工业大学 Ceramic material and preparation method thereof

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