CN103771841A - Preparation method of corundum-mullite complex phase ceramic material - Google Patents
Preparation method of corundum-mullite complex phase ceramic material Download PDFInfo
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- CN103771841A CN103771841A CN201410038608.3A CN201410038608A CN103771841A CN 103771841 A CN103771841 A CN 103771841A CN 201410038608 A CN201410038608 A CN 201410038608A CN 103771841 A CN103771841 A CN 103771841A
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Abstract
The invention discloses a preparation method of a corundum-mullite complex phase ceramic material. The preparation method comprises the following steps: 1) uniformly mixing 1-25% by weight of coal ash, 0-5% by weight of calcium oxide, 0-10% by weight of albite and 60-99% by weight of bauxite to obtain a raw material, wherein the content of aluminum oxide in bauxite is 50-68% by weight; 2) uniformly mixing the raw materials in a ball mill and carrying out ball milling till the grain size of the raw material is less than 74 mu m to obtain mixed powder; 3) adding 1-3% by weight of water glass into the mixed powder to be uniformly stirred, aging for 1-2 hours, and forming and preforming on a press or a pelletizer to obtain a blank; and 4) heating the blank to 1350-1420 DEG C at a rate of 5-15 DEG C/min, insulating for 40-120 minutes and furnace cooling to obtain the corundum-mullite complex phase ceramic material. The bauxite used in the preparation method is a lower grade raw material, so that the production energy consumption and cost are lowered and the resource utilization rate is improved while the demand on the operational performance of the material is satisfied.
Description
Technical field
The present invention relates to a kind of stupalith, particularly a kind of preparation method of corundum-mullite diphase ceramic material.
Background technology
Corundum is α-Al
2o
3al
2o
3thermal structure phase, density 3.98g/cm
3, belong to iris type, there is high rigidity, high-melting-point, high strength, the physics-chem characteristic that acid-alkali-corrosive-resisting etc. are excellent, is a kind of important engineering ceramic material, its range of application is very extensive.Mullite is Al
2o
3-SiO
2the binary compound of unique stable existence under normal pressure in two component system, belongs to rhomboidal crystal, and its chemical formula is 3Al
2o
3-2SiO
2, density 3.16, performance and corundum ceramic are suitable, and high-temperature mechanics and calorifics are particularly outstanding, are a kind of high-temperature structural materials of excellence.
Because mullite crystal is generally column or prism-shaped, and that corundum body is generally is granular, by the comprehensively two-fold advantage of corundum crystal and mullite crystal of the corundum-mullite diphase ceramic material of two kinds of different mutually compound rear formation of ceramic thing of corundum and mullite, make this material all be better than in every respect single-phase mullite material or corundum material.The material with this class excellent properties is relatively applicable to being applied to refractory materials and well fracturing propping agent, but consider that this class materials consumption is huge, if synthesize the production cost that has seriously improved material with pure raw material, therefore need to develop a kind of new technology that adopts natural mineral raw and synthetic this type of diphase ceramic material of industrial residue.
Flyash is to receive and catch the thin ash getting off in the flue gas from coal combustion, is one of industrial residue of the current quantity discharged maximum of China, and China present stage, bed drain purge year has reached 3,000 ten thousand tons.Along with the development of power industry, the flyash quantity discharged of coal-burning power plant increases year by year.A large amount of flyash does not add processing, will produce airborne dust, atmosphere pollution; Can cause river to silt up if enter water system, and toxic chemical substance wherein also can work the mischief to human body and biology.And the main component SiO of flyash
2, Al
2o
3can be used as the raw material of synthetic corundum-mullite Multiphase pottery, other compositions are as FeO, Fe
2o
3, CaO, TiO
2and some latent active ingredients contribute to the formation of ceramic cenotype under high temperature and can promote diphase ceramic material sintering.Thereby can utilize flyash to coordinate bauxitic clay mineral aggregate to carry out the production of corundum-mullite diphase ceramic material.
At present, the method for producing corundum or mullite homogeneous material is more ripe, and by less the two compound technology.Part Methods need to adopt chemosynthesis raw material, or needs the content of aluminum oxide in bauxitic clay, flyash higher, and this type of starting material source is less, cost is higher, has limited its application in actual production, has also reduced the comprehensive utilization ratio of resource simultaneously.In addition, the method for existing this type of composite diphase material of preparation needs first synthesize ceramic material to make the product product of definite shape and size by high temperature sintering conventionally again, and its technical process complexity, unstable product quality and energy consumption are higher.
Summary of the invention
In order to solve the problems of the technologies described above, the invention provides a kind of preparation method of corundum-mullite diphase ceramic material, the bauxitic clay that the method is selected is lower taste raw material, reduces production costs, improves resource utilization in meeting materials'use performance requriements.
Technical scheme of the present invention is as follows for this reason:
A preparation method for corundum-mullite diphase ceramic material, comprises the steps:
1) according to massfraction, 1～25% flyash, 0～5% calcium oxide, 0～10% albite and 60～99% bauxitic clay are mixed, obtain raw material, wherein, described bauxitic clay is that aluminium sesquioxide content is 50～68% bauxitic clay;
2) described raw material is placed in to ball mill and mixes and make its particle diameter to be less than 74 μ m, obtain mixed powder;
3) in described mixed powder, add the water glass that accounts for its quality 1～3% to stir, old 1～2h carries out moulding base on pressing machine or tablets press, obtains blank;
4) described blank is warmed up to 1350～1420 ℃ with the speed of 5～15 ℃/min, furnace cooling after insulation 40～120min, obtains described corundum-mullite diphase ceramic material.
Described flyash is F class II level concrete powder coal ash described in GB/T1596-2005.
The temperature-rise period of step 4) is divided into two steps, and the first step is warmed up to 600～800 ℃ with the speed of 5～10 ℃/min by room temperature, and second step is warmed up to 1350～1420 ℃ with the speed of 10～15 ℃/min.
Described albite is Powdered.
Described calcium oxide is obtained by calcium carbonate, calcite in powder, terra alba decomposes.
The bauxitic clay that this preparation method selects is lower taste raw material, reduces production energy consumption and cost, raising resource utilization in meeting materials'use performance requriements.
Accompanying drawing explanation
Fig. 1 is the X-ray diffraction curve that embodiment 1～5 makes product;
Fig. 2 is the cross-section morphology figure that embodiment several 2 makes product.
Embodiment
Below in conjunction with embodiment, the preparation method of high blending flyash ceramsite propping agent of the present invention is described in detail.
Embodiment 1
A preparation method for corundum-mullite diphase ceramic material, comprises the steps:
1) according to massfraction, 15.3% flyash, 2.9% calcium oxide and 81.8% bauxitic clay are mixed, obtain raw material, wherein, described bauxitic clay is that aluminium sesquioxide content is 65% bauxitic clay, and described calcium oxide is obtained by calcium carbonate thermolysis at 800～1000 ℃;
2) described raw material being placed in to ball mill, is that 1:1 adds corundum ball according to raw material and corundum ball mass ratio, and after ball milling 2h, 200 mesh standard sieves are crossed in discharging, obtain the mixed powder that particle diameter is less than 74 μ m;
3) in described mixed powder, add the water glass that accounts for its quality 2% to stir 30min, old 1h, then inserted in the mould of pressing machine, at 10MPa forming under the pressure, after the demoulding, obtain blank;
4) described blank is warmed up to 600 ℃ with the speed of 5 ℃/min in retort furnace, then is warmed up to 1360 ℃ with the speed of 10 ℃/min, furnace cooling after insulation 40min, obtains described corundum-mullite diphase ceramic material.
Described flyash is F class II level concrete powder coal ash described in GB/T1596-2005.
The density that the present embodiment makes corundum-mullite diphase ceramic material is 2.59g/cm
3, bending strength is 125.6 ± 10MPa.The performance that prior art obtains this type of material is: density 2.50g/cm
3～2.90g/cm
3, bending strength 120～200MPa, correlation data, showing to utilize the present embodiment method to make product does not affect its use properties.
A preparation method for corundum-mullite diphase ceramic material, comprises the steps:
1) according to massfraction, 5% flyash, 7% albite and 88% bauxitic clay are mixed, obtain raw material, wherein, described bauxitic clay is that aluminium sesquioxide content is 68% bauxitic clay;
2) described raw material being placed in to ball mill, is that 1:1 adds corundum ball according to raw material and corundum ball mass ratio, and after ball milling 3h, 200 mesh standard sieves are crossed in discharging, obtain the mixed powder that particle diameter is less than 74 μ m;
3) in described mixed powder, add the water glass that accounts for its quality 1.5% to stir 30min, old 1h, then inserted in the mould of pressing machine, at 10MPa forming under the pressure, after the demoulding, obtain blank;
4) described blank is warmed up to 600 ℃ with the speed of 5 ℃/min in retort furnace, then is warmed up to 1400 ℃ with the speed of 15 ℃/min, furnace cooling after insulation 1h, obtains described corundum-mullite diphase ceramic material.
Described flyash is F class II level concrete powder coal ash described in GB/T1596-2005.
The density that the present embodiment makes corundum-mullite diphase ceramic material is 2.82g/cm
3, bending strength is 190.6 ± 12MPa.The performance that prior art obtains this type of material is: density 2.50g/cm
3～2.90g/cm
3, bending strength 120～200MPa, correlation data, showing to utilize the present embodiment method to make product does not affect its use properties.
Embodiment 3
A preparation method for corundum-mullite diphase ceramic material, comprises the steps:
1) according to massfraction, 8.2% flyash, 2.9% lime powder and 88.9% bauxitic clay are mixed, obtain raw material, wherein, described bauxitic clay is that aluminium sesquioxide content is 55% bauxitic clay, and described calcium oxide is obtained by calcite thermolysis at 900～1200 ℃;
2) described raw material being placed in to ball mill, is that 1:1 adds corundum ball according to raw material and corundum ball mass ratio, and after ball milling 2.5h, 200 mesh standard sieves are crossed in discharging, obtain the mixed powder that particle diameter is less than 74 μ m;
3) in described mixed powder, add the water glass that accounts for its quality 3% to stir 30min, old 1h, then inserted in the mould of pressing machine, at 10MPa forming under the pressure, after the demoulding, obtain blank;
4) described blank is warmed up to 600 ℃ with the speed of 5 ℃/min in retort furnace, then is warmed up to 1380 ℃ with the speed of 15 ℃/min, furnace cooling after insulation 1.5h, obtains described corundum-mullite diphase ceramic material.
Described flyash is F class II level concrete powder coal ash described in GB/T1596-2005.
The density that the present embodiment makes corundum-mullite diphase ceramic material is 2.57g/cm
3, bending strength is 118.1 ± 5MPa.The performance that prior art obtains this type of material is: density 2.50g/cm
3～2.90g/cm
3, bending strength 120～200MPa, correlation data, showing to utilize the present embodiment method to make product does not affect its use properties.
Embodiment 4
A preparation method for corundum-mullite diphase ceramic material, comprises the steps:
1) according to massfraction, 5.1% flyash, 2.9% lime powder and 92% bauxitic clay are mixed, obtain raw material, wherein, described bauxitic clay is that aluminium sesquioxide content is 60% bauxitic clay, and described calcium oxide is obtained by terra alba thermolysis at 800～1200 ℃;
2) described raw material being placed in to ball mill, is that 1:1 adds corundum ball according to raw material and corundum ball mass ratio, and after ball milling 4h, 200 mesh standard sieves are crossed in discharging, obtain the mixed powder that particle diameter is less than 74 μ m;
3) in described mixed powder, add the water glass that accounts for its quality 2% to stir 30min, old 1h, then inserted in the mould of pressing machine, at 10MPa forming under the pressure, after the demoulding, obtain blank;
4) described blank is warmed up to 600 ℃ with the speed of 5 ℃/min in kiln, then is warmed up to 1420 ℃ with the speed of 10 ℃/min, furnace cooling after insulation 1h, obtains described corundum-mullite diphase ceramic material.
Described flyash is F class II level concrete powder coal ash described in GB/T1596-2005.
The density that the present embodiment makes corundum-mullite diphase ceramic material is 2.62g/cm
3, bending strength is 119.3 ± 8MPa.The performance that prior art obtains this type of material is: density 2.50g/cm
3～2.90g/cm
3, bending strength 120～200MPa, correlation data, showing to utilize the present embodiment method to make product does not affect its use properties.
Embodiment 5
A preparation method for corundum-mullite diphase ceramic material, comprises the steps:
1) according to massfraction, 1.5% flyash, 6.5% lime powder and 92% bauxitic clay are mixed, obtain raw material, wherein, described bauxitic clay is that aluminium sesquioxide content is 65% bauxitic clay, and described calcium oxide is obtained by calcite thermolysis at 900～1200 ℃;
2) described raw material being placed in to ball mill, is that 1:1 adds corundum ball according to raw material and corundum ball mass ratio, and after ball milling 3h, 200 mesh standard sieves are crossed in discharging, obtain the mixed powder that particle diameter is less than 74 μ m;
3) in described mixed powder, add the water glass that accounts for its quality 2% to stir 30min, old 1h, then inserted in the mould of pressing machine, at 10MPa forming under the pressure, after the demoulding, obtain blank;
4) described blank is warmed up to 600 ℃ with the speed of 5 ℃/min in kiln, then is warmed up to 1400 ℃ with the speed of 10 ℃/min, furnace cooling after insulation 1h, obtains described corundum-mullite diphase ceramic material.
Described flyash is F class II level concrete powder coal ash described in GB/T1596-2005.
The density that the present embodiment makes corundum-mullite diphase ceramic material is 2.83g/cm
3, bending strength is 124.5 ± 10MPa.The performance that prior art obtains this type of material is: density 2.50g/cm
3～2.90g/cm
3, bending strength 120～200MPa, correlation data, showing to utilize the present embodiment method to make product does not affect its use properties.
Embodiment 6
A preparation method for corundum-mullite diphase ceramic material, comprises the steps:
1) according to massfraction, the bauxitic clay of 24.6% flyash and 75.4% is mixed, obtain raw material, wherein, described bauxitic clay is that aluminium sesquioxide content is 50% bauxitic clay;
2) described raw material being placed in to ball mill, is that 1:1 adds corundum ball according to raw material and corundum ball mass ratio, and after ball milling 2h, 400 mesh standard sieves are crossed in discharging, obtain the mixed powder that particle diameter is less than 48 μ m;
3) in described mixed powder, add the water glass that accounts for its quality 3% to stir 30min, old 1h, then inserted in the mould of pressing machine, at 20MPa forming under the pressure, after the demoulding, obtain blank;
4) described blank is warmed up to 800 ℃ with the speed of 5 ℃/min in retort furnace, then is warmed up to 1350 ℃ with the speed of 10 ℃/min, furnace cooling after insulation 1h, obtains described corundum-mullite diphase ceramic material.
Described flyash is F class II level concrete powder coal ash described in GB/T1596-2005.
The density that the present embodiment makes corundum-mullite diphase ceramic material is 2.61g/cm
3, bending strength is 161.5 ± 15MPa.The performance that prior art obtains this type of material is: density 2.50g/cm
3～2.90g/cm
3, bending strength 120～200MPa, correlation data, showing to utilize the present embodiment method to make product does not affect its use properties.
Embodiment 7
A preparation method for corundum-mullite diphase ceramic material, comprises the steps:
1) according to massfraction, 5% flyash, 7% albite and 88% bauxitic clay are mixed, obtain raw material, wherein, described bauxitic clay is that aluminium sesquioxide content is 68% bauxitic clay;
2) described raw material being placed in to ball mill, is that 1:1 adds corundum ball according to raw material and corundum ball mass ratio, and after ball milling 3h, 400 mesh standard sieves are crossed in discharging, obtain the mixed powder that particle diameter is less than 38 μ m;
3) described mixed powder is placed in to tablets press, successively sprays into the water glass that accounts for powder quality 15～18%, make the described mixed powder balling-up blank of reuniting under tablets press effect;
4) described blank is warmed up to 600 ℃ with the speed of 5 ℃/min in rotary kiln, then is warmed up to 1400 ℃ with the speed of 15 ℃/min, furnace cooling after insulation 1h, obtains described corundum-mullite diphase ceramic material.
Described flyash is F class II level concrete powder coal ash described in GB/T1596-2005.
The ceramsite propping agent volume density obtaining in the present embodiment is 1.55g/cm
3, volume density is 2.76g/cm
3, under 52MPa, percentage of damage is 5.36%, degree of sphericity > 8, and acid solubility 4.89%, its performance index reach the oil and gas industry standard SY/T5108-2006 of the People's Republic of China (PRC) to the requirement of propping agent performance index.
Performance test:
Make the thing phase composite of stupalith by X-ray diffraction analysis embodiment 1～5, test result as shown in Figure 1.As seen from the figure: in material, containing corundum and mullite principal crystalline phase, formed corundum-mullite diphase ceramic material.
Fig. 2 is the fracture scanning electron photomicrograph of the sample that obtains of embodiment 2, the crystal grain of different shape as seen from the figure, wherein polyhedral is corundum crystal, long bar-shaped be mullite crystal.
Claims (4)
1. a preparation method for corundum-mullite diphase ceramic material, is characterized in that comprising the steps:
1) according to massfraction, 1～25% flyash, 0～5% calcium oxide, 0～10% albite and 60～99% bauxitic clay are mixed, obtain raw material, wherein, described bauxitic clay is that aluminium sesquioxide content is 50～68% bauxitic clay;
2) described raw material is placed in to ball mill and mixes, be milled to particle diameter and be less than 74 μ m, obtain mixed powder;
3) in described mixed powder, add the water glass that accounts for its quality 1～3%, stir, old 1～2h carries out moulding base on pressing machine or tablets press, obtains blank;
4) described blank is placed in process furnace, is warmed up to 1350～1420 ℃ with the speed of 5～15 ℃/min, furnace cooling after insulation 40～120min, obtains described corundum-mullite diphase ceramic material.
2. preparation method as claimed in claim 1, is characterized in that: described flyash is F class II level concrete powder coal ash.
3. preparation method as claimed in claim 1, it is characterized in that: the temperature-rise period of step 4) is divided into two steps, the first step is warmed up to 600～800 ℃ with the speed of 5～10 ℃/min by room temperature, and second step is warmed up to 1350～1420 ℃ with the speed of 10～15 ℃/min.
4. preparation method as claimed in claim 1, is characterized in that: described albite is Powdered.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104609842A (en) * | 2014-05-19 | 2015-05-13 | 北京大学 | Method for preparing mullite-phase multiphase material by utilizing high-alumina fly ash |
| CN105130388A (en) * | 2015-08-24 | 2015-12-09 | 天津城建大学 | Preparation method for mullite whisker reinforced ceramic material |
| CN105712725A (en) * | 2016-03-28 | 2016-06-29 | 无锡锡能锅炉有限公司 | Refractory brick for pulverized coal boiler |
| CN107151554A (en) * | 2016-03-03 | 2017-09-12 | 中国科学院过程工程研究所 | For riverfrac treatment or the Superlight ceramsites proppant and preparation method of anhydrous pressure break |
| CN108911712A (en) * | 2018-07-25 | 2018-11-30 | 贵州大学 | A kind of preparation method of high-content aluminium oxide ceramics |
| CN112919893A (en) * | 2021-03-04 | 2021-06-08 | 中国地质大学（北京） | Method for preparing mullite complex phase ceramic by low-temperature sintering of bauxite tailings |
| CN113072366A (en) * | 2021-03-04 | 2021-07-06 | 中国地质大学（北京） | Method for preparing mullite complex-phase ceramic by sintering bauxite tailings and potassium feldspar at low temperature |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102515803A (en) * | 2011-12-23 | 2012-06-27 | 长沙理工大学 | Method for adding bauxite clinker to fly ash for preparing mullite-corundum product |
-
2014
- 2014-01-27 CN CN201410038608.3A patent/CN103771841A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102515803A (en) * | 2011-12-23 | 2012-06-27 | 长沙理工大学 | Method for adding bauxite clinker to fly ash for preparing mullite-corundum product |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104609842A (en) * | 2014-05-19 | 2015-05-13 | 北京大学 | Method for preparing mullite-phase multiphase material by utilizing high-alumina fly ash |
| CN104609842B (en) * | 2014-05-19 | 2016-09-21 | 北京大学 | A kind of method utilizing aluminous fly-ash to prepare mullite phase composite diphase material |
| CN105130388A (en) * | 2015-08-24 | 2015-12-09 | 天津城建大学 | Preparation method for mullite whisker reinforced ceramic material |
| CN107151554A (en) * | 2016-03-03 | 2017-09-12 | 中国科学院过程工程研究所 | For riverfrac treatment or the Superlight ceramsites proppant and preparation method of anhydrous pressure break |
| CN105712725A (en) * | 2016-03-28 | 2016-06-29 | 无锡锡能锅炉有限公司 | Refractory brick for pulverized coal boiler |
| CN108911712A (en) * | 2018-07-25 | 2018-11-30 | 贵州大学 | A kind of preparation method of high-content aluminium oxide ceramics |
| CN112919893A (en) * | 2021-03-04 | 2021-06-08 | 中国地质大学（北京） | Method for preparing mullite complex phase ceramic by low-temperature sintering of bauxite tailings |
| CN113072366A (en) * | 2021-03-04 | 2021-07-06 | 中国地质大学（北京） | Method for preparing mullite complex-phase ceramic by sintering bauxite tailings and potassium feldspar at low temperature |
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Application publication date: 20140507 |