CN101531523A - Method for synthesizing mullite through utilization of waste - Google Patents
Method for synthesizing mullite through utilization of waste Download PDFInfo
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- CN101531523A CN101531523A CN200910021989A CN200910021989A CN101531523A CN 101531523 A CN101531523 A CN 101531523A CN 200910021989 A CN200910021989 A CN 200910021989A CN 200910021989 A CN200910021989 A CN 200910021989A CN 101531523 A CN101531523 A CN 101531523A
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- ash float
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Abstract
The invention relates to a method for synthesizing mullite through the utilization of waste. Fly-ash floating beads are put in a ball mill and are subjected to dry milling; alumina coccolith is used as a grinding medium and is subjected to grinding and iron removing; the fly-as floating beads subjected to iron removing and industrial pure alumina are subjected to mixing and ball milling to obtain a mixed material; the mixed material is put in an alumina crucible, and the alumina crucible is placed in a silicon carbide rod resistance furnace and sintered to obtain a sample; and finally the sample is poured into a material stirrer for stirring to obtain the mullite. The method uses industrial waste of the fly-ash floating beads to synthesize the mullite, so that the method contributes to saving natural resource reducing production cost and is favorable for environmental protection. The used fly-ash floating beads are mainly micron-level spherical particles; compared with natural mineral, the raw materials do not need to be broken by a large-power pulverizer and the mixed material is even; the synthesizing temperature is lower than that of the conventional production process, and mineral resources and energy are saved; and through the control of the adding amount of alumina and the adjustment of the mixture ratio of the raw materials, mullite aggregates with different alumina contents can be synthesized.
Description
Technical field
The present invention relates to utilize waste material synthesizing high temperature method of ceramic material, particularly a kind of method of utilizing the waste mullite synthesizing.
Background technology
Mullite (3Al
2O
32SiO
2) be the alumina hydrochlorate mineral of aluminium, be Al
2O
3-SiO
2The crystalline compound of system unique stable existence under normal pressure, has the refractoriness height, thermal shock resistance, chemical resistance of concrete, creep-resistant property are good, the refractoriness under load height, volume stability is good, and electrical insulating property is strong etc., it is desirable high grade refractory, be widely used in the industry such as metallurgy, glass, pottery, chemistry, electric power, national defence, combustion gas and cement (old winter, Chen Nanchun. the progress of mullite [J]. mineral products and geology, 2004 (2): 18-22).
The natural mullite mineral of occurring in nature seldom, industrial mullite is mainly synthetic.At present, compound probability with the method for mullite mainly contain electric smelting method and sintering process (Shen Xiaoqing. the preparation research of ultra-fine mullite powder [D]. Zhengzhou University's master thesis, 2002:4-6).The electric smelting method is that the fusion in electric arc of mixed raw material is formed, shortcoming be current consumption big, to synthesis condition requirement harshness; Sintering process by the difference of raw materials used character be divided into inorganic silicon-aluminum gel method, organosilicon alumina gel method and mineral facies political reform (Wei Xiaohui, Sun Jialin, Sun Gengchen. the low temperature of mullite synthesizes [J]. refractory materials, 2008,42 (3): 229-231).Wherein, inorganic silicon-aluminum gel method and organosilicon alumina gel method are to adopt inorganic and organic raw material to make the sial colloid by certain chemical constitution respectively, at high temperature calcining forms then, and its shortcoming is that energy consumption is higher, and the organic raw material that uses in the organic gel method costs an arm and a leg.The mineral facies political reform is to place the kiln high-temperature calcination to form natural mineral such as alumine, kaolin, agalmatolite, the shortcoming of this method is the energy consumption height, because there are bigger difference in its mineral composition and mullite between forming, cause the mullite transformation efficiency not high simultaneously, the waste resource.
Summary of the invention
The purpose of this invention is to provide a kind of method of utilizing the synthetic high aluminum-containing mullite of depleted fly ash float sintering, not only raw material sources are extensive, production cost is low for this method, energy consumption is little, and turn waste into wealth, the alumina content height of institute's mullite synthesizing, crystal property is good.
For achieving the above object, the technical solution used in the present invention is:
1) at first, fly ash float is put into ball mill for dry grinding, utilize the alumina balls masonry to be abrasive media, the mass ratio of control abrading-ball and fly ash float is (2~3): 1, grind 0.5~3h, adopt permanent magnet deironing twice after crossing then 120 mesh sieves, and then adopt electromagnetism deironing twice, make Fe in the raw material
2O
3Content be lower than 0.5%;
2) secondly, get above-mentioned after deironing is handled fly ash float and the technical pure aluminum oxide with fly ash float: technical pure aluminum oxide=1: the mass percent of (0.5~3) is put into the ball mill for dry grinding mixing, utilize the alumina balls masonry to be grinding medium, the mass ratio of control abrading-ball and fly ash float is (2~3): 1, grind 0.5~3h, cross 120 mesh sieves then and get compound;
3) then, compound behind the above-mentioned dry grinding mixing is put into alumina crucible, the alumina crucible that compound is housed is placed in the globars resistance furnace, be warming up to 700~1400 ℃ with the temperature rise rate of 5 ℃/min from room temperature, insulation 1~4h gets sample behind the naturally cooling;
4) last, naturally cooled sample poured in the material stirrer stirs, cross the 20-80 mesh sieve after, namely get mullite.
Main raw material of the present invention is the trade waste of coal-burning power plant's discharging, not only helps to save natural resource with the fly ash float mullite synthesizing, reduces production costs, and helps environment protection; Used fly ash float is mainly micron-size spherical particles, compares with natural mineral, and raw material need not to use high-power crusher in crushing, and batch mixing is even; Synthesis temperature all is lower than traditional processing technology, has saved the mineral wealth and the energy; By the add-on of controlled oxidation aluminium, regulate proportioning raw materials, can synthesize the mullite aggregate of different alumina contents.
Embodiment
Embodiment 1: at first, fly ash float is put into ball mill for dry grinding, utilize the alumina balls masonry to be abrasive media, the mass ratio of control abrading-ball and fly ash float is 2:1, grind 3h, adopt permanent magnet deironing twice after crossing then 120 mesh sieves, and then adopt electromagnetism deironing twice, make Fe in the raw material
2O
3Content be lower than 0.5%; Secondly, get above-mentioned after deironing is processed fly ash float and the technical pure aluminium oxide with fly ash float: the mass percent of technical pure aluminium oxide=1:0.5 is put into the ball mill for dry grinding mixing, utilize the alumina balls masonry to be abrasive media, the mass ratio of control abrading-ball and fly ash float is 2:1, grind 3h, cross then 120 mesh sieves and get compound; Then, the compound behind the above-mentioned dry grinding mixing is put into alumina crucible, the alumina crucible that compound is housed is placed in the Elema resistance furnace, be warming up to 700 ℃ from room temperature with the heating rate of 5 ℃/min, insulation 4h naturally must sample after the cooling; At last, naturally cooled sample poured in the material stirrer stirs, cross 80 mesh sieves after, namely get alumina content greater than 40% high aluminum-containing mullite.
Embodiment 2: at first, fly ash float is put into ball mill for dry grinding, utilize the alumina balls masonry to be abrasive media, the mass ratio of control abrading-ball and fly ash float is 2.5:1, grind 2h, adopt permanent magnet deironing twice after crossing then 120 mesh sieves, and then adopt electromagnetism deironing twice, make Fe in the raw material
2O
3Content be lower than 0.5%; Secondly, get above-mentioned after deironing is processed fly ash float and the technical pure aluminium oxide with fly ash float: the mass percent of technical pure aluminium oxide=1:1 is put into the ball mill for dry grinding mixing, utilize the alumina balls masonry to be abrasive media, the mass ratio of control abrading-ball and fly ash float is 2.5:1, grind 2h, cross then 120 mesh sieves and get compound; Then, the compound behind the above-mentioned dry grinding mixing is put into alumina crucible, the alumina crucible that compound is housed is placed in the Elema resistance furnace, be warming up to 900 ℃ from room temperature with the heating rate of 5 ℃/min, insulation 3h naturally must sample after the cooling; At last, naturally cooled sample poured in the material stirrer stirs, cross 60 mesh sieves after, namely get alumina content greater than 60% high aluminum-containing mullite.
Embodiment 3: at first, fly ash float is put into ball mill for dry grinding, utilize the alumina balls masonry to be abrasive media, the mass ratio of control abrading-ball and fly ash float is 3:1, grind 0.5h, adopt permanent magnet deironing twice after crossing then 120 mesh sieves, and then adopt electromagnetism deironing twice, make Fe in the raw material
2O
3Content be lower than 0.5%; Secondly, get above-mentioned after deironing is processed fly ash float and the technical pure aluminium oxide with fly ash float: the mass percent of technical pure aluminium oxide=1:3 is put into the ball mill for dry grinding mixing, utilize the alumina balls masonry to be abrasive media, the mass ratio of control abrading-ball and fly ash float is 3:1, grind 0.5h, cross then 120 mesh sieves and get compound; Then, the compound behind the above-mentioned dry grinding mixing is put into alumina crucible, the alumina crucible that compound is housed is placed in the Elema resistance furnace, be warming up to 1400 ℃ from room temperature with the heating rate of 5 ℃/min, insulation 1h naturally must sample after the cooling; At last, naturally cooled sample poured in the material stirrer stirs, cross 20 mesh sieves after, namely get alumina content greater than 80% high aluminum-containing mullite.
Embodiment 4: at first, fly ash float is put into ball mill for dry grinding, utilize the alumina balls masonry to be abrasive media, the mass ratio of control abrading-ball and fly ash float is 2.2:1, grind 1h, adopt permanent magnet deironing twice after crossing then 120 mesh sieves, and then adopt electromagnetism deironing twice, make Fe in the raw material
2O
3Content be lower than 0.5%; Secondly, get above-mentioned after deironing is processed fly ash float and the technical pure aluminium oxide with fly ash float: the mass percent of technical pure aluminium oxide=1: 2 is put into the ball mill for dry grinding mixing, utilize the alumina balls masonry to be abrasive media, the mass ratio of control abrading-ball and fly ash float is 2.7:1, grind 1h, cross then 120 mesh sieves and get compound; Then, the compound behind the above-mentioned dry grinding mixing is put into alumina crucible, the alumina crucible that compound is housed is placed in the Elema resistance furnace, be warming up to 1000 ℃ from room temperature with the heating rate of 5 ℃/min, insulation 2h naturally must sample after the cooling; At last, naturally cooled sample poured in the material stirrer stirs, cross 40 mesh sieves after, namely get alumina content greater than 70% high aluminum-containing mullite.
Embodiment 5: at first, fly ash float is put into ball mill for dry grinding, utilize the alumina balls masonry to be abrasive media, the mass ratio of control abrading-ball and fly ash float is 2.8:1, grind 1.5h, adopt permanent magnet deironing twice after crossing then 120 mesh sieves, and then adopt electromagnetism deironing twice, make Fe in the raw material
2O
3Content be lower than 0.5%; Secondly, get above-mentioned after deironing is processed fly ash float and the technical pure aluminium oxide with fly ash float: the mass percent of technical pure aluminium oxide=1:1.5 is put into the ball mill for dry grinding mixing, utilize the alumina balls masonry to be abrasive media, the mass ratio of control abrading-ball and fly ash float is 2.3:1, grind 2.6h, cross then 120 mesh sieves and get compound; Then, the compound behind the above-mentioned dry grinding mixing is put into alumina crucible, the alumina crucible that compound is housed is placed in the Elema resistance furnace, be warming up to 1200 ℃ from room temperature with the heating rate of 5 ℃/min, insulation 1.5h naturally must sample after the cooling; At last, naturally cooled sample poured in the material stirrer stirs, cross 50 mesh sieves after, namely get alumina content greater than 65% high aluminum-containing mullite.
Claims (6)
1, a kind of method of utilizing the waste mullite synthesizing is characterized in that:
1) at first, fly ash float is put into ball mill for dry grinding, utilize the alumina balls masonry to be abrasive media, the mass ratio of control abrading-ball and fly ash float is (2~3): 1, grind 0.5~3h, adopt permanent magnet deironing twice after crossing then 120 mesh sieves, and then adopt electromagnetism deironing twice, make Fe in the raw material
2O
3Content be lower than 0.5%;
2) secondly, get above-mentioned after deironing is handled fly ash float and the technical pure aluminum oxide with fly ash float: mass percent technical pure aluminum oxide=1:(0.5~3) is put into the ball mill for dry grinding mixing, utilize the alumina balls masonry to be grinding medium, the mass ratio of control abrading-ball and fly ash float is (2~3): 1, grind 0.5~3h, cross 120 mesh sieves then and get compound;
3) then, compound behind the above-mentioned dry grinding mixing is put into alumina crucible, the alumina crucible that compound is housed is placed in the globars resistance furnace, be warming up to 700~1400 ℃ with the temperature rise rate of 5 ℃/min from room temperature, insulation 1~4h gets sample behind the naturally cooling;
4) last, naturally cooled sample poured in the material stirrer stirs, cross the 20-80 mesh sieve after, namely get mullite.
2, the method for utilizing the discarded object mullite synthesizing according to claim 1, it is characterized in that: at first, fly ash float is put into ball mill for dry grinding, utilize the alumina balls masonry to be abrasive media, the mass ratio of control abrading-ball and fly ash float is 2:1, grinds 3h, excessively adopts twice of permanent magnet deironing behind 120 mesh sieves then, and then adopt electromagnetism deironing twice, make Fe in the raw material
2O
3Content be lower than 0.5%; Secondly, get above-mentioned after deironing is processed fly ash float and the technical pure aluminium oxide with fly ash float: the mass percent of technical pure aluminium oxide=1:0.5 is put into the ball mill for dry grinding mixing, utilize the alumina balls masonry to be abrasive media, the mass ratio of control abrading-ball and fly ash float is 2:1, grind 3h, cross then 120 mesh sieves and get compound; Then, the compound behind the above-mentioned dry grinding mixing is put into alumina crucible, the alumina crucible that compound is housed is placed in the Elema resistance furnace, be warming up to 700 ℃ from room temperature with the heating rate of 5 ℃/min, insulation 4h naturally must sample after the cooling; At last, naturally cooled sample poured in the material stirrer stirs, cross 80 mesh sieves after, namely get alumina content greater than 40% high aluminum-containing mullite.
3, the method for utilizing the discarded object mullite synthesizing according to claim 1, it is characterized in that: at first, fly ash float is put into ball mill for dry grinding, utilize the alumina balls masonry to be abrasive media, the mass ratio of control abrading-ball and fly ash float is 2.5:1, grinds 2h, excessively adopts twice of permanent magnet deironing behind 120 mesh sieves then, and then adopt electromagnetism deironing twice, make Fe in the raw material
2O
3Content be lower than 0.5%; Secondly, get above-mentioned after deironing is processed fly ash float and the technical pure aluminium oxide with fly ash float: the mass percent of technical pure aluminium oxide=1:1 is put into the ball mill for dry grinding mixing, utilize the alumina balls masonry to be abrasive media, the mass ratio of control abrading-ball and fly ash float is 2.5:1, grind 2h, cross then 120 mesh sieves and get compound; Then, the compound behind the above-mentioned dry grinding mixing is put into alumina crucible, the alumina crucible that compound is housed is placed in the Elema resistance furnace, be warming up to 900 ℃ from room temperature with the heating rate of 5 ℃/min, insulation 3h naturally must sample after the cooling; At last, naturally cooled sample poured in the material stirrer stirs, cross 60 mesh sieves after, namely get alumina content greater than 60% high aluminum-containing mullite.
4, the method for utilizing the discarded object mullite synthesizing according to claim 1, it is characterized in that: at first, fly ash float is put into ball mill for dry grinding, utilize the alumina balls masonry to be abrasive media, the mass ratio of control abrading-ball and fly ash float is 3:1, grinds 0.5h, excessively adopts twice of permanent magnet deironing behind 120 mesh sieves then, and then adopt electromagnetism deironing twice, make Fe in the raw material
2O
3Content be lower than 0.5%; Secondly, get above-mentioned after deironing is processed fly ash float and the technical pure aluminium oxide with fly ash float: the mass percent of technical pure aluminium oxide=1:3 is put into the ball mill for dry grinding mixing, utilize the alumina balls masonry to be abrasive media, the mass ratio of control abrading-ball and fly ash float is 3: 1, grind 0.5h, cross then 120 mesh sieves and get compound; Then, the compound behind the above-mentioned dry grinding mixing is put into alumina crucible, the alumina crucible that compound is housed is placed in the Elema resistance furnace, be warming up to 1400 ℃ from room temperature with the heating rate of 5 ℃/min, insulation 1h naturally must sample after the cooling; At last, naturally cooled sample poured in the material stirrer stirs, cross 20 mesh sieves after, namely get alumina content greater than 80% high aluminum-containing mullite.
5, the method for utilizing the discarded object mullite synthesizing according to claim 1, it is characterized in that: at first, fly ash float is put into ball mill for dry grinding, utilize the alumina balls masonry to be abrasive media, the mass ratio of control abrading-ball and fly ash float is 2.2:1, grinds 1h, excessively adopts twice of permanent magnet deironing behind 120 mesh sieves then, and then adopt electromagnetism deironing twice, make Fe in the raw material
2O
3Content be lower than 0.5%; Secondly, get above-mentioned after deironing is processed fly ash float and the technical pure aluminium oxide with fly ash float: the mass percent of technical pure aluminium oxide=1:2 is put into the ball mill for dry grinding mixing, utilize the alumina balls masonry to be abrasive media, the mass ratio of control abrading-ball and fly ash float is 2.7:1, grind 1h, cross then 120 mesh sieves and get compound; Then, the compound behind the above-mentioned dry grinding mixing is put into alumina crucible, the alumina crucible that compound is housed is placed in the Elema resistance furnace, be warming up to 1000 ℃ from room temperature with the heating rate of 5 ℃/min, insulation 2h naturally must sample after the cooling; At last, naturally cooled sample poured in the material stirrer stirs, cross 40 mesh sieves after, namely get alumina content greater than 70% high aluminum-containing mullite.
6, the method for utilizing the discarded object mullite synthesizing according to claim 1, it is characterized in that: at first, fly ash float is put into ball mill for dry grinding, utilize the alumina balls masonry to be abrasive media, the mass ratio of control abrading-ball and fly ash float is 2.8:1, grinds 1.5h, excessively adopts twice of permanent magnet deironing behind 120 mesh sieves then, and then adopt electromagnetism deironing twice, make Fe in the raw material
2O
3Content be lower than 0.5%; Secondly, get above-mentioned after deironing is processed fly ash float and the technical pure aluminium oxide with fly ash float: the mass percent of technical pure aluminium oxide=1:1.5 is put into the ball mill for dry grinding mixing, utilize the alumina balls masonry to be abrasive media, the mass ratio of control abrading-ball and fly ash float is 2.3:1, grind 2.6h, cross then 120 mesh sieves and get compound; Then, the compound behind the above-mentioned dry grinding mixing is put into alumina crucible, the alumina crucible that compound is housed is placed in the Elema resistance furnace, be warming up to 1200 ℃ from room temperature with the heating rate of 5 ℃/min, insulation 1.5h naturally must sample after the cooling; At last, naturally cooled sample poured in the material stirrer stirs, cross 50 mesh sieves after, namely get alumina content greater than 65% high aluminum-containing mullite.
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Cited By (8)
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CN101844145A (en) * | 2010-04-06 | 2010-09-29 | 邱南海 | Method for extracting Mulgrain sand by waste industrial refuse |
CN101845222A (en) * | 2010-05-21 | 2010-09-29 | 南京大学 | Mullite/polyaniline composite material with core-shell structure and preparation method thereof |
CN101775659B (en) * | 2010-01-14 | 2011-11-23 | 陕西理工学院 | Process for preparing mullite whisker or flaky alumina by using coal ash |
CN102515820A (en) * | 2011-12-06 | 2012-06-27 | 天津大学 | Environment-friendly lightweight porous mullite ceramic and preparation method thereof |
CN102765944A (en) * | 2012-07-23 | 2012-11-07 | 徐州工业职业技术学院 | Method for preparing mullite powder from fly ash |
CN107573048A (en) * | 2017-09-16 | 2018-01-12 | 景德镇陶瓷大学 | A kind of acicular mullite hollow ball material and preparation method thereof |
CN108424152A (en) * | 2018-04-09 | 2018-08-21 | 山东宇佳新材料有限公司 | A kind of preparation method of silicon nitride combined silicon carbide fly ash base composite refractory |
CN112707716A (en) * | 2019-10-24 | 2021-04-27 | 中国科学院过程工程研究所 | Mullite-corundum composite ceramic, and preparation method and application thereof |
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2009
- 2009-04-10 CN CN200910021989A patent/CN101531523A/en active Pending
Cited By (10)
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CN101775659B (en) * | 2010-01-14 | 2011-11-23 | 陕西理工学院 | Process for preparing mullite whisker or flaky alumina by using coal ash |
CN101844145A (en) * | 2010-04-06 | 2010-09-29 | 邱南海 | Method for extracting Mulgrain sand by waste industrial refuse |
CN101844145B (en) * | 2010-04-06 | 2012-09-19 | 邱南海 | Method for extracting Mulgrain sand by waste industrial refuse |
CN101845222A (en) * | 2010-05-21 | 2010-09-29 | 南京大学 | Mullite/polyaniline composite material with core-shell structure and preparation method thereof |
CN102515820A (en) * | 2011-12-06 | 2012-06-27 | 天津大学 | Environment-friendly lightweight porous mullite ceramic and preparation method thereof |
CN102765944A (en) * | 2012-07-23 | 2012-11-07 | 徐州工业职业技术学院 | Method for preparing mullite powder from fly ash |
CN102765944B (en) * | 2012-07-23 | 2014-08-06 | 徐州工业职业技术学院 | Method for preparing mullite powder from fly ash |
CN107573048A (en) * | 2017-09-16 | 2018-01-12 | 景德镇陶瓷大学 | A kind of acicular mullite hollow ball material and preparation method thereof |
CN108424152A (en) * | 2018-04-09 | 2018-08-21 | 山东宇佳新材料有限公司 | A kind of preparation method of silicon nitride combined silicon carbide fly ash base composite refractory |
CN112707716A (en) * | 2019-10-24 | 2021-04-27 | 中国科学院过程工程研究所 | Mullite-corundum composite ceramic, and preparation method and application thereof |
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Application publication date: 20090916 |