CN102910923B - Method for synthesizing corundum-mullite composite phase material by using bauxite tailings - Google Patents
Method for synthesizing corundum-mullite composite phase material by using bauxite tailings Download PDFInfo
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- CN102910923B CN102910923B CN201210461103.9A CN201210461103A CN102910923B CN 102910923 B CN102910923 B CN 102910923B CN 201210461103 A CN201210461103 A CN 201210461103A CN 102910923 B CN102910923 B CN 102910923B
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- Prior art keywords
- corundum
- mullite
- bauxite gangue
- bauxite
- raw material
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- 229910001570 bauxite Inorganic materials 0.000 title claims abstract description 38
- 239000000463 material Substances 0.000 title claims abstract description 19
- 229910052863 mullite Inorganic materials 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 13
- 230000002194 synthesizing effect Effects 0.000 title abstract description 7
- 239000002131 composite material Substances 0.000 title abstract description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 239000012141 concentrate Substances 0.000 claims abstract description 8
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 5
- 239000011707 mineral Substances 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims abstract description 5
- 239000002245 particle Substances 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims abstract description 4
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 12
- 239000013078 crystal Substances 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- 239000012071 phase Substances 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 9
- 238000001994 activation Methods 0.000 claims description 7
- 238000001354 calcination Methods 0.000 claims description 7
- 229910052593 corundum Inorganic materials 0.000 claims description 6
- 239000010431 corundum Substances 0.000 claims description 6
- 238000005245 sintering Methods 0.000 claims description 6
- 230000004913 activation Effects 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 4
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 238000003786 synthesis reaction Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000000354 decomposition reaction Methods 0.000 claims description 2
- 229910001648 diaspore Inorganic materials 0.000 claims description 2
- 238000009413 insulation Methods 0.000 claims description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052622 kaolinite Inorganic materials 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- 230000009257 reactivity Effects 0.000 claims description 2
- 230000000717 retained effect Effects 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 239000007790 solid phase Substances 0.000 claims description 2
- 239000004575 stone Substances 0.000 claims description 2
- 239000011819 refractory material Substances 0.000 abstract description 6
- 239000002253 acid Substances 0.000 abstract 2
- 238000002386 leaching Methods 0.000 abstract 2
- 230000003213 activating effect Effects 0.000 abstract 1
- 238000004321 preservation Methods 0.000 abstract 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 8
- 239000002910 solid waste Substances 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical class O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 238000004131 Bayer process Methods 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- HIGRAKVNKLCVCA-UHFFFAOYSA-N alumine Chemical compound C1=CC=[Al]C=C1 HIGRAKVNKLCVCA-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
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- Compositions Of Oxide Ceramics (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
A method for synthesizing a corundum-mullite composite phase material by using bauxite tailings, and belongs to the field of refractory materials. A raw material for synthesizing corundum-mullite is the bauxite tailings. The method comprises the steps of grinding by a ball mill and homogenizing the isabelline granulated bauxite tailings with original particle size being about 100 mu m as the raw material to obtain the mineral powder with the average particle size being smaller than 10mu m; activating and roasting the grinded mineral powder for 2-4hours at the temperature of 630-820DEG C; performing acid leaching on the roasted mineral powder with the liquid-solid ration of about 1:10 in 2.5mol/L-4.3mol/L hydrochloric acid for 1-3hours at the temperature higher than 90 DEG C; performing temperature preservation on the finished concentrate subjected to the acid leaching for 3-6 hours at the temperature of 1450-1650 DEG C; and synthesizing under air atmosphere. According to the invention, the raw material is rich, the price is low, the synthesized corundum-mullite composite phase material is very pure, various performances of the material are remarkably improved, high added value is realized, and the method is a new path for preparing high temperature refractory materials.
Description
Technical field
The invention belongs to fire resisting material field, particularly a kind of corundum-mullite composites.
Background technology
Because mullite has good high-temperature mechanics, high temperature thermal property, make mullite synthesizing goods there is higher density and purity, lower heat-conduction coefficient and thermal expansivity, thermal structure intensity is high, high temperature creep rate is low, and heat-shock resistance and chemical corrosion are strong, fusing point advantages of higher; And corundum good springiness, fusing point is high, at high temperature has good wear-resisting, chemical resistance of concrete and volume stability, and hardness is large, and refractoriness is high; Mullite crystal is generally column or prism-shaped in addition, corundum body is generally granular, so prepare corundum-mullite composites, will collect the two-fold advantage of corundum crystal and mullite crystal, thereby make this material all be better than in every respect single-phase mullite material or corundum material.The general alumine that adopts, with sintering process or electric smelting legal person work mullite synthesizing, if still synthesized with pure raw material, has seriously improved the production cost of material, especially as refractory materials at present.Therefore, adopt natural matter can significantly reduce the production cost of material undoubtedly.
China's bauxite feature is low alumina-silica ratio, can only adopt ore dressing-alumina producing Bayer process, the main solid waste producing after ore dressing is bauxite gangue, bauxite raw ore per ton will produce the bauxite gangue of approximately 20% ~ 30% quality, mine tailing is not large-scale developed and utilized at present, generally just in tailing dam, stacks.The accumulation of mine tailing can cause the problems such as alkalization of soils, environmental pollution.Aluminium industry is at development, and mine tailing amount will be increasing, and therefore, the development and utilization of bauxite gangue, has become the task of top priority.The main chemical compositions of bauxite gangue is Al
2o
3and SiO
2, the two content sum, generally in 70% left and right, separately has a small amount of Fe
2o
3, TiO
2, K
2o etc.Al
2o
3with SiO
2be the main component of industrial production aluminosilicate series refractory material, can consider with bauxite gangue as the raw material of producing aluminosilicate series refractory material.
summary of the invention:
The object of the invention is the existing resource in conjunction with China, make full use of and promote solid waste resource recovery to recycle, selected solid waste bauxite gangue to carry out synthetic fire resistive material, make corundum-mullite composites, not only take full advantage of existing resource, also reduced the pollution that solid waste is brought, greatly reduced production costs simultaneously.
By a method for bauxite gangue synthetic corundum-mullite complex phase material, mainly take bauxite gangue as raw material, Al in bauxite gangue
2o
3content weight percent is 45% ~ 65% left and right, SiO
2content is 20% ~ 25% left and right, contains 10 ~ 15% Fe simultaneously
2o
3and 2% ~ 4% K
2o, all the other materials are mainly crystal water.
Its synthetic method is:
(1) bauxite gangue raw material is isabelline particulate state, initial size is of a size of 100 μ m left and right, for reducing the particle diameter of mineral powder granular, increase its specific surface area, increase its chemical reactivity, and its chemical composition is uniformly distributed, by breeze levigate and homogenizing in ball mill, the median size of the breeze obtaining is less than 10 μ m.
(2) bauxite gangue after levigate at 630 ℃ ~ 820 ℃ calcination for activation 2 to 4 hours, the diaspore in calcination for activation process in bauxite gangue, kaolinite, Erie's stone ore is met and is progressively decomposed, and obtains Al after decomposition
2o
3, SiO
2, K
2o and Fe
2o
3deng, the chemically reactive of these compositions improves a lot before comparing roasting, hydrochloric acid removal of impurities flow process and sintering synthesis flow after being conducive to.
(3) breeze after the bauxite gangue roasting after calcination for activation with about liquid-solid ratio 1:10 in the hydrochloric acid of concentration 2.5mol/L to 4.3mol/L in more than 90 ℃ acidleach 1.5 to 3.5 hours, most Fe
2o
3with K
2o can be dissolved among hydrochloric acid, most Al
2o
3with SiO
2can be retained among solid phase, through solid-liquid separation process, obtain pure concentrate substantially free from foreign meter.
(4) after the concentrate moulding obtaining after acidleach, 1450 ℃～1650 ℃ insulations, within 3～6 hours, carry out sintering and synthesize, synthetic atmosphere is air, the Al in concentrate
2o
3with SiO
2composition reacts and generates mullite-corundum complex phase.
Through test, and the composition of composite diphase material that utilized XRD analysis, test-results shows: synthetic is corundum-mullite composites, can find out that crystal morphology is typical long column shape crystal and bulk crystals growth interlaced with each other, compact structure from the analysis of SEM fracture apperance.
The foreign matter content of bauxite gangue is higher, particularly Fe
2o
3with K
2o impurity, it will have a strong impact on the building-up process of mullite complex phase material, with ordinary process, cannot carry out mullite synthesizing composite diphase material with bauxite gangue.This seminar is through research for many years, discovery is first carried out 2 to 4 hours calcination for activation at 630 ℃ ~ 820 ℃ to bauxite gangue, the concentrate obtaining again with about liquid-solid ratio 1:10 in the hydrochloric acid of concentration 2.5mol/L to 4.3mol/L in more than 90 ℃ acidleach 1 to 3 hours, can significantly reduce the Fe in mine tailing
2o
3with K
2o impurity, the Al after acidleach in mine tailing
2o
3with SiO
2chemically reactive also significantly improve, it can obtain corundum-mullite composites in 3～6 hours at 1450 ℃～1650 ℃ sintering.
The invention has the advantages that: because the main raw material of synthetic corundum-mullite is bauxite gangue, it is a kind of discarded resource, synthetic corundum-mullite composites has very high added value, so be another new way of preparing high-performance refractory material, and meet the industry policy of " recycling economy " that country advocates.
accompanying drawing explanation:
Fig. 1: with the process flow sheet of bauxite gangue synthetic corundum-mullite complex phase material
Fig. 2: by the XRD figure spectrum of the synthetic corundum-mullite complex phase of bauxite gangue
Fig. 3: take bauxite gangue as the synthetic corundum-mullite composites SEM figure of raw material
embodiment:
1. raw material is chosen
Raw material is bauxite gangue in Henan, and the chemical analysis results of bauxite gangue is as shown in table 1:
Table 1: the chemical composition of bauxite gangue
| ? | Al 2O 3 | SiO 2 | Fe 2O 3 | TiO 2 | K 2O | Crystal water |
| Bauxite gangue | 49.87 | 22.45 | 13.1 | 2.61 | 2.25 | 9.72 |
2. synthesis step: see Fig. 1
From XRD figure, in mark, see very clearly and under this test conditions, synthesized very pure corundum-mullite composites.
From the analysis of SEM fracture apperance, can find out that crystal morphology is typical column crystal, the intensive growth of mutually staggered.
Claims (1)
1. by a method for bauxite gangue synthetic corundum-mullite complex phase material, it is characterized in that:
Take bauxite gangue as raw material, Al in bauxite gangue
2o
3content weight percent is 45%～65%, SiO
2content is 20%～25%, contains 10～15% Fe simultaneously
2o
3, 2%～4% K
2o, 2%～4% TiO
2, all the other are crystal water;
The step of synthetic corundum-mullite is:
(1) bauxite gangue raw material is isabelline particulate state, initial size is of a size of 100 μ m, for reducing the particle diameter of mineral powder granular, increase its specific surface area, increase its chemical reactivity, and its chemical composition is uniformly distributed, by breeze levigate and homogenizing in ball mill, the median size of the breeze obtaining is less than 10 μ m;
Bauxite gangue after levigate at 630 ℃～820 ℃ calcination for activation 2 to 4 hours, the diaspore in calcination for activation process in bauxite gangue, kaolinite, Erie's stone ore is met progressively and to be decomposed, and obtains Al after decomposition
2o
3, SiO
2, K
2o and Fe
2o
3, the chemically reactive of these compositions improves a lot before comparing roasting, hydrochloric acid removal of impurities flow process and sintering synthesis flow after being conducive to;
(3) bauxite gangue after calcination for activation with the ratio of liquid-solid ratio 1:10 in the hydrochloric acid of concentration 2.5mol/L to 4.3mol/L in more than 90 ℃ acidleach 1.5 to 3.5 hours, most Fe
2o
3with K
2o can be dissolved among hydrochloric acid, most Al
2o
3with SiO
2can be retained among solid phase, through solid-liquid separation process, obtain pure concentrate free from foreign meter;
After the concentrate moulding obtaining after acidleach, 1450 ℃～1650 ℃ insulations, within 3～6 hours, carry out sintering and synthesize, synthetic atmosphere is air, the Al in concentrate
2o
3with SiO
2composition reacts and generates mullite-corundum complex phase.
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| CN103693970A (en) * | 2013-10-14 | 2014-04-02 | 河南省新密市久隆耐火材料有限公司 | Method for preparing synthetic corundum using waste and old alumina brick |
| CN106316441B (en) * | 2016-08-23 | 2019-03-22 | 福建省德化县富盛陶瓷有限公司 | Introduce the porous heat preserving ceramic and preparation method of alumina tailing base |
| CN108911712A (en) * | 2018-07-25 | 2018-11-30 | 贵州大学 | A kind of preparation method of high-content aluminium oxide ceramics |
| CN114195535A (en) * | 2021-12-30 | 2022-03-18 | 义马瑞辉新材料有限公司 | Preparation method for producing refined mullite corundum high-temperature material at low carbon |
| CN114455956A (en) * | 2022-02-10 | 2022-05-10 | 中国地质科学院郑州矿产综合利用研究所 | Method for preparing electrofused mullite from bauxite under coal |
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