热处理过程中层状铝硅酸盐矿物中铝的结构变化及酸溶行为研究
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摘要
层状铝硅酸盐矿物是一类非常重要的非金属矿物，由于其特殊的晶体结构特点，具有可塑性、耐火性、化学稳定性等多种工艺性能，它广泛应用于陶瓷、橡胶、涂料、耐火材料等领域。随着非金属矿物材料在功能材料应用领域的快速扩展，以层状铝硅酸盐矿物为原料采用热处理制备高性能的陶瓷、耐高温的特种耐火材料以及纳米多孔材料的研究在国内外已见报导。
本文选择了三种具有代表性的层状铝硅酸盐矿物：高岭石、叶蜡石和伊利石作为研究对象，综合运用热分析、X-射线衍射、红外光谱、固体核磁共振等分析方法，研究了这三种矿物中的铝在热处理过程中结构变化及在酸中的溶解行为。为以层状铝硅酸盐矿物为原材料制备多孔材料、高性能陶瓷和耐火材料等提供了理论指导，论文的主要结论如下：1)层状铝硅酸盐矿物中铝的热行为研究
高岭石：低于450℃时为高岭石阶段，结构为铝氧八面体，只存在Al~Ⅵ；450～550℃范围内发生脱羟基反应，高岭石中结构水被脱除，物相为高岭石和偏高岭石，存在Al~Ⅳ，Al~Ⅴ，Al~Ⅵ3种配位结构；550～991℃范围内为偏高岭石阶段，铝的3种配位结构依然存在；高于991℃时，逐渐生成γ-Al_2O_3和莫来石，Al~Ⅴ消失，只存在Al~Ⅳ和Al~Ⅵ。
叶蜡石：低于500℃时，主要物相为叶蜡石，只存在Al~Ⅵ；500-932℃之间，叶蜡石脱水，铝的物相为脱水叶蜡石和叶蜡石，且存在三种配位结构的铝：Al~Ⅳ、Al~Ⅴ和Al~Ⅵ；932-1141℃温度段，铝的物相主要为脱水叶蜡石和少量的初晶莫来石阶段；高于1141℃时，铝的物相为莫来石，只存在两种配位的铝：Al~Ⅳ和Al~Ⅵ。
伊利石：低于543℃时，物相为伊利石，由于存在四面体中的Al~(3+)替代Si~(4+)的影响，原矿中存在Al~Ⅵ和Al~Ⅳ，543-1001℃期间，伊利石脱除羟基，物相为伊利石和脱水伊利石，存在Al~Ⅴ、Al~Ⅵ和Al~Ⅳ，其中Al~Ⅴ的数量很少；1001-1181℃时，铝的主要物相为脱水伊利石；高于1181℃时，铝的主要物相为莫来石，铝的配位为Al~Ⅵ和Al~Ⅳ。
2)热活化后层状铝硅酸盐矿物中铝的酸溶行为研究
经热处理高岭石比叶蜡石和伊利石中的铝在酸中的溶解性能均要好。
高岭石：未经热活化的高岭石中Al~Ⅵ在酸中的溶解能力差；经过热活化后生成偏高岭石(Al~Ⅳ、Al~Ⅴ和Al~Ⅵ)，其中Al~Ⅴ在酸中的溶解最好，Al~Ⅳ和Al~Ⅵ在酸中能力较差；继续升高温度偏高岭石生成不溶于酸的γ-Al_2O_3和莫来石(Al~Ⅳ和Al~Ⅵ)，Al~Ⅳ和Al~Ⅵ在酸中的溶解很差。酸溶试验结果表明高岭石在活化温度为900℃，活化时间为15min，溶出温度为120℃，HCl质量分数为20％，溶出时间为120min，L／S为10时，Al_2O_3的溶出率可以达到最大值为97％。酸溶后，高岭石的比表面积由22．42 m~2／g上升到304．84m~2／g。
叶蜡石：未经过热活化的叶蜡石中铝在酸中的溶解能力差；经过热活化后，在750℃时，叶蜡石中铝在酸中的溶解能力相比整个热处理过程是最好的；脱水叶蜡石在酸中的溶解能力很差；到高温生成的莫来石中Al~Ⅳ和Al~Ⅵ不溶于酸。酸溶试验表明在活化温度为750℃，活化时间为15min，H_28O_4质量分数为20％，溶出温度为150℃，溶出时间为120min，L／S为5时，叶蜡石中Al_2O_3溶出率达到最大值为20．38％。
伊利石：相比高岭石和叶蜡石来说，伊利石中的铝在酸中的溶解性能最差。在650℃时，伊利石中铝在酸中的溶解能力在整个热处理过程中是最好的，脱水伊利石只有少量的铝溶于酸；到高温度生成的莫来石中Al~Ⅳ和Al~Ⅵ不溶于酸。酸溶试验的结果表明在活化温度为650min，活化时间为15min，H_2SO_4质量分数为20％，溶出温度为150℃，溶出时间为120 min，液固比(L／S)为10时，伊利石中Al_2O_3溶出率达到最大值为16．13％。
Most layered silicates are important nonmetallic minerals, and they are endowed with many process properties such as plasticity, fire resistance, and chemical stability etc. for their special crystal structure. They are widely used in fields of ceramic, rubber, coating, fire resistance materials etc. Nanometer porous material, high quality ceramics and fire resistance materials with layered silicates had been made in both domestic and overseas with quick development of functional materials.
In the text, three representative layered silicates are chosen as research objects, structural transformation and acid dissociation behaviors of aluminum of kaolinite, pyrophyllite and illite, were studied by Thermogravimetry-Differential scanning calorimetry (TG-DSC), Aluminum-27 Magic angle spinning nuclear magnetic resonance (Al MAS NMR), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) etc.. The results provide a theoretical base for preparation nanometer porous materials, high quality ceramics and fire resistance materials etc. by using layered silicates. It can be concluded as follows:
1) Thermal behaviors of aluminum of layered silicates
Kaolinite: Al-O octahedral sheets remain Al~Ⅵunder 450℃in kaolinite; hydroxyl groups are removed from 450℃to 550℃, kaolinite transforms to metakaolin, and Al~Ⅵchanges into Al~Ⅳ, Al~Ⅴbecause of dehydroxylation; from 550℃to 991℃, there exsits coordination of Al~Ⅳ, Al~Ⅴ, Al~Ⅵin metakaolin; accompanied by formation ofγ-Al_2O_3 and mullite above 991℃, the aluminum's structure changes to Al~Ⅵand Al~Ⅳ
Pyrophyllite: Phase composition is pyrophyllite with Al~Ⅵunder 500℃; between 500℃to 932℃, hydroxyl groups are removed, and pyrophyllite transforms into dehydrated pyrophyllite, whose coordinations of aluminum are Al~ⅣAl~Ⅴand Al~Ⅵ; from 932℃to 1141℃, aluminum's phase changes into dehydrated pyrophyllite and primary mullite; above 1141℃, the formation of mullite causes the change of aluminum structure to Al~Ⅳand Al~Ⅵ.
Illite: aluminum structures are Al~Ⅳand Al~Ⅵas a result of substitution of Al~(3+) for Si~(4+) in tetrahedra of illite below 543℃; from 543℃to 1001℃, OH groups are removed, and illite transforms into dehydrated illite with three aluminum structure of Al~Ⅳ, Al~Ⅴ, Al~Ⅵ, but few quantity of Al~Ⅴ, between 1001℃and 1181℃, and the main phases are dehydrated illite; above 1181℃, aluminum phases change into mullite with Al~Ⅳand Al~Ⅵ.
2) Acid dissociation behaviors of aluminum of thermally activated layered silicates
It was shown that the acid dissociation of aluminum of thermally activated kaolinte is better than those on activated pyrophyllite and activated illite.
Kaolinite: The acid dissociation of Al~Ⅵof kaolinite raw ore is bad, after thermal treatment, the acid dissociation properties of different coordination aluminum of metakaolin are different, Al~Ⅴof metokaolin is well, while Al~Ⅳand Al~Ⅵof metakaolin is bad; however, Al~Ⅳand Al~Ⅵofγ-Al_2O_3 and mullite are unable to dissolve in acid. Results obtained by acid dissociation shows a maximum Al_2O_3 leaching ratio of 97% can be obtained under the conditions of activating at 900℃for 15min, and acid leaching at 120℃for 120min with mass fraction 20% of HCl solution, and liquid/solid of 10. Specific surface area increases from 22.42 m /g of kaolinite to 304.84 m /g of leached kaolinite.
Pyrophyllite: When activation temperature goes up to 750℃, the acid dissociation of aluminum in pyrophyllite is improved; but the acid dissociation properties of aluminum in dehydrated pyrophyllite are very bad, Al~Ⅳand Al~Ⅵof mullite are unable to dissolve in acid. Results of acid dissociation show that Al_2O_3 leaching ratio reaches a maximum of 20.38% under the conditions of activating at 750℃for 15min, and acid leaching at 150℃for 120min with mass fraction 20% of H_2SO_4 solution, and leaching liquid/solid of 5.
Iillite: Compared to kaolinite and pyrophyllite, the acid dissociation properties of aluminum of thermally activated illite are the worst. The acid dissociation of illite is the best at the activating temperature of 650℃, few aluminum of dehydrated illite dissolves in acid, but Al~Ⅳand Al~Ⅵof mullite are unable to dissolve in acid. Results of acid dissociation show that Al_2O_3 leaching ratio reaches a maximum of 16.13% under the conditions of activating at 650℃for 15min, and acid leaching at 150℃for 120min with mass fraction 20% of H_2SO_4 solution, and leaching liquid/solid of 5.
本文选择了三种具有代表性的层状铝硅酸盐矿物：高岭石、叶蜡石和伊利石作为研究对象，综合运用热分析、X-射线衍射、红外光谱、固体核磁共振等分析方法，研究了这三种矿物中的铝在热处理过程中结构变化及在酸中的溶解行为。为以层状铝硅酸盐矿物为原材料制备多孔材料、高性能陶瓷和耐火材料等提供了理论指导，论文的主要结论如下：1)层状铝硅酸盐矿物中铝的热行为研究
高岭石：低于450℃时为高岭石阶段，结构为铝氧八面体，只存在Al~Ⅵ；450～550℃范围内发生脱羟基反应，高岭石中结构水被脱除，物相为高岭石和偏高岭石，存在Al~Ⅳ，Al~Ⅴ，Al~Ⅵ3种配位结构；550～991℃范围内为偏高岭石阶段，铝的3种配位结构依然存在；高于991℃时，逐渐生成γ-Al_2O_3和莫来石，Al~Ⅴ消失，只存在Al~Ⅳ和Al~Ⅵ。
叶蜡石：低于500℃时，主要物相为叶蜡石，只存在Al~Ⅵ；500-932℃之间，叶蜡石脱水，铝的物相为脱水叶蜡石和叶蜡石，且存在三种配位结构的铝：Al~Ⅳ、Al~Ⅴ和Al~Ⅵ；932-1141℃温度段，铝的物相主要为脱水叶蜡石和少量的初晶莫来石阶段；高于1141℃时，铝的物相为莫来石，只存在两种配位的铝：Al~Ⅳ和Al~Ⅵ。
伊利石：低于543℃时，物相为伊利石，由于存在四面体中的Al~(3+)替代Si~(4+)的影响，原矿中存在Al~Ⅵ和Al~Ⅳ，543-1001℃期间，伊利石脱除羟基，物相为伊利石和脱水伊利石，存在Al~Ⅴ、Al~Ⅵ和Al~Ⅳ，其中Al~Ⅴ的数量很少；1001-1181℃时，铝的主要物相为脱水伊利石；高于1181℃时，铝的主要物相为莫来石，铝的配位为Al~Ⅵ和Al~Ⅳ。
2)热活化后层状铝硅酸盐矿物中铝的酸溶行为研究
经热处理高岭石比叶蜡石和伊利石中的铝在酸中的溶解性能均要好。
高岭石：未经热活化的高岭石中Al~Ⅵ在酸中的溶解能力差；经过热活化后生成偏高岭石(Al~Ⅳ、Al~Ⅴ和Al~Ⅵ)，其中Al~Ⅴ在酸中的溶解最好，Al~Ⅳ和Al~Ⅵ在酸中能力较差；继续升高温度偏高岭石生成不溶于酸的γ-Al_2O_3和莫来石(Al~Ⅳ和Al~Ⅵ)，Al~Ⅳ和Al~Ⅵ在酸中的溶解很差。酸溶试验结果表明高岭石在活化温度为900℃，活化时间为15min，溶出温度为120℃，HCl质量分数为20％，溶出时间为120min，L／S为10时，Al_2O_3的溶出率可以达到最大值为97％。酸溶后，高岭石的比表面积由22．42 m~2／g上升到304．84m~2／g。
叶蜡石：未经过热活化的叶蜡石中铝在酸中的溶解能力差；经过热活化后，在750℃时，叶蜡石中铝在酸中的溶解能力相比整个热处理过程是最好的；脱水叶蜡石在酸中的溶解能力很差；到高温生成的莫来石中Al~Ⅳ和Al~Ⅵ不溶于酸。酸溶试验表明在活化温度为750℃，活化时间为15min，H_28O_4质量分数为20％，溶出温度为150℃，溶出时间为120min，L／S为5时，叶蜡石中Al_2O_3溶出率达到最大值为20．38％。
伊利石：相比高岭石和叶蜡石来说，伊利石中的铝在酸中的溶解性能最差。在650℃时，伊利石中铝在酸中的溶解能力在整个热处理过程中是最好的，脱水伊利石只有少量的铝溶于酸；到高温度生成的莫来石中Al~Ⅳ和Al~Ⅵ不溶于酸。酸溶试验的结果表明在活化温度为650min，活化时间为15min，H_2SO_4质量分数为20％，溶出温度为150℃，溶出时间为120 min，液固比(L／S)为10时，伊利石中Al_2O_3溶出率达到最大值为16．13％。
Most layered silicates are important nonmetallic minerals, and they are endowed with many process properties such as plasticity, fire resistance, and chemical stability etc. for their special crystal structure. They are widely used in fields of ceramic, rubber, coating, fire resistance materials etc. Nanometer porous material, high quality ceramics and fire resistance materials with layered silicates had been made in both domestic and overseas with quick development of functional materials.
In the text, three representative layered silicates are chosen as research objects, structural transformation and acid dissociation behaviors of aluminum of kaolinite, pyrophyllite and illite, were studied by Thermogravimetry-Differential scanning calorimetry (TG-DSC), Aluminum-27 Magic angle spinning nuclear magnetic resonance (Al MAS NMR), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) etc.. The results provide a theoretical base for preparation nanometer porous materials, high quality ceramics and fire resistance materials etc. by using layered silicates. It can be concluded as follows:
1) Thermal behaviors of aluminum of layered silicates
Kaolinite: Al-O octahedral sheets remain Al~Ⅵunder 450℃in kaolinite; hydroxyl groups are removed from 450℃to 550℃, kaolinite transforms to metakaolin, and Al~Ⅵchanges into Al~Ⅳ, Al~Ⅴbecause of dehydroxylation; from 550℃to 991℃, there exsits coordination of Al~Ⅳ, Al~Ⅴ, Al~Ⅵin metakaolin; accompanied by formation ofγ-Al_2O_3 and mullite above 991℃, the aluminum's structure changes to Al~Ⅵand Al~Ⅳ
Pyrophyllite: Phase composition is pyrophyllite with Al~Ⅵunder 500℃; between 500℃to 932℃, hydroxyl groups are removed, and pyrophyllite transforms into dehydrated pyrophyllite, whose coordinations of aluminum are Al~ⅣAl~Ⅴand Al~Ⅵ; from 932℃to 1141℃, aluminum's phase changes into dehydrated pyrophyllite and primary mullite; above 1141℃, the formation of mullite causes the change of aluminum structure to Al~Ⅳand Al~Ⅵ.
Illite: aluminum structures are Al~Ⅳand Al~Ⅵas a result of substitution of Al~(3+) for Si~(4+) in tetrahedra of illite below 543℃; from 543℃to 1001℃, OH groups are removed, and illite transforms into dehydrated illite with three aluminum structure of Al~Ⅳ, Al~Ⅴ, Al~Ⅵ, but few quantity of Al~Ⅴ, between 1001℃and 1181℃, and the main phases are dehydrated illite; above 1181℃, aluminum phases change into mullite with Al~Ⅳand Al~Ⅵ.
2) Acid dissociation behaviors of aluminum of thermally activated layered silicates
It was shown that the acid dissociation of aluminum of thermally activated kaolinte is better than those on activated pyrophyllite and activated illite.
Kaolinite: The acid dissociation of Al~Ⅵof kaolinite raw ore is bad, after thermal treatment, the acid dissociation properties of different coordination aluminum of metakaolin are different, Al~Ⅴof metokaolin is well, while Al~Ⅳand Al~Ⅵof metakaolin is bad; however, Al~Ⅳand Al~Ⅵofγ-Al_2O_3 and mullite are unable to dissolve in acid. Results obtained by acid dissociation shows a maximum Al_2O_3 leaching ratio of 97% can be obtained under the conditions of activating at 900℃for 15min, and acid leaching at 120℃for 120min with mass fraction 20% of HCl solution, and liquid/solid of 10. Specific surface area increases from 22.42 m /g of kaolinite to 304.84 m /g of leached kaolinite.
Pyrophyllite: When activation temperature goes up to 750℃, the acid dissociation of aluminum in pyrophyllite is improved; but the acid dissociation properties of aluminum in dehydrated pyrophyllite are very bad, Al~Ⅳand Al~Ⅵof mullite are unable to dissolve in acid. Results of acid dissociation show that Al_2O_3 leaching ratio reaches a maximum of 20.38% under the conditions of activating at 750℃for 15min, and acid leaching at 150℃for 120min with mass fraction 20% of H_2SO_4 solution, and leaching liquid/solid of 5.
Iillite: Compared to kaolinite and pyrophyllite, the acid dissociation properties of aluminum of thermally activated illite are the worst. The acid dissociation of illite is the best at the activating temperature of 650℃, few aluminum of dehydrated illite dissolves in acid, but Al~Ⅳand Al~Ⅵof mullite are unable to dissolve in acid. Results of acid dissociation show that Al_2O_3 leaching ratio reaches a maximum of 16.13% under the conditions of activating at 650℃for 15min, and acid leaching at 150℃for 120min with mass fraction 20% of H_2SO_4 solution, and leaching liquid/solid of 5.
引文
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