一水硬铝石和层状硅酸盐矿物的晶体结构与表面性质研究
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摘要
根据矿物学、晶体化学、表面化学和浮选理论，通过浮选实验、Zeta电位及接触角测定，采用红外光谱、X射线衍射、偏光显微镜、扫描电子显微镜、原子力显微镜等近代和现代测试方法，对一水硬铝石和二八面体型层状硅酸盐矿物的晶体结构、化学组成与表面润湿性、电性、可浮性及药剂作用机理进行了研究。
由晶体化学计算可知，高岭石、叶蜡石和伊利石三种矿物晶体端面上单位面积断裂键数皆有如下关系：N_(Si-O(110)＜N_(Si-O(010)＜NSi-O(100)，N_(Al-O(110)＜N_(Al-O(010)＜N_(Al-O(100)，从理论上解释了高岭石、叶蜡石和伊利石三种矿物晶体端面上晶面润湿性的各向异性。矿物晶体底面(001)层间静电能的大小决定其层面润湿性，其大小关系为：高岭石(TOa型)≥伊利石(TOaT型(含层间阳离子))＞叶蜡石(TOaT型)。矿物亲水性大小关系为：高岭石≈伊利石＞叶蜡石；与接触角测试的结果一致。并解释了在几种常规捕收剂作用下，矿物表面润湿性的变化规律。
对于一水硬铝石矿物来说，三个主要晶面(010)、(100)和(001)上的单位面积断裂键数有如下关系：N_(Al-O(010)＜N_(Al-O(100)＜N_(Al-O(001)；一水硬铝石表面吸附的动力学模拟可以说明，一水硬铝石的(010)晶面、(100)晶面和(001)晶面，分别吸附几种捕收剂离子的吸附能(负值)大小为：(010)晶面的吸附能＞(100)晶面的吸附能＞(001)晶面的吸附能；分别吸附这些药剂离子的单位面积吸附量
(molecules·cell一，·nm一，)的大小顺序为:(010)晶面>(100)晶面>
(001)晶面。由对一水硬铝石矿物与油酸钠作用前后表面原子力-
位移曲线分析，定量地计算出其表面的平均粘附力和单位面积上平均
粘附能的大小，与接触角测试的结果一致;揭示经捕收剂作用之后，
一水硬铝石由高能表面变为低能表面。
通过红外光谱分析可知，十二胺(阳离子捕收剂)和油酸钠(阴
离子捕收剂)在一水硬铝石、高岭石、伊利石和叶蜡石表面的吸附主
要以静电力作用的物理吸附为主，与矿物的表面电性有关。
通过测定多种一水硬铝石的主要化学组成和相应的表面等电点
(l’eP)值，发现一水硬铝石在蒸馏水中的ieP值与其铝硅比值线性相
关，随铝硅比增大，其ieP值增大，并拟和出了一水硬铝石表面等电
点值的经验公式为:i印(cal)‘=一20.3 X 5102(矶%)+7.74 X A12O3(wt%)
+18.8 X TioZ伪沈%)。高岭石、伊利石和叶蜡石这三种二八面体型层
状硅酸盐矿物的结构单元层结构由TOa型、TOaT型(含层间阳离
子)至TOaT型，(A12O3/5102)比值由0.86变为0.42，其表面Zeta
电位值则相应地减少了，而与其层间电荷面密度关系不大。矿物端面
的理论表面零电点(Pz。)值的大小顺序为:高岭石(7 .76)>伊利
石(6.84))叶蜡石(6.26)。
硬质和软质高岭土具有相近的表面等电点(l’eP)值，几种硬质高
岭土的ieP值变化范围为2.6一3.8。在较宽的pH值范围，硬质高岭土
比软质高岭土的电位低。ieP值与其中510:的重量百分含量(wt%)
呈负相关，与A12O3的，沈%呈正相关，而高岭石的结晶度指数(HI)
并不是决定高岭石l’eP值的主要因数。在高岭石晶体端面上等电点
处，高岭土表面的Zeta电位与T Fe的叭沈%呈负相关性，与高岭石的
结晶度指数(扭)呈正相关。
通过DLVO理论计算，分析了高岭石、伊利石和叶蜡石三种二
八面体型层状硅酸盐矿物片状颗粒在水溶液中的团聚与分散行为，在
酸性溶液中主要以“端面一底面，，形式团聚，在中性溶液中主要以“端面
一底面”、“端面一端面”形式存在，在碱性溶液中主要以分散的形式存
在，与沉降实验和SEM观察结果基本一致。
In this work, the studies relating to the crystal structure, chemical composition wettability, electrokinetics and floatability of diaspore and dioctahedral phyllosilicates as well as the mechanisms of their interactions with flotation reagents were carried out. It was based on mineralogy, crystal chemistry, surface chemistry and flotation theory, with the help of the zeta potential measurement, contact angle measurement, flotation test, polar microscope, scanning electron microscope, X-ray diffraction, infrared spectroscopy and atomic force microscope.
The number of the broken bonds per unit area for different crystal planes of kaolinite, pyrophyllite and illite, which was calculated by crystal chemistry of the minerals, is in the order of Nsi-O(110)= illite > pyrophyllite, the same with the order of hydrophilicity. The results were approximately consistent with the measured value of contact angles.
The wettability of minerals is interpreted in the absence and presence of collectors.
Among the three crystal planes in diaspore, the number of Al-O broken bond per unit area in the crystal plane subject to the following order: NAMXOOI) > NAI-OOOO) > NAI-O(OIO)- The molecule kinetics method was employed to simulate the adsorption of the collectors on diaspore. Adsorptive energy and adsorptive capacity of the collectors on the various surfaces of diaspore were in the order of (010)>(100)>(001). The atomic force microscope (AFM) was used to measure the adhesional energy per area and surface force on the diaspore interface in the absence and presence of collector (sodium oleate). The results were approximately consistent with the measured value of contact angles. It showed that diaspore was turned from high energy surface to low energy surface after interacting with collectors.
With the help of infrared spectroscopy, it is known that the linkage between dodecylamine (cationic collector) and sodium oleate (anionic collector) and diaspore, kaolinite, illite and pyrophyllite is fundamentally electrostatic forces, which contributes to physical adsorption. The adsorption is related with surface electric property of minerals.
The effect of chemical composition of diaspores on their electrokinetics was investigated. Increasing Si2 content in a diaspore sample was found to decrease its iso-electric point (iep). A linear
correlation appeared to exist between the measured iso-electric point and alumina to silica mass ratio in diaspore samples. A empirical equation of iep for diaspore was conducted below: zep(cal),- = -20.3xSiO2(wt%) + 7.74xAl2O3(wt%)+18.8xTiO2(wt%). The structure layer turns from TOa type to TOaT type ( balanced by interlamellar cations ) , then to TOaT type for kaolinite , illite and pyrophyllite, respectively; alumina to silica mass ratio turns from 0.86 to 0.42; the surface zeta potentials turn small, but they show little relation with their surface charge density. The decreasing order of the measured iep or calculated pzc from kaolinite to illite, and then to pyrophyllite correlated well with that of the number of broken Al-O bonds and the ratio of broken Al-O to Si-O bonds. The calculated point of zero charge (pzc} of edge plane is in the order of kaolinite (7.76) > illite (6.84) > pyrophyllite (6.26).
The surface zeta potential variation of hard kaolin as a function of pH was almost the same as that of soft kaolin. The iep of hard kaolin varied from 2.5 to 3.8. SiO2(wt%) of the severa
由晶体化学计算可知，高岭石、叶蜡石和伊利石三种矿物晶体端面上单位面积断裂键数皆有如下关系：N_(Si-O(110)＜N_(Si-O(010)＜NSi-O(100)，N_(Al-O(110)＜N_(Al-O(010)＜N_(Al-O(100)，从理论上解释了高岭石、叶蜡石和伊利石三种矿物晶体端面上晶面润湿性的各向异性。矿物晶体底面(001)层间静电能的大小决定其层面润湿性，其大小关系为：高岭石(TOa型)≥伊利石(TOaT型(含层间阳离子))＞叶蜡石(TOaT型)。矿物亲水性大小关系为：高岭石≈伊利石＞叶蜡石；与接触角测试的结果一致。并解释了在几种常规捕收剂作用下，矿物表面润湿性的变化规律。
对于一水硬铝石矿物来说，三个主要晶面(010)、(100)和(001)上的单位面积断裂键数有如下关系：N_(Al-O(010)＜N_(Al-O(100)＜N_(Al-O(001)；一水硬铝石表面吸附的动力学模拟可以说明，一水硬铝石的(010)晶面、(100)晶面和(001)晶面，分别吸附几种捕收剂离子的吸附能(负值)大小为：(010)晶面的吸附能＞(100)晶面的吸附能＞(001)晶面的吸附能；分别吸附这些药剂离子的单位面积吸附量
(molecules·cell一，·nm一，)的大小顺序为:(010)晶面>(100)晶面>
(001)晶面。由对一水硬铝石矿物与油酸钠作用前后表面原子力-
位移曲线分析，定量地计算出其表面的平均粘附力和单位面积上平均
粘附能的大小，与接触角测试的结果一致;揭示经捕收剂作用之后，
一水硬铝石由高能表面变为低能表面。
通过红外光谱分析可知，十二胺(阳离子捕收剂)和油酸钠(阴
离子捕收剂)在一水硬铝石、高岭石、伊利石和叶蜡石表面的吸附主
要以静电力作用的物理吸附为主，与矿物的表面电性有关。
通过测定多种一水硬铝石的主要化学组成和相应的表面等电点
(l’eP)值，发现一水硬铝石在蒸馏水中的ieP值与其铝硅比值线性相
关，随铝硅比增大，其ieP值增大，并拟和出了一水硬铝石表面等电
点值的经验公式为:i印(cal)‘=一20.3 X 5102(矶%)+7.74 X A12O3(wt%)
+18.8 X TioZ伪沈%)。高岭石、伊利石和叶蜡石这三种二八面体型层
状硅酸盐矿物的结构单元层结构由TOa型、TOaT型(含层间阳离
子)至TOaT型，(A12O3/5102)比值由0.86变为0.42，其表面Zeta
电位值则相应地减少了，而与其层间电荷面密度关系不大。矿物端面
的理论表面零电点(Pz。)值的大小顺序为:高岭石(7 .76)>伊利
石(6.84))叶蜡石(6.26)。
硬质和软质高岭土具有相近的表面等电点(l’eP)值，几种硬质高
岭土的ieP值变化范围为2.6一3.8。在较宽的pH值范围，硬质高岭土
比软质高岭土的电位低。ieP值与其中510:的重量百分含量(wt%)
呈负相关，与A12O3的，沈%呈正相关，而高岭石的结晶度指数(HI)
并不是决定高岭石l’eP值的主要因数。在高岭石晶体端面上等电点
处，高岭土表面的Zeta电位与T Fe的叭沈%呈负相关性，与高岭石的
结晶度指数(扭)呈正相关。
通过DLVO理论计算，分析了高岭石、伊利石和叶蜡石三种二
八面体型层状硅酸盐矿物片状颗粒在水溶液中的团聚与分散行为，在
酸性溶液中主要以“端面一底面，，形式团聚，在中性溶液中主要以“端面
一底面”、“端面一端面”形式存在，在碱性溶液中主要以分散的形式存
在，与沉降实验和SEM观察结果基本一致。
In this work, the studies relating to the crystal structure, chemical composition wettability, electrokinetics and floatability of diaspore and dioctahedral phyllosilicates as well as the mechanisms of their interactions with flotation reagents were carried out. It was based on mineralogy, crystal chemistry, surface chemistry and flotation theory, with the help of the zeta potential measurement, contact angle measurement, flotation test, polar microscope, scanning electron microscope, X-ray diffraction, infrared spectroscopy and atomic force microscope.
The number of the broken bonds per unit area for different crystal planes of kaolinite, pyrophyllite and illite, which was calculated by crystal chemistry of the minerals, is in the order of Nsi-O(110)
The wettability of minerals is interpreted in the absence and presence of collectors.
Among the three crystal planes in diaspore, the number of Al-O broken bond per unit area in the crystal plane subject to the following order: NAMXOOI) > NAI-OOOO) > NAI-O(OIO)- The molecule kinetics method was employed to simulate the adsorption of the collectors on diaspore. Adsorptive energy and adsorptive capacity of the collectors on the various surfaces of diaspore were in the order of (010)>(100)>(001). The atomic force microscope (AFM) was used to measure the adhesional energy per area and surface force on the diaspore interface in the absence and presence of collector (sodium oleate). The results were approximately consistent with the measured value of contact angles. It showed that diaspore was turned from high energy surface to low energy surface after interacting with collectors.
With the help of infrared spectroscopy, it is known that the linkage between dodecylamine (cationic collector) and sodium oleate (anionic collector) and diaspore, kaolinite, illite and pyrophyllite is fundamentally electrostatic forces, which contributes to physical adsorption. The adsorption is related with surface electric property of minerals.
The effect of chemical composition of diaspores on their electrokinetics was investigated. Increasing Si2 content in a diaspore sample was found to decrease its iso-electric point (iep). A linear
correlation appeared to exist between the measured iso-electric point and alumina to silica mass ratio in diaspore samples. A empirical equation of iep for diaspore was conducted below: zep(cal),- = -20.3xSiO2(wt%) + 7.74xAl2O3(wt%)+18.8xTiO2(wt%). The structure layer turns from TOa type to TOaT type ( balanced by interlamellar cations ) , then to TOaT type for kaolinite , illite and pyrophyllite, respectively; alumina to silica mass ratio turns from 0.86 to 0.42; the surface zeta potentials turn small, but they show little relation with their surface charge density. The decreasing order of the measured iep or calculated pzc from kaolinite to illite, and then to pyrophyllite correlated well with that of the number of broken Al-O bonds and the ratio of broken Al-O to Si-O bonds. The calculated point of zero charge (pzc} of edge plane is in the order of kaolinite (7.76) > illite (6.84) > pyrophyllite (6.26).
The surface zeta potential variation of hard kaolin as a function of pH was almost the same as that of soft kaolin. The iep of hard kaolin varied from 2.5 to 3.8. SiO2(wt%) of the severa
引文
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