超细粉体电气石机械力化学效应及表面改性的研究
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摘要
电气石是一种独特的自发电极性矿物,具有发射远红外和诱发负离子功能,广泛应用于环保、功能性纺织品及建材等领域。其超细粉体具有特殊的超细效应,但团聚现象严重影响其应用性能,因此提高其粉体分散性具有重要理论意义。
本文运用化学全分析、电子探针分析、ICP、X射线衍射分析、红外光谱测试、差热分析等分析方法对新疆阿勒泰云母二矿电气石的矿物学特征进行了测试,并对超细粉体电气石的制备工艺进行了研究,通过对新疆电气石矿物超细前后物化性质的分析,总结了超细前后电气石矿物粉体相关性质的变化规律,对产生变化的原因进行了探讨,为矿物粉体的利用提供了重要的基础数据,归纳总结了超细粉体电气石的机械力化学效应。最后利用沉降时间、沉降体积百分数、中位粒径分布、Zeta电位测定等手段,根据胶体的分散稳定理论选用不同类型分散剂(聚丙烯酸钠、聚丙烯酸钾,多聚磷酸钠、六偏磷酸钠,十二烷基苯磺酸钠)对超细粉体电气石进行表面改性,确定了最佳改性工艺条件,制备出在水溶液中具有良好分散性能的超细粉体,并对改性后样品进行静态负离子测试;最后采用FTIR、DTA-TC和SEM对表面改性后的超细粉体电气石结构和表面特性进行了表征和研究,对其在水中分散性和稳定性机理进行分析,建立了电气石表面的吸附模型,并提出水溶性表面改性剂与电气石的作用机理。
本文主要结论:该矿电气石样品为镁电气石;选用机械破碎法即采用介质搅拌磨连续磨矿、二阶段循环研磨的工艺,通过合理地使用研磨介质,优化工艺条件制备了粒度细、分布窄、颗粒形状规则的超细粉体,研磨60 min后粒径增加达到极限,最小粒径为0.619μm,所制得粉体比表面积最大值达33.47 m2/g。根据实验获得的中位粒径和比表面积随时间变化的数据,采用MATLAB程序进行超细粉碎曲线拟合研究,建立了相关数学模型。机械力化学效应研究表明:电气石在研磨过程中晶格发生膨胀,属晶格畸变范畴,电气石的一些振动精细结构消失,谱峰出现简并和宽化的特征,[SiO4]引起的谱带逐渐消失和红移;超细粉体除脱吸附水外的吸热效应的最大值温度有所降低,由原样的1004℃降低至907℃,降低幅度达97℃;超细粉碎后粉体矫顽力增大;超细粉碎导致晶格周期性的破坏,提高了晶格极性振动的非简谐效应,有效改善电气石在一定波长范围内的红外辐射率。负离子测试结果表明:随粒度减小,所诱生的负离子在一定程度上增多,但当粒径小到一定程度时则开始减小。
超细粉体电气石表面改性最佳工艺条件为:在改性实验温度83℃,pH值为11的条件下,改性剂为聚丙烯酸钠与多聚磷酸钠复配改性剂,最佳用量为1.8%(其中聚丙烯酸钠1.2%,多聚磷酸钠0.6%);改性助剂为白炭黑,最佳用量为4.0%。结果表明10wt%固含量电气石水分散体系的稳定性强烈地受分散剂的用量和pH值的影响。改性后粉体Zeta电位绝对值从9.5mv提高到28.6mv;改性后负离子增量提高达9.30%。FTIR和DTA-TG测试结果表明:改性剂聚丙烯酸钠与多聚磷酸钠与电气石表面的羟基产生键合作用,聚丙烯酸钠中的羧基(-COOH)与电气石颗粒表面的羟基(-OH)发生了脱水酯化反应,白炭黑则基本不引起电气石本身性质的变化。
改性机理为:改性剂赋予粒子表面较高的Zeta电位,增加粒子间的静电排斥作用,并在粒子表面形成空间稳定作用或空缺稳定作用,使粉体在水中的分散稳定性能提高。白炭黑吸附于粒子表面,可降低粒子间的液桥力,粒子间距增大,减少粒子的相互粘结,提高电气石的分散性能。电气石的吸附模型为:改性电气石的表面形成三种吸附层,内层为化学吸附层,改性剂与电气石表面的羟基产生作用;中层为物理吸附层;外层为改性助剂。改性剂分别以化学及物理吸附作用于电气石表面,白炭黑则充填于电气石之间。
本项研究为国家自然科学基金“极性矿物电气石与半导体氧化物(ZnO等)复合微粒的环境作用机理研究”及教育部高等院校博士学科点专项科研基金“环境材料电气石粉末覆膜强化机理研究”资助项目。
Tourmaline, one kind of unique spontaneous electropolar mineral, has the function of emitting far infrared rays and releasing anoin. Therefore it is widely applied in many fields such as environmental protection, functionality textile and building materials etc. Though ultrafine powder of tourmaline has special effects, its application performance is serious influenced by reuniting mutually. So it is important that enhances ultrafine powder of tourmaline's dispersivity. This article utilizes the chemistry analysis, EMPA, ICP, XRD, FTIR, DTA,TG analysis methods to carry on the test to mineralogy characteristic of tourmaline from Xinjiang Altay mica second mine, and has conducted the research to ultrafine powder of tourmaline's preparation craft. It has summaried ultrafine powder of tourmaline mechanochemical effects. Finally based on colloidal dispersion stabilization theory, by using sedimentation time, sedimentation volume, medium particle distribution, Zeta electric potential determination etc, it had investigated by employing sodium polyacyrlate, potassium polyacrylate (polymer surfactants), sodium polyphosphate, sodium hexametaphophate (inorganic), sodium dodecyl benzene sulfonate (organic) which carries on the superficial modification to ultrafine powder of tourmaline. Finally it has determined the best modified technological conditions. Using FTIR, DTA, TC and SEM, it has established ultrafine tourmaline’s stabilization mechanism andsurface adsorption model, and proposes water-soluble superficial modifier and tourmaline action mechanism. The contents of this dissertation are as follows:
Xinjiang Altay mica second mine tourmaline sample's is the magnesium tournaline. Through using grinding medium reasonably and optimization technological conditions, has gotten regular morphology ultrafine tourmaline which distributes narrowly. After grinding 60 min the particle size increases achieves the limit, and the minimum particle size is 0.619μm. The maximum specific surface area reaches 33.47 m2/g. Using MATLAB program to conduct ultrafine grinding curve fitting research to the tourmaline, has established its mathematical model.
After superfine, mechanochemical effects research indicated: the crystal lattice has the inflation in the process of lapping, but it is the lattice distortion category. The ultrafine grinding causes tourmaline some vibration fine structure vanishing and the peak to present the characteristic which degenerate and wide, the band which [SiO4] causes vanishes gradually and red shift. In the superfine process, the mechanical energy transforms to internal energy of tourmaline, which causes heat absorption effect maximum value temperature to have reduces (1004℃reduces by the original 907℃, reduces the scope to reach 97℃). Indicated to the smallest particle size tourmaline magnetism nature's research, tourmaline coercive force increases. The ultrafine grinding causes the crystal lattice periodic destruction, enhances the crystal lattice polarity vibration non-simple harmonics effect, and improves the tourmaline in certain wavelength range infrared emissivity effectively. The anoin test result indicated: Ultrafine powder of tourmaline produces the anoin increases to a certain extent. When the particle size slightly increases to certain extent, the anoin amount reduces.
The ultrafine powder of tourmaline superficial modification processing best modified formula and the technological conditions are: At temperature 83℃, pH is 11 conditions, compound modifier (sodium polyacyrlate gathered with sodium polyphosphate), the best amount used is 1.8% (sodium polyacyrlate 1.2%, gather sodium polyphosphate 0.6%).The modified assistant is silica, the best amount used is 4.0%. Dispersing agent member dissociation balanced related with pH value, also the dispersing agent member's dissociation balanced immediate influenced dispersing agent member's charged situation and the solution extension condition. Finally, affects the powder body's electrostaticstatic steric function. Results show that water dispersion system stability which has 10wt% tourmaline intensely is influenced by dispersing agent amount and pH value.
The test result indicated: compound modifier has bonding with tourmaline surface hydroxyl. Carboxyl in sodium polyacyrlate (-COOH) has had dehydrated esterification response with ultrafine tourmaline pellet surface hydroxyl (-OH). But silica basically does not change the tourmaline itself nature. Zeta electric potential's absolute value also enhances from 9.5mv to 28.6mv, therefore greatly enhanced electrostatic repulsion function between tourmaline.
According to analysising the modification mechanism, it has gotten the adsorption model of tourmaline. Modifier acts on tourmaline surface respectively by chemical adsorption and physisorption. Silica fills between tourmaline. When the sample disperses in the water, the modifier endows with ultrafine tourmaline surface high Zeta electric potential and increases the electrostatic repulsion function between the ultrafine tourmaline. In addition, it will also form steric stabilization or vacancy stabilization in the ultrafine tourmaline surface. Thus improve the stability of the powder dispersion in the water. Silica adsorption on the the ultrafine tourmaline surface, may reduce the fluid bridge strength between the granule.Thus the granule spacing increases, reducing mutual caking and enhancing dispersion. The modification mechanism is: The modified tourmaline's surface forms three kind of adsorbed layers. The inner layer is chemistry adsorbed layer, which modifier has reaction with tourmaline surface hydroxyl. The outer layer is the modifier assistant.
This research is subsidized project by NNSF“The compound particle's the polar mineral tourmaline with the semiconductor oxide (ZnO and so on) environment action mechanism research”and Ministry of Education institutions of universities for doctor subject the special scientific research foundation“The environment material tourmaline powder membrae tectoria strengthens the mechanism research”.
本文运用化学全分析、电子探针分析、ICP、X射线衍射分析、红外光谱测试、差热分析等分析方法对新疆阿勒泰云母二矿电气石的矿物学特征进行了测试,并对超细粉体电气石的制备工艺进行了研究,通过对新疆电气石矿物超细前后物化性质的分析,总结了超细前后电气石矿物粉体相关性质的变化规律,对产生变化的原因进行了探讨,为矿物粉体的利用提供了重要的基础数据,归纳总结了超细粉体电气石的机械力化学效应。最后利用沉降时间、沉降体积百分数、中位粒径分布、Zeta电位测定等手段,根据胶体的分散稳定理论选用不同类型分散剂(聚丙烯酸钠、聚丙烯酸钾,多聚磷酸钠、六偏磷酸钠,十二烷基苯磺酸钠)对超细粉体电气石进行表面改性,确定了最佳改性工艺条件,制备出在水溶液中具有良好分散性能的超细粉体,并对改性后样品进行静态负离子测试;最后采用FTIR、DTA-TC和SEM对表面改性后的超细粉体电气石结构和表面特性进行了表征和研究,对其在水中分散性和稳定性机理进行分析,建立了电气石表面的吸附模型,并提出水溶性表面改性剂与电气石的作用机理。
本文主要结论:该矿电气石样品为镁电气石;选用机械破碎法即采用介质搅拌磨连续磨矿、二阶段循环研磨的工艺,通过合理地使用研磨介质,优化工艺条件制备了粒度细、分布窄、颗粒形状规则的超细粉体,研磨60 min后粒径增加达到极限,最小粒径为0.619μm,所制得粉体比表面积最大值达33.47 m2/g。根据实验获得的中位粒径和比表面积随时间变化的数据,采用MATLAB程序进行超细粉碎曲线拟合研究,建立了相关数学模型。机械力化学效应研究表明:电气石在研磨过程中晶格发生膨胀,属晶格畸变范畴,电气石的一些振动精细结构消失,谱峰出现简并和宽化的特征,[SiO4]引起的谱带逐渐消失和红移;超细粉体除脱吸附水外的吸热效应的最大值温度有所降低,由原样的1004℃降低至907℃,降低幅度达97℃;超细粉碎后粉体矫顽力增大;超细粉碎导致晶格周期性的破坏,提高了晶格极性振动的非简谐效应,有效改善电气石在一定波长范围内的红外辐射率。负离子测试结果表明:随粒度减小,所诱生的负离子在一定程度上增多,但当粒径小到一定程度时则开始减小。
超细粉体电气石表面改性最佳工艺条件为:在改性实验温度83℃,pH值为11的条件下,改性剂为聚丙烯酸钠与多聚磷酸钠复配改性剂,最佳用量为1.8%(其中聚丙烯酸钠1.2%,多聚磷酸钠0.6%);改性助剂为白炭黑,最佳用量为4.0%。结果表明10wt%固含量电气石水分散体系的稳定性强烈地受分散剂的用量和pH值的影响。改性后粉体Zeta电位绝对值从9.5mv提高到28.6mv;改性后负离子增量提高达9.30%。FTIR和DTA-TG测试结果表明:改性剂聚丙烯酸钠与多聚磷酸钠与电气石表面的羟基产生键合作用,聚丙烯酸钠中的羧基(-COOH)与电气石颗粒表面的羟基(-OH)发生了脱水酯化反应,白炭黑则基本不引起电气石本身性质的变化。
改性机理为:改性剂赋予粒子表面较高的Zeta电位,增加粒子间的静电排斥作用,并在粒子表面形成空间稳定作用或空缺稳定作用,使粉体在水中的分散稳定性能提高。白炭黑吸附于粒子表面,可降低粒子间的液桥力,粒子间距增大,减少粒子的相互粘结,提高电气石的分散性能。电气石的吸附模型为:改性电气石的表面形成三种吸附层,内层为化学吸附层,改性剂与电气石表面的羟基产生作用;中层为物理吸附层;外层为改性助剂。改性剂分别以化学及物理吸附作用于电气石表面,白炭黑则充填于电气石之间。
本项研究为国家自然科学基金“极性矿物电气石与半导体氧化物(ZnO等)复合微粒的环境作用机理研究”及教育部高等院校博士学科点专项科研基金“环境材料电气石粉末覆膜强化机理研究”资助项目。
Tourmaline, one kind of unique spontaneous electropolar mineral, has the function of emitting far infrared rays and releasing anoin. Therefore it is widely applied in many fields such as environmental protection, functionality textile and building materials etc. Though ultrafine powder of tourmaline has special effects, its application performance is serious influenced by reuniting mutually. So it is important that enhances ultrafine powder of tourmaline's dispersivity. This article utilizes the chemistry analysis, EMPA, ICP, XRD, FTIR, DTA,TG analysis methods to carry on the test to mineralogy characteristic of tourmaline from Xinjiang Altay mica second mine, and has conducted the research to ultrafine powder of tourmaline's preparation craft. It has summaried ultrafine powder of tourmaline mechanochemical effects. Finally based on colloidal dispersion stabilization theory, by using sedimentation time, sedimentation volume, medium particle distribution, Zeta electric potential determination etc, it had investigated by employing sodium polyacyrlate, potassium polyacrylate (polymer surfactants), sodium polyphosphate, sodium hexametaphophate (inorganic), sodium dodecyl benzene sulfonate (organic) which carries on the superficial modification to ultrafine powder of tourmaline. Finally it has determined the best modified technological conditions. Using FTIR, DTA, TC and SEM, it has established ultrafine tourmaline’s stabilization mechanism andsurface adsorption model, and proposes water-soluble superficial modifier and tourmaline action mechanism. The contents of this dissertation are as follows:
Xinjiang Altay mica second mine tourmaline sample's is the magnesium tournaline. Through using grinding medium reasonably and optimization technological conditions, has gotten regular morphology ultrafine tourmaline which distributes narrowly. After grinding 60 min the particle size increases achieves the limit, and the minimum particle size is 0.619μm. The maximum specific surface area reaches 33.47 m2/g. Using MATLAB program to conduct ultrafine grinding curve fitting research to the tourmaline, has established its mathematical model.
After superfine, mechanochemical effects research indicated: the crystal lattice has the inflation in the process of lapping, but it is the lattice distortion category. The ultrafine grinding causes tourmaline some vibration fine structure vanishing and the peak to present the characteristic which degenerate and wide, the band which [SiO4] causes vanishes gradually and red shift. In the superfine process, the mechanical energy transforms to internal energy of tourmaline, which causes heat absorption effect maximum value temperature to have reduces (1004℃reduces by the original 907℃, reduces the scope to reach 97℃). Indicated to the smallest particle size tourmaline magnetism nature's research, tourmaline coercive force increases. The ultrafine grinding causes the crystal lattice periodic destruction, enhances the crystal lattice polarity vibration non-simple harmonics effect, and improves the tourmaline in certain wavelength range infrared emissivity effectively. The anoin test result indicated: Ultrafine powder of tourmaline produces the anoin increases to a certain extent. When the particle size slightly increases to certain extent, the anoin amount reduces.
The ultrafine powder of tourmaline superficial modification processing best modified formula and the technological conditions are: At temperature 83℃, pH is 11 conditions, compound modifier (sodium polyacyrlate gathered with sodium polyphosphate), the best amount used is 1.8% (sodium polyacyrlate 1.2%, gather sodium polyphosphate 0.6%).The modified assistant is silica, the best amount used is 4.0%. Dispersing agent member dissociation balanced related with pH value, also the dispersing agent member's dissociation balanced immediate influenced dispersing agent member's charged situation and the solution extension condition. Finally, affects the powder body's electrostaticstatic steric function. Results show that water dispersion system stability which has 10wt% tourmaline intensely is influenced by dispersing agent amount and pH value.
The test result indicated: compound modifier has bonding with tourmaline surface hydroxyl. Carboxyl in sodium polyacyrlate (-COOH) has had dehydrated esterification response with ultrafine tourmaline pellet surface hydroxyl (-OH). But silica basically does not change the tourmaline itself nature. Zeta electric potential's absolute value also enhances from 9.5mv to 28.6mv, therefore greatly enhanced electrostatic repulsion function between tourmaline.
According to analysising the modification mechanism, it has gotten the adsorption model of tourmaline. Modifier acts on tourmaline surface respectively by chemical adsorption and physisorption. Silica fills between tourmaline. When the sample disperses in the water, the modifier endows with ultrafine tourmaline surface high Zeta electric potential and increases the electrostatic repulsion function between the ultrafine tourmaline. In addition, it will also form steric stabilization or vacancy stabilization in the ultrafine tourmaline surface. Thus improve the stability of the powder dispersion in the water. Silica adsorption on the the ultrafine tourmaline surface, may reduce the fluid bridge strength between the granule.Thus the granule spacing increases, reducing mutual caking and enhancing dispersion. The modification mechanism is: The modified tourmaline's surface forms three kind of adsorbed layers. The inner layer is chemistry adsorbed layer, which modifier has reaction with tourmaline surface hydroxyl. The outer layer is the modifier assistant.
This research is subsidized project by NNSF“The compound particle's the polar mineral tourmaline with the semiconductor oxide (ZnO and so on) environment action mechanism research”and Ministry of Education institutions of universities for doctor subject the special scientific research foundation“The environment material tourmaline powder membrae tectoria strengthens the mechanism research”.
引文
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