铝土矿选矿尾矿制备聚合物填料的研究
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摘要
铝土矿选矿尾矿是我国特有的有色金属尾矿,铝工业的发展遗留下来大量的尾矿,它的存在已成为制约矿业可持续发展、占用农田、林地、危及矿区及周边生态环境的主要因素。尾矿除含少量金属杂质外,主要矿物相结构与目前塑料填料市场所用的铝硅酸盐矿物结构类似,在塑料填料市场有着广阔的应用前景。
尾矿主要化学成分为三氧化二铝(Al_2O_3)和二氧化硅(SiO_2),质量百分比达70%;矿物相以一水硬铝石和高岭石为主,质量百分比达50%。该尾矿在选矿时已进行了磨矿,粒度较细(d_(90)≤65μm),易超细加工,本研究利用铝土矿选矿厂尾矿库里的矿浆作原料,烘干后,分别用干法和湿法两种方式对干粉进行超细加工,获得优化的粉磨工艺。粉磨后的粉体粒度均匀、d_(90)≤10μm、呈类球状、化学性质稳定、热稳定性好、有一定的阻燃能力,符合塑料填料的基本要求。
研究工作中采用钛酸酯偶联剂、硅烷偶联剂、硅油及季铵盐表面活性剂,对超细尾矿粉体进行表面处理,证明不同表面活性剂存在一个最佳用量范围,根据尾矿粉体特性,通过分析与比较,选用硅烷偶联剂(KH)钛酸酯偶联剂(NDZ)对粉体进行复合改性,效果显著,改性后粉体的活化指数为90%;润湿角为130°;吸油量为14ml/100g;粉体的分散性得到改善,比表面积由10.9m~2/g增加至11.7m~2/g。这些结果表明,表面处理改变了尾矿粉体的表面极性,其表面由亲水性变为疏水性,改性后的尾矿粉体以低聚态粒子形式存在,粉体的分散性得到改善;用红外光谱对改性尾矿粉体进行分析,发现改性填料在2959.71cm~(-1)存在偶联剂特征峰,说明尾矿粉体表面存在偶联剂化学键;扫描电镜(SEM)的形貌观察及能谱(EDAX)分析发现,尾矿中不同矿物表面结合改性剂具有选择性,一水硬铝石以NDZ为主,高岭石以KH为主。
选用处理较好的改性尾矿粉体,共混聚氯乙烯(PVC)基料,造粒、熔融挤出、制备PVC复合材料。对复合材料进行物理、力学、热性能研究,结果表明,填料发挥了其成分复杂的多组分效应,填充PVC复合材料的刚性和耐热性比纯PVC基体有所提高,在填料为40份时,流动加工性好;并且偶联剂有增塑、润滑作用,改性尾矿粉体能够均匀分散在PVC基体中,填充的PVC的力学性能好,悬臂梁缺口冲击强度为7.8kJ/m~2、拉伸强度为33.8MPa、断裂伸长率为17%、维卡软化温度为86.1℃。扫描电镜(SEM)的断面形貌观察发现,改性尾矿粉体填料具有成核作用,加入后不改变PVC基体的晶型,界面结合牢固,填料在PVC基体中相容性、润湿性好。PVC制品性能指标达到企业提供的标准,性能满足应用要求。本研究工作为提高铝土矿选矿尾矿的附加值,新材料的开发和环境治理提供新的思路,具有重要的意义。
Bauxite tailing is a kind of industrial solid waste, which results from the development of Al industry. It restricts the sustainable development of mining, occupys farmland and pollutes environment. Tailing contains a few metal impurities. Its main mineral structure is the same as layered aluminous silicate mineral which is .used as plastic filler. It has a broad market prospect.
The main chemical components of tailing are aluminum oxide (Al_2O_3) and silicon oxide(SiO_2), of which the content is as high as 70%. The main mineral phase of tailing includes diaspore and kaolin which take up as much as 50%. Tailing is easy for ultra-fine processing because of its small size (d_(90)≤65μm). The main study makes use of ore pulp as raw material. It is adopted both wet and dry ultra-fine processing in order to obtain excellent grinding technology. The size of tailing powder is homogeneous (d_(90)≤10μm); its morphology is near-spherical. It has stable chemical properties, good thermal stability and fire-resistant. It can meet the requirements of plastic filler.
The surface modification of tailing is respectively treated by titanic ester coupling agent, saline coupling agent, silicone oil and quaternary ammonium salt, which testifies that the content of different coupling agent exists an optimal range. According to analysis and comparison, titanic ester coupling agent and saline coupling agent were selected to modify composite, of which the effect of modification is good. Activation index is more than 90%; contact angle is as high as 130°; oil absorption is less than 14 ml/100g. The results show that the modification changes the polarity of the surface of tailing powder, which changes from hydrophilic to hydrophobic. Modified tailing powder is mostly in oligomic state and the dispersion degree is improved. In order to discuss modification mechanism, the unmodified and modified tailing powder are studied by IR. The bond at 2959.71cm~(-1) indicates the chemical band function between coupling agents and powder surface. Modified tailing powder is studied by SEM and EDAX, which show that the different mineral phase of tailing has selectivity to adsorb modifier, i.e., diaspore adsorbs NDZ, and kaolin adsorbs KH.
The best modified powder is added as filler in polyvinyl chloride (PVC) matrix to produce PVC composite by melt extrude. The physical, mechanical and thermal properties of PVC composite are studied. The results as follows: the filler has multi-component affection; the rigid and heat-resistant of filled PVC composite are improved. PVC composite owns well flow and process properties when the filler content is 40Phr; the coupling agents have plasticizing and lubricative effect; modified filler can be distributed uniformly in the PVC matrix, which finally determines the higher properties of the PVC composite: izod notched impact strength is 7.8kJ/m~2; tensile strength is 33.8MPa; break extensibility is 17%; vicat malacia temperature is 86.1℃. Break appearance is studied by SEM, which shows that the filler has nucleation effect, indicating a better compatibility between PVC and filler and stable associated interface. Properties of PVC composite meet the standard of enterprise. The study is important for increasing the added value of tailing, developing new material and protecting environment.
尾矿主要化学成分为三氧化二铝(Al_2O_3)和二氧化硅(SiO_2),质量百分比达70%;矿物相以一水硬铝石和高岭石为主,质量百分比达50%。该尾矿在选矿时已进行了磨矿,粒度较细(d_(90)≤65μm),易超细加工,本研究利用铝土矿选矿厂尾矿库里的矿浆作原料,烘干后,分别用干法和湿法两种方式对干粉进行超细加工,获得优化的粉磨工艺。粉磨后的粉体粒度均匀、d_(90)≤10μm、呈类球状、化学性质稳定、热稳定性好、有一定的阻燃能力,符合塑料填料的基本要求。
研究工作中采用钛酸酯偶联剂、硅烷偶联剂、硅油及季铵盐表面活性剂,对超细尾矿粉体进行表面处理,证明不同表面活性剂存在一个最佳用量范围,根据尾矿粉体特性,通过分析与比较,选用硅烷偶联剂(KH)钛酸酯偶联剂(NDZ)对粉体进行复合改性,效果显著,改性后粉体的活化指数为90%;润湿角为130°;吸油量为14ml/100g;粉体的分散性得到改善,比表面积由10.9m~2/g增加至11.7m~2/g。这些结果表明,表面处理改变了尾矿粉体的表面极性,其表面由亲水性变为疏水性,改性后的尾矿粉体以低聚态粒子形式存在,粉体的分散性得到改善;用红外光谱对改性尾矿粉体进行分析,发现改性填料在2959.71cm~(-1)存在偶联剂特征峰,说明尾矿粉体表面存在偶联剂化学键;扫描电镜(SEM)的形貌观察及能谱(EDAX)分析发现,尾矿中不同矿物表面结合改性剂具有选择性,一水硬铝石以NDZ为主,高岭石以KH为主。
选用处理较好的改性尾矿粉体,共混聚氯乙烯(PVC)基料,造粒、熔融挤出、制备PVC复合材料。对复合材料进行物理、力学、热性能研究,结果表明,填料发挥了其成分复杂的多组分效应,填充PVC复合材料的刚性和耐热性比纯PVC基体有所提高,在填料为40份时,流动加工性好;并且偶联剂有增塑、润滑作用,改性尾矿粉体能够均匀分散在PVC基体中,填充的PVC的力学性能好,悬臂梁缺口冲击强度为7.8kJ/m~2、拉伸强度为33.8MPa、断裂伸长率为17%、维卡软化温度为86.1℃。扫描电镜(SEM)的断面形貌观察发现,改性尾矿粉体填料具有成核作用,加入后不改变PVC基体的晶型,界面结合牢固,填料在PVC基体中相容性、润湿性好。PVC制品性能指标达到企业提供的标准,性能满足应用要求。本研究工作为提高铝土矿选矿尾矿的附加值,新材料的开发和环境治理提供新的思路,具有重要的意义。
Bauxite tailing is a kind of industrial solid waste, which results from the development of Al industry. It restricts the sustainable development of mining, occupys farmland and pollutes environment. Tailing contains a few metal impurities. Its main mineral structure is the same as layered aluminous silicate mineral which is .used as plastic filler. It has a broad market prospect.
The main chemical components of tailing are aluminum oxide (Al_2O_3) and silicon oxide(SiO_2), of which the content is as high as 70%. The main mineral phase of tailing includes diaspore and kaolin which take up as much as 50%. Tailing is easy for ultra-fine processing because of its small size (d_(90)≤65μm). The main study makes use of ore pulp as raw material. It is adopted both wet and dry ultra-fine processing in order to obtain excellent grinding technology. The size of tailing powder is homogeneous (d_(90)≤10μm); its morphology is near-spherical. It has stable chemical properties, good thermal stability and fire-resistant. It can meet the requirements of plastic filler.
The surface modification of tailing is respectively treated by titanic ester coupling agent, saline coupling agent, silicone oil and quaternary ammonium salt, which testifies that the content of different coupling agent exists an optimal range. According to analysis and comparison, titanic ester coupling agent and saline coupling agent were selected to modify composite, of which the effect of modification is good. Activation index is more than 90%; contact angle is as high as 130°; oil absorption is less than 14 ml/100g. The results show that the modification changes the polarity of the surface of tailing powder, which changes from hydrophilic to hydrophobic. Modified tailing powder is mostly in oligomic state and the dispersion degree is improved. In order to discuss modification mechanism, the unmodified and modified tailing powder are studied by IR. The bond at 2959.71cm~(-1) indicates the chemical band function between coupling agents and powder surface. Modified tailing powder is studied by SEM and EDAX, which show that the different mineral phase of tailing has selectivity to adsorb modifier, i.e., diaspore adsorbs NDZ, and kaolin adsorbs KH.
The best modified powder is added as filler in polyvinyl chloride (PVC) matrix to produce PVC composite by melt extrude. The physical, mechanical and thermal properties of PVC composite are studied. The results as follows: the filler has multi-component affection; the rigid and heat-resistant of filled PVC composite are improved. PVC composite owns well flow and process properties when the filler content is 40Phr; the coupling agents have plasticizing and lubricative effect; modified filler can be distributed uniformly in the PVC matrix, which finally determines the higher properties of the PVC composite: izod notched impact strength is 7.8kJ/m~2; tensile strength is 33.8MPa; break extensibility is 17%; vicat malacia temperature is 86.1℃. Break appearance is studied by SEM, which shows that the filler has nucleation effect, indicating a better compatibility between PVC and filler and stable associated interface. Properties of PVC composite meet the standard of enterprise. The study is important for increasing the added value of tailing, developing new material and protecting environment.
引文
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