运用铝土矿选矿尾矿制备功能性颜填料及其应用性能
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摘要
铝土矿选矿尾矿具有产出量大、粒度细、成分复杂的特点,能否对其合理应用关系到“选矿-拜耳法”新工艺的推广。高的铁含量及常规除铁法的不经济限制了其在耐火材料和建材中的应用。因此,作为填料应用于高聚物应是一较有前景的利用方向之一。然其较深的颜色限制了其大规模应用,故需寻找简单经济的增白方法。
依据铁的磷酸盐为白色或浅黄白色的事实,采用将磷酸与尾矿反应再煅烧除碳的工艺流程对尾矿进行了增白处理。磷酸加入量和煅烧温度是影响增白尾矿白度的关键因素。煅烧温度对尾矿白度的影响视磷酸用量的多少而不同：在磷酸用量不足的情况下,煅烧温度对白度几乎无影响；在磷酸用量充足的情况下,白度随煅烧温度的升高而增大,至550℃达到最大值72%后随煅烧温度的升高而降低。煅烧温度均为550℃C时,白度随磷酸加入量的增加而增大,但增加幅度减小,磷含量达到4.5%时,白度基本不再随磷含量的增加而变化。
增白尾矿大部分颗粒表面由于包裹了一层磷酸盐,颗粒表面酸碱性质得到改善,因而对聚氯乙烯热稳定性影响较小,但其仍然显著影响聚氯乙烯的热降解及其燃烧性能。增白尾矿降低了聚氯乙烯在氩气中的降解温度,减弱了挥发性气体HCl及芳香族化合物苯的释出量,增大了降解反应的活化能及频率因子,减少了聚氯乙烯在第一降解阶段的质量损失；增白尾矿降低了聚氯乙烯在空气中的第一降解阶段温度和第三降解阶段温度,提高了第二降解阶段温度,减弱了有毒气体HCl及芳香族化合物苯的释出量,增大了各降解阶段的反应活化能及频率因子减少了聚氯乙烯在第二降解阶段的质量损失。增白尾矿减小了聚氯乙烯燃烧时的总释烟量、总释热量及质量损失速率,缩短了聚氯乙烯的引燃时间。
采用干法表面化学反应法和湿化学法对增白尾矿粉体进行了改性处理。在改性剂相同的情况下,湿法改性效果优于干法改性效果；在其它改性条件相同的情况下,混合改性剂的改性效果优于单一改性剂的改性效果。湿法改性中当改性剂的比例为0.4：1.6时,活化指数达到较大值80%。改性后的增白尾矿在聚氯乙烯中的分散性及界面结合状态得到改善,对基体力学性能的影响减小。
运用铝土矿选矿尾矿和磷酸为原料,在磷铝摩尔比为2.5,缩聚温度为300℃C,缩聚时间8h的条件下,制备了片状形貌的三聚磷酸铝。分别运用滑石、氧化锌及硅灰石对所制备的三聚磷酸铝进行改性以改善颜料pH值,运用常规测试方法及电化学方法比较了改性三聚磷酸铝与商品防腐颜料磷酸锌的防腐性能。氧化锌改性三聚磷酸铝具有最优的防腐性能,在其饱和液中浸泡48h的钢板表面仅发生非扩散性点腐蚀。涂有含氧化锌改性三聚磷酸铝颜料涂层的钢板,在3.5%NaCl电解液中浸泡初期的阻抗为108Ω.cm-2,20天时降为6.5×107Ω.cm-2,20天后稍有上升,浸泡40天时阻抗上升至7×107Ω.cm-2
Bauxite tailings with the characteristics of a large amount of the output, fine grain size and complex components, whether it can been reasonably recycled relates to the promotion of new technology of " beneficiation-Bayer ". High iron content and being impracticable for removing iron from bauxite-tailings by conventional methods limit its application in refractory and building materials. Therefore, as fillers in polymer should be more promising directions. However, its deeper color limits its large-scale applications, so need to find a simple and economic method to whiten bauxite tailings.
According to the facts that iron phosphate being white or yellow white, bauxite tailings were whitened by using the process route of phosphoric acid to react with bauxite tailings and then the reaction products being calcined for removal carbon. The addition amount of phosphoric acid and calcination temperature is the key factors to affect on the whiteness of bauxite tailings. The effects of calcination temperature on whiteness largely depend on the amount of phosphoric acid phosphate:the whiteness of bauxite tailings almost can't been improved through the calcination in the insufficient dosage of phosphoric acid; while, the whiteness firstly increase, reach the maximum of72%at550℃, then decrease with calcination temperature in sufficient dosage of phosphoric acid conditions.
The phosphate coated with most particles of whitening bauxite tailings meliorate the superficial acid and alkali nature of particles of bauxite tailings, so less effect on the thermal stability of polyvinyl chloride(PVC), but it still significantly influences the thermal degradation and combustion performance of PVC. The whitening tailings reduced the degradation temperature of PVC, weakened release quantity of volatile gases HCl and aromatic compounds benzene, increased the activation energy and frequency factor of degradation reaction, and reduced the mass loss in the first degradation stage of polyvinyl chloride when PVC degraded in argon; The whitening tailings reduced the temperatures of the first degradation stage and the third stage of PVC, improved the temperature of the second degradation stage, weakened the release volume of toxic gases HC1and aromatic compounds benzene, reduced the mass loss of the second degradation stage, decreased the activation energy and frequency factor of the first degradation stage, and increased the activation energy of the second degradation stage when PVC degraded in air. The whitening tailings decreased the total smoke released, total heat released and the ratio of mass loss and shorten the ignition time when PVC combusted.
The whitening bauxite tailings were modified by using surface chemical reaction of dry method and wet chemical method. The modification effect of the wet chemical method is better than the one of dry method at the same modifier being used. The modification effect of mixture of different modifier used is better than the one of a single modifier used under the same other modification conditions. In experiment, the largest activation index obtained is80%, when modifier ratio of0.4:1.6and wet chemical method were used. The dispersion of the modified whitening tailings in PVC and the interface bonding condition were improved, the influences on mechanics properties of matrix was reduced after the bauxite tailings modification.
Aluminum tri-polyphosphate was synthesized from bauxite tailings and phosphoric acid when P/Al molar ratio of2.5, condensation temperature of300℃and condensation time of8h. Talc, zinc oxide and wollastonite were respectively used to modify the aluminum tripolyphosphate in order to meliorate the pH value of aluminum tripolyphosphate. The possibility of using modified aluminum tripolyphosphate as an anticorrosive pigment was also investigated by routine method and electrochemical impedance spectroscopy. Zinc oxide modified aluminum tripolyphosphate has the best corrosion resistance. Steel board dipping in the saturated solution of zinc oxide modified aluminum tripolyphosphate for48h occured only non-proliferation of pitting corrosion. The impedance of steel board with coating with zinc oxide modified aluminum tripolyphosphate pigment was108Ω.cm-2in first immersion stage, down to6.5×107Ω.cm-2at immersion of20days and increase to7×107Ωcm-2up to immersion for40days.
依据铁的磷酸盐为白色或浅黄白色的事实,采用将磷酸与尾矿反应再煅烧除碳的工艺流程对尾矿进行了增白处理。磷酸加入量和煅烧温度是影响增白尾矿白度的关键因素。煅烧温度对尾矿白度的影响视磷酸用量的多少而不同：在磷酸用量不足的情况下,煅烧温度对白度几乎无影响；在磷酸用量充足的情况下,白度随煅烧温度的升高而增大,至550℃达到最大值72%后随煅烧温度的升高而降低。煅烧温度均为550℃C时,白度随磷酸加入量的增加而增大,但增加幅度减小,磷含量达到4.5%时,白度基本不再随磷含量的增加而变化。
增白尾矿大部分颗粒表面由于包裹了一层磷酸盐,颗粒表面酸碱性质得到改善,因而对聚氯乙烯热稳定性影响较小,但其仍然显著影响聚氯乙烯的热降解及其燃烧性能。增白尾矿降低了聚氯乙烯在氩气中的降解温度,减弱了挥发性气体HCl及芳香族化合物苯的释出量,增大了降解反应的活化能及频率因子,减少了聚氯乙烯在第一降解阶段的质量损失；增白尾矿降低了聚氯乙烯在空气中的第一降解阶段温度和第三降解阶段温度,提高了第二降解阶段温度,减弱了有毒气体HCl及芳香族化合物苯的释出量,增大了各降解阶段的反应活化能及频率因子减少了聚氯乙烯在第二降解阶段的质量损失。增白尾矿减小了聚氯乙烯燃烧时的总释烟量、总释热量及质量损失速率,缩短了聚氯乙烯的引燃时间。
采用干法表面化学反应法和湿化学法对增白尾矿粉体进行了改性处理。在改性剂相同的情况下,湿法改性效果优于干法改性效果；在其它改性条件相同的情况下,混合改性剂的改性效果优于单一改性剂的改性效果。湿法改性中当改性剂的比例为0.4：1.6时,活化指数达到较大值80%。改性后的增白尾矿在聚氯乙烯中的分散性及界面结合状态得到改善,对基体力学性能的影响减小。
运用铝土矿选矿尾矿和磷酸为原料,在磷铝摩尔比为2.5,缩聚温度为300℃C,缩聚时间8h的条件下,制备了片状形貌的三聚磷酸铝。分别运用滑石、氧化锌及硅灰石对所制备的三聚磷酸铝进行改性以改善颜料pH值,运用常规测试方法及电化学方法比较了改性三聚磷酸铝与商品防腐颜料磷酸锌的防腐性能。氧化锌改性三聚磷酸铝具有最优的防腐性能,在其饱和液中浸泡48h的钢板表面仅发生非扩散性点腐蚀。涂有含氧化锌改性三聚磷酸铝颜料涂层的钢板,在3.5%NaCl电解液中浸泡初期的阻抗为108Ω.cm-2,20天时降为6.5×107Ω.cm-2,20天后稍有上升,浸泡40天时阻抗上升至7×107Ω.cm-2
Bauxite tailings with the characteristics of a large amount of the output, fine grain size and complex components, whether it can been reasonably recycled relates to the promotion of new technology of " beneficiation-Bayer ". High iron content and being impracticable for removing iron from bauxite-tailings by conventional methods limit its application in refractory and building materials. Therefore, as fillers in polymer should be more promising directions. However, its deeper color limits its large-scale applications, so need to find a simple and economic method to whiten bauxite tailings.
According to the facts that iron phosphate being white or yellow white, bauxite tailings were whitened by using the process route of phosphoric acid to react with bauxite tailings and then the reaction products being calcined for removal carbon. The addition amount of phosphoric acid and calcination temperature is the key factors to affect on the whiteness of bauxite tailings. The effects of calcination temperature on whiteness largely depend on the amount of phosphoric acid phosphate:the whiteness of bauxite tailings almost can't been improved through the calcination in the insufficient dosage of phosphoric acid; while, the whiteness firstly increase, reach the maximum of72%at550℃, then decrease with calcination temperature in sufficient dosage of phosphoric acid conditions.
The phosphate coated with most particles of whitening bauxite tailings meliorate the superficial acid and alkali nature of particles of bauxite tailings, so less effect on the thermal stability of polyvinyl chloride(PVC), but it still significantly influences the thermal degradation and combustion performance of PVC. The whitening tailings reduced the degradation temperature of PVC, weakened release quantity of volatile gases HCl and aromatic compounds benzene, increased the activation energy and frequency factor of degradation reaction, and reduced the mass loss in the first degradation stage of polyvinyl chloride when PVC degraded in argon; The whitening tailings reduced the temperatures of the first degradation stage and the third stage of PVC, improved the temperature of the second degradation stage, weakened the release volume of toxic gases HC1and aromatic compounds benzene, reduced the mass loss of the second degradation stage, decreased the activation energy and frequency factor of the first degradation stage, and increased the activation energy of the second degradation stage when PVC degraded in air. The whitening tailings decreased the total smoke released, total heat released and the ratio of mass loss and shorten the ignition time when PVC combusted.
The whitening bauxite tailings were modified by using surface chemical reaction of dry method and wet chemical method. The modification effect of the wet chemical method is better than the one of dry method at the same modifier being used. The modification effect of mixture of different modifier used is better than the one of a single modifier used under the same other modification conditions. In experiment, the largest activation index obtained is80%, when modifier ratio of0.4:1.6and wet chemical method were used. The dispersion of the modified whitening tailings in PVC and the interface bonding condition were improved, the influences on mechanics properties of matrix was reduced after the bauxite tailings modification.
Aluminum tri-polyphosphate was synthesized from bauxite tailings and phosphoric acid when P/Al molar ratio of2.5, condensation temperature of300℃and condensation time of8h. Talc, zinc oxide and wollastonite were respectively used to modify the aluminum tripolyphosphate in order to meliorate the pH value of aluminum tripolyphosphate. The possibility of using modified aluminum tripolyphosphate as an anticorrosive pigment was also investigated by routine method and electrochemical impedance spectroscopy. Zinc oxide modified aluminum tripolyphosphate has the best corrosion resistance. Steel board dipping in the saturated solution of zinc oxide modified aluminum tripolyphosphate for48h occured only non-proliferation of pitting corrosion. The impedance of steel board with coating with zinc oxide modified aluminum tripolyphosphate pigment was108Ω.cm-2in first immersion stage, down to6.5×107Ω.cm-2at immersion of20days and increase to7×107Ωcm-2up to immersion for40days.
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