油页岩灰渣提取氧化铝及其应用
摘要
本着综合利用油页岩灰渣的原则,根据油页岩灰渣的矿物组成与化学成分特征,提出了一系列综合利用油页岩灰渣中铝元素的方法。主要研究方法及成果如下：
1.首次进行以油页岩灰渣提取氧化铝的研究,并确定了最佳提取工艺。结果表明,在最佳工艺条件下,提取出的氧化铝纯度为98.87%-99.40%,对油页岩中氧化铝的回收率达76.08%-79.86%。
2.研究了以油页岩灰渣为铝源制备纳米氧化铝的制备工艺,并讨论了分散作用机理。结果表明,分散方法有效阻止了氢氧化铝的团聚。混合表面活性剂与二氧化碳的流速对粒氧化铝粒径大小均有重要影响。
3.以油页岩灰渣提取氧化铝为基质材料,成功制备了新型多孔性壳交联的氧化铝-壳聚糖(Al2O3-CCS)杂化微球吸附剂。
4.探究了不同条件下A12O3-CCS吸附剂对苯酚和Cu2+的吸附与解附行为。实验结果表明,吸附剂能有效地去除苯酚和Cu2+,并具备较好的再生和重复使用的性能。分别使用Langmuir模型和Freundlich模型对实验数据进行了拟合,模拟结果表明,吸附过程均属于单层吸附。
Oil shale ash is the residue of the retorting or burning of oil shale. A great quantity of oil shale ash not only occupied land, but also results in serious environmental pollution. Meanwhile, this will limited the utilization and development of oil shale industry. Therefore, it is significant to find a feasible and reasonable treatment of oil shale ash.
In this paper, we adhered to the principle of comprehensive utilization of oil shale ash, proposing a series of method for comprehensive utilization of oil shale ash. In detail, firstly the extraction of alumina from oil shale ash was researched; secondly, the precursor of alumina was treated by combined dispersion (surfactant, ultrasonics, and azeotropic distillation) to prepare nano alumina; to improve further the added value of oil shale ash, the alumina was modified with chitosan to synthesize functional alumina hybrid adsorbent. Addtionally, the adsorption behavior of heavy metals and phenolic compounds on alumina hybrid adsorbent were investigated. The main conclusions are as follows.
1. The extraction of alumina from oil shale ash was originally researched and the optimum parameters were determined. The experiments results show that the purity percent is 98.87～99.4% and the extraction percent is 76.08～79.86%, under optimal conditions (temperature 750℃, calnations time 2-3h and so on).
2. The preparation of nano alumina from oil shale ash was researched. Also, the dispersion mechanism was discussed. The results show that the combined method of surface modification, ultrasonic oscillation, and azeotropic distillization could prevent the agglomeration of precursor of alumina. On the other hand, this method can prevent the second agglomeration of alumina during the calcination. The effection of mixed surfactant (PEG6000:PEG10000:PEG20000 1:1:1) is better than one. High flow rate of carbon dioxide result in the agglomeration of alumina and big particle size. The optimum flow rate is 5 mL/min, and the particle size of obtained alumina is less than 100 nm.
3 The shell corsslinked alumina-chitosan hybrid adsorbent was prepared. In detail, the alumina was used as matrix of adsorbents. The malonate was used as bridge between the alumina and chitosan. The sodium polyphosphate was crosslinking reagent. The BET results show that the specific surface area is 225.31 m2/g, the volume of pore is 0.473 cm3/g, the pore diameter is 8.4 nm, the pore type is ink bottle. The pores exist in 4.8 nm and 3.5 nm. The pore of adsorbent is mesoporous. The chitosan percent of this sorbent is 12.86 wt.%.
4. The adsorption behavior of phenol on Al2O3-CCS was investigated. The results show that the adsorbent has the maximum equilibrium adsorption capacity at pH 7.0, than pH 9.0 and low pH value. Initial concentration of phenol has on the adsorption capacity of Al2O3-CCS beads. With the increase of initial concentration, the adsorption capacity increased. The adsorption efficiency of phenol is high when the adsorbent was used in low initial concentration of phenol. Additionally, with the shaking time increasing, the relative recovery of phenol was also increased. The regeneration and reusability of Al2O3-CCS improve that the sorbent can be used to removal phenol from contaminated water. The Langmuir model and Freundlich model was used to analyze the data. The results of calculation reveal that:the adsorption behavior of phenol on Al2O3 was in basic agreements with single-layer adsorption model. It also been determined that the saturated adsorption capacity of phenol were 89.21 mg/g (pH=5.0),139.86 mg/g (pH=7.0),91.41 mg/g (pH=9.0), respectively.
5. The adsorption behavior of Copper(II) on Al2O3-CCS was investigated. The results show that the adsorbent has the maximum equilibrium adsorption capacity at pH 2.5, than pH 5.0 and 7.0. Initial concentration of Cu(II) has on the adsorption capacity of Al2O3-CCS beads. With the increase of initial concentration, the adsorption capacity increased. The adsorption efficiency of Cu(II) is high when the adsorbent was used in low initial concentration of Cu(II). Additionally, with the shaking time increasing, the relative recovery of Cu(II) was also increased. The regeneration and reusability of Al2O3-CCS improve that the sorbent can be used to removal Cu(II) from contaminated water. The Langmuir model and Freundlich model was used to analyze the data. The results of calculation reveal that:the adsorption behavior of Cu(II) on Al2O3 was in basic agreements with single-layer adsorption model. It also been determined that the saturated adsorption capacity of Cu(II) were 315.46mg/g (pH=2.5),292.40mg/g (pH=5.0),106.95 mg/g (pH=7.0), respectively.
1.首次进行以油页岩灰渣提取氧化铝的研究,并确定了最佳提取工艺。结果表明,在最佳工艺条件下,提取出的氧化铝纯度为98.87%-99.40%,对油页岩中氧化铝的回收率达76.08%-79.86%。
2.研究了以油页岩灰渣为铝源制备纳米氧化铝的制备工艺,并讨论了分散作用机理。结果表明,分散方法有效阻止了氢氧化铝的团聚。混合表面活性剂与二氧化碳的流速对粒氧化铝粒径大小均有重要影响。
3.以油页岩灰渣提取氧化铝为基质材料,成功制备了新型多孔性壳交联的氧化铝-壳聚糖(Al2O3-CCS)杂化微球吸附剂。
4.探究了不同条件下A12O3-CCS吸附剂对苯酚和Cu2+的吸附与解附行为。实验结果表明,吸附剂能有效地去除苯酚和Cu2+,并具备较好的再生和重复使用的性能。分别使用Langmuir模型和Freundlich模型对实验数据进行了拟合,模拟结果表明,吸附过程均属于单层吸附。
Oil shale ash is the residue of the retorting or burning of oil shale. A great quantity of oil shale ash not only occupied land, but also results in serious environmental pollution. Meanwhile, this will limited the utilization and development of oil shale industry. Therefore, it is significant to find a feasible and reasonable treatment of oil shale ash.
In this paper, we adhered to the principle of comprehensive utilization of oil shale ash, proposing a series of method for comprehensive utilization of oil shale ash. In detail, firstly the extraction of alumina from oil shale ash was researched; secondly, the precursor of alumina was treated by combined dispersion (surfactant, ultrasonics, and azeotropic distillation) to prepare nano alumina; to improve further the added value of oil shale ash, the alumina was modified with chitosan to synthesize functional alumina hybrid adsorbent. Addtionally, the adsorption behavior of heavy metals and phenolic compounds on alumina hybrid adsorbent were investigated. The main conclusions are as follows.
1. The extraction of alumina from oil shale ash was originally researched and the optimum parameters were determined. The experiments results show that the purity percent is 98.87～99.4% and the extraction percent is 76.08～79.86%, under optimal conditions (temperature 750℃, calnations time 2-3h and so on).
2. The preparation of nano alumina from oil shale ash was researched. Also, the dispersion mechanism was discussed. The results show that the combined method of surface modification, ultrasonic oscillation, and azeotropic distillization could prevent the agglomeration of precursor of alumina. On the other hand, this method can prevent the second agglomeration of alumina during the calcination. The effection of mixed surfactant (PEG6000:PEG10000:PEG20000 1:1:1) is better than one. High flow rate of carbon dioxide result in the agglomeration of alumina and big particle size. The optimum flow rate is 5 mL/min, and the particle size of obtained alumina is less than 100 nm.
3 The shell corsslinked alumina-chitosan hybrid adsorbent was prepared. In detail, the alumina was used as matrix of adsorbents. The malonate was used as bridge between the alumina and chitosan. The sodium polyphosphate was crosslinking reagent. The BET results show that the specific surface area is 225.31 m2/g, the volume of pore is 0.473 cm3/g, the pore diameter is 8.4 nm, the pore type is ink bottle. The pores exist in 4.8 nm and 3.5 nm. The pore of adsorbent is mesoporous. The chitosan percent of this sorbent is 12.86 wt.%.
4. The adsorption behavior of phenol on Al2O3-CCS was investigated. The results show that the adsorbent has the maximum equilibrium adsorption capacity at pH 7.0, than pH 9.0 and low pH value. Initial concentration of phenol has on the adsorption capacity of Al2O3-CCS beads. With the increase of initial concentration, the adsorption capacity increased. The adsorption efficiency of phenol is high when the adsorbent was used in low initial concentration of phenol. Additionally, with the shaking time increasing, the relative recovery of phenol was also increased. The regeneration and reusability of Al2O3-CCS improve that the sorbent can be used to removal phenol from contaminated water. The Langmuir model and Freundlich model was used to analyze the data. The results of calculation reveal that:the adsorption behavior of phenol on Al2O3 was in basic agreements with single-layer adsorption model. It also been determined that the saturated adsorption capacity of phenol were 89.21 mg/g (pH=5.0),139.86 mg/g (pH=7.0),91.41 mg/g (pH=9.0), respectively.
5. The adsorption behavior of Copper(II) on Al2O3-CCS was investigated. The results show that the adsorbent has the maximum equilibrium adsorption capacity at pH 2.5, than pH 5.0 and 7.0. Initial concentration of Cu(II) has on the adsorption capacity of Al2O3-CCS beads. With the increase of initial concentration, the adsorption capacity increased. The adsorption efficiency of Cu(II) is high when the adsorbent was used in low initial concentration of Cu(II). Additionally, with the shaking time increasing, the relative recovery of Cu(II) was also increased. The regeneration and reusability of Al2O3-CCS improve that the sorbent can be used to removal Cu(II) from contaminated water. The Langmuir model and Freundlich model was used to analyze the data. The results of calculation reveal that:the adsorption behavior of Cu(II) on Al2O3 was in basic agreements with single-layer adsorption model. It also been determined that the saturated adsorption capacity of Cu(II) were 315.46mg/g (pH=2.5),292.40mg/g (pH=5.0),106.95 mg/g (pH=7.0), respectively.
引文
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