橘子皮化学改性及其对重金属离子吸附行为的研究
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摘要
现代工业的迅速发展产生了大量含重金属废水,对环境和人体健康造成严重危害。如何消除重金属的危害并有效地回收贵重金属是当今环境保护工作面临的突出问题。生物吸附技术作为新兴的重金属去除技术,愈来愈受到人们的关注。与传统的重金属离子去除方法相比,生物吸附法的吸附原料来源广泛,且在原料的成本及环境保护方面显示出较大的优势,因此具有广阔的应用前景。
本论文选用农林废弃物质橘子皮(OP)为原料,对其进行化学改性,制备了一系列重金属离子生物吸附剂,并通过对水溶液中Cu2+,Pb2+,Cd2+,Zn2+和Ni2+吸附行为的研究,考察了改性橘子皮生物吸附剂的吸附性能。采用现代分析检测技术,如BET-N2吸附法、红外光谱分析和扫描电镜等,对改性前后橘子皮的比表面积、表面电荷、结构、形貌进行了表征,探讨了橘子皮化学改性的机理,优化了改性反应的条件。通过静态吸附实验,考察了在不同加入量、pH、温度、初始浓度以及干扰离子存在的条件下,改性橘子皮生物吸附剂对重金属离子吸附效果的影响,并对吸附热力学及吸附动力学行为进行了研究；同时,对改性橘子皮的再生技术以及对含金属离子的实际工业废水的处理效果进行了试验。通过动态吸附实验,测定了不同床层高度、不同流量和不同初始浓度下的透过曲线,考察了床层高度、溶液流速和初始浓度对吸附过程的影响。
用氢氧化钠、氢氧化钠和氯化钙以及丙烯酸甲酯对橘子皮分别进行了皂化、皂化交联和接枝共聚三种方式改性处理。改性研究结果表明,使用氢氧化钠、氢氧化钠和氯化钙以及丙烯酸甲酯对橘子皮进行改性时,反应物料配比、各反应阶段的反应温度和反应时间等因素影响改性橘子皮的吸附容量以及改性物质产率或接枝率。在结构形貌方面,扫描电镜观察表明,与OP相比,皂化改性橘子皮(SOP)和皂化交联改性橘子皮(SCOP)的表面变得粗糙多孔,比表面积增大；在表面电性方面,Zeta电位和总负电荷测定结果表明SOP和SCOP表面所带的负电荷增多,有利于与重金属离子相互吸引。IR图谱分析表明皂化及皂化交联改性使橘子皮中甲酯化的羧基水解为羧基,活性官能团的数目提高。接枝共聚改性后的橘子皮(OPAA)由于分子表面接枝聚丙烯酸,使外观形貌变得光滑,比表面积减少,但由于羧基官能团数目的剧增,使表面所带负电荷随之急剧增加。IR图谱分析也表明聚丙烯酸被接枝到主要组成的分子上。
静态吸附实验结果表明,吸附过程的最佳pH值为5.0-6.0；随着固体吸附剂加入量的提高,改性橘子皮对水溶液中重金属离子的去除率也随之提高,当固液比为4 g/L时,SOP和SCOP对水溶液中Cu2+,Pb2+,Cd2+,Zn2+和Ni2+具有较好的吸附效果；除SCOP对Cd2+的吸附外,所有其它吸附过程的吸附量随温度的升高而减小,热力学数据说明改性橘子皮生物吸附剂对重金属离子的吸附过程是自发进行的、熵减小的放热过程。改性橘子皮生物吸附剂对重金属离子的吸附均符合Langmuir等温吸附模式。与OP相比,SOP、SCOP和OPAA对水中重金属离子的吸附容量均得到提高,特别是OPAA,对Cu2+,Pb2+, Cd2+,Zn2+和Ni2+的吸附容量比改性前分别提高了6.5,4.3,4.6,18.5和16.5倍,也优于文献记载的其它生物吸附材料的最大吸附容量。SOP和SCOP对水溶液中重金属离子的吸附是一个符合准二级动力学方程的快速吸附过程,20min达到吸附平衡。OPAA对重金属离子的吸附在2h基本达到平衡,吸附反应速率先快后慢,吸附过程符合准二级动力学方程,而且吸附过程由膜扩散和颗粒内扩散联合控制,颗粒内扩散速率大小是决定整个吸附反应速度的关键。水溶液中常见的K+、Na+、Ca2+、Mg2+阳离子的存在以及其它重金属离子的存在对改性橘子皮生物吸附剂吸附性能的影响比较复杂,没有确定的规律可循,总体来说重金属离子的存在对吸附的遏制作用大于常见阳离子。使用0.1mol/L HCl溶液对吸附饱和的改性橘子皮生物吸附剂解吸,解吸率可达到90%以上。通过3-4次吸附-解吸循环试验表明,改性橘子皮的吸附容量未发生明显的变化,可以循环利用。
SCOP的动态吸附过程研究表明,较大的流速、较高的初始浓度和较短的床层长度将使床层穿透加快。根据静态吸附实验结果,将Pb2+和Zn2+混合溶液在pH 2.5时通过装有SOP、SCOP和OPAA的固定床进行分离,结果表明可以通过装有这三种吸附剂的固定床实现水溶液中Pb2+的富集、Pb2+与Zn2+的分离或从Zn2+溶液中富集Pb2+。
使用改性橘子皮生物吸附剂对实际水样进行了处理,结果表明,经过改性橘子皮生物吸附剂的吸附,废水中重金属离子含量达到了国家工业废水的排放标准。
吸附过程中溶液的pH降低、Na+、K+、Ca2+和Mg2+的释放量测定结果以及红外光谱、能谱和X-荧光光谱分析结果表明,在改性橘子皮生物吸附剂吸附重金属离子过程中以离子交换机制为主。
通过本研究,获得了高效利用废弃物质橘子皮和净化重金属污染废水的基础性数据,对实现资源综合利用具有经济和环境双重意义,为生物废弃物质的资源化及深度利用提供一种新的思路,并为开发高效、低成本的重金属污染治理技术奠定良好的基础。
Nowadays heavy metals are among the most important pollutants in source and treated water and are becoming a severe public health problem. These metal ions can be harmful to aquatic life, and water contaminated by toxic metal ions remains a serious public health problem for human health. Consequently, it is urgent to find new technologies for removing heavy metal ions from wastewater. So, biosorption can be a promising alternative method to treat industrial effluents, mainly because of its low cost, high metal binding capacity, high efficiency in dilute effluents and environmental friendly.
In this paper, a series of biosorbents were prepared using orange peel from agriculture residues by chemical modification and adsorption properties of Cu2+,Pb2+,Cd2+,Zn2+and Ni2+ on these biosorbents in aqueous solution were studied. The structure and morphology of orange peel and modified orange peel were characterized by lots of instruments, such as BET-N2 adsorption, infrared spectroscopy and scanning electron microscopy technique. Also the physical and chemical characteristics such as surface area, surface charge, were examined. The modifying mechanisms of orange peel were discussed, and the reaction conditions of modification were optimized. By using batch adsorption techniques, the influence of pH, adsorbent dosage, concentration and temperature on adsorption effect was investigated. In addition,the adsorption thermodynamics and the adsorption kinetics were studied systematically. Furthermore,the technologies of desorption and reuse for the modified orange peel and technological applications for the wastewater were also tested. By the column adsorption experiments, the figures of breakthrough curve were determined in different experimental conditions, such as flow rate of solution, initial concentration of adsorbent and the column height to inspect on the adsorption effects.
The chemical modification of orange peel are in the methods of saponification(SOP), saponification-crosslinking(SCOP) and graft copolymerization(OPAA) with sodium hydroxide, sodium hydroxide and calcium chloride and methyl acrylate in this paper. When orange peel were modified by sodium hydroxide, sodium hydroxide and calcium chloride and methyl acrylate, the modification conditions, such as material ratio,reaction temperature and reaction time,must be controlled strictly,which could affect the adsorption capacity and the yield of the modified orange peel.
The changes of physical structure and chemical properties of series of modified orange peel were characterized by using a variety of analytical instruments and methods. The results of scanning electronic microscope showed that the SOP and SCOP become rough porous in structural morphology, surface area was increased. The determination results of zeta potential and total negative charge show that the surface of modified orange peel has more negative charge than raw orange peel, which facilitates the electrostatic interaction with cations.For FT-IR spectrum of the SOP and SCOP, results indicated that the methyl esters were hydrolyzed with NaOH and ester group was converted to carboxylate ions, which improved the number of active functional groups. IR analysis of OPAA shows that polyacrylic acid was grafted to the main components of the orange peel.After the graft copolymerization of orange peel with methyl acrylate, the appearance of morphology was smooth and specific surface area decreased as a result of grafting polyacrylic acid. But due to the number of carboxyl functional groups increased, at the same pH value, the zeta potentials of OPAA are more negative than those of OP and total negative charge of OPAA is more than that of OP, which indicate that the amount of-COOH of OPAA is more than that of OP because of grafting with PMA on the OP.
The adsorption process is a function of pH, metal ion concentration, time, temperature and the adsorbent dose. The optimum pH value was found out 5.0～6.0.The adsorption percentage increased with the increase of adsorbent dose.It was found that the adsorption effects of SOP and SCOP to Cu2+,Pb2+,Cd2+,Zn2+ and Ni2+ is better when adsorbent dose was 4g/L.In all other adsorption processes, adsorption capacity decreases with the adsorption temperature increasing and enthalpy, Gibbs free energy and entropy change were negtive except Cd2+ adsorption on SCOP. In the adsorption process,the enthalpy change(ΔH) was negative, which demonstrated that the adsorption process was of exothermic process.The free energy change(ΔG) was negative, which indicated the adsorption process was spontaneous.The entropy change (ΔS) was also negative because of the increasing of order caused by the new ion-bonds and the decreasing of disorder in aqueous solutions. The experimental adsorption data for modified orange peel were fitted to the Langmuir adsorption model.From Langmuir isotherm, the adsorption capacity for heavy metal ions on the modified orange peel increased compared with the OP. Especially for OPAA, the highest metal uptake for Cu2+,Pb2+,Cd2+, Zn2+and Ni2+ were 289.0,492.6,293.3,393.7 and 162.6mg/g, which is respectively about 6.5,4.3,4.6,18.5 and 16.5 time higher than that of the unmodified biomass and also much higher than some other biosorbents reported in literatures. It was found that the adsorption of heavy metals on SOP and SCOP was a fast adsorption process that could be reached equilibrium in 20 minutes. The adsorption process was mainly fitted the pseudo-second-order equation. The removal rate of heavy metals on OPAA was rapid in the first 30 min, and leveled off after 2h. The biosorption kinetics followed the pseudo-second order model and intra-particle diffusion model.In addition,the intra-particle diffusion was the main rate-controlling step.The existence of common cations such as K+, Na+, Ca2+, Mg2+ and other heavy metal ions in water interfered the adsorption of modified orange peel, but had no definite pattern. The loaded biosorbent was regenerated using 0.1 mol/L HCl solution and could be used repeatedly for four times with little loss of adsorption capacity.
At dynamic process of SCOP, the figure of breakthrough curve was strongly dependent on experimental conditions, such as flow rate of solution, initial concentration of adsorbent and the column height. Higher flow rate, bigger initial concentration of adsorbent and shorter column height will quicken the breakthrough of column. A mutual chromatographic separation test was carried out by using SOP, SCOP and OPAA between Pb2+ and Zn2+, i.e.,a small amount of Pb2+ was separated from a large excess of Zn2+ using a column packed with the modified orange peel.These results suggest that effective mutual separation and pre-concentration of Pb2+ away from Zn2+ using modified orange peel can be satisfactorily achieved.
The practical treatments were studied by using modified orange peel to dispose of electroplating wastewater. The results clearly indicate that the proposed method is prospective for the removal of heavy metal ions from wastewater.
Different experimental approaches were applied to show mechanistic aspects, especially the role of calcium, sodium and hydrogen present in the biosorbents in ion exchange mechanism.
In this paper, the direction of research conforms to China's current ecological protection, recycling economy and environmental policy. Based on the findings above, a new high-performance, low-cost approach and a new way of thinking will be provide to treat the heavy metals contamination by using orange peel discarded.
本论文选用农林废弃物质橘子皮(OP)为原料,对其进行化学改性,制备了一系列重金属离子生物吸附剂,并通过对水溶液中Cu2+,Pb2+,Cd2+,Zn2+和Ni2+吸附行为的研究,考察了改性橘子皮生物吸附剂的吸附性能。采用现代分析检测技术,如BET-N2吸附法、红外光谱分析和扫描电镜等,对改性前后橘子皮的比表面积、表面电荷、结构、形貌进行了表征,探讨了橘子皮化学改性的机理,优化了改性反应的条件。通过静态吸附实验,考察了在不同加入量、pH、温度、初始浓度以及干扰离子存在的条件下,改性橘子皮生物吸附剂对重金属离子吸附效果的影响,并对吸附热力学及吸附动力学行为进行了研究；同时,对改性橘子皮的再生技术以及对含金属离子的实际工业废水的处理效果进行了试验。通过动态吸附实验,测定了不同床层高度、不同流量和不同初始浓度下的透过曲线,考察了床层高度、溶液流速和初始浓度对吸附过程的影响。
用氢氧化钠、氢氧化钠和氯化钙以及丙烯酸甲酯对橘子皮分别进行了皂化、皂化交联和接枝共聚三种方式改性处理。改性研究结果表明,使用氢氧化钠、氢氧化钠和氯化钙以及丙烯酸甲酯对橘子皮进行改性时,反应物料配比、各反应阶段的反应温度和反应时间等因素影响改性橘子皮的吸附容量以及改性物质产率或接枝率。在结构形貌方面,扫描电镜观察表明,与OP相比,皂化改性橘子皮(SOP)和皂化交联改性橘子皮(SCOP)的表面变得粗糙多孔,比表面积增大；在表面电性方面,Zeta电位和总负电荷测定结果表明SOP和SCOP表面所带的负电荷增多,有利于与重金属离子相互吸引。IR图谱分析表明皂化及皂化交联改性使橘子皮中甲酯化的羧基水解为羧基,活性官能团的数目提高。接枝共聚改性后的橘子皮(OPAA)由于分子表面接枝聚丙烯酸,使外观形貌变得光滑,比表面积减少,但由于羧基官能团数目的剧增,使表面所带负电荷随之急剧增加。IR图谱分析也表明聚丙烯酸被接枝到主要组成的分子上。
静态吸附实验结果表明,吸附过程的最佳pH值为5.0-6.0；随着固体吸附剂加入量的提高,改性橘子皮对水溶液中重金属离子的去除率也随之提高,当固液比为4 g/L时,SOP和SCOP对水溶液中Cu2+,Pb2+,Cd2+,Zn2+和Ni2+具有较好的吸附效果；除SCOP对Cd2+的吸附外,所有其它吸附过程的吸附量随温度的升高而减小,热力学数据说明改性橘子皮生物吸附剂对重金属离子的吸附过程是自发进行的、熵减小的放热过程。改性橘子皮生物吸附剂对重金属离子的吸附均符合Langmuir等温吸附模式。与OP相比,SOP、SCOP和OPAA对水中重金属离子的吸附容量均得到提高,特别是OPAA,对Cu2+,Pb2+, Cd2+,Zn2+和Ni2+的吸附容量比改性前分别提高了6.5,4.3,4.6,18.5和16.5倍,也优于文献记载的其它生物吸附材料的最大吸附容量。SOP和SCOP对水溶液中重金属离子的吸附是一个符合准二级动力学方程的快速吸附过程,20min达到吸附平衡。OPAA对重金属离子的吸附在2h基本达到平衡,吸附反应速率先快后慢,吸附过程符合准二级动力学方程,而且吸附过程由膜扩散和颗粒内扩散联合控制,颗粒内扩散速率大小是决定整个吸附反应速度的关键。水溶液中常见的K+、Na+、Ca2+、Mg2+阳离子的存在以及其它重金属离子的存在对改性橘子皮生物吸附剂吸附性能的影响比较复杂,没有确定的规律可循,总体来说重金属离子的存在对吸附的遏制作用大于常见阳离子。使用0.1mol/L HCl溶液对吸附饱和的改性橘子皮生物吸附剂解吸,解吸率可达到90%以上。通过3-4次吸附-解吸循环试验表明,改性橘子皮的吸附容量未发生明显的变化,可以循环利用。
SCOP的动态吸附过程研究表明,较大的流速、较高的初始浓度和较短的床层长度将使床层穿透加快。根据静态吸附实验结果,将Pb2+和Zn2+混合溶液在pH 2.5时通过装有SOP、SCOP和OPAA的固定床进行分离,结果表明可以通过装有这三种吸附剂的固定床实现水溶液中Pb2+的富集、Pb2+与Zn2+的分离或从Zn2+溶液中富集Pb2+。
使用改性橘子皮生物吸附剂对实际水样进行了处理,结果表明,经过改性橘子皮生物吸附剂的吸附,废水中重金属离子含量达到了国家工业废水的排放标准。
吸附过程中溶液的pH降低、Na+、K+、Ca2+和Mg2+的释放量测定结果以及红外光谱、能谱和X-荧光光谱分析结果表明,在改性橘子皮生物吸附剂吸附重金属离子过程中以离子交换机制为主。
通过本研究,获得了高效利用废弃物质橘子皮和净化重金属污染废水的基础性数据,对实现资源综合利用具有经济和环境双重意义,为生物废弃物质的资源化及深度利用提供一种新的思路,并为开发高效、低成本的重金属污染治理技术奠定良好的基础。
Nowadays heavy metals are among the most important pollutants in source and treated water and are becoming a severe public health problem. These metal ions can be harmful to aquatic life, and water contaminated by toxic metal ions remains a serious public health problem for human health. Consequently, it is urgent to find new technologies for removing heavy metal ions from wastewater. So, biosorption can be a promising alternative method to treat industrial effluents, mainly because of its low cost, high metal binding capacity, high efficiency in dilute effluents and environmental friendly.
In this paper, a series of biosorbents were prepared using orange peel from agriculture residues by chemical modification and adsorption properties of Cu2+,Pb2+,Cd2+,Zn2+and Ni2+ on these biosorbents in aqueous solution were studied. The structure and morphology of orange peel and modified orange peel were characterized by lots of instruments, such as BET-N2 adsorption, infrared spectroscopy and scanning electron microscopy technique. Also the physical and chemical characteristics such as surface area, surface charge, were examined. The modifying mechanisms of orange peel were discussed, and the reaction conditions of modification were optimized. By using batch adsorption techniques, the influence of pH, adsorbent dosage, concentration and temperature on adsorption effect was investigated. In addition,the adsorption thermodynamics and the adsorption kinetics were studied systematically. Furthermore,the technologies of desorption and reuse for the modified orange peel and technological applications for the wastewater were also tested. By the column adsorption experiments, the figures of breakthrough curve were determined in different experimental conditions, such as flow rate of solution, initial concentration of adsorbent and the column height to inspect on the adsorption effects.
The chemical modification of orange peel are in the methods of saponification(SOP), saponification-crosslinking(SCOP) and graft copolymerization(OPAA) with sodium hydroxide, sodium hydroxide and calcium chloride and methyl acrylate in this paper. When orange peel were modified by sodium hydroxide, sodium hydroxide and calcium chloride and methyl acrylate, the modification conditions, such as material ratio,reaction temperature and reaction time,must be controlled strictly,which could affect the adsorption capacity and the yield of the modified orange peel.
The changes of physical structure and chemical properties of series of modified orange peel were characterized by using a variety of analytical instruments and methods. The results of scanning electronic microscope showed that the SOP and SCOP become rough porous in structural morphology, surface area was increased. The determination results of zeta potential and total negative charge show that the surface of modified orange peel has more negative charge than raw orange peel, which facilitates the electrostatic interaction with cations.For FT-IR spectrum of the SOP and SCOP, results indicated that the methyl esters were hydrolyzed with NaOH and ester group was converted to carboxylate ions, which improved the number of active functional groups. IR analysis of OPAA shows that polyacrylic acid was grafted to the main components of the orange peel.After the graft copolymerization of orange peel with methyl acrylate, the appearance of morphology was smooth and specific surface area decreased as a result of grafting polyacrylic acid. But due to the number of carboxyl functional groups increased, at the same pH value, the zeta potentials of OPAA are more negative than those of OP and total negative charge of OPAA is more than that of OP, which indicate that the amount of-COOH of OPAA is more than that of OP because of grafting with PMA on the OP.
The adsorption process is a function of pH, metal ion concentration, time, temperature and the adsorbent dose. The optimum pH value was found out 5.0～6.0.The adsorption percentage increased with the increase of adsorbent dose.It was found that the adsorption effects of SOP and SCOP to Cu2+,Pb2+,Cd2+,Zn2+ and Ni2+ is better when adsorbent dose was 4g/L.In all other adsorption processes, adsorption capacity decreases with the adsorption temperature increasing and enthalpy, Gibbs free energy and entropy change were negtive except Cd2+ adsorption on SCOP. In the adsorption process,the enthalpy change(ΔH) was negative, which demonstrated that the adsorption process was of exothermic process.The free energy change(ΔG) was negative, which indicated the adsorption process was spontaneous.The entropy change (ΔS) was also negative because of the increasing of order caused by the new ion-bonds and the decreasing of disorder in aqueous solutions. The experimental adsorption data for modified orange peel were fitted to the Langmuir adsorption model.From Langmuir isotherm, the adsorption capacity for heavy metal ions on the modified orange peel increased compared with the OP. Especially for OPAA, the highest metal uptake for Cu2+,Pb2+,Cd2+, Zn2+and Ni2+ were 289.0,492.6,293.3,393.7 and 162.6mg/g, which is respectively about 6.5,4.3,4.6,18.5 and 16.5 time higher than that of the unmodified biomass and also much higher than some other biosorbents reported in literatures. It was found that the adsorption of heavy metals on SOP and SCOP was a fast adsorption process that could be reached equilibrium in 20 minutes. The adsorption process was mainly fitted the pseudo-second-order equation. The removal rate of heavy metals on OPAA was rapid in the first 30 min, and leveled off after 2h. The biosorption kinetics followed the pseudo-second order model and intra-particle diffusion model.In addition,the intra-particle diffusion was the main rate-controlling step.The existence of common cations such as K+, Na+, Ca2+, Mg2+ and other heavy metal ions in water interfered the adsorption of modified orange peel, but had no definite pattern. The loaded biosorbent was regenerated using 0.1 mol/L HCl solution and could be used repeatedly for four times with little loss of adsorption capacity.
At dynamic process of SCOP, the figure of breakthrough curve was strongly dependent on experimental conditions, such as flow rate of solution, initial concentration of adsorbent and the column height. Higher flow rate, bigger initial concentration of adsorbent and shorter column height will quicken the breakthrough of column. A mutual chromatographic separation test was carried out by using SOP, SCOP and OPAA between Pb2+ and Zn2+, i.e.,a small amount of Pb2+ was separated from a large excess of Zn2+ using a column packed with the modified orange peel.These results suggest that effective mutual separation and pre-concentration of Pb2+ away from Zn2+ using modified orange peel can be satisfactorily achieved.
The practical treatments were studied by using modified orange peel to dispose of electroplating wastewater. The results clearly indicate that the proposed method is prospective for the removal of heavy metal ions from wastewater.
Different experimental approaches were applied to show mechanistic aspects, especially the role of calcium, sodium and hydrogen present in the biosorbents in ion exchange mechanism.
In this paper, the direction of research conforms to China's current ecological protection, recycling economy and environmental policy. Based on the findings above, a new high-performance, low-cost approach and a new way of thinking will be provide to treat the heavy metals contamination by using orange peel discarded.
引文
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