应用硅藻土处理含重金属离子废水相关理论基础及关键技术研究
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摘要
含重金属离子废水的有效处理对于水体重金属污染控制与修复意义重大。目前含重金属离子废水处理方法主要有离子交换、化学沉淀、电动力修复、生物修复和吸附。在众多方法中,吸附法由于稳定、可靠、简单、低耗、低二次污染等优势而被广泛应用。作为一种重要的废水处理方法,其关键在于吸附材料的选择。针对含重金属离子废水处理,吸附材料必须能够有效地吸附与固定重金属离子,同时具备来源丰富、价格便宜、再生容易等优势。在系列吸附材料中硅藻土较好地符合了这些要求。
硅藻土因具有多孔结构、大比表面积和众多活性基团,常被用作吸附材料。但是由于含有杂质和理化构造缺陷而存在吸附能力一般,可操作性差等不足,使硅藻土在含重金属离子废水处理应用中具有一定局限性。针对上述问题,本文围绕硅藻土开展了吸附、改性、成形及应用等系列研究,获取了一大批科学数据,对于水体重金属污染的有效防治和硅藻土资源的充分利用具有十分重要的意义。主要研究结果如下：
(1)天然硅藻土对各重金属离子的吸附量,随着吸附时间的延长而迅速增大之后趋于平衡；随着吸附剂浓度的增加而先增大后减小；随着pH值的增大而不断增大；随着离子初始浓度的增大而先增大后减小；而温度对吸附量的影响规律不明显。对各重金属离子吸附能力大小顺序为Zn2+>Fe3+> Cd2+>Cu2+> Pb2+> Mn2+,吸附能力与各离子的水合半径及水合自由能密切相关。
(2)天然硅藻土对Pb2+的最佳吸附条件为Wo8.0g/L、Co400mg/L、pH7.0、 T25℃、t120min,对Cd2+的为Wo6.0g/L、Co200mg/L、pH5.0、T25℃、t120min,对Cu2+的为W06.0g/L、C0300mg/L、pH5.0、T25℃、t120min,对Zn2+的为W8.0g/L、C0500mg/L、pH6.0、T25℃、t120min,对Mn2+的为W08.0g/L、Co150mg/L pH4.5、T25℃、t120min,对Fe3+的为W04.0g/L、C0400mg/L、pH5.0、T25℃t120min。
(3)最适合描述天然硅藻土对Pb2+、Cd2+、 Cu2+、Zn2+、Mn2+、Fe3+的等温吸附模型分别为Tenkin、Tenkin、Langmuir、Tenkin、Freundlich和Freundlich模型；最适合描述天然硅藻土对各重金属离子的吸附动力学属性的模型是二级动力学模型；天然硅藻土对各重金属离子的吸附是容易进行的,以物理过程为主；吸附过程是自发的、吸热的、无序性增加的,吸附过程速率控制步骤均为发生在微孔内的吸附反应；经典吸附模型应用于天然硅藻土/重金属离子体系时存在明显的吸附剂浓度效应问题和参数值不稳定现象,平衡吸附量qe不是Ce的唯一函数,而是Ce与W0两个变量的函数,qe与Ce/W0具有一一对应的函数关系。
(4)常规化学改性结果表明,最佳焙烧温度和酸液浓度(HCl,v/v)分别为400℃和10%；最佳钠盐、钡盐改性浓度(n/v)分别为0.4mol/L和0.05mol/L；最佳PAM改性浓度(m/v)为20g/L。焙烧、酸洗改性机制为去除硅藻土表面及孔道内的杂质,钠盐改性机制为增强硅藻土表面负电性,钡盐改性机制为通过沉积晶体擦除表面杂质,而PAM包覆改性表象上可以大幅度提升硅藻土的吸附容量(较天然硅藻土增加了近5倍),实质上主要是PAM自身絮凝作用的结果。
(5)深度柱撑改性结果表明,与常规改性技术相比,聚羟基铝柱撑能够有效改善硅藻土的孔隙结构,显著提升硅藻土吸附能力,对Pb2+的吸附容量可达14.02mg/g(较天然硅藻土提高了39.88%),在众多吸附剂当中处于中上水平。最佳改性条件为：柱化剂浓度0.1～0.2mo1/L,A1/土比(n/m)10mmol/g,反应温度80。C反应时间120min,老化温度105℃,老化时间16h。
(6)成形样品研发结果表明,粉体硅藻土最适投加比为93.0%,超细碳粉的最适投加比为7.0%,最适烧成温度范围为800-1000℃,最适焙烧时间为90min,最适硅藻土粉体粒径为2.40μm。硅藻土成形样品为有一定强度,大小尺寸均匀、粒径约为5mm,褐色椭圆颗粒；成形样品仍保留了原有的多孔形貌,表面杂质得到了清除,孔径增大,孔隙结构更加明朗；物相组成以方石英相为主。
(7)硅藻土成形样品对Pb2+的吸附容量较天然硅藻土提高了7.58%,吸附能力没有下降反而得到了适度提升,说明成形过程对硅藻土的孔隙结构并没有造成破坏,反而有适度改善。成形样品可操作性也明显优于粉体硅藻土,试验结果达到了预期的目的,即在保证硅藻土吸附能力的前提下明显提高其可操作性。
(8)应用硅藻土处理含Fe3+废水中试研究表明,以硅藻土成形样品为核心填料的组合处理工艺可以有效处理含Fe3+废水,出水水质可达GB/T18921-2002《城市污水再生利用、景观环境用水水质标准》要求。利用硅藻土成形样品再生酸洗废液与H202制备Fenton试剂处理垃圾渗滤液切实可行,硅藻土成形样品再生酸洗废液成功的利用实现了以废治废的环保理念。
The effective treatment of wastewater containing heavy metal ions is much important for the control and remediation of water heavy metal pollution. At present, the methods used for treatment of wastewater containing heay metal ions mainly includes ion exchange, colloid precipitation, electronic remediation, bioremediation and adsorption. Compared with other methods, the adsorption is used more widely due to its advantages of stable, reliable, simple, low power consumption, low repeated pollution. As an important method for wastewater treatment, the key issue of adsorption is adsorbent choice. For treatment of wastewater containing heavy metal ions, adsorbent should be in possession of potential for adsorbing and fixing heavy metal ions effectively, as well as rich source, low cost and easy regeneration. Diatomite is selected from series adsorbents due to it fit to all demands for adsorption application.
Diatomite has micropore structure, large specific surface area and many active chemical groups. Hence, it is commonly used for adsorbent. However, diatomite has disadvantage of normal adsorption performance and poor maneuverability due to impurities and structure defects, these disadvantages limits application of diatomite in treatment of wastewater containing heavy metal ions. In order to improve the adsorption performance and maneuverability of diatomite, the studies on diatomite adsorption, modification, shaping and application have been conducted, a large number of scientific data have been acquired, and these data is very significant for the effective control of water heavy metal pollution and fully utility of diatomite store. Main results obtained from this study are summarized as follows.
(1) Adsorption density (qe) of each heavy metal ions on natural diatomite increased swiftly at the begining and then slowly attained equilibrium with contact time prolonging, increased firstly and then decreased with increasing adsorbent concentration, increased constantly with increasing solution initial pH value, and increased at the beginning and then decreased with increasing ion initial concentration. However, the effect of solution temperature on ion adsorption was not obvious. The adsorption capacity of each heavy metal ions followed the sequence:Zn2+>Fe3+> Cd2+>Cu2+>Pb2+>Mn2+, and it was closely related with ions hydrated radius and hydration free energy.
(2) The optimal conditions for Pb2+ions adsorption on natural diatomite is Wo8.0g/L, Co400mg/L, pH7.0, T2℃, t120min, that of Cd2+is Wo6.0g/L, Co200mg/L, pH5.0, T25℃,t120min, that of Cu2+is Wo6.0g/L, Co300mg/L, pH5.0, T25℃,/120min, that of Zn2+is Wo8.0g/L, Co500mg/L, pH6.0, T25℃, t120min, that of Mn2+is Wo8.0g/L, Co150mg/L, pH4.5, T25℃, t120min, that of Fe3+Wo4.0g/L, Co400mg/L, pH5.0,725℃, t120min.
(3) The most suitable isotherm model for describing adsorption of Pb2+, Cd2+Cu2+, Zn2+, Mn2+, Fe3+on natural diatomite was Tenkin, Tenkin, Langmuir, Tenkin, Freundlich and Freundlich, respectively. The most suitable kinetic model for describing adsorption of each ion is Pseudo-second-order. The nature of each ion adsorption on natural diatomite was physical, favorable, and the control step of each ion adsorption process was adsorption reaction happened in diatomite micro-pores. The adsorption process of each ion on natural diatomite was spontaneous, endothermic, and disorder enhancing. Classical isotherm models have problems of obvious adsorption concentration effect and unstable parameters, equilibrium ion adsorption density qe is not single function of the equilibrium ion concentration Ce in bulk solution, while is the function of two variable viz. Ce and Wo, qe only depends on Ce/Wo.
(4) The results of normal chemical modification indicated that, the optimal calcination temperature was400℃, the optimal acid solution (HC1) concentration (v/v) was10%, the optimal concentration of NaCl (n/v), BaCl1(n/v) and PAM (m/v) for diatomite modification was0.4mol/L,0.05mol/L and20g/L, respectively. Calcination and acid solution immersing only can remove the impurities from surface and pores of natural diatomite, modification by NaCl mainly increased diatomite adsorption capacity by enhancing surface negative charge, modification by BaCl2and H2SO4mainly improved diatomite pore structure by deposited crystal polishing, and PAM coated modification apparently increased adsorption capacity significantly (Adsorption density of Pb2+on diatomite modified by PAM is five times of natural diatomite). In fact, Pb2+ions removal mainly depended on PAM self flocculation.
(5) The results of deep pillaring modification indicated that, compared with normal modification methods, polyhydroxyl-aluminum pillaring can improve diatomite pore structure obviously. Diatomite adsorption capacity attained greatly increase after pillaring. The adsorption capacity of Pb2+on pillared diatomite reached14.02mg/g, and it was higher than most other adsorbents. The experimental data showed that pillared diatomite yielding the optimal adsorption density (qe) of Pb2+was synthesized using the following parameters:addition of pillaring solution containing Al3+-oligomers with a concentration range of0.1-0.2mol/L to a suspension containing Na+-diatomite to obtain the required Al/diatomite ratio of10mmol/g; synthesis temperature of80℃for120min; aging at a temperature of105℃for16h.
(6) The development of shaped diatomite sample indicated that, the optimal addition ratio of powder diatomite and superfine carbon was93.0%and7.0%, the optimal sintering temperature range was800-1000℃, the optimal calcination time was90min, the optimal diatomite particle size was2.40μm, while preparing pillared diatomite. The shaped diatomite sample was homogeneous brown oval particle with a size of5mm, and was not easy broken. The shaped diatomite samples remained original pore structure, its surface impurities was removed, its pore size was increased, and its pore structure became clear. The main phase of shaped diatomite samples was cristobalite.
(7) The adsorption property of shaped diatomite samples was increased by7.58%compared with natural diatomite; it indicated that shaping didn't destroy diatomite pore structure, instead improved. The maneuverability of shaped diatomite samples was better than natural diatomite. The aim of shaping attained, viz. increasing diatomite maneuverability significantly based on ensuring its adsorption property.
(8) The results of diatomite application in treatment of wastewater containing Fe3+ions indicated that, industry wastewater containing Fe3+can be disposed effectively by the treatment process with core material of shaped diatomite samples, the effluent quality reached the requirement of GB/T18921-2002. it was feasible to dispose landfill leachate by Fenton reagent which prepared by H2O2and waste acid solution obtained from shaped diatomite sample regeneration. The successful use of waste acid solution achieved environmental protection idea "waste control by waste".
硅藻土因具有多孔结构、大比表面积和众多活性基团,常被用作吸附材料。但是由于含有杂质和理化构造缺陷而存在吸附能力一般,可操作性差等不足,使硅藻土在含重金属离子废水处理应用中具有一定局限性。针对上述问题,本文围绕硅藻土开展了吸附、改性、成形及应用等系列研究,获取了一大批科学数据,对于水体重金属污染的有效防治和硅藻土资源的充分利用具有十分重要的意义。主要研究结果如下：
(1)天然硅藻土对各重金属离子的吸附量,随着吸附时间的延长而迅速增大之后趋于平衡；随着吸附剂浓度的增加而先增大后减小；随着pH值的增大而不断增大；随着离子初始浓度的增大而先增大后减小；而温度对吸附量的影响规律不明显。对各重金属离子吸附能力大小顺序为Zn2+>Fe3+> Cd2+>Cu2+> Pb2+> Mn2+,吸附能力与各离子的水合半径及水合自由能密切相关。
(2)天然硅藻土对Pb2+的最佳吸附条件为Wo8.0g/L、Co400mg/L、pH7.0、 T25℃、t120min,对Cd2+的为Wo6.0g/L、Co200mg/L、pH5.0、T25℃、t120min,对Cu2+的为W06.0g/L、C0300mg/L、pH5.0、T25℃、t120min,对Zn2+的为W8.0g/L、C0500mg/L、pH6.0、T25℃、t120min,对Mn2+的为W08.0g/L、Co150mg/L pH4.5、T25℃、t120min,对Fe3+的为W04.0g/L、C0400mg/L、pH5.0、T25℃t120min。
(3)最适合描述天然硅藻土对Pb2+、Cd2+、 Cu2+、Zn2+、Mn2+、Fe3+的等温吸附模型分别为Tenkin、Tenkin、Langmuir、Tenkin、Freundlich和Freundlich模型；最适合描述天然硅藻土对各重金属离子的吸附动力学属性的模型是二级动力学模型；天然硅藻土对各重金属离子的吸附是容易进行的,以物理过程为主；吸附过程是自发的、吸热的、无序性增加的,吸附过程速率控制步骤均为发生在微孔内的吸附反应；经典吸附模型应用于天然硅藻土/重金属离子体系时存在明显的吸附剂浓度效应问题和参数值不稳定现象,平衡吸附量qe不是Ce的唯一函数,而是Ce与W0两个变量的函数,qe与Ce/W0具有一一对应的函数关系。
(4)常规化学改性结果表明,最佳焙烧温度和酸液浓度(HCl,v/v)分别为400℃和10%；最佳钠盐、钡盐改性浓度(n/v)分别为0.4mol/L和0.05mol/L；最佳PAM改性浓度(m/v)为20g/L。焙烧、酸洗改性机制为去除硅藻土表面及孔道内的杂质,钠盐改性机制为增强硅藻土表面负电性,钡盐改性机制为通过沉积晶体擦除表面杂质,而PAM包覆改性表象上可以大幅度提升硅藻土的吸附容量(较天然硅藻土增加了近5倍),实质上主要是PAM自身絮凝作用的结果。
(5)深度柱撑改性结果表明,与常规改性技术相比,聚羟基铝柱撑能够有效改善硅藻土的孔隙结构,显著提升硅藻土吸附能力,对Pb2+的吸附容量可达14.02mg/g(较天然硅藻土提高了39.88%),在众多吸附剂当中处于中上水平。最佳改性条件为：柱化剂浓度0.1～0.2mo1/L,A1/土比(n/m)10mmol/g,反应温度80。C反应时间120min,老化温度105℃,老化时间16h。
(6)成形样品研发结果表明,粉体硅藻土最适投加比为93.0%,超细碳粉的最适投加比为7.0%,最适烧成温度范围为800-1000℃,最适焙烧时间为90min,最适硅藻土粉体粒径为2.40μm。硅藻土成形样品为有一定强度,大小尺寸均匀、粒径约为5mm,褐色椭圆颗粒；成形样品仍保留了原有的多孔形貌,表面杂质得到了清除,孔径增大,孔隙结构更加明朗；物相组成以方石英相为主。
(7)硅藻土成形样品对Pb2+的吸附容量较天然硅藻土提高了7.58%,吸附能力没有下降反而得到了适度提升,说明成形过程对硅藻土的孔隙结构并没有造成破坏,反而有适度改善。成形样品可操作性也明显优于粉体硅藻土,试验结果达到了预期的目的,即在保证硅藻土吸附能力的前提下明显提高其可操作性。
(8)应用硅藻土处理含Fe3+废水中试研究表明,以硅藻土成形样品为核心填料的组合处理工艺可以有效处理含Fe3+废水,出水水质可达GB/T18921-2002《城市污水再生利用、景观环境用水水质标准》要求。利用硅藻土成形样品再生酸洗废液与H202制备Fenton试剂处理垃圾渗滤液切实可行,硅藻土成形样品再生酸洗废液成功的利用实现了以废治废的环保理念。
The effective treatment of wastewater containing heavy metal ions is much important for the control and remediation of water heavy metal pollution. At present, the methods used for treatment of wastewater containing heay metal ions mainly includes ion exchange, colloid precipitation, electronic remediation, bioremediation and adsorption. Compared with other methods, the adsorption is used more widely due to its advantages of stable, reliable, simple, low power consumption, low repeated pollution. As an important method for wastewater treatment, the key issue of adsorption is adsorbent choice. For treatment of wastewater containing heavy metal ions, adsorbent should be in possession of potential for adsorbing and fixing heavy metal ions effectively, as well as rich source, low cost and easy regeneration. Diatomite is selected from series adsorbents due to it fit to all demands for adsorption application.
Diatomite has micropore structure, large specific surface area and many active chemical groups. Hence, it is commonly used for adsorbent. However, diatomite has disadvantage of normal adsorption performance and poor maneuverability due to impurities and structure defects, these disadvantages limits application of diatomite in treatment of wastewater containing heavy metal ions. In order to improve the adsorption performance and maneuverability of diatomite, the studies on diatomite adsorption, modification, shaping and application have been conducted, a large number of scientific data have been acquired, and these data is very significant for the effective control of water heavy metal pollution and fully utility of diatomite store. Main results obtained from this study are summarized as follows.
(1) Adsorption density (qe) of each heavy metal ions on natural diatomite increased swiftly at the begining and then slowly attained equilibrium with contact time prolonging, increased firstly and then decreased with increasing adsorbent concentration, increased constantly with increasing solution initial pH value, and increased at the beginning and then decreased with increasing ion initial concentration. However, the effect of solution temperature on ion adsorption was not obvious. The adsorption capacity of each heavy metal ions followed the sequence:Zn2+>Fe3+> Cd2+>Cu2+>Pb2+>Mn2+, and it was closely related with ions hydrated radius and hydration free energy.
(2) The optimal conditions for Pb2+ions adsorption on natural diatomite is Wo8.0g/L, Co400mg/L, pH7.0, T2℃, t120min, that of Cd2+is Wo6.0g/L, Co200mg/L, pH5.0, T25℃,t120min, that of Cu2+is Wo6.0g/L, Co300mg/L, pH5.0, T25℃,/120min, that of Zn2+is Wo8.0g/L, Co500mg/L, pH6.0, T25℃, t120min, that of Mn2+is Wo8.0g/L, Co150mg/L, pH4.5, T25℃, t120min, that of Fe3+Wo4.0g/L, Co400mg/L, pH5.0,725℃, t120min.
(3) The most suitable isotherm model for describing adsorption of Pb2+, Cd2+Cu2+, Zn2+, Mn2+, Fe3+on natural diatomite was Tenkin, Tenkin, Langmuir, Tenkin, Freundlich and Freundlich, respectively. The most suitable kinetic model for describing adsorption of each ion is Pseudo-second-order. The nature of each ion adsorption on natural diatomite was physical, favorable, and the control step of each ion adsorption process was adsorption reaction happened in diatomite micro-pores. The adsorption process of each ion on natural diatomite was spontaneous, endothermic, and disorder enhancing. Classical isotherm models have problems of obvious adsorption concentration effect and unstable parameters, equilibrium ion adsorption density qe is not single function of the equilibrium ion concentration Ce in bulk solution, while is the function of two variable viz. Ce and Wo, qe only depends on Ce/Wo.
(4) The results of normal chemical modification indicated that, the optimal calcination temperature was400℃, the optimal acid solution (HC1) concentration (v/v) was10%, the optimal concentration of NaCl (n/v), BaCl1(n/v) and PAM (m/v) for diatomite modification was0.4mol/L,0.05mol/L and20g/L, respectively. Calcination and acid solution immersing only can remove the impurities from surface and pores of natural diatomite, modification by NaCl mainly increased diatomite adsorption capacity by enhancing surface negative charge, modification by BaCl2and H2SO4mainly improved diatomite pore structure by deposited crystal polishing, and PAM coated modification apparently increased adsorption capacity significantly (Adsorption density of Pb2+on diatomite modified by PAM is five times of natural diatomite). In fact, Pb2+ions removal mainly depended on PAM self flocculation.
(5) The results of deep pillaring modification indicated that, compared with normal modification methods, polyhydroxyl-aluminum pillaring can improve diatomite pore structure obviously. Diatomite adsorption capacity attained greatly increase after pillaring. The adsorption capacity of Pb2+on pillared diatomite reached14.02mg/g, and it was higher than most other adsorbents. The experimental data showed that pillared diatomite yielding the optimal adsorption density (qe) of Pb2+was synthesized using the following parameters:addition of pillaring solution containing Al3+-oligomers with a concentration range of0.1-0.2mol/L to a suspension containing Na+-diatomite to obtain the required Al/diatomite ratio of10mmol/g; synthesis temperature of80℃for120min; aging at a temperature of105℃for16h.
(6) The development of shaped diatomite sample indicated that, the optimal addition ratio of powder diatomite and superfine carbon was93.0%and7.0%, the optimal sintering temperature range was800-1000℃, the optimal calcination time was90min, the optimal diatomite particle size was2.40μm, while preparing pillared diatomite. The shaped diatomite sample was homogeneous brown oval particle with a size of5mm, and was not easy broken. The shaped diatomite samples remained original pore structure, its surface impurities was removed, its pore size was increased, and its pore structure became clear. The main phase of shaped diatomite samples was cristobalite.
(7) The adsorption property of shaped diatomite samples was increased by7.58%compared with natural diatomite; it indicated that shaping didn't destroy diatomite pore structure, instead improved. The maneuverability of shaped diatomite samples was better than natural diatomite. The aim of shaping attained, viz. increasing diatomite maneuverability significantly based on ensuring its adsorption property.
(8) The results of diatomite application in treatment of wastewater containing Fe3+ions indicated that, industry wastewater containing Fe3+can be disposed effectively by the treatment process with core material of shaped diatomite samples, the effluent quality reached the requirement of GB/T18921-2002. it was feasible to dispose landfill leachate by Fenton reagent which prepared by H2O2and waste acid solution obtained from shaped diatomite sample regeneration. The successful use of waste acid solution achieved environmental protection idea "waste control by waste".
引文
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