膨润土基吸附材料的制备、表征及其吸附性能研究
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摘要
膨润土(bentonite)具有价格低廉、储量丰富、环境友好、吸附容量大等优点，被广泛用作水处理吸附剂的基础材料。膨润土具有特殊二维空间结构、矿物表面吸附作用、层间阳离子交换作用、孔道过滤作用及特殊纳米结构效应等特性，层间结构可控、表面性质可改，经活化、改性或复合改性处理，可制得多种高效膨润土基吸附材料。
本文以阳离子淀粉(CS)、羟基铝(Al-OH)、十六烷基三甲基溴化铵(CTMAB)为改性剂，制备了一系列性能优异的膨润土基吸附材料。全面研究了阳离子淀粉/膨润土吸附材料的制备工艺，阳离子淀粉在膨润土上的吸附等温线、动力学及热力学行为，运用多种技术手段进行了表征；系统研究了阳离子淀粉/膨润土吸附材料对水中特征污染物——染料、有毒有机物、重金属离子以及磷酸盐的吸附机制、吸附规律及影响因素；深入研究了羟基铝和CTMAB改性膨润土对水中不同染料的吸附特性，为拓展膨润土的功能及其在废水处理中的应用提供了理论基础和技术依据。论文主要取得了以下创新性成果：
1.首次合成了新型吸附材料——季铵型阳离子淀粉/膨润土(CS-bentonite)。以季铵型阳离子淀粉作为改性剂，制备了新型淀粉/膨润土吸附材料。与钠基膨润土相比，所得产品表面形貌、电动特性和层间距都发生了变化：比表面积由33.96m~2/g增加到57.76m~2/g，Zeta电位由-24.01mV升高到-13.01mV，层间距由1.244nm增大到1.515nm。利用透射电镜分析(TEM)、扫描电镜分析(SEM)、红外光谱(FTIR)、热重-差热分析(TG-DSC)等对其结构进行了表征，证明新型阳离子淀粉/膨润土吸附材料出现片层剥离，淀粉插层成功，其絮凝性能提高，表面疏水性增强。吸附稳定性实验证明所制备的产品脱附率低，符合废水处理的要求。
2.研究了季铵型阳离子淀粉/膨润土吸附材料合成的制备工艺、反应机理、理论参数以及产品性能特征。以直接影响产品吸附性能的聚合物含量为主要控制指标，通过进行单因素影响实验和设计正交试验，得到最佳制备工艺为：反应温度60℃，反应时间2.0h，体系pH值7.0，阳离子淀粉浓度7.0g/L。阳离子淀粉在膨润土上的吸附动力学数据与拟二级动力学方程相符，吸附等温线符合Langmuir吸附模型；△G~θ为负值，说明吸附过程为自发进行；△S~θ为正值，说明整个吸附体系的熵增加；0<△H~θ<63kJ/mol，说明反应是吸热反应，升温有利于膨润土对阳离子淀粉的吸附，且过程以物理吸附为主。
3.系统研究了淀粉/膨润土吸附材料对水中染料亚甲基兰(MB)和刚果红(CR)、对硝基苯酚(PNP)、重金属离子(Cr(Ⅵ))和磷(PO_4~(3-))等污染物吸附机理及影响因素。阳离子淀粉/膨润土对水中MB、CR和PNP以表面吸附和层间有机相分配为主；对水中Cr(Ⅵ)的吸附以表面吸附和表面配位为主；对PO_4~(3-)以表面吸附为主。染料、对硝基苯酚、Cr(Ⅵ)离子在淀粉/膨润土上的吸附等温线符合Langmiur等温线模型，磷酸根符合Freundlich型等温线模型。四种特征污染物吸附过程都符合拟二级动力学方程，说明吸附过程包括外部液膜扩散、表面吸附和颗粒内扩散等复杂过程。
4、研究了Al-OH和CTMAB改性膨润土去除染料的性能。羟基铝柱撑膨润土（Al-OH-bentonite）对酸性湖蓝A (ATBA)、碱性品红(BV14)和碱性品绿(BG)三种染料的吸附效果要优于钠化膨润土，吸附率均达到95%以上；吸附等温线符合Henry和Langmuir等温线模型，动力学曲线符合拟二级动力学模型；吸附能力大小为：BG>BV14>ATBA。CTMAB有机插层膨润土(CTMAB-bentonite)对酸性品蓝（AB25）、酸性蓝（AB93）、酸性湖蓝A（ATBA）和酸性金黄G（AGYG）的吸附率超过95%，吸附实验数据分别符合Freundlich等温线模型和拟二级动力学方程，吸附能力大小分别为：ATAB>AGYG>AB93>AB25。
本论文通过对新型吸附材料——季铵型阳离子淀粉/膨润土吸附材料对水中染料亚甲基兰和刚果红、对硝基苯酚、Cr(Ⅵ)和磷酸根等污染物的吸附作用研究，得到了其吸附效果、机理、等温线模型及动力学参数，探讨了吸附作用机理，具有较高的理论意义和应用价值。以具有致癌、致畸、致突变结构的染料为研究对象，研究其在羟基铝和CTMAB改性膨润土上的吸附作用，为膨润土处理染料废水提供了理论依据。
Bentonite is an inexpensive, abundant clay mineral, which has good sorptioncapacity and friendly to environment, so it can be used as the basis raw materials incheap bentonite products as adsorbents. The bentonite has some characters, such asspecial2-d space structure, sorption function on mineral surface, high cation exchangecapacity between layers, hole filter function and special nano structure effect. Thestructure between layer and surface properties of the bentonite can be controlled.Therefore, a series of high efficiency and multi-function bentonite complex adsorbentscan be prepared through the activation, modification or multi-modification processing.
In this dissertation, cationic starch, hydroxyl aluminium and CTMAB agents arechosen as raw materials to prepare modified bentonites. A series of novel sorptivematerials with special structures and functions derived from bentonite was synthesizedand their performances on removing dyes, organic compounds, heavy metals andphosphorus in the water were studied at the same time. The relationship betweenstructure characteristics and properties of modified bentonites was explored by modernanalytical and testing technology. As the key points, the sorption mechanism, influencingfactors and laws of cationic starch bentonite (CS-bentonite) as adsorbents on dyes,organic pollutants, heavy metal ions, and phosphorus removal from water were studied.A system experimental investigation about the sorption mechanism, influencing factorsand laws of hydroxyl aluminium and CTMAB modified bentonite materials on dealingwith dye wastewater was made. These studies were tried to provide essential principlesand techniques of the functional modifications of bentonites and the applications onwastewater treatments. The innovative achievements can be summarized as follows:
1. A novel sorptive material of quaternary ammonium cationic starch-bentonite wassynthesized. Quaternary ammonium cationic starch has a series of virtues such as abundance in resources, low price, biodegradability, non-toxicity and good specificationand was used as raw materials to prepare novel sorptive materials in this study. Thesurface topography, electrokinetic chemistry characteristics and layer spacing of theCS-bentonite synthesized had been changed. The specific surface area, Zeta potential andlayer spacing of the modified bentonite were increased from33.96m~2/g,-24.01mV and1.2.44nm to57.76m~2/g,-13.01mV and1.515nm, respectively. The structure ofCS-bentonite was characterized by TEM, SEM, IR, TG-DSC, etc, proving that theexfoliated layers of CS-bentonite were formed, the intercalation of cationic starch wassucceed, the flocculation characteristics were increased and the surface hydrophobicitywas enhanced. The experiment results of sorption stability showed that the desorptionrate of the novel CS-bentonite synthesized was low, meeting the requirements of thepractical application for treating wastewater. As a result, these results show the directionfor the research and development of the novel absorbents.
2. The preparation technology, reaction mechanism, theoretical parameters andperformance features of activation of quaternary ammonium salt cationicstarch-bentonite complex sorption materials were comprehensive explored. Takingpolymer content as the main control index which impacts absorption ability, theorthogonal test was systematacially investigated. The optimum technology of preparationof the high performance starch-bentonite composite sorption materials had been explored:the starch initial concentration, reaction temperature, reaction time and reaction systempH value are7.0g/L,60℃,2.0hand7.0, respectively. The sorption dynamics betweenthe bentonite and cationic starch indicates that the cationic starch sorption is more fit tothe first-order kinetics law and the sorption isotherm is more fit to Langmuir model. Thermodynamics data shows that△G~θ＜0, indicates that sorption process is spontaneous,△S~θ＞0shows that the entropy of whole sorption system increases，0<△H~θ<63kJ/molindicates that the reaction is exothermic and warming is beneficial to the sorption ofbentonite for cationic starch. These research results have high academic and pragmaticimportance. Especially they have theoretical significance for development of neweconomic and stable adsorbents.
3. The sorption mechanism and influencing factors of CS-bentonite materials sorbed wastewater pollutants, such as dyes (Methylene Blue and Congo Red), p-nitrophenol,Cr(Ⅵ) and phosphate had been studied systematically. The results show that cationicstarch-bentonite reacts with dye in water mainly by surface sorption and interlayerorganic phase partitioning; reacts with p-nitrophenol in water mainly by surface sorptionand interlayer organic phase partitioning; reacts with Cr(Ⅵ) mainly by surface sorptionand surface complexation; reacts with phosphate mainly by surface sorption. Thesorption isotherms of dye, p-nitrophenol and Cr(Ⅵ) reacting with the starch/bentoniteaccords with Langmiur isotherms model, but the isotherms of phosphate reacting withthe starch/bentonite accords with Freundlich isotherms model. All the sorption process ofthe four characteristic of pollutants accord with pseudo-second-order kinetic equationwhich suggests that the sorption process are complex, such as external liquid filmdiffusion, surface sorption and intraparticle diffusion. These studies of sorption ruleprovide the consultation basis for the development and utilization of starch-bentonite.
4. The removal of dyes by hydroxy aluminum (Al-OH) and cetyl trimethylammonium bromide (CTMAB) modified bentonite was deeply studied. The sorptioneffects of hydroxy aluminum pillared bentonite on Acid Turquoise Blue A(ATBA), BasicViolet14(BV14) and Basic Green (BG) are better than sodium bentonite with muchmore than95%sorption efficiency; the sorption isotherms accords with Henry andLangmuir isotherms model, kinetic curves conform the proposed second-order kineticsmodel and the order of sorption capability is BG>BV14>ATBA。The sorption ratio ofCTMAB organic intercalation bentonite on Acid Blue25(AB25), Acid Blue29(AB29),Acid Turquoise Blue A(ATBA) and Acid Golden Yellow G (AGYG) dyes are more than95%, the four acid dyes’ sorption experiment data are in line with Freundlich isothermsmodel and proposed second-order kinetics equation, the order of sorption capability isATAB>AGYG>AB93>AB25.
According to the studying the sorption effect of new adsorbent material—quaternaryammonium type Cationic starch-bentonite complexes on the wastewater dyes (MethyleneBlue and Congo Red), p-nitrophenol, Cr(Ⅵ) and phosphate, the sorption effect,mechanism, isotherms model and kinetic parameters were gotten; Opening up thesorption action mechanism and enriching the sorption effect theory in this research will have strong theoretical significance and application value. Study about sorption effect ofdyes on the Al-OH and CTMAB modified bentonites can provide more systematicresearch base for bentonite’s dye wastewater treatment.
本文以阳离子淀粉(CS)、羟基铝(Al-OH)、十六烷基三甲基溴化铵(CTMAB)为改性剂，制备了一系列性能优异的膨润土基吸附材料。全面研究了阳离子淀粉/膨润土吸附材料的制备工艺，阳离子淀粉在膨润土上的吸附等温线、动力学及热力学行为，运用多种技术手段进行了表征；系统研究了阳离子淀粉/膨润土吸附材料对水中特征污染物——染料、有毒有机物、重金属离子以及磷酸盐的吸附机制、吸附规律及影响因素；深入研究了羟基铝和CTMAB改性膨润土对水中不同染料的吸附特性，为拓展膨润土的功能及其在废水处理中的应用提供了理论基础和技术依据。论文主要取得了以下创新性成果：
1.首次合成了新型吸附材料——季铵型阳离子淀粉/膨润土(CS-bentonite)。以季铵型阳离子淀粉作为改性剂，制备了新型淀粉/膨润土吸附材料。与钠基膨润土相比，所得产品表面形貌、电动特性和层间距都发生了变化：比表面积由33.96m~2/g增加到57.76m~2/g，Zeta电位由-24.01mV升高到-13.01mV，层间距由1.244nm增大到1.515nm。利用透射电镜分析(TEM)、扫描电镜分析(SEM)、红外光谱(FTIR)、热重-差热分析(TG-DSC)等对其结构进行了表征，证明新型阳离子淀粉/膨润土吸附材料出现片层剥离，淀粉插层成功，其絮凝性能提高，表面疏水性增强。吸附稳定性实验证明所制备的产品脱附率低，符合废水处理的要求。
2.研究了季铵型阳离子淀粉/膨润土吸附材料合成的制备工艺、反应机理、理论参数以及产品性能特征。以直接影响产品吸附性能的聚合物含量为主要控制指标，通过进行单因素影响实验和设计正交试验，得到最佳制备工艺为：反应温度60℃，反应时间2.0h，体系pH值7.0，阳离子淀粉浓度7.0g/L。阳离子淀粉在膨润土上的吸附动力学数据与拟二级动力学方程相符，吸附等温线符合Langmuir吸附模型；△G~θ为负值，说明吸附过程为自发进行；△S~θ为正值，说明整个吸附体系的熵增加；0<△H~θ<63kJ/mol，说明反应是吸热反应，升温有利于膨润土对阳离子淀粉的吸附，且过程以物理吸附为主。
3.系统研究了淀粉/膨润土吸附材料对水中染料亚甲基兰(MB)和刚果红(CR)、对硝基苯酚(PNP)、重金属离子(Cr(Ⅵ))和磷(PO_4~(3-))等污染物吸附机理及影响因素。阳离子淀粉/膨润土对水中MB、CR和PNP以表面吸附和层间有机相分配为主；对水中Cr(Ⅵ)的吸附以表面吸附和表面配位为主；对PO_4~(3-)以表面吸附为主。染料、对硝基苯酚、Cr(Ⅵ)离子在淀粉/膨润土上的吸附等温线符合Langmiur等温线模型，磷酸根符合Freundlich型等温线模型。四种特征污染物吸附过程都符合拟二级动力学方程，说明吸附过程包括外部液膜扩散、表面吸附和颗粒内扩散等复杂过程。
4、研究了Al-OH和CTMAB改性膨润土去除染料的性能。羟基铝柱撑膨润土（Al-OH-bentonite）对酸性湖蓝A (ATBA)、碱性品红(BV14)和碱性品绿(BG)三种染料的吸附效果要优于钠化膨润土，吸附率均达到95%以上；吸附等温线符合Henry和Langmuir等温线模型，动力学曲线符合拟二级动力学模型；吸附能力大小为：BG>BV14>ATBA。CTMAB有机插层膨润土(CTMAB-bentonite)对酸性品蓝（AB25）、酸性蓝（AB93）、酸性湖蓝A（ATBA）和酸性金黄G（AGYG）的吸附率超过95%，吸附实验数据分别符合Freundlich等温线模型和拟二级动力学方程，吸附能力大小分别为：ATAB>AGYG>AB93>AB25。
本论文通过对新型吸附材料——季铵型阳离子淀粉/膨润土吸附材料对水中染料亚甲基兰和刚果红、对硝基苯酚、Cr(Ⅵ)和磷酸根等污染物的吸附作用研究，得到了其吸附效果、机理、等温线模型及动力学参数，探讨了吸附作用机理，具有较高的理论意义和应用价值。以具有致癌、致畸、致突变结构的染料为研究对象，研究其在羟基铝和CTMAB改性膨润土上的吸附作用，为膨润土处理染料废水提供了理论依据。
Bentonite is an inexpensive, abundant clay mineral, which has good sorptioncapacity and friendly to environment, so it can be used as the basis raw materials incheap bentonite products as adsorbents. The bentonite has some characters, such asspecial2-d space structure, sorption function on mineral surface, high cation exchangecapacity between layers, hole filter function and special nano structure effect. Thestructure between layer and surface properties of the bentonite can be controlled.Therefore, a series of high efficiency and multi-function bentonite complex adsorbentscan be prepared through the activation, modification or multi-modification processing.
In this dissertation, cationic starch, hydroxyl aluminium and CTMAB agents arechosen as raw materials to prepare modified bentonites. A series of novel sorptivematerials with special structures and functions derived from bentonite was synthesizedand their performances on removing dyes, organic compounds, heavy metals andphosphorus in the water were studied at the same time. The relationship betweenstructure characteristics and properties of modified bentonites was explored by modernanalytical and testing technology. As the key points, the sorption mechanism, influencingfactors and laws of cationic starch bentonite (CS-bentonite) as adsorbents on dyes,organic pollutants, heavy metal ions, and phosphorus removal from water were studied.A system experimental investigation about the sorption mechanism, influencing factorsand laws of hydroxyl aluminium and CTMAB modified bentonite materials on dealingwith dye wastewater was made. These studies were tried to provide essential principlesand techniques of the functional modifications of bentonites and the applications onwastewater treatments. The innovative achievements can be summarized as follows:
1. A novel sorptive material of quaternary ammonium cationic starch-bentonite wassynthesized. Quaternary ammonium cationic starch has a series of virtues such as abundance in resources, low price, biodegradability, non-toxicity and good specificationand was used as raw materials to prepare novel sorptive materials in this study. Thesurface topography, electrokinetic chemistry characteristics and layer spacing of theCS-bentonite synthesized had been changed. The specific surface area, Zeta potential andlayer spacing of the modified bentonite were increased from33.96m~2/g,-24.01mV and1.2.44nm to57.76m~2/g,-13.01mV and1.515nm, respectively. The structure ofCS-bentonite was characterized by TEM, SEM, IR, TG-DSC, etc, proving that theexfoliated layers of CS-bentonite were formed, the intercalation of cationic starch wassucceed, the flocculation characteristics were increased and the surface hydrophobicitywas enhanced. The experiment results of sorption stability showed that the desorptionrate of the novel CS-bentonite synthesized was low, meeting the requirements of thepractical application for treating wastewater. As a result, these results show the directionfor the research and development of the novel absorbents.
2. The preparation technology, reaction mechanism, theoretical parameters andperformance features of activation of quaternary ammonium salt cationicstarch-bentonite complex sorption materials were comprehensive explored. Takingpolymer content as the main control index which impacts absorption ability, theorthogonal test was systematacially investigated. The optimum technology of preparationof the high performance starch-bentonite composite sorption materials had been explored:the starch initial concentration, reaction temperature, reaction time and reaction systempH value are7.0g/L,60℃,2.0hand7.0, respectively. The sorption dynamics betweenthe bentonite and cationic starch indicates that the cationic starch sorption is more fit tothe first-order kinetics law and the sorption isotherm is more fit to Langmuir model. Thermodynamics data shows that△G~θ＜0, indicates that sorption process is spontaneous,△S~θ＞0shows that the entropy of whole sorption system increases，0<△H~θ<63kJ/molindicates that the reaction is exothermic and warming is beneficial to the sorption ofbentonite for cationic starch. These research results have high academic and pragmaticimportance. Especially they have theoretical significance for development of neweconomic and stable adsorbents.
3. The sorption mechanism and influencing factors of CS-bentonite materials sorbed wastewater pollutants, such as dyes (Methylene Blue and Congo Red), p-nitrophenol,Cr(Ⅵ) and phosphate had been studied systematically. The results show that cationicstarch-bentonite reacts with dye in water mainly by surface sorption and interlayerorganic phase partitioning; reacts with p-nitrophenol in water mainly by surface sorptionand interlayer organic phase partitioning; reacts with Cr(Ⅵ) mainly by surface sorptionand surface complexation; reacts with phosphate mainly by surface sorption. Thesorption isotherms of dye, p-nitrophenol and Cr(Ⅵ) reacting with the starch/bentoniteaccords with Langmiur isotherms model, but the isotherms of phosphate reacting withthe starch/bentonite accords with Freundlich isotherms model. All the sorption process ofthe four characteristic of pollutants accord with pseudo-second-order kinetic equationwhich suggests that the sorption process are complex, such as external liquid filmdiffusion, surface sorption and intraparticle diffusion. These studies of sorption ruleprovide the consultation basis for the development and utilization of starch-bentonite.
4. The removal of dyes by hydroxy aluminum (Al-OH) and cetyl trimethylammonium bromide (CTMAB) modified bentonite was deeply studied. The sorptioneffects of hydroxy aluminum pillared bentonite on Acid Turquoise Blue A(ATBA), BasicViolet14(BV14) and Basic Green (BG) are better than sodium bentonite with muchmore than95%sorption efficiency; the sorption isotherms accords with Henry andLangmuir isotherms model, kinetic curves conform the proposed second-order kineticsmodel and the order of sorption capability is BG>BV14>ATBA。The sorption ratio ofCTMAB organic intercalation bentonite on Acid Blue25(AB25), Acid Blue29(AB29),Acid Turquoise Blue A(ATBA) and Acid Golden Yellow G (AGYG) dyes are more than95%, the four acid dyes’ sorption experiment data are in line with Freundlich isothermsmodel and proposed second-order kinetics equation, the order of sorption capability isATAB>AGYG>AB93>AB25.
According to the studying the sorption effect of new adsorbent material—quaternaryammonium type Cationic starch-bentonite complexes on the wastewater dyes (MethyleneBlue and Congo Red), p-nitrophenol, Cr(Ⅵ) and phosphate, the sorption effect,mechanism, isotherms model and kinetic parameters were gotten; Opening up thesorption action mechanism and enriching the sorption effect theory in this research will have strong theoretical significance and application value. Study about sorption effect ofdyes on the Al-OH and CTMAB modified bentonites can provide more systematicresearch base for bentonite’s dye wastewater treatment.
引文
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