负载型纳米铁铜二元金属的合成与改性及其修复地下水中有机氯污染物的基础研究
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摘要
作为人类重要的水资源,地下水环境面临着日益严重的污染。在我国,地下水环境的污染面积、污染程度和污染物的种类正不断扩大。TCE等卤代烃类污染物具有较强的毒性和致癌性,是浅层地下水中主要的有机污染物之一,其较难生物降解,传统的处理方式耗资大、周期长,且存在降解不完全等问题。近年来研究发现,纳米铁金属粒子是一种高效的还原脱卤剂,能够有效地将卤代烃类的有机物转化为气态烃类。纳米铁粒径小,比表面积大,表面活性高,将其制成浆料直接注入污染的地下水中,是一种新型的原位修复技术,能够实现对污染物的快速降解。
目前,纳米铁在地下水环境的原位修复中应用尚存在一些问题,如纳米粒子微小的尺寸和极高的表面能使其在水体中易于团聚,难分散;单纯纳米铁颗粒脱氯速度慢,稳定性差,易失活;亲水性纳米铁与疏水性的DNAPL(dense nonaqoueous phase liquid)类有机氯代烃分子难于接触而反应;纳米颗粒降解有机卤化物的途径和反应动力学还有待进一步研究。为此,许多学者在纳米铁的合成与修饰,降解有机卤化物的效能,降解污染物的机理等方面开展大量研究。
本论文针对这些问题,结合国家自然科学基金“乳化炭载纳米铁原位修复地下水中有机氯代烃”的部分研究,进行了负载型纳米铁及负载型纳米二元金属的合成研究,并考察负载型纳米材料的组成和形态对三氯乙烯(TCE)还原脱氯性能的影响;研究了表面改性的负载型纳米材料对TCE的还原降解及脱氯性能的长期稳定性;探讨了负载型纳米材料脱氯反应的动力学和反应机理。
(一)在乙醇—水反应体系中,以石墨为载体,采用液相还原和载体沉淀的方式制备负载型纳米Fe0。又分别用分步法和同步法,制备负载型纳米Fe/Cu二元金属复合材料。
合成的纳米Fe0均匀分散于石墨表面,单个铁颗粒粒径为50~80nm,是由许多微小粒子组成的球状团簇,晶形为微晶态体心立方形α-Fe0。Fe负载量为15wt%的负载铁比表面积为23.8 m2/g,高于其它Fe负载量的材料。选用一步法和两步法分别合成了负载型纳米Fe/Cu二元金属,负载型二元金属的比表面积、在石墨表面的形态及大小与单纯纳米Fe0基本相近。
(二)分别应用负载型纳米Fe0、不同方式制备的负载型纳米Fe/Cu对TCE进行还原脱氯。
负载型纳米Fe0、采用分步法制备的负载型纳米Fe/Cu二元金属及非负载型的纳米Fe/Cu二元金属这几种材料中,负载型纳米Fe/Cu二元金属对TCE具有最高的还原脱氯性能,反应体系中Fe0浓度为10g/L,能够在5小时内将10mg/L的TCE全部去除;非负载型纳米二元金属在溶液中易团聚,团聚后其脱氯反应活性降低;具有较高比表面积的负载型纳米Fe0对TCE的脱氯性能并不高。
采用Fe2+和Cu2+同步还原制备的纳米二元金属还原脱氯性能较差;由于石墨载体对Fe0的分散有效地控制了纳米粒子的团聚,干法和湿法两种方式均适用于合成负载型纳米材料的后处理。
二元金属中Cu与Fe0的质量百分比为4wt%时,材料对TCE具有最快的还原脱氯速率。Cu的含量较高或较低时,纳米二元金属的还原脱氯性能下降。
Fe2+浓度为0.2mol/L时,合成了晶须状结构的纳米Fe0;Fe2+浓度为0.02mol/L时,球状纳米Fe0的粒径分布不均匀;Fe2+浓度为0.05 mol/L时,得到粒径均匀的球状纳米铁,此结构的二元金属具有最高的还原脱氯性能。
(三)采用生物降解性良好,对环境无毒的阳离子表面活性剂十六烷基三甲基溴化铵CATB,对负载型纳米Fe/Cu二元金属进行表面改性处理。
负载型纳米Fe/Cu复合材料改性后,部分表面由亲水性转变为疏水性,有利于与疏水性的TCE分子相吸附,在脱氯反应中加强了吸附TCE分子的性能,加速了还原降解。当Fe0投加量为5g/L时,4小时将10mg/L的TCE去除完全。Fe0投加浓度太高时,过多H2占据Fe0的活性反应位及溶液pH的升高,抑制了TCE的还原脱氯反应。
杂质离子NO3-,SO42-对负载纳米二元金属的还原脱氯没有影响,溶液中离子强度增加使脱氯更快速。在36天周期内的长期脱氯实验中,改性材料具有较高的稳定性和还原性能,改性后纳米铁不易氧化失活。
(四)采用准一级反应动力学模型研究了负载型纳米Fe/Cu二元金属还原TCE的反应动力学,探讨了复合材料对TCE的脱氯还原机理。
通过线性回归,脱氯反应较好的符合准一级反应动力学模型;当Cu在Fe上质量百分比为4wt%时,脱氯反应的表观反应速率常数Kobs最大;TCE初始浓度在较高浓度范围的表观速率常数比浓度较低时的Kobs要低;表面积归一化反应速率常数Ksa在Fe0投加量在1.25g/L的反应条件下最高,加大Fe0浓度时,Ksa均有所下降。
在对TCE的还原脱氯过程中,TCE的π电子与Cu的空轨道能够形成过渡络合物Cu…Cl…R,H2O在纳米Fe0表面被还原形成高还原性的新生态H2*,两者反应使得TCE脱去Cl-而被还原;石墨作为载体与纳米铁组成许多微小原电池,电池反应中H2O同时得到电子而生成H2,溶液pH在反应后升高。
三种二氯乙烯中间副产物在脱氯反应中没有检测到,由于TCE的脱氯是在具有催化活性的金属表面依次快速进行直到完全脱氯,中间产物不会从金属表面脱附而在液相中累积。
Fe3O4为二元金属脱氯后的腐蚀产物,当其在Fe0表面生成量过多而将铁表面逐渐包覆后,金属的还原活性逐渐减弱直到完全失活。
Groundwater as the important water source of human is now encountered enormous contamination. In our country, the groundwater contamination scale, degree and the variety of pollutants are becoming larger. Halogenated hydrocarbons such as trichloroethylene (TCE), which are strongly toxic and carcinogenic are found the main contaminants in shallow groundwater. Halogenated hydrocarbons are difficult to biodegrade and the conventional treatments technologies for it required long-term operational periods, incurring high operation costs. It is also found that the halogenated hydrocarbons could not degraded completely and produce the more toxic interim products under some remediation technologies. Recent studies show that nano zero-valent iron (ZVI) is the new and highly effective reductant on the transforming halogenated organic contamination to hydrocarbons. The nano scale ZVI particles have the small sizes, the large surface areas and high surface reactivity. The nano ZVI slurry can be directly injected under pressure to contaminated groundwater for remediation. This treatment method is a new in situ remediation technology which can be rapidly removed the pollutants in short term.
There are also some drawbacks on the in situ remediation of groundwater with nano ZVI. For example, nano ZVI particles have the potential of congregation in the solution due to their high surface area and high surface energy. Nano ZVI has the lower efficiency of the dechlorination and the poor stabilization in the air. It is not easy to contact and react between the dense nonaqueous phase liquids (DNAPL) such as TCE and the hydrophilic nano ZVI. The pathways and mechanisms of dechlorination by nano ZVI also require the more studies. Accordingly many researchers work on the preparation and modification of nano ZVI. The efficiency and mechanism of nano ZVI on the destroying halogenated hydrocarbons are also the interesting focus.
In our research,which is a part of the project funded by National Science Committee named“The in-situ remediation of chlorinated hydrocarbons in groundwater with supported nano scale iron emulsion”the preparation of supported nano ZVI and nano Fe/Cu bimetal are presented. This study is aimed to: research the dechlorination efficiency of supported nano materials with different shapes and composition; research the effect of the surface modified supported nano metal on the removal of TCE and assess their stability; characterize and discuss the dechlorination kinetic and mechanism by supported nano metals.
1. Synthesis of supported nano ZVI was achieved by liquid phase reduction and deposition while the graphite was the carrier of iron particles in ethanol/water system. The supported nano Fe/Cu bimetal was prepared by two methods of one-step and two-step.
The nano ZVI particles with the size of 50~100nm were well dispersed on the surface of graphite. The individual iron nanocluster was composed by many small particles and is theα-Fe0.The surface area of supported nano iron with Fe loading of 15wt% was 23.8 m2/g and higher than other materials. The supported nano bimetal have the similar shape, size and surface area with the supported nano iron.
2. The supported nano iron and nano bimetal were utilized in the dechlorination of TCE.
The supported nano bimetal prepared by two-step was the most powerful reductant as compared to the supported nano iron and non-supported nano bimetal on the dechlorination of TCE. The 10mg/L TCE was completely removed in 5 hours by the supported nano bimetal. The non-supported nano bimetal was apt to aggregate in the aqueous phase so that its reactivity decreased in the reduction. The supported nano iron has the lower efficiency on the TCE reduction despite with the high surface area.
The supported nano bimetal synthesized while the Fe2+and Cu2+ were reducing at the same time had the poor dechlorination efficiency. The nano bimetal particles were not easy to congregate due to the carrying by support, so the dry and wet treatment methods on nano metal were applicable at the end of synthesizing.
The supported nano bimetal with 4wt% Cu on Fe0 had the fastest dechlorination rate. The material with higher or lower Cu mass neither has the better reducing effect on TCE.
The nano iron had the whisker shape while the Fe2+ concentration was 0.02mol/L during the synthesizing. The size of nano iron was non-uniformly when the Fe2+ concentration was 0.2mol/L and the nano iron has the uniformly sphere shape when the Fe2+ concentration was 0.05mol/L. The nano bimetal with this shape had the fastest dechlorination rate on TCE.
3. The cationic surfactant Cetyltrimethyl Ammonium Bromide (CTAB) that has the better effect of biodegradation and is nontoxic to the environment was used to modify the surface of the supported nano bimetal.
The hydrophilic surface of supported nano bimetal was transformed to the hydrophobic after modification. The hydrophobic bimetal was advantageous to contact with the nonaqueous TCE molecule and had the effect of dechlorination and sorption. When the Fe0 was 5g/L, the 10mg/L TCE could be completely removed in 4 hours. When the dosage of Fe0 was larger, the active reaction site of Fe0 was occupied by the excess H2 and the pH was increasing so that dechlorination was be prohibited. The ion of NO3-,SO42- could not weaken the dechlorination efficiency of modified supported nano bimetal because the enhancing ionic intensity facilitated the TCE reduction. During the 36 days of continuous dechlorination, the modified supported nano bimetal has the highly stable property and was not easy to be oxidized.
4. The kinetic of TCE dechlorination was studied according the pseudo-first order model. The mechanism of dechlorination was also discussed in the paper.
The dechlorination reaction by nano bimetal was better followed the pseudo-first order equation. When the Cu was 4wt% percent of Fe0, the apparent rate constants Kobs of dechlorination was the largest; the apparent rate constants Kobs of dechlorination at the high initial TCE concentration was smaller than the constants at the low initial TCE concentration; the surface-normalized rate constant Ksa had the maximum value when the Fe0 dosage is 5g/L.
Theπelectron of TCE could be bonded with empty electron orbit of Cu to become the Cu…Cl…R transition substance and the high reactivity H2* was also produced on the surface of Fe0. The H2* attacked the Cu…Cl…R on the surface of bimetal so the Cl- was broken away. The graphite and the nano iron composed large numbers of galvanic cell. The H2O obtained the electrons to produce H2 in the galvanic reaction and the pH value of solution was increasing.
The three kinds of dichloromethane of interim dechlorination products were not detected during the reaction. Because the Cl elimination of TCE was took place on the surface of nano bimetal with catalytic reactivity, the intermediate products were adsorbed on the metal and could not transplant to the liquid phase.
It was found that Fe3O4 was the corrosion product of Fe oxidation after dechlorination. The attenuation of reduction activity of nano metal could be attributed to excess oxide precipitates on the surface. Fe3O4 entirely covered on nano metal surface eventually lead the losing of reduction reactivity.
目前,纳米铁在地下水环境的原位修复中应用尚存在一些问题,如纳米粒子微小的尺寸和极高的表面能使其在水体中易于团聚,难分散;单纯纳米铁颗粒脱氯速度慢,稳定性差,易失活;亲水性纳米铁与疏水性的DNAPL(dense nonaqoueous phase liquid)类有机氯代烃分子难于接触而反应;纳米颗粒降解有机卤化物的途径和反应动力学还有待进一步研究。为此,许多学者在纳米铁的合成与修饰,降解有机卤化物的效能,降解污染物的机理等方面开展大量研究。
本论文针对这些问题,结合国家自然科学基金“乳化炭载纳米铁原位修复地下水中有机氯代烃”的部分研究,进行了负载型纳米铁及负载型纳米二元金属的合成研究,并考察负载型纳米材料的组成和形态对三氯乙烯(TCE)还原脱氯性能的影响;研究了表面改性的负载型纳米材料对TCE的还原降解及脱氯性能的长期稳定性;探讨了负载型纳米材料脱氯反应的动力学和反应机理。
(一)在乙醇—水反应体系中,以石墨为载体,采用液相还原和载体沉淀的方式制备负载型纳米Fe0。又分别用分步法和同步法,制备负载型纳米Fe/Cu二元金属复合材料。
合成的纳米Fe0均匀分散于石墨表面,单个铁颗粒粒径为50~80nm,是由许多微小粒子组成的球状团簇,晶形为微晶态体心立方形α-Fe0。Fe负载量为15wt%的负载铁比表面积为23.8 m2/g,高于其它Fe负载量的材料。选用一步法和两步法分别合成了负载型纳米Fe/Cu二元金属,负载型二元金属的比表面积、在石墨表面的形态及大小与单纯纳米Fe0基本相近。
(二)分别应用负载型纳米Fe0、不同方式制备的负载型纳米Fe/Cu对TCE进行还原脱氯。
负载型纳米Fe0、采用分步法制备的负载型纳米Fe/Cu二元金属及非负载型的纳米Fe/Cu二元金属这几种材料中,负载型纳米Fe/Cu二元金属对TCE具有最高的还原脱氯性能,反应体系中Fe0浓度为10g/L,能够在5小时内将10mg/L的TCE全部去除;非负载型纳米二元金属在溶液中易团聚,团聚后其脱氯反应活性降低;具有较高比表面积的负载型纳米Fe0对TCE的脱氯性能并不高。
采用Fe2+和Cu2+同步还原制备的纳米二元金属还原脱氯性能较差;由于石墨载体对Fe0的分散有效地控制了纳米粒子的团聚,干法和湿法两种方式均适用于合成负载型纳米材料的后处理。
二元金属中Cu与Fe0的质量百分比为4wt%时,材料对TCE具有最快的还原脱氯速率。Cu的含量较高或较低时,纳米二元金属的还原脱氯性能下降。
Fe2+浓度为0.2mol/L时,合成了晶须状结构的纳米Fe0;Fe2+浓度为0.02mol/L时,球状纳米Fe0的粒径分布不均匀;Fe2+浓度为0.05 mol/L时,得到粒径均匀的球状纳米铁,此结构的二元金属具有最高的还原脱氯性能。
(三)采用生物降解性良好,对环境无毒的阳离子表面活性剂十六烷基三甲基溴化铵CATB,对负载型纳米Fe/Cu二元金属进行表面改性处理。
负载型纳米Fe/Cu复合材料改性后,部分表面由亲水性转变为疏水性,有利于与疏水性的TCE分子相吸附,在脱氯反应中加强了吸附TCE分子的性能,加速了还原降解。当Fe0投加量为5g/L时,4小时将10mg/L的TCE去除完全。Fe0投加浓度太高时,过多H2占据Fe0的活性反应位及溶液pH的升高,抑制了TCE的还原脱氯反应。
杂质离子NO3-,SO42-对负载纳米二元金属的还原脱氯没有影响,溶液中离子强度增加使脱氯更快速。在36天周期内的长期脱氯实验中,改性材料具有较高的稳定性和还原性能,改性后纳米铁不易氧化失活。
(四)采用准一级反应动力学模型研究了负载型纳米Fe/Cu二元金属还原TCE的反应动力学,探讨了复合材料对TCE的脱氯还原机理。
通过线性回归,脱氯反应较好的符合准一级反应动力学模型;当Cu在Fe上质量百分比为4wt%时,脱氯反应的表观反应速率常数Kobs最大;TCE初始浓度在较高浓度范围的表观速率常数比浓度较低时的Kobs要低;表面积归一化反应速率常数Ksa在Fe0投加量在1.25g/L的反应条件下最高,加大Fe0浓度时,Ksa均有所下降。
在对TCE的还原脱氯过程中,TCE的π电子与Cu的空轨道能够形成过渡络合物Cu…Cl…R,H2O在纳米Fe0表面被还原形成高还原性的新生态H2*,两者反应使得TCE脱去Cl-而被还原;石墨作为载体与纳米铁组成许多微小原电池,电池反应中H2O同时得到电子而生成H2,溶液pH在反应后升高。
三种二氯乙烯中间副产物在脱氯反应中没有检测到,由于TCE的脱氯是在具有催化活性的金属表面依次快速进行直到完全脱氯,中间产物不会从金属表面脱附而在液相中累积。
Fe3O4为二元金属脱氯后的腐蚀产物,当其在Fe0表面生成量过多而将铁表面逐渐包覆后,金属的还原活性逐渐减弱直到完全失活。
Groundwater as the important water source of human is now encountered enormous contamination. In our country, the groundwater contamination scale, degree and the variety of pollutants are becoming larger. Halogenated hydrocarbons such as trichloroethylene (TCE), which are strongly toxic and carcinogenic are found the main contaminants in shallow groundwater. Halogenated hydrocarbons are difficult to biodegrade and the conventional treatments technologies for it required long-term operational periods, incurring high operation costs. It is also found that the halogenated hydrocarbons could not degraded completely and produce the more toxic interim products under some remediation technologies. Recent studies show that nano zero-valent iron (ZVI) is the new and highly effective reductant on the transforming halogenated organic contamination to hydrocarbons. The nano scale ZVI particles have the small sizes, the large surface areas and high surface reactivity. The nano ZVI slurry can be directly injected under pressure to contaminated groundwater for remediation. This treatment method is a new in situ remediation technology which can be rapidly removed the pollutants in short term.
There are also some drawbacks on the in situ remediation of groundwater with nano ZVI. For example, nano ZVI particles have the potential of congregation in the solution due to their high surface area and high surface energy. Nano ZVI has the lower efficiency of the dechlorination and the poor stabilization in the air. It is not easy to contact and react between the dense nonaqueous phase liquids (DNAPL) such as TCE and the hydrophilic nano ZVI. The pathways and mechanisms of dechlorination by nano ZVI also require the more studies. Accordingly many researchers work on the preparation and modification of nano ZVI. The efficiency and mechanism of nano ZVI on the destroying halogenated hydrocarbons are also the interesting focus.
In our research,which is a part of the project funded by National Science Committee named“The in-situ remediation of chlorinated hydrocarbons in groundwater with supported nano scale iron emulsion”the preparation of supported nano ZVI and nano Fe/Cu bimetal are presented. This study is aimed to: research the dechlorination efficiency of supported nano materials with different shapes and composition; research the effect of the surface modified supported nano metal on the removal of TCE and assess their stability; characterize and discuss the dechlorination kinetic and mechanism by supported nano metals.
1. Synthesis of supported nano ZVI was achieved by liquid phase reduction and deposition while the graphite was the carrier of iron particles in ethanol/water system. The supported nano Fe/Cu bimetal was prepared by two methods of one-step and two-step.
The nano ZVI particles with the size of 50~100nm were well dispersed on the surface of graphite. The individual iron nanocluster was composed by many small particles and is theα-Fe0.The surface area of supported nano iron with Fe loading of 15wt% was 23.8 m2/g and higher than other materials. The supported nano bimetal have the similar shape, size and surface area with the supported nano iron.
2. The supported nano iron and nano bimetal were utilized in the dechlorination of TCE.
The supported nano bimetal prepared by two-step was the most powerful reductant as compared to the supported nano iron and non-supported nano bimetal on the dechlorination of TCE. The 10mg/L TCE was completely removed in 5 hours by the supported nano bimetal. The non-supported nano bimetal was apt to aggregate in the aqueous phase so that its reactivity decreased in the reduction. The supported nano iron has the lower efficiency on the TCE reduction despite with the high surface area.
The supported nano bimetal synthesized while the Fe2+and Cu2+ were reducing at the same time had the poor dechlorination efficiency. The nano bimetal particles were not easy to congregate due to the carrying by support, so the dry and wet treatment methods on nano metal were applicable at the end of synthesizing.
The supported nano bimetal with 4wt% Cu on Fe0 had the fastest dechlorination rate. The material with higher or lower Cu mass neither has the better reducing effect on TCE.
The nano iron had the whisker shape while the Fe2+ concentration was 0.02mol/L during the synthesizing. The size of nano iron was non-uniformly when the Fe2+ concentration was 0.2mol/L and the nano iron has the uniformly sphere shape when the Fe2+ concentration was 0.05mol/L. The nano bimetal with this shape had the fastest dechlorination rate on TCE.
3. The cationic surfactant Cetyltrimethyl Ammonium Bromide (CTAB) that has the better effect of biodegradation and is nontoxic to the environment was used to modify the surface of the supported nano bimetal.
The hydrophilic surface of supported nano bimetal was transformed to the hydrophobic after modification. The hydrophobic bimetal was advantageous to contact with the nonaqueous TCE molecule and had the effect of dechlorination and sorption. When the Fe0 was 5g/L, the 10mg/L TCE could be completely removed in 4 hours. When the dosage of Fe0 was larger, the active reaction site of Fe0 was occupied by the excess H2 and the pH was increasing so that dechlorination was be prohibited. The ion of NO3-,SO42- could not weaken the dechlorination efficiency of modified supported nano bimetal because the enhancing ionic intensity facilitated the TCE reduction. During the 36 days of continuous dechlorination, the modified supported nano bimetal has the highly stable property and was not easy to be oxidized.
4. The kinetic of TCE dechlorination was studied according the pseudo-first order model. The mechanism of dechlorination was also discussed in the paper.
The dechlorination reaction by nano bimetal was better followed the pseudo-first order equation. When the Cu was 4wt% percent of Fe0, the apparent rate constants Kobs of dechlorination was the largest; the apparent rate constants Kobs of dechlorination at the high initial TCE concentration was smaller than the constants at the low initial TCE concentration; the surface-normalized rate constant Ksa had the maximum value when the Fe0 dosage is 5g/L.
Theπelectron of TCE could be bonded with empty electron orbit of Cu to become the Cu…Cl…R transition substance and the high reactivity H2* was also produced on the surface of Fe0. The H2* attacked the Cu…Cl…R on the surface of bimetal so the Cl- was broken away. The graphite and the nano iron composed large numbers of galvanic cell. The H2O obtained the electrons to produce H2 in the galvanic reaction and the pH value of solution was increasing.
The three kinds of dichloromethane of interim dechlorination products were not detected during the reaction. Because the Cl elimination of TCE was took place on the surface of nano bimetal with catalytic reactivity, the intermediate products were adsorbed on the metal and could not transplant to the liquid phase.
It was found that Fe3O4 was the corrosion product of Fe oxidation after dechlorination. The attenuation of reduction activity of nano metal could be attributed to excess oxide precipitates on the surface. Fe3O4 entirely covered on nano metal surface eventually lead the losing of reduction reactivity.
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