EDTA存在下光诱导铁氧化物的形成及机理
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摘要
由于纳米铁氧化物在催化、防腐、颜料、磁记录材料等领域有着广泛的应用,使得纳米铁氧化物的制备备受关注。从制备铁氧化物的原料区分可以将其分为两大类:一类是以Fe(Ⅲ)盐为原料,另一类则是以Fe(Ⅱ)盐为原料。本文以FeSO_4和NaOH为原料,主要研究了Fe(OH)_2悬浮液在不同条件下的氧化机制,旨在找出其规律,为今后以FeSO_4为原料制备不同的铁氧化物提供必要的实验数据。本文的创新之处在于采用O_3作氧化剂氧化Fe(OH)_2悬浮液并得到了一种新型的筏状γ-FeOOH,另外本文率先将可见光的影响引入实验体系,并对其影响机制进行了初步探讨。
本文作者在前人工作的基础上,改用O_3作氧化剂研究了O_3氧化Fe(OH)_2悬浮液的过程,找到了其主要影响因素——初始pH值和EDTA,并分别对二者进行了研究。结果表明在弱碱性范围内pH值对产物的影响非常敏感,当初始pH值为8.6或8.5时可以得到纯相的γ-FeOOH,当初始pH值升高到8.7时得到的则是纯相的α-FeOOH。通过对产物进行透射电镜表征可以发现得到的γ-FeOOH为纳米筏状结构,α-FeOOH为无定形态。在室温下,O_3氧化Fe(OH)_2生成何种产物取决于氧化速率和pH:在pH值大于8.7时O_3在水中能够分解出氧化能力极强的新生态氧[O]和羟基自由基[·OH],快速将Fe(Ⅱ)氧化,并快速成核转化为非晶态α-FeOOH。当pH值小于8.7时,O_3分解为O_2可能占主导,O_2与配合物Fe~Ⅱ-EDTA的作用,通过电子转移可产生超氧负离子(O_2~-·),可使Fe(Ⅱ)快速生成γ-FeOOH。
通过实验发现,加入适量的EDTA可以明显地加快反应速率,并且可以提高所得产物的纯度,增大EDTA的浓度对反应过程及产物并没有太大影响,主要是因为过量的EDTA络合Fe(Ⅱ)的一种保护作用。
初始pH值和EDTA浓度是O_3氧化Fe(OH)_2悬浮液过程中的两个重要影响因素,同时也是空气氧化Fe(OH)_2悬浮液过程中的两个重要因素。本文分别探讨了初始pH值和EDTA浓度对反应过程及所得产物的影响。结果表明在初始pH值为8.6时可以得到纯的γ-FeOOH,随着pH值的升高则有利于α-FeOOH的生成,当初始pH值为9.0时可以得到纯相的α-FeOOH,pH值继续升高则有利于铁黑的生成。实验表明适量的EDTA的加入可以明显地加快反应速率,缩短反应时间,原因可能是因为EDTA和溶解氧形成电子转移络合物,并通过外层电子转移反应生成超氧负离子(O_2~-·),故而提高了Fe(Ⅱ)的氧化反应速率。EDTA浓度的增加反而降低了反应速率可能是因为过量的EDTA络合Fe(Ⅱ)的一种保护作用。
在污水处理过程中Fe(Ⅲ)通常作为光催化剂使用,大气中的Fe(Ⅱ)/Fe(Ⅲ)可以降解草
Because of the widely application of nanosized iron oxides in many aspects, such as catalysis, antisepsis, pigments and magnetic recording materials, the preparation of the nanosized iron oxides attracts much attention. The preparation methods can be divided into two sorts according to their raw materials: one is based on Fe(Ⅱ)ion as its raw material;the other is Fe(Ⅲ)ion. The novelty of the article lies in the new style raft-like lepidocrocite prepared by O_3 oxidant, moreover, we firstly take into account of the light in the research and give primary discuss on its influential mechanism.In this article, we used FeSO_4 and NaOH as the raw material, and investigated the oxidation mechanisms of Fe(OH)_2 suspension at different conditions. The present work is aimed to find the rule, in order that we can supply necessary basis for the preparation of iron oxides in later use.The author used O_3 as the oxidant to investigate the oxidation process of Fe(OH)_2 suspension, and did respective researches on its main influential factors: initial pH and the concentration of EDTA. The results indicated that the initial pH has more effect on the product at higher pH. At pH 8.6 or 8.5, pure lepidocrocite was obtained;when pH >8.7, the main product is pure goethite. TEM images showed that lepidocrocite was raft-like, while goethite was amorphous. At room temperature, the species of the transformation products for Fe(OH)_2 depend on both pH and oxidation speed. The result in the current system may be explained by the following mechanism. According to literature data O_3 in aqueous solution pH>8.7 is decomposed to newly-formed[O], which is a very strong oxidant, and[·OH]. Fe(Ⅱ) can be oxidized speedly to form amorphous α-FeOOH. When pH<8.7, O_3 is predominately decomposed to O_2 and O_2 is transformed to [O_2~-·] by the interaction between O_2 and FeⅡ-EDTA. Thus Fe(OH)_2 can be transformed speedly to y-FeOOH. The results also suggested that trace of EDTA could accelerate the reaction rate noticeably, as well as enhance the purity of the product. While more EDTA in the system seemed no more effect. It's may be attributed to the protective function between EDTA and Fe(Ⅱ)ion.Initial pH and the concentration of EDTA were also the two main influential factors in the air oxidation. The results revealed that when pH 8.6 we can obtain pure lepidocrocite, as the
rising of pH, more goethite was prepared. When pH 9.0, we can obtain pure goethite, the higher pH was suitable to the preparation of magnetite. We can conclude that the cooperation of trace of EDTA reduced the reaction time. It was considered that EDTA can form the charge-transfer complexes with the dissolved oxygen and superoxide anions(OY) were produced via a outer-sphere electron transformation. As a result, the oxidation rate of Fe( II )ion was accelerated. The slow down of the reaction with the increasing of EDTA may be attributed to the protective function between EDTA and Fe( II )ion.Fe(III)ion was usually used as light catalyst in the disposal of sewage, the iron-catalyzed photochemical decomposed oxalic acid and generation of hydrogen peroxide in atmospheric liquid phases. In our experiment system, according to the results, we found that light played some role in the reaction. Moreover the results revealed that increasing of light intensity, the reaction was sped up, and more lepidocrocite was obtained. We also compared with different lamps, and found that ultraviolet-light was in favor of the formation of magnetite.In the research, transmission electron microscopy(TEM), X-ray diffraction(XRD), and infrared(IR) spectrum were applied as our token method, and we gave some explanations on the reaction mechanism of Fe( II )ion oxidation by air under the light effect.
本文作者在前人工作的基础上,改用O_3作氧化剂研究了O_3氧化Fe(OH)_2悬浮液的过程,找到了其主要影响因素——初始pH值和EDTA,并分别对二者进行了研究。结果表明在弱碱性范围内pH值对产物的影响非常敏感,当初始pH值为8.6或8.5时可以得到纯相的γ-FeOOH,当初始pH值升高到8.7时得到的则是纯相的α-FeOOH。通过对产物进行透射电镜表征可以发现得到的γ-FeOOH为纳米筏状结构,α-FeOOH为无定形态。在室温下,O_3氧化Fe(OH)_2生成何种产物取决于氧化速率和pH:在pH值大于8.7时O_3在水中能够分解出氧化能力极强的新生态氧[O]和羟基自由基[·OH],快速将Fe(Ⅱ)氧化,并快速成核转化为非晶态α-FeOOH。当pH值小于8.7时,O_3分解为O_2可能占主导,O_2与配合物Fe~Ⅱ-EDTA的作用,通过电子转移可产生超氧负离子(O_2~-·),可使Fe(Ⅱ)快速生成γ-FeOOH。
通过实验发现,加入适量的EDTA可以明显地加快反应速率,并且可以提高所得产物的纯度,增大EDTA的浓度对反应过程及产物并没有太大影响,主要是因为过量的EDTA络合Fe(Ⅱ)的一种保护作用。
初始pH值和EDTA浓度是O_3氧化Fe(OH)_2悬浮液过程中的两个重要影响因素,同时也是空气氧化Fe(OH)_2悬浮液过程中的两个重要因素。本文分别探讨了初始pH值和EDTA浓度对反应过程及所得产物的影响。结果表明在初始pH值为8.6时可以得到纯的γ-FeOOH,随着pH值的升高则有利于α-FeOOH的生成,当初始pH值为9.0时可以得到纯相的α-FeOOH,pH值继续升高则有利于铁黑的生成。实验表明适量的EDTA的加入可以明显地加快反应速率,缩短反应时间,原因可能是因为EDTA和溶解氧形成电子转移络合物,并通过外层电子转移反应生成超氧负离子(O_2~-·),故而提高了Fe(Ⅱ)的氧化反应速率。EDTA浓度的增加反而降低了反应速率可能是因为过量的EDTA络合Fe(Ⅱ)的一种保护作用。
在污水处理过程中Fe(Ⅲ)通常作为光催化剂使用,大气中的Fe(Ⅱ)/Fe(Ⅲ)可以降解草
Because of the widely application of nanosized iron oxides in many aspects, such as catalysis, antisepsis, pigments and magnetic recording materials, the preparation of the nanosized iron oxides attracts much attention. The preparation methods can be divided into two sorts according to their raw materials: one is based on Fe(Ⅱ)ion as its raw material;the other is Fe(Ⅲ)ion. The novelty of the article lies in the new style raft-like lepidocrocite prepared by O_3 oxidant, moreover, we firstly take into account of the light in the research and give primary discuss on its influential mechanism.In this article, we used FeSO_4 and NaOH as the raw material, and investigated the oxidation mechanisms of Fe(OH)_2 suspension at different conditions. The present work is aimed to find the rule, in order that we can supply necessary basis for the preparation of iron oxides in later use.The author used O_3 as the oxidant to investigate the oxidation process of Fe(OH)_2 suspension, and did respective researches on its main influential factors: initial pH and the concentration of EDTA. The results indicated that the initial pH has more effect on the product at higher pH. At pH 8.6 or 8.5, pure lepidocrocite was obtained;when pH >8.7, the main product is pure goethite. TEM images showed that lepidocrocite was raft-like, while goethite was amorphous. At room temperature, the species of the transformation products for Fe(OH)_2 depend on both pH and oxidation speed. The result in the current system may be explained by the following mechanism. According to literature data O_3 in aqueous solution pH>8.7 is decomposed to newly-formed[O], which is a very strong oxidant, and[·OH]. Fe(Ⅱ) can be oxidized speedly to form amorphous α-FeOOH. When pH<8.7, O_3 is predominately decomposed to O_2 and O_2 is transformed to [O_2~-·] by the interaction between O_2 and FeⅡ-EDTA. Thus Fe(OH)_2 can be transformed speedly to y-FeOOH. The results also suggested that trace of EDTA could accelerate the reaction rate noticeably, as well as enhance the purity of the product. While more EDTA in the system seemed no more effect. It's may be attributed to the protective function between EDTA and Fe(Ⅱ)ion.Initial pH and the concentration of EDTA were also the two main influential factors in the air oxidation. The results revealed that when pH 8.6 we can obtain pure lepidocrocite, as the
rising of pH, more goethite was prepared. When pH 9.0, we can obtain pure goethite, the higher pH was suitable to the preparation of magnetite. We can conclude that the cooperation of trace of EDTA reduced the reaction time. It was considered that EDTA can form the charge-transfer complexes with the dissolved oxygen and superoxide anions(OY) were produced via a outer-sphere electron transformation. As a result, the oxidation rate of Fe( II )ion was accelerated. The slow down of the reaction with the increasing of EDTA may be attributed to the protective function between EDTA and Fe( II )ion.Fe(III)ion was usually used as light catalyst in the disposal of sewage, the iron-catalyzed photochemical decomposed oxalic acid and generation of hydrogen peroxide in atmospheric liquid phases. In our experiment system, according to the results, we found that light played some role in the reaction. Moreover the results revealed that increasing of light intensity, the reaction was sped up, and more lepidocrocite was obtained. We also compared with different lamps, and found that ultraviolet-light was in favor of the formation of magnetite.In the research, transmission electron microscopy(TEM), X-ray diffraction(XRD), and infrared(IR) spectrum were applied as our token method, and we gave some explanations on the reaction mechanism of Fe( II )ion oxidation by air under the light effect.
引文
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