异丙醇铝中含铁有机物的形成、分离及高纯铝醇盐应用研究
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摘要
异丙醇铝是制备高技术陶瓷、发光材料、高纯氧化铝纳米粉和功能膜等先进材料的重要前驱体。几年内我国多家新厂建成并以铝为主要原料,将其转化成异丙醇铝后采用醇盐水解法制备高纯超细氧化铝。然而,异丙醇铝在应用中遇到的最大问题是铁、硅、镁等杂质含量高,其中危害最大的是铁。根据文献报道和相关理论,异丙醇与金属铁不发生反应。而实验中发现：在金属铝与异丙醇反应过程中,铝中的铁杂质也参与反应,形成一种低沸点化合物并在异丙醇铝蒸馏纯化过程中随异丙醇铝蒸出,这种现象早在1981年Dobizha E. V.的研究中就有所发现,但未见深入研究的报道。为了弄清铝醇盐中铁杂质的反应与控制规律,获得高纯度铝醇盐及后续产品,本文首先对杂质铁与异丙醇反应的条件进行研究；在此基础上初步探讨了杂质铁转化为低沸点有机物的基本规律；然后研究了异丙醇铝中含铁有机物的分离方法及工艺过程；进一步,以异丙醇铝为前驱体,研究了氧化铝基发光材料的制备及铁杂质对其发光性能的影响,主要研究内容和结果如下：
1、研究了金属铝中杂质铁与异丙醇反应的条件及规律。在异丙醇与金属铝反应制备异丙醇铝过程中,通过改变铝中铁含量、反应气氛、催化剂种类、铁杂质的形态等,探讨了含铁有机物的生成条件及规律,考察了异丙醇、异丙醇铝在含铁有机物生成反应中的作用。实验采用电感耦合等离子体原子发射光谱(ICP-AES)、紫外-可见吸收光谱(UV-Vis)对产品进行表征。结果表明,异丙醇和异丙醇铝的存在是含铁有物生成的必要条件,同时氧气对其生成具有促进作用,原料铝对其生成具有抑制作用；异丙醇铝合成体系中存在二价、三价两种价态的铁并且两种价态的铁可以在氧气和金属铁的作用下相互转换。
2、探讨了在异丙醇铝-异丙醇体系中含铁有机物生成的可能机理。基于上述反应条件和规律,利用电化学相关理论,结合EDTA滴定、氢核磁(1HNMR)、元素分析(EA)、红外(FT-IR), X射线光电子能谱(XPS)等分析结果,推测了铁杂质在异丙醇铝-异丙醇体系中发生反应的可能机理,即：铝片在与异丙醇反应后留下的小尺寸铁微粒,由于高的反应活性,和异丙醇直接反应生成二价含铁化合物；该二价含铁化合物被氧气氧化成三价含铁化合物；三价含铁化合物则在异丙醇铝／异丙醇的存在下又被金属铁还原成二价含铁化合物。上述价态转变的过程是不断循环进行的。
3、研究了异丙醇铝中含铁有机物的分离方法。根据上面推测的反应机理和含铁化合物的传统性质,提出了“螯合-蒸馏法”和“吸附-蒸馏法”两种纯化异丙醇铝中痕量铁的方法,同时考察了精馏对异丙醇铝纯化的效果。实验采用电感耦合等离子体原子发射光谱(ICP-AES)、紫外-可见吸收光谱(UV-Vis)对产品进行表征。结果表明：氧配位螯合剂——配体-O是采用“螯合-蒸馏法”有效脱除异丙醇铝中痕量铁的螯合剂；吸附剂(S)使铝片反应后留下的小尺寸铁被吸附发生团聚,失去反应活性从而达到纯化的目的；精馏对异丙醇铝也具有很好的纯化效果,但是存在对设备要求较高,能耗大等缺点。
4、以异丙醇铝为原料,采用模板水热辅助溶胶凝胶法制备γ-Al2O3:Eu3+发光粉,采用葡萄糖水热碳球为模板,利用醇盐水蒸气水解,制备中空γ,δ,α-Al2O3球和中空γ-Al2O3:Eu3+发光粉。借助于热重(TG/DTG)、X射线衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)和荧光分光光度计等表征手段,对产物的形成过程、结构、形貌以及光谱性能进行了分析,同时考察了铁杂质对γ-Al2O3:Eu3+发光粉及中空γ-Al2O3:Eu3+发光粉发光性能的影响。结果表明,制备的γ-Al2O3:Eu3+发光粉为立方晶型,激发光谱呈现典型的Eu3+离子特征发光,铁杂质的存在对其具有发光猝灭效应；制备的中空γ,δ,α-Al2O3球具有光滑的表面形貌,颗粒形态好、大小均匀；制备的中空γ-Al2O3:Eu3+发光粉为立方晶型,激发光谱呈现典型的Eu3+离子特征发光,原料中的铁杂质对其发光性能也具有猝灭作用。
Aluminum isopropoxide (AIP) is an important precursor of ceramic materials, phosphors, high purity alumina nanomaterials, functional membranes and so on. In newly found factories, aluminum alkoxide is used as starting material to prepare high purity and ultrafine alumina via Sol-Gel technique. However, the biggest problem restricting the utilization of aluminum alkoxide is the high impurity content in products, such as iron, silicon, and magnesium, especially the iron impurity. According to the reported references and the relevant theories, iron can not react with isopropanol. However, it was definitely found that the low boiling-point iron-containing compounds were distilled accompanied with AIP, which means that iron impurity in Al can take part in the reaction. Though Dobizha E. V. reported this phenomenon in 1981, it did not draw further attention. With the aim to elucidate the control regulation of iron impurity in aluminum alkoxide and obtain high purity aluminum alkoxide as well as downstream products, the reaction conditions of iron impurity and isopropanol were investigated firstly. In addition, plausible formation mechanism of iron-containing compound was presumed. On the basis of above results, separation method and technology process of iron-containing compound in the synthesis system of AIP were studied. Furthermore, alumina-based luminescent materials excited by Europium were prepared using aluminum alkoxide as starting materials. The luminescence effect on phosphors arising from iron impurity was studied in this paper. The contents and results in this dissertation are listed below:
1. The reaction conditions and regulation of iron impurity in Al with isopropanol were studied by changing the factors, such as different iron content of Al, reaction atmosphere, catalyst, morphological iron, etc. The function of isopropanol and AIP on the formation of this compound was also investigated. ICP-AES and UV-Vis adsorption spectra were used to characterize the products. It is found that, AIP and isopropanol are the necessary condition for formation of this compound. Oxygen can enhance the formation of it and Al can inhibit the formation of it. It was proved that there are two kinds of iron valence state (ferrous and ferric) in the system of preparing AIP, which can mutual conversion by the action of oxygen and metal iron.
2. A possible mechanism for the formation of iron-containing compound in the system of AIP-isopropanol was presumed. The obtained products were characterized by the means of EDTA titration method,1H NMR, elemental analysis, IR and XPS. According to the present results and electrochemical relevant theories, a plausible mechanism for the reaction of iron with isopropanol in the system of AIP-isopropanol was proposed. It is consisted of three consecutive steps, namely:small size iron particle created by Al reacting with isopropanol have high reactivity and can react with isorpopanol forming ferrous compound. The ferrous compound is immediately oxygenated to ferric compound, and then the ferric compound can be reduced to the ferrous compound in the presence of AIP and isopropanol. The above redox procedure is carried out cycling constantly.
3. According to the above possible mechanism and the characteristics of iron compound, the separation of iron-containing compound from AIP was studied by exploring "chelate-distillation" and "adsorption-distillation" methods which are effective for removing trace iron from AIP. The effect of rectification on the purification of AIP was further investigated. ICP-AES and UV-Vis adsorption spectra were used to characterize the products. It is found that, O-containing chelating agent——Ligand-O is an effective chelating agent for removing trace iron from AIP with "chelate-distillation" method. Small size iron particles created by Al reacting with isopropanol are agglomerated by sorbent (S) to reduce the reaction activity with the aim of puritification. Although the rectification has good effect on the purification of AIP, it requires expensive equipment and high energy consumption.
4. Eu3+-dopedγ-Al2O3 phosphor was prepared from aluminum alkoxide via hydrothermal assisted Sol-Gel method,γ,δ,α-Al2O3 hollow microspheres andγ-Al2O3:Eu3+ phosphor with hollow spherical structure were prepared from aluminum alkoxide using carbon microspheres prepared from hydrothermal method of glucose solution as templates. The forming process, structure, morphology and luminescent properties of the obtained products were characterized by means of TG, XRD, TEM, SEM and fluorescence spectrophotometer. The luminescence effect onγ-Al2O3:Eu3+ phosphor and hollow spheres ofγ-Al2O3:Eu3+ phosphor arising from iron impurity was studied in this part. The results indicate that theγ-Al2O3:Eu3+ phosphor shows pure cube phase. Luminescence test indicated that theγ-Al2O3:Eu3+ phosphor emits an intense characteristic luminescence of Eu3+ ions. The results revealed that iron impurity cause the quenching for luminescence ofγ-Al2O3:Eu3+ phosphors. The as-preparedγ-,δ-andα-alumina hollow microspheres with smooth surface show well-defined spherical morphology and narrow size-distribution. The obtainedγ-Al2O3:Eu3+ phosphor with hollow spherical structure shows pure cube phase. Luminescence test indicated that it emits an intense characteristic luminescence of Eu3+ ions. The results reveal that iron impurity cause the quenching of luminescence ofγ-Al2O3:Eu3+ phosphors with hollow sphereical structure as well.
1、研究了金属铝中杂质铁与异丙醇反应的条件及规律。在异丙醇与金属铝反应制备异丙醇铝过程中,通过改变铝中铁含量、反应气氛、催化剂种类、铁杂质的形态等,探讨了含铁有机物的生成条件及规律,考察了异丙醇、异丙醇铝在含铁有机物生成反应中的作用。实验采用电感耦合等离子体原子发射光谱(ICP-AES)、紫外-可见吸收光谱(UV-Vis)对产品进行表征。结果表明,异丙醇和异丙醇铝的存在是含铁有物生成的必要条件,同时氧气对其生成具有促进作用,原料铝对其生成具有抑制作用；异丙醇铝合成体系中存在二价、三价两种价态的铁并且两种价态的铁可以在氧气和金属铁的作用下相互转换。
2、探讨了在异丙醇铝-异丙醇体系中含铁有机物生成的可能机理。基于上述反应条件和规律,利用电化学相关理论,结合EDTA滴定、氢核磁(1HNMR)、元素分析(EA)、红外(FT-IR), X射线光电子能谱(XPS)等分析结果,推测了铁杂质在异丙醇铝-异丙醇体系中发生反应的可能机理,即：铝片在与异丙醇反应后留下的小尺寸铁微粒,由于高的反应活性,和异丙醇直接反应生成二价含铁化合物；该二价含铁化合物被氧气氧化成三价含铁化合物；三价含铁化合物则在异丙醇铝／异丙醇的存在下又被金属铁还原成二价含铁化合物。上述价态转变的过程是不断循环进行的。
3、研究了异丙醇铝中含铁有机物的分离方法。根据上面推测的反应机理和含铁化合物的传统性质,提出了“螯合-蒸馏法”和“吸附-蒸馏法”两种纯化异丙醇铝中痕量铁的方法,同时考察了精馏对异丙醇铝纯化的效果。实验采用电感耦合等离子体原子发射光谱(ICP-AES)、紫外-可见吸收光谱(UV-Vis)对产品进行表征。结果表明：氧配位螯合剂——配体-O是采用“螯合-蒸馏法”有效脱除异丙醇铝中痕量铁的螯合剂；吸附剂(S)使铝片反应后留下的小尺寸铁被吸附发生团聚,失去反应活性从而达到纯化的目的；精馏对异丙醇铝也具有很好的纯化效果,但是存在对设备要求较高,能耗大等缺点。
4、以异丙醇铝为原料,采用模板水热辅助溶胶凝胶法制备γ-Al2O3:Eu3+发光粉,采用葡萄糖水热碳球为模板,利用醇盐水蒸气水解,制备中空γ,δ,α-Al2O3球和中空γ-Al2O3:Eu3+发光粉。借助于热重(TG/DTG)、X射线衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)和荧光分光光度计等表征手段,对产物的形成过程、结构、形貌以及光谱性能进行了分析,同时考察了铁杂质对γ-Al2O3:Eu3+发光粉及中空γ-Al2O3:Eu3+发光粉发光性能的影响。结果表明,制备的γ-Al2O3:Eu3+发光粉为立方晶型,激发光谱呈现典型的Eu3+离子特征发光,铁杂质的存在对其具有发光猝灭效应；制备的中空γ,δ,α-Al2O3球具有光滑的表面形貌,颗粒形态好、大小均匀；制备的中空γ-Al2O3:Eu3+发光粉为立方晶型,激发光谱呈现典型的Eu3+离子特征发光,原料中的铁杂质对其发光性能也具有猝灭作用。
Aluminum isopropoxide (AIP) is an important precursor of ceramic materials, phosphors, high purity alumina nanomaterials, functional membranes and so on. In newly found factories, aluminum alkoxide is used as starting material to prepare high purity and ultrafine alumina via Sol-Gel technique. However, the biggest problem restricting the utilization of aluminum alkoxide is the high impurity content in products, such as iron, silicon, and magnesium, especially the iron impurity. According to the reported references and the relevant theories, iron can not react with isopropanol. However, it was definitely found that the low boiling-point iron-containing compounds were distilled accompanied with AIP, which means that iron impurity in Al can take part in the reaction. Though Dobizha E. V. reported this phenomenon in 1981, it did not draw further attention. With the aim to elucidate the control regulation of iron impurity in aluminum alkoxide and obtain high purity aluminum alkoxide as well as downstream products, the reaction conditions of iron impurity and isopropanol were investigated firstly. In addition, plausible formation mechanism of iron-containing compound was presumed. On the basis of above results, separation method and technology process of iron-containing compound in the synthesis system of AIP were studied. Furthermore, alumina-based luminescent materials excited by Europium were prepared using aluminum alkoxide as starting materials. The luminescence effect on phosphors arising from iron impurity was studied in this paper. The contents and results in this dissertation are listed below:
1. The reaction conditions and regulation of iron impurity in Al with isopropanol were studied by changing the factors, such as different iron content of Al, reaction atmosphere, catalyst, morphological iron, etc. The function of isopropanol and AIP on the formation of this compound was also investigated. ICP-AES and UV-Vis adsorption spectra were used to characterize the products. It is found that, AIP and isopropanol are the necessary condition for formation of this compound. Oxygen can enhance the formation of it and Al can inhibit the formation of it. It was proved that there are two kinds of iron valence state (ferrous and ferric) in the system of preparing AIP, which can mutual conversion by the action of oxygen and metal iron.
2. A possible mechanism for the formation of iron-containing compound in the system of AIP-isopropanol was presumed. The obtained products were characterized by the means of EDTA titration method,1H NMR, elemental analysis, IR and XPS. According to the present results and electrochemical relevant theories, a plausible mechanism for the reaction of iron with isopropanol in the system of AIP-isopropanol was proposed. It is consisted of three consecutive steps, namely:small size iron particle created by Al reacting with isopropanol have high reactivity and can react with isorpopanol forming ferrous compound. The ferrous compound is immediately oxygenated to ferric compound, and then the ferric compound can be reduced to the ferrous compound in the presence of AIP and isopropanol. The above redox procedure is carried out cycling constantly.
3. According to the above possible mechanism and the characteristics of iron compound, the separation of iron-containing compound from AIP was studied by exploring "chelate-distillation" and "adsorption-distillation" methods which are effective for removing trace iron from AIP. The effect of rectification on the purification of AIP was further investigated. ICP-AES and UV-Vis adsorption spectra were used to characterize the products. It is found that, O-containing chelating agent——Ligand-O is an effective chelating agent for removing trace iron from AIP with "chelate-distillation" method. Small size iron particles created by Al reacting with isopropanol are agglomerated by sorbent (S) to reduce the reaction activity with the aim of puritification. Although the rectification has good effect on the purification of AIP, it requires expensive equipment and high energy consumption.
4. Eu3+-dopedγ-Al2O3 phosphor was prepared from aluminum alkoxide via hydrothermal assisted Sol-Gel method,γ,δ,α-Al2O3 hollow microspheres andγ-Al2O3:Eu3+ phosphor with hollow spherical structure were prepared from aluminum alkoxide using carbon microspheres prepared from hydrothermal method of glucose solution as templates. The forming process, structure, morphology and luminescent properties of the obtained products were characterized by means of TG, XRD, TEM, SEM and fluorescence spectrophotometer. The luminescence effect onγ-Al2O3:Eu3+ phosphor and hollow spheres ofγ-Al2O3:Eu3+ phosphor arising from iron impurity was studied in this part. The results indicate that theγ-Al2O3:Eu3+ phosphor shows pure cube phase. Luminescence test indicated that theγ-Al2O3:Eu3+ phosphor emits an intense characteristic luminescence of Eu3+ ions. The results revealed that iron impurity cause the quenching for luminescence ofγ-Al2O3:Eu3+ phosphors. The as-preparedγ-,δ-andα-alumina hollow microspheres with smooth surface show well-defined spherical morphology and narrow size-distribution. The obtainedγ-Al2O3:Eu3+ phosphor with hollow spherical structure shows pure cube phase. Luminescence test indicated that it emits an intense characteristic luminescence of Eu3+ ions. The results reveal that iron impurity cause the quenching of luminescence ofγ-Al2O3:Eu3+ phosphors with hollow sphereical structure as well.
引文
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