金属酞菁/La_(0.8)Ce_(0.2)NiO_3复合催化剂的制备及光催化氧化DBT研究
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摘要
光催化氧化脱硫作为一种新型氧化脱硫技术,因其能耗低、无污染受到人们广泛关注。在众多的光催化剂中,金属酞菁敏化半导体材料作为一种高效的深度脱硫催化剂成为研究热点。本文在参考国内外已有研究成果的基础上,采用改进的固相法和液相法分别合成了无取代和取代两个系列的金属酞菁。采用浸渍法将制备的金属酞菁负载于钙钛矿型复合氧化物上,形成酞菁负载光催化剂。利用制备的催化剂对模拟燃油中的二苯并噻吩进行光催化氧化实验,探讨酞菁结构和光催化活性之间的关系,摸索光催化氧化脱硫的反应机理,为酞菁敏化半导体催化剂的研究和应用提供有益的借鉴和启示。
论文主要内容概括为以下几个方面：
1.采用溶胶-凝胶法制备了复合金属氧化物LaNiO3及Ce掺杂复合氧化物La1-xCexNiO3(x=0.1,0.2,0.4,0.6,0.8)。并对所合成的复合金属氧化物进行了X-射线粉末衍射、扫描电镜和光电子能谱分析。以二苯并噻吩的正辛烷溶液为模拟柴油,自制的复合氧化物为催化剂,在模拟太阳光的照射下进行光催化氧化脱硫测试。研究不同焙烧温度对氧化物脱硫活性的影响,确定最佳焙烧温度,挑选出活性最佳的氧化物。通过与空白实验的对比筛选出催化活性较好的La0.8Ce0.2NiO3氧化物。
2.采用微波-固相法分别制备了无取代金属酞菁MPc、MTAP和MPTpz (M=Mn(Ⅱ), Fe(Ⅱ), Co(Ⅱ), Ni(Ⅱ), Cu(Ⅱ)),采用液相法合成了取代金属酞菁MTNPc、MTAPc和MTcPc (M=Mn(Ⅱ),Fe(Ⅱ),Co(Ⅱ),Ni(Ⅱ),Cu(Ⅱ)),共合成金属酞菁30个。并对所得金属酞菁进行了元素分析,红外光谱和紫外光谱等表征。采用浸渍法制备了六个系列的金属酞菁/La0.8Ce0.2NiO3复合催化剂,采用XRD对其进行了表征,证明所合成金属酞菁均以无定形态存在。SEM测试结果表明：负载后氧化物的孔洞数明显降低。采用XPS技术进一步确定了复合催化剂的组成和各元素价态。通过对比纯氧化物和负载氧化物的谱图,可初步确定新的化学键(M-O键)的生成。
3.通过对光催化氧化反应主要影响因素的研究,确定了光催化氧化反应的最佳条件为：催化剂用量为3g·L-1, H2O2的用量为H2O2:S=100:1。在最佳反应条件下,分别对自制的负载金属酞菁催化剂光催化氧化DBT活性进行了测试,其中CoTcPc/La0.8Ce0.2NiO3的脱硫率可以达到94.9%,模拟柴油中硫含量降至49ppm,达到国家Ⅳ标准值(50ppm)。同时对光催化反应的产物进行了鉴定,结果表明：主要氧化产物为CO2, SO42-, DBTO和DBTO2。
4.在光催化反应的基础上,研究了中心金属离子和取代基对催化剂光催化活性的影响,结果表明：中心离子对催化剂活性的影响与金属离子的价电子构型有关,具有变价的金属离子(Fe2+,Co2+)具有较高的催化活性；取代基对催化剂催化活性的影响主要与取代基的性质有关,吸电子基团(羧基,硝基)取代有利于活性提高,给电子基团(氨基)使催化剂活性降低。对负载金属酞菁催化剂的动力学和反应机理进行了研究,结果显示,催化剂光催化氧化DBT的反应符合一级反应动力学方程,催化反应速率最快的CoTNPc/La0.8Ce0.2NiO3的半衰期为74min。催化反应可能同时按照三种不同的路径(Ⅰ型机理、Ⅱ型机理和半导体光催化机理)进行。
5.以CoTcPc/La0.8Ce0.2NiO3为催化剂,考察了该催化剂对不同含硫化合物(噻吩,苯并噻吩)的脱除效果,结果表明：该催化剂对不同含硫化合物均具有较高的催化活性,催化活性顺序为二苯并噻吩>苯并噻吩>噻吩。以CoTcPc/La0.8Ce0.2NiO3为催化剂,对其稳定性进行了研究,结果表明：循环利用5次后,催化活性基本保持不变,循环使用10次后,催化活性有所降低,但仍保持一定的催化活性,说明该催化剂具有较好的稳定性。
Photocatalytic oxidation desulfurization, as a new type of oxidation desulfurization technology, has intrigued widely attention, because of its low energy consumption and pollution-free characteristics. In numerous photocatalysts, as a kind of efficient deep desulfurization catalyst, metal phthalocyanine sensitized semiconductor materials have become the research hot spot. In this article, on the basis of related research in domestic and overseas, two series of metal phthalocyanines were synthesized by the improved solid phase and liquid phase methods respectively, and then loaded them on the surface of perovskite composite oxides by impregnation method to prepare the new photocatalysts. Photocatalysts were used to oxidate dibenzothiophene in the model fuel. The relationship between the structure and catalytic activity was discussesed, and the reaction mechanism was also suggested, which provides beneficial references and enlightenment to the research of phthalocyanine sensitized semiconductor catalyst.
The main comments were summarized as follows:
1. Metal oxides LaNiO3and La1-xCexNiO3(x=0.1,0.2,0.1,0.2,0.8) were synthesized by sol-gel method, and charactered by the X-ray powder diffraction (XRD), scanning electron microscopy (SEM) and X-ray photoelectron spectrometer (XPS). Photocatalytic oxidation desulfurization tests were carried out under the irradiation of simulated sunlight, in which the solution of dibenzothiophene in octane was selected as the model diesel. The favorable burning temperature was selected by studying the influence of different calcination temperature on the oxide desulfurization activity. Compared with blank experiment, Lao.8Ceo.2Ni03was selected as the best catalyst supportor.
2. Metal phthalocyanines MPc, MTAP, MPTpz, MTNPc, MTAPc and MTcPc (M=Mn(II), Fe(II), Co(II), Ni(II), Cu(II)) were synthesized by microwave-solid phase and liquid phase methods respectively, and charactered by Element analysis (EA), Infrared spectrum (IR) and Ultraviolet visible spectroscopy (UV-vis). Six series of metal phthalocyanine/La0.8Ce0.2NiO3catalysts were prepared by immersion method. XRD results show that they exist in amorphous form. According to the results of SEM, it can be concluded that the number of holes on composite metal oxides after loaded decreased significantly. Furthermore, the composition and elements valence of catalysts were determined by XPS technology. By comparing the spectra of the pure oxide and loaded oxide, it can be determined that new chemical bond were built.
3. The main factors of the activity on the photocatalytic oxidation reaction were studied, and the best conditions can be concluded as follows:the amount of catalyst is3g·L-1and the ratio of hydrogen peroxide and sulphur is100:1. Under the best reaction condation, the catalytic activity of three series of metal phthalocyanines was discussed, it was demonstrated that center metal ion and N atom all infllence the activity. Among them, CoTcPc/Lao.8Ceo.2Ni03catalyst has the best photocatalytic activity, the desulfurization rate of which can reach94.9%under simulated sunlight for5h. The sulfur content remained in model diesel is49ppm, which can meet the national IV standard of desel. Finally, the reaction products were predicted through different tests, which may include CO2, SO42-, DBTO and DBTO2.
4. On the basis of photocatalytic reaction, the effect of center metal ions and the substituent on photocatalytic activity was studyed. The results show that the center ion effect on catalyst activity is associated with valence electron configuration of metal ion. The metal phthalocyanines with varied valence (Fe+, Co+), have higher catalytic activity. Substituent effect on the activity of catalyst is mainly related to the nature of the substituents, electron-withdrawing groups (carboxyl, nitro) make the activity improved, and electron-donating group (amino) makes the catalyst activity decreased. In addation, the dynamics and reaction mechanism of the six series of loaded metal phthalocyanine catalysts were studied. The results showed that the reactions follow pseudo-first-order reaction kinetics equation, and CoTNPc/La0.8Ce0.2NiO3is the best photocatalyst with the half-life of74min. The catalytic reaction may be carried out in accordance with the three different paths at the same time:the mechanism of type I and type II and the mechanism of semiconductor photocatalytic reaction.
5. Taking CoTcPc/La0.8Ce0.2NiO3as catalyst, the desulfurization rate of different sulfur compounds was studied. The catalytic activity order is as follows:dibenzothiophene> benzothiophene> thiophene. In addition, the stability of catalyst was also discussed. The results show that photocatalyst does not changed after five times recycles, and after ten times recycles, the catalytic activity decreases, but still maintains a certain catalytic activity, it can be concluded that the catalyst has good stability.
论文主要内容概括为以下几个方面：
1.采用溶胶-凝胶法制备了复合金属氧化物LaNiO3及Ce掺杂复合氧化物La1-xCexNiO3(x=0.1,0.2,0.4,0.6,0.8)。并对所合成的复合金属氧化物进行了X-射线粉末衍射、扫描电镜和光电子能谱分析。以二苯并噻吩的正辛烷溶液为模拟柴油,自制的复合氧化物为催化剂,在模拟太阳光的照射下进行光催化氧化脱硫测试。研究不同焙烧温度对氧化物脱硫活性的影响,确定最佳焙烧温度,挑选出活性最佳的氧化物。通过与空白实验的对比筛选出催化活性较好的La0.8Ce0.2NiO3氧化物。
2.采用微波-固相法分别制备了无取代金属酞菁MPc、MTAP和MPTpz (M=Mn(Ⅱ), Fe(Ⅱ), Co(Ⅱ), Ni(Ⅱ), Cu(Ⅱ)),采用液相法合成了取代金属酞菁MTNPc、MTAPc和MTcPc (M=Mn(Ⅱ),Fe(Ⅱ),Co(Ⅱ),Ni(Ⅱ),Cu(Ⅱ)),共合成金属酞菁30个。并对所得金属酞菁进行了元素分析,红外光谱和紫外光谱等表征。采用浸渍法制备了六个系列的金属酞菁/La0.8Ce0.2NiO3复合催化剂,采用XRD对其进行了表征,证明所合成金属酞菁均以无定形态存在。SEM测试结果表明：负载后氧化物的孔洞数明显降低。采用XPS技术进一步确定了复合催化剂的组成和各元素价态。通过对比纯氧化物和负载氧化物的谱图,可初步确定新的化学键(M-O键)的生成。
3.通过对光催化氧化反应主要影响因素的研究,确定了光催化氧化反应的最佳条件为：催化剂用量为3g·L-1, H2O2的用量为H2O2:S=100:1。在最佳反应条件下,分别对自制的负载金属酞菁催化剂光催化氧化DBT活性进行了测试,其中CoTcPc/La0.8Ce0.2NiO3的脱硫率可以达到94.9%,模拟柴油中硫含量降至49ppm,达到国家Ⅳ标准值(50ppm)。同时对光催化反应的产物进行了鉴定,结果表明：主要氧化产物为CO2, SO42-, DBTO和DBTO2。
4.在光催化反应的基础上,研究了中心金属离子和取代基对催化剂光催化活性的影响,结果表明：中心离子对催化剂活性的影响与金属离子的价电子构型有关,具有变价的金属离子(Fe2+,Co2+)具有较高的催化活性；取代基对催化剂催化活性的影响主要与取代基的性质有关,吸电子基团(羧基,硝基)取代有利于活性提高,给电子基团(氨基)使催化剂活性降低。对负载金属酞菁催化剂的动力学和反应机理进行了研究,结果显示,催化剂光催化氧化DBT的反应符合一级反应动力学方程,催化反应速率最快的CoTNPc/La0.8Ce0.2NiO3的半衰期为74min。催化反应可能同时按照三种不同的路径(Ⅰ型机理、Ⅱ型机理和半导体光催化机理)进行。
5.以CoTcPc/La0.8Ce0.2NiO3为催化剂,考察了该催化剂对不同含硫化合物(噻吩,苯并噻吩)的脱除效果,结果表明：该催化剂对不同含硫化合物均具有较高的催化活性,催化活性顺序为二苯并噻吩>苯并噻吩>噻吩。以CoTcPc/La0.8Ce0.2NiO3为催化剂,对其稳定性进行了研究,结果表明：循环利用5次后,催化活性基本保持不变,循环使用10次后,催化活性有所降低,但仍保持一定的催化活性,说明该催化剂具有较好的稳定性。
Photocatalytic oxidation desulfurization, as a new type of oxidation desulfurization technology, has intrigued widely attention, because of its low energy consumption and pollution-free characteristics. In numerous photocatalysts, as a kind of efficient deep desulfurization catalyst, metal phthalocyanine sensitized semiconductor materials have become the research hot spot. In this article, on the basis of related research in domestic and overseas, two series of metal phthalocyanines were synthesized by the improved solid phase and liquid phase methods respectively, and then loaded them on the surface of perovskite composite oxides by impregnation method to prepare the new photocatalysts. Photocatalysts were used to oxidate dibenzothiophene in the model fuel. The relationship between the structure and catalytic activity was discussesed, and the reaction mechanism was also suggested, which provides beneficial references and enlightenment to the research of phthalocyanine sensitized semiconductor catalyst.
The main comments were summarized as follows:
1. Metal oxides LaNiO3and La1-xCexNiO3(x=0.1,0.2,0.1,0.2,0.8) were synthesized by sol-gel method, and charactered by the X-ray powder diffraction (XRD), scanning electron microscopy (SEM) and X-ray photoelectron spectrometer (XPS). Photocatalytic oxidation desulfurization tests were carried out under the irradiation of simulated sunlight, in which the solution of dibenzothiophene in octane was selected as the model diesel. The favorable burning temperature was selected by studying the influence of different calcination temperature on the oxide desulfurization activity. Compared with blank experiment, Lao.8Ceo.2Ni03was selected as the best catalyst supportor.
2. Metal phthalocyanines MPc, MTAP, MPTpz, MTNPc, MTAPc and MTcPc (M=Mn(II), Fe(II), Co(II), Ni(II), Cu(II)) were synthesized by microwave-solid phase and liquid phase methods respectively, and charactered by Element analysis (EA), Infrared spectrum (IR) and Ultraviolet visible spectroscopy (UV-vis). Six series of metal phthalocyanine/La0.8Ce0.2NiO3catalysts were prepared by immersion method. XRD results show that they exist in amorphous form. According to the results of SEM, it can be concluded that the number of holes on composite metal oxides after loaded decreased significantly. Furthermore, the composition and elements valence of catalysts were determined by XPS technology. By comparing the spectra of the pure oxide and loaded oxide, it can be determined that new chemical bond were built.
3. The main factors of the activity on the photocatalytic oxidation reaction were studied, and the best conditions can be concluded as follows:the amount of catalyst is3g·L-1and the ratio of hydrogen peroxide and sulphur is100:1. Under the best reaction condation, the catalytic activity of three series of metal phthalocyanines was discussed, it was demonstrated that center metal ion and N atom all infllence the activity. Among them, CoTcPc/Lao.8Ceo.2Ni03catalyst has the best photocatalytic activity, the desulfurization rate of which can reach94.9%under simulated sunlight for5h. The sulfur content remained in model diesel is49ppm, which can meet the national IV standard of desel. Finally, the reaction products were predicted through different tests, which may include CO2, SO42-, DBTO and DBTO2.
4. On the basis of photocatalytic reaction, the effect of center metal ions and the substituent on photocatalytic activity was studyed. The results show that the center ion effect on catalyst activity is associated with valence electron configuration of metal ion. The metal phthalocyanines with varied valence (Fe+, Co+), have higher catalytic activity. Substituent effect on the activity of catalyst is mainly related to the nature of the substituents, electron-withdrawing groups (carboxyl, nitro) make the activity improved, and electron-donating group (amino) makes the catalyst activity decreased. In addation, the dynamics and reaction mechanism of the six series of loaded metal phthalocyanine catalysts were studied. The results showed that the reactions follow pseudo-first-order reaction kinetics equation, and CoTNPc/La0.8Ce0.2NiO3is the best photocatalyst with the half-life of74min. The catalytic reaction may be carried out in accordance with the three different paths at the same time:the mechanism of type I and type II and the mechanism of semiconductor photocatalytic reaction.
5. Taking CoTcPc/La0.8Ce0.2NiO3as catalyst, the desulfurization rate of different sulfur compounds was studied. The catalytic activity order is as follows:dibenzothiophene> benzothiophene> thiophene. In addition, the stability of catalyst was also discussed. The results show that photocatalyst does not changed after five times recycles, and after ten times recycles, the catalytic activity decreases, but still maintains a certain catalytic activity, it can be concluded that the catalyst has good stability.
引文
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