利用铝型材厂工业废渣制备多孔陶瓷及稀土催化剂性能研究
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摘要
多孔陶瓷广泛应用于汽车尾气净化器、催化剂载体、消声材料和隔热材料等行业。堇青石多孔陶瓷具有几何表面积大、热膨胀系数小、耐热冲击性好和成本低等特点,作为汽车尾气催化剂载体,具有其它材料不可替代的效果。稀土复合氧化物催化剂因其综合性能佳,催化能力强,而引起了人们广泛的关注。
本文利用铝型材厂的工业废渣代替传统的工业氧化铝,与片状结构的高岭土、滑石合成了片状结构堇青石陶瓷,开发了技术路线简单易行,烧成温度低,高定向排列,高纯度的堇青石制备工艺。采用同步热分析仪、X射线衍射仪、扫描电子显微镜、热膨胀系数仪等手段,对片状结构堇青石陶瓷的制备工艺、显微结构和热膨胀系数进行了系统地研究,详细分析了原料的种类、配方、烧成制度以及晶核剂等对合成堇青石的影响。铝型材厂工业废渣预烧后Al_2O_3的含量达到90%以上,完全可取代工业氧化铝作为合成堇青石的主要原料。堇青石的理论组成点并不是合成堇青石的最佳配方,当Al_2O_3和MgO的含量略高于理论组成点,SiO_2的含量略低于理论组成点时,对合成堇青石有利。烧成温度能够显著影响堇青石的合成、晶相结构以及热膨胀系数等性能,烧成温度为1380℃时,片状堇青石生长最完全,热膨胀系数达1.82×10-6℃-1。保温时间的长短显著的影响晶体发育及反应程度,保温时间为4 h时,合成的片状堇青石大小均匀,热膨胀系数达到1.73×10-6℃-1。以堇青石熟料作为晶核剂,可以在一定程度上解决堇青石成核困难的问题,能明显促使高温下堇青石的形成和发育,且晶粒发育较好,同时还有利于降低堇青石的热膨胀系数。
首次以水溶性高分子材料为添加剂,以自制片状堇青石粉为主要原料,采用挤出成型技术,创新性地制备了多孔堇青石蜂窝陶瓷载体。对载体的制备工艺、形貌、物相组成、孔密度、热膨胀系数、抗热震性等进行了表征分析。以片状堇青石为原料,采用挤出成型方法有利于堇青石晶体的定向排列,使载体热膨胀系数各向异性,降低热膨胀系数,提高抗热震性。采用水溶性粘结剂替代传统桐油等油性粘结剂,可大大改善泥料的润滑性及可塑性,杜绝有害废气的产生。本实验制得的堇青石蜂窝陶瓷载体以片状结构为主,沿壁面方向呈现一定的定向排列,载体热膨胀系数仅为8.565×10-7℃-1(30-800℃),室温到650℃的急热急冷循环次数达5次以上,抗热震好;孔密度达90.6孔/cm2(±2.5%),壁厚为0.16 mm。
同时,为研究La-Sr-Co-O系列催化剂的催化性能,首次选用多孔莫来石纤维陶瓷为催化剂载体,采用真空浸渍法分别制备了负载型La_(1-x)Sr_xCoO_(3-δ)(x=0.2,0.4,0.6和0.8)和La_(1-x)Sr)xCo_(0.9)Pd_(0.1O3-δ)(x=0.2,0.4,0.6和0.8)钙钛矿氧化物催化剂。采用同步热分析仪、X射线衍射、扫描电子显微镜、比表面积分析仪、烟气分析仪等手段,对催化剂的物相组成、显微结构和催化性能进行了系统地研究,研究A位和B位取代对催化剂催化活性的影响,评估了各催化剂对NO+CO气体的催化性能,并分析Pd掺入对催化剂NO+CO催化活性的影响。
催化剂能较好地与多孔莫来石纤维陶瓷结合并具有较好的分散性,以多孔莫来石纤维陶瓷作为La-Sr-Co-O和La-Sr-Co-Pd-O系列催化剂的载体,抑制了钙钛矿结构形成过程中SrCO3的生成;贵金属Pd掺入La-Sr-Co-O催化剂中可抑制La(OH)3杂相的生成,Sr2+对La3+的A位取代大大增加了催化剂的氧格空位。
催化测试结果表明,多孔莫来石陶瓷载体负载La_(1-x)Sr_xCoO_(3-δ)催化剂和La_(1-x)Sr)xCo_(0.9)Pd_(0.1O3-δ)催化剂对CO+NO均有较好的催化氧化还原特性,Pd的掺入明显增加了La-Sr-Co-O催化剂的催化活性。La_(1-x)Sr_xCoO_(3-δ)系列催化剂中,La0.6Sr0.4CoO3-δ的CO催化氧化能力最强,La_(0.4)Sr_(0.6)CoO_(3-δ)的NO催化还原能力最强,La_(0.8)Sr_(0.2)CoO_(3-δ)单位表面积的CO催化氧化和NO催化还原活性都最强。La_(1-x)Sr)xCo_(0.9)Pd_(0.1O3-δ)系列催化剂中,La_(0.6)Sr_(0.4)Co_(0.9)Pd_(0.1O3-δ)的CO整体催化氧化和NO整体催化还原活性都较高,La_(0.4)Sr_(0.6)Co_(0.9)Pd_(0.1O3-δ)对CO单位表面催化氧化活性最高,各催化剂对NO单位表面催化还原活性则随着温度的不同而变化,温度对La_(0.4)Sr_(0.6)Co_(0.9)Pd_(0.1O3-δ)钙钛矿氧化物催化剂的催化还原活性影响最为显著。
Porous ceramics are widely used in automobile exhaust purifications, catalyst supports, sound-deadening insulation and furnace insulation materials. Cordierite ceramics have wonderful effects as a catalyst carrier and the high temperature flue gas filters because of great surface area, low thermal expansion coefficient, good thermal shock resistance and low cost, which other materials can not be replaced. Rare earth oxides have aroused widespread concern for their excellent comprehensive properties and good catalytic ability.
In this research, plate-shaped cordierite was successfully synthesized by aluminium industrial residues with talcum powder and kaolin. The preparation process, microstructure and thermal expansion coefficient of the compounds were systematically investigated by thermogravimetric differential scanning calorimetry, X-ray diffraction, scanning electron microscopy, hermal expansion coefficient instrument etc.
The Al_2O_3 content of the burn aluminium industrial residues is over 90%, which can completely replace industrial alumina as the main raw material of cordierite. The theoretical composition of cordierite cordierite is not the best formula of synthesis. It is benefit to fabricate cordierite when the contents of Al_2O_3 and MgO are higher than the theoretical compositions, and the SiO2 content is below the theoretical composition. Sintering temperature can significantly affect the synthesis of cordierite, crystal structure, thermal expansion coefficient and other properties. The pure sheet cordierite was obtained at thermal expansion coefficient of 1.82×10-6℃-1 when the sintering temperature was 1380℃.
Holding time significantly affected the crystal growth and the degree of reaction. When the holding time was 4 h, the prepared cordierites were uniform size and the thermal expansion coefficient was 1.73×10-6℃-1. Cordierite clinker as a nucleating agent can significantly promote the formation and development of cordierite and as well as help to reduce the thermal expansion coefficient of cordierite, which can solve the difficult problem of cordierite nucleation in a certain extent.
Porous cordierite honeycomb ceramic supports were prepared by extrusion technology using self-made sheet cordierite powder as main raw material and water-soluble polymers as additives for the first time. The preparation process, microstructure, phase composition, cell density, thermal expansion coefficient and thermal shock resistance of the samples were systematically investigated.
The sheet cordierite powder as raw material and extrusion methods are conducive to cordierite crystal oriented arrangement, which due to the anisotropy of thermal expansion coefficient vector, lower thermal expansion coefficient, and high thermal shock resistance. With water-soluble adhesive binder to instead of tung oil can improve the lubricity and plastic of the mud significantly, and prevent the generation of harmful emissions during the process. In this study, the obtained cordierite honeycomb ceramic supports with mainly of sheet structure show a certain alignment along the wall. The carrier thermal expansion coefficient, cell density and wall thickness are 8.565×10-6℃-1 (30-800℃), 90.6 holes/cm2, 0.16 mm, respectively.
The porous mullite fiber ceramics were used as catalytic supports for the first time. Supported La_(1-x)Sr_xCoO_(3-δ) and La_(1-x)Sr)xCo_(0.9)Pd_(0.1O3-δ) (x=0.2, 0.4, 0.6, and 0.8) perovskite-type oxide catalysts were prepared by vacuum impregnation method. The phase composition, microstructure and catalytic properties of the catalysts were systematically investigated by thermogravimetric differential scanning calorimetry, X-ray diffraction, scanning electron microscopy, specific surface area analyzer and flue gas analyzing apparatus etc. The affect of the element substituent on the catalytic activity was discussed deeply, and the catalytic properties of the catalyst on NO + CO gas were assessed.
The catalyst particles can bind with the porous mullite fiber ceramics and disperse uniformly on the surface of the supports. SrCO3 phase was not found in porous mullite fiber ceramic supported La_(1-x)Sr_xCoO_(3-δ) catalysts, which indicated that the supports depressed the growth of SrCO3 phase. La(OH)3 peaks were not observed in supported La_(1-x)Sr)xCo_(0.9)Pd_(0.1O3-δ) perovsite-type catalysts, which showed that Pd-doped perovskite oxide catalysts was helpful to inhibit the growth of La(OH)3 crystal phase. The Sr-doping to the La-position is benefit to increase the oxygen vacancies of the perovsite-type catalysts.
The investigation of catalytic activity showed that La_(1-x)Sr_xCoO_(3-δ) and La_(1-x)Sr)xCo_(0.9)Pd_(0.1O3-δ) perovskite-type catalysts supported on porous mullite fiber ceramics exhibited significant catalytic redox activity. The catalytic activity of La-Sr-Co-O catalysts was improved notably due to the Pd doping. For all supported La_(1-x)Sr_xCoO_(3-δ) perovskite-type catalysts, supported La0.6Sr0.4CoO3-δcatalysts showed the highest CO integral oxidizability, while supported La_(0.4)Sr_(0.6)CoO_(3-δ) perovskite-type catalysts exhibited the highest NO integral reducibility. And supported La_(0.8)Sr_(0.2)CoO_(3-δ) perovskite-type catalysts presented the best redox activity of the unit surface area. The integral redox of supported La_(0.6)Sr_(0.4)Co_(0.9)Pd_(0.1O3-δ) perovskite-type catalysts for CO+NO was higher than the rest of supported La_(1-x)Sr)xCo_(0.9)Pd_(0.1O3-δ) perovskite-type oxide catalysts. Supported La_(0.4)Sr_(0.6)Co_(0.9)Pd_(0.1O3-δ) perovskite-type catalysts showed the highest CO oxidizability of unit surface area among supported La_(1-x)Sr)xCo_(0.9)Pd_(0.1O3-δ) perovskite-type catalysts. Meanwhile the best dramatic effect by catalytic temperature was observed on supported La_(0.4)Sr_(0.6)Co_(0.9)Pd_(0.1O3-δ) perovskite-type catalyst.
本文利用铝型材厂的工业废渣代替传统的工业氧化铝,与片状结构的高岭土、滑石合成了片状结构堇青石陶瓷,开发了技术路线简单易行,烧成温度低,高定向排列,高纯度的堇青石制备工艺。采用同步热分析仪、X射线衍射仪、扫描电子显微镜、热膨胀系数仪等手段,对片状结构堇青石陶瓷的制备工艺、显微结构和热膨胀系数进行了系统地研究,详细分析了原料的种类、配方、烧成制度以及晶核剂等对合成堇青石的影响。铝型材厂工业废渣预烧后Al_2O_3的含量达到90%以上,完全可取代工业氧化铝作为合成堇青石的主要原料。堇青石的理论组成点并不是合成堇青石的最佳配方,当Al_2O_3和MgO的含量略高于理论组成点,SiO_2的含量略低于理论组成点时,对合成堇青石有利。烧成温度能够显著影响堇青石的合成、晶相结构以及热膨胀系数等性能,烧成温度为1380℃时,片状堇青石生长最完全,热膨胀系数达1.82×10-6℃-1。保温时间的长短显著的影响晶体发育及反应程度,保温时间为4 h时,合成的片状堇青石大小均匀,热膨胀系数达到1.73×10-6℃-1。以堇青石熟料作为晶核剂,可以在一定程度上解决堇青石成核困难的问题,能明显促使高温下堇青石的形成和发育,且晶粒发育较好,同时还有利于降低堇青石的热膨胀系数。
首次以水溶性高分子材料为添加剂,以自制片状堇青石粉为主要原料,采用挤出成型技术,创新性地制备了多孔堇青石蜂窝陶瓷载体。对载体的制备工艺、形貌、物相组成、孔密度、热膨胀系数、抗热震性等进行了表征分析。以片状堇青石为原料,采用挤出成型方法有利于堇青石晶体的定向排列,使载体热膨胀系数各向异性,降低热膨胀系数,提高抗热震性。采用水溶性粘结剂替代传统桐油等油性粘结剂,可大大改善泥料的润滑性及可塑性,杜绝有害废气的产生。本实验制得的堇青石蜂窝陶瓷载体以片状结构为主,沿壁面方向呈现一定的定向排列,载体热膨胀系数仅为8.565×10-7℃-1(30-800℃),室温到650℃的急热急冷循环次数达5次以上,抗热震好;孔密度达90.6孔/cm2(±2.5%),壁厚为0.16 mm。
同时,为研究La-Sr-Co-O系列催化剂的催化性能,首次选用多孔莫来石纤维陶瓷为催化剂载体,采用真空浸渍法分别制备了负载型La_(1-x)Sr_xCoO_(3-δ)(x=0.2,0.4,0.6和0.8)和La_(1-x)Sr)xCo_(0.9)Pd_(0.1O3-δ)(x=0.2,0.4,0.6和0.8)钙钛矿氧化物催化剂。采用同步热分析仪、X射线衍射、扫描电子显微镜、比表面积分析仪、烟气分析仪等手段,对催化剂的物相组成、显微结构和催化性能进行了系统地研究,研究A位和B位取代对催化剂催化活性的影响,评估了各催化剂对NO+CO气体的催化性能,并分析Pd掺入对催化剂NO+CO催化活性的影响。
催化剂能较好地与多孔莫来石纤维陶瓷结合并具有较好的分散性,以多孔莫来石纤维陶瓷作为La-Sr-Co-O和La-Sr-Co-Pd-O系列催化剂的载体,抑制了钙钛矿结构形成过程中SrCO3的生成;贵金属Pd掺入La-Sr-Co-O催化剂中可抑制La(OH)3杂相的生成,Sr2+对La3+的A位取代大大增加了催化剂的氧格空位。
催化测试结果表明,多孔莫来石陶瓷载体负载La_(1-x)Sr_xCoO_(3-δ)催化剂和La_(1-x)Sr)xCo_(0.9)Pd_(0.1O3-δ)催化剂对CO+NO均有较好的催化氧化还原特性,Pd的掺入明显增加了La-Sr-Co-O催化剂的催化活性。La_(1-x)Sr_xCoO_(3-δ)系列催化剂中,La0.6Sr0.4CoO3-δ的CO催化氧化能力最强,La_(0.4)Sr_(0.6)CoO_(3-δ)的NO催化还原能力最强,La_(0.8)Sr_(0.2)CoO_(3-δ)单位表面积的CO催化氧化和NO催化还原活性都最强。La_(1-x)Sr)xCo_(0.9)Pd_(0.1O3-δ)系列催化剂中,La_(0.6)Sr_(0.4)Co_(0.9)Pd_(0.1O3-δ)的CO整体催化氧化和NO整体催化还原活性都较高,La_(0.4)Sr_(0.6)Co_(0.9)Pd_(0.1O3-δ)对CO单位表面催化氧化活性最高,各催化剂对NO单位表面催化还原活性则随着温度的不同而变化,温度对La_(0.4)Sr_(0.6)Co_(0.9)Pd_(0.1O3-δ)钙钛矿氧化物催化剂的催化还原活性影响最为显著。
Porous ceramics are widely used in automobile exhaust purifications, catalyst supports, sound-deadening insulation and furnace insulation materials. Cordierite ceramics have wonderful effects as a catalyst carrier and the high temperature flue gas filters because of great surface area, low thermal expansion coefficient, good thermal shock resistance and low cost, which other materials can not be replaced. Rare earth oxides have aroused widespread concern for their excellent comprehensive properties and good catalytic ability.
In this research, plate-shaped cordierite was successfully synthesized by aluminium industrial residues with talcum powder and kaolin. The preparation process, microstructure and thermal expansion coefficient of the compounds were systematically investigated by thermogravimetric differential scanning calorimetry, X-ray diffraction, scanning electron microscopy, hermal expansion coefficient instrument etc.
The Al_2O_3 content of the burn aluminium industrial residues is over 90%, which can completely replace industrial alumina as the main raw material of cordierite. The theoretical composition of cordierite cordierite is not the best formula of synthesis. It is benefit to fabricate cordierite when the contents of Al_2O_3 and MgO are higher than the theoretical compositions, and the SiO2 content is below the theoretical composition. Sintering temperature can significantly affect the synthesis of cordierite, crystal structure, thermal expansion coefficient and other properties. The pure sheet cordierite was obtained at thermal expansion coefficient of 1.82×10-6℃-1 when the sintering temperature was 1380℃.
Holding time significantly affected the crystal growth and the degree of reaction. When the holding time was 4 h, the prepared cordierites were uniform size and the thermal expansion coefficient was 1.73×10-6℃-1. Cordierite clinker as a nucleating agent can significantly promote the formation and development of cordierite and as well as help to reduce the thermal expansion coefficient of cordierite, which can solve the difficult problem of cordierite nucleation in a certain extent.
Porous cordierite honeycomb ceramic supports were prepared by extrusion technology using self-made sheet cordierite powder as main raw material and water-soluble polymers as additives for the first time. The preparation process, microstructure, phase composition, cell density, thermal expansion coefficient and thermal shock resistance of the samples were systematically investigated.
The sheet cordierite powder as raw material and extrusion methods are conducive to cordierite crystal oriented arrangement, which due to the anisotropy of thermal expansion coefficient vector, lower thermal expansion coefficient, and high thermal shock resistance. With water-soluble adhesive binder to instead of tung oil can improve the lubricity and plastic of the mud significantly, and prevent the generation of harmful emissions during the process. In this study, the obtained cordierite honeycomb ceramic supports with mainly of sheet structure show a certain alignment along the wall. The carrier thermal expansion coefficient, cell density and wall thickness are 8.565×10-6℃-1 (30-800℃), 90.6 holes/cm2, 0.16 mm, respectively.
The porous mullite fiber ceramics were used as catalytic supports for the first time. Supported La_(1-x)Sr_xCoO_(3-δ) and La_(1-x)Sr)xCo_(0.9)Pd_(0.1O3-δ) (x=0.2, 0.4, 0.6, and 0.8) perovskite-type oxide catalysts were prepared by vacuum impregnation method. The phase composition, microstructure and catalytic properties of the catalysts were systematically investigated by thermogravimetric differential scanning calorimetry, X-ray diffraction, scanning electron microscopy, specific surface area analyzer and flue gas analyzing apparatus etc. The affect of the element substituent on the catalytic activity was discussed deeply, and the catalytic properties of the catalyst on NO + CO gas were assessed.
The catalyst particles can bind with the porous mullite fiber ceramics and disperse uniformly on the surface of the supports. SrCO3 phase was not found in porous mullite fiber ceramic supported La_(1-x)Sr_xCoO_(3-δ) catalysts, which indicated that the supports depressed the growth of SrCO3 phase. La(OH)3 peaks were not observed in supported La_(1-x)Sr)xCo_(0.9)Pd_(0.1O3-δ) perovsite-type catalysts, which showed that Pd-doped perovskite oxide catalysts was helpful to inhibit the growth of La(OH)3 crystal phase. The Sr-doping to the La-position is benefit to increase the oxygen vacancies of the perovsite-type catalysts.
The investigation of catalytic activity showed that La_(1-x)Sr_xCoO_(3-δ) and La_(1-x)Sr)xCo_(0.9)Pd_(0.1O3-δ) perovskite-type catalysts supported on porous mullite fiber ceramics exhibited significant catalytic redox activity. The catalytic activity of La-Sr-Co-O catalysts was improved notably due to the Pd doping. For all supported La_(1-x)Sr_xCoO_(3-δ) perovskite-type catalysts, supported La0.6Sr0.4CoO3-δcatalysts showed the highest CO integral oxidizability, while supported La_(0.4)Sr_(0.6)CoO_(3-δ) perovskite-type catalysts exhibited the highest NO integral reducibility. And supported La_(0.8)Sr_(0.2)CoO_(3-δ) perovskite-type catalysts presented the best redox activity of the unit surface area. The integral redox of supported La_(0.6)Sr_(0.4)Co_(0.9)Pd_(0.1O3-δ) perovskite-type catalysts for CO+NO was higher than the rest of supported La_(1-x)Sr)xCo_(0.9)Pd_(0.1O3-δ) perovskite-type oxide catalysts. Supported La_(0.4)Sr_(0.6)Co_(0.9)Pd_(0.1O3-δ) perovskite-type catalysts showed the highest CO oxidizability of unit surface area among supported La_(1-x)Sr)xCo_(0.9)Pd_(0.1O3-δ) perovskite-type catalysts. Meanwhile the best dramatic effect by catalytic temperature was observed on supported La_(0.4)Sr_(0.6)Co_(0.9)Pd_(0.1O3-δ) perovskite-type catalyst.
引文
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