蜂窝状金属丝网载体涂层制备及催化还原NO_x研究
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摘要
NO_x排放造成的大气污染日趋严重，采用整体催化剂的净化方法是目前治理尾气排放最为有效的措施之一。金属蜂窝载体与陶瓷蜂窝载体相比较具有更好的耐冲击性能、延展性能和机械性能且导热性好、启动快，可提供比陶瓷蜂窝体大得多的开孔率及几何表面积，在现代尾气治理领域受到越来越广泛的关注。但是，蜂窝状金属载体目前加工工艺复杂，生产成本高，而且金属载体的比表面积很小，使用时需要在表面负载一层高比表面积的陶瓷涂层。金属载体与陶瓷涂层材料的热膨胀系数相差较大，使得载体与涂层之间的结合强度较差，涂层易皲裂、剥落。金属载体与活性涂层的结合强度在一定程度上制约了金属蜂窝催化剂的推广应用，如何改善并提高涂层在基体合金表面的结合强度已成为研究者关注的问题。
本文围绕Fe-Cr-Al丝网加工成蜂窝状金属丝网载体，采用电沉积法在蜂窝状金属丝网载体表面制备氧化铝涂层，利用SEM、XRD、EDX和BET等表征技术并结合超声波检测、热冲击性能实验等手段，考察了铁铬铝高温处理、电沉积电压、电沉积时间、沉积液中铝含量和铝粒径等多个因素对涂层性能的影响。具体工作如下：
研究过程中设计开发出两台蜂窝状金属丝网载体加工设备。通过复合电沉积法制备涂层，具体考察了影响涂层的因素，例如电沉积液、沉积电压、沉积时间，沉积液中添加剂的含量、添加剂的粒径、焙烧时间和焙烧温度等。实验结果显示，以添加剂和氧化铝的乙醇溶液为电沉积液，可以在蜂窝状金属丝网基体表面制备适宜厚度的氧化铝涂层。采用H_2SO_4对金属丝网载体进行预处理可以清洗其表面的污染物，通过加入添加剂，在900℃焙烧2h等方法提高涂层与金属基体的结合力，增强了涂层的抗热振性能和抗机械振动性能，氧化铝涂层的表面形态以及性质没有因焙烧温度的升高而被损坏。SEM电镜显示涂层表面均匀没有皲裂，XRD表明氧化铝涂层仍是主要以γ-Al_2O_3晶形存在。
制备了Pd／Al_2O_3、Pd／CeZr／Al_2O_3、Pd／CeZr／TiO_2／Al_2O_3三种蜂窝状金属丝网载体催化剂，并采用丙烯选择催化还原NO_x的实验来评价对NO_x的催化活性。结果表明Pd含量为0．186％时，Pd／CeZr／TiO_2／Al_2O_3蜂窝状金属丝网催化剂在低温条件下具有较高的催化活性，而且催化活性窗口较宽。制备了V_2O_5-WO_3／TiO_2三元催化剂并用氨气选择催化还原NO_x的实验来评价对NO_x的催化活性。结果表明V(3)-W(7)／TiO_2催化剂具有更好的热稳定性和较高的脱硝效率。
After-treatment control technique, especially catalytic convert is an effective method to solve the increasing serious atmospheric pollution from the NO_x emission. Metallic monoliths offer plenty of advantages over ceramic monoliths, such as stronger mechanical, strength, higher ductilitical, higher thermal conductibility, lower pressure drop, and now have become most attractive supports in emissions controls. However, the metallic monoliths could not be applied in practice because of the complex of processing and the low specific surface area. It is necessary to deposit the ceramic oxide washcoat with high surface area over metallic monoliths. Since thermal expansion coefficient of the metallic support is different from the ceramic oxide washcoat, the adhesion of washcoat is poor which leads to the washcoat chap and flake away. The poor coating binding strength between the metallic substrate and the washcoat has attracted more attention by the most researchers.
After the wrie-mesh honeycomb was manufactured by making alternatively corrugated and plain wire meshes and the coating technique of theγ-Al_2O_3 based ceramic washcoat on surface of FeCrAl metallic substrate by electrophoretic deposition was investigated in this paper.Partly including thepretreatment condition of the metallic substrate and preparation of slurry.The washcoat quality was measured by SEM, XRD, EDX and BET, ultrasonic vibration and thermal shock test. The main works are as following:
The wrie-mesh honeycomb was manufactured by two equipment, The manufacture process of wire-mesh honeycomb was simply, which could reduce the price of wire-mesh honeycomb .Washcoat deposited on metallic wire mesh was prepared usingγ-Al_2O powders by electrophoretic deposition. The preparation parameters of washcoat were investigated, such as the deposited solution, the deposited voltage, the deposited time. Wire meshes were dipped in H_2SO_4 solution for wiping off the dirts and enhancing the cohesion between the wire mesh and washcoat. The ability of thermal resistant and vibration resistant was improved by adding additives and higher calcinations temperature, the washcoat calcine at 900℃for 2h and the phase structure of washcoat doesn't change due to increase temperature. SEM showed that alumina washcoat was even and no chap. XRD revealedγ-Al_2O_3 was main monocrystalline presented in the coating.
The selective catalytic reduction of NO_x by C_3H_6 was investigated over Pd/Al_2O_3, Pd/ CeZr/Al_2O_3, Pd/CeZr/TiO_2/Al_2O_3 wire-mesh honeycomb. The results showed that 0.186%-Pd/CeZr/TiO_2/Al_2O_3 wire-mesh honeycomb catalyst exhibited high catalytic activity at low temperature over a broad temperature range. The selective catalytic reduction of NO_x by NH_3 was investigated over V_2O_5-WO_3/TiO_2 wire-mesh honeycomb. The results showed that V(3)-W(7)/TiO_2 catalyst provided with more thermal stability and better performance of removing NO_x.
本文围绕Fe-Cr-Al丝网加工成蜂窝状金属丝网载体，采用电沉积法在蜂窝状金属丝网载体表面制备氧化铝涂层，利用SEM、XRD、EDX和BET等表征技术并结合超声波检测、热冲击性能实验等手段，考察了铁铬铝高温处理、电沉积电压、电沉积时间、沉积液中铝含量和铝粒径等多个因素对涂层性能的影响。具体工作如下：
研究过程中设计开发出两台蜂窝状金属丝网载体加工设备。通过复合电沉积法制备涂层，具体考察了影响涂层的因素，例如电沉积液、沉积电压、沉积时间，沉积液中添加剂的含量、添加剂的粒径、焙烧时间和焙烧温度等。实验结果显示，以添加剂和氧化铝的乙醇溶液为电沉积液，可以在蜂窝状金属丝网基体表面制备适宜厚度的氧化铝涂层。采用H_2SO_4对金属丝网载体进行预处理可以清洗其表面的污染物，通过加入添加剂，在900℃焙烧2h等方法提高涂层与金属基体的结合力，增强了涂层的抗热振性能和抗机械振动性能，氧化铝涂层的表面形态以及性质没有因焙烧温度的升高而被损坏。SEM电镜显示涂层表面均匀没有皲裂，XRD表明氧化铝涂层仍是主要以γ-Al_2O_3晶形存在。
制备了Pd／Al_2O_3、Pd／CeZr／Al_2O_3、Pd／CeZr／TiO_2／Al_2O_3三种蜂窝状金属丝网载体催化剂，并采用丙烯选择催化还原NO_x的实验来评价对NO_x的催化活性。结果表明Pd含量为0．186％时，Pd／CeZr／TiO_2／Al_2O_3蜂窝状金属丝网催化剂在低温条件下具有较高的催化活性，而且催化活性窗口较宽。制备了V_2O_5-WO_3／TiO_2三元催化剂并用氨气选择催化还原NO_x的实验来评价对NO_x的催化活性。结果表明V(3)-W(7)／TiO_2催化剂具有更好的热稳定性和较高的脱硝效率。
After-treatment control technique, especially catalytic convert is an effective method to solve the increasing serious atmospheric pollution from the NO_x emission. Metallic monoliths offer plenty of advantages over ceramic monoliths, such as stronger mechanical, strength, higher ductilitical, higher thermal conductibility, lower pressure drop, and now have become most attractive supports in emissions controls. However, the metallic monoliths could not be applied in practice because of the complex of processing and the low specific surface area. It is necessary to deposit the ceramic oxide washcoat with high surface area over metallic monoliths. Since thermal expansion coefficient of the metallic support is different from the ceramic oxide washcoat, the adhesion of washcoat is poor which leads to the washcoat chap and flake away. The poor coating binding strength between the metallic substrate and the washcoat has attracted more attention by the most researchers.
After the wrie-mesh honeycomb was manufactured by making alternatively corrugated and plain wire meshes and the coating technique of theγ-Al_2O_3 based ceramic washcoat on surface of FeCrAl metallic substrate by electrophoretic deposition was investigated in this paper.Partly including thepretreatment condition of the metallic substrate and preparation of slurry.The washcoat quality was measured by SEM, XRD, EDX and BET, ultrasonic vibration and thermal shock test. The main works are as following:
The wrie-mesh honeycomb was manufactured by two equipment, The manufacture process of wire-mesh honeycomb was simply, which could reduce the price of wire-mesh honeycomb .Washcoat deposited on metallic wire mesh was prepared usingγ-Al_2O powders by electrophoretic deposition. The preparation parameters of washcoat were investigated, such as the deposited solution, the deposited voltage, the deposited time. Wire meshes were dipped in H_2SO_4 solution for wiping off the dirts and enhancing the cohesion between the wire mesh and washcoat. The ability of thermal resistant and vibration resistant was improved by adding additives and higher calcinations temperature, the washcoat calcine at 900℃for 2h and the phase structure of washcoat doesn't change due to increase temperature. SEM showed that alumina washcoat was even and no chap. XRD revealedγ-Al_2O_3 was main monocrystalline presented in the coating.
The selective catalytic reduction of NO_x by C_3H_6 was investigated over Pd/Al_2O_3, Pd/ CeZr/Al_2O_3, Pd/CeZr/TiO_2/Al_2O_3 wire-mesh honeycomb. The results showed that 0.186%-Pd/CeZr/TiO_2/Al_2O_3 wire-mesh honeycomb catalyst exhibited high catalytic activity at low temperature over a broad temperature range. The selective catalytic reduction of NO_x by NH_3 was investigated over V_2O_5-WO_3/TiO_2 wire-mesh honeycomb. The results showed that V(3)-W(7)/TiO_2 catalyst provided with more thermal stability and better performance of removing NO_x.
引文
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