WO2007019801A1 - A honeycomb ceramic particle-capturing filter carrier, a particle-capturing filter assembly and a particle-capturing filter device composed of the carriers, as well as the methods for making the same - Google Patents

A honeycomb ceramic particle-capturing filter carrier, a particle-capturing filter assembly and a particle-capturing filter device composed of the carriers, as well as the methods for making the same Download PDF

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WO2007019801A1
WO2007019801A1 PCT/CN2006/002092 CN2006002092W WO2007019801A1 WO 2007019801 A1 WO2007019801 A1 WO 2007019801A1 CN 2006002092 W CN2006002092 W CN 2006002092W WO 2007019801 A1 WO2007019801 A1 WO 2007019801A1
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particle
filter
honeycomb ceramic
carrier
clay
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PCT/CN2006/002092
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English (en)
French (fr)
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Qinghua Chen
Dianyi Li
Yi Li
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Priority to KR1020087005712A priority Critical patent/KR101310787B1/ko
Priority to US12/063,813 priority patent/US8114184B2/en
Priority to JP2008526359A priority patent/JP2009504389A/ja
Priority to EP06775410.1A priority patent/EP1925353B1/en
Publication of WO2007019801A1 publication Critical patent/WO2007019801A1/zh
Anticipated expiration legal-status Critical
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    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/0006—Honeycomb structures
    • C04B38/0009—Honeycomb structures characterised by features relating to the cell walls, e.g. wall thickness or distribution of pores in the walls
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
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Definitions

  • the present invention relates to a honeycomb ceramic particulate trapping filter carrier, a particulate trapping filter and a particulate trapping filter device comprising the carrier, and a method of producing the same. More particularly, the present invention relates to a SiC-based wall flow type honeycomb ceramic capture filter carrier for use in an automobile (mainly a diesel vehicle) or an industrial exhaust gas catalytic purification device, the carrier-constituting particulate trap filter and particulate trapping Filtration devices, and methods for their preparation. Background technique
  • the exhaust catalytic converter consists mainly of a casing, a particulate trap filter and a catalyst.
  • the performance of the catalyst and particulate trap filter directly affects the activity of the catalyst, the effect of particulate trapping and the effect of exhaust gas purification.
  • Japan NGK Corporation and IBIDEN Company proposed to produce a particulate trapping filter using pure silicon carbide (see European Patent EP1142619A1), and the preparation method thereof is produced by extrusion, due to the particularity of pure silicon carbide particulate filter carrier production. Therefore, the whole body is formed by a split combination method, and a wall flow type design structure is formed by a universal cross-sealing method, and the trap filter is applied in diesel vehicle particle collection and regeneration.
  • the pure silicon carbide carrier has outstanding fire resistance at high temperature and can reach 2200 ° C. It has obvious high temperature advantage in the soot capture and regeneration process of diesel vehicles.
  • the carrier has a high sintering temperature (the sintering temperature is set to 2100 ° C to 2300 ° C in the present embodiment to obtain the average pore diameter in the European Patent No. 1 142 619 A1 [0065]. Further, the singering time is set to 0.1 hours to 5 hours. Further, the interior of a furnace has an inert atmosphere during sintering, and the pressure in that atmosphere is the Normal pressure", ⁇ sintering temperature at 2100-230 °C to ensure that the pore size range is between 6 ⁇ -15 ⁇ , and the porosity ranges from 35% to 50%.
  • the sintering temperature is set to 2100 ° C to 2300 ° C in the present embodiment to obtain the average pore diameter in the European Patent No. 1 142 619 A1 [0065].
  • the singering time is set to 0.1 hours to 5 hours.
  • the interior of a furnace has an inert atmosphere during sintering, and the pressure in that atmosphere is the Normal pressure", ⁇ sintering temperature
  • the sintering time is from 0.1 to 5 hours, and an inert gas atmosphere is maintained in the sintering furnace throughout the sintering process, and the pressure in the sintering furnace is atmospheric pressure atmospheric pressure). Since the sintering temperature has exceeded 2000 ° C, the requirements for the sintering equipment are very high and the equipment investment is also large, the inert gas atmosphere protection is required, the production process control is complicated, and the energy consumption is too high, so the price is high, The wide application of carriers has created great resistance. Especially in developing countries, it is very difficult to promote the use of this technology. Therefore, the improvement of product cost performance is an urgent technical problem in the technical field. Summary of the invention
  • the object of the present invention is to provide a honeycomb ceramic microparticle-collecting filter carrier based on silicon carbide as a base material, a common clay as a binder, a particle trap filter composed of the carrier, and Particle capture filter unit. Meanwhile, the present invention also provides a method of preparing the particulate trapping filter carrier, the particulate filter trap, and the particulate trapping filter device.
  • honeycomb ceramic particle collecting and filtering carrier which is made of the following raw materials by weight: silicon carbide 1, clay 0.05 ⁇ 0.5, flour 0.1 ⁇ 0.35, engine oil 0.025 ⁇ 0.05, water 0.2 ⁇ 0.35; carrier product is 4 holes ⁇ 62 holes / cm 2 honeycomb type; honeycomb wall thickness is 0.2 ⁇ L2mm; its microporosity is 40% ⁇ 70%, ⁇ through hole rate > 30%; microporous pores The radius is distributed between 1 and 50 ⁇ m.
  • the clay is an industrial clay or a pigment grade clay
  • the engine oil is selected from one of a heavy fraction lubricating oil or a synthetic lubricating oil; or a mixture thereof.
  • the silicon carbide is preferably composed of two kinds of silicon carbide having a particle size difference of 200 to 400 mesh and a weight fraction of between 1:4 and 3:4.
  • the invention provides a preparation method of the honeycomb ceramic particle collection filter carrier, and the method comprises the following steps -
  • the step (2) of the silicon carbide is sieved by a vibrating sieve, and the two kinds of silicon carbide having a difference in particle size of 200 to 400 mesh and a weight fraction of between 1:4 and 3:4 are used.
  • the opening ratio is >30%, and the pore radius of the micropores is between 1 and 50 ⁇ m. If the pore radius of the micropores is higher than 50 ⁇ m, the particles will leak and fail to achieve the trapping effect; the optimal average pore radius is distributed between 10 and 30 ⁇ m;
  • the honeycomb ceramic particles after firing have a wall thickness of about 0.2 to 1.2 mm, and a wall thickness of >1.2 mm, the porosity of the pores is small, and the back pressure is multiplied, which has a great influence on the power of the engine.
  • the wall thickness ⁇ 0.2mm will reduce the mechanical strength of the wall, so it will also affect the use; the optimum wall thickness is between 0.2 ⁇ 0.6mm;
  • silicon carbide graded paired porosity has an important effect.
  • two or more kinds of silicon carbide with different particle sizes should be used.
  • the particle size should be 200 ⁇ 400 mesh difference, such as 200 mesh + 400 mesh.
  • the appropriate combination of silicon carbide will achieve the appropriate effect.
  • the above description is only an example.
  • the combination method is not only one kind; the amount of silicon carbide should account for 50% ⁇ 95% of the total active ingredient.
  • Clay should be selected from industrial clay or pigment grade clay.
  • the clay of >200 mesh should be selected as the high temperature binder phase.
  • the amount of clay should be selected according to the gradation of silicon carbide. It should be selected by simulation to be slightly higher than seepage.
  • the amount of diameter formation is good, generally between 5% and 50%.
  • the present invention also provides a particulate trapping filter comprising a plurality of said honeycomb ceramic microparticles to collect a filter carrier, wherein the carriers are connected by an adhesive layer, and the weight of the binder is
  • the composition is: silicon carbide 1, clay 0.2 ⁇ 1, water glass 0.06 ⁇ 0.35; coating thickness is l-3mm.
  • the present invention also provides a method for preparing a particulate trapping filter, comprising the following steps: (1) using the honeycomb ceramic microparticles to collect a filter carrier as an assembly;
  • the surface of the green body is brushed with a bonding slurry, dried and formed by surface treatment to obtain a particle collecting filter.
  • the application volume of the particulate trap filter should match the displacement of the automobile.
  • the experimental study of the present invention shows that the optimal matching method is that the particle trap filter volume is 1 to 2.5 times the displacement of the diesel vehicle.
  • the regeneration of particulate trapping filters can be carried out by chemical and physical methods, such as catalytic continuous regeneration of CRT, fuel injection, electric heating, etc. These devices are best used and will be used in on-board inspection systems for automotive and diesel vehicles (OBD systems). Used in combination.
  • the present invention also provides a particulate trapping filter apparatus comprising a stainless steel outer casing, a filter welded and packaged in a stainless steel outer casing, an insulating gasket wrapped around the outer portion of the filter, an intake pipe and an air outlet pipe, characterized in that The filter is the particle trap filter of the present invention.
  • the present invention also provides a method for preparing a particulate trapping filter device, the method comprising: wrapping the particulate trap filter of the present invention with an insulating gasket, soldering and encapsulating it in a stainless steel casing, and welding the intake pipe And an air outlet pipe, forming a particulate trapping filter device, which is applied to diesel vehicle engine exhaust gas particle collection and filtration and post-treatment.
  • the basic principle of the invention The principle of hemofiltration (seepage) in physical and chemical research is adopted, so that a refractory material with a matrix of SiC can be fired at a lower temperature while maintaining a certain degree of refractoriness; Under the premise of reducing certain refractoriness and meeting the basic requirements of catalytic or filter materials, the purpose of saving energy, reducing costs, expanding production, and expanding the scope of use can be achieved.
  • the basic requirement is that the volume or weight ratio of the clay used as the binder phase should be close to or appropriately exceed the percolation limit. In a typical three-dimensional material, the ratio should be 5% to 50%, depending not only on the type of material but also on the material.
  • the microstructure of the material has specific lower limits for the specific material.
  • a porous honeycomb ceramic body is formed using advanced extrusion molding techniques. With the traditional sintering technology, special requirements such as fire resistance, thermal conductivity, thermal expansion, porosity and mechanical and mechanical properties are achieved by adjusting the formulation.
  • the present invention has the following beneficial effects:
  • the product has the following outstanding performance characteristics: 1 Due to the advanced extrusion molding process, the honeycomb ceramic carrier has a large number of straight holes per unit surface area and can be 4 to 62 holes/cm 2 . 2 The carrier is formed by the principle of grading and seepage, and the pores are extremely rich in micropores (the size and distribution of the pores can be adjusted by powder grading, binder or pore former), which is beneficial to the loading of the catalyst. Conducive to diesel vehicle exhaust particulate capture and filtration. 3 It is used for the capture, filtration and regeneration of diesel vehicle exhaust particulates. It can be periodically removed by chemical methods or by injection or electric heating to ensure the smooth and effective operation of the diesel vehicle exhaust particulate trapping filter.
  • the sintering temperature of the products produced requires a high temperature of 2100 ° C to 2300 ° C.
  • the requirements for sintering equipment are high and the equipment investment is also large, and inert gas is required.
  • the atmosphere is protected, the production process is complicated to control, and the energy consumption is too high. Therefore, the price of the product is very high.
  • the product produced by the present invention has a sintering temperature of less than 1,350 ° C and is protected from sintering by an inert gas atmosphere. Therefore, the production cost of the product is greatly reduced, energy consumption and equipment investment are saved, and the cost performance of the product is relatively better.
  • using the universal cross-sealing method A wall flow type particle trap filter is formed.
  • the preparation method has the advantages of abundant raw materials, low cost, easy molding and reasonable sintering process.
  • honeycomb ceramic particle collecting and filtering carrier with SiC as a basic raw material provided by the invention can be firstly used for the treatment of automobile exhaust gas, and can be widely applied to the exhaust gas purification problem of the diesel locomotive, and is used for collecting and decomposing soot and harmful gases.
  • the present invention effectively reduces environmental pollution of diesel vehicles and other motor vehicle exhaust gases.
  • Figure 1 is a schematic view of a square particle trap filter of the present invention
  • Figure 2 is a schematic view of a circular particle trap filter of the present invention
  • Figure 3 is a schematic view of a racetrack shaped particle trap filter of the present invention.
  • Figure 4 is a schematic view of the exhaust gas particulate trapping filter device used in the exhaust gas particulate trapping and post-treatment of diesel automobile engines.
  • the raw materials are composed of silicon carbide, selected clay, flour, heavy distillate lubricating oil and water.
  • the composition of the raw materials is silicon carbide 1, clay 0.5, flour 0.35, engine oil 0.05, water 0.35; silicon carbide powder is 200 mesh powder. It is mixed with 400 mesh powder in a ratio of 1:3; the clay has a particle size of 1200 mesh.
  • Flour and water are mixed into a slurry, gelatinized at 65 ° C ⁇ 100 ° C, ready for use; the silicon carbide, clay and heavy fraction lubricating oil are mixed in a blender for 1 hour, then added to the flour paste, stirred for 1 hour , forming a uniform mud pack for use.
  • the mud was sieved through a 100 mesh sieve and then extruded with a 1.2 mm, 25 hole/square inch (25 CPSI) mold to form a 57 x 57 x 254 mm 3 sample for use. Dry at room temperature Block with the fork hole, heat at 5 °C / min to 600 ⁇ for 6 ⁇ 12 hours; then raise the temperature to 1250 ⁇ for 6 ⁇ 12 hours, cool the furnace to room temperature and exit the kiln to form the finished product. Product performance is shown in Table 1.
  • Example 1 was repeated, with the following differences: The composition by weight of the raw materials was silicon carbide 1, clay 0.15, flour 0.35, heavy fraction lubricating oil 0.05, water 0.35; silicon carbide powder using 200 mesh powder and 500 mesh powder to 3: The ratio of 4 is mixed; the clay has a particle size of 1000 mesh.
  • Example 1 was repeated, with the following differences: The composition by weight of the raw materials was silicon carbide 1, clay 03, flour 0.18, heavy fraction lubricating oil 0.03, water 0.25; silicon carbide powder used 200 mesh powder and 600 mesh powder to 1: The ratio of 4 is mixed; the clay has a particle size of 200 mesh.
  • Example 1 was repeated, with the following differences: The composition by weight of the raw materials was silicon carbide 1, clay 0.4, flour 0.3, synthetic lubricating oil 0.04, water 0.30; silicon carbide powder using 250 mesh powder and 450 mesh powder in a ratio of 1:3 Mixed; clay has a particle size of 800 mesh.
  • Example 5 The composition by weight of the raw materials was silicon carbide 1, clay 0.4, flour 0.3, synthetic lubricating oil 0.04, water 0.30; silicon carbide powder using 250 mesh powder and 450 mesh powder in a ratio of 1:3 Mixed; clay has a particle size of 800 mesh.
  • Example 5 The composition by weight of the raw materials was silicon carbide 1, clay 0.4, flour 0.3, synthetic lubricating oil 0.04, water 0.30; silicon carbide powder using 250 mesh powder and 450 mesh powder in a ratio of 1:3 Mixed; clay has a particle size of 800 mesh.
  • Example 5 The composition by weight of the raw materials was silicon carbide 1, clay 0.4, flour 0.3, synthetic lubricating oil 0.04, water
  • the composition of the raw materials is silicon carbide 1, clay 0.2, flour 0.35, synthetic lubricating oil 0.05, water 0.35; silicon carbide powder is 200 mesh powder and 400 mesh powder was mixed in a ratio of 1:3; the clay had a particle size of 1200 mesh.
  • the flour and water were mixed into a slurry, and gelatinized at 65 ° C to 100 ° C for use; the remaining raw materials were mixed in a blender for 2 hours, then the flour paste was added, and the mixture was thoroughly stirred for 2 hours to form a uniform mud.
  • the mud was sieved through a 120 mesh sieve and then extruded through a die having a wall thickness of 1.0 mm and 25 holes per square inch (25 CPSI) to form a sample of 36 x 36 x 254 mm 3 for use.
  • the composition of the raw materials is silicon carbide 1, clay 0.1, flour 0.35, synthetic lubricant and heavy Distillate lubricating oil 0.05, water 0.35; silicon carbide powder was mixed with 220 mesh powder and 440 mesh powder in a ratio of 1:3; the clay had a particle size of 1200 mesh.
  • the mud was sieved through a 150 mesh sieve and then extruded with a wall thickness of 0.6 mm and a 120 hole/square inch (120 CPSI) die to form a 36 x 36 x 254 mm 3 sample for use.
  • the composition of the binder is: silicon carbide 1, clay 0.2, water glass 0.06;
  • the layer thickness is about 1 mm, and the assembly is bonded one by one to form a desired particle-collecting filter preform in the shape of a square cylinder, a rectangular cylinder, a raceway elliptical cylinder or a cylinder;
  • the composition of the binder is: silicon carbide 1, clay 1, water glass 0.35;
  • the layer thickness is about 3 mm, and the assembly is bonded one by one to form a desired particle-collecting filter preform in the shape of a square cylinder, a rectangular cylinder, a racetrack elliptical cylinder or a cylinder;
  • the surface of the green body is brushed with a bonding paddle, dried and shaped to obtain a particle trapping filter.
  • the particle trap filter 2 prepared in Embodiment 7 or 8 is externally wrapped with an insulating gasket 1, welded and packaged in a stainless steel casing 3, and welded to the intake pipe 4 and the gas outlet pipe 5 to form exhaust gas particles.
  • a capture filter device is used for exhaust gas particulate capture and post-treatment of diesel vehicle engines.

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Description

一种蜂窝陶瓷微粒捕集过滤载体、 该载体构成的微粒捕集过滤器和 微粒捕集过滤装置及它们的制备方法 技术领域
本发明涉及蜂窝陶瓷微粒捕集过滤载体、 该载体构成的微粒捕集过滤器 和微粒捕集过滤装置及它们的制备方法。 更具体地说， 本发明涉及一种汽车 (主要是柴油车） 或工业废气催化净化装置采用的 SiC基壁流式蜂窝陶瓷捕 集过滤载体， 该载体构成的微粒捕集过滤器和微粒捕集过滤装置， 以及它们 的制备方法。 背景技术
现代社会的发展使汽车保有量出现了大幅度增长， 而尾气排放所产生的 污染也大量增加。 汽车集中的发达地区， 特别是大城市， 尾气排放产生的污 染已占这些地区大气污染的 50%〜60%。 随着人们对生存环境的重视， 降低 汽车尾气排放， 治理尾气污染已成为国内外关注的话题。 从技术上而言， 降 低汽车尾气排放的措施有机前措施、 机内措施和机后措施等三种方法， 目前 国内外主要是采用上述三种措施结合的方法治理尾气， 随着尾气排放标准逐 渐提高， 机外措施就显得更加重要， 即用催化净化的方法来降低尾气污染物 的排放。 汽车 （柴油车） 尾气催化净化器主要由外壳、 微粒捕集过滤器和催 化剂三部分组成。催化剂及微粒捕集过滤器的性能直接影响着催化剂的活性、 微粒捕集的效果和尾气净化效果。
现有技术中， 日本 NGK公司和 IBIDEN公司提出用纯的碳化硅生产微 粒捕集过滤器 (见欧洲专利 EP1142619A1 ), 其制备方法采用挤压方式生产， 由于纯碳化硅微粒过滤载体生产的特殊性， 因而采用分体组合的方式构成整 体， 并且采用世界通用的交叉封孔的方法形成壁流式设计结构， 该捕集过滤 器在柴油车微粒捕集再生中得到了应用。 纯碳化硅载体在高温下耐火性能突 出， 可以达到 2200°C， 在柴油车碳烟捕集和再生过程中有明显的高温优势。 但是， 该载体由于烧结温度高 (在欧洲专利 EP1142619A1 【0065】条中对烧 结温度和工艺的描述是" The sintering temperature is set to 2100°C to 2300°C in the present embodiment to obtain the average pore diameter of 6μιη-15μηι and a porosity of 35% to 50%. Further, the singtering time is set to 0.1 hours to 5 hours. Further, the interior of a furnace has an inert atmosphere during sintering, and the pressure in that atmosphere is the normal pressure", 艮卩烧结温度在 2100-230 °C 以保证获得孔径范围在 6μπι-15μπι之间， 并获得孔隙率范围在 35%-50%之间。 烧结时间在 0.1-5小时， 在整个烧结过程中， 烧结炉内要保 持有惰性气体气氛， 烧结炉内的压力为常压大气压）。 由于烧结温度已超过 2000°C， 对烧结设备的要求很高并且设备投入也是很大的， 需要惰性气体气 氛保护， 生产工艺控制复杂， 能耗太高， 因此， 其价格居高不下， 对该载体 的广泛应用形成了极大的阻力， 特别是在发展中国家， 推广使用该技术非常 困难， 因此， 产品性价比的提高是本技术领域一个急待解决的技术难题。 发明内容
本发明的目的在于针对现有技术的不足，提供一种以碳化硅为基础原料， 普通粘土为粘结料的蜂窝陶瓷微粒捕集过滤载体、 一种由该载体构成的微粒 捕集过滤器及微粒捕集过滤装置。 同时， 本发明还提供所述微粒捕集过滤载 体、 微粒过滤捕集器和微粒捕集过滤装置的制备方法。
本发明的目的通过下述技术方案予以实现。
本发明提供了一种蜂窝陶瓷微粒捕集过滤载体， 该载体是由下述重量份 数的原料制成的： 碳化硅 1， 粘土 0.05〜0.5， 面粉 0.1〜0.35， 机油 0.025〜 0.05 , 水 0.2〜0.35； 载体产品为 4 孔〜 62 孔 /平方厘米的蜂窝型；蜂窝体壁 厚为 0.2〜L2mm; 其微孔孔隙率为 40%〜70%，· 通孔率 > 30%; 微孔孔隙半 径分布在 1〜50μπι。
其中， 所述的粘土为工业粘土或颜料级粘土； 所述的机油选自重质馏份 润滑油或合成润滑油中的一种； 或它们的混合物。
所述的碳化硅优选地由两种颗粒度相差 200〜400 目， 重量份数比在 1:4〜3:4之间的碳化硅组成。
本发明提供了所述蜂窝陶瓷微粒捕集过滤载体的制备方法， 该方法包括 下列步骤-
( 1 ) 按配比称量各组分；
(2)将碳化硅与粘土充分混合均匀； 然后加入机油， 在搅拌机内充分搅 拌， 待用；
(3) 将面粉和水在常温下混合成浆， 在 65°C〜100°C下熟化成糊精； (4) 将糊精和步骤 （2) 的所得物在搅拌机内混合， 搅拌 1〜3小时；
(5) 对泥料进行混炼和筛制， 使泥料充分均匀；
(6) 用模具挤压成横截面为不同几何外形的载体， 形成 4 孔〜 62 孔 / 平方厘米的蜂窝型陶瓷素坯， 经室温干燥和叉孔封堵， 形成蜂窝陶瓷微粒捕 集过滤载体生坯；
(7)以< 5°C/分钟的速度加温到 600°C〜900°C保温 2〜； 12小时； 然后将 温度升到 1250°C〜1350°C保温 0.5〜12小时， 随炉冷却到室温出窑， 制得所 需的蜂窝陶瓷微粒捕集过滤载体。
优选地， 步骤（2)碳化硅用震动筛筛分，釆用两种颗粒度相差 200〜400 目， 重量份数比在 1:4〜3:4之间的碳化硅搭配。
本发明深入系统的试验结果表明：
( 1 ) 烧成后的蜂窝陶瓷微粒捕集过滤载体产品微孔孔隙率在 40%〜
70%, 其中开孔率 >30%，· 微孔孔隙半径分布在 1〜50μηι之间。如果微孔孔隙 半径高于 50μπι， 那么， 微粒就会泄漏， 达不到捕集效果； 最佳的平均孔隙 半径分布在 10〜30μιη之间；
(2) 烧成后的蜂窝陶瓷微粒捕集过滤载体壁厚约为 0.2〜1.2mm， 壁厚 >1.2 mm则气孔通孔率较小， 背压会成倍增加， 对发动机的功率影响较大； 壁厚 <0.2mm 则壁面机械强度会相应降低， 因此也会影响使用； 最佳壁厚在 0.2〜0.6mm之间；
(3 )碳化硅级配对孔隙率的形成有重要影响， 一般应该采用两种以上颗 粒度不同的碳化硅，颗粒度搭配应该两两相差 200〜400目为好，如采用（200 目 +400目）碳化硅进行适当搭配会取得恰当的效果， 以上的叙述仅仅是一个 范例， 搭配方法不仅此一种； 碳化硅的量应该占总有效成分的 50%〜95%。
(4) 粘土应该选用工业粘土或颜料级粘土作为对象， 应该选择>200 目 的粘土作为高温粘结相， 粘土的使用量应该根据碳化硅的级配选择， 应该用 模拟的方法选择稍高于渗流径形成的量为好， 一般应在 5%-50%之间。
本发明还提供了一种微粒捕集过滤器， 该微粒捕集过滤器包括多个所述 的蜂窝陶瓷微粒捕集过滤载体， 载体间通过粘结剂层连接， 所述粘结剂的重 量份组成为： 碳化硅 1 ,粘土 0.2〜1, 水玻璃 0.06〜0.35； 涂层厚度为 l-3mm。
本发明还提供了一种微粒捕集过滤器的制备方法， 其包括下列步骤： ( 1 ) 使用所述的蜂窝陶瓷微粒捕集过滤载体作为组合件；
(2)用粘结剂均匀涂抹于需要粘结的所述的蜂窝陶瓷微粒捕集过滤载 体组合件表面相互粘结而成， 所述的粘结剂的重量份组成为： 碳化硅 1 , 粘土 0.2〜1, 水玻璃 0.06〜0.35 ； 涂层厚度约为 l〜3mm， 将组合件一 一粘合， 形成所需的各种几何形状的微粒捕集过滤器初坯；
(3 )用粘结浆料刷涂初坯表面，干燥成形并经表面处理后制得微粒捕 集过滤器。
该微粒捕集过滤器的应用体积应该和汽车的排量匹配， 本发明的试验研 究表明最佳的匹配方式为:微粒捕集过滤器体积是柴油车的排量的 1〜2.5倍。
微粒捕集过滤器的再生问题可以采用化学物理方法， 如催化连续再生 CRT, 喷油燃烧、 电加热等， 这些装置的应用最好和将要采用的汽车、 柴油 车车载在线检测系统 （OBD系统） 联合使用。 本发明还提供了一种微粒捕集过滤装置， 包括不锈钢外壳， 焊接并封装 于不锈钢外壳内的过滤器、包裹在过滤器外部的隔热衬垫、进气管和出气管， 其特征在于所述的过滤器是本发明所述的微粒捕集过滤器。
本发明还提供了一种微粒捕集过滤装置的制备方法， 该方法包括： 将本 发明所述的微粒捕集过滤器外部包裹隔热衬垫，焊接并封装于不锈钢外壳内， 并焊接进气管和出气管， 形成微粒捕集过滤装置， 该装置应用于柴油车发动 机尾气微粒捕集过滤和后处理。
本发明的基本原理： 采用了物理化学研究中的愈渗 （渗流） 原理， 使一 个基体为 SiC的耐火材料， 可以在保持一定的耐火度的前提下， 在较低的温 度下得以烧成； 在降低一定耐火度、 同时满足催化或过滤材料的基本要求的 前提下， 达到节约能源、 降低成本、 扩大生产、 扩充使用范围的目的。 基本 要求是， 作为粘结相使用的粘土的体积或重量比应该接近或适当超过渗流极 限， 在通常三维材料中该比值应该为 5%〜50%， 该百分比不仅取决于材料种 类， 还取决于材料的微观结构， 对于具体的材料有具体的下限值。 应用先进 的挤压成型技术形成多孔的蜂窝陶瓷坯体。 采用传统的烧结技术， 通过调节 配方， 达到具有适当的耐火、 导热、 热膨胀、 孔隙率和力学机械性能等特殊 要求。
与现有技术相比本发明具有以下有益效果：
( 1 )产品具有以下几个突出的性能特点： ①由于采用先进的挤压成型工 艺,蜂窝陶瓷载体单位表面积的直孔数众多,可在 4〜62孔 /平方厘米。 ②载体 由于用级配和渗流原理,孔壁上形成极其丰富的微细孔 (孔的大小和分布可以 用粉末级配、 粘接剂或造孔剂加以调节)，有利于催化剂的负载,同时也有利于 柴油车尾气微粒捕集过滤。 ③用于柴油车尾气微粒的捕集过滤和再生， 可以 定期用化学方法或喷油或电加热的方法除去捕集的微粒， 保证柴油车尾气微 粒捕集过滤器的畅通和有效工作。
(2)使用工业碳化硅和粘土为主要原料， 材料来源广泛、 价格低廉、 成 型容易，烧结可使用传统粘土耐火材料烧结设备， 大大简化了生产加工过程， 得到的陶瓷体不仅多孔， 而且导热、 孔隙度和机械强度足以用于汽车、 化工 等行业的催化捕集过滤载体。
(3 )与 IBIDEN所申请的专利内容相比， 其生产产品的烧结温度要求达 到 2100°C 至 2300°C的高温，对烧结设备的要求很高并且设备投入也是很大 的， 同时需要惰性气体气氛保护， 生产工艺控制复杂， 能耗太高， 因此， 其 产品价格非常高。 而本发明生产的产品的烧结温度低于 1350°C， 且不用惰性 气体气氛保护烧结。 因此， 产品的生产成本大大降低， 节约了能耗和设备的 投入， 产品的性价比相对更加优良。 同时， 采用世界通用的交叉封孔的方法， 形成壁流式微粒捕集过滤器。 其制备方法原料丰富， 成本低廉， 成型容易， 烧结工艺合理。
(4) 具有十分广泛的应用范围， 例如： 冶金行业的熔渣过滤、 热交换; 环境处理问题中的污水过滤及净化等； 化工行业中的催化剂载体； 航空、 航 天材料的制备等。 本发明提供的以 SiC为基本原料的蜂窝陶瓷微粒捕集过滤 载体首先可用于汽车尾气的处理，并可推广应用于柴油机车的尾气净化问题， 用于捕集、 分解烟尘及有害气体。 本发明有效地减少柴油车以及其它机动车 辆尾气对环境的污染。
附图说明
图 1 是本发明的方形微粒捕集过滤器示意图；
图 2是本发明的圆形微粒捕集过滤器的示意图；
图 3是本发明的跑道形微粒捕集过滤器的示意图；
图 4本发明应用于柴油汽车发动机尾气微粒捕集和后处理时，其尾气微 粒捕集过滤装置的示意图
其中图号
1隔热衬垫 2过滤器 3不锈钢外壳 4进气管 5出气管
具体实施方式
通过下面给出的具体实施例可以进一步清楚地了解本发明。 但它们不是 对本发明的限定。
实施例 1
以碳化硅、 精选粘土、 面粉、 重质馏份润滑油、 水为原料， 原料的重量 份组成为碳化硅 1， 粘土 0.5， 面粉 0.35， 机油 0.05， 水 0.35; 碳化硅粉采用 200目粉和 400目粉以 1 : 3的比例混合； 粘土的颗粒度为 1200目。 将面粉 和水混合成浆， 在 65°C〜100°C下糊化， 备用； 将碳化硅、 粘土和重质馏份 润滑油在搅拌机内混合 1小时， 然后加入面粉糊， 充分搅拌 1小时， 形成均 匀泥团备用。 将泥团用 100 目筛过筛， 然后用壁厚为 1.2mm、 25孔 /平方英 寸 （25CPSI) 的模具挤压， 形成 57x57x254 mm3的样品备用。 经过室温干燥 和叉孔封堵， 以 5 °C/分钟的速度加温到 600Ό保温 6〜12小时； 然后将温度 升到 1250Ό保温 6〜12小时， 随炉冷却到室温出窑， 形成成品。 产品性能见 表 1。
样品尺寸： 57x57x254 mm3, 载体型号： MJK-1
Figure imgf000008_0001
实施例 2
重复实施例 1， 有以下不同： 原料的重量份组成为碳化硅 1， 粘土 0.15， 面粉 0.35， 重质馏份润滑油 0.05 , 水 0.35 ； 碳化硅粉采用 200 目粉和 500 目粉以 3 : 4的比例混合； 粘土的颗粒度为 1000目。
实施例 3
重复实施例 1， 有以下不同： 原料的重量份组成为碳化硅 1， 粘土 03， 面粉 0.18， 重质馏份润滑油 0.03， 水 0.25 ; 碳化硅粉采用 200目粉和 600目 粉以 1 : 4的比例混合； 粘土的颗粒度为 200目。
实施例 4
重复实施例 1, 有以下不同： 原料的重量份组成为碳化硅 1， 粘土 0.4，面 粉 0.3， 合成润滑油 0.04， 水 0.30; 碳化硅粉采用 250目粉和 450目粉以 1 : 3 的比例混合； 粘土的颗粒度为 800目。 实施例 5
以碳化硅、 精选粘土、 面粉、 合成润滑油、 水为原料， 原料的重量份组 成为碳化硅 1， 粘土 0.2，面粉 0.35， 合成润滑油 0.05， 水 0.35 ; 碳化硅粉采用 200目粉和 400目粉以 1 : 3的比例混合； 粘土的颗粒度为 1200目。 将面粉 和水混合成浆， 在 65°C〜100°C糊化后备用； 将其余原料在搅拌机内混合 2 小时， 然后加入面粉糊， 充分搅拌 2小时， 形成均匀泥团备用。 将泥团用 120目筛过筛，然后用壁厚为 1.0 mm， 25孔 /平方英寸（25CPSI) 的模具挤压， 形成 36x36x254 mm3的样品备用。
经过室温干燥， 交叉堵孔后， 以 1 °C/分钟的速度加温到 900°C保温 2〜6 小时； 然后将温度升到 1350°C保温 0.5〜2小时， 随炉冷却到室温出窑， 形成 成品， 性能如表 2所示。
表 2.样品尺寸： 36x36x254 mm3， 载体型号： MJK-2
Figure imgf000009_0001
1 '
实施例 6
1
以碳化硅、精选粘土、面粉、合成润滑油和重质馏寸份润滑油、水为原料， 原料的重量份组成为碳化硅 1，粘土 0.1,面粉 0.35，合成润 o滑油和重质馏份润 滑油 0.05,水 0.35 ； 碳化硅粉采用 220目粉和 440目粉以 1 : 3的比例混合； 粘土的颗粒度为 1200目。 将面粉和水混合成浆， 在 65〜100°C糊化后备用； 将其余原料在搅拌机内混合一小时， 然后加入面粉糊， 充分搅拌 1〜3小时， 形成均匀泥团备用。
将泥团用 150 目筛过筛， 然后用壁厚为 0.6 mm, 120 孔 /平方英寸 ( 120CPSI) 的模具挤压， 形成 36x36x254 mm3的样品备用。
经过室温干燥并交叉封孔后， 以 3°C/分钟的速度加温到 800°C保温 4〜6 小时； 然后将温度升到 1300Ό保温 1〜4小时， 随炉冷却到室温出窑， 形成 成品， 产品性能如表 3。
表 3. (样品尺寸： 36x36x254 mmj, 载体型号： MJK-3 )
产品化学组成 【（a-SiC) + (β-SiC) +粘土】烧结体
材料密度 （g/cm3) 3. 65
壁面材料比重 （g/cm3) 1.48
载体视在比重 （g/cm3) 0.78
单位英寸孔数 /壁厚 （CPSI il) 120/24
背压 (mb) < 70—200
微孔分布范围 μηι 1—50
开孔率 >30%
耐火度 （°c) 1500
正常使用温度 （°c) 实施例 7
参见图 1到 3所示，
( 1 ) 采用实施例 1至 6中制备的任何一种微粒捕集过滤载体作为组合件;
(2) 用粘结剂均匀涂抹于需要粘结的微粒捕集过滤载体组合件表面相互 粘结， 所述的粘结剂的重量份组成为： 碳化硅 1， 粘土 0.2, 水玻璃 0.06； 涂层厚度约为 1mm, 将组合件一一粘合， 形成所需的方柱体、 长方柱体、 跑道椭圆柱体或圆柱体等形状的微粒捕集过滤器初坯；
(3) 用粘结浆料刷涂初坯表面， 干燥成形并经表面处理后制得微粒捕集 过滤器。
实施例 8
(4) 采用实施例 1至 6中制备的任何一种微粒捕集过滤载体作为组合件;
(5 ) 用粘结剂均匀涂抹于需要粘结的微粒捕集过滤载体组合件表面相互 粘结，所述的粘结剂的重量份组成为：碳化硅 1，粘土 1， 水玻璃 0.35 ; 涂层厚度约为 3mm, 将组合件一一粘合， 形成所需的方柱体、 长方 柱体、 跑道椭圆柱体或圆柱体等形状的微粒捕集过滤器初坯；
(6) 用粘结桨料刷涂初坯表面， 干燥成形并经表面处理后制得微粒捕集 过滤器。
实施例 9
参见图 4所示，将实施例 7或 8制备的微粒捕集过滤器 2外部包裹隔热衬 垫 1， 焊接并封装于不锈钢外壳 3内， 并焊接进气管 4和出气管 5， 形成尾气 微粒捕集过滤装置，该装置应用于柴油车发动机尾气微粒捕集过滤和后处理。 上述各种实施例只是对本发明做示例性说明， 本发明不以上述实施例为 限。

Claims

权 利 要 求
1.一种蜂窝陶瓷微粒捕集过滤载体， 该载体是由下述重量份数的 原料制成的：碳化硅 1 , 粘土 0.05〜0.5，面粉 0.1〜0.35， 机油 0.025〜 0.05, 水 0.2〜0.35；载体产品为 4孔〜 62孔 /平方厘米的蜂窝型； 蜂窝 体壁厚 0.2〜1.2mm; 其微孔孔隙率为 40%〜70%； 通孔率 > 30%; 微 孔孔隙半径分布在 1〜50μιη之间。
2.根据权利要求 1 所述的蜂窝陶瓷微粒捕集过滤载体， 其中所述 的粘土为工业粘土或颜料级粘土。
3.根据权利要求 1 所述的蜂窝陶瓷微粒捕集过滤载体， 其中所述 的机油选自重质馏份润滑油或合成润滑油中的一种；或它们的混合物。
4. 根据权利要求 1所述的蜂窝陶瓷微粒捕集过滤载体， 其中所述 的微孔孔隙平均半径分布在 10〜30μιη。
5. 根据权利要求 1所述的蜂窝陶瓷微粒捕集过滤载体， 其中所述 的碳化硅由两种颗粒度相差 200〜400目， 重量份数比在 1 :4〜3:4之间 的碳化硅组成。
6.—种权利要求 1所述的蜂窝陶瓷微粒捕集过滤载体的制备方法， 该方法包括下列步骤：
( 1 ) 按配比称量各组分；
(2)将碳化硅与粘土充分混合均匀； 然后加入机油， 在搅拌机内 充分搅拌， 待用；
(3 )将面粉和水在常温下混合成浆， 在 65°C〜100°C下熟化成糊 精；
(4) 将糊精和步骤 （2 ) 的所得物在搅拌机内混合， 搅拌 1〜3 小时；
( 5 ) 对泥料进行混炼和筛制， 使泥料充分均匀；
(6) 用模具挤压成横截面为不同几何外形的载体， 形成 4 孔〜 62 孔 /平方厘米的蜂窝型陶瓷素坯， 经室温干燥和叉孔封堵， 形成蜂 窝陶瓷微粒捕集过滤载体生坯；
(7) 以< 5 /分钟的速度加温到 600°C〜900°C保温 2〜12小时； 然后将温度升到 1250°C〜1350°C保温 0.5〜12小时， 随炉冷却到室温 出窑， 制得所需的蜂窝陶瓷微粒捕集过滤载体。
7. 根据权利要求 6 所述的蜂窝陶瓷微粒捕集过滤载体的制备方 法， 其中步骤 （2) 中将碳化硅用震动筛筛分， 采用两种颗粒度相差 200〜400目， 重量份数比在 1 :4~3:4之间的碳化硅搭配。
8.—种微粒捕集过滤器， 该微粒捕集过滤器包括多个权利要求 1 至 5中任一权利要求所述的蜂窝陶瓷微粒捕集过滤载体， 载体间通过 粘结剂层连接，所述粘结剂的重量份组成为：碳化硅 1，粘土0.2〜1， 水 玻璃 0.06〜0.35； 涂层厚度为 l〜3mm。
9. 一种权利要求 8所述的微粒捕集过滤器的制备方法，该方法包 括下列步骤：
( 1 )使用权利要求 1至 5中任一权利要求所述的蜂窝陶瓷微粒 捕集过滤载体作为组合件；
(2)用粘结剂均匀涂抹于需要粘结的权利要求 1至 5中任一权 利要求所述的蜂窝陶瓷微粒捕集过滤载体组合件表面相互粘结而 成， 所述的粘结剂的重量份组成为： 碳化硅 1， 粘土 0.2〜1, 水玻 璃 0.06〜0.35； 涂层厚度约为 〜 3mm， 将组合件一一粘合， 形成 所需的各种几何形状的微粒捕集过滤器初坯；
(3 )用粘结浆料刷涂初坯表面， 干燥成形并经表面处理后制得 微粒捕集过滤器。
10. 一种微粒捕集过滤装置， 包括不锈钢外壳， 焊接并封装于不 锈钢外壳内的过滤器、 包裹在过滤器外部的隔热衬垫、 进气管和出气 管， 其特征在于所述的过滤器是权利要求 8所述的微粒捕集过滤器。
11. 一种权利要求 10所述的微粒捕集过滤装置的制备方法，该方 法包括： 将权利要求 8所述的微粒捕集过滤器外部包裹隔热衬垫， 焊 接并封装于不锈钢外壳内， 并焊接进气管和出气管， 形成微粒捕集过 滤^ ¾置
PCT/CN2006/002092 2005-08-17 2006-08-17 A honeycomb ceramic particle-capturing filter carrier, a particle-capturing filter assembly and a particle-capturing filter device composed of the carriers, as well as the methods for making the same Ceased WO2007019801A1 (en)

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KR20080060221A (ko) 2008-07-01
US20080236123A1 (en) 2008-10-02
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CN100386150C (zh) 2008-05-07

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