CN109647088B - 一种低背压和高碳烟过滤效率柴油颗粒过滤器的制备方法 - Google Patents
一种低背压和高碳烟过滤效率柴油颗粒过滤器的制备方法 Download PDFInfo
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Abstract
本发明公开了一种低背压和高碳烟过滤效率的柴油颗粒过滤器制备方法。柴油颗粒过滤器采用蜂窝陶瓷壁流式载体,载体涂层是双层涂层结构;底层直接涂覆到载体形成,包括耐高温抗氧化的陶瓷粉末颗粒,形成多孔陶瓷薄膜,其中,底层孔隙率大于蜂窝陶瓷壁流式载体过滤壁的孔隙率;顶层涂覆具有催化氧化碳烟颗粒的催化材料,形成催化层直接与碳烟颗粒接触。本发明通过优化底层涂层结构的孔隙率和孔尺寸,以及优化顶层催化层的催化材料、涂层上载量,提高涂层对碳烟颗粒的过滤效率,同时降低DPF背压,增加碳烟颗粒在DPF过滤壁的表面沉积,进一步增加顶层催化涂层与碳烟颗粒的接触,从而加速碳烟颗粒的催化氧化脱除能力。
Description
技术领域
本发明属于机动车、船舶发动机尾气处理技术领域,特别涉及一种具有良好低背压,同时具有高碳烟过滤效率的柴油颗粒过滤器的制备技术。
背景技术
柴油机具有热效率高,经济性好的显著优点,但是也伴随着排放大量的碳烟颗粒物(Particulate Matter简称:PM)及NOx等对环境和人体健康造成严重危害的废气,随着各国法律法规对环保要求的加严,对NOx和PM的脱除成为必然的趋势,尤其是针对PM的脱除,采用壁流式蜂窝陶瓷颗粒过滤器(Diesel Particulate Filters简称:DPF)也已成为必然的选择。
在后处理净化系统中,DPF作为有效脱除PM的关键单元,能非常有效捕集PM,其捕集效率高达90%及以上,但是伴随着DPF前后压差急剧增加,发动机的运行效率受到显著影响,因此需要及时将捕集到的PM进行有效的去除,以便使整个后处理系统维持在一个较低的背压状态。
根据大量研究表明,DPF对碳烟颗粒的捕集,主要分为两个阶段,即第一个阶段,在碳烟颗粒捕集初期,大部分颗粒进入壁的内部,沉积在孔内,此阶段称为深层捕集,第二阶段,大量碳烟颗粒沉积到壁表面,称为表层捕集。在第一阶段内,随着捕集时间增加,捕集碳烟颗粒的量增加,背压成指数增加,随着进入第二阶段,背压随着碳烟捕集的增加,呈线性增加,这充分说明了,整个捕集系统背压的增加明显受到第一阶段碳烟捕集的影响,进一步分析,其原因是因为初始阶段大量的小尺寸的碳烟颗粒沉积到壁内孔中,导致堵塞,因此要解决此问题,则要求将碳烟颗粒捕集在壁表面,防止其进入壁的内孔之中。
发明内容
本发明根据现有技术的不足公开了一种具有低背压和高碳烟过滤效率的柴油颗粒过滤器制备方法。本发明要解决的问题是提供一种具有双涂层结构的碳烟颗粒过滤器,解决碳烟过滤器背压高,过滤效率低的问题,通过对底层涂层结构的优化,调控涂层孔隙率及孔径尺寸的分布,同时对顶层涂层的结构优化,制备得到一种具有低背压和高碳烟过滤效率的柴油颗粒过滤器,将更加有效地捕集碳烟颗粒,同时进行脱除。
本发明制备的具有低背压和高碳烟过滤效率的柴油颗粒过滤器,是一种具有两层涂层结构,底层未与气流直接接触,采用整体式涂覆工艺属于填充层,顶层属于催化层,与气流直接接触。
本发明通过以下技术方案实现:
一种具有低背压和高碳烟过滤效率的柴油颗粒过滤器制备方法,包括:
所述催化剂涂层在载体表面构成两层涂层结构;其中,载体表面是底层涂层,属于填充层;底层涂层表面是顶层涂层,属于催化层,与气流和碳烟颗粒直接接触;
所述底层涂层,包括耐高温抗氧化的陶瓷粉末颗粒及其混合物,至少包含碳化硅组成,不含贵金属;根据载体本身的孔径分布,按照平均孔径尺寸的1%~10%范围,优选陶瓷粉末颗粒尺寸,结合涂覆量,优化填充层的厚度,实现涂层孔隙率及孔径尺寸的调控;所述顶层涂层,则为催化层,由涂层材料和浸渍在涂层材料上的活性组分制成,顶层活性组分由含Pt和/或Pd贵金属盐制成,催化剂涂层中贵金属总含量为0.5~3.0g/ft3。
本发明通过合适的涂层结构设计,采用底层优先对过滤壁进行涂覆,形成一层多孔结构的薄膜,其孔隙率大于过滤壁孔隙率,一般大于60%,这主要目的是在阻止捕集的初始阶段,碳烟颗粒进入过滤壁的内孔中,导致背压增加,同时使碳烟颗粒集中捕集在过滤壁的表面,在增加对碳烟捕集效率的同时,也增加过滤壁与催化层的接触程度,从而加速碳烟颗粒的氧化脱除。
在涂覆顶层中,通过优选具有良好储氧能力的高含铈的储氧材料,同时负载少量的活性成分贵金属,贵金属包括Pt或/和Pd,将有效地提高碳烟颗粒的氧化脱除效率,进一步减小背压。
通过调整涂覆结构,优化底层涂层结构的孔隙率,优化顶层催化层,实现低背压,高过滤效率碳烟颗粒。
所述底层涂层材料为耐高温抗氧化的陶瓷粉末颗粒及其混合物,至少包含碳化硅;底层涂层材料的其他组分包含至少一种单相化合物,并与陶瓷粉末颗粒构成混合物;单相化合物包含但不限于氧化锆,二氧化硅,氧化钨,碳化氮,碳化钨,碳化钽,碳化铪,氮化硅,硼化硅,氮化硼,氧化铝等;
陶瓷粉末颗粒尺寸要求:100nm~1000nm,形貌为不规整的多边形。
其涂覆量为2.0~5.0g/L,厚度10μm~20μm,孔隙率大于60%。
所述顶层催化涂层,采用具有高储氧能力的高含铈催化材料,至少含二氧化铈,占顶层涂层质量含量≥80%,其他成分至少包含:氧化铝,氧化钨,二氧化硅,氧化镧,氧化钛,氧化钇,氧化银,氧化镨,氧化锶等中的一种或两种以上,其涂覆量要求10.0~30.0g/L,同时负载少量贵金属Pt和Pd,催化剂涂层中贵金属总含量为0.5~3.0g/ft3,增加催化层对碳烟颗粒的捕集效率和氧化脱除能力。
进一步本发明上述方法制备的颗粒过滤器,包括底层涂层涂覆和顶层涂层涂覆;催化剂涂层制备工艺包括底层涂层涂覆、和顶层涂层涂覆;
一、底层涂覆工艺具体如下:
1)制浆:
将重量比例是去离子水:冰醋酸:粘接剂=2:1:1的组分混合并采用高能球磨机球磨成胶,然后添加陶瓷颗粒和添加剂,添加剂质量含量占底层涂层总含量的1wt%,进行球磨。
添加剂是聚乙二醇、无机纤维素、玻璃纤维中任选取一种或两种。
2)涂覆:
采用整体式涂覆方法,由下至上灌浆涂覆,浆料灌入载体的高度,通过液面传感器进行识别,即当浆液面达到设定的高度时,通过传感器报警提示,此时,即可停止浆液的灌入;达到所需的涂层上载量即可,然后烘干干燥,焙烧后待用,焙烧温度:550℃~850℃。
二、顶层涂覆工艺具体如下:
1)制浆:
将重量比例是去离子水:冰醋酸:粘接剂=2:1:1的组分混合并采用高能球磨机球磨成胶,然后添加含活性组分的催化材料,活性组分为贵金属Pt和Pd,然后进行球磨。
2)涂覆:
采用整体式涂覆方法,由下至上灌浆涂覆,浆料灌入载体的高度,通过液面传感器进行识别,即当浆液面达到设定的高度时,通过传感器报警提示,此时,即可停止浆液的灌入;达到所需的涂层上载量即可,然后烘干干燥,焙烧即可,焙烧温度:450℃~650℃。
针对底层涂覆工艺具体包括:将重量比例是去离子水:冰醋酸:粘接剂=2:1:1的组分混合并采用高能球磨机球磨成胶,按重量要求,加入无机陶瓷粉末颗粒和添加剂,再经过充分球磨制成浆液形成底层涂层的浆液;
利用上灌浆方式,将浆液匀速缓慢的灌入到DPF之中,当达到设计的涂覆高度后,即停止灌浆。然后经过120℃,2h干燥,再进行550~850℃焙烧工艺,进行焙烧5h,即完成底层涂层的涂覆。
针对顶层涂层涂覆工艺具体包括:将重量比例是去离子水:冰醋酸:粘接剂=2:1:1的组分混合并采用高能球磨机球磨成胶,按重量要求,加入含贵金属活性成分的催化材料,再经过充分球磨制成浆液形成顶层涂层的浆液;
利用上灌浆方式,将浆液匀速缓慢的灌入到已经涂覆了底层涂层的DPF之中,当达到设计的涂覆高度后,即停止灌浆。然后经过120℃,2h干燥,再进行450~650℃焙烧工艺,进行焙烧3h,即完成顶层涂层的涂覆。
浆料灌入载体的高度,通过液面传感器进行识别,即当浆液面达到设定的高度时,通过传感器报警提示,此时,即可停止浆液的灌入。
顶层催化涂层上载量:10~30g/L,底层涂层上载量:2~5g/L。
本专利通过双层涂层结构设计,在碳烟颗粒捕集的初始阶段,将有效地阻止其进入过滤壁的内孔中,并集中地捕集在过滤壁的表面;为了解决双层涂层结构可能对背压造成进一步增加的影响,则对涂覆底层进行优良设计,即要求其孔隙率大于过滤壁本身的孔隙率,且要求孔分布比较均匀,进一步增加过滤壁对碳烟颗粒的过滤效率。
通过双涂层设计,在降低背压的情况下,增加了碳烟颗粒的效率,同时进一步增加碳烟颗粒与涂覆顶层催化层的接触程度,将有效加速碳烟颗粒的催化氧化,从而增加了DPF的被动再生效率,相应地减少碳烟颗粒的主动再生频次,也就减少了燃油的消耗。这对整个内燃机尾气后处理系统的成本降低,将有明显的影响。
本发明的效果是:
通过优化底层涂层结构的孔隙率和孔尺寸,以及优化顶层催化层的催化材料、涂层上载量,提高涂层对碳烟颗粒的过滤效率,同时降低DPF背压,增加碳烟颗粒在DPF过滤壁的表面沉积,进一步增加顶层催化涂层与碳烟颗粒的接触,从而加速碳烟颗粒的催化氧化脱除能力。
本发明通过调节底层涂层结构的孔隙率及孔隙尺寸,要求制备得到的催化剂涂层大于过滤壁的孔隙率,并通过优化涂层无机陶瓷颗粒的粒径,涂层含量等因素而实现。本发明设置底层涂层,降低了碳烟颗粒进入DPF过滤壁的内孔对孔的堵塞,降低DPF背压。
本发明通过调整底层涂层结构,优化顶层催化涂层催化材料,降低DPF过滤壁产生的背压,增加碳烟颗粒的捕集率,相应地增加顶层催化涂层与碳烟颗粒的接触程度,实现快速催化氧化,脱除碳烟颗粒的目的。
附图说明
图1为本发明制备涂覆后的DPF背压统计数据;纵坐标背压,单位:kPa;横坐标为时间,单位:min;
图2为本发明制备涂覆后的DPF对碳烟颗粒的捕集效率;纵坐标为捕集效率,单位:%;横坐标为时间,单位:min。
具体实施方式
下面结合具体实施方式对本发明进一步说明,具体实施方式是对本发明原理的进一步说明,不以任何方式限制本发明,与本发明相同或类似技术均没有超出本发明保护的范围。
以下实施例贵金属总量为3g/ft3,所用白载体是堇青石材料的蜂窝陶瓷载体(300目/in2),共计两层涂层,分为底层和顶层。
实施例1
具有低背压和高碳烟过滤效率的柴油颗粒过滤器制备技术,包括如下步骤:
一、底层浆液的配制:将重量比例是去离子水:冰醋酸:粘接剂=2:1:1的组分混合并采用高能球磨机球磨成胶,然后添加玻璃纤维,质量含量1.0wt%,以及碳化硅陶瓷粉末,其尺寸范围200~500nm,总固含量为5%,继续球磨30min。形成底层浆液。
二、底层浆液的涂覆:
采用整体式涂覆方法,由下至上灌浆涂覆,浆料灌入载体的高度,通过液面传感器进行识别,即当浆液面达到设定的高度时,通过传感器报警提示,此时,即可停止浆液的灌入;达到所需的涂层上载量即可,上载量要求3g/L。然后在120℃烘干干燥2h,在850℃下进行焙烧5h,即完成底层涂覆。
三、顶层浆液的配制:将重量比例是去离子水:冰醋酸:粘接剂=2:1:1的组分混合并采用高能球磨机球磨成胶,按重量要求,加入含贵金属活性成分的催化材料二氧化铈-二氧化镨复合氧化物,其中二氧化铈含90%,经过30min,充分球磨制成浆液形成顶层涂层的浆液;
四、顶层浆液的涂覆:
利用上灌浆方式,将浆液匀速缓慢的灌入到已经涂覆了底层涂层的DPF之中,当达到设计的涂覆高度后,即停止灌浆。然后经过120℃,2h干燥,再进行650℃焙烧工艺,进行焙烧3h,即完成顶层涂层的涂覆。
浆料灌入载体的高度,通过液面传感器进行识别,即当浆液面达到设定的高度时,通过传感器报警提示,此时,即可停止浆液的灌入。顶层催化涂层上载量:上载量20g/L。
检测例
本发明DPF背压检测方法具体如下:
根据本发明,制备催化单元样品,然后放在发动机上面,进行台架试验,样品规格:190.5*203.2/300cpsi,对催化单元样品开始台架试验后不同时间条件下的背压进行测试,同时测试没有涂层的DPF在相应空速下的背压,以进行对比。用压差传感器检测DPF前后端气流压力,采集压力。
捕集效率测试方法:在某固定的测试工况下,在DPF的后端采集碳烟颗粒的质量,然后根据碳烟减少量的百分比,进行计算。
得到如表1、、表2及图1和图2所示数据。
表1:不同时间,不同涂覆状态DPF背压统计表
5min | 20min | 40min | 60min | 80min | |
DPF-w/oWC | 1.58 | 4.2 | 5 | 6 | 7.3 |
DPF-w/SingleWC | 1.65 | 5.6 | 6.2 | 7.1 | 8.8 |
DPF-w/DoubleWC | 1.62 | 4.5 | 5.3 | 6.4 | 7.6 |
表2不同时间,不同涂覆状态DPF捕集效率统计表
5min | 10min | 15min | 20min | |
DPF-w/oWC | 58.99% | 73.31% | 84.03% | 95.78% |
DPF-w/SingleWC | 61.28% | 84.59% | 90.23% | 97.22% |
DPF-w/DoubleWC | 72.58% | 90.18% | 92.61% | 97.35% |
结果表明经过涂层设计改造后,采用双涂层设计方案涂覆DPF,在明显降低直接涂覆后背压的同时,加快了碳烟颗粒捕集能力,仅比没有经过涂覆的白载体背压略高。说明了采用本发明能实现降低涂覆后背压,同时提高碳烟颗粒的过滤效率。
Claims (5)
1.一种低背压和高碳烟过滤效率的柴油颗粒过滤器制备方法,其特征在于:所述柴油颗粒过滤器采用蜂窝陶瓷壁流式载体,载体涂层是双层涂层结构;
底层直接由包括耐高温抗氧化的陶瓷粉末颗粒制成的底层涂层材料涂覆到载体形成多孔陶瓷薄膜,其中,底层孔隙率大于蜂窝陶瓷壁流式载体过滤壁的孔隙率;底层涂层材料至少包括构成耐高温抗氧化陶瓷粉末颗粒的碳化硅;其中,底层涂层其涂覆量为2.0~5.0g/L,涂层厚度10μm~20μm,孔隙率大于60%,陶瓷粉末颗粒尺寸:100nm~1000nm,形貌为不规整的多边形;
顶层涂覆具有催化氧化碳烟颗粒的催化材料,形成催化层直接与碳烟颗粒接触。
2.根据权利要求1所述的低背压和高碳烟过滤效率的柴油颗粒过滤器制备方法,其特征在于:所述底层涂层材料还包含单相化合物,单相化合物与陶瓷粉末颗粒构成混合底层涂层材料;单相化合物是氧化锆、二氧化硅、氧化钨、碳化氮、碳化钨、碳化钽、碳化铪、氮化硅、硼化硅、氮化硼、氧化铝中的一种或多种的混合物。
3.根据权利要求1所述的低背压和高碳烟过滤效率的柴油颗粒过滤器制备方法:其特征在于:所述顶层催化涂层,包括具有高储氧能力的含铈催化材料,至少含二氧化铈,占顶层涂层质量含量≥80%;其他成分至少包含:氧化铝,氧化钨,二氧化硅,氧化镧,氧化钛,氧化钇,氧化银,氧化镨,氧化锶中的一种或两种以上;顶层涂覆量10.0~30.0g/L,顶层催化涂层负载贵金属Pt和Pd,贵金属总含量为0.5~3.0g/ft3。
4.根据权利要求1至3任一项所述的低背压和高碳烟过滤效率的柴油颗粒过滤器制备方法,其特征在于:包括底层涂层涂覆和顶层涂层涂覆;
一、底层涂覆工艺如下:
1)制浆:
将重量比例是去离子水:冰醋酸:粘接剂=2:1:1的组分混合并采用高能球磨机球磨成胶;然后添加陶瓷粉末颗粒和添加剂继续球磨,添加剂质量占底层涂层总质量的1wt%;
2)涂覆:
采用整体式涂覆方法,由下至上灌浆涂覆,浆料灌入载体的高度,通过液面传感器进行识别,即当浆液面达到设定的高度时,即停止浆液的灌入,上载量2~5g/L;然后烘干干燥,焙烧后待用,焙烧温度:550℃~850℃;
二、顶层涂覆工艺如下:
1)制浆:
将重量比例是去离子水:冰醋酸:粘接剂=2:1:1的组分混合并采用高能球磨机球磨成胶,然后添加含活性组分的催化材料,活性组分为贵金属Pt和Pd,然后进行球磨;
2)涂覆:
采用整体式涂覆方法,由下至上灌浆涂覆,浆料灌入载体的高度,通过液面传感器进行识别,即当浆液面达到设定的高度时,通过传感器报警提示,此时,即可停止浆液的灌入;上载量10~30g/L,然后烘干干燥,焙烧即可,焙烧温度:450℃~650℃。
5.根据权利要求4所述的低背压和高碳烟过滤效率的柴油颗粒过滤器制备方法,其特征在于:所述添加剂是聚乙二醇、无机纤维素、玻璃纤维中任选取一种或两种。
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