CN113769730A - 一种铯钒掺杂镧系金属的复合氧化物催化剂的制备方法 - Google Patents
一种铯钒掺杂镧系金属的复合氧化物催化剂的制备方法 Download PDFInfo
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Abstract
本发明提供了一种铯钒掺杂镧系金属的复合氧化物催化剂的制备方法,包括步骤S1:十一氧钒酸二铯(Cs2V4O11)粉末的准备;步骤S2:将镧系稀土金属硝酸盐加入去离子水中,搅拌,混合均匀,制成浓度为30%的溶液;步骤S3:将氧化铝和步骤S1准备的80~100g十一氧钒酸二铯(Cs2V4O11)粉末混合入步骤S2的10~20g硝酸盐溶液中,加入去30~80g的离子水搅拌,混合均匀;步骤S4:催化剂粉末的制成。本发明以碱金属掺杂镧系稀土金属的复合氧化物作为活性组分的非贵金属催化剂碳烟起燃温度低,最大碳烟燃烧温度低,催化剂具有高活性。
Description
技术领域
本发明属于降低柴油机尾气PM排放的催化剂制备技术领域,具体涉及一种铯钒掺杂镧系金属的复合氧化物催化剂的制备方法。
背景技术
目前,造成大气污染的主要污染物之一就是颗粒物,而移动源PM排放是城市大气颗粒物的最主要来源。随着世界各国排放法规限值的不断收紧,后处理技术成为研究热点。壁流式捕集器DPF是目前捕集柴油机颗粒效率最高,应用最为广泛的后处理技术之一。DPF虽然能高效捕集碳烟颗粒物,但是不能氧化颗粒物。随着捕集颗粒的增多,其背压增大,进一步导致发动机性能恶化。因此当颗粒物累积到一定水平之后,DPF需要再生,即氧化清除颗粒。
被动再生是DPF氧化碳烟颗粒的方式之一。柴油机的排气温度一般为150~400℃,而碳烟颗粒自发氧化的温度一般为550℃。通过催化剂降低碳烟的起燃温度,使碳烟在较低的排气温度下能自发地氧化燃烧,DPF完成被动再生。涂覆该种催化剂的催化器也被成为CDPF催化器。
贵金属催化剂Pt、Pd和Rh等是目前CDPF催化剂中性能较好,应用较多的催化剂,但是贵金属价格昂贵,并且容易生成硫酸盐,极易使催化剂发生硫中毒现象。
发明内容
为了克服现有技术的不足,本发明提供了一种铯钒掺杂镧系金属的复合氧化物催化剂的制备方法,该催化剂不包含贵金属,且具有高活性和高耐久性。
为实现上述目的,本发明提供的一种铯钒掺杂镧系金属的复合氧化物催化剂的制备方法,包括如下步骤:
步骤S1:十一氧钒酸二铯(Cs2V4O11)粉末的准备:首先通过将硫酸铯和硫酸氧钒加入去离子水中,制成十一氧钒酸二铯(Cs2V4O11)溶液,接着对溶液依次进行干燥、焙烧和粉碎,制成粒径2~1000μm的十一氧钒酸二铯(Cs2V4O11)微粒;
步骤S2:将镧系稀土金属硝酸盐加入去离子水中,搅拌,混合均匀,制成浓度为30%的溶液;
步骤S3:将氧化铝和步骤S1准备的80~100g十一氧钒酸二铯(Cs2V4O11)粉末混合入步骤S2的10~20g硝酸盐溶液中,加入去30~80g的离子水搅拌,混合均匀;
步骤S4:催化剂粉末的制成:将步骤S3准备的混合溶液依次进行干燥、焙烧和粉碎,制成粒径2~1000μm的催化剂微粒。
进一步地,步骤S1和步骤S4中烘干温度为100~120℃,烘干时间为3~6小时,焙烧温度为400~600℃,焙烧时间为1~6h。
进一步地,镧系稀土金属为镧、铈、镨、钕、钷、钐、铕、钆、铽、镝、钬、铒、铥和镱中的至少一种或多种。
本发明制备的催化剂的碳烟起燃温度低,最大氧化颗粒速率温度低,CO2选择性强,具有很高的活性。
附图说明
图1是一种铯钒掺杂镧系金属的复合氧化物催化剂的制备方法流程图;
图2是本发明实施例1 Cs-V-Ce(5%)的氧化活性曲线图;
图3是本发明实施例2 Cs-V-La(5%)的氧化活性曲线图;
图4是本发明实施例3 Cs-V-Ce(5%)-La(5%)的氧化活性曲线图;
图5是本发明对比例1 Cs-V的氧化活性曲线图。
具体实施方式
下面结合附图和实施例对本发明的技术方案作进一步说明。
实施例1 Cs-V-Ce
如图1所示,本发明提供了一种铯钒掺杂镧系金属的复合氧化物催化剂的制备方法,包括如下步骤:
步骤S1十一氧钒酸二铯(Cs2V4O11)粉末的准备:首先通过将硫酸铯和硫酸氧钒加入去离子水中,制成十一氧钒酸二铯(Cs2V4O11)溶液,接着对溶液依次进行干燥、焙烧和粉碎,制成粒径2~1000μm的十一氧钒酸二铯(Cs2V4O11)微粒;
步骤S2将硝酸铈加入去离子水中,搅拌,混合均匀,制成浓度为30%的溶液;
步骤S3将氧化铝和步骤S1准备的80~100g十一氧钒酸二铯(Cs2V4O11)粉末混合入步骤S2的10~20g硝酸铈溶液中,加入去30~80g的离子水搅拌,混合均匀;
步骤S4催化剂粉末的制成:将步骤S3准备的混合溶液依次进行干燥、焙烧和粉碎,制成粒径2~1000μm的催化剂微粒。
进一步地,所述步骤S1和步骤S4中烘干温度为100~120℃,烘干时间为3~6小时,焙烧温度为400~600℃,焙烧时间为1~6h。
图2所示,实施例1的催化剂其碳烟起燃温度为300℃,最大氧化颗粒速率温度为435℃,其CO2选择性为100%。
实施例2
本实施例掺杂的镧系稀土金属与实施例1不同,步骤S1经过与实施例1相同的制备工艺制成十一氧钒酸二铯(Cs2V4O11)微粒。
本实施例的掺杂元素为镧,步骤S2掺杂源选用硝酸镧,接着经过与实施例1相同的制备工艺制成粒径2~1000μm催化剂微粒。
图3所示,实施例2的催化剂其碳烟起燃温度为270℃,最大氧化颗粒速率温度为398℃,其CO2选择性为91%。
实施例3
本实施例掺杂的镧系稀土金属与实施例1和实施例2不同,步骤S1经过与实施例1和实施例2相同的制备工艺制成十一氧钒酸二铯(Cs2V4O11)微粒。
本实施例的掺杂元素为镧和铈,步骤S2掺杂源选用硝酸铈和硝酸镧,分别将硝酸铈和硝酸镧加入去离子水中,搅拌,混合均匀,分别制成浓度为30%的硝酸铈溶液和硝酸镧溶液;
步骤S3将氧化铝和步骤S1准备的80~100g十一氧钒酸二铯(Cs2V4O11)粉末混合入步骤S2的10~20g硝酸铈溶液和10~20g硝酸镧溶液的混合溶液中,加入去30~80g的离子水搅拌,混合均匀。接着经过与实施例1相同的制备工艺制成粒径2~1000μm催化剂微粒。
图4所示,实施例3的催化剂其碳烟起燃温度为350℃,最大氧化颗粒速率温度为430℃,其CO2选择性为80%。
对比例1
为了对比掺杂镧系金属元素后催化剂性能的改进,设置了本对比例1。
本对比例1的催化剂是通过与实施例1、实施例2和实施例3相同的制备工艺制成的2~1000μm十一氧钒酸二铯(Cs2V4O11)微粒。
图5所示,实施例4的催化剂其碳烟起燃温度为345℃,最大氧化颗粒速率温度为450℃,其CO2选择性接近100%。
因此,基于铯钒碱金属掺杂之后的实施例1、2和3,其碳烟起燃温度和最大氧化颗粒速率温度都有所降低,即掺杂后的活性都增加。在本发明所有实施例中优选的是实施例2,其碳烟起燃温度最低,最大氧化颗粒速率温度最低,且CO2选择性大于90%,具有最强的活性。
Claims (3)
1.一种铯钒掺杂镧系金属的复合氧化物催化剂的制备方法,其特征在于:包括如下步骤:
步骤S1:十一氧钒酸二铯(Cs2V4O11)粉末的准备:首先通过将硫酸铯和硫酸氧钒加入去离子水中,制成十一氧钒酸二铯(Cs2V4O11)溶液,接着对溶液依次进行干燥、焙烧和粉碎,制成粒径2~1000μm的十一氧钒酸二铯(Cs2V4O11)微粒;
步骤S2:将镧系稀土金属硝酸盐加入去离子水中,搅拌,混合均匀,制成浓度为30%的溶液;
步骤S3:将氧化铝和步骤S1准备的80~100g十一氧钒酸二铯(Cs2V4O11)粉末混合入步骤S2的10~20g硝酸盐溶液中,加入去30~80g的离子水搅拌,混合均匀;
步骤S4:催化剂粉末的制成:将步骤S3准备的混合溶液依次进行干燥、焙烧和粉碎,制成粒径2~1000μm的催化剂微粒。
2.根据权利要求1所述一种铯钒掺杂镧系金属的复合氧化物催化剂的制备方法,其特征在于:所述步骤S1和步骤S4中烘干温度为100~120℃,烘干时间为3~6小时,焙烧温度为400~600℃,焙烧时间为1~6h。
3.根据权利要求1所述一种铯钒掺杂镧系金属的复合氧化物催化剂的制备方法,其特征在于:所述镧系稀土金属为镧、铈、镨、钕、钷、钐、铕、钆、铽、镝、钬、铒、铥和镱中的至少一种或多种。
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