CN111715024A - 用于燃料电池空气净化的吸附催化材料及其智能设计方法 - Google Patents
用于燃料电池空气净化的吸附催化材料及其智能设计方法 Download PDFInfo
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- CN111715024A CN111715024A CN202010523145.5A CN202010523145A CN111715024A CN 111715024 A CN111715024 A CN 111715024A CN 202010523145 A CN202010523145 A CN 202010523145A CN 111715024 A CN111715024 A CN 111715024A
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- fuel cell
- adsorption
- air purification
- molecular sieve
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Abstract
本发明公开了用于燃料电池空气净化的吸附催化材料及其智能设计方法。利用空气净化装置消除进气中大部分的悬浮颗粒物和有害气体,从而显著降低此类物质对PEMFC耐久性和性能的影响。本发明提供的第一种用于燃料电池空气净化的锰基吸附催化材料,包括一层Mn基催化剂层和两层分子筛层,形成三明治夹层结构,具有表面酸性位点和氧化还原位点的双活性中心。本发明提供的第二种用于燃料电池空气净化的锰基吸附催化材料,呈核壳纳米结构,有内至外分为三层;最外层及最内层均为分子筛层。中间层为Mn基催化剂层。本发明提出的锰基吸附催化材料,其能够有效提高对燃料电池进气中的污染物的吸附和传质扩散的效率。
Description
技术领域
本发明属于新能源汽车技术领域。具体涉及一种用于燃料电池空气净化的Mn基吸附催化材料,以及适用于该类型催化材料设计和性能调控的智能制备方法。
背景技术
在燃料电池领域,通过空气净化器的过滤、吸附、催化功能,持续稳定去除进气中的粉尘、氮氧化物、硫氧化物、挥发性有机物等多种污染物质,使进入燃料电池阴极的空气始终保持清洁,可大幅缓解由空气中的有害物质引起的电动势降低,有助于燃料电池长期保持较高的输出电压。考虑到内燃机汽车尾气中所含的多种污染物广泛存在于机动车道及周边区域的空气中,且车载燃料电池直接从外部环境获取发电所需的氧气,在实际运行过程中,进入燃料电池阴极的空气可能含有低浓度的固体颗粒物、NH3、SO2、O3、NO、NO2、VOCs、甲醛等多种污染物质混合的复合型污染物,因此,空气净化器能够实现污染物高效、稳定去除的关键在于研发对上述多种污染物都具有吸附催化活性,吸附容量大,使用寿命长的高效吸附催化材料。
在低浓度废气净化领域,以铂、钯、铑、银、钌等贵金属为活性组分的贵金属催化剂对大部分空气污染物都具有良好的催化活性,且由于其对NOx、VOCs等物质的催化效率显著而被广泛应用于汽车尾气净化器。但贵金属催化剂成本高,资源有限,无法大规模使用,且在废气中的含硫污染物可能导致催化剂中毒失活,因而贵金属催化剂在成本和使用寿命上并未达到燃料电池空气净化的要求。由高锰酸盐、碱盐、碱性氢氧化物、碱性氧化物等浸渍的改性活性炭、氧化铝、沸石分子筛等吸附材料具备吸附去除多种污染物分子的能力,具有成本低、吸附容量较高,适应性广的特点。然而这类吸附材料无法有效地分解污染物,当达到吸附饱和以后需及时更换滤料,长期使用易造成堵塞和压力损失,未被完全吸附的,以及温度升高时脱附的有害物质会进入燃料电池降低其电动势和工作效率。
专利申请号200480038752.1、专利名称燃料电池用空气的净化方法和装置及燃料电池提供了去除空气中硫化合物的吸附催化材料和过滤网层叠式净化过滤装置,该装置通过去除模拟进气中的硫化合物,使得其浓度在5ppb或以下,防止由硫化合物引起的电动势降低。由于该吸附催化材料只涉及含低浓度SO2的模拟废气,而实际空气中存在粉尘、CO、NOx、VOCs、O3等复合污染物,其是否适用于实际道路环境下的车载燃料电池仍待进一步论证。
专利申请号201910360520.6、专利名称一种新型氢燃料电池空气滤芯公布了包含颗粒物过滤层、吸附净化层、防炭灰过滤层的空气滤芯,并提供了构成所述吸附净化层的碳纳米纤维气凝胶的制备方法,但该方法所提供的该制备过程的详细数据可能建立在操作人员经验或有限的单因素实验的基础上,未充分考察制备过程所涉及的聚丙烯腈溶液浓度、石墨烯添加量、预氧化处理和碳化处理的温度等可能影响碳纳米纤维气凝胶吸附性能的关键制备条件的具体水平及其优化方案。
发明内容
本发明的目的在于提供一种用于燃料电池空气净化的Mn基吸附催化材料以及适用于该类型催化材料设计和性能调控的智能制备方法。
本发明提供的第一种用于燃料电池空气净化的锰基吸附催化材料,包括一层Mn基催化剂层和两层分子筛层,形成三明治夹层结构,具有表面酸性位点和氧化还原位点的双活性中心。
作为优选,用于燃料电池空气净化的锰基吸附催化材料中,Mn基催化剂层的负载量为10.5wt%,分子筛层的硅铝比为40,焙烧时间为6.3h,焙烧温度为490℃。
作为优选,所述的Mn基催化剂层采用α-MnO2、β-MnO2、γ-MnO2、MnO、Mn3O4、Mn2O3和Mn2O7中的一种或多种。
作为优选,所述的分子筛层采用纳米ZSM-5沸石分子筛晶粒组成的多级孔分子筛膜。多级孔孔径为2nm~50nm。
作为优选,所述多级孔ZSM-5分子筛层采用电泳法、两步变温水热法或二次水热法以长度为微米级、厚度为纳米级的片状Mn基催化剂为支撑体原位成膜。
作为优选,该用于燃料电池空气净化的吸附催化材料,负载在蜂窝陶瓷上。
用于燃料电池空气净化的吸附催化材料的设计方法如下:
步骤一、通过中心组合设计方法设计实验,以Mn基催化剂负载量、ZSM-5分子筛硅铝比、催化剂焙烧时间和焙烧温度作为关键参数,制定n组基础催化剂制备方案,30≤n≤50。
步骤二、根据中心组合设计方法给出的基础催化剂制备方案分别进行催化材料制备,并对制得的n种催化剂分别进行性能测试,得到n种催化剂的四个关键参数与其相对应的吸附催化效率所组成的基础实验数据集。
步骤三、以四个关键参数作为输入变量,吸附催化效率为输出变量,建立多层前馈神经网络。通过多层前馈神经网络得到四个关键参数与吸附催化效率的关系。
步骤四、采用遗传算法构建虚拟催化剂空间,以最大化吸附催化效率为优化目标,搜索虚拟催化剂空间,得到最大的吸附催化效率所对应的四个关键参数的数值。以所得的以Mn基催化剂负载量、ZSM-5分子筛硅铝比、催化剂焙烧时间和焙烧温度,进行吸附催化材料的制备。
本发明提供的第二种用于燃料电池空气净化的吸附催化材料,呈核壳纳米结构,有内至外分为三层;最外层及最内层均为分子筛层。中间层为Mn基催化剂层。
本发明具有的有益效果是:
1、本发明提出的ZSM-5@Mn@ZSM-5结构的吸附催化材料,其能够有效提高对燃料电池进气中的污染物的吸附和传质扩散的效率。
2、本发明上同时具备的表面酸性位点和氧化还原位点可按照不同的复合污染物物化性质进行调控,满足不同环境下的燃料电池近期的吸附催化要求。
3、本发明能够同步去除含有低浓度SO2、NO2、VOCs、O3、NH3、甲醛的复合废气,可时间长稳定吸附。
4、本发明的设计只需要少量的基础实验(30-50组)就可完成建模和预测,降低了材料开发成本,缩短了材料研发和测试周期。
5、本发明所提出的催化材料智能制备方法适应性广,可用于快速优化筛选其他多制备参数影响的催化材料。
附图说明
图1为本发明实施例1的结构示意图;
图2为本发明实施例2的结构示意图。
具体实施方式
以下结合附图对本发明作进一步说明。
实施例1
如图1所示,一种用于燃料电池空气净化的吸附催化材料,能够负载在蜂窝陶瓷上,呈片状纳米结构,包括一层Mn基催化剂层和两层分子筛层。分子筛层采用多级孔ZSM-5沸石分子筛。两层分子筛层分别设置在Mn基催化剂层的两侧,形成ZSM-5@Mn@ZSM-5的三明治夹层结构,具有表面酸性位点和氧化还原位点的双活性中心。
Mn基催化剂层采用不同晶型的MnO2(α-MnO2、β-MnO2、γ-MnO2)、MnO、Mn3O4、Mn2O3和Mn2O7中的一种或多种。多级孔ZSM-5分子筛的上的多级孔孔径介于微孔和介孔之间(即2nm~50nm)。多级孔ZSM-5分子筛层采用电泳法、两步变温水热法或二次水热法以Mn基催化剂为支撑体制备。Mn基催化剂的负载量为10.5wt%,多级孔ZSM-5分子筛的硅铝比(SiO2/Al2O3)为40,焙烧时间为6.3h,焙烧温度为490℃。
该用于燃料电池空气净化的吸附催化材料是通过基于多层前馈神经网络和遗传算法寻优(MLPNN-GA)的智能制备和模拟方法,研究Mn基材固有物化性质、制备工艺和活性组分负载量与材料吸附催化效率之间的关系,开发和筛选得到,其具体设计方法如下:
步骤一、通过响应面分析法(Response surface methodology,RSM)中的中心组合设计方法(Central composite design,CCD)设计实验,以Mn基催化剂负载量、ZSM-5分子筛硅铝比、催化剂焙烧时间和焙烧温度作为关键参数,制定n组基础催化剂制备方案;不同组基础催化剂制备方案的四个关键参数不完全相同。30≤n≤50。
步骤二、根据中心组合设计方法给出的基础催化剂制备方案分别进行催化材料制备(即按照设定的Mn基催化剂负载量、ZSM-5分子筛硅铝比、催化剂焙烧时间和焙烧温度制备出催化材料),并对制得的n种催化剂分别进行性能测试,得到n种催化剂的四个关键参数与其相对应的吸附催化效率所组成的基础实验数据集。
步骤三、以四个关键参数作为输入变量,吸附催化效率为输出变量,在Matlab平台建立基于上述数据集的多层前馈神经网络(Muhilayerperceptron neural network,MLPNN),并调整该多层前馈神经包括网络训练函数、隐层神经元数量、学习率在内的参数,使其达到期望的预测精度;多层前馈神经网络的调整过程属于现有技术,在此不做赘述。通过多层前馈神经网络得到四个关键参数与吸附催化效率的关系,即在基础实验数据集的基础上,获得不同关键参数对应的一种或多种污染物的吸附催化效率大小。
步骤四、采用Matlab优化工具箱中的遗传算法(Genetic algorithm,GA),设定并调整遗传算法的包括迭代次数、种群数量、搜索区域边界在内的参数,构建虚拟催化剂空间,以最大化吸附催化效率为优化目标,搜索虚拟催化剂空间,得到吸附催化效率最大的催化剂对应的四个关键参数的数值。
通过模拟实验,将所研发的Mn基催化剂负载于蜂窝陶瓷,分两层设置于柱状板式结构空气净化装置内,每层厚度2cm,直径16cm,前段设有过滤除尘,控制空气流量2500-3500L/min,温度25~100℃,进气为含有SO2、NO2、VOCs、O3、NH3、甲醛的复合污染物,各污染物浓度均控制在50ppb到1ppm之间,测试结果显示,所述Mn基吸附催化材料可实现SO2、NO2、VOCs、O3、甲醛脱除率≥95%,NH3脱除率≥80%,且稳定吸附1500h以上。通过改变作为输出变量的吸附催化效率对应的污染物类型,即可得到针对不同污染物的最佳制备条件,调控表面酸性位点和氧化还原位点,满足不同环境下的燃料电池近期的吸附催化要求。
本实施例涉及的智能制备方法通过对该催化材料制备过程的四个关键变量的精确调控,为多变量影响的吸附催化材料开发问题提供了一种可行的策略。该策略在本实施例中,通过对金属锰负载量的调控,避免了锰过量导致活性组分团聚现象的发生,也保证了该吸附催化材料不会因活性组分过少而出现催化活性降低的问题;通过对ZSM-5分子筛硅铝比的调控,使得所制备的分子筛膜具备晶粒小、孔道短、晶内扩散阻力小和比表面积大的特点,有利于反应物的扩散以及与催化剂氧化活性位点的直接接触;通过对焙烧温度和焙烧时间的调控,确保最后获得的锰基催化吸附材料在微观结构上主要呈现所期望的三明治核壳结构,减小无定型和其他结构催化剂的产出概率。该智能制备方法在上述变量呈连续非线性变化的条件下,找到了协调这些关键变量的值使得所制备的锰基催化材料接近或达到其最大吸附催化效率的平衡点。
实验验证所预测的吸附催化材料制备方案,以现有的Mn基负载分子筛催化剂(Mn/ZSM-5催化材料)、Ce、Cu、Fe等金属元素掺杂的M-Mn/ZSM-5催化材料、本实施例涉及的车载燃料电池的进气催化剂ZSM-5@Mn@ZSM-5进行对比试验如下:
使用本实施例涉及的进气催化剂ZSM-5@Mn@ZSM-5作为实验组;使用现有的Mn/ZSM-5催化材料作为第一对照组;使用Ce、Cu、Fe等金属元素掺杂的M-Mn/ZSM-5催化材料作为第二对照组;实验组、第一对照组和第二对照组中催化剂的质量相等。
试验条件为:各组催化剂均负载于统一规格的蜂窝陶瓷,分两层设置于柱状板式结构空气净化装置内,每层厚度2cm,直径16cm,净化器前段设有过滤除尘,输入的被处理废气中含有SO2、NO2、VOCs、O3、NH3、甲醛中的一种或多种污染物,污染物浓度均控制在50ppb到1ppm之间,进气流量2500-3500L/min,且温度控制在25℃~100℃的条件下;
对于第一对照组,现有的Mn/ZSM-5催化材料在吸附催化只含有一种污染物的单一废气时可实现甲醛、NH3、典型VOCs(如甲苯、苯乙烯等)90%左右的单独去除率,对NOx降解率可达90%到95%,但在SO2和H2O共同输入的情况下其对于NOx降解率降至70%左右;可见,现有的Mn/ZSM-5催化材料对含有多种污染物的混合废气净化效率不高;由于车载燃料电池直接从空气中收集气体,故气体中的污染物种类较多,属于混合废气,现有的Mn/ZSM-5催化材料对混合废气较低的净化效率会大大降低车载燃料电池的寿命。
对于第二对照组,Ce、Cu、Fe等金属元素掺杂的M-Mn/ZSM-5催化材料在处理混合废气时需要在300℃以上的条件下才能达到较高的活性,并且使用寿命无法满足燃料电池空气净化所要求的1500h。
对于实验组,本实施例涉及的车载燃料电池的进气催化剂ZSM-5@Mn@ZSM-5针对混合废气,可实现SO2、NO2、VOCs、O3、甲醛脱除率≥95%,NH3脱除率≥80%,PM10以下大气气溶胶脱除率≥99%,并且稳定吸附达1500h以上。因此,本实施例涉及的车载燃料电池的进气催化剂相比于现有的催化剂,具备更高的吸附催化效率,能够有效延长车载燃料电池的寿命。
实施例2
如图2所示,一种用于燃料电池空气净化的锰基吸附催化材料,能够负载在蜂窝陶瓷上,呈核壳纳米结构,有内至外分为三层;最外层及最内层均为分子筛层。中间层为Mn基催化剂层。Mn基催化剂层采用不同晶型的MnO2(α-MnO2、β-MnO2、γ-MnO2)、MnO、Mn3O4、Mn2O3和Mn2O7中的一种或多种。分子筛层采用多级孔ZSM-5沸石分子筛膜。多级孔ZSM-5分子筛的上的多级孔孔径介于微孔和介孔之间(即2nm~50nm)。多级孔ZSM-5分子筛膜采用电泳法、两步变温水热法或二次水热法以Mn基催化剂为支撑体制备。核壳结构的缺点在于其阻止了反应物与催化活性位点的直接接触而不利于催化活性的提高。与传统的微米级沸石不同,本实施例所涉及的沸石分子筛以纳米级的微孔沸石作为壳层,不仅能够锚定锰基催化剂纳米颗粒,且由于微孔沸石自身具有丰富孔道,可以保证脱附的污染物与活性组分直接接触而不降低催化活性,有助于提高非均相催化体系的传质和吸附催化效率。
Claims (8)
1.用于燃料电池空气净化的吸附催化材料,其特征在于:包括一层Mn基催化剂层和两层分子筛层,形成三明治夹层结构,具有表面酸性位点和氧化还原位点的双活性中心。
2.根据权利要求1所述的用于燃料电池空气净化的吸附催化材料,其特征在于:用于燃料电池空气净化的吸附催化材料中,Mn基催化剂层的负载量为10.5wt%,分子筛层的硅铝比为40,焙烧时间为6.3h,焙烧温度为490℃。
3.用于燃料电池空气净化的吸附催化材料,其特征在于:呈核壳纳米结构,有内至外分为三层;最外层及最内层均为分子筛层;中间层为Mn基催化剂层。
4.根据权利要求1或3所述的用于燃料电池空气净化的吸附催化材料,其特征在于:所述的Mn基催化剂层采用α-MnO2、β-MnO2、γ-MnO2、MnO、Mn3O4、Mn2O3和Mn2O7中的一种或多种。
5.根据权利要求1或3所述的用于燃料电池空气净化的吸附催化材料,其特征在于:所述的分子筛层采用纳米ZSM-5沸石分子筛晶粒组成的多级孔分子筛膜;多级孔孔径为2nm~50nm。
6.根据权利要求5所述的用于燃料电池空气净化的吸附催化材料,其特征在于:所述多级孔ZSM-5分子筛层采用电泳法、两步变温水热法或二次水热法以长度为微米级、厚度为纳米级的片状Mn基催化剂为支撑体原位成膜。
7.根据权利要求1或3所述的用于燃料电池空气净化的吸附催化材料,其特征在于:其负载在蜂窝陶瓷上。
8.如权利要求1所述的用于燃料电池空气净化的吸附催化材料的设计方法,其特征在于:步骤一、通过中心组合设计方法设计实验,以Mn基催化剂负载量、ZSM-5分子筛硅铝比、催化剂焙烧时间和焙烧温度作为关键参数,制定n组基础催化剂制备方案,30≤n≤50;
步骤二、根据中心组合设计方法给出的基础催化剂制备方案分别进行催化材料制备,并对制得的n种催化剂分别进行性能测试,得到n种催化剂的四个关键参数与其相对应的吸附催化效率所组成的基础实验数据集;
步骤三、以四个关键参数作为输入变量,吸附催化效率为输出变量,建立多层前馈神经网络;通过多层前馈神经网络得到四个关键参数与吸附催化效率的关系;
步骤四、采用遗传算法构建虚拟催化剂空间,以最大化吸附催化效率为优化目标,搜索虚拟催化剂空间,得到最大的吸附催化效率所对应的四个关键参数的数值;以所得的以Mn基催化剂负载量、ZSM-5分子筛硅铝比、催化剂焙烧时间和焙烧温度,进行吸附催化材料的制备。
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