CN113680360A - 一种多价态异质结铁基催化剂及其应用 - Google Patents
一种多价态异质结铁基催化剂及其应用 Download PDFInfo
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- 229910052742 iron Inorganic materials 0.000 title claims abstract description 40
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- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 12
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Abstract
本发明提供一种多价态异质结铁基催化剂及其应用，属于催化剂制备技术领域。所述多价态异质结铁基催化剂由以下质量份数的各组份组成：60~75份磁铁矿石粉作催化剂、15~20份纳米镁粉作还原剂、5~10份草木灰作加氢助剂、5~10份石英粉作助磨剂。该催化剂的原料成本低、制备方法简单、使用条件温和。使用时，经过一定浓度的氢气进行预活化，可以显著提高低碳烯烃的选择性和二氧化碳的转化率。
Description
技术领域
本发明属于催化剂制备技术领域，涉及一种铁基催化剂，具体涉及一种多价态异质结铁基催化剂及其应用。
背景技术
随着二氧化碳含量的不断升高，全球温室效应愈加显著。将二氧化碳加氢精制生产低碳烯烃等高质量化工产品，不仅可以减少二氧化碳排放，也为化工行业的可持续发展提供方案。由于二氧化碳直接加氢制低碳烯烃能垒较高，且低碳烯烃选择性差，副产品甲烷、一氧化碳等附加值低，经济效益差，需采用高效的催化剂。现有二氧化碳加氢制低碳烯烃一般采用逆水煤气变换结合费托合成路线（RWGS+FTS）和甲醇路线两种方案，所对应的催化剂分别为铁基催化剂和金属氧化物/沸石复合催化剂。但是，使用铁基催化剂时，产物中低碳烯烃的选择性差（＜58%）。虽然金属氧化物/沸石复合催化剂（如ZnO-ZrO2/SAPO-34）的低碳烯烃的选择性高（~80%），但二氧化碳转化率低（＜20%）。目前二氧化碳加氢催化剂普遍寿命短，对操作及设备要求高，能耗大，成本高。
发明内容
为了解决现有技术中的不足，本发明的目的一在于提供一种多价态异质结铁基催化剂，目的二在于提供所述多价态异质结铁基催化剂在二氧化碳加氢制备低碳烯烃方面的应用。本发明所述多价态异质结铁基催化剂原料成本低，制备方法简单，能显著提高低碳烯烃选择性以及二氧化碳转化率。
为了实现上述目的，本发明采用的具体方案如下：
一种多价态异质结铁基催化剂，包括以下质量份数的各组份：60~75份磁铁矿石粉、15~20份纳米镁粉、5~10份草木灰和5~10份石英粉；
所述多价态异质结铁基催化剂采用以下步骤制备而成：
1）在球磨罐中依次加入以下质量份数的物料：磁铁矿石粉60~75份、纳米镁粉15~20份、草木灰5~10份、石英粉5~10份，球磨罐中的磨球与物料的质量比为55:1~30:1；用氢气置换球磨罐中的空气，待球磨罐中的空气完全被氢气替代后，将球磨罐置于球磨机上球磨3~5小时，得粉体；
2）将步骤 1）得到的粉体置于压片机中进行冷压成型，冷压压强为250~300 MPa，破碎造粒后制得多价态异质结铁基催化剂。
作为对上述方案的进一步优化，所述磁铁矿石粉的粒度为200目以下。
作为对上述方案的进一步优化，所述镁粉的粒度为100 nm以下。
作为对上述方案的进一步优化，步骤 1）中的球磨气氛为氢气，球磨机的主轴转速为500~600 rpm。
作为对上述方案的进一步优化，步骤 2）中制得的多价态异质结铁基催化剂的粒径为 0.5~1 mm。
本发明另外还提供所述多价态异质结铁基催化剂在二氧化碳加氢制备低碳烯烃方面的应用。
本发明的有益效果主要表现如下：
在本发明所述多价态异质结铁基催化剂的原料组成中，磁铁矿石粉作催化剂、纳米镁粉作还原剂、草木灰作加氢助剂、石英粉作助磨剂，通过纳米镁粉将磁铁矿石粉在高能机械力作用下进行部分化学还原，通过助磨剂控制还原程度，形成含有多价态铁的粉体，经冷压成型、破碎造粒制备得到颗粒状的多价态异质结铁基催化剂。本发明利用机械力化学还原作用原理，以纳米镁粉为还原剂，将磁铁矿石粉在球磨过程中部分还原。高能机械力作用不仅可以减小颗粒尺寸、晶粒尺寸，而且可局部还原铁氧化物至多价态：如Fe3+、Fe2+、Fe0等，并产生氧空位缺陷。氧空位缺陷可作为陷阱位，高效捕获镁原子和K2CO3（草木灰），形成局域异质结构。用催化剂对二氧化碳加氢反应时，催化剂表面局域异质结构为二氧化碳分子提供活性位点，改变二氧化碳分子吸附结构，提高二氧化碳的转化率和低碳烯烃的选择性。
具体实施方式
下面将结合本发明实施例，对本发明技术方案进行清楚、完整地描述。
实施例1
一种二氧化碳加氢制取低碳烯烃的多价态异质结铁基催化剂，由以下质量份数的各组份组成：磁铁矿石粉60份、纳米镁粉20份、草木灰10份、石英粉10份。
所述磁铁矿石粉的粒度为200目以下。
所述镁粉的粒度均为100 nm以下。
一种二氧化碳加氢制取低碳烯烃的多价态异质结铁基催化剂，包括以下制备步骤：
1）在球磨罐中依次加入以下质量份数的物料：磁铁矿石粉60份、镁粉20份、草木灰10份、石英粉10份，球磨罐中的磨球与物料的质量比为55:1，然后用氢气置换球磨罐中的空气，待球磨罐中的空气完全被氢气替代后，将球磨罐置于球磨机上球磨5小时，球磨机的主轴转速为500 rpm，得粉体；
2）将步骤 1）得到的粉体置于压片机中进行冷压成型，冷压压强为300 MPa，破碎造粒后制得多价态异质结铁基催化剂。
步骤 1）中的球磨气氛为氢气。
步骤 2）中制得的多价态异质结铁基催化剂的粒径为0.5~1 mm。
对多价态异质结铁基催化剂产品进行如下试验：
将多价态异质结铁基催化剂装入连续操作的固定床反应器，加热至400 ℃，持续通入氢气4小时，气体流速50 ml/min，进行催化剂的活化。后调至温度320 ℃，压强1.0MPa，以氢碳比为3:1通入二氧化碳和氢气，气体流速二氧化碳：17.5 ml/min，氢气52.5 ml/min，氩气：10 ml/min。通过气相色谱法测得加氢后低碳烯烃的选择性为49.5%，二氧化碳转化率为21.3%。
实施例2
一种二氧化碳加氢制取低碳烯烃的多价态异质结铁基催化剂，由以下质量份数的各组份组成：磁铁矿石粉75份、纳米镁粉15份、草木灰5份、石英粉5份。
所述磁铁矿石粉的粒度为200目以下。
所述镁粉的粒度均为100 nm以下。
一种二氧化碳加氢制取低碳烯烃的多价态异质结铁基催化剂，包括以下制备步骤：
1）在球磨罐中依次加入以下质量份数的物料：磁铁矿石粉75份、镁粉15份、草木灰5份、石英粉5份，球磨罐中的磨球与物料的质量比为55:1，然后用氢气置换球磨罐中的空气，待球磨罐中的空气完全被氢气替代后，将球磨罐置于球磨机上球磨5小时，球磨机的主轴转速为500 rpm，得粉体；
2）将步骤 1）得到的粉体置于压片机中进行冷压成型，冷压压强为300 MPa，破碎造粒后制得多价态异质结铁基催化剂。
步骤 1）中的球磨气氛为氢气。
步骤 2）中制得的多价态异质结铁基催化剂的粒径为0.5~1 mm。
对多价态异质结铁基催化剂产品进行如下试验：
将多价态异质结铁基催化剂装入连续操作的固定床反应器，加热至400 ℃，持续通入氢气4小时，气体流速50 ml/min，进行催化剂的活化。后调至温度320 ℃，压强1.0MPa，以氢碳比为3:1通入二氧化碳和氢气，气体流速二氧化碳：17.5 ml/min，氢气52.5 ml/min，氩气：10 ml/min。通过气相色谱法测得加氢后低碳烯烃的选择性为50.6%，二氧化碳转化率为20.7%。
需要说明的是，以上所述的实施方案应理解为说明性的，而非限制本发明的保护范围，本发明的保护范围以权利要求书为准。对于本领域技术人员而言，在不背离本发明实质和范围的前提下，对本发明作出的一些非本质的改进和调整仍属于本发明的保护范围。
Claims (6)
1.一种多价态异质结铁基催化剂，其特征在于：包括以下质量份数的各组份：60~75份磁铁矿石粉、15~20份纳米镁粉、5~10份草木灰和5~10份石英粉；
所述多价态异质结铁基催化剂采用以下步骤制备而成：
1）在球磨罐中依次加入以下质量份数的物料：磁铁矿石粉60~75份、纳米镁粉15~20份、草木灰5~10份、石英粉5~10份，球磨罐中的磨球与物料的质量比为55:1~30:1；用氢气置换球磨罐中的空气，待球磨罐中的空气完全被氢气替代后，将球磨罐置于球磨机上球磨3~5小时，得粉体；
2）将步骤 1）得到的粉体置于压片机中进行冷压成型，冷压压强为250~300 MPa，破碎造粒后制得多价态异质结铁基催化剂。
2.根据权利要求1所述的多价态异质结铁基催化剂，其特征在于：所述磁铁矿石粉的粒度为200目以下。
3.根据权利要求1所述的多价态异质结铁基催化剂，其特征在于：所述镁粉的粒度为100 nm以下。
4.根据权利要求1所述的多价态异质结铁基催化剂，其特征在于：步骤 1）中的球磨气氛为氢气，球磨机的主轴转速为500~600 rpm。
5.根据权利要求1所述的多价态异质结铁基催化剂，其特征在于：步骤 2）中制得的多价态异质结铁基催化剂的粒径为 0.5~1 mm。
6.根据权利要求1-5任意一种所述的多价态异质结铁基催化剂在二氧化碳加氢制备低碳烯烃方面的应用。
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| CN112916020A (zh) * | 2019-12-06 | 2021-06-08 | 中国科学院大连化学物理研究所 | 用于二氧化碳加氢制高碳烃的铁基催化剂及其制备和应用 |
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| CN115475626B (zh) * | 2022-10-04 | 2023-11-17 | 中国石油大学(华东) | 一种二氧化碳加氢制备长链烃联产低碳烯烃的催化剂制备方法 |
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