CN110496594A - 一种高分离系数一氧化碳吸附剂的制备方法及吸附剂 - Google Patents

一种高分离系数一氧化碳吸附剂的制备方法及吸附剂 Download PDF

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CN110496594A
CN110496594A CN201910905270.XA CN201910905270A CN110496594A CN 110496594 A CN110496594 A CN 110496594A CN 201910905270 A CN201910905270 A CN 201910905270A CN 110496594 A CN110496594 A CN 110496594A
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CN110496594B (zh
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王业勤
严莎
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Sichuan Yalian Hydrogen Energy Technology Co ltd
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Abstract

本发明提供一种高分离系数一氧化碳吸附剂的制备方法，属于一氧化碳吸附剂技术领域，氢气(氢能)净化领域。包括：1)将经过焙烧的水铝石与硝酸铝混合，充分研磨成超细粉；2)将上述步骤得到的细粉与沸石分子筛、柠檬酸、氯化亚铜、铁盐、田菁粉混合，充分研磨成超细粉；3)向上述混合料中加脱盐水搅拌，依次经成型、烘干脱水、还原活化后得到高分离系数一氧化碳吸附剂。本发明还提供利用所述方法制备得到的吸附剂。本发明制备得到的一氧化碳吸附剂可以显著提高CO与其它气体的分离系数，在吸附温度30℃，吸附压力1bar(a)时，CO/CO2的分离系数可达4.9～10，CH4、N2吸附量非常小，CH4＜0.8ml/g、N2＜0.2ml/g，几乎不吸附。

Description

一种高分离系数一氧化碳吸附剂的制备方法及吸附剂
技术领域
本发明属于一氧化碳吸附剂技术领域，同时也可用于氢气(氢能)净化领域，具体为一种高分离系数一氧化碳吸附剂的制备方法及吸附剂，也可以用于氢气中少量CO气体的脱除。
背景技术
CO是当今合成化工产品的重要原料，这些产品包括甲醇、甲醛、醋酸、醋酐、异氰酸酯、乙二醇、DMF、羰基合成、F-T合成、碳酸二甲酯、草酸二乙酯、乙二醇、DMF、羰基合成、FT合成、二甲基酰胺和农药除草剂等。随着C1化学应用技术的发展，CO在有机合成、低压羟基合成工艺中的重要作用将更加明显。
CO来源广泛，它可以来自天然气及石油的蒸汽转化或部分氧化制得的合成气，也可以来自炼铁高炉气、炼钢转炉气、电石炉气、合成氨装置的铜洗驰放气、水煤气和半水煤气等各种各样的富含CO的混合气。进行CO的化工利用，是变废为宝，变害为利的化工与环保相得益彰的重要途径。在众多的获得CO的途径中，变压吸附(PSA)以其工艺流程简单、投资省、成本低、CO产品纯度高等优点成为首选。但实现获得高纯度的CO的PSA工艺的关键是开发研制新型的高效CO吸附剂。
吸附剂的选择吸附性能好是分离过程可以顺利实现的基本条件。选择吸附剂的关键是组份之间的分离系数要尽可能大。分离系数是指在达到吸附平衡时，各组分之间的吸附量之比，分离系数越大，分离越容易。
目前燃料电池用的氢气对CO含量要求极高，根据《GB/T 37244质子交换膜燃料电池汽车用燃料氢气》国家标准要求，CO小于等于200ppb(v/v)，本发明可以用于氢气中脱除微量的CO，使其满足燃料电池用氢的要求。
发明内容
本发明的目的在于提供一种高分离系数一氧化碳吸附剂的制备方法及吸附剂，利用本发明制备方法制备得到的CO吸附剂可以从各种富含CO的工业尾气或工业废气中回收高纯度的CO；或者从含有少量CO的混合气体中脱除CO，以达到净化气体的目的。它具有吸附量大、效率高、与CO2分离系数高、与CH4、N2几乎不吸附、磨损低等优点。
本发明目的通过以下技术方案来实现：
一种高分离系数一氧化碳吸附剂的制备方法，包括以下步骤：
1)将经过焙烧的水铝石与硝酸铝混合，充分研磨成超细粉；
2)将上述步骤得到的细粉与沸石分子筛、柠檬酸、氯化亚铜、铁盐、田菁粉混合，充分研磨成超细粉；
3)向上述混合料中加脱盐水搅拌，依次经成型、烘干脱水、还原活化后得到高分离系数一氧化碳吸附剂。
进一步，步骤1)中，超细粉的粒径＜20μm；采用焙烧后的水铝石大多数以γ-Al2O3，活性高、比表面积大、分散性好；同时增加硝酸铝可以提高薄水铝石在成型过程中的粘结性。
进一步，步骤2)中，超细粉的粒径为＜30μm，进一步优选为＜10μm。
进一步，制备方法中，原料的加入量按质量百分比计为：沸石分子筛40％-55％，水铝石10％-15％，硝酸铝0.5％-2％，柠檬酸6-8％，氯化亚铜20％-30％，铁盐：0.5％-7％，田菁粉1％-2.5％。
进一步，所述铁盐为硝酸铁、硝酸亚铁，硫酸铁、硫酸亚铁，卤化铁，卤化亚铁中的一种或几种。
进一步，所述水铝石为薄水铝石或拟薄水铝石。
进一步，所述焙烧的水铝石为将水铝石在450-550℃马弗炉中焙烧4-6h。
进一步，所述还原活化所用还原气是CO或CO与H2的混合气体，还原温度为300-500℃，还原时间为4-8h。活化后，吸附剂性能达到最优。
一种高分离系数一氧化碳吸附剂，所述吸附剂采用上述制备方法制备得到。
与现有技术相比，本发明具有以下有益效果：
本发明提供一种高分离系数CO吸附剂，该吸附剂是基于π配位键吸附理论的一种Cu+的π络合吸附剂，具体说是利用热单层分散的方法对多孔介质上的单层或接近单层盐进行分散。
本发明吸附剂通过调整氯化亚铜或铁盐的质量百分比含量，可以调整CO/CO2的分离系数，使CO/CO2的分离系数达到3～10。
本发明制备得到的一氧化碳吸附剂可以显著提高CO与其它气体的分离系数，在吸附温度30℃，吸附压力1bar(a)时，CO/CO2的分离系数可达4.9～10，CH4、N2吸附量非常小，CH4＜0.8ml/g、N2＜0.2ml/g，几乎不吸附。
附图说明
图1为在30℃的吸附温度下，实施例1中CO吸附剂对气体的吸附等温线。
图2为在70℃的吸附温度下，实施例2中CO吸附剂对气体的吸附等温线。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。
实施例1
本实施例各原料及加入量如下：
HY分子筛42％、薄水铝石13.8％、九水硝酸铝0.5％、柠檬酸6％、氯化亚铜30％、硝酸亚铁6.2％、田菁粉1.5％。
具体制备方法如下：
1)将薄水铝石在500℃马弗炉中焙烧4h后，与九水硝酸铝混合，充分研磨成粒径＜20μm的超细粉；
2)将上述步骤得到的细粉与HY分子筛、柠檬酸、氯化亚铜、硝酸亚铁、田菁粉混合，放入球磨机中充分研磨成粒径＜20μm的超细粉；
3)向上述混合料中加入脱盐水搅拌，依次经成型、在80℃下烘干脱水、还原活化后得到高分离系数一氧化碳吸附剂。其中，还原活化的还原气为CO，还原温度为350℃，还原时间8h。
在30℃的吸附温度下，本实施例CO吸附剂对气体的吸附等温线如图1所示，在吸附压力1bar(a)时，气体的吸附量：CO 21.5ml/g，CO2 2.22ml/g，CH4 0.58ml/g，N2 0.11ml/g，CO与其他气体的分离系数比为：CO/CO2＝9.68；CO/N2＝195.5；CO/CH4＝37.07。
实施例2
本实施例各原料及加入量如下：
NaY分子筛45％、拟薄水铝石15％、九水硝酸铝0.6％、柠檬酸8％、氯化亚铜25％、氯化铁5.4％、田菁粉1％。
具体制备方法如下：
1)将拟薄水铝石在450℃马弗炉中焙烧6h后，与九水硝酸铝混合，充分研磨成粒径＜10μm的超细粉；
2)将上述步骤得到的细粉与NaY分子筛、柠檬酸、氯化亚铜、氯化铁、田菁粉混合，放入球磨机中充分研磨成粒径＜10μm的超细粉；
3)向上述混合料中加入脱盐水搅拌，依次经成型、在80℃温度下烘干脱水、还原活化后得到高分离系数一氧化碳吸附剂。其中，还原活化的还原气为CO和H2的混合气体(H2体积为5％)，还原温度为300℃，还原时间4h。
在70℃的吸附温度下，本实施例CO吸附剂对气体的吸附等温线如图2所示，当压力为1bar(a)时，气体的吸附量：CO 15.36ml/g，CO2 2.53ml/g，CH4 0.331ml/g，N2 0.041ml/g，CO与其他气体的分离系数比为：CO/CO2＝6.07；CO/N2＝347.6；CO/CH4＝46.4。
实施例3
本实施例各原料及加入量如下：
NaY分子筛51％、薄水铝石12.3％、九水硝酸铝1.65％、柠檬酸6.4％、氯化亚铜26％、硝酸铁1.65％、田菁粉1％。
具体制备方法如下：
1)将薄水铝石在550℃马弗炉中焙烧2h后，与九水硝酸铝混合，充分研磨成粒径＜10μm的超细粉；
2)将上述步骤得到的细粉与NaY分子筛、柠檬酸、氯化亚铜、硝酸铁、田菁粉混合，放入球磨机中充分研磨成粒径＜10μm的超细粉；
3)向上述混合料中加入脱盐水搅拌，依次经成型、在100℃下烘干脱水、还原活化后得到高分离系数一氧化碳吸附剂。其中，还原活化的还原气为CO，还原温度为400℃，还原时间4h。
在30℃的吸附温度下，在吸附压力1bar(a)时各气体的吸附量：CO 29.01ml/g，CO25.02ml/g，CH4 0.8ml/g，N2 0.2ml/g，与其他气体的分离系数比为：CO/CO2＝5.78；CO/N2＝145.1；CO/CH4＝36.3。
实施例4
本实施例各原料及加入量如下：
HY分子筛49％、拟薄水铝石12％、九水硝酸铝1.0％、柠檬酸6％、氯化亚铜24％、氯化铁7.0％、田菁粉1％。
具体制备方法如下：
1)将拟薄水铝石在450℃马弗炉中焙烧6h后，与九水硝酸铝混合，充分研磨成粒径＜10μm的超细粉；
2)将上述步骤得到的细粉与HY分子筛、柠檬酸、氯化亚铜、氯化铁、田菁粉混合，放入球磨机中充分研磨成粒径＜10μm的超细粉；
3)向上述混合料中加入脱盐水搅拌，依次经成型、在80℃温度下烘干脱水、还原活化后得到高分离系数一氧化碳吸附剂。其中，还原活化的还原气为CO和H2的混合气体(H2体积为5％)，还原温度为300℃，还原时间4h。
在70℃的吸附温度下，在吸附压力1bar(a)时各气体的吸附量：CO 20.50ml/g，CO23.02ml/g，CH4 0.43ml/g，N2 0.19ml/g，与其他气体的分离系数比为：CO/CO2＝6.79；CO/N2＝107.89；CO/CH4＝47.67。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。

Claims (7)

1.一种高分离系数一氧化碳吸附剂的制备方法，其特征在于，包括以下步骤：
1)将经过焙烧的水铝石与硝酸铝混合，充分研磨成超细粉；
2)将上述步骤得到的细粉与沸石分子筛、柠檬酸、氯化亚铜、铁盐、田菁粉混合，充分研磨成超细粉；
3)向上述混合料中加脱盐水搅拌，依次经成型、烘干脱水、还原活化后得到高分离系数一氧化碳吸附剂。
2.如权利要求1所述一种高分离系数一氧化碳吸附剂的制备方法，其特征在于，制备方法中，原料的加入量按质量百分比计为：沸石分子筛40％-55％，水铝石10％-15％，硝酸铝0.5％-2％，柠檬酸6％-8％，氯化亚铜20％-30％，铁盐：0.5％-7％，田菁粉1％-2.5％。
3.如权利要求1所述一种高分离系数一氧化碳吸附剂的制备方法，其特征在于，所述铁盐为硝酸铁、硝酸亚铁，硫酸铁、硫酸亚铁，卤化铁，卤化亚铁中的一种或几种。
4.如权利要求1所述一种高分离系数一氧化碳吸附剂的制备方法，其特征在于，所述水铝石为薄水铝石或拟薄水铝石。
5.如权利要求1所述一种高分离系数一氧化碳吸附剂的制备方法，其特征在于，所述焙烧的水铝石为将水铝石在450-550℃马弗炉中焙烧4-6h。
6.如权利要求1所述一种高分离系数一氧化碳吸附剂的制备方法，其特征在于，所述还原活化所用还原气是CO或CO与H2的混合气体，还原温度为300-500℃，还原时间为4-8h。
7.一种高分离系数一氧化碳吸附剂，其特征在于，所述吸附剂采用权利要求1至6任一项所述的制备方法制备得到。
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