氢气纯化吸附材料研究进展

doi:10.16085/j.issn.1000-6613.2023-1691

摘要/Abstract

摘要：

氢能作为未来重要的能源组成，其来源具有多样性。其中工业制氢和副产氢过程通常会伴随多种杂质，如H₂O、CO₂、CO、N₂、烃类、硫化物等，而杂质对氢气的实际应用影响较大，因此对工业粗氢和副产氢进行纯化处理是满足各类合格用氢需求的关键环节。吸附分离是目前工业上最为常用的氢气纯化技术之一，其中吸附材料的性能直接影响分离效率和工艺操作成本，研发高性能、低成本吸附材料是吸附分离技术应用于氢气纯化的重点研究方向。本文简述了常见的氢气纯化技术及吸附分离机理，重点归纳总结了活性炭、沸石分子筛和金属有机骨架材料（MOFs）对氢气中所含CH₄、CO₂、CO杂质的吸附脱除行为，讨论了吸附材料性能优化的研究现状，总结了上述吸附材料在工业应用中的优缺点，并认为未来氢气纯化吸附材料的研究应在吸附机理和计算方面有所侧重。

关键词: 氢气纯化, 吸附材料, 活性炭, 沸石分子筛, 金属有机骨架

Abstract:

Hydrogen, as an important energy component in the future, has diverse sources. Industrial hydrogen production and by-product hydrogen processes often come with various impurities, such as H₂O, CO₂, CO, N₂, hydrocarbons, sulfides, etc. Impurities have a significant impact on the practical application of hydrogen gas. Therefore, purifying industrial crude hydrogen and by-product hydrogen is the key step in meeting various qualified hydrogen requirements. Adsorption separation is currently one of the most commonly used industrial hydrogen purification technologies, where the performance of adsorption materials directly affects separation efficiency and process operating costs. Developing high-performance and low-cost adsorption materials is the key research direction for the application of adsorption separation technology in hydrogen purification. This article briefly described common hydrogen purification technologies and adsorption separation mechanisms with a focus on summarizing the adsorption and removal behavior of CH₄, CO₂, and CO impurities in hydrogen by activated carbon, zeolite molecular sieves and metal-organic framework materials (MOFs). The research status of optimizing the performance of adsorption materials was discussed, and the advantages and disadvantages of the above adsorption materials in industrial applications were summarized. It was believed that research on hydrogen purification adsorption materials should focus on adsorption mechanisms and calculations.

Key words: hydrogen purification, adsorption materials, activated carbon, zeolites, metal-organic framework materials (MOFs)

中图分类号:

TQ42

苏士焜, 刘唐, 金也, 郑金玉. 氢气纯化吸附材料研究进展[J]. 化工进展, 2024, 43(10): 5612-5632.

SU Shikun, LIU Tang, JIN Ye, ZHENG Jinyu. Advances of adsorption materials for hydrogen purification[J]. Chemical Industry and Engineering Progress, 2024, 43(10): 5612-5632.

图/表 15

表1 部分工业粗氢的组成（质量分数）[4] ( 单位：%)

气源	H₂	CO	CO₂	CH₄	N₂	H₂O	其他
煤气化气	25~35	35~45	15~25	0.1~0.3	0.5~1	15~20	0.2~1
甲烷重整气	70~75	10~15	10~15	1~3	0.1~0.5	—	—
甲醇重整气	75~80	0.5~2	20~25	—	—	—	—
焦炉煤气	45~60	5~10	2~5	25~30	2~5	—	2.5~5
合成氨尾气	60~75	—	—	—	15~20	1~3	11~18
生物质气	25~35	30~40	10~15	10~20	1	—	0.5~2

表2 常见的氢气纯化方法[10]

方法	原理	典型进料气	产品氢纯度/%	技术难点
低温分离	相对挥发度的差别	石化废气，含氢在30%~80%内	90~98	不易得到高纯度氢气
聚合物膜分离	穿过膜的扩散速率差别	石化废气和氨吹扫气	92~98	He、CO₂、H₂O也可能会穿过膜
钯膜分离	氢气选择性渗透	任何含氢气体	≥99.999	硫化物和不饱和烃会削弱膜的渗透性
金属氢化物分离	氢与金属形成金属氢化物的可逆反应	氨吹扫气	99.999	O₂、CO、硫化物会使材料中毒
变压吸附	吸附剂选择性吸附杂质	任何富氢气体	99.999	吹扫气阶段有氢气损失，回收率相对较低

表3 氢气及主要杂质的物理性质[38]

气体名称	动力学直径/Å	极化率/Å³	偶极矩/Å	四极矩/Å²
H₂	2.83~2.90	0.8042	0	0.662
CH₄	3.76	2.593	0	0
CO₂	3.30	2.911	0	4.30
CO	3.69~3.76	1.950	0.11	2.50
N₂	3.64	1.740	0	1.52

图1 MOFs孔道结构及尺寸筛分效应示意图[44]

图2 量子筛效应及其对氢同位素的分离[48]

表4 用于吸附拟合常见的吸附模型[59-61]

吸附模型	模型表达式	参数及意义
Langmuir	$q = q m b p / (1 + b p)$	q为吸附量，q_m为最大吸附量，b为Langmuir平衡常数，p为压力
扩展Langmuir	$q i = q m i b i p i / (1 + ∑ j = 1 n b j p j)$	q_i 和p_i 为气体混合物吸附量和分压，q_m_i 、b_i 为纯组的对应方程拟合参数，j为混合物中各纯组分，n为混合物中的气体种类数
Toth	$q = q m b p / [1 + (b p) n] 1 / n$	q为吸附量，q_m为最大吸附量，b为Toth平衡常数，n是和吸附剂不均匀性相关的量纲为1参数，p为压力
扩展Toth	$q i = q m i b i p i 1 + ∑ j = 1 n (b j p j) t i 1 / t i$	q_i 和p_i 为气体混合物吸附量和分压，q_m_i 、b_i 、t_i 为纯组分i的对应方程拟合参数，j为混合物中各纯组分，n为混合物中的气体种类数
Virial	$p = q × e x p (2 S A q + 3 2 S 2 B q 2 + . . .) K H$	p为压力，q为吸附量，K_H为Henry常数，S为吸附剂比表面积，A、B为Virial系数

表4 用于吸附拟合常见的吸附模型[59-61]

吸附模型	模型表达式	参数及意义
Langmuir	$q = q m b p / (1 + b p)$	q为吸附量，q_m为最大吸附量，b为Langmuir平衡常数，p为压力
扩展Langmuir	$q i = q m i b i p i / (1 + ∑ j = 1 n b j p j)$	q_i 和p_i 为气体混合物吸附量和分压，q_m_i 、b_i 为纯组的对应方程拟合参数，j为混合物中各纯组分，n为混合物中的气体种类数
Toth	$q = q m b p / [1 + (b p) n] 1 / n$	q为吸附量，q_m为最大吸附量，b为Toth平衡常数，n是和吸附剂不均匀性相关的量纲为1参数，p为压力
扩展Toth	$q i = q m i b i p i 1 + ∑ j = 1 n (b j p j) t i 1 / t i$	q_i 和p_i 为气体混合物吸附量和分压，q_m_i 、b_i 、t_i 为纯组分i的对应方程拟合参数，j为混合物中各纯组分，n为混合物中的气体种类数
Virial	$p = q × e x p (2 S A q + 3 2 S 2 B q 2 + . . .) K H$	p为压力，q为吸附量，K_H为Henry常数，S为吸附剂比表面积，A、B为Virial系数

图3 活化前后样品的XPS谱图及铜改性前后活性炭的CO吸附量变化曲线

图4 LTA和FAU型沸石分子筛结构示意[92-93]

图5 X分子筛的SEM图和孔径分布图（从左至右依次为13X、LiX、LiPdAgX）[102]

表5 分子筛离子交换改性总结

交换离子	分子筛	交换条件	吸附气体	参考文献
碱金属离子	13X	0.5mol/L盐溶液，固液比1∶80，353K下反应4h	CO、CH₄、N₂	[96]
碱金属离子和H⁺	RHO	1mol/L盐溶液，固液比1∶10，353K下反应4h	CO₂	[97]
Na⁺、K⁺、Cs⁺、NH₄⁺、Ca²⁺、Mg²⁺、Ba²⁺	天然斜发沸石分子筛	2mol/L盐溶液，固液比1∶10，微沸下反应84h	CO、CH₄、O₂、N₂	[98]
碱金属离子	13X、NaY	1mol/L盐溶液，固液比1∶10，350K下反应5h	CO₂	[99]
Ca²⁺、Mg²⁺	13X	1mol/L盐溶液，固液比1∶10，353K微波下反应0.5h	CO、CH₄、CO₂、H₂	[100]
NH₄⁺、Li⁺、Cu²⁺	13X	1mol/L盐溶液，固液比1∶5，353K下反应4h	CH₄、CO₂、N₂	[101]
Li⁺、Pd²⁺、Ag⁺	13X	0.4mol/L的Li⁺溶液，343K下反应3h得到LiX；依次于 PdCl₂、AgNO₃、LiCl₂中交换得到LiPdAgX	CO₂	[102]

图6 CO2和CH4在不同分子筛上的吸附等温线和穿透曲线

图7 不同MOFs材料不同吸附压力下对CO2吸附的结构快照

图8 不同MOFs材料的结构示意图

表6 MOFs对H2及杂质的吸附数据

MOFs	吸附气体	吸附条件	吸附量/mmol·g^-1	选择性	参考文献
MOF-5	CO₂ CH₄ H₂	298K、4MPa	22.5 10 0.8	—	[116]
MOF-5	CH₄ H₂	300K、3MPa	9 0.58	—	[115]
MOF-74	CO₂ H₂ CO₂∶H₂=1∶4	313K、4MPa	13 2 —	— 380	[121]
MOF-74	CO₂∶H₂=1∶4 CH₄∶H₂=1∶1 CO₂∶CH₄∶H₂=4∶1∶20	313K、4MPa	—	380 15 300	[122]
Cu-BTC	CO₂ CH₄ CO H₂	308K、0.6MPa 308K、0.6MPa 303K、0.08MPa 303K、0.5MPa	9.2 3.1 0.65 0.41	—	[124]
Cu-TDPAT	CO₂∶H₂= 1:4 CH₄∶H₂= 1:1	298K、4MPa	12.5 8	80 —	[126]
UiO-66	CO₂；CO₂∶H₂= 3:7 CH₄；CH₄∶H₂=3:7 CO；CO∶H₂=3:7 H₂	298K、4MPa	8.2 6.7 5 1.4	100 18 12 —	[130]
UiO-66-Br	CO₂；CO₂∶H₂=3∶7 CH₄；CH₄∶H₂=3∶7 CO；CO∶H₂=3∶7 H₂	298K、4MPa	7 5 4.5 1.2	130 21 15 —	[130]
UTSA-16	CO₂ CH₄ CO H₂	298K、4MPa 298K、4MPa 298K、0.5MPa 298K、4MPa	4.9 2.4 0.9 0.5	— — —	[133]

图9 5A@MOF-74用于氢气纯化示意图及各材料吸附容量对比[139]

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