化工进展 ›› 2023, Vol. 42 ›› Issue (1): 236-246.DOI: 10.16085/j.issn.1000-6613.2022-0511
李攀1,2,3(), 王彪1,2,3, 徐骏浩1, 王贤华4, 胡俊豪1,2,3(), 宋建德2, 白净1,2,3, 常春1,2,3
收稿日期:
2022-03-29
修回日期:
2022-05-20
出版日期:
2023-01-25
发布日期:
2023-02-20
通讯作者:
胡俊豪
作者简介:
李攀(1987—),男,副教授,研究方向为生物质资源化利用。E-mail:lipanhust@163.com。
基金资助:
LI Pan1,2,3(), WANG Biao1,2,3, XU Junhao1, WANG Xianhua4, HU Junhao1,2,3(), SONG Jiande2, BAI Jing1,2,3, CHANG Chun1,2,3
Received:
2022-03-29
Revised:
2022-05-20
Online:
2023-01-25
Published:
2023-02-20
Contact:
HU Junhao
摘要:
生物质催化热解获得生物油等高质产品是最有前途替代传统化石能源的方法之一,但在热解过程中存在着严重的催化剂失活问题,其中积炭是导致催化剂失活的最主要因素。本文对近年来生物质催化热解领域的催化剂积炭问题进行综述,重点介绍催化剂积炭失活原因及表征方法、积炭的影响因素分析(催化剂结构、催化剂酸性与反应温度)、抑制催化剂积炭的方法(催化剂改性、高压反应条件等)以及积炭催化剂再生方法(氧化灼烧再生、臭氧低温再生、非热等离子体再生等),并介绍了近年来新兴的微波催化热解技术对催化剂积炭的抑制和消除作用,然后针对该领域目前所面临的困难和发展方向进行展望,以期为生物质催化热解过程中催化剂积炭问题研究提供理论基础。
中图分类号:
李攀, 王彪, 徐骏浩, 王贤华, 胡俊豪, 宋建德, 白净, 常春. 生物质热解催化剂积炭问题的研究进展[J]. 化工进展, 2023, 42(1): 236-246.
LI Pan, WANG Biao, XU Junhao, WANG Xianhua, HU Junhao, SONG Jiande, BAI Jing, CHANG Chun. Research progress on carbon deposition of catalysts for biomass pyrolysis[J]. Chemical Industry and Engineering Progress, 2023, 42(1): 236-246.
催化剂 | 生物质原料 | 处理方法 | 结论 | 参考文献 |
---|---|---|---|---|
ZSM-5 | 呋喃 | 催化热解 | 部分积炭具有催化活性为活性积炭,ZSM-5容易积炭 | [ |
多层纳米ZSM-5片,HZSM-5 | 纤维素 | 蒸汽热解 | 积炭沉积在催化剂的微孔阻碍活性位点,可以通过增加中孔降低失活率 | [ |
La、Pr、Ce、Y、Gd、Zr改性Ni | 木质纤维素 | 快速催化热解 | La改性Ni催化剂具有较大孔径、适度酸性和最佳的抗积炭性能 | [ |
ZSM-5 | 木质素 | 催化热解 | H2氛围中,催化剂积炭较少 | [ |
USY | 半纤维素 | 催化热解 | USY酸性较强,孔道狭窄易积炭,但在高压反应条件下促进物质扩散,减少积炭生成 | [ |
HZSM-5 | 柳枝稷和 聚乙烯 | 催化共热解 | 聚乙烯衍生的烃蒸气有助于减少积炭的形成,HZSM-5积炭严重,脱氧率高 | [ |
镍/渣(镁渣钢渣、高炉渣、 黄铁矿渣、硅酸钙渣) | 松锯末 | 热解催化重整 | 在催化剂测试中负载在镁渣上的镍活性最高,反应过程中生成石墨碳和无定形碳 | [ |
白云石 | 松木 | 催化热解 | 白云石不易积炭,但催化性能较弱,生物油等产品产率低 | [ |
碳基催化剂 | 纤维素 | 微波催化热解 | 微波与碳基催化剂的协同作用可以有效抑制积炭生成,但碳基催化剂本身易积炭失活 | [ |
整体式催化剂 | 牛粪 | 催化热解 | 积炭沉积在外表面,目标产物产率更高,催化剂回收、再生效率更高 | [ |
CoO、Cr2O3、CuO、Fe2O3、 Mn2O3、NiO、TiO2、V2O5和CeO2 | 白杨 | 催化热解 | 不同的金属氧化物,积炭行为不同,V-、Mn-、Cu-和Co-基容易形成积炭 | [ |
表1 生物质热解中催化剂积炭的研究
催化剂 | 生物质原料 | 处理方法 | 结论 | 参考文献 |
---|---|---|---|---|
ZSM-5 | 呋喃 | 催化热解 | 部分积炭具有催化活性为活性积炭,ZSM-5容易积炭 | [ |
多层纳米ZSM-5片,HZSM-5 | 纤维素 | 蒸汽热解 | 积炭沉积在催化剂的微孔阻碍活性位点,可以通过增加中孔降低失活率 | [ |
La、Pr、Ce、Y、Gd、Zr改性Ni | 木质纤维素 | 快速催化热解 | La改性Ni催化剂具有较大孔径、适度酸性和最佳的抗积炭性能 | [ |
ZSM-5 | 木质素 | 催化热解 | H2氛围中,催化剂积炭较少 | [ |
USY | 半纤维素 | 催化热解 | USY酸性较强,孔道狭窄易积炭,但在高压反应条件下促进物质扩散,减少积炭生成 | [ |
HZSM-5 | 柳枝稷和 聚乙烯 | 催化共热解 | 聚乙烯衍生的烃蒸气有助于减少积炭的形成,HZSM-5积炭严重,脱氧率高 | [ |
镍/渣(镁渣钢渣、高炉渣、 黄铁矿渣、硅酸钙渣) | 松锯末 | 热解催化重整 | 在催化剂测试中负载在镁渣上的镍活性最高,反应过程中生成石墨碳和无定形碳 | [ |
白云石 | 松木 | 催化热解 | 白云石不易积炭,但催化性能较弱,生物油等产品产率低 | [ |
碳基催化剂 | 纤维素 | 微波催化热解 | 微波与碳基催化剂的协同作用可以有效抑制积炭生成,但碳基催化剂本身易积炭失活 | [ |
整体式催化剂 | 牛粪 | 催化热解 | 积炭沉积在外表面,目标产物产率更高,催化剂回收、再生效率更高 | [ |
CoO、Cr2O3、CuO、Fe2O3、 Mn2O3、NiO、TiO2、V2O5和CeO2 | 白杨 | 催化热解 | 不同的金属氧化物,积炭行为不同,V-、Mn-、Cu-和Co-基容易形成积炭 | [ |
元素分析 | 积炭的碳、氢、硫、氮含量,氢碳原子比 |
---|---|
TGA | 积炭含量、类型 |
TGA+IR | 积炭分解情况 |
TPO | 积炭类型、部位 |
TEOM | 积炭失重动力学 |
IR、Raman | 积炭组成(脂肪碳、芳香碳), 酸中心失活情况 |
UV-Vis | 积炭组成(烯烃碳、碳正离子) |
FTIR | 积炭结构和组成 |
1H NMR | 积炭组成(脂肪碳、芳香碳) |
13C MAS NMR | 积炭组成(脂肪碳、芳香碳) |
ESR | 积炭组成、自由基信息 |
SEM、TEM | 积炭部分及分布 |
XPS | 积炭部分(表面)、形貌 |
XRD | 积炭晶形 |
索氏抽提+GC/MS | 可溶性积炭的化学组成 |
分子筛酸溶解法+GC/MS | 积炭的化学组成 |
液氮物理吸附+孔容分析 | 积炭部位(孔道内分布) |
表2 分子筛积炭表征方法[47]
元素分析 | 积炭的碳、氢、硫、氮含量,氢碳原子比 |
---|---|
TGA | 积炭含量、类型 |
TGA+IR | 积炭分解情况 |
TPO | 积炭类型、部位 |
TEOM | 积炭失重动力学 |
IR、Raman | 积炭组成(脂肪碳、芳香碳), 酸中心失活情况 |
UV-Vis | 积炭组成(烯烃碳、碳正离子) |
FTIR | 积炭结构和组成 |
1H NMR | 积炭组成(脂肪碳、芳香碳) |
13C MAS NMR | 积炭组成(脂肪碳、芳香碳) |
ESR | 积炭组成、自由基信息 |
SEM、TEM | 积炭部分及分布 |
XPS | 积炭部分(表面)、形貌 |
XRD | 积炭晶形 |
索氏抽提+GC/MS | 可溶性积炭的化学组成 |
分子筛酸溶解法+GC/MS | 积炭的化学组成 |
液氮物理吸附+孔容分析 | 积炭部位(孔道内分布) |
催化剂 | 原料 | 表征方法 | 结论 | 参考文献 |
---|---|---|---|---|
ZSM-5 | 呋喃 | 原位漫反射傅里叶变换红外光谱(DRIFTS) | 在呋喃热解中,活性积炭的主要成分是聚甲基苯甲醛 | [ |
Ni/HZSM-5 | 典型塑料 | 扫描电镜(SEM) | 失活催化剂表面粗糙、模糊,沟壑丛生,团聚现象明显 | [ |
Ni/MCM-41 | 木屑 | 透射电镜(TEM) | MCM-41具有长而有序的中孔结构,Ni颗粒均匀分散在MCM-41载体中 | [ |
Ni/CeO2-Al2O3 | 生物油/生物甘油混合物 | X射线衍射(XRD) | Ni呈现最强峰,贵金属的掺入没有影响催化剂尺寸;Ni/CeO2-Al2O3是更耐失活和积炭的催化剂 | [ |
Ni/La2O3-α-Al2O3 | 松木屑 | 氧化程序升温(TPO) | 沉积在Ni/La2O3-α-Al2O3的积炭主要有两种包封状积炭和丝状积炭 | [ |
Ni/ZSM-5,Ni/MCF,Ni/ZrO2 | 纤维素 | 热重分析(TG) | Ni/ZrO的积炭量比Ni/ZSM-5、Ni/MCF少两倍,积炭量最小。并在400~600℃时,大部分积炭被除去 | [ |
表3 生物质热解中催化剂积炭的表征方法
催化剂 | 原料 | 表征方法 | 结论 | 参考文献 |
---|---|---|---|---|
ZSM-5 | 呋喃 | 原位漫反射傅里叶变换红外光谱(DRIFTS) | 在呋喃热解中,活性积炭的主要成分是聚甲基苯甲醛 | [ |
Ni/HZSM-5 | 典型塑料 | 扫描电镜(SEM) | 失活催化剂表面粗糙、模糊,沟壑丛生,团聚现象明显 | [ |
Ni/MCM-41 | 木屑 | 透射电镜(TEM) | MCM-41具有长而有序的中孔结构,Ni颗粒均匀分散在MCM-41载体中 | [ |
Ni/CeO2-Al2O3 | 生物油/生物甘油混合物 | X射线衍射(XRD) | Ni呈现最强峰,贵金属的掺入没有影响催化剂尺寸;Ni/CeO2-Al2O3是更耐失活和积炭的催化剂 | [ |
Ni/La2O3-α-Al2O3 | 松木屑 | 氧化程序升温(TPO) | 沉积在Ni/La2O3-α-Al2O3的积炭主要有两种包封状积炭和丝状积炭 | [ |
Ni/ZSM-5,Ni/MCF,Ni/ZrO2 | 纤维素 | 热重分析(TG) | Ni/ZrO的积炭量比Ni/ZSM-5、Ni/MCF少两倍,积炭量最小。并在400~600℃时,大部分积炭被除去 | [ |
催化剂 | 生物质原料 | 处理方法 | 结论 | 参考文献 |
---|---|---|---|---|
ZrO2改性ZSM-5挤出物 | 橡木 | 热解和蒸汽升级催化 | 积炭沉积为蛋壳空间分布,起初积炭在B酸上形成,促进深度脱氧和裂解,然后积炭沉积在外表面,在ZrO2上形成更多富氢积炭 | [ |
Ni/La2O3-Al2O3、Ni/Al2O3和商业镍催化剂(G90-LDP) | 松木废料 | 热解催化重整 | 生成无定形积炭,La2O3使积炭气化,其碱性和吸水能力可抑制积炭生成 | [ |
Ni/镁渣和Ni/γ-Al2O3 | 松锯末 | 热解催化重整 | Ni/镁渣的积炭率、石墨化程度较低,抗积炭能力较强 | [ |
MCM-41/ZSM-5 | 纤维素、木质素和向日葵茎 | 生物油原位催化升级 | MCM-41作为积炭沉积的牺牲层降低了 ZSM-5的失活率 | [ |
Na、Mg、La改性Ni/SiO2 | 愈创木酚 | 蒸汽重整 | La改性Ni/SiO2催化剂后积炭量最低 | [ |
HZSM-5、Fe/ZSM-5、Ni/ZSM-5和FeNi/ZSM-5 | 软木锯末 | 热解和蒸汽升级催化 | 积炭形成取决于酸性位点强度和金属,FeNi/ZSM-5催化时产品的芳烃产率高,积炭量少 | [ |
酸脱铝、化学液相沉积改性ZSM-5 | 松锯末 | 热解催化重整 | 改性后催化剂积炭重要前驱体生成量减少40%左右,有效抑制积炭的生成 | [ |
化学液相沉积改性HZSM-5 | 竹子 | 微波催化热解 | 催化剂比表面积增加10%,积炭量明显减少 | [ |
HF脱铝HZSM-5 | 纤维素 | 快速催化热解 | 脱铝过程中布朗斯台德酸位点的减少,积炭量大幅减少,芳烃产率增加44.9% | [ |
碱洗HZSM-5减弱酸度、增加介孔结构 | 稻壳 | 微波催化热解 | 碱洗后,催化剂外表面强酸位点减少,内表面为弱酸环境,积炭生成量减少4.6% | [ |
CaO、碱洗HZSM-5 | 竹子和废旧轮胎 | 共热解 | 双重催化显著提升目标产物相对含量,并抑制因酸性过强而产生的积炭等不良产物 | [ |
表4 通过改性抑制催化剂积炭的方法
催化剂 | 生物质原料 | 处理方法 | 结论 | 参考文献 |
---|---|---|---|---|
ZrO2改性ZSM-5挤出物 | 橡木 | 热解和蒸汽升级催化 | 积炭沉积为蛋壳空间分布,起初积炭在B酸上形成,促进深度脱氧和裂解,然后积炭沉积在外表面,在ZrO2上形成更多富氢积炭 | [ |
Ni/La2O3-Al2O3、Ni/Al2O3和商业镍催化剂(G90-LDP) | 松木废料 | 热解催化重整 | 生成无定形积炭,La2O3使积炭气化,其碱性和吸水能力可抑制积炭生成 | [ |
Ni/镁渣和Ni/γ-Al2O3 | 松锯末 | 热解催化重整 | Ni/镁渣的积炭率、石墨化程度较低,抗积炭能力较强 | [ |
MCM-41/ZSM-5 | 纤维素、木质素和向日葵茎 | 生物油原位催化升级 | MCM-41作为积炭沉积的牺牲层降低了 ZSM-5的失活率 | [ |
Na、Mg、La改性Ni/SiO2 | 愈创木酚 | 蒸汽重整 | La改性Ni/SiO2催化剂后积炭量最低 | [ |
HZSM-5、Fe/ZSM-5、Ni/ZSM-5和FeNi/ZSM-5 | 软木锯末 | 热解和蒸汽升级催化 | 积炭形成取决于酸性位点强度和金属,FeNi/ZSM-5催化时产品的芳烃产率高,积炭量少 | [ |
酸脱铝、化学液相沉积改性ZSM-5 | 松锯末 | 热解催化重整 | 改性后催化剂积炭重要前驱体生成量减少40%左右,有效抑制积炭的生成 | [ |
化学液相沉积改性HZSM-5 | 竹子 | 微波催化热解 | 催化剂比表面积增加10%,积炭量明显减少 | [ |
HF脱铝HZSM-5 | 纤维素 | 快速催化热解 | 脱铝过程中布朗斯台德酸位点的减少,积炭量大幅减少,芳烃产率增加44.9% | [ |
碱洗HZSM-5减弱酸度、增加介孔结构 | 稻壳 | 微波催化热解 | 碱洗后,催化剂外表面强酸位点减少,内表面为弱酸环境,积炭生成量减少4.6% | [ |
CaO、碱洗HZSM-5 | 竹子和废旧轮胎 | 共热解 | 双重催化显著提升目标产物相对含量,并抑制因酸性过强而产生的积炭等不良产物 | [ |
催化剂 | 再生方法 | 结论 | 参考文献 |
---|---|---|---|
ZSM-5 | 臭氧低温再生 | 失活催化剂上几乎97.4%的积炭完全去除;催化剂骨架保持良好 | [ |
工业废弃催化剂 | 溶剂萃取方法 | 可在低温下有效除去催化剂孔道中的积炭,再生活性高 | [ |
Pt-Sn/γ-Al2O3 | 氢气、氮气吹扫 | 氢气再生,去除积炭的低密度组分,积炭流动性更高,活性位点可及性更强 | [ |
MnO x -CeO2 | NO2氛围灼烧 | 积炭在350~400℃时被除去,比常规空气灼烧再生低200℃左右 | [ |
BaZr/Fe | CO2氛围灼烧 | 催化剂内部和表面的积炭被部分去除,再生的催化剂恢复部分活性,稳定性较好 | [ |
沸石催化剂 | 非热等离子体再生 | 低能量的非热等离子体在293K温度下实现催化剂完全再生,去除积炭 | [ |
表5 催化剂积炭失活常用的再生方法
催化剂 | 再生方法 | 结论 | 参考文献 |
---|---|---|---|
ZSM-5 | 臭氧低温再生 | 失活催化剂上几乎97.4%的积炭完全去除;催化剂骨架保持良好 | [ |
工业废弃催化剂 | 溶剂萃取方法 | 可在低温下有效除去催化剂孔道中的积炭,再生活性高 | [ |
Pt-Sn/γ-Al2O3 | 氢气、氮气吹扫 | 氢气再生,去除积炭的低密度组分,积炭流动性更高,活性位点可及性更强 | [ |
MnO x -CeO2 | NO2氛围灼烧 | 积炭在350~400℃时被除去,比常规空气灼烧再生低200℃左右 | [ |
BaZr/Fe | CO2氛围灼烧 | 催化剂内部和表面的积炭被部分去除,再生的催化剂恢复部分活性,稳定性较好 | [ |
沸石催化剂 | 非热等离子体再生 | 低能量的非热等离子体在293K温度下实现催化剂完全再生,去除积炭 | [ |
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