VOCs在活性炭中的堆积：形成机制及影响因素

doi:10.16085/j.issn.1000-6613.2022-2376

摘要/Abstract

摘要：

活性炭吸附是含挥发性有机物（volatile organic compounds，VOCs）工业有机废气净化的有效方法。然而，在实际应用中常见吸附了VOCs的活性炭难以完全脱附，尤其是在净化含苯乙烯、丁二烯等成分的废气时甚至出现脱附后活性炭吸附容量大幅衰减的现象。本文评价近年来活性炭吸/脱附的研究进展，梳理活性炭吸附性能衰减的原因，识别活性炭孔隙堆积物种类和探讨堆积物的形成机制，以厘清影响堆积形成的关键因素。结果表明，被吸附的VOCs在活性炭循环吸/脱附过程中通过热解、偶联、聚合、热氧化反应及化学吸附等方式形成堆积物，堵塞孔道，堆积物可能是化学吸附物种、半焦/焦炭和聚合物；其中高吸附温度、低再生升温速率、高吹扫气流速、高沸点及动力学直径较大的VOCs和高微孔率的活性炭更易导致堆积形成；脱附温度、再生吹扫气含氧量、VOCs分子结构、活性炭表面官能团及无机成分对堆积的影响还未有定论。研究开发高效再生方法、活性炭定向制备与改性或是缓解堆积的技术途径。

关键词: 挥发性有机物, 活性炭, 堆积, 机制, 影响因素

Abstract:

Activated carbon adsorption is an efficient approach to the purification of industrial organic waste gases containing volatile organic compounds (VOCs). However, it is common that activated carbon adsorbed with VOCs is difficult to be completely desorbed, especially in the purification of exhaust gases containing styrene and butadiene, in which the adsorption capacity of activated carbon decreases significantly after desorption. This paper conducted a critical survey on the state-of-the-art of research on activated carbon adsorption/desorption in recent years, and then summarized the reasons for the decay of adsorption performance of activated carbon, identified the species in the heel substances, as well we discussed heel formation mechanism with aim to clarify the influencing factors. The results indicated that the adsorbed VOCs formed heel and block the pore through pyrolysis, coupling, polymerization, thermal oxidation reactions and chemisorption during the cyclic adsorption/desorption process of activated carbon. Heel may be chemisorbed species, semi-coke/coke and polymers. Factors including high adsorption temperatures, low regeneration heating rates, high purge gas flow rates, VOCs with high boiling points and large kinetic diameters and activated carbons with high microporosity may result in the heel formation; meanwhile, it was difficult to figure out the influence of desorption temperatures, oxygen impurities in desorption purge gas, molecular structure of VOCs, activated carbon surface oxygen groups and inorganic composition at present. More efficient regeneration methods, directional preparation and modification of activated carbon may be the technical ways to mitigate heel in activated carbon during VOCs purification.

Key words: VOCs, activated carbon, heel, mechanism, influencing factor

中图分类号:

X511

周红阳, 周逸寰, 张连秀, 梁鼎成, 解强. VOCs在活性炭中的堆积：形成机制及影响因素[J]. 化工进展, 2023, 42(11): 5969-5980.

ZHOU Hongyang, ZHOU Yihuan, ZHANG Lianxiu, LIANG Dingcheng, XIE Qiang. Heel of VOCs in activated carbon: Formation mechanism and influencing factors[J]. Chemical Industry and Engineering Progress, 2023, 42(11): 5969-5980.

图/表 5

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吸附质	吸附剂平均孔径或微孔率	结论	参考文献
苯酚、邻甲酚	GAC 2.48nm ACF 1.76nm/2.10nm	吸附质的低聚反应随着孔径增加而增加，多聚体的形成与吸附剂的孔径有关	[50]
邻甲酚、2-乙基苯酚（单一吸附质及二元吸附质）	GAC 1~50nm ACF 1.92nm/2.1nm/2.38nm/2.51nm	对于单一吸附质，ACF的孔径越小，吸附能力更高，而且不易发生低聚反应；对于二元吸附质，竞争吸附会导致ACF吸附位点减少，任一吸附质低聚反应均减少	[51]
苯酚、2-甲基苯酚、2-乙基苯酚（单一吸附质、二元及三元吸附质）	GAC 0.8~80nm ACF 0.8nm/1.28nm	对于三元吸附质，尽管单溶质和二元溶质系统会在ACF上发生低聚，但由于孔径较窄（12.8Å临界孔径，1Å=0.1nm），阻碍三元溶质系统发生低聚反应	[52]
2-甲基苯酚、2-硝基苯酚、2-氯苯酚（二元及三元吸附质）	GAC 0.4nm~80nm ACF 0.8nm/1.28nm	孔径范围较窄，临界孔径较大能有效阻碍低聚反应，但是低聚反应还与吸附剂的竞争吸附有关	[53]
DBT	PACS微孔率36.9%/30.2%/39.8%/31.3%	PACS的窄微孔有较高的吸附潜力，在解吸过程中，随着温度升高，DBT中的硫会与活性炭表面化学键结合，而且DBT会发生聚合反应形成聚合物难以从PACS中去除	[54]
苯酚、2-甲基苯酚、2-乙基苯酚	未经碱活化AC微孔率60.7% 碱活化AC微孔率52.8%/55.0%/64.9%/71.6%/72.4%	以烟煤为原料，KOH活化制备的微孔率较高，酸性官能团更多的活性炭能有效地阻止酚类化合物发生低聚	[55]
TMB	ACFC 0.6nm/0.7nm/0.86nm	孔径较小的ACFC 10经过再生循环后吸附容量降低83%，而孔径较大的ACFC 15和ACFC 20的吸附容量分别只有9%和5%的变化	[24]
苯、甲苯	AC 微孔率54%/74%/79%/80%/86%	窄微孔数量越多会降低活性炭循环再生效率	[56]
9种含有不同有机基团的化合物	AC 微孔率30%/43%/78%/88%/78%	孔隙堆积的形成与活性炭微孔体积成线性关系，即微孔体积越大，活性炭孔隙堆积量越多	[48]
TMB	AC 微孔率37.1%/85.5%/97.2%	微孔率最高的活性炭脱附过程产生的堆积量最多，而每个样品的中、大孔体积几乎保持不变	[43]

吸附质	吸附剂平均孔径或微孔率	结论	参考文献
苯酚、邻甲酚	GAC 2.48nm ACF 1.76nm/2.10nm	吸附质的低聚反应随着孔径增加而增加，多聚体的形成与吸附剂的孔径有关	[50]
邻甲酚、2-乙基苯酚（单一吸附质及二元吸附质）	GAC 1~50nm ACF 1.92nm/2.1nm/2.38nm/2.51nm	对于单一吸附质，ACF的孔径越小，吸附能力更高，而且不易发生低聚反应；对于二元吸附质，竞争吸附会导致ACF吸附位点减少，任一吸附质低聚反应均减少	[51]
苯酚、2-甲基苯酚、2-乙基苯酚（单一吸附质、二元及三元吸附质）	GAC 0.8~80nm ACF 0.8nm/1.28nm	对于三元吸附质，尽管单溶质和二元溶质系统会在ACF上发生低聚，但由于孔径较窄（12.8Å临界孔径，1Å=0.1nm），阻碍三元溶质系统发生低聚反应	[52]
2-甲基苯酚、2-硝基苯酚、2-氯苯酚（二元及三元吸附质）	GAC 0.4nm~80nm ACF 0.8nm/1.28nm	孔径范围较窄，临界孔径较大能有效阻碍低聚反应，但是低聚反应还与吸附剂的竞争吸附有关	[53]
DBT	PACS微孔率36.9%/30.2%/39.8%/31.3%	PACS的窄微孔有较高的吸附潜力，在解吸过程中，随着温度升高，DBT中的硫会与活性炭表面化学键结合，而且DBT会发生聚合反应形成聚合物难以从PACS中去除	[54]
苯酚、2-甲基苯酚、2-乙基苯酚	未经碱活化AC微孔率60.7% 碱活化AC微孔率52.8%/55.0%/64.9%/71.6%/72.4%	以烟煤为原料，KOH活化制备的微孔率较高，酸性官能团更多的活性炭能有效地阻止酚类化合物发生低聚	[55]
TMB	ACFC 0.6nm/0.7nm/0.86nm	孔径较小的ACFC 10经过再生循环后吸附容量降低83%，而孔径较大的ACFC 15和ACFC 20的吸附容量分别只有9%和5%的变化	[24]
苯、甲苯	AC 微孔率54%/74%/79%/80%/86%	窄微孔数量越多会降低活性炭循环再生效率	[56]
9种含有不同有机基团的化合物	AC 微孔率30%/43%/78%/88%/78%	孔隙堆积的形成与活性炭微孔体积成线性关系，即微孔体积越大，活性炭孔隙堆积量越多	[48]
TMB	AC 微孔率37.1%/85.5%/97.2%	微孔率最高的活性炭脱附过程产生的堆积量最多，而每个样品的中、大孔体积几乎保持不变	[43]

样品	吸附质	再生方法	结论	参考文献
AC	正十二烷	微波加热	微波加热对吸附剂完全再生时所需的最小能量是传导加热再生所需能量的6%	[38]
AC	甲基乙基酮	微波加热	吸附甲基乙基酮的活性炭经微波再生基本恢复吸附能力。在20次吸附/再生循环后，吸附容量从13.5g甲乙酮（MEK）/100g GAC降至12.5g MEK/100g GAC	[73]
AC	甲基乙基酮和甲苯	微波加热	在微波功率为600W的条件下，微波再生可在8min内去除大部分吸附质，去除率高达93.03%	[72]
SiC-AC	甲苯	微波加热	SiC-AC中掺杂了高导热材料碳化硅，提高了活性炭的导热性能，再生时可以均匀地分散微波辐射过程中的热量，甲苯可以快速解吸，减少堆积，节约能耗	[74]
PAC	CAP	超声	超声辅助解吸方法有效地恢复了中孔和大孔的体积和比表面积；超声过程中产生的HO·自由基也可能在PAC再生中发挥重要作用，但是再生PAC对吸附质分子的选择性显著降低	[75]
ACF	正己烷、甲基乙基酮和甲苯	超临界CO₂	在超临界CO₂再生实验中，较高压力更有利于再生，但在每个压力条件下的最佳操作温度为318K	[76]

样品	吸附质	再生方法	结论	参考文献
AC	正十二烷	微波加热	微波加热对吸附剂完全再生时所需的最小能量是传导加热再生所需能量的6%	[38]
AC	甲基乙基酮	微波加热	吸附甲基乙基酮的活性炭经微波再生基本恢复吸附能力。在20次吸附/再生循环后，吸附容量从13.5g甲乙酮（MEK）/100g GAC降至12.5g MEK/100g GAC	[73]
AC	甲基乙基酮和甲苯	微波加热	在微波功率为600W的条件下，微波再生可在8min内去除大部分吸附质，去除率高达93.03%	[72]
SiC-AC	甲苯	微波加热	SiC-AC中掺杂了高导热材料碳化硅，提高了活性炭的导热性能，再生时可以均匀地分散微波辐射过程中的热量，甲苯可以快速解吸，减少堆积，节约能耗	[74]
PAC	CAP	超声	超声辅助解吸方法有效地恢复了中孔和大孔的体积和比表面积；超声过程中产生的HO·自由基也可能在PAC再生中发挥重要作用，但是再生PAC对吸附质分子的选择性显著降低	[75]
ACF	正己烷、甲基乙基酮和甲苯	超临界CO₂	在超临界CO₂再生实验中，较高压力更有利于再生，但在每个压力条件下的最佳操作温度为318K	[76]

样品	改性剂	浓度	—COOH/mmol·g^-1	—COOR/mmol·g^-1	—OH/mmol·g^-1	参考文献
AC	HNO₃ （体积分数）	0	0.025	0.099	0.249	[83]
		20%	0.275	0.276	0.299
		40%	0.703	0.743	0.614
		80%	0.131	0.651	0.050
AC	HNO₃（mol/L）	0	0.25	0.6	0.45	[84]
		7	1.5	4.37	8.37	[84]
AC1	HNO₃（体积分数）	0	0.5036	0.0454	0.1037	[85]
		32.5%	1.5151	0.4265	0.5146
AC2		0	0.5097	0.1459	0.2144
		32.5%	1.7144	0.4406	0.5496
AC	HNO₃（体积分数）	0	0.08	0.29	—	[86]
		35%	0.47	0.09	0.02
		65%	0.58	0.18	0.02