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2024 , Vol. 12 >Issue 4: 365 - 372

DOI: https://doi.org/10.3969/j.issn.2095-560X.2024.04.001

Selective Preparation of Aromatic Hydrocarbons by Catalytic Pyrolysis of Pine Wood with Fly Ash-Based HZSM-5

  • Chengbo ZHANG 1 ,
  • Xi LUO 2 ,
  • Qingxi QU 1 ,
  • Qi NIU 1 ,
  • Dan YAN 2 ,
  • Qiuhong ZHOU 2 ,
  • Kai LI , 1, † ,
  • Qiang LU 1
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  • 1. National Engineering Research Center of New Energy Power Generation, North China Electric Power University, Beijing 102206, China
  • 2. Changjiang Institute of Survey, Planning, Design and Research Co. Ltd., Wuhan 430010, China

Received date: 2024-03-04

  Revised date: 2024-04-02

Copyright

版权所有 © 《新能源进展》编辑部
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Abstract

Fly ash was utilized as a raw material to prepare fly ash-based HZSM-5 (FA-HZSM-5) catalysts by acid washing and alkali fusion pretreatment coupled with hydrothermal method. The catalysts were then applied to the catalytic pyrolysis of pine wood for the production of aromatics. The effects of pretreatment parameters such as hydrochloric acid concentrations and alkali/ash ratios on the physicochemical properties of FA-HZSM-5 were systematically investigated. Furthermore, the regulatory mechanisms of catalyst preparation conditions and pyrolysis process parameters on the selective preparation of aromatics were revealed. The results show that FA-HZSM-5 possessed a larger pore structure and mild acid strength than commercial HZSM-5. These characteristics were conducive to generating monocyclic aromatic hydrocarbons (MAHs) while significantly reducing the yields of polycyclic aromatic hydrocarbons (PAHs). When the hydrochloric acid concentration was 10%, the alkali/ash ratio was 1.5, the pyrolysis temperature was 650 °C, and the catalyst/pine ratio was 20, the maximum aromatics yield reached 10.82%. Among these, the MAHs yield was 7.65%, and the PAHs yield was 3.17%, reduced by 26.11% compared to the yield from catalytic pyrolysis using commercial HZSM-5.

Key words： fly ash; HZSM-5; pyrolysis; monocyclic aromatic hydrocarbons

Cite this article

Chengbo ZHANG , Xi LUO , Qingxi QU , Qi NIU , Dan YAN , Qiuhong ZHOU , Kai LI , Qiang LU . Selective Preparation of Aromatic Hydrocarbons by Catalytic Pyrolysis of Pine Wood with Fly Ash-Based HZSM-5[J]. Advances in New and Renewable Energy, 2024 , 12(4) : 365 -372 . DOI: 10.3969/j.issn.2095-560X.2024.04.001

0 引言

在碳中和背景下,生物质作为唯一一种可再生碳源,其高效转化利用受到广泛关注。通过热解/催化热解技术,可以将生物质定向转化成多种绿色燃料和化工原料,有利于减少化石能源的消耗[1,2]。苯、甲苯、二甲苯（benzene-toluene-xylene, BTX）等芳烃不仅是重要的化工原料,而且可以作为高密度液态有机氢载体,解决氢气储运难题[3,4]。因此,开发生物质催化热解选择性制备芳烃技术,不仅能够实现生物质的高值转化,而且有利于实现氢的绿色储运,降低储运成本,对实现“双碳”目标具有重要意义。
HZSM-5是一种硅酸铝沸石,因其独特的三维交叉孔道结构、合适的酸性以及与BTX动力学直径相近的孔径,对芳烃具有突出的择形效果,广泛应用于生物质热解选择性制备芳烃研究[5,6]。目前,商业HZSM-5主要采用纯度较高的硅源（如正硅酸乙酯、硅酸钠）、铝源（如偏铝酸钠、硫酸铝）等化工原料合成,制备成本较高,严重阻碍了其规模化工业应用[7,8]。飞灰是煤、生物质燃烧发电的残渣,作为世界上规模最大的工业固废,年产量达数十亿吨[9]。飞灰的主要成分为SiO2和Al2O3,和HZSM-5分子筛具有类似的化学组成,在合成HZSM-5分子筛方面极具发展潜力。这不仅可以降低HZSM-5的制备成本,而且可以拓宽飞灰的综合利用途径[10]。
然而,飞灰组分比较复杂,除玻璃体中可溶性的SiO2和Al2O3外,还含有大量的惰性硅铝组分（如莫来石、石英等晶体结构）以及少量的钙、铁等杂原子[11]。莫来石等物质稳定性较好,不仅难以作为活性硅铝源参与晶化过程,而且还会作为杂质掺杂在合成的分子筛中,影响其性能[12]。钙元素会在分子筛合成过程中与硅源发生反应形成硅酸钙,阻碍晶化过程,而铁元素则会直接掺入分子筛骨架,影响其晶体结构和色泽[13,14]。因此,如何对飞灰进行预处理,降低钙、铁等杂原子含量,将惰性硅铝组分转化成无定型SiO2和Al2O3,激发飞灰活性,是实现飞灰制备高品质HZSM-5的关键[12,15-16]。
基于此,本文耦合酸洗与碱熔对飞灰进行预处理,采用水热法制备系列飞灰基HZSM-5催化剂（FA-HZSM-5）,并应用于松木催化热解选择性制备芳烃。考察预处理过程中盐酸浓度、碱灰比对FA-HZSM-5理化特性的影响,探究预处理条件及热解工艺参数对热解产物分布的影响,优化催化剂制备方法,以期获得松木催化热解制备芳烃的最佳工况。

1 实验部分

1.1 实验原料及试剂

氢氧化钠（NaOH）、盐酸（HCl,36% ~ 38%）、氯化铵（NH4Cl）以及四丙基氢氧化铵（TPAOH,25%）购自国药集团。商业HZSM-5（CO-HZSM-5,硅铝比 = 25）购自南开大学催化剂有限公司。
实验所用飞灰来源于内蒙古某生物质电厂。飞灰呈黑色,经过球磨、筛分后,取粒径小于0.18 mm的颗粒置于105 ℃烘箱中干燥24 h,并保存于干燥皿中备用。原料的灰分、挥发分和固定碳按照《固体生物质燃料工业分析方法》（GB/T 28731-2012）进行分析,其含量分别为88.85%、3.93%和7.22%。采用电感耦合等离子体-原子发射光谱仪（electron- coupled plasma atomic emission spectrometry, ICP-AES）（美国,Agilent,Agilent725）对飞灰以及分子筛进行元素分析。飞灰的元素组成如表1所示,其硅含量较高,为29.20%,其次主要为Cl、K、Al、Ca、Fe等。
Table 1 The elemental composition of fly ash

表1 飞灰的元素组成

元素 含量/% 元素 含量/%
Si 29.20 S 1.51
Ca 1.94 P 1.01
Cl 5.35 Fe 1.61
K 4.94 Na 0.53
Al 4.25 F 0.32
Mg 0.59 Ti 0.27

1.2 催化剂的制备

将飞灰按固液比1∶20（g/mL）置于不同浓度（5%、10%、15%）的盐酸溶液中洗涤5 h,然后抽滤至中性并进行干燥,再将NaOH和酸洗飞灰按一定的碱灰比（1、1.5、2）混合均匀后置于马弗炉中,并以10 ℃/min的速率升温至700 ℃碱熔活化3 h。
向活化产物中加入去离子水,在80 ℃下搅拌6 h,随后离心取上清液备用。按SiO2、TPAOH、H2O摩尔比约1∶0.25∶80加入模板剂TPAOH,并调节pH至9.5 ~ 11,待形成凝胶后陈化12 h。将所得的凝胶装入高压反应釜中,在200 ℃下晶化12 h。依次对产物进行过滤、洗涤、干燥后,以10 ℃/min的速率升温至550 ℃保持6 h以去除模板剂,得到Na型ZSM-5。
将Na型ZSM-5置于2 mol/L的NH4Cl溶液中[固液比为1∶25（g/mL）],在80 ℃水浴2 h,并重复3次;最后以5 ℃/min的速率升温至550 ℃焙烧3 h,得到飞灰基HZSM-5,命名为FA-HZSM-5-x-y,其中x、y分别为盐酸浓度和碱灰比。

1.3 催化剂的表征

利用X射线衍射分析仪（X-ray diffraction, XRD）（德国,Bruker,D8 ADVANCE）、全自动气体吸附分析仪（美国,Micromeritics,ASAP 2460）和化学吸附分析仪（美国,Micromeritics,Autochem II 2920）等对催化剂的理化性质进行表征,重点分析其晶貌结构、孔结构特性和酸性质。

1.4 Py-GC/MS实验

采用微型热裂解仪（pyrolysis, Py）（美国,Agilent,CDS 5200HP）与气相色谱质谱联用仪（gas chromatography mass spectrometry, GC/MS）（美国,Agilent,Agilent 8860 + 5977B）耦合实验系统对松木热解产物进行分析。实验采用非原位催化热解模式。每次实验松木用量均为0.1 mg,催化剂用量按照不同催化剂/松木比（质量比为5、10、15、20、25）确定。热解温度分别为550、600、650、700 ℃,热解时间均为20 s。利用外标法确定芳烃产率。每次实验重复3次以保证结果可靠性。

2 结果讨论

2.1 催化剂表征结果

图1为FA-HZSM-5-10%-1.5和CO-HZSM-5的XRD谱图。由图可知,FA-HZSM-5-10%-1.5具有与CO-HZSM-5相似的衍射峰,在2θ = 7.94°、8.90°、23.00°、23.90° 和24.42° 均出现HZSM-5的特征衍射峰[17],且无明显杂晶峰出现,表明以飞灰为原料成功制备了具有较高结晶度的HZSM-5。在孔结构方面,FA-HZSM-5-10%-1.5与CO-HZSM-5的N2吸脱附等温曲线类型相似[图2（a）],均表现出混合的I型和IV型且都存在H4型滞后回线,表明两者都存在微孔和介孔结构[17,18]。CO-HZSM-5催化剂的比表面积和总孔容分别为299.41 m2/g和0.144 cm3/g,而FA-HZSM-5-10%-1.5的比表面积略有减小（253.63 m2/g）,但其总孔容较大（0.312 cm3/g）,是CO-HZSM-5孔容的2.17倍,这主要与FA-HZSM-5-10%-1.5中较多的介孔有关。如表2所示,CO-HZSM-5催化剂主要以微孔为主,微孔率达92.36%,而FA-HZSM-5-10%-1.5则含有较多的介孔,微孔率仅为20.83%,且平均孔径也较大。FA-HZSM-5-10%-1.5的平均孔径达4.91 nm,远高于CO-HZSM-5的1.93 nm。
Fig. 1 XRD patterns of CO-HZSM-5 and FA-HZSM-5-10%-1.5

图1 CO-HZSM-5和FA-HZSM-5-10%-1.5的XRD谱图

Fig. 2 N2 adsorption/desorption isotherms (a) and NH3-TPD patterns (b) of CO-HZSM-5 and FA-HZSM-5-10%-1.5

图2 CO-HZSM-5和FA-HZSM-5-10%-1.5的N2吸附-脱附曲线（a）和NH3-TPD谱图（b）

Table 2 The textural characteristics of CO-HZSM-5 and FA-HZSM-5-10%-1.5

表2 CO-HZSM-5和FA-HZSM-5-10%-1.5的孔结构参数

样品 比表面积/(m2/g) 微孔比表面积/(m2/g) 总孔容/(cm3/g) 微孔孔容/(cm3/g) 微孔率/% 平均孔径/nm
CO-HZSM-5 299.41 286.79 0.144 0.133 92.36 1.93
FA-HZSM-5-10%-1.5 253.63 124.60 0.312 0.065 20.83 4.91
图2 （b）为FA-HZSM-5-10%-1.5和CO-HZSM-5的氨程序升温脱附（NH3 temperature programmed desorption, NH3-TPD）谱图。氨气分子在两种催化剂上均有2个明显的解吸峰。解吸峰温度越高,催化剂酸性位点越强[19]。100 ~ 350 ℃的解吸峰对应Si-OH基团产生的弱酸性位点,而350 ~ 600 ℃的解吸峰对应Si-OH-Al基团产生的强酸性位点[20,21]。与CO-HZSM-5相比,FA-HZSM-5-10%-1.5的酸量显著降低,其中弱酸量从1 229.94 μmol/g降低至478.50 μmol/g,强酸量从780.27 μmol/g降低至343.70 μmol/g。HZSM-5的酸量通常与其硅铝比有关[22],硅铝比越低,酸性越强。元素分析结果表明FA-HZSM-5-10%-1.5的硅铝比为37,明显高于CO-HZSM-5的硅铝比。在以飞灰为原料制备FA-HZSM-5-10%-1.5的过程中,预处理阶段引入的酸液会造成一定的铝元素流失,晶化过程中部分硅铝元素会生成方钠石等其他沸石杂晶,从而提高了FA-HZSM-5-10%-1.5催化剂的有效硅铝比,降低了其酸性[17,23]。

2.2 催化剂制备条件对芳烃产率的影响

2.2.1 盐酸浓度
利用盐酸预处理可除去飞灰中的氧化铁、氧化钙等杂质,提升分子筛成品的质量与性能。以FA-HZSM-5-x-1.5为催化剂,在热解温度为650 ℃、催化剂/松木比为20的条件下开展松木催化热解实验,探究盐酸浓度对芳烃产率的影响,结果如图3所示。松木催化热解产物主要为5种芳烃,包括苯、甲苯、二甲苯等单环芳烃（monocyclic aromatic hydrocarbons, MAHs）和萘、甲基萘等多环芳烃（polycyclic aromatic hydrocarbons, PAHs）。当盐酸浓度为5%时,芳烃产率为7.35%;随着盐酸浓度提升至10%,芳烃产率达到最大,为10.82%,其中MAHs产率从5.52%增长至7.65%,PAHs产率从1.83%增长至3.17%。这归因于盐酸浓度过低时,氧化铁、氧化钙等碱性氧化物杂质的脱除不充分,残留的铁元素会阻碍晶化过程中硅铝元素的成键[24],而钙元素则会同硅铝酸盐反应形成硅铝酸钙产物,使获得的分子筛中有杂晶存在[17,25]。而进一步提高盐酸浓度至15%,芳烃产率则会降低,原因为当盐酸浓度过高时,酸会进一步同飞灰中的Al2O3反应,致使部分铝元素溶解流失,进而使所制备的FA-HZSM-5催化剂的硅铝比过高[17]。过高的硅铝比意味着分子筛酸性降低,不利于低聚、脱氢环化和芳构化等反应的发生,从而影响芳烃的生成[17,23]。
Fig. 3 Effects of hydrochloric acid concentrations on the yields of aromatics: (a) MAHs; (b) PAHs

图3 盐酸浓度对芳烃产率的影响：（a）单环芳烃;（b）多环芳烃

2.2.2 碱灰比
在碱熔过程中,NaOH可以活化飞灰中石英和莫来石等惰性组分,以提高分子筛的产率和纯度,因此NaOH用量（碱灰比）对FA-HZSM-5催化性能有着显著的影响。为探究碱灰比对芳烃产率的影响,在热解温度为650 ℃及催化剂/松木比为20的条件下,开展FA-HZSM-5-10%-y催化松木快速热解实验。芳烃产率分布如图4所示。随着碱灰比增加,芳烃产量呈现先增加后减小的趋势,当碱灰比为1.5时,所有芳烃产率均达到最大。此时,MAHs产率为7.65%,PAHs产率为3.17%。在碱熔过程中,NaOH可以削弱或破坏石英、莫来石晶相中SiO2和Al2O3之间的键结构。在键结构的断裂点处产生大量断层和自由端,引起颗粒运动,诱发热力学不稳定状态,进而形成可溶性无定形Si、Al和羟基方钠石[16]。同时,Na+ 还会在晶化过程中促进分子筛的成核和结晶[16]。当碱灰比较小时,飞灰中包含的大部分石英、莫来石等惰性物质不能转化成NaAlSiO4,且缺少Na+ 参与成核和结晶过程,不利于分子筛的制备[26,27];而碱灰比较大时,溶液碱性过高,会促进晶化过程中方钠石结构的形成,致使所得的FA-HZSM-5中包含方钠石等其他沸石杂晶[12]。
Fig. 4 Effects of alkali/ash ratios on the yields of aromatics: (a) MAHs; (b) PAHs

图4 碱灰比对芳烃产率的影响：（a）单环芳烃;（b）多环芳烃

2.3 热解条件对芳烃产率的影响

2.3.1 热解温度
为探究热解温度（550、600、650、700 ℃）对芳烃产物的影响,在催化剂/松木比为20时,以FA-HZSM-5-10%-1.5为催化剂开展松木催化热解实验,产物分布如图5所示。当热解温度从550 ℃升至650 ℃时,MAHs产率从4.71%增长至7.65%,PAHs产率从2.01%增长至3.17%。需要指出的是,MAHs产率增幅明显高于PAHs。其原因在于适当的高温不仅可以促进松木充分裂解产生较多的挥发性组分,还有利于酚类等中间产物通过脱氧反应转化为芳烃[28,29]。但进一步升高温度会致使热解产物发生二次裂解反应,生成一氧化碳和小分子碳氢化合物[30,31],最终导致芳烃产率下降。
Fig. 5 Effects of pyrolysis temperatures on the yields of aromatics: (a) MAHs; (b) PAHs

图5 热解温度对芳烃产率的影响：（a）单环芳烃;（b）多环芳烃

2.3.2 催化剂/松木比
以FA-HZSM-5-10%-1.5为催化剂,在热解温度为650 ℃时探究催化剂/松木比（5、10、15、20、25）对芳烃产物生成的影响,结果如图6所示。在催化剂/松木比为20时,芳烃产率达到最大为10.82%,而当催化剂/松木比为5和25时,芳烃产率分别降低至4.94%和9.80%。催化剂用量的增加可以提供更多的酸性位点,促进脱水、脱氧和脱羧等反应[32],有利于芳烃的生成。但当催化剂过量时,热解气分子在催化剂床层停留时间会延长,导致部分单环芳烃在分子筛孔道内进一步聚合、重组,产生焦炭、焦油等副产物[33]。同时,这些副产物也会使孔道发生堵塞,进一步降低催化效果。此外,催化剂用量过大还会增加催化剂投入,提高催化热解运行成本,不利于工业化应用。
Fig. 6 Effects of catalyst/pine ratios on the yields of aromatics: (a) MAHs; (b) PAHs

图6 催化剂/松木比对芳烃产率的影响：（a）单环芳烃;（b）多环芳烃

2.4 FA-HZSM-5与CO-HZSM-5催化效果对比

以FA-HZSM-5-10%-1.5和CO-HZSM-5为催化剂,分别在各自最佳工况下开展松木催化热解实验,并对芳烃产物分布进行对比,结果如图7所示。以CO-HZSM-5作为催化剂时,松木催化热解所得芳烃最大产率为11.79%,其中MAHs产率为7.50%,PAHs产率为4.29%。而以FA-HZSM-5-10%-1.5为催化剂时,芳烃最大产率则略有降低,为10.82%,但MAHs和PAHs产率变化不一,其中MAHs产率略增加至7.65%,而PAHs产率（3.17%）则降低了26.11%。这主要归因于FA-HZSM-5-10%-1.5较大的孔径有利于热解中间产物进入催化剂与活性位点接触,发生脱氧以及芳构化反应,形成芳烃,同时降低产物在孔道内的停留时间,避免其进一步反应形成焦炭[34];而其较弱的酸强度则避免了热解产物进一步发生开环、缩合和脱氢反应形成链状脂肪烃和积碳[35]。
Fig. 7 Effects of the catalyst type on the yields of aromatics: (a) MAHs; (b) PAHs

图7 催化剂种类对芳烃产率的影响：（a）单环芳烃;（b）多环芳烃

3 结论

以飞灰为原料制备了FA-HZSM-5催化剂,并将其用于生物质催化热解,实现了单环芳烃的选择性制备。酸洗和碱熔预处理能够有效脱除飞灰中的金属杂质,激发惰性硅铝组分活性,提升FA-HZSM-5的催化性能。当盐酸浓度为10%、碱灰比为1.5时,所制备的FA-HZSM-5-10%-1.5有利于松木热解选择性制备芳烃。在Py-GC/MS实验中,以FA-HZSM-5-10%-1.5为催化剂,当热解温度为650 ℃、催化剂/松木比为20时,芳烃产率最大为10.82%,其中MAHs产率为7.65%。相较于CO-HZSM-5,FA-HZSM-5-10%-1.5不仅促进了MAHs等芳烃产物的选择性制备,而且降低了PAHs的产率。

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