磁性MgFe2O4及其核壳催化剂制备与煤热解性能研究

doi:10.11949/0438-1157.20220341

化工学报 ›› 2022, Vol. 73 ›› Issue (7): 3026-3037.DOI: 10.11949/0438-1157.20220341

• 催化、动力学与反应器 • 上一篇下一篇

磁性MgFe₂O₄及其核壳催化剂制备与煤热解性能研究

陈永安^1,²(),周安宁^1,²(),李云龙^1,³,石智伟^1,²,贺新福^1,²,焦卫红^1,²

^1.西安科技大学化学与化工学院，陕西西安 710054
^2.自然资源部煤炭资源勘探与综合利用重点实验室，陕西西安 710021
^3.陕西煤业化工集团神木天元化工有限公司，陕西榆林 719319

收稿日期:2022-03-06 修回日期:2022-04-24 出版日期:2022-07-05 发布日期:2022-08-01
通讯作者: 周安宁
作者简介:陈永安（1997—），男，硕士研究生， 2920452554@qq.com
基金资助:
陕西省煤炭联合基金项目(2019JPL-10)

Preparation and coal pyrolysis performance of magnetic MgFe₂O₄ and its core-shell catalysts

Yong’an CHEN^1,²(),Anning ZHOU^1,²(),Yunlong LI^1,³,Zhiwei SHI^1,²,Xinfu HE^1,²,Weihong JIAO^1,²

^1.School of Chemistry and Chemical Engineering, Xi’an University of Science and Technology, Xi’an 710054, Shaanxi, China
^2.Key Laboratory of Coal Resources Exploration and Comprehensive Utilization, MNR, Xi’an 710021, Shaanxi, China
^3.Shaanxi Coal Industry Chemical Group, Shenmu Tianyuan Chemical Co. , Yulin 719319, Shaanxi, China

Received:2022-03-06 Revised:2022-04-24 Online:2022-07-05 Published:2022-08-01
Contact: Anning ZHOU

摘要/Abstract

摘要：

采用溶胶-凝胶法制得MgFe₂O₄前体，经焙烧得到MgFe₂O₄催化剂，再经St?ber法制得核壳结构催化剂MgFe₂O₄@SiO₂和MgFe₂O₄@SiO₂@HZSM-5(MSH)，利用VSM、XRD、SEM、FT-IR、N₂物理吸附等手段研究了催化剂的磁性能和结构特征；在固定床反应器上，考察了N₂气氛下磁性催化剂对补连塔富油煤的催化热解特性及回收再生性能。结果表明：MgFe₂O₄为立方尖晶石结构，饱和磁化强度达到181.50 emu/g，具有良好热稳定性能。上述系列磁性催化剂均呈现出良好的催化活性，其中MSH催化活性最好。与非催化热解相比，MSH催化热解焦油产率提高了57.7%，焦油中脂肪烃和苯类含量增加约2倍，稠环芳烃含量下降8.6%~9.8%。采用磁选方法可有效实现催化剂回收，经700℃下焙烧处理，可实现回收催化剂的再生。SiO₂包覆有助于提高核壳结构催化剂的磁热稳定性和催化寿命。

关键词: 催化热解, 磁性MgFe₂O₄, 包覆, 焦油, 回收, 再生

Abstract:

The MgFe₂O₄ precursor was prepared by the sol-gel method, the MgFe₂O₄ catalyst was obtained by calcination, and the core-shell structure catalyst MgFe₂O₄@SiO₂ and MgFe₂O₄@SiO₂@HZSM-5 (MSH) were prepared by the St?ber method. The magnetic properties and structural characteristics of the catalysts were investigated by VSM, XRD, SEM, FT-IR, and N₂ physical adsorption. In a fixed bed reactor, under an N₂ atmosphere, the magnetic catalysts were investigated for the catalytic properties and recovery and regeneration of tar-rich coal from the Bulianta (BLT). The results show that the MgFe₂O₄ has a cubic spinel structure with a saturation magnetization of 181.50 emu/g and good thermal stability. The above series of magnetic catalysts all show good catalytic activity, among which MSH has the best catalytic activity. Compared with non-catalytic pyrolysis, the tar yield of MSH catalytic pyrolysis increased by 57.7%, the content of aliphatic hydrocarbons and benzene in the tar increased by about 2 times, and the content of polycyclic aromatic hydrocarbons decreased by 8.6%—9.8%. The magnetic separation method can effectively realize the recovery of the catalyst, and regeneration of the catalyst can be realized by roasting in 700℃. The SiO₂ coating helps to improve the magnetocaloric stability and catalytic lifetime of the core-shell catalyst.

Key words: catalytic pyrolysis, magnetic MgFe₂O₄, coating, tar, recovery, regeneration

中图分类号:

TQ 530.2

陈永安, 周安宁, 李云龙, 石智伟, 贺新福, 焦卫红. 磁性MgFe₂O₄及其核壳催化剂制备与煤热解性能研究[J]. 化工学报, 2022, 73(7): 3026-3037.

Yong’an CHEN, Anning ZHOU, Yunlong LI, Zhiwei SHI, Xinfu HE, Weihong JIAO. Preparation and coal pyrolysis performance of magnetic MgFe₂O₄ and its core-shell catalysts[J]. CIESC Journal, 2022, 73(7): 3026-3037.

图/表 13

表1 补连塔煤的工业分析与元素分析

Table 1 Proximate analysis and ultimate analysis of BLT-coal

Proximate analysis/%(mass，ad)				Ultimate analysis/%(mass，ad)
M	A	V	FC^①	C	H	N	S	O^①
9.58	4.4	30.42	55.6	82.42	5.16	1.23	0.26	10.93

图1 MgFe2O4系列催化剂制备流程

Fig.1 Preparation process of MgFe2O4 series catalyst

图2 实验装置

Fig.2 Experimental apparatus

图3 磁性催化剂催化热解回收再生过程概念流程图

Fig.3 Schematic diagram of magnetic catalyst catalytic pyrolysis recovery and regeneration process

图4 磁性催化剂的SEM图

Fig.4 SEM images of magnetic catalyst

图5 磁性催化剂的XRD谱图、 N2吸脱附等温曲线、FT-IR谱图和VSM磁化曲线

Fig.5 XRD patterns, N2 adsorption and desorption isotherm curve, FT-IR spectra and VSM magnetization curve of magnetic catalyst

表2 磁性催化剂的比表面积和孔结构参数

Table 2 Specific surface area and pore structure parameters of magnetic catalyst

催化剂	S_BET/(m²/g)	D_BJH/nm	V_total/(10^-2 cm³/g)
MgFe₂O₄	9.94	26.19	7.32
MgFe₂O₄@SiO₂	35.35	14.01	14.82
MSH	321.13	4.20	7.32

图6 MgFe2O4的XRD与VSM分析

Fig.6 XRD and VSM analysis of MgFe2O4

表3 磁性催化剂对热解产物分布的影响

Table 3 Effect of magnetic catalyst on distribution of pyrolysis products

催化剂	半焦产率/%	焦油产率/%	气体产率/%	水产率/%
none	68.13 65.76 64.94 65.67	9.42 14.25 12.16 14.86	16.19 14.46 16.73 14.82	6.26 5.53 6.17 4.61
MgFe₂O₄
MgFe₂O₄@SiO₂
MSH

表4 不同催化剂上BLT-coal热解焦油组分含量

Table 4 Content of BLT-coal pyrolysis tar on different catalysts

催化剂	苯类/%	酚类/%	脂肪烃类/%	稠环芳烃类/%	其他/%
none	1.37	18.04	12.85	34.22	33.52
MgFe₂O₄	4.18	18.58	18.28	28.67	30.29
MgFe₂O₄@SiO₂	4.02	18.21	17.98	28.91	30.88
MSH	4.12	17.84	23.53	25.63	29.88

图7 磁性催化剂催化热解机理① 煤常规裂解及油气内扩散过程;② 煤常规热解生成的自由基之间的缩聚脱氢形成半焦;③ 煤大分子界面催化裂解形成油气;④ 油气扩散与催化裂化反应形成轻质油及煤气;⑤ 裂解自由基二次缩聚形成半焦或在催化剂表面积炭

Fig.7 Catalytic pyrolysis mechanism of magnetic catalyst

图8 再生催化剂VSM磁化曲线

Fig.8 VSM magnetization curve of regenerated catalyst

表5 再生磁性催化剂对热解产物分布的影响

Table 5 Effect of recovery of magnetic catalyst on distribution of pyrolysis products

催化剂	半焦产率/%	焦油产率/%	气体产率/%	水产率/%
1R-MgFe₂O₄	65.97	13.23	14.98	5.82
1R-MgFe₂O₄@SiO₂	65.01	11.54	16.98	6.47
1R-MSH	66.63	13.08	15.12	5.17

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磁性MgFe₂O₄及其核壳催化剂制备与煤热解性能研究

Preparation and coal pyrolysis performance of magnetic MgFe₂O₄ and its core-shell catalysts

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