化工进展 ›› 2021, Vol. 40 ›› Issue (2): 890-900.DOI: 10.16085/j.issn.1000-6613.2020-0584
汪佩华1(), 秦志峰1,2,3(), 吴琼笑4, 李聪明1, 苗茂谦1, 常丽萍1, 孙鹏程2, 曾剑2, 王立华2, 谢克昌1
收稿日期:
2020-04-14
修回日期:
2020-06-15
出版日期:
2021-02-05
发布日期:
2021-02-09
通讯作者:
秦志峰
作者简介:
汪佩华(1995—),男,硕士研究生,研究方向为工业催化。E-mail:基金资助:
Peihua WANG1(), Zhifeng QIN1,2,3(), Qiongxiao WU4, Congming LI1, Maoqian MIAO1, Liping CHANG1, Pengcheng SUN2, Jian ZENG2, Lihua WANG2, Kechang XIE1
Received:
2020-04-14
Revised:
2020-06-15
Online:
2021-02-05
Published:
2021-02-09
Contact:
Zhifeng QIN
摘要:
采用分步浸渍法制备了不同磷添加方式改性的NiMo/Al2O3催化剂,在固定床微反装置上考察了该系列催化剂对焦炉煤气中噻吩加氢脱硫(HDS)性能的影响,采用BET、X射线衍射(XRD)、H2程序升温还原(H2-TPR)、NH3程序升温脱附(NH3-TPD)、C4H4S(H2)程序升温脱附[C4H4S(H2)-TPD]、X射线光电子能谱(XPS)、高清透射电镜(HRTEM)和拉曼(Raman)等分析手段对催化剂进行表征。结果表明,不同磷添加方式制备NiMo/Al2O3催化剂的HDS性能存在较大差异。其中,催化剂PNi-Mo/Al和PMo-Ni/Al表面弱吸附解离活性位增强,对焦炉煤气中噻吩有较好的低温加氢脱硫活性,以含292.5mg/m3噻吩的模拟焦炉煤气为原料时,PNi-Mo/Al在250℃下对噻吩的脱硫率达61%。对于PNi-Mo/Al和PMo-Ni/Al催化剂,先浸渍P、Ni或者P、Mo时,P优先和载体Al2O3作用,减弱了活性金属组分Ni、Mo与载体间的相互作用,而又防止Ni或者Mo与载体间相互作用过低而聚集,提高了Ni、Mo在载体表面的均匀分散,生成能够促进硫化形成Ⅱ型活性相Ni-Mo-S的NiMoO4物种。NiMoO4和MoO3之间的协同作用提高了催化剂的硫化度,使HDS活性得以提高。
中图分类号:
汪佩华, 秦志峰, 吴琼笑, 李聪明, 苗茂谦, 常丽萍, 孙鹏程, 曾剑, 王立华, 谢克昌. 磷添加方式对NiMo/Al2O3催化剂加氢脱硫性能的影响[J]. 化工进展, 2021, 40(2): 890-900.
Peihua WANG, Zhifeng QIN, Qiongxiao WU, Congming LI, Maoqian MIAO, Liping CHANG, Pengcheng SUN, Jian ZENG, Lihua WANG, Kechang XIE. Effect of phosphorus adding manners on the performance of NiMo/Al2O3 catalyst in hydrodesulfurization[J]. Chemical Industry and Engineering Progress, 2021, 40(2): 890-900.
气体组分 | 体积分数/% | 气体组分 | 体积分数/% |
---|---|---|---|
H2 | 57.46 | N2 | 3.95 |
CO | 6.90 | O2 | 0.48 |
CO2 | 2.99 | CnHm | 2.42 |
CH4 | 25.80 | C4H4S | 438.75mg/m3 |
表1 模拟焦炉煤气气氛组成
气体组分 | 体积分数/% | 气体组分 | 体积分数/% |
---|---|---|---|
H2 | 57.46 | N2 | 3.95 |
CO | 6.90 | O2 | 0.48 |
CO2 | 2.99 | CnHm | 2.42 |
CH4 | 25.80 | C4H4S | 438.75mg/m3 |
样品 | 各组分质量分数/% | 比表面积 /m2·g-1 | 孔体积 /cm3·g-1 | 孔径 /nm | ||
---|---|---|---|---|---|---|
MoO3 | NiO | P | ||||
γ-Al2O3 | — | — | — | 212 | 0.39 | 7.91 |
P/Al | 0 | 0 | 1 | 181 | 0.36 | 7.58 |
PNi/Al | 0 | 5 | 1 | 181 | 0.34 | 7.58 |
PMo/Al | 15 | 0 | 1 | 185 | 0.34 | 7.93 |
P-NiMo/Al | 15 | 5 | 1 | 139 | 0.36 | 8.06 |
PNi-Mo/Al | 15 | 5 | 1 | 126 | 0.31 | 8.97 |
PMo-Ni/Al | 15 | 5 | 1 | 144 | 0.29 | 8.07 |
NiMo-P/Al | 15 | 5 | 1 | 161 | 0.30 | 7.84 |
NiMoP/Al | 15 | 5 | 1 | 179 | 0.31 | 7.36 |
表2 催化剂物理性能
样品 | 各组分质量分数/% | 比表面积 /m2·g-1 | 孔体积 /cm3·g-1 | 孔径 /nm | ||
---|---|---|---|---|---|---|
MoO3 | NiO | P | ||||
γ-Al2O3 | — | — | — | 212 | 0.39 | 7.91 |
P/Al | 0 | 0 | 1 | 181 | 0.36 | 7.58 |
PNi/Al | 0 | 5 | 1 | 181 | 0.34 | 7.58 |
PMo/Al | 15 | 0 | 1 | 185 | 0.34 | 7.93 |
P-NiMo/Al | 15 | 5 | 1 | 139 | 0.36 | 8.06 |
PNi-Mo/Al | 15 | 5 | 1 | 126 | 0.31 | 8.97 |
PMo-Ni/Al | 15 | 5 | 1 | 144 | 0.29 | 8.07 |
NiMo-P/Al | 15 | 5 | 1 | 161 | 0.30 | 7.84 |
NiMoP/Al | 15 | 5 | 1 | 179 | 0.31 | 7.36 |
样品 | 表面Mo组成/% | 原子比 | |||
---|---|---|---|---|---|
n(Mo4+)/n(Mo) | n(Mo6+)/n(Mo) | n(Mo5+)/n(Mo) | Ni/(Ni+Mo) | S/Mo | |
NiMo/Al | 21 | 58 | 21 | 0.14 | 0.27 |
P-NiMo/Al | 26 | 51 | 23 | 0.14 | 0.35 |
PNi-Mo/Al | 58 | 35 | 7 | 0.17 | 1.37 |
PMo-Ni/Al | 43 | 25 | 32 | 0.19 | 1.16 |
NiMoP/Al | 32 | 43 | 25 | 0.16 | 0.39 |
NiMo-P/Al | 35 | 48 | 17 | 0.16 | 1.13 |
表3 硫化物催化剂表面Mo物种组成和Ni/(Ni+Mo)、S/Mo原子比
样品 | 表面Mo组成/% | 原子比 | |||
---|---|---|---|---|---|
n(Mo4+)/n(Mo) | n(Mo6+)/n(Mo) | n(Mo5+)/n(Mo) | Ni/(Ni+Mo) | S/Mo | |
NiMo/Al | 21 | 58 | 21 | 0.14 | 0.27 |
P-NiMo/Al | 26 | 51 | 23 | 0.14 | 0.35 |
PNi-Mo/Al | 58 | 35 | 7 | 0.17 | 1.37 |
PMo-Ni/Al | 43 | 25 | 32 | 0.19 | 1.16 |
NiMoP/Al | 32 | 43 | 25 | 0.16 | 0.39 |
NiMo-P/Al | 35 | 48 | 17 | 0.16 | 1.13 |
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