NiW/SAPO-11催化剂对煤焦油加氢尾油模型化合物二十烷加氢异构性能的影响

赵旭红; 吴玉起; 代正华; 钟梅; 靳立军; 刘洋; 亚力昆江·吐尔逊; 李建; 周玉生

doi:10.19906/j.cnki.JFCT.2023068

NiW/SAPO-11催化剂对煤焦油加氢尾油模型化合物二十烷加氢异构性能的影响

doi: 10.19906/j.cnki.JFCT.2023068

赵旭红^1,,
吴玉起^1,,
代正华^1,,
钟梅^1, ,,
靳立军^{1, 2,},
刘洋^1, ,,
亚力昆江·吐尔逊¹,
李建¹,
周玉生^3,

1.
新疆大学省部共建碳基能源资源化学与利用国家重点实验室化工学院新疆煤炭清洁转化与化工过程重点实验室,新疆乌鲁木齐 830017
2.
大连理工大学化工学院精细化工国家重点实验室煤化工研究所, 辽宁大连 116024
3.
新疆宣力环保能源股份有限公司, 新疆哈密 839009

基金项目: 新疆维吾尔自治区重大科技专项(2021A01002-3)，国家自然科学基金(22169019，22279110)和“天池英才”引进计划资助

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Tel: 13669931725, E-mail: zhongmei0504@126.com

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出版历程
- 收稿日期: 2023-07-24
- 修回日期: 2023-08-26
- 录用日期: 2023-08-28
- 网络出版日期: 2023-09-18
- 刊出日期: 2024-03-10

Effect of NiW/SAPO-11 catalyst on hydroisomerization performance of model compound eicosane for tail oil hydrogenation of coal tar

ZHAO Xuhong^1
,,
WU Yuqi^1
,,
DAI Zhenghua^1
,,
ZHONG Mei^{1
, ,},
JIN Lijun^{1, 2
,},
LIU Yang^{1
, ,},
Yalkunjang Tursun¹,
LI Jian¹,
ZHOU Yusheng^3
,

1.
State Key Laboratory of Chemistry and Utilization of Carbon Based Energy Resources, Xinjiang University, Urumqi 830017, China
2.
State Key Laboratory of Fine Chemicals, Institute of Coal Chemical Engineering, School of Chemical Engineering, Dalian University of Technology, Dalian 116024, China
3.
Xinjiang Xuanli Environmental Protection Energy Co., LTD., Hami 839009, China

Funds: The project was supported by the Major Science and Technology Project of Xinjiang Uygur Autonomous Region (2021A01002-3), the National Natural Science Foundation of China (22169019, 22279110) and “Tianchi Talents” Introduction Plan.

摘要

摘要: 以SAPO-11分子筛为载体，采用机械化学法制备Ni系催化剂，引入W调节其电子结构、晶粒尺寸与形态分布以及催化剂的孔结构、酸性与酸量等，基于对XRD、TEM、BET、NH₃-TPD、吡啶吸附红外等结果的深入分析，探究催化剂NiW配比对催化剂性质和煤焦油加氢尾油模型化合物正二十烷（n-C₂₀）加氢异构性能的影响规律。结果表明，Ni/SAPO-11负载W后，比表面积不同程度增加，W质量分数为0.5%时比表面积达到最大值149 m²/g；Ni的平均粒径减小，W质量分数为1%时降至最小值4.43 nm，比Ni/SAPO-11减小36%，且Ni⁰的含量和表面酸量均最高。此外，W促进了Ni的还原，使得还原峰温向低温方向移动。XPS分析表明，随着W含量的增加，Ni⁰的结合能降低，W⁵⁺的结合能升高。二十烷（n-C₂₀）的加氢异构产物分布显示，3Ni1W/SAPO-11作用下n-C₂₀的转化率和异二十烷（i-C₂₀）的收率均最高，分别为88.23%和75.72%，且以单支链异二十烷（Mono-i-C₂₀）为主，收率达71.65%。在线取样结果显示，n-C₂₀在金属位点与酸功能的双重作用下先生成单支链异构体，随着反应的进行向多支链异构体转化，不稳定的多支链异构体会进一步裂解成小分子烷烃。
- SAPO-11 /
- 长链烷烃 /
- NiW催化剂 /
- 加氢异构
Abstract: Ni-based catalysts were prepared by mechanochemical method with SAPO-11 zeolite as the carrier, and W was introduced to adjust the electronic structure, grain size and morphology of Ni particle, as well as pore structure, acidity, and acid amount of the catalyst. The effect of NiW ratios on catalyst properties and the hydro-isomerization properties of n-eicosane (n-C₂₀), which is a model compound for coal tar hydrogenation tail oil, was explored by XRD, TEM, BET, NH₃-TPD and Py-FTIR. The results show that the specific surface area of Ni/SAPO-11 increases with the addition of W, and reaches the maximum value of 149 m²/g at the W addition of 0.5%. The average particle size of Ni decreases with the addition of W, and reaches to the minimum value of 4.43 nm at the W addition of 1%, which is 36% less than that of Ni/SAPO-11. At this time, the content of Ni⁰ and the amount of surface acid are the highest. In addition, W promotes the reduction of Ni, causing the reduction peak temperature to move toward lower temperature. XPS results show that with the increase of W content, the binding energy of Ni⁰ decreases while that of W⁵⁺ increases. The isomers distribution of eicosane (n-C₂₀) shows that the conversion of n-C₂₀ and the yield of i-C₂₀ are the highest in the presence of 3Ni1W/SAPO-11, which are 88.23% and 75.72%, respectively. It is mainly the mono-i-C₂₀ with a yield of 71.65%. The on-line sampling results show that n-C₂₀ generates the mono-branched isomer under the action of metal site and acid function. With the reaction, the mono-branched isomer is transformed into the multi-branched isomer, and the unstable multi-branched isomer is cracked into small molecule alkanes.
- SAPO-11 /
- long-chain alkanes /
- NiW catalysts /
- hydro-isomerization

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FIG. 3018. FIG. 3018.

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图 1 催化剂的XRD谱图（a）和局部放大图（b）

Figure 1 XRD patterns (a) and local magnification (b) of catalyst

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图 2 催化剂的N₂吸附-脱附曲线（a）和孔径分布（b）

Figure 2 N₂ adsorption-desorption curves (a) and pore size distributions (b) of catalysts

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图 3 催化剂的TEM（a1）−（e1）和HRTEM（a2）−（e2）图与Ni的粒径分布（a3）−（e3）

Figure 3 The TEM (a1)−(e1) and HRTEM (a2)−(e2) images of catalysts and size distribution of Ni (a3)−(e3)

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图 4 3Ni1W/SAPO-11中Ni 2p （a）和W 4f （b）的分峰拟合图

Figure 4 Peak fitting profiles of Ni 2p (a) and W 4f (b) in 3Ni1W/SAPO-11

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图 5 Ni和W组分的结合能（a）与形态分布（b）

Figure 5 Binding energy (a) and morphology distribution (b) of Ni and W species

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图 6 催化剂的H₂-TPR曲线

Figure 6 H₂-TPR profiles for different catalysts

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图 7 催化剂的NH₃-TPD曲线（a）和Py-FTIR谱图（b）

Figure 7 NH₃-TPD profiles (a) and Py-FTIR spectra (b) of catalysts

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图 8 催化剂对n-C₂₀加氢异构反应性能的影响

Figure 8 Effect of catalyst on hydrogenation isomerization of n-C₂₀

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图 9 n-C₂₀加氢异构行为随时间的变化

Figure 9 Hydro-isomerism behavior of n-C₂₀ with varied reaction time

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图 10 n-C₂₀在3Ni1W/SAPO-11上主要的加氢异构反应路径

Figure 10 The main hydro-isomerization reaction pathway of n-C₂₀ on 3Ni1W/SAPO-11

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表 1 催化剂的孔结构参数和相对结晶度

Table 1 Pore structure parameters and relative crystallinity of catalysts

Sample	S_BET^a/(m²·g⁻¹)	S_mic^b/(m²·g⁻¹)	S_ext^c/(m²·g⁻¹)	d/nm	v/(cm³·g⁻¹)	C^d/%
SAPO-11	184	131	53	6.52	0.30	100
4Ni/SAPO-11	111	58	53	8.32	0.23	84.93
3.5Ni0.5W/SAPO-11	149	109	40	3.49	0.13	85.80
3Ni1W/SAPO-11	123	75	48	4.91	0.15	88.39
2.5Ni1.5W/SAPO-11	113	67	46	5.17	0.15	86.83
4W/SAPO-11	134	77	57	7.76	0.26	89.28
^a: BET method; ^b: t-plot method; ^c: S_ext was calculated by subtracting micropore area from BET area; ^d: The relative crystallinity derived from XRD analysis using the ratio of the sum of zeolite peaks to background with the parent SAPO-11 as reference.

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表 2 催化剂的酸性分布

Table 2 Acid site distribution of catalysts

Sample	Weak acidity/(mmol·g⁻¹)	Medium strong acidity/(mmol·g⁻¹)	Total/(mmol·g⁻¹)
SAPO-11	0.33	0.55	0.88
4Ni/SAPO-11	0.19	0.38	0.57
3.5Ni0.5W/SAPO-11	0.28	0.41	0.69
3Ni1W/SAPO-11	0.30	0.45	0.75
2.5Ni1.5W/SAPO-11	0.29	0.40	0.69
4W/SAPO-11	0.25	0.36	0.61

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表 3 催化剂的理化性质

Table 3 Physicochemical properties of the catalysts

Sample	Acidity/(μmol·g⁻¹)		d_Ni/nm	D_Ni^a/%	C_Ni^b/(μmol·g⁻¹)	C_Ni/C_B
Sample	C_B	C_L	d_Ni/nm	D_Ni^a/%	C_Ni^b/(μmol·g⁻¹)	C_Ni/C_B
SAPO-11	47.28	139.03	−	−	−	−
4Ni/SAPO-11	14.02	58.03	6.96	13.95	95.08	6.78
3.5Ni0.5W/SAPO-11	30.89	35.23	5.78	16.80	100.17	3.24
3Ni1W/SAPO-11	35.30	39.37	4.43	21.92	112.03	3.17
2.5Ni1.5W/SAPO-11	34.25	42.43	4.85	20.02	93.36	2.72
4W/SAPO-11	41.34	125.81	−	−	−	−
^a: Ni dispersion (dispersion (%)=97.1/d_Ni); ^b: Calculated from the metal content and metal dispersity of Ni.

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表 4 不同催化剂在类似反应条件下的催化性能

Table 4 The catalytic performance of different catalysts under similar reaction conditions

Carrier	Metal	Loading/%	Reactant	Temperature /℃	Pressure /MPa	Conversion /%	Yield /%	Ref.
SAPO-11	NiGa	6	n-C₁₆	360	2	96.76	64.90	[27]
ZSM-22	Pt	0.5	n-C₁₆	320	4	>80.00	>71.00	[51]
ZSM-48	Pt	−	n-C₁₆	320	4	<87.9	<80	[49]
SAPO-11	NiW	20	n-C₁₆	340	2	79.5	71.18	[9]
SAPO-11	NiCu	4.5	n-C₈	340	2	70.00	66.50	[21]
SAPO-11	NiW	4	n-C₂₀	320	3	88.23	75.72	this work

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