FCC催化剂传质强化活性位利用效率的可视化分析

doi:10.11949/0438-1157.20240115

化工学报 ›› 2024, Vol. 75 ›› Issue (9): 3198-3209.DOI: 10.11949/0438-1157.20240115

• 催化、动力学与反应器 • 上一篇下一篇

FCC催化剂传质强化活性位利用效率的可视化分析

王冉¹(), 王焕², 熊晓云³, 关慧敏¹, 郑云锋³, 陈彩琳¹, 秦玉才¹(), 宋丽娟¹^,²

^1.辽宁石油化工大学石油化工学院，辽宁抚顺 113001
^2.中国石油大学(华东)化学化工学院，山东青岛 266580
^3.中国石油石油化工研究院兰州石油化工研究中心，甘肃兰州 730060

收稿日期:2024-01-25 修回日期:2024-05-19 出版日期:2024-09-25 发布日期:2024-10-10
通讯作者: 秦玉才
作者简介:王冉（1998—），女，硕士研究生，2248409310@qq.com
基金资助:
国家自然科学基金项目(U20A20120);中国石油天然气股份有限公司科技专项(KYWX-22-002);辽宁省兴辽计划项目(XLYC2203165)

Visual analysis of mass transfer enhanced active site utilization efficiency of FCC catalyst

Ran WANG¹(), Huan WANG², Xiaoyun XIONG³, Huimin GUAN¹, Yunfeng ZHENG³, Cailin CHEN¹, Yucai QIN¹(), Lijuan SONG¹^,²

^1.College of Petrochemical Engineering, Liaoning Petrochemical University, Fushun 113001, Liaoning, China
^2.College of Chemistry and Chemical Engineering, China University of Petroleum, Qingdao 266580, Shandong, China
^3.PetroChina Lanzhou Petrochemical Research Center, Lanzhou 730060, Gansu, China

Received:2024-01-25 Revised:2024-05-19 Online:2024-09-25 Published:2024-10-10
Contact: Yucai QIN

摘要/Abstract

摘要：

流化催化裂化(FCC)催化剂传质性能抑制活性位利用效率是影响其催化性能的关键因素，选用6种不同基质材料制备的FCC催化剂样品，在系统分析催化孔结构和酸性质的基础上，利用激光共聚焦荧光显微成像技术和吸附穿透曲线法模拟考察了重油大分子的传质扩散行为；并运用单分子荧光成像技术，以B酸中心催化噻吩低聚反应生成低聚物的数量作为判据考察了系列催化剂的活性位利用效率。研究发现，相比于传统的高岭土和拟薄水铝石作为基质材料，本课题组设计开发的大孔富B酸的基质材料(APM-9)明显优化了大分子在FCC催化剂上的传质性能，从而显著提升了活性位的利用效率。发展了一种新颖的FCC催化剂结构参数与其传质性能、酸中心利用效率构效关系建立的方法，可为催化剂基质材料的设计和优化提供数据支撑和理论指导。

关键词: FCC催化剂, 大孔基质, 荧光显微成像技术, 传质, 酸催化

Abstract:

The mass transfer performance of fluid catalytic cracking (FCC) catalysts inhibits the utilization efficiency of active sites, which is a key factor affecting its catalytic performance. In this paper, FCC catalyst samples prepared by 6 different matrix materials were selected, and the catalytic pore structure and acid properties were systematically analyzed. The mass transfer and diffusion behavior of heavy oil macromolecules were simulated by laser confocal fluorescence microscopy and adsorption penetration curve method. The utilization efficiency of active sites of the catalysts was investigated by using single molecule fluorescence imaging technique, and the number of oligomers produced by the oligomerization of thiophene catalyzed by B acid site was used as the criterion. It was found that compared with traditional kaolin and pseudo-boehmite as matrix materials, the macro-porous matrix material (APM-9) with abundant B acid sites designed and developed by our team significantly optimized the uploading performance of macromolecules on FCC catalysts, thus significantly improving the utilization efficiency of active sites. In this paper, a novel method to establish the structure-activity relationship between FCC catalyst structure parameters, its mass transfer performance and acid center utilization efficiency is developed, which can provide data support and theoretical guidance for the design and optimization of catalyst matrix materials.

Key words: FCC catalyst, macro-porous matrix, fluorescence microscopic imaging technique, mass transfer, acid catalysis

中图分类号:

O 603

王冉, 王焕, 熊晓云, 关慧敏, 郑云锋, 陈彩琳, 秦玉才, 宋丽娟. FCC催化剂传质强化活性位利用效率的可视化分析[J]. 化工学报, 2024, 75(9): 3198-3209.

Ran WANG, Huan WANG, Xiaoyun XIONG, Huimin GUAN, Yunfeng ZHENG, Cailin CHEN, Yucai QIN, Lijuan SONG. Visual analysis of mass transfer enhanced active site utilization efficiency of FCC catalyst[J]. CIESC Journal, 2024, 75(9): 3198-3209.

图/表 17

图1 随机光学波动成像（STORM）与共聚焦成像（CFM）的原理

Fig.1 Principles of stochastic optical reconstruction microscopy （STORM） and confocal imaging microscopy (CFM)

图2 6种FCC催化剂的SEM图像

Fig.2 SEM images of the six FCC catalysts

图3 6种催化剂样品的织构性质

Fig.3 Texture information of six catalyst samples

表1 6种催化剂样品织构性质参数

Table 1 Texture property parameters of six catalyst samples

样品	比表面积/ （m²·g^-1）	微孔面积/ （m²·g^-1）	介孔面积/（m²·g^-1）	总孔体积/（cm³·g^-1）	微孔体积/（cm³·g^-1）	介孔体积/（cm³·g^-1）
CAT-1	156	88	68	0.167	0.046	0.121
CAT-2	186	95	91	0.198	0.050	0.148
CAT-3	188	95	93	0.202	0.050	0.152
CAT-4	185	98	87	0.218	0.056	0.162
CAT-5	190	101	89	0.229	0.059	0.170
CAT-6	193	104	88	0.248	0.061	0.187

图4 压汞法分析6种催化剂样品的大孔孔径分布曲线

Fig.4 Distribution curves of macropore size for six catalyst samples measured by mercury intrusion method

图5 6种催化剂样品的NH3-TPD谱图

Fig.5 NH3-TPD spectra of six catalyst samples

图6 6种催化剂样品NH3-TPD谱图的分峰拟合曲线

Fig.6 Peak fitting curves of NH3-TPD spectra of six catalyst samples

表2 6种FCC催化剂的酸密度分布定量数据

Table 2 Quantitative data on acid density distribution of six FCC catalysts

样品	弱酸量/ (mmol·g^-1)	中强酸量/ (mmol·g^-1)	强酸量/ (mmol·g^-1)
CAT1	4.07	11.55	15.70
CAT2	4.11	12.45	15.79
CAT3	5.10	14.09	16.70
CAT-4	5.98	16.75	18.87
CAT-5	6.58	21.37	18.99
CAT-6	6.50	21.77	19.41

图7 6种催化剂样品脱附吡啶后的FTIR谱图

Fig.7 FTIR spectra of pyridine desorption of six catalyst samples

表3 催化剂酸性数据

Table 3 Catalyst acidity

样品	酸量/(mmol·g^-1)
	150℃		400℃
	B酸	L酸	B酸	L酸
CAT-1	0.065	0.064	0.043	0.010
CAT-2	0.069	0.070	0.047	0.014
CAT-3	0.087	0.071	0.067	0.010
CAT-4	0.072	0.082	0.056	0.009
CAT-5	0.086	0.135	0.057	0.005
CAT-6	0.089	0.137	0.061	0.010

图8 催化剂样品的吸附穿透曲线

Fig.8 The adsorption penetration curves of catalyst samples

表4 6种催化剂样品上萘、菲、吖啶的吸附穿透点与饱和时间

Table 4 Adsorption penetration and saturation time of naphthalene， phenanthrene and acridine on six catalyst samples

样品	时间/min			时间/min
样品	萘穿透	菲穿透	吖啶穿透	萘饱和	菲饱和	吖啶饱和
CAT-1	1.92	3.71	10.70	6.10	9.21	43.37
CAT-2	2.59	4.55	13.87	7.01	11.18	50.73
CAT-3	2.84	4.93	18.85	7.28	12.35	54.18
CAT-4	3.32	5.37	20.02	8.87	14.34	59.20
CAT-5	3.75	6.62	21.45	9.10	16.91	66.09
CAT-6	3.84	6.98	23.41	9.17	18.47	73.10

表5 Yoon-Nelson模型拟合所得6种催化剂样品上萘、菲、吖啶的吸附速率常数

Table 5 The adsorption rate constants of naphthene， phenanthrene and acridine for six catalyst samples obtained by fitting Yoon-Nelson model

探针分子	K_CAT-1/min^-1	K_CAT-2/min^-1	K_CAT-3/min^-1	K_CAT-4/min^-1	K_CAT-5/min^-1	K_CAT-6/min^-1
萘	1.3461	1.1570	1.1327	1.1145	1.0281	0.8897
菲	1.0907	0.9867	0.9335	0.8698	0.7798	0.7454
吖啶	0.2875	0.2562	0.2540	0.2531	0.2260	0.1950

图9 6种催化剂微球球心最大切面上罗丹明B分子的荧光分布（比色条显示不同颜色所代表的荧光强度）

Fig.9 Fluorescence mapping of the maximum section surface of catalyst samples soaked in Rhodamine B probe (color bar displays the fluorescence intensity)

表6 Fick第一定律计算罗丹明B在6种催化剂样品中的扩散系数

Table 6 The diffusion coefficients of Rhodamine B in six catalyst samples calculated by the Fick’s first law

催化剂	L_18min/m	D_eff/(m²·s^-1)
CAT-1	1.76×10^-5	2.72×10^-15
CAT-2	2.16×10^-5	3.63×10^-15
CAT-3	2.63×10^-5	6.04×10^-15
CAT-4	3.01×10^-5	1.10×10^-14
CAT-5	3.22×10^-5	1.65×10^-14
CAT-6	3.69×10^-5	6.68×10^-14

图10 6种FCC催化剂上噻吩二聚产物（绿色）和三聚产物（红色）的单分子成像

Fig.10 Single molecule imaging of dimeric products (green) and trimeric products (red) on the six FCC catalyst samples

图11 6种FCC催化剂样品上噻吩二聚和三聚产物总荧光亮点数的统计对比

Fig.11 Statistical comparison of total fluorescence brightness points of thiophene dimers and trimers in the six FCC catalyst samples

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FCC催化剂传质强化活性位利用效率的可视化分析

Visual analysis of mass transfer enhanced active site utilization efficiency of FCC catalyst

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