脱铝丝光分子筛应用于MTP反应: Al的落位和晶体形貌的影响

doi:10.1016/S1872-2067(20)63726-3

催化学报 ›› 2021, Vol. 42 ›› Issue (7): 1147-1159.DOI: 10.1016/S1872-2067(20)63726-3

脱铝丝光分子筛应用于MTP反应: Al的落位和晶体形貌的影响

任栎, 王博文, 陆琨, 彭如斯, 关业军^#(), 蒋金刚, 徐浩^$(), 吴鹏^*()

华东师范大学化学与分子工程学院, 绿色化学与化工过程上海市重点实验室, 上海200062

收稿日期:2020-09-05 接受日期:2020-10-10 出版日期:2021-07-18 发布日期:2020-12-10
通讯作者: 关业军,徐浩,吴鹏
基金资助:
国家重点研发计划(2016YFA0202804);国家自然科学基金(21533002);国家自然科学基金(21872052);国家自然科学基金(21972044);中央高校基本科研业务费专项资金

Selective conversion of methanol to propylene over highly dealuminated mordenite: Al location and crystal morphology effects

Li Ren, Bowen Wang, Kun Lu, Rusi Peng, Yejun Guan^#(), Jin-gang Jiang, Hao Xu^$(), Peng Wu^*()

Shanghai Key Laboratory of Green Chemistry and Chemical Process, School of Chemistry and Molecular Engineering, East China Normal University, Shanghai 200062, China

Received:2020-09-05 Accepted:2020-10-10 Online:2021-07-18 Published:2020-12-10
Contact: Yejun Guan,Hao Xu,Peng Wu
About author:^$ E-mail: hxu@chem.ecnu.edu.cn
^# E-mail: yjguan@chem.ecnu.edu.cn;
^* Tel/Fax: +86-21-62232292; E-mail: pwu@chem.ecnu.edu.cn;
Supported by:
Ministry of Science and Technology of the People’s Republic of China(2016YFA0202804);National Natural Science Foundation of China(21533002);National Natural Science Foundation of China(21872052);National Natural Science Foundation of China(21972044);Fundamental Research Funds for the Central Universities

摘要/Abstract

摘要：

甲醇制烯烃/丙烯工艺(MTO/MTP)是当前煤基碳资源绿色催化转化的重要过程之一. 在MTO/MTP工艺中, 分子筛通常面临低碳烯烃选择性低、水热稳定性差和寿命短等挑战. 开发高选择性和高稳定性的分子筛催化剂对煤基乙烯/丙烯等化学品的工业生产具有重要意义. 本文选择了具有12元环孔道的低硅丝光分子筛(Si/Al = 6)为母体, 对其进行脱铝处理制备了一系列不同Al含量的高硅丝光(Si/Al = 51-436)催化剂. 通过N₂-吸附、NH₃程序升温脱附、羟基红外光谱、CD₃CN-IR和Py-IR等技术对脱铝前后分子筛的孔道结构、酸密度、酸强度和铝的落位进行了深入研究, 并将其与MTP反应性能进行关联. 结果表明, 骨架Al的脱除在晶体中引入了介孔. 随着Si/Al的提高, 分子筛的酸量和酸强度同时降低. 深度脱铝后的丝光分子筛中只存在少量位于8元环侧口袋与12元环交叉口处的T2和T4位Al原子.
Si/Al高于150的脱铝丝光分子筛在MTP反应中丙烯选择性高达63%, 丙烯/乙烯的比值高达10. 与低硅丝光分子筛相比, 深度脱铝的丝光分子筛表现出更好的稳定性和更长的寿命. 相同反应条件下, 低硅丝光样品(Si/Al = 6)反应2 h后完全失活(转化率低于10%), 而高硅丝光样品(Si/Al = 274)反应132 h后转化率仍然高于80%. 丝光分子筛在脱铝处理后催化性能得到大幅提升的原因为: 酸密度和酸强度的降低显著改变了双循环机理历程, 反应中芳烃循环的比重下降, 烯烃循环得到了增强, 进而提高了丙烯选择性并抑制了积碳速率. 此外, 脱铝后保留下来的Al原子(活性中心)位于12元环孔道, 其大孔结构与脱铝引入的介孔孔道为反应物、中间体及产物的扩散提供了充足的空间, 进一步抑制了副反应的发生和积碳的生成. 进一步研究丝光分子筛形貌对MTP反应的影响发现, 丝光分子筛尺寸的变化不改变产物分布, 但显著影响催化剂寿命, 其原因在于丝光分子筛c-轴长度的增加使得烃池物种的扩散受到限制, 导致催化剂的寿命降低.

关键词: 丝光分子筛, 甲醇制丙烯, 脱铝, Al落位, 晶粒尺寸

Abstract:

The growing consumption of light olefins has stimulated intensive researches on methanol to olefin (MTO) process which possesses great advantages for coal conversion to value-added chemicals in an environmentally benign way. The catalysts commonly used for MTO process faces several challenges such as poor selectivity control, low hydrothermal stability and short lifetime. In the present study, we prepared a series of mordenite zeolites with variable Al contents (Si/Al molar ratios of 51-436) by a sequential dealumination treatment of air-calcination and acid leaching. The textural properties, acidity and Al location before and after the dealumination treatment have been systematically studied and their effect on MTO especially the methanol to propylene (MTP) performance was thoroughly investigated. The mordenite zeolites with the Si/Al ratios over 150 selectively catalyzed methanol conversion in the MTP pathway, providing a high propylene selectivity of 63% and propylene/ethylene ratio of > 10. Compared to the low-silica MOR catalysts, highly dealuminated MOR showed much higher stability and longer lifetime, which can be further enhanced via harsh hydrothermal pretreatment. Furthermore, the lifetime was highly related to the crystal size along c-axis. The excellent performance of highly dealuminated MOR is likely ascribed to the mesopores formed upon dealumination and the scarce Al sites located in the T sites shared by the 8-member ring (MR) side pockets and 12-MR pore channels.

Key words: Mordenite, Methanol to propylene, Dealumination, Al location, Crystal size

任栎, 王博文, 陆琨, 彭如斯, 关业军, 蒋金刚, 徐浩, 吴鹏. 脱铝丝光分子筛应用于MTP反应: Al的落位和晶体形貌的影响[J]. 催化学报, 2021, 42(7): 1147-1159.

Li Ren, Bowen Wang, Kun Lu, Rusi Peng, Yejun Guan, Jin-gang Jiang, Hao Xu, Peng Wu. Selective conversion of methanol to propylene over highly dealuminated mordenite: Al location and crystal morphology effects[J]. Chinese Journal of Catalysis, 2021, 42(7): 1147-1159.

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图/表 14

Fig. 1. XRD patterns of the M-200 samples with different Si/Al ratios. (1) M-200(6); (2) M-200(51); (3) M-200(98); (4) M-200(171); (5) M-200(274); (6) M-200(436). The numbers in parentheses indicate the Si/Al atomic ratios, the same below.

Table 1 Textural properties of various M-200 samples.

Sample	Si/Al ratio	Surface area (m² g^-1)			Pore volume (cm³ g^-1)
Sample	Si/Al ratio	S_total^a	S_micro^b	S_ext^c	V_total^d	V_micro^b	V_meso^e
M-200(6)	6	494	481	13	0.27	0.19	0.08
M-200(51)	51	496	446	50	0.30	0.18	0.12
M-200(98)	98	493	445	48	0.32	0.18	0.14
M-200(171)	171	526	463	63	0.36	0.18	0.18
M-200(274)	274	525	477	48	0.35	0.19	0.16
M-200(436)	436	525	477	48	0.34	0.19	0.15

Scheme 1. (a) Mordenite (MOR topology) structure showing four tetrahedral atoms (T1-T4) and ten oxygen atoms (O1-O10) with different locations. The main 12-MR channels and small 8-MR channels, parallelly running along the c-axis, are interconnected by 8-MR side pockets (marked in green and orange) along the b-axis. T1 is located in the junction of 8-MR and 12-MR pores, T2 and T4 are located in the intersection of 8-MR side pockets and 12-MR channels, while T3 is situate in the intersection of 8-MR side pockets and 8-MR channels, (b) 8-MR channels (marked in blue), 12-MR channels (marked in green) and the 8-MR side pockets interconnecting 12- and 8-MR channels (marked in orange) in the MOR structure.

Fig. 2. Deconvoluted FTIR spectra of M-200(6) (A) and M-200(98) (B) in the OH vibration region.

Fig. 3. CD3CN adsorbed FT-IR spectra of various M-200 samples at 423 K. (a) M-200(6); (b) M-200(51); (c) M-200(98); (d) M-200(171); (e) M-200(274); (f) M-200(436).

Fig. 4. The changes of relative Al distributions with the Al content. ASP: the sum area of the 2315 and 2277 cm-1 bands related to the Al ions in 8-MR side pockets; A12MR: the area of 2297 cm-1 band associated to the Al ions in 12-MR; AF: the total area of 2277, 2297 and 2315 cm-1 bands assigned to the whole Al ions in framework.

Fig. 5. Methanol conversion and the product selectivities as a function of time on stream over M-200(6) (a) and M-200(274) (b). Reaction conditions: catalyst, 0.1 g; WHSV = 1 h-1; temperature, 723 K; N2 gas flow rate, 20 mL min-1.

Table 2 The product distribution in the MTP reaction over the M-200(x) samples.

Catalyst	MeOH conv. (%)	P/E ratio	HTI	ethylene/2MBu	Product selectivity (%)
Catalyst	MeOH conv. (%)	P/E ratio	HTI	ethylene/2MBu	CH₄	C_2-4⁰	C₂⁼	C₃⁼	C₄⁼	C₅₊^N	Ar.	C_2-4⁼
M-200(6)	100	0.3	0.40	129.7	32.8	12.8	38.9	12.0	2.3	0.3	0.9	53.2
M-200(51)	100	3.7	0.38	8.6	12.2	6.0	12.2	44.9	10.0	4.8	9.9	67.1
M-200(98)	100	6.0	0.14	6.0	2.1	4.0	9.8	58.2	16.1	5.1	4.7	84.1
M-200(171)	99.1	9.5	0.13	2.9	0.7	3.9	6.7	62.6	17.6	7.9	0.6	86.9
M-200(274)	98.9	10.9	0.08	2.3	0.5	2.9	6.2	63.2	18.6	8.0	0.6	88.0
M-200(436)	98.9	11.6	0.08	2.1	0.5	2.7	5.5	63.9	18.5	8.6	0.3	87.9

Fig. 6. (a) Dependence of propylene selectivity on the relative percentage of Al ions in 12-MR vs. the total Al ions; (b) Dependence of propylene selectivity, P/E ratio and MTP lifetime on the Al content. The propylene selectivity and P/E ratio were obtained at TOS = 2 h, while the lifetime is defined as the time period with methanol conversion over 80%. Reaction conditions: catalyst, 0.1 g; WHSV = 1 h-1; temperature, 723 K; N2 gas flow rate, 20 mL min-1.

Fig. 7. Methanol conversion and product selectivity as a function of reaction temperatures (a) and weight space velocities (b) over M-200(274) catalyst. Reaction conditions: catalyst, 0.1 g; N2 gas flow rate, 20 mL min-1; (a) WHSV = 1 h-1; (b) temperature, 723 K.

Table 3 The product distribution in the MTP reaction over the MOR zeolites with different morphologies at comparable Si/Al ratios.

Catalyst	MeOH conv. (%)	P/E ratio	Product selectivity (%)
Catalyst	MeOH conv. (%)	P/E ratio	C_1-4⁰	C₂⁼	C₃⁼	C₄⁼	C₅₊^N	Ar.
M-50(154)	98.5	9.9	4.7	5.8	57.2	20.4	11.4	0.5
M-200(171)	99.1	9.5	4.7	6.7	62.6	17.5	7.9	0.6
M-400(190)	98.8	11.1	2.2	5.7	63.4	19.1	8.9	0.7
M-R(196)	99.3	10.0	3.8	6.2	62.6	18.1	8.8	0.5

Fig. 8. (a) Methanol conversion and propylene selectivity as a function of TOS over M-50(154) (1), M-200(171) (2), M-400(190) (3) and M-R(196) (4); (b) The propylene selectivity (TOS = 2 h) and the lifetime as a function of the crystal length along c-axis. Reaction conditions: catalyst, 0.1 g; WHSV = 1 h-1; temperature, 723 K; N2 gas flow rate, 20 mL min-1.

Fig. 9. GC-MS chromatograms of the hydrocarbon species retained on various used M-200 catalysts after MTP reaction at different temperature at TOS of 2 min. (1) M-200(6), 623 K; (2) M-200(274), 623 K; (3) M-200(274), 723 K. The MTP reaction conditions: catalyst, 0.1 g; WHSV = 1 h-1; N2 gas flow rate, 20 mL min-1.

Scheme 2. The reaction mechanism of the methanol to propylene over the dealumianted mordenite catalyst.

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脱铝丝光分子筛应用于MTP反应: Al的落位和晶体形貌的影响

Selective conversion of methanol to propylene over highly dealuminated mordenite: Al location and crystal morphology effects

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