调控铝在ITH沸石骨架中的位置以用于催化甲醇制烯烃

doi:10.1016/S1872-2067(23)64574-7

催化学报 ›› 2024, Vol. 56: 114-121.DOI: 10.1016/S1872-2067(23)64574-7

调控铝在ITH沸石骨架中的位置以用于催化甲醇制烯烃

范凯^a, 吴勤明^b, 刘烁^c, 孔海宇^c, 王森^d, 孟祥举^a^,^*(), 张维萍^c^,^*(), 肖丰收^b^,^*()

^a浙江省应用化学重点实验室, 浙江大学化学系, 浙江杭州310028, 中国
^b浙江大学化学与生物工程学院, 浙江杭州310028, 中国
^c大连理工大学精细化工国家重点实验室, 辽宁大连116012, 中国
^d中国科学院山西煤炭化学研究所, 煤转化国家重点实验室, 山西太原030001, 中国
^e巴斯夫股份有限公司, 德国
^f东京工业大学资源化学研究所, 日本
^g鲁汶大学表面化学与催化中心, 比利时

收稿日期:2023-10-27 接受日期:2023-11-29 出版日期:2024-01-18 发布日期:2024-01-10
通讯作者: *电子信箱: mengxj@zju.edu.cn (孟祥举), wpzhang@dlut.edu.cn (张维萍), fsxiao@zju.edu.cn (肖丰收).
基金资助:
国家重点研发计划项目(2022YFA1503602);国家自然科学基金项目(22288101);国家自然科学基金项目(22125204);巴斯夫INCOE项目

Adjusting Al location in the framework of ITH zeolites for catalytic conversion of methanol to olefins

Kai Fan^a, Qinming Wu^b, Shuo Liu^c, Haiyu Kong^c, Sen Wang^d, Eduard Kunkes^e, Trees De Baerdemaeker^e, Andrei-Nicolae Parvulescu^e, Nils Bottke^e, Toshiyuki Yokoi^f, Dirk E. De Vos^g, Xiangju Meng^a^,^*(), Weiping Zhang^c^,^*(), Feng-Shou Xiao^b^,^*()

^aKey Lab of Applied Chemistry of Zhejiang Province, Department of Chemistry, Zhejiang University, Hangzhou 310028, Zhejiang, China
^bCollege of Chemical and Biological Engineering, Zhejiang University, Hangzhou 310028, Zhejiang, China
^cState Key Laboratory of Fine Chemicals, Dalian University of Technology, Dalian 116012, Liaoning, China
^dState Key Laboratory of Coal Conversion, Institute of Coal Chemistry, Chinese Academy of Sciences, Taiyuan 030001, Shanxi, China
^eBASF SE, Ludwigshafen 67056, Germany
^fChemical Resources Laboratory, Tokyo Institute of Technology, Yokohama 226-8503, Japan
^gCentre for Surface Chemistry and Catalysis, KU Leuven, Kasteelpark Arenberg 23, Leuven 3001, Belgium

Received:2023-10-27 Accepted:2023-11-29 Online:2024-01-18 Published:2024-01-10
Contact: *E-mail: mengxj@zju.edu.cn (X. Meng), wpzhang@dlut.edu.cn (W. Zhang), fsxiao@zju.edu.cn (F.-S. Xiao).
Supported by:
National Key Research and Development Program of China(2022YFA1503602);National Natural Science Foundation of China(22288101);National Natural Science Foundation of China(22125204);BASF INCOE project

摘要/Abstract

摘要：

随着低碳烯烃需求量的增加, 甲醇制烯烃(MTO)成为由非石油资源制取低碳烯烃的关键技术, 其中沸石由于具有可调节的酸度、有序的微孔结构和较好的择型性能而被广泛用作MTO反应催化剂. ITQ-13沸石(ITH拓扑结构)由于其独特的九元环结构在MTO反应中表现出较好的丙烯选择性和反应寿命, 引起了广泛关注. 研究表明, 分子筛的酸中心分布与MTO反应性能密切相关, 因此, 研究ITQ-13沸石中铝分布与MTO反应性能的关系, 对进一步提升其MTO催化性能具有重要意义.

本文分别以与ITH具有共同基本结构单元(双四元环, D4Rs)的LTA沸石(LTA-ITH)和薄水铝石(C-ITH)为铝源, 合成了两类铝硅酸盐ITH沸石. X射线衍射、扫描电子显微镜以及氮气吸脱附表征结果表明, 这两类分子筛具有相似的片状形貌和微孔性质. 氨气程序升温脱附结果表明, 具有相近硅铝比的两类ITH沸石具有相近的酸量. 进一步采用²⁷Al 魔角旋转核磁共振(MAS NMR)、密度泛函理论计算和1-己烯裂解反应对两类ITH分子筛的铝分布进行研究. 结果表明, 两类分子筛具有不同的铝分布, LTA-ITH中有更多的铝进入ITH的正弦孔道与直孔道, 而C-ITH中有更多的铝分布在交叉孔道. 当前, 研究者普遍认为MTO反应过程遵循双循环烃池机理, ITH交叉孔道由于具有较大的空间, 相比于正弦孔道和直孔道, 更有利于芳烃循环中间体的产生, 从而有利于形成芳烃循环产物(乙烯), 而正弦孔道和直孔道却更有利于烯烃循环过程, 导致产生更多的丙烯. 对两类ITH进行了MTO催化性能测试, 结果表明, LTA-ITH比C-ITH表现出更高的丙烯选择性, 并且表现出更高的丙烯与乙烯的比率, 表明其烯烃循环过程得到加强, 这与²⁷Al MAS NMR以及1-己烯裂解反应得到的结论一致, 进一步证明ITH分子筛的铝分布得到有效调控.

综上, 本文阐明了ITH沸石中铝分布与其反应性能的关系, 为调整沸石骨架中的Al位点提供一种新策略, 为未来制备高效的MTO沸石基催化剂提供参考.

关键词: 骨架铝分布, 硅铝ITH分子筛, 甲醇制烯烃, 铝核磁

Abstract:

Adjusting location and distribution of Al sites in the zeolite framework is critical for catalysis, and typical strategies include using zeolites as starting Al source. However, this approach is still challenging for aluminosilicate ITH zeolite. Herein, the distribution of Al species in the framework of ITH was efficiently regulated by implementing LTA zeolite as the aluminum source added in the starting gels (LTA-ITH). The obtained LTA-ITH zeolites have similar nanosheet morphology, textual parameters, and acidic properties to those of conventional ITH synthesized from boehmite (C-ITH), while the results of ²⁷Al MAS NMR spectra and 1-hexene cracking indicate that they have a different Al distribution. The use of LTA zeolite in starting gel is favorable for the formation of more Al species in sinusoidal and straight channels, compared with the C-ITH. Catalytic tests in the conversion of methanol to light olefin showed that LTA-ITH exhibited enhanced catalyst lifetime and propene selectivity compared with the C-ITH, which is reasonably attributed to the different locations of Al species in their respective ITH frameworks.

Key words: Al location in the framework, Aluminosilicate ITH zeolite, Methanol to olefins, ²⁷Al MAS NMR spectroscopy

范凯, 吴勤明, 刘烁, 孔海宇, 王森, 孟祥举, 张维萍, 肖丰收. 调控铝在ITH沸石骨架中的位置以用于催化甲醇制烯烃[J]. 催化学报, 2024, 56: 114-121.

Kai Fan, Qinming Wu, Shuo Liu, Haiyu Kong, Sen Wang, Eduard Kunkes, Trees De Baerdemaeker, Andrei-Nicolae Parvulescu, Nils Bottke, Toshiyuki Yokoi, Dirk E. De Vos, Xiangju Meng, Weiping Zhang, Feng-Shou Xiao. Adjusting Al location in the framework of ITH zeolites for catalytic conversion of methanol to olefins[J]. Chinese Journal of Catalysis, 2024, 56: 114-121.

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图/表 9

Fig. 1. XRD patterns of the as-synthesized ITH zeolites (A) and H-form ITH zeolites (B), and SEM images (C) of the as-synthesized ITH zeolites with C-ITH-50 (a), LTA-ITH-50 (b), C-ITH-75 (c), LTA-ITH-75 (d), C-ITH-100 (e) and LTA-ITH-100 (f).

Table 1 Chemical compositions, textual parameters and acid properties of H-form LTA-ITH and C-ITH zeolites.

Zeolite	Si/Al ^a	Surface area ^b(m²/g)		Pore volume ^b(cm³/g)		Acidity by NH₃-TPD ^c(mmol/g)
Zeolite	Si/Al ^a	Total	Micro	Micro	Meso	Total	Weak	Strong
C-ITH-50	42	393	310	0.14	0.21	0.89	0.55	0.34
LTA-ITH-50	44	394	313	0.14	0.21	0.83	0.50	0.33
C-ITH-75	66	388	305	0.14	0.22	0.51	0.29	0.22
LTA-ITH-75	65	395	316	0.15	0.21	0.47	0.27	0.20
C-ITH-100	89	399	320	0.15	0.21	0.39	0.21	0.18
LTA-ITH-100	93	400	322	0.15	0.19	0.34	0.19	0.15

Fig. 2. Deconvoluted and simulated 27Al MAS NMR spectra of H-form C-ITH (A) and LTA-ITH (B) zeolites. The experimental spectra are shown in pink solid lines and the fitted ones are shown in yellow dashed lines.

Table 2 Deconvolutional data of the 27Al MAS NMR spectra of H-form ITH zeolites.

Zeolite	Al distribution (%)
Zeolite	Al_S 56 and 61 ppm	Al_I 48 and 53 ppm
C-ITH-100	47.9	52.1
C-ITH-75	42.7	57.3
C-ITH-50	39.6	60.4
LTA-ITH-100	62.8	37.2
LTA-ITH-75	51.5	48.5
LTA-ITH-50	40.8	59.2

Table 3 Catalytic data in 1-hexene cracking over the LTA-ITH-100 and C-ITH-100 zeolites.

Sample	Selectivity (C%)			C₂⁼/C₄⁼	C₄⁼/C₃⁼	Conversion (%)
Sample	C₂⁼	C₃⁼	C₄⁼	C₂⁼/C₄⁼	C₄⁼/C₃⁼	Conversion (%)
C-ITH-100	4.2	35.9	15.6	0.27	0.43	98.1
LTA-ITH-100	3.8	40.4	12.8	0.30	0.32	97.6

Fig. 3. MTO performance of the H-form ITH zeolites. The MTO reactions were carried out at atmospheric pressure, 480 ?°C and a methanol weight hourly space velocity (WHSVMethanol) of 2 h?1.

Table 4 Catalytic performances of various H-form ITH zeolites in the steady stage.

Zeolite	Selectivity (C%)					(P-E)/E	Lifetime (h)
Zeolite	C₂⁼	C₃⁼	C₄⁼	C₁^‒‒C₄^‒	BTX	(P-E)/E	Lifetime (h)
C-ITH-50	14.0	34.0	13.6	15.8	11.0	1.43	26.6
LTA-ITH-50	13.3	34.1	15.4	15.0	8.4	1.56	31.3
C-ITH-75	14.2	37.6	14.5	14.8	7.9	1.65	38.9
LTA-ITH-75	11.8	40.8	16.5	13.0	4.4	2.46	44.7
C-ITH-100	12.2	40.1	15.3	13.6	4.9	2.29	50.4
LTA-ITH-100	10.1	43.5	16.2	12.5	2.2	3.31	58.7

Fig. 4. Proposed schematic diagram of aromatic and alkene cycle mechanism for the MTO reaction.

Fig. 5. Dependences of (P-E)/E ratios in the MTO reaction (complete methanol conversion) on (A) AlS and (B) AlI percentages in the ITH zeolites.

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调控铝在ITH沸石骨架中的位置以用于催化甲醇制烯烃

Adjusting Al location in the framework of ITH zeolites for catalytic conversion of methanol to olefins

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