无机体系合成纳米丝光沸石组装体及其优异的二甲醚羰基化催化性能

doi:10.1016/S1872-2067(20)63777-9

催化学报 ›› 2021, Vol. 42 ›› Issue (9): 1468-1477.DOI: 10.1016/S1872-2067(20)63777-9

无机体系合成纳米丝光沸石组装体及其优异的二甲醚羰基化催化性能

曹凯鹏^a^,^b, 樊栋^a, 曾姝^a^,^b, 樊本汉^a^,^b, 陈南^a^,^b, 高铭斌^a^,^b, 朱大丽^a^,^b, 王林英^a, 田鹏^a^,^*(), 刘中民^a^,^b^,^#()

^a中国科学院大连化学物理研究所, 洁净能源国家实验室(筹), 甲醇制烯烃国家工程实验室, 辽宁大连116023
^b中国科学院大学, 北京100049

收稿日期:2020-11-19 接受日期:2021-02-02 出版日期:2021-09-18 发布日期:2021-05-16
通讯作者: 田鹏,刘中民
基金资助:
国家自然科学基金(21676262);国家自然科学基金(21991090);国家自然科学基金(21991091);中国科学院前沿科学重点研究项目(QYZDB-SSW-JSC040);中法分子筛联合实验室(LIA)资助

Organic-free synthesis of MOR nanoassemblies with excellent DME carbonylation performance

Kaipeng Cao^a^,^b, Dong Fan^a, Shu Zeng^a^,^b, Benhan Fan^a^,^b, Nan Chen^a^,^b, Mingbin Gao^a^,^b, Dali Zhu^a^,^b, Linying Wang^a, Peng Tian^a^,^*(), Zhongmin Liu^a^,^b^,^#()

^aNational Engineering Laboratory for Methanol to Oleﬁns, Dalian National Laboratory for Clean Energy, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, Liaoning, China
^bUniversity of Chinese Academy of Sciences, Beijing 100049, China

Received:2020-11-19 Accepted:2021-02-02 Online:2021-09-18 Published:2021-05-16
Contact: Peng Tian,Zhongmin Liu
About author:^# E-mail: liuzm@dicp.ac.cn
^* E-mail: tianpeng@dicp.ac.cn;
Supported by:
National Natural Science Foundation of China(21676262);National Natural Science Foundation of China(21991090);National Natural Science Foundation of China(21991091);Key Research Program of Frontier Sciences, Chinese Academy of Sciences(QYZDB-SSW-JSC040);funding from the French-Sino International Laboratory (LIA) “Zeolites”

摘要/Abstract

摘要：

乙醇是一种重要的有机化工原料和燃料/燃料添加剂. 二甲醚(DME)羰基化制乙酸甲酯(MAc)并进一步加氢制备乙醇提供了一条乙醇生产新途径. 作为该路线的核心过程, DME羰基化制备MAc反应具有原子经济性高和反应条件温和等特点, 近年来备受关注. 在DME羰基化制备MAc的多相催化剂中, 丝光沸石(MOR)是迄今为止最为高效的催化剂之一, 表现出优异的羰基化反应活性和高MAc选择性. 但传统的无机体系合成方法只能得到Si/Al比(SAR)介于5~7的MOR沸石, 且晶体尺寸通常较大.
本文设计了低碱度凝胶体系和晶种法相结合的合成策略, 在无有机模板条件下绿色高效合成了SAR最高为9.4的MOR沸石纳米组装体. 选取三个具有不同SAR(I-5.3, I-7.4和I-9.4)的样品进一步表征并与其催化性能相关联. 实验发现, 催化剂的酸强度随着SAR的提高而明显增强, 但是三个样品的总酸量以及Brønsted酸在主孔道和侧口袋的分布比例接近. 利用傅里叶变换红外和钠核磁技术分别对H-MOR及其Na-MOR母体样品中的酸羟基和Na⁺的空间分布进行分析, 发现质子在主孔道与侧口袋的分布比例与Na⁺的分布并不一致, 表明质子和Na⁺可以落位于同一T位的不同氧位. 通过对催化剂扩散性质以及酸性位的可接触性的表征, 发现低硅样品I-5.3和I-7.4尽管晶粒尺寸较小, 但由于孔道中骨架外铝的含量较高, 严重阻碍内扩散, 并且导致吡啶对12元环主孔道中酸中心的可接触性降低. 相对于低硅样品, 高硅样品I-9.4由于其相对较低的骨架铝密度和较低的脱铝程度, 表现出最优的传质性能以及吡啶对12元环主孔道中酸中心的可接触性, 催化剂主通道中的所有酸性位都能被吡啶所覆盖. 相应地, 样品I-9.4(吡啶修饰催化剂)在DME羰基化反应中表现出较高的催化活性与MAc选择性(接近100%), MAc产率高达6.8 mmol/g/h. 综上, 本文发展的无有机模板策略合成MOR沸石纳米组装体具有良好应用前景.

关键词: 丝光沸石, 无有机模板合成, 二甲醚羰基化, 酸性质, 扩散

Abstract:

Seed-assisted low alkalinity gel system was developed to explore the organic-free synthesis of MOR zeolite. MOR nanoassemblies with Si/Al ratio (SAR) up to 9.4 and high solid yield (84-94%) were successfully obtained under controlled low alkalinity conditions. Characterization results demonstrate that the acid strength increases in parallel with the SAR, while the total acid amount and the proton distribution in the main channels and the side pockets are similar for the samples. The proton distribution in the H-MOR is not straightforwardly related to the Na⁺ distribution in the as-synthesized MOR, implying the transfer of the protons among the oxygen sites of framework T atom. Relative to low-silica samples I-5.3 and I-7.4, sample I-9.4 displays the best mass transfer performance and accessibility of the acid sites by pyridine due to its relatively low Al density and mild dealumination degree. Correspondingly, sample I-9.4 (pyridine-modified catalyst) shows the best activity with ca. 100% selectivity of methyl acetate (MAc) in the DME carbonylation reaction. The high steady MAc yield (6.8 mmol/g/h) over sample I-9.4 suggests the promising application of MOR nanoassemblies synthesized by this economical organic-free strategy.

Key words: MOR zeolite, Organic-free synthesis, DME carbonylation, Acidity, Diffusion

曹凯鹏, 樊栋, 曾姝, 樊本汉, 陈南, 高铭斌, 朱大丽, 王林英, 田鹏, 刘中民. 无机体系合成纳米丝光沸石组装体及其优异的二甲醚羰基化催化性能[J]. 催化学报, 2021, 42(9): 1468-1477.

Kaipeng Cao, Dong Fan, Shu Zeng, Benhan Fan, Nan Chen, Mingbin Gao, Dali Zhu, Linying Wang, Peng Tian, Zhongmin Liu. Organic-free synthesis of MOR nanoassemblies with excellent DME carbonylation performance[J]. Chinese Journal of Catalysis, 2021, 42(9): 1468-1477.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(20)63777-9

https://www.cjcatal.com/CN/Y2021/V42/I9/1468

图/表 9

Table 1 Synthesis conditions, product SAR and solid yields of MOR zeolites.

Sample	Gel molar composition ^a				Time (h)	Product		Solid yield ^c(%)
Sample	SiO₂	Al₂O₃	Na₂O	H₂O	Time (h)	Phase	SAR ^b	Solid yield ^c(%)
I-5.3	1.0	0.08	0.13	15	30	MOR	5.3 (5.2)	88
I-7.0	1.0	0.06	0.13	15	30	MOR	7.0 (7.3)	84
I-9.4	1.0	0.05	0.08	15	30	MOR	9.4 (9.8)	94
I-11.9	1.0	0.04	0.08	15	30	MOR+U ^e	11.9	—
I-9.4-N ^d	1.0	0.05	0.08	15	110	MOR+MFI	—	—
I-9.4-H	1.0	0.05	0.13	15	13	MOR	8.1	81
I-9.4-L	1.0	0.05	0.067	15	110	MOR+Amorphous	—	—

Fig. 1. (a) XRD patterns of the as-synthesized MOR samples; (b) N2 adsorption-desorption isotherms of the H-MOR samples (the isotherms of I-7.0 and I-9.4 are offset by 50 and 100 cm3/g, respectively); (c-e) SEM images of the as-synthesized samples. The insets in (e) show the HRTEM image of sample I-9.4. (f) TEM image of sample I-9.4, corresponding SAED pattern viewed along the [001] direction and a schematic to illustrate the 12-MR channel system.

Fig. 2. (a) 27Al, (b) 29Si and (c) 23Na MAS NMR spectra of the as-synthesized samples. The samples were dehydrated at 400 °C for 12 h in vacuum before 23Na MAS NMR measurement.

Table 2 Textural properties of the samples.

Sample	Surface area ^a (m²/g)			Pore volume ^b (cm³/g)
Sample	S_BET	S_micro	S_ext	V_total	V_micro	V_meso
I-5.3	418	374	44	0.24	0.18	0.06
I-7.0	438	392	47	0.24	0.19	0.05
I-9.4	428	375	53	0.24	0.18	0.06

Fig. 3. Acidity of the H-MOR samples. (a) NH3-TPD profiles; (b) NH3-adsorption FTIR spectra; (c) FTIR spectra of H-MOR; (d) Deconvoluted bands corresponding to the acid hydroxyls in the 12-MR channels (HF) and the side pockets (LF). The numbers in (d) refer to the percentage of Br?nsted acids in the side pockets.

Table 3 Acid amounts of the H-MOR samples based on NH3-TPD and NH3-FTIR.

Sample	NH₃-TPD (mmol/g)				NH₃-FTIR ^b (mmol/g)
Sample	Weak	Moderate	Strong	M+S ^a	BAS	LAS	B+L ^c	BAS/LAS
I-5.3	1.03	0.4	0.79	1.19	1.01	0.17	1.18	5.82
I-7.0	0.97	0.32	0.82	1.14	0.83	0.15	0.98	5.53
I-9.4	0.77	0.26	0.89	1.15	0.91	0.08	0.99	10.87

Fig. 4. ν(OH) vibration region of the H-MOR samples (a) before and after pyridine adsorption at 150 °C, (b) after pyridine adsorption and desorption at 300 °C.

Fig. 5. (a) Uptake rate of MAc in pyridine-modified H-MOR measured by IGA (50 °C, 1 mbar). (b) Initial uptake rate. The scatters represent the experimental data while dash lines are fitting results by Eq. (2).

Fig. 6. (a) DME conversion during DME carbonylation over pyridine-modified H-MOR catalysts. (b) Hydrocarbon by-products (HCx) selectivity. Reaction conditions: 200 °C, 2 MPa, GHSV = 3600 mL/g/h. DME/CO/N2 = 5/35/60.

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无机体系合成纳米丝光沸石组装体及其优异的二甲醚羰基化催化性能

Organic-free synthesis of MOR nanoassemblies with excellent DME carbonylation performance

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