菱沸石分子筛膜的合成调控与气体分离研究进展

doi:10.15541/jim20200555

无机材料学报 ›› 2021, Vol. 36 ›› Issue (6): 579-591.DOI: 10.15541/jim20200555

所属专题：【虚拟专辑】分离膜，复相陶瓷(2020~2021)

菱沸石分子筛膜的合成调控与气体分离研究进展

李子宜¹(), 章佳佳¹, 邹小勤², 左家玉¹, 李俊¹, 刘应书¹(), 裴有康³^,⁴

1.北京科技大学能源与环境工程学院, 北京 100083
2.东北师范大学化学学院, 长春 130024
3.香港中文大学(深圳) 理工学院, 深圳 518172
4.明尼苏达大学机械工程系, 明尼阿波利斯 55455, 美国

收稿日期:2020-09-22 修回日期:2020-10-27 出版日期:2021-06-20 网络出版日期:2020-12-10
通讯作者: 刘应书, 教授. E-mail: ysliu@ustb.edu.cn
作者简介:李子宜(1990-), 男, 副教授. E-mail: ziyili@ustb.edu.cn
基金资助:
国家自然科学基金青年项目(21808012);中央高校基本科研业务费(FRF-IDRY-19-025)

Synthesis and Gas Separation of Chabazite Zeolite Membranes

LI Ziyi¹(), ZHANG Jiajia¹, ZOU Xiaoqin², ZUO Jiayu¹, LI Jun¹, LIU Yingshu¹(), PUI David Youhong³^,⁴

1. School of Energy and Environmental Engineering, University of Science and Technology Beijing, Beijing 100083, China
2. Institute of Chemistry, Northeast Normal University, Changchun 130024, China
3. School of Science and Engineering, The Chinese University of Hong Kong, Shenzhen 518172, China
4. Department of Engineering, University of Minnesota, Minneapolis 55455, USA

Received:2020-09-22 Revised:2020-10-27 Published:2021-06-20 Online:2020-12-10
Contact: LIU Yingshu, professor. E-mail: ysliu@ustb.edu.cn
About author:LI Ziyi(1990-), male, associate professor. E-mail: ziyili@ustb.edu.cn
Supported by:
National Natural Science Foundation of China(21808012);Fundamental Research Funds for the Central Universities(FRF-IDRY-19-025)

摘要/Abstract

摘要：

菱沸石(Chabazite, CHA)分子筛膜因其八元环小孔(0.38 nm)三维孔道结构、可调的表面特性、较高的材料稳定性与制备可重复性, 使其在轻质气体分离方面具有优异性能, 近年来逐渐成为分子筛膜研究热点之一。本综述介绍了两种CHA分子筛膜(SAPO-34膜、SSZ-13膜)的基本特性, 对比了CHA分子筛膜的合成方法(原位合成法、二次生长法、微波加热法)优缺点及其应用现状, 并重点针对主流的二次生长法制备SSZ-13膜与SAPO-34膜过程中关键条件对薄膜质量的影响规律进行了详细阐述, 包括铺种条件(载体种类、晶种类别、铺种方式), 水热合成条件(晶化时间、晶化温度、含水量、硅铝比、模板剂、阳离子种类)与煅烧方式(常规煅烧、分段煅烧、快速热处理), 经细化分析总结出上述两种膜的优选合成条件; 并进一步汇总了CHA分子筛膜表面化学调控(硅铝比调控、阳离子交换、杂原子替换、氨基功能化、表面修饰)对气体分离增强的策略, 总结了CHA分子筛膜在各种气体体系中的分离特点与单组分气体渗透特性。最后, 对CHA分子筛膜今后的发展和应用前景进行了展望。

关键词: 分子筛膜, 菱沸石, 合成制备, 表面化学调控, 气体分离, 综述

Abstract:

Chabazite (CHA) zeolite membranes exhibit superior performances in light gas separations owing to the eight-membered ring channel structure with small pore size (0.38 nm), adjustable surface characteristics, and high material stability and preparation reproducibility, and have gradually become one of the hot spots of zeolite membrane research in recent years. This review article first introduces the basic characteristics, the two typical CHA zeolite membranes (SAPO-34 and SSZ-13 membranes), then compares the synthesis and preparation methods of CHA zeolite membranes (in-situ synthesis, secondary growth synthesis, microwave heating methods) and analyzes their advantages and disadvantages in application status. The influences of their key synthesis conditions of the secondary growth as the mainstream synthesis method on the qualities of SSZ-13 and SAPO-34 membranes have been elaborated in detail, mainly including 1) the seeding conditions, such as carrier type, seeding crystal and seeding approach; 2) the hydrothermal synthesis conditions, such as crystallization time and temperature, water content, silica-to-alumina ratio, structure directing agent, and cation type; 3) the calcination approaches, such as conventional calcination, staged calcination, and rapid heating treatments. After comparative analysis, the preferred synthesis of the above two typical CHA zeolite membranes are proposed. Furthermore, the modulation of membrane surface chemistry is discussed for the enhancement in gas separation, such as silica-to-alumina ratio adjustment, ion exchange, heteroatom substitution, amino-group functionalization, and surface modification. The detailed characteristics of gas separation in various gas mixture systems and the permeation properties of different single gases on CHA zeolite membranes are analyzed and summarized as well. Finally, the future development of CHA zeolite membranes is prospected.

Key words: zeolite membrane, chabazite, synthesis, surface chemistry modulation, gas separation, review

中图分类号:

TQ127

李子宜, 章佳佳, 邹小勤, 左家玉, 李俊, 刘应书, 裴有康. 菱沸石分子筛膜的合成调控与气体分离研究进展[J]. 无机材料学报, 2021, 36(6): 579-591.

LI Ziyi, ZHANG Jiajia, ZOU Xiaoqin, ZUO Jiayu, LI Jun, LIU Yingshu, PUI David Youhong. Synthesis and Gas Separation of Chabazite Zeolite Membranes[J]. Journal of Inorganic Materials, 2021, 36(6): 579-591.

图/表 10

参考文献 106

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Method	Advantage	Disadvantage	Status of use
In-situ synthesis	① Simple production equipment ② Easy to use	① Low success rate ② Long synthesis time ③ Difficult to control	Less research, basically used for the synthesis of SAPO-34 membrane
Secondary growth	① Simple production equipment ② High success rate ③ Short synthesis time	① Tedious steps	More research, conducive to large-scale mass production
Microwave heating	① High success rate ② Short synthesis time	① Tedious steps ② High equipment cost ③ High energy consumption	New method, still in basic research stage

Method	Advantage	Disadvantage	Status of use
In-situ synthesis	① Simple production equipment ② Easy to use	① Low success rate ② Long synthesis time ③ Difficult to control	Less research, basically used for the synthesis of SAPO-34 membrane
Secondary growth	① Simple production equipment ② High success rate ③ Short synthesis time	① Tedious steps	More research, conducive to large-scale mass production
Microwave heating	① High success rate ② Short synthesis time	① Tedious steps ② High equipment cost ③ High energy consumption	New method, still in basic research stage

Influencing factors		SSZ-13	SAPO-34
Seed conditions	Support	α-Al₂O₃, mullite	α-Al₂O₃
	Seed crystal	Ball milled nano seeds	Flake nano seeds
	Seeding method	Dip coating	Wipe, electrophoretic deposition
Hydrothermal synthesis conditions	Formula (structure directing agent, Si/Al, water content, cationic species)	Non-pure silica: 1SiO₂ : (5-100)Al₂O₃ : (0.1-0.2)NaOH : (0-0.06)KOH(Oriented growth regulation) : (0.05-0.6)TMAdaOH : (0-0.05)TEAOH : (40-120)H₂O Pure silica : 1SiO₂ : (0.5-1.4)TMAdaOH : (0.5-1.4)HF : (3-6)H₂O	1Al₂O₃ : (1-2)P₂O₅ : (0.3-0.6)SiO₂ : (1-4)TEAOH : (0-1.6)DPA : (55-400)H₂O
	Temperature	160-170 ℃	180-230 ℃
	Time	24-72 h	6-30 h
Calcination conditions	Conventional calcination	400-550 ℃ (6-12 h), temperature rise and fall rate (0.2-1) ℃/min	400-480 ℃ (4-10 h), temperature rise and fall rate (0.5- 2) ℃/min
Calcination conditions	Rapid heat treatment	700-1000 ℃ (0.5-2 min)+conventional calcination	700 ℃ (1-5 min)+ conventional calcination

Influencing factors		SSZ-13	SAPO-34
Seed conditions	Support	α-Al₂O₃, mullite	α-Al₂O₃
	Seed crystal	Ball milled nano seeds	Flake nano seeds
	Seeding method	Dip coating	Wipe, electrophoretic deposition
Hydrothermal synthesis conditions	Formula (structure directing agent, Si/Al, water content, cationic species)	Non-pure silica: 1SiO₂ : (5-100)Al₂O₃ : (0.1-0.2)NaOH : (0-0.06)KOH(Oriented growth regulation) : (0.05-0.6)TMAdaOH : (0-0.05)TEAOH : (40-120)H₂O Pure silica : 1SiO₂ : (0.5-1.4)TMAdaOH : (0.5-1.4)HF : (3-6)H₂O	1Al₂O₃ : (1-2)P₂O₅ : (0.3-0.6)SiO₂ : (1-4)TEAOH : (0-1.6)DPA : (55-400)H₂O
	Temperature	160-170 ℃	180-230 ℃
	Time	24-72 h	6-30 h
Calcination conditions	Conventional calcination	400-550 ℃ (6-12 h), temperature rise and fall rate (0.2-1) ℃/min	400-480 ℃ (4-10 h), temperature rise and fall rate (0.5- 2) ℃/min
Calcination conditions	Rapid heat treatment	700-1000 ℃ (0.5-2 min)+conventional calcination	700 ℃ (1-5 min)+ conventional calcination

Serial number	Ref.	Thickness/μm	Temperature/℃	Pressure/MPa	Gas separation, X/Y	X permeance/ (×10^-8, mol·m^-2·s^-1·Pa^-1)	Separation selectivity, X/Y
1	Kalipcilar^[7]	10-40	25	-	H₂/n-C₄H₁₀	14	8.7
2	Zheng^[27]	10	30	0.2	C₂H₄/C₂H₆	0.29	11
3	Feng^[72]	4.3	20	0.138	Kr/Xe	12	35
4	Yang^[82]	3.7	22	-	H₂/C₃H₈	8.4	810

菱沸石分子筛膜的合成调控与气体分离研究进展

Synthesis and Gas Separation of Chabazite Zeolite Membranes

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Serial number	Ref.	Thickness/μm	Temperature/℃	Pressure/MPa	Gas separation, X/Y	X permeance/ (×10^-7, mol·m^-2·s^-1·Pa^-1)	Separation selectivity, X/Y
1	Kosinov^[14]	4-6	20	0.6	CO₂/CH₄	2.5	42
1	Kosinov^[14]	4-6	20	0.6	CO₂/N₂	2.5	12
2	Wu^[21]	6-8	20	0.27	CO₂/CH₄	2.1	178
2	Wu^[21]	6-8	20	0.27	N₂/CH₄	0.18	9
3	Song^[29]	6	25	0.2	CO₂/CH₄	5.6	56.5
3	Song^[29]	6	25	0.2	N₂/CH₄	0.89	10
4	Li^[31]	2	25	0.2	CO₂/CH₄	1.16	213
4	Li^[31]	2	25	0.2	N₂/CH₄	1.07	13
5	Yu^[57]	1.5	-24	0.9	CO₂/CH₄	79	76
6	Karakiliç^[64]	2-4	22	0.2	CO₂/CH₄	2.6	176
7	Qiu^[66]	0.44	20	0.14	CO₂/CH₄	48	153
8	Kida^[71]	-	40	0.1	CO₂/CH₄	17	54
8	Kida^[71]	-	40	0.1	H₂/CH₄	11	34
9	Tang^[81]	10	20	0.2	CO₂/CH₄	9.3	208
10	Kida^[83]	5	25	0.1	CO₂/CH₄	40	130
11	Imasaka^[98]	3	40	0.3	CO₂/CH₄	15	115
12	Maghsoudi^[99]	20	30	0.1	CO₂/CH₄	0.34	21.6
13	Yu^[100]	1.3	3	0.9	CO₂/CH₄	84	47
14	Li^[5]	5	80	0.14	CO₂/CH₄	2.0	270
15	Li^[19]	-	24	0.138	CO₂/CH₄	1.6	67
16	Carreon^[23]	-	22	0.138	CO₂/CH₄	3.8	170
17	Venna^[36]	-	22	0.138	CO₂/CH₄	5.0	245
17	Venna^[36]	-	22	0.138	CO₂/N₂	2.1	39
18	Huang^[40]	2	22	0.074	N₂/CH₄	4.93	11.3
19	Chen^[41]	2-3	25	0.1	CO₂/CH₄	1.18	160
20	Chang^[43]	-	-	4	CO₂/CH₄	6.1	88
21	Liu^[48]	3	30	0.1	CO₂/CH₄	12	95
22	Rehman^[53]	-	80	0.4	CO₂/CH₄	47.3	65
23	Liu^[55]	7-15	25	0.1	CO₂/N₂	18.5	29.8
24	Li^[74]	4-6	22	7	CO₂/CH₄	0.4	100
25	Zhang^[78]	-	20	4.6	CO₂/CH₄	8.2	55
26	Noble^[101]	-	22	0.14	CO₂/CH₄	1.2	170
27	Shi^[102]	2-4	22	0.14	CO₂/CH₄	23.2	186
28	Shi^[103]	4-5	22	0.14	CO₂/CH₄	16.8	256
29	Li^[104]	3	-	4	CO₂/CH₄	13.2	62
30	Bai^[105]	0.8	-	0.2	CO₂/CH₄	25.3	70

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