Construction of 6FDA-based polyimide carbon molecular sieve membranes for gas separation and its application

doi:10.11949/0438-1157.20221678

Abstract

Abstract:

Polymer gas separation membranes have the advantages of low price and easy processing, but there are problems such as gas separation performance is difficult to meet the industrial requirements, and the aging resistance and structural stability are poor. Carbon molecular sieve (CMS) membranes have high mechanical properties, high heat and chemical corrosion resistance, suitable gas transport paths, heteroatomic structure with good affinity for gas molecules and pore size structure with strong molecular discrimination, exhibiting excellent gas separation performance, thus receiving wide attention and being considered as a promising gas separation membrane. The 6FDA-based polyimide not only has larger rigidity and restricted conformation, but also has larger free volume, adjustable molecular structure, good pore formation and high carbon residue, and the gas separation performance of as-prepared CMS membranes are better than that prepared by other precursors, which is favored by the academic and industrial sectors. This paper introduces the structural design principle of CMS membranes precursors, carbonization mechanism during the pyrolysis processes and the control of microstructure, the influence of carbon structure on gas separation performance, the gas transport mechanism in the membrane, and the application of CMS membranes prepared by 6FDA-based polyimide in gas separation. In combination with our own scientific research practice, the strategy of the structure design and preparation of CMS membranes prepared by 6FDA-based polyimide is proposed to provide new ideas for the future application of CMS membranes in gas separation.

Key words: carbon molecular sieve membranes, 6FDA polyimide, gas, separation, transport processes

摘要：

高分子气体分离膜具有价格低和易加工等优点，但存在气体分离性能难以满足工业要求，以及耐老化性能和结构稳定性差等问题。炭分子筛膜不仅具有高力学性能，高耐热、耐化学腐蚀性能，而且存在适合气体传递的路径、对气体分子亲和性好的杂原子结构，以及分子辨识能力强的孔尺寸，表现出优异的气体分离性能，因而受到广泛的关注，被认为是最具应用前景的气体分离膜。6FDA型聚酰亚胺不仅具有较大的刚性和受限制的构象，且自由体积较大、分子结构可调、成孔性好和残炭量高，制备的炭分子筛膜的气体分离性能优于其他前体，受到学术界和工业部门的青睐。本文主要介绍了炭分子筛膜前体的结构设计原理，在热解过程中的炭化机理和微观结构的控制，炭结构对气体分离性能的影响，气体在膜中的传递机理，以及由6FDA型聚酰亚胺制备的炭分子筛膜在气体分离中的应用。结合科研实际，提出了6FDA型聚酰亚胺炭分子筛膜结构设计和制备的想法，为未来炭分子筛膜在气体分离中应用提供新的思路。

关键词: 炭分子筛膜, 6FDA型聚酰亚胺, 气体, 分离, 传递过程

CLC Number:

TQ 028.8

Rong WANG, Yonghong WANG, Xinru ZHANG, Jinping LI. Construction of 6FDA-based polyimide carbon molecular sieve membranes for gas separation and its application[J]. CIESC Journal, 2023, 74(4): 1433-1445.

王荣, 王永洪, 张新儒, 李晋平. 6FDA型聚酰亚胺炭分子筛气体分离膜的构筑及其应用[J]. 化工学报, 2023, 74(4): 1433-1445.

Figures/Tables 13

Table 1 Physicochemical properties of 6FDA-based polyimides with different diamine

聚酰亚胺	密度/(g/cm³）	T_g/℃	链间距/nm	自由体积/(cm³/g)	文献
6FDA-ODA	1.432	304	0.56	0.1142	[24]
6FDA-MDA	1.400	304	0.56	0.1143	[24]
6FDA-m-PD	1.474	298	—	0.160	[25]
6FDA-p-PD	1.473	351	—	0.161	[25]
6FDA-DABA	1.590	327	0.53	0.153	[26-27]

Fig.1 Synthesis of 6FDA-triptycene polyimide[28]

Fig.2 Chemical structure of 6FDA

Fig.3 Equation for the synthesis of 6FDA-based polyimide

Fig.4 Pyrolysis device used to generate carbon molecular sieve membranes[39]

Fig.5 Transformation from polyimide precursors to amorphous carbon molecular sieve membranes[41]

Fig.6 A simplified idealized slit-like pore structures and bimodal distribution of pores in carbon molecular sieve membranes[22]

Fig.7 (a) Undoped structure when pyrolyzed without oxygen; (b) Optimal selective structure with adequate amount of oxygen doped; (c) Overdoped structure when slightly higher oxygen was introduced during pyrolysis[39]

Fig.8 Gas transport mechanisms in carbon molecular sieve membranes[49]

Fig.9 Performance of 6FDA-mPDA/ DABA(3∶2) carbon molecular sieve membranes for CO2/CH4 separation[44]

Fig.10 Structure of thermally crosslinkable brominated 6FDA-based polyimide (BMPI) and carbon molecular sieve membranes performance for CO2/CH4 separation[62]

Fig.11 (a) The structure of the carbon molecular sieve membranes; (b) Structural changes in carbon molecular sieve membranes after being hyperaged below and above 250 °C; (c) Distribution of ultramicropores in carbon molecular sieve membranes[66]

Fig.12 Separation performance of XS1 (azeotropic imidization) and XS4 (chemical imidization) and comparison to 2008 and 2015 Robeson upper bound[75]

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