P25杂化炭膜的制备及其气体分离性能

doi:10.3724/SP.J.1077.2013.12352

无机材料学报 ›› 2013, Vol. 28 ›› Issue (5): 485-489.DOI: 10.3724/SP.J.1077.2013.12352 CSTR: 32189.14.SP.J.1077.2013.12352

P25杂化炭膜的制备及其气体分离性能

孙美悦¹, 李琳^1.2, 张萍萍¹, 徐家家¹, 郁焦竹¹, 王同华^1.2

(大连理工大学化工学院, 1. 精细化工国家重点实验室炭材料研究室; 2. 膜科学与技术研究开发中心, 大连 116024)

收稿日期:2012-05-16 修回日期:2012-07-12 出版日期:2013-05-10 网络出版日期:2013-04-22
作者简介:孙美悦(1987–), 女, 硕士研究生.
基金资助:
国家自然科学基金(20776024, 20976021, 20836006, 21176036);国家863计划项目(2009AA03Z215, 2012AA03A611)

Preparation and Gas Separation Performance of P25 Hybrid Carbon Membranes

SUN Mei-Yue¹, LI Lin^1.2, ZHANG Ping-Ping¹, XU Jia-Jia¹, YU Jiao-Zhu¹, WANG Tong-Hua^1.2

(1. Carbon Research Laboratory, State Key Laboratory of Fine Chemicals, School of Chemical Engineering, Dalian University of Technology, Dalian 116024, China; 2. R&D Center of Membrane Science, School of Chemical Engineering, Dalian University of Technology, Dalian 116024, China)

Received:2012-05-16 Revised:2012-07-12 Published:2013-05-10 Online:2013-04-22
About author:SUN Mei-Yue.
Supported by:
National Natural Science Foundation of China (20776024, 20976021, 20836006, 21176036);863 Program (2009AA03Z215, 2012AA03A611)

摘要/Abstract

摘要：

通过在炭膜前驱体中添加纳米二氧化钛-P25粒子制备了P25杂化炭膜, 并采用TG、SEM、TEM、XRD、气体渗透性能测试等表征方法探讨添加P25纳米粒子对杂化炭膜的热解过程、微观结构及气体渗透性能的影响。结果表明, P25纳米粒子的加入提高了聚合物膜的热稳定性; P25粒子因团聚形成一定的堆积间隙并与炭基体形成了界面孔隙。气体渗透性能测试表明, P25的引入显著地提高了气体渗透通量, 并随添加量增加提高而更加明显, 气体选择性略有降低, 分离机理仍以分子筛分为主; 炭化终温的提高可以显著增加气体选择性, 但气体渗透性有所降低。当P25添加量为20wt%, 炭化终温为700℃时, 所制备的杂化炭膜其H₂、CO₂、O₂、N₂、CH₄气体渗透性分别为1769.2、1558.6、410.2、55.5和26.8 Barrer。

关键词: 炭膜, 气体分离, 杂化炭膜, 二氧化钛

Abstract:

P25 hybrid carbon membranes were prepared by adding the commercial P25 particles into the precursor. Effects of P25 particles on the pyrolysis, carbon structure and gas separation performance of hybrid carbon membranes were characterized by means of TG, SEM, TEM and XRD. The results indicate that the thermal stability of polymer precursor is improved by the incorporation of P25 particles. Gas separation performances of hybrid carbon membrane are greatly improved with the addition of P25 particles due to the accumulate voids formed by the agglomeration of P25 particles and interfacial pores formed between P25 particles and carbon matrix. Molecular sieve mechanism is still conformed in the gas separation of hybrid carbon membranes. Gas permeability increases and gas selectivity remains with the increase of P25 loading. And the gas permeability reduces and gas selectivity increases as final carbonization temperature rises. The permeabilities of H₂, CO₂, O₂, N₂ and CH₄ are 1769.2, 1558.6, 410.2, 55.5, 26.8 Barrer, respectively, for the hybrid carbon membrane prepared with 20wt% P25 loading and at 700℃ carbonization temperature.

Key words: carbon membrane, gas separation, hybrid carbon membrane, titanium dioxide

中图分类号:

TQ174

孙美悦, 李琳, 张萍萍, 徐家家, 郁焦竹, 王同华. P25杂化炭膜的制备及其气体分离性能[J]. 无机材料学报, 2013, 28(5): 485-489.

SUN Mei-Yue, LI Lin, ZHANG Ping-Ping, XU Jia-Jia, YU Jiao-Zhu, WANG Tong-Hua. Preparation and Gas Separation Performance of P25 Hybrid Carbon Membranes[J]. Journal of Inorganic Materials, 2013, 28(5): 485-489.

图/表 8

图1 恒压力变体积法气体渗透性能测试装置图

Fig. 1 Gas permeability test instrument by constant pressure- variable volume method

图2 聚酰胺酸及P25杂化膜的热失重曲线图

Fig. 2 Thermal gravimetry curves of polyamic acid film and P25 hybrid polyamic acid film

图3 不同浓度P25杂化炭膜XRD图谱

Fig. 3 XRD patterns of P25 hybrid carbon membrane with different P25 loadings

图4 不同炭化终温P25杂化炭膜XRD图谱

Fig. 4 XRD patterns of P25 hybrid carbon membrane carbonized at different temperatures

图5 杂化炭膜断面SEM照片

Fig. 5 Cross sectional SEM images of P25 hybrid carbon membrane

图6 杂化炭膜TEM照片

Fig. 6 TEM images of P25 particles and P25 hybrid carbon membrane

图7 不同P25添加量杂化炭膜气体分离性能

Fig. 7 Gas separation performance of carbon membrane with different P25 loadings (a) Gas permeability; (b) Gas selectivity

图8 不同炭化终温P25杂化炭膜气体分离性能

Fig. 8 Gas separation performance of P25 hybrid carbon membrane with different carbonization temperatures (a) Gas permeability; (b) Gas selectivity

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P25杂化炭膜的制备及其气体分离性能

Preparation and Gas Separation Performance of P25 Hybrid Carbon Membranes

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