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Article(id=1210601627250200648, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1210601623135581115, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2024.10.007, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1714060800000, receivedDateStr=2024-04-26, revisedDate=1718294400000, revisedDateStr=2024-06-14, acceptedDate=null, acceptedDateStr=null, onlineDate=1766559519827, onlineDateStr=2025-12-24, pubDate=1729353600000, pubDateStr=2024-10-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1766559519827, onlineIssueDateStr=2025-12-24, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1766559519827, creator=13701087609, updateTime=1766559519827, updator=13701087609, issue=Issue{id=1210601623135581115, tenantId=1146029695717560320, journalId=1149653034449285133, year='2024', volume='57', issue='10', pageStart='1', pageEnd='141', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1766559518846, creator=13701087609, updateTime=1766564021205, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1210620507448275814, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1210601623135581115, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1210620507448275815, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1210601623135581115, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=53, endPage=59, ext={EN=ArticleExt(id=1210601627891929165, articleId=1210601627250200648, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Preparation and properties of copolymerized polyimide based thermally rearranged gas separation membranes, columnId=1203281640207393262, journalTitle=Insulating Materials, columnName=Special Issue on High Performance Polyimide Materials, runingTitle=null, highlight=null, articleAbstract=

Four kinds of copolymerized polyimide (PI) membranes were prepared through thermal imidization method after solution polymerization between two kinds of self-made diamine monomers 9,9′-bis[4-(4-amino-3-hydroxyphenoxy) phenyl] fluorene (BAHPPF) and 4-(4′-tertbutyl)phenyl-2,6-di(4′-aminophenyl)pyridine (TPAPP) and 4,4′-(hexafluoroisopropene)phthalic anhydride (6FDA), and the molar ratio of BAHPPF and TPAPP is 9∶1, 8∶2, 7∶3, and 6∶4, respectively. Then the corresponding copolymerized thermal rearrangement (TR) membranes were obtained after heat treatment at 450℃. The thermal, mechanical, and gas separation properties of the membrane materials were measured. The results show that the glass transition temperature of the copolymerized PI membranes is around 350℃. As the molar ratio of TPAPP increases, the tensile strength of the copolymerized PI membranes decreases. After thermal rearrangement, the mechanical properties of the copolymerized TR membranes decrease significantly, while the d values increase. When the molar ratio of BAHPPF and TPAPP is 8∶2, the copolymerized TR membrane exhibits the best gas permeability, and the permeation coefficients for H2, CO2, O2, and N2, is 346.4, 304.5, 72.43, and 13.34 Barrer respectively. Meanwhile, the O2/N2 separation performance of the four TR membranes is close to the Robeson upper limit in 2008.

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采用两种自制的二胺单体9,9′-双[4-(4-氨基-3-羟基苯氧基)苯基]芴（BAHPPF）和4-(4′-叔丁基)苯基-2,6-二(4′-氨基苯基)吡啶（TPAPP），分别以9∶1、8∶2、7∶3、6∶4的物质的量之比混合之后，与4,4′-(六氟异丙烯)二酞酸酐（6FDA）进行溶液聚合，通过热酰亚胺化法制备出4种共聚聚酰亚胺（PI）膜。然后经450℃热处理制得相应的共聚热重排（TR）膜。对膜材料的热性能、力学性能和气体分离性能进行了测试。结果表明：共聚PI膜的玻璃化转变温度约为350℃。随着TPAPP摩尔分数的增加，共聚PI膜的拉伸强度有所下降。热重排后，共聚TR膜的力学性能明显降低，但晶面间距d值显著增大。当BAHPPF与TPAPP物质的量之比为8∶2时，共聚TR膜的气体渗透性最好，对H2、CO2、O2和N2的渗透系数分别为346.40、304.50、72.43、13.34 Barrer。同时，4种TR膜的O2/N2分离性能均接近2008年的Robeson上限。

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鲁云华（1977-），女（汉族），辽宁辽阳人，教授，主要从事功能性聚酰亚胺材料的研究；
赵洪斌（1977-），男（汉族），辽宁本溪人，讲师，主要从事高性能聚酰亚胺材料的研究。
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吕鹏威（1998-），男（汉族），河南商丘人，硕士生，主要从事功能性聚酰亚胺材料的改性研究。

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吕鹏威（1998-），男（汉族），河南商丘人，硕士生，主要从事功能性聚酰亚胺材料的改性研究。

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吕鹏威（1998-），男（汉族），河南商丘人，硕士生，主要从事功能性聚酰亚胺材料的改性研究。

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Polyimide membrane structure and gas permeability[J]. Chinese Polymer Bulletin,2022(5):27-37., articleTitle=Polyimide membrane structure and gas permeability, refAbstract=null), Reference(id=1218266786370339734, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210601627250200648, doi=null, pmid=null, pmcid=null, year=2021, volume=61, issue=11, pageStart=2782, pageEnd=2791, url=null, language=null, rfNumber=[24], rfOrder=30, authorNames=PATELH D, ACHARYAN K, journalName=Polymer Engineering & Science, refType=null, unstructuredReference=PATELH D, ACHARYAN K. Synthesis and characteristics of HAB-6FDA thermally rearranged polyimide nanocomposite membranes[J]. 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样品厚度/µmTg/℃TTR/℃拉伸强度/MPa杨氏模量/GPa断裂伸长率/%
PIBT-9:161348414119.8±2.03.7±0.13.9±0.1
PIBT-8:258351410109.3±1.03.3±0.23.7±0.2
PIBT-7:35535340390.1±2.03.2±0.23.4±0.1
PIBT-6:45735540181.8±3.02.6±0.13.2±0.2
), ArticleFig(id=1218266781664330503, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210601627250200648, language=CN, label=表1, caption=

共聚PI膜的力学和热学性能

, figureFileSmall=null, figureFileBig=null, tableContent=
样品厚度/µmTg/℃TTR/℃拉伸强度/MPa杨氏模量/GPa断裂伸长率/%
PIBT-9:161348414119.8±2.03.7±0.13.9±0.1
PIBT-8:258351410109.3±1.03.3±0.23.7±0.2
PIBT-7:35535340390.1±2.03.2±0.23.4±0.1
PIBT-6:45735540181.8±3.02.6±0.13.2±0.2
), ArticleFig(id=1218266781769188109, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210601627250200648, language=EN, label=Table 2, caption=Gas separation performance of copolymerized TR membranes, figureFileSmall=null, figureFileBig=null, tableContent=
样品渗透系数/Barrer理想选择性
H2CO2O2N2CO2/N2O2/N2H2/N2
TRBT-9:1253.6223.152.418.8525.215.9228.65
TRBT-8:2346.4304.572.4313.3422.825.4325.97
TRBT-7:3304.8276.665.8411.9223.205.5225.57
TRBT-6:4210.5243.648.867.9826.386.1230.52
TR(HAB-6FDA)450℃[24]514.5412.5101.526.515.53.819.4
TR(BHAPPP-PMDA)[25]150.60162.1135.417.2422.394.8920.80
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共聚TR膜的气体分离性能

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样品渗透系数/Barrer理想选择性
H2CO2O2N2CO2/N2O2/N2H2/N2
TRBT-9:1253.6223.152.418.8525.215.9228.65
TRBT-8:2346.4304.572.4313.3422.825.4325.97
TRBT-7:3304.8276.665.8411.9223.205.5225.57
TRBT-6:4210.5243.648.867.9826.386.1230.52
TR(HAB-6FDA)450℃[24]514.5412.5101.526.515.53.819.4
TR(BHAPPP-PMDA)[25]150.60162.1135.417.2422.394.8920.80
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共聚聚酰亚胺基热重排气体分离膜的制备与性能
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吕鹏威 , 鲁云华 , 雷敏 , 肖国勇 , 赵洪斌 , 胡知之
绝缘材料 | 高性能聚酰亚胺材料专题 2024,57(10): 53-59
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绝缘材料 | 高性能聚酰亚胺材料专题 2024, 57(10): 53-59
共聚聚酰亚胺基热重排气体分离膜的制备与性能
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吕鹏威, 鲁云华, 雷敏, 肖国勇, 赵洪斌, 胡知之
作者信息
  • 辽宁科技大学 化学工程学院，辽宁 鞍山 114051

    • 吕鹏威（1998-），男（汉族），河南商丘人，硕士生，主要从事功能性聚酰亚胺材料的改性研究。

通讯作者:

鲁云华（1977-），女（汉族），辽宁辽阳人，教授，主要从事功能性聚酰亚胺材料的研究；
赵洪斌（1977-），男（汉族），辽宁本溪人，讲师，主要从事高性能聚酰亚胺材料的研究。
Preparation and properties of copolymerized polyimide based thermally rearranged gas separation membranes
Pengwei LÜ, Yunhua LU, Min LEI, Guoyong XIAO, Hongbin ZHAO, Zhizhi HU
Affiliations
  • School of Chemical Engineering, University of Science and Technology Liaonong, Anshan 114051, China
出版时间: 2024-10-20 doi: 10.16790/j.cnki.1009-9239.im.2024.10.007
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摘要
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采用两种自制的二胺单体9,9′-双[4-(4-氨基-3-羟基苯氧基)苯基]芴（BAHPPF）和4-(4′-叔丁基)苯基-2,6-二(4′-氨基苯基)吡啶（TPAPP），分别以9∶1、8∶2、7∶3、6∶4的物质的量之比混合之后，与4,4′-(六氟异丙烯)二酞酸酐（6FDA）进行溶液聚合，通过热酰亚胺化法制备出4种共聚聚酰亚胺（PI）膜。然后经450℃热处理制得相应的共聚热重排（TR）膜。对膜材料的热性能、力学性能和气体分离性能进行了测试。结果表明：共聚PI膜的玻璃化转变温度约为350℃。随着TPAPP摩尔分数的增加，共聚PI膜的拉伸强度有所下降。热重排后，共聚TR膜的力学性能明显降低，但晶面间距d值显著增大。当BAHPPF与TPAPP物质的量之比为8∶2时，共聚TR膜的气体渗透性最好，对H2、CO2、O2和N2的渗透系数分别为346.40、304.50、72.43、13.34 Barrer。同时，4种TR膜的O2/N2分离性能均接近2008年的Robeson上限。

共聚聚酰亚胺  /  热重排  /  气体分离膜  /  吡啶环  /  芴基

Four kinds of copolymerized polyimide (PI) membranes were prepared through thermal imidization method after solution polymerization between two kinds of self-made diamine monomers 9,9′-bis[4-(4-amino-3-hydroxyphenoxy) phenyl] fluorene (BAHPPF) and 4-(4′-tertbutyl)phenyl-2,6-di(4′-aminophenyl)pyridine (TPAPP) and 4,4′-(hexafluoroisopropene)phthalic anhydride (6FDA), and the molar ratio of BAHPPF and TPAPP is 9∶1, 8∶2, 7∶3, and 6∶4, respectively. Then the corresponding copolymerized thermal rearrangement (TR) membranes were obtained after heat treatment at 450℃. The thermal, mechanical, and gas separation properties of the membrane materials were measured. The results show that the glass transition temperature of the copolymerized PI membranes is around 350℃. As the molar ratio of TPAPP increases, the tensile strength of the copolymerized PI membranes decreases. After thermal rearrangement, the mechanical properties of the copolymerized TR membranes decrease significantly, while the d values increase. When the molar ratio of BAHPPF and TPAPP is 8∶2, the copolymerized TR membrane exhibits the best gas permeability, and the permeation coefficients for H2, CO2, O2, and N2, is 346.4, 304.5, 72.43, and 13.34 Barrer respectively. Meanwhile, the O2/N2 separation performance of the four TR membranes is close to the Robeson upper limit in 2008.

copolymerized polyimide  /  thermal rearrangement  /  gas separation membrane  /  pyridine ring  /  fluorenyl
吕鹏威, 鲁云华, 雷敏, 肖国勇, 赵洪斌, 胡知之. 共聚聚酰亚胺基热重排气体分离膜的制备与性能. 绝缘材料, 2024 , 57 (10) : 53 -59 . DOI: 10.16790/j.cnki.1009-9239.im.2024.10.007
Pengwei LÜ, Yunhua LU, Min LEI, Guoyong XIAO, Hongbin ZHAO, Zhizhi HU. Preparation and properties of copolymerized polyimide based thermally rearranged gas separation membranes[J]. Insulating Materials, 2024 , 57 (10) : 53 -59 . DOI: 10.16790/j.cnki.1009-9239.im.2024.10.007
正文
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0 引言
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气体膜分离技术是利用不同种类气体分子在膜材料中的渗透速率和选择性差异来实现分离的一种“绿色分离技术”，由于具有选择性高、操作简单和能耗低等特点，在化工、环境和医药等领域有着重要应用[1-3]。膜材料是该技术的关键，因此提高分离膜材料的分离性能一直是该领域研究人员的目标。在膜材料中，聚酰亚胺（PI）因其优异的热稳定性和化学稳定性以及高气体分离选择性而受到广泛关注[4]。然而，低渗气性的缺陷限制了传统聚酰亚胺在气体分离膜中的应用。因此，为获得性能更加优异的气体分离膜，人们一直致力于开发新型PI膜材料。
聚酰亚胺材料具有灵活的结构可设计性，通过在二酐或二胺单体中引入刚性扭曲结构、大体积取代基、非对称结构等，可以有效增加分子链间的距离，减小分子链间的相互作用，增大自由体积，从而提高膜材料的气体渗透通量[5-6]。袁清等[7]通过2,3,6,7,-四甲酸三蝶烯二酐单体与2,2-双三氟甲基联苯胺的缩聚反应，制备了一种具有微孔结构的三蝶烯聚酰亚胺（T-PI）。三蝶烯基团的引入使T-PI易溶于多种常用的有机溶剂，且热稳定性能良好。而且T-PI膜对H2和CO2的渗透系数分别为518 Barrer和810 Barrer，对CO2/CH4的理想选择性为21.9，接近2008年的Robeson上限，说明具有较好的分离性能[8]。
近年来，由含羟基聚酰亚胺衍生的热重排（TR）聚合物由于具有独特的微孔结构，显示出高气体渗透通量和适中的选择性，在气体分离领域吸引了人们的广泛关注。DU P Y等[9]利用3,3-二氨基酚酞与4,4′-(六氟异亚丙基)二邻苯二甲酸酐（6FDA）聚合，经化学亚胺化合成聚酰亚胺，热处理后得到具有交联结构的TR聚合物。研究结果表明，400℃下制得的TR膜对CO2的渗透率达到613 Barrer，CO2/CH4选择性为33.5，分离性能超过了2008年的Robeson上限。
除了通过单体的结构设计和热重排对PI膜材料的分离性能进行改善外，共聚也是一种简单、易操作的改性方法[10]。王丽娜等[11]利用6FDA与1,3-苯二胺（mPDA）和2,6-二氨基甲苯（2,6-DAT）共聚，合成了一系列新型共聚聚酰亚胺6FDA-2,6-DAT/mPDA。在35℃、0.2 MPa下，H2/N2、O2/N2和CO2/CH4的分离性能均接近或突破Robeson上限。因此，在本课题组前期研究的基础上，本研究以具有“Y型”吡啶环结构的4-(4′-叔丁基)苯基-2,6-二(4′-氨基苯基)吡啶（TPAPP）[12]和含有Cardo芴基的9,9′-双[4-(4-氨基-3-羟基苯氧基)苯基]芴（BAHPPF）为二胺，混合之后与6FDA进行共聚，经热酰亚胺化制备共聚PI膜，再经450℃热处理得到相应的共聚TR膜。研究二胺BAHPPF和TPAPP的物质的量之比对共聚PI和TR膜结构和性能的影响。BAHPPF中含有柔性醚键和大体积Cardo芴基，TPAPP中含有“Y型”吡啶环结构，两者共聚可对共聚PI的分子链刚性以及可重排比例进行有效调控，从而优化膜材料的微观结构和性能。
1 实验
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1.1 主要原材料
9,9′-双[4-(4-氨基-3-羟基苯氧基)苯基]芴（BAHPPF）和4-(4′-叔丁基)苯基-2,6-二(4′-氨基苯基)吡啶（TPAPP），实验室自制，纯度>98%；4,4′-(六氟异亚丙基)二邻苯二甲酸酐（6FDA），纯度>98%，天津众泰材料科技有限公司；N,N-二甲基乙酰胺（DMAC），分析纯，国药集团化学试剂有限公司。
1.2 膜试样的制备
共聚PI膜和TR膜的制备过程如图1所示。在装有机械搅拌装置的圆底烧瓶中，加入一定物质的量之比的BAHPPF和TPAPP以及溶剂DMAC，在室温下搅拌，直到固体完全溶解后，加入与二胺单体相同物质的量的二酐单体6FDA。将反应液在冰水浴中连续搅拌12 h得到固含量为15%的聚酰胺酸（PAA）溶液。然后，将PAA溶液直接刮涂在干净的玻璃板上，采用以下梯度升温程序进行热亚胺化：40℃/4 h+80℃/1 h+150℃/1 h+200℃/1 h+250℃/0.5 h，此时亚胺化程度可达95.15%[13]。水浴中脱膜后，将膜试样转移至管式炉中在300℃热处理1 h，得到共聚PI膜。接下来，在N2气氛下，以3℃/min的加热速率缓慢加热至450℃，并保持1 h，得到共聚TR膜[14]。按照BAHPPF和TPAPP物质的量之比9∶1、 8∶2、7∶3和6∶4对共聚PI和TR膜进行命名，如PIBT-9:1和TRBT-9:1。
1.3 性能测试与表征
采用傅里叶变换红外光谱仪（FTIR，Nicolet iS10型，美国赛默飞公司）对共聚PI膜和TR膜的化学结构进行表征，扫描范围为500～4 000 cm-1；采用热重分析仪（TGA，STA 449F3型，德国耐驰公司）对共聚PI膜进行热行为测试，N2气氛，升温速率为10℃/min，测试温度为20～800℃；采用动态热机械分析仪（DMA，8000型，美国珀金埃尔默公司）对膜样品进行测试，测试温度为50～400℃，升温速率为10℃/min，频率为1 Hz；采用万能材料拉伸试验机（HY-0580型，上海恒翼精密仪器有限公司）对膜样品进行力学性能测试，样品尺寸为7 cm×1 cm，拉伸速率为10 mm/min；采用X-射线衍射仪（XRD，BLKII-5FF-SX型，荷兰帕纳科公司）对膜样品进行物相分析，2θ=5°～70°，扫描速度为5°/min，波长λ为1.54 Å。根据布拉格方程nλ=2dsinθ（其中n=1），计算出晶面间距d值。
在实验室自制的气体渗透性测试装置上，利用恒压-变体积方法对共聚TR膜进行纯气体渗透性测试。选取4种常见的小分子气体：H2、CO2、O2和N2，其分子动力学直径分别为2.89、3.30、3.46、3.64 Å。每种膜至少测试3个样品，结果取平均值，测量精度为±10%。气体渗透率（P）和理想选择性（α）的计算公式分别如式（1）和式（2）所示[15]。
Pi=F×LΔP×S
α1/2=P1P2
式（1）～（2）中：Pi为i气体的渗透率，Barrer（1 Barrer=3.35×10-16 mol·m-1·s-1·Pa-1）；F为渗透气体的体积流量，cm3(STP)/s；S为样品的有效面积，cm2；ΔP为样品的上、下游压差，Pa；L为膜样品厚度，cm；α为气体1对气体2的理想选择性。
2 结果与讨论
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2.1 化学结构
图2为共聚PI膜和TR膜试样的FTIR图。从图2(a)可以看出，1 783 cm-1和1 720 cm-1处是酰亚胺环上C=O的伸缩振动峰，1 370 cm-1处是酰亚胺环上C-N的伸缩振动峰，3 400 cm-1和1 254 cm-1处是-OH和C-F键的特征吸收峰。这些特征吸收峰的存在说明成功合成了具有酰亚胺环结构的PI共聚物。从图2(b)可以看出，1 783、1 720、1 370 cm-1处的酰亚胺环特征吸收峰减弱，同时在1 553 cm-1和1 057 cm-1处出现苯并噁唑结构的特征吸收峰，说明重排反应已发生[16]。
2.2 热性能
图3为共聚PI膜的损耗因子-温度（tanδ-T）曲线。从图3可以看出，4种共聚PI试样均只有一个显著的tanδ峰，反映了大分子链段的运动状态，即聚合物从玻璃态到橡胶态的α转变。根据tanδ峰的位置可以确定共聚PI膜的玻璃化转变温度（Tg），见表1。从表1可以看出，这些共聚PI的Tg均较高，在350℃左右，这主要是因为Cardo芴基和“Y型”吡啶环结构的空间位阻较大，阻碍了分子链的运动，增加了大分子链的刚性；此外，邻近的-OH之间可形成氢键，增加了分子链间的相互作用，也有利于Tg的提高。从表1还可以看出，随着TPAPP摩尔分数的增加，共聚PI的Tg略有提高，这主要是由于“Y型”吡啶环结构刚性较大，空间位阻作用也较大，且减少了柔性链接-O-的含量，分子链段运动受限，从而提高了聚合物的Tg[17]。
图4为共聚PI膜的TGA测试结果。从图4(a)可以看出，4种共聚PI膜主要表现出两个显著的失重阶段：第一个阶段发生在350～450℃，为含邻羟基的酰亚胺环结构发生重排形成刚性的苯并噁唑结构，并释放出CO2引起失重[18]；第二个阶段发生在540℃附近，主要由聚酰亚胺分子骨架的断裂、分解引起[19]。从图4(b)可以看出，热重排温度（TTR）即DTG曲线第一个失重峰对应的温度随TPAPP摩尔分数的增加略有下降，这可能是因为-OH含量减少，分子链间相互作用减弱所致。由图4(b)可以看出，CO2的释放量在400℃左右达到最大，这主要是由热重排反应释放的。
2.3 力学性能
4种共聚PI膜的应力-应变曲线如图5所示，具体力学数据见表1。从图5(a)可以看出，随着TPAPP摩尔分数的增加，共聚PI膜的力学性能逐渐下降。PIBT-9∶1和PIBT-6∶4的拉伸强度分别为119.8 MPa和81.8 MPa。这可能是由于“Y型”吡啶环结构增多，增加了分子链刚性，但减小了分子链间相互作用所致[20]。
以PIBT-8:2为例研究热处理温度对共聚TR膜力学性能的影响，结果如图5(b)所示。从图5(b)可以看出，随热处理温度升高，共聚TR膜材料的力学性能显著降低。当热处理温度为450℃时，其拉伸强度、杨氏模量和断裂伸长率分别下降到56.4 MPa、2.1 GPa和2.1%。这主要是因为重排反应后形成了刚性的苯并噁唑结构，同时由于CO2的释放，在材料内部形成了大量的微孔结构[21]，从而造成力学性能的降低[22]。
2.4 微观结构分析
共聚PI膜和TR膜的XRD测试结果如图6所示。从图6(a)可以看出，4种共聚PI膜主要表现出一个较宽的衍射峰，表明它们是无定形结构。这主要是因为Cardo芴基和“Y型”吡啶环结构的空间体积较大，同时未形成氢键的-OH和-(CF3)2-结构的存在以及间位取代结构都增加了大分子链间的距离，减少了分子链间的相互作用，阻碍了分子链的紧密堆积。热重排后，4种共聚TR膜的XRD曲线上均出现了两个衍射峰，见图6(b)。这可能是因为重排反应使聚合物链的微观结构重新调整，分子链形成新的堆积与排列[9]。与共聚PI膜相比，共聚TR膜的第一个衍射峰向低角度方向移动，使d值由0.53 nm增大到0.59 nm。通常分子链间距离越大，层间距越大，可形成更多的自由体积，有利于提供更多的气体分子传输通道，从而提高膜材料的气体渗透率[23]。
2.5 气体分离性能
采用4种高纯度气体分别测试了4种共聚TR膜的气体渗透系数，并计算出理想选择性，结果见表2。从表2可以看出，在4种共聚TR膜中，H2和CO2的渗透系数显著高于O2和N2，这与气体分子的动力学直径密切相关。此外，随着TPAPP摩尔分数的增加，共聚TR膜的气体渗透系数呈现出先增大后减小的趋势。这说明当两种二胺单体以适当的物质的量之比聚合时，才会显著提高共聚TR膜的气体渗透性。当BAHPPF和TPAPP的物质的量之比为8∶2时，TRBT-8:2对H2、CO2、N2和O2的渗透系数分别达到346.4、304.5、72.43、13.34 Barrer，CO2/N2理想选择性为22.82，O2/N2理想选择性为5.43。
图7为4种共聚TR膜的O2/N2分离性能评价。从图7可以看出，这些膜试样的分离性能均接近2008年的Robeson上限，并高于一些已报道的文献值，说明其具有较好的气体分离能力[24-25]。
3 结论
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本文以自制的二胺单体TPAPP和BAHPPF按照4个物质的量之比分别与二酐单体6FDA进行溶液共聚，合成了4种PAA溶液。经热亚胺化和热重排处理分别得到了共聚PI膜和TR膜材料，对其进行结构和性能表征，得出以下结论：
（1）所得的共聚PI膜表现出优异的热性能和力学性能，Tg值主要集中在350℃左右。随着TPAPP摩尔分数的增加，共聚PI膜的力学性能表现出下降趋势。随着热处理温度的升高，共聚TR膜的力学性能也显著降低。经热重排后，共聚TR膜的d值显著增大。
（2）气体渗透性测试表明，当BAHPPF与TPAPP的物质的量之比为8∶2时，共聚TR膜表现出最高的气体渗透性，对H2、CO2、O2和N2的渗透系数分别达到了346.4、304.5、72.43、13.34 Barrer，CO2/N2的理想选择性为22.82，O2/N2的理想选择性为5.43，接近2008年 Robeson上限。
基金
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  • 国家自然科学基金资助项目(22278051)
文献
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参考文献 引证文献
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2024年第57卷第10期
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doi: 10.16790/j.cnki.1009-9239.im.2024.10.007
  • 接收时间：2024-04-26
  • 首发时间：2025-12-24
  • 出版时间：2024-10-20
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  • 收稿日期：2024-04-26
  • 修回日期：2024-06-14
基金
国家自然科学基金资助项目(22278051)
作者信息
    辽宁科技大学 化学工程学院，辽宁 鞍山 114051

通讯作者:

鲁云华（1977-），女（汉族），辽宁辽阳人，教授，主要从事功能性聚酰亚胺材料的研究；
赵洪斌（1977-），男（汉族），辽宁本溪人，讲师，主要从事高性能聚酰亚胺材料的研究。
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2种不同金属材料的力学参数
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Family		 属数
Number of
genus		 种数
Number of
species		 占总种数比例
Percentage of
total species (%)		 属
Genus		 种数
Number of
species		 占总种数比例
Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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