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1. 大连理工大学化工学院 精细化工国家重点实验室,大连,116012
2. 辽宁科技大学化学工程学院,鞍山,114051
纸质出版日期:2016-8-1,
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鲁云华, 郝继璨, 李琳, 宋晶, 费明月, 肖国勇, 赵洪斌, 胡知之, 王同华. 热致刚性膜材料的合成与气体分离性能研究[J]. 高分子学报, 2016,(8):1145-1150.
Yun-hua Lu, Ji-can Hao, Lin Li, Jing Song, Ming-yue Fei, Guo-yong Xiao, Hong-bin Zhao, Zhi-zhi Hu, Tong-hua Wang. Synthesis of Thermally Induced Rigid Membranes and Their Gas Separation Properties[J]. Acta Polymerica Sinica, 2016,(8):1145-1150.
鲁云华, 郝继璨, 李琳, 宋晶, 费明月, 肖国勇, 赵洪斌, 胡知之, 王同华. 热致刚性膜材料的合成与气体分离性能研究[J]. 高分子学报, 2016,(8):1145-1150. DOI: 10.11777/j.issn1000-3304.2016.16117.
Yun-hua Lu, Ji-can Hao, Lin Li, Jing Song, Ming-yue Fei, Guo-yong Xiao, Hong-bin Zhao, Zhi-zhi Hu, Tong-hua Wang. Synthesis of Thermally Induced Rigid Membranes and Their Gas Separation Properties[J]. Acta Polymerica Sinica, 2016,(8):1145-1150. DOI: 10.11777/j.issn1000-3304.2016.16117.
以丙酮为溶剂,将9,9-双(4-羟基苯基)芴(BHF)于室温下进行硝化反应得到二硝基化合物9,9-双(3-硝基-4-羟基苯基)芴,再经Pd/C-水合肼还原得到9,9-双(3-氨基-4-羟基苯基)芴(BAHF).采用上述二胺单体BAHF、与9,9-双(4-氨基苯基)芴(BAF)和六氟二酐(6FDA)通过低温溶液缩聚反应制备出一种含酚羟基的共聚聚酰胺酸溶液,经热酰亚胺化和热致重排反应得到共聚聚酰亚胺(CPI)和聚(酰亚胺-苯并恶唑)(PI-PBO)热致刚性膜材料.采用核磁(NMR)、红外光谱(FTIR)、X-射线衍射仪(XRD)、热重分析仪(TGA)、差示扫描量热仪(DSC)和气体渗透性能测试等手段对所制得膜材料的结构、热性能和气体分离性能进行表征.研究结果表明,所制得的热致刚性膜主要表现出非晶结构,为无规共聚物,其Tg为340℃.随热处理温度升高,热致刚性膜的气体渗透性逐渐增加,450℃制得的热致刚性膜对O2、N2、H2、CH4和CO2的渗透通量分别达到229.03、53.26、1497.35、33.52和818.76 Barrer.
Using acetone as a solvent
a dinitro compound 9
9-bis(3-nitro-4-hydroxyphenyl) fluorene was synthesized by the nitration reaction of 9
9-bis(4-hydroxyphenyl) fluorene (BHF) using concentrated nitric acid at room temperature.And then
9
9-bis(3-amino-4-hydroxyphenyl) fluorene (BAHF) was obtained via the catalytic reduction with hydrazine hydrate and Pd/C.The copoly(amic acid) containing phenolic hydroxyl was synthesized from the diamine BAHF
9
9-bis(4-aminophenyl) fluorene (BAF) and 4
4'-hexafluoroisopropylidinedi(phtalic anhydride) (6FDA) via the low-temperature solution polycondensation reaction.The thermally induced rigid membrane materials of copolyimide (CPI) and poly(imide-benzoxazole) (PI-PBO) were prepared by the thermal imidization and thermally induced rearrangement reaction.The structure
thermal properties and gas separation performance of these membrane materials were characterized by nuclear magnetic resonance (NMR)
Fourier transform infrared spectroscopy (FTIR)
X-ray diffraction (XRD)
thermogravimetric analyzer (TGA)
differential scanning calorimetry (DSC) and gas permeation performance testing means.The experimental results show that these thermally induced rigid membranes mainly exhibit amorphous structure
and the glass transition temperature (Tg) is about 340℃.It means that the CPI was a random copolymer.With the increase of thermal treatment temperature
the gas permeabilities of H2
O2
N2
CH4 and CO2 of thermally induced rigid membranes increased gradually.When the thermal treatment temperature reached 450℃
the gas permeabilities of O2
N2
H2
CH4 and CO2 of the thermally induced rigid membrane were 229.03 and 53.26
1497.35
33.52 and 818.76 Barrer separately.These thermally induced rigid membranes containing bulky fluorene and hexafluoroisopropyl groups could be expected to be used in the gas separation applications.
共聚聚酰亚胺热致刚性膜分离性能芴基酚羟基
CopolyimidesThermally induced rigid membraneGas separationFluorenePhenolic hydroxyl
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