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桂林理工大学材料科学与工程学院,桂林,541004
纸质出版日期:2013-7-20,
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魏志波, 白蕊, 张发爱. 甲基丙烯酸甲酯在改性介孔分子筛SBA-15孔道中的溶液聚合[J]. 高分子学报, 2013,(7):849-855.
Zhi-Bo Wei, Rui Bai, Fa-Ai Zhang. MMA SOLUTION POLYMERIZATION IN THE CHANNELS OF MODIFIED MESOPOROUS MOLECULAR SIEVES SBA-15[J]. Acta Polymerica Sinica, 2013,(7):849-855.
魏志波, 白蕊, 张发爱. 甲基丙烯酸甲酯在改性介孔分子筛SBA-15孔道中的溶液聚合[J]. 高分子学报, 2013,(7):849-855. DOI: 10.3724/SP.J.1105.2013.12288.
Zhi-Bo Wei, Rui Bai, Fa-Ai Zhang. MMA SOLUTION POLYMERIZATION IN THE CHANNELS OF MODIFIED MESOPOROUS MOLECULAR SIEVES SBA-15[J]. Acta Polymerica Sinica, 2013,(7):849-855. DOI: 10.3724/SP.J.1105.2013.12288.
水热法合成了介孔分子筛SBA-15
分别用硅烷偶联剂KH-151
KH-560和KH-570对SBA-15进行了改性
将不同类型的改性介孔分子筛(M-SBA-15)作为微反应器
把含MMA的甲苯溶液载入到微反应器中
通过溶液聚合法使得MMA在孔道内部形成聚合物.通过XRD
FTIR
N2吸附/脱附
GPC
1H-NMR
TG和DSC测试手段对M-SBA-15和PMMA/M-SBA-15复合材料以及孔道内PMMA进行了分析测试.研究表明
改性介孔分子筛仍保留了有序介孔材料的基本特性
M-SBA-15和相应的复合材料的比表面积、孔径以及孔容降低
表明PMMA载入到介孔分子筛的孔道中.与传统的溶液聚合所得的PMMA相比
介孔孔道内所得的PMMA的分子链的间规立构度有所提高
其分子量约为传统溶液聚合的十几倍
初始热稳定性明显提高
玻璃化转变温度提高9~11℃.此外
KH-151改性SBA-15载入最多的PMMA
所得的PMMA的分子量和玻璃化转变温度最高.
SBA-15 was synthesized by hydrothermal method
and modified with silane coupling reagents vinyl triethoxylsilane (KH-151)
-glycidylpropyltrimethoxysilane (KH-560) and -methacryloxypropyl- trimethoxysilane (KH-570)
respectively.Then different types of modified mesoporous sieves (M-SBA-15) were used as microreactors which were loaded with methyl methacrylate and initiator in toluene.Mesoporous channels were covered by PMMA in the form of thin coating via solution polymerization.M-SBA-15
PMMA/M-SBA-15 composites and PMMA polymerized in the channels were characterized by X-Ray diffraction (XRD)
N2 adsorption/desorption
gel permeation chromatography (GPC)
1H-nuclear magnetism resonance spectrum (1H-NMR)
Fourier transform infrared spectra (FTIR)
thermal gravimetric analysis (TGA) and differential scanning calorimeter (DSC).The results showed that modified mesoporous sieves and parts of the composites still retained the basic features of order mesoporous materials.Compared with SBA-15
BET surface areas
pore size and pore volume of both the modified mesoporous sieves and corresponding polymer composites decreased obviously.This confirmed that PMMA was loaded into the mesoporous channels.Molecular weight of PMMA in the channels of the mesoporous sieves was ten times more than that of traditional PMMA via solution polymerization.In addition
thus prepared PMMA exhibited higher initial thermal temperature
and glass transition temperature (an increase of 9~11 K) due to the little weak bonds formation and higher molecular weight.Furthermore
KH-151 modified SBA-15 loaded the highest PMMA content
and the PMMA possessed the highest molecular weight and Tg.
介孔分子筛硅烷偶联剂微反应器溶液聚合复合材料
Mesoporous sieveCompositesMicroreactorSilane coupling reagentsSolution polymerization
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