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纸质出版日期:2006-8-20,
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宋春梅, 薛海丽, 庄小璐, 黄奕. 异佛尔酮二异氰酸酯自聚产物的13C-NMR研究[J]. 高分子学报, 2006,(5):660-665.
SONG Chunmei, XUE Haili, ZHUANG Xiaolu, HUANG Yi. THE 13C-NMR ANALYSIS OF POLYISOCYANURATE MADE FROM ISOPHORONE DIISOCYANATE[J]. Acta Polymerica Sinica, 2006,(5):660-665.
研究了用季铵盐N
N
N-三甲基-N-(2-羟基乙基)-氢氧化铵为催化剂时异佛尔酮二异氰酸酯(IPDI)自聚产物的合成
用13C-NMR、1H-NMR、不失真地极化转移增强(DEPT)、13C-1H异核远程相关(HMBC)实验表征了产物结构.结果表明
自聚产物是三聚异氰酸酯
主要含有三聚体异氰脲基、异氰酸根.一维核磁谱及二维化学位移相关谱分辨出两种羰基
确定了氮上4种不同取代结构的分子链连接情况.对自聚产物的碳谱图进行了全归属.
Polyisocyanurate from IPDI was synthesized by using quaternary amine salt
N
N
N-trimethyl—N-(2-hydroxyethyl)ammonium hydroxide(TMR-3) as catalyst.The structure analysis and characterization of the product was studied by NMR(1H
13C
DEPT
13C-1H-HMBC).The peaks at δ3.509~3.650
4.094—5.047
3.052— 3.374
3.749—3.766 of the 1H-NMR spectrum were attributed to the hydrogen proton on the 1’。carbon atom connecting with the nitrogen atom of N=C=O
the hydrogen proton on the 1”acarbon of the IPDI trimer
the hydrogen proton on the 10”a carbon connecting with the nitrogen atom of N=C=O
the hydrogen proton on the 10’a carbon of the IPDI trimer
respectively.The peaks at δ 122.07—122.41
δ 123.04~123.41 of the 13C—NMR spectra belonged to the double bonded carbon of N=C=O of 12"and 11".The peaks at δ 150.06.δ 150.87—150.97 of the 13C—NMR spectra belonged to the carbon on the carbonyl group of the IPDI trimer of 11”and l2’.The peaks at δ 48.75~49.01.δ 49.07—50.78 of the 13C—NMR spectra belonged to the tertiary carbon of 1’and 1”.The peaks at δ 51.14.δ 57.18~57.20 of the 13C—NMR spectra belonged to the l0”carbon of methylene.The peaks at δ 54.70
δ 57.18~57.20 of the 13C-NMR spectra belonged to the l0’carbon of methylene.The results show the main product of IPDI self-polymerization was trimer isocyanurate.Trimefized isocyanuric and isocyanate groups were main groups in the polyisocyanurate.1D and 2D NMR can differentiate two sorts of earbonyl groups and establish the connections of all carbon and hydrogen atoms of mixed structures that originated from four different substitutions.The calculated area values of peaks demonstrated the structure characterization of the polyisocyanurate.
异佛尔酮二异氰酸酯三聚核磁共振分析不失真地极化转移增强(DEPT)13C1-H异核远程相关
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