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基于镍（II）配位阴离子引发体系的一种合成高1,4-结构含量的端羟基聚丁二烯的新策略。

A novel synthetic strategy for hydroxyl-terminated polybutadiene containing high -1,4 contents based on a Ni(ii)-coordinated anionic initiating system.

作者信息

Min Xin

机构信息

Department of Applied Chemistry, School of Nature and Applied Sciences, Northwestern Polytechnical University Dongxiang Road 1 710072 Xi'an China

出版信息

RSC Adv. 2019 Nov 29;9(67):39037-39045. doi: 10.1039/c9ra04531g. eCollection 2019 Nov 27.

DOI:10.1039/c9ra04531g
PMID:35540646
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC9075970/
Abstract

In this study, novel hydroxyl-terminated polybutadiene (HTPB) with a high -1,4 content was developed using a -butyl dimethyl siloxy dimethyl propyl lithium (Li)-naphthenate nickel (Ni)-boron trifluoride (B) initiating system (Li-Ni-B). The effects of the material ratio and the addition sequence on the -1,4 content and molecular weight of HTPB were studied, and the results were discussed. The optimal Li/Ni ratio was 10 : 1, and the optimal Li/B ratio was 1 : 2. HTPB prepared by the Li-Ni-B system was characterized by Fourier transform infrared spectroscopy (FTIR), H nuclear magnetic resonance (H-NMR) spectroscopy, and C nuclear magnetic resonance (C-NMR) spectroscopy. The results suggested high -1,4 contents in HTPB synthesized using Li-Ni-B (-1,4 > 95%). The comparison of the -1,4 contents in the HTPB samples obtained by anionic polymerization and the Li-Ni-B system revealed the advantages of the latter compared to the former.

摘要

在本研究中，使用丁基二甲基硅氧基二甲基丙基锂（Li）-环烷酸镍（Ni）-三氟化硼（B）引发体系（Li-Ni-B）开发了具有高1,4-含量的新型端羟基聚丁二烯（HTPB）。研究了原料配比和添加顺序对HTPB的1,4-含量和分子量的影响，并对结果进行了讨论。最佳Li/Ni比为10∶1，最佳Li/B比为1∶2。采用傅里叶变换红外光谱（FTIR）、氢核磁共振（H-NMR）光谱和碳核磁共振（C-NMR）光谱对Li-Ni-B体系制备的HTPB进行了表征。结果表明，使用Li-Ni-B合成的HTPB中1,4-含量较高（1,4-＞95%）。通过阴离子聚合和Li-Ni-B体系获得的HTPB样品中1,4-含量的比较揭示了后者相对于前者的优势。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebcf/9075970/b64305458471/c9ra04531g-f10.jpg
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https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebcf/9075970/826ee6b3ac91/c9ra04531g-f5.jpg
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https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebcf/9075970/e83a6e523f94/c9ra04531g-f8.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebcf/9075970/553c04f048a3/c9ra04531g-f9.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebcf/9075970/b64305458471/c9ra04531g-f10.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebcf/9075970/b5651f8fcf99/c9ra04531g-s1.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebcf/9075970/ccc436390240/c9ra04531g-f1.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebcf/9075970/6283f90df0d5/c9ra04531g-f2.jpg
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https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebcf/9075970/826ee6b3ac91/c9ra04531g-f5.jpg
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https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebcf/9075970/d063fac97f50/c9ra04531g-f7.jpg
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https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebcf/9075970/553c04f048a3/c9ra04531g-f9.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ebcf/9075970/b64305458471/c9ra04531g-f10.jpg

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本文引用的文献

1
Utilization of steric hindrance of alkyl lithium-based initiator to synthesize high 1,4 unit-containing hydroxyl- terminated polybutadiene.利用烷基锂引发剂的空间位阻合成高1,4-单元含量的端羟基聚丁二烯。
R Soc Open Sci. 2018 May 30;5(5):180156. doi: 10.1098/rsos.180156. eCollection 2018 May.
2
eta 6-Arene complexes of Ni(II), efficient catalysts for 1,3-butadiene and styrene polymerization.
Chem Commun (Camb). 2003 Jan 7(1):78-9. doi: 10.1039/b209838e.