In this study, novel hydroxyl-terminated polybutadiene (HTPB) with a high cis-1,4 content was developed using a tert-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 cis-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), 1H nuclear magnetic resonance (1H-NMR) spectroscopy, and 13C nuclear magnetic resonance (13C-NMR) spectroscopy. The results suggested high cis-1,4 contents in HTPB synthesized using Li–Ni–B (cis-1,4 > 95%). The comparison of the cis-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.
Hydroxyl-terminated polybutadiene (HTPB) with high cis-1,4 content (>95.0%) has been prepared via a two-step method by taking commercial butadiene rubber (BR9000) as a starting material, including the one-pot synthesis of aldehyde-group-terminated polybutadiene (ATPB) in high efficiency and the subsequent reduction reaction. The double bonds distributed in linear polybutadiene were first epoxidized and then cleaved at the exact epoxidized sites. The epoxidation reaction by 3-chloroperbenzoic acid and chain-cleavage reaction by periodic acid are controllable, highly efficient, selective, and quantitative. Along with an epoxy percent increase, the molecular weight of ATPB prepared via a one-pot method decreased with a relatively narrow polydispersity index. The aldehyde groups in the chain ends were reduced by NaBH4 to produce HTPB, in which the high cis-1,4 content of BR was retained.
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