木质素磺酸钠的酚化改性及其环氧树脂的制备

Phenolation Modification of Sodium Lignosulfonates and Its Utilization in Preparation of Lignin-based Epoxy Resin

摘要: 采用木质素磺酸钠与氢溴酸反应,以十六烷基三丁基溴化磷为催化剂对木质素磺酸钠进行酚化改性;然后,在碱性条件下加入环氧氯丙烷进行环氧化反应,制备木质素基环氧树脂.用元素分析、凝胶渗透色谱、紫外光谱、红外光谱、核磁共振等对木质素磺酸钠、酚化木质素及木质素基环氧树脂的结构变化进行表征.结果表明:木质素磺酸钠酚化改性后,部分甲氧基脱落,生成酚羟基,其酚羟基摩尔分数提高了2.6倍,可以满足制备木质素基环氧树脂的酚羟基摩尔分数的条件.

Abstract: Lignin-based epoxy resin is synthesized by a phenolated lignosulfonate,which comes from sodium lignosulfonate through phenolated reaction with HBr and tributhexadecylphosphonium bromide as catalysts.The phenolated lignosulfonate is epoxidized by epichlorohydrin to produce lignin-based epoxy resin.The components and structure of phenolated product are characterized by the elemental analysis,Gel permeation chromatography (GPC),Fourier transform infrared spectrometer (FT-IR),ultraviolet-visible spectrometry (UV),and ¹H-nuclear magnetic resonance (¹H-NMR).Results show that parts of the methyloxygen group of sodium lignosulfonate are transformed into phenolic hydroxy,and the content of the phenolic hydroxy group of phenolic products increases 2.6 times than that of sodium lignosulfonate,which satisfies the requirement of prepared lignin-based epoxy resin.