Effects of Precipitation pH of Black Liquor on Characteristics of Precipitated and Acetone-Fractionated Kraft Lignin

Two important steps in utilizing technical kraft lignin (KL) from black liquor to synthesize lignin-phenol-formaldehyde (LPF) resin are its extraction via precipitation and fractionation. However, the effects of precipitation pH and acetone fractionation on the characteristics of hardwood KL have not been studied for LPF resins. Therefore, this paper reports the effects of the precipitation pH of black liquor and acetone fractionation on the characteristics of KL from mixed hardwood species for LPF resins. The precipitation was conducted at various pH levels from 3 to 9 of black liquor to obtain crude KL (C-KL), which was used in acetone fractionation to produce acetone-soluble KL (AS-KL) and acetone-insoluble KL (AI-KL). Precipitation at pH 3 and 9 produced the highest and lowest yields of C-KL, respectively. As expected, the C-KL infrared spectra were similar regardless of the precipitation pH levels. As the pH increased, the molecular weight of C-KL increased. However, the molecular weight of AS-KL and AI-KL after acetone fractionation increased to a maximum of 4,170 and 47,190 g/mol at pH 7, then decreased to 3,210 and 19,970 g/mol at pH 9, respectively. The smallest molecular weights of AS-KL and AI-KL were 3,210 and 15,480 g/mol and were found at pH 9 and 3, respectively. These results suggest that both AS-KL at pH 9 and AI-KL at pH 3 have good potential as starting lignins for synthesizing LPF resins that require cross-linking for polymerization.