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Abstract In order to effectively practice the Aqueous Lignin Purification with Hot Agents (ALPHA) process for lignin purification and fractionation, the temperatures and feed compositions where regions of liquid–liquid equilibrium (LLE) exist must be identified. To this end, pseudo‐ternary phase diagrams for the lignin–acetic acid–water system were mapped out at 45–95 °C and various solvent: feed lignin mass ratios (S : F). For a given temperature, the accompanying SL (solid–liquid), SLL (solid–liquid–liquid), and one‐phase regions were also located. For the first time, ALPHA using acetic acid (AcOH)–water solution was applied to a lignin recovered via the commercial LignoBoost process. In addition to determining tie‐line compositions for the two regions of LLE that were discovered, the distribution of lignin and key impurities (the latter can negatively impact lignin performance for materials applications) between the two liquid phases was also measured. As a representative example, lignin isolated in the lignin‐rich phase was reduced 7x in metals and 4x in polysaccharides by using ALPHA with a feed solvent composition of 50–55 % AcOH and an S : F of 6 : 1, with said lignin being obtained at a yield of 50–70 % of the feed lignin and having a molecular weight triple that of the feed. 

Herein, we have synthesized high-performance, low-cost ionomer biocomposites comprised of sulfonated poly(ether ether ketone) (SPEEK) and softwood Kraft lignin with proton selectivities three- to ten-fold higher than that of neat SPEEK.