The solubility and softening behavior of lignin from acid-catalyzed ethanol/water pulping was determined in various ethanol/water solvent mixtures and a process relevant temperature range. Operation conditions for an optimized lignin separation process have been derived from the determined lignin phase behavior. A continuous lignin separation and solvent recovery process has been developed in lab scale and was successfully up-scaled to a dedicated pilot plant at Fraunhofer CBP (WO2016062676A1). Agglomeration of softened lignin particles and lignin “stickiness” were adjusted by temperature (38–44 °C at 80–120 mbar) and ethanol content of the lignin dispersion (6–9 wt %). In this manner, ethanol recovery by evaporation and lignin particle formation were facilitated simultaneously, which was monitored by inline infrared spectroscopy. The agglomeration behavior of different lignins was monitored via inline particle size analysis. Optimal process conditions resulted in good filterability of the lignin dispersion with average filter cake resistances of 10¹¹ to 10¹³ m^–2 and lignin yields close to 100 wt % of water-insoluble lignin.

中文翻译：

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从有机溶剂制浆酒中连续分离木质素：木质素颗粒形成与溶剂回收相结合

在各种乙醇/水溶剂混合物中和工艺相关的温度范围内，测定了酸催化的乙醇/水制浆中木质素的溶解度和软化行为。从确定的木质素相行为得出了优化的木质素分离过程的操作条件。已经在实验室规模上开发了连续的木质素分离和溶剂回收工艺，并已成功升级至Fraunhofer CBP的专用中试工厂（WO2016062676A1）。通过温度（80-120 mbar下38-44°C）和木质素分散液的乙醇含量（6-9 wt％）来调节软化的木质素颗粒的团聚和木质素的“粘性”。以这种方式，同时促进了通过蒸发回收乙醇和木质素颗粒的形成，这通过在线红外光谱法进行监测。通过在线粒度分析监测不同木质素的团聚行为。最佳工艺条件导致木质素分散体具有良好的过滤性，平均滤饼阻力为10¹¹至10 ¹³ m ^–2，木质素收率接近于100 wt％的水不溶性木质素。