Klein Stephanie Elisabeth, Rumpf Jessica, Kusch Peter, Albach Rolf, Rehahn Matthias, Witzleben Steffen, Schulze Margit
Department of Natural Sciences, Bonn-Rhein-Sieg University of Applied Sciences von-Liebig-Straße 20 D-53359 Rheinbach Germany
Technical University Darmstadt Alarich-Weiß-Straße 4 D-64287 Darmstadt Germany.
RSC Adv. 2018 Dec 10;8(71):40765-40777. doi: 10.1039/c8ra08579j. eCollection 2018 Dec 4.
Polyurethane (PU) coatings were successfully produced using unmodified kraft lignin (KL) as an environmentally benign component in contents of up to 80 wt%. Lignin samples were precipitated from industrial black liquor in aqueous solution working at room temperature and different pH levels (pH 2 to pH 5). Lignins were characterized by UV-Vis, FTIR, pyrolysis-GC/MS, SEC and P-NMR. Results show a correlation between pH level, OH number and molecular weight of isolated lignins. Lignin-based polyurethane coatings were prepared in an efficient one step synthesis dissolving lignin in THF and PEG in an ultrasonic bath followed by addition of 4,4-diphenylmethanediisocyanate (MDI) and triethylamine (TEA). Crosslinking was achieved under very mild conditions (1 hour at room temperature followed by 3 hours at 35 °C). The resulting coatings were characterized regarding their physical properties including ATR-IR, TGA, optical contact angle, light microscopy, REM-EDX and AFM data. Transparent homogeneous films of high flexibility resulted from lignins isolated at pH 4, possessing a temperature resistance up to 160 °C. Swelling tests revealed a resistance against water. Swelling in DMSO depends on index, pH of precipitation and catalyst utilization for PU preparation. According to AFM studies, surface roughness is between 10 and 28 nm.
采用未改性的硫酸盐木质素(KL)作为环境友好型成分,成功制备了含量高达80 wt%的聚氨酯(PU)涂料。木质素样品在室温及不同pH值(pH 2至pH 5)的水溶液中从工业黑液中沉淀出来。通过紫外可见光谱(UV-Vis)、傅里叶变换红外光谱(FTIR)、热解气相色谱/质谱联用(pyrolysis-GC/MS)、尺寸排阻色谱(SEC)和磷核磁共振(P-NMR)对木质素进行了表征。结果表明,分离出的木质素的pH值、羟值和分子量之间存在相关性。通过将木质素溶解在四氢呋喃(THF)中,聚乙二醇(PEG)溶解在超声浴中,然后加入4,4'-二苯基甲烷二异氰酸酯(MDI)和三乙胺(TEA),以高效的一步法合成制备了木质素基聚氨酯涂料。在非常温和的条件下(室温下1小时,然后在35℃下3小时)实现交联。对所得涂层的物理性能进行了表征,包括衰减全反射红外光谱(ATR-IR)、热重分析(TGA)、光学接触角、光学显微镜、扫描电子显微镜-能谱分析(REM-EDX)和原子力显微镜(AFM)数据。在pH 4下分离得到的木质素形成了具有高柔韧性的透明均匀薄膜,其耐热性高达160℃。溶胀试验表明该涂层具有耐水性。在二甲基亚砜(DMSO)中的溶胀取决于指数、沉淀pH值和聚氨酯制备中催化剂的用量。根据原子力显微镜研究,表面粗糙度在10至28纳米之间。