2-(4-Ethyl formate phenyl azo) phenol lignin-modified polymer (AL-azo-COOEt), a novel lignin-based azo polymer, has been successful y synthesized from alkali lignin (AL) recovered from pulping black liquor. The micel ization process of the AL-azo-COOEt polymer was also studied. The synthetic products were characterized by elemental analysis, Fourier transform infrared (FT-IR) spectra, proton nuclear magnetic resonance (1H NMR) spectroscopy, and ulraviolet-visible (UV-Vis) spectroscopy. The formation of the micel es was monitored by laser light scattering (LLS), and a scanning electron microscope (SEM) and transmission electron microscope (TEM) were used to characterize the surface morphology of the col oidal spheres. X-ray photoelectron spectroscopy (XPS) and elemental analysis were used to obtain the surface element distribution and average element content of the col oidal spheres, respectively. Results show that lignin-based azo polymer AL-azo-COOEt can form uniform solid col oidal spheres by hydrophobic aggregation. Col oidal spheres formed gradual y when the water content increased beyond the critical water content (CWC), The CWC has a linear relationship with the logarithm of the initial concentration of AL-azo-COOEt (C0). The col oidal spheres consist of a relatively hydrophobic interior and a relatively hydrophilic surface. The AL-azo-COOEt col oidal spheres can load Doxorubicin (DOX) and the in vitro release can be control ed by adjusting the pH of buffered solution.%利用造纸废液中的碱木素(AL)合成了木质素基偶氮聚合物(AL-azo-COOEt)，并研究其自组装胶体化过程。木质素偶氮聚合物的成功合成通过核磁共振氢谱(1H NMR)、紫外-可见(UV-Vis)光谱、傅里叶变换红外(FT-IR)光谱和元素分析等表征方法得到证实。激光光散射(LLS)监测了AL-azo-COOEt的胶体化过程，自组装形成的胶体球利用透射电镜(TEM)、扫描电镜(SEM)、X射线光电子能谱仪(XPS)和元素分析等进行表征。结果表明，木质素偶氮聚合物通过疏水聚集作用可以形成规整的实心胶体球，且为内部较疏水外部较亲水性质的结构。木质素偶氮聚合物胶体球可以包载疏水性药物阿霉素(DOX)，且其缓释性能可以通过缓冲溶液的pH值来调控。
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