Improved Synthesis of Cellulose Carbamates with Minimum Urea Based on an Easy Scale-up Method

Cellulose carbamates (CCs) were successfully prepared from cellulose/urea (CU) mixtures based on an easy scale-up method and minimum urea. Urea content and the reaction conditions on the nitrogen content of the reacted CU (RCU) mixtures and CCs were systematically investigated. RCU mixtures and CCs were characterized with elemental analysis, Fourier transform infrared spectroscopy, X-ray diffraction, NMR spectrometry and solubility testing. The result indicated that almost all of urea was involved in the derivatization reaction and cellulose was converted into CC with absence of byproducts. The nitrogen content of CCs increased with an increase of the urea content and the reaction temperature, as well as the reaction time. CCs retained the cellulose I crystalline, and the degree of polymerization hardly changed with the reaction conditions. CCs prepared from CU mixtures with the urea content of 3.4-4.6 wt % displayed good solubility in NaOH/ZnO aqueous solutions. Especially, RCU mixtures without washing could be also well dissolved in NaOH/ZnO solutions and its solubility could reach 97%. This work provided a simple, pollution-free and economic pathway for preparing CCs, which is expected to be useful for the CarbaCell process.