Abstract
Here, a new pretreatment method has been developed to produce CNFs from micro-fibrillated cellulose (MFC) by supercritical CO 2 pretreatment followed with ball-milling (SCB). MFC was obtained from cotton stalk by chemical purification.Experimental factors were controlled to enhance the properties of SCB-CNF, meanwhile a comparative study was conducted with the method of TEMPO oxidation and microfluid homogenization (TMH).
Compared to TMH-CNF, the SCB-CNF has such advantages as Energy saving, high efficiency and environmental protection, indicating a wide application in heat-resistant materials, load materials and other fields.
The solid yields of P-MFC after supercritical CO 2 pretreatment gradually decreased together with the temperature and the reaction time.
Scanning electron microscope (SEM) images of the SCB-CNF and TMH-CNF show that the morphology of the SCB-CNF was basically acicular but that of the TMH-CNF was mainly soft fibrous. The SCB-CNF is smaller in width and shorter in length, and its size is between CNC and CNF.
Thermal gravimetric results suggest that the thermal stability of the SCB-CNF was substantially higher than those of the TMH-CNF.
XRD results indicate that the crystallinity showed an initial increasing trend and then declined with increasing temperature and reaction time, and the crystallinity value of SCB-CNF was larger than that of CNFs. The smaller SCB-CNF became rougher and had a larger surface area. High crystallinity make good thermal stability, short and coarse fiber, easier to disperse than CNF, less energy consumption for dispersion, better than 3D mesh. It can be widely used in polymer composites, reinforcing agents, membrane materials and other fields.
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