Ammonium persulfate (APS) mediated
oxidation has been used in conjunction
with acids under extended reaction times to produce highly crystalline
cellulose nanomaterials. Opportunities exist to tailor the surface
chemistry and morphological properties of nanocellulose using the
economically attractive APS process. Here, the response surface methodology
is applied to establish a set of predictable and reproducible guidelines
for the synthesis of cellulose nanofibers with specific characteristics.
The effect of varying treatment conditions on the APS oxidation of
bleached and unbleached wood and non-wood pulps has been assessed
by adjusting specifically the APS dosage, oxidation time, and temperature.
The surface charge, crystallinity, and aspect ratio of the resulting
nanocellulose have been systematically characterized. As-prepared
materials exhibited a wide range of carboxylic acid contents on their
surface from 0.6 to 1.4 mmol/g, while the crystallinity index changed
from 72 to 88%. The morphological characteristics of the cellulose
nanofibrils can be varied in the 48–80, 2.7–4.5, and
146–247 nm ranges for the aspect ratio, diameter, and length,
respectively. More importantly, the environmentally friendly ammonium
persulfate, opposed to TEMPO-mediated oxidation, has been effective
at generating similar structural and chemical properties in lignin-containing
feedstocks without any pretreatment or adjustment of experimental
conditions.