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4.1.

Yield
Cellulose was successfully isolated from cleaned and dried raw corncob powder through a
straight forward process. The color of the raw corncob powder reduced with each step of
delignification and hemicellulose removal to become pure white.

After that cellulose nanocrystals were produced by sulfuric acid hydrolysis.

The yields of the CNC, with respect to the initial amount of dried TCC was found 46 wt.%,;
this values are consistent with the literature data(Alves, Pires, Neto, Oliveira, & Pasquini,
2013).

With long reaction time, higher concentration of the acid and acid to fiber ratio increment, the
decrement in yield was expected(Singh, Gaikwad, Park, & Lee, 2017).

The acid hydrolysis was able to hydrolyze the cellulose chains to separate the crystalline part
from the amorphous part.

The decrease in the level of yield by employing higher acid concentrations may be related to
the hydrolysis process in which cellulose is degraded into its building blocks namely glucose.
On the other hand, the treatments with low acid concentrations results in low dispersity
values or aggregation of the structures.

The increase in the time and temperature of the hydrolysis process higher than the maximum
point may generate glucose via the degradation of cellulose which in turn lowers the
production yield of the CNCs.

Higher levels of acid may also degrade the crystalline parts of the sample in addition to the
amorphous part that lowers the production yield of CNCs.

These differences among the results may be related to the different CNCs yield calculation
methods, nature of the utilized raw materials, acid concentration, time and the temperature
plus the formulation conditions during the production of CNCs(Hemmati, Mahdi,
Kashaninejad, & Barani, 2018)

The optimum yield…….

The yield of the CNCs obtained was varied depending on parameter interaction from
experimental design
Furthermore, the optimal conditions to obtain the highest yield of CNCs are determined as
follows: sulfuric acid concentration 13.5%, reaction time 4.7 h, and ball milling time 2.2 h.
Under the optimal conditions, the obtained yield of CNCs is 88.4%, which is not significantly
different from the predicted value of 89.7% at 95% confidence interval.

The yields of CNC-WS and CNC-CS were 31.2% and 32.4%, respectively, which were
similar to the conventional CNCs preparation by mineral acids (about 30%).
The yields of the SCBW, with respect to the initial amount of dried fibers, for SCBW20,
SCBW30 and SCBW40 were 79.26, 74 and 65 wt% respectively; these values are consistent
with the literature data.
Among the several methods for preparing CNW, acid hydrolysis is the most well-known and
widely used (22). This process breaks down the disordered and amorphous parts of the
cellulose, releasing single and well-defined crystals.
Thus, this process is based on the quicker hydrolysis kinetics presented by amorphous
regions, as compared to crystalline ones (21-23). The decreasing yields with longer reaction
time is expected as cellulose chains in the less ordered regions are hydrolyzed to separate the
crystalline domains that reduce in sizes as the surface chains are further hydrolyzed, while
cellulose fragments are broken into soluble oligo- and monosaccharides

After bleaching, the purified cellulose fibers were then subjected to a sulfuric acid hydrolysis
in which CNCs was isolated showing high stability in water.
The hydrolysis process was conducted at different hydrolysis time (30, 45 and 60 min),
temperature (40, 50 and 60 oC) and with different acid concentration of (50, 57.5 and 65%).
After hydrolysis, different steps such as successive centrifugation, dialysis, ultrasonication
and freeze drying were performed to get purified CNCs.
The yield of the CNCs obtained was varied depending on parameter interaction from
experimental design. Figure 4.2 shows the obtained suspension of cellulose nanocrystals.

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