Influence of Soda-Anthraquinone Pulping Parameters on the Pulp Properties of Kenaf

(Hibiscus Cannabinus L.) V36 Cultivar in Producing Rayon Grade Pulp

I. Rushdan, J. Latifah, & S. Mahmudin

Forest Research Institute Malaysia (FRIM), 52109 Kepong, Selangor Darul Ehsan

INTRODUCTION
East coast of Peninsular Malaysia is famous for her batik. The most expensive batik is made
from silk. Silk is an expensive material and can be substituted by rayon, also known as
artificial silk. The rayon was imported since there is no local manufacturer available. Rayon is
made from dissolving pulp. Dissolving pulp is made from lignocelluloses material either
wood or non-wood. Today, there are hundreds hectares of kenaf plantation in the east coast
and in the future, thousands of hectares kenaf plantation will be established. The utilisation of
kenaf for dissolving pulp and subsequently producing rayon will assist the batik industry in
the east coast.
The objective of pulping is to liberate the fibres from the raw material. Pulping is a
multivariable heterogeneous reaction process. In a multivariable system, the effect of a single
variable is not comparable, unless all other conditions are fixed at the exact same condition,
vis., a one-variable-at-a-time experiment. This approach is insufficient because it does not
elucidate the effect of everyone factor, and the interactions between different factors cannot
be observed (Anderson & Whitcomb 2000). One technique particularly suited to this
application is Response Surface Methodology (RSM), which merges the methods of planned
and efficient experimental design with least squares modelling to identify optimum conditions
for the process response. The basic theoretical aspects, fundamental assumptions and
experimental implications of RSM have been discussed elsewhere (Anderson & Whitcomb
2005).
The main objective of this study was to statistically investigate the influence of three
pulping variables, cooking temperature, time-at-temperature and alkali charge, on pulp
quality. Their influences are measured by four response variables: screened yield, Kappa
number, fibre strength and pulp viscosity. The complex effects of pulping variables on each
response variable were, as mentioned earlier, examined and analysed by the statistical
experimental design RSM utilising the central composite design (CCD) approach. To
facilitate the analyses, statistical software DESIGN-EXPERT of Stat-Ease, Inc. USA was
used to optimise the above-mentioned three parameters.

MATERIALS AND METHODS

The raw material used in this study was whole kenaf of five months old, a variety of V36 and
was obtained from a trial plot at the Malaysia Agricultural Research and Development
Institute (MARDI), Serdang, Selangor. The whole supply of raw material was taken from one
harvest, and it was ensured within practical limits to minimise the variations in the raw
material supply. Before pulping, the raw material was chipped, sorted, washed, cleaned and
air-dried.

Experimental design
Response surface methodology was utilised to optimise the pulping process and a central
composite design (CCD) was adopted. CCD involves outlining the composition of the
experimental process conditions around a central combination and then subsequently used to
develop the regression models. For a three independent variable process (k=3), this design
consists of factorial design points with eight (2k, k =3) runs, three centre points, and six (2 k)

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axial or star points. The central combination for the experimental design was as follows:
cooking temperature T = 170 oC, time-at-temperature t = 90 min and alkali charge A = 25%,
with variable ranges of 160 to 180 oC, 60 to 120 minutes and 20 to 30%, respectively.

Pulping
Pulping trials were carried out in a M/K System digester. In each pulping, 250g (o.d.) of
whole kenaf were cooked. The conditions employed throughout the experiment were as
follows: liquid to the material ratio was 8:1, AQ was 0.1% of kenaf and time to maximum
temperature was 90 min. At the end of digestion, the softened pulp was disintegrated for 5
min in a hydrapulper, washed on a screen and screened using Somerville fractionators. Kappa
number, fibre strength and pulp viscosity was determined according to TAPPI T 236, T 231
and T 230 (TAPPI 1994).

RESULTS & DISCUSSION

Response surface analysis of soda-AQ pulping
The results are summarising in table.

Name Units Obs Minimum Maximum

Screened Yield % 20 26.64 44.40
Kappa no 20 5.25 22.68
Fibre Strength N 20 35.42 170.99
Pulp Viscosity cP 19 2.86 36.73

By employing DESIGN-EXPERT of Stat-Ease, a computer-aided response surface analyser,

the most compatible model among mean, linear, quadratic and cubic expressions are fitted to
each response based on all the statistical analysis results available. For some of the responses,
transformation (mathematical conversion of response values) was needed to correct the non-
normality in the error term. The appropriate choice of transformations depends on the subject
matter and/or statistical considerations. Based on statistical analysis of each coefficient, the
insignificant coefficients, which have values nearest to zero, are eliminated from the models
to reduce the response surface model and to obtain better estimation models. The following
equations 4 to 9 are reduced models for each response:

Screened yield, = 109.71266-0.35176 * T - 1.298110.003 * t - 0.46998* A ……(1)

%

Kappa no = 861.51612 - 8.30048 * T - 0.71084 * t - 5.99017 * A + ……(2)

0.020554 * T2 + 2.430090.004* t2 + 0.035336 * A2 +
3.56667 0.003 * T* t +0.022750 * T* A +6.333330.004 * t* A

Fibre Strength, = -6882.62940 +76.40723 * T+0.033378 *t +54.29180* A - ……(3)

Nm/g 0.20624* T2 - 0.31784* T* A

Pulp Viscosity, = 104.29094+0.16611* T-0.11604* t+0.68327* A +0.14644* ……(4)

cP A2 -0.050475 * T* A

T = Cooking Temperature (oC), t = Time at Temperature (min), A = Alkali Charge (%)

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 Optimisation of pulping conditions
The response values obtained allow the calculation of mathematical estimation models for
each response and are subsequently used to find the optimum set of operating conditions for
the independent variables and to characterise the nature of the response surface.
The optimisation module in DESIGN-EXPERT will search for a combination of factor
levels that simultaneously satisfy the requirements placed on each of several responses. The
fundamental operating concepts of numerical optimisation used in this study have been
discussed elsewhere (Myers and Montgomery 1995). With computer-aided software,
optimisation of the pulping condition can be easily determined to the desired values or ranges
of responses. In producing pulp rayon grade, the pulp should be high yield, low kappa
number, high strength and high viscosity. The selected ranges of values of responses
(response criteria) that were used and the associated pulping conditions chosen by DESIGN-
EXPERT are pulping at 161.22oC for 120 minutes with 20% alkali charge makes the best
compromise for high pulp screened yield (45%) and low residual lignin content (Kappa
number = 13). Nevertheless, other values or ranges of responses could also be selected for
different end usage of pulps. As such, it would be the desired properties of the final product
that will dictate the optimised conditions.

CONCLUSION
The overall effect of soda-AQ pulping of kenaf is promising. A rayon grade pulp with good
bleaching characteristics (low Kappa number) and a good yield could be easily obtained.
Response surface methodology (RSM) with central composite design is a powerful tool for
optimisation of a process such as pulping which involves several processing variables and
several response variables. It also allows the study on the interaction effects of the former
with the later. Quadratic models provided a good fit relationship between the three pulping
variables, viz. cooking temperature, time-at-temperature and alkali charge studied.

REFERENCES
Anderson, M.J. & Whitcomb, P.J. 2000. DOE Simplified: Practical Tools for Effective
Experimentation. Productivity Press, New York, USA.
Anderson, M.J. & Whitcomb, P.J. 2005. RSM Simplified: Optimizing Processes Using
Response Surface Methods for Design of Experiments. Productivity Press, New
York, USA.
TAPPI. 1994. TAPPI Test Methods 1994-1995. TAPPI Press, Atlanta, USA.
Myers RH, Montgomery DC (1995) Response surface methodology: process and product
optimization using designed experiments. Wiley, New York, USA.