ELSEVIER S0032-3861(96)00235-2
Polymer Vol. 37 No. 18, pp. 4141-4148, 1996
Copyright © 1996 Elsevier Science Ltd
Printed in Great Britain. All rights reserved
0032-3861/96/$15.00 + 0.00
Kinetic investigation of the free-radical
crosslinking copolymerization of styrene
with a mixture of divinylbenzene isomers
acting as the crosslinker
S. Sajjadi*, S. A. M. Keshavarz and M. Nekoomanesh
Polymer Research Center of Iran, PO Box 14185/458, Tehran, /ran
(Received 2 November 1994; revised 3 July 1995)
The objective of this paper is to study the crosslinking copolymerization of styrene (S) with a mixture of
para- and meta-divinylbenzenes (mixed-DVBs). The crosslinking copolymerization, initiated with benzoyl
peroxide (BPO), was performed at temperatures of 70, 80, and 90°C. The mole ratio of DVB to S was kept
small, i.e. within 4-8%. At various stages of the polymerization the overall conversion of the monomers to
sol and gel were measured by gravimetry. The sol and gel formations with time were also measured. The gels
were characterized by equilibrium swelling measurements as a function of the overall degree of conversion.
The experimental data were then incorporated into the kinetic model developed by Tobita and Hamielec.
The kinetic parameters involved in the crosslinking copolymerization of S/DVB were also estimated. A
satisfactory agreement of the results obtained from the experimental measurements with the predictions of
the model was observed. Copyright © 1996 Elsevier Science Ltd.
(Keywords: crosslinking; free-radical copolymerization; kinetics)
INTRODUCTION
Most modern ion-exchange resins consist of a synthetic
polymer backbone to which is attached a functional
group that gives each ion exchanger its specific properties.
The polymer matrices are usually crosslinked to make
them insoluble and to give them mechanical strength
and stability. The most common matrices are styrene-
divinylbenzene (S/DVB) copolymers in which DVB is the
crosslinking agent, and is typically present in 4-12%
concentration.
The copolymerization of DVB with S was first
studied by Staudinger and Heuer 1, who demonstrated
that crosslinking does occur for S/DVB systems.
Storey 2 compared the initial rates of the S/p-DVB
copolymerization with those measured for S and p-DVB
hompolymefization and concluded that crosslinking
results in an increase in the reaction rate. Gel times were
measured and it was concluded that the higher the content
of crosslinker, then the less would be the conversion
required to reach the gelation point. The overall first-order
rate constants for S/p-DVB copolymerization over a
broad range of compositions, initiated by 1% BPO at
temperatures of 70 and 90°C, were calculated. The
conversion-time curves obtained from dilatometric
measurements for 4, 10, and 20% p-DVB at 70°C were
also reported. It was postulated that all of the double
bonds in the S/p-DVB system are of equal reactivity.
*To whom correspondence should be addressed. Present address:
Department of Chemical Engineering, Loughborough University of
Technology, Loughborough Leicestershire LE11 3TU, UK
Hild and Okasha 3 studied the kinetics of the free-radical
copolymerization of S and commercial DVB (para- and
meta-isomers) in the presence of carbon tetrachloride as
a chain transfer agent. In further work they investigated
the kinetics of free-radical crosslinking copolymerization
of S with p-DVB or m-DVB in benzene solution at
60°C 4. The DVB proportions were kept small with
respect to styrene, in order to reduce the importance of
the DVB radicals in the reaction media. The consump-
tions of S and DVB isomers were measured as a function
of time. The radical reactivity ratios of S with respect to
both m-DVB and p-DVB were also obtained.
5
Malinsky et al. evaluated the copolymer composition
of S with p-DVB or m-DVB, and indicated that after one
of the vinyl groups in the DVB isomers has reacted, the
reactivity of the remaining vinyl group then falls. It was
also concluded that the pendant double bonds in both
the p-DVB and m-DVB units have the same reactivity.
They also evaluated the effect of concentration of the
DVB isomers on the conversion at the gel point. This
conversion was found to depend on the concentration of
DVB at lower values of the latter (< 20%).
Wiley et al. 6 measured the reactivity ratios of S/m-
DVB and S/p-DVB at low conversion by differential
analysis. In further work, they used the integrated form
of the copolymerization equation to determine the
7
reactivity ratios. This method was claimed to avoid
errors encountered in the low-conversion data that was
required for the differential analysis.
Hild and Okasha 8 investigated the crosslinking
copolymerization of S/p-DVB and S/m-DVB in the
post-gel state, and determined the swelling degree and
POLYMER Volume 37 Number 18 1996 4141