Chemical Degradation of Epoxidized Natural Rubber
Using Periodic Acid: Preparation of Epoxidized Liquid
Natural Rubber
P. Phinyocheep,
1,2
C. W. Phetphaisit,
1,2
D. Derouet,
3
I. Campistron,
3
J. C. Brosse
3
1
Department of Chemistry, Faculty of Science, Mahidol University, Rama VI Road,
Phayathai, Bangkok 10400, Thailand
2
Institute of Science and Technology for Research and Development, Mahidol University, Salaya Campus,
Puthamonthon, Nakorn Pathom 73170, Thailand
3
Laboratoire de Chimie Organique Macromoleculaire-Chimie des Polyme `res, UMR CNRS 6011, Universite ´ de Maine,
Avenue Olivier Messiaen, 72085 Le Mans Cedex 9, France
Received 16 October 2003; accepted 14 April 2004
DOI 10.1002/app.20812
Published online in Wiley InterScience (www.interscience.wiley.com).
ABSTRACT: Oxidative degradation of epoxidized natural
rubber (ENR) was effectively performed in latex phase by
using periodic acid at 30°C. The ENR was prepared from the
epoxidation of natural rubber in latex phase using performic
acid generated in situ by the reaction of hydrogen peroxide
and formic acid. The prepared ENR latex was subsequently
treated with periodic acid. It was found that the higher the
amount of the periodic acid employed the faster the molec-
ular weight of the ENR decreased. Different epoxidation
levels of the ENR had no significant effect on the degrada-
tion reaction. Based on
1
H NMR analysis, the epoxide con-
tent in the epoxidized liquid natural rubber (ELNR) ob-
tained was about the same as that observed in the ENR
before degradation. FT-IR analysis showed an increase in
carbonyl signal after prolonged reaction time or when
higher amounts of periodic acid were employed. © 2004
Wiley Periodicals, Inc. J Appl Polym Sci 95: 6 –15, 2005
Key words: degradation; epoxidation; modification; rubber;
telechelics
INTRODUCTION
Chemical modifications or functionalizations of poly-
meric materials are of wide interest to research scien-
tists as they often produce new materials that cannot
be prepared or are costly to prepare by means of
conventional polymerization reactions. These meth-
ods are also used to improve the properties of some
commercial polymers or to introduce specific reactive
intermediates on the polymer chains for further mod-
ification. Epoxide function is considered to be one of
the most important intermediate in organic synthesis.
The introduction of epoxides on the backbone of nat-
ural rubber (NR) will render NR essentially resistant
to oil.
1
The epoxide function is also susceptible to
various chemical reactions involving hydrogen-donor
molecules, such as amines, alcohols, and carboxylic
acids. The NR is a high-molecular-weight natural
polymer. Therefore, degradation of NR into low-mo-
lecular-weight rubber and functionalization with spe-
cific functional groups, such as epoxide, would widen
the applications of NR. It is possible to lower the
molecular weight of the NR before the process of
introducing functional groups to NR is conducted.
Oxidative degradation of NR promoted by phenylhy-
drazine/oxygen system has been reported.
2
The
method was employed by Phinyocheep and Duang-
thong
3
to prepare liquid natural rubber (LNR) before
conducting an epoxidation reaction by using perfomic
acid generated in situ from the reaction of formic acid
and hydrogen peroxide. However, the obtained LNR
has a brown color, which may be due to the contam-
ination of the reagents used or to the nonrubber con-
stituents in the NR. Oxidative degradation of depro-
teinized NR by using potassium persulfate provided
the LNR with a light color.
4,5
However, the epoxida-
tion of deproteinized LNR in latex phase using in situ
performic acid carried in our laboratory was accom-
panied by side reactions, such as epoxide ring opening
reaction, leading to 1,2-diol unit and formyl addition
adducts.
Lead tetraacetate, Pb(OAc)
4
and periodic acid
(H
5
IO
6
) are chemicals of interest used for degradation
of the polyisoprenic chain. Typically, both reagents
cause cleavage of vic-glycols to yield carbonyl com-
pounds. Studied by Burfield and Gan,
6
Pb(OAc)
4
was
found to cause degradation of hydrolyzed epoxidized
synthetic rubber (EIR) faster than that of EIR. Syn-
thetic polyisoprene sample (IR), which presumably
contains no 1,2-diols, was also slowly degraded by
Correspondence to: P. Phinyocheep (scppo@mahidol.ac.th).
Journal of Applied Polymer Science, Vol. 95, 6 –15 (2005)
© 2004 Wiley Periodicals, Inc.