Composites: Part A 31 (2000) 97106

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New polymer mortars containing polymeric wastes.

Part 1. Microstructure and mechanical properties
M.C. Bignozzi, A. Saccani, F. Sandrolini*
Dipartimento di Chimica Applicata e Scienza dei Materiali, Facolta` di Ingegneria, Universita di Bologna, Via Risorgimento 2, I-40136 Bologna, Italy
Received 8 March 1999; received in revised form 19 July 1999; accepted 6 August 1999

Abstract
Recycling industrial wastes as filler components and/or aggregates in polymer mortars makes these materials very interesting from an
ecological and safety point of view. In addition, the resulting materials have useful physical and mechanical properties. Four recycled fillers
(powdered rubbers, tyre rubbers, micronized tyre fibers and milled electrical cable wastes) have been used to formulate new polymer mortars.
The comparison of their mechanical properties and microstructures with those of a plain polymer mortar indicates that the presence of
recycled waste affects the physicalmechanical behavior (compressive and flexural strengths, microstructure). The use of silane coupling
agents has been also considered and its effect in leading to more compact materials is reported and discussed. q 2000 Elsevier Science Ltd.
All rights reserved.
Keywords: Polymer mortars; A. Recycling; B. Mechanical properties

1. Introduction
Polymer mortars and concretes have obtained wide
acceptance as materials for many applications thanks to
their versatility in formulation and processing combined
with high-strength and rapid setting properties. Chemical
and corrosion resistance, ease of placement, long durability,
low permeability, high damping and dynamic and thermal
stability are some of the advantages that make these polymer composites suitable for precast components, bridge
deck overlays, artificial marbles, repair materials for
concrete structures and machine tool basements [111].
Moreover, as great interest has been shown recently in
construction materials with ecological and safety characteristics [1222], polymer mortars and polymer concrete are
very attractive because of their capability for using recycled
waste products. The importance of this new aspect of polymer composites has been developed primarily through two
different approaches. On the one hand, as the high cost of
the resin is usually considered the main factor limiting the
growth of polymer concrete and mortars, a lot of work
[1518] has been done on the production of unsaturated
polyester resins from recycled poly(ethyleneterephthalate)
(PET). On the other hand, industrial wastes such as fly ash
* Corresponding author. Tel.: 139-0520-93205; fax: 139-0520-93213.
E-mail address: franco.sandrolini@mail.ing.unibo.it (F. Sandrolini).

[12,13], slag and wood chips [23] have been successfully

used for replacing or partially substituting the filler components in polymer mortars. However, only a few examples of
the use of recycled organic fillers have been reported [19
22,24].
The characteristics of particulate polymer composites
depend upon different factors such as the type and the
amount of the binder [25], the amount, size and type of
aggregates and fillers. Fine fillers such as calcium carbonate
are largely used in polymer mortars and plastic materials
because of their low cost. The ability to fill the voids
between solid particles (thus replacing polymeric materials)
and to be easily dispersed in the mixture makes fillers very
useful in polymer mortar preparations. However, the higher
stiffness and strengths obtained through filling are often
associated with drawbacks, such as reduced workability
and processability.
The aim of the present work has been to prepare new
polymer mortars formulated with recycled plastic fillers to
obtain materials with tailored mechanical and physical characteristics. For this purpose, some organic fillers, characterized by different size and origin, have been used in the
mixture formulations. Powdered rubbers deriving from
acrylonitrilebutadiene rubber production, tyre rubber,
micronized tyre fibers deriving from milled waste tyres
and plastic granulates coming from milled waste electrical
cables, were selected as recycled fillers for the work. To

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PII: S1359-835 X( 99)00 063-9

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Table 1
Properties of recycled organic fillers
Filler

Size (mm)

Density a at 238C (g/cm 3)

TR
MTF
EC
PR

0.0751.0

310
0.1250.5

1.31
1.38
1.33
1.20

Calculated by volumetric titration [32].

further enhance the mechanical properties of the new polymer mortar composites, the use of coupling agents was also
investigated in the presence of the organic fillers. It is well
known that coupling agents usually act as modifiers of the
interfacial bond between the aggregate [26,27] and the polymer matrix, but their action as promoters of filler dispersion
and modifiers of matrix morphology has to be considered
[28,29]. In order to evaluate the effect of the filler nature and
its size distribution in the composites and the use of a
coupling agent, the mechanical properties and microstructures of the new polymer mortars have been compared with
the behavior of a plain polymer mortar. Recycled polymeric
and rubber waste based materials can be also considered
very attractive for their potential applications as noise
barriers and high skid resistance pavements, as recently
studied [30,31]. Regarding this, the damping effect of the
organic filler additions in the new polymer mortar formulations is being studied and results will be published in a
following paper.

2. Experimental procedure
2.1. Materials
Commercially available orthophthalate type unsaturated
polyester resin (FS0956/AMV/I SIRESTER) was used as
binder with a 50% dimethylphthalate solution of 2-butanone
peroxide as catalyst. The resin has a styrene content of
31 wt%. Normal silica sand (UNI EN 196-1), with a size
distribution 0.0752.0 mm, was used as the base inorganic
aggregate to reproduce the standard preparations of cement
mortars. Commercially available calcium carbonate (Cari,
Bologna, Italy) with an average size of 2.5 mm was used as a
fine filler. Tyre rubber (TR) (Remida, Modena, Italy),
micronized tyre fibers (MTF) (Remida, Modena, Italy),
waste electrical cable (EC) (Metalferro, Teramo, Italy)
and powdered rubber (PR) (Reevs, Lodi, Italy), a byproduct
of rubber production, were used as recycled organic fillers.
Their properties are given in Table 1. Micronized tyre fibers
are mainly composed of polyester fibers ( < 50%), rayon
( < 20%) and nylon ( < 30%), powdered rubbers are
based on acrylonitrilebutadiene rubber while waste electrical cables are chiefly formed from polyvinylchloride,
polyethylene and some thermosets.
Titanium(IV)(triethanolaminato)isopropoxide (Aldrich),

3-aminopropyltriethoxysilane (Aldrich), 3-glycidoxypropyltrimethoxysilane (Aldrich) and Silanogran V (Kettlitz)

were used as coupling agents.
2.2. Specimen preparation
In a previous experimental study [24] the maximum
amount of polymeric waste replacing an equal volume of
inorganic aggregate in mortar formulations, still keeping a
workable mixture and without a marked reduction in
mechanical properties, was found to be 3 vol%. This
amount of sand has been replaced by a different organic
filler in all mixtures. Polymer mortars, with recycled plastic
fillers, were prepared according to the following procedure.
Sand, organic fillers and calcium carbonate were firstly
mixed in a Hobart mixer (UNI EN 196-1) and afterwards
the unsaturated polyester resin premixed with the catalyst,
was added. The binder formulation and the mix proportions
of the mortars studied are reported in Table 2: 3 vol% of
sand was replaced by an equivalent volume of recycled filler
and the samples were designated, respectively, EC3, PR3,
TR3 and MTF3. Polymer mortar without any organic filler
was also prepared as a control sample and designated by S.
The influence of coupling agents on the mechanical properties was investigated using treated aggregates. Coupling
agents titanium(IV)(triethanolaminato)isopropoxide, 3aminopropyltriethoxysilane, 3-glycidoxypropyltrimethoxysilane and Silanogran V were added directly to the sand
and were dispersed by intimate contact of the sand grains
when mixed manually. 1% (based on the resin content) of
the coupling agent was used. Preliminary experimental
studies were carried out to determine which coupling
agent had the best performance. It was observed that the
most effective from a mechanical and microstructural
point of view was 3-glycidoxypropyltrimethoxysilane.
Accordingly, five samples designated S p, EC3 p, PR3 p,
TR3 p and MTF3 p were prepared using 3-glycidoxypropyltrimethoxysilane according to the procedure described
above. Their composition was equivalent to that of specimens S, EC3, PR3, TR3 and MTF3, apart from the presence
of the silane.
Prismatic mechanical test specimens 40 mm 40 mm
160 mm of all the mixtures were molded and cured for
14 days at room temperature and ,40% RH, and stored
under these conditions until tested.
2.3. Characterization
Measurements of the mechanical strengths (both
compressive, s c, and flexural, s f), were carried out on all
samples using an Amsler Wolpert testing machine
(200 kN): at least five measurements for each composition
were made. Dynamic elasticity modulus was determined by
ultrasonic measurements using a Controls Ultrasonic Tester
E46. Pore size distribution measurements were carried out
with a mercury porosimeter, Carlo Erba 2000, equipped
with a macropore unit. Microstructural observations were

Sample

Binder FS0956 (wt%) a

Sand (wt%) a

CaCO3 (wt%) a

Coupling agent (wt%) b

Recycled filler type

Recycled filler (wt%) a

Replaced sand (vol%) c

S
EC3
PR3
TR3
MTF3
Sp
EC3 p
PR3 p
TR3 p
MTF3 p

12.0
12.0
12.0
12.0
12.0
12.0
12.0
12.0
12.0
12.0

76.00
74.80
74.90
74.80
74.70
75.88
74.68
74.78
74.68
74.58

12.0
12.0
12.0
12.0
12.0
12.0
12.0
12.0
12.0
12.0

1
1
1
1
1

EC
PR
TR
MTF

EC
PR
TR
MTF

1.2
1.1
1.2
1.3

1.2
1.1
1.2
1.3

3
3
3
3

3
3
3
3

Based on the whole composition.

Based on the resin content.
c
Vol% of replaced sand by recycled filler (sand density has been assumed equal to 2.5 g/cm 3).
b

M.C. Bignozzi et al. / Composites: Part A 31 (2000) 97106

Table 2
Mix proportions of polyester mortars

99

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M.C. Bignozzi et al. / Composites: Part A 31 (2000) 97106

Table 3
Mechanical properties and standard deviations of modified and unmodified
composite polyester resin mortars
Sample

s f (MPa)

s c (Mpa)

E (GPa)

S
EC3
PR3
TR3
MTF3
Sp
EC3 p
PR3 p
TR3 p
MTF3 p

31.1 ^ 1.7
23.7 ^ 1.9
25.6 ^ 1.7
25.1 ^ 2.1
25.3 ^ 1.9
33.9 ^ 2.2
31.3 ^ 2.0
32.5 ^ 1.3
30.6 ^ 1.4
27.7 ^ 2.6

108.8 ^ 2.6
98.4 ^ 2.9
86.9 ^ 1.9
89.4 ^ 1.2
87.8 ^ 2.1
117.1 ^ 2.6
107.4 ^ 2.2
90.6 ^ 1.8
100.4 ^ 1.8
93.4 ^ 3.0

28.1 ^ 0.7
26.5 ^ 0.1
24.4 ^ 0.2
24.7 ^ 0.1
23.8 ^ 0.7
27.1 ^ 0.7
27.2 ^ 0.1
25.0 ^ 0.4
25.6 ^ 0.3
23.8 ^ 0.5

performed on the undisturbed fracture surface resulting

from flexural tests with a Philips 501 B scanning electron
microscope (SEM): phases recognition was aided by the use
of EDAX 9800 micro-analysis. Disks (46 mm thick), for
electrical characterization, were obtained from flexural test
fragments by sawing. A suitable three-terminal configuration was deposited on the disks by gold evaporation in
vacuo. Electrical volume conductivity, at 258C and 50 ^
10% RH, was measured according to ASTM D257 under
an electrical field of 1 kV/cm, applied by a Keithley 237
power supply. Currents flowing through the samples were
recorded as a function of time up to 3600 s with a Keithley
617 electrometer. A detailed description of cells, instrumentation and measuring procedures is reported elsewhere [33
35].

3. Results and discussion

Mechanical characteristics of samples EC3, TR3, PR3
and MTF3, containing 3 vol% of different plastic fillers

are reported in Table 3 and compared to the mechanical

properties of the control polymer mortar, S. The compressive (s c) and flexural (s f) strengths of the mixtures investigated are 87108 MPa and 2531 MPa, respectively, and
the dynamic elastic modulus 23.828.2 GPa. All the specimens prepared with the recycled fillers show mechanical
characteristics lower than the control sample S, but
compressive strength values are higher than the compressive strength of an ordinary Portland cement (OPC) mortar
(about 50 MPa after 28 days curing, with a water/cement
ratio of about 0.5 [36,37]). Concerning the flexural strength,
the effect of the filler does not depend on its nature, although
for sample EC3 the decrease in compressive strength and
elastic modulus is less evident than those observed for the
other organic filler based composites.
The mechanical properties of samples EC3 p, TR3 p, PR3 p
MTF3 p and S p, prepared using the coupling agent 3-glycidoxypropyltrimethoxysilane, are also reported in Table 3
and compared to the similar polymer mortars prepared without using the organo-silane compound. As can be observed,
there is an overall increase in both the above flexural and
compressive strengths due to the silane treatment of the
sand, even if it is more remarkable for the polymer mortars
containing organic based fillers than for the reference
sample. Polymer mortars containing 3 vol% of electrical
cables based fillers (EC3 p) show the highest above flexural
strength increase (,32%), whereas samples containing
3 vol% of tyre rubbers based fillers (TR3 p) show the highest
above compressive strength increase (,12%). In addition,
the mechanical properties of samples prepared with the
coupling agent are in some cases almost the same as those
of the untreated plain polymer mortar S that was used as the
reference sample.
The role of the coupling agent is known to be not only to
create physicalchemical bridges between the polyester
matrix and sand by forming interpenetrating networks

Fig. 1. FT-IR spectra of the coupling agent 3-glycidoxypropyltrimethoxysilane at different times.

M.C. Bignozzi et al. / Composites: Part A 31 (2000) 97106

101

Fig. 2. Total intruded volume for samples S, S p, EC3, EC3 p, MTF3 and MTF3 p.

promoting adhesion, but also to increase the filler dispersion

by wetting the particulate surfaces to uniformly spread the
resin during the mixing [2629]. In order to investigate
further which was the prevalent effect here, FT-IR measurements on 3-glycidoxypropyltrimethoxysilane were made,
after contact for different times with the sand at room conditions: the hydrolysis of the methoxy groups linked to the
Si atom should have occurred and the SiOH band should
have appeared under these conditions, which reproduced the
experimental procedure used in polymer mortar preparation.
After 1 h, the presence of the peak characteristic of the
SiOH bond (35003600 cm 21) was not detected (Fig. 1).
Similar FT-IR spectra (not reported), without the evidence
of the SiOH peak, were obtained for the coupling agent
after its contact with the recycled organic fillers. This result
appears to indicate that, in the present study, the prevalent
effect of the coupling agent is the promotion of filler disper-

sion. Figs. 2 and 3 show the results of mercury intrusion

measurements for all the samples. All the materials have
lower porosity compared to the conventional cementitious
based composite that usually ranges between 50 and
70 mm 3 of Hg intruded volume per gram [36]. The addition
of organic fillers increases the overall porosity accordingly
to a more difficult procedure in sample preparation due to a
less workable mixture: however, the use of the coupling
agent always leads to more compact materials. In order to
evaluate the effect of microstructural modifications in the
range of smaller porosity, Figs. 4 and 5 report mercury
intrusion in pores of size smaller than 0.1 mm. In this
porosity range the coupling agent has almost no effect on
the plain polymer mortars (which are however the least
porous of all) and on the samples containing tyre rubber
(TR3 p) and powdered rubber (PR3 p) based fillers. The silane
treatment leads to lower porosity for polymer mortars

Fig. 3. Total intruded volume for samples PR, PR3 p, TR3 and TR3 p.

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M.C. Bignozzi et al. / Composites: Part A 31 (2000) 97106

Fig. 4. Total intruded volume for porosity whose dimension is lower than 0.1 mm for samples S, S p, EC3, EC3 p, MTF3 and MTF3 p.

formulated with micronized tyre fibers (MTF3 p) compared

to the relevant untreated sample (MTF3), whereas the
results are reversed for electrical cable (EC3 p) based fillers
below a pore size of 0.01 mm.
Figs. 6 and 7 show SEM microstructures of S and S p
samples. Both samples show a similar compact matrix
with a few voids in the surface near to the aggregates
thus indicating that the coupling agent appears not to
influence the microstructure in this case. Figs. 8 and 9
refer to polymer mortars EC3 and EC3 p and, Figs. 10
and 11 to samples MTF3 and MTF3 p. Organic particles
were recognized by their morphology and with the aid of
local EDAX analysis: again the microstructure of the
modified samples containing the coupling agent are similar to the relevant unmodified polymer mortars. However,
a slightly more compact microstructure can be observed
for EC3 p in Fig. 9 and a better adhesion of the filler phase
is shown by the decrease of the voids between matrix and
organic particles. A similar behavior can be observed in

Fig. 11 for MTF3 p sample, where the coupling agent

seems to improve the adhesion between all the different
phases present in the composite material. Figs. 12 and 13
refer to samples PR3 and PR3 p containing powdered
rubber: again, though the filler appears to be well
embedded in the matrix, the coupling agent leads to a
more compact microstructure.
In several polymer mortar applications (conduits, outdoor
insulators, etc.) electrical properties are extremely important: therefore the volume electrical conductivity of the new
formulations have been determined at room temperature.
Electrical conductivity of unmodified and modified samples
is reported in Figs. 14 and 15 as a function of time after
voltage application. All samples, regardless of their composition, behave as insulating materials showing large charging transients as a function of time. Electrical conductivity
varies from 1:7 10214 to 3:1 10216 S=cm for polymer
mortars untreated with the coupling agent, whereas conductivity values of the samples containing the silane compound

Fig. 5. Total intruded volume for porosity whose dimension is lower than 0.1 mm for samples PR3, PR3 p, TR3 and TR3 p.

M.C. Bignozzi et al. / Composites: Part A 31 (2000) 97106

Fig. 6. SEM observations of sample S (160 , marker 10 mm).

103

Fig. 9. SEM observations of sample EC3 p (40 ).

Fig. 7. SEM observations of sample S p (160 ).

Fig. 10. SEM observations of sample MTF3 (320 , marker 10 mm).

Fig. 8. SEM observations of sample EC3 (40 , marker 10 mm).

Fig. 11. SEM observations of sample MTF3 p (320 , marker 10 mm).

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M.C. Bignozzi et al. / Composites: Part A 31 (2000) 97106

Fig. 12. SEM observations of sample PR3 (1250 ).

Fig. 14. Volume conductivity of samples S, EC3, TR3, PR3, MTF3.

mortar formulations has been investigated from a

mechanical and microstructural point of view. The following conclusions may be drawn:

Fig. 13. SEM observations of sample PR3 p (1250 ).

are 1:7 10213 to 3:3 10215 S=cm: The organic filler

addition results in a slight volume electrical conductivity increase for samples TR3 and EC3 that can be
considered negligible, whereas for MTF3 and PR3 the
increase is more evident and it is presumably owed to
impurities contained in the relevant organic fillers. The
coupling agent reduces the porosity of the samples, but
increases the electrical conductivity of all samples: the
latter effect may be ascribed to the introduction of ionic
charge carriers induced by the long-term hydrolysis of
3-glycidoxypropyltrimethoxysilane.

Compressive and flexural strengths of the resin composites prepared using recycled organic fillers decrease with
reference to a plain polymer mortar, but they are still
higher than the mechanical properties shown by an ordinary Portland cement (OPC) mortar. However, the addition of recycled organic fillers increases sample porosity,
particularly at the interphases between the resin/extender
matrix and the filler grains.
The use of 3-glycidoxypropyltrimethoxysilane treated
aggregates improves the mechanical behavior of the
new polymer composites and decreases the porosity,
thus leading to more compact materials. As the observed
porosity reduction is higher in the macroporosity range,
the coupling agent appears to mainly act as a wetting
agent.
The presence of recycled organic fillers and coupling
agent leads to higher electrical conductivity values in
comparison with those of a plain polymer mortar: the
organic filler introduction has a minor influence on the
electrical conductivity than the addition of the coupling
agent in the composite formulations. However, all the
composite materials obtained can be still classified as
insulators.

Acknowledgements
4. Conclusions
The influence of organic recycled fillers in new polymer

Financial support of Consorzio R&S (Carpi, Modena,

Italy) and MURST 60% are gratefully acknowledged.

M.C. Bignozzi et al. / Composites: Part A 31 (2000) 97106

105

Fig. 15. Volume conductivity of samples S p, EC3 p, TR3 p, PR3 p, MTF3 p treated with silane coupling agent.

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