Accepted Manuscript

Exploitation of waste date seeds of Phoenix dactylifera in form of polymeric particle

biocomposite: Investigation on adhesion, cohesion and wear

Alessandro Ruggiero, Petr Valášek, Miroslav Müller

PII: S1359-8368(16)31422-6
DOI: 10.1016/j.compositesb.2016.08.014
Reference: JCOMB 4462

To appear in: Composites Part B

Received Date: 26 July 2016

Revised Date: 17 August 2016
Accepted Date: 17 August 2016

Please cite this article as: Ruggiero A, Valášek P, Müller M, Exploitation of waste date seeds of Phoenix
dactylifera in form of polymeric particle biocomposite: Investigation on adhesion, cohesion and wear,
Composites Part B (2016), doi: 10.1016/j.compositesb.2016.08.014.

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Exploitation of waste date seeds of Phoenix dactylifera in form of polymeric

particle biocomposite: investigation on adhesion, cohesion and wear *

Alessandro Ruggieroa+, Petr Valášekb, Miroslav Müllerb

a
University of Salerno, Department of Industrial Engineering, Salerno, Italy
b
Czech University of Life Sciences Prague, Faculty of Engineering, Department of Material

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Science and Manufacturing Technology, Prague, Czech Republic

Abstract

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An interaction of polymers with biological fillers can optimize their mechanical properties or
it can lead to a possibility to substitute commonly used both biological as well as synthetic
materials, e.g. wood. The paper focuses on a possibility to exploit the waste from a process of

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date fruit processing – the plant Phoenix dactylifera - represented by a stone and residues of
flesh in a form of biocomposites with a technologically undemanding process of a
preparation. A description of adhesive and cohesive characteristics belongs to factors

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influencing the application area of these materials. Variable concentrations 0.5-10.0 wt. % of
microparticles prepared from the fruits – dates – in a form of the stones and the flesh in the
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epoxy resin were experimentally tested. The particles did not significantly decrease the
adhesive characteristics of the resin. The low concentration of the filler did not decrease the
cohesion of the system, it came up to 10.8% increase of the shear strength and up to 11%
increase of the wear resistance at the specific concentrations of used biofillers. The date stone-
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based particles increased the abrasive wear resistance. SEM was used for the evaluation of a
morphology of particles and a fracture surface analysis.
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Key words: adhesion; cohesion; microparticles; stone; flesh; tribology; wear

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1. Introduction
Biocomposites are materials consist of single phases based on organic materials or
they combine organic materials (phases) with inorganic phases [1-3]. The design of new
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materials based on natural renewable resources is essential for both environmental and
*
The results of this work have been presented at the 2016 International Workshop on
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Multiscale Innovative Materials and Structures (MIMS16), Cetara (Salerno), Italy, 28-30
October 2016
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+ Corresponding Author: Prof. Alessandro Ruggiero – Department of Industrial Engineering-

University of Salerno, Via Giovanni Paolo II, nr. 132 84084 Fisciano ITALY Tel. +39 089964312
Fax +39 089964037 Mobile +39 3478647854 [email protected]
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economic analyses [4]. Plastics filled with natural fillers have been introduced as new sources
of raw materials in various industries and have found their way through many applications
such as automotive, building and furniture's industries. Biocomposites belong among
materials which have been developed in a progressive way, however, the biological essence of
the material hints a certain restrictions. Polymers filled with fibres create a great part of these
biocomposites [2].
Also organic particles can find their utilization, e.g. Funabashi et al. [5] used

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polyuretan for filling with particle fillers in a form of wooden powder, coffee grounds and
powdered cellulose. The polyuretan saturation with these fillers ranged in the interval 10 to
90 wt. %, when the particle size corresponded to the interval 12 µm (the cellulose) to

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1726 µm (the coffee grounds). The research also proved a clear influence of a shape of the
filler particles on resultant mechanical characteristics.
Mousavi et al. [6] show that adding maleic anhydride and eggshell nanoparticles

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instigates an improvement in mechanical properties as well as better adhesion among
polymer, starch and corn particles. Also wooden sawdust belong among widespread natural
particle fillers [7-8]. Also powders prepared not only from common types of trees can be used

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for filling of polymers. Ge et al. [9] state e.g. a utilization of a bamboo powder in the
interaction with PVC and they refer to the use of these materials for a surface treatment of
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materials in the area of wood constructions. Another possibility is filling the polymers with
fruit husks. El Moumen et al. [10] present in their study a utilization of argan nut husks in a
form of microparticles, these particles were used for filling of PP matrix. Siracusa et al. [11]
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performed similar research who dealt with a composite system based on a polymer and a
powder from olive husks. Crespo et al. [12] describe mechanical properties of a composite
based on almond husks, obtained as a by-product of the agri-food industry. They were used as
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a filler combined with PVC thermoplastic matrix. Yang et al. [13] describe increasing
modulus of the elasticity at thermosetting polymers with an inclusion of rice-husk flour.
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Shivamurthy et al. [14] used cakes formed during a process of seeds pressing in their
experiment. This secondary raw material (waste cakes) was added into an epoxy resin in a
form of particles of the size 36.6 µm. Biohusks can be also used according to Gope et al. [15]
for optimizing of an impact strength of epoxy resins.
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Mentioned references show a wide use of biological materials in the area of the
composite systems. A plant Phoenix dactylifera belongs also among plants whose secondary
products can be used in the interaction with polymers in a similar way as e.g. fruit husks.
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Phoenix dactylifera (see Fig. 1) is a plant which is widespread in the subtropical belt
and it is grown for its fruits – dates above all. Plants are grown in North Africa, in the area of
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Middle East, in China but also in other countries. Dates form a significant component of food
in some countries. Said et al. [16] state that e.g. up to 85,000 tons of date waste per annum is
produced in Algeria. This biomass is easily available in countries of its origin and a price of
this commodity is negligible. The date seeds are used for food preparation, they can be a
source of the date oil. The fruits are not the only commodities which are used industrially. In
terms of a material engineering the date wood above all has been used so far in a form of
building materials, the date leaves are used as a source of the cellulose and in the area of the
composite systems there are used fibres of this plant in the interaction with the polymeric
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materials. Al Maadeed et al. [17] describe also a possibility to use the wood powder of date
palms.

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Fig. 1 Date palm plant [18]

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The aim of the performed experiment is to describe possibilities of the utilization of
secondary biological materials formed during the use of date fruits of the plant Phoenix
dactylifera in the interaction with reactoplastics, the stones above all with the respect to
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residues of a flesh on the stones. The secondary biological materials – agricultural waste can
contribute to solving a lack of raw materials for the particleboard industry, as well as to
decreasing of ecological problems concerning their combustion. The utilization is possible
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also in terms of influencing an adhesion of resins and their price. The reactoplastics in a form
of the epoxy resin were chosen for their good mechanical properties and low technological
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demands for a preparations of composite systems above all. The experiment defines basic
adhesive and cohesive characteristics of the reactoplastics filled with the particles prepared by
a sieve analysis. The dimensional sorting was used owing to the proved influence of the
particle size on observed characteristics [19-21], i.e. the cohesion and the adhesion of the
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system. The results were amended with a hardness and an abrasive wear resistance owing to
the potential application area (surface treatments) following from the references [22]. The
electron microscopy (SEM) was used for a description of the particle filler and the interaction
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of the matrix and the filler.

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2. Experimental program
Materials - fillers
Phoenix dactylifera (L.) fruit is considered as one of the oldest and nutritionally richest
fruits on earth [23]. When processing the dates – fruits of the plant Phoenix dactylifera – the
biomass comes into being which can be further utilized in the form of microparticles for
filling of the resins according to the conclusions coming from the references. The utilization
of all forming commodities during the process of fruit processing can increase the economical
efficiency of this process which is important in poor subtropical countries above all. The date
kernels are of minimum economic value and they are used e.g. in a form of fuel but also as a
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source for a production of α-amylase and invertase at an industrial scale [16]. Remaining
stones of seeds (dates) can be regarded as the waste during the process of the whole fruits
processing. They often carry remaining flesh fibres on their surface differing in their
properties. If the fruits (dates) are pressed, the whole dates are pressed and the cakes come
into being from the whole dates where both the flesh and the stone are present. That is why
the paper focuses on the description of basic mechanical characteristics of biocomposites
prepared from both date stones (DS) and date flesh itself (DF) – the country of the origin:

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China. The results can serve for a prediction of a behaviour of composite systems when the
stone with any remaining flesh will be used in the interaction with the polymer (see Fig. 2 –
the stone with remaining flesh and SEM analysis of particles – 5.0 kV).

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Particular commodities (secondary raw materials – stones and flesh) from which the
microparticles were prepared were dried in a drier under the temperature 105 °C (the drying
time 20 h), then they were hashed by means of the manual knife mill with 20,000 turns·min-1.

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Gained particles were dimensionally sorted by means of analytical sieves when particular
sizes of the microparticles were gained. Particles which went through the sieve with the
dimension of meshes 100 µm and 200 µm were used. So, 4 types of the fillers were prepared:

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DS 0-100 µm, DS 100-200 µm and DF 0-100 µm, DF 100-200 µm.

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Fig. 2 Date stone with remaining flesh (above), SEM: morphology of particle from
stone (left), SEM: morphology of particle from flesh (right)
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Materials – matrix (resin)

The low-molecular two-component epoxy resin Glue Epox Rapid was used as the
matrix – one component (A) is the low-molecular resin with an addition of additives and
second component (B) is polyamidic hardener, basic characteristics are summed up in the tab.
1. The resin was used owing to its perfect adhesion to a variety of materials and to the short
hardening time. Composites formed from the matrices from the reactive resins, i.e. the
reactoplastics, require no technological inputs, i.e. extruders and they are profusely used for

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the experimental description of mechanical properties.

Table 1. Specification of epoxy resin

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Density A Density B Mixing ratio Lap-shear strength
Resin -3
[g·cm ] [g·cm-3] A:B [MPa]
Glue Epox Rapid 1.14-1.16 1.06 100:45 12.9

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Sample preparation
Any special technological procedure (such as vacuum) was not used for the
preparation of composite mixtures. The procedure of the preparation was chosen with a

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respect to the minimization of resulting price of the composite and with a respect to
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possibilities and needs of developing countries. The particles were mechanically mixed into
the resin. The samples were cast into the moulds from a two-component silicone rubber
(hardness, abrasion, tensile strength) or they were applied directly on treated adherent (tensile
shear strength). Composites were prepared with different weight percentages of the filler
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because of the determination of the effect of the particle inclusion on mechanical properties
as: 0.5%, 1.0%, 2.5%, 5.0%, 7.5% and 10.0%.
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Morphological and optical study

Following the technological preparation the porosity of unfilled resin was described at
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first. The fluorescence confocal microscope (Axio Imager Zeiss LSM 800) was used for this
analysis of pores in the resin without the filler. This porosity influences also mechanical
properties of forming composites. The electron microscope - SEM - (Tescan Mira 3 GXM)
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equipped with an energy dispersive X-ray was used for the optical analysis of fillers and the
optical analysis of fracture surfaces. SEM analysis was also used for a check of the filler
distribution – particles in the matrix, e.g. by the evaluation of fracture surfaces.
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Mechanical testing
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Adhesion characteristics (shear strength) were assessed on steel adherents with a

thickness of 1.5 mm in accordance with the standard CSN EN 1465. The surfaces of steel
sheets S235J0 were blasted using the synthetic corundum (Al2O3) of the fraction F80 under
the angle of 90°. Then the surface was cleaned and degreased using perchlorethylene and
prepared to the composite application. Adequate surface treatment of adherents is required
before applying resins [24-25]. The lapping was according to the standard 12.5 ± 0.25 mm
(see Fig. 3-A).
The test samples determined for the specification of the cohesive strength by means of the
tensile strength were prepared according to the requirements of the standard CSN EN
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ISO 3167. Test samples were tested on a universal testing machine. A speed of a cross beam
motion was 6 mm·min-1. The setting of the tensile characteristics was performed in
accordance with the standard CSN EN ISO 527 (see Fig. 3-B).
The hardness of test specimens was measured by the method Shore D (CSN EN ISO 868).
The two-body abrasion was tested on a rotating cylindrical drum device with the abrasive
cloth of the grain size P220 (Al2O3 grains) according to the standard CSN 62 1466 (see Fig. 3-
C). The testing specimen is in the contact with the abrasive cloth and it covers the distance of

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60 m. During one drum turn of 360° it is provoked the testing specimen left above the
abrasive cloth surface. Consequent impact of the testing specimen simulates the concussion.
The pressure force is 10 N. The mean of the testing specimens was 15.5 ± 0.1 mm and their

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height was 20.0 ± 0.1 mm. The mass losses were measured on analytic scales weighing on
0.1 mg. The mean and the standard deviation were calculated from measured data. The values
were rounded to three decimal places.

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Fig. 3: A-Model of lap-shear tensile strength testing, B-Sample for tensile strength testing, C-
Schema of equipment for two-body abrasive wear testing
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For the statistical comparison the T-test and ANOVA were used when the zero hypothesis
H0 (p>0.05) states an agreement of the statistical sets of data (α=0.05). The validity of the
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zero hypothesis confirms that the inclusion of fillers did not statistically significantly change
the values of observed parameter compared with the unfilled resin.
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3. Experimental results and discussion

The tab. 2 shows the optical analysis of the particle size after the sieve analysis performed
by means of the electron microscopy (v-variation coefficient). The definition of the particle
size is key for resultant mechanical properties of the composite [26], e.g. Nakamura et al. [27]
clearly describe decreasing strength of polymeric matrices with increasing dimension of used
microparticles. SEM analysis confirmed that microparticles of irregular shapes (DS as well as
DF) had predominated in the experiment which can optimize the mechanical binding between
the resin and the filler according to Chang and Yeih [28].
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Table 2. Filler specification – particle size after sieve analysis

Particles Mean [µm] SD [µm] v [%]
Date Stone (DS) 0-100 µm 48 22 45.8
Date Stone (DS) 100-200 µm 149 42 28.2
Date Flesh (DF) 0-100 µm 61 31 50.8
Date Flesh (DF) 100-200 µm 174 35 20.1

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Chosen technological undemanding process of the material preparation reflects
requirements of developing countries and requirements for quick and simple preparation of
composites. Air pores are created during the application of resins without the use of vacuum.

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These pores then influence the mechanical properties of forming composites. The presence of
pores in applied epoxy resin is analysed by 3D picture from the fluorescence confocal
microscope (Fig. 4). The resin was coloured by a fluorescence powder for highlighting of

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pores. E.g. the vacuum infusion method can be used for the minimization of the porosity and
for good placement of the filler.

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Fig. 4 Confocal microscopy: Porosity of unfilled resin (above), SEM: air bubble influencing

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adhesive characteristic of composite layer MAG 1.70 kx (below)

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Cohesive characteristic – tensile strength
The cohesive strength of the system was evaluated by means of the tensile strength
(see Fig. 5). The unfilled resin reached the tensile strength 50.42 ± 1.80 MPa. A mild increase
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of these values occurred at low concentrations of the fillers in the interval 0-100 µm 0.5% and
1.0%, however, the zero hypothesis H0 was still valid (p>0.06). The fall of the values of up to
35% (DF 10%) occurred at higher concentrations. The hypothesis H0 was valid at DS until the
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concentration 5% (p>0.08), at DF until the concentration 2.5% (p>0.06).

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Fig. 5 Tensile strength of composite with DS, DF particles 0-100 µm (left), tensile strength of
composite with DS, DF particles 100-200 µm (right)

The statistically insignificant increase was found in the particle size interval 100-
200 µm (DS, DF) only at the concentration 0.5% (p>0.51), the statistically significant fall was
observed identically (DS, DF) from 15%, see Fig. 5. This fall reached up 52% at DF. The
results correspond to the conclusions of Hristov et al. [29] who state that good tensile strength
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can be reached at polymers with small portion of organic microparticles - wood powder 15-
50 µm in their case. The results also correspond to conclusions of Nakamura et al. [27] who
state that the fall of the polymer (PP) tensile strength occurs with increasing particle size.
More considerable fall of the values with increasing concentration was observed in case of
this experiment at larger particles. SEM analysis of fracture surfaces at the voltage 5.0 kV is
presented in Fig. 6.

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Fig. 6 Fracture surface Epoxy/DS MAG 2.64 kx (left), Fracture surface Epoxy/DF
MAG 2.64 kx (right)
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Adhesive characteristics – shear tensile strength

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An optimum preparation of the adherent surface leads to required wetting of the

adherent with the resin, so also with the composite system – it leads to the enlargement of an
efficient surface and to the optimization of the bond strength [30-32]. The description of the
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roughness parameters and the optical analysis of the boundary adherent / composite system
belong among key factors utilisable for descriptions of the mutual interaction of phases. The
blasting of steel adherent surfaces can be indicated as one of the most efficient surface
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treatment method [33], see adherent after grit blasting - Fig. 7.

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Fig. 7 SEM: Grit blasted surface of adherent before applying composite system MAG 499 x

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The parameters Ra = 2.02 ± 0.36 µm, Rz = 10.18 ± 1.62 µm were determined by the
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contact roughness instrument. SEM analysis of the interaction of the adherent and the resin
proved good wettability on such treated surface (see Fig. 8).
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Fig. 8 Interaction in boundary adherent /unfilled resin MAG 1.04 kx (left), interaction in
boundary adherent / resin with DF particle MAG 2.42 kx (right)

The lap-shear tensile strength of the treated adherent of the unfilled resin corresponded
to 12.01 ± 0.73 MPa which is in accordance with the value stated by the producer according
to the standard (see Fig. 9). The DF particles from the interval 0-100 µm did not considerably
influence the lap-shear tensile strength in observed interval (p>0.07), the statistically
demonstrable increase of the lap-shear tensile strength (up of 10.8%) was observed at the DS
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particles at the concentrations 2.5% (p=0.03) and 10% (p=0.02). However, it is necessary to
add that the inclusion led to the increase of the variation coefficients (up to 12.3%).

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Fig. 9 Lap-shear tensile strength of composite with DS, DF particles 0-100 µm (left), lap-
shear tensile strength of composite with DS, DF particles 100-200 µm (right)

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The statistically significant change of values (p>0.17) did not occur in the observed
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interval at the particles DS and DF from the interval 100-200 µm. Nevertheless, the lap-shear
tensile strength was increased at the DS filler at the validity of the hypothesis H0, however,
the most of 6.5%. All composite systems were failed by the adhesive type, as well as the
unfilled resin. The width of the cleft was defined only by the composite system itself, no
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distance wires were used. The results confirmed the assumption coming from many studies
[28, 34, 35] that the strength of the solid adherents can be increased by microparticles of tens
of micrometers.
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Smaller values of the observed characteristic at DF can be explained by SEM analysis

of the adhesive bond cuts when the DF particles were not optimally wetted with the resin as it
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is visible from Fig. 10 (right). Smaller wettability of particular phases leads according to
many authors [25, 36] to smaller mechanical characteristics of composite systems.
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Fig. 10 Cut through adhesive bond Epoxy/DS MAG 3.03 kx (left), Cut through adhesive bond
Epoxy/DF MAG 5.51 kx (right)
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Hard particles – date stone increased the hardness Shore D, whereas the hardness was
decreased at softer parts of the flesh, proportionally to the increasing portion of the fillers in
the matrix, see Tab. 3. These conclusions are in accordance with the experiments of Satapathy
and Bijwe [37] who state that the change of the resin hardness is proportional to the amount of
microparticles and it is unfolded from the microparticle hardness itself. The addition of
walnut particles in the biocomposite decreased the ultimate strength both in the compression
and the tension. However, the addition of walnut particles in the biocomposite increased the

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hardness. The hardness of particle systems can be in a certain correlation with the abrasive
wear resistance.

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Table 3. Hardness of biocomposites
wt. %
Hardness ShoreD

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0 0.5 1.0 2.5 5.0 7.5 10.0
DS 0-100 µm 88.9 89.2 89.3 89.2 89.4 90.1 90.1
SD 0.84 0.88 0.60 0.96 1.20 0.80 0.95
DF 0-100 µm 88.9 88.6 88.8 88.6 87.9 86.8 86.3

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SD 0.84 1.05 0.63 0.98 0.74 1.10 1.30
DS 100-200 µm 88.9 89.4 89.2 89.3 89.7 90.1 90.5
SD
DF 100-200 µm
0.84
88.9
1.03
88.9
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1.19
88.1
0.82
87.9
0.59
87.0
1.00
86.4
0.68
85.7
SD 0.84 1.26 1.31 0.97 0.56 1.37 1.11
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The results of the performed experiment proved a validity of the hypotheses and the
conclusions stated by Singh [38] in the experiment describing the epoxy resin and the walnut
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– the addition decreased the ultimate strength in the tension and increased the hardness. Hard
inorganic and organic particles among which the particles prepared from the date stones can
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be ranked increased the wear resistance (in contrast with the particles prepared from the date
flesh), proportionally to increasing portion of DS in the resin (up of 11%, see Tab. 4). This
increase of the abrasive wear resistance by means of hard particles is at good interaction of
the particles and the matrix in accordance with the conclusions of many authors [37-41].
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Similar results were reached also at analogical natural particles prepared from the seeds of the
plant Jatropha Curcas L. [3]. The inclusion of the particles from the date flesh mildly
decreased the abrasive wear resistance, maximum of 11%, see Tab. 4. However, the inclusion
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of DF 100-200 µm increased the mass losses up of 12.8%.

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Table 4. Abrasive wear resistance of biocomposites – mass losses

Mass losses wt. %
[g] 0 0.5 1.0 2.5 5.0 7.5 10.0
DS 0-100 µm 0.377 0.380 0.374 0.374 0.358 0.344 0.322
SD 0.006 0.006 0.002 0.007 0.006 0.004 0.003
DF 0-100 µm 0.377 0.376 0.386 0.397 0.403 0.410 0.409
SD 0.006 0.003 0.006 0.003 0.007 0.008 0.003
DS 100-200 µm 0.377 0.375 0.380 0.368 0.328 0.319 0.320
SD 0.006 0.002 0.006 0.002 0.003 0.006 0.004
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DF 100-200 µm 0.377 0.382 0.380 0.380 0.394 0.425 0.425

SD 0.007 0.006 0.003 0.007 0.007 0.006 0.011

4. Conclusions
Generally it can be said that the interest in the composites filled with bioparticles has been
increasing both in the academic and also private (industrial) area [42-43]. The reason is
according to Danyadi and Renner [42] a low price, a simple availability and a renewability of

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these fillers, but the biological essence of the material can be withal limited in many areas (an
absorbability, different mechanical properties). The date stones (or the stones with remaining
flesh) are of no economic value.

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The paper describes the alternatives to wood-base products which are desirable in the
developing countries above all.
However, the new formed material can be also regarded as the filled adhesive based on

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the performed experiments when the particle inclusion significantly decreases the application
price at keeping very good adhesive properties.
The genus Phoenix of the family Arecaceae includes 13 palms. The results of this

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experiment can open the usage possibilities of the biomass created at the cultivation of these
palms. However, the experiment results can be implemented also on other plants during
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whose utilization the similar-based biomass (stones) comes into being.

The results described by this experiment promise the position in the industrial application
scale, in terms of the economical undemandingness and the environmental friendliness above
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all, and they can be summed up in a following way:
• It was observed that the reinforcement shows a homogeneous distribution.
• The inclusion of the stone particles from the dates in the epoxy resin does not decrease
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the cohesion of the system at the low concentration, it increases the adhesion of the
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steel adherent, the hardness and the abrasive wear resistance.

• The particles from the date flesh were not completely wetted with the epoxy resin
according to SEM analysis. This was showed by smaller adhesive and cohesive
characteristics, however, the flesh presence does not fundamentally influence the
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characteristics of the composite date seed / epoxide.

Acknowledgement
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This paper has been made with the assistance of the grant IGA TF CZU:
2016:31140/1312/3109.
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The research was conducted thanks to the cooperation between the Applied Mechanics Lab of
the Department of Industrial Engineering of the University of Salerno (IT) and the
Department of Material Science and Manufacturing Technology of the Czech University of
Life Sciences Prague (CULS), Faculty of Engineering, Prague, Czech Republic.

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