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Chemistry Africa

, Volume 2, Issue 1, pp 135–142 | Cite as

Use of Tunisian Opuntia ficus-indica Cladodes as a Low Cost Renewable Admixture in Cement Mortar Preparations

  • Chiraz El AziziEmail author
  • Halim Hammi
  • Mohamed Aymen Chaouch
  • Hatem Majdoub
  • Adel Mnif
Original Article
  • 125 Downloads

Abstract

The present study deals with the influence of Opuntia ficus-indica cladodes powder on the durability and the mechanical properties of Portland cement mortar, including setting time and compressive strength. A control specimen with ordinary Portland cement was made and in other specimens, cement was replaced with 1, 2.5 and 4% of Opuntia ficus-indica cladode’s powder by weight of cement. The obtained results showed that setting times decreased notably with the addition of Opuntia ficus-indica cladodes and that there is an enhancement of the mechanical strength and the resistance to acetic and hydrochloric 5% acid solution compared with the standard specimen.

Keywords

Opuntia ficus-indica Portland cement Setting time Compressive strength Durability Mortar 

1 Introduction

Back in the old days, natural organic admixtures were used in mortar and concrete to improve the mechanical strength and sustainability of structure, which in turn showed a better performance. This is one of the main reasons why many old structures still exist [1].

Nowadays, conservation of natural resources and preservation of environment is a necessity of any development. Thus, to address this alarming situation, attention has been focused on the vegetable biomass because of many advantages. The most important is that biomass is low-priced. The production of biomass does not involve the hitting process and the cost of transportation is eliminated as production can takes place on site, thus cost analysis of available biomass offers more savings and could balance the final cost of mortar. Furthermore, it is more readily available since biomass is a renewable material and because very little handling charges are required. Finally, the production process of green admixtures is environmental friendly [2, 3]. After the twentieth century, and with the rapid development of technology and material science, the discovery of renewable materials is considered of great importance.

That’s why natural organic admixtures are massively reintroduced in the formulations of cement mortar. For example, two organic wastes were assessed in the civil engineering areas as an additive to the mortar. Barreca et al. [4] used olive seeds which improved the heat insulation performances of mortar and reduced its final density, whereas Khedari et al. and Manan et al. [5, 6] investigated the use of coconut fiber and coconut shell in lightweight concrete, respectively. Opuntia ficus-indica (OFI) cactus is native to Mexico but also present in the Mediterranean basin, South Africa, Middle-East, India, Thailand and Australia [7]. It grows in semi-arid and arid environments [8].This plant can produce from 20 to 100 t of cladodes/ha per year, in areas having rainfall from 150 to 400 mm/year, without fertilization [9] Generally, cladodes are large and have a high content of water (90%), ash (20% of dry matter) and calcium (1.4% of dry matter), with low amounts of crude fiber (10% of dry matter) and phosphorous (0.2% of dry matter) [10, 11, 12, 13].

Locally available in Tunisia, for about 500,000 ha, OFI large plantations have been cultivated in central and southern regions of the country where it plays a basic role in animal’s diet, in addition to its significant involvement in the reduction of the sand movement and rangeland erosion [14, 15, 16].

In a previous study, Chandra et al. studied the use of cactus in mortars and concrete which improved the workability of mortar and freeze–thaw resistance [1]. Furthermore, Nopal mucilage and marine brown algae extracts were used as viscosity enhancing admixtures for cement based materials [17, 18, 19, 20, 21, 22].

From these advantages, the purpose of this research was to investigate the influence of the partial substitution of Portland cement by OFI cladodes powder on the mechanical strength development, setting time and durability towards the acid environment of the made mortars.

2 Experimental

2.1 Materials

Portland cement (type CEM II 32.5 N) in accordance with the Tunisian standard NT 47-1 and European standard EN 197-1, with a compressive strength of 32 MPa at 28 days, was used for the manufacture of mortars. Fine natural medium sand with a maximum nominal size of 600 µm (about 95% of the particles characterized by a diameter smaller than 550 µm) was taken and measured by a laser particle MICROTRAC S3500.

Cladodes, circular or oval, have a length of 15–40 cm, a width of 28 cm and a thickness of up to 2.5 cm. They are bluish green. Cladodes (6 months) from OFI (spiny cladodes) were collected in the area of Soliman [Nabeul-Tunisia (36°41′44.3″N 10°27′38.2″E)] in March 2016. After manually spines removal, cladodes were washed, cutted, dried at 40 °C for 24 h in oven and then, the material was ground in a ball mill (Retsch R200) at 55 rpm for 30 min. The material obtained was separated, on representative fraction’s size: ≤ 212 and ≤ 600 µm.

2.2 Chemical Composition and Particle Size Distribution

The chemical composition of OFI cladodes powder was estimated using various methods.

Ash content was evaluated under the AOAC standard method 942.05 [23].'The amounts of pectin, hemicellulose and α-cellulose were determined by sequential extraction in distilled water (2 × 2 h at 70 °C), KOH aqueous solution (24%) (24 h at 25 °C) and NaOH aqueous solution (4.3%) (24 h at 25 °C). Hollocellulose content was estimated as described by Marzouk et al. [24].Total lipid content was determined by Soxhlet extraction with. a mixture of dichloromethane:methanol (2:1, v/v) [25].

The determination of the particle size distribution of OFI cladode’s powder was realized by laser equipment MICROTRAC S3500, according to the dispersion of the material in water without a dispersing agent.

2.3 XRD and SEM Analysis

The XRD of the specimen was performed using a Philips PW 3050/60 2θ goniometer and a PW 3373/00 copper cathode, at a scanning speed of 2°/min between 10° and 70° and the XRD results are fitted by the X’pert High score software.

Scanning Electron Microscope (SEM) was also used to investigate the morphology of the modified mortars by FEI (ESEM) apparatus.

2.4 Dosage of Mortars

The mix proportions of the reference mortar were 1:3 (cement CEM II 32.5 N: sand, w/w).

OFI mortars were prepared by adding 0, 1, 2.5 and 4% of Portland cement replacement by OFI cladodes powders. The mortar specimens are prepared according to the European standard EN 196-1 with constant mixing water rates: W/C = 0.5 [26].

2.5 Mortar Specimens

The compressive strengths of the mortars were determined at curing age of 28 days at 20 °C, using 3 samples of (40 × 40 × 160) mm for each composition. The tests were performed in a press EMIIC universal testing DL130000 with a loading speed of 500 N/s.

For the durability tests due to acid attack, cube specimens are immersed in 5% acetic acid solution and then in 5% hydrochloric acid solution. Weight measurements for each mixture are performed weekly up to 6 weeks and the results were compared with the initial weight. Briefly, cubes were cleaned quickly 3 times with running water to remove the altered mortar and then dried for 30 min according to ASTM C 267-96 before each weight measurement. Three mortar specimens were tested for each assay.

The initial and final setting times of the pastes, made with normal consistency (W/C = 0.26) according to EN 196-3 test method (Vicat apparatus), were evaluated [27].

Mix proportions of the mortars were elaborated after a preliminary study. Ei designates a mortar in which OFI was used as Portland cement replacement (from 0%to 4% by weight of binder).The maximum fraction’s sizes of OFI material were 212 µm and 600 µm.

3 Results and Discussion

3.1 Particle Size Distribution, Chemical Composition and XRD Analysis

The used OFI cladodes have bimodal particle size distributions for the two fractions (OFI powder ≤ 212 μm and OFI powder ≤ 600 µm) with two distinct populations. So, for the samples with a size ≤ 212 μm with a mode M distribution the first population has a mode M1 = 40 μm and the second M2 = 150 μm; secondly for the samples with a size ≤ 600 μm with a mode M distribution the first population has a mode M1 = 60 μm and the second M2 = 350 μm (Fig. 1).
Fig. 1

Particle size distribution of OFI cladodes powder: aOFI powder ≤ 212 μm, bOFI powder ≤ 600 µm

The approximate composition of OFI cladodes is displayed in Table 1. From these data; we notice that the main components of OFI cladodes powder were polysaccharides, mainly pectin and lignocellulosic material.
Table 1

Chemical composition of OFI cladodes

Component

Percentage (%)

Water

92.50 ± 1.23

Lipids

0.28 ± 0.03

Ashes

0.70 ± 0.05

Pectins

2.98 ± 0.17

Hemicellulose

1.08 ± 0.09

α-Cellulose

0.49 ± 0.06

In addition, the analysis of OFI cladodes powder by XRD revealed the presence of Calcium Oxalate and cellulose as major phases (Fig. 2), However there is a presence of an amorphous phase showed by the background in form of hump [8, 10].
Fig. 2

XRD analysis of OFI cladodes powder

The effect of partial substitution of Portland cement by OFI material on the mechanical and chemical performance of mortars was studied by a full factorial experimental design 22 with two factors namely the percentage of substituted OFI material and its granulometry.

3.2 Mortar Specimens

The results of the mechanical strength analysis are shown in Table 2, and revealed that mortar with 1 and 2.5% OFI material presented higher average of compressive strength values than the reference (E0) at 28 days. The compressive strength increased approximately to 54 MPa at 28 days for E5 and to 51 MPa for E1 which is a notable increase of the mechanical performances compared to the standard (28 MPa). Nevertheless, the compressive strength of the mortar with 4% of OFI material was lower than that of the reference one. Thus, we can conclude that increasing the OFI material-to-cement ratio in the mortar was found to enhance compressive strength until an amount of 2.5% of substitution.
Table 2

Compressive strength of the reference and OFI made mortars

Samples

Substitution (%)

Granulometry (µm)

Compressive strength (MPa) (± 0.04)

E0

0

28.62

E1

1

≤ 212

51.37

E2

4

≤ 212

18.97

E3

1

≤ 600

42.80

E4

4

≤ 600

11.67

E5

2.5

≤ 212

54.52

E6

2.5

≤ 600

49.05

The possible mechanism generated by the addition OFI cladodes powder could be due to the formation a very complex matrix, thereby prolonging the hydration of Portland cement by sequestering water inside the liquid traps. This was supported by the higher compressive strength values after the addition of OFI material compared to the standard specimen [28].

The effect of the studied factors (OFI substitution percentage of and granulometry) on mechanical strength, exhibited through interaction diagrams (Fig. 3), showed that, for the same substitution percentage, the increase of the granulometry reduces the compressive strength. Therefore, we can conclude that it is better to use approximately the same range of Portland cement size.
Fig. 3

Interaction study of X1 × X2 effects, at 28 days on the response a compression strength (MPa), b initial and final setting time(s), c weight loss (%) of CH3COOH and HCl attack

The setting time of the prepared mortars are shown in Fig. 4, in comparison with the reference mix (E0).The results asserts that the partial replacement of Portland cement by OFI material accelerates the setting time of the mortars. This could be mainly due to the presence of pectin substances which is the water-soluble polymer consisting of 1,4-linked α-1,4 linked d-galacturonic acid with a part of the carboxyl group esterified by a methyl group, and as it has been reported by Zsivanovits G et al. that the Ca2+ ions present in pectin solution helps the formation of three-dimensional gel networks [29], then, it might be suggested that the accelerating behavior of the pectin is due to its impact on C3S hydration. Therefore, the presence of soluble pectin in the cement highly influences the concentrations of Ca2+ ions in the pore solution. The decrease of Ca2+ ions from the solution, due to the formation of pectin network, is followed by a decrease in calcium concentrations. Thereby, this shortfall of enough Ca2+ ions in the pore solution accelerates the freeing of calcium from the C3S into the liquid phase that responds to form initial hydration products [29, 30].
Fig. 4

Initial and final setting times of the prepared mortars

The mechanism of attachment of divalent ions called ‘egg box’ is commonly reported in the literature [31, 32]. Martínez-Molina et al. [19] suggested that some additions helped to make harder the paste and might be an alternative as a curing accelerator.

The results of the mortars resistance to acetic and hydrochloric acid are shown in Fig. 5. The resistance was estimated by the weight loss percentage of the reference (E0) and OFI mortars introduced in 5% acetic acid and 5% hydrochloric acid by the period of immersion. From these data, we notice that, for all mixtures and for both aggressive acids, specimens of OFI mortars presented better performance than the reference one.
Fig. 5

Weight loss percentage of OFI mortars immersed in a acetic acid, b hydrochloric acid

At the final immersion period, the weight loss of OFI mortars was less than that of the control one, which proves the high resistance to acetic and hydrochloric acid solutions.

The improved acid resistance of the OFI containing specimens could be attributed, on one hand, to the important cellulose amount in OFI cladodes powder, and on the other hand, to the presence of calcium. These two components form solid phases sealing the pore network of the mortar, reducing water movement and, therefore, increasing the mortar impermeability and the overall acid resistance of OFI specimens. Similar findings were observed by C G Hernández Carrillo to improve the increase of mortar durability performance with the use of OFI material [13].

3.3 Optimum Characteristics

From the obtained results, excepting 4% OFI mortars, we noticed that the mechanical and chemical properties (compressive strength, durability) of the mortar were improved with OFI material substitution.

Thus, it was estimated that the composition of E1 mortar enhance mechanical performance with a rise of 79.5%, decrease weight loss after weak and strong acid attack, with an apparent accelerating effect (86 min) compared to the reference one. Characterization of the optimum formulation by XRD and SEM was carried out to study the mechanical behavior at 28, 90 and 110 days after mortar cube fabrication.

3.4 Compressive Strength

The plots compressive strengths evolution were generated in order to compare the mechanical performance of E1 mortar to that of E0 mortar, in the period between day 28 and day 110 (Fig. 6). Thus, we observed that the compressive strength of E1 mortar was improved steadily with the time.
Fig. 6

Evolution of compressive strength at different ages of E0 and E1

3.5 X-Rays Diffraction (XRD)

The results of the analysis of E1 mortar by XRD at 28, 90 and 110 days were illustrated in Fig. 7. We note that, whatever the mortar age, the only phases encountered were typical to those of Portland cement mortars. This asserts that no chemical reaction between OFI material and cement hydrated phases has been occurred.
Fig. 7

Comparative DRX of 28, 90 and 110 days cured Cement–OFI 1% pastes; (open square) Portlandite Ca(OH)2, (open diamond) Quartz SiO2, (open circle) Calcite CaCO3 , (open triangle) Alite (C3S) Ca3SiO5, (open star) Ettringite (3CaO·Al2O3·3CaSO4·32H2O)

However, the addition of OFI material to the cementitious matrix generated the enhancement of the kinetics of hydration process. This is reflected on the accelerating-effect of OFI mortar setting times.

Moreover, the usefulness of qualitative analysis from the characteristic diffractograms permitted to depict the conversion of calcium hydroxide, which is easily attacked by acid solution, to C–S–H. This results in the strengthening and densification of the transition zone, which improves its resistance to microcracking and thus increasing the overall mortar resistance to acid [33].

3.6 Scanning Electron Microscope Observations

SEM observations (Fig. 8) revealed the same results shown by the reference mortars which displayed hydrated phases as portlandite large amorphous crystals CSH gel and Ettringite needles. However, the E1 mortar was characterized by a more compact morphology which proved the significant reduction in permeability imparted by the use of OFI, thus the increase in mechanical strength and durability. These results are in accordance with those observed in the XRD spectrum analysis.
Fig. 8

SEM photographs of E0 (a, c, e) and E1 (b, d, f) after 28, 90 and 110 days

4 Conclusion

This paper analyzes the mechanical properties, setting time behavior and durability of cementitious materials after the substitution of Portland cement with 1–4% of Opuntia ficus-indica (OFI) cladode’s powder. The main results showed a noticeable accelerating effect after the addition of OFI material. In addition, OFI-containing mortars were found to be more resistant after acetic and hydrochloric acid solutions (5%) attack than those without OFI.

Thus, the optimal composition of the OFI mortar was E1 since the enhancement of the mechanical strength was about 79.5% and the weight loss was reduced under acetic and hydrochloric acid treatment compared to E0 (without addition of OFI).

According to these findings, it can be concluded that the replacement of a certain amount of Portland cement by OFI cladode’s powders in the mortar could be a promising target to obtain better mechanical and chemical enhancer for cement-based mortars with a lower Portland cement consumption. This can contribute in solving the current environmental problems associated with the CO2 emissions and the rising cost of fossil fuel consumption in the production of cement.

Notes

Compliance with Ethical Standards

Conflict of Interest

On behalf of all authors, the corresponding author states that there is no conflict of interest.

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Copyright information

© The Tunisian Chemical Society and Springer Nature Switzerland AG 2019

Authors and Affiliations

  • Chiraz El Azizi
    • 1
    Email author
  • Halim Hammi
    • 1
  • Mohamed Aymen Chaouch
    • 2
  • Hatem Majdoub
    • 2
  • Adel Mnif
    • 1
  1. 1.Useful Material Valorization Laboratory, National Center for Research in Materials SciencesTechnopole Borj CedriaSolimanTunisia
  2. 2.Laboratoire des Interfaces et des Matériaux Avancés (LIMA), Faculté des Sciences de MonastirUniversité de MonastirMonastirTunisia

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