Textile Dye removal by Adsorption on Olive Grain as Solid Waste from the Olive Oil Extraction

 

Mohamed Bilal Goudjil^1,4*, Nabila Sid⁴, Asma Omar Ayachi^2,4, Souad Zighmi^2,4,
Djamila Hamada^1,4, Zineb Mahcene³, Salah Eddine Bencheikh^1,5, Segni Ladjel^1,4

¹University Ouargla, Faculty. Applied Sciences, Laboratory. Process Engineering, Ouargla 30000, Algeria.

²University Ouargla, Faculty. Applied Sciences, Laboratory. Engineering Laboratory of Water and Environment in Middle Saharian, Ouargla 30000, Algeria.

³University Ouargla, Faculty. Sciences of the nature and life, Laboratory. Protection of Ecosystems in Arid and Semi-Arid Zones, Ouargla, Algeria.

⁴University Ouargla, Faculty. Applied Sciences, Department of Process Engineering, Ouargla 30000, Algeria.

⁵University Ghardaia, Faculty. Science and Technology, Department of Process Engineering, Ghardaia, Algeria.

 

ABSTRACT:

This study is part of the framework for the enhancement of agro-food waste ( olive grains) for the adsorption of a cationic dye by two methods, the first is to use its waste in a natural form (biosorbent) and the second is to the preparation and characterization chemically of an activated carbon from grain by using an activating agent (nitric acid), we studied the influence of several parameters (concentration of methylene blue, mass of olive grains, pH and temperature). The kinetic data was modeled by pseudo first order equations, pseudo-second order and intraparticle diffusion model; The Langmuir-Freundlich model was chosen for the representation of the experimental results. The experimental results are shown that the effect of the mass of adsorbent on the adsorption capacity increased respectively with increasing the mass of adsorbent and dye adsorption is promoted in a room temperature. Modeling results showed that the adsorption of methylene blue on olive grain follows the second order pseudo model for all concentrations in both adsorption and bio-sorption. The study of the isotherm shows that the Langmuir model well describes the process of adsorption of methylene blue on olive grains. All these results show that olive grains could use effectively as a low-cost adsorbent for the removal of cationic dye of an aqueous solution.

 

 

 

INTRODUCTION:

The intensive use of dyes in life has led to many problems both in the environment and in food¹. It is important to mention that in the environment, pollution is due to effluent discharges from the industrial sector by the incorporation of several synthetic dyes.

 

Dyes are used in many industrial sectors such as for textiles, paper, leather and in the food and cosmetic industries. They have a reputation for being toxic and persistent substances in the environment; they need physico-chemical techniques to degrade them.^2-4

 

The treatment of industrial waste containing this type of dye is of great interest. A wide variety of physical, chemical and biological techniques have been developed and tested in the treatment of effluents loaded with dyes. These ways include flocculation, precipitation, ion exchange, membrane–filtration processes (nanofiltration, electrodialysis, reverse osmosis), irradiation and ozonation⁴. However, these procedures are expensive and lead to the generation of large quantities of sludge or the formation of drifts^5,6.

 

Among the methods of treatment of liquid discharges, adsorption remains a relatively used technique and easy to carry out. Activated carbon is the most widely used adsorbent due to its high capacity for adsorbing organic materials.

 

However, this adsorbent has a high cost and remains difficult to regenerate. The search for another effective and less expensive adsorbent therefore proves to be interesting.^2,7

 

In this context, the use of a natural waste as adsorbent has a great interest because of its abundance in large quantities often undervalued.

 

In this context, this study aimed to evaluate the residues generated during the extraction of olive oil (olive grain) in the natural state (bio sorption) and to transform into activated carbon (adsorption) with activation and without chemical activation for the removal of textile dyes (methyl blue) in a simulated solution.

 

MATERIAL AND METHODS:

Preparation of the primary material:

The olive is the fruit of the olive tree, a fruit tree characteristic of the Mediterranean regions. Botanically, it is a drupe, skin smooth, fleshy mesocarp rich in fat, containing a wood core, which contains a seed. Its ovoid shape is typical. The olive waste used in this work is collected in the Ouargla -Algeria region. After collection, the grains obtained are washed and then dried in an oven, for 24 hours at 110°C to prevent possible deterioration of the physico-chemical properties of the material. Olive seeds subjected to grinding and sieving to get homogeneous and small-sized materials characterized by a diameter between 0.08 mm and 0.1 mm (0.08≤d <0.1).

 

Preparation of activated carbon:

Activating agent:  

In this study, nitric acid was used as the Activating Agent, sometimes called azotic acid, is a chemical compound with the crude formula HNO₃ and a molecular weight equal to 63.02 g.mol^-1. In aqueous solution, it has a strong oxidizing power and therefore can react with reducing agents, such as metals, to lead to the formation of species of lower oxidation, provides major nitrogen species a priori present in the nitric acid concentrated or likely to appear during its reduction, in liquid phases⁸.

 

Chemical activation:

After sieving, the olive seeds are washed with distilled water heated to 75°C, the latter drying at 90°C for 2h before being activated.

 

The dried sample (50g) was impregnated for 24 hours with solutions of nitric acid in various concentrations. The impregnation rate (Xp, mmol. g^-1) is defined as the ratio of the mass of NHO₃ (mmol) to the mass of dry olive grains used as precursor (g). The physico-chemical properties of activated carbons prepared with Xp = 0; 1.5; 3; 4.5 (mmol.g-1), were studied. The impregnated samples were washed with heated distilled water, until pH_H2O = 7 ± 0.5 was obtained. They are dried in an oven at 110°C for 24 h. All samples are then carbonized for 1 hour at 600°C with a temperature increase rate of 10°C.min^-1

 

Preparation of dye used (adsorbate-biosorbate):

Methylene blue is an organic compound whose name in systematic nomenclature is 3,7-bis-phenazathionium, soluble in water and more lightly in alcohol. Methylene blue is a nitrogen derivative⁹, it is most commonly used in dyeing cotton, wood and silk. It is in the form of a dark blue crystalline powder. It can cause eye burns responsible for permanent injuries in the eyes of humans and animals. Its inhalation can give rise to breathing difficulties, leading to anemia after prolonged adsorption. A stock solution of methylene blue was prepared at 1 g in 1 liter of distilled water. Test solutions for use in the analysis, were obtained by serial dilutions to desired concentrations in order to establish the calibration curve that has been defined to determine the residual concentrations of the dye as a function of time in the tests of adsorption and biosorption.

 

The residual concentration of the dye is determined using a UV-Visible spectrophotometer at the wavelength 660 nm which corresponds to the maximum absorption of methylene blue.

 

Adsorption Experiments:

All tests are carried out on organic waste in the natural state (bio-sorption) and in the transforming state into activated carbon (adsorption) with activation and without chemical activation. The studies were performed in a batch process by investigating the effect of experimental variables such as pH (2–12), initial MB concentration (5, to 40 mg·L⁻¹), contact time, adsorbent dosage and temperature (10, 25, 40, 50°C). The initial pH of the solution was adjusted with 0.1 M hydrochloric acid (HCl) and sodium hydroxide (NaOH) solution and determined with pH meter. A certain amount of waste of olive grains was added to a 250mL conical flask solution containing 100 mL of solution at certain concentrations of MB. Each mixture was oscillated at 100rpm at 25°C for 210 minutes (measurements are taken every 30 minutes). After the adsorption process, the samples were filtered and analyzed, the absorbance reading is made at 660 nm. All tests were carried out three times.

 

Calculation formulas:

To determine the BM residual concentrations in the liquid phase at the instant (t), we use the following linear equation:

 

Y=0.0352 x +0.0106                                                    (1)

 

The equation is obtained from BM calibration curve, with:

Y: absorbance (A) at time (t)

X: the residual concentration of BM at time (t)

 

- To calculate the amount of BM adsorbed at equilibrium qe (mg/g) We used the following formula¹⁰:

 

q_e = (C₀ – Ce) * V)/W                                                 (2)

 

q_e: is the quantity adsorbed on activated carbon per g of activated carbon (mg/g).

C₀: is the initial concentration of BM in (mg/L)

Ce: concentration of BM in the aqueous phase at equilibrium (mg/L)

V: volume of the solution

W: mass of dry adsorbent (g)

 

BM adsorption kinetics:

To study the adsorption kinetics, we determine the dye fixing capacity (qt) as a function of time. The adsorption equilibrium is practically achieved after a certain time of adsorbent-adsorbate contact. These mathematical models were chosen on the one hand for its simplicity and on the other hand by its application in the field of adsorption of organic compounds on different adsorbents^{11, 12}. BM biosorption-adsorption tests are carried out as a function of contact time in a range of 0 to 210 min. A mixture of 0.25 g of mass of adsorbents of olive grains and of initial concentration of 20 mg/L of BM at a volume of 100 mL, this mixture is then left with magnetic stirring at room temperature and at pH = 7.

 

First order model:

Lagergren proposed a kinetic model of pseudo-first order ^{13, 14} :

 

 

dq_t

––– = K¹ (qₑ - q_t)                                                         (3)

dt

 

qₑ and qt are respectively the quantities of solute adsorbed at equilibrium and at time t and K₁ the first order speed constant (min^-1).

 

The integration of this equation between 0 and t for time and 0 and qt for the quantity adsorbed, leads to the following relation:      

 

ln(q_e - q_t ) = ln(q_e) - K¹t                                              (4)

 

The quantity adsorbed qt at time t is calculated using the relation (2)

 

Pseudo-second order model¹⁵:

This model reflects the existence of a balance between species in solution and adsorbed species, the second-order model follows the equation:

 

dq_t

––– = K₂ (qₑ - q_t)²                                                          (5)

dt

 

who has the solution:

 

     1         1   

––––– = –––––  +  K₂*t                                                 (6)

 qₑ - q_t          qₑ

 

And is written in the following linear form:

t          1             1

– = –––––  +  (–––)*t                                                    (7)

q        qₑ² K₂            q

 

K₂: second order speed constant (mg.g^-1.min^-1).

Note that k₂ and q_e are determined by plotting ( ) as a function of  “t”

 

Intra-particle diffusion model¹⁶:

The equation of this model is given by the following equation:

 

q_e = Kd √ t + C                                                            (8)

 

: is the intra-particle diffusion rate constant.

 

Adsorption isotherm models:

In order to determine the type of BM adsorption isotherm on active carbon, we tried to reproduce the experimental data using the Langmuir and Freundlich isotherm equations¹⁷. The parameters for these adsorption models were calculated by regression using the linear form of the isotherm equations.

 

Langmuir model:

Langmuir's equation is given by the following relation :

        b q_t C_e

q_e = –––––––––––                                                       (9)

        1 + b.C_e

According to Weber's representation:

C_e       1           C_e

– = –––––  +  –––                                                       (10)

q_e        q_t.b        qt

 

With:

Cₑ: concentration at equilibrium (mg/L).

qₑ: quantity adsorbed at equilibrium (mg/g).

qt: maximum amount of adsorption (mg/g).

b: Langmuir constant (L/mg).

 

Freundlich model:

The Freundlich model is given by the following equation:

 

q_e = K_F.C_e^1/n                                                                (11)

 

K_F: is a parameter related essentially to the maximum adsorption capacity.

n : is a parameter related to the energies of interaction coefficient with the recovery rate.

The linearization of this equation gives the following equation:

 

ln q_e = ln K_F + (1/n) ln C_e                                          (12)

 

Calculate the specific surface area:

The estimation of the specific surface of an adsorbent is conventionally based on measurements of the adsorption capacity of this adsorbent for a given solute, the molecule of this solute having to have an acceptable surface. It suffices to determine the value of the adsorption capacity of the monolayer from the adsorption isotherm. The specific surface was determined by the methylene blue adsorption method. After plotting the curves of the isotherms, we concluded the maximum capacity value qm (mg. g^-1) which adsorbed by the activated carbon. The latter (qm) allows the estimation of the surface area of the sample covered by the BM molecule.

The specific surface is calculated from the following equation¹⁸:

 

SBM = (Qm . Na . S) / M                                         (13)

 

With, SBM: specific surface determined using BM as adsorbate (m² g^-1)

Qm: maximum adsorption capacity (mg. g^-1)

S: area occupied by a BM molecule (175 A²)¹⁹.

N_a : number of Avogadro.

M : molecular weight of BM

 

RESULTS AND DISCUSSION:

Effect of initial dye concentration:

The effect of the concentration of dyes on the absorption of BM by olive grains at 25°C is shown in Figure 1. It can be observed that the capacity of the adsorption increases with the increase in time to a constant value, at this stage the amount of BM adsorbed by the adsorbent was in a state of dynamic equilibrium. The results clearly demonstrate that the quantity adsorbed increases with the use of olive grain waste in the form of activated carbon by an impregnation rate of 4.5 (amount of BM adsorbed = 13,42 mg/g) better than the use in pyrolyzed form (without activation q_e = 11,03 mg/g) or in the state natural (q_e= 3,72 mg/g).

 

Fig. 1: Initial concentration effect on BM adsorption

 

We also observe that the increase in the initial concentration leads to an increase in the adsorption of dyes. We notice that the equilibrium is reached after 30 min first for all the initial concentrations of BM, this indicates that the speed of absorption is very fast. Adsorption is rapid during the first minutes of the reaction, this can be interpreted by the fact that at the start of adsorption, the number of active sites available on the surface of the adsorbent are much greater than that of the sites remaining after a while.

 

For high contact time the molecule it needs time to distribute within pores of the adsorbent for the rest of the non-adsorbed amount is interpreted by the saturation of the surface of the adsorbent (all sites adsorption are occupied)^20-22.

 

 

Effect of the quantity of waste:

We note in the figures below (Figure 2) that the increase in mass of the adsorbent has the effect of improving the BM removal rate, increased mass of adsorbent means greater waste surface, therefore, a larger number of possible active sites.

 

But for the amount of adsorption decreases with the addition of adsorbent, this behavior can be explained:

- As long as the amount of added adsorbent in the dye solution is low, the dye cations can easily access the adsorption sites. The addition of adsorbent can increase the number of adsorption sites but the dye cations more difficult to approach these sites due to congestion;

- A large quantity of adsorbent can create particles agglomeration, resulting in a reduction of the total area of adsorption and therefore, a decrease in the amount of adsorbate per unit mass of adsorbent ²³. Same result is watched by KM Faizal et al²⁴.

 

Fig. 2: Effect of the amount of waste used on the adsorption of BM by Olive Grains

 

 

Fig.3: Effect of quantity of adsorbent mass on BM adsorption.

 

We find that the adsorption percentages increase with the increase in the amount of adsorbent. This is attributed to the increase in contact area and the availability of active sites. The adsorption capacity increases respectively with the increase in the impregnation rate and regardless of the initial concentration (Figure 3).

 

pH effect:

The initial pH of colored solutions is an important parameter to control the adsorption process, it has an effect on the amount adsorbed. It can change :

1) the charge of the surface of the adsorbent,

2) the degree of ionization of the adsorbate

3) and the degree of dissociation of the functional groups from the active sites of the adsorbent²⁵.

The results are shown in Figure 4.

 

Fig. 4 : Effect of solution pH on the adsorption of BM by olive grains:

 

Fig.5: Effect of temperature on the adsorption of BM by olive grains.

 

A slight increase in the adsorbed amount of BM is observed when the pH of the solution increases, the results show that the adsorbed amount of BM by olive grains is particularly important for the pH is basic (pH=12). The adsorption can be envisaged by electrostatic interactions between the different charges of active carbon and dyes. The surface of activated carbon is negatively charged and the cationic dye (BM) molecules in solution are positively charged²⁶. These interactions increase when the pH increases because the carbon surface becomes more and more negative when the solution becomes more and more basic²⁷. The same result is observed by Kuang Y, Aljeboree A and their colleagues ^{21, 28}. Furthermore, pH=6 is the perfect value giving maximum adsorption of the MB dye on defatted jojoba, jackfruit skin, wheat straw,  Palm Frond and Palm Leaflets was noticed in previous studies^29-32.

 

Temperature effect:

The results of Figure 5 showed that the temperature factor does not seem to have an influence on the quantity of the dye adsorbed by the olive grains. In this case, the thermodynamic study is useless. Indeed, in this temperature range, the adsorbent structure is not affected and it is the same for the stability of the dye. Therefore, this adsorption process promotes room temperature, so it is an economical process for the treatment of coloring solutions.

 

Modeling of adsorption by the Langmuir and Freundlich models:

In order to determine the type of BM adsorption isotherm on active carbon, we tried to reproduce the experimental data using the Langmuir and Freundlich isotherm equations. The parameters for these adsorption models were calculated by regression using the linear form of the isotherm equations.

 

The results of the Langmuir and Freundlich models equational parameters are collated in Table 1.

 

Table. 1: Results of the parameters of the Langmuir and Freundlich models

 

The monolayer scope of the adsorbate on the adsorbent surface at steady temperature is spoken to by the Langmuir isotherm. The Langmuir isotherm insights towards surface homogeneity while the Freundlich show portrays the adsorption inside a confined extend as it were. It is able of depicting the adsorption of natural and inorganic compounds on a wide assortment of adsorbents ³³.

 

The results provided show that:

- The correlation coefficients obtained according to the Freundlich model between (0.4 and 0.87) which concludes that this model does not adequately describe the experimental results of the BM adsorption isotherm.

- For the Langmuir model, the coefficients obtained between (0.91-0.98). It seems that this model adequately describes the experimental results of the BM adsorption isotherm.

 

BM adsorption kinetics:

BM adsorption tests are performed as a function of contact time in a range of 0 to 210 min. A mixture of 0.25 g of adsorbent mass (CAD-1.5 - OAC-4.5 - CAD -0, natural state)) and initial concentration of 20 mg /L at a volume of 100 mL, the mixture was then allowed under magnetic stirring at room temperature and at pH = 7.

Pseudo first order model:

 

Fig. 6 :  kinetic model representation of the pseudo first order.

 

Fig.7:  kinetic model representation of Pseudo second order.

 

According to the results, the first order pseudo coefficients between (0.14 - 0.31) and the second order pseudo coefficients between (0.99-1) which shows that the adsorption kinetics are perfectly described by the model second order pseudo kinetics for the adsorbent studied. Similar results were also found in earlier literature^{34, 35}.

 

Specific surface of activated carbon:

All the results of the surfaces obtained are given in Table 2. We can deduct from this table two essential observations: the specific surfaces obtained by chemical activation are relatively higher than those obtained by the use of waste in its natural state (bio-sorption) or without chemical activation. As regards the chemical activation, the surface area increases with the weight ratio HNO₃ / carbon. The best specific surface (429.3 m².g^-1) is obtained for chemical activation with an impregnation rate equal to 4.5%.

 

Table 2: Calculation results for specific surface area of activated carbon

 

CONCLUSION:

This study's main objective was to demonstrate the value of using a natural substance like system (bio-sorbent / biosorbat) and (adsorbent / adsorbate) to discolor industrial wastewater containing a cationic dye; methylene blue. The results obtained are shown that the effect of the mass of adsorbent on the adsorption capacity increases respectively with the increase in the mass of adsorbent. Also, a chemical modification of the waste improves the adsorbent properties of the solid and the adsorption capacity. The study of the pH effect shows that the adsorption capacity is better in both basic /neutral media, than in acidic medium and that the adsorption of methylene blue is favored at room temperature. The modeling results showed that the adsorption of methylene blue on the olive grain follows the pseudo-second order model for all concentrations with a correlation factor R = (0.99 - 1), both of adsorption and bio-sorption. The study of the isotherm indicates that the Langmuir model describes well the adsorption process of the methylene blue in olive grains. All these results show that olive grains could be effectively used as adsorbent at low cost to remove the cationic dye from an aqueous solution.

 

CONFLICT OF INTEREST:

The authors declare no conflict of interest.

 

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Received on 10.07.2020                    Modified on 03.08.2020

Accepted on 30.08.2020                   ©AJRC All right reserved