A natural dye in water-based drilling fluids: Swelling inhibitive characteristic and side effects

Petroleum xxx (2016) 1e12

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Original Article

A natural dye in water-based drilling fluids: Swelling inhibitive characteristic and side effects Aghil Moslemizadeh a, *, Seyed Reza Shadizadeh b a b

Department of Petroleum Engineering, Ahwaz Faculty of Petroleum Engineering, Petroleum University of Technology, P. O. Box 63134, Ahwaz, Iran Department of Petroleum Engineering, Abadan Faculty of Petroleum Engineering, Petroleum University of Technology, Abadan, Iran

a r t i c l e i n f o

a b s t r a c t

Article history: Received 30 June 2016 Received in revised form 22 August 2016 Accepted 23 August 2016

The development of eco-friendly shale inhibitors is still an area which has attracted a lot of attention in the drilling industry. Henna extract is a natural dye which has recently shown considerable inhibition and weak deflocculation properties in clay-water system. This study aims to investigate swelling inhibitive feature and side effects of Henna extract in water-based drilling fluids (WBDFs). It was carried out through extensive experiments including adsorption measurements on shale by batch equilibrium, inhibition evaluation by dynamic linear swelling and cuttings dispersion, wettability alteration via contact angle measurements, compatibility by rheological properties determinations and fluid loss measurements, and lubricity. Both in natural pH and adjusted pH to 9, Linear adsorption model was more suitable for anticipating the adsorption behavior of Henna extract on the given shale sample. The results of the linear swelling and cuttings dispersion tests demonstrated that Henna extract in drilling fluid formulations diminished the swelling and dispersion characteristics of the addressed shale sample. Moreover, contact angle measurements showed that Henna extract expanded the hydrophobicity of shale formations, preventing and promoting water adsorption and shale stability respectively. This issue definitely introduces wettability alteration as a mechanism for shale stability by Henna extract. Compatibility determinations additionally uncovered that Henna extract is compatible with common WBDFs additives. As indicated by the lubricity tests, Henna extract enhanced the lubricity of WBDFs, a finding which can be of an incredible significance in directional drilling. Among others, advantages such as environmental friendliness, low cost, accessibility, and the counter corrosion property make the applicability of Henna extract in WBDFs profoundly suitable. Copyright © 2016, Southwest Petroleum University. Production and hosting by Elsevier B.V. on behalf of KeAi Communications Co., Ltd. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

Keywords: Shale inhibitors Natural dye Water-based drilling fluids (WBDFs) Adsorption Wettability Compatibility Lubricity

1. Introduction The first and perhaps the most costly step in oil and gas wells development is drilling the wellbore. This step has always been encountered with the problems of wellbore stability. These problems which could result in a waste of US$ 1 billion per year

* Corresponding author. E-mail address: [email protected] (A. Moslemizadeh). Peer review under responsibility of Southwest Petroleum University.

Production and Hosting by Elsevier on behalf of KeAi

worldwide are both mechanical and physico-chemical [1,2]. Mechanical effects are potentially connected to drilling operation and could be handled by restoring the stress-strength balance and trajectory control [3]. Nevertheless, physico-chemical effects which are time dependent come from interaction between solid (i.e shale) and aqueous filtration of drilling fluids [1e3]. Shales are common sedimentary rocks with laminated layered characteristics and high clay content [4]. They account for about 75% of drilled formations and causing 90% of wellbore stability problems [5]. When drilling through water sensitive shales using conventional water-based drilling fluids (WBDFs), shales absorb water and find high potential to hydrate and swell. This results in a lot of operational problems which in some cases leads to suspension of the well prior to reaching the target [6]. The swelling characteristic of shales strongly relies on the amount and types

http://dx.doi.org/10.1016/j.petlm.2016.08.007 2405-6561/Copyright © 2016, Southwest Petroleum University. Production and hosting by Elsevier B.V. on behalf of KeAi Communications Co., Ltd. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

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of clay minerals present [7]. In contrast to other clay minerals, sodium saturated smectites have attained increasing attention owing to high hydration and swelling capacity as well as occurrence frequencies during drilling operations [8]. Inhibition of shale swelling was already achieved by use of oil-based drilling fluids (OBDFs). However, the high cost and environmental damage limited their wide use [9]. Since, a number of efforts have been made to improve the inhibitive properties of WBDFs through introducing typical additives known as “shale inhibitors”. The literature reports the use of potassium chloride as an inorganic salt, partially hydrolyzed polyacrylamide (PHPA), silicates, polyoxyalkyleneamine, poly(oxypropylene)diamine, polyether diamine, poly (oxypropylene)amidoamine, dopamine, bis (hexamethylene) triamine, hydrophobized hyperbranched polyglycerols, amine-terminated polyamidoamine dendrimers, 4.40 methylenebis-cyclohexanamine, and bio-based/chemical-based surfactants [10e25]. It is noteworthy that the inhibitive property of most of these inhibitors is assessed in the absence of WBDF additives, water-clay-inhibitor. Our belief is that this is not adequate for applicability of every product in WBDFs because one product may provides good inhibition performance while disturbs the performance of other additives or its performance becomes weak in presence of special additives. Therefore, a real study needs to be made in order to assess and identify the inhibition performance and side effects of every new inhibitor, respectively. With increasing environmental restrictions, natural surfactants have attracted too much attention within the petroleum industry [26e31]. Henna extract, a natural dye, is a bio-based additive which recently showed deflocculation and inhibition features at low and high concentrations, respectively [15]. This has been achieved through a number of experiments carried out on clay-water-Henna extract system. However, the inhibitive feature of Henna extract and its side effects in form of WBDFs have not yet been reported in the literature. Since, this study is complementary and somehow terminative to previous study in connection with inhibition property of Henna extract. To this end, a wide range of experiments were carried out: adsorption onto shale cuttings via batch equilibrium, inhibition by linear swelling and shale cuttings dispersion, wettability alteration via contact angle measurements, compatibility by rheological properties determinations and fluid loss measurements, and lubricity. 2. Materials and methods 2.1. Materials 2.1.1. Henna extract Henna, Lowsonia inermis L, is an odoriferous plant and a member of Lythraceae family. It is a shrub or small tree with 2e6 m in high and spine-tipped branchlets. Its leaves are characterized as smooth, opposite, sub-sessile, elliptically shaped and broadly lanceolate, with depressed veins clearly visible on the dorsal surface [32,33]. Henna is commonly found in Algebria, India, Pakistan, Egypt, Yemen, Iran, and Afghanistan. In addition to tattooing applications, it can also be employed for different purposes comprising treatment, dye, drug, etc [33,34]. Some features including being a naturally occurring material and thus environmentally friendly characteristics, low cost, high availability, acting as anti-corrosion in various metallic mediums, improving cement resistance against acid attack, and deflocculation as well as swelling inhibition of clay particles are the major reasons for more attention towards Henna in petroleum industry [15,35e41]. For purpose of this study, Henna extract which is

derived from Henna leaves was provided by Ebnemasouyeh Company, Tehran, Iran. Ostovari et al. [34] showed that the main constituents of Henna extract are Lawsone (2-hydroxy-1,4 naphthoquinone, C10H6O3), gallic acid (3,4,5- trihydroxybenzoic acid, C7H6O5), dextrose (aD-Glucose, C6H12O6), and tannic acid (Fig. 1). Table 1 shows the major properties of Henna extract. 2.1.2. Water-based drilling fluid additives In order to prepare WBDFs, different additives were used: green starch, low viscosity polyanionic cellulose (PAC-LV), xanthan gum (XC-Polymer), partially hydrolyzed polyacrylamide (PHPA), potassium chloride (Merck, 99.5%), sodium chloride (Merck, 99.5%), barite, caustic soda, and clouding glycol. These additives were provided by National Iranian Drilling Company. 2.1.3. Shales Two shale samples named Pabdeh and Kazhdumi were used in this study (Table 2). Kazhdumi shale was extracted from the outcrop of Kazhdumi formation, Khuzestan, southern Iran. To do this, a large shale sample was extracted and preserved well. Several core plugs were obtained from the large shale sample and subsequently stored in oil tank for preventing any interaction. Another shale sample was taken from the drill cuttings during drilling through Pabdeh formation in Ahwaz oil field, Khuzestan, southern Iran. The cuttings were air dried at 105  C and then utilized in different parts of this study. Kazhdumi shale was utilized in contact angle measurements due to required core sample for this test, while Pabdeh one was implemented for other experiments owing to its high swelling potential than Kazhdumi shale. X-ray diffraction (XRD) analysis was implemented to characterize the semi-quantitative mineral compositions of shale samples. In this analysis, the detector moved in a circle pattern around the sample and recorded the number of X-Rays (intensity which was recorded as counts per second or CPS) observed at each detector position (2-theta which was recorded as degree). Fig. 2 shows XRD patters, intensity versus 2-theta, for Pabdeh and Kazhdumi shales. After comparing these patterns with the standard patterns, the semi-quantitative mineral compositions of each shale sample were determined as shown in Table 3. 2.2. Methods 2.2.1. Adsorption measurements In this study, batch equilibrium experiments were implemented to acquire the adsorption isotherms of Henna extract on shale cuttings. In this connection, different concentrations of Henna extract aqueous solution were prepared both in natural pH and adjusted pH of 9. The conductivity of each concentration was measured by Sartorius PP-20 conductivity meter in order to acquire reference conductivity curve. Thereafter, 100 ml of each concentration was mixed with 20 g dried (at 105  C) shale cuttings with sieve mesh N.200 (particle size less than 75 microns). The dispersion was stirred by magnetic stirrer for 24 h to reach equilibrium and then a certain amount of them was centrifuged at 6000 rpm for 2 h. Finally, the conductivity of supernatant solution was measured and the left out concentration was obtained using reference conductivity curve. This phase of study was carried out at 28  C and atmospheric pressure. The amount of Henna extract adsorbed per unit mass of shale was determined by the following equation.

q¼

1000  VSol  mshale



c c


(1)

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Fig. 1. Representative chromatogram and corresponding mass spectra of Henna extract. Peaks: 1, lawsone; 2, gallic acid; 3, dextrose; x, unknown [40].

Table 1 Properties of Henna extract [15]. Product

Dry extract of Lawsonia inermis (Henna)

Used part Color Odor Solubility in water Solubility in alcohol pH (30 g/L) LOD (105  C/6 h) Total ash (550  C/4 h) Description Application

Leaves Brown Specific odor Soluble Soluble 4.6e5 5% 14.36% Fine powder Hair dye, body paint, tattoo dye, special shampoo, anti-corrosion

Table 2 Shale samples specifications. Formation Well N.

Oilfield

Depth State (m)

Pabdeh 488 Ahwaz 3344 Kazhdumi Outcrop Outcrop 2

Description CEC (meq/100 g)

Khuzestan Cutting Khuzestan Core

19 10

where q is Henna extract adsorption on shale cuttings, mg/g shale; VSol, the volume of Henna extract solution, L; c , the Henna extract concentration in initial solution before equilibrium with shale cuttings, g/L; c, the Henna extract concentration in aqueous solution after equilibrium with shale cuttings, g/L; and mshale, is the total mass of shale cuttings, g. The uncertainty via this approach was less than 4% for all the measurements. A step by step procedure of adsorption measurements is presented in Fig. 3. In the current study, four celebrated adsorption isotherm models were employed to foresee the equilibrium Henna extract

adsorption at solideliquid interface. The brief description and mathematical equations of these adsorption models are given below. 2.2.1.1. Langmuir model. Langmuir isotherm model presumes monolayer adsorption. According to this model there is no cooperation between the adsorbate's molecules. Langmuir isotherm describes a kind of adsorption process in which the adsorbate's molecules can only attract at a fixed number of sites [41]. Equation (2) presents the mathematical expression of this isotherm model [42]:

qe ¼

Kad qo Ce 1 þ Kad Ce

(2)

where, qe is the equilibrium adsorption at solideliquid interface, mg/g-shale; Ce is the equilibrium concentration in the solution, mg/L; Kad represents the energy of adsorption, L/mg; and qo is the adsorption capacity, mg/g-shale. In order to find Kad and qo, it is enough to plot 1/qe versus 1/Ce in Cartesian scale, leading to a linear curve with the slope of 1/q0Kadd and the y-intercept of 1/q0. 2.2.1.2. Freunlich isotherm model. Freunlich isotherm model is an empirical equation which describes non-ideal and reversible adsorption meaning that adsorption is not limited to monolayer [41,43]. This model states that the ratio of solute onto a certain mass of adsorbent to the solute dosage in the aqueous phase changes at various solution dosages [44]. According to this model, there is no saturation point for adsorbent, representing a limitless surface coverage or multilayer sorption on the surface [43,45]. The Freunlich isotherm model is denoted with [43]: 1=n

qe ¼ KF Ce

(3)

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Fig. 2. XRD patterns of shale samples: a) Pabdeh; b) Kazhdumi.

Table 3 The semi-quantitative mineral compositions of shale samples determined by XRD analysis. Minerals

Kazhdumi (mass%)

Pabdeh (mass%)

Montmorillonite Illite Kaolinite Quartz Calcite Dolomite Gypsum Anatase Hematite

10 2 11 17 49 6 5 0 0

14 4 19 14 36.5 0 8 0.5 4

qe ¼ B ln AT þ B ln Ce

(5)

where AT is Tamkin isotherm equilibrium binding constant, L/ mg; and B is a constant related to the heat of sorption. A plot of equilibrium adsorption (qe) versus lnCe leads to a straight line which can be easily used to extract the magnitudes of B and AT.

where KF is the Freunlich constant related to the capacity of adsorption and n is the Freunlich exponent related to the adsorption intensity. 2.2.1.3. Linear isotherm model. Among all the adsorption models, this model is the simplest one which is based on the Henry equation as follows [45,46]:

qe ¼ KH Ce

layer. The adsorption is demonstrated by uniform distribution of binding energies, up to some maximum binding energy. Equation (5) indicates the mathematical equation of Temkin model [45e49].

(4)

In Equation (5), KH represents a constant for the linear isotherm model in units of L/m2. 2.2.1.4. Temkin isotherm model. This isotherm model has a factor that explicitly takes into the account adsorbenteadsorbate. According to the work of different experimental researchers, Tamkin concluded that there is a linear opposite trend between the coverage and the heat of adsorption of all molecules in the

2.2.2. Dynamic linear swelling tests The effect of Henna extract on inhibiting shale swelling was assessed by OFIT dynamic linear swellmeter. Initially, several pills were prepared by compressing 10 g of shale cuttings (between sieve mesh N.100 and N.200) under a pressure of 41 MPa for 30 min using hydraulic compactor. The pills were then placed in linear swelling cup assembly (LSCA) located between the stirring hot plate and linear variable differential transducer. It should be also noted that the fluid is in dynamic condition via a magnetic bar located at the bottom of LSCA. Continuing, the prepared drilling fluids were poured in the LSCA. Finally, the linear swelling data were recorded as a function of time at 82  C and under atmospheric pressure condition. To investigate the inhibitive performance of Henna extract in conjunction with WBDFs, three stages were carried out. First, a very simple WBDF (Table 4, test fluid N.1) was incorporated with two concentrations of Henna extract (10 g/L and 30 g/L). At the second stage, three different WBDFs (Table 4, test fluid N.2 to N.4) were incorporated with 30 g/L Henna extract. Finally, the inhibitive performance of Henna extract aqueous solution (30 g/L) was

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Fig. 3. Box chart of adsorption measurements via the batch equilibrium experiments.

Table 4 Designed WBDFs compositions. Test fluid N.

Compositions

1# 2#

25 g/L Starch þ 7.5 g/L PAC-LV þ 3 g/L XC 55 g/L KCL þ 110 g/L NaCL þ 25 g/L Starch þ 7.5 g/L PACLV þ 3 g/L XC þ 2.5 g/L PHPA þ 30 vol% glycol 55 g/L KCL þ 110 g/L NaCL þ 25 g/L Starch þ 7.5 g/L PACLV þ 3 g/L XC þ 2.5 g/L PHPA 55 g/L KCL þ 30 g/L Starch þ 7.5 g/L PAC-LV þ 6 g/L XC þ 500 g/L barite

3# 4#

compared to the distilled water and 30 g/L potassium chloride and polyamine aqueous solutions as two most commonly shale inhibitors. 2.2.3. Cuttings dispersion tests It is generally accepted that fluid with good inhibition potential must keep the size of shale cuttings when they are going up along the wellbore annulus. This can be simulated using cuttings dispersion tests very well [50]. For doing this test, shale cuttings were sieved using sieve mesh N.5 and N.10. The cuttings between these two mesh sizes were used in this test so that 20 g of them were added to 350 ml test fluid. Then, the fluid samples were rolled under high temperature condition (105  C) for 16 h. Continuing, the left out cuttings were recovered using mesh size N.10 and washed up with potassium chloride aqueous solution. The recovered cuttings were dried at 105  C. Finally, percentage of recovered cuttings was acquired for different test fluids by comparing the weight of them before and after hot rolling. All test fluids were adjusted to pH of about 9. The test fluids were distilled water, 30 g/L Henna extract, 30 g/L potassium chloride, 30 g/L polyamine, and test fluids N.2

to N.4 (Table 4) and their incorporation with 30 g/L Henna extract. 2.2.4. Contact angles measurements Wettability alteration can be considered as a good strategy for shale stability. In this study, the influence of Henna extract on shale wettability alteration was investigated by static contact angle measurements. Airewater contact angles were measured using Attension Theta Optical Tensiometer equipped with a video camera, four syringe steel needles, an adjustable environmental measuring chamber, and a LED light source. The steps taken to conduct the test were as follows: a) preparing the small shale disks with the smooth surface, b) immersing the shale disks in the test fluids for 24 h, c) extracting and drying the shale disks at room condition, d) placing the shale disks in environmental chamber of Theta apparatus and deposing the water droplets on their surfaces surrounded by air, e) saving the images of free droplets in computer, f) analyzing the saved images using the sessile drop method (fitting of Young-Laplace equation to the drop shape). This test was conducted at 28  C and at the atmospheric pressure condition. It is noteworthy that there were some off-trend samples which examined several times. This method has a measurement uncertainty below 5%. The test fluids for this phase of study were: a) pure Henna extract aqueous solutions both in natural pH and adjusted pH to 9; b) test fluid No.2 to No.4 and their incorporation with 30 g/L Henna extract. 2.2.5. Compatibility tests In addition to performance, the second factor which is vital for applicability of every additive in drilling fluids is its compatibility with other additive. Therefore, this test was carried out to investigate the compatibility between Henna extract and

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common WBDF additives. This phase of study was carried out by incorporating test fluid N.2 to N.4 (Table 4) with 30 g/L Henna extract, aging the fluid samples for 4 h at 105  C in the rolling oven, and finally measuring the alteration in their dial readings and filtrate loss before and after incorporating the Henna extract. Before hot rolling, all test fluids were adjusted to about pH 9. The properties comprising apparent viscosity, plastic viscosity, and yield point were calculated from 600 to 300 rpm dial readings using the following formula [51].

Apparent vis cos ity ðAVÞ ¼

4600 ðcpÞ 2

(6)

Plastic vis cos ity ðPVÞ ¼ 4600  4300 ðcpÞ

(7)

Yield point ðYPÞ ¼ 4300  AV ðpaÞ

(8)

The amount of 10 min gel strength was obtained by operating viscometer at 600 rpm for 10 s, shutting off it for 10 min, and finally recording the maximum dial reading after starting rotation at 3 rpm. The acquired gel strength is in pound per 100 square feet which was expressed in Pascal in order to the sake of the consistency. The filter loss of the test fluids was measured in milliliters under a pressure of 0.7 Mpa through a special filter paper (i.e., baroid filter paper) for 30 min. 2.2.6. Lubricity tests The effect of Henna extract on lubricity of WBDFs was investigated using EP/Lubricity tester (Fann Instrument Company, USA). This test was carried out by incorporating test fluid N.2 to 4 with 30 g/L Henna extract and measuring the change in torque reading parameter (TRP) before and after the incorporation of Henna extract. 3. Results and discussion 3.1. Adsorption measurements Conductivity against concentration is presented in Fig. 4 for Henna extract aqueous solution both in natural pH and adjusted pH of 9. When Henna extract comes into contact with distilled water, hydrogen atoms will be dissociated from the chemical structure of Henna extract constituents leading to an inflection in the conductivity curves close to 15 g/L [15]. The amount of Henna extract adsorbed per unit mass of shale cuttings both in natural pH and adjusted pH of 9 are presented in Fig. 5. The adsorption of

Fig. 5. Adsorption isotherms of Henna extract on shale cuttings both in natural pH and adjusted pH of 9.

Henna extract onto the shale cuttings is enhanced with increasing Henna extract concentration. Over the range of initial Henna extract concentrations (varying from 1 g/L to 50 g/L), the amount of adsorbed Henna extract onto the shale cuttings increased from 4.39 mg/g to 58.69 mg/g and from 4.07 mg/g to 51.74 mg/g for natural pH and adjusted pH of 9, respectively. Both in natural pH and adjusted pH of 9, the slope of adsorption curve above 30 g/L is lower than below it indicating sufficient Henna extract available to cover all the adsorption sites. It should also be noted that lower affinity of Henna extract in adjusted pH of 9 is due to the effect of caustic soda added as a pH adjustment agent, which adversely affects the adsorption of Henna extract on surface of shale cuttings. As mentioned earlier in the context, four celebrated adsorption models which include Linear, Freundlich, Langmuir, and Temkin were implemented to reveal the adsorption behavior of Henna extract on surface of shale cuttings. To this end, the experimental data (qe versus Ce) were plotted according to Linear, Freundlich, Langmuir, and Temkin models. All the computed parameters are given in Table 5. The constants for each model were then employed to foresee the amount of Henna extract adsorbed on shale cuttings. Figs. 6 and 7 show the experimental data compared to the predicted values by the isotherm models for natural pH and adjusted pH of 9, respectively. Based on the values of regression coefficient (R2) and average absolute percentage relative error (AAPRE), equilibrium adsorption behavior of Henna extract on shale cuttings hardly obeys the Freundlich, Langmuir, and Temkin adsorption models. Therefore, the Linear model is more suitable for predicting this adsorption behavior (natural pH: R2 ¼ 0.9185, AAPRE ¼ 30.2214%; adjusted pH to 9: R2 ¼ 0.9586, AAPRE ¼ 17.6957). The Linear model predicted that the adsorption of Henna extract increased linearly with increasing Henna extract concentration. 3.2. Dynamic linear swelling tests

Fig. 4. Conductivity versus Henna extract concentrations both in natural pH and adjusted pH of 9.

Linear swelling data of shale cuttings exposed to test fluid N.1 and its incorporation with 10 g/L and 30 g/L Henna extract are shown in Fig. 7. The percentage of shale swelling decreased with increasing in Henna extract concentrations. Compared to base fluid (test fluid N.1), the ultimate swelling percentage decreased by factors of 1.98% and 5% after incorporating with 10 g/L and 30 g/L Henna extract, respectively. Fig. 8(aec) shows the swelling data of shale cuttings exposed to test fluid N.2 to N.4 as well as their incorporation with 30 g/L

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Table 5 Parameters of adsorption models employed in this study. Isotherm models

Correlations

AAPRE %

R2

Parameters

Langmuirnatural

0:02606ðCe Þ qe ¼ 1þ0:0011ðC eÞ

31.9980

0.7834

Kad 0.0011

q0 23.696

44.0057

0.6682

31.9980 44.0057

0.8792 0.7882

0.0026 KF 0.1547 0.3372 KH 0.0017 0.0014 AT 0.0025 0.0036

17.9212 n 1.7863 2.2286 c 6.6065 2.6802 B 11.4240 8.0863

LangmuirpH

pH

¼ 9

natural pH

Freunlich FreunlichpH

¼ 9

0:0465ðCe Þ qe ¼ 1þ0:0026ðC eÞ 0:5598

qe ¼ 0:1547ðCe Þ

0:4487

qe ¼ 0:3372ðCe Þ

Linearnatural pH Linear pH ¼ 9

qe ¼ 0:0017 Ce þ 6:6065qe ¼ 0:0014 Ce þ 2:6802

30.2214 17.6957

0.9185 0.9586

Temkinnatural pH TemkinpH ¼ 9

qe ¼ 11:424 LnðCe Þ  68:374qe ¼ 8:0863 LnðCe Þ  45:434

103.1820 103.0370

0.7170 0.5968

Fig. 7. Dynamic linear swelling test results for shale cuttings exposed to test fluid N.1 incorporated with different concentrations of Henna extract at 82  C and atmospheric pressure.

to potassium chloride and polyamine. In contrast to distilled water, the ultimate swelling of shale cuttings decreased by factors of 5.16%, 6.17%, and 6.98% after incorporating with potassium chloride, polyamine, and Henna extract aqueous solution, respectively. The aforementioned results indicated that Henna extract could strongly reduced the hydration and subsequently the swelling potential of shale cuttings both in the presence and absence of common WBDF additives. In addition, Henna extract had a comparable performance compared to potassium chloride and polyamine under the considered experimental condition. 3.3. Cuttings dispersion tests Fig. 6. Adsorption equilibrium data based on Linear, Freundlich, Langmuir, and Temkin adsorption models for natural pH (a) and adjusted pH to 9 (b).

Henna extract, respectively. The ultimate swelling percentage of shale cuttings exposed to test fluid N.2, N.3, and N.4 reduced by factors of 4.19%, 2.8%, and 2.2% after modification by Henna extract, respectively. Two swelling curves in each graph are dissociated from the primary time of test, indicating the inhibitive property of Henna extract as an excellent shale inhibitor. The swelling data of shale cuttings exposed to distilled water and 30 g/L potassium chloride, polyamine, and Henna extract aqueous solutions are shown in Fig. 9. All the swelling curves emerged with an analogous trend so that they increased sharply within the first few hours. Shale cuttings in distilled water had continuous swelling until about 5 h and then came out with a constant trend. The inhibition vigor of other three samples is almost the same, but there is a little difference between them. In other words, Henna extract had a better performance compared

Further investigation on the inhibitive feature of Henna extract was made via cuttings dispersion tests (Fig. 10). The shale cuttings recovery for test fluid N.2, N.3, and N.4 increased by factors of 11.8%, 9.02%, and 11.26% after modification by 30 g/L Henna extract. Moreover, the recovery rate in distilled water was 31.13%, indicating high tendency to hydrate and disperse. However, it was observed to have a sharp increase after modification by 30 g/L Henna extract (51.35%). Therefore, it can be concluded that Henna extract had a comparable performance in comparison with potassium chloride (51.59%) and polyamine (53.93%). The test outcome shows that Henna extract has a superior inhibitive property which can strongly affect long-term interaction between the shale cuttings and aqueous phase of drilling fluids. 3.4. Contact angle measurements The physico-chemical aspect of shale instability is directly connected to the shale-drilling fluid interaction. Since,

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Fig. 9. Dynamic linear swelling test results for shale cuttings exposed to distilled water and potassium chloride, polyamine, and Henna extract aqueous solutions of 30 g/L at 82  C and atmospheric pressure.

Fig. 10. Shale cutting recovery rate with different test fluids.

Fig. 8. Dynamic linear swelling test results for shale cuttings exposed to: (a) test fluid N.2 incorporated with 30 g/L Henna extract; (b): test fluid N.3 incorporated with 30 g/L Henna extract; (c) test fluid N.4 incorporated with 30 g/L Henna extract at 82  C and atmospheric pressure.

wettability alteration from hydrophilic to hydrophobic can be considered as a good approach to attain shale stability. In the case of Henna extract, the motivation behind this issue was the decrease in hydrophilic properties of sandstone [52,53]. To assess the influence of Henna extract on hydrophilic property of shale formations, airewater contact angles for shale disks exposed to different test fluids were determined by fitting the YoungLaplace equation to the drop shape. Airewater contact angles for shale disks exposed to various concentrations of Henna extract aqueous solution are shown in Fig. 11. It was 31.86 and 31.82 for distilled water at natural pH and adjusted pH of 9, respectively. The wettability of shale disks was more influenced by Henna extract in natural pH than adjusted pH of 9 as the maximum alteration of airewater contact angle was 13.1 and 11.82 for these two states, respectively. This is probably due to the negative impact of caustic soda which is trying to limit the adsorption of Henna extract on absorbent. The potential of Henna extract to change the wettability of shale was also investigated in the form of drilling fluid formulations (Fig. 12). After modification by Henna extract, the contact angles of shale

disks exposed to test fluid N.2 to N.4 rose by factor of about 7.63%, 10.32, and 16.5%, respectively. The test outcome indicated that the hydrophilic property of shale is reduced by adsorbed Henna extract, leading to less water adsorption and subsequently shale stability. 3.5. Compatibility tests One of the main factors for applicability of shale inhibitors in WBDFs is their compatibility with other additives which could be found out by observation of enormous alteration in rheological properties as well as fluid loss before and after addition of the inhibitor. Therefore, compatibility investigation is highly essential for the applicability of every shale inhibitor. The results of compatibility tests which was performed on test fluid N.2 to N.4 along with its incorporation with 30 g/L Henna extract are listed in Table 6. The rheological properties, fluid loss, and less frequent the mud cake thickness of the designed test fluids were observed to decrease after modification by Henna extract. For the better observation of the alteration of properties due to Henna extract, the percentage of decrease in every parameter was determined by comparison before and after incorporating the Henna extract. Apparently, Henna extract had no significant effect on rheological properties (especially for test fluid N.5, heavier fluid) and had also a positive effect on controlling fluid loss. The results also indicated that, Henna extract did not have any effect on mud density. Since no significant alteration was observed, the compatibility of Henna extract with the common WBDF

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Fig. 11. Contact angle measurements for shale disks exposed to different concentrations of Henna extract aqueous solution (both in natural pH and adjusted pH of 9).

Fig. 12. Contact angle measurements for shale disks exposed to test fluid N.2 to N.4 and their modification by 30 g/L Henna extract: (a) test fluid N.2; (b) test fluid N.3; (c) test fluid N.4.

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Table 6 Compatibility tests results. Properties

Test fluid N. 2#

71 q600 q300 48 Gel 10-min (pa) 4.5 Decrease (%) 11.11 API FL (ml) 9.60 Decrease (%) 14.58 PV (cp) 23 Decrease (%) 17.39 YP (pa) 12.5 Decrease (%) 12.00 AV (cp) 35.5 Decrease (%) 15.49 Mud density (pcf) 70 Decrease (%) 0.0 Mud cake thickness (mm) 2.5 Decrease (%) 4

2# þ HE 3#

3# þ HE 4#

4# þ HE

60 41 4

45 33 2

85 61 5.5

8.2 19 11 30 70 2.4

57 40 2.5 20 9.2 13.04 17 29.41 11.5 8.69 28.5 22.8 70 0 2.3 4.3

8 12 10.5 22.5 70 2.2

90 64 6 8.33 3.2 0 26 7.69 19 2.63 45 5.55 86 0 2.9 0

3.2 24 18.5 42.5 86 2.9

HE: Henna extract.

additives was fully evident. It is noteworthy that the decrease in rheological properties and increase in fluid loss of the designed WBDFs have been reported after modification by polyoxyalkyleneamine [16]. 3.6. Lubricity tests Drilling fluids should provide sufficient lubricity to reduce the friction forces between the wellbore and drill string. The results of lubricity tests performed on the test fluid N.2 to N.4 and its incorporation with 30 g/L Henna extract are shown in Table 7. After modification by Henna extract, the values of TRP reduced by a factor of 11.4%, 16.66%, and 2.32% for test fluid N.2, N.3, and N.4, respectively. Therefore, the ability of Henna extract for enhancing lubricity of designed WBDFs is fully obvious. This was completely visible from the fatty appearance of Henna extract aqueous solution. This characteristic can improve lubricity to the drill string in the open hole which is of a high importance in directional drilling (especially in Extended-Reach Drilling Wells) where the drill string is constantly in contact with the wellbore wall. 3.7. Advantages of Henna extract as a shale inhibitor in WBDFs Drilling is one of the major operations in the upstream petroleum industry which can extremely influence the environment especially in offshore sector. This is definitely due to the associated wastes with it which are mainly drilling cuttings and the fluid used to lift the cuttings [54]. A variety of chemical components are added to drilling fluids for different purposes which can adversely impact the environment. As earlier mentioned in the text, shale inhibitors are added to drilling fluids Table 7 Lubricity tests results. Test fluid N.

TRP

Decrease (%)

2# 2# þ 30 g/LHenna extract 3# 3# þ 30 g/L Henna extract 4# 4# þ 30 g/L Henna extract

17.5 15.5 21 17.5 21.5 21

11.4

TRP: Torque reading parameter.

16.66 2.32

as an effective way to control shale-water interaction, so they can also impact the environment. Henna extract is a natural dye which is traditionally used as a hair and skin dye, so it cannot have environmental problems as well as is highly useful in offshore drilling operations. Henna can be found in abundance in Iran as vast areas of agriculture lands are dedicated to cultivate it. Therefore, there is no concern on availability of Henna for drilling purposes. Significant export of Henna from southern of Iran to other countries approves this claim. Henna is quite an inexpensive natural dye which can be purchased with an average price of $1/Kg of leaves; thereby, low cost is an appropriate feature for Henna extract which distinguishes it from other inhibitors. The other merits of Henna extract which paves the way for its applicability in WBDFs are compatibility, anti-corrosion property, and lubricity improvement. 3.8. Probable mechanism for shale stability by Henna extract The results of current study show that Henna extract is able to improve the inhibitive property of WBDFs and 30 g/L could be introduced as the optimum concentration for it. Shale stability could be achieved through various mechanisms comprising cation exchange, coating, plugging the pore matrix, plastering the micro-cracks, osmotic backflow (i.e. generating the high osmotic pressure) and increase in filtrate viscosity. According to the results from this study and those of available in the literature, coating is probably the main mechanism for shale stability by Henna extract. When WBDFs incorporated with Henna extract come into contact with water-sensitive shales, Henna extract absorbs on shale through hydrogen bonding between hydroxyl groups of its constituents and oxygen atoms available on silica surface of montmorillonite (a familiar member of smectite clays and the main responsible for shale instability). In much simpler words, Henna extract coats the surface of shale particles which in effect causes shale more hydrophobic and consequently stable. 4. Conclusions In the present research, a comprehensive set of experiments was carried out to assess the swelling inhibitive characteristic and side effects of Henna extract in WBDFs. The following conclusions were obtained: The adsorption measurements indicated that the adsorption behavior of Henna extract on the addressed shale cuttings under scrutiny had an acceptable agreement with Linear adsorption isotherm model so that the correlation coefficients were 0.9185 and 0.9586 for natural pH and adjusted pH to 9, respectively. From dynamic linear swelling, Henna extract diminished the swelling capacity of the addressed shale sample effectively. Based on the shale cuttings dispersion tests, it was found that the tendency of the given shale formation to disperse into the aqueous phase decreased significantly after exposing to Henna extract. Henna extract increased the hydrophobicity of shale formations very well. This issue proposes wettability alteration as the mechanism for shale stability by Henna extract. The determinations of compatibility revealed that Henna extract was compatible with the common WBDF additives and had a positive impact on the amount of fluid loss. In addition, the results of the lubricity test indicated that Henna extract increased the lubricity of WBDFs. This finding is highly significant in directional drilling where the drill string is constantly in contact with the wellbore wall. To sum up, several advantages such as high performance, lubricity improvement, environmental friendliness, compatibility with WBDF additives, anti-corrosion, low cost, and

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availability make the applicability of Henna extract as a potential candidate for shale stability in WBDFs. Acknowledgements The authors would like to thank Petroleum University of Technology (PUT) and National Iranian Drilling Company (NIDC) for their laboratory support. Nomenclature

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