Preparation of Drilling Fluids From Tagan Superhydrophobic Clay: Superhydrophobic Clay Testing

doi:10.21203/rs.3.rs-4619644/v1

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Preparation of Drilling Fluids From Tagan Superhydrophobic Clay: Superhydrophobic Clay Testing

https://doi.org/10.21203/rs.3.rs-4619644/v1

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This paper reports a process for obtaining superhydrophobic clays from Tagan bentonite to produce anhydrous drilling fluids from superhydrophobic organo-clays. Various cationic surfactants were used as superhydrophobisers. An organophilic (superhydrophobic) clay with a contact angle of 170° was obtained in the presence of tetrakis(decyl)ammonium bromide (TKAB). Placing a water drop on the surface of the resulting superhydrophobic clay powders and measuring the contact angle of the water drop on the powder are challenging because the water drop runs off quickly, similar to a mercury drop. The distribution and stability of organophilic clay particles in diesel fuel fluid obtained by TKAB were determined optically. The organophilic clay particles based on TKAB formed a stable suspension in diesel fuel and did not mix with the water phase. In the water phase, the TKAB-based organophilic clay could remain on the surface of the water phase for more than 365 days. Thermo-gravimetric analysis and differential scanning calorimetry were performed on Tagan clay and organo-clay obtained by TKAB because drilling melts can be subjected to high underground temperatures. A methodology for obtaining drilling fluid was proposed based on these data. The resulting drilling fluid belongs to the type of drilling fluids based on organo-clay in the presence of anhydrous petroleum products with thixotropic properties. This drilling fluid was prepared according to the characteristics of Kumkol oil. The formulation of the resulting anhydrous drilling fluids and their technical characteristics are presented.

superhydrophobic clay

Tagan clay

drilling fluid

Kumkol oil

thixotropic properties

polymers

The production of organo-clays has attracted worldwide attention because of the increasing demand for clay composite materials [1-8]. Many difficulties have been encountered in developing methods for producing such organo-clays, e.g. the best clays or improving the quality of clay to produce superhydrophobic organo-clays with water contact angles of >150°. Such superhydrophobic organo-clays must also be extremely stable in non-polar fluids. In this direction, foreign companies, such as Rockwood and Cloisite Southern Clay Products (Cloisitliler, USA), Nanofil, Sued Chemie (Germany) and Nanocore, are actively working on organo-clay production [1,9].

The methods of obtaining superhydrophobic montmorillonite (MMT) have been reported [9]; however, only octadecylamine was used, and the water contact angle was only 157° [9]. Previous studies [1-11] examined methodologies for obtaining organo-clays from different clays using various modifiers but reported water contact angles of 90°–150°. In the present study, superhydrophobic organo-clay was obtained in powder form that could not support a waterdrop; hence, the water contact angle was greater than 170°. Such superhydrophobic clay was introduced into a liquid with very low polarity and showed high long-term stability. Therefore, this paper proposes an optimal organo-clay to obtain stable thixotropic drilling fluids [11]. This montmorillonite type has a high potential for super hydrophobisation and supramolecular intercalation by any modifier molecules.

The objective of this study was to obtain organophilic clay of the best quality from Tagan MMT, possessing excellent stability in an organic environment, and a technology for producing drilling fluids was proposed based on it. The resulting organophilic clay exhibited thixotropic properties in an anhydrous environment.

The novelty of the work is that superhydrophobic organo-clays based on Tagan clay with water contact angles of >170° were obtained, comparing when maximally degree according to the results of another articles [1-11, 22-36] were no more than 150-157°. Due to increased contact angle the obtained organoclay revieled high degree of stability and distribution in a non-polar liquid. In addition, the suitability of the resulting organo-clay for preparing the drilling fluid was determined, and technological schemes for producing the organo-clay and preparing a drilling fluid based on the organo-clay were proposed.

Materials

This study used Na–MMT from Tagan Field (Quarry 12) bentonite clay (East Kazakhstan region). The conditional chemical formula of bentonite was (OH)₄Si₈Al₄O₂₀·n(interlayered)H₂O. Tagan bentonite has a light pink colour with dark pink spots. This type is sometimes called Tagan medical bentonite.

Despite the considerable information on the adsorption of various surfactants according to Kazakhstan’s clay types, few studies have examined the manufacture of organo-clays from Tagan bentonite clay [1]. The Tagan deposit occupies a special place among the types of domestic clay deposits because the bentonite clay in the Tagan deposit comprises 95% MMT, and their inter-layer spaces can expand very wide (till 19 Å) in a liquid, i.e. they have high adsorption abilities [1,9]. The various bentonites differ in chemical and mineralogical composition, physical-chemical properties and external features. Bentonite clay from the 12^th horizons Tagan deposit (Ust-Kamenogorsk, Kazakhstan) in this study is one of the famous clays used today because its quality characteristics are superior to the reference Wyoming bentonite (USA). Many global manufacturers claim this because the clay swells very well. In addition, the adsorption properties are so attractive that it is exported to France as a pure enterosorbent.

MMTs, as a raw material, do not show evident catalytic and adsorption activity, so they must be activated or converted in advance. The clay was purified by washing through decantation, and thermo-acid activation was performed. The MMTs were first dried at 90°C for two hours. The clay was mixed 1:3 with a 15% sulfuric acid solution, then mixed continuously at 90°C for two hours and heated in an acid solution in a water bath. After two hours, the bentonite was filtered, placed in a porcelain plate and washed with an aqueous ammonia solution, followed by distilled water until the pH was neutral. The bentonite filtrate was dried in a laboratory dryer at 80°C. Dried activated MMT was obtained, sieved through a sieve and placed in a Glass Conical Flask with a ground stopper.

Several surfactants produced by Sigma-Aldrich were used as hydrophobisers to process the Na–MMT [12]:

Tetrakis (decyl) ammonium bromide (ТКАB)-C₄₀H₈₄BrN-CAS: 14937-42-9
Didecyl dimethyl ammonium bromide (DCDAB)-C₂₂H₄₈BrN-CAS: 7173-51-5
Trimethyloctadecylammonium bromide (ТМODАB) C₂₁H₄₆BrN-CAS: 1120-02-01
Cetylpyridinium bromide (CPB) C₂₁H₃₈BrN-CAS:57-09-0
Octadecylamin (ОДА) C₁₈H₃₉N-CAS: 124-30-1 [9] for comparisons from before performed works

4) The stability of superhydrophobic clays in organic environments was evaluated. Diesel fuel with a low dielectric permeability was used as the liquid to test the ability of the superhydrophobic clays to disperse in the organic media. The diesel fuel contained organic compounds from C₈H₁₈ to C₁₇H₃₆. Diesel fuel is a complex mixture of organic compounds: paraffins, ultimate 10%–40% (general formula C_nH_2n+2); naphthenic–polymethylene, 20%–60% (general formula C_nH_2n); and arene–aromatic hydrocarbons compounds, 14%–30% (general formula C_nH_2n−6) and their derivatives. The average molecular weight was 110–230 amu, and the boiling points were 170°C–380°C. The dielectric constant of the diesel fuel used in this study was ε = 2.05 [13]

The reagents required to produce the drilling fluids were as follows:

Superhydrophobic clay obtained by KTAB-modified Tagan Na–MMT was used as the organo-modified clay (organo-clay). The organo-clay had structure-forming, rheology-regulating properties and could reduce the water supply of drilling fluids and crust-forming components.
Limestone (Ca(OH)) was used to prevent the accumulation of carbonates in water-based drilling fluids. It increases the pH and amount of calcium cations in the drilling fluid and improves the resistance of the drilling mud to the aggressive effects of hydrogen sulfide.
Polyacrylamide (PAA) film was used to cover and protect the wall of the well to prevents the penetration of filtrate into the rock structure. This promoted the formation of a strong filtration crust and improved the lubricating properties of the solution.
Halite was used to aid in making the walls of the well stronger.

1) Preparation of the hydrophobic solutions for clay processing

In the hydrophobisation process, 100 ml surfactant (CTAB, TKAB, TMODAB, CPB, ODA and DCDMAB) solutions were prepared at concentrations of 1 M and 0.1 M. Na–MMT clay in the 1–5G range was placed in the prepared solutions and stirred for 5–6 hours in a heated laboratory magnetic mixer at 70°C. The powder was placed in a Petri dish and dried in a laboratory dryer until the weight stabilised, crushed to very fine particles and sieved to 0.63 microns. Subsequently, the hydrophobicity of the types of organo-clays was determined.

2) Transmission electron microscopy (Kazakh Japanese Innovation Centre, KazSAU, Almaty) was used to characterise the morphology of the clay [14].

3) Goniometer LK-1 was used to measure the contact angle of a drop lying on the surface of a powder of hydrophobic clays using sessile-drop goniometry techniques. The Goniometer LK-1 was fabricated based on a horizontal microscope and a digital HD video camera, and the contact angle of a lying droplet on the display could be calculated [15]. The powder was pressed through two glass plates and smoothed before determining the waterdrop contact angles on the hydrophobic clay powder surfaces.

4) X-ray diffraction (XRD) was carried out on an automated diffractometer Drone–3 using CuКa-radiation and β-filter. The conditions for capturing diffractograms are as follows: U = 35kV; I = 20mА; θ–2θ capture; detector 2°/min. X-ray phase analysis on a semi-quantitative basis was performed on the diffractograms of powder samples using equal suspensions and artificial mixtures. The quantitative ratio of the crystal phases was determined. The interpretation of diffractograms was carried out using the data from the ICDD card file: PDF2 powder diffractometric database (powder Diffractometric File) and diffractograms of Minerals Pure from impurities. The content calculation was carried out for the main phases.

5) The stability of the dispersed phase was determined by sedimentation in an organic medium using a photoelectrocalorimeter.

6) Methods of differential scanning calorimetry and thermo-gravimetric analysis (DSC and TGA) were used to assess the effect of chemical changes in organo-clay composition under the influence of temperature because drilling fluids are exposed to extremely high temperatures in the subsurface. These methods were carried out to study physicochemical and chemical processes occurring in a substance under the condition of a controlled change in temperature.

7) The rheological properties of drilling fluids and Kumkol oil taken as samples were also determined using indirect methods. The following measurements were performed: determining the density of a liquid using a hydrometer, determining the pH of a solution using a pH metre and determining viscosity using a rheometer. The relationship between the shear rate and shear stress of Kumkol oil and drilling fluids based on TKAB organo-clay was determined using the Rheometer MCR 702 Multi-Drive (Anton Paar) device.

Clay minerals contain different types of alumina-silicates, the main types of which change from one to another in natural conditions over a billion years [16–18]. The alumina-silicate skeleton in clays consists mainly of alternating parallel two-dimensional sheets formed by a silicate tetrahedron and an aluminium octahedron [19–21]. The location of these sheets and the degree and nature of exchange within them determine the chemical and physical properties of materials, including the adsorption properties.

Natural alumina-silicates can be divided into two groups depending on their crystal lattice–crystalline and amorphous [21–22]. Amorphous alumina-silicates are characterised by their ability to swell in the ion-exchange process, similar to ion-exchange resins.

Three types of bentonite clay in the Tagan MMT deposit were fixed: alkaline (pink colour), alkaline earth and pharmaceutical. Owing to the peculiarities of the genesis of the Tagan deposit, the different properties of MMTs and bentonite clays make it possible to use them in various industrial technologies. Alkaline bentonites are used to produce drilling fluids.

The complete chemical composition of the clay was determined by X-ray fluorescence spectroscopy at the Centre for Physicochemical Methods and Analysis of the Faculty of Chemistry and Chemical Technology. Table 1 lists the chemical composition.

Table 1

Oxide chemical composition of Tagan clay
The amount of oxides in the mineral	СаO	MgO	Fe₂O₃	Al₂O₃	SiO₂	Na₂O	K₂O	The residue after burning
Quantitative proportion of oxides in raw MMT mineral, %	15	4	6	10	30	1.5	4	69.5
Quantitative proportion of oxides in the mineral Na–MMT, %	4	0.9	4	9.8	31	0.6	0.91	84.8

Many other elements and oxides were found in the clay composition, along with Fe, Al, Si, Zn, Ti, Ca and Mn, by determining the elemental composition of Tagan bentonite and X-ray fluorescence analysis. In addition, the composition of Tagan MMT was calcium–sodium MMT because of the large amount of calcium for determining the elemental composition. The MMT of the Tagan deposit was isolated from the calcium and magnesium ions by performing decantation washing, thermal activation and acid activation operations. In addition, the swelling property, ion-exchange capacity and inter-pack spaces of the clay also increased.

MMT undergoes self-dispersion in aqueous media and spreads into individual plates up to 1 nm thick and 20–250 nm in diameter [23–24] as shown in Fig. 1.

X-ray analysis was performed to determine the mineral composition of Tagan bentonite and organo-сlay. Tables 2 and 3 lists the results.

Table 2

Mineral composition of Tagan MMT
Mineral	Formula	Quantity,%
MMT	(Na,Н)_0.3(Al,Mg, Ca)₂Si₄O₁₀(OH)₂·xH₂O	96.4
Quartz	SiO₂	3.6

Table 3

Mineral composition of Tagan organo-clay
Mineral	Formula	Quantity,%
MMT	(Na,Н)_0.3(Al,Mg, Ca)₂Si₄O₁₀(OH)₂·xH₂O	94–97
Quartz	SiO₂	2–4
Amorphous phase	-	1–2

The mineral composition of Tagan bentonite and organo-clay by XRD revealed the mineral MMT, quartz and amorphous phases.

Several methods for the hydrophobisation of MMT are currently used. The most common methods for the hydrophobisation of MMT include surface modification, modifier intercalation and bio-hydrophobisation methods [25]. Each of these methods has its advantages and disadvantages, and the requirements depend on the choice and research goals of the method and the requirements for the final product. For example, the bio-hydrophobisation method is environmentally friendly and effective in some cases. Hence, the choice of hydrophobisation method should be based on a thorough assessment of the requirements of the final product and the possibilities of using various methods, considering their advantages and disadvantages [26].

In structural arrangements, some Si⁴⁺ ions in the crystal are exchanged with Al³⁺ ions, which results in an excess negative charge that is compensated for by the alkali and alkaline earth cations, which are not bound in the lattice and can exchange for other cations [23,27–35]. Accordingly, clay particles can have uncompensated negative charges on the surface, and an interaction between amino groups and clay particles can also be conducted by forming hydrogen bonds.

The mechanism for the adsorption of cationic surfactants on the surface of clay particles involves electrostatic interactions. These interactions can be observed in the diagram below as an example of the interaction of clay particles and alkylammonium bromide (AlkAB) (Figs. 2a and 2b).

The clay mineral was hydrophobised using the intercalation method. The primary consideration was selecting the optimal hydrophobiser. A drop of water was placed on the surfaces of organo-clay powder treated with various hydrophobisers, and the water contact angles were measured using the Goniometer LK-1. Table 4 lists the contact angles found for each of the organo-clays.

Table 4. Contact angles of waterdrops planted on the surface of various types of organo-modified clay powders

Among the organo-clays in Table 4, the maximum contact angle was 170° with TKAB. This result can be explained by the structure of the TKAB molecule having four long non-polar hydrocarbon chains that give it four times more hydrophobicity than the others. The end side of hydrocarbon TKAB has few spaces when tightly packed together compared to that of CPB, which has a benzene ring on the end, so even with the greatest concentration, the maximum water contact angle did not exceed 128°. As for the others, the contact angles of the waterdrops at a low superhydrophobiser concentration (0.1 M) were higher than those at a high concentration (1 M), shown in Table 4. In particular, the contact angle decreased from 39° to 9° in the case of CPB, and it decreased from 135° to 128° in the case of TMODAB. Upon increasing the hydrophobiser concentration, the contact angle of the organo-clays also decreased. This decrease depends on the features of these molecules, i.e. the position and chain length that the molecule occupies on the surface of a solid particle. Such a deviation occurred from an excessive surfactant concentration. Therefore, the surfactant molecule forms a bilayer, resulting in a reverse hydrophilic surface [36–41], as shown in Fig. 3.

The contact angles of waterdrops increased in another group of hydrophobisers as the concentration of the surfactant molecule increased.

Figure 4 shows changes in the optically observed light conductivity values of the suspension of organo-clays obtained by various hydrophobisers in the diesel fuel liquid for a certain period. Experimental measurements of the sedimentation kinetics revealed that the organo-clay obtained in the presence of TKAB exhibited the lowest light transmittance and its equivalent was 23%. The organo-clay with the highest contact angle (170°) was used in the following investigations. The organo-clay obtained only in the presence of TKAB was used because this is the most necessary superhydrophobic surfactant. Figure 5 shows the Fourier transform infrared (FTIR) spectra, which were obtained to ensure that TKAB had adsorbed on the clay surface.

The FTIR spectra revealed the intercalation of surfactants into the inter-layer space of MMT. FTIR spectroscopy is a universal method for studying a solid using computerised optical methods to observe the functional groups, especially those that determine the surface groups of atoms of a clay mineral. The results (Fig. 5) showed the oscillations of Si–O–Si bonds in the wide bands at 1036 сm^− 1. The peaks at 471 cm^− 1 and 527 cm^− 1 reflect the oscillations of the Me–O bond. The peak at 914 cm^− 1 was assigned to the oscillation of Si–О–Si bonds. The peaks at 3100–3500 сm^− 1 (particularly 3627 cm^− 1) were attributed to bound water molecules in the MMT molecule, and the peak at 1631 сm^− 1 was assigned to deformation oscillations that reflect hydrogen bonds.

The peaks at 1444–1469 cm^− 1 were assigned to C–H stretching modes, indicating C–H bonds. The peaks on 2850.91 сm^− 1, 2954.66 сm^− 1, 2872.68 сm^− 1, 2994.66 сm^− 1 and 2920.56 сm^− 1 were assigned to –CH₂– and –CH₃ bonds. These results showed that the adsorption of TKAB takes place on the surface of MMT.

DSC and TGA revealed a weight loss between 140°C–200°C. These results revealed that various interphase changes occur here (green curve in Fig. 6). During the process, the weight decreased as the temperature increased, i.e. water was removed from the material and it became more crystalline [31]. The weight change was 15.788 mg. In addition, the melting point changed (purple curve).

The organo-clay obtained by TKAB showed more significant weight loss than Na–MMT (Fig. 7). Hence, the hydrocarbon chain containing TKAB was oxidised in the presence of oxygen and was released in the form of CO₂. It undergoes phase changes and releases gas as oxides, leading to significant weight loss. The mass of the organo-clay obtained in the presence of TKAB was 15.577 mg lower than that of Na–MMT. TKAB causes a certain amount of clay to merge into single particles in the inter-layer space between them.

The production of drilling fluids with an organic medium, not a water environment, releases significant amounts of heat. Therefore, a drilling fluid was developed using diesel fuel as an anhydrous medium, and its technical characteristics were determined. The complete process of producing drilling fluid based on organo-clay in an anhydrous medium is illustrated in Fig. 8. Figures 9a and 9b show time-lapse images in diesel fuel fluid for 48 hours.

The drilling fluid was prepared following the requirements for all drilling fluids, and the technical characteristics, such as the density, viscosity and pH of the medium, were examined. Tables 5–6 show these characteristics.

Thixotropic properties are observed in high-viscosity and bituminous oils because they are complex, high-molecular-weight compounds. Such properties in oil can be found in paraffins, resins and asphaltenes. Figure 10 shows the viscosity of the time-dependent liquids during shear stress.

The thixotropic properties of drilling fluids containing organo-clays were measured within 48 hours (Fig. 10). The rheological changes were completed within 24 hours. The technical descriptions of the drilling fluid and the Kumkol Field oil were relatively close to each other, and the polymer solution could form a sliding layer in the drilling well, providing an optimal effect on the light movement of the wellbore. Thus, this drilling fluid can be used to drill Kumkol oil and similar field oils.

From Tagan bentonite of Kazakhstan, organo-clay types were developed at different concentrations using four cationic surfactants: CPB, DCDAB, ТМODАB and TKAB. A drop of water was placed on the surfaces of the obtained organophilic clay powders. At a high TKAB concentration, the water contact angle was 170° and > 140° at other TKAB concentrations. An effective way to determine the stability of an organic environment was developed using an optical method. The zeta-potentials of MMT and TKAB organo-clay were determined using a zetasiser device. TKAB molecules were bound to the flesh of the clay. This paper revealed a path for forming a modified organo-clay with TKAB, and a technological scheme for obtaining organo-clay was obtained. The most organophilic clay type was selected by comparing the hydrophobicity of all the resulting organo-clays.

Acknowledgements

The authors would like to acknowledge financial support for the grant funding of the Kazakhstan state government scientific project AP19674742 (IRN), ‘Technology for obtaining a new organomineral composite material based on natural bentonite of East Kazakhstan’.

Funding

This scientific research was funded by a from the Kazakhstan state government scientific projects AP19674742 (IRN) ‘Technology for obtaining a new organo-mineral composite material based on natural bentonite of East Kazakhstan’ (ИРН AP19674742 «Технология получения нового органоминерального композиционного материала на основе природного бентонита Восточного Казахстана»). The funding source was the Science Committee of the Ministry of Science and Higher Education of the Republic of Kazakhstan. The authors express their gratitude for this allocated grant funding.

Information about authors*

Ibraimova Dana Mykty-Kereevna (corresponding author) — Candidate of chemical sciences, Senior Lecturer, Al-Farabi Kazakh National University; Al-Farabi ave., 71, 050040, Almaty, Kazakhstan; e-mail: [email protected]; https://orcid.org/0000-0002-1761-9745

Rozhkova Olga Vladimirovna — Doctor of chemical sciences, Professor, Academician of the National Academy of Natural Sciences of the Republic of Kazakhstan, JSC “Science and Technology Solutions”, Satbayev street, 22/5, 050013, Almaty, Kazakhstan; NAO “Saken Seifullin Kazakh Agrotechnical University”, Zhenis street, 62, 100011, Astana, Kazakhstan. e-mail: [email protected]; https://orcid.org/0000-0001-8163-7035

Kulichikhin Valeriy Grigorievich, — Corresponding Member of the Russian Academy of Sciences, Doctor of chemical sciences, Professor, Head of Rheology polymers Department of V.I.Topchiev Institute of Petrochemical Synthesis RAS, 119991, GSP-1, Leninsky avenue, 29 , Moscow, Russia, [email protected]; https://orcid.org/0000-0001-8989-866X

Musabekov Kuanyshbek Bituovich — Doctor of chemical sciences, Academician of the National Academy of Natural Sciences of the Republic of Kazakhstan, Professor, Al-Farabi Kazakh National University; Al-Farabi ave., 71, 050040, Almaty, Kazakhstan; e-mail: [email protected]; https://orcid.org/0000-0003-1114-1901

Khamitova Tolkyn Ondirisovna — PhD, Associate Professor, The Department of Soil Science and Agrochemisrty, Agronomic Faculty, Kazakh Agro Technical University Named after Saken Seifullin, Nur-Sultan 010000, Kazakhstan; e-mail: [email protected]; https://orcid.org/0000-0002-4691-3732

Rozhkov Vitaly Igorevich — Candidate of technical sciences NAO “Saken Seifullin Kazakh Agrotechnical University”, Zhenis street, 62, 100011, Astana, Kazakhstan; e-mail: [email protected]; https://orcid.org/0000-0002-3232- 5972

Maryinsky Svetlana Georgievna— Candidate of Biological Sciences. Director of Altai Geological-Ecological Institute LLP, Ust-Kamenogorsk, K. Liebknecht street, building 21 [email protected] https://orcid.org/0000-0003-0659-6397

The data that support the findings of this study are available from the Laboratory of Kazakh Japan Innovation Centre (https://www.facebook.com/kjickaznau/about ) they have no own website, but have own webpage on the Facebook for sharing the news] of The Kazakh State Agrarian Research University (https://www.kaznaru.edu.kz/university/about) and from the Laboratory of Karaganda Buketov University (Kazakhstan) (https://buketov.edu.kz/en/ ) restrictions apply to the availability of these data, which were used under licence for the current study, and so are not publicly available. Data are however available from the authors upon reasonable request and with permission of [TEM analysis results from [email protected] and of TGA and DSC analysis results from [email protected] ].

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Preparation of Drilling Fluids From Tagan Superhydrophobic Clay: Superhydrophobic Clay Testing

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