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Article

A New Application for Salted Water-Based Fluids with Palygorskite: Formulation Designing for Temporary Plug and Abandonment Operations of Petroleum Wells

by
Ruth Luna do Nascimento Gonçalves
1,*,
Anna Carolina Amorim Costa
1,
Mário César de Siqueira Lima
1,
Karine Castro Nóbrega
1,
Waleska Rodrigues Pontes da Costa
1,
Laura Rafaela Cavalcanti de Oliveira
1,
Renalle Cristina Alves de Medeiros Nascimento
2,
Michelli Barros
3,
Tiago Almeida de Oliveira
3 and
Luciana Viana Amorim
1
1
Department of Petroleum Engineering, Federal University of Campina Grande, Campina Grande 58429-900, PB, Brazil
2
Santo Agostinho Faculty, Federal Rural University of Pernambuco, Cabo de Santo Agostinho 21941-915, PE, Brazil
3
Department of Statistics, University of the State of Paraíba, Campina Grande 58429-500, PB, Brazil
*
Author to whom correspondence should be addressed.
Appl. Sci. 2025, 15(6), 2980; https://doi.org/10.3390/app15062980
Submission received: 11 January 2025 / Revised: 5 February 2025 / Accepted: 5 March 2025 / Published: 10 March 2025
(This article belongs to the Special Issue Advanced Drilling, Cementing, and Oil Recovery Technologies)
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Abstract

:
Palygorskite has shown satisfactory performance in salted water-based fluids, especially as a rheological agent. However, this type of formulation has been used in the petroleum industry only in well drilling operations. This study proposes the development of a salted water-based fluid with palygorskite, which presents an adequate performance as a liquid barrier element in temporary abandonment operations of wells. Based on a factorial design, seven fluid formulations were prepared with varying concentrations of palygorskite and PAC LV and were tested by measuring the HPHT filtrate volume, rheological properties, density, and pH. For comparison purposes, the results of the seven formulations were evaluated against a formulation without palygorskite and analyzed for their performance in abandonment operations. The results showed that the presence of palygorskite reduces filtrate volumes by at least 21%, thereby helping control the pressure exerted by the fluid column, which is the primary requirement for abandonment operations. Furthermore, the fluid that contained the highest amount of palygorskite and PAC LV (20 g and 8 g, respectively) showed the best results regarding filtrate control (11.2 mL) and solid sedimentation. Therefore, it is a very promising alternative for use as a well barrier element in the temporary abandonment of wells.

1. Introduction

The abandonment operation generally occurs at the end of the well’s productive life. It involves the placement of barrier elements to contain the fluids inside the reservoir, preventing the contamination of other formations or even aquifers [1,2]. Recently, this operation has sparked discussions among operators, motivated by the “plug & abandonment wave” of wells that need to be permanently abandoned around the world [3]. This phenomenon is associated with the natural aging of numerous mature wells that have been in operation for several decades, as well as the relatively shorter average lifespan of currently drilled wells, particularly horizontal and unconventional ones, which ensure higher production efficiency [4]. In recent years, there has been growing concern about the need to carry out safe abandonment operations due to incidents of fluid leaks from both plugged and unplugged wells. These leaks can have severe and long-term effects on the environment and local communities. Remediation efforts can require significant investments, and the reputation of the operating company may also be negatively impacted [5,6].
Abandoning a well can be a time-consuming and expensive operation, depending on its conditions [3]. Additionally, the forecast of an increasing number of wells to be abandoned in the coming years and the operational challenges related to these operations reiterate the need for new strategies to carry them out safely and economically. One of the most prominent strategies is the development of alternative materials to be used as barrier elements.
Portland cement is commonly used as a barrier material for the abandonment of petroleum wells [3,4], despite its known limitations. During its placement inside the well, for example, the cement can become unstable and may result in crack formation. Additionally, it may undergo mechanical or chemical degradation. Furthermore, the operational costs of using Portland cement are higher, since a rig is required for pumping and placing the cement paste [1,7,8]. Therefore, alternative materials to cement that ensure operational safety and cost reduction in well abandonment have been considered [3,4,7,8,9,10,11]. These studies have primarily focused on elements that, like cement plugs, constitute mechanical barriers. Thus, the use of liquid barriers, consisting of columns of fluids with sufficient hydrostatic pressure to contain fluids from permeable intervals and prevent their flow into the well, despite being provided for in some regulatory guidelines, such as the Brazilian [12] and Norwegian [13] standards, is still sparsely explored in the literature.
In the oil industry, the study of products and formulations of fluids is usually related to well drilling operations. In this scenario, the use of clay-based aqueous fluid formulations has been consolidated for many decades, and these formulations have gained prominence due to their commercial availability, simplicity in preparation, low cost, and compatibility with different types of formations [14,15,16]. Furthermore, when the clay mineral used to compose these fluids is palygorskite, it is possible to obtain advantages such as high thermal resistance and the ability to maintain rheological properties even with exposure to salts, which may be in the fluid formulation itself or be added from influxes of formation waters or via contact with saline formations [14,17,18].
Most of the work found in the literature that concerns palygorskite-based aqueous fluids has considered technical standards and operational aspects relevant to its application in drilling operations, such as its capacity for carrying cuttings [18,19,20]. However, the use and qualification of this type of formulation as a barrier element in well abandonment is still sparsely explored in the petroleum industry, so there are no studies in the literature that address the possibility of this application, nor specifications or regulatory standards that guide its qualification. In this sense, this work proposes the development of a formulation of a salted water-based fluid added with palygorskite, with an adequate performance for application as a liquid barrier element in temporary abandonment operations of petroleum wells.

2. Materials and Methods

2.1. Materials

Palygorskite and low-viscosity polyanionic cellulose (PAC LV) were the main materials used as additives in this experimental work and were used as viscosifying and filtrate controller agents, respectively. The industrialized sample of palygorskite, originally from Greece, was used as received, without any additional treatment or modification, while the PAC LV was obtained from Denver Especialidades Químicas (Cotia, SP, Brazil).

2.2. Characterization Techniques for the Palygorskite Sample

The chemical composition of the palygorskite sample was obtained using the energy-dispersive X-ray fluorescence (XRF) technique, in a BRUKER S2 PUMA—SERIES II equipment (Bruker, Karlsruhe, Germany), using a Pd tube (Bruker, Karlsruhe, Germany) with a maximum power of 50 W, a maximum voltage of 50 kV, a maximum current of 1 mA, and a HighSense Silicon Drift Detector (HighSense SDD) (Bruker, Karlsruhe, Germany).
The mineralogical composition of the sample was obtained via X-ray diffraction (XRD) in a Bruker D2Phaser (Bruker, Karlsruhe, Germany). equipped with a Lynxeye detector (Bruker, Karlsruhe, Germany), and copper radiation (CuKα, λ = 1.54 Å) with a Ni filter, a current of 10 mA, and a voltage of 30 kV. A 2θ scan was performed from 2° to 70°, with a step of 0.01°. Phase identification was performed using the crystallographic information files provided by the Inorganic Crystal Structure Database (ICSD), and quantitative analysis was performed using the Rietveld method.
The morphology of the palygorskite sample was analyzed using scanning electron microscopy. The image was taken with a Tescan Mira 4 (Tescan, Brno, Czech Republic) scanning electron microscope, using a backscattered electron detector (BSE) (Tescan, Brno, Czech Republic). The sample was dispersed on a carbon tape for high-vacuum SEM analysis, and it was covered with gold film using a Denton Vacuum Desk V vaporizer (Denton Vacuum, Moorestown, NJ, USA), with a voltage of 30 V applied for 60 s. The image was obtained at a magnitude of 50 kx.

2.3. Fluid Preparation

The fluid formulation proposed to be used as a barrier element presents a saturated NaCl brine (36 g/100 mL) as the continuous phase, added with palygorskite, PAC LV, and NaOH. To obtain an optimized formulation, considering the influence of palygorskite and PAC LV on the properties required for well abandonment, the content of these additives was varied based on a 2 × 2 factorial design, with three more formulations corresponding to the center points, totaling seven formulations, as shown in Table 1 and Table 2.
To prepare the fluid, the content of PAC LV was initially pre-hydrated in 150 mL of deionized water, remaining at room temperature for 16 h. After this, 200 mL of the saturated NaCl brine and the amount of palygorskite corresponding to each experiment were added, in this order, to a Silverson high-shear shaker, model L5, with a stirring interval of 5 min between each component. After the addition of palygorskite, the fluid was homogenized for 20 min. Finally, 0.5 g of NaOH was added, and the fluid was stirred for another 5 min.
For comparison purposes, an additional formulation (named F0) was prepared without the addition of palygorskite and with the highest polymer content determined in the factorial design (8 g).

2.4. Fluid Characterization

All formulations, prepared according to the factorial design, in 350 mL aliquots, were characterized based on the properties that influence the maintenance of the hydrostatic pressure of the fluid column in an abandonment operation, that is, filtrate volume, rheological behavior, and density. Furthermore, the pH was checked to monitor the yield of the products in the formulation and to avoid problems with corrosion.
The filtrate volume of the formulations was determined under conditions of a high pressure and a high temperature in an HPHT filter press (387 series, Fann, Houston, TX, USA), under a temperature of 150 °F (65.6 °C) and a pressure of 300 psi (2.07 mPa). The filtrate was collected for 30 min. For this parameter, the regression of experimental data was performed using the Statistica software, version 7.0.
For the study of the rheological behavior, a Fann 35A viscometer was used to record the dial readings at 600, 300, 200, 100, 6, and 3 rpm, following the API 13B-I standard [21]. From these readings, the measurements of the apparent viscosity (µa), plastic viscosity (µp), and yield point (YP) were obtained using Equations (1)–(3):
μa (cP) = L600/2,
μp (cP) = L600 − L300,
YP (lfb 100ft−2) = L300 − μp
The pH values of the formulations were measured using a pH meter (model Plus, LineLab, São Leopoldo, Brazil), and the density values were recorded using a mud balance (model 140, Fann, Houston, TX, USA).

3. Results and Discussion

3.1. Mineralogy, Chemistry, and Morphology of the Palygorskite Sample

The chemical composition of the palygorskite sample used is presented in Table 3.
The presence of Si, Al, and Mg demonstrates that the sample is a magnesium–aluminum phyllosilicate. These are the main elements that constitute the chemical composition of palygorskites, which has the ideal formula MgAlSi8O20OH3(OH2)4.X[R2+(H2O)4], with X having the possibility to be replaced by Na, Fe, or Mn [22].
Palygorskite commonly presents higher Al content, close to or greater than 10%, as can be observed in the results reported by Galan and Ferrero, Meireles et al., and Zhang et al. [23,24,25] that studied samples of this clay from Spain, Brazil, and China, respectively. However, for samples extracted from deposits located in Greece, such as the one used in this study, this content tends to be lower (close to or less than 5%). Regarding Al content, similar results to those presented in Table 3 were reported by Kastritis and Kacandes, Gionis et al., and Georgopoulos et al. [26,27,28]. Furthermore, a high Fe content was also identified (13.11%), which is also common for palygorskite samples from Greece, according to the works already cited. Thus, the chemical composition of the palygorskite used in this study is within the expected range.
Regarding the mineralogical composition of the sample, the XRD pattern and the quantification of the identified phases are presented in Figure 1 and Table 4, respectively.
Figure 1 illustrates the XRD pattern of palygorskite. The XRD pattern shows crystalline phases corresponding to the presence of palygorskite, antigorite, and quartz. These constituents were, respectively, identified using the crystallographic file numbers 75975, 98794, and 16331, provided by the Inorganic Crystal Structure Database (ICSD). It is possible to verify that the sample presented a sharp and symmetrical peak at 20°, a value close to 8.50°, which typifies the presence of the clay mineral palygorskite, and main peaks corresponded to the presence of impurities such as antigorite and quartz, close to 12.5° and 26.5°, respectively, in addition to the identification of secondary peaks of these minerals.
Quantification using the Rietveld method, as presented in Table 4, shows that this clay is rich in palygorskite, with more than 77% of the sample being made up of this clay mineral, as well as a minimal fraction of quartz corresponding to only 1.16%. Antigorite, on the other hand, presented a considerable fraction of 20.94%. Antigorite belongs to the serpentine group and has the ideal formula Mg6Si4O10(OH)8 [29], which is in accordance with what was observed in the XRF analysis (Table 3). The presence of serpentines in palygorskite samples was also identified by Gionis et al., Zotiadis and Argyraki, and Georgopoulos et al. [27,28,30]. Since the clay sample is mostly composed of palygorskite, it is expected that the properties of the investigated fluid formulations will be predominantly influenced by this clay mineral in comparison to antigorite or quartz.
The morphology observed through scanning electron microscopy of the palygorskite sample is shown in Figure 2.
The microscopy image shows the fibrous morphology of the sample, which is composed of individual bundles. It is also possible to observe that some fibers are grouped, forming larger aggregates. These fibers correspond to the presence of the minerals palygorskite and antigorite, as this last one can also assume a fiber-like morphology [31,32].
The fibrous morphology of the particles can hinder the formation of a thin and impermeable filter cake, as observed in the studies conducted by Neaman and Singer and Asghari and Esmaeilzadeh [33,34], who used palygorskite as an additive for drilling fluids. The presence of permeable filter cakes results in a considerable loss of the fluid–liquid phase to the formation and can compromise the hydrostatic pressure exerted by the fluid column against the formation. Under these conditions, the fluid formulation needs to be added with a filtrate control agent, since maintaining hydrostatic pressure is essential for the safety of abandonment operations.
On the other hand, the elongated shape of palygorskite particles ensures unique colloidal properties to this clay [35], such as resistance to high concentrations of electrolytes, since the rheological behavior of these suspensions results from the mechanical interference between the particles and is not influenced by electrostatic forces. In this way, it is possible to guarantee the control of the fluid density with the use of brines, without compromising the rheological behavior, which could lead to the sedimentation of solids. This phenomenon is undesirable as it would compromise the homogeneity of the fluid column and the hydrostatic pressure exerted inside the well.

3.2. Characterization of the Salted Water-Based Fluid Formulations

The regression equation that correlates the palygorskite (P) and PAC LV (C) contents with the filtrate volume, the relevant data for the analysis of variance (ANOVA), the response surface generated based on the model, and the values of this property for each formulation are presented in Equation (4), Table 5, and Figure 3a,b, respectively.
VF = (14.51 ± 0.24) − (0.05P ± 0.32) − (3.25C ± 0.32) − (0.35P.C ± 0.32)
The mathematical model, obtained through the regression of the experimental data, presented a good fit, with a coefficient of determination of 97.18%. Furthermore, at a 95% confidence level, it can also be considered statistically significant and useful for predictive purposes, as the Fcalculated/Ftabulated ratio was greater than five [36].
Equation (1) and the response surface presented in Figure 3a indicate that only the PAC content exerts a significant influence on the filtrate volume, and the variation in the palygorskite content does not cause changes in this property. Polymers of the same nature as PAC LV have ionized carboxylic groups. Thus, the resulting electrostatic repulsion causes its molecular chains in solution to hydrate and assume an extended conformation, with repulsion also occurring between adjacent chains. Because of this hydration, the filtrate volume is reduced. This mechanism was explained by Damodaran et al. [37].
Despite not having shown a statistically significant influence on the filtrate volume, palygorskite still plays an important role in this property. As can be seen in Figure 3b, formulation F0, prepared without the addition of clay and with 8 g of PAC LV, presented a filtrate volume of 15.2 mL. In contrast, formulation F3, for example, which has the same polymer content and 10 g of palygorskite, presented a filtrate volume of 12 mL, which represents a reduction of approximately 21%. When the clay content was increased to 20 g (F4), this reduction was even greater, approximately 26%. This result indicates that the action of clay together with the polymer is essential for filtrate control. The interaction mechanism between PAC LV and palygorskite can be explained through electrostatic interactions. When added to clay-containing suspensions, such as the formulations studied, PAC LV is adsorbed onto the surface of the clay particles, increasing the negative surface charge due to its polyanionic nature. This increase in charge intensifies the electrostatic repulsion between the particles, preventing their aggregation and promoting the stabilization of the system by keeping them in suspension. As a result, the volume of free water available is reduced, which improves fluid properties that depend on this arrangement, such as filtrate control. The interaction of this polymer with clays was studied by Yang et al. [38].
Although the results obtained from the factorial design have demonstrated the influence of additive content in minimizing the filtrate volume, the interpretation of these results is limited due to the absence of comparative parameters within the international standards in force that allow for the qualification, based on this property, of fluids used as a barrier element for well abandonment. Therefore, the analysis of the results presented in Figure 4 was conducted based on a comparison with aqueous palygorskite drilling fluids developed for applications in well drilling (Table 6).
As shown in Table 6, some palygorskite aqueous drilling fluid formulations presented filtrate volumes lower than or close to those obtained in this work. However, it is worth highlighting that the filtrate volumes of these formulations were, for the most part, obtained in an API filter press and, therefore, under less severe test conditions than those used in this study, which do not represent the field conditions of the petroleum wells to be abandoned.
Even so, it is clear that the most efficient filtration control is obtained with palygorskite fluids whose formulation contains a significant number of additives, such as that proposed by Lijuan et al. [41], who obtained an HPHT filtrate volume of 11 mL, a value practically equal to the minimum obtained in this work, which was 11.2 mL. However, the formulation proposed by the authors demands a higher cost and complexity in preparation when compared to the one proposed in this study.
Regarding the type and number of additives in the formulation, only the fluid developed by Zou et al. [39] presents greater similarity with the formulation proposed in this work. However, its performance is inferior in terms of filtration control, so the minimum filtrate volume value (26.2 mL) is considerably higher than the filtrate volumes of the seven fluids formulated based on the factorial design carried out in this work. Thus, it highlights that the interaction between the additives used in the formulations proposed in this work, in appropriate proportions, ensured promising filtration control, especially for formulations with a higher PAC LV content (8 g), that is, F3 and F4, which may present themselves as suitable alternatives as barrier elements for well abandonment.
Table 7 presents the values of the readings obtained from the viscometer for the speeds of 600, 300, 200, 100, 6, and 3 rpm and the values of the apparent viscosity (μa), plastic viscosity (μp), and yield point (YP) of each formulation.
Since the readings at higher speeds were not obtained for some formulations, as shown in Table 7, the statistical regression of these data was not possible. However, it is possible to infer that the increase in the PAC LV content acts predominantly on the rheological behavior of the formulations, since very high readings, which exceeded the capacity of the equipment, were verified for all formulations with the maximum content of this additive, including formulation F0, which was prepared without the addition of palygorskite. A similar behavior was described by Al-Hameedi et al. [42] with a fluid containing bentonite. The authors observed substantial increases in the viscosity and yield point of the fluids as the PAC LV content increased, with the highest concentration of the polymer (4% w/w) resulting in values higher than the reading capacity of the equipment used.
On the other hand, when comparing formulations F1 and F2 with the same content of PAC LV (4 g) and 10 and 20 g of palygorskite, respectively, it is noted that the addition of a higher clay content results in increases in the value of all the rheological parameters analyzed. This behavior is due to the mechanism by which palygorskite acts as a viscosifying agent, since the length of the fibers and the number of silanol groups on the surface of the particles help to aggregate the fibers and form a random network that traps water, increasing the viscosity of the suspensions [43].
The increase observed in the rheological parameters, attributed to the interaction between the PAC LV and palygorskite particles and, above all, to the increase in PAC LV content, demonstrated, preliminarily, a positive aspect of these formulations, since this behavior minimizes the solid sedimentation of the fluids. This was confirmed by the homogeneous appearance of the fluid F4 (Figure 4), which was prepared with the maximum content of PAC LV and palygorskite, after resting at room temperature for 10 days, with no apparent solid sedimentation.
It is also worth highlighting that the substantial increases in the values of rheological parameters observed for this formulation (F4) do not represent a limitation regarding its use in well abandonment operations when considering a possible overload during its pumping, since in this type of operation, the fluid is not continuously recirculated in the well, as it happens during drilling operations. Therefore, based on the analysis of filtrate volume results and rheological behavior, as well as considering the implications of these parameters on the operational requirements of the abandonment operation, the fluid prepared with a higher content of PAC LV and palygorskite (F4) showed the most promising behavior for application as a barrier element, presenting a smaller filtrate volume and capacity to maintain solids in suspension for 10 days, which guarantees the maintenance of the hydrostatic pressure of the fluid column for temporary abandonment operations.
The pH and density values, in lb/gal, of the palygorskite formulations are presented in Table 8.
In general, regardless of the formulations, the fluids presented a basic pH, with a range of values between 12.69 and 13.87. Furthermore, it is possible to observe a slight influence of the palygorskite content on this property, since the formulations without palygorskite (F0) and with the lowest content of this clay (F1 and F3) presented the highest pH values, and the formulations with the highest content (F2 and F4) presented the lowest values. A similar trend was observed by Santanna et al. and Choupani et al. [17,44], in which palygorskite suspensions in salt water had their pH values slightly reduced with increasing clay concentrations.
Regarding the density of the fluids, the results demonstrated that there was no variation considered significant in this property, with values between 9.4 and 9.6 lb/gal. Considering the application of the palygorskite fluids as barrier elements for well abandonment, it is possible to predict that the density values observed are suitable for the operational window of most of the wells to be abandoned, since they are, in their majority, depleted. For wells whose operational window requires higher densities, it is possible to meet this requirement using more concentrated brines or the addition of weighting agents to the formulation.
Finally, it is important to emphasize that this study focused on developing a fluid formulation considered promising for the temporary abandonment of petroleum wells, with properties suitable for maintaining hydrostatic pressure. However, further testing is required to assess its performance under field conditions, considering the time and temperature to which it will be exposed to throughout the operation.

4. Conclusions

This work aimed to develop a salted water-based fluid with added palygorskite to be used as a liquid well barrier for the temporary abandonment of petroleum wells. The characterization of the clay showed that the studied sample has a chemical composition that is characteristic of palygorskite extracted from Greece. In the XRD analysis, the minerals palygorskite, antigorite, and quartz were identified, with the first being the predominant clay mineral, presenting a percentage of 77.9% in the mineralogical composition. The presence of this clay in the composition of the studied formulations contributed to the improvement of filtrate control, although the sample morphology was not considered suitable for this property. Furthermore, among the seven formulations prepared from the factorial design, with varying amounts of palygorskite and PAC LV, the fluid prepared with the maximum concentration of these additives (20 and 8 g/350 mL, respectively) presented the most satisfactory performance, since it ensured the lowest filtrate volume and did not demonstrate a tendency for solids sedimentation. Finally, the highlighted formulation was considered efficient, compared to others found in the literature that use this type of clay, as it provides optimized properties using a simplified and low-cost formulation. This study therefore attests that a salted water-based fluid with palygorskite constitutes a highly promising alternative for application as a liquid barrier element in the temporary abandonment of petroleum wells.

Author Contributions

Conceptualization, L.V.A.; methodology, R.L.d.N.G., A.C.A.C., W.R.P.d.C. and L.R.C.d.O.; software, T.A.d.O. and M.B.; validation, T.A.d.O. and M.B.; formal analysis, L.V.A. and R.C.A.d.M.N.; investigation, R.L.d.N.G., A.C.A.C., W.R.P.d.C., L.R.C.d.O. and M.C.d.S.L.; resources, L.V.A. and R.C.A.d.M.N.; data curation, L.V.A. and T.A.d.O.; writing—original draft preparation, R.L.d.N.G. and K.C.N.; writing—review and editing, L.V.A. and M.B.; visualization, R.L.d.N.G. and K.C.N.; supervision, L.V.A.; project administration, L.V.A. and R.C.A.d.M.N.; funding acquisition, L.V.A. and R.C.A.d.M.N. All authors have read and agreed to the published version of the manuscript.

Funding

This research was funded by PETROBRAS, grant number 0050.0120134.21.9.

Institutional Review Board Statement

Not applicable.

Informed Consent Statement

Not applicable.

Data Availability Statement

The original contributions presented in this study are included in the article. Further inquiries can be directed to the corresponding author.

Conflicts of Interest

The authors declare no conflicts of interest.

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Applsci 15 02980 g001
Figure 1. X-ray diffractogram of the palygorskite sample. P—palygorskite; A—antigorite; Q—quartz.
Figure 1. X-ray diffractogram of the palygorskite sample. P—palygorskite; A—antigorite; Q—quartz.
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Figure 2. Morphology of the palygorskite sample.
Figure 2. Morphology of the palygorskite sample.
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Figure 3. Response surface (a) and values (b) of the HPHT filtrate volume of the salted water-based fluid with palygorskite.
Figure 3. Response surface (a) and values (b) of the HPHT filtrate volume of the salted water-based fluid with palygorskite.
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Figure 4. Appearance of the fluid F4 (in triplicate) after resting at room temperature for 10 days.
Figure 4. Appearance of the fluid F4 (in triplicate) after resting at room temperature for 10 days.
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Table 1. Factorial design matrix for salted water-based fluid with palygorskite.
Table 1. Factorial design matrix for salted water-based fluid with palygorskite.
ExperimentPAC LV ContentPalygorskite Content
F1−1−1
F2−1+1
F3+1−1
F4+1+1
F500
F600
F700
Table 2. Coding of PAC LV and palygorskite content levels.
Table 2. Coding of PAC LV and palygorskite content levels.
Levels
Variables−10+1
PAC LV content, g/350 mL468
Palygorskite content, g/350 mL101520
Table 3. Chemical composition of the palygorskite sample.
Table 3. Chemical composition of the palygorskite sample.
OxidePercentage (%)
Al2O35.70
SiO250.97
Fe2O313.11
MgO16.22
Other Oxides2.08
Table 4. Quantification of phases identified in XRD analysis.
Table 4. Quantification of phases identified in XRD analysis.
PhasePercentage (%)
Palygorskite77.90
Antigorite20.94
Quartz1.16
Table 5. Analysis of variance for the HPHT filtrate volume of the salted water-based fluid with palygorskite.
Table 5. Analysis of variance for the HPHT filtrate volume of the salted water-based fluid with palygorskite.
Coefficient of Determination (R2)Fcalculated/Ftabulated
97.18%9.95
Table 6. Performance of palygorskite drilling fluids regarding filtrate control.
Table 6. Performance of palygorskite drilling fluids regarding filtrate control.
AuthorFormulationTest MethodSummary of Results
Zou et al. [39]400 mL of fresh water + 4% of salt + 6.4% of palygorskite + Variable content of PAC or Xanthomonas Compestris PolymerAPI filtrate volume *FVAPI between 26.2 and 163.8 mL
Santanna et al. [17]Water + palygorskite + Hydroxypropylamnine + PAC + NaCl + cationic Polymer + triazine + MgO + calcium carbonate + lubricantAPI filtrate volume *FVAPI between 3.9 and 6.0 mL
Wei et al. [40]water + 1.5 wt% composite bentonite + 1.5 wt% palygorskite + 3 wt% KCl + 3 wt% Nano-SiO2-1 + 0.4 wt% MMH-1 (Mixture of metal hydroxides) + 2 wt% DFD (modified starch) + 0.3 wt% LV-CMC + 0.3 wt% LV-PAC + 0.05 wt% FC-1 (fluorocarbon surfactant) + 0.01 wt% PTEE-1 (polytetrafluoroethylene) + 0.1 wt% OS-1 (silicone surfactant) + 3 wt% polymeric alcohol + 0.1 wt% NaOHAPI filtrate volume *FVAPI = 7.2 mL (room temperature)
FVAPI = 6.8 mL (after aging for 16 h at 120 °C)
Lijuan et al. [41]2.5% base mud + 0.4% NaOH+ 0.1% ZDP-1 (polymer anti-salt calcium and temperature resistance) + 8% SMP-3 (resin filter loss reducer) + 2% SPNH (lignite filter loss reducer) + 3% ZDF-1+ 2% ZDGF (blocking) + 30% NaCl + 0.3% CaO + 1.5% CaCO3 (2800 mesh) + 4% white oil + 0.4% Span-80 + barite + 1.5% SF260 (viscosity reducer)HPHT filtrate volume11 mL
* Filtration carried out at room temperature, with a pressure of 100 psi.
Table 7. Readings obtained from the Fann 35A viscometer for the salted water-based fluid with palygorskite.
Table 7. Readings obtained from the Fann 35A viscometer for the salted water-based fluid with palygorskite.
FormulationL600L300L200L100L6L3μa (cP)μp (cP)YP (lb/100 ft2)
0*2391951342315***
19663483032483330
211578603753583741
3**2541803522***
4***2305034***
5237168136901481196999
62331671349014811766101
7227161129861381146695
* Values not determined as the equipment’s reading capacity was exceeded.
Table 8. pH and density values for the studied formulations of the salted water-based fluid with palygorskite.
Table 8. pH and density values for the studied formulations of the salted water-based fluid with palygorskite.
F0F1F2F3F4F5F6F7
pH13.8713.4313.0413.3712.6913.1813.2713.32
Density (lb/gal)9.49.49.69.59.69.59.59.5
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Gonçalves, R.L.d.N.; Costa, A.C.A.; Lima, M.C.d.S.; Nóbrega, K.C.; da Costa, W.R.P.; Oliveira, L.R.C.d.; Nascimento, R.C.A.d.M.; Barros, M.; Oliveira, T.A.d.; Amorim, L.V. A New Application for Salted Water-Based Fluids with Palygorskite: Formulation Designing for Temporary Plug and Abandonment Operations of Petroleum Wells. Appl. Sci. 2025, 15, 2980. https://doi.org/10.3390/app15062980

AMA Style

Gonçalves RLdN, Costa ACA, Lima MCdS, Nóbrega KC, da Costa WRP, Oliveira LRCd, Nascimento RCAdM, Barros M, Oliveira TAd, Amorim LV. A New Application for Salted Water-Based Fluids with Palygorskite: Formulation Designing for Temporary Plug and Abandonment Operations of Petroleum Wells. Applied Sciences. 2025; 15(6):2980. https://doi.org/10.3390/app15062980

Chicago/Turabian Style

Gonçalves, Ruth Luna do Nascimento, Anna Carolina Amorim Costa, Mário César de Siqueira Lima, Karine Castro Nóbrega, Waleska Rodrigues Pontes da Costa, Laura Rafaela Cavalcanti de Oliveira, Renalle Cristina Alves de Medeiros Nascimento, Michelli Barros, Tiago Almeida de Oliveira, and Luciana Viana Amorim. 2025. "A New Application for Salted Water-Based Fluids with Palygorskite: Formulation Designing for Temporary Plug and Abandonment Operations of Petroleum Wells" Applied Sciences 15, no. 6: 2980. https://doi.org/10.3390/app15062980

APA Style

Gonçalves, R. L. d. N., Costa, A. C. A., Lima, M. C. d. S., Nóbrega, K. C., da Costa, W. R. P., Oliveira, L. R. C. d., Nascimento, R. C. A. d. M., Barros, M., Oliveira, T. A. d., & Amorim, L. V. (2025). A New Application for Salted Water-Based Fluids with Palygorskite: Formulation Designing for Temporary Plug and Abandonment Operations of Petroleum Wells. Applied Sciences, 15(6), 2980. https://doi.org/10.3390/app15062980

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