3.1. Aspect and Mechanical Properties of Offshore and Onshore Plugs
As shown in
Figure 1, the plugs formed according to the methodology proposed for offshore wells presented very different physical aspects in terms of the type of organic fluid used before hydration. The plug formed by pellets previously immersed in diesel presented a firm and cohesive appearance, while the plugs formed by pellets previously immersed in olefin, showed high fragility and fragmented during demolding.
The fragility of the plug obtained with pellets previously immersed in olefin is probably due to the lower cohesion after hydration in water, since bentonite clay is wettable by olefin, which results in its adsorption and formation of an oily film around the clay particles [
25]. This behavior is further strengthened by the viscosity of the oil phase [
26]. Therefore, since olefin is more viscous than diesel, the oily fraction of this organic fluid is more easily adsorbed by the material, reducing the cohesion of the particles after hydration.
Thus, although olefin and diesel have demonstrated satisfactory results in the displacement of bentonite pellets, based on the swelling potential of the pellets in water after the previous contact with these fluids [
21], the fragility presented by the plug previously immersed in olefin shows that the choice of the appropriate fluid used in this stage of the abandonment operation in offshore wells must necessarily consider the physical aspect and mechanical properties of the plug obtained after swelling.
The plug formed from direct hydration of the pellets in water, following the methodology compatible with onshore operational conditions is shown in
Figure 2 and also presents a firm and cohesive physical appearance.
The graphs presented in
Figure 3 show the results of compressive strength (expressed in terms of force as a function of the height of the specimen) and adhesion for the plug formed by pellets previously immersed in diesel, identified as “offshore plug”, and for the one formed without contact with organic fluids, identified as “onshore plug”. These tests were not performed for the plug formed by pellets previously immersed in olefin due to its high fragility, which made it difficult to obtain test specimens.
Although the interpretation of the results of mechanical properties of bentonite plugs is limited by the absence of technical standards and regulations that specify the requirements for these parameters, it is worth highlighting that the use of these elements in onshore wells, addressed in this study, has reached level 8 of the TRL scale (Technology Readiness Level), and its application is already completed and qualified through testing, so that the mechanical properties presented by the onshore plug are considered as a comparison parameter for the other plugs analyzed.
According to the analysis of
Figure 3(a), it was observed that the onshore plug presented the highest compressive strength, recording a maximum force at the moment of specimen rupture of 51.1N. The offshore plug presented an average force of 28.4N, which represents a reduction around 44%. A similar behavior was observed for the adhesion results, presented in the graph in
Figure 3(b), for which a reduction of 38% is observed for the offshore plug, in relation to the onshore plug.
The reduction in compression resistance for the offshore plug may be related to the adverse effects on the hydration of pellets, resulting from the methodology used to prepare the plug, since diesel, which is hydrophobic, prevents the interaction of bentonite particles with water molecules [
27].
Regarding the reduction observed for adhesion tests, it is worth highlights that this mechanical property is governed by complex factors, including the force that holds the molecules together, which is called cohesion, and the force that keeps the molecules in contact with the substrate surface. For bentonite plugs, interaction with non-polar fluids, such as diesel, is capable of attenuating the cohesion of the material, resulting in a greater propensity for detachment. Furthermore, the lubricating effect of diesel can cause a sliding and slipping effect between the bentonite particles, reducing the friction angle and, therefore, minimizing adhesion [
27].
Although the onshore plug presented higher compression resistance and adhesion, these results do not impair the application of the offshore plug as a barrier element in well abandonment, since the loads to be supported during the operation, and the surfaces (casings or formations) to which the barrier must adhere, are particular for each well. It must be considered when designing the operation, taking into account the operational procedure adopted for the pellets placement and its implications on mechanical properties.
3.2. Aspect and Mechanical Properties of Plugs after Interaction with Formation Waters
The interaction tests with formation waters have also used only offshore (diesel) and onshore plugs, given the low cohesion and integrity of plugs formed from pellets previously immersed in olefin (
Figure 1). However, it was found that the plugs formed by pellets immersed in diesel present low resistance to the formation waters, since after contact with any of the four formulations, they easily fragmented, making it impossible to obtain the specimens to carry out the mechanical tests, as recorded in
Figure 4. In this way, only the plugs obtained from the methodology proposed for onshore wells, with no prior immersion in organic fluids, presented satisfactory integrity even after contact with the formation waters, and made it possible to carry out the mechanical tests.
The visual appearance of the base of the onshore plugs and each formation water, before and after immersion is shown in
Figure 5 and
Figure 6, respectively.
The formation waters that presented the higher salinities (FW2 and FW3) presented also a greater amount of clay particles, while the samples with lower salinities (FW1 and FW4) presented a clearer appearance. This behavior results from the disintegrating action of the ionic environment to the bentonite pellets, since montmorillonite mineral layers are easily infiltrated by cations and it results in volume increasing [
28]. These layers may expand until they break, resulting in the loss of their initial cohesion and disintegration into smaller particles. This process is accelerated by the high salinity of the formation water, which increases the speed of expansion and disintegration of the pellet. Thus, this degradation occurs more markedly for plugs immersed in waters with higher salinity [
23,
29].
Figure 7 shows that, despite the presence of particles in the formation water, the integrity of the plugs was maintained after remove it from the metal mold, and they present a similar appearance to the onshore plug in its initial state.
The maintenance of the physical aspect of the onshore plug, even after contact with the formation waters, is justified by the significant interaction between the particles after hydration, which results in greater cohesion. This behavior attests that the proportion of water and the methodology used for hydration of the pellets was adequate.
After contact with the synthetic formation waters, the plugs have shown an increase in the opening between the metal mold plates (
Figure 8). This behavior demonstrates that there was absorption of formation water during immersion and attests that the infiltration of electrolytes causes an increase in the volume of the clay mineral montmorillonite [
28]. The volume of each formation water absorbed is shown in
Table 2.
As shown in
Table 2, all plugs absorbed part of the formation water during immersion. However, the volume absorbed by the plugs immersed in more saline waters (FW2 and FW3) was slightly greater.
The mechanical properties presented by the onshore plug after contact with the formation waters are shown in
Figure 9.
The compressive strength for each specimen, presented in
Table 3, was obtained from the results presented in the graph in
Figure 9(a).
As shown in
Figure 9(a) and according to the data in
Table 3, the bentonite plugs showed a reduction in compressive strength after immersion in the formation waters. However, even the largest reductions, which are in the order of 13%, observed for the most saline formulations (FW2 and FW3), were not very significant. This behavior highlights the high resistance of the plug to formation fluids and the correlation of this mechanical property with the salinity of the fluid in the subsurface.
The reduction in compressive strength upon contact with formation waters can be attributed to the reduction in expansion and expansion pressure on a macro scale [
30], which can compromise the physical integrity of the plug [
23,
31]. In this way, the salinity of the formation water can adversely affect the resistance of the plug.
Besides compressive strength, the adhesion of plugs in contact with synthetic formation waters was also affected by the presence of electrolytes (
Figure 9(b)), so that plugs in contact with more saline waters presented reduction on this property. The adhesion of the plugs in contact with more saline waters (FW2 and FW3) was approximately 33% and 37% lower, respectively, in relation to the onshore plug, while the adhesion of the plugs in contact with the less saline waters (FW1 and FW4) was approximately 20% and 28% lower, respectively. These results reinforce the correlation between the salinity of the formation water and the mechanical properties of the plug, also observed in the compressive strength test, however, for the adhesion tests the reduction observed is more significant.
The parameters that determine clay resistance are complex and influenced by a series of electrical and chemical interactions between particles [
32], as well as the contact stress interparticle. When particles are close together, the contact stress increases, resulting in a denser and more resistant plug. Therefore, it is important to consider the effect of external tensions which can cause variations in the space between particles and in their orientation, resulting in an imbalance in the electrical forces [
33]. In deep wells, the in-situ condition may improve the mechanical stability of the plugs, as observed previously, when comparing mechanical properties of bentonite plugs on laboratory and large-scale tests [
34]. Thus, it is expected that the loss of integrity presented by offshore plugs and the reduction in the mechanical properties of the onshore plug, observed after the contact with formation waters in laboratory tests, will be much less pronounced under field conditions, ensuring the successful performance of these elements in well abandonment, regardless of the operational procedure used for their placement.