Silane Coupling Research Articles

Progress in Application of Silane Coupling Agent for Clay Modification to Flame Retardant Polymer.

Polymer composites are widely used in various fields of production and life, and the study of preparing environmentally friendly and flame retardant clay/polymer composites has gradually become a global research hotspot. But how to efficiently surface modify clay and apply it to the field of flame retardant polymers is still a potential challenge. One of the most commonly used surface modification methods is the modification of clay with silane coupling agents. The hydrolysable groups of the silane coupling agent first hydrolyze to generate hydroxyl groups. These hydroxyl groups then undergo a condensation reaction with the hydroxyl groups on the surface of the clay, allowing for organic functional groups to be grafted onto the clay surface. The organic functional groups and polymer matrix react to generate chemical bonds so that the composite material's interface is more closely combined. Thus, the dispersion of clay in the organic polymer material and the compatibility of the two is better, which improves the flame retardant effect of the composite material. This paper introduces the classification of a silane coupling agent and the mechanism and process of silane coupling agent-modified clay, outlines the mechanism of silane coupling agent-modified clay flame retardant polymers, reviews the research results on flame retardant polymers of various clays after surface treatment with silane coupling agents in recent years, and highlights the synergistic flame retardant effect of clay and flame retardant organized by silane coupling agents. Finally, it is found that the current research in the field of silane coupling agent-modified clay in flame retardants is focused on the modification of montmorillonite, sepiolite, attapulgite, and kaolinite by KH-550, KH-560, and KH-570, and the development trends in this field are also prospected.

Mechanical Properties and Crystallinity of Specific PLA/Cellulose Composites by Surface Modification of Nanofibrillated Cellulose.

Polylactic acid (PLA) has inherent drawbacks, such as its amorphous structure, which affect its mechanical and barrier properties. The use of nanofibrillated cellulose (NFC) mixed with PLA for the production of composites has been chosen as a solution to the above problems. A PLA/NFC composite was produced by solution casting. Before use, the cellulose was modified using a silane coupling agent. The composite films were investigated via X-ray diffraction, as well as by mechanical, physical, thermal analyses and by differential scanning calorimeter. The crystallinity was four times that of pure PLA and the water vapor transmission rate decreased by 76.9% with the incorporation of 10 wt% of NFC. The tensile strength of PLA/NFC blend films increased by 98.8% with the incorporation of 5 wt% of NFC. The study demonstrates that the addition of NFC improved the properties of PLA. This provides a solid foundation for the enhancement of the performance of PLA products.

Preparation of PdNi bimetallic loaded amino modified porous carbon material catalyst based on chitosan and its applications

The utilization efficiency of palladium-based catalysts has sharply increased in many catalytic reactions. However, numerous studies have shown that preparing alloys of palladium with other metals has superior catalytic activity than pure palladium. Additionally, hierarchical porous carbon has gradually developed into an excellent carrier for loading bimetallic nanoparticles. In this study, we firstly pyrolyzed chitosan, sodium bicarbonate and nickel nitrate to create highly dispersed porous carbon materials doped with Ni NPs. The carbon materials were then grafted with silane coupling agent (APTMS) to afford them with amino groups on the surface. Taking advantage of the fact that Pd2+ can react with Ni in spontaneous reduction reaction, Pd was deposited on the surface of Ni to produce PdNi bimetallic-loaded carbon catalysts containing amino groups. The resulting catalysts were examined by a series of characterizations and were found to have a hierarchically porous structure and large specific surface area, which increased the number of active sites of the catalysts. In comparison to other Pd catalysts, the PdNi/HPCS-NH2 catalysts displayed remarkable activity for Suzuki coupling reaction and hydro reduction of nitroaromatics, which exhibited a high turnover frequency value (TOF) of 37,857 h−1 and 680.9 h−1, respectively. These were mainly due to the high dispersion of the PdNi NPs and the superior structure of the carriers. Moreover, the catalysts did not experience a significant decline in activity after ten cycles. All in all, this investigation has created a new approach for the fabrication of novel carriers for Pd catalysts, which is in line with the concept of green chemistry and recyclable.

Application of low‐molecular‐weight polyethylene glycol‐modified silica in natural rubber composites

AbstractSilica serves as the primary filler in the fabrication of eco‐friendly tires, and achieving an optimal dispersion of polar silica within the natural rubber matrix is crucial for crafting high‐performance rubber composites. In this study, biodegradable surfactants polyethylene glycol (PEG) with molecular weights of 200, 400, and 800 were employed to modify silica. The modified silica was characterized by Fourier‐transform infrared spectroscopy; PEG‐modified silica with different molecular weights was compounded with Si69, a conventional silane coupling agent, in the formulation. This aimed to reduce Si69 dosage and mitigate the emission of volatile organic gases, such as ethanol, generated during the silanization reaction between Si69 and silica. Experimental findings revealed that compared with natural rubber composites containing six parts of Si69, the addition of PEG‐modified silica enhanced filler dispersion in the composite while reducing Si69 dosage by three parts. This led to accelerated vulcanization rates, effectively decreased energy consumption during production, and significantly improved wet slip resistance, while maintaining optimal rolling resistance. Rubber composites prepared with PEG800‐modified silica exhibited a 10% increase in elongation at break, a 12% increase in tensile product coefficient, and a 19% enhancement in wet slip resistance.Highlights Silica is modified by polyethylene glycol with molecular weight of 200, 400, and 800. The amount of silane coupling agent and VOC emissions are reduced. The interfacial bonding between silica and rubber matrix is enhanced. The tensile product coefficient and wet slip resistance are improved by 12% and 19%.

Flame-retardant coatings with ultraviolet resistance by doping KH-560 modified nano-silica into Na2SiO3/NaOH-activated copper tailings geopolymer

Copper tailings (CTs) are the industrial waste that causes resource wastage and pollution issues; recycling approaches of CTs remain challenging and are worth exploring. Herein, the Na2SiO3/NaOH-activated CTs geopolymer coating is prepared by doping melamine polyphosphate (MPP), aluminum diethyl phosphate (ADP), and nano-silica modified by silane coupling agent KH-560 (KH-560@nano-silica). The flame retardancy and ultraviolet (UV) aging resistance of the coating are evaluated through various techniques. Cone calorimeter results indicate that 4 wt% KH-560@nano-silica reduces the peak heat release rate from 84.84 to 43.98 kW·m−2 and increases the flame retardancy index from 1.00 to 6.60. Moreover, 4 wt% KH-560@nano-silica diminishes the degree of decline in flame retardancy of the coating after UV aging by 63.02 %. Thermogravimetric analysis shows that 4 wt% KH-560@nano-silica increases the temperature of 5 % weight loss and 30 % weight loss of the coatings by 42.93 % and 60.99 %, respectively. Furthermore, microscopic analysis indicates that nano-silica and the catalytic charring of CTs and flame retardants contribute to forming dense and continuous residue. According to a three-dimensional diffusion model, the activation energy (Eα) increases from 154.69 to 171.94 kJ·mol−1 at 717 ∼ 987°C. Meanwhile, the coating exhibits a formaldehyde adsorption rate of 61.79 %. In conclusion, this study expands the application scope of inorganic geopolymers in the flame-retardant industry, offering a new strategy for the high-value recovery and utilization of CTs.

Dual surface-modification by oleic acid and epoxy-based silane coupling agent providing cerium oxide nanoparticles as additive in pentaerythritol oleate with improved high-temperature adsorption performance and tribological properties

An epoxy-based silane coupling agent (KH560) was grafted onto the surface of oleic acid-modified cerium oxide (CeO2-OA) nanoparticles in order to improve the competitive adsorption ability of the anti-wear additives in ester oils and simultaneously hinder the additive desorption owing to thermal disturbance under high-temperature condition. The as-prepared oleic acid-epoxy silane co-modified cerium oxide (CeO2-OA/E) nanoparticles were characterized. The effect of temperature on the adsorption behavior of trityl phosphate (TCP, a commercial high-temperature antifriction agent), CeO2-OA and CeO2-OA/E in PETO was studied using a dissipative quartz microbalance. Their tribological properties as the additives in pentaerythritol oleate (PETO), a polar ester base oil, were evaluated with a four-ball machine and a ball-on-block friction and wear tester; and their tribomechanism was explored with respect to their adsorption behavior on rubbed steel surfaces at elevated temperatures. It was found that the secondary surface-capping of CeO2-OA by the KH560 silane coupling agent resulted in great increases in the surface potential (from 54 mV to 396 mV) and thermal stability as well (the thermal decomposition temperature rose from 185 °C to 254 °C). Among the tesetd lubricant additives, CeO2-OA/E exhibited the highest adsorption mass, because of the highest surface potential the chemisorption ascribed to the epoxy group of the silane coupling agent. Particularly, CeO2-OA/E added in PETO exhibited better friction reduction and anti-wear properties at 150 °C than CeO2-OA and TCP, because CeO2-OA/E added in PETO formed tribofilm composed of CeO2 and SiO2 with excellent thermal stability as well as friction-reduction and antiwear effects through stable chemical adsorption and tribochemical reaction at elevated temperatures.

Horn sheath-inspired lightweight composites with enhanced impact resistance

The natural Caprinae horn sheaths possess excellent mechanical properties due to the synergistic effects of the porous and corrugated lamellar structure. However, research on bioinspired designs based on this structure remains absent. In this work, we attempted to integrate hollow glass microspheres modified by silane coupling agents into A. pernyi silk fabric, and finally fabricate a horn sheath-inspired composite using the vacuum-assisted resin transfer molding. The impact strength of the horn sheath-inspired composite reaches up to 150 kJ m-2 with a low density of 1290 kg m-³. Fracture morphology analysis and finite element simulation confirmed the toughening mechanisms, including crack deflection and interfacial bonding due to the synergistic effects of the porous structure and the corrugated silk fabrics. This study provides a bioinspired strategy to lightweight and tough composites, with significant potential in impact-critical applications.

Properties of EPDM Nanocomposites Reinforced with Modified Montmorillonite.

Considering the dilemma of obtaining economic and high-performance composites based on non-polar and main-chain-saturated ethylene propylene diene monomer rubber (EPDM), we proposed an effective and universal filler modification and nanocomposite preparation method. Specifically, the montmorillonite (MMT) surface was coated with polydopamine (PDA) to obtain DMMT, which was confirmed by XRD, XPS, FTIR, and TGA. After compounding DMMT gel with the solid EPDM via the gel compounding method, a silane coupling agent, vinyltrimethoxysilane, was introduced to construct covalent interactions between rubber and filler. Compared with the unmodified MMT filler EPDM, the EPDM/DMMT nanocomposite showed much fewer filler aggregates in the matrix. The highest tensile strength of the composites reached 6.5 MPa with 10 phr DMMT, almost 200% higher than that of pure EPDM.

Achieving the hydrophobic alteration by functionalized nano-silica for improving shale hydration inhibition

Shale hydration is the primary cause of wellbore instability during drilling processes. In this study, two non-fluorinated silane-coupling agents, octyltriethoxysilane (OTES) and (3-Aminopropyl) triethoxysilane (APTES), were grafted onto the nano-silica surface to develop a hydrophobic material (SHM). Various performance characterizations, including infrared spectroscopy, thermogravimetric analysis, surface tension, wetting alteration, capillary self-suction height, bentonite expansion, and shale dispersion, were employed to investigate the shale inhibition properties of SHM comprehensively. Experimental results revealed that SHM could significantly improve shale hydration inhibition. For instance, in a 2 % SHM liquids, the shale hot rolling recovery rate increased from 25.39 % to 83.78 %, and the bentonite expansion height decreased from 7.65 mm to 2.80 mm. The inhibition performance was notably superior to potassium chloride (KCl) and polyether amine (PEA). Inhibition mechanisms analysis unveiled that the outstanding inhibitory effect of SHM was achieved through electrostatic adsorption, wettability alteration, and surface tension reduction. Firstly, SHM contained numerous amine groups that could demonstrate strong adsorption on the clay surface through electrostatic and hydrogen bonding interactions. Secondly, with long hydrophobic alkyl chains, it formed a highly hydrophobic film enveloping the shale surface, effectively preventing water from invading. Thirdly, it reduced liquid surface tension, further minimizing the water infiltration. As a result, the use of SHM significantly enhanced shale hydration inhibition during the shale drilling process.

Improvement of interfacial adhesion of aramid fiber/polycarbonate composites by surface modification with graphene oxide modified sizing agents

AbstractVarious sizing agents were prepared to enhance the interfacial properties between aramid fiber (AF) and polycarbonate (PC), as well as to enhance the mechanical properties of AF/PC composites. It was found that PC sizing agent, P‐GO sizing agent, and PSi‐GO sizing agent effectively coated the surface of AF from the FTIR and XPS and SEM results. The IFSS and mechanical properties of composites reinforced with fibers treated by the sizing agents exhibited significant improvement, as well as their single fiber tensile strength also improved. Specifically, when AF was treated with PSi‐GO sizing agent, the interfacial shear properties between AF and PC increased by a remarkable 78.69%, reaching 22.89 MPa compared to the original AF/PC composite, the tensile strength of the single‐filament exhibited an increment of 12.4% to 26.4 cN/dtex. Moreover, the tensile strength, flexural strength, and impact strength of the composite increased by 5.43%, 77.74%, and 54.71%, respectively. These improvement can be attributed to the GO with a higher concentration of chemical groups and excellent dispersion with modified with the silane agent. These findings suggest that coating the AF with sizing agents can effectively enhance its interfacial adhesion with the matrix, which is useful for its application as the reinforcement in the composites.Highlights Adding GO to the sizing agent to change the Aramid fabric surface properties. Silane coupling agent was used to improve the dispersion of GO on the fiber surface. GO modified sizing agent can improve the flexural strength, tensile strength, and interlaminar shear strength of the composites.

Mechanical Properties of Ultra-High-Performance Concrete with Amorphous Alloy Fiber: Surface Modification by Silane Coupling Agent KH-550.

Amorphous alloy fiber has the advantages of high tensile strength and high corrosion resistance compared with steel fiber, but its interfacial bonding with cement matrix is poor and requires surface modification treatment. In this study, the surface modification of amorphous alloy fiber was carried out by using silane coupling agent KH-550 solution, and its effect on the mechanical properties of ultra-high-performance concrete was investigated. The results showed that the amorphous alloy fibers modified with 15% concentration silane coupling agent KH-550 solution can effectively improve the mechanical properties of the ultra-high-performance concrete, where the interfacial bond strength with the cement matrix reached 3.29 MPa and the roughness reached 3.85. The compressive strength, flexural strength, tensile strength, and peak stress of the ultra-high-performance concrete mixed with modified amorphous alloy fibers could reach up to 133.6 MPa, 25.5 MPa, 8.32 MPa, and 114.26 MPa, respectively, which were 2.9%, 6.3%, 10.9%, and 4.3% higher than those of the ultra-high-performance concrete with unmodified amorphous alloy fibers. As the surface of the fiber was modified, its properties changed and the bonding effect with the cement matrix was better, which in turn improved the mechanical properties of the ultra-high-performance concrete.

Effectiveness of a silane coupling agent in a resin luting cement

The objective of this study was to investigate a new silane-containing self-adhesive resin luting cement with both shear bond strength and contact angle studies to determine if silane in a resin cement would chemically bond to a lithium disilicate surface. The silane-containing cement, Panavia SA Cement Universal (Kuraray, Tokyo, Japan) was tested against a control case where a traditional silane treatment was paired with resin-luting cement, Duo-Link Universal (Bisco Inc., Schaumburg, IL, USA) with immediate shear bond strength testing on both polished and etched lithium disilicate, as well as after thermocycling. It was determined that micromechanical retention provided a substantial contribution to bond strength. However, after an aging study with 20,000 thermocycles and then storage for 6 months in 37 °C water, the silane-containing, self-adhesive resin cement significantly decreased in shear bond strength when compared to the control. From contact angle studies, while it was shown that the paste containing the silane did effectively increase hydrophobicity of the treated lithium disilicate surface, it required over 3 h contact time, which was not representative of clinical use.

Composite silica aerogel based on HNTs-modified APP with enhanced thermal insulation and flame retardancy performance for organosilicon resin

Efficient thermal insulation and flame-retardant materials are crucial in reducing energy consumption and minimizing fire hazards. This work presents a novel method for preparing a composite aerogel: a silane coupling agent was used as a chemical bridge to synthesize a new flame retardant AKH (modified APP with HNTs). AKH was incorporated into the silica sol to fabricate the SA-AKH composite aerogel. SA-AKH features a dense three-dimensional network skeletal structure, excellent thermal stability, and a high specific surface area. When integrated into organosilicon resin, SA-AKH significantly enhances the flame resistance of composite materials. During cone calorimetry testing (CCT), SSAKH4 exhibited a peak heat release rate (PHRR) of 281.88 kW/m2 and total smoke production (TSP) of 5.52 m2, representing a decrease of 30.8 % and 4.5 %, respectively, compared to SSA4. The composite material, derived from the unique mesoporous structure of aerogel combined with the flame retardant and hollow characterization of AKH, demonstrates exceptional flame retardancy and smoke suppression. SA-AKH is expected to make novel advancements in the field of high-efficiency insulation and flame-resistant composites.

Bionic repair protective coatings with high toughness and bond strength based on anionic waterborne polyurethane-modified cement

Protection and repair of surface cracks play pivotal roles in enhancing their effective service life. Inspired by the bionic shell principle, an anionic waterborne polyurethane (WPU) was designed. The Synthetic WPU was applied to sulphoaluminate (SAC) and ordinary Portland (OPC) cements to prepare composite coatings. The results showed that with the increase in polymer-to-cement ratio (P/C), attributable to the electrostatic adsorption and complexation of R-COO-, the content of CH, AH3 and AFm increased, while the content of AFt decreased due to the inhibitory effect of WPU on hydration reactions. The molecular dynamics model indicated that the oxygen atoms in WPU can not only form ion pairs with Ca2+ in AFt but also form strong hydrogen bonds with the H in the hydroxyl group of AFt and the H in water molecules. Hence, for P/C exceeding 10 %, combined with Flory-Huggins theory, a continuous interpenetration polymer network (IPN) comprising multiphase composites was successfully demonstrated, bolstered by the macromolecular structure composed of —OH, —COOH, Ca2+ and Al3+ serving as a bridge. The network was more pronounced in coatings with SAC than in those with OPC due to synergistic effects caused by rapid hydration reactions. Due to the presence of IPN and the Si-O-Si bonds caused by the hydrolysis condensation reaction of silane coupling agent, the tensile and bond strengths exhibited an upward trend with increasing P/C, surging by up to 326 % and 180 %, respectively. The value reached 6.81 MPa and 2.2 MPa. And the addition of WPU enhanced crack resistance.

Long-Term Bonding Performance of One-Bottle vs. Two-Bottle Bonding Agents to Lithium Disilicate Ceramics.

The aim of this study was to compare the long-term bonding performance to lithium disilicate (LDS) ceramic between one-bottle and two-bottle bonding agents. Bonding performance was investigated under these LDS pretreatment conditions: with hydrofluoric acid (HF) only, without HF, with a two-bottle bonding agent (Tokuyama Universal Bond II) only. Shear bond strengths between LDS and nine resin cements (both self-adhesive and conventional adhesive types) were measured at three time periods: after one-day water storage (Base), and after 5000 and 20,000 thermocycles (TC 5k and TC 20k respectively). Difference in degradation between one- and two-bottle bonding agents containing the silane coupling agent was compared by high-performance liquid chromatography. With HF pretreatment, bond strengths were not significantly different among the three time periods for each resin cement. Without HF, ESTECEM II and Super-Bond Universal showed significantly higher values than others at TC 5k and TC 20k when treated with the recommended bonding agents, especially at TC 20k. Difference in degradation between one- and two-bottle bonding agents containing the silane coupling agent was compared by high-performance liquid chromatography (HPLC). For both cements, these values at TC 20k were also not significantly different from pretreatment with only Tokuyama Universal Bond II. For LDS, long-term bond durability could be maintained by pretreatment with Tokuyama Universal Bond II instead of the hazardous HF.

Graphite Oxide-Based Coatings on ZK60A Magnesium Alloy: Effect of Chitosan and Silane Coupling Agents on the Corrosion Resistance

Graphite Oxide-Based Coatings on ZK60A Magnesium Alloy: Effect of Chitosan and Silane Coupling Agents on the Corrosion Resistance

Design of a double-layered material as a long-acting moisturizing hydrogel-elastomer and its application in the field protection of elephant ivories excavated from the Sanxingdui Ruins.

The sudden change in the environment from a dark, low-oxygen, low-temperature, high-humidity underground stable environment to an environment with much-improved temperature and humidity, a high oxygen content, enhanced light exposure, and increased harmful organisms has greatly affected the stability of the ivory unearthed from the Sanxingdui site. Therefore, the implementation of an effective emergency protection strategy for ivory excavated at Sanxingdui is imperative and urgently needed. However, the current gauze technique used at many archaeological sites suffers from short timescales, poor transparency of the material, and susceptibility to reverse osmosis of the ivory. Therefore, in this study, a transparent poly(acrylamide-acrylic acid) (P(AM-AA)) hydrogel-poly(dimethylsiloxane) (PDMS) elastomer bilayer was designed for the effective protection of excavated ivory. In this system, a hydrophobic PDMS elastomer was constructed on the surface of the hydrogel by the introduction of a silane coupling agent to inhibit the loss of water from the hydrogel to the external environment, thus prolonging the preservation of ivory by the protective material. The covalent interface between the hydrogel and the elastomer allowed the double-layer composite to exhibit excellent interfacial bonding. In addition, the double-layer material demonstrated a high mechanical strength of 1.2 MPa and a water binding ratio of ∼31%, which allowed it to form strong hydrogen bonds with the silanol structure. When the hydrogel was placed in an air environment (temperature: 25 °C; relative humidity: 65% RH), the water-retention rate of the double-layer material was still more than 60% after 5 days, thus the double-layer material showed excellent performance. Meanwhile, the double-layer material had a transmittance of more than 90% and exhibited a high degree of transparency, which makes it possible to promptly observe the changes occurring on the surface of the ivory. The combination of the aforementioned properties makes the bilayer a promising material for moisturizing and protecting excavated ivory in situ. Based on these properties, we used the prepared P(AM-AA)/PDMS double-layer material directly for wrapping the K8 ivory with the highest water content at Sanxingdui. The weight retention rate of the ivory was around 70% after 50 days of placement (temperature: 25 °C; relative humidity: 60% RH), the macroscopic morphology did not change significantly and the mechanical properties of the wrapped ivory were basically unchanged, which indicated that the double-layer material has an excellent on-site protection effect on the ivory excavated from Sanxingdui. This work provides new ideas and methods for the temporary conservation of wet heritage.

Mechanical and thermal properties of rice husk/glass fiber/polylactic acid composites

AbstractPolylactic acid (PLA) composites reinforced with rice husk and glass fiber can improve the properties in the aera of the material for vehicle application. In this work, the PLA composite was made and its properties were evaluated using scanning electron microscope (SEM), Fourier transform infrared spectroscopy (FTIR), and thermogravimetric analysis (TGA). SEM observed that the polymer matrix contained a uniform dispersion of 10 wt% rice husks. The tensile strength and bending strength of the composite are 45.8 and 48.2 MPa, respectively, which are 52% and 41% higher than that of the base material PLA. TGA revealed that the thermal stability of the composite deteriorated with increasing rice husk content. The DTG curve indicated that the incorporation of rice husk and glass fiber led to a reduction in the maximum degradation rate of the PLA matrix. As a result, the thermal degradation of the PLA composite exhibited enhanced stability. The average apparent activation energy (Ea) of the composite, determined using the Friedman (FD), Flynn Wall Ozawa (FWO), Starink (ST), and Kissinger (KS) models, falls within the range of 90 to 120 kJ mol−1.Highlights Silane coupling agent was used to improve the interfacial compatibility of fillers. The synergistic action of rice husk and glass fiber fillers enhances the mechanical properties of polylactic acid composites. The mean apparent activation energy (Ea) of the composite was calculated using four models, with values in the range of 90 to 120 kJ mol−1. The Flynn Wall Ozawa and Starink models showed better stability against temperature changes compared to the Friedman model.

High-Strength Controllable Resin Plugging Agent and Its Performance Evaluation for Fractured Formation.

Lost circulation is a common and complicated situation in drilling engineering. Serious lost circulation may lead to pressure drop in the well, affect normal drilling operations, and even cause wellbore instability, formation fluid flooding into the wellbore, and blowout. Therefore, appropriate preventive and treatment measures need to be taken to ensure the safe and smooth operation of drilling operations. So, it is necessary to conduct in-depth research on the development and performance of the plugging materials. In this study, urea formaldehyde resin with high temperature resistance and strength was used as the main raw material, and the curing conditions were optimized and adjusted by adding a variety of additives. The curing time, compressive strength, temperature resistance, and other key performance indexes of the resin plugging agent were studied, and a resin plugging agent system with excellent plugging performance was prepared. The formula is as follows: 25% urea formaldehyde resin +1% betaine +1% silane coupling agent KH-570 + 3% ammonium chloride +1% hexamethylenetetramine +1% sodium carboxymethyl cellulose. The optimal curing temperature is between 60 and 80 °C, with a controllable curing time of 1-3 h. Experimental studies examined the rheological and curing properties of the resin plugging agent system. The results showed that the viscosity of the high-strength curable resin system before curing remained stable with increasing shear rates. Additionally, the storage modulus and loss modulus of the resin solutions increased with shear stress, with the loss modulus being greater than the storage modulus, indicating a viscous fluid. The study also investigated the effect of different salt ion concentrations on the curing effect of the resin plugging system. The results showed that formation water containing Na+ at concentrations between 500 mg/L and 10,000 mg/L increased the resin's curing strength and reduced curing time. However, excessively high concentrations at lower temperatures reduced the curing strength. Formation water containing Ca2+ increased the curing time of the resin plugging system and significantly impacted the curing strength, reducing it to some extent. Moreover, the high-strength curable resin plugging agent system can effectively stay in various fracture types (parallel, wedge-shaped) and different fracture sizes, forming a high-strength consolidation under certain temperature conditions for effective plugging. In wedge-shaped fractures with a width of 10 mm, the breakthrough pressure of the high-strength curable resin plugging agent system reached 8.1 MPa. As the fracture width decreases, the breakthrough pressure increases, reaching 9.98 MPa in wedge-shaped fractures with an outlet fracture width of 3 mm, forming a high-strength plugging layer. This research provides new ideas and methods for solving drilling fluid loss in fractured loss zones and has certain application and promotion value.

Super-hydrophobic ceramic membrane with dense and robust silane grafting for efficient water-in-oil emulsion separation

Separate water from water-in-oil (W/O) emulsions is essential in oil resources recycling and wastewater treatment. Hydrophobic ceramic membranes (HCM) have shown great potential in the dehydration of W/O emulsions but developing high-performance HCM is still a challenge due to the difficulty in hydrophobic modification of ceramic membranes. In this study, an HCM with high grafting density and robust structure was prepared by the grafting silane coupling agent onto an attapulgite (ATP) ceramic membrane. The hexadecyltrimethoxysilane (HDTMS) was chosen for membrane surface modification considering its reaction activity and stability based on molecular dynamic simulation. The effect of the HDTMS contents in the grafting solution and reaction time on the membrane properties were examined. The ATP membrane grafted by HDTMS solution with a content of 9600 ppm for 24 h had a water contact angle of 161° and oil permeability larger than 2207.5 L·m−2·h−1·bar−1 (LMHB). When dealing with W/O emulsions with a water content of 10000 ppm, the steady permeability, permeability recovery ratio, and water rejection of ATP-based HCM was 362 LMHB, 97 %, and 99 %, respectively. Ascribe to the –OH-rich nature of ATP, the performance of HCM in this work is superior to most membranes including Al2O3, ZrO2, and SiC. Hydrophobic-modified ATP provides a new idea for the development of high-performance HCM based on natural mineral ceramics.