HIGH-PERFORMANCE COMPOSITE MATERIAL FOR HYDROGEN STORAGE APPLICATIONS AND ITS PRODUCTION METHOD.
Patent Information
- Application Number
- TR202603979
- Authority / Receiving Office
- TR · TR
- Patent Type
- Applications
- Current Assignee / Owner
- Filing Date
- 2026-03-17
- Publication Date
- 2026-06-22
Abstract
Description
1 TARIFF HIGH-PERFORMANCE COMPOSITE FOR HYDROGEN STORAGE APPLICATIONS MATERIAL AND ITS PRODUCTION METHOD Technical Area The invention describes the efficient adsorption of hydrogen gas under low temperature and pressure conditions. For this purpose, activated carbon obtained from red plum kernels, palladium (Pd) and agglomeration containing mesoporous silica (MCM-41) and / or microporous NaY zeolite. Preparation and application of a novel composite material with a high surface area that has been prevented. It is related. The invention is particularly useful in the field of hydrogen storage technologies, as it surpasses existing adsorbent materials by 10%. technical issues such as limited capacity, low cycle durability, and agglomeration of metal particles. It offers an innovative composite material that aims to overcome these problems. Pd / active carbon / sodium Y zeolite composite structure, microporous activated carbon and regular crystal structure It is obtained through the synergistic combination of microporous NaY zeolite. Traditionally The activated carbons used have a high surface area and microporosity, enabling physical adsorption. 15 While providing this, mesoporous silicas (e.g., MCM-41) resist hydrogen despite the diffusion advantage. They cannot establish direct chemical interaction; palladium-doped systems, however, can chemically interact. Although suitable for adsorption, the metal particles are not homogeneously distributed and repeat. Performance loss in use constitutes a significant limitation. A development in the present invention... The composite Pd / AC / MCM-41 has a chemical bonding capacity of Pd with hydrogen that is 20 times that of AC. Its microporous structure enables physical adsorption, and MCM-41's regular mesoporous structure... Its form combines a homogeneous metal distribution within an integrated structure. Thus, through the synergistic interaction of both physical and chemical adsorption mechanisms agglomeration of Pd particles while achieving higher hydrogen storage capacity This prevents cyclical stability, improves it, and increases adsorption efficiency even at low temperatures. It has been optimized. This unique structure, within the scope of hydrogen economy, includes fuel cells and portable vehicles. High-performance, sustainable, and environmentally friendly solutions for energy systems and gas purification processes. It offers a user-friendly solution. State of the Art 30 The safe, efficient, and economical storage of hydrogen is crucial for the hydrogen economy. It is of critical importance for its development. Today, activated carbons are used for hydrogen storage purposes. zeolites, mesoporous silicas, metal-organic lattice structures (MOFs), and precious metals 2 Various adsorbent materials are used, such as reinforced nanocomposites and activated carbon. The materials, thanks to their high surface area and microporous structures, facilitate the physical conductivity of hydrogen. While providing a suitable environment for adsorption, their interactions with hydrogen molecules are limited. Because of its level, it exhibits low capacity at room temperature. Zeolites, especially Sodium Y zeolite (NaY) has gas retention properties due to its ion exchange capacity and microporous crystal structure. Although it exhibits this property, it has limited hydrogen adsorption capacity when used alone. Mesoporous silicas, particularly MCM-41, possess regular pore structures and good diffusion. Although their properties provide an advantage in gas transfer, they do not contain chemically active centers. Therefore, it is unable to interact directly with hydrogen. Metal-supported In these systems, palladium-doped structures are particularly suitable for the chemical adsorption of hydrogen. Although it provides a suitable environment, the metal particles are not homogeneously distributed and agglomeration occurs over time. Due to the tendency it exhibits, there is a decrease in surface activity and cyclical performance losses. This occurs. Therefore, current techniques have limited hydrogen adsorption capacity. One-way adsorption based solely on physical or solely chemical adsorption mechanisms. Interaction, uncontrolled growth of metal particles, and performance in reuse 15 Technical problems such as declines are commonly encountered. Furthermore, cyclical stability... low temperature and the need for challenging operating conditions such as high pressure / very low temperature The news is that these materials are used in industrial-scale hydrogen storage applications. It restricts its use. The present invention is designed to overcome these technical limitations using activated carbon, MCM-41 and 20 It presents a unique composite structure that integrates the synergistic properties of palladium. The invention The Pd / AC / MCM-41 composite and Pd / activated carbon / sodium Y zeolite composite included in this scope are activated. The microporous structure of carbon enhances the physical adsorption capacity of MCM-41. homogeneous distribution and ease of diffusion of Pd particles through its mesoporous structure, It combines palladium's ability to form chemical bonds with hydrogen. 25 Thus, the disadvantages of standalone systems are eliminated, both physically and mentally. where chemical adsorption functions simultaneously, agglomeration is prevented, and more a high-performance hydrogen with high surface area and cyclic stability Storage material is obtained. Thanks to this innovative structure, low temperature and pressure Even under these conditions, optimized hydrogen storage capacity is achieved, and energy conversion is 30%. reliable and beyond current techniques for systems and fuel cell applications A sustainable solution is being presented. Patent document US8372369B2 describes a hydrogen spillover method. To increase storage capacity, using metal particles (e.g., Pd, Pt, Ru, Rh, Ni, etc.) a "receiver" material (activated carbon, zeolites – including MCM-41 –, MOF / COF etc.) is collected 35 3 The method of preparation is described. The invention involves preparing the receiving material with a metal salt solution. ultrasonic processing during doping and / or plasma after doping by anticipating processing, creating a chemical barrier between the metal particles and the receiving surface. the formation of bridges, thus atomic structures formed by the dissociation of H₂ on metals. It ensures the efficient transport of hydrogen to the recipient. In the described methods, the metal load is 5 It is generally kept at a level not exceeding 10% of the mass; between processing steps drying / degassing, heat treatment in an inert or H₂ atmosphere, and surface treatment with plasma if necessary. Modification is involved. Isotherm data obtained at room temperature, ultrasonic and plasma. that these processes significantly increase storage capacity by strengthening the spillover effect It shows. 10 Patent document number US20110172087A1 describes a micropore (<2 nm) and nano-channel. Homogeneous metal nanoparticles (<2 nm) into a porous carbon template with a (<2.5 nm) network. By arranging them in this way, it aims to store high levels of hydrogen at room temperature. The method is described. The invention primarily involves the use of a porous template, such as activated carbon, in acid. by adjusting pore sizes through oxidation, creating mesopore channels, 15 then a mixture containing an electrocatalyst precursor (e.g., H₂PtCl₆) and a reducing agent (e.g., ethylene glycol) It describes the process of depositing metal nanoparticles from solution onto pore walls; this architecture, It enables efficient diffusion of atomic hydrogen produced by spillover into micropores. The document states that with proper pore size adjustment and metal placement, ~6% at room temperature and 6.9 MPa is achieved. It was possible to achieve hydrogen retention up to wt., the critical parameters of the method (pore volume, 20 The fractal channel network and reduction conditions have been detailed. Patent document number US20040213998A1 describes a solid-state hydrogen storage system. within this scope, hydrogen storage on mesoporous supports (particularly MCM-41) The discussion focuses on composite storage solutions based on the accumulation of materials. The invention utilizes the hexagonal and non-intersecting channel architecture of the MCM-41 to develop the storage phase (e.g., 25 (metal / alloy / hydride) placement as a thin coating / precipitate into or on the channel, For this, thermal spray (plasma / arc), vapor deposition (sputter / evaporation) or gas phase can be used. It envisages the application of techniques such as concentration. High specific surface area / low A larger active area is obtained on the surface due to the mass advantage, loading / unloading kinetics. It improves; furthermore, the material is placed in cassette / container modules for logistics and safety. 30 A "cassette-based" storage and distribution architecture is described for its use. Patent document US8079464B2 describes a core / shell hydrogen structure. The invention refers to a storage system for hydrogen in the core portion with a high surface area. The shell is made of an absorbent material (activated carbon, zeolite, MOF, aerogel, etc.) and is crystalline and / or It consists of a layer of amorphous metal hydride, and if necessary, an interlayer of amorphous hydride can be added. 35 4 It describes a multi-component architecture in which it is placed. The metal hydride shell catalytically absorbs H₂. By dissociating, it forms channels for the transport of atomic hydrogen to the nuclear sorbent; this This results in a low-energy, rechargeable storage system. The document, different geometries (particle / shell configurations), manufacturing steps (unit storage) (preparation of particles and assembly in the system) and operating conditions 5 It details. Patent document US11072524B2 describes an atomic vacancy without the presence of a metal. from a carbon-based, autocatalytic hydrogen storage material It is mentioned that the invention involves ion beam processing in graphene / nanografene derivative hydrocarbon structures. to produce atomic voids by irradiation and short-term annealing, then high-temperature 10 It describes conditioning the material under filament-activated hydrogen; the resulting “Autocatalytic structure” in hydrogen adsorption, and especially in non-endothermic / even It plays a decisive role in exothermic release behavior. The document also states that specific pressures... storage / release methods within temperature ranges and pressure-temperature control It also describes a storage device architecture. 15 The investigations revealed that the current materials used in hydrogen storage technologies... Despite advantages such as high surface area and porosity, storage capacity is limited in the room. because it remains limited at the specified temperature, and metal nanoparticles cannot be distributed homogeneously. where agglomeration problems arise and in adsorption-desorption cycles It appears that performance losses have become inevitable. Activated carbons are only 20 Because it provides physical adsorption, it shows limited effectiveness except at low temperatures. Mesoporous silicas lack chemically active centers despite their regular pore architectures. Therefore, it cannot directly interact with hydrogen, and in metal-supported systems, the metal... Particle aggregations that occur during loading reduce storage capacity, and This negatively affects cyclical stability. This situation results in high 25 at low pressures and temperatures. developing efficient, long-lasting and reliable storage systems This is a technical deficiency. The present invention aims to provide a solution to these technical shortcomings using palladium. Activated carbon obtained from red plum kernels and MCM-41 mesoporous silica The invention involves the integration of activated carbon in a synergistic composite structure. Its microporous structure enhances physical adsorption, while the regular mesopores of MCM-41... 30 The channels ensure a homogeneous distribution of Pd nanoparticles, preventing agglomeration. Palladium, on the other hand, allows for the chemical adsorption of hydrogen. Furthermore, synthesis... the combined application of ultrasonic dispersion and ethylene glycol reduction techniques in the process, The Pd adheres effectively to the surface and minimizes performance loss over long cycles. This enables the invention to overcome the limited capacity of existing techniques, unstable metal 35 by eliminating problems such as dispersion and low cycle durability in hydrogen storage High capacity, stable performance, and reliable operation under low temperature and pressure conditions. It presents an innovative composite material. Ultimately, the problems mentioned above, which cannot be solved with the current technology, are related to the technical aspects. This has made it necessary to make an innovation in the field. 5 Purpose of the Invention The present invention meets the aforementioned requirements while eliminating all disadvantages. High for hydrogen storage applications, which removes and brings some additional advantages. It relates to a high-performance composite material and its production method. 10 The main purpose of the invention is to address the low capacity of existing materials in hydrogen storage technologies. its main problems such as limited cycle strength and agglomeration of metal particles The goal is to eliminate this. This allows for high performance even under low temperature and pressure conditions. by obtaining a high-performance, stable and long-lasting hydrogen storage system This contributes to the development of the hydrogen economy. 15 One aim of the invention is to examine the capacity of palladium to chemically interact with hydrogen and with activated carbon. its microporous structure and the regular mesoporous form of MCM-41 synergistically combine The goal is to bring them together. Thanks to this integrated structure, both physical and chemical adsorption is possible. By working together, the mechanisms achieve a higher hydrogen storage capacity. One aim of the invention is to investigate the relationship between the crystal structure and micropores of Sodium Y zeolite (NaY) and Pd 20 allowing for homogeneous distribution and ensuring the stability of Pd thanks to its ion exchange capacity. to increase. One aim of the invention is to ensure a homogeneous distribution of Pd particles on the support surface. The aim is to prevent the agglomeration problem. Thus, the active surface area of the metal is preserved, and it can be used again. Performance loss during use is minimized and cyclical stability is increased. 25 Another objective of the invention is to utilize ultrasonic dispersion and ethylene glycol reduction in the synthesis process. The aim is to offer an innovative production method by applying these techniques together. This method, Pd controlled reduction of ions and metal particles on porous structures It enhances the long-term performance of the material by ensuring homogeneous placement. Another objective of the invention is to produce biomass-based activated carbon 30 from red plum kernels. The aim is to offer an environmentally friendly and sustainable hydrogen storage solution through its use. 6 This approach provides both a low-cost production method and advanced utilization of waste biomass. It contributes to its transformation. Another aim of the invention is to enable hydrogen to function effectively in different phases thanks to its multi-porous structure. The aim is to ensure retention. The high surface area provided by micropores and The adsorption rate is increased thanks to the diffusion channels facilitated by the mesopores, and 5 Hydrogen storage capacity is optimized. Another purpose of the invention is for fuel cell systems, portable energy devices, and gas purification. Reliable and high-performance hydrogen storage in energy technologies such as processes. The aim is to provide materials that will enable more efficient, stable, and reliable energy conversion applications. Scalable solutions become possible. 10 All the purposes mentioned above and those that will emerge from the detailed explanation below. The present invention aims to achieve high performance in hydrogen storage applications. It is a method for producing a high-performance composite material and includes the following steps: is; a) Active 15 with a microporous structure obtained by pyrolysis and activation of red plum kernels. Obtaining Carbon (AC), b) Activated carbon and Mesoporous Silica (MCM-41) or Sodium Y Zeolite (NaY Zeolite) dry mixing of powders, c) Preparation of a 0.5% to 2% PdCl₂ solution with palladium (Pd) and deionized water, d) Activated carbon and mesoporous silica or sodium γ-zeolite 20 into ethylene glycol. the mixture is added and placed in an ultrasonic bath at a frequency of 35-45 kHz for 20-60 minutes. mixing, e) After ultrasonic treatment, PdCl₂ solution is added dropwise to the mixture. charging of particles f) Adjusting the pH of the mixture to a range of 9-11 and immersing it in an ultrasonic bath for 5 minutes. being kept waiting for a certain period of time, g) The mixture is heated at a temperature of 100 to 140 °C for a period of 2-5 hours to dissolve ethylene glycol. reduction by h) Separation of the composite formed after reduction by filtration and subsequent drying. 7 All the purposes mentioned above and those that will emerge from the detailed explanation below. The present invention aims to achieve high performance in hydrogen storage applications. It is a high-performance composite material that contributes to the physical adsorption of hydrogen. obtained from red plum kernels through pyrolysis and activation, with a microporous structure. and Activated Carbon (AC) with a high specific surface area, Palladium nanoparticles and 5 Homogeneous distribution of palladium nanoparticles and facilitation of gas diffusion. Mesoporous silica or sodium Y has a regular mesoporous structure to provide this. It contains zeolite. The structural and characteristic features and all the advantages of the invention are given in the figures below. Thanks to the detailed explanation written with references to the figures, it is clearer than ever. 10 This will be understood, and therefore the evaluation should also take these figures and detailed explanations into account. It must be done by taking it. Figures that will help understand the invention. Figure 1 shows the schematic flowchart of the composite material production method, which is the subject of the invention. It is the appearance. Reference Numbers 1. Production of Activated Carbon (AC) 2. Powder mix preparation 20 3. Preparation of the PD solution 4. Ultrasonic dispersion step 5. Addition of Pd solution 6. pH adjustment 7. Reduction step 25 8. Filtering and Drying Step 8 Detailed Description of the Invention This detailed explanation focuses solely on the innovation in the invention to provide a better understanding of the subject. This is explained with examples that will not create any limiting effects. Accordingly, the following: The descriptions and diagrams illustrate high-performance hydrogen storage applications. PdACMCM 41 and Pd / AC / NaY zeolite composite materials are described. 5 The invention describes a high-performance composite material for hydrogen storage applications and This relates to the production method. The production method that is the subject of the invention involves the following process steps: includes; a) Active material with a microporous structure obtained through pyrolysis and activation of red plum kernels. Obtaining carbon (AC), 10 b) Activated carbon and mesoporous silica (MCM-41) or sodium Y zeolite (NaY) dry mixing of powders, c) Preparation of a 0.5% to 2% PdCl₂ solution with palladium (Pd) and deionized water, d) Ethylene glycol mixed with activated carbon and mesoporous silica or sodium Y zeolite The mixture is added and the mixture is placed in an ultrasonic bath at a frequency of 35-45 kHz for 20-60 minutes. mixing, e) After ultrasonic treatment, PdCl₂ solution is added dropwise to the mixture. charging of particles f) Adjusting the pH of the mixture to a range of 9-11 and immersing it in an ultrasonic bath for 5 minutes. being kept waiting for a certain period of time, 20 g) The mixture is heated at a temperature of 100 to 140 °C for a period of 2-5 hours to dissolve ethylene glycol. reduction by h) Separating the composite formed after reduction by filtration and then drying it. In an application of the method described in the invention; in step b) Activated carbon and Mesoporous 25 This involves mixing silica (MCM-41), preferably in a ratio of 1:1 – 1.5:1 by weight. The method described in the invention involves, in step (d), palladium (Pd) and deionized water, preferably 1% PdCl₂. The solution is being prepared. 9 In an application of the method described in the invention; in step d), activated carbon is added to ethylene glycol and an MCM-41 Mesoporous Silica mixture is added and ultrasonically treated in a bath, preferably at 40 kHz. It is mixed at the same frequency every 30 minutes. In one application of the method described in the invention; in step (e), the PdCl₂ solution is added drop by drop to the mixture. This involves adding Pd particles to the droplet at a loading rate of 5 to 15% by weight. 5 In one application of the method described in the invention; step f) the mixture is mixed by adding 2 M NaOH solution. This involves adjusting the pH to a range of 9-11, preferably above 10. The composite obtained in step (h) of the method described in the invention is preferably heated to a temperature of 90 to 120 °C. It is dried for 12-24 hours within this range. This drying is preferably done in an oven. is being carried out. 10 The invention is derived from Pd / AC / MCM 41 composite or Pd / AC / NaY zeolite composite obtained by this method. It is a material. The subject of the invention is a composite material, specifically Pd / AC / MCM 41 composite material, in one application. and to contribute to the physical adsorption of hydrogen from red plum kernels. 15 obtained by pyrolysis and activation, with a microporous structure and high specific surface area. Containing Activated Carbon (AC), Palladium nanoparticles and Palladium nanoparticles to ensure homogeneous distribution and facilitate gas diffusion It contains Mesoporous Silica (MCM 41), which has a mesoporous structure. The subject of the invention is a Pd / AC / MCM 41 composite material containing 35-45% activated carbon and 45-55% by weight. It contains mesoporous silica (MCM 41) and 5-15% palladium nanoparticles. 20 The subject of the invention is a Pd / AC / MCM 41 composite material preferably containing 40% activated carbon by weight, 50% It contains mesoporous silica (MCM 41) and 10% palladium nanoparticles. The subject of the invention is a composite material in an application of Pd / AC / NaY zeolite composite material. and to contribute to the physical adsorption of hydrogen from red plum kernels. 25 obtained by pyrolysis and activation, with a microporous structure and high specific surface area. Containing Activated Carbon (AC), Palladium nanoparticles and Palladium nanoparticles to ensure homogeneous distribution and facilitate gas diffusion It contains sodium Y zeolite with a mesoporous structure. The subject of the invention is a Pd / AC / NaY zeolite composite material containing 30-60% activated carbon by weight. It contains sodium Y zeolite and 5-15% palladium nanoparticles. 30 The subject of the invention is a Pd / AC / NaY zeolite composite material preferably containing 45% activated carbon by weight, 45% It contains sodium Y zeolite and 10% palladium nanoparticles. Palladium (Pd): A transition metal that can chemically interact with hydrogen, forming H₂ on its surface. It provides the capacity to retain molecules by separating them (dissociative adsorption). Within the composite It is the main active phase of hydrogen adsorption. 5 Activated Carbon (AC): Prepared from red plum kernels. It has a high surface area and... Thanks to its microporous structure, it contributes to the physical adsorption of hydrogen. Similarly... Over time, it provides a suitable environment for the dispersion of Pd particles on the surface. MCM-41: A silica-based support material with a regular mesopore structure. Pd It ensures the homogeneous distribution of particles, prevents agglomeration, and promotes the diffusion of gases. It makes it easier. Sodium Y Zeolite (NaY): A microporous aluminosilicate with a crystalline structure. Porous Its regularity ensures a more stable and homogeneous distribution of Pd. High ion exchange. Its capacity supports metal loading. By increasing diffusion efficiency, it enhances the adsorption process. contributes 15 Thanks to this three-part structure (AC, Pd, and MCM-41 or NaY), it offers both physical (AC) and chemical (Pd) properties. and a hydrogen capture system optimized in terms of structural arrangement (MCM-41 / NaY) It has been obtained. Each component supports the performance of the other, thus the overall composite... Hydrogen adsorption capacity is increased. Ethylene glycol is used in the synthesis process for the reduction of PdCl₂. It is both a solvent and a 20 It acts as a reducing agent. This process is carried out under ultrasonic dispersion and reflex conditions. This is achieved. Pd is not permanent in the final composite product but is activated during production. It creates surfaces that can interact with hydrogen by enabling the transformation into a metallic phase. It makes it possible to carry out the reduction process in a controlled manner and at low temperatures. The invention involves achieving the chemical adsorption of hydrogen by placing H₂ molecules on its surface. A palladium (Pd) phase capable of forming Pd–H bonds by decomposition, the aforementioned palladium (Pd) It enables the reduction of phase ions in the solution medium and also acts as a solvent. An Ethylene Glycol used to undertake the Palladium (Pd) Phase (3) salts mentioned. Deionized water used for preparing the solution and the pH of the aforementioned solution A Sodium Hydroxide (NaOH) Solution 30 used to adjust the value to the range of 9–11. It includes. 11 The Activated Carbon (AC) and Sodium Y Zeolite (NaY) or MCM-41 mentioned in the invention. To ensure homogeneous distribution of mesoporous silica in ethylene glycol. An ultrasonic bath is used. Palladium is present in the aforementioned ethylene glycol environment. Reduction of (Pd) phase ions at a temperature range of 100–140 °C for 2–5 hours. A heating unit is used that provides this. The wet 5 obtained after reduction. To allow the composite to separate from the solution and become permanent, it must be heated at a temperature of 90–120 °C for 12–24 hours. A drying oven that operates throughout is also used. The invention is based on Pd / AC / MCM-41 and developed for hydrogen storage applications. Composite materials operate on the principle of physical and chemical adsorption. It is based on the synergistic functioning of its mechanisms. The system, red plum 10 Thanks to its microporous structure and high surface area obtained from its nuclei, hydrogen Activated Carbon (AC) contributes to the binding of molecules through Van der Waals interactions. It is built upon; the aforementioned Activated Carbon (AC) pore structure and the physical properties of hydrogen While performing adsorption, it is organized to facilitate the diffusion of hydrogen. MCM-41 Mesoporous Silica offers a high surface area with its mesoporous morphology, and 15 They work together, and the aforementioned MCM-41 Mesoporous Silica internal channels are also Pd Preventing metal agglomeration by preparing the ground for homogeneous distribution of nanoparticles It blocks them. The Palladium (Pd) Phase in the system separates H₂ molecules on its surface. They provide active sites that form Pd–H bonds, thus enabling the chemical (dissociative) release of hydrogen. This enables the adsorption of the aforementioned Palladium (Pd) Phase from ionic to metallic state. reduction and efficient dispersion of solvent and reducing agent on the composite. This is achieved through ethylene glycol, which acts as a primary carrier. Within this ethylene glycol, Pd Deionized water is used to facilitate the uptake of ions into the solution. when used, in order to control the reduction conditions and ensure efficient metal loading. A Sodium Hydroxide (NaOH) Solution is then introduced to adjust the pH value to the range of 9–11; 25 Additionally, the aforementioned Activated Carbon (AC) and the aforementioned MCM-41 Mesoporous Silica An ultrasonic bath that ensures the homogeneous distribution of particles in an ethylene glycol medium. Using this method, the pores are effectively prepared for Pd loading. The reduction reaction is carried out using ethylene. Palladium (Pd) phase ions in glycol medium undergo a 2– temperature range of 100–140 °C. This is carried out by a Heating Unit that enables the conversion to metallic Pd⁰ over a period of 30 hours; this step takes 30 hours. By creating a thin and homogeneous distribution of Pd on the support, it minimizes agglomeration. The wet composite obtained after the reaction is separated from the solution and then dries to 90–120°C. The process is made permanent by using a drying oven that operates at °C temperature for 12–24 hours. Thus... The microporous structure of the aforementioned Activated Carbon (AC) enhances its physical adsorption capacity. increasing, the homogeneous 35 of the aforementioned MCM-41 Mesoporous Silica Pd particles While facilitating dispersion and diffusion, the aforementioned Palladium (Pd) Phase 12 It makes it possible for hydrogen to be held together by chemical bonds; as a result of the interaction of all elements. high hydrogen capacity, low agglomeration tendency, increased cycle durability and low Reliable hydrogen storage performance is achieved under specific temperature and pressure conditions. An example study for the invention, whose workflow diagram is given in Figure 1, is shown below in Figure 5. This process has been carried out, and a Pd / AC / MCM-41 composite is obtained; Obtaining Activated Carbon (AC) (1): by pyrolysis and activation of red plum kernels Obtaining Activated Carbon (AC) with a microporous structure Preparation of powder mixture (2): 3 grams of activated carbon and 2.4 grams of MCM-41, in dry form, sensitive It is weighed on a balance and a homogeneous powder mixture is obtained. 10 Preparation of Pd solution (3): Aqueous solution of 1% PdCl2 with PdCl₂ and deionized water It is prepared. Ultrasonic dispersion (4): activated carbon and MCM- into 750 mL ethylene glycol solution 41 ingredients are added to the mixture. This mixture is kept in an ultrasonic bath (40 kHz, 30 minutes). Addition of Pd solution (5) Aqueous solution of 1% PdCl2 is added dropwise to the mixture 15 The metal load is set to 10%. pH adjustment (6): Then, pH value above 10 by adding 2 M NaOH solution. It is removed. This mixture is then left in an ultrasonic bath for another 5 minutes. Reduction step (7) (Pd²⁺ → Pd⁰): The mixture obtained after ultrasonic treatment is heated to 120 °C It is heated in a regulated oil bath under reflex conditions for 3 hours. During this process, 20 Ethylene glycol reduces the Pd²⁺ ions in (PdCl₂) to form metallic Pd⁰ particles. Reflex This process ensures the efficiency of the reduction reaction by preventing solvent loss at a constant temperature. It enables this to happen. The process is carried out at atmospheric pressure and in a closed system. Filtering and Drying step (8): The resulting wet composite is filtered and dried in an oven at 110 °C for 24 It is dried for 25 hours. Final product: The dried material is obtained as a Pd / AC / MCM-41 composite. Final product It becomes ready for characterization. 13 The subject of this invention is another study conducted for the production of Pd / AC / NaY zeolite composite. This is explained below. Obtaining Activated Carbon (AC) (1): by pyrolysis and activation of red plum kernels Obtaining Activated Carbon (AC) with a microporous structure Preparation of powder mixture (2): 3 grams of activated carbon and 3 grams of sodium Y zeolite, in dry form, sensitive 5 It is weighed on a scale, and a homogeneous powder mixture is obtained. Preparation of Pd solution (3): Aqueous solution of 1% PdCl2 with PdCl₂ and deionized water It is prepared. Ultrasonic dispersion (4): activated carbon and sodium Y in 800 mL ethylene glycol solution Zeolite mixture is added. This mixture is kept in an ultrasonic bath (40 kHz, 30 minutes). 10 Addition of Pd solution (5) Aqueous solution of 1% PdCl2 is added dropwise to the mixture The metal load is set to 10%. pH adjustment (6): Then, pH value above 10 by adding 2 M NaOH solution. It is removed. This mixture is then left in an ultrasonic bath for another 5 minutes. Reduction step (7) (Pd²⁺ → Pd⁰): The mixture obtained after ultrasonic treatment is heated to 120 °C. It is heated in a regulated oil bath under reflex conditions at atmospheric pressure for 3 hours. During this process, ethylene glycol reduces the Pd²⁺ ions in (PdCl₂) and metallic Pd⁰ ions. Particles are formed. In this way, Pd transforms into the active phase and is homogeneously distributed to the support materials. It disperses. The reflex process prevents solvent loss at a constant temperature, thus allowing the reduction reaction to proceed. This ensures efficient execution. The process is carried out at atmospheric pressure and in a closed system. 20 Filtering and Drying step (8): The resulting wet composite is filtered and dried in an oven at 100 °C for 24 It is dried for hours. Final product: The dried material is obtained as a Pd / AC / NaY zeolite composite. Final product It becomes ready for characterization. The Pd / AC / MCM-41 composite material and Pd / AC / NaY zeolite developed within the scope of this invention. composite material, hydrogen gas under low temperature and / or pressure conditions It can be used for adsorption purposes in fixed-bed and fluidized bed applications. (Fluidized-bed) or simple adsorption cells, at atmospheric or controlled pressure. It can be used below. The application temperature is generally between 77 K and 30 K, and the relative pressure is 0–1. 14 It can be within this range. Hydrogen gas is injected onto the composite material and at specific intervals. Adsorption / desorption isotherms are obtained. • The material must be vacuum-dried and free of moisture before use. Since porous structures can retain moisture, this negatively affects adsorption capacity. It can affect. 5 • Hydrogen gas should be used in its pure or high purity (99.999%) form. Mixed gas Substances such as CO₂, O₂, H₂O vapor, etc., can reduce adsorption efficiency. • To prevent oxidation of Pd during use, the system must be free of moisture and oxygen. recommended. • The material can be used in multiple adsorption-desorption cycles. However, long 10 With prolonged use, effects such as passivation (PdO formation) that may occur on the Pd surface should be observed. should be taken into consideration. • The material must be protected from extreme temperatures (>200 °C) and corrosive chemicals. • After use, performance can be monitored through characterization (BET, XRD, SEM). 20
Claims
REQUESTS 1. A high-performance composite material for hydrogen storage applications. It is a production method, and its characteristic is; a) microporous structure formed by pyrolysis and activation of red plum kernels Obtaining Activated Carbon (AC), 5 b) Activated carbon and Mesoporous Silica (MCM-41) or Sodium Y Zeolite (NaY Zeolite) dry mixing of powders, c) Preparation of a 0.5% to 2% PdCl₂ solution with palladium (Pd) and deionized water, d) Ethylene glycol mixed with activated carbon and mesoporous silica or sodium zeolite The mixture is added and the mixture is placed in an ultrasonic bath at a frequency of 35-45 kHz for 20-60 minutes. mixing within the range, e) After ultrasonic treatment, PdCl₂ solution is added dropwise to the mixture. charging of particles f) Adjusting the pH of the mixture to a range of 9-11 and immersing it in an ultrasonic bath for 5 minutes. being kept waiting for a certain period of time, 15 g) The mixture is heated at a temperature of 100 to 140 °C for a period of 2-5 hours to remove ethylene. reduction with glycol h) Separation of the composite formed after reduction by filtration and subsequent drying. It includes the steps involved in the process.
2. A method conforming to Claim 1, characterized by: Activated carbon and Mesoporous Silica. This involves mixing them in a ratio of 1:1 to 1.5:1 by weight.
3. A method that complies with Claim 1, characterized by the weight ratio of activated carbon and sodium β-zeolite. This involves mixing them in ratios of 1:1 to 1.5:
1.
4. A method that conforms to claim 1, characterized by the addition of PdCl₂ solution to the mixture drop by drop. This involves adding 5 to 15% by weight of Pd particles.
5. A method conforming to claim 1, characterized by the addition of a 2 M NaOH solution to the mixture. This involves adjusting the pH to the range of 9-11. 16 6. This is a method that complies with Claim 1, and its characteristic feature is that the resulting composite is heated to 90 to 120 °C. This involves drying the product within a specific temperature range for 12-24 hours.
7. It is a high-performance composite material for hydrogen storage applications, feature; Red plums contribute to the physical adsorption of hydrogen. obtained from their nuclei through pyrolysis and activation, having a microporous structure and Activated Carbon (AC) with a high specific surface area, Palladium nanoparticles and Homogeneous distribution of palladium nanoparticles and gas diffusion 10 with a regular mesopore structure to facilitate Mesoporous Silica or Sodium Y Zeolite It includes.
8. A composite material conforming to Claim 6, with the characteristic of having 35-45% active by weight. It contains carbon, 45-55% Mesoporous Silica (MCM 41), and 5-15% Palladium.
9. A composite material conforming to Claim 6, with the characteristic of having 30-60% active by weight. It contains carbon, 30-60% sodium zeolite, and 5-15% palladium.