METHOD FOR REMOVING Cu(II) FROM AQUEOUS MEDIA USING A BIOADSORBENT BASED ON BOILED CHICKPEA HUSK.

TR202605416A3Pending Publication Date: 2026-09-21KOCAELİ ÜNİVERSİTESİ BİLİMSEL ARAŞTIRMA PROJELERİ KOORDİNASYON BİRİMİ +1
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Patent Information

Application Number
TR202605416
Authority / Receiving Office
TR · TR
Patent Type
Applications
Current Assignee / Owner
Filing Date
2026-04-10
Publication Date
2026-09-21

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Abstract

The invention presents a bioadsorption method with clearly defined process steps and operating conditions for the evaluation of boiled chickpea hulls of domestic / industrial origin as a bioadsorbent within the scope of sustainable waste management and water treatment. The method involves (i) washing the waste chickpea hulls with pure water and drying them in an oven at 80 °C for 48 hours in the material preparation step; (ii) pulverizing the dried hulls in a laboratory-type mill (e.g.(iii) preparation of bioadsorbent powder in the 0.1–1 g dose range suitable for adsorption by grinding with IKA A11); (iv) verification of morphology by SEM, specific surface area by BET and surface functional groups by FT-IR in the characterization step; (v) contact of chickpea husk powder with Cu(NO) solutions in the range of 10–50 ppm prepared from Cu(NO) in the bioadsorption step by mixing them in 50 mL falcon tubes for 5–45 min under pH 2–6 and 25–55 °C conditions; (v) determination of the removal percentage by FAAS in the analytical determination step. This method, although different agricultural wastes have been reported as bioadsorbents in the literature, enables the first systematic and parameter-defined use of boiled chickpea husk powder in heavy metal removal. It offers advantages such as fast experimental cycles, environmentally friendly / economical adsorbent, simple equipment and the potential for expandability to dyes and organic pollutants in addition to Cu(II).
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Description

1 TARIFF Aqueous solution with boiled chickpea husk-based bioadsorbent. METHOD FOR REMOVING Cu(II) FROM MEDIA Technical Area The invention has potential in areas such as sustainable waste management, environmental engineering, and the chemical industry. Obtaining bioadsorbent from boiled chickpea husks for use and this adsorption of Cu(II) ions from Cu(II)-containing aqueous solutions by bioadsorbent powder It relates to a bioadsorption method that provides this. The invention specifically addresses sustainable waste management and water treatment in domestic / industrial settings. In the removal of heavy metals from aqueous solutions of boiled chickpea hulls. It is used as a bioadsorbent, an environmentally friendly / economical bioadsorption method. It is related. State of the Art 15 With the increase in industrial activities in recent years, heavy metal ions (especially Cu(II), The accumulation of Pb(II), Cd(II), Ni(II) and Zn(II) in surface and groundwater is a significant environmental problem. This has become the case. The bioaccumulation tendencies and toxic effects of these metals in aquatic ecosystems. It reduces biodiversity and poses serious risks to human health. Copper, in particular, is used in numerous metallurgical, electroplating, textile, pesticide, and paint industries. It is an ion frequently encountered in wastewater streams due to its widespread use, and it has acute toxicity. and stands out as a target pollutant due to its effect on catalytic oxidative stress in biological systems. In this context, the efficient, economical and sustainable extraction of Cu(II) from aqueous environments is being carried out. The removal of particles in this way is a subject of intense interest in the fields of environmental engineering and adsorption science. It is a subject of research. 25 Treatment technologies developed for this purpose are generally chemical, physicochemical, and biological. It is based on processes. Each method is evaluated based on selectivity, operating cost, energy requirement, and waste. It has different advantages and limitations in terms of its production and reuse potential. In practice, the removal of metal ions at low concentrations (ppm–ppb levels) is particularly important. This is challenging, and therefore adsorption techniques based on surface interactions have become increasingly popular in recent years. This comes to the forefront. However, the efficiency of adsorption processes depends on the surface of the adsorbent. It is strongly dependent on the properties, processing conditions and solution chemistry; this is due to the available This limits methodological diversity and comparability of results in the literature. 2 Known methods for removing heavy metal ions (especially Cu(II)) from aqueous environments Methods include chemical precipitation / neutralization (precipitation of metal hydroxide / sulfite / sulfur). coagulation–flocculation (colloid stability with Al / Fe salts and polymeric coagulants) 5 Pressure / polarization-based processes, specific binding with ion exchange resins, active Adsorption with carbon and synthetic sorbents and advanced oxidation-electrochemical techniques These approaches are widely used in laboratory and field applications. together; excessive chemical consumption and high sludge formation (neutralization / coagulation), Management of concentrated saline wastewater and membrane fouling / fouling, ion exchanger 10 regeneration of acid-base charge and selectivity loss in adsorbent-adsorbate systems Low concentrations (ppm–ppb) lead to decreased yield, and the formation of highly valuable / complex substances (Cl⁻, SO₄²⁻, organic ligand) matrix effects, competing ions, and high operating costs. It encounters limitations. This is a bioadsorbent for agricultural and lignocellulosic waste (bark, stem, seeds, etc.) 15 This has made its evaluation attractive from an environmental and economic point of view; however, in the literature Many reported bioadsorbents undergo multi-stage chemical activation (H₃PO₄, ZnCl₂, KOH, (HNO₃, etc.) and energy-chemically intensive pretreatments such as high-temperature carbonization / pyrolysis. These pre-treatments require the following: surface area / porosity and functional group density. Although it increases secondary waste and corrosive current production, scalability and operational safety 20 This creates a disadvantage in terms of experimentation. On the other hand, in bioadsorption studies, experimentation... heterogeneity of designs —uncertainty of adsorbent particle size, dose-time-pH– inconsistent selection of temperature windows, initial concentration, film / internal diffusion and isotherm– discrete assessment of the effects on kinetic behavior—data This weakens its comparability; moreover, by-processes such as Cu(OH)₂ precipitation 25 Although pH control is critical to avoid precipitation risk at ≈pH>6, in most protocols The adsorption-precipitation distinction is not sufficiently isolated. At the analytical end, flame atomic... Although techniques such as absorption (FAAS), ICP-OES / ICP-MS are common, some reports suggest that mass absorption may be ineffective. It fails to adequately define the balance and blank validations of experiments; also, reuse / Structural degradation and dissolution of the adsorbent in regeneration protocols (acidic elution, etc.) 30 The risks cannot be clarified. In short, low-cost raw materials and chemicals in the known technique... Simple setup without activation, standardized working window, and analytical validation. supported by a chain, non-precipitation adsorption of Cu(II) can be clearly observed. The need for an integrated approach continues. 35 3 Patent document number WO2016125041A1, which was found during the literature search, a method for removing metals from aqueous environments using bioadsorbents It relates to the method. The document mentioned refers to natural biomaterials and / or microbial... biomass in membrane, disc, composite membrane, granules, beads, filter bed and serpentine forms. They are converted into carrier matrices such as; the metal-containing flow passes through these matrices to specific 5 Heavy metals such as Cu(II), Zn(II), Pb(II) are removed by passing them through contact time and under low pressure. It reveals a process in which lignocellulosic waste powders are collected from shellfish. Powders (such as shrimp shells) and bacterial / algal / fungal biomass, alone or synergistically. Used in mixtures; particle size, dose, and pH affect removal efficiency. It is determined by isotherm and kinetic approaches. Adsorbent matrices are repeated in bead form. 10 It is designed to be usable in elution / reuse cycles (for example (with diluted mineral acids) it has been shown that capacity loss is limited; furthermore, low Continuous operation with pressurized biopolymer multi-screens and multi-stage bioreactor schemes. Examples have been presented. Patent document number WO2014012134A1 describes an agricultural waste-based... from bioadsorbent composition and its use in Cu(II), Zn(II), Pb(II) removal It is mentioned that the invention applies to materials such as watermelon rind, sugarcane stalks, and garden grass. Washing, drying, and grinding of lignocellulosic waste, either alone or... Used in mixtures with approximately 1:1:1 ratio; pH, initial concentration, dose and particle size 20 A bioadsorption platform that systematically investigates the effects of size on metal retention. It describes the peak of Cu(II) removal around pH≈6 in the samples; particle size As the size decreases, the Langmuir monolayer capacity increases; the dose is in the range of 0.5–5 g / L. It has been shown that increasing the percentage of Cu(II) removal reaches saturation. In regeneration studies, Cu loaded with 0.1 N H₂SO₄ was desorbed with high efficiency. and limited number of adsorption-desorption cycles of the same adsorbent It has been reported that it can be reused with a loss of performance; surface analysis with FT-IR analysis. The role of functional groups (–OH, –COOH, etc.) in metal bonding has been supported. Patent document number CN102728327A describes a modified orange peel. The preparation of bioadsorbent and its use in heavy metal removal are discussed. 30 The invention involves cleaning, drying, grinding, and sifting orange peel waste. after saponification in ethanol / NaOH and cross-linking with epichlorohydrin the formation of a skeleton; followed by cysteine ​​or in the presence of sodium carbonate catalysis. It involves functionalization with diethylenetriamine. The resulting cross-linked and amine / thiol Functional bioadsorbent adsorbs Cu(II), Pb(II), Ni(II), Zn(II) ions in the pH range of 2.0–6.0, at room temperature 35°C. It can effectively remove substances at temperatures with contact times of 2 minutes to 2 hours; after the process 4 where solid-liquid separation is easy and the adsorbent can be reused by elution (regeneration). It has been stated that it can be used. The process offers low cost, reuse, and high adsorption. With the goal of increasing capacity, it adopts the "waste-to-waste treatment" approach; in industrial wastewater. It also enables metal recovery. Studies have shown that existing bioadsorption solutions are suitable for agricultural waste or 5 Microbial biomass is converted into adsorbent form through simple pre-processing steps such as washing, drying, and grinding. bring (powder, granules, beads, membrane, filter bed), pH–dose–particle size–starting point It focuses on optimizing the effect of variables such as concentration within an isotherm / kinetic framework; regeneration / reuse is mostly carried out with mineral acids and Cu(II), For highly valuable cations such as Zn(II) and Pb(II), performance peaks are around pH≈6. It appears that this has been reported. However, adsorbent preparation is involved in numerous solutions. chemical activation (cross-linking with epichlorohydrin, amine / thiol functionalization, etc.) This requires; it increases the energy-chemical input and secondary waste load of the process; In membrane / composite architectures, the long-term interaction between carrier polymer and biomass is crucial. it can lead to stability and flow resistance (pressure loss) problems, and also regeneration 15 It appears that capacity losses accumulate in these cycles. In current techniques... Observed complexity of preparation, high chemical consumption, and lack of standardization; operational simplicity, low cost, chemical-free preparation, and specific operating intervals. This reveals the need for a defined, scalable and repeatable method. It provides. In this context, it is particularly reliable at low concentrations of heavy metal ions and 20 a bioadsorption approach that enables sustainable removal It needs to be improved. In conclusion, due to the negative aspects described above and the current solutions, the subject matter... Due to its shortcomings, an improvement in the relevant technical field is necessary. 25 It has been made. Purpose of the Invention The present invention meets the aforementioned requirements and eliminates all disadvantages. 30 extracted from boiled chickpea shells, which removes and offers some additional advantages. Standardization of Cu(II) removal from aqueous media using bioadsorbent It relates to an established bioadsorption method. The main purpose of the invention is to process boiled chickpea hulls without requiring chemical activation. conversion of bioadsorbent powder and removal of Cu(II) ions from aqueous environments from this powder effective use of a standardized method in its removal The goal is to ensure this by washing only with pure water, drying at 80°C for 48 hours, and grinding. With a simple preparation procedure consisting of 5 steps, it is low-cost, environmentally friendly and 5 A repeatable adsorbent is obtained. The aim of the invention is to define the conditions of adsorption experiments within clear intervals, thereby improving the method. The aim is to increase its comparability and scalability. This will allow for pH 2–6 and 25–55 °C. Temperature, initial Cu(II) concentration of 10–50 ppm, adsorbent dose of 0.1–1 g, contact time of 5–45 min. and can be transferred to different matrices with parameter windows such as a 50 mL working volume. A standard for implementation is established. One aim of the invention is to create an experiment that will differentiate between adsorption and chemical precipitation. The aim is to ensure the design allows for control of the upper pH limit and contact time / temperature. With this management, unwanted precipitation artifacts such as Cu(OH)₂ are prevented and the actual Adsorption contribution can be measured reliably. One aim of the invention is to ensure the analytical accuracy of the obtained removal data. This allows for the establishment of mass balance via the determination of remaining Cu(II) using FAAS, 20 The verifiability of measurements increases, and data quality meets patent and regulatory expectations. Another objective of the invention is to influence the surface chemistry and particle properties of the bioadsorbent during adsorption. The aim is to systematically examine the effect of grinding on performance. In this way, the specific properties increased by grinding can be investigated. surface area and through the natural –OH / –COOH functional groups of the lignocellulosic matrix 25 Electrostatic attraction / coordination coupling is optimized. Another aim of the invention is to experimentally determine the steps that determine mass transfer and velocity. The aim is to ensure separation. In this way, the film can be separated by selecting the mixing conditions and contact times. The effect of intraparticle diffusion regimes on diffusion is evaluated parametrically and 30 This provides direct input to process design. Another aim of the invention is to minimize the energy / chemical footprint through a preparation procedure. The goal is to reduce secondary waste generation. This, in turn, eliminates the need for acid / base / oxidant use. The non-detectable, non-activation approach increases operational safety and sustainable treatment. 35 It contributes to their practices. 6 Another aim of the invention is to achieve high removal even at low concentrations (10–50 ppm). The aim is to make it possible to achieve these percentages. This will enable efficient weighting even in challenging matrices. Metal removal can be achieved, and the output quality can be brought closer to regulatory limits. Another aim of the invention is to transfer the method outputs to engineering-scale designs. The aim is to simplify things. This allows for clearly defined parameter ranges and an analytical validation chain. Initial design criteria for scaling up continuous systems (column / reactor) It can be used as follows. Another objective of the invention is to ensure consistent quality in batch-by-batch production of the adsorbent. This allows for temperature / time and particle size control during the washing-drying-grinding steps. This minimizes performance fluctuations between lots and increases process reliability. Another objective of the invention is to apply the method to different heavy metals and complex matrices. The aim is to provide an experimental framework to prepare for its scalability. In this way, pH and Selectivity / process window is optimized by adjusting the temperature window, unlike other methods. This also lays the groundwork for applicability to cations and multi-component wastewater. Another aim of the invention is to provide 20 fast cycle and simple equipment requirements in field applications. The aim is to provide ease of operation. This allows for the same transition from 50 mL working volumes to pilot volumes. Efficient treatment is possible with short contact times according to these principles, and the total treatment cost is reduced. It is dropped. The present invention addresses this technical gap by using boiled chickpea hulls as a bioadsorbent. 25 The steps and parameter ranges for its evaluation are clearly standardized. It seals using the bioadsorption method: first, the waste shells are washed with pure water only, It is then dried in an oven at 80°C for 48 hours and ground into powder; thus Food chain origin, low cost and repeatable, requiring no chemical activation. An adsorbent is obtained. Adsorption experiments were conducted using 10–50 ppm 30-degree Cu(NO₃)₂. Using Cu(II) solutions in the range of pH 2–6 (precipitation artifacts) (with the upper limit maintained to exclude), in 50 mL Falcon tubes at temperatures of 25–55 °C, The process is carried out with contact times of 5–45 min and adsorbent doses of 0.1–1 g; external film resistance is determined by mixing. is minimized, and the contact time window allows for the passage of film diffusion → intraparticle diffusion. This allows for capture. Under these conditions, the thermodynamic / kinetic character of bioadsorption is; 35 pH through the degree of protonation of surface –OH / –COOH functional groups 7 the effect of temperature on activation energy and enta l pi indicator's contribution to adsorption capacity, mass transfer of input concentration and It can be systematically observed in terms of its reflection in nonlinear isotherm behavior. At the end of the experiment, the remaining Cu(II) in the solution was determined by FAAS to determine the mass balance and removal efficiency. It is calculated reliably; thus, a metric chain is formed in which adsorption is separated from precipitation. 5 This is achieved through a single-step heat drying + mechanical grinding process during the preparation phase. Its use reduces the energy / chemical footprint while minimizing secondary waste production; pH– Clear definition of temperature-concentration-time-dose intervals allows for comparison of method data and It makes it scalable; applicability is increased with fast cycle times, even at low concentrations. In conclusion, the invention benefits from the accessibility of the raw material, operational simplicity, and non-settling properties. Components of standardization based on adsorption isolation and analytical verification. by combining chemical / energy intensive pretreatment in known techniques, parameter uncertainty and a practical and sustainable bioadsorption method that addresses validation deficiencies. It reveals. The invention, for the purposes of chickpeas described above, involves the chemical processing of their shells. Converted into bioadsorbent powder without requiring activation, Cu(II) from aqueous environments It is a standardized bioadsorption method for removal, and the following process It includes the following steps; a) Obtaining waste boiled chickpea shells and removing foreign matter 20 purification, b) By subjecting the shells to successive washing, resting, and straining processes. removal of soluble pollutants, c) Spreading the washed shells on trays and drying them in an oven, d) To prevent the dried material from reabsorbing moisture, place it in the desiccator at room 25°C. cooling at temperature and storing in closed containers, e) Obtaining adsorbent powder by grinding the shells into powder in a grinder and sieving them. to be done f) Preparation of Cu(NO₃)₂ stock solution and working concentrations of 10–50 ppm Adjustment with volumetric dilutions within the range of 30 g) For each application, the working volume should be transferred to test tubes and the solution pH should be set to 2–6 setting within the range h) Operating temperature in a thermostatically controlled water bath between 25–55 °C ensuring it is secured, i) adding the bioadsorbent powder to the solution and shaking the mixture or 35 mixing 8 j) After the contact time, the mixture is separated into solid and liquid using a suitable porous filter. filtering or centrifuging and obtaining the clear supernatant, k) Determination of the residual Cu(II) concentration in the upper phase by FAAS and the removal percentage. Calculation of adsorption capacity per unit mass, l) Conducting parallel empty run and possible sedimentation control and mass 5 verification of balance, m) Low normality acidity if reuse of the adsorbent is desired. Elution-based regeneration, followed by rinsing and drying, for the next cycle. If conditioning or regeneration is not to be performed, then according to waste management legislation. disposal. 10 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 becomes clearer. This will be understood. Therefore, the evaluation should also take these figures and detailed explanations into account. It must be done by taking 15. Figures that will help understand the invention. Figure 1: The subject of the invention is the chemical activation of boiled chickpea hulls without requiring chemical activation. Regarding the removal of Cu(II) from aqueous environments by converting bioadsorbent into powder. This is a flowchart view of a standardized bioadsorption method. 20 Reference Numbers S1 - Raw Material Sourcing and Selection S2 - Washing S3 - Drying 25 S4 - Conditioning and Preservation S5 - Grinding and Screening S6 - Adsorbent Characterization S7 - Preparation of Cu(NO₃)₂ Stock and Working Solutions S8 - Volume Measurement and pH Adjustment 30 S9 - Ensuring Temperature Control S10 - Addition of Bioadsorbent Dose and Establishment of Contact S11 - Separating Solids from Liquids S12 - Performing Analytical Determination and Calculation (FAAS) S13 - Verification of Mass Balance by Blank Test and Sedimentation Control 35 9 S14 - Regeneration / Disposal S15 - Modeling and Reporting Detailed Description of the Invention This detailed explanation of the invention only provides 5 points to help better understand the subject. and is explained in a way that will not create any limiting effects. The invention involves converting chickpea husks into bioadsorbent powder without requiring chemical activation. a standardized method for removing Cu(II) from aqueous environments by conversion It is related to the bioadsorption method. 10 The method described in the invention involves the following steps: a) Obtaining waste boiled chickpea husks and removing foreign matter purification, b) By subjecting the shells to successive washing, resting and straining processes 15 removal of soluble pollutants, c) The washed shells are preferably spread in a single layer on trays and placed in the oven. drying, d) To prevent the dried material from reabsorbing moisture, the chamber is placed in the desiccator. cooling at temperature and storing in closed containers, 20 e) Obtaining adsorbent powder by grinding the shells into powder in a grinder and sieving them. to be done f) Preparation of Cu(NO₃)₂ stock solution and working concentrations of 10–50 ppm Adjustment through volumetric dilutions within the range, g) For each application, the working volume should be taken into tubes and the solution pH should be set to 2–6. setting within the range h) Operating temperature in a thermostatically controlled water bath between 25–55 °C ensuring it is secured, i) adding the bioadsorbent powder to the solution and shaking the mixture or mixing 30 j) After the contact time, the mixture is separated into solid and liquid using a suitable porous filter. filtering or centrifuging and obtaining the clear supernatant, k) Determination of the residual Cu(II) concentration in the upper phase by FAAS and the removal percentage. Calculation of adsorption capacity per unit mass, l) Conducting parallel empty run and possible sedimentation control and mass verification of balance, m) Low normality acidity if reuse of the adsorbent is desired. Elution-based regeneration, followed by rinsing and drying, for the next cycle. If no conditioning or regeneration is to be performed, then according to waste management legislation, 5 disposal In step (c) of the method described in the invention, the washed shells are spread out in a single layer on trays. It is preferably dried in an oven at 80 °C for 48 hours. In the method described in the invention, in step (e), the shells are ground into powder in a grinder and The resulting powder material is then sieved, preferably through a sieve with a mesh size of 250–500 µm. In the method described in the invention; in step (g), the working volume is preferably taken into 50 mL tubes and The pH of the solution is adjusted to a range of 2–6 by adding microdoses of acid or base. 15 The method described in the invention involves dissolving bioadsorbent powder, preferably in the range of 0.1–1 g. This involves adding and shaking or stirring the mixture. An application of the method described in the invention is the addition of bioadsorbent powder to the solution and 20 the mixture is shaken at a speed of 100–300 rpm for 5–45 minutes, or It involves mixing. Figure 1 shows the chemical activation of chickpea husks, which is the subject of the invention, without requiring any chemical activation. 25 regarding the removal of Cu(II) from aqueous media by converting bioadsorbent into powder. A flowchart of a standardized bioadsorption method is given. A preferred application of the method described in the invention involves the following steps: • Verification of the source of boiled chickpea hulls of waste origin, foreign purification from contaminants and creation of sample acceptance records (Raw Material Supply 30 and the Choice, S1) • Sequential washing, settling, and filtration cycles of shells with pure or deionized water. Treatment and removal of surface soluble contaminants (Washing, S2) • The washed shells are spread in a single layer on trays and baked in an oven at 80°C for 48 hours. Drying and verification that the moisture content has fallen below the target level (Drying, S3) 35 11 • To prevent the dried material from reabsorbing moisture, it must be placed in the desiccator at room temperature. cooling and storage in closed containers (Conditioning and Storage, p4) • Grinding the conditioned shells into powder using a laboratory-type grinder, the resulting product by sieve fractionation of the powder to a target granulometry, for example in the range of 250–500 µm. Bringing and homogenizing (Grinding and Sieving, S5) 5 • If requested, pre-experimental characterization of the adsorbent can be carried out and Morphology by SEM, specific surface area by BET, and surface functional groups by FT-IR. Verification (Adsorbent Characterization, S6) • Preparation of Cu(NO₃)₂ stock solution and working concentrations in the range of 10–50 ppm. Adjustment by volumetric dilutions (Cu(NO₃)₂ Stock and Working Solutions 10 Preparation, S7) • For each experiment, the working volume should be transferred to 50 mL tubes, and the solution pH should be between 2 and 6. Adjustment by adding microdoses of acid or base (Volume Measurement and pH Adjustment). S8) • The operating temperature should be fixed at 25–55 °C in a thermostatically controlled water bath. (Ensuring Temperature Control, S9) • Add the weighed bioadsorbent dose to the solution in the range of 0.1–1 g and mix the mixture. Shaking or mixing at a specified speed for 5–45 minutes (Bioadsorbent) Adding the Dose and Establishing Contact, S10) • After the contact time, the mixture should be filtered through a suitable porous filter for solid-liquid separation. 20 or centrifuging and obtaining the clear supernatant (Solid-Liquid Separation), S11) • Determination of residual Cu(II) concentration in the upper phase by FAAS and its removal percentage and unit price. Calculation of adsorption capacity per unit mass (Analytical Determination and Calculation) To be done (FAAS), S12) 25 • Conducting a parallel blank experiment and potential sedimentation control, and determining mass balance. Verification (Verification of Mass Equilibrium by Blank Test and Sedimentation Control, p. 13) • If reuse of the adsorbent is desired, use acidic elution with low normality. regeneration is performed, followed by rinsing and drying, for the next cycle. If no conditioning or regeneration is to be performed, then according to waste management legislation, 30 disposal (Regeneration / Disposal, p. 14) • Evaluation of experimental results using isotherm models and kinetic approaches, and analysis of data. Documentation in accordance with the standard reporting template (Modeling and Reporting (S15) 35 12 The working principle of the bioadsorption method that is the subject of the invention; Raw Material Supply and Selection. Verification of the source of boiled chickpea hulls of waste origin with (S1), foreign It starts with the purging of substances and the creation of traceability records, Subsequently, pure / deionized to remove soluble contaminants from the shell surface. Applying sequential washing-resting-filtering cycles using water and surface 5 Washing (S2) is carried out to prepare for adsorption, and the moisture To eliminate the disruptive effect on adsorption kinetics, it must be in a single layer. Drying of the spread-out shells in an oven at 80 °C / 48 hours is called Drying (S3). This ensures that the chamber in the desiccator is sealed to prevent re-moisture absorption after drying. Conditioning and Preservation 10: Cooling to temperature and storing in closed containers. (S4) is carried out to increase the active surface of the adsorbent and mass transfer. To reduce their resistance, the shells are ground into powder using a laboratory-type grinder. Adjusting the granulometric distribution to the target range (e.g., 250–500 µm) by sieve fractionation. and completion of homogenization within the scope of Grinding and Sieving (S5) is required. The morphology of the adsorbent in this state was determined by scanning electron microscopy, and its specific surface area was 15. nitrogen adsorption method and surface functional groups by infrared spectroscopy Verification of adsorption should be carried out within the framework of Adsorbent Characterization (S6). In order to prepare the metal solution to be used in the circuit, the stock of Cu(NO₃)₂ the formation and adjustment of working concentrations of Cu(NO₃)₂ in the range of 10–50 mg L⁻¹ Preparation of Stock and Working Solutions (S7) is provided for each experiment, working 20 The volume should be transferred to 50 mL tubes and the solution pH should be kept between 2–6 using microdose acid / base. Avoiding sedimentation artifacts by setting the volume and pH with the addition of volume. The adjustment is carried out within the scope of (S8), mass transfer and velocity constants. To control its temperature sensitivity, the environment is kept in a thermostatically controlled water bath in the 25–55 °C range. Ensuring temperature control (S9) and fixing the temperature is guaranteed, 25 film diffusion and intraparticle diffusion regimes under specified hydrodynamic conditions In order to enable its separation, the adsorbent dose is added to the solution in the range of 0.1–1 g and Shaking the mixture for 5–45 minutes before adding the bioadsorbent dose. To be carried out within the scope of Establishing Contact (S10), following the completion of contact. Filtration with a suitable porous filter or centrifugation for separating the solid phase from the liquid phase 30 The implementation is carried out within the scope of Solid-Liquid Separation (S11), above Determination of residual Cu(II) concentration in phase by flame atomic absorption spectrometry and calculation of removal percentage and adsorption capacity per unit mass Completion of Analytical Determination and Calculation (S12) Parallel blank experiments and possible 35 to verify adsorption by separating it from precipitation. Running the Cu(OH)₂ formation control and closing the mass balance in the Empty Experiment 13 and ensuring Mass Balance Verification by Precipitation Control (S13), the adsorbent If reuse is intended, the load is removed by acidic elution at low normality. desorption, rinsing and drying, then conditioning for the next cycle. or disposal in accordance with appropriate regulations if regeneration is not to be carried out. The regeneration / disposal process (S14) is carried out and the resulting experiment is 5. their outputs are classified as isotherms (e.g., Langmuir / Freundlich) and kinetics (pseudo-first / pseudo-second order, evaluation using Weber-Morris approaches and reporting the results according to a standard reporting template. Proper documentation of Modeling and Reporting (S15) It is based on the principle of completion; thus, the aforementioned S8 pH adjustment and the aforementioned The coordinated operation of the S9 temperature stabilization with the aforementioned S10 contact / mixing step is crucial. 10 This is provided as a combined verification of the aforementioned S11 phase separation and the aforementioned S12 analytical determination. In establishing the chain, the validity of the method is ensured with the aforementioned S13 mass balance. is being taken and the process involves cyclical operation with the aforementioned S14 regeneration and the aforementioned S15 Through modeling, it becomes possible to transfer the design to an engineering scale. 20

Claims

14 REQUESTS 1. Chickpea husks can be converted into bioadsorbent powder without requiring chemical activation. A standardized 5 for the removal of Cu(II) from aqueous media by conversion. It is a bioadsorption method, and its characteristic feature is; a) Obtaining waste boiled chickpea husks and removing foreign matter purification, b) By subjecting the shells to successive washing, resting, and straining processes. Removal of soluble pollutants, 10 c) Spreading the washed shells on trays and drying them in an oven, d) To prevent the dried material from reabsorbing moisture, the chamber is placed in the desiccator. cooling at temperature and storing in closed containers, e) Obtaining adsorbent powder by grinding the shells into powder in a grinder and sieving them. 15 f) Preparation of Cu(NO₃)₂ stock solution and working concentrations of 10–50 ppm Adjustment through volumetric dilutions within the range, g) For each application, the working volume should be transferred to test tubes and the solution pH should be set to 2–6 setting within the range h) The operating temperature is between 25–55 °C in a thermostatically controlled water bath. ensuring it is secured, i) adding the bioadsorbent powder to the solution and shaking the mixture or mixing j) After the contact time, the mixture is separated into solid and liquid using a suitable porous filter. filtering or centrifuging and obtaining the clear supernatant, 25 k) Determination of residual Cu(II) concentration in the upper phase by FAAS and removal percentage Calculation of adsorption capacity per unit mass, l) Conducting parallel empty run and possible sedimentation control and mass verification of balance, m) If reuse of the adsorbent is desired, a low normality acidic 30 Regeneration by elution, rinsing and drying after the next step. Waste if it is not to be conditioned for the cycle or regenerated. disposal in accordance with management legislation It includes the steps involved in the process.

2. A method that conforms to Claim 1, characterized by: in step c), the shells are 35°C for 48 hours. It is dried in an oven.

3. A method that complies with Claim 1, characterized by the fact that in step (e), the powder material is absorbed by 250–500 µm. It is sifting through a sieve within a certain range.

4. This is a method that conforms to Claim 1, and its characteristic is that in step g), the working volume is 50 mL in tubes. by taking and adding microdoses of acid or base to the solution pH in the range of 2–6. It is the adjustment.

5. A method that complies with Claim 1, characterized by the fact that the bioadsorbent powder is in the range of 0.1–1 g. This involves adding it to the solution and shaking or stirring the mixture.

6. This is a method that complies with Claim 1, and its characteristic is the addition of bioadsorbent powder to the solution and 10 the mixture is shaken at a speed of 100–300 rpm for 5–45 minutes, or It involves mixing.