KINETIC GEOCHEMICAL ANALYSIS METHOD OF CEMENTITIOUS PASTICIDE FILLING IN A CONTINUOUS WATER FLOW MEDIUM AND KINETIC MOISTURE CELL USED IN THIS METHOD

TR202612850A2Pending Publication Date: 2026-09-21KARADENIZ TEKNIK UNIVERSITESI TEKNOLOJI TRANSFERI UYGULAMA & ARASTIRMA MERKEZI MUDURLUGU
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Patent Information

Application Number
TR202612850
Authority / Receiving Office
TR · TR
Patent Type
Applications
Current Assignee / Owner
Filing Date
2026-07-30
Publication Date
2026-09-21

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Abstract

The invention relates to an analytical method for determining the kinetic geochemical behavior of cementitious paste filler material, prepared from fine-grained waste generated from mining activities, under conditions of continuous water flow, and to a kinetic moisture cell that enables the application of this method.
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Description

1 TARIFF KINETICS OF CEMENTITIOUS PASTE FILLING IN A CONTINUOUS WATER FLOW MEDIUM. GEOCHEMICAL ANALYSIS METHOD AND KINETICS USED IN THIS METHOD MOISTURE CELL TECHNICAL FIELD The invention is derived from fine-grained waste generated as a result of mining activities. the prepared cementitious paste filling material is constantly exposed to water flow Analytical method for determining the kinetic geochemical behavior under certain conditions and is related to the kinetic moisture cell that enables the application of this method. 10 STATE OF THE ART Cementitious paste filling in underground mining, resulting from mining activities. in the evaluation of fine-grained waste generated and underground production cavities It is a commonly used waste management method in filling. Cementitious putty 15 The filler is in a fluid state during the production phase and gains strength and durability over time. The winner is ultimately a solid and whole material that can maintain its structural integrity. It transforms into its current form. Kinetic geochemical analyses of sulfur-containing mining wastes are general. This is done according to the ASTM D5744-13 standard. The classic method in question, 20 Long-term analysis of granular waste materials under high oxidation conditions It is aimed at examining their behavior. In this method, waste material is exposed to dry and humid air. exposed to contact, then weekly with water in a limited liquid / solid ratio. The leachate is collected by washing. However, cementitious paste filling material, unlike the granular waste used in the classical method, is 25%. It differs from other materials. Cementitious putty filler material is produced during the manufacturing process. It is fluid and gains strength and durability over time, approximately in 3 to 7 days. It starts, and after about 28 days, it is able to maintain its structural integrity and is unique. It acquires a solid structure with a axial compressive strength of 1 MPa or higher. This Therefore, in order to analyze cementitious paste filling material using classical methods, 30 2 its structural integrity is disrupted, it disintegrates, and forms a suitable grain size smaller than 6 mm. It needs to be transformed. In geochemical analyses, the particle size and whether the material is in a monolithic or granular state are determined. Its presence has a significant impact on the analysis results. Cementitious paste The breakdown of the filler material into a granular form makes the material reactive 5 increasing the surface area and achieving a level of height that would not occur under actual application conditions. This can lead to the acquisition of oxidation values. Therefore, classical kinetics test methods, actual underground application of cementitious paste filling material It is insufficient to represent its structure. Furthermore, the classical method involves subjecting the waste to high oxidation conditions for a long period of 10 years. It was developed to study seasonal behavior. However, underground production The cement paste filling material stored in the openings was removed after the mine was closed and largely protected from oxidation, especially after the groundwater level rises. It can withstand these conditions. Cementitious paste filling material, underground production. by briefly coming into contact with the air in the mine openings in their cavities 15 It can undergo oxidation, and after this process, which takes approximately 40 days, it becomes free. By sealing the surfaces, contact with air can be completely cut off. Contact with air... The cut cementitious paste fill stops remain until the mine reaches the end of its service life. It can remain without being exposed to air and water contact. After the mine was closed and the groundwater level rose, the underground mine 20 Cement paste filling material stored in the openings undergoes seasonal changes within its structure. Depending on rainfall and groundwater regimes, a continuous water flow can occur. Mining openings, once mining operations are completed, gradually fill with groundwater. It is starting, the rising groundwater level is where the cement paste fill stops are located When it started to pass through the regions, the cement paste fill stored underground 25 Water can flow slowly and continuously through its structure. This situation, underground This is a common occurrence in paste filling applications. In existing classical methods, dry and moist air inlets are in 10 cm diameter cells. from the bottom lid of the cell, that is, from the bottom of the sample, in cells with a diameter of 20 cm This is done from the top cover of the cell, that is, from the upper surface of the sample. ASTM D5744-30 In addition to the 13 standards, it also complies with EPA Method 1627 and TCLP Method 1311. 3 The geochemical characterization cells used are also air and wash-based test setups. They show similarities in this respect. However, these cell designs were changed after the mine was closed. then cement paste that is cut off from contact with air and remains in constant contact with groundwater. Long-term in-situ conditions of the filling material in a laboratory environment. It is not adequately represented. 5 Therefore, the cementitious paste filling material should be in a monolithic and unbroken state. By preserving its monolithic structure, contact with air is prevented, and a continuous low-flow water supply is ensured. under exposed conditions (while maintaining a constant water level / amount inside the cell) a new method that allows for geochemical analysis and this method A suitable cell structure is needed for its implementation. 10 THE PURPOSE OF THE INVENTION The purpose of the invention is to apply cementitious paste as a filling material after the mine has been closed. laboratory analysis of geochemical behavior under conditions of continuous contact with groundwater The aim is to ensure that it is determined in the environment. 15 One aim of the invention is to produce cementitious paste filler material using classical methods. without being broken down or granulated, directly inside the cell pouring and curing, and analysis in a solid, whole, integral, and monolithic form. to provide. Another objective of the invention is to allow cementitious paste filling material to interact with air at 20°C. Kinetic humidity to represent the conditions under which contact is broken in a laboratory environment. The goal is to present a cell design where the air inlets are absent or sealed. Another objective of the invention is to remove from the structure of cementitious paste filler material. by allowing water to pass through at a low and continuous flow rate, after the mine was closed then permanent groundwater that may appear as the groundwater level rises 25 The goal is to simulate this interaction in a laboratory setting. Another aim of the invention is to improve classic washing based on weekly and limited liquid / solid ratios. Instead of the process, the leakage is obtained by passing a continuous stream of water through the sample. The goal is to collect and analyze the water. Another objective of the invention is to make the cementitious paste filler material acid mineral 30 the potential for creating drainage and its time-dependent environmental impacts, on site 4 determining it in a more controlled analysis environment closer to the application conditions to provide. BRIEF DESCRIPTION OF THE FIGURES Figure 1 shows the kinetic moisture content of the cementitious paste filler sample from the previous technique at 5°C. General view of the cell. Figure 2 shows the kinetics of the cementitious paste filler in a continuous water flow environment, which is the subject of the invention. General view of the kinetic moisture cell used in geochemical analysis. The corresponding values ​​for the references given in the figures are: 10 1. Plexiglas clear tube 2. Plexiglas perforated circular disc 3. PVC bottom and top covers 4. Bolts, nuts, screws, and a leak-proof base gasket connecting the covers. 5. Water inlet connection pipe 15 on the top cover 6. Liquid outlet valve and connections on the bottom cover. DETAILED DESCRIPTION OF THE INVENTION The invented method involves the processing of fine-grained materials resulting from mining activities. Cementitious paste filling material prepared from waste, exposed to continuous water flow 20 The aim is to determine the geochemical behavior of the organism under the conditions in which it is kept. The method... The potential of cementitious paste filling material to create acid mine drainage and Time-dependent environmental impacts are being determined. Within the scope of this invention, cementitious paste filling material is used, as in classical methods. a sample that is broken down or granulated and then placed into the cell later 25 It is not used as such. Cementitious paste filler material, kinetic moisture subject to the invention. It is poured directly into the cell and cures inside the cell, becoming solid and whole. It acquires a solid and monolithic form. Thus, the application of the sample in the field... A laboratory analysis environment similar in structure is obtained. The aforementioned method To make this possible, the kinetic moisture cell created within the scope of the invention will analyze 30 the transparent plexiglass tube (1) that forms the cylindrical outer wall into which the material will be placed It contains. The plexiglass transparent tube (1) is a hollow tube structure. Plexiglass transparent The height of the pipe (1) is a minimum of 203 mm, the inner diameter is a minimum of 102 mm and the wall thickness is 6.35 The diameter is mm. A circular disc with perforated plexiglass (2) is placed inside a transparent plexiglass tube (1). It contains a perforated circular disc (2) of plexiglass, inside a transparent plexiglass tube (1). It functions as a fixed perforated base. The inner diameter of the perforated circular disc (2) of plexiglas is 5 It is 102 mm in diameter and 3.15 mm in thickness. Filter paper on a perforated circular disc (2) of plexiglass. or permeable membrane is installed. Filter paper or permeable membrane, It helps the sample remain stable within the cell. Cementitious paste. preserving the intracellular positioning of the filler sample and the filtration process. To be done properly, the filter is placed on the circular disc (2) with perforated plexiglass. This is achieved with paper or permeable membrane. The kinetic moisture cell, which is the subject of the invention, is placed under and on top of the plexiglass transparent tube (1). It includes fitted PVC bottom and top covers (3). Each of the PVC bottom and top covers (3) It is 40 mm thick, and the lids are square in shape with dimensions of 150 x 150 mm. It allows air and water in. Solution and leaching inlet and outlet connections can be mounted on the covers in question. Invention 15 In the case of the new cell structure, the air inlets are closed or on the cell... It is designed to prevent air from entering. PVC bottom and top covers (3) and plexiglass transparent tube (1), the covers are connected to each other. connected to each other by means of bolt, nut, screw and sealing base gasket (4) It is interlocked. The connecting elements (4), bottom cover, top cover and plexiglass transparent 20 These connecting elements ensure that the tube (1) is tightly connected to each other. a fixed structure that will allow the system to be placed in the analysis setup after it has been shut down and It creates a leak-proof structure. The top cover contains the water inlet connection pipe (5). Water inlet connection pipe (5) ensures the continuous and low-flow water supply to the cell. Water inlet 25 with connecting pipe (5), elastic hose, clamp and similar auxiliary parts. It is used. The bottom cover contains the liquid outlet valve and its connections (6). Liquid outlet valve and connections (6) to ensure drainage of leakage solutions from the sample. It includes auxiliary parts such as taps, elastic hoses, clamps, and the like. Solution 30 The outlet is designed to be opened and closed with a tap. 6 In applying the method, the cementitious paste filling material to be analyzed It is placed in the moisture cell. A plexiglass transparent tube (1) is placed inside the sample. It forms the volume in which it is placed. Plexiglas perforated circular disc (2), plexiglas transparent It is fixed inside the tube (1) and filter paper or permeable membrane is placed on it. is placed. After the sample is placed inside the cell, a transparent plexiglass tube (1), 5 The cell is assembled by PVC bottom and top covers (3) and connecting elements (4). It is being closed. After the cell is closed and placed in the system, a kinetic humidity cell test is performed. is initiated. In the system described in the invention, a low flow rate is continuously applied to the cell. Water is supplied from the top cover. The water supply is via the water inlet located on the top cover. It is carried out via the connecting pipe (5). 10 passing through the sample body. Filtrate water is discharged through the liquid outlet valve and connections (6) located on the bottom cover. This process involves taking the water inlet connection pipe (5) on the top cover and the liquid on the bottom cover. outlet valve and connections (6) are used. Because the cell structure that is the subject of the invention does not have air inlets, or Because it is sealed, the cementitious paste filler sample is prevented from coming into contact with air. 15 This eliminates the need for dry and humid air supply, which is common in conventional cells. being removed, cement paste filling material is being left in the air after the mine is closed. The conditions under which contact is broken are represented in a laboratory setting. In the method described in the invention, a monolithic and integral structure is created in which contact with air is prevented. 20% of the cementitious paste filling material is continuously injected into the material at a low flow rate. Water flow is being passed through. The water passing through the sample is continuously treated as leachate. The cementitious materials are collected in this manner and analyzed weekly. This analysis is used to determine the cementitious properties. the behavior exhibited by the putty filling material when continuously exposed to groundwater Geochemical behaviors can be studied in a laboratory setting under controlled conditions. The new method developed within the scope of the invention conforms to the ASTM D5744-13 standard. Similarity in general cell structure with the specified kinetic moisture cell test method. However, the fact that the analysis material is a cementitious paste filler sample, The fact that the sample is found in a solid and monolithic form within the cell, allowing air into the cells preventing inlet and performing the washing process with a continuous water flow at a low rate. It differs from the classical method in this respect. 30 7 The analytical material used in the classical method is granular mining waste. However, the analytical material used in the method described in the invention is cementitious paste filler. It is a sample. In the classical method, the analytical material placed in the cells has a granular structure. However, in the method that is the subject of the invention, the analytical material placed in the cells has a mixed structure. It is a cementitious paste that hardens as a filling material. In the classic method, air is introduced into the cells. During the feeding process, air entry into the cells was prevented in the method described in this invention. In the classic method, it is done once a week with a liquid / solid ratio of 1:1 or less. During the washing process, the material is washed at a low flow rate using the method described in the invention. And the washing process is carried out continuously by passing water through it constantly. Thanks to this structure, 10 years after the mine was closed and the groundwater level rose... then the cementitious paste filling material will perform in-situ conditions Chemical reactions are more accurately simulated in a laboratory setting. Thus, the time-dependent geochemical behavior of cementitious paste filling material. Its characteristics can be determined. Within the scope of the invention, the cementitious paste filler sample should not disintegrate and 15 Analysis in monolithic form, reactive surface area in granular samples to prevent high oxidation values ​​that may arise due to the increase It provides a contribution. Thus, the cementitious paste filling material is real. Environmental characterization data that is closer to the structure in practice is obtained. Since the newly developed method does not require an air supply, unlike the classic 20 Many of the elements and equipment involved in the method are not needed. Instead, a pure water tank that will provide a continuous water supply to the cells and a continuous supply of water from the cells A simpler test using a water collection tank to collect leachate. The mechanism is being created. 30

Claims

8 REQUESTS 1. Prepared from fine-grained waste generated as a result of mining activities. Cementitious paste filling material, continuously water-resistant, with airtight sealant. Kinetics 5 used in determining geochemical behavior under flow conditions It is a moisture cell, and its characteristic feature is that it analyzes the cementitious paste filling material to be analyzed. placed directly inside the cell, forming a solid, whole, integral, and monolithic form. the plexiglass transparent tube (1) which forms the hollow cylindrical outer wall that it will win fixed inside a plexiglass transparent tube (1), with filter paper or permeable material on top Circular disc with perforated plexiglass (2) in which the membrane is placed, 10 of the transparent plexiglass tube (1) cement paste filler sample attached to the bottom and top with air without dry air and humid air inlet connections to prevent contact PVC bottom and top covers (3) which are square in shape, PVC bottom and top covers (3) bolt, nut, screw and that securely clamp the plexiglass transparent tube (1) The fasteners, consisting of a leakproof base seal (4), are located on the top cover 15 and a water inlet that ensures a continuous supply of water to the cell at a low flow rate. connecting pipe (5), located in the lower cover and leaking through the sample body by including liquid outlet valve and connections (6) that provide drainage of solutions It is characteristic.

2. Conditions under which cementitious paste filling material is continuously exposed to water flow 20 the potential for acid mine drainage and time-dependent environmental factors It is a kinetic geochemical analysis method aimed at determining the effects, and its characteristic feature is; cementitious paste filler material, which is in a paste-like consistency in its fresh state, circular disc with perforated plexiglass inside a transparent plexiglass tube (1) (2) 25 on the filter paper or permeable membrane positioned on top placement of the cementitious paste filling material inside the cells The cell takes on a solid, whole, unified and monolithic form through curing, and the PVC bottom and Closed with top covers (3) and bolt, nut, screw and leakproof base gasket (4) securing it with cement paste prevents the cementitious filler material from coming into contact with air. To prevent this, dry air and humid air should not be supplied to the cell, above 30 Water flows into the cell at a low rate through the water inlet connection pipe (5) located on the cover and 9 Continuous water supply and liquid outlet valve and connections located in the bottom cover (6) seepage passing through the cementitious paste filling material It is characterized by including the process steps involved in obtaining the solutions. 10 20 30