A source control inhibitor for preventing CO over-limit and its preparation method and application

Abstract

The application discloses a kind of source control of preventing and treating CO overrun inerting agent and its preparation method and application, the inerting agent of source control includes mass ratio 1: (1.5-2) inhibiting main agent and base oil;Wherein, the inhibiting main agent is polyglycerol fatty acid ester and / or vitamin E derivative;The base oil is naphthenic mineral oil.The inerting agent of source control of the application can target effect on the coordination structure of high-activity excitation material in coal, utilize the multi-hydroxy structure of source control of inerting agent and the metal center of coordination structure competition coordination at normal temperature, destroy the coordination structure of high-activity excitation material, realize its oxidation activity inerting, greatly reduce the output of CO.

Description

Technical Field

[0001] This invention relates to the field of CO control technology, and more specifically, to a source-inhibiting inert agent for preventing CO over-limit, its preparation method, and its application. Background Technology

[0002] In western mining areas, coal seams are mostly low-rank coals prone to spontaneous combustion. Excessive CO concentrations frequently occur in the return air corners of working faces, posing a significant safety hazard. On one hand, long-term CO exposure harms miners' health, causing symptoms such as dizziness and fatigue. On the other hand, as a key early warning gas for coal spontaneous combustion, abnormally high CO levels can interfere with early predictions, leading to warning failures. Current prevention and control measures mainly employ leak sealing, nitrogen injection, grouting, and ventilation control. While these can control CO emissions to some extent, they fail to fundamentally suppress the tendency of coal to spontaneously combust at room temperature.

[0003] In terms of inhibition technology, existing coal spontaneous combustion inhibitors are mostly designed for high-temperature conditions, and their application at room temperature has significant limitations. For example, polymeric emulsion inhibitors have high viscosity and poor permeability; microencapsulated inhibitors have slow release and complex processes; composite inhibitors are prone to stratification and precipitation, and have weak adhesion; latex-type inhibitors have insufficient fluidity and slow film formation. These products generally suffer from poor permeability at room temperature, low stability, short inhibition time, and low efficiency, making it difficult to meet the long-term protection needs of room-temperature coal seams in western mines.

[0004] The root cause lies in the presence of a class of highly reactive activating substances in low-rank coals in western China, whose structure is based on alkali / alkaline earth metals (such as... , This is a coordination system with a metal center and aromatic organic compounds as ligands. This substance can rapidly oxidize with oxygen at room temperature (0-50℃), becoming a core source of low-temperature CO production. Traditional antioxidant inhibitors primarily target free radicals generated in large quantities at coal temperatures ≥80℃, and cannot effectively inhibit the oxidation reaction of this type of active structure at low temperatures.

[0005] Therefore, there is an urgent need to develop a novel inhibitor that can target this organic-inorganic coordination structure and stably and efficiently inhibit coal oxidation at room temperature, so as to fundamentally solve the problem of excessive CO concentration in the return air corner, improve the reliability of coal spontaneous combustion early warning, and ensure safe production in coal mines. Summary of the Invention

[0006] In order to overcome the above-mentioned defects of the prior art, the embodiments of the present invention provide a source-inhibiting inert agent for preventing CO over-limit, its preparation method and application, and solve the problem that low-rank coal is prone to rapid oxidation at room temperature, which leads to excessive CO concentration in the return air corner and affects safety.

[0007] To achieve the above objectives, the first aspect of this invention provides a source inhibitor and inerting agent for preventing CO over-limit, the source inhibitor and inerting agent comprising an inhibitory main agent and a base oil in a mass ratio of 1:(1.5-2); wherein the inhibitory main agent is a polyglycerol fatty acid ester and / or a vitamin E derivative; and the base oil is a cycloalkyl mineral oil.

[0008] The active activating substance targeted by this source-inhibiting inert agent can be activated for oxidation at 0-50℃. Specifically, low-rank coal contains highly active activating substances, which are primarily composed of alkali and alkaline earth metal elements (such as...). , The inhibitor has a coordination structure with a metal center and an aromatic side chain for the organic ligand. At room temperature, the polyhydroxyl structure of the inhibitor, consisting of polyglycerol fatty acid ester and / or vitamin E derivative, can compete with the metal center for coordination. UV-Vis spectrophotometry analysis showed that after spraying the inhibitor containing polyglycerol fatty acid ester and / or vitamin E derivative at room temperature (0-50℃), the absorbance of the coal sample at the characteristic absorption peak of the coordination structure (280nm) decreased from 0.82 to 0.35. This indicates that the inhibitor's competition with the metal center of the highly active activating substance in the coal can disrupt the original coordination structure, inertize its oxidative activity, and thus reduce CO production, mitigating the safety hazards caused by excessive CO concentration.

[0009] A second aspect of this invention provides a method for preparing a source-inactivating agent, comprising the following steps: The base oil is gradually heated to 60-70°C. Add the vacuum-dried inhibitor, keep the system temperature constant, stir to dissolve, and obtain a homogeneous and clear base oil solution; Pour the base oil solution into deionized water, maintaining the system temperature at 40-60°C. High-speed shearing yields a stable, non-stratified primary emulsion; The primary emulsion was gradually cooled to 30°C. The mixture was stirred continuously and deionized water was added until it was evenly mixed. After standing, a milky white, uniform source inhibitor and inert agent with no stratification or precipitation and a particle size distribution between 100-500nm was obtained.

[0010] By selecting naphthenic mineral oil as the base oil, the temperature is raised to 60-70°C at a certain heating rate. The inhibitor, which has undergone vacuum drying, is added to accelerate its dissolution and remove moisture and impurities, ensuring the homogeneity of the base oil solution and resulting in a homogeneous and clear base oil. The resulting base oil solution is then slowly poured into deionized water, while maintaining the system temperature at 40-60°C. Under the premise of continuous high-speed shearing, the dispersion and fusion between the oil phase and the aqueous phase are enhanced, improving the stability of the primary emulsion and effectively reducing the risk of stratification; finally, the primary emulsion is gradually cooled to 30°C at a certain cooling rate. The following steps, along with continuous addition of deionized water during stirring until the mixture is homogeneous, ensure the dispersibility and contact area of ​​the source inhibitor mixture, improve its stability during storage and use, and prevent the source inhibitor from becoming ineffective.

[0011] By sequentially preparing a base oil solution, a primary emulsion, and a final inhibitory inert agent, and controlling and ensuring the system temperature during mixing and stirring to guarantee full integration between the components, the resulting inhibitory inert agent is homogeneous, stable, and possesses excellent inhibition capabilities.

[0012] A third aspect of this invention provides the application of a source-inhibiting inert agent in preventing CO exceedance at the upper corner of an underground coal mine working face. When the source-inhibiting inert agent is sprayed onto the coal face at room temperature, it is diluted with deionized water to a mass concentration of 10%-15%, and sprayed at least once every 24 hours, with each spray consisting of 50-100 ml. ; The mass ratio of the source-inhibiting inert agent to the fire-prevention and extinguishing grout is (1:5)-(1:10).

[0013] When using source-inhibiting inert agents, the dilution or mass ratio of the source-inhibiting inert agents can be optimized according to the specific application scenario of preventing CO exceedance in the upper corner of the underground working face of coal mines, so as to maximize the inhibitory performance of the source-inhibiting inert agents and ensure the rationality of the application.

[0014] When the source-inhibiting inert agent is sprayed onto the surface of the coal face at room temperature, no additional temperature control equipment is required, making it suitable for complex underground working environments and improving construction convenience. Before spraying, it is preferable to dilute the source-inhibiting inert agent with deionized water, as deionized water avoids interference from impurities. The preferred mass concentration of the diluted source-inhibiting inert agent is 10%-15%. This concentration range not only avoids problems such as waste and decreased permeability caused by excessive concentration, but also prevents uneven coverage of highly active activating substances and insufficient inertization effect due to insufficient concentration. Furthermore, spraying should be done at least once every 24 hours, with each application consisting of 50-100 ml of the agent. This ensures that a uniform protective film can be continuously formed on the surface of the coal, thereby inhibiting the oxidation reaction of low-rank coal and reducing the amount of CO produced by oxidation.

[0015] When the source-inhibiting inertizer and the fire-prevention grout are mixed at room temperature, the preferred mass ratio of the source-inhibiting inertizer and the fire-prevention grout is (1:5) to (1:10). This mass ratio range allows the source-inhibiting inertizer and the grouting material to be fully integrated and evenly dispersed. While ensuring the fluidity and sealing performance of the grouting material, the source-inhibiting inertizer can also be transported to the deep part of the coal body by utilizing the penetration ability of the grout. At the same time, compared with the use of grout or source-inhibiting inertizer alone, when the source-inhibiting inertizer and the fire-prevention grout are mixed, the source-inhibiting inertizer and the fire-prevention grout work together to increase the range of inertization oxidation, improve the fire prevention and extinguishing effect, and thus effectively reduce the amount of CO produced.

[0016] This source-inhibiting inerting agent is not only suitable for dilution and spraying on the surface of coal at the working face, and for fire extinguishing operations mixed with grout at room temperature, but it can also be applied to other specific application scenarios without significant adjustments to the construction process, while taking into account both its inerting and prevention effects and on-site operation efficiency.

[0017] The beneficial effects of this invention are: (1) Inhibitors and inertizers containing polyglycerol fatty acid esters and / or vitamin E derivatives can target the coordination structure of highly active activating substances in coal. By utilizing the polyhydroxy structure of the inhibitor and inertizer to compete with the metal center of the coordination structure at room temperature, the coordination structure of highly active activating substances is destroyed, thereby inertizing their oxidation activity and greatly reducing CO production. (2) By selecting cycloalkyl mineral oil as the base oil and adding a vacuum-dried inhibitor, the homogeneity of the base oil solution is ensured, and the resulting base oil is in a homogeneous and clear state. Under the premise of keeping the system temperature within a certain range, continuous high-speed shearing is carried out to enhance the dispersion and fusion between the oil phase and the water phase. After the primary emulsion is cooled by gradient, deionized water is continuously added during the continuous stirring process until the mixture is uniform, which improves the stability of the inhibitor and inert agent and gives it excellent inhibition ability. (3) By diluting the source-inhibiting inert agent or mixing it with other fire extinguishing materials and applying it to different scenarios, it can exert its excellent oxidation inertization and prevention effects while ensuring on-site operation efficiency. Attached Figure Description

[0018] Figure 1 This is a graph showing the change in CO gas concentration during the early morning shift when the source-inhibiting inert agent of Embodiment 7 of the present invention was applied to a working face of a mine. Figure 2 This is a graph showing the CO gas concentration change during a mid-shift test of the source-suppressing inert agent used in Example 7 of this invention at a mine working face. Figure 3 This is a graph showing the change in CO gas concentration during the night shift when the source-inhibiting inert agent of Embodiment 7 of the present invention was applied to a working face of a mine. Figure 4 As shown in Comparative Example 1, the oxidation experiment was conducted using the source-inhibiting inert agent and the halide salt inhibitor of the present invention. Gas concentration change graph; Figure 5 As shown in Comparative Example 1, the oxidation experiment was conducted using the source-inhibiting inert agent and the halide salt inhibitor of the present invention. Gas concentration change graph; Figure 6 As shown in Comparative Example 1, the oxidation experiment was conducted using the source-inhibiting inert agent and the halide salt inhibitor of the present invention. Gas concentration change graph; Figure 7 In Comparative Example 2, the source-inhibiting inert agents from Examples 7 and 1-4 were obtained through oxidation experiments. Gas concentration change graph; Figure 8 In Comparative Example 3, the source-inhibiting inert agents from Examples 7 and 5 were tested using oxidation experiments. Gas concentration change graph; Figure 9 In Comparative Example 4, the source-inhibiting inert agents from Examples 7 and 6 were tested using oxidation experiments. Gas concentration change graph; Figure 10 As a comparative example 5, the oxidation of QLS raw coal and QLS inhibited coal samples at room temperature produces... Gas concentration comparison chart; Figure 11 As a comparative example 5, the oxidation of YM raw coal and YM inhibited coal samples under normal temperature conditions... Gas concentration comparison chart; Figure 12 As shown in Comparative Example 5, the oxidation of MDL raw coal and MDL inhibited coal samples at room temperature produces... Gas concentration comparison chart; Figure 13 As a comparative example 5, the oxidation of BJ raw coal and BJ inhibited coal samples under normal temperature conditions... Gas concentration comparison chart; Figure 14 The XRD diffraction patterns of the raw coal sample, inhibited coal sample 1, and inhibited coal sample 2 in Comparative Example 6 are shown in the figure. Detailed Implementation

[0019] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0020] Example 1 A source-inhibiting inert agent for preventing CO over-limit, the source-inhibiting inert agent comprising deionized water and an inhibitory main agent and a base oil in a mass ratio of 1:(1.5-2); wherein the inhibitory main agent is a polyglycerol fatty acid ester and / or a vitamin E derivative; and the base oil is a cycloalkyl mineral oil.

[0021] Six portions of the inhibitor were weighed, wherein the inhibitor was prepared by mixing polyglycerol fatty acid esters and vitamin E derivatives (TPGS) in equal mass. The weighed inhibitor was placed in a vacuum drying oven and dried at 60°C. Vacuum drying for 3 hours under vacuum conditions of (-0.08) to (-0.1) MPa to completely remove free and adsorbed water from the raw material. After drying, remove and cool to room temperature for later use.

[0022] Based on the above-mentioned raw materials, the specific method for preparing the source inhibitor and inerting agent includes the following steps: S1. Preparation of base oil solution: Weigh out the naphthenic mineral oil as the base oil and place it in a three-necked flask equipped with a stirrer. Stir with 5-10... The rate of heating increases to 60 Add the vacuum-dried inhibitor to the heated base oil, and maintain the system temperature at 60°C. Unchanged, at 300-500 Continue stirring at the specified stirring rate for 15-20 minutes until the main inhibitor is completely dissolved and the system is in a homogeneous and clear state, thus obtaining the base oil solution, which is then kept warm for later use.

[0023] S2. Preparation of primary emulsion: Maintain a stable temperature of both the base oil solution and deionized water at 40-60°C. Slowly pour the base oil solution along the wall of the beaker into deionized water. (3000-5000...) The system was subjected to continuous high-speed shearing at a certain rate for 15-20 minutes, during which the system temperature was kept constant; after shearing, a milky white, homogeneous, stable, and non-stratified primary emulsion was obtained.

[0024] S3. Preparation of the finished product source-inhibiting and inertizing agent: The obtained primary emulsion was placed in a cooling device and cooled naturally or by a water bath for 2-3 hours. Stirring at a rate of 30°C and cooling down The preferred temperature is 25-30°C. ; with 150-200 Stir the primary emulsion at a high speed and slowly add an appropriate amount of deionized water, stirring continuously for 5-8 minutes until the system is uniformly mixed; take samples for testing to confirm that the product is a milky white homogeneous emulsion, which does not separate into layers or precipitate after standing for 24 hours, and has a particle size distribution between 100-500nm, thus finally obtaining the source inhibitor and inerting agent for preventing CO over-limit in the upper corner of the downhole working face.

[0025] This source-inhibiting inert agent uses naphthenic mineral oil as the base oil, taking advantage of its good solubility, and is heated in a gradient to 60-70°C. The optimal value is 60. Then add the vacuum-dried inhibitor, keeping the system temperature constant, optimally 60°C. Unchanged, at 300-500 The continuous stirring at a high stirring rate not only accelerated the dissolution of the inhibitor but also removed moisture and impurities from it, ensuring the homogeneity and stability of the base oil solution. The insulated oil phase was then mixed with the water phase, maintaining a constant system temperature, and subjected to continuous high-speed shearing to ensure full integration between the base oil solution and deionized water. Finally, the system temperature was reduced to 30°C using a gradient cooling method. The following steps, including continuous stirring and the addition of deionized water, ensure the dispersibility and stability of the inhibitor, allowing it to perform its optimal inhibition properties.

[0026] The preparation of this source-inhibiting inert agent is simple, requires no extreme conditions, and uses an equal mass mixture of polyglycerol fatty acid esters and vitamin E derivatives (TPGS) as the main inhibitor. This enhances the inertization ability against highly active activating substances in coal and ensures that the main inhibitor is uniformly dispersed in the base oil. The prepared source-inhibiting inert agent can inhibit CO generated by coal oxidation at the source, effectively solving the problem of excessive CO in the upper corner of the well.

[0027] Example 2 A source-inhibiting inert agent for preventing CO over-limit, the source-inhibiting inert agent comprising deionized water, an inhibitory main agent and a base oil in a mass ratio of 1:(1.5-2), and a modifier; wherein the inhibitory main agent is a polyglycerol fatty acid ester and / or a vitamin E derivative; the base oil is a naphthenic mineral oil; and the mass ratio of the inhibitory main agent to the modifier is (5-6):(0.1-0.5).

[0028] Weigh out 6 parts of the inhibitor and 0.5 parts of the modifier. The inhibitor is prepared by mixing polyglycerol fatty acid ester and vitamin E derivative (TPGS) in equal mass. The modifier is prepared by mixing cuprous oxide and cobalt dioxide in equal mass.

[0029] Based on the above-mentioned raw materials, the specific method for preparing the source inhibitor and inerting agent includes the following steps: S1. Preparation of modified inhibitory main agent; S11. Place the weighed inhibitor into a vacuum drying oven at a temperature of 60°C. Vacuum drying for 3 hours under vacuum conditions of (-0.08) - (-0.1) MPa to completely remove free water and adsorbed water from the raw material. After drying, remove and cool to room temperature for later use. S12. Add an appropriate amount of anhydrous ethanol to the weighed modifier, place it in an ultrasonic disperser, and ultrasonically disperse it for 40 minutes at a power of 300W and a frequency of 40kHz. Confirm that the particle size of the modifier in the dispersed suspension is ≤500nm by laser particle size analyzer, and a uniform and stable inorganic suspension is obtained. S13. Preparation of solvent system: Food-grade glycerin and ethanol were mixed to prepare a composite solvent; the inhibitor, after vacuum drying, was added to the composite solvent, and the mixture was placed on a stirring device and stirred at room temperature at 200-300 °C. Stir at a constant speed for 15 minutes until the inhibitor is completely dissolved to obtain a homogeneous and transparent organic solution. S14. Slowly pour the prepared inorganic suspension into the organic solution, first at 600... The mixture was mechanically stirred at a high speed for 2 hours to ensure thorough mixing of the two phases, then transferred to an ultrasonic disperser for ultrasonic treatment for 30 minutes to further improve the homogeneity of the system; subsequently, the mixture was placed in a rotary evaporator and evaporated at 45°C. The anhydrous ethanol and composite solvent in the system were completely removed by vacuum distillation under vacuum conditions of (-0.07) to (-0.09) MPa, and finally a viscous modified inhibitor with no obvious particles and uniform state was obtained and sealed for later use.

[0030] S2, Prepare base oil solution; S21. Weigh out the naphthenic mineral oil as the base oil and place it in a three-necked flask equipped with a stirrer. Stir with 5-10... The rate of heating increases to 60 ; S22. Add the prepared viscous modified inhibitor to the heated base oil at a ratio of 1.5-2 times the mass of the base oil to the mass of the modified inhibitor, and maintain the system temperature at 60°C. Unchanged, at 300-500 Stir continuously at the stirring rate for 15-20 minutes until the modified inhibitor is completely dissolved and the system is in a homogeneous and clear state, thus obtaining the base oil solution, which is then kept warm for later use.

[0031] S3. Prepare the primary emulsion; Maintain a stable temperature of both the base oil solution and deionized water at 40-60°C. Slowly pour the base oil solution along the wall of the beaker into deionized water at a flow rate of 3000-5000 ml. The system was subjected to continuous high-speed shearing at a certain rate for 15-20 minutes, during which the system temperature was kept constant; after shearing, a milky white, homogeneous, stable, and non-stratified primary emulsion was obtained.

[0032] S4. Prepare the finished product source-inhibiting inert agent; S41. Place the obtained primary emulsion in a cooling device and cool it naturally or by water bath for 2-3 minutes. Stirring at a rate of 30°C and cooling down The preferred temperature is 25-30°C. ; S42, with 150-200 Stir the primary emulsion at a high speed and slowly add an appropriate amount of deionized water, continuing to stir for 5-8 minutes until the system is evenly mixed; S43. Sampling and testing confirmed that the product was a milky white homogeneous emulsion that did not separate into layers or precipitate after standing for 24 hours, and had a particle size distribution between 100-500 nm. This was the final source-inhibiting inert agent for preventing CO over-limit in the upper corner of the downhole working face.

[0033] Compared to Example 1, this embodiment introduces a modifier consisting of an equal mass mixture of cuprous oxide and cobalt dioxide to prepare a modified inhibitor, thereby improving the overall performance of the source-inhibiting inert agent. The modifier and the inhibitor work synergistically to achieve multi-target blocking of coal oxidation, improve CO inhibition efficiency, and enhance the inertization effect. Simultaneously, the modified inhibitor exhibits better solubility in naphthenic mineral oils, resulting in a more homogeneous base oil solution and reducing the likelihood of precipitation during subsequent emulsification and cooling processes, thus ensuring the stability of the source-inhibiting inert agent. Furthermore, the modifier demonstrates good chemical stability, stronger resistance to downhole operating conditions, and extended action period.

[0034] Example 3 A source-inhibiting inert agent for preventing CO over-limit, the source-inhibiting inert agent comprising deionized water, a main inhibitor and base oil in a mass ratio of 1:(1.5-2), a modifier, and an emulsifier; wherein the main inhibitor is a polyglycerol fatty acid ester and / or a vitamin E derivative; the base oil is a naphthenic mineral oil; and the mass ratio of the main inhibitor, the modifier, and the emulsifier is (5-6):(0.1-0.5):(1-3).

[0035] Weigh out 6 parts of the inhibitor, 0.5 parts of the modifier, and 2 parts of the emulsifier. The inhibitor is prepared by mixing polyglycerol fatty acid ester and vitamin E derivative (TPGS) in equal mass. The modifier is prepared by mixing cuprous oxide and cobalt dioxide in equal mass. The emulsifier is prepared by mixing lecithin and fatty alcohol polyoxyethylene ether in a mass ratio of 3:2.

[0036] Based on the above-mentioned raw materials, the specific method for preparing the source inhibitor and inerting agent includes the following steps: S1. Preparation of modified inhibitory main agent; S11. Place the weighed inhibitor into a vacuum drying oven at a temperature of 60°C. Vacuum drying for 3 hours under vacuum conditions of (-0.08) - (-0.1) MPa to completely remove free water and adsorbed water from the raw material. After drying, remove and cool to room temperature for later use. S12. Add an appropriate amount of anhydrous ethanol to the weighed modifier, place it in an ultrasonic disperser, and ultrasonically disperse it for 40 minutes at a power of 300W and a frequency of 40kHz. Confirm that the particle size of the modifier in the dispersed suspension is ≤500nm by laser particle size analyzer, and a uniform and stable inorganic suspension is obtained. S13. Preparation of solvent system: Food-grade glycerin and ethanol were mixed to prepare a composite solvent; the inhibitor, after vacuum drying, was added to the composite solvent, and the mixture was placed on a stirring device and stirred at room temperature at 200-300 °C. Stir at a constant speed for 15 minutes until the inhibitor is completely dissolved to obtain a homogeneous and transparent organic solution. S14. Slowly pour the prepared inorganic suspension into the organic solution, first at 600... The mixture was mechanically stirred at a high speed for 2 hours to ensure thorough mixing of the two phases, then transferred to an ultrasonic disperser for ultrasonic treatment for 30 minutes to further improve the homogeneity of the system; subsequently, the mixture was placed in a rotary evaporator and evaporated at 45°C. The anhydrous ethanol and composite solvent in the system were completely removed by vacuum distillation under vacuum conditions of (-0.07) to (-0.09) MPa, and finally a viscous modified inhibitor with no obvious particles and uniform state was obtained and sealed for later use.

[0037] S2, Prepare base oil solution; S21. Weigh out the naphthenic mineral oil as the base oil and place it in a three-necked flask equipped with a stirrer. Stir with 5-10... The rate of heating increases to 60 ; S22. Add the prepared viscous modified inhibitor to the heated base oil at a ratio of 1.5-2 times the mass of the base oil to the mass of the modified inhibitor, and maintain the system temperature at 60°C. Unchanged, at 300-500 Stir continuously at the stirring rate for 15-20 minutes until the modified inhibitor is completely dissolved and the system is in a homogeneous and clear state, thus obtaining the base oil solution, which is then kept warm for later use.

[0038] S3. Preparation of oil-phase emulsion matrix; The prepared base oil solution is then diluted with 3-5 ml of water. The rate of heating increases to 70-75°C Then, slowly add the weighed emulsifier in batches according to the preset proportions; maintain the system temperature at 70-75 degrees Celsius. 300-500 Continue stirring at a constant rate until the emulsifier is completely dispersed and there are no obvious particles in the system; then lower the system temperature to 40-60°C. and with 100-200 By continuously stirring and maintaining the temperature at low speed, a uniform and stable oil-phase emulsion matrix was obtained.

[0039] S4. Prepare the primary emulsion; Maintain a stable temperature of both the oil phase emulsion matrix and deionized water at 40-60°C. Slowly pour the oil-phase emulsion matrix along the beaker wall into deionized water; simultaneously start the high-speed shear emulsifier at 3000-5000... The mixture was subjected to continuous high-speed shearing at a certain rate for 15-20 minutes, while the system temperature was kept constant. After shearing, a milky white, homogeneous, stable primary emulsion without stratification was obtained.

[0040] S5. Prepare the finished product source-inhibiting inert agent; S51. Place the obtained primary emulsion in a cooling device and cool it naturally or by water bath for 2-3 minutes. Stirring at a rate of 30°C and cooling down The preferred temperature is 25-30°C. ; S52. Apply at a ratio of 1-1.2 times the mass of the oil phase emulsifying matrix, using 150-200... Stir the primary emulsion at a high speed and slowly add an appropriate amount of deionized water, continuing to stir for 5-8 minutes until the system is evenly mixed; S53. Sampling and testing confirmed that the product was a milky white homogeneous emulsion that did not separate into layers or precipitate after standing for 24 hours, and had a particle size distribution between 100-500 nm. This was the final source-inhibiting inert agent for preventing CO over-limit in the upper corner of the downhole working face.

[0041] Compared to Examples 1 and 2, this embodiment adds an emulsifier to inhibit the synergistic effect of the main agent, modifier, and emulsifier, further improving the inerting performance of the source-inhibiting inerting agent. The emulsifier is a 3:2 compound of lecithin and fatty alcohol polyoxyethylene ether, which can significantly reduce the interfacial tension between oil and water and enhance the emulsification stability of the system. Compared to Examples 1-2, the finished product of this embodiment showed no stratification or precipitation even after standing for more than 24 hours, and the particle size distribution was more concentrated in the optimal range of 100-500 nm. After adding the emulsifier, the oil phase emulsion matrix and the aqueous phase are more fully integrated, improving the spreadability of the source-inhibiting inerting agent on the coal surface, solving the problem of insufficient permeation of coal pores in Examples 1-2, and enhancing the inerting ability to inhibit the oxidation of coal and the generation of CO.

[0042] Example 4 A source-inhibiting and inertizing agent for preventing CO over-limit, the source-inhibiting and inertizing agent comprising deionized water, an inhibitory main agent and base oil in a mass ratio of 1:(1.5-2), a modifier, an emulsifier, and a stabilizer; wherein the inhibitory main agent is a polyglycerol fatty acid ester and / or a vitamin E derivative; the base oil is a naphthenic mineral oil; the mass ratio of the inhibitory main agent, the modifier, the emulsifier, and the stabilizer is (5-6):(0.1-0.5):(1-3):(6-7).

[0043] Weigh out 6 parts of the inhibitor, 0.5 parts of the modifier, 2 parts of the emulsifier, and 6 parts of the stabilizer. The inhibitor is prepared by mixing polyglycerol fatty acid ester and vitamin E derivative (TPGS) in equal mass. The modifier is prepared by mixing cuprous oxide and cobalt dioxide in equal mass. The emulsifier is prepared by mixing lecithin and fatty alcohol polyoxyethylene ether in a mass ratio of 3:2. The stabilizer is prepared by mixing sodium alginate and sodium hexametaphosphate in equal mass.

[0044] Based on the above-mentioned raw materials, the specific method for preparing the source inhibitor and inerting agent includes the following steps: S1. Preparation of modified inhibitory main agent; S11. Place the weighed inhibitor into a vacuum drying oven at a temperature of 60°C. Vacuum drying for 3 hours under vacuum conditions of (-0.08) - (-0.1) MPa to completely remove free water and adsorbed water from the raw material. After drying, remove and cool to room temperature for later use. S12. Add an appropriate amount of anhydrous ethanol to the weighed modifier, place it in an ultrasonic disperser, and ultrasonically disperse it for 40 minutes at a power of 300W and a frequency of 40kHz. Confirm that the particle size of the modifier in the dispersed suspension is ≤500nm by laser particle size analyzer, and a uniform and stable inorganic suspension is obtained. S13. Preparation of solvent system: Food-grade glycerin and ethanol were mixed to prepare a composite solvent; the inhibitor, after vacuum drying, was added to the composite solvent, and the mixture was placed on a stirring device and stirred at room temperature at 200-300 °C. Stir at a constant speed for 15 minutes until the inhibitor is completely dissolved to obtain a homogeneous and transparent organic solution. S14. Slowly pour the prepared inorganic suspension into the organic solution, first at 600... The mixture was mechanically stirred at a high speed for 2 hours to ensure thorough mixing of the two phases, then transferred to an ultrasonic disperser for ultrasonic treatment for 30 minutes to further improve the homogeneity of the system; subsequently, the mixture was placed in a rotary evaporator and evaporated at 45°C. The anhydrous ethanol and composite solvent in the system were completely removed by vacuum distillation under vacuum conditions of (-0.07) to (-0.09) MPa, and finally a viscous modified inhibitor with no obvious particles and uniform state was obtained and sealed for later use.

[0045] S2, Prepare base oil solution; S21. Weigh out the naphthenic mineral oil as the base oil and place it in a three-necked flask equipped with a stirrer. Stir with 5-10... The rate of heating increases to 60 ; S22. Add the prepared viscous modified inhibitor to the heated base oil at a ratio of 1.5-2 times the mass of the base oil to the mass of the modified inhibitor, and maintain the system temperature at 60°C. Unchanged, at 300-500 Stir continuously at the stirring rate for 15-20 minutes until the modified inhibitor is completely dissolved and the system is in a homogeneous and clear state, thus obtaining the base oil solution, which is then kept warm for later use.

[0046] S3. Preparation of oil-phase emulsion matrix; The prepared base oil solution is then diluted with 3-5 ml of water. The rate of heating increases to 70-75°C Then, slowly add the weighed emulsifier in batches according to the preset proportions; maintain the system temperature at 70-75 degrees Celsius. 300-500 Continue stirring at a constant rate until the emulsifier is completely dispersed and there are no obvious particles in the system; then lower the system temperature to 40-60°C. and with 100-200 By continuously stirring and maintaining the temperature at low speed, a uniform and stable oil-phase emulsion matrix was obtained.

[0047] S4. Prepare an aqueous system; S41. Add the preset amount of deionized water to a clean and dry beaker and place it on a constant temperature stirring device. S42. Add the stabilizer to the deionized water according to the preset ratio, at 200-300... Stir at a constant speed for 5-8 minutes until the stabilizer is completely dissolved; S43, with 3-5 The rate will raise the system temperature to 40-60°C. By maintaining a stable temperature, a homogeneous aqueous system was obtained.

[0048] S5. Prepare the primary emulsion; Maintain a stable temperature of both the oil-phase emulsion matrix and the aqueous system at 40-60°C. Slowly pour the oil-phase emulsion matrix along the beaker wall into the aqueous phase system; simultaneously start the high-speed shear emulsifier at 3000-5000... The mixture was subjected to continuous high-speed shearing at a certain rate for 15-20 minutes, while the system temperature was kept constant. After shearing, a milky white, homogeneous, stable primary emulsion without stratification was obtained.

[0049] S6. Prepare the finished product source-inhibiting inert agent; S61. Place the obtained primary emulsion in a cooling device and cool it naturally or by water bath for 2-3 minutes. Stir at a rate of 20-30°C and cool down. The preferred temperature is 25-30 degrees Celsius. ; S62. Apply at a ratio of 1-1.2 times the mass of the oil phase emulsifying matrix, using 150-200... Stir the primary emulsion at a high speed and slowly add an appropriate amount of deionized water, continuing to stir for 5-8 minutes until the system is evenly mixed; S63. Sampling and testing confirmed that the product was a milky white homogeneous emulsion that did not separate into layers or precipitate after standing for 24 hours, and had a particle size distribution between 100-500 nm. This was the final source-inhibiting inert agent for preventing CO over-limit in the upper corner of the downhole working face.

[0050] Compared to Examples 1-3, this embodiment adds a stabilizer. The added stabilizer, in a corresponding mass ratio, works synergistically with the inhibitor, modifier, and emulsifier, resulting in superior inerting performance of the source-inhibiting inerting agent compared to those in Examples 1-3. The stabilizer is a mixture of sodium alginate and sodium hexametaphosphate by mass, further reducing the risk of demulsification. The source-inhibiting inerting agent remains free of stratification and precipitation even after longer standing time, exhibiting greater stability in the 100-500nm particle size range, and significantly improved resistance to downhole temperature and vibration. Simultaneously, the addition of the stabilizer to the aqueous phase system allows for more complete integration of the aqueous and oil phase emulsion matrix, enhancing the penetration and adhesion persistence of the source-inhibiting inerting agent in coal pores, thus resolving the stability issues of Examples 1-3.

[0051] Example 5 An inhibitory inert agent for preventing CO over-limit, comprising deionized water, an inhibitory main agent and base oil in a mass ratio of 1:(1.5-2), an emulsifier, a stabilizer, and an inhibitory excipient; wherein the inhibitory main agent is a polyglycerol fatty acid ester and / or a vitamin E derivative; the base oil is a naphthenic mineral oil; and the mass ratio of the inhibitory main agent, the emulsifier, the stabilizer, and the inhibitory excipient is (5-6):(1-3):(6-7):(1-2).

[0052] Weigh out 6 parts of the main inhibitor, 2 parts of the emulsifier, 6 parts of the stabilizer, and 1 part of the excipient inhibitor. The main inhibitor is prepared by mixing polyglycerol fatty acid ester and vitamin E derivative (TPGS) in equal mass ratios; the emulsifier is prepared by mixing lecithin and fatty alcohol polyoxyethylene ether in a mass ratio of 3:2; the stabilizer is prepared by mixing sodium alginate and sodium hexametaphosphate in equal mass ratios; and the excipient inhibitor is prepared by mixing borate / boric acid and potassium dihydrogen phosphate / sodium dihydrogen phosphate in a mass ratio of 2:1.

[0053] Based on the above-mentioned raw materials, the specific method for preparing the source inhibitor and inerting agent includes the following steps: S1. Preparation of base oil solution; Weigh out the naphthenic mineral oil as the base oil and place it in a three-necked flask equipped with a stirrer. Stir with 5-10... The rate of heating increases to 60 Add the inhibitor to the heated base oil and maintain the system temperature at 60°C. Unchanged, at 300-500 Continue stirring at the specified stirring rate for 15-20 minutes until the main inhibitor is completely dissolved and the system is in a homogeneous and clear state, thus obtaining the base oil solution, which is then kept warm for later use.

[0054] S2. Preparation of oil-phase emulsion matrix; The prepared base oil solution is then diluted with 3-5 ml of water. The rate of heating increases to 70-75°C Then, slowly add the weighed emulsifier in batches according to the preset proportions; maintain the system temperature at 70-75 degrees Celsius. 300-500 Continue stirring at a constant rate until the emulsifier is completely dispersed and there are no obvious particles in the system; then lower the system temperature to 40-60°C. and with 100-200 By continuously stirring and maintaining the temperature at low speed, a uniform and stable oil-phase emulsion matrix was obtained.

[0055] S3. Preparation of an aqueous system; S31. Add the preset amount of deionized water to a clean and dry beaker and place it on a constant temperature stirring device. S32. Add the stabilizer to the deionized water according to the preset ratio, at 200-300... Stir at a constant speed for 5-8 minutes until the stabilizer is completely dissolved; S33, then add an inhibitory adjuvant and continue at 200-300. Stir at the same rate for 8-10 minutes until the system is mixed evenly with no sediment or suspended particles. S34, with 3-5 The rate will raise the system temperature to 40-60°C. By maintaining a stable temperature, a homogeneous aqueous system was obtained.

[0056] S4. Prepare the primary emulsion; Maintain a stable temperature of both the oil-phase emulsion matrix and the aqueous system at 40-60°C. The oil-phase emulsion matrix is ​​slowly poured into the aqueous phase system along the beaker wall; the temperature error is within... Simultaneously start the high-speed shear emulsifier at 3000-5000 The mixture was subjected to continuous high-speed shearing at a certain rate for 15-20 minutes, while the system temperature was kept constant. After shearing, a milky white, homogeneous, stable primary emulsion without stratification was obtained.

[0057] S5. Prepare the finished product source-inhibiting inert agent; S51. Place the obtained primary emulsion in a cooling device and cool it naturally or by water bath for 2-3 minutes. Stirring at a rate of 30°C and cooling down The preferred temperature is 25-30°C. ; S52. Apply at a ratio of 1-1.2 times the mass of the oil phase emulsifying matrix, using 150-200... Stir the primary emulsion at a high speed and slowly add an appropriate amount of deionized water, continuing to stir for 5-8 minutes until the system is evenly mixed; S53. Sampling and testing confirmed that the product was a milky white homogeneous emulsion that did not separate into layers or precipitate after standing for 24 hours, and had a particle size distribution between 100-500 nm. This was the final source-inhibiting inert agent for preventing CO over-limit in the upper corner of the downhole working face.

[0058] Compared to Examples 2-4, this embodiment replaces the modifier with an inhibitory excipient; compared to Example 4, it retains the emulsifier and stabilizer, and its stability is similar to that of Examples 3-4, but superior to Examples 1-2. No stratification or precipitation occurs after standing for 24 hours, and the particle size remains stable within the optimal range of 100-500 nm. Simultaneous dissolution of the stabilizer and inhibitory excipient in the aqueous phase system ensures uniform dispersion of the inhibitory excipient, enhances the compatibility of the components, and improves the permeability to the coal body.

[0059] Example 6 A source-inhibiting inert agent for preventing CO over-limit, comprising deionized water, a main inhibitor and base oil in a mass ratio of 1:(1.5-2), a modifier, an emulsifier, a stabilizer, and an inhibitory adjuvant; wherein the main inhibitor is a polyglycerol fatty acid ester or a vitamin E derivative; the base oil is a naphthenic mineral oil; and the main inhibitor, modifier, emulsifier, stabilizer, and inhibitory adjuvant are in a mass ratio of (5-6):(0.1-0.5):(2-3):(6-7):(1-1.5).

[0060] Weigh out 6 parts of the main inhibitor, 0.5 parts of the modifier, 2 parts of the emulsifier, 6 parts of the stabilizer, and 1 part of the inhibitory excipient. The main inhibitor is either polyglycerol fatty acid ester or vitamin E derivative (TPGS); the modifier is either cuprous oxide or cobalt dioxide; the emulsifier is either lecithin or fatty alcohol polyoxyethylene ether; the stabilizer is either sodium alginate or sodium hexametaphosphate; and the inhibitory excipient is either borate / boric acid or potassium dihydrogen phosphate / sodium dihydrogen phosphate.

[0061] Based on the above-mentioned raw materials, the specific method for preparing the source inhibitor and inerting agent includes the following steps: S1. Preparation of modified inhibitory main agent; S11. Place the weighed inhibitor into a vacuum drying oven at a temperature of 60°C. Vacuum drying for 3 hours under vacuum conditions of (-0.08) - (-0.1) MPa to completely remove free water and adsorbed water from the raw material. After drying, remove and cool to room temperature for later use. S12. Add an appropriate amount of anhydrous ethanol to the weighed modifier, place it in an ultrasonic disperser, and ultrasonically disperse it for 40 minutes at a power of 300W and a frequency of 40kHz. Confirm that the particle size of the modifier in the dispersed suspension is ≤500nm by laser particle size analyzer, and a uniform and stable inorganic suspension is obtained. S13. Preparation of solvent system: Food-grade glycerin and ethanol were mixed to prepare a composite solvent; the inhibitor, after vacuum drying, was added to the composite solvent, and the mixture was placed on a stirring device and stirred at room temperature at 200-300 °C. Stir at a constant speed for 15 minutes until the inhibitor is completely dissolved to obtain a homogeneous and transparent organic solution. S14. Slowly pour the prepared inorganic suspension into the organic solution, first at 600... The mixture was mechanically stirred at a high speed for 2 hours to ensure thorough mixing of the two phases, then transferred to an ultrasonic disperser for ultrasonic treatment for 30 minutes to further improve the homogeneity of the system; subsequently, the mixture was placed in a rotary evaporator and evaporated at 45°C. The anhydrous ethanol and composite solvent in the system were completely removed by vacuum distillation under vacuum conditions of (-0.07) to (-0.09) MPa, and finally a viscous modified inhibitor with no obvious particles and uniform state was obtained and sealed for later use.

[0062] S2, Prepare base oil solution; Weigh out the naphthenic mineral oil as the base oil and place it in a three-necked flask equipped with a stirrer. Stir with 5-10... The rate of heating increases to 60 Add the prepared viscous modified inhibitor to the heated base oil, and maintain the system temperature at 60°C. Unchanged, at 300-500 Stir continuously at the stirring rate for 15-20 minutes until the modified inhibitor is completely dissolved and the system is in a homogeneous and clear state, thus obtaining the base oil solution, which is then kept warm for later use.

[0063] S3. Preparation of oil-phase emulsion matrix; The prepared base oil solution is then diluted with 3-5 ml of water. The rate of heating increases to 70-75°C Then, slowly add the weighed emulsifier in batches according to the preset proportions; maintain the system temperature at 70-75 degrees Celsius. 300-500 Continue stirring at a constant rate until the emulsifier is completely dispersed and there are no obvious particles in the system; then lower the system temperature to 40-60°C. and with 100-200 By continuously stirring and maintaining the temperature at low speed, a uniform and stable oil-phase emulsion matrix was obtained.

[0064] S4. Prepare an aqueous system; S41. Add the preset amount of deionized water to a clean and dry beaker and place it on a constant temperature stirring device. S42. Add the stabilizer to the deionized water according to the preset ratio, at 200-300... Stir at a constant speed for 5-8 minutes until the stabilizer is completely dissolved; S43, then add an inhibitory adjuvant and continue at 200-300. Stir at the same rate for 8-10 minutes until the system is mixed evenly with no sediment or suspended particles. S44, with 3-5 The rate will raise the system temperature to 40-60°C. By maintaining a stable temperature, a homogeneous aqueous system was obtained.

[0065] S5. Prepare the primary emulsion; Maintain a stable temperature of both the oil-phase emulsion matrix and the aqueous system at 40-60°C. The oil-phase emulsion matrix is ​​slowly poured into the aqueous phase system along the beaker wall; the temperature error is within... Simultaneously start the high-speed shear emulsifier at 3000-5000 The mixture was subjected to continuous high-speed shearing at a certain rate for 15-20 minutes, while the system temperature was kept constant. After shearing, a milky white, homogeneous, stable primary emulsion without stratification was obtained.

[0066] S6. Prepare the finished product source-inhibiting inert agent; S61. Place the obtained primary emulsion in a cooling device and cool it naturally or by water bath for 2-3 minutes. Stirring at a rate of 30°C and cooling down The preferred temperature is 25-30°C. ; S62. Apply at a ratio of 1-1.2 times the mass of the oil phase emulsifying matrix, using 150-200... Stir the primary emulsion at a high speed and slowly add an appropriate amount of deionized water, continuing to stir for 5-8 minutes until the system is evenly mixed; S63. Sampling and testing confirmed that the product was a milky white homogeneous emulsion that did not separate into layers or precipitate after standing for 24 hours, and had a particle size distribution between 100-500 nm. This was the final source-inhibiting inert agent for preventing CO over-limit in the upper corner of the downhole working face.

[0067] The source-inhibiting inert agent provided in this embodiment consists of an inhibitory main agent, a modifier, an emulsifier, a stabilizer, and an inhibitory excipient. Each raw material uses a single chemical, reducing problems such as component antagonism and agglomeration. This source-inhibiting inert agent retains the advantages of modification and emulsification stability, exhibiting stronger inertization properties, stability, and practicality compared to Examples 1-5. The components have a synergistic effect, capable of inertizing highly active activating substances in coal, and its effect in inhibiting CO production is stronger than that of Examples 1-5, with a longer effective duration.

[0068] Example 7 A source-inhibiting inert agent for preventing CO over-limit, comprising deionized water and an inhibitory main agent and base oil in a mass ratio of 1:(1.5-2), as well as a modifier, emulsifier, stabilizer, and inhibitory auxiliary agent; wherein the inhibitory main agent is a mixture of polyglycerol fatty acid ester and vitamin E derivative; the base oil is a naphthenic mineral oil; and the inhibitory main agent, modifier, emulsifier, stabilizer, and inhibitory auxiliary agent are in a mass ratio of (5-6):(0.1-0.5):(2-3):(6-7):(1-1.5).

[0069] Weigh out 6 parts of the main inhibitor, 0.5 parts of the modifier, 2 parts of the emulsifier, 6 parts of the stabilizer, and 1 part of the inhibitory excipient. The main inhibitor is prepared by mixing polyglycerol fatty acid ester and vitamin E derivative (TPGS) in equal mass; the modifier is prepared by mixing cuprous oxide and cobalt dioxide in equal mass; the emulsifier is prepared by mixing lecithin and fatty alcohol polyoxyethylene ether in a mass ratio of 3:2; the stabilizer is prepared by mixing sodium alginate and sodium hexametaphosphate in equal mass; and the inhibitory excipient is prepared by mixing borate / boric acid and potassium dihydrogen phosphate / sodium dihydrogen phosphate in a mass ratio of 2:1.

[0070] Based on the above-mentioned raw materials, the specific method for preparing the source inhibitor and inerting agent includes the following steps: S1. Preparation of modified inhibitory main agent; S11. Place the weighed inhibitor into a vacuum drying oven at a temperature of 60°C. Vacuum drying for 3 hours under vacuum conditions of (-0.08) - (-0.1) MPa to completely remove free water and adsorbed water from the raw material. After drying, remove and cool to room temperature for later use. S12. Add an appropriate amount of anhydrous ethanol to the weighed modifier, place it in an ultrasonic disperser, and ultrasonically disperse it for 40 minutes at a power of 300W and a frequency of 40kHz. Confirm that the particle size of the modifier in the dispersed suspension is ≤500nm by laser particle size analyzer, and a uniform and stable inorganic suspension is obtained. S13. Preparation of solvent system: Food-grade glycerin and ethanol were mixed to prepare a composite solvent; the inhibitor, after vacuum drying, was added to the composite solvent, and the mixture was placed on a stirring device and stirred at room temperature at 200-300 °C. Stir at a constant speed for 15 minutes until the inhibitor is completely dissolved to obtain a homogeneous and transparent organic solution. S14. Slowly pour the prepared inorganic suspension into the organic solution, first at 600... The mixture was mechanically stirred at a high speed for 2 hours to ensure thorough mixing of the two phases, then transferred to an ultrasonic disperser for ultrasonic treatment for 30 minutes to further improve the homogeneity of the system; subsequently, the mixture was placed in a rotary evaporator and evaporated at 45°C. The anhydrous ethanol and composite solvent in the system were completely removed by vacuum distillation under vacuum conditions of (-0.07) to (-0.09) MPa, and finally a viscous modified inhibitor with no obvious particles and uniform state was obtained and sealed for later use.

[0071] S2, Prepare base oil solution; Weigh out the naphthenic mineral oil as the base oil and place it in a three-necked flask equipped with a stirrer. Stir with 5-10... The rate of heating increases to 60 Add the prepared viscous modified inhibitor to the heated base oil, and maintain the system temperature at 60°C. Unchanged, at 300-500 Stir continuously at the stirring rate for 15-20 minutes until the modified inhibitor is completely dissolved and the system is in a homogeneous and clear state, thus obtaining the base oil solution, which is then kept warm for later use.

[0072] S3. Preparation of oil-phase emulsion matrix; The prepared base oil solution is then diluted with 3-5 ml of water. The rate of heating increases to 70-75°C Then, slowly add the weighed emulsifier in batches according to the preset proportions; maintain the system temperature at 70-75 degrees Celsius. 300-500 Continue stirring at a constant rate until the emulsifier is completely dispersed and there are no obvious particles in the system; then lower the system temperature to 40-60°C. and with 100-200 By continuously stirring and maintaining the temperature at low speed, a uniform and stable oil-phase emulsion matrix was obtained.

[0073] S4. Prepare an aqueous system; S41. Add the preset amount of deionized water to a clean and dry beaker and place it on a constant temperature stirring device. S42. Add the stabilizer to the deionized water according to the preset ratio, at 200-300... Stir at a constant speed for 5-8 minutes until the stabilizer is completely dissolved; S43, then add an inhibitory adjuvant and continue at 200-300. Stir at the same rate for 8-10 minutes until the system is mixed evenly with no sediment or suspended particles. S44, with 3-5 The rate will raise the system temperature to 40-60°C. By maintaining a stable temperature, a homogeneous aqueous system was obtained.

[0074] S5. Prepare the primary emulsion; Maintain a stable temperature of both the oil-phase emulsion matrix and the aqueous system at 40-60°C. The oil-phase emulsion matrix is ​​slowly poured into the aqueous phase system along the beaker wall; the temperature error is within... Simultaneously start the high-speed shear emulsifier at 3000-5000 The mixture was subjected to continuous high-speed shearing at a certain rate for 15-20 minutes, while the system temperature was kept constant. After shearing, a milky white, homogeneous, stable primary emulsion without stratification was obtained.

[0075] S6. Prepare the finished product source-inhibiting inert agent; S61. Place the obtained primary emulsion in a cooling device and cool it naturally or by water bath for 2-3 minutes. Stirring at a rate of 30°C and cooling down The preferred temperature is 25-30°C. ; S62. Apply at a ratio of 1-1.2 times the mass of the oil phase emulsifying matrix, using 150-200... Stir the primary emulsion at a high speed and slowly add an appropriate amount of deionized water, continuing to stir for 5-8 minutes until the system is evenly mixed; S63. Sampling and testing confirmed that the product was a milky white homogeneous emulsion that did not separate into layers or precipitate after standing for 24 hours, and had a particle size distribution between 100-500 nm. This was the final source-inhibiting inert agent for preventing CO over-limit in the upper corner of the downhole working face.

[0076] The source-inhibiting inert agent provided in this embodiment consists of an inhibitory main agent, a modifier, an emulsifier, a stabilizer, and an inhibitory auxiliary agent, and each component is a mixture in a specific ratio. Compared with Examples 1-5 and Example 6, this source-inhibiting inert agent has the best inertization performance and stability. It can block coal oxidation at multiple targets, has higher inertization efficiency, and enhanced stability. It does not stratify after standing for 24 hours, and its anti-interference ability and effective time far exceed those of Examples 1-5. Compared with Example 6, it reduces the limitations of the inertization performance of a single raw material, plays a synergistic role, and more uniformly covers the highly active activating substances in the coal body, thus achieving a better inertization effect.

[0077] To verify the actual effectiveness of the heat source suppressant and inerting agent, it was sprayed on the upper corner of the working face of Mine A in the western part of the mine from May 15th to May 19th, 2024. The spraying and injection volumes of the heat source suppressant and inerting agent over the five days were 350 kg, 325 kg, 167 kg, 302 kg, and 287 kg, respectively, totaling 1431 kg. Please refer to [link / reference]. Figure 1-3 Based on the changes in CO concentration in the return air corner of the 5-20111 working face during the morning, noon, and night shifts before and after spraying the source suppressor and inerting agent, it can be seen that after mixing the source suppressor and inerting agent and injecting deionized water at the tail end of the machine, the CO gas concentration decreased significantly during the morning, noon, and night shifts, indicating that the two materials have a very significant effect on the treatment of CO gas in the return air corner.

[0078] Comparative Example 1 Calcium chloride, a commonly used brine salt inhibitor in coal mines, was selected. ) and magnesium chloride ( The source-inhibiting and inertizing agents of this invention were subjected to room-temperature oxidation experiments to verify the room-temperature inhibition effect of the source-inhibiting and inertizing agents of this invention. Specifically: Preparation of inhibited coal samples: Crush fresh coal samples and sieve out 40-80 mesh coal powder, then seal them in a sealed bag for later use; weigh equal amounts of raw coal samples and spray them separately with equal amounts of the brine salt inhibitor calcium chloride ( ), magnesium chloride (halogen salt inhibitor) The present invention describes the preparation of an inhibited coal sample on a raw coal sample using the source-inhibiting inert agent.

[0079] Room temperature oxidation experiment: Each inhibited coal sample was placed into a coal sample container continuously purged with argon gas, and heated to 30°C in a water bath. After drawing in negative pressure, a fixed amount of dry air is immediately introduced. Then, the sensor and thermometer are turned on, and the coal sample is oxidized for 20 hours in the closed pipeline formed by the coal sample container and the sensor. The changes in coal sample temperature and generated gas are recorded.

[0080] The inhibition rates of different inhibitors on the room temperature oxidation of coal samples are shown in Table 1 below: Table 1: Statistical table of inhibition rates of different inhibitors on room temperature oxidation of coal samples

[0081] The inhibition rate refers to the percentage of the difference in CO concentration between the raw coal sample and the inhibited coal sample, divided by the CO concentration produced by the raw coal sample.

[0082] Combination Figure 4-6 It can be concluded that among the three inhibitors, the CO production of coal samples treated with calcium chloride and magnesium chloride halide inhibitors after 20 hours of oxidation was very close to that of raw coal, indicating poor inhibition. In contrast, the source-inhibiting inert agent of this invention exhibits excellent inhibition of the oxidation reaction of coal samples at room temperature, with CO production significantly lower than that of raw coal and coal samples treated with the two halide inhibitors. Therefore, calcium chloride and magnesium chloride cannot effectively inhibit the oxidation reaction of coal at room temperature, while the source-inhibiting inert agent of this invention has a stronger inhibitory effect on highly active activating substances in coal at room temperature, thus providing better inhibition of room-temperature oxidation of coal samples.

[0083] Comparative Example 2 To verify the inhibitory effect of the source-suppressing inertizer of the present invention and the roles of the emulsifier and inhibitory excipient in the source-suppressing inertizer, raw coal samples and inhibited coal samples were prepared, and room temperature oxidation experiments were conducted to verify the inhibitory effect of the source-suppressing inertizer of the present invention in preventing CO over-limit at the upper corner of the underground working face at room temperature. Specifically: Preparation of inhibited coal samples: Fresh coal samples were crushed and sieved to obtain coal powder of 40-80 mesh, which was then placed in sealed bags for later use; multiple 50g portions of Qinglongsi coal samples were weighed and sprayed with 10ml of deionized water, the source inhibitor and inert agent of Example 7 and Examples 1-4, respectively, and were respectively named as raw coal sample, inhibited coal sample 1, inhibited coal sample 2, inhibited coal sample 3, inhibited coal sample 4, and inhibited coal sample 5.

[0084] Room temperature oxidation experiment: The above raw coal samples and each inhibited coal sample were placed into coal sample containers with argon gas continuously flowing through them, and the water bath was heated to 30°C. After drawing in negative pressure, a fixed amount of dry air is immediately introduced. Then, the sensor and thermometer are turned on, and the coal sample is oxidized for 20 hours in the closed pipeline formed by the coal sample container and the sensor. The changes in coal sample temperature and generated gas are recorded.

[0085] Please see Figure 7 Through room-temperature oxidation experiments on raw coal samples and various inhibited coal samples, it was found that the source-inhibiting inert agents of this invention all exhibit excellent inhibition effects under room-temperature conditions, effectively suppressing the amount of CO produced during coal oxidation. Furthermore, during the experiments, the inhibitory excipient stabilized the pH value of the source-inhibiting inert agent at 6.5-7.5, providing a favorable coordination environment; the emulsifier enhanced the penetration and coverage of the source-inhibiting inert agent, thereby improving its inhibition performance.

[0086] Comparative Example 3 To verify the modifying effect of the modifier in the source-inhibiting inert agent on the main inhibitor, raw coal samples and inhibited coal samples were prepared, and room-temperature oxidation experiments were conducted. Specifically: Preparation of inhibited coal sample: Crush and sieve fresh coal sample to obtain 40-80 mesh coal powder, put it into a sealed bag and seal it for later use; weigh a 50g Qinglongsi coal sample, spray 10ml of the source inhibitor and inerting agent in Example 5 to prevent CO from exceeding the limit in the upper corner of the underground working face, and obtain inhibited coal sample 6.

[0087] Room temperature oxidation experiment: The above raw coal sample, inhibited coal sample 1, and inhibited coal sample 6 were respectively placed into coal sample containers continuously purged with argon gas, and heated to 30°C in a water bath. After drawing in negative pressure, a fixed amount of dry air is immediately introduced. Then, the sensor and thermometer are turned on, and the coal sample is oxidized for 20 hours in the closed pipeline formed by the coal sample container and the sensor. The changes in coal sample temperature and generated gas are recorded.

[0088] Please see Figure 8 By comparing the CO production from the oxidation of raw coal samples, inhibited coal sample 1, and inhibited coal sample 6 at room temperature, the modification effect of the modifier on the main inhibitor in the source-inhibiting inert agent used to prevent CO exceeding the upper corner of the underground working face can be verified. The experiment showed that the modifier can modify and optimize the main inhibitor, significantly improving the emulsification and inhibition effects of the source-inhibiting inert agent.

[0089] Comparative Example 4 To further verify the inhibitory effect of the source-inhibiting inert agent and compare the inhibitory effects of single reagents in Example 6 and mixed reagents in Example 7, raw coal samples and inhibited coal samples were prepared and subjected to room temperature oxidation experiments. In Example 6, "single reagents" refers to a single reagent prepared from a single raw material, comprising the main inhibitor, modifier, emulsifier, stabilizer, and inhibitory excipient. In Example 7, "mixed reagents" refers to a mixed reagent prepared from a mixture of raw materials, comprising the main inhibitor, modifier, emulsifier, stabilizer, and inhibitory excipient. The specific experimental procedure is as follows: Preparation of inhibited coal sample: Crush and sieve fresh coal sample to obtain 40-80 mesh coal powder, put it into a sealed bag and seal it for later use; weigh a 50g Qinglongsi coal sample, spray 10ml of the source inhibitor and inerting agent for preventing CO over-limit in the upper corner of the underground working face in Example 6, and obtain inhibited coal sample 7.

[0090] Room temperature oxidation experiment: The above raw coal sample, inhibited coal sample 1, and inhibited coal sample 7 were respectively placed into coal sample containers continuously purged with argon gas, and heated to 30°C in a water bath. After drawing in negative pressure, a fixed amount of dry air is immediately introduced. Then, the sensor and thermometer are turned on, and the coal sample is oxidized for 20 hours in the closed pipeline formed by the coal sample container and the sensor. The changes in coal sample temperature and generated gas are recorded.

[0091] Please see Figure 9 By comparing the CO production at room temperature of raw coal samples, inhibited coal sample 1, and inhibited coal sample 7, it was found that the CO production of inhibited coal sample 1 and inhibited coal sample 7 was much lower than that of raw coal samples. Therefore, both the source inhibitor and inerting agent prepared with a single reagent in Example 6 and the source inhibitor and inerting agent prepared with a mixed reagent in Example 7 have good inhibition effects at room temperature. Furthermore, the CO production of inhibited coal sample 1 is slightly lower than that of inhibited coal sample 7. Therefore, the source inhibitor and inerting agent prepared with a mixed reagent in Example 7 has a slightly stronger inhibition effect at room temperature than the source inhibitor and inerting agent prepared with a single reagent in Example 6.

[0092] Comparative Example 5 To verify the inhibitory effect of the source-inhibiting inert agent of this invention on different types of coal samples, inhibitory coal samples were prepared by selecting different types of raw coal samples, and room temperature oxidation experiments were conducted. Specifically: Preparation of inhibited coal samples: Select coal samples from Qinglongsi, Yimin, Madiliang, and Banji. Crush and sieve the coal samples into 40-80 mesh coal powder, and seal them in sealed bags for later use. Weigh two 50g portions of each of the coal samples, and add 10ml of deionized water and the source inhibitor / inertizer from Example 7 to each sample. These samples are respectively named QLS raw coal, QLS inhibited coal sample, YM raw coal, YM inhibited coal sample, MDL raw coal, MDL inhibited coal sample, BJ raw coal, and BJ inhibited coal sample.

[0093] Room temperature oxidation experiment: The above-mentioned QLS raw coal, QLS inhibited coal sample, YM raw coal, YM inhibited coal sample, MDL raw coal, MDL inhibited coal sample, BJ raw coal, and BJ inhibited coal sample were respectively placed into coal sample containers continuously purged with argon gas, and heated to 30°C in a water bath. After drawing in negative pressure, a fixed amount of dry air is immediately introduced. Then, the sensor and thermometer are turned on, and the coal sample is oxidized for 20 hours in the closed pipeline formed by the coal sample container and the sensor. The changes in coal sample temperature and generated gas are recorded.

[0094] Please see Figure 10-13 By comparing the CO levels produced by QLS raw coal and QLS inhibited coal samples, YM raw coal and YM inhibited coal samples, MDL raw coal and MDL inhibited coal samples, and BJ raw coal and BJ inhibited coal samples, it can be found that the CO levels produced by each inhibited coal sample are significantly lower than those produced by the raw coal sample. Therefore, it can be verified that the source-inhibiting inert agent of the present invention has a good inhibition effect on various types of coal samples at room temperature, and can effectively prevent the problem of CO exceeding the limit in the upper corner of the underground working face.

[0095] Comparative Example 6 To verify the inhibition mechanism of the source-inhibiting inert agent of this invention, the influence of the source-inhibiting inert agent on the coordination structure of highly active excitation substances in coal molecules was analyzed by XRD, that is, the influence of the source-inhibiting inert agent on the aromatic microcrystalline structure of coal molecules was analyzed. Specifically: Coal samples were selected: raw coal samples, inhibited coal sample 1 after spraying with the source suppressor and inerting agent in Example 7, and inhibited coal sample 2 after spraying with the source suppressor and inerting agent in Example 1.

[0096] The microcrystalline structure of the raw coal sample, inhibited coal sample 1, and inhibited coal sample 2 were tested using a Japanese XRD-7000 X-ray diffractometer as follows: The raw coal sample, inhibited coal sample 1, and inhibited coal sample 2 were placed evenly on the surface of an aluminum frame, and then scanned using copper target irradiation. The angular range is The tube voltage is 40kV, the tube current is 30mA, and the scanning speed is 4. To obtain Figure 14 The XRD diffraction patterns of the raw coal sample, inhibited coal sample 1, and inhibited coal sample 2 are shown in the comparison diagram.

[0097] Through comparative experimental analysis, it was found that the source-inhibiting inert agent of the present invention can affect the aromatic microcrystalline structure of coal molecules, destroy the excitation structure, and thus effectively inhibit the oxidation reaction of coal samples.

[0098] It should be noted that this application is not limited to the above-described embodiments. The above embodiments are merely examples, and any embodiments with the same structure and effect as the technical concept within the scope of this application are included in the technical scope of this application. Furthermore, various modifications that can be conceived by those skilled in the art to the embodiments, and other ways of constructing by combining some of the constituent elements of the embodiments, without departing from the spirit of this application, are also included in the scope of this application.

Claims

1. A source-inhibiting inerting agent for preventing CO over-limit, characterized in that, The source-inhibiting inert agent comprises a main inhibitor and base oil in a mass ratio of 1:(1.5-2); The inhibitor is prepared by mixing polyglycerol fatty acid ester and vitamin E derivative TPGS in equal mass; the base oil is a naphthenic mineral oil.

2. The source-inhibiting inert agent for preventing CO over-limit as described in claim 1, characterized in that, The source-inhibiting inert agent also includes at least one of the following: modifier, emulsifier, stabilizer, and inhibitory excipient.

3. The source-inhibiting inert agent for preventing CO over-limit as described in claim 2, characterized in that, The inhibitor, modifier, emulsifier, stabilizer and inhibitory excipient are mixed in the following mass ratio: (5-6): (0.1-0.5): (2-3): (6-7): (1-1.5).

4. The source-inhibiting inert agent for preventing CO over-limit as described in claim 3, characterized in that, The modifier is at least one of cuprous oxide and cobalt dioxide; when the modifier is a mixture of cuprous oxide and cobalt dioxide, the mass ratio of cuprous oxide to cobalt dioxide is (1-1.5):1; The emulsifier is at least one of lecithin and fatty alcohol polyoxyethylene ether; when the emulsifier is a mixture of lecithin and fatty alcohol polyoxyethylene ether, the mass ratio of lecithin to fatty alcohol polyoxyethylene ether is (1-1.5):

1. The stabilizer is at least one of sodium alginate and sodium hexametaphosphate; when the stabilizer is a mixture of sodium alginate and sodium hexametaphosphate, the mass ratio of sodium alginate to sodium hexametaphosphate is (1.5-2):(1-1.5). The inhibitory excipient is at least one of borate / boric acid and potassium dihydrogen phosphate / sodium dihydrogen phosphate; when the inhibitory excipient is a mixture of borate / boric acid and potassium dihydrogen phosphate / sodium dihydrogen phosphate, the mass ratio of borate / boric acid to potassium dihydrogen phosphate / sodium dihydrogen phosphate is (1-2):

1.

5. A method for preparing the source-inhibiting inert agent as described in any one of claims 1-4, characterized in that, Includes the following steps: The base oil is gradually heated to 60-70°C. Add the vacuum-dried inhibitor, keep the system temperature constant, stir to dissolve, and obtain a homogeneous and clear base oil solution; Pour the base oil solution into deionized water, maintaining the system temperature at 40-60°C. High-speed shearing yields a stable, non-stratified primary emulsion; The primary emulsion was gradually cooled to 30°C. The mixture was stirred continuously and deionized water was added until it was evenly mixed. After standing, a milky white, uniform source inhibitor and inert agent with no stratification or precipitation and a particle size distribution between 100-500nm was obtained.

6. The method for preparing the source-inhibiting inert agent as described in claim 5, characterized in that, The vacuum drying process refers to placing the inhibitor in a vacuum drying oven and drying it for 3 hours at a temperature of 60°C and a vacuum degree of (-0.08) - (-0.1) MPa. The heating rate of the gradient heating is 5-10. The cooling rate of the gradient cooling is 2-3. .

7. The method for preparing the source-inhibiting inert agent as described in claim 5, characterized in that, The inhibitor is a modified inhibitor; The preparation of the modified inhibitor includes: Anhydrous ethanol was added to a pre-prepared modifier and then subjected to nanoscale ultrasonic dispersion to obtain an inorganic suspension. A composite solvent was prepared by mixing glycerol and ethanol, and an inhibitor that had been vacuum dried was added. The mixture was stirred and dissolved to obtain an organic solution. An inorganic suspension and an organic solution were mixed, and the mixture was subjected to ultrasonic treatment to remove anhydrous ethanol and composite solvent from the system, thereby obtaining a modified inhibitor.

8. The application of the source-inhibiting inert agent as described in any one of claims 1-4 in preventing CO exceedance at the upper corner of the working face in underground coal mines, characterized in that, When the source-inhibiting inert agent is sprayed onto the coal face, it should be diluted with deionized water to a mass concentration of 10%-15%, and sprayed at least once every 24 hours, with each spray being 50-100 ml. ; The mass ratio of the source-inhibiting inert agent to the fire-prevention and extinguishing grout is (1:5)-(1:10).

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