Preparation process of mining inorganic nano quick-setting environment-friendly material

Abstract

The invention belongs to the technical field of mining grouting materials, and particularly relates to a preparation process of a mining inorganic nano quick-setting environment-friendly material, which comprises the following steps: (1) preparing magnetic nanoparticles with different coating thicknesses by adopting a co-separation extraction method; (2) adding the magnetic nanoparticles with different coating thicknesses prepared in the step (1) into a liquid A and / or a liquid B of the double-component grouting material as a raw material of the double-component grouting material; and (3) uniformly mixing the solution A and the solution B to obtain the mineral inorganic nano quick-setting environment-friendly material. The multiple stirring devices are arranged, the reaction raw materials in the different stirring devices are different in proportion, the materials in the stirring devices are sequentially subjected to solid-liquid separation and drying, and the different dried materials are mixed in the mixing device and then calcined, so that the gradient magnetic nanoparticles can be rapidly prepared at low cost; when a magnetic field assists in grouting, the dispersity is higher, the gelation time can be shortened, and the impermeability and the water plugging effect are improved.

Description

Technical Field

[0001] The invention belongs to the technical field of mining grouting materials, and in particular relates to a preparation process of an inorganic nano quick-setting environmentally friendly material for mining. Background Art

[0002] In the field of deep mining, under the influence of high ground stress and strong mining action, the broken coal mine roadway has brought a threat to the safe production of coal mines, and grouting reinforcement is a powerful means to control the broken coal rock mass in the roadway. Many studies on grouting reinforcement materials have been carried out in the prior art. For example, CN117986495A discloses a hot water-resistant acrylate grouting material and a preparation method thereof, and improves the crosslinking density of the polymer generated by acrylate polymerization by improving the crosslinking agent. Although organic polymer material is a good anti-seepage plugging slurry material, it can solve the problem of broken coal rock mass to a certain extent, but its cost is relatively high, and there are major safety hazards such as corrosiveness, toxicity, flammability, and easy aging in application, which brings unstable factors to the safe production of coal mines. Therefore, some new inorganic reinforcement materials for mining have emerged, such as CN114751714A discloses a mining inorganic quick-setting double liquid grouting reinforcement material, which avoids the large-scale use of polymer materials, and the nano-active material therein has good impermeability and water blocking effect after magnetization treatment.

[0003] In actual application, the inventors found that when grouting, under a magnetic field of a specific strength, the magnetic nanoparticles with a certain magnetic gradient are more easily adapted to the magnetic field force at different positions, and thus more easily achieve rapid and uniform dispersion of the slurry, optimize the gel time and anti-seepage performance of the slurry and the water plugging effect. To this end, magnetic nanoparticles with different coating thicknesses are prepared in advance before construction, and then mixed in proportion when preparing the slurry. However, this method requires the preparation and extraction of magnetic nanoparticles from different preparation batches separately, and the steps are cumbersome and time-consuming. Summary of the invention

[0004] In order to solve the problems of the background technology, the present invention provides a preparation process of an inorganic nano quick-setting environmentally friendly material for mining.

[0005] The technical solution of the present invention is as follows:

[0006] The present invention provides a preparation process of an inorganic nanometer quick-setting environmentally friendly material for mining, comprising the following steps:

[0007] (1) Magnetic nanoparticles with different coating thicknesses were prepared by co-separation and extraction method;

[0008] (2) adding the magnetic nanoparticles with different coating thicknesses prepared in step (1) as raw materials for a two-component grouting material to liquid A and / or liquid B of the two-component grouting material;

[0009] (3) The liquid A and the liquid B are mixed evenly to obtain the inorganic nano quick-setting environmentally friendly material for mining.

[0010] Preferably, the co-separation and extraction method specifically comprises the following steps:

[0011] S1: The controller controls the stirring device to produce a first mixed material having magnetic metal precursors of different weights, specifically:

[0012] S11: water and surfactant enter into a plurality of stirring devices through a first pipeline and a first feeding part respectively, so that the surfactant and water are evenly mixed;

[0013] S12: When the water reaches a first preset flow rate and the surfactant reaches a first weight threshold, the controller controls the first pipeline and the first feed section to stop working, and no water and surfactant are added to the stirring device; the controller controls the second feed section to feed the magnetic metal precursor nickel nitrate and / or ferric nitrate into multiple stirring devices, and the preset weight threshold of the magnetic metal precursor in each stirring device is different, and stirring is continued to mix evenly;

[0014] S13: When the magnetic metal precursor reaches the corresponding preset weight threshold, the controller controls the second feeding part to stop working, and no longer adds the magnetic metal precursor to the stirring device; the controller controls the second pipeline to work, so that the concentrated ammonia water enters the stirring device, and continues to stir and mix evenly;

[0015] S14: When the pH value of the solution reaches a preset pH value, the controller controls the second pipeline to stop working, and no more concentrated ammonia water is added to the stirring device; the controller controls the third pipeline to work, so that the ethyl orthosilicate enters the stirring device, and continues to stir and mix evenly;

[0016] S15: When the ethyl orthosilicate reaches the second preset flow rate, the controller controls the third pipeline to stop working, and no longer adds ethyl orthosilicate to the stirring device; the controller controls the fourth pipeline to work, so that ethanol enters the stirring device, continues to stir, and mixes evenly to obtain the first mixed material of the corresponding stirring device;

[0017] S2: The controller controls the first mixed material of one of the stirring devices to enter the separation device through the first feeding part;

[0018] S3: adding ethanol through the fifth pipeline, and after several alcohol washings, obtaining a second mixed material;

[0019] S4: The controller controls the second feeding part to work, so that the second mixed material starts to enter the drying device and is dried to obtain the third mixed material;

[0020] After the second mixed material completely enters the drying device, the controller controls the first mixed material of the remaining stirring device to enter the separation device through the first feeding part, and starts to repeat step S3. During the alcohol washing, the controller controls the third feeding part to work, so that the third mixed material enters the mixing device;

[0021] S5: After all the third mixed materials of different stirring devices enter the mixing device, they are mixed to obtain a fourth mixed material;

[0022] After the mixing is completed, when the controller controls the third feeding part to stop working, step S1 is repeated, and the controller controls the first pipeline and the first feeding part to work. During this period, the controller controls the fourth feeding part to work and delivers the fourth mixed material to the calcining device.

[0023] Furthermore, the first feeding part and the second feeding part are both provided with weight sensors, and the controller calculates the addition amount of the surfactant and the magnetic metal precursor according to the weight sensor signal.

[0024] The first pipeline, the third pipeline, the fourth pipeline and the fifth pipeline are all provided with flow meters, and the controller calculates the addition amount of water, tetraethyl orthosilicate and ethanol according to the flow signal.

[0025] The stirring device is provided with a pH sensor, and the controller calculates the addition amount of concentrated ammonia water according to the pH sensor signal.

[0026] The working states of the first material feeding part, the second material feeding part, the third material feeding part and the fourth material feeding part are controlled by valves arranged in the material feeding channels.

[0027] The separation device is also provided with a sixth pipeline for removing separation waste liquid.

[0028] Preferably, the surfactant is sodium dodecylbenzene sulfonate or sodium fatty alcohol ether sulfate.

[0029] The concentrated ammonia water is ammonia water with a mass concentration of 19%-35%.

[0030] The calcination is carried out at 250-270° C. for 2-4 hours.

[0031] Beneficial Effects

[0032] The present invention adopts a co-separation and extraction method to prepare magnetic nanoparticles with different coating thicknesses when preparing inorganic nano-speed setting environmental protection materials for mining, and then adds the prepared magnetic nanoparticles with different coating thicknesses as raw materials for two-component grouting materials to liquid A and / or liquid B of the two-component grouting materials, and then evenly mixes the liquid A and liquid B to obtain the inorganic nano-speed setting environmental protection materials for mining, which is easier to adapt to the magnetic field force at different positions in the magnetic field-assisted grouting construction, and then it is easier to achieve rapid and uniform dispersion of the slurry, and the gel time and anti-seepage performance and water blocking effect of the slurry can be further improved. In particular, the co-separation and extraction method is adopted to prepare magnetic nanoparticles with different coating thicknesses, and by adopting multiple stirring devices, the reaction raw materials in different stirring devices have different ratios, the materials in the stirring devices are sequentially subjected to solid-liquid separation and drying, and the different dried materials are mixed in the mixing device and then calcined, so that magnetic nanoparticles with gradient composition can be prepared more quickly, efficiently and at low cost. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] Figure 1 The present invention is a process flow chart for preparing the inorganic nanometer quick-setting environmentally friendly material for mining.

[0034] Figure 2 A simplified diagram of a system for preparing an inorganic nanometer quick-setting environmentally friendly material for mining provided in an embodiment of the present invention.

[0035] Figure 3 for Figure 2 Example of piping arrangement for a medium mixing device.

[0036] Description of reference numerals:

[0037] 1. stirring device, 11. first pipeline, 12. second pipeline, 13. third pipeline, 14. fourth pipeline, 15. first feeding section, 16. second feeding section, 17. first conveying section, 2. separation device, 21. fifth pipeline, 22. sixth pipeline, 23. second conveying section, 3. drying device, 34. third conveying section, 4. mixing device, 45. fourth conveying section, 5. calcining device. DETAILED DESCRIPTION

[0038] The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the accompanying drawings in the embodiments of the present invention.

[0039] Example 1

[0040] A preparation process of inorganic nanometer quick-setting environmentally friendly material for mining, comprising the following steps:

[0041] (1) Magnetic nanoparticles with different coating thicknesses were prepared by co-separation and extraction method.

[0042] (2) Adding the magnetic nanoparticles with different coating thicknesses prepared in step (1) as raw materials for a two-component grouting material into liquid A and / or liquid B of the two-component grouting material.

[0043] (3) The liquid A and the liquid B are mixed evenly to obtain the inorganic nano quick-setting environmentally friendly material for mining.

[0044] The co-separation and extraction method referred to in this embodiment means that when preparing magnetic nanoparticles with different coating thicknesses, magnetic nanoparticles with different coating thicknesses are not prepared separately and then mixed in proportion when preparing the slurry, but multiple stirring devices are directly used for online reaction production. The proportions of the reaction raw materials (magnetic material precursor raw materials and SiO2 drive raw materials) in different stirring devices are different. The multiple stirring devices use a common set of product separation and extraction systems. The prepared magnetic nanoparticles with different coating thicknesses are mixed online in the mixing device and then calcined together. This co-separation and extraction method can prepare magnetic nanoparticles with gradient composition more quickly, efficiently and at a low cost.

[0045] The inorganic nanometer quick-setting environmentally friendly material for mining prepared in step (1) can be used as one of the raw materials of the two-component grouting material in the following step (2). It can be added to liquid A which is mainly composed of powder, and can also be added to liquid B which is a solidifying liquid. Before construction, the inorganic nanometer quick-setting environmentally friendly material for mining of the present invention can be obtained by evenly mixing liquid A and liquid B in step (3).

[0046] Example 2

[0047] This embodiment mainly provides an industrialized means for realizing the co-separation and extraction method based on the embodiment 1.

[0048] For a clearer understanding, this example first introduces a preparation system used in the present invention, such as Figure 2 As shown, it includes a stirring device 1, a separation device 2, a drying device 3, a mixing device 4, and a calcining device 5.

[0049] The three stirring devices 1 are connected to the separation devices 2 via the first feeding parts 17 , respectively. The first feeding parts 17 are all provided with valves to control the working state so that the materials in the stirring devices 1 enter the separation devices 2 in sequence.

[0050] For each stirring device 1, Figure 3 As shown. A stirring shaft is provided in the stirring device for uniformly mixing the materials. A first pipeline 11, a second pipeline 12, a third pipeline 13, a fourth pipeline 14, a first feed part 15, and a second feed part 16 are provided above the stirring device for adding water, concentrated ammonia water, tetraethyl orthosilicate, ethanol, a surfactant, and a magnetic metal precursor nickel nitrate and / or iron nitrate, respectively.

[0051] A fifth pipeline 21 is provided above the separation device 2 for adding ethanol into the separation device 2. A sixth pipeline 22 is provided on the side wall of the separation device 2 for discharging separation waste liquid.

[0052] The separation device 2 is connected to the drying device 3 via the second feeding part 23 at its lower part. The drying device 3 is connected to the mixing device 4 via the third feeding part 34 . The mixing device 4 is connected to the calcining device 5 via the fourth feeding part 45 .

[0053] The working states of the second material delivery part 23 , the third material delivery part 34 and the fourth material delivery part 45 are controlled by valves arranged in the material delivery channels.

[0054] The system can adapt to the production process and synchronously obtain magnetic nanoparticles with different coating thicknesses online.

[0055] Specifically, the preparation steps of this embodiment can be as follows:

[0056] S1: The controller controls the multiple stirring devices 1 to produce a first mixed material with different raw material addition amounts, specifically:

[0057] S11: Water and surfactant enter into a plurality of stirring devices 1 through a first pipeline 11 and a first feed part 15 respectively, so that the surfactant and water are evenly mixed.

[0058] Wherein, the surfactant is sodium dodecylbenzene sulfonate or sodium fatty alcohol ether sulfate.

[0059] S12: When the water reaches the first preset flow rate and the surfactant reaches the first weight threshold, the controller controls the first pipeline 11 and the first feed part 15 to stop working, and no longer add water and surfactant to the stirring device 1; the controller controls the second feed part 16 to feed the magnetic metal precursor nickel nitrate and / or iron nitrate into multiple stirring devices 1, and the preset weight threshold of the magnetic metal precursor in each stirring device 1 is different, and stirring continues to be uniform.

[0060] S13: When the magnetic metal precursor reaches the corresponding preset weight threshold, the controller controls the second feed part 16 to stop working and no longer add the magnetic metal precursor to the stirring device 1; the controller controls the second pipeline 12 to work, so that the concentrated ammonia water enters the stirring device 1, and continues to stir and mix evenly.

[0061] Preferably, the concentrated ammonia water is ammonia water with a mass concentration of 19%-35%.

[0062] S14: When the pH value of the solution reaches the preset pH value, the controller controls the second pipeline 12 to stop working, and no more concentrated ammonia water is added to the stirring device 1; the controller controls the third pipeline 13 to work, so that the ethyl orthosilicate enters the stirring device 1, and continues to stir and mix evenly.

[0063] S15: When the ethyl orthosilicate reaches the second preset flow rate, the controller controls the third pipeline 13 to stop working, and no longer adds ethyl orthosilicate to the stirring device 1; the controller controls the fourth pipeline 14 to work, so that ethanol enters the stirring device 1, continues to stir, and mixes evenly to obtain the first mixed material of the corresponding stirring device 1.

[0064] S2: The controller controls the first mixed material of one of the stirring devices 1 to enter the separation device 2 through the first feeding part 17 .

[0065] Solid-liquid separation is carried out in the separation device 2 to preserve the solid material.

[0066] S3: adding ethanol through the fifth pipeline 21, and after several alcohol washings, obtaining a second mixed material.

[0067] The separation device 2 is also provided with a sixth pipeline 22 for discharging separation waste liquid.

[0068] S4: The controller controls the second feeding part 23 to work, so that the second mixed material starts to enter the drying device 3 and is dried to obtain the third mixed material;

[0069] After the second mixed material completely enters the drying device 3, the controller controls the first mixed material of the remaining stirring device 1 to enter the separation device 2 through the first feeding part 17, and starts to repeat step S3. During the alcohol washing, the controller controls the third feeding part 34 to work, so that the third mixed material enters the mixing device 4.

[0070] S5: After all the third mixed materials from different stirring devices 1 enter the mixing device 4, they are mixed to obtain a fourth mixed material;

[0071] After the mixing is completed, when the controller controls the third feeding part 34 to stop working, step S1 is repeated, and the controller controls the first pipeline 11 and the first feeding part 15 to work. During this period, the controller controls the fourth feeding part 45 to work to deliver the fourth mixed material to the calcining device 5.

[0072] Preferably, the calcination is carried out at 250-270° C. for 2-4 hours.

[0073] After the fourth mixed material is sent to the calcining device for calcination, the inorganic nano-rapid-setting environmentally friendly material for mining is obtained, which can be used as one of the raw materials of grouting material for magnetic field-assisted grouting construction. It can be added to liquid A which is mainly composed of powder, and can also be added to liquid B which is a solidifying phase. For example, the grouting material is composed of liquid A and liquid B, and the components of liquid A are inorganic nano-rapid-setting environmentally friendly material for mining, cement, citric acid, fly ash, and water, and the components of liquid B are water, ultrafine limestone, and water glass.

[0074] It should be noted that although this embodiment preferentially achieves the purpose of different ratios of reaction raw materials by using different preset weight thresholds of the magnetic metal precursor in each stirring device 1, it is obvious that those skilled in the art can achieve this purpose by arbitrarily changing one or more other raw materials.

[0075] Preferably, the first feed section 15 and the second feed section 16 are both provided with weight sensors, and the controller calculates the addition amount of the surfactant and the magnetic metal precursor according to the weight sensor signal, so that the size of the obtained core-shell structure has obvious differences.

[0076] In this embodiment, in order to simultaneously obtain inorganic nanometer quick-setting environmentally friendly materials for mining with different specifications, multiple stirring devices 1 are provided, and different stirring devices 1 have different raw material addition amounts. The materials in the stirring devices 1 are sequentially subjected to solid-liquid separation and drying, and the different dried materials are mixed in the mixing device 4 and then calcined. This process can prepare inorganic nanometer quick-setting environmentally friendly materials for mining with obvious size differences, with obvious gradient composition after magnetic treatment, high dispersibility, avoid aggregation, and thus increase the fluidity of the grouting material, shorten the gel time, improve the impermeability and water blocking effect, and have high compressive strength, and can avoid the complexity of production equipment and improve production efficiency.

[0077] In this embodiment, the first pipeline 11, the third pipeline 13, the fourth pipeline 14 and the fifth pipeline 21 are all provided with flow meters, and the controller calculates the addition amount of water, tetraethyl orthosilicate and ethanol according to the flow signal.

[0078] The stirring device is provided with a pH sensor, and the controller calculates the addition amount of concentrated ammonia water according to the pH sensor signal.

[0079] Meanwhile, for the convenience of control, the working states of the first feeding part 17 , the second feeding part 23 , the third feeding part 34 and the fourth feeding part 45 are controlled by valves arranged in the feeding channels.

[0080] The above description is only a preferred embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Any changes or substitutions that can be easily conceived by any technician familiar with the technical field within the technical scope disclosed by the present invention should be covered within the protection scope of the present invention.

Claims

1. A preparation process of inorganic nano quick-setting environmentally friendly materials for mining, characterized in that: The steps include: (1) Magnetic nanoparticles with different coating thicknesses were prepared by co-separation and extraction method; (2) adding the magnetic nanoparticles with different coating thicknesses prepared in step (1) as raw materials for a two-component grouting material to liquid A and / or liquid B of the two-component grouting material; (3) The liquid A and the liquid B are mixed evenly to obtain the inorganic nano quick-setting environmentally friendly material for mining.

2. The preparation process of a mining inorganic nano quick-setting environmentally friendly material according to claim 1, characterized in that: The co-separation and extraction method specifically comprises the following steps: S1: The controller controls the stirring device (1) to produce a first mixed material having magnetic metal precursors of different weights, specifically: S11: water and surfactant enter into a plurality of stirring devices (1) through a first pipeline (11) and a first feed section (15) respectively, so that the surfactant and water are evenly mixed; S12: When the water reaches a first preset flow rate and the surfactant reaches a first weight threshold, the controller controls the first pipeline (11) and the first feed section (15) to stop working and no longer add water and surfactant to the stirring device (1); the controller controls the second feed section (16) to feed the magnetic metal precursor nickel nitrate and / or iron nitrate into a plurality of stirring devices (1), wherein the preset weight threshold of the magnetic metal precursor in each stirring device (1) is different, and stirring is continued to ensure uniform mixing; S13: When the magnetic metal precursor reaches a corresponding preset weight threshold, the controller controls the second feed part (16) to stop working, and no longer feeds the magnetic metal precursor into the stirring device (1); the controller controls the second pipeline (12) to work, so that the concentrated ammonia water enters the stirring device (1), and continues stirring to mix evenly; S14: When the pH value of the solution reaches a preset pH value, the controller controls the second pipeline (12) to stop working, and no more concentrated ammonia water is added to the stirring device (1); the controller controls the third pipeline (13) to work, so that the ethyl orthosilicate enters the stirring device (1), and continues to stir and mix evenly; S15: When the amount of tetraethyl orthosilicate reaches a second preset flow rate, the controller controls the third pipeline (13) to stop working, and no longer adds tetraethyl orthosilicate to the stirring device (1); the controller controls the fourth pipeline (14) to work, so that ethanol enters the stirring device (1), and continues stirring and mixing evenly, thereby obtaining a first mixed material of the corresponding stirring device (1); S2: The controller controls the first mixed material of one of the stirring devices (1) to enter the separation device (2) through the first feeding part (17); S3: adding ethanol through the fifth pipeline (21), and washing with alcohol several times to obtain a second mixed material; S4: the controller controls the second material feeding part (23) to operate, so that the second mixed material starts to enter the drying device (3) and is dried to obtain a third mixed material; After the second mixed material completely enters the drying device (3), the controller controls the first mixed material of the remaining stirring device (1) to enter the separation device (2) through the first feeding part (17), and starts to repeat step S3. During the alcohol washing, the controller controls the third feeding part (34) to operate, so that the third mixed material enters the mixing device (4); S5: After all the third mixed materials from the different stirring devices (1) enter the mixing device (4), they are mixed to obtain a fourth mixed material; After the mixing is completed, when the controller controls the third feeding part (34) to stop working, step S1 is repeated, and the controller controls the first pipeline (11) and the first feeding part (15) to work. During this period, the controller controls the fourth feeding part (45) to work to deliver the fourth mixed material to the calcining device (5).

3. The preparation process of inorganic nano quick-setting environmentally friendly material for mining according to claim 2 is characterized in that: The first feeding part (15) and the second feeding part (16) are both provided with weight sensors, and the controller calculates the addition amount of the surfactant and the magnetic metal precursor according to the weight sensor signal.

4. The preparation process of inorganic nano quick-setting environmentally friendly material for mining according to claim 2 is characterized in that: The first pipeline (11), the third pipeline (13), the fourth pipeline (14) and the fifth pipeline (21) are all provided with flow meters, and the controller calculates the addition amount of water, tetraethyl orthosilicate and ethanol according to the flow signal.

5. The preparation process of inorganic nano quick-setting environmentally friendly material for mining according to claim 2, characterized in that: The stirring device is provided with a pH sensor, and the controller calculates the addition amount of concentrated ammonia water according to the pH sensor signal.

6. The preparation process of inorganic nano quick-setting environmentally friendly material for mining according to claim 2, characterized in that: The working states of the first material delivery part (17), the second material delivery part (23), the third material delivery part (34) and the fourth material delivery part (45) are controlled by valves arranged in the material delivery channels.

7. The preparation process of inorganic nanometer quick-setting environmentally friendly material for mining according to claim 2, characterized in that: The separation device (2) is also provided with a sixth pipeline (22) for removing separation waste liquid.

8. The preparation process of inorganic nanometer quick-setting environmentally friendly material for mining according to claim 2 is characterized in that: The surfactant is sodium dodecylbenzene sulfonate or sodium fatty alcohol ether sulfate.

9. The preparation process of inorganic nano quick-setting environmentally friendly material for mining according to claim 2, characterized in that: The concentrated ammonia water is ammonia water with a mass concentration of 19%-35%.

10. The preparation process of inorganic nanometer quick-setting environmentally friendly material for mining according to claim 2, characterized in that: The calcination is carried out at 250-270° C. for 2-4 hours.

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