Ultrahigh-water inorganic cemented filling and fire preventing and extinguishing material as well as preparation method and application thereof

Abstract

The invention provides an ultrahigh-water inorganic cemented filling and fire preventing and extinguishing material as well as a preparation method and application thereof. The material comprises a material A and a material B in a mass ratio of (6-8): 1, the material A is prepared from the following raw materials in parts by weight: 36 to 50 parts of fluidized bed combustion ash, 90 to 120 parts of phosphate tailings, 4.5 to 13 parts of water glass, 7.5 to 27.5 parts of calcium oxide, 3 to 4.5 parts of sodium sulfate and 36 to 100 parts of auxiliaries; the material B is prepared from the following raw materials in parts by weight: 3.5 to 4.5 parts of sodium aluminate, 7 to 7.5 parts of sodium carbonate, 5.5 to 6.5 parts of calcium oxide, 8 to 10.5 parts of anhydrous calcium sulfate and 1.5 to 2.5 parts of bentonite. The water cement ratio of the material is high, and the performance requirements of high-water-content materials for coal mine underground filling and fire prevention and extinguishing are met. In addition, the invention further provides a preparation method of the material, and the preparation process is simple and low in process cost. Finally, the material is applied to a coal mine goaf.

Description

Technical Field

[0001] The present application relates to the field of underground coal mine safety prevention and control technology, and in particular to an ultra-high water inorganic cementitious filling and fire prevention and extinguishing material, a preparation method and an application thereof. Background Art

[0002] Coal mine fire prevention and extinguishing materials are widely used in the coal mining process. At present, with the changes in coal mine geological conditions and the increase in mining depth, higher requirements are placed on the performance of coal mine fire prevention and extinguishing materials, especially for coal mine goafs. Fire prevention and extinguishing materials must not only have good fire extinguishing performance, but also have good fire retardant performance. When solving the technical problem of spontaneous combustion in coal mine goafs, most traditional fire prevention and extinguishing materials, namely silicate cement materials and organic chemical fire prevention and extinguishing materials, are used. The current fire prevention and extinguishing materials have poor pressure-bearing density. When used for filling and plugging air leakage and isolating the goaf fire area, cracks are prone to appear after a certain pressure, forming new air leakage channels, and the pressure-bearing density is poor. At the same time, relying solely on silicate cement to isolate the outside air from entering to extinguish the fire, the fire extinguishing effect is poor. Summary of the invention

[0003] The present application aims to solve one of the technical problems in the related art at least to some extent.

[0004] On the one hand, the present application proposes an ultra-high water content inorganic cementitious filling and fire prevention material, which utilizes solid waste from coal mining as filling material. Under reasonable components and dosage ratios, its high coagulation strength and water-cement ratio meet the performance requirements of high water content materials for underground filling and fire prevention in coal mines.

[0005] On the other hand, the present application proposes a method for preparing an ultra-high water content inorganic cementitious filling and fire extinguishing material, which has a simple preparation process and low process cost and has strong scalability.

[0006] On the other hand, the present application proposes an application of an ultra-high water content inorganic cementitious filling and fire-proof extinguishing material. When the material is used, it only needs to be stirred and mixed with tap water to prepare a filling slurry of a certain concentration. The solid water content is high, and the solidified body has good compressive resistance and bearing performance. The initial setting time is long and can be transported for a long time. It meets the performance requirements of high-water materials for underground filling and fire-proof extinguishing in coal mines and has broad application prospects.

[0007] According to the embodiment of the first aspect of the present application, a super-high water content inorganic cementitious filling and fire extinguishing material is provided, comprising material A and material B in a mass ratio of 6-8:1; The material A comprises the following raw materials in parts by weight: 36-50 parts of solid sulfur ash, 90-120 parts of phosphate tailings, 4.5-13 parts of water glass, 7.5-27.5 parts of calcium oxide, 3-4.5 parts of sodium sulfate, and 36-100 parts of additives; the additives include a binder, an improver, a retarder, and a thickening and water-retaining agent; The second material comprises the following raw materials in parts by weight: 3.5-4.5 parts of sodium aluminate, 7-7.5 parts of sodium carbonate, 5.5-6.5 parts of calcium oxide, 8-10.5 parts of anhydrous calcium sulfate, and 1.5-2.5 parts of bentonite.

[0008] In some embodiments, the auxiliary agent includes, by weight, 6-25 parts of the binder, 3-7.5 parts of the improver, 9-22.5 parts of the retarder and 18-45 parts of the thickening and water-retaining agent.

[0009] In some embodiments, the binder includes silicate cement and slag powder in a mass ratio of 3:1.

[0010] In some embodiments, the improver includes calcium lignin sulfonate, naphthalene sulfonate formaldehyde condensate water reducer and polycarboxylate water reducer in a mass ratio of 3:2:1.

[0011] In some embodiments, the retarder includes desulfurized gypsum powder, sodium gluconate and sodium citrate in a mass ratio of 1:1:1.

[0012] In some embodiments, the thickening and water-retaining agent comprises hydroxypropyl methylcellulose and sodium aluminate in a mass ratio of 1:2.

[0013] In some embodiments, the material A has a specific surface area of ​​300-500m 2 / kg powder; the second material has a specific surface area of ​​600-650m 2 / kg of powder.

[0014] In some embodiments, the surface area of ​​the material B is greater than the specific surface area of ​​the material A.

[0015] The ultra-high water content inorganic cementitious filling and fire prevention and extinguishing materials of the embodiments of the present application use solid sulfur ash and phosphorus tailings as the main materials. Solid sulfur ash is the main solid waste of power plants, and phosphorus tailings is the main solid waste of mining. It can reduce costs while effectively solving the land occupation problem and environmental pollution problem. In addition, the application of reasonable additives improves the coagulation strength of the material. In addition, when the second material encounters fire, it can generate silicate gel and aluminate gel, which will also release crystal water and absorb heat, achieving the effect of isolating air and absorbing heat to achieve fire extinguishing, meeting the performance requirements of high water content materials for underground filling and fire prevention and extinguishing in coal mines.

[0016] According to an embodiment of the second aspect of the present application, a method for preparing an ultra-high water content inorganic cementitious filling and fire extinguishing material is proposed, comprising the following steps: Weigh the raw materials in material A according to the chemical measurement, grind and mix the raw materials to obtain material A; Weigh the raw materials in material B according to the chemical measurement, grind and mix the raw materials to obtain material B; The material A and the material B are mixed in a mass ratio of 6-8:1 to obtain the material described in any of the above embodiments; when used, the ratio of the amount of water added to the total weight of the material A and the material B is 6-11:1.

[0017] The preparation method of the embodiment of the present application has a simple process, and material A and material B are prepared separately by grinding, and material A and material B are mixed according to a stoichiometric ratio. The process cost of the present application is low and has strong scalability.

[0018] According to an embodiment of the third aspect of the present application, it is proposed that the material described in any of the above embodiments is used in a coal mine goaf, and the ratio of water to the total weight of the material A and the material B is 6-11:1.

[0019] The application method of the embodiment of the present application has low material consumption and low process cost. The ratio of the water volume to the total weight of the material A and the material B of the ultra-high water content inorganic cementitious filling and fire extinguishing material of the present application when in use is 6-11:1, which can significantly reduce the consumption of high-water content materials and the process cost of use in underground coal mines.

[0020] Additional aspects and advantages of the present application will be given in part in the description below, and in part will become apparent from the description below, or will be learned through the practice of the present application. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] The above and / or additional aspects and advantages of the present application will become apparent and easily understood from the following description of the embodiments in conjunction with the accompanying drawings, in which: Figure 1 It is a flow chart for preparing ultra-high water content inorganic cementitious filling and fire extinguishing materials according to one embodiment of the present application. DETAILED DESCRIPTION

[0022] Embodiments of the present application are described in detail below, and examples of the embodiments are shown in the accompanying drawings, wherein the same or similar reference numerals throughout represent the same or similar elements or elements with the same or similar functions. The embodiments described below with reference to the accompanying drawings are exemplary and are only used to explain the present application, and cannot be construed as limiting the present application. On the contrary, the present application includes all changes, modifications and equivalents that fall within the spirit and connotation of the appended claims.

[0023] The technical solution of the embodiment of the present application provides a super-high water inorganic cementitious filling and fire-proof extinguishing material, a preparation method and an application. For super-high water inorganic cementitious filling and fire-proof extinguishing materials, solid sulfur ash and phosphorus tailings are used as the main materials, which can effectively solve the land occupation problem and environmental pollution problem while reducing the cost; in addition, the application of reasonable additives improves the coagulation strength of the material. In addition, when encountering fire, the second material can achieve the effect of isolating air and absorbing heat to extinguish the fire, meeting the performance requirements of high-water materials for filling and fire-proof extinguishing in coal mines. For the preparation method of super-high water inorganic cementitious filling and fire-proof extinguishing materials, the process cost is low and has strong scalability. For the application of super-high water inorganic cementitious filling and fire-proof extinguishing materials, the material consumption is small and the process cost is low. Among them, the ratio of the amount of water to the total weight of the first material and the second material in the super-high water inorganic cementitious filling and fire-proof extinguishing materials of the present application is 6-11:1, which can significantly reduce the amount of high water materials and the process cost of underground use in coal mines.

[0024] "Scope" disclosed in the present application is limited in the form of lower limit and upper limit, and a given range is limited by selecting a lower limit and an upper limit, and the selected lower limit and upper limit define the boundary of a special range. The scope limited in this way can be including end values ​​or not including end values, and can be arbitrarily combined, that is, any lower limit can be combined with any upper limit to form a scope. For example, if the scope of 60-120 and 80-110 is listed for a specific parameter, it is understood that the scope of 60-110 and 80-120 is also expected. In addition, if the minimum range values ​​1 and 2 are listed, and if the maximum range values ​​3, 4 and 5 are listed, the following scope can be all expected: 1-3, 1-4, 1-5, 2-3, 2-4 and 2-5. In the present application, unless otherwise specified, the numerical range "ab" represents the abbreviation of any real number combination between a and b, wherein a and b are real numbers. For example, the numerical range "0-5" means that all real numbers between "0-5" are listed in this document, and "0-5" is just an abbreviation of these numerical combinations. In addition, when a parameter is expressed as an integer ≥ 2, it is equivalent to disclosing that the parameter is, for example, an integer of 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, etc.

[0025] In the description of the embodiments of the present application, the term "and / or" is only a description of the association relationship of the associated objects, indicating that there may be three relationships. For example, A and / or B can represent: A exists alone, A and B exist at the same time, and B exists alone. In addition, the character " / " in this article generally indicates that the associated objects before and after are in an "or" relationship.

[0026] To achieve the above-mentioned purpose, according to the embodiment of the first aspect of the present application, an ultra-high water content inorganic cementing filling and fire extinguishing material is proposed, comprising material A and material B with a mass ratio of 6-8:1, wherein material A has a specific surface area of ​​300-500m 2 / kg powder; Material B has a specific surface area of ​​600-650m 2 / kg of powder, and the specific surface area of ​​material B is greater than that of material A.

[0027] Material A includes the following raw materials in parts by weight: 36-50 parts of solid sulfur ash, 90-120 parts of phosphate tailings, 4.5-13 parts of water glass, 7.5-27.5 parts of calcium oxide, 3-4.5 parts of sodium sulfate, and 36-100 parts of additives; the additives include binders, improvers, retarders and thickeners; Material B includes the following raw materials in parts by weight: 3.5-4.5 parts of sodium aluminate, 7-7.5 parts of sodium carbonate, 5.5-6.5 parts of calcium oxide, 8-10.5 parts of anhydrous calcium sulfate and 1.5-2.5 parts of bentonite.

[0028] Calculated by weight, there are 36-50 parts of solid sulfur ash, 90-120 parts of phosphate tailings, 4.5-13 parts of water glass, 7.5-27.5 parts of calcium oxide, 3-4.5 parts of sodium sulfate, and 36-100 parts of additives; the additives include binders, improvers, retarders, and thickeners. Solid sulfur ash is the main solid waste from power plants, and phosphate tailings is the main solid waste from mining. Both are accumulated in large quantities near the mines. Using them as filling materials effectively solves the problems of land occupation and environmental pollution, and can reduce the cost of filling. In addition, the reasonable auxiliary ingredients and the addition of auxiliary agents in Material A improve the filling strength of ultra-high water inorganic cementitious filling and fire extinguishing materials, and are not prone to gaps after long-term use.

[0029] In some embodiments, the weight percentage of the solid sulfur ash in material A is 40-50 parts; for example, in some embodiments, the weight percentage of the solid sulfur ash is 36 parts, 37 parts, 38 parts, 39 parts, 40 parts, 41 parts, 42 parts, 43 parts, 44 parts, 45 parts, 46 parts, 47 parts, 48 ​​parts, 49 parts, 50 parts, etc. Solid sulfur ash is the main solid waste of power plants, which is piled up in large quantities near the mine. Using it as a filling material effectively solves the land occupation problem and environmental pollution problem, and can reduce the filling cost at the same time.

[0030] In some embodiments, the weight percentage of the phosphorus tailings is 100-120 parts; for example, in some embodiments, the weight percentage of the phosphorus tailings is 90 parts, 91 parts, 92 parts, 93 parts, 94 parts, 95 parts, 96 parts, 97 parts, 98 parts, 99 parts, 100 parts, 101 parts, 102 parts, 103 parts, 104 parts, 105 parts, 106 parts, 107 parts, 108 parts, 109 parts, 110 parts, 111 parts, 112 parts, 113 parts, 114 parts, 115 parts, 116 parts, 117 parts, 118 parts, 119 parts, 120 parts, etc. Phosphorus tailings are the main solid waste of mining, which are piled up in large quantities near the mine pit. Using them as filling materials effectively solves the problems of land occupation and environmental pollution, and can reduce the filling cost at the same time.

[0031] In some embodiments, the weight percentage of water glass is 6-8 parts; for example, in some embodiments, the weight percentage of water glass is 4.5 parts, 5 parts, 5.5 parts, 6 parts, 6.5 parts, 7 parts, 7.5 parts, 8 parts, 8.5 parts, 9 parts, 9.5 parts, 10 parts, 10.5 parts, 11 parts, 11.5 parts, 12 parts, 12.5 parts, 13 parts, etc. The main component of water glass is sodium silicate, and its main function in this application is to react with other substances to form silicate gel, which can absorb and bind a large amount of water.

[0032] In some embodiments, the weight proportion of calcium oxide is 15-25 parts; for example, in some embodiments, the weight proportion of calcium oxide is 7.5 parts, 8 parts, 8.5 parts, 9 parts, 9.5 parts, 10 parts, 10.5 parts, 11 parts, 11.5 parts, 12 parts, 12.5 parts, 13 parts, 13.5 parts, 14 parts, 14.5 parts, 15 parts, 15.5 parts, 16 parts, 16.5 parts, 17 parts, 17.5 parts, 18 parts, 18.5 parts, 19 parts, 19.5 parts, 20 parts, 20.5 parts, 21 parts, 21.5 parts, 22 parts, 22.5 parts, 23 parts, 23.5 parts, 24 parts, 24.5 parts, 25 parts, 25.5 parts, 26 parts, 26.5 parts, 27 parts, 27.5 parts, etc. The main component of calcium oxide is calcium carbonate. Its main function in this application is that calcium oxide and other substances are stirred evenly and quickly hydrated with water to form Ca(OH)2. 2+ Ions react with solid waste under the action of water to produce flocculation reaction. This reaction process reduces the thickness of the water film between solid waste particles, reduces the plasticity of solid waste, increases the bonding force between soil particles, and improves soil strength and water stability. At the same time, calcium oxide is used as a desiccant for material A, which is conducive to the preservation of material A.

[0033] In some embodiments, the weight percentage of sodium sulfate is 3-4 parts; for example, in some embodiments, the weight percentage of sodium sulfate is 3 parts, 3.5 parts, 4 parts, 4.5 parts, etc. The main component of sodium sulfate is calcium carbonate, and its main function in this application is to improve the strength of the cemented filling body. A higher weight of sodium sulfate will reduce the strength of the filling body, and a lower weight of sodium sulfate cannot achieve the enhancement of the strength of the cemented filling body.

[0034] In the embodiment of the present application, the auxiliary agent includes a binder, an improver, a retarder and a thickener and water-retaining agent; in terms of weight, the auxiliary agent includes 6-25 parts of a binder, 3-7.5 parts of an improver, 9-22.5 parts of a retarder and 18-45 parts of a thickener and water-retaining agent.

[0035] For example, in some embodiments, the weight percentage of the binder is 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts, 16 parts, 17 parts, 18 parts, 19 parts, 20 parts, 21 parts, 22 parts, 23 parts, 24 parts, 25 parts, etc. The binder includes silicate cement and slag powder in a mass ratio of 3:1. The hydration reaction of the binder can promote each other to achieve a better gelling effect, so that the filling materials can be closely bonded together. Through the mutual promotion of the solid sulfur ash, the thick water-retaining agent and the binder, the filling strength of the ultra-high water inorganic cementing filling and the fire-proof extinguishing material is improved, and it is not easy to produce gaps after long-term application.

[0036] For example, in some embodiments, the weight proportions of the modifier are 3 parts, 3.5 parts, 4 parts, 4.5 parts, 5 parts, 5.5 parts, 6 parts, 6.5 parts, 7 parts, and 7.5 parts, wherein the modifier includes calcium lignin sulfonate, naphthalene sulfonate formaldehyde condensate water reducer and polycarboxylate water reducer in a mass ratio of 3:2:1. The main function of the modifier is that when the cement particles absorb enough water reducer, a stable solvated water film is formed on the cement surface by means of the association of sulfonate ions with hydrogen bonds in water molecules, and the hydrogen bonds between water molecules. This film plays a three-dimensional protective role, prevents direct contact between cement particles, and acts as a lubricant between particles.

[0037] For example, in some embodiments, the weight percentage of the retarder is 9 parts, 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts, 16 parts, 17 parts, 18 parts, 19 parts, 20 parts, 21 parts, 22 parts, 22.5 parts, etc. The retarder includes desulfurized gypsum powder, sodium gluconate and sodium citrate in a mass ratio of 1:1:1. The main function of the retarder is to delay the hydration reaction of the cementitious filling body, thereby prolonging the setting time of the cementitious filling body.

[0038] For example, in some embodiments, the weight percentage of the thickening and water-retaining agent is 18 parts, 19 parts, 20 parts, 21 parts, 22 parts, 23 parts, 24 parts, 25 parts, 26 parts, 27 parts, 27 parts, 28 parts, 29 parts, 30 parts, 31 parts, 32 parts, 33 parts, 34 parts, 35 parts, 36 parts, 37 parts, 38 parts, 39 parts, 40 parts, 41 parts, 42 parts, 43 parts, 44 parts, 45 parts, etc. The thickening and water-retaining agent includes hydroxypropyl methylcellulose and sodium aluminate in a mass ratio of 1:2. After the ultra-high water inorganic cementitious filling and fire-proof extinguishing material are mixed with water to form a slurry, the thickening and water-retaining agent can increase the viscosity and cohesiveness of the slurry and reduce the water seepage of the slurry. The aluminum ions generated by ionization in the slurry can accelerate the formation of calcium sulfonate and absorb a large amount of free water in the slurry.

[0039] In some embodiments, material B includes, by weight, 3.5-4.5 parts of sodium aluminate, 7-7.5 parts of sodium carbonate, 5.5-6.5 parts of calcium oxide, 8-10.5 parts of anhydrous calcium sulfate, and 1.5-2.5 parts of bentonite.

[0040] For example, in some embodiments, the weight percentage of sodium aluminate is 3.5 parts, 3.6 parts, 3.7 parts, 3.8 parts, 3.9 parts, 4.0 parts, 4.1 parts, 4.2 parts, 4.3 parts, 4.4 parts, 4.5 parts, etc. When the ultra-high water content inorganic cementitious filling and fire extinguishing material is used and encounters fire, the crystal water in the gypsum is released and absorbs heat, and sodium aluminate can generate silicate gel and aluminate gel. These two gel components can also absorb and combine a large amount of water and exist in the needle-shaped or mesh structure gaps in the calcium sulfide. When encountering fire, they will also release crystal water and absorb heat.

[0041] In some embodiments, the weight percentage of sodium carbonate is 7 parts, 7.1 parts, 7.2 parts, 7.3 parts, 7.4 parts, 7.5 parts, etc. Sodium carbonate is an inert solid that can isolate the outside air. Therefore, the sodium aluminate and sodium carbonate in the second material can extinguish the fire by isolating the air and absorbing heat, and the fire extinguishing effect is better.

[0042] In some embodiments, the weight percentage of calcium oxide is 5.5 parts, 5.6 parts, 5.7 parts, 5.8 parts, 5.9 parts, 6.0 parts, 6.1 parts, 6.2 parts, 6.3 parts, 6.4 parts, 6.5 parts, etc. The main function of calcium oxide is that calcium oxide and other substances are evenly stirred, and hydration is quickly generated when encountering water to form Ca (OH) 2. Calcium hydroxide can also react with carbon dioxide in the air to form hard calcium carbonate, further improving the strength of the material. Adding calcium oxide to the second material can provide rapid hardening ability, improve the ultra-high water property of the material, and improve the stability of the material; at the same time, calcium oxide is used as a desiccant for the second material, which is conducive to the preservation of the second material.

[0043] In some embodiments, the weight percentage of anhydrous calcium sulfate is 8-10.5 parts, for example, in some embodiments, the weight percentage of anhydrous calcium sulfate is 8 parts, 8.5 parts, 9.0 parts, 9.5 parts, 10 parts, 10.5 parts, etc. When preparing the slurry, hydrated calcium sulfate absorbs a large amount of water to become gypsum. The thermal conductivity of gypsum is low. When it encounters fire, the crystal water therein is released and absorbs heat.

[0044] For example, in some embodiments, the weight percentage of bentonite is 1.5 parts, 1.6 parts, 1.7 parts, 1.8 parts, 1.9 parts, 2.0 parts, 2.1 parts, 2.2 parts, 2.3 parts, 2.4 parts, 2.5 parts, etc. In this embodiment, bentonite has good flame retardant properties and good water absorption and expansion properties.

[0045] Therefore, the material A of the embodiment of the present application uses solid sulfur ash and phosphorus tailings as the main materials. Solid sulfur ash is the main solid waste of power plants, and phosphorus tailings is the main solid waste of mining. It can reduce costs while effectively solving the land occupation problem and environmental pollution problem; in addition, the application of reasonable additives improves the coagulation strength of the material. In addition, the material B of the embodiment of the present application can generate silicate gel and aluminate gel when encountering fire, which will also release crystal water and absorb heat, achieving the effect of isolating air and absorbing heat to achieve fire extinguishing, meeting the performance requirements of high-water materials for underground filling and fire prevention and extinguishing in coal mines.

[0046] According to the embodiment of the second aspect of the present application, a method for preparing an ultra-high water content inorganic cementitious filling and fire extinguishing material is proposed. Figure 1 , including the following steps: Weigh the raw materials in material A according to the chemical measurement, grind and mix the raw materials to obtain material A; Weigh the raw materials in material B according to the chemical measurement, grind and mix the raw materials to obtain material B; Material A and material B are mixed in a mass ratio of 6-8:1 to obtain the material in any of the above embodiments; when used, the ratio of the amount of water added to the total weight of material A and material B is 6-11:1.

[0047] The preparation method of the embodiment of the present application has a simple process, and material A and material B are prepared separately by grinding, and material A and material B are mixed according to a stoichiometric ratio. The process cost of the present application is low and has strong scalability.

[0048] According to an embodiment of the third aspect of the present application, it is proposed that the material in any of the above embodiments is used in a coal mine goaf, and the ratio of water to the total weight of material A and material B is 6-11:1.

[0049] The application method of the embodiment of the present application has low material consumption and low process cost. The ratio of water volume to the total weight of material A and material B of the ultra-high water content inorganic cementitious filling and fire extinguishing material of the present application when in use is 6-11:1, which can significantly reduce the consumption of high-water content materials and the process cost of use in underground coal mines.

[0050] To facilitate further understanding of the present application, the scheme of the present application is further described below in conjunction with the embodiments. Those skilled in the art will understand that the description in the present application is only part of the examples, and any other suitable specific examples are within the scope of the present application.

[0051] Example 1 The present embodiment provides an ultra-high water content inorganic cementitious filling and fire extinguishing material, and its preparation method and specific operating parameters are as follows: weigh 36 parts of solid sulfur ash, 90 parts of phosphate tailings, 10 parts of water glass, 10 parts of calcium oxide, 3 parts of sodium sulfate, 10 parts of binder, 5 parts of improver, 11 parts of retarder, 20 parts of thickening and water-retaining agent, and put the raw materials into the screening and split-pass pulverizer system in the three-bin mill for grinding, and evenly mix the ground raw materials to obtain material A.

[0052] Weigh 3.5 parts of sodium aluminate, 7.5 parts of sodium carbonate, 5.5 parts of calcium oxide, 8 parts of anhydrous calcium sulfate, and 1.5 parts of bentonite, and put the raw materials into the screening and splitting grinding system in the three-bin mill for grinding, and evenly mix the ground raw materials to obtain material B; The material A and the material B are uniformly mixed in a mass ratio of 7.5:1 to obtain an ultra-high water content inorganic cementitious filling and fire extinguishing material. When used, tap water is injected into the ultra-high water content inorganic cementitious filling and fire extinguishing material, and the ratio of the water volume to the total weight of the material A and the material B is 11:1, and stirred for 5 minutes to prepare a filling slurry.

[0053] Example 2 Compared with Example 1, the material A in this embodiment includes 40 parts of sulfur-fixing ash, 95 parts of phosphate tailings, 5 parts of water glass, 10 parts of calcium oxide, 3.5 parts of sodium sulfate, 15 parts of binder, 6.5 parts of improver, 15 parts of retarder, and 20 parts of thickening and water-retaining agent. The raw materials are respectively put into the screening and splitting grinding mill system in the three-bin mill for grinding treatment, and the ground raw materials are uniformly mixed to obtain material A.

[0054] Weigh 4 parts of sodium aluminate, 7 parts of sodium carbonate, 6 parts of calcium oxide, 9 parts of anhydrous calcium sulfate and 2 parts of bentonite, respectively put the raw materials into the screening and splitting grinding mill system in the three-bin mill for grinding, and evenly mix the ground raw materials to obtain material B.

[0055] The material A and the material B are uniformly mixed in a mass ratio of 7.5:1 to obtain an ultra-high water content inorganic cementitious filling and fire extinguishing material. When used, tap water is injected into the ultra-high water content inorganic cementitious filling and fire extinguishing material, and the ratio of the water volume to the total weight of the material A and the material B is 10:1, and stirred for 10 minutes to prepare a filling slurry.

[0056] Example 3 Compared with Example 1, the material A in this embodiment includes 40 parts of sulfur-fixing ash, 100 parts of phosphate tailings, 5 parts of water glass, 15 parts of calcium oxide, 4 parts of sodium sulfate, 11 parts of binder, 5 parts of improver, 10 parts of retarder, and 20 parts of thickening and water-retaining agent. The raw materials are respectively put into the screening and splitting grinding mill system in the three-bin mill for grinding treatment, and the ground raw materials are uniformly mixed to obtain material A.

[0057] Weigh 4.5 parts of sodium aluminate, 7.5 parts of sodium carbonate, 6.5 parts of calcium oxide, 9.5 parts of anhydrous calcium sulfate and 2 parts of bentonite, respectively put the raw materials into the screening and splitting grinding mill system in the three-bin mill for grinding, and evenly mix the ground raw materials to obtain material B.

[0058] The material A and the material B are uniformly mixed in a mass ratio of 7:1 to obtain a super-high water content inorganic cementitious filling and fire extinguishing material. When used, tap water is injected into the super-high water content inorganic cementitious filling and fire extinguishing material, and the ratio of the water volume to the total weight of the material A and the material B is 9:1, and stirred for 8 minutes to prepare a filling slurry.

[0059] Example 4 Compared with Example 1, the material A in this embodiment includes 42 parts of sulfur-fixing ash, 100 parts of phosphate tailings, 7 parts of water glass, 17 parts of calcium oxide, 4.5 parts of sodium sulfate, 10 parts of binder, 6.5 parts of improver, 10 parts of retarder, and 20 parts of thickening and water-retaining agent. The raw materials are respectively put into the screening and splitting grinding mill system in the three-bin mill for grinding treatment, and the ground raw materials are uniformly mixed to obtain material A.

[0060] Weigh 4.5 parts of sodium aluminate, 7.5 parts of sodium carbonate, 6.5 parts of calcium oxide, 10 parts of anhydrous calcium sulfate and 2.5 parts of bentonite, respectively put the raw materials into the screening and splitting grinding mill system in the three-bin mill for grinding, and evenly mix the ground raw materials to obtain material B.

[0061] The material A and the material B are uniformly mixed in a mass ratio of 7:1 to obtain a super-high water content inorganic cementitious filling and fire extinguishing material. When used, tap water is injected into the super-high water content inorganic cementitious filling and fire extinguishing material, and the ratio of the water volume to the total weight of the material A and the material B is 8:1, and stirred for 10 minutes to prepare a filling slurry.

[0062] Example 5 Compared with Example 1, the material A in this embodiment includes 36 parts of solid sulfur ash, 90 parts of phosphate tailings, 4.5 parts of water glass, 7.5 parts of calcium oxide, 3 parts of sodium sulfate, 9 parts of binder, 6 parts of improver, 12 parts of retarder, and 21 parts of thickening and water-retaining agent. The raw materials are respectively put into the screening and splitting grinding mill system in the three-bin mill for grinding treatment, and the ground raw materials are uniformly mixed to obtain material A.

[0063] Weigh 4.5 parts of sodium aluminate, 7.5 parts of sodium carbonate, 6.5 parts of calcium oxide, 10.5 parts of anhydrous calcium sulfate and 2.5 parts of bentonite, respectively put the raw materials into the screening and splitting grinding mill system in the three-bin mill for grinding, and evenly mix the ground raw materials to obtain material B.

[0064] The material A and the material B are uniformly mixed in a mass ratio of 6:1 to obtain a super-high water content inorganic cementitious filling and fire extinguishing material. When used, tap water is injected into the super-high water content inorganic cementitious filling and fire extinguishing material, and the ratio of the water volume to the total weight of the material A and the material B is 7:1, and stirred for 8 minutes to prepare a filling slurry.

[0065] Example 6 Compared with Example 1, the material A in this embodiment includes 42 parts of solid sulfur ash, 96 parts of phosphate tailings, 4.5 parts of water glass, 7.5 parts of calcium oxide, 3 parts of sodium sulfate, 6 parts of binder, 3 parts of improver, 9 parts of retarder, and 18 parts of thickening and water-retaining agent. The raw materials are respectively put into the screening and splitting grinding mill system in the three-bin mill for grinding treatment, and the ground raw materials are uniformly mixed to obtain material A.

[0066] Weigh 4.5 parts of sodium aluminate, 7.5 parts of sodium carbonate, 6.5 parts of calcium oxide, 10.5 parts of anhydrous calcium sulfate and 2.5 parts of bentonite, respectively put the raw materials into the screening and splitting grinding mill system in the three-bin mill for grinding, and evenly mix the ground raw materials to obtain material B.

[0067] The material A and the material B are uniformly mixed in a mass ratio of 6:1 to obtain an ultra-high water content inorganic cementitious filling and fire extinguishing material. When used, tap water is injected into the ultra-high water content inorganic cementitious filling and fire extinguishing material in a ratio of 6:1 to the total weight of the material A and the material B, and stirred for 8 minutes to prepare a filling slurry.

[0068] Comparative Example 1 The present comparative example provides an ultra-high water content inorganic cementitious filling and fire extinguishing material, and its preparation method and specific operating parameters are as follows: weigh 23 parts of solid sulfur ash, 52 parts of phosphate tailings, 10 parts of water glass, 10 parts of calcium oxide, 3 parts of sodium sulfate, 10 parts of binder, 5 parts of improver, 11 parts of retarder, 20 parts of thickening and water-retaining agent, and respectively put the raw materials into the screening and split-pass pulverizer system in the three-bin mill for grinding treatment, and evenly mix the ground raw materials to obtain material A.

[0069] Weigh 3.5 parts of sodium aluminate, 7.5 parts of sodium carbonate, 5.5 parts of calcium oxide, 8 parts of anhydrous calcium sulfate, and 1.5 parts of bentonite, and put the raw materials into the screening and splitting grinding system in the three-bin mill for grinding, and evenly mix the ground raw materials to obtain material B; The material A and the material B are uniformly mixed in a mass ratio of 7.5:1 to obtain an ultra-high water content inorganic cementitious filling and fire extinguishing material. When used, tap water is injected into the ultra-high water content inorganic cementitious filling and fire extinguishing material, and the ratio of the water volume to the total weight of the material A and the material B is 11:1, and stirred for 5 minutes to prepare a filling slurry.

[0070] Comparative Example 2 This comparative example provides an ultra-high water content inorganic cementing filling and fire extinguishing material, the preparation method and specific operating parameters of which are as follows: Material A includes 40 parts of solid sulfur ash, 95 parts of phosphate tailings, 5 parts of water glass, 10 parts of calcium oxide, 3.5 parts of sodium sulfate, 15 parts of cementing agent, 6.5 parts of improver, 15 parts of retarder, and 20 parts of thickening and water retaining agent. The raw materials are respectively put into the screening and splitting grinding mill system in the three-bin mill for grinding treatment, and the raw materials after grinding treatment are uniformly mixed to obtain Material A.

[0071] Weigh 3 parts of sodium aluminate, 6 parts of sodium carbonate, 5 parts of calcium oxide, 9 parts of anhydrous calcium sulfate and 2 parts of bentonite, respectively put the raw materials into the screening and split-path pulverizer system of the three-bin mill for grinding, and evenly mix the ground raw materials to obtain material B.

[0072] The material A and the material B are uniformly mixed in a mass ratio of 7.5:1 to obtain an ultra-high water content inorganic cementitious filling and fire extinguishing material. When used, tap water is injected into the ultra-high water content inorganic cementitious filling and fire extinguishing material, and the ratio of the water volume to the total weight of the material A and the material B is 10:1, and stirred for 10 minutes to prepare a filling slurry.

[0073] Comparative Example 3 The present comparative example provides an ultra-high water content inorganic cementitious filling and fire extinguishing material, and its preparation method and specific operating parameters are as follows: weigh 25 parts of solid sulfur ash, 85 parts of phosphate tailings, 10 parts of water glass, 10 parts of calcium oxide, 3 parts of sodium sulfate, 10 parts of binder, 5 parts of improver, 11 parts of retarder, 15 parts of thickening and water-retaining agent, and respectively put the raw materials into the screening and split-pass pulverizer system in the three-bin mill for grinding treatment, and evenly mix the ground raw materials to obtain material A.

[0074] Weigh 5 parts of sodium aluminate, 8 parts of sodium carbonate, 5.5 parts of calcium oxide, 8 parts of anhydrous calcium sulfate, and 1.5 parts of bentonite, and put the raw materials into the screening and splitting grinding system in the three-bin mill for grinding, and evenly mix the ground raw materials to obtain material B; The material A and the material B are uniformly mixed in a mass ratio of 7.5:1 to obtain an ultra-high water content inorganic cementitious filling and fire extinguishing material. When used, tap water is injected into the ultra-high water content inorganic cementitious filling and fire extinguishing material, and the ratio of the water volume to the total weight of the material A and the material B is 11:1, and stirred for 5 minutes to prepare a filling slurry.

[0075] Comparative Example 4 This comparative example provides an ultra-high water content inorganic cementing filling and fire extinguishing material, and its preparation method and specific operating parameters are as follows: Material A includes 60 parts of solid sulfur ash, 100 parts of phosphate tailings, 4.5 parts of water glass, 7.5 parts of calcium oxide, 3 parts of sodium sulfate, 9 parts of cementing agent, 6 parts of improver, 12 parts of retarder, and 21 parts of thickening and water retaining agent. The raw materials are respectively put into the screening and splitting grinding mill system in the three-bin mill for grinding treatment, and the raw materials after grinding treatment are uniformly mixed to obtain Material A.

[0076] Weigh 8 parts of sodium aluminate, 7 parts of sodium carbonate, 6 parts of calcium oxide, 9 parts of anhydrous calcium sulfate and 2.5 parts of bentonite, respectively put the raw materials into the screening and splitting grinding mill system in the three-bin mill for grinding, and evenly mix the ground raw materials to obtain material B.

[0077] The material A and the material B are uniformly mixed in a mass ratio of 6:1 to obtain a super-high water content inorganic cementitious filling and fire extinguishing material. When used, tap water is injected into the super-high water content inorganic cementitious filling and fire extinguishing material, and the ratio of the water volume to the total weight of the material A and the material B is 7:1, and stirred for 8 minutes to prepare a filling slurry.

[0078] Experimental example The filling slurry prepared in the above embodiments was injected into the position required to be filled in the coal mine, and the initial setting time, solid water content, 7d and 28d unconfined compressive strength and fire extinguishing effect of the silicate cement filling slurry after molding were tested. The results are shown in Table 1.

[0079] Table 1 Test results of filling slurry

[0080] It can be seen from the results in Table 1 that the ultra-high water content of the inorganic cementitious filling and fire-fighting material of the present application is high, the solidified body has good compressive resistance and bearing performance, and the initial setting time is long, so it can be transported for a long time, meeting the performance requirements of high water materials for underground filling and fire-fighting in coal mines, and has broad application prospects.

[0081] In the description of this specification, the description with reference to the terms "one embodiment", "some embodiments", "example", "specific example", or "some examples" etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present application. In this specification, the schematic representations of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described may be combined in any one or more embodiments or examples in a suitable manner. In addition, those skilled in the art may combine and combine the different embodiments or examples described in this specification and the features of the different embodiments or examples, without contradiction.

[0082] Although the embodiments of the present application have been shown and described above, it can be understood that the above embodiments are exemplary and cannot be understood as limitations on the present application. Ordinary technicians in this field can change, modify, replace and modify the above embodiments within the scope of the present application.

Claims

1. A super high water content inorganic cementitious filling and fire extinguishing material, characterized in that: It includes material A and material B with a mass ratio of 6-8:1; The material A comprises the following raw materials in parts by weight: 36-50 parts of solid sulfur ash, 90-120 parts of phosphate tailings, 4.5-13 parts of water glass, 7.5-27.5 parts of calcium oxide, 3-4.5 parts of sodium sulfate, and 36-100 parts of additives; the additives include a binder, an improver, a retarder, and a thickening and water-retaining agent; The second material comprises the following raw materials in parts by weight: 3.5-4.5 parts of sodium aluminate, 7-7.5 parts of sodium carbonate, 5.5-6.5 parts of calcium oxide, 8-10.5 parts of anhydrous calcium sulfate, and 1.5-2.5 parts of bentonite.

2. The material according to claim 1, characterized in that The auxiliary agent includes, by weight, 6-25 parts of the binder, 3-7.5 parts of the improver, 9-22.5 parts of the retarder and 18-45 parts of the thickening and water-retaining agent.

3. The material according to claim 2, characterized in that The binder comprises silicate cement and slag powder in a mass ratio of 3:

1.

4. The material according to claim 2, characterized in that The improver comprises calcium lignin sulfonate, naphthalene sulfonate formaldehyde condensate water reducer and polycarboxylate water reducer in a mass ratio of 3:2:

1.

5. The material according to claim 2, characterized in that The retarder comprises desulfurized gypsum powder, sodium gluconate and sodium citrate in a mass ratio of 1:1:

1.

6. The material according to claim 2, characterized in that The thickening and water-retaining agent comprises hydroxypropyl methylcellulose and sodium aluminate in a mass ratio of 1:

2.

7. The material according to any one of claims 1 to 6, characterized in that The material A has a specific surface area of ​​300-500m 2 / kg powder; the second material has a specific surface area of ​​600-650m 2 / kg of powder.

8. The material according to any one of claims 1 to 6, characterized in that The specific surface area of ​​the material B is greater than the specific surface area of ​​the material A.

9. A method for preparing an ultra-high water content inorganic cementitious filling and fire extinguishing material, characterized in that: The following steps are involved: Weigh the raw materials in material A according to the chemical measurement, grind and mix the raw materials to obtain material A; Weigh the raw materials in material B according to the chemical measurement, grind and mix the raw materials to obtain material B; The material A and the material B are mixed in a mass ratio of 6-8:1 to obtain the material according to any one of claims 1-8; when used, the ratio of the amount of water added to the total weight of the material A and the material B is 6-11:

1.

10. The material according to any one of claims 1 to 8 is used in coal mine goaf, characterized in that: The ratio of water to the total weight of the material A and the material B is 6-11:1.

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