CN115073117A - Mining low-temperature ultrahigh-crystallization-water rapid-solidification filling support material and preparation method thereof - Google Patents
Mining low-temperature ultrahigh-crystallization-water rapid-solidification filling support material and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C04B28/141—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing calcium sulfate cements containing dihydrated gypsum before the final hardening step, e.g. forming a dihydrated gypsum product followed by a de- and rehydration step
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- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/14—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing calcium sulfate cements
- C04B28/142—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing calcium sulfate cements containing synthetic or waste calcium sulfate cements
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- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/14—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing calcium sulfate cements
- C04B28/142—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing calcium sulfate cements containing synthetic or waste calcium sulfate cements
- C04B28/143—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing calcium sulfate cements containing synthetic or waste calcium sulfate cements the synthetic calcium sulfate being phosphogypsum
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- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/14—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing calcium sulfate cements
- C04B28/145—Calcium sulfate hemi-hydrate with a specific crystal form
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- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/14—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing calcium sulfate cements
- C04B28/16—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing calcium sulfate cements containing anhydrite, e.g. Keene's cement
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- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/00724—Uses not provided for elsewhere in C04B2111/00 in mining operations, e.g. for backfilling; in making tunnels or galleries
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- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract
The invention relates to a mining low-temperature ultrahigh-crystallization-water rapid-setting filling support material, which is prepared from a material with a specific surface area of 350-600 m 2 The material A fine powder and the material B fine powder are/kg; wherein the fine powder of the material A is made of Al 2 O 3 Content (wt.)>Grinding 19% of mixed material consisting of cement clinker, solid waste, grinding aid, retarder, early agent and suspending agent to obtain the cement clinker; and the material B fine powder is obtained by grinding a mixed material consisting of gypsum, lime, solid waste, an accelerating agent, a reinforcing agent and a suspending agent. The slurry prepared from the fine powder A and the fine powder B is independently placed for 2-24 hours respectively and is not solidified, the slurry can be solidified after the two kinds of slurry are mixed for 5-45 minutes, and the material is a good filling support material, the water content in the material reaches more than 91.6%, and the material has the characteristics of wide raw material source, low cost, high resistance increasing speed, good toughness, no harm, no toxicity, no pollution and the like.
Description
Technical Field
The invention relates to the technical field of mine support materials, in particular to a mining low-temperature ultrahigh-crystallization-water rapid-setting filling support material and a preparation method thereof.
Background
With the continuous high-speed stable development of economy in China and the vigorous demand of energy and resources, the mining extension speed of mines is accelerated, the mining depth is further increased, with the increase of the mining depth and the increasingly complex mining conditions, the problems of ground pressure control and safety are increasingly highlighted, and the filling body is utilized to carry out ground pressure management, control surrounding rock caving and ground surface sinking, protect ground surface buildings, and alleviate large-area ground pressure activities so as to protect the safety of underground operation spaces. The method is widely applied to industries such as color, coal and the like.
In the process of tunneling or using a coal mine tunnel, the tunnel can be caved or an ultrahigh area can appear due to the fact that a top plate is broken or influenced by mining, and currently, high polymer materials, cement and filling materials are mainly adopted for grouting reinforcement or filling. The high polymer material has higher cost, is toxic and corrosive, is very easy to foam in the presence of water so as to reduce the flame retardance and have the risk of spontaneous combustion; in addition, the ventilation closed wall is one of common ventilation structures, the traditional closed wall construction method mainly comprises the modes of brick laying, concrete pouring, cement sand spraying and the like, the problems of large material transportation amount, long construction period, harsh operation environment and the like exist, more importantly, the wall body has small deformation amount, and after being influenced by mining, the wall body is cracked under pressure to cause gas leakage, and great potential safety hazards exist. In order to prevent the accidents, a filling and supporting material with good performance is required to be found to replace the traditional filling material.
When the filling material sold in the market is used for filling and supporting, two kinds of fine powder are respectively added with water and uniformly mixed to prepare two kinds of slurry, the two kinds of slurry are mixed and then conveyed to a position to be filled, in order to ensure that the two kinds of slurry can be solidified after being mixed, the water with the temperature higher than 15 ℃ is generally required for preparing the filling slurry, and when the temperature of the water for mine filling is low in winter, the water is required to be heated to the temperature higher than 15 ℃ for use.
When the temperature of water for mine filling is lower than 15 ℃ in winter, the situation that the filling slurry does not solidify often occurs.
Disclosure of Invention
The invention aims to solve the technical problem of providing a mining low-temperature ultrahigh-crystallization-water rapid-setting filling support material and a preparation method thereof.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
the mining low-temperature ultrahigh-crystallization-water rapid-setting filling support material is characterized by comprising materials with specific surface areas of 350-600 m 2 The material A fine powder and the material B fine powder are/kg;
wherein the fine powder of the material A is made of Al 2 O 3 Content (wt.)>Grinding 19% of mixed material consisting of cement clinker, solid waste, grinding aid, retarder, early agent and suspending agent to obtain the cement clinker;
and the material B fine powder is obtained by grinding a mixed material consisting of gypsum, lime, solid waste, an accelerating agent, a reinforcing agent and a suspending agent.
As an embodiment of the invention, the mixture ratio of the fine powder of the material A is as follows according to the parts by weight: 65-99.8 parts of cement clinker, 0.1-20 parts of solid waste, 0.05-5 parts of grinding aid, 0.05-3 parts of retarder, 0.05-5 parts of early agent and 0.05-2 parts of suspending agent.
As an embodiment of the invention, the specific surface area of the fine powder of the material A is 356-600 m 2 /kg；
The first material fine powder comprises the following components in parts by weight: 70-85 parts of cement clinker, 10-20 parts of solid waste, 0.5-2.7 parts of grinding aid, 0.5-2 parts of retarder, 1.6-4.8 parts of early agent and 0.4-0.5 part of suspending agent.
In one embodiment of the invention, the cement clinker is selected from any one of aluminate cement clinker, sulphoaluminate cement clinker, aluminoferrite cement clinker and fluoroaluminate cement clinker, or a mixture of any two or more of them;
the solid waste in the first material fine powder is any one or mixture of any two or more of slag powder, steel slag powder, copper slag powder, fly ash and silica fume.
As an embodiment of the invention, the grinding aid is one or a mixture of any two or more of triethanolamine, triisopropanolamine, ethylene glycol, propylene glycol, diethylene glycol, glycerol and sodium acetate;
the retarder is formed by mixing any one or any two or more than two of citric acid and salts thereof, boric acid and salts thereof, tartaric acid and salts thereof, oxalic acid, zinc salt, phosphate and lignosulfonate;
the early agent is any one or mixture of any two or more of potassium chloride, sodium chloride, calcium chloride, magnesium chloride, zinc chloride, lithium chloride and ferric oxide.
As an implementation mode of the invention, the proportion of the B material fine powder is as follows according to the parts by weight: 50-90 parts of gypsum, 5-50 parts of lime, 1-30 parts of other materials, 0.05-10 parts of an accelerator, 0.05-5 parts of a reinforcing agent and 0.05-2 parts of a suspending agent.
As an embodiment of the invention, the specific surface areas of the fine powder of the material B are 352-593 m 2 /kg；
The proportion of the material B fine powder is as follows by weight: 60-65 parts of gypsum, 19-25 parts of lime, 8-10 parts of solid waste, 3.2-6.4 parts of an accelerator, 1.5-4 parts of a reinforcing agent and 0.3-0.8 part of a suspending agent.
As an embodiment of the invention, the gypsum is a mixture of any two or more of dihydrate gypsum, natural anhydrite, phosphogypsum, fluorgypsum, salt gypsum and hemihydrate gypsum;
the lime is one or a mixture of two of quicklime and calcium hydroxide;
the solid waste in the material B is prepared by mixing one or two of carbide slag, alkali slag, boiling furnace slag and calcium carbonate powder.
As an embodiment of the invention, the accelerator is one or a mixture of two of a cement accelerator, ferric hydroxide, potassium carbonate, sodium carbonate, lithium hydroxide, potassium fluoride, sodium silicate and sodium fluosilicate sold in the market;
the reinforcing agent is one or a mixture of two of potassium sulfate, sodium sulfite, aluminum potassium sulfate, calcium formate, potassium tripolyphosphate and sodium tripolyphosphate.
In one embodiment of the invention, the suspending agent is composed of one or/and a mixture of methyl cellulose, carboxymethyl cellulose, hydroxypropyl methyl cellulose and hydroxyethyl cellulose.
In a second aspect, a preparation method of the mining low-temperature ultrahigh-crystallization-water rapid-setting filling supporting material is provided, and comprises the following steps:
(1) grinding a mixed material consisting of cement clinker, solid waste, grinding aid, retarder, early agent and suspending agent to a specific surface area of 350-600 m 2 The method comprises the following steps of (1) obtaining fine powder of the A material by kg, then adding water which is 1-11 times of the total weight of the fine powder of the A material and has the water temperature of more than 6 ℃ into the fine powder of the A material, and uniformly mixing the mixture to obtain slurry A;
(2) grinding a mixed material consisting of gypsum, lime, slag powder, an accelerating agent, a reinforcing agent and a suspending agent until the specific surface area is 350-600 m 2 Adding water which is 1-11 times of the total weight of the fine powder B and has the water temperature of more than 6 ℃ into the fine powder B, uniformly mixing the water and the fine powder to obtain slurry B;
(3) and mixing the slurry A and the slurry B according to the weight ratio of 1 (0.8-1.2), wherein the setting time of the obtained slurry is 5-45 minutes.
As an implementation mode of the invention, in the step (1), water which is 3-11 times of the total weight of the fine powder of the material A and has the water temperature of more than 6 ℃ is added and mixed uniformly.
As an implementation mode of the invention, in the step (1), water which is 5-11 times of the total weight of the fine powder of the material A and has the water temperature of more than 6 ℃ is added and mixed uniformly.
As an implementation mode of the invention, in the step (2), water which is 3-11 times of the total weight of the fine powder of the material A and has the water temperature of more than 6 ℃ is added and mixed uniformly.
As an implementation mode of the invention, in the step (2), water which is 5-11 times of the total weight of the fine powder of the material A and has the water temperature of more than 6 ℃ is added and mixed uniformly.
In one embodiment of the invention, in the step (3), the slurry A and the slurry B are mixed according to a weight ratio of 1:1, and the coagulation time of the obtained slurry is 5-10 minutes.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in:
(1) the invention adds cement clinker, solid waste, grinding aid, retarder and early-aging agent in specific mass percentage into the first material fine powderSelecting specific suspending agent types, substrate types and additive types, and grinding the mixture to a specific surface area of 350-600 m 2 Between/kg; and adding gypsum, lime, solid waste, an accelerator, a reinforcing agent and a suspending agent in a specific mass percentage into the fine powder of the material B, selecting a specific type of the suspending agent, a specific type of a matrix and a specific type of an additive, and grinding the mixture until the specific surface area is 350-600 m 2 The lower limit of the temperature of the used water for obtaining the uniform slurry is greatly reduced after the slurry of the two is mixed, and the open-air low-temperature water can be directly used even in the construction of a mine in winter.
(2) According to the invention, the slurry A obtained from the fine powder A and the slurry B obtained from the fine powder B are respectively and independently placed for 24 hours without solidification, but after the slurry A and the slurry B are mixed together, under the synergistic effect between the specific suspending agent and other additives, the slurry reaction speed can be promoted after the slurry prepared by using low-temperature water is mixed in winter, so that the slurry can be solidified within 5-10 minutes, and the composite material is a good filling support material.
(3) In the invention, when the slurry A and the slurry B are prepared by utilizing the fine powder A and the fine powder B, water which is 1-11 times of the total weight of the corresponding fine powder is added, the content (weight ratio) of the water can reach more than 91.6%, and particularly, when the water which is 5-11 times of the total weight of the corresponding fine powder is added, the slurry (filling and supporting material) obtained by mixing the slurry A and the slurry B has the characteristics of wide raw material source, low cost, high resistance increasing speed, good toughness, no harm, no toxicity, no pollution and the like.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in detail and fully with reference to the following embodiments.
Example 1
(1) 60 parts of sulphoaluminate cement clinker and 10 parts of fluoroaluminate cement clinker; 10 parts of copper slag powder and 10 parts of silica fume; grinding aid, namely 0.5 part of triisopropanolamine, 0.2 part of propylene glycol and 2 parts of sodium acetate; retarder, borax 0.5 part, zinc sulfate 1 part, sodium phosphate 0.5 part; early agent comprising potassium chloride 0.5 parts, calcium chloride 1 part, and zinc chloride 0 part3 parts of ferric oxide and 3 parts of ferric oxide; 5 kilograms of mixed material consisting of 0.2 portion of methyl cellulose and 0.3 portion of hydroxyethyl cellulose as suspending agent. Grinding for 55 minutes by using a test ball mill with the diameter of phi 500 multiplied by 500mm to obtain the powder with the specific surface area of 356m 2 Adding water which is 5 times of the total weight of the fine powder A into the fine powder A of the first material per kg, and uniformly mixing to obtain slurry A;
(2) 5 parts of dihydrate gypsum, 50 parts of natural anhydrite and 5 parts of salt gypsum; 25 parts of quicklime; 5 parts of alkaline residue and 5 parts of boiling furnace slag; the accelerating agent comprises 2 parts of ferric hydroxide, 1 part of sodium carbonate and 0.2 part of potassium fluoride; reinforcing agents, namely 1 part of sodium sulfate and 0.5 part of calcium formate; 5 kg of suspending agent, namely 5 kg of mixed material consisting of 0.1 part of carboxymethyl cellulose and 0.2 part of hydroxyethyl cellulose, and grinding for 40 minutes by using a test ball mill with the diameter of 500mm multiplied by 500mm, wherein the specific surface area is 352m 2 Adding water which is 5 times of the total weight of the fine powder of the material B into the mixture and uniformly mixing the mixture to obtain slurry B;
(3) the water temperature for preparing the slurry A and the slurry B was 7 ℃.
(4) And mixing the slurry A and the slurry B according to the weight ratio of 1:1 to obtain slurry, and then measuring the physical and mechanical properties of the slurry.
Example 2:
(1) 70 parts of aluminate cement clinker and 10 parts of fluoroaluminate cement clinker; 10 parts of slag powder and 7 parts of fly ash; grinding aid, triethanolamine 0.2 parts and diethylene glycol 0.3 parts; retarder, potassium sodium tartrate 0.3 shares, sodium lignosulphonate 0.2 shares; the early agent comprises 1 part of calcium chloride, 0.4 part of magnesium chloride and 0.2 part of ferric oxide; the suspending agent comprises 0.2 part of methyl cellulose and 0.2 part of carboxymethyl cellulose, and the weight of the mixed material is 5 kilograms. Grinding for 70 minutes by using a test ball mill with the diameter of phi 500 multiplied by 500mm to obtain the powder with the specific surface area of 512m 2 Adding water which is 6 times of the total weight of the fine powder A into the fine powder A of the first material per kg, and uniformly mixing to obtain slurry A;
(2) 60 parts of natural anhydrite and 5 parts of phosphogypsum; 10 parts of quicklime and 9 parts of calcium hydroxide; 5 parts of carbide slag and 3 parts of calcium carbonate powder; the accelerating agent comprises 1 part of potassium carbonate, 1.5 parts of sodium fluoride and 0.7 part of sodium fluosilicate; the reinforcing agent comprises 1 part of potassium sulfate, 2 parts of sodium sulfite and 1 part of potassium tripolyphosphate; suspending agent consisting of carboxymethyl cellulose 0.5 part and hydroxypropyl methyl cellulose 0.3 part, and the weight ratio of the suspending agent is 500mm × 500mmThe test ball mill grinds for 45 minutes, and the specific surface area is 530m 2 Adding water which is 6 times of the total weight of the fine powder of the material B into the mixture and uniformly mixing the mixture to obtain slurry B;
(3) the water temperature for preparing the slurry A and the slurry B is 8 ℃.
(4) And mixing the slurry A and the slurry B according to the weight ratio of 1:1 to obtain slurry, and then measuring the physical and mechanical properties of the slurry.
Example 3:
(1) 65 parts of aluminate cement clinker and 20 parts of iron aluminate cement clinker; 5 parts of steel slag powder and 5 parts of silica fume; grinding aid, such as 0.3 part of glycol, 0.4 part of glycerol and 1 part of sodium acetate; retarder, potassium citrate 0.5 part, oxalic acid 0.1 part, zinc sulfate 0.2 part; the early agent comprises 1 part of sodium chloride, 1 part of magnesium chloride and 0.1 part of lithium chloride; 5 kilograms of mixed material is composed of 0.1 portion of carboxymethyl cellulose and 0.3 portion of hydroxyethyl cellulose as suspending agent. Grinding for 75 minutes by using a test ball mill with the diameter of phi 500 multiplied by 500mm to obtain the powder with the specific surface area of 600m 2 Adding water which is 11 times of the total weight of the fine powder A into the fine powder A of the first material per kg, and uniformly mixing to obtain slurry A;
(2) 45 parts of natural anhydrite and 15 parts of fluorine gypsum; 20 parts of calcium hydroxide; 5 parts of alkaline residue and 5 parts of calcium carbonate powder; the accelerating agent comprises 4 parts of cement accelerating agent, 0.4 part of lithium hydroxide and 2 parts of sodium silicate; 2 parts of aluminum potassium sulfate and 1 part of sodium tripolyphosphate as reinforcing agents; 5 kilograms of mixed material consisting of 0.3 portion of carboxymethyl cellulose and 0.3 portion of hydroxypropyl methyl cellulose as suspending agent is ground for 50 minutes by a test ball mill with the diameter phi of 500 multiplied by 500mm, and the specific surface area is 593m 2 Adding water which is 11 times of the total weight of the fine powder of the second material into the mixture and uniformly mixing the mixture to obtain slurry B;
(3) the water temperature for preparing the slurry A and the slurry B is 8 ℃.
(4) And mixing the slurry A and the slurry B according to the weight ratio of 1:1 to obtain slurry, and then measuring the physical and mechanical properties of the slurry.
Comparative example 1:
(1) 70 parts of aluminate cement clinker and 10 parts of fluoroaluminate cement clinker; 10 parts of slag powder and 7 parts of fly ash; retarder, potassium sodium tartrate 0.3 shares, sodium lignosulphonate 0.2 shares; the early agent comprises 1 part of calcium chloride, 0.4 part of magnesium chloride and 0.2 part of ferric oxide; the suspending agent comprises 0.2 part of methyl cellulose and 0.2 part of carboxymethyl cellulose, and the weight of the mixed material is 5 kilograms. Grinding with a test ball mill of phi 500 × 500mm for 70 minutes to obtain fine powder A (surface area of the fine powder A is measured, as shown in Table 2), adding water 6 times of the total weight of the fine powder A, and mixing to obtain slurry A;
(2) 60 parts of natural anhydrite and 5 parts of phosphogypsum; 10 parts of quicklime and 9 parts of calcium hydroxide; 5 parts of carbide slag and 3 parts of calcium carbonate powder; the accelerating agent comprises 1 part of potassium carbonate, 1.5 parts of sodium fluoride and 0.7 part of sodium fluosilicate; the reinforcing agent comprises 1 part of potassium sulfate, 2 parts of sodium sulfite and 1 part of potassium tripolyphosphate; 5 kg of suspending agent, namely 5 kg of mixed material consisting of 0.5 part of carboxymethyl cellulose and 0.3 part of hydroxypropyl methyl cellulose, and grinding for 45 minutes by using a test ball mill with the diameter of 500mm multiplied by 500mm, wherein the surface area is 530m 2 Adding water which is 6 times of the total weight of the fine powder of the material B into the mixture and uniformly mixing the mixture to obtain slurry B;
(3) the water temperature for preparing the slurry A and the slurry B is 8 ℃.
(4) After slurry a and slurry B were mixed at a weight ratio of 1:1, the physical and mechanical properties were measured and compared with the slurry properties obtained in example 2, and the data are shown in table 2.
Comparative example 2:
(1) 70 parts of aluminate cement clinker and 10 parts of fluoroaluminate cement clinker; retarder, potassium sodium tartrate 0.3 shares, sodium lignosulphonate 0.2 shares; the suspending agent comprises 0.2 part of methyl cellulose and 0.2 part of carboxymethyl cellulose, and the weight of the mixed material is 5 kilograms. Grinding for 70 minutes by using a test ball mill with the diameter of phi 500 multiplied by 500mm to obtain the powder with the surface area of 446m 2 Adding water which is 6 times of the total weight of the fine powder A into the fine powder A of the first material per kg, and uniformly mixing to obtain slurry A;
(2) 60 parts of natural anhydrite and 5 parts of phosphogypsum; 10 parts of quicklime and 9 parts of calcium hydroxide; the accelerating agent comprises 1 part of potassium carbonate, 1.5 parts of sodium fluoride and 0.7 part of sodium fluosilicate; 5 kg of suspending agent, namely 5 kg of mixed material consisting of 0.5 part of carboxymethyl cellulose and 0.3 part of hydroxypropyl methyl cellulose, and grinding for 45 minutes by using a test ball mill with the diameter of phi 500 multiplied by 500mm, wherein the specific surface area is 533m 2 Adding water which is 6 times of the total weight of the fine powder of the material B into the mixture and uniformly mixing the mixture to obtain slurry B;
(3) the water temperature for preparing the slurry A and the slurry B is 8 ℃.
(4) After slurry a and slurry B were mixed at a weight ratio of 1:1, the physical and mechanical properties were measured and compared with the slurry properties obtained in example 2, and the data are shown in table 3.
Comparative example 3:
(1) 70 parts of aluminate cement clinker and 10 parts of fluoroaluminate cement clinker; grinding aid, triethanolamine 0.2 parts and diethylene glycol 0.3 parts; retarder, potassium sodium tartrate 0.3 shares, sodium lignosulphonate 0.2 shares; the early agent is a mixture of 1 part of calcium chloride, 0.4 part of magnesium chloride and 0.2 part of ferric oxide, and the weight of the mixture is 5 kg. Grinding for 70 minutes by using a test ball mill with the diameter of phi 500 multiplied by 500mm to obtain the powder with the surface area of 501m 2 Adding water which is 6 times of the total weight of the fine powder A into the fine powder A of the first material per kg, and uniformly mixing to obtain slurry A;
(2) 60 parts of natural anhydrite and 5 parts of phosphogypsum; 10 parts of quicklime and 9 parts of calcium hydroxide; the accelerating agent comprises 1 part of potassium carbonate, 1.5 parts of sodium fluoride and 0.7 part of sodium fluosilicate; the intensifier is 5 kg of mixed material consisting of 1 part of potassium sulfate, 2 parts of sodium sulfite and 1 part of potassium tripolyphosphate, and the mixed material is ground for 45 minutes by a test ball mill with the diameter of phi 500 multiplied by 500mm, and the surface area of the mixed material is 539m 2 Adding water which is 6 times of the total weight of the fine powder of the material B into the mixture and uniformly mixing the mixture to obtain slurry B;
(3) the water temperature for preparing the slurry A and the slurry B is 8 ℃.
(4) After slurry a and slurry B were mixed at a weight ratio of 1:1, the physical and mechanical properties were measured and compared with the slurry properties obtained in example 2, and the data are shown in table 3.
Comparative example 4:
(1) 70 parts of aluminate cement clinker and 10 parts of fluoroaluminate cement clinker; 10 parts of slag powder and 7 parts of coal ash; grinding aid, triethanolamine 0.2 parts and diethylene glycol 0.3 parts; retarder, potassium sodium tartrate 0.3 shares, sodium lignosulphonate 0.2 shares; the early agent comprises 1 part of calcium chloride, 0.4 part of magnesium chloride and 0.2 part of ferric oxide; suspending agent: 0.7 part of potassium ethyl xanthate constitutes 5 kg of mixed material. Grinding for 70 minutes by using a test ball mill with the diameter of phi 500 multiplied by 500mm to obtain the powder with the surface area of 514m 2 A fine powder of the first material/kg, thenAdding water of which the weight is 6 times of that of the fine powder A, and uniformly mixing to obtain slurry A;
(2) 60 parts of natural anhydrite and 5 parts of phosphogypsum; 10 parts of quicklime and 9 parts of calcium hydroxide; 5 parts of carbide slag and 3 parts of calcium carbonate powder; the accelerating agent comprises 1 part of potassium carbonate, 1.5 parts of sodium fluoride and 0.7 part of sodium fluosilicate; the reinforcing agent comprises 1 part of potassium sulfate, 2 parts of sodium sulfite and 1 part of potassium tripolyphosphate; 0.8 part of redispersible latex powder (VAE) to form 5 kg of mixed material, and the mixed material is ground for 45 minutes by a test ball mill with the diameter of 500mm multiplied by 500mm, and the surface area is 537m 2 Adding water which is 6 times of the total weight of the fine powder of the material B into the mixture and uniformly mixing the mixture to obtain slurry B;
(3) the water temperature for preparing the slurry A and the slurry B is 8 ℃.
(4) After slurry a and slurry B were mixed at a weight ratio of 1:1, the physical and mechanical properties were measured and compared with the slurry properties obtained in example 2, and the data are shown in table 3.
Effect example 1:
the physical properties and uniaxial compressive strength of the fine powder A and the fine powder B obtained in examples 1 to 3 and the slurry were measured by JC/T984-2011, and the results are shown in Table 1:
as can be seen from table 1, in examples 1 to 3, slurry a and slurry B, which were obtained from fine powder a and fine powder B, respectively, using water at 6 ℃ to 8 ℃, were able to solidify in a short time after mixing, and the upper and lower layers were well uniform after mixing, and the compressive strengths of 1d, 7d, and 28d all satisfied the strength requirements of fillers of different designs.
Effect example 2:
the physical property profiles of the A charge fine powder, the B charge fine powder, and the slurry obtained from comparative example 1 and example 2, respectively, are shown in Table 2:
as can be seen from Table 2, when no grinding aid is added, the specific surface area of the obtained powder is small and the particle size of the material is large when the powder is ground for the same time under the same grinding conditions; in addition, when the specific surface of the powder is too low, although the slurry A and the slurry B obtained from the fine powder A and the fine powder B using water of 6 ℃ to 8 ℃ can be solidified after mixing, the solidification time is prolonged, and the mixing is not uniform, and the strength after mixing is small.
Effect example 3:
the physical property pairs of the A charge fine powder, the B charge fine powder, and the slurry obtained from comparative examples 2 to 4, and example 2, respectively, are shown in Table 3:
as can be seen from table 3, after the fine powder a lacks solid waste, a grinding aid, and an early agent, and the fine powder B lacks solid waste, an accelerator, and a reinforcing agent, and the fine powder a and the fine powder B are mixed with water at 8 ℃ to prepare slurry a and slurry B, the initial setting time is long and the strength is low after the slurry a and the slurry B are mixed. In addition, after the fine powder A is lack of solid waste and suspending agent, and the fine powder B is lack of solid waste and suspending agent, the fine powder A and the fine powder B are respectively mixed by water with the temperature of 8 ℃ to prepare slurry A and slurry B, and the initial setting time is long and the strength is low after the slurry A and the slurry B are mixed. In addition, after the suspending agent (hydroxyethyl cellulose) in the fine powder A and the fine powder B in the application is replaced by the common potassium ethylxanthate, after the fine powder A and the fine powder B are respectively prepared into the slurry A and the slurry B by mixing water with the temperature of 8 ℃, the initial setting time is long and the strength is low after the slurry A and the slurry B are mixed.
Claims (10)
1. The mining low-temperature ultrahigh-crystallization-water rapid-solidification filling support material is characterized by comprising a material with a specific surface area of 350-600 m 2 The material A fine powder and the material B fine powder are/kg;
wherein the fine powder of the material A is made of Al 2 O 3 Content (wt.)>19 percent of cement clinker, solid waste and grinding aidGrinding a mixed material consisting of the retarder, the early-stage admixture and the suspending agent to obtain the composite material;
and the material B fine powder is obtained by grinding a mixed material consisting of gypsum, lime, solid waste, an accelerating agent, a reinforcing agent and a suspending agent.
2. The mining low-temperature ultrahigh-crystalline water rapid-hardening filling support material as claimed in claim 1, characterized in that the mixture ratio of the fine powder of the material A is as follows by weight: 65-99.8 parts of cement clinker, 0.1-20 parts of solid waste, 0.05-5 parts of grinding aid, 0.05-3 parts of retarder, 0.05-5 parts of early agent and 0.05-2 parts of suspending agent.
3. The mining low-temperature ultrahigh-crystalline water rapid-hardening filling support material as claimed in claim 1, characterized in that the specific surface areas of the fine powder of the material A are 356-600 m 2 /kg；
The first material fine powder comprises the following components in parts by weight: 70-85 parts of cement clinker, 10-20 parts of solid waste, 0.5-2.7 parts of grinding aid, 0.5-2 parts of retarder, 1.6-4.8 parts of early agent and 0.4-0.5 part of suspending agent.
4. The mining low-temperature ultrahigh-crystalline water rapid-setting filling and supporting material as claimed in any one of claims 1 to 3, wherein the cement clinker is selected from one or a mixture of any two or more of aluminate cement clinker, sulphoaluminate cement clinker, aluminoferrite cement clinker and fluoroaluminate cement clinker;
the solid waste in the first material fine powder is any one or mixture of any two or more of slag powder, steel slag powder, copper slag powder, fly ash and silica fume.
5. The mining low-temperature ultrahigh-crystal water rapid-setting filling supporting material as claimed in claim 4, wherein the grinding aid is one or a mixture of any two or more of triethanolamine, triisopropanolamine, ethylene glycol, propylene glycol, diethylene glycol, glycerol and sodium acetate;
the retarder is formed by mixing any one or any two or more than two of citric acid and salts thereof, boric acid and salts thereof, tartaric acid and salts thereof, oxalic acid, zinc salt, phosphate and lignosulfonate;
the early agent is any one or mixture of any two or more of potassium chloride, sodium chloride, calcium chloride, magnesium chloride, zinc chloride, lithium chloride and ferric oxide.
6. The mining low-temperature ultrahigh-crystalline water rapid-hardening filling supporting material as claimed in claim 1, characterized in that the proportion of the fine powder of the material B is as follows by weight: 50-90 parts of gypsum, 5-50 parts of lime, 1-30 parts of solid waste, 0.05-10 parts of an accelerator, 0.05-5 parts of a reinforcing agent and 0.05-2 parts of a suspending agent.
7. The mining low-temperature ultrahigh-crystalline water rapid-hardening filling supporting material as claimed in claim 1, characterized in that the specific surface areas of the fine powder of the second material are 352-593 m 2 /kg；
The proportion of the material B fine powder is as follows by weight: 60-65 parts of gypsum, 19-25 parts of lime, 8-10 parts of solid waste, 3.2-6.4 parts of an accelerator, 1.5-4 parts of a reinforcing agent and 0.3-0.8 part of a suspending agent.
8. The mining low-temperature ultrahigh-crystalline water rapid-setting filling supporting material as claimed in claim 1, 6 or 7, wherein the gypsum is a mixture of any two or more of dihydrate gypsum, natural anhydrite, phosphogypsum, fluorgypsum, salt gypsum and hemihydrate gypsum;
the lime is one or a mixture of two of quicklime and calcium hydroxide;
the solid waste in the material B is prepared by mixing any one or two of carbide slag, alkali slag, boiling furnace slag and calcium carbonate powder;
the accelerator is one or a mixture of two of cement accelerator, ferric hydroxide, potassium carbonate, sodium carbonate, lithium hydroxide, potassium fluoride, sodium silicate and sodium fluosilicate sold in the market;
the reinforcing agent is one or a mixture of two of potassium sulfate, sodium sulfite, aluminum potassium sulfate, calcium formate, potassium tripolyphosphate and sodium tripolyphosphate.
9. The mining low-temperature ultrahigh-crystalline water rapid-setting filling and supporting material as claimed in claim 1, characterized in that the suspending agent is composed of one or/and a mixture of methylcellulose, carboxymethylcellulose, hydroxypropyl methylcellulose and hydroxyethyl cellulose.
10. The preparation method of the mining low-temperature ultrahigh-crystallization-water rapid-setting filling support material is characterized by comprising the following steps of:
(1) grinding a mixed material consisting of cement clinker, solid waste, grinding aid, retarder, early agent and suspending agent to a specific surface area of 350-600 m 2 Adding water which is 1-11 times of the total weight of the fine powder A and has the water temperature of more than 6 ℃ into the fine powder A, and uniformly mixing to obtain slurry A;
(2) grinding a mixed material consisting of gypsum, lime, solid waste, an accelerating agent, a reinforcing agent and a suspending agent to a specific surface area of 350-600 m 2 Adding water which is 1-11 times of the total weight of the fine powder B and has the water temperature of more than 6 ℃ into the fine powder B, uniformly mixing the water and the fine powder to obtain slurry B;
(3) and mixing the slurry A and the slurry B according to the weight ratio of 1 (0.8-1.2), wherein the setting time of the obtained slurry is 5-45 minutes.
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