CN117430366A - Additive for foaming cement filling material of deep mine and preparation method thereof - Google Patents
Additive for foaming cement filling material of deep mine and preparation method thereof Download PDFInfo
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- CN117430366A CN117430366A CN202311325154.3A CN202311325154A CN117430366A CN 117430366 A CN117430366 A CN 117430366A CN 202311325154 A CN202311325154 A CN 202311325154A CN 117430366 A CN117430366 A CN 117430366A
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- filling material
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- 239000004568 cement Substances 0.000 title claims abstract description 68
- 238000005187 foaming Methods 0.000 title claims abstract description 64
- 239000000654 additive Substances 0.000 title claims abstract description 37
- 230000000996 additive effect Effects 0.000 title claims abstract description 37
- 239000000463 material Substances 0.000 title claims abstract description 34
- 238000011049 filling Methods 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000006260 foam Substances 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910001868 water Inorganic materials 0.000 claims abstract description 24
- 230000000087 stabilizing effect Effects 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 230000003014 reinforcing effect Effects 0.000 claims abstract description 13
- 230000002195 synergetic effect Effects 0.000 claims abstract description 12
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 8
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical group OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 14
- 239000012744 reinforcing agent Substances 0.000 claims description 11
- 239000002270 dispersing agent Substances 0.000 claims description 10
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 8
- 239000000835 fiber Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 8
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 239000004156 Azodicarbonamide Substances 0.000 claims description 6
- XOZUGNYVDXMRKW-AATRIKPKSA-N azodicarbonamide Chemical group NC(=O)\N=N\C(N)=O XOZUGNYVDXMRKW-AATRIKPKSA-N 0.000 claims description 6
- 235000019399 azodicarbonamide Nutrition 0.000 claims description 6
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 5
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 4
- JGIATAMCQXIDNZ-UHFFFAOYSA-N calcium sulfide Chemical group [Ca]=S JGIATAMCQXIDNZ-UHFFFAOYSA-N 0.000 claims description 4
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical group [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 4
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 4
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 4
- 235000011152 sodium sulphate Nutrition 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 125000000373 fatty alcohol group Chemical group 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 239000004566 building material Substances 0.000 abstract description 2
- 230000007547 defect Effects 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 28
- 230000000052 comparative effect Effects 0.000 description 11
- 238000003756 stirring Methods 0.000 description 10
- 238000010521 absorption reaction Methods 0.000 description 8
- 238000001035 drying Methods 0.000 description 8
- -1 sodium fatty alcohol Chemical class 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 238000009413 insulation Methods 0.000 description 7
- 239000011734 sodium Substances 0.000 description 6
- 229910052708 sodium Inorganic materials 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 5
- 230000009172 bursting Effects 0.000 description 5
- 239000003245 coal Substances 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000011381 foam concrete Substances 0.000 description 4
- 229910017604 nitric acid Inorganic materials 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 150000002191 fatty alcohols Chemical class 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000006703 hydration reaction Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000005543 nano-size silicon particle Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 239000004604 Blowing Agent Substances 0.000 description 1
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 229920005830 Polyurethane Foam Polymers 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- 239000004088 foaming agent Substances 0.000 description 1
- 239000008233 hard water Substances 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000011496 polyurethane foam Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000003469 silicate cement Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/02—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding chemical blowing agents
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/40—Porous or lightweight materials
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/70—Grouts, e.g. injection mixtures for cables for prestressed concrete
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses an additive of a foaming cement filling material for a deep mine and a preparation method thereof, belonging to the technical field of building materials. The additive of the deep mine foaming cement filling material comprises the following raw materials in parts by mass: 30-40 parts of foaming component, 3-5 parts of foam stabilizing component, 0.4-0.8 part of synergistic component, 0.5-1 part of reinforcing component, 0.4-1.2 parts of toughening component, 0.6-1 part of auxiliary agent and 51-65.1 parts of water. According to the invention, a series of components and auxiliary agents are introduced by optimizing the raw material formula, so that the defects of low strength, poor toughness and low foaming multiple of the foaming cement are overcome, and the foaming cement is suitable for the environment of high ground temperature and high ground pressure of a deep mine. The additive designed by the invention does not contain any harmful substances, avoids environmental pollution, and is convenient and quick to construct and lower in cost.
Description
Technical Field
The invention relates to the technical field of building materials, in particular to an additive of a foaming cement filling material for a deep mine and a preparation method thereof.
Background
At present, with continuous exploitation and utilization of coal resources, coal resources at the shallow part of the surface gradually become depleted. The average mining depth of the current coal seam is about 600m, and the coal resources exceeding kilometers account for 53.3 percent. However, the geological conditions of the deep mine are complex, the geological environment is poor, and accident disasters are frequent; many goafs can be left in the mineral exploitation process, if filling is not carried out in time, the exploitation efficiency can be affected, and the life safety of operators can be threatened.
The geological conditions of the deep mine are complex, the geological environment is poor due to high temperature and high pressure, the concentration of gas and mine dust is too high, disasters such as goaf collapse and the like are frequent, the life safety of miners is seriously threatened, and the safe and efficient exploitation of coal mine resources is restricted. This requires that the filling material for deep mines have fire resistance to prevent fires, foam quickly to block harmful gases, strength and toughness to long accommodate deep high stress formation movement, and low production costs to facilitate large scale filling.
The research of foaming cement at present is mainly focused on the field of building outer walls, and focuses on the directions of quick demoulding, fire prevention, heat preservation, heat insulation, sound insulation, foam stabilization, light weight and the like; however, the requirements of the foaming cement for mines are as follows: the toughness is good (foam stabilization), and the material can adapt to stratum movement for a long time; the expansion multiple is high, and the material consumption is reduced; has certain strength.
The filling material used in the mine engineering at present is mainly a pure organic polymer, namely polyurethane foam filling material, and although the material has good elasticity and high binding power, the cost of the material is higher and is not suitable for filling large-volume cavities; and the pure polyurethane material has no flame retardance and is not suitable for the deep high-temperature mine environment. Therefore, it is urgently needed to design an additive for foaming cement, so that the prepared filling material has the characteristics of rapid foaming, flame retardance, heat insulation, high strength, high toughness, low cost and the like, and is more suitable for the high-temperature high-pressure environment of a deep mine.
Disclosure of Invention
The invention aims to provide an additive for a foaming cement filling material for a deep mine and a preparation method thereof, which are used for solving the problem that the existing filling material is not suitable for the high-temperature high-pressure environment of the deep mine. When the additive provided by the invention is used for the foaming cement filling material of the deep mine, the foaming multiplying power and the foaming speed of the foaming cement filling material can be improved, and the foaming cement filling material has certain strength and toughness, excellent flame retardance and heat insulation performance and low cost; the additive does not contain any harmful substances, and environmental pollution is avoided.
In order to achieve the above purpose, the present invention provides the following technical solutions:
one of the technical schemes of the invention is as follows: the additive for the foaming cement filling material of the deep mine comprises the following raw materials in parts by mass:
30-40 parts of foaming component, 3-5 parts of foam stabilizing component, 0.4-0.8 part of synergistic component, 0.5-1 part of reinforcing component, 0.4-1.2 parts of toughening component, 0.6-1 part of auxiliary agent and 51-65.1 parts of water.
Preferably, the foaming component is hydrogen peroxide; the foam stabilizing component is fatty alcohol polyoxyethylene ether sodium sulfate and/or sodium dodecyl sulfate.
More preferably, the foam stabilizing component is sodium fatty alcohol polyoxyethylene ether sulfate and sodium dodecyl sulfate with a mass ratio of 1:1.
The invention selects hydrogen peroxide as a foaming agent, and the hydrogen peroxide can decompose and release a large amount of oxygen in an alkaline environment during cement hydration to generate a large amount of bubbles. The fatty alcohol polyoxyethylene ether sodium sulfate and the sodium dodecyl sulfate are selected as foam stabilizing components, are not easy to decompose in an alkaline and high-temperature composite environment, and can also be used as an anionic surfactant to effectively reduce the surface tension of bubbles, so that the foam is not easy to break, and the stability of the foam is improved; the molecular chain of the foam stabilizing component contains a certain amount of active groups, can be adsorbed on the surface of the foam and are arranged according to a rule, so that the elasticity of a liquid film is increased, and the foam can realize self-repairing under the action of external force.
Preferably, the synergistic component is azodicarbonamide.
According to the invention, the azodicarbonamide is selected as a synergistic component, is yellow powder, is nontoxic and odorless, is insoluble in gasoline, alcohol, benzene, pyridine and water, can penetrate into concrete, and is greatly exothermic in the cement hydration reaction process, nitrogen, carbon dioxide, water and ammonia are generated by the thermal decomposition of the azodicarbonamide, the generated ammonia reacts with hydrogen peroxide to generate nitrogen and water, and a large amount of gas is discharged in the whole reaction process, so that the foaming efficiency is greatly improved; and partial ammonia gas can react with oxygen generated by decomposing hydrogen peroxide in alkaline environment to generate nitric oxide and water, nitric oxide can be oxidized into nitrogen dioxide by oxygen, nitric acid can be generated by the reaction of nitrogen dioxide and water, nitric acid is a highly oxidative corrosive liquid, and is stable in property under normal conditions, however, when partial organic matters are encountered, especially when the organic matters are in a high-temperature state or are subjected to strong mechanical impact, bursting can occur, mainly because nitric acid can react with the organic matters (dispersing agent-sodium polyacrylate) and generate combustible gas, in addition, nitric acid is rapidly decomposed at high temperature, a large amount of gas can be generated in a short time (greatly improving foaming efficiency), and physical bursting can also be generated under high-pressure environment. Bursting produces more foam and air holes to further increase the foaming efficiency.
Preferably, the reinforcing component is nano-silica.
According to the invention, nano silicon dioxide is selected as the reinforcing component, and the reinforcing component can be uniformly distributed in the foam in the bursting process, so that the strength of the foam is improved.
Preferably, the toughening component is a polyvinyl alcohol fiber.
According to the invention, polyvinyl alcohol fibers are selected as toughening components of the foaming cement, and the brittleness and toughness of the foaming cement are improved by utilizing the high strength and high modulus of the fibers so as to adapt to deep high-ground stress environments; the fiber is uniformly dispersed in the foaming cement in the bursting process, when the filling material is subjected to external force, the fiber can bear a part of load, and meanwhile, the fiber can also prevent and inhibit the expansion of cracks, so that the brittleness of the foaming cement is improved, and the toughness of the foaming cement is greatly improved.
Preferably, the auxiliary agent is a reinforcing agent and/or a dispersing agent; the reinforcing agent is calcium sulfide and/or sodium sulfide; the dispersing agent is sodium polyacrylate.
More preferably, the reinforcing agent is calcium sulfide and sodium sulfide in a mass ratio of 1:1.
The strength of the foaming cement can be improved by the selected reinforcing agent so as to adapt to the high-ground stress environment. Sodium polyacrylate is selected as the dispersing agent to prevent aggregation and sedimentation of the components.
The second technical scheme of the invention is as follows: the preparation method of the additive for the foaming cement filling material for the deep mine comprises the following steps:
and mixing the raw materials to obtain the additive of the foaming cement filling material for the deep mine.
The third technical scheme of the invention: the application of the additive in preparing the foaming cement filling material for the deep mine is provided.
Preferably, the additive is added to the cement in an amount of 5wt%.
The beneficial technical effects of the invention are as follows:
according to the invention, a series of components and auxiliary agents are introduced by optimizing the raw material formula, so that the defects of foamed cement, low strength, poor toughness, coarse foaming, low multiplying power, low foaming speed, uneven foaming and the like are overcome, and the strength and toughness of the material are improved, so that the foamed cement is suitable for the high-ground-temperature high-pressure environment of a deep mine. The additive designed by the invention does not contain any harmful substances, avoids environmental pollution, and has the advantages of convenient construction, high foaming multiple, less material consumption and lower cost. The preparation method of the foaming cement additive is simple and easy to implement, and the foaming cement additive can be prepared in a mine at any time.
Detailed Description
Various exemplary embodiments of the invention will now be described in detail, which should not be considered as limiting the invention, but rather as more detailed descriptions of certain aspects, features and embodiments of the invention. It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
In addition, for numerical ranges in this disclosure, it is understood that each intermediate value between the upper and lower limits of the ranges is also specifically disclosed. Every smaller range between any stated value or stated range, and any other stated value or intermediate value within the stated range, is also encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention.
The terms "comprising," "including," "having," "containing," and the like as used herein are open-ended terms, meaning including, but not limited to.
The foaming component used in the following examples and comparative examples of the present invention is hydrogen peroxide; the reinforcing component is nano silicon dioxide; the toughening component is polypropylene alcohol fiber; the dispersing agent is sodium polyacrylate; the foam stabilizing component consists of fatty alcohol polyoxyethylene ether sodium sulfate and sodium dodecyl sulfate in a mass ratio of 1:1; the synergistic component is azodicarbonamide; the reinforcing agent consists of calcium sulfide and sodium sulfide in a mass ratio of 1:1.
The raw materials used in the following examples and comparative examples of the present invention are all commercially available products.
Example 1
The foaming cement additive comprises the following raw materials in parts by weight:
30 parts of foaming component, 3 parts of foam stabilizing component, 0.4 part of synergistic component, 0.5 part of reinforcing component, 0.4 part of toughening component, 0.3 part of reinforcing agent, 0.3 part of dispersing agent and 65.1 parts of water.
The preparation method of the foaming cement additive comprises the following steps:
pouring the foam stabilizing component, the reinforcing component, the toughening component, the reinforcing agent and the dispersing agent into a stirrer, stirring for 1min at 15 ℃, adding the synergistic component and 50 ℃ water, continuously stirring for 2min, gradually adding the foaming component during stirring, and obtaining the foaming cement additive after stirring is completed.
The reason for selecting multiple stirring in the preparation process is as follows: in the primary stirring (15 ℃) process, stirring is performed to make the raw materials mixed more uniformly so as to promote the subsequent reaction activity, so that the temperature capable of ensuring the thermal stability of components such as sodium fatty alcohol-polyoxyethylene ether sulfate is selected. In the subsequent stirring (50 ℃ water), stirring is performed to ensure the resource utilization efficiency (inhibit the thermal decomposition of raw materials) and simultaneously make the activity of components such as azodicarbonamide as higher as possible so as to fully foam; moreover, the invention has been found after research that in the reaction system of the invention, the foaming effect of hot water heating is far higher than that of direct heating.
Example 2
The foaming cement additive comprises the following raw materials in parts by weight:
35 parts of foaming component, 4 parts of foam stabilizing component, 0.6 part of synergistic component, 0.8 part of reinforcing component, 0.8 part of toughening component, 0.4 part of reinforcing agent, 0.4 part of dispersing agent and 58 parts of water.
The preparation of the foamed cement additive is described in example 1.
Example 3
The foaming cement additive comprises the following raw materials in parts by weight:
40 parts of foaming component, 5 parts of foam stabilizing component, 0.8 part of synergistic component, 1 part of reinforcing component, 1.2 parts of toughening component, 0.5 part of reinforcing agent, 0.5 part of dispersing agent and 51 parts of water.
The preparation of the foamed cement additive is described in example 1.
Comparative example 1
The only difference from example 3 is that the addition of the reinforcing component was omitted.
Comparative example 2
The only difference from example 3 is that the addition of toughening components was omitted.
Comparative example 3
The only difference from example 3 is that the addition of the synergistic component is omitted.
Comparative example 4
The only difference from example 3 is that the addition of auxiliary agent was omitted.
Comparative example 5
The only difference from example 3 is that the foam stabilizing component is replaced with sodium fatty alcohol polyoxyethylene ether sulfate of equal mass.
Comparative example 6
The only difference from example 3 is that the foam stabilizing component is replaced by equal mass of sodium dodecyl sulfate.
Effect verification
Foamed cement was prepared using the products of examples 1 to 3 and comparative examples 1 to 6 as a foamed cement additive. The preparation method comprises the following steps:
mixing the prepared additive with cement, stirring for 5min with a cement stirrer, covering a layer of preservative film on the surface, standing and foaming. Demolding until the cement has initial strength, and curing in a drying oven at 50 ℃ for 7d.
The components of the cement are as follows: 70wt% of PII silicate cement and 30wt% of fly ash; the cement content is 95% of the total mass.
(1) The compressive strength of the produced foamed cement was tested:
the compressive strength of the foamed cement was tested according to the standards of JG/T266-2011, foam concrete, GB/T5486-2008, inorganic hard Heat insulation product test method. Cutting the test piece into standard cubes with the dimensions of 100mm multiplied by 100mm, putting the cut test piece into a drying box at 60 ℃ for drying until the weight is constant, and then testing the compressive strength, wherein the compressive strength is calculated according to the following formula:
sigma-compressive strength of the test specimen in MPa;
f, the destructive load of the sample, and the unit N;
a-area of pressure applied to test specimen in mm 2 。
(2) Testing the water absorption of the foamed cement:
the water absorption of the foamed cement was tested according to the standards of JG/T266-2011 foam concrete and GB/T5486-2008 inorganic hard Heat insulation product test method. Cutting a test piece into standard cubes with the dimensions of 100mm multiplied by 100mm, drying the cut test piece in a drying box at 60 ℃ until the weight is constant, adding water according to the steps in the specification after cooling, fishing out the test piece from the water after 24 hours, wiping off the surface moisture, weighing, and calculating the water absorption according to the following formula:
w-water absorption of sample, unit;
m 1 the mass of the dried sample in g;
m 2 the mass of the sample after absorption of water, in g.
(3) Dry density of the foamed cement was tested:
the water absorption of the foamed cement was tested according to the standards of JG/T266-2011 foam concrete and GB/T5486-2008 inorganic hard Heat insulation product test method. Cutting the test piece into standard cubes with the dimensions of 100mm multiplied by 100mm, putting the cut test piece into a drying box at 60 ℃ for drying to constant weight, and weighing the mass m of the test piece after cooling 1 Then measuring the length, width and height of the test piece, and calculating the volume V of the test piece. The dry density is calculated as follows:
ρ -dry density of sample;
v-the volume of the test piece;
m 1 the mass of the dried sample in g.
(4) Testing the heat conductivity coefficient of the foaming cement:
the thermal conductivity of the foamed cement was measured according to GB/T10294 and the foamed cement was cut into 300mm by 20mm cement slabs. Before the heat conductivity test, the materials are dried in a drying box at 60 ℃ to constant weight, and are cooled and then tested on a DRM-II type heat conductivity tester.
(5) Testing the elastic modulus of the foamed cement:
the elastic modulus of the foamed cement was measured according to GB/T50081-2019 and the foamed cement was cut into prismatic standard test pieces of 150mm. Times.150 mm. Times.300 mm. 6 test pieces were prepared, of which 3 were subjected to uniaxial compressive strength measurement and the other 3 were subjected to elastic modulus measurement. Elastic modulus measurement is carried out by adopting a dial gauge, and the gauge length is 150mm.
When the elastic modulus is measured, the elastic modulus is loaded to an initial load value F with a reference stress of 0.5MPa 0 After a constant load of 60s, the deformation readings at each measuring point are recorded within the following 30s, and immediately thereafter the load value F is continuously and evenly applied to 1/3 of the axial compressive strength fcp a Deformation readings were recorded at each station after 60s holding constant load and over the following 30s, the modulus of elasticity was calculated as follows:
Δn＝ε a -ε 0
E c -elastic modulus of the foamed cement, unit MPa;
F a -load in N with a stress of 1/3 of the axial compressive strength;
F 0 -initial load at a stress of 0.5MPa, unit N;
a-area of pressure applied to test specimen in mm 2 ；
L-measuring gauge length, taking 150mm;
Δn-last slave F 0 Loading to F a The average value of deformation of two sides of the test piece is in mm;
ε a —F a the average value of deformation at two sides of the test piece;
ε 0 —F 0 and (3) an average value of deformation of two sides of the test piece.
(6) Determination of foaming times of foamed Cement
The foaming ratio of the foaming cement is tested according to JG/T266-2011 foam concrete. And filling foaming cement into a bottomless glass barrel with the volume of 250mL and the diameter of 60mm, and scraping the two ends of the bottomless glass barrel to determine the mass of the foaming cement. The foaming multiple M is calculated according to the following formula:
wherein:
m is foaming multiple;
v-glass barrel volume;
density of rho-blowing agent aqueous solution in g/mm 3 ；
G 1 -glass barrel mass;
G 2 glass barrels and foam mass in g.
The test results of effect verification (1) to (6) are shown in table 1.
Table 1 performance test
From the test data of comparative example 6 in table 1, it can be obtained that when the foam stabilizing component is sodium dodecyl sulfate alone, the sample water absorption rate is increased because sodium dodecyl sulfate has non-negative commonality, has more superior surface activity and has better hard water resistance than sodium fatty alcohol polyoxyethylene ether sulfate; as can be seen from the test data of comparative example 5, when the foam stabilizing component is sodium polyoxyethylene fatty alcohol sulfate alone, the water absorption rate is also increased because the environmental temperature of the deep stratum is high, and sodium polyoxyethylene fatty alcohol sulfate is easily decomposed in an environment exceeding 50 ℃, resulting in a decrease in the performance of the material.
The above embodiments are only illustrative of the preferred embodiments of the present invention and are not intended to limit the scope of the present invention, and various modifications and improvements made by those skilled in the art to the technical solutions of the present invention should fall within the protection scope defined by the claims of the present invention without departing from the design spirit of the present invention.
Claims (9)
1. The additive for the foaming cement filling material of the deep mine is characterized by comprising the following raw materials in parts by mass:
30-40 parts of foaming component, 3-5 parts of foam stabilizing component, 0.4-0.8 part of synergistic component, 0.5-1 part of reinforcing component, 0.4-1.2 parts of toughening component, 0.6-1 part of auxiliary agent and 51-65.1 parts of water.
2. The additive of claim 1 wherein the foaming component is hydrogen peroxide; the foam stabilizing component is fatty alcohol polyoxyethylene ether sodium sulfate and/or sodium dodecyl sulfate.
3. An additive according to claim 1 wherein the synergistic component is azodicarbonamide.
4. An additive according to claim 1, wherein the reinforcing component is silica.
5. An additive according to claim 1, wherein the toughening component is a polyvinyl alcohol fibre.
6. Additive according to claim 1, characterized in that the auxiliary agent is a reinforcing agent and/or a dispersing agent; the reinforcing agent is calcium sulfide and/or sodium sulfide; the dispersing agent is sodium polyacrylate.
7. A method for preparing an additive for a foamed cement filling material for a deep mine according to any one of claims 1 to 6, comprising the steps of:
and mixing the raw materials to obtain the additive of the foaming cement filling material for the deep mine.
8. Use of an additive according to any one of claims 1-6 for the preparation of a foamed cement filling material for deep mines.
9. Use according to claim 8, wherein the additive is added to the cement in an amount of 5wt%.
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