CN112919874A - Cement-based filling material containing various solid wastes and preparation method and application thereof - Google Patents
Cement-based filling material containing various solid wastes and preparation method and application thereof Download PDFInfo
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- 238000011049 filling Methods 0.000 title claims abstract description 86
- 239000004568 cement Substances 0.000 title claims abstract description 56
- 239000000463 material Substances 0.000 title claims abstract description 56
- 239000002910 solid waste Substances 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 239000002893 slag Substances 0.000 claims abstract description 48
- 239000010881 fly ash Substances 0.000 claims abstract description 45
- 239000010440 gypsum Substances 0.000 claims abstract description 42
- 229910052602 gypsum Inorganic materials 0.000 claims abstract description 42
- 238000006703 hydration reaction Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000002002 slurry Substances 0.000 claims abstract description 8
- 239000008399 tap water Substances 0.000 claims abstract description 7
- 235000020679 tap water Nutrition 0.000 claims abstract description 7
- 238000005086 pumping Methods 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- 239000011398 Portland cement Substances 0.000 claims description 5
- 238000007580 dry-mixing Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 25
- 238000010791 quenching Methods 0.000 abstract description 12
- 230000000171 quenching effect Effects 0.000 abstract description 12
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- 239000000843 powder Substances 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 6
- 239000011372 high-strength concrete Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
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- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 3
- 238000004364 calculation method Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
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- 239000004571 lime Substances 0.000 description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 3
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- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- 206010016807 Fluid retention Diseases 0.000 description 1
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- 229910052918 calcium silicate Inorganic materials 0.000 description 1
- -1 calcium silicate hydrates Chemical class 0.000 description 1
- VMLAJPONBZSGBD-UHFFFAOYSA-L calcium;hydrogen carbonate;hydroxide Chemical class [OH-].[Ca+2].OC([O-])=O VMLAJPONBZSGBD-UHFFFAOYSA-L 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
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- 238000002474 experimental method Methods 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
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- XJKVPKYVPCWHFO-UHFFFAOYSA-N silicon;hydrate Chemical compound O.[Si] XJKVPKYVPCWHFO-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
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- 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
- 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
- C04B28/144—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 a flue gas desulfurization product
-
- 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
- C04B18/00—Use of agglomerated or waste materials or refuse as fillers for mortars, concrete or artificial stone; Treatment of agglomerated or waste materials or refuse, specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B18/04—Waste materials; Refuse
- C04B18/06—Combustion residues, e.g. purification products of smoke, fumes or exhaust gases
- C04B18/08—Flue dust, i.e. fly ash
-
- 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
- C04B18/00—Use of agglomerated or waste materials or refuse as fillers for mortars, concrete or artificial stone; Treatment of agglomerated or waste materials or refuse, specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B18/04—Waste materials; Refuse
- C04B18/14—Waste materials; Refuse from metallurgical processes
- C04B18/141—Slags
- C04B18/142—Steelmaking slags, converter slags
-
- 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
- C04B2111/00034—Physico-chemical characteristics of the mixtures
- C04B2111/00146—Sprayable or pumpable mixtures
-
- 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
- C04B2111/00663—Uses not provided for elsewhere in C04B2111/00 as filling material for cavities or the like
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Environmental & Geological Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Civil Engineering (AREA)
- Combustion & Propulsion (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a cement-based filling material containing various solid wastes and a preparation method and application thereof, and belongs to the technical field of mine goaf filling. The filling material of the invention comprises the following raw materials by mass percent: 5-14% of desulfurized gypsum, 22-35% of fly ash, 24-35% of water-quenched slag, 5-6% of cement and 25-35% of tap water. The filling body is prepared by using three solid wastes of desulfurized gypsum, fly ash and water quenching slag and adding a small amount of cement, so that the problem of environmental pollution caused by the stockpiling of the solid wastes is solved, and meanwhile, the solid wastes, the cement and water in the filling material are subjected to hydration reaction to generate a large amount of hydration products, so that the filling body with high strength is formed, and the strength required by underground mining of the filling body can be met. In addition, the invention has simple process, the prepared filling slurry has good fluidity, and can enter a goaf by filling in a self-flowing or pumping mode. The invention brings new innovation for the traditional mining filling technology.
Description
Technical Field
The invention belongs to the technical field of mine goaf filling, and particularly relates to a cement-based filling material containing various solid wastes, and a preparation method and application thereof.
Background
Solid waste treatment technology is one of the major challenges facing environmental protection and sustainable development. Due to the operations of burning the fossil fuel, processing mineral resources and the like, a large amount of solid waste is generated, wherein the desulfurized gypsum, the fly ash and the water quenching slag are three common urban industrial solid wastes.
Fly ash is the solid residue remaining after coal combustion in coal-fired power plants. The large accumulation of the fly ash not only occupies a large amount of land resources, but also causes serious pollution to air, water and soil. Traditionally, the mode of treating the fly ash is landfill and solid stockpiling, which cannot fundamentally solve the problem of environmental pollution caused by the fly ash and greatly waste the useful secondary resource. The desulfurized gypsum is a byproduct of flue gas desulfurization of a coal-fired power plant by adopting a wet lime/limestone-gypsum method. At present, a part of desulfurized gypsum is mainly stored in a heap and becomes the second most solid waste of a thermal power plant, which not only occupies land resources, but also is unfavorable for the environment. Water quenching slag can be generated after blast furnace slag generated in blast furnace iron making is subjected to water quenching treatment, and the existing water quenching slag also has the problem that a large amount of water quenching slag is stockpiled and is not reasonably utilized all the time.
The presence of these solid wastes not only causes serious pollution to the air and ground water, but also occupies a large amount of land. With the introduction of the concept of "non-waste cities", the effective utilization of solid waste has become a world's hot research spot. Chinese patent application CN102381847A discloses a blast furnace water-quenched slag gel material for mine filling and a preparation method thereof, the invention firstly dries blast furnace water-quenched slag, then respectively crushes ordinary portland cement clinker, anhydrite, calcined lime and the dried water-quenched slag to obtain each component powder, and finally mixes and grinds 35-40% ordinary portland cement clinker powder, 35-40% water-quenched slag powder, 10-15% anhydrite powder and 8-12% calcined lime powder according to weight percentage, and controls the weight of the powder with the granularity larger than 0.08mm in the ground product not to exceed 5% of the total weight of the ground product, namely the inventionObtaining the blast furnace water-quenched slag cementing material for mine filling. The filling material of the invention requires a large amount of cement to be added, which leads to an increase in filling cost. In addition, the two processes of drying and crushing in the manufacturing process of the filling material also greatly increase the filling cost. The solid waste utilized by the invention is single in type, and only one solid waste of water quenching slag is utilized. The invention of China patent application CN102765889A discloses a method for preparing tailing waste stone high-strength concrete containing fly ash, which firstly adopts a step mixed grinding process to grind blast furnace water-quenched slag to a specific surface area of 300m2/kg-400m2Mixing the ground blast furnace water quenched slag with cement clinker and desulfurized gypsum, wherein the mass percentages of the three materials are 35-50% of ground blast furnace water quenched slag powder, 35-45% of cement clinker and 10-20% of desulfurized gypsum, and grinding the three materials to the specific surface of 600m2/k-700m2kg to obtain a cementing material 1, then mixing 55-65% of the cementing material 1 and 35-45% of I-grade fly ash by mass percent to obtain a special cementing material 2 for preparing the tailing waste stone high-strength concrete containing fly ash, finally mixing 25-35% of the cementing material 2 by mass percent with 20-30% of mineral processing tailings as fine aggregate and 35-55% of mining waste stone as concrete coarse aggregate to obtain a tailing waste stone high-strength concrete dry-basis mixture containing fly ash, then adding a high-efficiency water reducing agent accounting for 0.3-1.4% of the dry basis weight of the cementing material 2 and water accounting for 21-35% of the dry basis weight of the cementing material 2, uniformly stirring, pouring into a mould for vibration molding, and obtaining the tailing waste stone high-strength concrete prefabricated member containing the fly ash after normal warm-humid curing or standard curing. The invention mainly utilizes tailings and waste rocks to prepare high-strength concrete, and a small amount of fly ash and desulfurized gypsum are added into the high-strength concrete. The invention has different applications from the product of the invention, the types of treated solid wastes are different, and the proportion of the added fly ash and the desulfurized gypsum is different from the invention. In addition, the manufacturing cost is greatly increased by the middle-grade mixed grinding process.
In order to manage the safety problem caused by the collapse of the underground goaf, the mine usually utilizes tailings to fill the goaf. But the cyanide-containing tailings are strictly forbidden to be used for filling the underground goaf according to the relevant environmental protection requirements. The filling body capable of meeting the strength required by underground mining filling body is prepared by reasonably proportioning various solid wastes and a small amount of cement, so that the safety problem brought by a goaf and the environmental pollution problem brought by the accumulation of a large amount of solid wastes on the earth surface are solved, and meanwhile, an important reference is provided for the resource utilization of the solid wastes.
Disclosure of Invention
The invention provides a cement-based filling material containing various solid wastes and a preparation method and application thereof, aiming at the problem that the conventional municipal industrial solid wastes cannot realize reasonable resource utilization, the three solid wastes of desulfurized gypsum, fly ash and water-quenched slag are used together with a small amount of cement to prepare a filling body, so that the problem of environmental pollution caused by the stockpiling of the solid wastes is solved, and meanwhile, the solid wastes, the cement and water in the filling material are subjected to hydration reaction to generate a large amount of hydration products, so that the filling body with high strength is formed, and the strength required by underground mining filling bodies can be met.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a cement-based filling material containing various solid wastes, which comprises the following raw materials in percentage by mass: 5-14% of desulfurized gypsum, 22-35% of fly ash, 24-35% of water-quenched slag, 5-6% of cement and 25-35% of tap water.
Further, the cement is ordinary portland cement, and the strength grade is 42.5R or 52.5R.
Preferably, the mass ratio of the solid waste to the cement is (11-13): 1, more preferably 12: 1.
preferably, the mass ratio of the desulfurized gypsum to the fly ash to the water quenching slag is (1-2): (3-5): (4-6), more preferably 2:4: 4.
another aspect of the present invention provides a method for preparing the above cement-based filling material containing various solid wastes, comprising the steps of:
(1) respectively weighing fly ash, desulfurized gypsum, water-quenched slag and cement according to the mass ratio, and dry-mixing and mixing the components;
(2) and adding tap water into the mixed material, and stirring and mixing to obtain the cement-based filling material slurry.
Further, the dry mixing time in the step (1) is 3-5 minutes.
Further, the stirring time in the step (2) is 3-5 minutes.
In another aspect, the present invention provides a use of the above cement-based filling material containing various solid wastes: and filling the filling material into the underground goaf through a pipeline by using self weight or pumping, and obtaining the high-strength filling body after hydration reaction.
Compared with the prior art, the invention has the following positive effects:
(1) the invention solves the problem of environmental pollution caused by solid waste stockpiling by preparing a filling body by using three solid wastes of desulfurized gypsum, fly ash and water quenching slag and adding a small amount of cement.
(2) According to the filling material, solid waste, cement and water are subjected to hydration reaction to generate a large amount of hydration products, so that a filling body with high strength is formed, the strength of the filling body can reach 2.11MPa when the curing time is 7 days, and the strength of the filling body can reach 2.60MPa when the curing time is 14 days. Thereby meeting the strength required by underground mining of the filling body.
From the chemical reaction angle, the calcium oxide, the aluminum oxide and the silicon dioxide in the fly ash and the water-quenched slag and the calcium sulfate and the cement in the desulfurized gypsum are synergistic to generate a compact gel structure through hydration reaction, so that the strength of the filling material is greatly improved. Furthermore, from a particle size perspective, the water-quenched slag particles are larger, while the fly ash and desulfurized gypsum particles are smaller. The three components have synergistic effect, and the produced hydrated product can fill the inner pores and cracks to the maximum extent and can also improve the strength of the filling material.
(3) The preparation method of the cement-based filling material containing various solid wastes is simple in process, and the prepared filling slurry is good in fluidity and can enter a goaf through filling in a self-flowing or pumping mode.
Drawings
FIG. 1 shows uniaxial compressive strengths of test pieces prepared by curing the cement-based filling material prepared in example 1 of the present invention for 7 days and 14 days;
FIG. 2 shows the main failure modes of the cement-based pack prepared in example 1 of the present invention during compression (a)1:4: 5; (b)1:5: 6; (c)1.5:5: 4;
FIG. 3 is an internal image of a cement-based pack prepared in example 1 of the present invention after collapse;
FIG. 4A is a graph showing the effect of the ratio of desulfurized gypsum on the strength of the packing in example 1 of the invention;
FIG. 4B is a graph showing the effect of the ratio of fly ash on the strength of the filler in example 1 of the present invention;
FIG. 4C is a graph showing the influence of the ratio of water-quenched slag on the strength of a filler in example 1 of the present invention;
FIG. 5 shows the cement-based filling material prepared in example 1 of the present invention, which was cured for 7 days and 14 days, and desulfurized gypsum: fly ash: the observation result of the scanning electron microscope of the test piece with the water-quenched slag ratio of 2:3:6 and 2:4:4 is as follows: (a) the age is 7 days, and the mixture ratio is as follows: 2:3: 6; (b) the age is 7 days, and the mixture ratio is as follows: 2:4: 4; (c) the age is 14 days, and the mixture ratio is as follows: 2:3: 6; (d) the age is 14 days, and the mixture ratio is as follows: 2:4: 4;
FIG. 6 is an EDS (electron-scanning Spectroscopy) spectrum (2:3:6) of a filling body scanning image of a cement-based filling material prepared in example 1 of the present invention, which is cured for 14 days.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in further detail below.
Example 1: macroscopic and microscopic performance research of the cement-based filling material
In this example, fly ash, desulfurized gypsum, water-quenched slag, ordinary portland cement p.o.42.5r, and tap water were used as materials for preparing the sample, wherein the chemical compositions of cement, fly ash, desulfurized gypsum, and water-quenched slag are shown in table 1. The ratio of the sample cement to the solid waste was 1:12, and the concentration was 70%.
The experimental protocol is shown in table 2. Firstly, the fly ash, the cement, the desulfurized gypsum, the water-quenched slag and the water are weighed by a standard electronic scale, and the precision reaches 0.01 g. The cement, the fly ash, the desulfurized gypsum and the water quenching slag are dry-mixed for 3 minutes, then a proper amount of water is added for stirring for 3 minutes until the slurry is fully dispersed, then the prepared slurry is poured into a prepared mould (50mm multiplied by 100mm), and the mould is beaten by a thin iron stick to be compacted and molded. The mold is placed in a constant temperature (20 +/-1 ℃) and humidity (90 +/-5%) maintenance box of HSBY-40B for maintenance for 7 days and 14 days respectively.
TABLE 1 ratio of chemical components of cement, fly ash, desulfurized gypsum and water-quenched slag
TABLE 2 Experimental protocols
After curing and solidification for 7 days and 14 days, the test piece is subjected to uniaxial compressive strength test to obtain the mechanical strength performance of the test piece. After curing for 7 days and 14 days, desulfurized gypsum: the uniaxial compressive strength of a test piece with the ratio of the fly ash to the water-quenched slag being 2:4:4 is highest, the test piece cured for 7 days reaches 2.11MPa, the test piece cured for 14 days reaches 2.60MPa, and the engineering requirements can be met.
The failure mode of the filling is mainly tensile failure. But the failure modes of the pack are different in different strength ranges. There are three main modes of failure, depending on the instability at the bottom of the pack. When the age is 14 days and the strength of the filling body is between 1.32 and 1.56MPa, the failure mode mainly appears as shown in (a) in figure 2; when the strength of the filling body is 1.89MPa and 1.91MPa, respectively, the failure mode mainly behaves as shown in (b) of FIG. 2; when the strength of the pack is between 2.48 and 2.6MPa, the failure mode is mainly shown in FIG. 2 (c).
As can be seen from fig. 2 and 3, the filling body has a distinct stratification. This is because the water-quenched slag particles having a large diameter are deposited on the lower portion during the solidification of the pack, resulting in poor water retention of the bottom portion, easy loss of water from the bottom portion during the solidification, and macroscopic color difference. This is why the bottom instability of the filling body during the destruction process is different. In addition, the filling begins to fail during the strain softening phase of the stress-strain curve. The macroscopic failure mode is mainly the loose expansion of coarse particles at the bottom of the filling body (a 2, b2, c2 in fig. 2). Tensile cracks (a 3, b3, c3 in fig. 2) parallel to the loading direction appeared on the surface of the filling body near the peak of the curve. As the stress increases, the crack width and length increase (a 5, b5, c5 in fig. 2), eventually throughout the pack. At the same time, the bottom of the filling body gradually expands, and finally the instability is destroyed (a 6, b6, c6 in fig. 2).
L25 (3) in a three-factor three-level configuration3) And (3) an orthogonal experimental table, wherein the influence sensitivity of the desulfurized gypsum, the fly ash and the water-quenched slag on the strength of the filling body is analyzed through range calculation, the calculation result is shown in table 3, and the R value in the table represents the influence sensitivity of the solid waste on the strength of the filling body. The larger the R value of the material, the more sensitive the material is to the effect of the strength of the pack. The change rule of the R value is the same for 7 days and 14 days. According to the calculation results in the table, the sensitivity sequence of the strength influence factors of the desulfurized gypsum, the fly ash and the water quenching slag on the filling body is that the fly ash>Water-quenched slag>And (4) desulfurized gypsum. The observation result shows that the difference of the R values of the water-quenched slag and the fly ash is not more than 0.05, which shows that the content of the water-quenched slag also has important influence on the strength of the filling body. And the R value of the desulfurized gypsum is only 0.37, which shows that the influence of the change of the content of the desulfurized gypsum on the strength of the filling body is relatively weak.
TABLE 3 results of range analysis
As can be seen in fig. 4A-4C, the strength of the pack increases with increasing desulfurized gypsum and fly ash content and decreases with increasing water quenched slag content. Further optimization of the solid waste ratio can be guided by the relationship between solid waste ratio and intensity. For example, the strength of the pack can be increased by increasing the ratio of desulfurized gypsum to fly ash and decreasing the ratio of water-quenched slag. Meanwhile, in the optimized process ratio, the solid waste is increased or decreased according to the sensitivity of the solid waste to the strength.
And then, observing the sample by using a scanning electron microscope, and observing the microstructure of the test piece. Before the experiment, the sample to be observed is dried, and then the sample is subjected to one-time carbon spraying treatment by vacuum coating. The treated sample can be observed by a scanning electron microscope. FIG. 5 is a scanning electron microscope observation result of a test piece which is cured for 7 days and 14 days and has a ratio of 2:3:6 to 2:4:4 (desulfurized gypsum: fly ash: water-quenched slag), as shown in the figure, solid phase particles mainly comprise fly ash and desulfurized gypsum, the two substances have small particle sizes, can be filled between water-quenched slag particles with larger particle sizes, and reduce the internal pores of the filler, so that the filler is more compact. In addition, the fly ash and the desulfurized gypsum have certain cementing property, and can generate a large amount of hydration products, so that the strength of the filling body is increased. A large amount of flocculated material is present on the surface of the solid particles and adheres to the surface of the solid particles. Figure 6 is an EDS energy spectrum of the flocculated material. From FIG. 6, it is presumed that these flocculated substances are calcium silicate hydrates formed by the reaction of calcium oxide, aluminum oxide, silicon dioxide and water, and it is due to the presence of these calcium carbonate hydrates that the uniaxial compressive strength of the test piece is enhanced.
From the chemical reaction angle, the calcium oxide, the aluminum oxide and the silicon dioxide in the fly ash and the water-quenched slag and the calcium sulfate and the cement in the desulfurized gypsum are synergistic to generate a compact gel structure through hydration reaction, so that the strength of the filling material is greatly improved. Furthermore, from a particle size perspective, the water-quenched slag particles are larger, while the fly ash and desulfurized gypsum particles are smaller. The three components have synergistic effect, and the produced hydrated product can fill the inner pores and cracks to the maximum extent and can also improve the strength of the filling material.
Example 2: preparation and application of cement-based filling material
According to the mass ratio of 5: 25: 30: 5 weighing fly ash, desulfurized gypsum, water quenching slag and cement respectively, and dry-mixing the components until the components are completely mixed; adding tap water into the mixed material, stirring, and fully stirring to obtain filling slurry of the underground goaf; and filling the stirred filling slurry into the underground goaf through a pipeline by using self weight or pumping, and obtaining the high-strength filling body after a period of hydration reaction.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. The cement-based filling material containing various solid wastes is characterized by comprising the following raw materials in percentage by mass: 5-14% of desulfurized gypsum, 22-35% of fly ash, 24-35% of water-quenched slag, 5-6% of cement and 25-35% of tap water.
2. The cement-based filling material containing various solid wastes according to claim 1, wherein the cement is ordinary portland cement and has a strength grade of 42.5R or 52.5R.
3. The cement-based filling material containing various solid wastes according to claim 1, wherein the mass ratio of the solid wastes to the cement is (11-13): 1.
4. the cement-based filling material containing a plurality of solid wastes according to claim 3, wherein the mass ratio of the solid wastes to the cement is 12: 1.
5. the cement-based filling material containing various solid wastes according to claim 1, wherein the mass ratio of the desulfurized gypsum to the fly ash to the water-quenched slag is (1-2): (3-5): (4-6).
6. The cement-based filling material containing various solid wastes according to claim 5, wherein the mass ratio of the desulfurized gypsum to the fly ash to the water-quenched slag is 2:4: 4.
7. a method for preparing the cement-based filling material containing a plurality of solid wastes according to any one of claims 1 to 6, comprising the steps of:
(1) respectively weighing fly ash, desulfurized gypsum, water-quenched slag and cement according to the mass ratio, and dry-mixing and mixing the components;
(2) and adding tap water into the mixed material, and stirring and mixing to obtain the cement-based filling material slurry.
8. The method for preparing a cement-based filling material containing various solid wastes according to claim 7, wherein the dry-mixing time in the step (1) is 3 to 5 minutes.
9. The method for preparing a cement-based filling material containing various solid wastes according to claim 7, wherein the stirring time in the step (2) is 3 to 5 minutes.
10. The use of the cement-based filling material containing various solid wastes according to any one of claims 1 to 6, wherein the filling material is filled into an underground goaf through a pipeline by using the self weight or pumping, and a high-strength filling body is obtained after hydration reaction.
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