CN113548865B - Fractal gangue cemented filling material and preparation method thereof - Google Patents

Fractal gangue cemented filling material and preparation method thereof Download PDF

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CN113548865B
CN113548865B CN202110985727.XA CN202110985727A CN113548865B CN 113548865 B CN113548865 B CN 113548865B CN 202110985727 A CN202110985727 A CN 202110985727A CN 113548865 B CN113548865 B CN 113548865B
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gangue
fractal
filling material
reducing agent
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CN113548865A (en
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吴疆宇
马丹
浦海
尹乾
孟庆彬
王逸鸣
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China University of Mining and Technology CUMT
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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
    • 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
    • C04B12/00—Cements not provided for in groups C04B7/00 - C04B11/00
    • C04B12/005—Geopolymer cements, e.g. reaction products of aluminosilicates with alkali metal hydroxides or silicates
    • 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
    • C04B28/143—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
    • 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
    • C04B7/00—Hydraulic cements
    • C04B7/24—Cements from oil shales, residues or waste other than slag
    • 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
    • C04B2111/00017—Aspects relating to the protection of the environment
    • 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
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00—Technologies relating to the processing of minerals
    • Y02P40/10—Production of cement, e.g. improving or optimising the production methods; Cement grinding

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)

Abstract

The invention discloses a fractal gangue cemented filling material and a preparation method thereof, and belongs to the technical field of coal mine filling materials. The feed comprises the following raw materials in parts by weight: 25-35 parts of fractal gangue, 5-12 parts of slag powder, 3-5 parts of gypsum powder, 22-32 parts of fly ash, 2-8 parts of plant fiber, 14-18 parts of cement, 2-5 parts of bentonite, 6-14 parts of a water reducing agent, 0.5-3 parts of an additive and 30-62 parts of water. The fractal gangue cemented filling material has good mechanical property and fluidity and good stability, and effectively solves the technical problems of poor mechanical property and poor stability of gangue cemented filling bodies in the prior art.

Description

Fractal gangue cemented filling material and preparation method thereof
Technical Field
The invention relates to the technical field of coal mine filling materials, in particular to a fractal gangue cemented filling material and a preparation method thereof.
Background
Although China has abundant coal resources and has important significance on the development of national economy, the coal is affected by 'under three' coal pressing in the process of coal industrial development, and the development of coal resources is severely restricted. Meanwhile, a large amount of gangue produced in the coal mining process is accumulated on the ground surface in a large amount, and great threat is generated to the natural environment. Therefore, the effective treatment of the problem of 'three lower' coal pressing and gangue accumulation is an important problem in the development of the coal industry in China, and the gangue cemented filling technology becomes the first choice for solving the two problems, so the research on gangue cemented filling bodies becomes the focus.
However, in the prior art, when gangue is used for preparing a gangue cementing filling body, the problems of limited mechanical strength and poor stability exist, the optimal mechanical strength can be achieved after cementing is completed, and once a cementing structure is damaged by external force, the cementing structure cannot be recovered, so that the overall mechanical strength is not continued.
Disclosure of Invention
In view of the above, the invention provides a fractal gangue cemented filling material and a preparation method thereof, and the fractal gangue cemented filling material has good mechanical properties and good stability, and effectively solves the technical problems of poor mechanical properties and poor stability of gangue cemented filling bodies in the prior art.
In order to achieve the technical purpose, the invention provides the following technical scheme:
the fractal gangue cemented filling material comprises the following raw materials in parts by weight:
25-35 parts of gangue, 5-12 parts of slag powder, 3-5 parts of gypsum powder, 22-32 parts of fly ash, 2-8 parts of plant fiber, 14-18 parts of cement, 2-5 parts of bentonite, 6-14 parts of a water reducing agent, 0.5-3 parts of an additive and 30-62 parts of water.
Further, the particle size of the gangue is 0.5-10 mm. The fractal gangue material is divided into the intervals of 0.5-1.0mm, 1.0-2.0mm, 2.0-4.0mm, 4.0-6.0mm, 6.0-8.0mm and 8.0-10.0mm, and the fractal gangue has different particle size distribution fractal characteristics, namely different fractal dimensions of gangue particle size distribution, fractal gangue with different particle size grades and the like, and is uniformly mixed. The gangue with the grain diameter of 0.5-10mm is beneficial to forming a skeleton structure by the cemented filling body and can ensure the pumping and transporting performance.
The gangue is screened, and the particle size distribution of the gangue obeys the following fractal equation (1):
Figure BDA0003230633270000021
d is the fractal dimension of the particle size distribution of the gangue; diThe aperture of the current grading screen; dminThe minimum particle size of the gangue; dmaxThe maximum particle size of the gangue; miHas a particle diameter between di-dminThe mass of gangue between the two; mtThe total mass of the gangue; piIs of a particle diameter smaller than diThe mass fraction of the gangue.
And screening to obtain the gangue with different particle size distribution fractal characteristics.
The value range of the fractal dimension D of the particle size distribution of the fractal gangue is 2.0-3.0.
The higher the fractal dimension, the higher the fine aggregate content, so the slump of the cementitious filling material will be smaller. Given a fractal dimension in the range of 2.1-2.9, it can be concluded that the cemented filling material with an intermediate fractal dimension, e.g. around 2.5, is the highest in strength, while both 2.1 and 2.9 are lower. The influence rule of the fractal dimension on the strength and the flowability of the material is inconsistent. Table 1 shows the mass distribution (%) of the gangue in the particle size range and table 2 shows the cumulative particle size mass distribution (%) of the gangue.
TABLE 1 particle size distribution (%)
Figure BDA0003230633270000031
TABLE 2 cumulative particle size mass distribution (%)
Figure BDA0003230633270000032
Further, the slag powder reaches above S95 grade.
Further, the gypsum comprises one or more of phosphogypsum, fluorgypsum, lemon gypsum and waste ceramic mould gypsum.
Further, the content of CaO in the fly ash is more than or equal to 7 wt%, and SiO is2The content is more than or equal to 45wt percent.
Further, the plant fiber is one or more of straw fiber, straw fiber and wood fiber.
The plant fiber is cheap, reproducible and environment-friendly, plays a role in water retention and anti-cracking in a cemented porous medium system, and can improve the toughness and the deformation performance of the cemented filling material in the contribution of mechanical strength. The cemented filling body is compressed and deformed under the action of the overlying rock layer, the overlying rock layer sinks and deforms to release energy, and the cemented filling body inhibits the overlying rock layer from sinking and absorbs the energy at the same time, so that the regulation of the deformation performance of the cemented filling material is the key for accurately controlling the movement of the rock layer.
Further, the water reducing agent is one or more of a naphthalene-based high-efficiency water reducing agent, a melamine-based high-efficiency water reducing agent, a fatty acid-based high-efficiency water reducing agent and a polycarboxylate-based high-efficiency water reducing agent.
Further, the admixture is a retarder, a water-retaining agent and an alkali activator.
The invention also provides a preparation method of the fractal gangue cemented filling material, which comprises the following steps:
after all the raw materials are pretreated, adding water into a mixture obtained by mixing and grinding slag powder, gypsum powder, cement, fly ash, bentonite and an alkali activator, and stirring for 10min at the rotating speed of 150 rpm; then adding a water reducing agent, a retarder, a water-retaining agent and plant fibers, and stirring for 5min at the rotating speed of 150 rpm; and finally adding the gangue and the balance of water, and stirring at the rotating speed of 50rpm for 10min to obtain the fractal gangue cemented filling material.
The invention adds water, the former water is used to improve the alkalinity of the gel slurry as much as possible to excite the active substance as much as possible, and the latter water is used to regulate the workability and fluidity of the whole cement filling material.
Further, the pretreatment comprises the steps of screening the raw materials, removing impurities, grinding and drying.
The fly ash is activated for 4-8h at 20 ℃ after being pretreated and then is reused.
Further, the grinding is carried out until the particle size of the active excitation mixture (slag powder, gypsum powder, cement, fly ash, bentonite and alkali activator) is less than 50 μm. Compared with the prior art, the invention has the beneficial effects that:
the invention utilizes the waste rocks with different grain diameters to be mixed and then is evenly mixed with other raw materials, the fly ash is activated to prevent the slurry from being hydrated continuously after being conveyed to a filling place, so that the phenomenon of low strength is caused, and then the mixture is evenly stirred at a proper rotating speed to obtain the filling material with good mechanical property. The fractal gangue cementing filling material with good mechanical property and high stability is prepared by organically combining all raw materials through reasonable matching and a set preparation method and exerting the synergistic effect.
The gangue with fractal characteristics is screened out through the gangue, so that the gangue with the optimal particle size distribution can be obtained, and the mechanical characteristics of the gangue are facilitated. Meanwhile, the invention activates the activity of various materials through grinding and alkali excitation, improves the gelling property and saves cement.
The fractal gangue cemented filling material can greatly treat waste gangue accumulated in coal mines, improve the gangue paste filling and mining efficiency, reduce the paste filling and mining cost and keep the sustainable development of coal mine paste filling and mining; the plant fiber reinforced cemented filling material further improves the resource utilization rate of solid waste, can serve for structural filling mining and deep filling mining, and continues to liberate more 'three lower' coal pressing resources in China.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description 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. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, 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. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The specification and examples are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
The particle size of the fractal gangue used in the invention is 0.5-10 mm. The specific range is 0.5-1.0mm, 1.0-2.0mm, 2.0-4.0mm, 4.0-6.0mm, 6.0-8.0mm and 8.0-10.0mm, and they have different particle size distribution fractal characteristics, i.e. different particle size distribution fractal dimensions of the waste rock, fractal waste rock with different particle size grades and the like, and the quality is uniformly mixed.
Example 1
The feed comprises the following raw materials in parts by weight:
30 parts of fractal gangue, 8 parts of slag powder, 4 parts of fluorgypsum powder, 28 parts of fly ash, 5 parts of plant fiber, 16 parts of cement, 3 parts of bentonite, 10 parts of naphthalene-based superplasticizer, 2 parts of additive (0.8 part of retarder, 0.4 part of water-retaining agent and 0.8 part of alkali activator) and 45 parts of water.
The preparation method comprises the following steps:
screening all the raw materials, removing impurities, grinding until the particle size of an active excitation mixture (slag powder, gypsum powder, cement, fly ash, bentonite and an alkali activator) is less than 50 mu m, drying, and activating the fly ash at 20 ℃ for 4-8h for later use;
adding water into the mixture of the treated slag powder, gypsum powder, cement, fly ash, bentonite and alkali activator which are mixed and ground, and stirring for 10min at the rotating speed of 150 rpm; then adding a water reducing agent, a retarder, a water-retaining agent and plant fibers, and stirring for 5min at the rotating speed of 150 rpm; and finally adding the gangue and the balance of water, and stirring at the rotating speed of 50rpm for 10min to obtain the fractal gangue cemented filling material.
Example 2
The feed comprises the following raw materials in parts by weight:
25 parts of fractal gangue, 12 parts of slag powder, 3 parts of phosphogypsum powder, 22 parts of fly ash, 8 parts of plant fiber, 14 parts of cement, 5 parts of bentonite, 6 parts of a fatty acid-based high-efficiency water reducing agent, 0.5 part of an additive (0.1 part of a retarder, 0.2 part of a water-retaining agent, 0.3 part of an alkali activator) and 62 parts of water.
The preparation method is the same as example 1.
Example 3
The feed comprises the following raw materials in parts by weight:
35 parts of fractal gangue, 5 parts of slag powder, 5 parts of waste ceramic mold gypsum powder, 32 parts of fly ash, 2 parts of plant fiber, 18 parts of cement, 2 parts of bentonite, 14 parts of polycarboxylate superplasticizer, 3 parts of additive (1.5 parts of retarder, 0.5 part of water-retaining agent, 1 part of alkali activator) and 30 parts of water.
The preparation method is the same as example 1.
Example 4
The feed comprises the following raw materials in parts by weight:
28 parts of fractal gangue, 11 parts of slag powder, 3.5 parts of lemon gypsum powder, 30 parts of fly ash, 6 parts of plant fiber, 15 parts of cement, 5 parts of bentonite, 11 parts of melamine high-efficiency water reducing agent, 1.5 parts of additive (0.5 part of retarder, 0.4 part of water-retaining agent, 0.6 part of alkali activator) and 50 parts of water.
The preparation method is the same as example 1.
Comparative example 1
The difference from example 1 is that no gangue was added.
Comparative example 2
The difference from the example 1 is that fractal gangue with the same particle size is selected.
Comparative example 3
The difference from example 1 is that the fly ash is not subjected to an activation treatment.
Comparative example 4
The difference from example 1 is that the rotation speed during stirring was 100 rpm.
Test example 1
The fractal gangue cemented filling material prepared in the examples 1-4, the comparative examples 1-4 and the comparison group (the cemented filling material in the prior art comprises 79 parts of slag powder, 5 parts of fly ash, 6 parts of cement clinker, 5 parts of gypsum, 3.3 parts of lime and 1.7 parts of composite modifier) is maintained in an environment with the temperature of 19-21 ℃ and the relative humidity of more than 95%, the maintenance time is 3d, 7d and 28d respectively, and then the test block is subjected to a compression test, and the results are shown in table 3.
TABLE 3
Figure BDA0003230633270000091
As can be seen from table 3, the fractal gangue cemented filling material prepared by the method has high compressive strength, small slump, large expansion degree and low bleeding rate, and the performances of the fractal gangue cemented filling material which is not prepared according to the requirements of the invention obviously have a downward trend, which indicates that the performances of the fractal gangue cemented filling material prepared by the raw material proportion and the preparation method of the invention can be obviously improved.
Test example 2
The fractal gangue cemented filling material prepared in examples 1-4, comparative examples 1-4 and a control group (the cemented filling material in the prior art comprises 79 parts of slag powder, 5 parts of fly ash, 6 parts of cement clinker, 5 parts of gypsum, 3.3 parts of lime and 1.7 parts of composite modifier) was reused for 6 times, and the results are shown in table 4.
TABLE 4
Figure BDA0003230633270000101
It can be seen from table 4 that after 6 times of recycling, the fractal gangue cemented filling material prepared in the embodiment of the present invention has very little change in each property and basically no influence on the property, while the filling materials prepared in the comparative example and the control group have obvious damage phenomenon in each property after 6 times of recycling, which indicates that the fractal gangue cemented filling material prepared in the embodiment of the present invention has better stability.
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 and improvements made within the spirit and principle of the present invention are intended to be included therein.

Claims (8)

1. The fractal gangue cemented filling material is characterized by comprising the following raw materials in parts by weight:
25-35 parts of gangue, 5-12 parts of slag powder, 3-5 parts of gypsum powder, 22-32 parts of fly ash, 2-8 parts of plant fiber, 14-18 parts of cement, 2-5 parts of bentonite, 6-14 parts of a water reducing agent, 0.5-3 parts of an additive and 30-62 parts of water;
the particle size of the waste rock is 0.5-10mm, and the waste rock is specifically divided into intervals of 0.5-1.0mm, 1.0-2.0mm, 2.0-4.0mm, 4.0-6.0mm, 6.0-8.0mm and 8.0-10.0 mm;
the fly ash is activated for 4-8h at 20 ℃ after being pretreated and then is reused.
2. The fractal gangue cementitious filling material according to claim 1, wherein the slag powder reaches above S95 level.
3. The fractal gangue cementitious filling material according to claim 1, wherein the gypsum comprises one or more of phosphogypsum, fluorgypsum, lemon gypsum and waste ceramic mould gypsum.
4. The fractal gangue cementitious filling material according to claim 1, wherein the water reducing agent is one or more of a naphthalene-based high-efficiency water reducing agent, a melamine-based high-efficiency water reducing agent, a fatty acid-based high-efficiency water reducing agent and a polycarboxylate-based high-efficiency water reducing agent.
5. The fractal gangue cementitious filling material according to claim 1, wherein the additive is a retarder, a water-retaining agent and an alkali activator.
6. The preparation method of the fractal gangue cemented filling material as defined in any one of claims 1 to 5, which is characterized by comprising the following steps:
after all the raw materials are pretreated, adding water into a mixture obtained by mixing and grinding slag powder, gypsum powder, cement, fly ash, bentonite and an alkali activator, and stirring for 10min at the rotating speed of 150 rpm; then adding a water reducing agent, a retarder, a water-retaining agent and plant fibers, and stirring for 5min at the rotating speed of 150 rpm; and finally adding the gangue and the balance of water, and stirring at the rotating speed of 50rpm for 10min to obtain the fractal gangue cemented filling material.
7. The preparation method according to claim 6, wherein the pretreatment comprises screening, impurity removal, grinding and drying of the raw materials.
8. The method of claim 7, wherein the milling is to a particle size of the reactive challenge mixture of less than 50 μm.
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