CN115504691A - Cementing material for coal mine paste filling and preparation method and application thereof - Google Patents
Cementing material for coal mine paste filling and preparation method and application thereof Download PDFInfo
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- CN115504691A CN115504691A CN202211197946.2A CN202211197946A CN115504691A CN 115504691 A CN115504691 A CN 115504691A CN 202211197946 A CN202211197946 A CN 202211197946A CN 115504691 A CN115504691 A CN 115504691A
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- coal mine
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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
-
- 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
- C04B7/14—Cements containing slag
- C04B7/147—Metallurgical slag
- C04B7/153—Mixtures thereof with other inorganic cementitious materials or other activators
- C04B7/1535—Mixtures thereof with other inorganic cementitious materials or other activators with alkali metal containing activators, e.g. sodium hydroxide or waterglass
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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
- C04B7/00—Hydraulic cements
- C04B7/14—Cements containing slag
- C04B7/147—Metallurgical slag
- C04B7/153—Mixtures thereof with other inorganic cementitious materials or other activators
- C04B7/21—Mixtures thereof with other inorganic cementitious materials or other activators with calcium sulfate containing activators
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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
- 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
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses a cementing material for filling paste in coal mines as well as a preparation method and application thereof, wherein the cementing material comprises the following components in percentage by mass: 25-45% of mineral powder, 40-70% of magnesium slag powder, 3-8% of cement and 2-7% of an excitant, wherein the excitant comprises the following components in percentage by mass: (10-15) sodium hydroxide and dihydrate gypsum. The mineral powder, the magnesium slag powder, the cement and the excitant in the cementing material composition for coal mine paste filling can play a role of each material well, the dosage of high-cost cement is reduced, the cementing material plays a role in gelling, and the strength required by process design is met under the condition of small dosage, so that the filling cost is reduced.
Description
Technical Field
The invention relates to the technical field of paste filling, in particular to a cementing material for coal mine paste filling and a preparation method and application thereof.
Background
The paste filling technology is a green mining technology for coal mines and other mines, and is a technology for effectively controlling ground surface subsidence by utilizing coal gangue, slag, fly ash, tailings and the like as filling aggregates, adding a certain amount of cementing materials, adding water, mixing to prepare paste slurry, conveying the paste slurry to a goaf by utilizing the action of pump pressure or gravity, and solidifying and hardening the slurry in the goaf to play a supporting role.
The main filling cost of the paste filling material is the price and the dosage of the cementing material. In recent years, as the production cost of clinker is increased, the price of cement is increased year by year, and the filling cost is higher and higher. Therefore, the coal mine paste filling cost is high, a cementing material with low cost is urgently needed to replace cement, and the effects of low cost and high strength are achieved in coal mine paste filling.
The magnesium slag is waste slag discharged from a magnesium metal plant, and generally, the discharged magnesium slag for producing 1 ton of magnesium varies from 8 tons to 20 tons according to different magnesium ores. According to investigation, the yield of magnesium slag produced by the large-volume industrial solid waste in Yulin city in 2020 is up to 252.1 ten thousand tons. And the emission amount thereof will increase year by year with the development of the magnesium smelting industry. However, the utilization rate of the magnesium slag is very low, and the magnesium slag discharged by a plurality of magnesium plants in China is discarded as waste, so that not only is the resource waste caused, but also a large amount of land resources are occupied, the environment is polluted, and the growth of crops and the health of human beings are seriously threatened. Effectively and reasonably utilizes the magnesium slag, improves the utilization rate of resources and achieves the purpose of using waste to prepare waste.
Disclosure of Invention
Aiming at the problems, the invention provides the cementing material for coal mine paste filling and the preparation method and the application thereof, the cementing material not only reasonably utilizes magnesium slag powder and reduces environmental pollution, but also can reduce the cement consumption and save the cost on the premise that the coal mine paste filling material meets the process requirements.
In order to achieve the purpose, the invention provides a cementing material for filling paste in a coal mine, which comprises the following components in percentage by mass: 25-45% of mineral powder, 40-70% of magnesium slag powder, 3-8% of cement and 2-7% of an excitant, wherein the excitant comprises the following components in percentage by mass: (10-15) sodium hydroxide and dihydrate gypsum.
Of the above components, the cement as a hydraulic material can rapidly dissolve Ca (OH) by reacting with water 2 And continuously dissolving Ca (OH) in the continuous hydration process 2 The process is as follows:
2(3CaO·SiO 2 )+6H 2 O→3CaO·2SiO 2 ·3H 2 O+3Ca(OH) 2
2(2CaO·SiO 2 )+4H 2 O→3CaO·2SiO 2 ·3H 2 O+3Ca(OH) 2
sodium hydroxide can be quickly dissolved in water to obtain Na + 、OH - Ions, which continuously provide a high pH liquid phase environment for slag hydration.
Na(OH) 2 →Na + +2OH -
OH hydrolyzed from cement and sodium hydroxide - Al ions in the slag can be excited. Silicon-oxygen tetrahedra and Al in the structure of slag glass bodies at the site of cleavage of the silicon-oxygen chain 3+ In place of Si 4+ The alundum tetrahedron formed is unstable and reacts with high alkaline medium under the action of OH - In the presence of the active SiO, the slag vitreous body is disintegrated to precipitate the active SiO 2 With Al 2 O 3 The rearrangement and composition of the crystal lattice occur to produce the zeolite substances (sodium zeolite and calcium zeolite) with strength. The main component of the magnesium slag is C 2 S, hydrolysis to produce Ca (OH) 2 Increase OH in the solution - And Ca 2+ Concentration, ca 2+ Reacting with ionized active oxide of slag to generate early hydration products such as nepheline hydrate (cancrinite), calcium mica hydrate, calcium aluminate hydrate, calcium silicate hydrate, etc. The reaction process is as follows:
active Al 2 O 3 +m 1 Ca(OH) 2 +n 1 H 2 O→m 1 CaO·Al 2 O 3 ·n 1 H 2 O
Active SiO 2 +m 2 Ca(OH) 2 +n 2 H 2 O→m 2 CaO·SiO 2 ·n 2 H 2 O
According to the theory of alkali slag cement: all soluble alkali metal compounds and calcium-containing and calcium-free aluminosilicate systems can form cement-like gelled systems which can be set and hardened in water, in nature and under steam-curing conditions. The magnesium slag has good volcanic ash activity, and the mineral composition mainly comprises C 2 And S. The invention relates to a composite cementing material alkali-activated cement, which is a modification of the traditional alkali-activated slag cement and an attempt to better utilize various industrial waste residues.
Meanwhile, the solution contains dihydrate gypsum, and the SO provided by the dihydrate gypsum in the liquid phase 4 2- Supplying Ca to the magnesium slag 2+ With active Al 2 O 3 And hydrated calcium aluminate (m) 1 CaO·Al 2 O 3 ·n 1 H 2 O) to generate hydrated calcium sulphoaluminate (ettringite), and the hydrated calcium sulphoaluminate continuously grows and is mutually overlapped with each other along with the progress of hydration (as shown in figure 1, the needle rod-shaped structure is the hydrated calcium sulphoaluminate). As the hydration reaction continues, the hydration product ettringite is connected with each other to form a net-shaped supporting structure (as shown in figure 2, ettringite grows in a cross way, a large amount of needle-shaped and rod-shaped crystals grow into cluster-shaped ettringite in gaps, the size is larger, about 5 mu m, although cracks exist on the surface, a large amount of hydration products exist at the cracks, the needle-shaped and rod-shaped crystals are mutually overlapped to form a bridge to well connect the original cracks), the zeolite product and a small amount of calcium silicate hydrate and calcium aluminate hydrate are filled into the net-shaped ettringite to form a firm and compact whole (as shown in figure 3, the needle-shaped ettringite is mutually interwoven and overlapped to form a firm and compact structureSpace, which has a positive effect on the strength of the paste test piece) so that it has sufficient strength. The reaction process is as follows:
3CaO·Al 2 O 3 +3CaSO 4 +32H 2 O→3CaO·Al 2 O 3 ·3CaSO 4 ·32H 2 O
the 28-day cement hydration products are shown in figure 4, where it can be seen that the products are primarily hydrated calcium aluminate, natrolite, scolecite, cancrinite, palygorskite, gypsum, calcium silicate hydrate, ettringite, and the like.
Preferably, the cementing agent comprises the following components in percentage by mass: 30-40% of mineral powder, 45-60% of magnesium slag powder, 5-8% of cement and 3-7% of an excitant.
Still more preferably, the cementing agent comprises the following components in percentage by mass: 30% of mineral powder, 58% of magnesium slag powder, 7% of cement and 5% of an excitant.
Preferably, the mass coefficient of the ore powder is not less than 1.8.
Preferably, the specific surface area of the ore powder is not less than 400m 2 /kg。
Preferably, the mass coefficient of the magnesium slag powder is not less than 1.6.
Preferably, the passing rate of the square-hole sieve with the fineness of 0.080mm of the magnesium slag powder is not lower than 90%.
Preferably, the pass rate of the square-hole sieve with the cement fineness of 0.080mm is not lower than 90%.
The second aspect of the invention provides a preparation method of the cementing material for coal mine paste filling, which comprises the following steps:
s1, premixing components of an excitant;
s2, uniformly mixing the mineral powder, the magnesium slag powder, the cement and the excitant according to a ratio to obtain the cementing material.
The coal mine paste filling material comprises coal gangue, water and a coal mine paste filling cementing material, wherein the coal mine paste filling cementing material is the coal mine paste filling cementing material or the coal mine paste filling cementing material prepared by the preparation method.
Through the technical scheme, the invention has the following beneficial effects:
1. the mineral powder, the magnesium slag powder, the cement and the excitant in the cementing material composition for coal mine paste filling can play a role of each material well, reduce the consumption of high-cost cement, play a role in gelling in a coal mine paste filling material, and meet the strength required by process design under the condition of small consumption of the cementing material, thereby reducing the filling cost.
2. The magnesium slag used in the cementing material is derived from waste materials generated by smelting magnesium by a Pidgeon process, and the magnesium slag as industrial waste slag discharged in the magnesium smelting industry can be completely applied to cementing materials, so that the cementing material has great significance to magnesium plants, and provides a new material for the cement industry.
Drawings
FIG. 1 is a schematic view of the continuous growth and mutual overlapping of calcium sulfoaluminate hydrate during hydration of a cementitious material according to the present invention;
FIG. 2 is a schematic view of the reticulated support structure formed by ettringite during hydration of the cement of the present invention;
FIG. 3 is a schematic illustration of zeolite products, calcium silicate hydrate and calcium aluminate hydrate filled into reticulated ettringite during hydration of the cement of the present invention;
figure 4 is an XRD pattern of the cement of the present invention after 28 days hydration.
Detailed Description
The following examples are provided to illustrate specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the preferred embodiment of the invention, are given by way of illustration and explanation only, not limitation.
In the following examples, the fine ore is creep steel slag, and the average chemical composition is shown in table 1; the magnesium slag powder is grinded Tianyu magnesium slag, and the average chemical composition of the grinded magnesium slag is shown in Table 2; the cement is chamotte cement of an honest cement plant, and the average chemical components are shown in table 3; the purity of sodium hydroxide is 99%, and the dihydrate Gypsum is two-stage natural dihydrate Gypsum, caSO 4 ·H 2 The O content was 92.5wt%. All essencesThe components and contents of the binders in the examples and comparative examples are shown in table 4.
TABLE 1 average chemical composition table/wt% of fused slag used in examples of the present invention
| Composition (I) | SiO 2 | Al 2 O 3 | Fe 2 O 3 | CaO | MgO |
| Content (wt.) | 24.96 | 9.51 | 3.34 | 47.75 | 3.46 |
TABLE 2 average chemical composition table/wt% of the milled magnesium slag used in the examples of the present invention
| Composition (I) | SiO 2 | Al 2 O 3 | Fe 2 O 3 | CaO | MgO |
| Content (wt.) | 29.20 | 4.40 | 3.05 | 38.15 | 6.99 |
Most of free calcium oxide and magnesium oxide are consumed in the grinding process of the magnesium slag, and the free calcium oxide and the magnesium oxide in the magnesium slag can be quickly converted into active Ca (OH) 2 Active Mg (OH) 2 The water can be consumed rapidly in the hydration process, and the volume expansion phenomenon can not occur.
TABLE 3 average chemical composition table/wt% of cement clinker used in the examples of the present invention
| Composition (I) | SiO 2 | Al 2 O 3 | Fe 2 O 3 | CaO | MgO |
| Content (wt.) | 30.20 | 8.13 | 4.09 | 52.35 | 2.27 |
TABLE 4 Components and content/wt% of Binder in examples and comparative examples
| Mineral powder | Magnesium slag powder | Cement | Sodium hydroxide | Dihydrate gypsum | |
| Example 1 | 30 | 58 | 7 | 0.45 | 4.55 |
| Example 2 | 25 | 70 | 3 | 0.125 | 1.875 |
| Example 3 | 45 | 40 | 8 | 0.5 | 6.5 |
| Example 4 | 30 | 60 | 7 | 0.2 | 2.8 |
| Example 5 | 40 | 45 | 8 | 0.5 | 6.5 |
| Example 6 | 30 | 60 | 5 | 0.45 | 4.55 |
| Comparative example 1 | 30 | 63 | 7 | - | - |
| Comparative example 2 | 30 | 65 | - | 0.45 | 4.55 |
| Comparative example 3 | 25 | 45 | 25 | 0.45 | 4.55 |
| Comparative example 4 | - | 95 | 3 | 0.18 | 1.82 |
| Comparative example 5 | 30 | 58 | 7 | - | 5 |
| Comparative example 6 | 30 | 58 | 7 | 5 | - |
The preparation method of the cementing material in the above examples and comparative examples is as follows:
premixing sodium hydroxide and dihydrate gypsum (if there is one or none, the step is omitted) to obtain exciting agent;
and (3) uniformly mixing the mineral powder, the magnesium slag powder, the cement (if not, omitted) and the exciting agent to obtain the cementing material.
Examples of the experiments
The cementing materials of the examples 1 to 6 and the comparative examples 1 to 6 of the invention are used for preparing the coal mine paste filling material. The coal mine paste filling material is prepared from the following raw materials of coal gangue, water and the coal mine paste filling cementing material, wherein the raw materials comprise the following components in parts by weight: the usage amount of the coal gangue is 1202kg/m 3 The amount of water used is 397kg/m 3 The dosage of the cementing material is 190kg/m 3 。
And another group of control groups is arranged, and P.O 42.5 cement is used as a cementing material.
Uniaxial compressive strength tests were carried out according to the following standard GB/T50081-2002-common concrete mechanical property test method standards, and the obtained results are shown in Table 5.
TABLE 5 coal mine paste filling material Performance test results
It can be seen from examples 1 and 4 that the strength of the coal mine paste filling material is increased along with the increase of the content of the excitant. By comparing example 1 with example 6, it can be seen that the increase of the clinker ratio can improve the uniaxial compressive strength of the paste filling material for coal mines.
The strength of the example 1 is 8.69MPa, the strength of the comparative example 1 is 2.06MPa, and the comparative data show that the excitant can effectively excite the activity of each component in the cementing material and improve the strength. As can be seen by combining comparative example 5 with comparative example 6, the improvement in strength is quite limited by the use of sodium hydroxide alone or dihydrate gypsum, much less than when sodium hydroxide and dihydrate gypsum are used together. According to the observation of the strength data of the example 1 and the comparative example 2, the strength of the comparative example 2 is only 2.07MPa, and the comparative data shows that the clinker plays a positive role in improving the strength in the cementing material of the invention. Comparing example 2 with comparative example 3, it can be seen that the clinker amount exceeds a certain proportion, and the strength of the paste material of the coal mine is reduced.
In conclusion, the cementing material composition can effectively reduce the using amount of cement and the using cost of materials.
The preferred embodiments of the present invention have been described in detail with reference to the examples, but the present invention is not limited to the details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (10)
1. The cementing material for filling the paste in the coal mine is characterized by comprising the following components in percentage by mass: 25-45% of mineral powder, 40-70% of magnesium slag powder, 3-8% of cement and 2-7% of an excitant, wherein the excitant comprises the following components in percentage by mass: (10-15) sodium hydroxide and dihydrate gypsum.
2. The coal mine cementing material for filling paste, which is described in claim 1, is characterized by comprising the following components in percentage by mass: 30-40% of mineral powder, 45-60% of magnesium slag powder, 5-8% of cement and 3-7% of excitant.
3. The coal mine cementing material for filling paste, which is described in claim 2, is characterized by comprising the following components in percentage by mass: 30% of mineral powder, 58% of magnesium slag powder, 7% of cement and 5% of an excitant.
4. The coal mine paste filling cement according to any one of claims 1 to 3, wherein the mass coefficient of the ore powder is not less than 1.8.
5. The coal mine paste filling cement according to any one of claims 1 to 3, wherein the specific surface area of the ore powder is not less than 400m 2 /kg。
6. The coal mine paste filling cement according to any one of claims 1 to 3, wherein the magnesium slag powder mass coefficient is not less than 1.6.
7. The coal mine paste filling cementing material according to any one of the claims 1 to 3, wherein the magnesium slag powder has a fineness of 0.080mm and a square-hole sieve passing rate of not less than 90%.
8. The coal mine paste filling cementing material according to any one of claims 1 to 3, wherein the cement fineness is 0.080mm and the square mesh sieve passing rate is not lower than 90%.
9. A method of preparing a coal mine paste filling cement as claimed in any one of claims 1 to 8, comprising the steps of:
s1, premixing components of an excitant;
s2, uniformly mixing the mineral powder, the magnesium slag powder, the cement and the excitant according to a ratio to obtain the cementing material.
10. A coal mine paste filling material, characterized by comprising coal gangue, water and a coal mine paste filling cementing material, wherein the coal mine paste filling cementing material is the coal mine paste filling cementing material according to any one of claims 1 to 8 or the coal mine paste filling cementing material prepared by the preparation method according to claim 9.
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| CN117510164A (en) * | 2023-11-08 | 2024-02-06 | 陕西省建筑科学研究院有限公司 | Preparation method of magnesium slag-based ultrahigh water filling material |
| CN117510163A (en) * | 2023-11-08 | 2024-02-06 | 陕西省建筑科学研究院有限公司 | Preparation method of quick-hardening magnesium slag-based repair mortar |
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| CN117510164A (en) * | 2023-11-08 | 2024-02-06 | 陕西省建筑科学研究院有限公司 | Preparation method of magnesium slag-based ultrahigh water filling material |
| CN117510163A (en) * | 2023-11-08 | 2024-02-06 | 陕西省建筑科学研究院有限公司 | Preparation method of quick-hardening magnesium slag-based repair mortar |
| CN117510163B (en) * | 2023-11-08 | 2024-05-28 | 陕西省建筑科学研究院有限公司 | Preparation method of quick-hardening magnesium slag-based repair mortar |
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