CN114133178A - Multi-element coal-based solid waste composite acid-activated underground filling material and preparation method thereof - Google Patents
Multi-element coal-based solid waste composite acid-activated underground filling material and preparation method thereof Download PDFInfo
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- CN114133178A CN114133178A CN202111265642.0A CN202111265642A CN114133178A CN 114133178 A CN114133178 A CN 114133178A CN 202111265642 A CN202111265642 A CN 202111265642A CN 114133178 A CN114133178 A CN 114133178A
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- 239000003245 coal Substances 0.000 title claims abstract description 70
- 239000000463 material Substances 0.000 title claims abstract description 48
- 238000011049 filling Methods 0.000 title claims abstract description 42
- 239000002910 solid waste Substances 0.000 title claims abstract description 32
- 239000002131 composite material Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000002253 acid Substances 0.000 title claims abstract description 15
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 63
- 239000011398 Portland cement Substances 0.000 claims abstract description 13
- 239000002893 slag Substances 0.000 claims description 56
- 239000004568 cement Substances 0.000 claims description 36
- 239000002245 particle Substances 0.000 claims description 31
- 239000010881 fly ash Substances 0.000 claims description 29
- 239000010440 gypsum Substances 0.000 claims description 22
- 229910052602 gypsum Inorganic materials 0.000 claims description 22
- 238000002156 mixing Methods 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 238000000498 ball milling Methods 0.000 claims description 7
- 230000000694 effects Effects 0.000 claims description 6
- 238000006703 hydration reaction Methods 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 3
- 239000003546 flue gas Substances 0.000 claims description 3
- 239000006227 byproduct Substances 0.000 claims description 2
- 238000006477 desulfuration reaction Methods 0.000 claims 1
- 230000023556 desulfurization Effects 0.000 claims 1
- 239000012190 activator Substances 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 238000005303 weighing Methods 0.000 description 15
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 12
- 238000005065 mining Methods 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 229910052593 corundum Inorganic materials 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 4
- 235000006408 oxalic acid Nutrition 0.000 description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 230000001965 increasing effect Effects 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000011435 rock Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 241001465754 Metazoa Species 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- YBCVMFKXIKNREZ-UHFFFAOYSA-N acoh acetic acid Chemical compound CC(O)=O.CC(O)=O YBCVMFKXIKNREZ-UHFFFAOYSA-N 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 239000002956 ash Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000404 calcium aluminium silicate Substances 0.000 description 1
- 235000012215 calcium aluminium silicate Nutrition 0.000 description 1
- WNCYAPRTYDMSFP-UHFFFAOYSA-N calcium aluminosilicate Chemical compound [Al+3].[Al+3].[Ca+2].[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O WNCYAPRTYDMSFP-UHFFFAOYSA-N 0.000 description 1
- 229940078583 calcium aluminosilicate Drugs 0.000 description 1
- 239000000378 calcium silicate Substances 0.000 description 1
- 229910052918 calcium silicate Inorganic materials 0.000 description 1
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 125000001967 indiganyl group Chemical group [H][In]([H])[*] 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 235000019614 sour taste Nutrition 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000052 vinegar Substances 0.000 description 1
- 235000021419 vinegar Nutrition 0.000 description 1
- 238000005406 washing Methods 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
- 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
- C04B28/02—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 hydraulic cements other than calcium sulfates
- C04B28/04—Portland 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
- 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
- C04B18/065—Residues from coal gasification
-
- 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
- C04B18/06—Combustion residues, e.g. purification products of smoke, fumes or exhaust gases
- C04B18/10—Burned or pyrolised refuse
-
- 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
- C04B18/12—Waste materials; Refuse from quarries, mining 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
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/04—Carboxylic acids; Salts, anhydrides or esters thereof
-
- 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
-
- 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)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Civil Engineering (AREA)
- Combustion & Propulsion (AREA)
- Mining & Mineral Resources (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention relates to the field of mine filling materials, and discloses a multi-element coal-based solid waste composite acid-activated underground filling material and a preparation method thereof. The invention takes the composite multi-element coal-based solid waste as a main raw material, the auxiliary doped superfine portland cement as a backfill material and the acetic acid as an activator to prepare the environment-friendly multi-element coal-based solid waste composite acid-activated underground filling material.
Description
Technical Field
The invention relates to the field of mine filling materials, in particular to a multi-element coal-based solid waste composite acid-excited underground filling material and a preparation method thereof.
Background
In recent years, with the rapid development of coal mining, coal-fired power generation and coal chemical industry, the rapid development of the eastern and national economy is supported and promoted, and simultaneously, a great amount of coal-based solid waste is left for each large mining area, wherein the coal-based solid waste mainly comprises gasified slag, coal gangue, fly ash, desulfurized gypsum, furnace bottom slag and the like. The two-Huai mining area is one of the national major coal production bases, the rapid development of the coal electric chemical industry generates a large amount of solid waste, the comprehensive utilization rate of the solid waste is low, a large amount of land is occupied, the environment is seriously polluted, and the rapid development of the regional ecological economy society is restricted.
Meanwhile, if underground coal mining is not properly filled, a goaf is formed underground, deformation and damage of an upper covering rock stratum are caused, and the phenomena of subsidence, water accumulation depression, subsidence lake and the like are formed on the surface in the area. The change of the geological structure in the subsidence area induces the collapse of houses, the crack of roads, the damage of farmlands and the like in the area, thereby seriously affecting the industrial and agricultural production and the life of residents, destroying the soil environment on the surface of the area, changing the local hydrogeological conditions on a large scale, aggravating the water and soil loss and changing the growth and inhabitation environment of animals and plants, and reducing the biological population year by year.
Disclosure of Invention
In order to solve the defects mentioned in the background art, the invention aims to provide a multielement coal-based solid waste composite acid-activated underground filling material and a preparation method thereof.
The purpose of the invention can be realized by the following technical scheme:
the multi-element coal-based solid waste composite acid-activated underground filling material comprises 5-40 wt% of cementing material, 20-55 wt% of fine aggregate and 40-75 wt% of coarse aggregate, wherein the cementing material comprises cement, desulfurized gypsum, acetic acid and water, the fine aggregate comprises gasified slag and fly ash, and the coarse aggregate comprises coal gangue and furnace bottom slag.
Preferably, the cementing material comprises the following components in percentage by mass: 20-40% of cement, 5-20% of desulfurized gypsum, 1-5% of acetic acid and 50-60% of water, wherein the cement is ordinary portland cement, the desulfurized gypsum is an industrial byproduct gypsum obtained by coal-fired or oil-fired industrial enterprises after treating sulfur dioxide in flue gas, the acetic acid (acetic acid) is an organic monobasic acid which is a source of sour taste and pungent smell in vinegar, and has industrial grade and purity of 5-30%.
Preferably, the fine aggregate comprises the following components in percentage by mass: 10-50% of gasified slag and 50-90% of fly ash, wherein the gasified slag is formed by incomplete combustion of coal and oxygen or oxygen-enriched air to generate CO and H2In the process, inorganic mineral substances in the coal undergo different physical and chemical transformations, and solid residues formed by residual carbon particles in the coal comprise the following components in percentage by mass: SiO 2231.73％、Al2O315.76％、CaO19.62％、 Fe2O318.25 percent of MgO4.57 percent and the bulk density is 2.24-2.68g/cm3The fly ash is fine ash collected from flue gas generated after coal combustion, is main solid waste discharged from a coal-fired power plant, and comprises the following components in percentage by mass: SiO 2255.33％、Al2O331.21％、Fe2O37.02 percent and CaO2.97 percent, and the bulk density is 1.07-2.4g/cm3The grain diameter of the gasified slag and the fly ash is 0.1-5 mm.
Preferably, the coarse aggregate comprises the following components in percentage by mass: 10-30% of coal gangue and furnace bottom slag70-90%, wherein the coal gangue is solid waste discharged in the coal mining process and the coal washing process, is a black gray rock which has lower carbon content and is harder than coal and is associated with a coal layer in the coal forming process, and comprises the following components in percentage by mass: SiO 2259.73％、Al2O320.16％、Fe2O35.51% and CaO1.96%, etc., and the bulk density is 1.7-1.9g/cm3The furnace bottom slag is bottom slag sent from the lower part of coal-fired power plants after being combusted by a boiler, and comprises the following components in percentage by mass: SiO 2244.81％、Al2O337.61％、Fe2O38.35 percent, CaO3.65 percent and the like, and the bulk density is 1.2-1.5g/cm3The grain diameter of the coal gangue and the furnace bottom slag is 5-25 mm.
A preparation method of a multi-element coal-based solid waste composite acid-excited underground filling material comprises the following steps:
(1) crushing coal gangue and furnace bottom slag into particles with the particle size of less than 25mm, preparing the particles into continuous-grade coarse aggregate, preparing fly ash and gasified slag into continuous-grade fine aggregate, and then ball-milling cement by adopting a ball mill into particles with the average particle size of less than 10 mu m;
(2) dissolving acetic acid in water, uniformly mixing, adding cement, uniformly stirring to form slurry, standing the cement slurry for 10-20min, adding desulfurized gypsum, fly ash and gasified slag after the acetic acid fully excites the hydration reaction activity of cement particles, quickly stirring for 30-90s, then adding coal gangue and bottom slag blocks, and quickly stirring for 30-90s to finish the preparation of the filling material for filling.
The invention has the beneficial effects that:
the invention fully utilizes the composite excitation effect of weak acid on cement, excites the hydration reaction activity of the cement, and improves the hydration reaction degree of cement micro particles so as to achieve the purposes of enhancing the mechanical property of the filling material and saving the consumption of the cement. Meanwhile, the cement particles are further ball-milled to the nanometer level, so that the back filling effect of the superfine cement particles is fully exerted, the effects of filling the inside of the nanometer cement particles and bonding the multi-coal-based solid wastes are realized, the form that the cement wraps the coarse aggregate in the traditional cement-based material is changed, the aim of further saving the cement is fulfilled, and the preparation cost of the material is reduced. Meanwhile, the contents of active calcium, active silicon and active aluminum in a hydration reaction environment are further improved by utilizing the calcium increasing, silicon increasing and aluminum increasing effects of the coal-based solid waste such as desulfurized gypsum, fly ash and the like, favorable conditions are provided for the formation of calcium silicate hydrate and calcium aluminosilicate hydrate, and finally, the preparation of the low-cost and high-performance multi-element coal-based solid waste filling material is realized under the condition of low cement consumption. The research and development of the filling material can not only realize large-scale safe consumption and resource utilization of multi-element coal-based solid waste, effectively relieve the environmental pollution problem caused by the multi-element coal-based solid waste, but also realize the backfill of the goaf, effectively prevent a series of environmental and economic problems caused by the collapse of the goaf, and fulfill the aim of killing two birds with one stone.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments.
Example 1
The preparation method of the multi-element coal-based solid waste composite acid-excited underground filling material comprises the following steps:
(1) firstly, crushing coal gangue and furnace bottom slag blocks into particle sizes below 25mm, respectively preparing continuous gradation, respectively preparing fly ash and gasified slag into continuous gradation, and putting 42.5-grade ordinary portland cement into a ball mill for continuous ball milling for 30 minutes to ensure that the particle sizes of cement particles are lower than 10 mu m.
(2) Weighing 1800g of ball-milled 42.5-grade ordinary portland cement, 200g of desulfurized gypsum and uniformly mixing, 1000g of water and 40g of acetic acid, uniformly mixing the two, weighing 7000g of well-graded fly ash and 1000g of gasified slag, uniformly mixing, finally weighing 11000g of well-graded coal gangue and 1000g of furnace bottom slag and uniformly mixing;
(3) firstly, adding acetic acid solution into the cement and the desulfurized gypsum powder which are uniformly mixed, standing for 15 minutes after uniform stirring, adding the fly ash and the gasified slag fine aggregate which are uniformly mixed, stirring for 60 seconds, finally adding the coal gangue and the furnace bottom slag which are uniformly mixed, and stirring for 90 seconds to obtain the filling material.
Example 2
The preparation method of the multi-element coal-based solid waste composite acid-excited underground filling material comprises the following steps:
(1) firstly, crushing coal gangue and furnace bottom slag blocks into particle sizes of less than 20mm, respectively preparing continuous gradation, respectively preparing fly ash and gasified slag into continuous gradation, putting 42.5-grade ordinary portland cement into a ball mill for continuous ball milling for 30 minutes, and ensuring that the particle sizes of cement particles are all lower than 10 mu m.
(2) Weighing 1600g of ball-milled 42.5-grade ordinary portland cement, 250g of desulfurized gypsum and uniformly mixing, 1200g of water and 40g of acetic acid, uniformly mixing the two, weighing 6000g of well-graded fly ash and 1100g of gasified slag and uniformly mixing, finally weighing 10000g of well-graded coal gangue and 1200g of furnace bottom slag and uniformly mixing;
(3) firstly, adding acetic acid solution into the cement and the desulfurized gypsum powder which are uniformly mixed, standing for 10 minutes after uniform stirring, adding the fly ash and the gasified slag fine aggregate which are uniformly mixed, stirring for 90 seconds, finally adding the coal gangue and the furnace bottom slag which are uniformly mixed, and stirring for 90 seconds to obtain the filling material.
Example 3
The preparation method of the multi-element coal-based solid waste composite acid-excited underground filling material comprises the following steps:
(1) firstly, crushing coal gangue and furnace bottom slag blocks into particle sizes below 25mm, respectively preparing continuous gradation, respectively preparing fly ash and gasified slag into continuous gradation, and putting 42.5-grade ordinary portland cement into a ball mill for continuous ball milling for 30 minutes to ensure that the particle sizes of cement particles are lower than 10 mu m.
(2) Weighing 2000g of ball-milled 42.5-grade ordinary portland cement, 300g of desulfurized gypsum and uniformly mixing, 1000g of water and 30g of acetic acid, uniformly mixing the two, weighing 7000g of well-graded fly ash and 1200g of gasified slag and uniformly mixing, and finally weighing 12000g of well-graded coal gangue and 800g of furnace bottom slag and uniformly mixing;
(3) firstly, adding acetic acid solution into the cement and desulfurized gypsum powder which are uniformly mixed, standing for 20 minutes after uniform stirring, adding the fly ash and gasified slag fine aggregate which are uniformly mixed, stirring for 60 seconds, finally adding the coal gangue and furnace bottom slag which are uniformly mixed, and stirring for 30 seconds to obtain the filling material.
Comparative example 1 (comparison of acetic acid to oxalic acid)
The preparation method of the multi-element coal-based solid waste composite acid-excited underground filling material comprises the following steps:
(1) firstly, crushing coal gangue and furnace bottom slag blocks into particle sizes below 25mm, respectively preparing continuous gradation, respectively preparing fly ash and gasified slag into continuous gradation, and putting 42.5-grade ordinary portland cement into a ball mill for continuous ball milling for 30 minutes to ensure that the particle sizes of cement particles are lower than 10 mu m.
(2) Weighing 1800g of ball-milled 42.5-grade ordinary portland cement, 200g of desulfurized gypsum and uniformly mixing, 1000g of water and 40g of oxalic acid, uniformly mixing the two, weighing 7000g of well-graded fly ash and 1000g of gasified slag, uniformly mixing, finally weighing 11000g of well-graded coal gangue and 1000g of furnace bottom slag and uniformly mixing;
(3) firstly, adding an oxalic acid solution into the cement and the desulfurized gypsum powder which are uniformly mixed, standing for 15 minutes after uniform stirring, adding the fly ash and the gasified slag fine aggregate which are uniformly mixed, stirring for 60 seconds, finally adding the coal gangue and the furnace bottom slag which are uniformly mixed, and stirring for 90 seconds to obtain the filling material.
COMPARATIVE EXAMPLE 2 (control without acetic acid addition)
The preparation method of the multi-element coal-based solid waste composite acid-excited underground filling material comprises the following steps:
(1) firstly, crushing coal gangue and furnace bottom slag blocks into particle sizes below 25mm, respectively preparing continuous gradation, respectively preparing fly ash and gasified slag into continuous gradation, and putting 42.5-grade ordinary portland cement into a ball mill for continuous ball milling for 30 minutes to ensure that the particle sizes of cement particles are lower than 10 mu m.
(2) Weighing 1800g of ball-milled 42.5-grade ordinary portland cement and 200g of desulfurized gypsum, uniformly mixing, weighing 7000g of fly ash with good gradation, 1000g of gasified slag, uniformly mixing, finally weighing 11000g of coal gangue with good gradation and 1000g of furnace bottom slag, and uniformly mixing;
(3) firstly, 1000g of water is added into the cement and the desulfurized gypsum powder which are uniformly mixed, the mixture is stirred uniformly and then is kept stand for 15 minutes, the fly ash and the gasified slag fine aggregate which are uniformly mixed are added, the mixture is stirred for 60 seconds, and finally the coal gangue and the furnace bottom slag which are uniformly mixed are added and stirred for 90 seconds, so that the filling material is obtained.
Performance detection
The filling materials prepared in examples 1 to 3 and comparative examples 1 to 2 were cast into a cubic mold of 100mm × 100mm × 100mm and slump was measured. And (5) after curing for 7d under natural conditions, removing the mold, and testing the compressive strength of the material 28 d.
TABLE 1 mechanical Property test of filling Material cast parts
As can be seen from Table 1, the compressive strength of the underground filling material 28d excited by the multi-element coal-based solid waste composite acid excited by acetic acid is over 5.5MP, while the filling material 7d excited by the oxalic acid has no compressive strength and the compressive strength of the underground filling material 28d is less than 1MPa under the same preparation conditions. The filling material 7d which is not excited by acid and does not ball mill cement still has compressive strength, and the 28d compressive strength only reaches 1.3MPa, which is 76.8 to 81.2 percent lower than that of the filling material in the embodiment 1, 2 and 328 d. Therefore, the advantages of the multielement coal-based solid waste composite acid excited by acetic acid for exciting the underground filling material are obvious.
It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed.
Claims (5)
1. The multielement coal-based solid waste composite acid-activated underground filling material is characterized by comprising 5-40 wt% of cementing material, 20-55 wt% of fine aggregate and 40-75 wt% of coarse aggregate, wherein the cementing material comprises cement, desulfurized gypsum, acetic acid and water, the fine aggregate comprises gasified slag and fly ash, and the coarse aggregate comprises coal gangue and furnace bottom slag.
2. The multi-element coal-based solid waste composite acid-excited downhole filling material according to claim 1, wherein the cementing material comprises the following components in percentage by mass: 20-40% of cement, 5-20% of desulfurized gypsum, 1-5% of acetic acid and 50-60% of water, wherein the cement is ordinary portland cement, the desulfurized gypsum is an industrial byproduct gypsum for flue gas desulfurization, and the acetic acid is industrial grade acetic acid with the purity of 5-30%.
3. The multi-element coal-based solid waste composite acid-activated downhole filling material of claim 1, wherein the fine aggregate comprises the following components in percentage by mass: 10-50% of gasified slag and 50-90% of fly ash, wherein the bulk density of the gasified slag is 2.24-2.68g/cm3(ii) a The bulk density of the fly ash is 1.07-2.4g/cm3The grain diameter of the gasified slag and the fly ash is 0.1-5.0 mm.
4. The multi-element coal-based solid waste composite acid-activated downhole filling material of claim 1, wherein the coarse aggregate comprises the following components in percentage by mass: 70-90% of coal gangue and 10-30% of furnace bottom slag, wherein the bulk density of the coal gangue is 1.7-1.9g/cm3(ii) a The bulk density of the furnace bottom slag is 1.2-1.5g/cm3The grain diameter of the coal gangue and the furnace bottom slag is 5-50 mm.
5. The preparation method of the multi-element coal-based solid waste composite acid excited downhole filling material according to any one of claims 1 to 4, characterized by comprising the following steps:
(1) crushing coal gangue and furnace bottom slag into particles with the particle size of less than 25mm, preparing the particles into continuous graded coarse aggregate, preparing fly ash and gasified slag into continuous graded fine aggregate, and then ball-milling cement by adopting a ball mill into particles with the average particle size of less than 10 mu m;
(2) dissolving acetic acid in water, uniformly mixing, adding cement, uniformly stirring to form slurry, standing the cement slurry for 10-20min, adding desulfurized gypsum, fly ash and gasified slag when the acetic acid fully excites the hydration reaction activity of cement particles, rapidly stirring for 30-90s, adding coal gangue and furnace bottom slag blocks, and rapidly stirring for 30-90s to finish the preparation of the filling material for filling.
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| CN117567091A (en) * | 2023-11-22 | 2024-02-20 | 中国矿业大学 | Mine water corrosion-resistant coal-based solid waste filling paste and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116143484A (en) * | 2022-11-11 | 2023-05-23 | 昆明理工大学 | Mine filling material based on coal gas slag, and preparation method and application thereof |
| CN116003055A (en) * | 2022-12-22 | 2023-04-25 | 陕西碳提取节能环保科技(集团)有限公司 | Coal chemical industry gasification slag coal gangue backfill and preparation method thereof |
| CN117567091A (en) * | 2023-11-22 | 2024-02-20 | 中国矿业大学 | Mine water corrosion-resistant coal-based solid waste filling paste and preparation method thereof |
| CN117567091B (en) * | 2023-11-22 | 2024-06-14 | 中国矿业大学 | Mine water corrosion-resistant coal-based solid waste filling paste and preparation method thereof |
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