CN111847924B - Tailing-based cementing material and preparation method thereof - Google Patents
Tailing-based cementing material and preparation method thereof Download PDFInfo
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- CN111847924B CN111847924B CN202010772265.9A CN202010772265A CN111847924B CN 111847924 B CN111847924 B CN 111847924B CN 202010772265 A CN202010772265 A CN 202010772265A CN 111847924 B CN111847924 B CN 111847924B
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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
- C04B7/24—Cements from oil shales, residues or waste other than slag
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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
- C04B7/24—Cements from oil shales, residues or waste other than slag
- C04B7/28—Cements from oil shales, residues or waste other than slag from combustion residues, e.g. ashes or slags from waste incineration
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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
- C04B7/36—Manufacture of hydraulic cements in general
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- 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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Abstract
The invention discloses a tailing-based cementing material and a preparation method thereof. The method comprises the steps of drying a tailing raw material, and sequentially carrying out mechanical ball milling activation treatment, thermal activation treatment and chemical agent activation treatment to obtain the tailing-based gelling material. The method activates the tailings by a combined excitation method of mechanical activation, thermal activation and chemical activation, utilizes the potential pozzolanic activity of the tailings to obtain a cementing material with better cementing property, the compressive strength of the consolidated cementing material can reach 10MPa to the maximum, the underground filling process is completely met, and the consolidated leachate meets the IV-class water body standard of surface water quality.
Description
Technical Field
The invention relates to a method for utilizing tailings, in particular to a method for preparing a cementing material by utilizing tailings to realize resource utilization of the tailings, and belongs to the technical field of solid waste resource utilization.
Background
The tailings refer to industrial solid waste discharged after crushing and flotation of raw ores, the discharge amount of the industrial solid waste is large, a special tailing pond needs to be built for stacking, the particle size of the tailings is small, heavy metals and other water-soluble compounds can permeate into environmental water after being stacked for a long time, and the heavy metals and the water-soluble compounds fly with wind to form floating dust, so that the surrounding ecological environment is easily polluted. Part of the sulfur-containing tailings is easy to form acidic wastewater under a series of chemical actions, which endangers the growth of animals, plants and crops and finally endangers the health of human bodies. Therefore, with the increase of industrial exploitation, the discharge amount and the remaining amount of tailings are continuously increased, and the comprehensive utilization of the tailings becomes a problem to be solved urgently for industrial development and environmental protection.
At present, domestic related comprehensive treatment of tailings is mostly concentrated on the aspects of underground filling admixtures, concrete admixtures, building fine aggregates and the like, the treatment methods need to be added with cement or other cementing materials to different degrees, the defects of high treatment cost, low utilization degree and the like exist, and the strength of the consolidated tailings admixtures and the leaching problem of heavy metals are all to be improved.
Chinese patent (CN201710007614) discloses preparation of a novel filling material of iron ore full tailings, which is prepared by utilizing tailings, cement and water in proportion, is used for filling goafs in mining areas and repairing seepage cracks in mines, and realizes comprehensive utilization of iron tailings. However, in the method, cement is used as a main cementing material, and the filling cost is high. The Chinese patent (CN201510166877) utilizes iron ore blast furnace water quenched slag, fly ash, cement clinker, lime and gypsum to prepare a novel tailing consolidation discharge cementing agent in proportion, and the consolidation discharge slurry with strength meeting the discharge requirement has good social significance and economic benefit for recycling industrial resources. However, the method mainly uses iron ore blast furnace water quenched slag, fly ash, cement clinker, lime and gypsum, and has low utilization degree of tailings. At present, the common cementing materials for development mainly comprise gypsum, slag, fly ash, smelting slag, coal gangue and the like.
Disclosure of Invention
Aiming at the defects of the comprehensive utilization technology of tailings in the prior art, the invention aims to provide the tailing-based cementing material with short consolidation time and high strength, the consolidation strength of the tailing-based cementing material completely meets the requirements of an underground filling process, and the consolidated leachate meets the IV-class water body standard of surface water quality.
The second purpose of the invention is to provide a preparation method of the tailing-based cementing material, which utilizes tailings as main raw materials, has high tailing utilization rate, wide tailing raw material source, large storage capacity, simple treatment mode and convenient operation, can be used for large-scale production, and reduces the ecological problem caused by the large-scale stockpiling of the tailings.
In order to achieve the technical purpose, the invention provides a preparation method of a tailing-based cementing material, which comprises the steps of drying tailing raw materials, and sequentially carrying out mechanical ball-milling activation treatment, thermal activation treatment and chemical agent activation treatment.
According to the technical scheme, tailings are activated through a combined excitation method of mechanical activation, thermal activation and chemical activation, potential pozzolanic activity of the tailings is utilized, the cementing material with good cementing performance is obtained, the compressive strength of the consolidated cementing material can reach 10MPa at most, the strength completely meets an underground filling process, and the leachate meets the IV-class water body standard of surface water quality after consolidation.
As a preferable scheme, the main mineral components of the tailing raw materials are quartz and dolomite, and the total mass ratio of the quartz and the dolomite is within the range of 58-75%. Tailings original D of the invention50The water content is about 150 mu m and 5-30%, and the waste belongs to general industrial solid waste. The tailings are iron tailings, copper tailings, gold tailings, lead-zinc tailings, other non-ferrous metal tailings or non-metal tailings and the like.
As a preferred embodiment, the conditions of the mechanical ball milling activation treatment are as follows: the rotating speed of the ball mill is 100-500 r/s, and the ball milling time is 10-120 min. The mechanical activation can destroy the surface of the material by mechanical force, reduce the particle size, change the crystal structure and surface physical and chemical properties, distort the crystal structure of the mineral, reduce the crystallization degree, and gradually generate phenomena such as lattice dislocation, defect, recrystallization and the like, and SiO2And A12O3The active gelation material is soluble and forms an amorphous state coated on the surface of particles, so that external water molecules can enter the interior of the active gelation material more quickly, the hydration reaction efficiency is improved, and the potential active gelation performance of tailings can be effectively excited through mechanical ball milling activation treatment. The rotation speed of the ball mill is more preferably 200 to 400 r/s.
As a preferable scheme, the mechanical ball milling activation treatment controls the grinding of the tailing raw materials to the particle size of 200-10 μm. The influence of the particle size of the tailings on the hydration hardening performance is large, so the gel performance can be improved to a certain extent by controlling the particle size of the tailings raw material powder.
As a preferred embodiment, the conditions of the thermal activation treatment are: and preserving the heat for 10-120 min at the temperature of 300-1000 ℃. Through the action of thermal activation, the crystal lattices of silicon-oxygen tetrahedron and aluminum-oxygen tetrahedron in tailings can be destroyed, the structure and surface physical and chemical properties of the crystal are changed, the crystal structure of the mineral is distorted, the crystallinity begins to be reduced, phenomena such as crystal lattice dislocation, defect, recrystallization and the like gradually occur, and SiO2And A12O3The particles are soluble, and form an amorphous state coated on the surfaces of the particles, so that external water molecules enter. The interior is faster, and the hydration reaction efficiency is improved. The heat activation treatment temperature is more preferably 400 to 600 ℃.
As a preferred scheme, in the thermal activation treatment process, the tailings subjected to the mechanical ball milling activation treatment are uniformly mixed with the biomass material; the biomass material is rice hull ash; the biomass material is less than or equal to 100 percent of the mass of the tailing materials. The biomass material is residual ash residue obtained by burning plant raw materials such as rice hulls and the like, such as rice hull ash. The ash contains a large amount of amorphous SiO2Capable of reacting with Ca (OH)2The reaction is carried out to generate C-S-H gel, so that the strength of the slurry is improved, the porous structure of the slurry enables the interior of the slurry to adsorb moisture, the volcanic ash reaction is facilitated, the gelling property of the added material is enhanced, and the strength of a consolidation body for consolidating tailings is enhanced. The biomass material is further preferably 10-50% of the mass of the tailing raw material.
As a preferable scheme, at least one chemical activating agent selected from sodium hydroxide, potassium hydroxide, calcium oxide, potassium oxide, sodium sulfate, calcium sulfate and cement clinker is added into the tailings subjected to the thermal activation treatment in the chemical agent activation treatment process. The substance or mixture without hydration activity can be converted into gelling material by adding chemical agent, such as alkali (lime, water glass, NaOH), clinker, sulfate (CaSO)4,Na2SO4) And depolymerizing the silicate network with a high degree of polymerization, and separating the silicon and aluminum anionic groups and the hydration product Ca(OH)2The calcium silicate hydrate, ettringite (AFt) and monosulfide calcium sulfoaluminate hydrate are further generated to generate the strength of the consolidation body.
As a preferable scheme, the addition amount of the chemical activating agent is 3-15% of the mass of the tailings subjected to thermal activation treatment; more preferably 5 to 10%.
According to the technical scheme, the tailing raw materials are sequentially subjected to mechanical ball milling activation treatment, thermal activation treatment and chemical agent activation treatment, the hydration activity of the tailing raw materials is stimulated to the maximum degree by utilizing the synergistic effect of the three activation treatments, the specific surface is increased, the crystal structure and the surface physical and chemical properties are changed, and the chemical agent excitation is combined, so that the active ingredients of the effective ingredients in the tailing raw materials are fully exerted.
The invention also provides a tailing-based cementing material which is obtained by the preparation method.
The invention provides a method for preparing a tailing-based cementing material by utilizing tailings, which comprises the following specific steps of:
1) putting a certain amount of raw tailings into a 105 ℃ blast drying oven to be dried to constant weight, grinding for 10-120 min by using a ball mill, and keeping for later use at the ball milling rotating speed of 100-500 r/s;
2) adding 0-100% of biomass material into the tailings obtained in the step 1), and uniformly mixing for later use;
3) placing the product obtained in the step 2) in a heating device at the temperature of 300-1000 ℃ and heating for 10-120 min;
4) adding a certain amount of one or more of sodium hydroxide, potassium hydroxide, calcium oxide, potassium oxide, sodium sulfate, calcium sulfate, cement clinker and the like into the product obtained in the step 3), and uniformly mixing for later use;
5) and (3) developing a clean slurry forming experiment on the product obtained in the step 4), preparing a clean slurry test block of 4cm multiplied by 4cm, curing for 1-28 days, testing the compressive strength and taking an average value.
Compared with the prior art, the technical scheme of the invention has the following beneficial technical effects:
1) the invention takes the solid waste resource tailings as raw materials, has wide sources and large reserves, not only can realize resource utilization, but also can reduce the ecological problem caused by the large stockpiling of the tailings.
2) In the process of preparing the tailing-based cementing material by utilizing the tailings, the method has the advantages of simple tailing treatment mode, convenient operation procedure and large-scale production.
3) The invention can also add agricultural solid waste in the process of preparing the tailing-based cementing material by utilizing the tailings, and is a good way for comprehensively treating the agricultural solid waste.
4) The tailing-based cementing material prepared by utilizing the tailings has good cementing property, the strength of the concretion in 28 days can reach 10MPa, the strength of the underground filling concretion is completely met, and the heavy metal leaching of the concretion meets the IV-class water body of the surface water environment quality.
Drawings
FIG. 1 is a scanning electron micrograph of the raw tailings used in example 1;
FIG. 2 is a graph of the particle size distribution of the raw tailings used in example 1;
FIG. 3 is a 28-day scanning electron microscope image of a tailing-based cementitious material solidification body prepared by a control experiment group 9;
fig. 4 is a control experiment group 9 tailing-based cementing material solidification body toxicity leaching detection.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
A preparation method of a tailing-based environment functional material comprises the following specific implementation steps:
1) taking 10kg of lead-zinc tailings (the total mass of quartz and dolomite accounts for about 70 percent, and the original D of the lead-zinc tailings50About 150 mu m and the water content of about 20 percent) is put into a 105 ℃ blast drying oven to be dried to constant weight, and then a ball mill (the rotating speed is 300r/s) is used for grinding the dried lead-zinc tailings for 120min and the dried lead-zinc tailings are reserved for standby application;
2) adding 0% of rice hull ash into the lead-zinc tailings obtained in the step 1), and uniformly mixing for later use;
3) placing the product obtained in the step 2) in a heating device, heating for 40min at the temperature of 500 ℃, and naturally cooling for later use;
4) adding 10% sodium sulfate into the product obtained in the step 3), and uniformly mixing for later use;
5) and (3) developing a clear paste forming experiment on the product obtained in the step 4), preparing a clear paste test block of 4cm multiplied by 4cm, curing for 28 days, testing the compressive strength and averaging.
Tests show that the average value of the 28-day compressive strength of the cementing material prepared by heating the cementing material for 40min at the heat treatment temperature of 500 ℃ by adopting the preparation method disclosed by the invention is 3.75MPa, the strength of the tailing underground filling body is met, and the cementing property is better.
Control experiment group
The following control experiment group was performed as example 1, and the specific operating conditions, raw materials and amounts thereof were as follows in table 1:
TABLE 1
Weight percent (%)
Example 2
A preparation method of a tailing-based cementing material comprises the following specific implementation steps:
1) taking 10kg of lead-zinc tailings (the total mass of quartz and dolomite accounts for about 70 percent, and the original D of the lead-zinc tailings50About 150 mu m and the water content of about 20 percent) is put into a 105 ℃ blast drying oven to be dried to constant weight, and then a ball mill (the ball milling rotating speed is 200r/s) is used for grinding the dried lead-zinc tailings for 20min and the dried lead-zinc tailings are reserved for standby application;
2) adding 30% of rice hull ash into the lead-zinc tailings obtained in the step 1), and uniformly mixing for later use;
3) placing the product obtained in the step 2) in a heating device, heating for 30min at the temperature of 400 ℃, and naturally cooling for later use;
4) adding cement clinker accounting for 8% of the product obtained in the step 3), and uniformly mixing for later use;
5) and (3) developing a clear paste forming experiment on the product obtained in the step 4), preparing a clear paste test block of 4cm multiplied by 4cm, curing for 28 days, testing the compressive strength and averaging.
Tests show that the compressive strength of the cementing material prepared by heating the cementing material for 30min at the heat treatment temperature of 400 ℃ in 28 days is 6.25MPa, the strength of a tailing filling body is met, and the cementing property is good.
Example 3
1) The concretion body concreted for 28 days in the embodiment 1 is crushed and sealed by absolute ethyl alcohol for 2 days;
2) drying the solid obtained in the step 1) at 70 ℃, and grinding the dried solid through a 5mm square-hole sieve for later use;
3) carrying out leaching toxicity detection on the solid in the step 2) by using a standard HJ/T300-2007;
the detection shows that the concretion leaching detection of the cementing material meets the IV-class water body of the surface water environment quality.
The above is not relevant and is applicable to the prior art.
While certain specific embodiments of the present invention have been described in detail by way of illustration, it will be understood by those skilled in the art that the foregoing is illustrative only and is not limiting of the scope of the invention, as various modifications or additions may be made to the specific embodiments described and substituted in a similar manner by those skilled in the art without departing from the scope of the invention as defined in the appending claims. It should be understood by those skilled in the art that any modifications, equivalents, improvements and the like made to the above embodiments in accordance with the technical spirit of the present invention are included in the scope of the present invention.
Claims (2)
1. A preparation method of a tailing-based cementing material is characterized by comprising the following steps: drying the tailing raw material, and sequentially carrying out mechanical ball milling activation treatment, thermal activation treatment and chemical agent activation treatment to obtain the tailing raw material;
the main mineral components of the tailing raw material are quartz and dolomite, and the total mass ratio of the quartz and the dolomite is within the range of 58-75%; the conditions of the mechanical ball milling activation treatment are as follows: the rotating speed of the ball mill is 100-500 r/s, and the ball milling time is 10-120 min; the mechanical ball milling activation treatment controls the grinding of the tailing raw material to the particle size of 200-10 mu m; in the thermal activation treatment process, the tailings subjected to mechanical ball milling activation treatment are uniformly doped with biomass materials; the biomass material is rice hull ash; the biomass material accounts for 10-50% of the mass of the tailing raw material; the conditions of the thermal activation treatment are as follows: preserving the heat for 10-120 min at the temperature of 300-1000 ℃; in the chemical agent activation treatment process, at least one chemical activator selected from sodium hydroxide, potassium hydroxide, calcium oxide, potassium oxide, sodium sulfate, calcium sulfate and cement clinker is added into the tailings subjected to thermal activation treatment; the addition amount of the chemical activating agent is 3-15% of the mass of the tailings subjected to thermal activation treatment.
2. A tailing-based cementitious material, characterized in that: the method according to claim 1.
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| CN112624697B (en) * | 2020-12-22 | 2022-07-19 | 中建西部建设新疆有限公司 | Shrinkage-reducing concrete based on modified quartz stone powder and preparation method thereof |
| CN112919846A (en) * | 2021-03-05 | 2021-06-08 | 江西理工大学 | Method for preparing concrete admixture from tailings |
| CN113200688B (en) * | 2021-04-14 | 2023-07-18 | 河南省宜居建材科技有限公司 | Method for preparing cementing material based on comprehensive tailings |
| CN113121132A (en) * | 2021-05-06 | 2021-07-16 | 昆明理工大学 | Alkali-activated tailing-based composite cementing material and preparation method thereof |
| CN113277819A (en) * | 2021-05-20 | 2021-08-20 | 武汉大学 | Method for preparing building material by using industrial solid waste |
| CN113233804A (en) * | 2021-06-07 | 2021-08-10 | 武汉大学 | Antimony tailing powder-based alkali-activated cementing material and preparation method thereof |
| CN113248216B (en) * | 2021-06-21 | 2021-10-01 | 北京科技大学 | Preparation and application method of rice hull ash-doped cemented filling material |
| CN113896501B (en) * | 2021-10-15 | 2022-10-11 | 武汉大学 | Lead-zinc tailing powder-based cementing material |
| CN114105502B (en) * | 2021-11-26 | 2022-12-20 | 北京科技大学 | Cementing material, historic building repair mortar and preparation method thereof |
| CN114507020A (en) * | 2021-12-29 | 2022-05-17 | 武汉大学(肇庆)资源与环境技术研究院 | Lead-zinc tailing base-activated cementing material and application thereof |
| CN116102281B (en) * | 2022-11-18 | 2023-07-25 | 湖南科技大学 | Method for quickly preparing high-activity mixed material at low temperature by utilizing shield drying soil and high-activity mixed material prepared by method and application of high-activity mixed material |
| CN116496008A (en) * | 2023-04-17 | 2023-07-28 | 中山大学 | Active composite powder based on steel slag and preparation method thereof |
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| CN105060742A (en) * | 2015-07-27 | 2015-11-18 | 中国科学院武汉岩土力学研究所 | Preparation method for low-grade manganese tailing-based binding material |
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| CN110590199A (en) * | 2019-08-29 | 2019-12-20 | 广东清大同科环保技术有限公司 | Lead-zinc tailing cementing material and preparation method thereof |
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