CN113896489A - Mine cemented filling material for cooperatively treating mercury-containing solid waste and preparation method thereof - Google Patents
Mine cemented filling material for cooperatively treating mercury-containing solid waste and preparation method thereof Download PDFInfo
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- CN113896489A CN113896489A CN202111181551.9A CN202111181551A CN113896489A CN 113896489 A CN113896489 A CN 113896489A CN 202111181551 A CN202111181551 A CN 202111181551A CN 113896489 A CN113896489 A CN 113896489A
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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
-
- 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
- C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B14/02—Granular materials, e.g. microballoons
- C04B14/30—Oxides other than silica
- C04B14/306—Zirconium oxide
-
- 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
- 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
- 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
- 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
- C04B2111/00767—Uses not provided for elsewhere in C04B2111/00 for waste stabilisation purposes
- C04B2111/00784—Uses not provided for elsewhere in C04B2111/00 for waste stabilisation purposes for disposal only
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Landscapes
- 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)
- Civil Engineering (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a mine cemented filling material for cooperatively treating mercury-containing solid waste and a preparation method thereof, belonging to the technical field of mine cemented filling. Specifically discloses a raw material of the cemented filling material, which comprises: steel slag, gypsum, zirconia, aggregate, microbial inoculum, mercury-containing solid waste and a water reducing agent; the preparation method comprises the following steps: crushing the mercury-containing solid waste, and mixing the crushed mercury-containing solid waste with a microbial inoculum to obtain a mixture A; mixing the slag, the steel slag, the water reducing agent and the gypsum, adding the mixture A, the zirconia and the aggregate to obtain a mixture B, adding water, mixing and stirring to obtain the cemented filling material for the mine. The mine cemented filling material disclosed by the invention is excellent in mechanical property, overcomes the defect of poor mechanical property of slag and steel slag as cementing materials, can be used for cooperatively treating mercury-containing solid waste, realizes zero seepage of heavy metal mercury, and has important application value in the field of mine filling and the field of mercury-containing solid waste treatment.
Description
Technical Field
The invention relates to the technical field of mine cemented filling, in particular to a mine cemented filling material for synergistically treating mercury-containing solid waste and a preparation method thereof.
Background
Filling is advantageous in improving ore recovery, improving rock formation control and reducing waste rock stockpiling on the ground, and can be used as regional support and local support, and when used as regional support, filling can reduce goaf subsidence. Furthermore, since the charging reduces the energy release rate and shear stress, the high face stress can also be reduced.
The cemented filling is characterized in that gel materials, inert aggregates such as fine sand, tailings and the like are mixed with water and stirred to prepare cemented filling slurry, then the slurry is conveyed and stacked to an underground goaf along a drill hole, a pipe, a groove and the like, and the slurry gradually forms an integral filling body with certain strength in the goaf. The cement is the most widely used cementing agent at present, but has the characteristics of high energy consumption and serious pollution; along with the popularization of mine filling mining technology, the cementing agent of the filling material is continuously updated and developed.
Toxic substances leached from industrial solid wastes can migrate in the natural environment, and the health of human bodies is influenced. Heavy metal mercury and compounds thereof have extremely strong toxicity, are not easy to metabolize in organisms, have enrichment function along with biological chains, and have long-term harmfulness and latency, so that the mercury-containing solid waste is necessary to be safely treated.
Currently, there are various treatment methods for solid waste, wherein safe landfill treatment is a technology with higher risk, and the technology has higher requirements on the seepage prevention of toxic substances. Therefore, curing/stabilization treatments are often required prior to solid waste landfills.
Slag and steel slag are used as main waste residues in metallurgical industry, are main objects of solid waste resource research, and can be used for preparing gel materials of cementing filling materials by replacing cement with the slag and the steel slag. However, the effect of using slag and steel slag as the cementing filler of the gel material is not ideal in terms of compressive strength, and the effect of preventing heavy metal from leaking is still to be enhanced when the gel material is used for solidifying and stabilizing waste containing heavy metal.
Aiming at the current situation, the cementing filler for the mine, which has high compressive strength and extremely strong anti-seepage effect on mercury-containing solid waste, has extremely important significance.
Disclosure of Invention
The invention aims to provide a mine cemented filling material for synergistically treating mercury-containing solid waste and a preparation method thereof, which are used for solving the problems in the prior art and enabling the mine cemented filling material to have the characteristics of high strength and excellent mercury curing effect.
In order to achieve the purpose, the invention provides the following scheme:
one purpose of the invention is to provide a mine cemented filling material for synergistic treatment of mercury-containing solid waste, which comprises the following raw materials in parts by weight:
15-18 parts of steel slag, 60-70 parts of slag, 10-25 parts of gypsum, 1-3 parts of zirconia, 550 parts of aggregate 450-;
the microbial inoculum is a mixture of bacillus and kaolin in a mass ratio of 1-1.2: 1; the bacillus is alkalophilic bacillus NTT33C6D 2.
Further, the aggregate is one or more of tailings, coal gangue and waste rocks.
Further, the water reducing agent is lignosulfonate or naphthalene sulfonate.
The invention also aims to provide a preparation method of the cemented filling material for the mine, which comprises the following steps:
crushing the mercury-containing solid waste, and mixing the crushed mercury-containing solid waste with a microbial inoculum to obtain a mixture A;
mixing slag, steel slag, a water reducing agent and gypsum, adding the mixture A, then adding zirconia and aggregate to obtain a mixture B, adding water into the mixture B, mixing and stirring to obtain the cemented filling material for the mine.
Further, the solid content of the system after adding water is 70-75%.
The invention also aims to provide application of the cemented filling material for mines in the field of mercury-containing solid waste treatment.
The invention discloses the following technical effects:
the invention adopts the microbial inoculum to stabilize the mercury-containing solid waste, the surface charge of the bacterial cells can adsorb mercury ions, and the mercury ions are biologically enriched, and meanwhile, the alkalophilic bacillus NTT33C6D2 can rapidly and stably generate sulfur ions through redox action and methylation, so that the stable mercury sulfide is formed by combining with the mercury ions, and the seepage of heavy metal mercury is avoided.
The zirconium oxide component in the filling material can act with CaO in the slag and the steel slag to form a stable complex, so that the mechanical strength of the slag and the steel slag is enhanced, and heavy metal mercury is further stably coated to avoid the seepage of the heavy metal mercury.
The mine cemented filling material disclosed by the invention is excellent in mechanical property, overcomes the defect of poor mechanical property of slag and steel slag as cementing materials, can be used for cooperatively treating mercury-containing solid waste, realizes zero seepage of heavy metal mercury, and has important application value in the field of mine filling and the field of mercury-containing solid waste treatment.
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 description and examples are intended to be illustrative 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 "parts" in the present invention are all parts by mass unless otherwise specified.
In the embodiment of the invention, the solid waste containing mercury is subjected to leaching experiments according to a leaching procedure specified in solid waste leaching toxicity leaching method sulfuric acid-nitric acid method (HJ/T299), the concentration of mercury in a leaching solution exceeds 0.1mg/L, and the source is tailings generated in the process of mercury ore mining and dressing.
In the examples of the present invention, the specific surface area of the ground slag was 480m2Kg, main chemical composition analysis is shown in Table 1.
TABLE 1
| Composition (I) | SiO2 | CaO | Al2O3 | Fe2O3 | MgO | SO3 | Pb |
| Content (%) | 32.71 | 38.63 | 15.44 | 0.42 | 8.34 | 0.25 | 0 |
In the embodiment of the invention, the steel slag is the tailings obtained by pretreating converter steel slag by a smoldering method and selecting iron, and the surface area of the powder is 475m2Kg, main chemical composition analysis is shown in Table 2.
TABLE 2
In the embodiment of the invention, the Bacillus alcalophilus NTT33C6D2 is purchased from China center for type culture Collection with the collection number of CCTCC NO: m2016317.
Example 1
The cementing filling material for the mine comprises the following raw materials:
15 parts of steel slag, 60 parts of slag, 25 parts of phosphogypsum, 1 part of zirconia, 550 parts of aggregate, 5 parts of microbial inoculum, 10 parts of mercury-containing solid waste and 1 part of water reducing agent.
The aggregate is tailings, the water reducing agent is sodium lignosulphonate, and the microbial inoculum is a mixture of bacillus alcalophilus NTT33C6D2 and kaolin in a mass ratio of 1: 1.
The preparation method comprises the following steps:
(1) crushing the mercury-containing solid waste into 100 meshes, and mixing with a microbial inoculum to obtain a mixture A;
(2) mixing slag, steel slag, a water reducing agent and phosphogypsum, adding the mixture A obtained in the step (1), adding zirconium oxide and aggregate, uniformly stirring to obtain a mixture B, adding water into a system to enable the solid content to be 75%, and mixing and stirring to obtain the cementing filling material for the mine.
Example 2
The cementing filling material for the mine comprises the following raw materials:
18 parts of steel slag, 65 parts of slag, 10 parts of phosphogypsum, 2 parts of zirconia, 500 parts of aggregate, 6 parts of microbial inoculum, 1 part of mercury-containing solid waste and 0.5 part of water reducing agent.
The aggregate is waste stone; the water reducing agent is sodium naphthalene sulfonate; the microbial inoculum is a mixture of bacillus alcalophilus NTT33C6D2 and kaolin in a mass ratio of 1: 1.
The preparation method comprises the following steps:
(1) crushing the mercury-containing solid waste to 80 meshes, and mixing with a microbial inoculum to obtain a mixture A;
(2) mixing slag, steel slag, a water reducing agent and phosphogypsum, adding the mixture A obtained in the step (1), adding zirconia and aggregate, uniformly stirring to obtain a mixture B, adding water into a system to enable the solid content to be 70%, and mixing and stirring to obtain the cementing filling material for the mine.
Example 3
The cementing filling material for the mine comprises the following raw materials:
17 parts of steel slag, 70 parts of slag, 15 parts of fluorgypsum, 3 parts of zirconia, 450 parts of aggregate, 4 parts of microbial inoculum, 8 parts of mercury-containing solid waste and 0.8 part of water reducing agent.
The aggregate is a mixture composed of tailings, coal gangue and the like in a mass ratio; the water reducing agent is sodium lignosulphonate;
the microbial inoculum is a mixture of bacillus alcalophilus NTT33C6D2 and kaolin in a mass ratio of 1.2: 1.
The preparation method comprises the following steps:
(1) crushing the mercury-containing solid waste into 100 meshes, and mixing with a microbial inoculum to obtain a mixture A;
(2) mixing the slag, the steel slag, the water reducing agent and the fluorgypsum, adding the mixture A obtained in the step (1), then adding the zirconium oxide and the aggregate, uniformly stirring to obtain a mixture B, then adding the water into the system to enable the solid content to be 72%, and mixing and stirring to obtain the cementing filling material for the mine.
Comparative example 1
The difference from example 1 is that no zirconia is added.
Comparative example 2
The difference from example 1 is that no microbial inoculum was added.
The compressive strength test and the mercury toxicity leaching test were conducted on the mine cemented fillers prepared in examples 1 to 3 and comparative examples 1 to 2 in a uniaxial infinite manner, and the test methods were as follows:
test groups: injecting the mine cemented filling materials prepared in the examples 1-3 and the comparative examples 1-2 into a standard test mold, and oscillating for 30s by using an oscillating table;
control group: and (3) replacing slag, steel slag and gypsum components with 32.5-grade cement to prepare the mine cemented filling material, injecting the obtained mine cemented filling material into a standard test mold, and vibrating for 30s by using a vibration table.
The preparation of the hardened body leachate is carried out according to HJ 557-2009-solid waste leaching toxicity leaching method horizontal oscillation method.
And (3) curing the test group and the control group for 24 hours in a module mode, placing the test group and the control group into a heat preservation box for curing after the module is removed, and detecting the uniaxial unconfined compressive strength and the mercury toxicity leaching value at different ages, wherein the results are shown in tables 3-4.
TABLE 3
TABLE 4
Note: the drinking water standard is that the concentration of mercury is less than 1ug/L, and the detection limit is less than 1 ug/L. "-" indicates that the mercury leach concentration is below the detection limit.
The results in table 3 show that the mine cemented filling material for synergistically treating mercury-containing solid wastes according to the present invention has excellent mechanical properties, and comparative example 1, in which no zirconia was added, has significantly reduced compressive strength as compared to example 1, because the zirconia component forms a stable complex with CaO in slag and steel slag, thereby significantly enhancing the mechanical properties of the filling material.
The mercury leaching experiment result in table 4 shows that the filling material of the invention can realize zero leaching of heavy metal mercury, compared with the comparative example 2 without adding microbial inoculum and the comparative example 1 without adding zirconia, the examples 1-4 have obvious effect of preventing the heavy metal mercury from leaching, which depends on the stabilizing effect of bacteria on mercury ions and the further stable coating of zirconia, and the double effects of the two can realize zero leaching of heavy metal mercury.
The results show that the filling material has important application value in the mine filling field and the mercury-containing solid waste treatment field.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (6)
1. The mine cementing filling material for synergistically treating mercury-containing solid waste is characterized in that raw materials comprise the following components in parts by weight:
15-18 parts of steel slag, 60-70 parts of slag, 10-25 parts of gypsum, 1-3 parts of zirconia, 550 parts of aggregate 450-;
the microbial inoculum is a mixture of bacillus and kaolin in a mass ratio of 1-1.2: 1; the bacillus is alkalophilic bacillus NTT33C6D 2.
2. The cementitious filler for mines according to claim 1, wherein the aggregate is one or more of tailings, coal gangue, and waste rock.
3. The cementitious filler for mines according to claim 1, wherein the water reducing agent is lignosulfonate or naphthalenesulfonate.
4. The method for producing a cementitious filler for mines according to any one of claims 1 to 3, comprising the steps of:
crushing the mercury-containing solid waste, and mixing the crushed mercury-containing solid waste with a microbial inoculum to obtain a mixture A;
mixing slag, steel slag, a water reducing agent and gypsum, adding the mixture A, then adding zirconia and aggregate to obtain a mixture B, adding water into the mixture B, mixing and stirring to obtain the cemented filling material for the mine.
5. The process according to claim 4, wherein the solids content of the system after the addition of water is 70 to 75%.
6. Use of the mine cementitious filler according to any one of claims 1 to 3 in the field of treatment of mercury-containing solid waste.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115869580A (en) * | 2022-11-29 | 2023-03-31 | 贵州大学 | Mercury tailing curing agent and using method thereof |
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2021
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| SE9003195D0 (en) * | 1990-10-05 | 1990-10-05 | Kurz Fredrik W A | PROVIDED TO IMPROVE THE ACTIVATION OF LATENT HYDRAULIC BASIC MACHINING TYPE WHEN MANUFACTURING BUILDING MATERIAL |
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| CN106495939A (en) * | 2016-10-14 | 2017-03-15 | 上海诺同农业科技有限公司 | Heavy metal-polluted soil renovation agent, preparation method and application |
| CN108439922A (en) * | 2018-04-04 | 2018-08-24 | 黄智慧 | A kind of concrete cement material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115869580A (en) * | 2022-11-29 | 2023-03-31 | 贵州大学 | Mercury tailing curing agent and using method thereof |
| CN115869580B (en) * | 2022-11-29 | 2024-03-01 | 贵州大学 | Mercury tailing curing agent and use method thereof |
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