CN113880539A - Mine karst cave filling slurry and preparation method thereof - Google Patents

Mine karst cave filling slurry and preparation method thereof Download PDF

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Publication number
CN113880539A
CN113880539A CN202111405308.0A CN202111405308A CN113880539A CN 113880539 A CN113880539 A CN 113880539A CN 202111405308 A CN202111405308 A CN 202111405308A CN 113880539 A CN113880539 A CN 113880539A
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CN
China
Prior art keywords
mine
phosphogypsum
red mud
filling slurry
fly ash
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Pending
Application number
CN202111405308.0A
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Chinese (zh)
Inventor
仇伟
唐安江
马连刚
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Guizhou Institute of Technology
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Guizhou Institute of Technology
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Priority to CN202111405308.0A priority Critical patent/CN113880539A/en
Publication of CN113880539A publication Critical patent/CN113880539A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/14Compositions 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
    • C04B28/142Compositions 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
    • C04B28/143Compositions 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
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B18/00Use 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
    • C04B18/04Waste materials; Refuse
    • C04B18/0409Waste from the purification of bauxite, e.g. red mud
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B18/00Use 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
    • C04B18/04Waste materials; Refuse
    • C04B18/06Combustion residues, e.g. purification products of smoke, fumes or exhaust gases
    • C04B18/08Flue dust, i.e. fly ash
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00017Aspects relating to the protection of the environment
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00724Uses not provided for elsewhere in C04B2111/00 in mining operations, e.g. for backfilling; in making tunnels or galleries
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/70Grouts, e.g. injection mixtures for cables for prestressed concrete
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2201/00Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/50Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/91Use of waste materials as fillers for mortars or concrete

Abstract

The invention discloses a mine karst cave filling slurry and a preparation method thereof, belonging to the technical field of mine filling, wherein the mine filling slurry consists of 30-60% of red mud, 20-40% of phosphogypsum, 10-20% of fly ash and 5-10% of modifier by mass percent; the mine filling slurry prepared by the invention is synthesized by grinding and mixing with water, has good fluidity, wide raw material source, lower production cost, simple process, and meeting the requirements on solidification time and strength, consumes a large amount of red mud and phosphogypsum industrial waste residues, and has important significance for energy conservation, emission reduction and environmental protection.

Description

Mine karst cave filling slurry and preparation method thereof
Technical Field
The invention belongs to the technical field of mine filling, and particularly relates to mine karst cave filling slurry and a preparation method thereof.
Background
At present, about hundred million tons of red mud are discharged all over the world every year, in recent years, along with the rapid development of alumina industries in various parts of China, the discharge of the red mud exceeds 5000 million tons per year, and the accumulated red mud accumulation amount reaches hundreds of millions of tons, which is the most important in the world. However, the utilization rate of the red mud in the world is about 15 percent, and the utilization rate of China is far lower than the level. A large amount of red mud accumulated for many years not only occupies a large amount of land and consumes more yard construction and maintenance and management costs, but also poses potential threats to the surrounding environment, and the disposal of the red mud becomes one of the technical bottlenecks restricting the development of the aluminum smelting industry.
With the rapid development of the phosphorus chemical industry, a wet-process phosphoric acid process with relatively low production cost is adopted in large quantities, so that a large amount of phosphogypsum waste residues are generated. According to calculation, 5-6 tons of phosphogypsum are produced per 1 ton of phosphoric acid, and the amount of the discharged phosphogypsum is about 500 million tons per year if the yield of 100 million tons produced per year in Guizhou is calculated. Therefore, how to effectively treat the phosphogypsum also becomes a key problem for solving the problem of environmental pollution of the phosphogypsum.
At present, the treatment technology of the phosphogypsum and the red mud is not mature enough, and although some effective measures are taken for the comprehensive utilization of the phosphogypsum and the red mud, certain problems still exist, such as low consumption, high treatment cost, high energy consumption and the like. The comprehensive utilization technology capable of simultaneously consuming a large amount of phosphogypsum and red mud is beneficial to the healthy development of the phosphorus chemical industry and the aluminum smelting industry.
On the other hand, after mining corresponding resources, a large number of goafs formed in the mining industry are easy to collapse, so that the land and vegetation are damaged, and even serious safety accidents are caused. The method for preparing filling slurry by utilizing various tailings and byproduct waste materials for backfilling is an important method for treating karst caves of abandoned mines and consuming a large amount of waste materials. In the prior art, chinese patent CN103130434A discloses a method for making a mine filling material by using bayer process red mud. The raw materials adopted are Bayer process red mud, fly ash, lime and gypsum, and the raw materials are uniformly mixed according to a certain weight percentage to form the mine filling material, wherein the amount of the Bayer process red mud and the amount of the fly ash respectively reach 40-60% and 15-25%, so that the application prospect is wide, but the problem of consumption of the Bayer process red mud can only be solved. Chinese patent CN102936121A discloses a composite material for mine roadway filling, which is prepared by mixing yellow phosphorus slag powder, an activator and a modifier according to the mass ratio of (19-22) to (10-17) to (1-4), adding 1-4 times of water by volume, and uniformly stirring to prepare slurry, wherein the amount of phosphogypsum used as the activator is small, and any one or more of sodium silicate, sodium fluosilicate, sodium hydroxide, sodium citrate, quicklime or slaked lime is required to be added as an additive. Therefore, the invention provides mine karst cave filling slurry and a preparation method thereof.
Disclosure of Invention
The invention provides the mine karst cave filling slurry and the preparation method thereof, which consume a large amount of red mud and phosphogypsum, and simultaneously provide the mine filling slurry which has the advantages of wide raw material source, low price, simple preparation method, low filling cost and good performance, thereby reducing the potential threat of the red mud and the phosphogypsum to the environment and having good economic and ecological benefits.
The invention provides mine karst cave filling slurry which is characterized by comprising the following raw materials in percentage by weight: 30-60% of red mud, 20-40% of phosphogypsum, 10-20% of fly ash, 5-10% of modifier and 2-4 times of water by volume.
Preferably, the red mud is one or a mixture of two or three of bayer process, sintering process or combination process red mud.
Preferably, the phosphogypsum is phosphogypsum dihydrate or phosphogypsum hemihydrate.
Preferably, the modifier is one or a mixture of two or three of lime, sodium silicate and cement.
The invention also provides a preparation method of the mine karst cave filling slurry, which is characterized by comprising the following steps:
step 1, weighing red mud, phosphogypsum and fly ash according to the formula, respectively grinding the red mud, the phosphogypsum and the fly ash into powder of 200 meshes, uniformly mixing, and then adding a modifier according to the formula to obtain raw slurry;
and 2, adding water with the formula amount into the raw slurry prepared in the step 1 to obtain the mine karst cave filling slurry.
Preferably, the viscosity of the mine filling slurry is 0.4-0.8 pa.s.
Compared with the prior art, the invention has the beneficial effects that:
(1) the red mud, the phosphogypsum, the fly ash and the modifier are used for preparing the mine cave filling slurry, and the phosphogypsum is acidic due to the fact that the phosphogypsum contains free sulfuric acid; the red mud is strong in alkalinity due to the fact that the red mud contains sodium hydroxide, and after the phosphogypsum is mixed with excessive red mud, acidity of the phosphogypsum is neutralized, and a substance with a gelling effect is generated; after the fly ash with certain activity is added, the phosphogypsum and the red mud are subjected to hydration reaction under the action of residual sodium hydroxide, modifier, salt and water to generate ettringite (AFt) and calcium silicate hydrate (C-S-H) gel. Along with the progress of hydration reaction, the ettringite and hydrated calcium silicate gel are continuously increased, and the strength of a hardened body is continuously improved; the modifier can promote and excite the gelation of the phosphogypsum, the red mud and the fly ash or the self-cementing material and has positive promotion effect on the early strength of the cementing material.
(2) The mine karst cave filling slurry prepared by the invention has stronger compressive strength, and the compressive strength can reach 1.3MPa, 2.1MPa and 3.5MPa respectively under the curing time of 7d, 14d and 28 d.
(3) The invention takes industrial waste residues such as red mud, phosphogypsum, fly ash and the like as main raw materials, under the action of a modifier, the main raw materials are activated to realize gelling and curing, and the novel mine cave filling cementing material is prepared; wide raw material sources, low production cost, simple process and convenient implementation and popularization.
Detailed Description
In order to make the technical solutions of the present invention better understood and enable those skilled in the art to practice the present invention, the following embodiments are further described, but the present invention is not limited to the following embodiments. The following experimental methods and detection methods are conventional methods unless otherwise specified, and the materials and reagents are commercially available.
Example 1
The mine karst cave filling slurry comprises the following components in percentage by weight: 30% of red mud, 40% of phosphogypsum, 20% of fly ash, 10% of modifier and 2 times of water by volume.
The preparation method of the mine karst cave filling slurry comprises the following steps:
step 1, weighing red mud, phosphogypsum and fly ash according to the formula, respectively grinding the red mud, the phosphogypsum and the fly ash into powder of 200 meshes, uniformly mixing, and then adding a modifier according to the formula to obtain raw slurry;
and 2, adding water with the formula amount into the raw slurry prepared in the step 1 to obtain the mine karst cave filling slurry.
Example 2
The mine karst cave filling slurry comprises the following components in percentage by weight: 60% of red mud, 20% of phosphogypsum, 10% of fly ash, 10% of modifier and 4 times of water by volume.
The preparation method of the mine karst cave filling slurry comprises the following steps:
step 1, weighing red mud, phosphogypsum and fly ash according to the formula, respectively grinding the red mud, the phosphogypsum and the fly ash into powder of 200 meshes, uniformly mixing, and then adding a modifier according to the formula to obtain raw slurry;
and 2, adding water with the formula amount into the raw slurry prepared in the step 1 to obtain the mine karst cave filling slurry.
Example 3
The mine karst cave filling slurry comprises the following components in percentage by weight: 50% of red mud, 25% of phosphogypsum, 15% of fly ash, 10% of modifier and 3 times of water by volume.
The preparation method of the mine karst cave filling slurry comprises the following steps:
step 1, weighing red mud, phosphogypsum and fly ash according to the formula, respectively grinding the red mud, the phosphogypsum and the fly ash into powder of 200 meshes, uniformly mixing, and then adding a modifier according to the formula to obtain raw slurry;
and 2, adding water with the formula amount into the raw slurry prepared in the step 1 to obtain the mine karst cave filling slurry.
Example 4
The mine karst cave filling slurry comprises the following components in percentage by weight: 40% of red mud, 40% of phosphogypsum, 15% of fly ash, 5% of modifier and 2 times of water by volume.
The preparation method of the mine karst cave filling slurry comprises the following steps:
step 1, weighing red mud, phosphogypsum and fly ash according to the formula, respectively grinding the red mud, the phosphogypsum and the fly ash into powder of 200 meshes, uniformly mixing, and then adding a modifier according to the formula to obtain raw slurry;
and 2, adding water with the formula amount into the raw slurry prepared in the step 1 to obtain the mine karst cave filling slurry.
Example 5
The mine karst cave filling slurry comprises the following components in percentage by weight: 60% of red mud, 20% of phosphogypsum, 15% of fly ash, 5% of modifier and 3 times of water by volume.
The preparation method of the mine karst cave filling slurry comprises the following steps:
step 1, weighing red mud, phosphogypsum and fly ash according to the formula, respectively grinding the red mud, the phosphogypsum and the fly ash into powder of 200 meshes, uniformly mixing, and then adding a modifier according to the formula to obtain raw slurry;
and 2, adding water with the formula amount into the raw slurry prepared in the step 1 to obtain the mine karst cave filling slurry.
Example 6
The mine karst cave filling slurry comprises the following components in percentage by weight: 60% of red mud, 25% of phosphogypsum, 10% of fly ash, 5% of modifier and 4 times of water by volume.
The preparation method of the mine karst cave filling slurry comprises the following steps:
step 1, weighing red mud, phosphogypsum and fly ash according to the formula, respectively grinding the red mud, the phosphogypsum and the fly ash into powder of 200 meshes, uniformly mixing, and then adding a modifier according to the formula to obtain raw slurry;
and 2, adding water with the formula amount into the raw slurry prepared in the step 1 to obtain the mine karst cave filling slurry.
The mine karst cave filling slurry prepared in the above examples 1 to 6 was filled in standard test molds of 70.7mm × 70.7mm × 70.7mm, respectively, cured in a constant temperature and humidity chamber (20 ± 2 ℃, humidity 60%) until demolding was possible, cured in a constant temperature and humidity chamber at a temperature of 20 ± 2 ℃ and a relative humidity of 95% or more for 7d, 14d, and 28d immediately after demolding, and the respective compressive strengths were measured and detected, and the results are shown in the following table 1:
TABLE 1 compressive Strength of mine cavern filling slurries prepared in examples 1 to 5
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.

Claims (6)

1. The mine karst cave filling slurry is characterized by comprising the following raw materials in percentage by weight: 30-60% of red mud, 20-40% of phosphogypsum, 10-20% of fly ash, 5-10% of modifier and 2-4 times of water by volume.
2. The mine karst cave filling slurry as claimed in claim 1, wherein the red mud is one or a mixture of two or three of Bayer process, sintering process or combination process red mud.
3. The mine cavern filling slurry as claimed in claim 1, wherein the phosphogypsum is dihydrate phosphogypsum or hemihydrate phosphogypsum.
4. The mine cavern filling slurry as recited in claim 1, wherein the modifier is one or a mixture of two or three of lime, sodium silicate and cement.
5. The preparation method of the mine cavern filling slurry as claimed in any one of claims 1 to 4, comprising the following steps:
step 1, weighing red mud, phosphogypsum and fly ash according to the formula, respectively grinding the red mud, the phosphogypsum and the fly ash into powder of 200 meshes, uniformly mixing, and then adding a modifier according to the formula to obtain raw slurry;
and 2, adding water with the formula amount into the raw slurry prepared in the step 1 to obtain the mine filling slurry.
6. The method for preparing the mine cavern filling slurry as recited in claim 5, wherein the viscosity of the mine cavern filling slurry is 0.4 to 0.8 pa.s.
CN202111405308.0A 2021-11-24 2021-11-24 Mine karst cave filling slurry and preparation method thereof Pending CN113880539A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114380518A (en) * 2022-01-25 2022-04-22 中国地质大学(武汉) Bayer process red mud-phosphogypsum baking-free cementing material and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104211313A (en) * 2014-07-02 2014-12-17 三峡大学 Phosphogypsum-based gelling material and its application in mine tailing filling
CN108947435A (en) * 2018-07-12 2018-12-07 昆明理工大学 A kind of filling in mine material and preparation method thereof of cooperative disposal mine heavy metal wastewater thereby
US20200231504A1 (en) * 2019-01-23 2020-07-23 Kunming University Of Science And Technology Method for synergistic stabilization/solidification of red mud and phosphogypsum
CN113061011A (en) * 2021-04-19 2021-07-02 贵州理工学院 Method for manufacturing red mud-modified phosphogypsum mine filling material

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104211313A (en) * 2014-07-02 2014-12-17 三峡大学 Phosphogypsum-based gelling material and its application in mine tailing filling
CN108947435A (en) * 2018-07-12 2018-12-07 昆明理工大学 A kind of filling in mine material and preparation method thereof of cooperative disposal mine heavy metal wastewater thereby
US20200231504A1 (en) * 2019-01-23 2020-07-23 Kunming University Of Science And Technology Method for synergistic stabilization/solidification of red mud and phosphogypsum
CN113061011A (en) * 2021-04-19 2021-07-02 贵州理工学院 Method for manufacturing red mud-modified phosphogypsum mine filling material

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114380518A (en) * 2022-01-25 2022-04-22 中国地质大学(武汉) Bayer process red mud-phosphogypsum baking-free cementing material and preparation method thereof

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