CN110981405A - Method for preparing novel inorganic polymeric material by using tailings - Google Patents
Method for preparing novel inorganic polymeric material by using tailings Download PDFInfo
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- CN110981405A CN110981405A CN202010005647.9A CN202010005647A CN110981405A CN 110981405 A CN110981405 A CN 110981405A CN 202010005647 A CN202010005647 A CN 202010005647A CN 110981405 A CN110981405 A CN 110981405A
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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
- C04B28/24—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 alkyl, ammonium or metal silicates; containing silica sols
- C04B28/26—Silicates of the alkali metals
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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
- 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
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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
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
- C04B20/02—Treatment
- C04B20/04—Heat treatment
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—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
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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
- 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
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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
- 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
Abstract
The invention discloses a method for preparing a novel inorganic polymeric material by using tailings. The invention uses copper mine tailings with high content of dickite in Fujian certain mine as raw materials, the copper mine tailings are calcined after reacting with potassium acetate, an alkali activator and water are added to perform in-situ polymerization reaction, and a novel inorganic polymeric material with the compressive strength of 8.5 MPa is prepared after maintenance, so that comprehensive utilization of resources is achieved.
Description
Technical Field
The invention belongs to the field of comprehensive utilization of copper ore tailings in a recycling manner, and particularly relates to a method for preparing a novel inorganic polymeric material by using copper ore tailings rich in dickite.
Background
The inorganic polymeric material is a material made of AlO4And SiO4The tetrahedral structure unit forms an inorganic polymer with a three-dimensional network structure. The inorganic non-metal material is produced by using burnt clay (metakaolin) or other silicon-aluminum mineral material with aluminum, silicon and oxygen as main elements as material and through normal temperature condensation polymerization under the excitation of alkali metal ion and other excitant. The material has excellent mechanical property, acid and alkali resistance, fire resistance and high temperature resistance, and is widely applied to the fields of building materials, high-strength materials, solid core and solid waste materials, sealing materials, high temperature resistant materials and the like. There are two main methods for the preparation of inorganic polymeric materials: one is inorganic polymer material synthesized at low temperature with silicate mineral under the excitation condition of strong alkali and sodium silicate. And the other method is to prepare the metakaolin into the aluminosilicate polymer material at room temperature by taking phosphoric acid solution as an exciting agent.
In the preparation of inorganic polymeric materials, metakaolinite, one of the raw materials, is typically calcined from kaolinite. Dickite and kaolinite have the same chemical composition and are formed by stacking silicon-oxygen tetrahedron and aluminum-oxygen octahedron, and the difference of structures lies in the stacking sequence of unit layers and the arrangement mode of octahedral vacancy is different. Previous studies have shown that, after calcination, dickite can also produce a metakaolite with the same structure as metakaolin, but no report on the use of metakaolite in the preparation of inorganic polymeric materials is found. After the dickite is intercalated with the potassium acetate, the interlayer disturbance is generated, so that the dehydroxylation temperature is reduced, the phase change temperature of the dickite transformed into the metadickite is reduced, and the energy is saved.
The tailings of Fujian copper ore mainly comprise dickite, alunite, quartz and other non-metallic minerals. The dickite contains Al and Si elements, the alunite contains Al elements, the quartz contains Si elements, and minerals in tailings are natural raw materials for preparing novel inorganic polymeric materials. The invention takes copper mine tailings with high content of Fujian landite as raw materials, adds potassium acetate to react and calcine, adds alkali activator to react, and prepares novel inorganic polymeric material after maintenance. The technology is low in energy consumption and environment-friendly, the preparation method is selected to prepare the inorganic polymer material suitable for goaf filling, the production cost is reduced, the storage capacity of the copper ore tailings can be reduced, a new way is provided for comprehensive utilization of tailing resources, a foundation is laid for further development of a mining area, and therefore full utilization and sustainable development of resources are achieved, and the method has very important theoretical and practical significance. At present, the country advocates the green mine construction vigorously, and requires coordination with the surrounding environment when developing and utilizing the mine, and gives restoration treatment or transformation innovation to the inevitable pollution, mine geological disasters and the like. Therefore, the comprehensive application research of the copper mine tailings with high content of the open rocks in Fujian province has an epoch background.
Disclosure of Invention
The invention aims to provide a novel inorganic polymeric material which is prepared by taking copper ore tailings with high content of some ore as a raw material, adding potassium acetate solution for reaction, calcining, adding alkali activator for reaction and maintaining, wherein the copper ore tailings are simple, efficient, energy-saving and economical. The method has the advantages of rich raw material sources, high resource utilization rate, simple and efficient process flow, reduction of the storage capacity of the tailing pond while comprehensive resource utilization of the tailings, economy, practicability and environmental protection.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing a novel inorganic polymeric material by using tailings comprises the following specific steps:
(1) drying and grinding the copper ore tailings rich in dickite, and then sieving the copper ore tailings with a 100-mesh sieve to obtain an initial raw material for preparing the inorganic polymeric material;
(2) mixing the initial raw material obtained in the step (1) with potassium acetate, adding water, stirring for 30 min, standing for reaction for 24h, naturally drying, and calcining the reactant in a muffle furnace;
(3) dissolving an alkali activator in water, adding the calcined product obtained in the step (2), mechanically stirring for 30 min, injecting into a mold, stirring for 10 min, stirring, vibrating, tamping to discharge redundant bubbles, covering a layer of preservative film, and standing for 24 h;
(4) and (3) demolding, and curing the demolded sample at 20 ℃ and 95% humidity for 28 d to obtain the novel inorganic polymer material with the compressive strength of 8.5 MPa.
Further, the mass ratio of the initial raw material and the potassium acetate in the step (2) is 5: 1.
further, the calcination temperature in the step (2) is 500-800 ℃, and the calcination time is 2-5 h.
Further, the alkali activator in the step (3) is a mixture of water glass and sodium hydroxide in a mass ratio of 3: 1.
Further, the mass ratio of the alkali-activator in the step (3) to the potassium acetate in the step (2) is 0.8: 1.
The copper ore tailings mainly comprise dickite, alunite, quartz and other non-metallic minerals, wherein the dickite content in the tailings reaches about 40%, and the tailings minerals contain Al and Si elements, so that the copper ore tailings are natural raw materials for preparing novel inorganic polymeric materials.
The novel inorganic polymeric material prepared by the method has the compressive strength of 8.5 MPa, and meets the strength requirement of the mine goaf filling material.
The invention has the following remarkable advantages:
(1) the invention uses copper ore tailings with high content of some open rocks as main raw materials, has low energy consumption and is green and environment-friendly, and an appropriate preparation method is selected to prepare the inorganic polymeric material;
(2) the invention provides a new way for the comprehensive utilization of copper ore tailing resources, and the invention can greatly reduce the storage capacity of a tailing pond, thereby realizing the full utilization and sustainable development of resources;
(3) the preparation process of the invention does not need high-temperature treatment, and the filling material synthesized at room temperature has high compressive strength;
(4) the preparation process is simple in flow, easy to operate, capable of realizing large-scale production and convenient to popularize.
Drawings
FIG. 1 is an X-ray diffraction pattern of the starting material and the novel inorganic polymeric material prepared by the different steps of example 1;
FIG. 2 is a scanning electron micrograph of the tailings (a) of example 1 and the prepared novel inorganic polymeric material (b).
Detailed Description
In order to make the present invention more comprehensible, the technical solutions of the present invention are further described below with reference to specific embodiments, but the present invention is not limited thereto.
Example 1
A method for preparing a novel inorganic polymeric material by using tailings comprises the following specific steps:
(1) drying the copper ore tailings, simply grinding the copper ore tailings, and then sieving the copper ore tailings with a 100-mesh sieve to obtain an initial raw material for preparing the novel inorganic polymeric material.
(2) Mixing 1 Kg of initial raw material and 0.2 Kg of potassium acetate, adding 150 ml of water, stirring for 30 min, standing for reaction for 24h, and naturally drying; placing the reactant in a muffle furnace, and calcining for 3 h at 500 ℃;
(3) putting alkali activator (0.6 Kg of water glass and 0.2 Kg of sodium hydroxide) and 200ml of distilled water into a beaker, uniformly mixing, treating 1 Kg of potassium acetate and adding a calcined product into the beaker, mechanically stirring for 30 min, injecting the mixture into a cylindrical die with the diameter of 6 cm and the height of 3cm, and stirring for 10 min; stirring, vibrating and tamping to discharge redundant bubbles, covering a layer of preservative film, demoulding after 24h, and curing the demoulded sample at 20 ℃ under the condition of 95% humidity for 28 d to obtain the novel inorganic polymeric material with the compressive strength of 8.5 MPa.
FIG. 1 shows X-ray diffraction patterns of a novel inorganic polymeric material, which is a product obtained by intercalating and modifying tailings of copper mine and potassium acetate in tailings, and a product obtained by intercalating and calcining potassium acetate in tailings. The novel inorganic polymer material prepared by adding the alkali activator for reaction can only see the diffraction peak of quartz.
FIG. 2 (a) is a scanning electron micrograph of the tailings, and FIG. 2 (b) is a scanning electron micrograph of the novel inorganic polymeric material prepared in example 1. The minerals in the tailings are loosely stacked, the quartz in the inorganic polymeric material reacts with the alkali activator and is cemented into a flocculent shape and a network shape, the structure is uniform and compact, the void structure is less, and the compressive strength of the sample is improved because the gel phase content endowing the sample with the strength performance is gradually increased.
Example 2
A method for preparing a novel inorganic polymeric material by using tailings comprises the following specific steps:
(1) drying the copper ore tailings, simply grinding the copper ore tailings, and then sieving the copper ore tailings with a 100-mesh sieve to obtain an initial raw material for preparing the novel inorganic polymeric material.
(2) Mixing 1 Kg of initial raw material and 0.2 Kg of potassium acetate, adding 150 ml of water, stirring for 30 min, standing for reaction for 24h, and naturally drying; putting the reactant of the tailings and the potassium acetate into a muffle furnace, and calcining for 2 hours at 600 ℃;
(3) putting alkali activator (0.6 Kg of water glass and 0.2 Kg of sodium hydroxide) and 200ml of distilled water into a beaker, uniformly mixing, treating 1 Kg of potassium acetate and adding a calcined product into the beaker, mechanically stirring for 30 min, injecting the mixture into a cylindrical die with the diameter of 6 cm and the height of 3cm, and stirring for 10 min; stirring, vibrating and tamping to discharge redundant bubbles, covering a layer of preservative film, demoulding after 24h, and curing the demoulded sample at 20 ℃ under the condition of 95% humidity for 28 d to obtain the novel inorganic polymeric material with the compressive strength of 7.8 MPa.
Example 3
A method for preparing a novel inorganic polymeric material by using tailings comprises the following specific steps:
(1) and drying the copper ore tailings, simply grinding the copper ore tailings, and then sieving the copper ore tailings with a 100-mesh sieve to obtain the initial raw material for preparing the inorganic polymeric material.
(2) Mixing 1 Kg of initial raw material and 0.5 Kg of potassium acetate, adding 150 ml of water, stirring for 30 min, standing for reaction for 24h, and naturally drying; putting the tailings and potassium acetate reactants into a muffle furnace, and calcining for 2 hours at 700 ℃;
(3) putting alkali activator (0.6 Kg of water glass and 0.2 Kg of sodium hydroxide) and 200ml of distilled water into a beaker, uniformly mixing, treating 1 Kg of potassium acetate and adding a calcined product into the beaker, mechanically stirring for 30 min, injecting the mixture into a cylindrical die with the diameter of 6 cm and the height of 3cm, and stirring for 10 min; stirring, vibrating and tamping to discharge redundant bubbles, covering a layer of preservative film, demoulding after 24h, and curing the demoulded sample at 20 ℃ under the condition of 95% humidity for 28 d to obtain the novel inorganic polymeric material with the compressive strength of 7.3 MPa.
Example 4
A method for preparing a novel inorganic polymeric material by using tailings comprises the following specific steps:
(1) and drying the copper ore tailings, simply grinding the copper ore tailings, and then sieving the copper ore tailings with a 100-mesh sieve to obtain the initial raw material for preparing the inorganic polymeric material.
(2) Mixing 1 Kg of initial raw material with 0.5 Kg of potassium acetate, adding 150 ml of water, stirring for 30 min, standing for 24h, and naturally drying; putting the reactant of the tailings and the potassium acetate into a muffle furnace, and calcining for 2 hours at 800 ℃;
(3) putting alkali activator (0.6 Kg of water glass and 0.2 Kg of sodium hydroxide) and 200ml of distilled water into a beaker, uniformly mixing, treating 1 Kg of potassium acetate and adding a calcined product into the beaker, mechanically stirring for 30 min, injecting the mixture into a cylindrical die with the diameter of 6 cm and the height of 3cm, and stirring for 10 min; stirring, vibrating and tamping to discharge redundant bubbles, covering a layer of preservative film, demoulding after 24h, and curing the demoulded sample at 20 ℃ under the condition of 95% humidity for 28 d to obtain the novel inorganic polymeric material with the compressive strength of 8.1 MPa.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (6)
1. A method for preparing novel inorganic polymeric material by using tailings is characterized by comprising the following steps: the method comprises the following steps:
(1) drying and grinding the copper ore tailings rich in dickite, and then sieving the copper ore tailings with a 100-mesh sieve to obtain an initial raw material for preparing the inorganic polymeric material;
(2) mixing the initial raw material obtained in the step (1) with potassium acetate, adding water, stirring for 30 min, standing for reaction for 24h, naturally drying, and calcining the reactant in a muffle furnace;
(3) dissolving an alkali activator in water, adding the calcined product obtained in the step (2), mechanically stirring for 30 min, injecting into a mold, stirring for 10 min, stirring, vibrating, tamping to discharge redundant bubbles, covering a layer of preservative film, and standing for 24 h;
(4) and (3) demolding, and curing the demolded sample at 20 ℃ and 95% humidity for 28 d to obtain the novel inorganic polymer material with the compressive strength of 8.5 MPa.
2. The method for preparing novel inorganic polymeric material using the mine tailings as claimed in claim 1, wherein: the mass ratio of the initial raw materials in the step (2) to the potassium acetate is 5: 1.
3. the method for preparing novel inorganic polymeric material using the mine tailings as claimed in claim 1, wherein: the calcination temperature in the step (2) is 500-800 ℃, and the calcination time is 2-5 h.
4. The method for preparing novel inorganic polymeric material using the mine tailings as claimed in claim 1, wherein: the alkali activator in the step (3) is a mixture of water glass and sodium hydroxide in a mass ratio of 3: 1.
5. The method for preparing novel inorganic polymeric material using the mine tailings as claimed in claim 1, wherein: the mass ratio of the alkali activator in the step (3) to the potassium acetate in the step (2) is 0.8: 1.
6. A novel inorganic polymeric material obtainable by the process according to any one of claims 1 to 5, wherein: the novel inorganic polymeric material has a compressive strength of 8.5 MPa and is used for filling materials and building materials.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116177988A (en) * | 2022-12-28 | 2023-05-30 | 北京科技大学 | Heat accumulating brick and preparation method and application thereof |
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|---|---|---|---|---|
| CN103613296A (en) * | 2013-12-04 | 2014-03-05 | 重庆大学 | Method for preparing alkali-activated gel material by use of low-temperature calcined intercalated kaolin |
| WO2016135347A1 (en) * | 2015-02-27 | 2016-09-01 | Imerys Ceramics France | Particulate compositions for the formation of geopolymers, their use and methods for forming geopolymers therewith, and geopolymers obtained therefrom |
| CN109209486A (en) * | 2018-11-06 | 2019-01-15 | 福州大学 | A method of Goaf Area filler is prepared using copper mining tailing |
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2020
- 2020-01-03 CN CN202010005647.9A patent/CN110981405A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103613296A (en) * | 2013-12-04 | 2014-03-05 | 重庆大学 | Method for preparing alkali-activated gel material by use of low-temperature calcined intercalated kaolin |
| WO2016135347A1 (en) * | 2015-02-27 | 2016-09-01 | Imerys Ceramics France | Particulate compositions for the formation of geopolymers, their use and methods for forming geopolymers therewith, and geopolymers obtained therefrom |
| CN109209486A (en) * | 2018-11-06 | 2019-01-15 | 福州大学 | A method of Goaf Area filler is prepared using copper mining tailing |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116177988A (en) * | 2022-12-28 | 2023-05-30 | 北京科技大学 | Heat accumulating brick and preparation method and application thereof |
| CN116177988B (en) * | 2022-12-28 | 2024-04-16 | 北京科技大学 | Heat accumulating brick and preparation method and application thereof |
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