CN115108739A - Copper tailing geopolymer with high gelling activity and preparation method thereof - Google Patents
Copper tailing geopolymer with high gelling activity and preparation method thereof Download PDFInfo
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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
- C04B7/14—Cements containing slag
- C04B7/147—Metallurgical slag
- C04B7/153—Mixtures thereof with other inorganic cementitious materials or other activators
- C04B7/1535—Mixtures thereof with other inorganic cementitious materials or other activators with alkali metal containing activators, e.g. sodium hydroxide or waterglass
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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
- C04B12/00—Cements not provided for in groups C04B7/00 - C04B11/00
- C04B12/005—Geopolymer cements, e.g. reaction products of aluminosilicates with alkali metal hydroxides or silicates
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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
- C04B28/006—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 mineral polymers, e.g. geopolymers of the Davidovits type
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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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- 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
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- 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
A copper tailing geopolymer with high gelling activity and a preparation method thereof are disclosed, wherein the copper tailing geopolymer consists of silicon-aluminum powder and alkali-activated solution. The method adopts the steps that composite alkali materials are added to fully excite the depolymerization reaction of the glass phase in the copper tailing geopolymer; adding metakaolin, active slag powder and depolymerized oligomeric Si (OH) 4 And
the CS (A) H gel is generated by the polycondensation reaction, so that the resource utilization of the copper tailings, the mineral admixture and the alkaline residue solid waste is realized. The invention takes the industrial solid wastes such as copper tailings, slag powder, kaolin, caustic sludge and the like as main silicon-aluminum raw materials, realizes secondary resource utilization of the industrial solid wastes, changes waste into valuable, and effectively relieves the problem of industrial solid wastesThe problem of space resource waste and environmental pollution caused by stacking.
Description
Technical Field
The invention relates to a copper tailing geopolymer with high gelling activity and a preparation method thereof, belonging to the technical field of geopolymers.
Background
According to statistics, the production of each ton of cement clinker consumes about 1.2t of limestone, 0.3t of clay, 80kg of gypsum, 110kg of coal fuel and 110kWh of power resource, and 0.930t of CO is discharged 2 . The cement yield in China accounts for more than 50% of the total world yield, but the energy consumption of cement production units is far higher than the average world level, so that the resource consumption and carbon emission pressure in China are high. On the other hand, the copper tailings, the slag powder, the kaolin and other industrial solid wastes as auxiliary cementing materials can partially replace cement clinker, and can effectively reduce the resource consumption and CO in the cement production process 2 And (4) discharging the amount. The preparation of geopolymer by using industrial solid wastes such as copper tailings and the like as auxiliary cementing materials can effectively promote the low-carbon production and the large-volume comprehensive recycling process of the cement industry.
Around the preparation technology of tailings geopolymer, publication number CN108640547B discloses an iron tailings/metakaolin based geopolymer and a preparation method thereof, wherein the iron tailings, metakaolin and alkaline residue are adopted to prepare a geopolymer material, so that the problem of treatment of two solid wastes of the iron tailings and the alkaline residue is effectively solved. Publication No. CN111253097B discloses a preparation method of a geopolymer cementing material of molybdenum tailings, which adopts molybdenum tailings and fly ash to prepare geopolymer, and provides an effective way for the comprehensive utilization of the molybdenum tailings. Publication No. CN113666690A discloses a geopolymer solidified material based on manganese tailing base and a preparation method thereof, which utilizes cement, manganese tailing, a multi-metal polluted soil sample and alkali liquor to hydrate to generate geopolymer, so as to realize physical coating of heavy metals such as Pb, Zn and the like in soil. Publication No. CN111018417B discloses a method for preparing a geopolymer finished product by using Sichuan typical rare earth tailings, wherein the geopolymer finished product has high strength and less heavy metal leaching, and solves the problem of rare earth tailings pollution in Sichuan.
The existing preparation technology difficulty of the tailing geopolymer is that the gelling activity of the tailing is low, the activity is usually excited by adopting a method of mechanical grinding, chemical activation and high-temperature reconstruction, and currently, the research on the gelling activity of the copper tailing geopolymer is insufficient.
Disclosure of Invention
The invention aims to solve the problem of low gelling activity of a copper tailing geopolymer and provides a copper tailing geopolymer with high gelling activity and a preparation method thereof.
The technical scheme of the invention is that the depolymerization reaction of the glass phase in the copper tailing geopolymer is fully excited by adding the composite alkali material; adding metakaolin, active slag powder and depolymerized oligomeric Si (OH) 4 And Al (OH) - 4 Generates CS (A) H gel by polycondensation reaction, and realizes the resource utilization of copper tailings, mineral admixture and alkaline residue solid waste.
The invention relates to a copper tailing geopolymer with high gelling activity, which consists of silicon-aluminum powder and alkali-activated solution.
The silicon-aluminum powder comprises: 50-75 wt% of copper tailings, 10-30 wt% of metakaolin and 5-20 wt% of slag powder; the sum of the mass percent of the solid powder is 100 wt%;
the alkali-activated solution is a mixed solution of a composite alkali material, a water reducing agent and water, the content of the composite alkali material is 10-30 wt% of the silicon-aluminum powder, the mass concentration of the water reducing agent is 1-3 wt%, and the water-gel ratio is 0.25-0.35.
The specific surface area of the silicon-aluminum powder is 300m 2 More than 90 percent of particles with the particle diameter of less than 80 mu m are contained in the feed.
The composite alkali material is prepared by compounding water glass and sodium hydroxide, and the modulus of the obtained alkali-activated solution is 1.2-2.0.
The water reducing agent is a naphthalene series water reducing agent.
The reaction equation for depolymerization is:
[-Si-O-Si-]+OH - →Si(OH) 4
OH in solution - The Al-O-Al, Si-O-Al and Si-O-Si bridge oxygen in the raw materials are sequentially destroyed to connect high polymerization covalent bonds, and the aluminosilicate precursor is gradually dissolved in a high-alkaline environment, so that the glass phase in the copper tailings is subjected to depolymerization reaction.
Aluminotetrahedra formed by the depolymerization reaction
The copper tailings are negatively charged, and heavy metal ions are isolated in a cage-shaped crystal structure in geopolymer by balancing the heavy metal ions with positive charges in the copper tailings.
When the Si/Al ratio in the cementing material is between 1 and 3, the tetrahedral space structure is most reasonable, and the comprehensive performance is optimal. Al conditioning by adding metakaolin 2 O 3 To prepare a geopolymer.
The equation for the polycondensation reaction is as follows:
Si(OH) 4 +Ca 2+ →C-S-H+H 2 O
si (OH) of organic polymer-like monomer formed by depolymerization 4 、
With active Ca in solution + The polycondensation reaction is carried out to generate inorganic high polymer with a net structure, including CSH gel and CAH gel.
The calcium content in the copper tailings is low, the CSH gel and the CAH gel are correspondingly generated less, and the polycondensation reaction can be promoted by adding the slag powder, so that the strength of the geopolymer of the copper tailings is improved.
Preparation method of copper tailing geopolymer material with high gelling activity, and miningFully exciting depolymerization reaction of a glass phase in the copper tailing geopolymer by adding a composite alkali material; adding metakaolin, active slag powder and depolymerized oligomeric Si (OH) 4 And
performing polycondensation reaction to generate CS (A) H gel, thereby realizing resource utilization of copper tailings, mineral admixture and alkaline residue solid waste; the method comprises the following specific steps:
(1) drying, grinding and crushing undisturbed copper tailings to powder to obtain copper tailing powder;
(2) weighing the copper tailing powder, the metakaolin and the slag powder in the step (1) according to the proportion, mechanically stirring for 60s, and uniformly mixing to obtain the alumino-silica powder;
(3) uniformly mixing a composite alkali material, a water reducing agent and water to prepare an alkali-activated solution;
(4) uniformly mixing the silicon-aluminum powder obtained in the step (2) with the alkali-activated solution obtained in the step (3) to obtain geopolymer slurry;
(5) and (4) filling the geopolymer slurry obtained in the step (4) into a standard die, forming by using a vibrating table or a vibrating table, curing in a curing box for 24 hours, demolding, and curing the test block to a specified age under standard curing conditions to obtain the copper tailing geopolymer.
The method has the advantages that industrial solid wastes such as copper tailings, slag powder, kaolin, caustic sludge and the like are used as main silicon-aluminum raw materials, secondary resource utilization of the industrial solid wastes is realized, waste is changed into valuable, and the problems of space resource waste and environmental pollution caused by industrial solid waste stockpiling are effectively solved. The copper tailings are used as main silicon-aluminum raw materials, and the slag powder, the kaolin and the caustic sludge are used as auxiliary raw materials to prepare the copper tailings geopolymer with high gelling activity, high-temperature calcination is not needed, and the preparation method has the advantages of simple preparation process, low energy consumption, small environmental pollution and the like, and is favorable for low-carbon popularization and application in the cement industry. Harmful heavy metal elements such as sulfur, arsenic, cadmium and the like are often associated in copper tailings, and the geopolymer prepared by the invention has negatively charged aluminoxy tetrahedron
The metal ions can be effectively balanced, the heavy metal ions are isolated in the cage-shaped crystal structure of the geopolymer, and the harmless utilization of the copper tailings can be realized.
Drawings
FIG. 1 is a process flow of the polymerization reaction of the geopolymer of the copper tailings with high gelling activity of the invention.
Detailed Description
A specific embodiment of the present invention is shown in fig. 1.
Example 1
The embodiment provides a copper tailing geopolymer material, which is prepared by the following steps:
(1) drying, grinding and crushing the copper tailing sample in an oven with the set temperature of 65 ℃ to obtain copper tailing powder, drying the slag powder and the metakaolin, and sieving the powdery raw materials through a 150-mesh standard sieve to obtain a test sample.
(2) Pouring the test sample obtained in the step (1) into a cement paste mixer according to the mass parts, stirring for 60s, and uniformly mixing to obtain the silicon-aluminum powder. Wherein, the copper tailings in the silicon-aluminum powder: metakaolin: the mass ratio of the slag powder is 60:25: 15.
(3) Weighing the composite alkali material, the naphthalene water reducer and the water according to the parts by weight, pouring the mixture into an alkali-resistant plastic container, and uniformly mixing to prepare the alkali-activated solution. The composite alkali material is prepared by compounding water glass and sodium hydroxide, the modulus is 1.7, the mixing amount is 20 wt%, the mixing amount of the naphthalene water reducing agent is 1.5 wt%, and the water-glue ratio is 0.30.
(4) And (3) pouring the silicon-aluminum powder in the step (2) and the alkali-activated solution in the step (3) into a stirring pot in sequence, stirring by using a cement paste mixer, selecting a manual stirring mode, stirring at a low speed for 120s at a stirring speed of 150r/min, stopping stirring for 15s, stirring at a high speed for 120s at a stirring speed of 290r/min, and stopping stirring. To obtain a geopolymer slurry.
(5) And (3) filling the geopolymer slurry obtained in the step (4) into a standard square die with the size of 20mm multiplied by 20mm, clamping the test die on a vibration table, and vibrating for 120s +/-5 s to stop the machine. And (4) curing for 24 hours in a standard curing room, then demolding, and then continuing standard curing to the specified age to obtain the copper tailing geopolymer. The standard curing conditions are a temperature of 20 +/-2 ℃ and a relative humidity of more than 95% RH.
The compressive strength of the copper tailing geopolymer 3d and 28d is tested by referring to the national standard GB/T17671-1999. The results show that: the unconfined compressive strength of 3d is 12.5MPa, the unconfined compressive strength of 28d is 30.7MPa, and the strength reaches the 32.5 grade requirement of composite portland cement in general portland cement (GB 175-2007).
Example 2
The embodiment provides a copper tailing geopolymer material, which is prepared by the following steps:
(1) drying, grinding and crushing the copper tailing sample in an oven with the set temperature of 65 ℃ to obtain copper tailing powder, drying the slag powder and the metakaolin, and sieving the powdery raw materials through a 150-mesh standard sieve to obtain a test sample.
(2) Pouring the test sample obtained in the step (1) into a cement paste mixer according to the mass parts, stirring for 60s, and uniformly mixing to obtain the silicon-aluminum powder. Wherein, the copper tailings in the silicon-aluminum powder: metakaolin: the mass ratio of the slag powder is 50:30: 20.
(3) Weighing the composite alkali material, the naphthalene water reducer and the water according to the parts by weight, pouring the mixture into an alkali-resistant plastic container, and uniformly mixing to prepare the alkali-activated solution. The composite alkali material is prepared by compounding water glass and sodium hydroxide, the modulus is 1.7, the mixing amount is 15 wt%, the mixing amount of the naphthalene water reducing agent is 1.5 wt%, and the water-glue ratio is 0.30.
(4) And (3) pouring the silicon-aluminum powder in the step (2) and the alkali-activated solution in the step (3) into a stirring pot in sequence, stirring by using a cement paste mixer, selecting a manual stirring mode, stirring at a low speed for 120s at a stirring speed of 150r/min, stopping stirring for 15s, stirring at a high speed for 120s at a stirring speed of 290r/min, and stopping stirring. To obtain a geopolymer slurry.
(5) And (3) filling the geopolymer slurry obtained in the step (4) into a standard square die with the size of 20mm multiplied by 20mm, clamping the test die on a vibration table, and vibrating for 120s +/-5 s to stop the machine. And (4) demolding after curing in a standard curing room for 24 hours, and then continuing standard curing to a specified age after demolding to obtain the copper tailing geopolymer. The standard curing conditions are a temperature of 20 +/-2 ℃ and a relative humidity of more than 95% RH.
The compressive strength of the copper tailing geopolymer 3d and 28d is tested by referring to the national standard GB/T17671-1999. The results show that: the unconfined compressive strength of 3d is 15.7MPa, the unconfined compressive strength of 28d is 35.3MPa, and the strength reaches the 32.5 grade requirement of composite portland cement in general portland cement (GB 175-2007).
Example 3
The embodiment provides a copper tailing geopolymer material, which is prepared by the following steps:
(1) drying, grinding and crushing the copper tailing sample in an oven with the set temperature of 65 ℃ to obtain copper tailing powder, drying the slag powder and the metakaolin, and sieving the powdery raw materials through a 150-mesh standard sieve to obtain a test sample.
(2) Pouring the test sample obtained in the step (1) into a cement paste mixer according to the mass parts, stirring for 60s, and uniformly mixing to obtain the silicon-aluminum powder. Wherein, the copper tailings in the silicon-aluminum powder: metakaolin: the mass ratio of the slag powder is 65:25: 10.
(3) Weighing the composite alkali material, the naphthalene water reducer and the water according to the parts by weight, pouring the mixture into an alkali-resistant plastic container, and uniformly mixing to prepare the alkali-activated solution. The composite alkali material is prepared by compounding water glass and sodium hydroxide, the modulus is 1.7, the doping amount is 20 wt%, the doping amount of the naphthalene water reducing agent is 1.5 wt%, and the water-to-glue ratio is 0.30.
(4) And (3) pouring the silicon-aluminum powder in the step (2) and the alkali-activated solution in the step (3) into a stirring pot in sequence, stirring by using a cement paste mixer, selecting a manual stirring mode, stirring at a low speed for 120s at a stirring speed of 150r/min, stopping stirring for 15s, stirring at a high speed for 120s at a stirring speed of 290r/min, and stopping stirring. To obtain a geopolymer slurry.
(5) And (3) filling the geopolymer slurry obtained in the step (4) into a standard square die with the size of 20mm multiplied by 20mm, clamping the test die on a vibration table, and vibrating for 120s +/-5 s to stop the machine. And (4) demolding after curing in a standard curing room for 24 hours, and then continuing standard curing to a specified age after demolding to obtain the copper tailing geopolymer. The standard curing conditions are a temperature of 20 +/-2 ℃ and a relative humidity of more than 95% RH.
The compressive strength of the copper tailing geopolymer 3d and 28d is tested by referring to the national standard GB/T17671-1999. The results show that: the unconfined compressive strength of 3d is 11.6MPa, the unconfined compressive strength of 28d is 28.9MPa, and the strength reaches the 32.5 grade requirement of composite portland cement in general portland cement (GB 175-2007).
The present embodiments are merely illustrative of the present application and it will be apparent to those skilled in the art that several equivalent substitutions or obvious modifications can be made without departing from the spirit of the invention and the scope of the invention is to be determined from the claims as filed.
Claims (8)
1. The copper tailing geopolymer material with high gelling activity is characterized in that the copper tailing geopolymer with high gelling activity is formed by exciting potential activity of silicon-aluminum powder under an alkaline environment to generate dissolution-depolymerization-polycondensation reaction to generate a copper tailing geopolymer;
the copper tailing geopolymer material consists of silicon-aluminum powder and alkali-activated solution;
the silicon-aluminum powder comprises: 50-75 wt% of copper tailings, 10-30 wt% of metakaolin and 5-20 wt% of slag powder; the sum of the mass percent of the solid powder is 100 wt%;
the alkali-activated solution is a mixed solution of a composite alkali material, a water reducing agent and water, the content of the composite alkali material is 10-30 wt% of the silicon-aluminum powder, the mass concentration of the water reducing agent is 1-3 wt%, and the water-gel ratio is 0.25-0.35.
2. The copper tailing geopolymer material with high gelling activity as claimed in claim 1, wherein the specific surface area of the silica-alumina powder is 300m 2 More than 90% of particles with the particle diameter of less than 80 mu m are contained in the granules per kg.
3. The high-gelling-activity copper tailing geopolymer material as claimed in claim 1, wherein the composite alkali material is prepared by compounding water glass and sodium hydroxide, and the modulus of the obtained alkali-activated solution is 1.2-2.0.
4. The copper tailing geopolymer material with high gelling activity as claimed in claim 1, wherein the water reducing agent is a naphthalene series water reducing agent.
5. The high-gelling-activity copper tailing geopolymer material as claimed in claim 1, wherein the depolymerization reaction equation is as follows:
[-Si-O-Si-]+OH-→Si(OH) 4
OH in solution - The Al-O-Al, Si-O-Al and Si-O-Si bridge oxygen in the raw materials are sequentially destroyed to connect high polymerization covalent bonds, and the aluminosilicate precursor is gradually dissolved in a high-alkaline environment, so that the glass phase in the copper tailings is subjected to depolymerization reaction.
6. The high-gelling-activity copper tailing geopolymer material as claimed in claim 1, wherein the formula of the polycondensation reaction is as follows:
Si(OH) 4 +Ca 2+ →C-S-H+H 2 O
si (OH) of organic polymer-like monomer produced by depolymerization reaction 4 、Al(OH) - 4 With active Ca in solution + The polycondensation reaction is carried out to generate inorganic high polymer with a net structure, including CSH gel and CAH gel.
7. The method for preparing the geopolymer material with high gelling activity of copper tailings according to any one of claims 1 to 6, wherein the method adopts additionThe composite alkali material fully excites the depolymerization reaction of the glass phase in the copper tailing geopolymer; adding metakaolin, active slag powder and depolymerized oligomeric Si (OH) 4 And Al (OH) - 4 Performing polycondensation reaction to generate CS (A) H gel, thereby realizing resource utilization of copper tailings, mineral admixture and alkaline residue solid waste; the method comprises the following specific steps:
(1) drying, grinding and crushing undisturbed copper tailings to powder to obtain copper tailing powder;
(2) weighing the copper tailing powder, the metakaolin and the slag powder in the step (1) according to the proportion, mechanically stirring for 60s, and uniformly mixing to obtain the alumino-silica powder;
(3) uniformly mixing a composite alkali material, a water reducing agent and water to prepare an alkali-activated solution;
(4) uniformly mixing the silicon-aluminum powder obtained in the step (2) with the alkali-activated solution obtained in the step (3) to obtain geopolymer slurry;
(5) and (4) filling the geopolymer slurry obtained in the step (4) into a standard die, forming by using a vibrating table or a vibrating table, curing in a curing box for 24 hours, demolding, and curing the test block to a specified age under standard curing conditions to obtain the copper tailing geopolymer.
8. The geopolymer material with high gelling activity as claimed in claim 5, wherein the aluminoxy tetrahedron is formed by depolymerization reaction
The copper tailings are negatively charged, and heavy metal ions are isolated in a cage-shaped crystal structure in geopolymer by balancing the heavy metal ions with positive charges in the copper tailings.
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| CN116444215A (en) * | 2023-04-24 | 2023-07-18 | 东南大学 | Copper tailing-slag-based geopolymer for rigid concrete pavement and preparation process thereof |
| CN118307253A (en) * | 2024-04-09 | 2024-07-09 | 江苏海洋大学 | Preparation method of alkaline residue-fly ash base polymer cementing material |
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| CN118307253A (en) * | 2024-04-09 | 2024-07-09 | 江苏海洋大学 | Preparation method of alkaline residue-fly ash base polymer cementing material |
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