CN113087419B - Preparation method of manganese slag-phosphorus slag-nickel iron slag composite alkali-activated cementing material - Google Patents
Preparation method of manganese slag-phosphorus slag-nickel iron slag composite alkali-activated cementing material Download PDFInfo
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- CN113087419B CN113087419B CN202110458700.5A CN202110458700A CN113087419B CN 113087419 B CN113087419 B CN 113087419B CN 202110458700 A CN202110458700 A CN 202110458700A CN 113087419 B CN113087419 B CN 113087419B
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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
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/10—Production of cement, e.g. improving or optimising the production methods; Cement grinding
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Abstract
The invention discloses a preparation method of a manganese slag-phosphorus slag-nickel iron slag composite alkali-activated cementing material, which comprises 3-8% of calcium hydroxide, 30-50% of manganese slag, 10-20% of phosphorus slag and 40-55% of nickel iron slag by mass. The composite alkali-activated cementing material simultaneously adopts industrial solid wastes such as manganese slag, phosphorus slag, nickel-iron slag and the like to prepare the composite cementing material, so that waste is changed into valuable, and the prepared composite cementing material has high strength, short setting time, simple preparation process, low cost and wide raw material source.
Description
Technical Field
The invention relates to the field of comprehensive utilization of building materials and industrial waste resources, in particular to a preparation method of a manganese slag-phosphorus slag-nickel iron slag composite alkali-activated cementing material.
Background
One of the important significances that alkali-activated cementitious materials deserves intensive research is their potential to replace part of the cement as a new building material. The alkali-activated cementing material does not need to be calcined at high temperature, which means that a large amount of energy is not consumed for preparing the alkali-activated cementing material, and a large amount of CO is not generated2And other toxic gases, and many of the raw materials of the alkali-activated cement are industrial byproducts, so that the influence of the preparation of the alkali-activated cement on the environment is greatly reduced compared with that of ordinary portland cement, and the method is also helpful for solving the problems of the existing industrial waste residue treatment and the existing industrial waste residue treatmentThe problem of utilization. In the prior art, researchers and researchers have conducted many studies on commonly used alkali-activated materials.
CN103351105A relates to an alkali-activated cementing material and a preparation method thereof, the alkali-activated cementing material provided by the invention takes calcium silicate slag as a main raw material and liquid water glass as an activator, and can be prepared under the condition of normal temperature without high-temperature calcination, and the formula of the raw material comprises the following components in percentage by mass: 70 percent of calcium silicate slag micro powder, 15 to 25 percent of mineral powder, 5 to 15 percent of superfine mineral powder and Na2Water glass (Na) with O content of 1-5% of powder weight2O·nSiO2The modulus n is 2.00 to 3.00). Compared with the prior art, the invention takes the calcium silicate slag as the main raw material, has low material production cost and low resource and energy consumption, embodies the concepts of environmental protection and circular economy, and has wide market application prospect.
CN104446045A relates to an alkali-activated cementing material prepared by utilizing siliceous iron tailings and a preparation method thereof, and the method comprises the following steps: 1) uniformly mixing siliceous iron tailing powder, fly ash and slag powder according to a ratio to obtain iron tailing powder-fly ash-slag powder composite powder; 2) mixing liquid water glass and water to prepare an alkali activator solution; 3) adding the alkali activator solution into the composite powder, and uniformly stirring to obtain alkali-activated cementing material slurry; 4) injecting the alkali-activated cementing material slurry into a mold for vibration molding, and maintaining at normal temperature until demolding is carried out, thereby obtaining an alkali-activated cementing material neat slurry test piece; 5) and (4) steaming the alkali-activated gelled material neat paste test piece. The invention has the beneficial effects that: the alkali-activated cementing material hardening slurry provided by the invention has excellent mechanical properties. The composite powder comprises 50-75% of siliceous iron tailing powder, 0-45% of fly ash and 5-50% of slag powder by mass, and also comprises liquid sodium silicate accounting for 5-15% of the weight of the composite powder and water accounting for 15-30% of the weight of the composite powder; the siliceous iron tailing powder is obtained by grinding crude ore of siliceous iron tailing to the specific surface area of 300m2/kg～600m2/kg。
At present, alkali-activated materials in the prior art are basically limited to conventional inorganic mineral powder and fly ash raw materials, the types of the raw materials are limited, and the absolute strength of slurry materials obtained after the alkali-activated materials are excited is limited. Therefore, it is highly desirable to develop a method,
disclosure of Invention
In view of the above, the invention provides a preparation method of a cementing material with manganese slag and nickel-iron slag as main components, and aims to solve the problems of environmental pollution and resource waste caused by electrolytic waste slag in the prior art and solve the problem of insufficient strength of the cementing material formed by a conventional fly ash alkali-activated material.
The ferronickel slag is a byproduct generated during ferronickel alloy smelting and purification, and is generally obtained by high-temperature melting and then quenching because the smelting temperature of metal is very high. According to statistics, the mass ratio of the electric furnace nickel-iron slag and the correspondingly produced nickel-iron alloy in China reaches 14:1, so that a large amount of electric furnace nickel-iron slag is discharged when the nickel-iron is extracted by adopting a high-temperature smelting method, the nickel-iron slag becomes one of main industrial waste slag discharged in China, and how to carry out scientific and environment-friendly treatment on the large-scale discharged nickel-iron slag is still a big problem puzzling many scholars.
The method brings serious environmental pollution problems while the electrolytic manganese industry is developed at a high speed, 7-9 tons of electrolytic manganese slag can be generated when 1 ton of manganese is produced, a large amount of electrolytic manganese slag is stacked, land resources are consumed, and Mn in the electrolytic manganese slag is accumulated along with the accumulation of time2+，Cr2+，Pb2+The heavy metal ions permeate underground along with rainwater, and cause serious harm to the environment and ecology. Therefore, how to efficiently utilize the electrolytic manganese slag becomes a hot point for research in the electrolytic manganese industry.
In combination with the problems of difficult utilization and serious waste of the nickel-iron slag and the manganese slag, the patent provides a preparation method of a cementing material taking the manganese slag and the nickel-iron slag as main components, so as to solve the defects of the problems in the prior art.
The composite alkali-activated cementing material is prepared by simultaneously adopting industrial solid wastes such as manganese slag, phosphorus slag, nickel-iron slag and the like, waste materials are changed into valuable materials, and the prepared cementing material has high strength, good acid and alkali resistance, simple preparation process, low cost and wide raw material sources. Compared with other conventional alkali-activated cementing materials in the prior art, the composite alkali-activated cementing material disclosed by the invention has a special and controllable tissue morphology, so that the setting time and early strength of the cementing material are regulated and controlled. Preferably, the cementing material disclosed by the invention also comprises an AFt ettringite structure besides a gel tissue, wherein AFt is a main structure for realizing the strength of the cementing material and shortening the gelling time; more preferably, the ettringite is wrapped by the gel structure to form a winding three-dimensional support structure, and the structure of the gel material is enhanced in a synergistic manner, so that the strength of the gel material is further enhanced.
The composite alkali activator comprises calcium hydroxide. The calcium hydroxide is used as an alkali activator, provides an alkaline environment in the hydration reaction process, and promotes the forward reaction.
The composite alkali exciting agent comprises manganese slag. The manganese slag is used as a sulfate excitant to provide calcium sulfate, and generates AFt (ettringite) with aluminum ions in an alkaline environment. AFt is a crystalline hydrated calcium sulphoaluminate produced by the combination of cement hydration products C-a-H (hydrated calcium aluminate) and sulphate ions. The ettringite is an important hydration product of the gypsum-containing aluminate cement, and has a relatively positive effect on the aspects of retarding the setting of the ettringite in the silicate cement, promoting the early strength development of the cement, compensating the shrinkage and the like. Preferably, the Aft structure of the present invention, in the form of a block, rod-like structure, is the primary support structure for the cementitious material.
The composite alkali activator comprises phosphorous slag. The phosphorous slag is used as A reaction precursor, Si-Al glass bodies are provided and decomposed into silicon-oxygen tetrahedrons and aluminum-oxygen tetrahedrons in an alkaline environment, and the silicon-oxygen tetrahedrons and the aluminum-oxygen tetrahedrons are mixed with calcium ions or sodium ions to generate C (N) -S-A-H (gel).
The composite alkali excitant comprises nickel-iron slag. The ferronickel slag is used as A reaction precursor, acts similarly to phosphorus slag, and also provides Si-Al glass body which is decomposed into silicon-oxygen tetrahedron and aluminum-oxygen tetrahedron under alkaline environment, and generates C (N) -S-A-H (gel) with calcium ions or sodium ions. Preferably, the gel structure of the cement of the present invention exhibits a continuous, gel-like morphology, distributed over a large area in the cement of the present invention.
In the composite alkali-activated cementing material, the reaction process (formula) is as follows: Si-Al glass + OH-+SO4 2-+Ca2 +→ AFt + C-S-A-H, the strength is improved after hydration reaction to form calcium vanadium body and wrap the intertwined gel (gel tissue).
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention discloses a preparation method of a manganese slag-phosphorus slag-nickel iron slag composite alkali-activated cementing material, which comprises the following components in percentage by mass:
3 to 8 percent of calcium hydroxide,
30 to 50 percent of manganese slag,
10 to 20 percent of phosphorus slag,
40 to 55 percent of nickel-iron slag,
the sum of the above components is 100%.
The calcium oxide content of the calcium hydroxide is more than 85 percent;
the specific surface area of the manganese slag is 600-800m2Per kg, grinding the powder to the particle size of 20-50 mu m;
the specific surface area of the phosphorus slag is 400-600m2Per kg, grinding the powder to a particle size of 50-80 μm;
the specific surface area of the ferronickel slag is 400-600m2Per kg, grinding the powder to the particle size of 20-60 mu m;
the preparation method comprises the following steps: adding the raw materials into a stirrer, wherein the water-to-glue ratio is selected from 0.3-0.5: 1, mixing uniformly.
In some embodiments, the above-mentioned gel material structure contains a gel structure-encapsulated ettringite structure.
In some embodiments, the ettringite structure is in the form of a block or rod.
In some embodiments, the gel tissue is a continuous gel-like substance.
In some embodiments, the water-to-glue ratio is more preferably 0.4: 1.
in some embodiments, the agitator has a stirring rate of 50 to 100 revolutions per minute and a stirring time of 10 to 60 minutes.
In some embodiments, the stirring further comprises pouring the obtained gel material into a mold, performing vibration molding, and curing at normal temperature until demolding is performed to obtain the alkali-activated gel material block sample with a specific shape.
In some embodiments, the demolded cement block sample is steam cured.
Compared with the prior art, the invention has the advantages that:
compared with the fly ash alkali-activated cementing material in the prior art, the composite alkali-activated cementing material has the advantages of controllable hydration and gelation time, increased strength, lower cost, wide material source, utilization of solid wastes, greenness and environmental protection, can be used for acid and alkali resistant parts, and has better corrosion resistance.
Drawings
FIG. 1 shows the microstructure of the gelled material of example 1 of the invention under a Scanning Electron Microscope (SEM).
FIG. 2 is an SEM photograph of the C-S-A-H gel structure in the cement of example 1 according to the present invention.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar modules or modules having the same or similar functionality throughout. The embodiments described below with reference to the accompanying drawings are illustrative only for the purpose of explaining the present invention, and are not to be construed as limiting the present invention.
Example 1
The components and the mass percentage thereof are as follows:
3 percent of calcium hydroxide,
30 percent of manganese slag,
20 percent of phosphorus slag,
47 percent of nickel-iron slag.
The calcium oxide content of the calcium hydroxide is 85%;
the specific surface area of the manganese slag is 600m2Per kg, grinding the powder to the particle size of 20-50 mu m;
the specific surface area of the phosphorous slag is 400m2Per kg, grinding the powder to a particle size of 50-80 μm;
the specific surface area of the ferronickel slag is 400m2Per kg, grinding the powder to the particle size of 20-60 mu m;
FIG. 1 shows the microstructure of the gelled material of example 1 of the invention under a Scanning Electron Microscope (SEM). The cement obtained in this example contains A predominant tissue-gel tissue (C-S-A-H) and A structure of ettringite aFt. Wherein the gel structure is in continuous gel form, and some gel materials also contain strengthening structure phase (spherical object in figure 2); the structure of the ettringite aFt presents a rod-shaped form with randomly distributed orientation, which forms a supporting structure of the whole gelled material; more importantly, in the embodiment, the gel structure C-S-A-H wraps the ettringite structure to form A compact and winding three-dimensional cross-linked network structure, so that the bonding force among the rod-shaped ettringites and the strength of the whole cementing material can be further enhanced.
FIG. 2 is an SEM photograph of the C-S-A-H gel structure in the cement of example 1 of the present invention, and it can be seen that the C-S-A-H gel structure is in A continuous gel form, and some gel substances further contain A strengthening structure phase (spheres in FIG. 2).
The raw materials are taken and evenly mixed to prepare the manganese slag-phosphorus slag-ferronickel slag composite alkali-activated cementing material. The water-cement ratio is 0.4, and through detection, the compressive strength of the manganese slag-phosphorus slag-nickel iron slag composite alkali-activated cementing material prepared by the invention reaches 12.4MPa in 7d, 35.7MPa in 28d, the initial setting time is 125min, and the final setting time is 300 min.
Example 2
The components and the mass percentage thereof are as follows:
5 percent of calcium hydroxide,
40 percent of manganese slag,
10 percent of phosphorus slag,
45 percent of nickel-iron slag.
The calcium oxide content of the calcium hydroxide is 90%;
the specific surface area of the manganese slag is 700m2Per kg, grinding the powder to the particle size of 20-50 mu m;
the specific surface area of the phosphorus slag is 500m2Per kg, grinding the powder to the particle size of 20-50 mu m;
the specific surface area of the ferronickel slag is 500m2Per kg, grinding the powder to the particle size of 20-50 mu m;
the raw materials are taken and evenly mixed to prepare the manganese slag-phosphorus slag-ferronickel slag composite alkali-activated cementing material. The water-cement ratio is 0.4, and through detection, the compressive strength of the manganese slag-phosphorus slag-nickel iron slag composite alkali-activated cementing material prepared by the invention reaches 18.6MPa in 7d, 45.7MPa in 28d, the initial setting time is 105min, and the final setting time is 275 min.
Example 3
The components and the mass percentage thereof are as follows:
8 percent of calcium hydroxide,
50 percent of manganese slag,
10 percent of phosphorus slag,
42 percent of nickel-iron slag.
The calcium oxide content of the calcium hydroxide is 90%;
the specific surface area of the manganese slag is 800m2/kg；
The specific surface area of the phosphorus slag is 600m2/kg；
The specific surface area of the ferronickel slag is 600m2/kg；
The raw materials are taken and evenly mixed to prepare the manganese slag-phosphorus slag-ferronickel slag composite alkali-activated cementing material. The water-cement ratio is 0.4, and through detection, the compressive strength of the manganese slag-phosphorus slag-nickel iron slag composite alkali-activated cementing material prepared by the invention reaches 24.5MPa in 7d, 50.4MPa in 28d, the initial setting time is 90min, and the final setting time is 255 min.
Example 4
The components and the mass percentage thereof are as follows:
5 percent of calcium hydroxide,
30 percent of manganese slag,
15 percent of phosphorus slag,
50% of nickel-iron slag.
The calcium oxide content of the calcium hydroxide is 90%;
the specific surface area of the manganese slag is 600m2Per kg, grinding the powder to the particle size of 20-50 mu m;
the specific surface area of the phosphorus slag is 600m2Per kg, grinding the powder to the particle size of 20-50 mu m;
the specific surface area of the ferronickel slag is 400m2Per kg, grinding the powder to the particle size of 20-50 mu m;
the raw materials are taken and evenly mixed to prepare the manganese slag-phosphorus slag-ferronickel slag composite alkali-activated cementing material. The water-cement ratio is 0.4, and through detection, the compressive strength of the manganese slag-phosphorus slag-nickel iron slag composite alkali-activated cementing material prepared by the invention reaches 17.6MPa in 7d, 42.3MPa in 28d, the initial setting time is 128min, and the final setting time is 300 min.
Example 5
The components and the mass percentage thereof are as follows:
5 percent of calcium hydroxide,
40 percent of manganese slag,
15 percent of phosphorus slag,
40% of nickel-iron slag.
The calcium oxide content of the calcium hydroxide is 95%;
the specific surface area of the manganese slag is 800m2Per kg, grinding the powder to the particle size of 20-50 mu m;
the specific surface area of the phosphorus slag is 600m2Per kg, grinding the powder to the particle size of 20-50 mu m;
the specific surface area of the ferronickel slag is 500m2Per kg, grinding the powder to the particle size of 20-50 mu m;
the raw materials are taken and evenly mixed to prepare the manganese slag-phosphorus slag-ferronickel slag composite alkali-activated cementing material. The water-cement ratio is 0.4, and through detection, the compressive strength of the manganese slag-phosphorus slag-nickel iron slag composite alkali-activated cementing material prepared by the invention reaches 21.5MPa in 7d, 47.6MPa in 28d, the initial setting time is 110min, and the final setting time is 260 min.
Example 6
The components and the mass percentage thereof are as follows:
5 percent of calcium hydroxide,
30 percent of manganese slag,
10 percent of phosphorus slag,
55 percent of nickel-iron slag.
The calcium oxide content of the calcium hydroxide is 90%;
the specific surface area of the manganese slag is 700m2Per kg, grinding the powder to the particle size of 20-50 mu m;
the specific surface area of the phosphorus slag is 600m2Per kg, grinding the powder to the particle size of 20-50 mu m;
the specific surface area of the ferronickel slag is 600m2Per kg, grinding the powder to the particle size of 20-50 mu m;
the raw materials are taken and evenly mixed to prepare the manganese slag-phosphorus slag-ferronickel slag composite alkali-activated cementing material. The water-cement ratio is 0.4, and through detection, the compressive strength of the manganese slag-phosphorus slag-nickel iron slag composite alkali-activated cementing material prepared by the invention reaches 21.4MPa in 7d, reaches 51.4MPa in 28d, and has the initial setting time of 105min and the final setting time of 265 min.
Comparative example 1
With reference to example 1, the composite alkali-activated cementing material was prepared by using the same preparation process parameters except that the components thereof did not contain manganese slag. By adopting the water-gel ratio of 0.4, the detection shows that the 7d compressive strength of the waste residue composite alkali-activated cementing material prepared by the invention reaches 10.3MPa, the 28d compressive strength reaches 32.5MPa, the initial setting time is 160min, and the final setting time is 400 min.
Comparative example 2
With reference to example 1, the composite alkali-activated cementitious material was prepared using the same preparation process parameters except that the composition did not contain nickel-containing iron slag. By adopting the water-gel ratio of 0.4, the detection shows that the 7d compressive strength of the waste residue composite alkali-activated cementing material prepared by the invention reaches 9.6MPa, the 28d compressive strength reaches 26.9MPa, the initial setting time is 150min, and the final setting time is 380 min.
Comparative example 3
With reference to example 1, the composite alkali-activated cementitious material was prepared using the same preparation process parameters except that the composition did not contain nickel-containing iron slag. By adopting the water-gel ratio of 0.4, the detection shows that the 7d compressive strength of the waste residue composite alkali-activated cementing material prepared by the invention reaches 8.2MPa, the 28d compressive strength reaches 23.7MPa, the initial setting time is 150min, and the final setting time is 390 min.
The compressive strength of each sample of the waste residue composite alkali-activated cementing material prepared by the embodiment of the invention is more than 20MPa in 7d and more than 50MPa in 28d, the initial setting time is shortened to 100min, and the final setting time is less than 300 min. Therefore, compared with other gel materials in the comparative example and the prior art, the gel material of the invention has the advantages of shortened gel time and higher early strength than other similar composite alkali-activated gel materials in the prior art.
In the description herein, references to the description of "one embodiment," "another embodiment," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment is included in at least one embodiment of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (5)
1. A preparation method of a manganese slag-phosphorus slag-nickel iron slag composite alkali-activated cementing material comprises the following components in percentage by mass:
3 to 8 percent of calcium hydroxide,
30 to 50 percent of manganese slag,
10 to 20 percent of phosphorus slag,
40 to 55 percent of nickel-iron slag,
the sum of the components is 100 percent, and the manganese slag is more than 30 percent;
the calcium oxide content of the calcium hydroxide is more than 85 percent;
the specific surface area of the manganese slag is 600-800m2Grinding the powder to the particle size of 20-50 mu m;
the specific surface area of the phosphorus slag is 400-600m2Grinding the powder to 50-80 mu m;
the specific surface area of the ferronickel slag is 400-600m2Grinding the powder to the particle size of 20-60 mu m;
the preparation method comprises the following steps: adding the raw materials into a stirrer, wherein the water-to-glue ratio is selected from 0.3-0.5: 1, mixing uniformly;
the gel material structure contains A gel structure which is A C-S-A-H structure and is in A continuous colloidal state, and part of colloidal substances also contain A spherical object strengthening tissue phase; the C-S-A-H structure wraps the ettringite structure to form A compact and wound three-dimensional cross-linked network structure; the ettringite structure, which presents a rod-like morphology with randomly distributed orientations, forms the supporting structure of the whole cement.
2. The preparation method of the manganese slag-phosphorus slag-nickel iron slag composite alkali-activated cementing material according to claim 1, wherein the water-to-gel ratio is selected to be 0.4: 1.
3. the method for preparing manganese slag-phosphorus slag-ferronickel slag composite alkali-activated cementing material according to claim 1, wherein the stirring speed of the stirrer is 50-100 r/min, and the stirring time is 10-60 min.
4. The preparation method of manganese slag-phosphorus slag-nickel iron slag composite alkali-activated cementing material according to claim 1, further comprising, after stirring, pouring the obtained cementing material into a mold, vibration molding, curing under normal temperature conditions until demolding, and obtaining a block sample of the alkali-activated cementing material with a specific shape.
5. The method for preparing manganese slag-phosphorus slag-nickel iron slag composite alkali-activated cementing material according to claim 4, wherein the stripped massive sample of the cementing material is steamed.
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| CN113087419A (en) | 2021-07-09 |
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