CN115432952B - Early-stage steel slag activity excitant and preparation method and application thereof - Google Patents

Early-stage steel slag activity excitant and preparation method and application thereof Download PDF

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CN115432952B
CN115432952B CN202211128811.0A CN202211128811A CN115432952B CN 115432952 B CN115432952 B CN 115432952B CN 202211128811 A CN202211128811 A CN 202211128811A CN 115432952 B CN115432952 B CN 115432952B
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steel slag
early
activity excitant
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stage activity
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CN115432952A (en
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吴少鹏
阎家杰
谢君
陈美祝
刘全涛
庞凌
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Wuhan University of Technology WUT
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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
    • C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
    • C04B40/0028—Aspects relating to the mixing step of the mortar preparation
    • C04B40/0039—Premixtures of ingredients
    • 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
    • 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
    • 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
    • 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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Soil Conditioners And Soil-Stabilizing Materials (AREA)

Abstract

The invention belongs to the technical field of steel slag additives, and discloses a steel slag early-stage activity excitant, a preparation method and application thereof. The steel slag early-stage activity excitant comprises the following raw materials in percentage by mass: 10-25% of quicklime, 5-15% of diethanol monoisopropanolamine, 30-45% of metakaolin and 20-50% of water. The steel slag early-stage activity excitant adopts an organic-inorganic composite formula, can effectively improve the early-stage activity of steel slag under the condition of small doping amount, and has a certain improvement effect on the mechanical property and working performance in the later stage; and the consumption of the steel slag in the cementing material can be further improved through improving the activity of the steel slag, and the cement-based composite material has positive effects of reducing the consumption of cement and improving the comprehensive utilization rate of the steel slag.

Description

Early-stage steel slag activity excitant and preparation method and application thereof
Technical Field
The invention belongs to the technical field of steel slag additives, and particularly relates to a steel slag early-stage activity excitant, a preparation method and application thereof.
Background
The steel slag is a main industrial waste slag produced in steel production, the discharge amount is huge and accounts for about 12% of the solid waste in steel industry, the actual comprehensive utilization rate of the steel slag in China is low, most of the steel slag is randomly piled up, a large amount of empty space is occupied, and the natural environment is seriously polluted, so that the problem of reasonable utilization of the steel slag is more and more important. The steel slag contains dicalcium silicate (C) 2 S) and tricalcium silicate (C) 3 S) and other active minerals, in recent years, many students have studied the application of steel slag in the form of auxiliary gel materials in the cement industry, however, due to the fact that the steel slag is low in activity, the gelation property is not easy to develop, the hydration speed is low, the final strength is low, and further utilization of the steel slag in cement-based materials is limited.
Chemical excitation is a very active and rapidly developed field, adopts a chemical excitation mode to release potential gel activity in steel slag, and provides a green approach for large-scale comprehensive utilization of the steel slag. The chemical excitation is to increase the activity of the steel slag by adding certain additives, the most common are alkali-exciting agents such as sodium carbonate and sodium hydroxide, and the solution after the alkali-exciting agents are added is alkaline, if the mixing amount is too low, the alkali is weak, the activity of the steel slag cannot be obviously increased, and if the mixing amount is too high, the early activity of the steel slag is improved, but the later mechanical property, the working property and the like are adversely affected. In recent years, other types of excitants, such as organic excitants, have been proposed by scholars, the cost of the excitants is too high, and the selected organic matters have high toxicity and cannot be put into practical production.
In conclusion, the development of a new steel slag early-stage activity excitant has important significance for improving the utilization rate of steel slag and realizing the sustainable development of the steel industry and the cement industry.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a steel slag early-stage activity excitant, and a preparation method and application thereof, wherein the steel slag early-stage activity excitant adopts an organic-inorganic composite formula, can effectively improve the early-stage activity of steel slag under the condition of small doping amount, and has a certain improvement effect on the mechanical property and working performance in the later stage.
In order to solve the technical problem, the invention provides a steel slag early-stage activity excitant, which comprises the following raw materials in percentage by mass: 10-25% of quicklime, 5-15% of diethanol monoisopropanolamine, 30-45% of metakaolin and 20-50% of water.
Preferably, the steel slag early-stage activity excitant consists of the following raw materials in percentage by mass: 15-25% of quicklime, 10-15% of diethanol monoisopropanolamine, 35-45% of metakaolin and 20-35% of water.
In the scheme, the CaO content of the quicklime is more than or equal to 90 percent, and the MgO content is less than or equal to 4 percent.
In the scheme, the particle size of the quicklime is less than or equal to 0.06mm, and the specific surface area is 300-400m 2 /kg。
In the scheme, the total effective content of the diethanol monoisopropanolamine is more than or equal to 99 percent.
In the above scheme, the metakaolin is Al 2 O 3 The content is 25-35%, siO 2 The content is 55-65%.
In the scheme, the particle size of the metakaolin is less than or equal to 0.07mm, and the specific surface area is 300-400m 2 /kg。
The invention also provides a preparation method of the steel slag early-stage activity excitant, which comprises the following steps: adding quicklime, diethanol isopropanolamine, metakaolin and water into stirring equipment according to mass percent, and uniformly stirring to obtain the steel slag early-stage activity excitant.
In the scheme, the stirring speed is 200-300r/min, and the stirring time is 5-15min.
The invention also provides an application of the steel slag early-stage activity excitant, which comprises the following steps: mixing the steel slag early-stage activity excitant with the steel slag, and uniformly stirring to obtain active steel slag; and mixing the active steel slag and cement to prepare active steel slag cement mortar or active steel slag cement concrete as a cementing material.
In the scheme, the CaO content of the steel slag is 35-45%, and SiO 2 The content is 15-25%, al 2 O 3 The content is 5-10%, fe 2 O 3 The content is 15-30%.
In the scheme, the grain diameter of the steel slag is less than or equal to 0.01mm, and the specific surface area is 400-500m 2 /kg。
In the scheme, the mixing amount of the steel slag early-stage activity excitant is 0.2-0.3% of the mass of the steel slag.
In the scheme, the stirring speed is 300-400r/min, and the stirring time is 10-20min.
In the scheme, the consumption of the active steel slag in the cementing material is 30-40%.
Compared with the prior art, the invention has the beneficial effects that:
1) The early-stage steel slag activity excitant consists of quicklime, diethanol monoisopropanolamine, metakaolin and water, wherein the quicklime can accelerate the early hydration process of active components in the steel slag, and also provides a proper alkaline environment for the diethanol monoisopropanolamine and the metakaolin, and under the alkaline environment, the diethanol monoisopropanolamine and Ca in the steel slag are mixed with each other 2+ 、Al 3+ 、Fe 3+ Equi-metallicThe complex action of ions is carried out, so that indissolvable metal ions are converted into soluble ions, dissolution of mineral phases, particularly inert phases, in the steel slag is promoted, the metakaolin and the dissolved metal ions are gelled, cementing of early hydration products of the steel slag is promoted, compactness of the early hydration products is improved, and meanwhile, alkali aggregate reaction is inhibited, so that the early activity excitant for the steel slag can effectively promote early activity of the steel slag under the condition of small doping amount, has a certain promotion effect on mechanical properties and working properties in the later stage, and does not have negative influence.
2) The early-stage steel slag activation excitant adopts an organic-inorganic composite formula, and the organic components select low-toxicity diethanol monoisopropanolamine and occupy less amount, so that compared with a pure organic excitant, the early-stage steel slag activation excitant can greatly reduce the cost and reduce the harm to the environment, and is suitable for industrial production.
3) The early-stage steel slag activity excitant can further improve the consumption of steel slag in the cementing material through improving the activity of the steel slag, and has positive effects of reducing the consumption of cement and improving the comprehensive utilization rate of the steel slag.
Detailed Description
For a better understanding of the present invention, the following examples are further illustrated, but are not limited to the following examples.
In the following examples, quicklime having a CaO content of 96.3%, a MgO content of 1.6%, a particle size of 0.06mm or less and a specific surface area of 374m was used 2 /kg; the total effective content of the diethanol monoisopropanolamine (DEIPA) adopted is 99.9 percent; al of the metakaolin used 2 O 3 The content is 29.7%, siO 2 The content is 58.7%, the grain diameter is less than or equal to 0.07mm, and the specific surface area is 358m 2 /kg; the grain diameter of the steel slag is less than or equal to 0.01mm, and the specific surface area is 467m 2 /kg; the cement adopted is ordinary Portland cement PO42.5; the main chemical compositions of the steel slag and the cement are shown in table 1.
TABLE 1
Raw materials MgO Al 2 O 3 SiO 2 P 2 O 5 SO 3 MnO CaO Fe 2 O 3
Steel slag 4.03％ 5.40％ 18.82％ 1.36％ 0.39％ 4.01％ 37.30％ 26.47％
Cement and its preparation method 0.84％ 6.13％ 21.61％ 0.19％ 3.95％ 3.94％ 58.19％ 4.00％
Examples 1 to 6
The raw material compositions of the steel slag early-stage activity excitants in examples 1 to 6 are shown in Table 2.
TABLE 2
Examples Quicklime (%) DEIPA(％) Metakaolin (%) Water (%)
Example 1 10 5 35 50
Example 2 15 10 40 35
Example 3 20 15 45 20
Example 4 25 5 30 40
Example 5 10 10 35 45
Example 6 15 15 40 30
The steel slag early-stage activity excitant in examples 1-6 is prepared by the following steps: adding quicklime, diethanol isopropanolamine, metakaolin and water into a stirring kettle according to mass percent, and uniformly stirring according to the speed and time shown in Table 3 to obtain the steel slag early-stage activity excitant.
TABLE 3 Table 3
Examples Stirring rate (r/min) Stirring time (min)
Example 1 200 5
Example 2 250 10
Example 3 300 15
Example 4 200 5
Example 5 250 10
Example 6 300 15
Comparative examples 1 to 4
Comparative examples 1 and 2 are steel slag early-stage activity activators without addition of diethanol monoisopropanolamine and without addition of metakaolin, respectively, and comparative examples 3 and 4 are conventional alkali activators Na, respectively 2 CO 3 And NaOH. The raw material components of each comparative example are shown in Table 4.
TABLE 4 Table 4
Figure BDA0003849216370000041
Application example 1
The steel slag early-stage activity excitants in examples 1-6 and comparative examples 1-2 are mixed with steel slag and stirred uniformly to obtain active steel slag; the active steel slag and cement are mixed to be used as cementing materials, and the active steel slag cement mortar is prepared according to GB/T17671-2021 method for testing cement mortar strength (ISO method). Meanwhile, an original steel slag cement mortar without any activator was also prepared as comparative example 5. The specific parameters are shown in Table 5.
TABLE 5
Figure BDA0003849216370000042
Figure BDA0003849216370000051
The 7d activity indexes of the original steel slag and the active steel slag were measured according to the GB/T51003-2014 annex B of the mineral admixture application technical Specification, and the 7d compressive strength and the 7d flexural strength of the original steel slag cement mortar and the active steel slag cement mortar were measured according to the GB/T17671-2021 cement mortar strength test method (ISO method), and the results are shown in Table 6.
TABLE 6
Examples 7d Activity index (%) 7d compressive Strength (MPa) 7d flexural Strength (MPa)
Example 1 74.89 4.66 23.74
Example 2 78.17 4.87 24.78
Example 3 79.13 4.94 25.08
Example 4 77.12 4.71 24.45
Example 5 77.21 4.79 24.48
Example 6 78.46 4.88 24.87
Comparative example 1 66.91 4.15 21.21
Comparative example 2 71.14 4.41 22.55
Comparative example 5 63.25 3.10 20.05
From the table above, the addition of the exciting agent can improve the early activity of the steel slag, and is characterized by improving the 7d activity index, the 7d compressive strength and the 7d flexural strength. Wherein, the steel slag early-stage activity excitant in comparative examples 1-2 has weaker effect, and the 7d activity index is only improved by 3.66-7.89% compared with comparative example 5; the steel slag early-stage activity excitant in the examples 1-6 has obvious effect, and the 7d activity index is 11.64-15.88% higher than that of the comparative example 5; this demonstrates that a good coordination is produced between quicklime, diethanol monoisopropanolamine and metakaolin, so that the steel slag early-stage activity excitant in examples 1-6 shows more excellent application effect.
Application example 2
Mixing the steel slag early-stage activity excitants in examples 1-6 and comparative examples 3-4 with steel slag, and uniformly stirring to obtain active steel slag; the active steel slag and cement are mixed to be used as cementing materials, and the active steel slag cement concrete is prepared according to GB/T50080-2016 Standard of common concrete mixture Performance test method. Meanwhile, an original steel slag cement concrete without any activator was also prepared as comparative example 6. The specific parameters are shown in Table 7.
TABLE 7
Figure BDA0003849216370000061
The compressive strength and flexural strength of the original steel slag cement concrete and the active steel slag cement concrete were measured according to GB/T50081-2019 "test method Standard for physical mechanical Properties of concrete", and the initial slump of the original steel slag cement concrete and the active steel slag cement concrete were measured according to GB/T50080-2016 "test method Standard for Performance of common concrete mix", the results are shown in Table 8.
TABLE 8
Figure BDA0003849216370000062
In terms of mechanical properties, the traditional alkali-activator in comparative examples 3-4 can improve early mechanical properties at a doping amount of 6%, the 7d compressive strength and the 7d flexural strength are both improved compared with comparative example 6, but have certain negative effects on later mechanical properties, and the 28d compressive strength and the 28d flexural strength are both reduced compared with comparative example 6, which is probably caused by the fact that the alkali-activator consumes a large amount of active minerals in steel slag concrete in the early stage; the steel slag early-stage activity excitant in examples 1-6 has larger improvement range of early-stage mechanical property and has a certain improvement effect on later-stage mechanical property under the condition of small doping amount of 0.2-0.3%, and does not generate negative effect. In addition, in the test process, if the steel slag dosage in the cementing material exceeds 30% when the alkali-activator is used, the strength of the concrete test block is reduced in a cliff shape, so that the steel slag dosage of comparative examples 3-4 is 30%; when the early-stage steel slag activity excitant in the examples 1-6 is used, the steel slag consumption in the cementing material can be increased to 30-40%, which has positive effects of reducing the consumption of cement and improving the comprehensive utilization rate of the steel slag.
In terms of working performance, slump is an index for reflecting workability of concrete, the larger the slump is, the better the fluidity of the concrete is, and the time loss of the slump can also reflect cohesiveness of the concrete; as can be seen from table 8, the conventional alkali-activator of comparative examples 3 to 4 reduced the initial slump and 60min slump of the concrete, adversely affecting both fluidity and cohesiveness of the concrete; the steel slag early-stage activity excitant in examples 1-6 can improve the initial slump of concrete and reduce the time loss of slump, on one hand, the surface tension of diethanol monoisopropanolamine can improve the workability of concrete, and on the other hand, metakaolin can reduce the porosity of concrete so as to increase the cohesiveness of concrete, and the workability of concrete is improved through the coordination of the two.
The above examples are presented for clarity of illustration only and are not limiting of the embodiments. Other variations or modifications of the above description will be apparent to those of ordinary skill in the art, and it is not necessary or exhaustive of all embodiments, and thus all obvious variations or modifications that come within the scope of the invention are desired to be protected.

Claims (7)

1. The application method of the steel slag early-stage activity excitant is characterized by comprising the following steps: mixing the steel slag early-stage activity excitant with the steel slag, and uniformly stirring to obtain active steel slag; mixing active steel slag and cement to prepare active steel slag cement mortar or active steel slag cement concrete; the mixing amount of the early-stage steel slag activity excitant is 0.2-0.3% of the mass of the steel slag; the consumption of the active steel slag in the cementing material is 35-40%;
the steel slag early-stage activity excitant comprises the following raw materials in percentage by mass: 10-25% of quicklime, 5-15% of diethanol monoisopropanolamine, 30-45% of metakaolin and 20-50% of water; al of the metakaolin 2 O 3 The content is 25-35%, siO 2 The content is 55-65%.
2. The application method of the steel slag early-stage activity excitant according to claim 1, wherein the steel slag early-stage activity excitant comprises the following raw materials in percentage by mass: 15-25% of quicklime, 10-15% of diethanol monoisopropanolamine, 35-45% of metakaolin and 20-35% of water.
3. The method for applying the steel slag early-stage activity excitant according to claim 1, wherein the CaO content of the quicklime is more than or equal to 90 percent and the MgO content is less than or equal to 4 percent; the total effective content of the diethanol monoisopropanolamine is more than or equal to 99 percent.
4. According to claim 1The application method of the steel slag early-stage activity excitant is characterized in that the particle size of the quicklime is less than or equal to 0.06mm, and the specific surface area is 300-400m 2 /kg; the grain diameter of metakaolin is less than or equal to 0.07mm, and the specific surface area is 300-400m 2 /kg。
5. The method for applying the steel slag early-stage activity excitant according to claim 1, wherein the method for preparing the steel slag early-stage activity excitant comprises the following steps: adding quicklime, diethanol isopropanolamine, metakaolin and water into stirring equipment according to mass percent, and uniformly stirring to obtain the steel slag early-stage activity excitant.
6. The method for using the steel slag early-stage activity excitant according to claim 5, wherein the stirring speed is 200-300r/min and the stirring time is 5-15min.
7. The method for using the steel slag early-stage activity excitant according to claim 1, wherein the CaO content of the steel slag is 35-45%, siO 2 The content is 15-25%, al 2 O 3 The content is 5-10%, fe 2 O 3 The content is 15-30%; the grain diameter of the steel slag is less than or equal to 0.01mm, and the specific surface area is 400-500m 2 /kg。
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