CN113620672B - Partially calcined limestone-calcined clay cement-based material and preparation method thereof - Google Patents

Partially calcined limestone-calcined clay cement-based material and preparation method thereof Download PDF

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CN113620672B
CN113620672B CN202111055160.2A CN202111055160A CN113620672B CN 113620672 B CN113620672 B CN 113620672B CN 202111055160 A CN202111055160 A CN 202111055160A CN 113620672 B CN113620672 B CN 113620672B
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calcined
limestone
cement
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clay
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CN113620672A (en
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胡传林
董烨民
阮云星
钱雄
王发洲
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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
    • 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
    • C04B28/02—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 hydraulic cements other than calcium sulfates
    • C04B28/04—Portland cements
    • 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
    • C04B20/06—Expanding clay, perlite, vermiculite or like granular materials
    • 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
    • C04B28/02—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 hydraulic cements other than calcium sulfates
    • C04B28/06—Aluminous cements
    • 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
    • C04B28/14—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 calcium sulfate cements
    • C04B28/141—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 calcium sulfate cements containing dihydrated gypsum before the final hardening step, e.g. forming a dihydrated gypsum product followed by a de- and rehydration step
    • 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
    • C04B28/14—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 calcium sulfate cements
    • C04B28/145—Calcium sulfate hemi-hydrate with a specific crystal form
    • 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
    • C04B28/14—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 calcium sulfate cements
    • C04B28/16—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 calcium sulfate cements containing anhydrite, e.g. Keene's cement
    • 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

Abstract

The invention relates to a partially calcined limestone-calcined clay cement-based material and a preparation method thereof. The raw materials of the partially calcined limestone-calcined clay cement-based material contain gelling components, and the gelling components comprise calcined clay, partially calcined limestone and cement; the partially calcined limestone has a core-shell structure, the outer layer of the partially calcined limestone is loose calcium oxide, and the inner layer of the partially calcined limestone is compact calcium carbonate; the content of calcium oxide in the partially calcined limestone is 5 to 75 percent. According to the invention, the cement is replaced by the partially calcined limestone and the calcined clay, and the additional alkali environment and the calcium hydroxide are provided by the partially calcined limestone, so that the volcanic ash reaction characteristic of the calcined clay is promoted, the later strength increase rate of the system is accelerated, the system still has good mechanical properties under the condition that the cement is replaced by the partially calcined limestone and the calcined clay in a high proportion, and the obtained cement product can meet the requirements of engineering construction.

Description

Partially calcined limestone-calcined clay cement-based material and preparation method thereof
Technical Field
The invention relates to the technical field of building materials, in particular to a partially calcined limestone-calcined clay cement-based material and a preparation method thereof.
Background
The fuel consumption and limestone decarburization in the cement production process generate carbon dioxide, which causes greenhouse effect. Currently, an effective measure to reduce carbon dioxide emissions in the cement industry is to add supplementary cementitious materials to the cement to reduce the amount of cement used. However, the auxiliary cementing materials are mainly derived from wastes generated in industrial processes, and have limited yield and large quality difference, so that the high requirements of the cement industry are difficult to meet.
In response to the problem of limited supply of supplementary cementitious materials (industrial by-products), researchers at home and abroad believe that both calcined clay and limestone materials have great potential and are widely distributed and abundant worldwide. The invention patent of international patent number EP2253600 (A1), named as "Portland limestone catalyzed clay", describes that the combination of calcined clay and limestone replaces cement to form a limestone-calcined clay-cement combined ternary cementing material system with wide application prospect. However, when the cement content in the ternary cementitious material system is further reduced (accounting for 0-50% of the total mass of the cementitious material), a large amount of calcined clay which does not participate in the reaction exists in the system, so that the mechanical properties of the calcined clay are significantly reduced, and the requirements of engineering construction cannot be met.
Disclosure of Invention
In view of the above, there is a need to provide a partially calcined limestone-calcined clay cement-based material and a preparation method thereof, so as to solve the technical problems of the prior art that a large amount of unreacted calcined clay exists in a ternary cementing material system in which limestone and calcined clay are mixed in a large amount instead of cement, and the mechanical properties of the material are significantly reduced.
A first aspect of the present invention provides a partially calcined limestone-calcined clay cement-based material having a raw material containing a gelling component comprising calcined clay, partially calcined limestone and cement;
the partially calcined limestone has a core-shell structure, the outer layer of the partially calcined limestone is loose calcium oxide, and the inner layer of the partially calcined limestone is compact calcium carbonate; the content of calcium oxide in the partially calcined limestone is 5 to 75 percent.
A second aspect of the invention provides a method for preparing a partially calcined limestone-calcined clay cement-based material, comprising the steps of:
and uniformly mixing the partially calcined limestone, the calcined clay, the cement, the gypsum, the water and the water reducing agent, and pouring and molding to obtain the partially calcined limestone-calcined clay cement-based material.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, cement is replaced by part of calcined limestone and calcined clay, and extra alkali environment and calcium hydroxide are provided by part of calcined limestone, so that the volcanic ash reaction characteristic of the calcined clay is promoted, the later strength increase rate of the system is accelerated, the system still has good mechanical properties under the condition that cement is replaced by part of calcined limestone and calcined clay in a high proportion, and the obtained cement product can meet the requirements of engineering construction;
the large-doping-amount partially calcined limestone-calcined clay cement-based material prepared by the method is formed by pouring, has a simple preparation process and has a good application prospect.
Drawings
FIG. 1 is a 28d cumulative pore size plot for example 2 of the present invention and comparative example 1;
FIG. 2 is a 28d pore diameter differential curve for inventive example 2 and comparative example 1.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
A first aspect of the invention provides a partially calcined limestone-calcined clay cement-based material having a raw material comprising a gelling component comprising calcined clay, partially calcined limestone and cement;
the partially calcined limestone has a core-shell structure, the outer layer of the partially calcined limestone is loose calcium oxide, and the inner layer of the partially calcined limestone is compact calcium carbonate; the content of calcium oxide in the partially calcined limestone is 5% to 75%, further 20% to 60%, further 50% to 60%, further 52%.
In one embodiment of the invention, the calcined clay is prepared by separately calcining raw clay at a temperature of 550-900 ℃, further calcining at a temperature of 800 ℃; the partially calcined limestone is prepared by separately calcining the calcareous raw material at 600-1000 ℃ for 10-360 min, further calcining at 800-1000 ℃ for 10-60 min, further calcining at 950 ℃ for 10-30 min.
In the invention, the forming process of calcined clay is essentially a process of converting the dehydroxylation of kaolinite in raw clay into higher-age clay with reactivity, the calcining temperature is not more than 900 ℃, and recrystallization caused by overhigh temperature is avoided. The calcination time for calcining the clay is not strictly limited, and can be selected by the skilled person according to the needs. In some preferred embodiments of the invention, the calcination time is from 0.1 to 6 hours.
According to the invention, the raw clay and the calcareous raw material are calcined separately within the respective optimal temperature and time ranges, so that the reactivity of partial calcined limestone and calcined clay can be improved, and the partial calcined limestone and calcined clay can reach the optimal levels respectively. In some embodiments of the invention, the raw clay, when calcined alone, has a calcination temperature of 800 ℃ and a calcination time of 1 hour; the calcination temperature of the calcareous raw material is 950 ℃, and the calcination time is 10min.
In another embodiment of the present invention, the calcined clay and the partially calcined limestone are prepared by uniformly mixing raw clay and calcareous material and calcining at 700-900 deg.C for 10-30 min. Preferably, the temperature of the mixed calcination is 800 ℃ and the time is 10min.
According to the invention, through mixing and calcining the raw clay and the calcareous raw material, the uniformity between the raw clay and the calcareous raw material can be improved, the associativity between the raw clay and the calcareous raw material is stronger, and the mechanical property is improved.
According to the invention, calcium hydroxide is formed after part of calcium oxide on the surface of calcined limestone meets water to provide an extra alkali environment, so that on one hand, the dissolution of active silicon-aluminum elements in calcined clay is facilitated, and on the other hand, the calcium hydroxide and the calcined clay have a volcanic ash reaction to form more reaction products, so that the later strength increase rate of the system is accelerated; meanwhile, the core-shell structure of the partially calcined limestone provides more nucleation sites, which is beneficial for forming a layer of compact hydration product around the hydration product, thereby effectively improving the mechanical property and reducing the porosity, and finally greatly reducing the dosage of cement on the premise of reducing the mechanical property to a small extent.
In the invention, the particle size of the calcined clay is 0.1-1000 mu m; the kaolin content of the raw clay is between 10% and 100%, preferably between 50% and 100%.
In the invention, the calcareous raw material is one or more of limestone, dolomite, marble, calcite, aragonite and shells.
In the invention, the mass ratio of calcined clay to partially calcined limestone is 1: (0.2 to 1), further 1: (0.4-0.6), and further 1.
In the invention, the total mass of the calcined clay and the partially calcined limestone accounts for 5-99%, further 50-90%, further 80-90% and further 80% of the gelling component. In the mass ratio range, the cement can be replaced by the calcined clay and the partially calcined limestone with large mixing amount, and the obtained product has higher mechanical property and can meet the requirements of engineering construction.
In the invention, the cement is at least one of ordinary portland cement and sulphoaluminate cement. Further, the cement is at least one of ordinary portland cement of strength grade 32.5, 42.5, or 52.5.
In the present invention, the gelling component further comprises: and (3) gypsum. Further, gypsum accounts for 1-5% of the gelling component, and further 2-3%. Further, the gypsum is one or more of dihydrate gypsum, hemihydrate gypsum and anhydrite gypsum.
In the invention, the raw materials of the cement-based material also comprise: a water reducing agent. Further, the water reducing agent accounts for 1-5% of the gelling component. Further, the water reducing agent is a high-performance polycarboxylic acid water reducing agent.
In the invention, the cement-based material also comprises the following raw materials: and (3) water. Further, the mass ratio of the water to the gelling component is (0.2-0.6): 1, further (0.3 to 0.4): 1.
in the invention, when the total amount of the calcined clay and the partially calcined limestone exceeds 50% of the cement-based material, although the cement content in the system is low and the calcined clay content is high, calcium oxide on the surface of the partially calcined limestone forms calcium hydroxide when meeting water, so that more reaction products can be formed, and the dosage of the cement can be greatly reduced on the premise of reducing the mechanical property to a small extent.
A second aspect of the invention provides a method for preparing a partially calcined limestone-calcined clay cement-based material, comprising the steps of:
and uniformly mixing the partially calcined limestone, the calcined clay, the cement, the gypsum, the water and the water reducing agent, and pouring and molding to obtain the partially calcined limestone-calcined clay cement-based material.
The partially calcined limestone-calcined clay cement-based material prepared by the method is formed by pouring, has a simple preparation process and has a good application prospect.
In the following examples and comparative examples, the preparation method of the partially calcined limestone-calcined clay cement-based material is as follows, unless otherwise specified:
(1) Uniformly mixing part of calcined limestone, calcined clay, cement and gypsum to obtain a gelling component;
(2) And adding water and a water reducing agent into the gelled component, mixing and stirring, and pouring and forming to obtain the partially calcined limestone-calcined clay cement-based material.
Wherein the cement is ordinary portland cement with the strength grade of 52.5; the content of kaolinite in the raw clay is 50 percent, and the main chemical components of the raw clay comprise the following components in percentage by weight: siO 2 2 ：53.84％；Al 2 O 3 ：38.07％；CaO：0.03％；Fe 2 O 3 :1.92 percent; the content of calcium carbonate in the limestone is 98 percent; the gypsum is dihydrate gypsum; the water reducing agent is a high-performance polycarboxylic acid water reducing agent, and the solid content ratio of the water reducing agent is 16%.
In examples 1 to 6, calcined clay was prepared by separately calcining raw clay at a temperature of 800 ℃ for 1 hour, and partially calcined limestone was prepared by separately calcining limestone, and the specific raw material composition was shown in table 1.
TABLE 1
Figure BDA0003254336010000061
In examples 7 to 9, calcined clay and partially calcined limestone were prepared by mixing and calcining raw clay and limestone, and the specific raw material composition is shown in table 2.
TABLE 2
Figure BDA0003254336010000071
Comparative example 1
The only difference compared to example 2 is that the raw materials of the uncalcined limestone-calcined clay cement-based material comprise: 202.5g of ordinary portland cement, 600g of calcined clay, 300g of limestone powder, 22.5g of gypsum, 431.52g of water and 22g of water reducing agent.
Comparative example 2
The only difference compared to example 2 is that the raw materials of the calcium oxide-calcined clay cement-based material comprise: 202.5g of ordinary portland cement, 600g of calcined clay, 300g of calcium oxide, 22.5g of gypsum, 431.52g of water and 49.82 g of water reducing agent.
Comparative example 3
Compared with the example 2, the difference is only that the raw materials of the pure cement-based material comprise: 1125g of ordinary portland cement and 450g of water.
The mechanical property test is carried out according to GB/T17671-1999 cement mortar strength test method, and the test results are shown in Table 3.
The porosity is tested by a mercury intrusion method, the testing instrument is a high-performance automatic mercury intrusion instrument, and the testing result is shown in figures 1-2.
TABLE 3 compressive Strength of comparative examples 1 to 3 and examples 1 to 9 at 1d, 3d, 7d and 28d
Figure BDA0003254336010000081
As can be seen from Table 3, the 28d compressive strength of the examples 1-3 and examples 7-8 of the invention is higher than that of the comparative example 1, which shows that the later strength of the system is increased by partially calcining limestone and obviously increased; the reason is that the partial calcined limestone outer layer loose calcium oxide generates calcium hydroxide when meeting water, an extra alkali environment and calcium hydroxide are provided for the system, the volcanic ash reaction characteristic of the calcined clay is promoted, and more hydration products are formed.
Comparative example 2 the strength development tendency was similar to that of examples 1 to 3, but the 28d compressive strength was lower compared to example 2 using the optimum calcination system, and the complete use of calcium oxide resulted in higher energy consumption during the preparation process.
From the examples 2, 4 to 6 and 3, it can be known that, under the condition of doping the partially calcined limestone powder prepared by the same calcination system, the calcined clay and the partially calcined limestone powder have certain compressive strength within the range of 50 to 100% instead of cement content, and when the doping amount is up to 80%, good mechanical properties can be still maintained, which indicates that the system of the invention can significantly reduce the dosage of cement on the premise of reducing the mechanical properties to a small extent.
From examples 7 to 9, it is understood that the calcination of raw clay and limestone mixture to prepare calcined clay and partially calcined limestone powder is also feasible as a substitute for cement, but the calcination conditions need to be strictly controlled to optimize the reactivity of both.
Referring to fig. 1-2, fig. 1 is a graph of the 28d cumulative pore diameter for comparative example 1 and example 2; FIG. 2 is a 28d pore diameter differential curve for comparative example 1 and example 2. As can be seen from the figure, the total porosity of example 2 is significantly reduced, only by half of the total porosity of comparative example 1, the significant reduction in porosity indicating that the microstructure of the heavily doped partially calcined limestone-calcined clay cement-based material becomes denser. In addition, the pore size obtained from the pore size differential curve is significantly smaller in example 2 than in comparative example 1, which shows that the pore structure of the large-doped partially calcined limestone-calcined clay cement-based material is significantly refined, and the pore size distribution evolves toward smaller gel pores.
Compared with the prior art, the invention has the following beneficial effects:
(1) Can replace cement with large mixing amount. The content of the partially calcined limestone and the calcined clay replacing the ordinary portland cement is 50% -90%, and the dosage of the cement can be remarkably reduced on the premise of reducing the mechanical property to a small extent.
(2) The strength is high. The 28d strength of the large-doping-amount limestone-calcined clay cement-based material is only 20.7MPa, and after partial calcined limestone is used, the 28d compressive strength is obviously improved to 49.3MPa and is improved by 138 percent.
(3) The microstructure is dense. The porosity of the large-doping-amount partially calcined limestone-calcined clay cement-based material is obviously reduced, and compared with the large-doping-amount limestone-calcined clay cement-based material with the same doping amount, the durability is better improved.
(4) Effectively reduces the emission of carbon dioxide and lowers the economic cost. Because the calcination temperature of the calcined clay is lower than the calcination temperature of the cement clinker, the calcined clay is easy to grind and has low price, the emission of carbon dioxide and the economic cost are obviously reduced by adding the large amount of the calcined clay.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.

Claims (9)

1. The partially calcined limestone-calcined clay cement-based material is characterized in that raw materials of the partially calcined limestone-calcined clay cement-based material contain gelling components, wherein the gelling components comprise calcined clay, partially calcined limestone and cement, and the total mass of the calcined clay and the partially calcined limestone accounts for 80-90% of the gelling components;
the partially calcined limestone has a core-shell structure, the outer layer of the partially calcined limestone is loose calcium oxide, and the inner layer of the partially calcined limestone is compact calcium carbonate; the content of calcium oxide in the partially calcined limestone is 50% -75%.
2. The partially calcined limestone-calcined clay cement-based material as claimed in claim 1, wherein the calcined clay is made by calcining raw clay alone at a temperature of 550 to 900 ℃, and the partially calcined limestone is made by calcining calcareous raw material alone at a temperature of 600 to 1000 ℃ for 10 to 360min.
3. The partially calcined limestone-calcined clay cement-based material of claim 2, wherein the raw clay, when calcined alone, has a calcination temperature of 800 ℃ and a calcination time of 1 hour; the calcination temperature of the calcareous raw material is 950 ℃, and the calcination time is 10min.
4. The partially calcined limestone-calcined clay cement-based material as claimed in claim 1, wherein the calcined clay and the partially calcined limestone are prepared by mixing raw clay and calcareous material uniformly and calcining at 700 to 900 ℃ for 10 to 30min.
5. The partially calcined limestone-calcined clay cement-based material as claimed in claim 4, wherein the temperature of the mixed calcination is 800 ℃ for 10min.
6. The partially calcined limestone-calcined clay cement-based material according to claim 2 or 4, wherein the raw clay has a kaolinite content comprised between 50% and 100%; the calcareous raw material is one or more of limestone, dolomite, marble, calcite, aragonite and shells.
7. The partially calcined limestone-calcined clay cement-based material according to claim 1, wherein the mass ratio of calcined clay to partially calcined limestone is 1: (0.2 to 1).
8. The partially calcined limestone-calcined clay cement-based material as claimed in claim 1, wherein said raw materials comprise, in addition to the above materials: gypsum, a water reducing agent and water.
9. A method of preparing a partially calcined limestone-calcined clay cement-based material as claimed in claim 8, comprising the steps of:
and uniformly mixing the partially calcined limestone, the calcined clay, the cement, the gypsum, the water and the water reducing agent, and pouring and molding to obtain the partially calcined limestone-calcined clay cement-based material.
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