CN114920473A - Multi-element low-carbon less-clinker composite cement and preparation method thereof - Google Patents

Multi-element low-carbon less-clinker composite cement and preparation method thereof Download PDF

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CN114920473A
CN114920473A CN202210754697.6A CN202210754697A CN114920473A CN 114920473 A CN114920473 A CN 114920473A CN 202210754697 A CN202210754697 A CN 202210754697A CN 114920473 A CN114920473 A CN 114920473A
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clinker
cement
low
carbon
composite cement
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林忠财
刘宇轩
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Hunan University
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Hunan University
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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
    • C04B7/02—Portland cement
    • C04B7/04—Portland cement using raw materials containing gypsum, i.e. processes of the Mueller-Kuehne type
    • 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
    • C04B7/17—Mixtures thereof with other inorganic cementitious materials or other activators with calcium oxide containing activators
    • C04B7/19—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
    • 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
    • C04B7/21—Mixtures thereof with other inorganic cementitious materials or other activators with calcium sulfate containing activators
    • 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
    • C04B7/36—Manufacture of hydraulic cements in general
    • C04B7/38—Preparing or treating the raw materials individually or as batches, e.g. mixing with fuel
    • 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

Abstract

The invention discloses a multi-element low-carbon less-clinker composite cement and a preparation method thereof. The composite cement comprises the following components in percentage by weight: portland cement clinker: 25% -50%, activated kaolin material: 15% -30%, slag: 0-50%, limestone: 2-15%, gypsum: 0 to 5 percent. The activated kaolin material is natural clay or industrial solid waste coal gangue (the kaolin content is more than or equal to 30 percent), the activation is carried out by crushing, grinding and low-temperature calcination at 600-800 ℃, and then the composite cement is prepared by batching, homogenizing and grinding. Based on the synergistic hydration effect of kaolin, limestone and slag, the consumption of the multielement low-carbon few-clinker composite cement clinker can be as low as 25%, and the composite cement clinker has the advantages of quick strength development, good later-period performance and compact microstructure, can overcome the technical defects of high carbon emission and poor performance of few-clinker cement of the conventional ordinary portland cement, can effectively consume solid wastes, reduces the cement cost, and is beneficial to low-carbon sustainable development of the cement industry.

Description

Multi-element low-carbon less-clinker composite cement and preparation method thereof
Technical Field
The invention belongs to the technical field of building materials, and particularly relates to multi-element low-carbon less-clinker composite cement and a preparation method thereof.
Background
The fuel consumption and limestone decomposition in cement production process produce a large amount of carbon dioxide, a greenhouse gas. The admixture is used for replacing cement clinker, so that the cement cost can be reduced, the energy consumption and the carbon dioxide emission can be reduced, and the low-carbon green sustainable development trend of the current cement industry is realized. According to statistics, the average substitution rate of the cement clinker in China is about 32.2%. Based on cement hydration, multi-component synergistic reaction mechanism, coagulation hardening and other physical and chemical theories, the low-carbon composite cement with less clinker and multi-component is developed, so that the performance of the composite cement can be effectively improved, and the microcosmic compactness and mechanical properties of cement concrete are improved. Under the same performance requirement, the cement clinker substitution rate can be obviously improved, and the cement clinker substitution rate has obvious advantages in energy conservation and emission reduction.
In recent years, researchers at home and abroad generally consider clay-limestone burning composite cement system (namely LC) 3 Cement) which has wide raw material sources and abundant reserves and has great potential. European patent EP2253600A1, "Portland lime cementitious boundary" discloses a clay-Limestone-cement composite ternary composite cement system, which has later-stage mechanical properties and durability comparable to those of ordinary Portland cement, and the clinker substitution rate is 50% at most, but the clinker substitution rate has the defects of slow strength development, low early strength and the like, and the application of the clinker in engineering is influenced to a certain extent. Meanwhile, when the cement content in the ternary composite cement system is further reduced, a large amount of clay and limestone which do not participate in the reaction exist in the system, so that the mechanical property of the system is remarkably reduced, and the requirement of engineering cannot be met.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide low-carbon and few-clinker composite cement and a preparation method thereof.
In order to realize the purpose, the invention forms the technical scheme of the low-carbon and few-clinker composite cement based on the synergistic hydration promotion effect of metakaolin, slag and limestone:
the multielement low-carbon less clinker composite cement comprises the following components in percentage by weight: 25-50% of silicate cement clinker, activated kaolin material: 15% -30%, slag: 0-50%, limestone: 2-15%, gypsum: 0 to 5 percent.
In the multi-element low-carbon and low-clinker composite cement, the activated kaolin material is one of activated natural clay or industrial solid waste coal gangue, and preferably, the metakaolin content of the active ingredient is more than or equal to 30%.
In the multi-element low-carbon and low-clinker composite cement, the ratio of the active ingredient metakaolin in the limestone and the activated kaolin material is 0.25-1.00.
In the multi-element low-carbon and low-clinker composite cement, the slag is granulated blast furnace slag, and preferably the specific surface area of the slag is more than or equal to 300m 2 The activity index is more than or equal to 95 percent in 28 days per kg.
The multi-element low-carbon and low-clinker composite cement is prepared by the following steps:
step 1) crushing the activated kaolin material until the particle size is less than 10-20mm, ball-milling the crushed activated kaolin material at the rotating speed of 450r/min for 5-40min to form powder until the residue is less than 10% of that of a square-hole sieve with the particle size of 80 mu m, raising the temperature to 800 ℃ at the speed of 5-20 ℃/min by using a muffle furnace, and preserving the heat for 1-2h to excite the activity of the activated kaolin material to obtain the activated kaolin material containing metakaolin.
And 2) carrying out batching, homogenizing and grinding on 25-50% of portland cement clinker, 15-30% of activated kaolin material, 0-50% of slag, 2-15% of limestone and 0-5% of gypsum to obtain the multi-element low-carbon and clinker-less composite cement.
The steps of burdening, homogenizing and grinding the multi-element low-carbon less-clinker composite cement in the step 2) can be carried out according to one of the following methods:
method 1) grinding first and then mixing: according to the weight proportion, the ground portland cement clinker, the activated kaolin material, the slag, the limestone and the gypsum are uniformly mixed to obtain the multi-element low-carbon low-clinker composite cement, and the fineness of the multi-element low-carbon low-clinker composite cement is less than 10% after passing through 80 mu m square holes.
Method 2) mixing and grinding: and (2) mixing and grinding ungrinkled portland cement clinker, activated kaolin material, slag, limestone and gypsum according to the weight proportion to obtain the multi-element low-carbon less-clinker composite cement, wherein the fineness of the multi-element low-carbon less-clinker composite cement is less than 10% after passing through 80 mu m square holes.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention uses a plurality of admixtures to prepare the low-carbon cement, and can reduce the consumption of cement clinker by 75 percent while meeting the performance requirement, thereby obviously reducing the production cost of the cement and the emission of carbon dioxide.
2. The active kaolin material used in the invention has wide raw material sources, can effectively utilize solid wastes such as coal gangue, muck and the like, and is beneficial to the reduction of the solid wastes and the resource utilization.
3. The multi-element low-carbon less-clinker composite cement prepared by the invention has the advantages of high early strength, quick strength development, high later-stage rupture strength and high compressive strength, and can be widely applied to structural materials such as buildings, pavements and the like.
Drawings
FIG. 1 is a thermogravimetric analysis diagram of a multi-element low-carbon less-clinker composite cement and activated kaolin material-limestone composite cement;
FIG. 2 is an X-ray diffraction analysis chart of multi-component low-carbon less-clinker composite cement and activated kaolin material-limestone composite cement;
FIG. 3 is a diagram of the results of isothermal hydration heat of multi-component low-carbon less-clinker composite cement and activated kaolin material-limestone composite cement;
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the following description taken in conjunction with the accompanying drawings.
Example 1: the multi-element low-carbon less-clinker composite cement has a clinker substitution rate of 65 percent and comprises the following components in percentage by weight: 35% of portland cement clinker, 15% of activated kaolin material, 3.8% of limestone, 41.2% of slag and 5% of gypsum.
The activated kaolin material is calcined coal gangue, and the kaolin content of the activated kaolin material is 98%.
The portland cement clinker is a concrete admixture detection reference cement which accords with GB 8076- 2 The slag is S95 level granulated blast furnace slag powder, the grain size is 300 meshes, and limestone and gypsum are analytically pure reagents.
The preparation method of the multi-element low-carbon less-clinker composite cement comprises the following steps:
step 1) preparing activated kaolin materialCrushing the material to the diameter of less than or equal to 20mm, grinding for 30min at 450r/min by using a planetary all-directional ball mill, containing the material by using a corundum crucible, calcining for 2h at 800 ℃ by using a muffle furnace at the temperature rise rate of 10 ℃/min, wherein the specific surface area of the activated kaolin material is 450m 2 /kg。
And 2) preparing portland cement clinker, activated kaolin material, limestone, slag and gypsum according to the weight percentage, and mixing for 2 hours by using a dry powder premixer until the raw materials are uniform to prepare the multi-element low-carbon and low-clinker composite cement.
Example 2: the multi-element low-carbon less-clinker composite cement has a clinker substitution rate of 75%, and comprises the following components in percentage by weight: 25% of portland cement clinker, 15% of activated kaolin material, 3.8% of limestone, 51.2% of slag and 5% of gypsum.
The activated kaolin material is calcined coal gangue, and the kaolin content of the activated kaolin material is 98%.
The portland cement clinker is a concrete admixture detection reference cement conforming to GB 8076-2008, the strength grade is 42.5, and the specific surface area is 350m 2 The slag is S95-grade granulated blast furnace slag powder, the granularity is 300 meshes, and the limestone and the gypsum are analytically pure reagents.
The preparation method of the multi-element low-carbon less-clinker composite cement comprises the following steps:
step 1) crushing the activated kaolin material to the diameter of less than or equal to 20mm, grinding for 30min at 450r/min by using a planetary all-directional ball mill, containing the material by using a corundum crucible, calcining for 2h at 800 ℃ by using a muffle furnace at the temperature rise rate of 10 ℃/min, wherein the specific surface area of the activated kaolin material is 450m 2 /kg。
And 2) preparing portland cement clinker, activated kaolin material, limestone, slag and gypsum according to the weight percentage, and mixing for 2 hours by using a dry powder premixer until the raw materials are uniform to prepare the multi-element low-carbon and low-clinker composite cement.
The principle of the invention is as follows: the limestone and aluminum phase in the cement can generate synergistic effect, so that the hydration product calcium sulphoaluminate is promoted to be converted into calcium carbonate aluminate with more stable thermodynamics and lower density, the content of ettringite is indirectly stabilized, and the later microstructure of the set cement is compacted; meanwhile, the activity of the mineral powder is rapidly excited in the early stage of hydration (1-3 days) in a composite cement system, so that the early strength of the multi-element low-carbon and low-clinker composite cement is rapidly developed; in addition, the synergistic effect of the higher territory, the limestone and the mineral powder enhances the cementing effect among microscopic products, and effectively improves the mechanical property, the macroscopic bending resistance and the compressive strength of the microscopic structures.
To verify the technical effects of the examples, comparative examples 1, 2 and 3 were set, wherein comparative example 1 was pure cement, comparative example 2 was slag cement having a clinker substitution rate of 65%, comparative example 3 was activated kaolin material-limestone composite cement having the same contents of activated kaolin material and limestone as those of example 1, and the slag in example 1 was replaced with quartz, which is an inert admixture. The superior characteristics of the properties of the multi-component low-carbon and low-clinker composite cement proposed herein are illustrated by comparing different cement properties.
Comparative example 1: the pure cement comprises 100 percent of portland cement clinker which is standard cement for detecting concrete admixture meeting GB 8076-2008, and the strength grade is 42.5.
Comparative example 2: the slag cement has a clinker substitution rate of 65 percent and comprises the following components in percentage by weight: 35% of portland cement clinker, 60% of slag and 5% of gypsum.
The portland cement clinker is a concrete admixture detection reference cement which accords with GB 8076- 2 The slag is S95-grade granulated blast furnace slag powder, the granularity is 300 meshes, and the gypsum is an analytically pure reagent.
The preparation method of the slag cement comprises the following steps:
step 1) preparing portland cement clinker, slag and gypsum according to the weight percentage, and mixing for 2 hours by using a dry powder premixer until the raw materials are uniform to prepare the slag cement.
Comparative example 3: the activated kaolin material-limestone composite cement has a clinker substitution rate of 65 percent and comprises the following components in percentage by weight: 35% of portland cement clinker, 15% of activated kaolin material, 3.8% of limestone, 41.2% of quartz and 5% of gypsum.
The portland cement clinker is a concrete admixture detection reference cement conforming to GB 8076-2008, the strength grade is 42.5, and the specific surface area is 350m 2 300 meshes per kg, quartz, limestone and gypsum are analytical pure reagents.
The preparation method of the activated kaolin material-limestone composite cement comprises the following steps:
step 1) crushing the activated kaolin material to the diameter of less than or equal to 20mm, grinding for 30min at 450r/min by using a planetary all-directional ball mill, containing the material by using a corundum crucible, calcining for 2h at 800 ℃ by using a muffle furnace at the temperature rise rate of 10 ℃/min, wherein the specific surface area of the activated kaolin material is 450m 2 /kg。
And 2) preparing portland cement clinker, activated kaolin material, limestone, quartz and gypsum according to the weight percentage, and mixing for 2 hours by using a dry powder premixing instrument until the raw materials are uniform to prepare the activated kaolin material-limestone composite cement.
According to the method for testing the strength of cement mortar in GB/T17671-1999, prismatic cement mortar test pieces with the size of 40mm multiplied by 160mm are manufactured, the water cement ratio is 0.5, the cement mortar ratio is 1: 3, curing the poured test piece in a standard curing box (the temperature is 20 +/-1 ℃ and the relative humidity is 95%) for 24 hours, removing the mould, then continuously putting the test piece into the standard curing box to be cured to a specified age, and testing the mechanical properties of the cement of the examples and the comparative examples, wherein the test results are shown in table 1, and the hydration and microstructure research results of the examples 1 and the comparative examples 3 are shown in fig. 1-3.
TABLE 1
Figure BDA0003721971340000051
Figure BDA0003721971340000061
As can be seen from Table 1, the multi-component low-carbon and low-clinker composite cement of the present patent has significantly improved early strength and later compressive flexural strength compared with slag cement (comparative example 2) and activated kaolin material-limestone composite cement (comparative example 3), and is close to or even exceeds the pure cement test piece (comparative example 1). In addition, under the condition of 75% clinker substitution rate, the compressive strength of the multi-element low-carbon low-clinker composite cement can reach 24.2MPa in 3 days and 50.7MPa in 28 days, and the applicability and the remarkable carbon reduction potential of the multi-element low-carbon low-clinker composite cement in practical industrial application are shown.
FIGS. 1, 2 and 3 show the results of thermogravimetric analysis, X-ray diffraction analysis and isothermal hydration heat release of the multi-component low-carbon and low-clinker composite cement (example 1) and the activated kaolin material-limestone composite cement, respectively. The results show that the activity of the mineral powder in the multi-element low-carbon and clinker-less composite cement is quickly excited in 1-3 days in the early stage of cement hydration, and meanwhile, the aluminum phase and the limestone in the composite cement generate a synergistic effect to generate low-density calcium carbonate aluminate, so that the refinement of microscopic pores of the cement is promoted, and the multi-element low-carbon and clinker-less composite cement has the excellent characteristics of high substitution rate, early strength and high strength compared with the existing low-carbon and clinker-less cement.
The above description is only a preferred embodiment of the present invention, but should not be interpreted as limiting the scope of the present invention. It should be noted that various changes and modifications can be made by those skilled in the art without departing from the spirit of the invention, and these changes and modifications are all within the scope of the invention. The protection scope of the present invention should be subject to the appended claims.

Claims (6)

1. A multi-element low-carbon less-clinker composite cement. The composite cement is characterized by comprising the following components in percentage by weight: 25-50% of portland cement clinker, activated kaolin material: 15% -30%, slag: 0-50%, limestone: 2-15%, gypsum: 0 to 5 percent.
2. The multi-element low-carbon low-clinker composite cement as claimed in claim 1, wherein the activated kaolin material is one of natural clay or industrial solid waste coal gangue, and the content of metakaolin as an active ingredient is not less than 30%.
3. The multi-element low-carbon and low-clinker composite cement as claimed in claim 1, wherein the ratio of the active ingredient metakaolin in the limestone and activated kaolin material is 0.25-1.00.
4. The multi-element low-carbon low-clinker composite cement as claimed in claim 1, wherein the slag is granulated blast furnace slag with a specific surface area of more than or equal to 300m 2 The activity index is more than or equal to 95 percent in 28 days per kg.
5. A method for preparing the multi-component low-carbon and low-clinker composite cement as claimed in claims 1 to 4, characterized by comprising the following steps:
step 1) crushing the activated kaolin material until the particle size is less than 10-20mm, ball-milling the crushed material at the rotating speed of 450r/min for 5-40min to form powder, raising the temperature to 800 ℃ at the speed of 5-20 ℃/min by using a muffle furnace, and preserving the heat for 1-2h to excite the activity of the powder, thereby obtaining the activated kaolin material containing metakaolin.
And 2) carrying out batching, homogenizing and grinding on 25-50% of portland cement clinker, 15-30% of activated kaolin material, 0-50% of slag, 2-15% of limestone and 0-5% of gypsum to obtain the multi-element low-carbon and clinker-less composite cement.
6. The method for preparing the multi-element low-carbon and low-clinker composite cement of claim 4, wherein the batching, homogenizing and grinding method in the step 2) is one of the following two methods:
(1) grinding and mixing: and uniformly mixing the ground Portland cement clinker, activated kaolin material, slag, limestone and gypsum according to the weight mixture ratio to obtain the multi-element low-carbon and clinker-less composite cement, wherein the fineness of the multi-element low-carbon and clinker-less composite cement is less than 10% after passing through a square hole with the size of 80 mu m.
(2) Mixing and grinding: and (2) mixing and grinding ungrinkled portland cement clinker, activated kaolin material, slag, limestone and gypsum according to the weight proportion to obtain the multi-element low-carbon less-clinker composite cement, wherein the fineness of the multi-element low-carbon less-clinker composite cement is less than 10% after passing through 80 mu m square holes.
CN202210754697.6A 2022-06-30 2022-06-30 Multi-element low-carbon less-clinker composite cement and preparation method thereof Pending CN114920473A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115403340A (en) * 2022-09-21 2022-11-29 江苏科技大学 Preparation method of high early strength and high corrosion resistance composite aluminate cement-based material

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115403340A (en) * 2022-09-21 2022-11-29 江苏科技大学 Preparation method of high early strength and high corrosion resistance composite aluminate cement-based material

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