CN109592938B - Cement-based nano porous material and preparation method thereof - Google Patents
Cement-based nano porous material and preparation method thereof Download PDFInfo
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- CN109592938B CN109592938B CN201811618998.6A CN201811618998A CN109592938B CN 109592938 B CN109592938 B CN 109592938B CN 201811618998 A CN201811618998 A CN 201811618998A CN 109592938 B CN109592938 B CN 109592938B
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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
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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
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Abstract
The invention provides a cement-based nano porous material and a preparation method thereof. The preparation method comprises the following steps of mixing bentonite and water in a mass ratio of 1: 2-50, and uniformly stirring to obtain bentonite slurry; mixing cement and water in a mass ratio of 1: 0-2, and uniformly stirring to obtain cement paste; mixing bentonite slurry and cement slurry in any volume ratio, and uniformly stirring to obtain intermediate slurry; and curing the intermediate slurry, and then drying to obtain the cement-based nano porous material. The cement-based nano-porous material comprises the material prepared by the method. The invention has the advantages of simple process, low cost, controllable material structure, wide raw material source and wide material application.
Description
Technical Field
The invention relates to the field of building materials, in particular to a cement-based nano porous material and a preparation method thereof.
Background
And partial nano pores, namely partial nano-sized capillary pores and C-S-H gel pores, exist in the cement-based material. Wherein the C-S-H gel porosity of the fully hydrated portland cement paste accounts for about 16%. The content of nano-scale capillary pores is influenced by the water consumption, and the excessive water can improve the content of the nano-scale capillary pores to a certain extent, but can also cause the pore diameter of the capillary pores to be enlarged and the proportion of the nano-scale capillary pores to be reduced. Therefore, it is difficult to efficiently construct nanopores in large quantities by merely increasing the excess free water or increasing the C-S-H gel content. Due to the limitation of the content of the nano-pores, the hardened cement paste still shows higher thermal conductivity.
Disclosure of Invention
In view of the deficiencies in the prior art, it is an object of the present invention to address one or more of the problems in the prior art as set forth above. For example, it is an object of the present invention to provide a cement-based nanoporous material capable of having a large number of nanopores and a method for preparing the same.
In order to achieve the above objects, an aspect of the present invention provides a method for preparing a cement-based nanoporous material. The preparation method comprises the following steps of mixing bentonite and water in a mass ratio of 1: 2-50, and uniformly stirring to obtain bentonite slurry; mixing cement and water in a mass ratio of 1: x, and uniformly stirring to obtain cement paste, wherein x is more than 0 and less than or equal to 2; mixing bentonite slurry and cement slurry in any volume ratio, and uniformly stirring to obtain intermediate slurry; and curing the intermediate slurry, and then drying to obtain the cement-based nano porous material.
The invention also provides a preparation method of the cement-based nano porous material. The preparation method comprises the following steps of mixing bentonite and water in a mass ratio of 1: 2-50, and uniformly stirring to obtain bentonite slurry; mixing bentonite slurry and cement in a volume ratio of 10-99: 1-90, and uniformly stirring to obtain intermediate slurry; and curing the intermediate slurry, and then drying to obtain the cement-based nano porous material.
According to an exemplary embodiment of the present invention, 0.12 < x ≦ 2.
According to an exemplary embodiment of the present invention, when the bentonite slurry and the cement slurry are mixed, the volume ratio of the bentonite slurry to the cement slurry is 10-99: 1-90.
According to an exemplary embodiment of the present invention, the particle size of the bentonite may be below 150 μm.
According to an exemplary embodiment of the present invention, the bentonite may include a modified bentonite capable of being converted into a gel.
According to an exemplary embodiment of the present invention, the method further comprises the step of standing after obtaining the bentonite slurry to fully hydrate or swell the bentonite.
In still another aspect, the present invention provides a cement-based nanoporous material comprising the material prepared by the preparation method as described above. The volume of the holes in the cement-based nano porous material is less than 90%, and the holes are uniformly distributed in the material. The pore diameter of the pores can be below 100 nm.
Compared with the prior art, the invention has the advantages of simple process, low cost, controllable material structure, wide raw material source and wide material application.
Drawings
The above and other objects and features of the present invention will become more apparent from the following description taken in conjunction with the accompanying drawings, in which:
FIG. 1 shows a schematic flow diagram of a method of preparing a cement-based nanoporous material in an exemplary embodiment of the invention;
FIG. 2 shows a microscopic scanning electron microscope image of a cement-based nanoporous material cured for 24 hours;
FIG. 3 shows a microscopic scanning electron micrograph of the cement-based nanoporous material after 28 days of curing;
figure 4 shows a graph comparing a cement-based nanoporous material with a prior art cement material.
Detailed Description
Hereinafter, the cement-based nanoporous material and the method for preparing the same according to the present invention will be described in detail with reference to the accompanying drawings and exemplary embodiments.
The occupation ratio of nanometer-scale pores in the conventional cement-based material is less; conventional techniques rely on excess free water or increased C-S-H gel content to effectively build nanopores in cement-based materials in large quantities. And the montmorillonite has an interlayer structure similar to that of C-S-H gel, and water molecules easily enter the interlayer under the action of interlayer cations and the hydration energy of the bottom surface of a crystal layer, so that a multilayer or single-layer montmorillonite sheet layer is easily formed under the condition of sufficient water absorption. The montmorillonite sheet is easy to react with cement hydrate, and is beneficial to preventing the montmorillonite sheet from rearranging. And the montmorillonite can carry a large amount of water, can provide water for pores of the cement-based material, and forms a large amount of pore spaces, thereby providing existing spaces for the montmorillonite microstructure. Namely, the fully hydrated montmorillonite not only can provide water for forming cement-based capillary pores, but also can be delaminated and assembled in the capillary pores to refine and divide the capillary pores; in addition, the montmorillonite sheet layer is rich in a large amount of hydroxyl which can react with cement hydration products to generate interaction, and the structural rearrangement of the montmorillonite microstructure during conventional drying is avoided, so that a large amount of porous materials with a nano-pore structure are formed.
Therefore, the invention provides a cement-based nano porous material taking cement and bentonite as raw materials and a preparation method thereof.
The invention provides a preparation method of a cement-based nano porous material. Fig. 1 shows a schematic flow diagram of a method for preparing a cement-based nanoporous material in an exemplary embodiment of the invention.
In an exemplary embodiment of the present invention, the method for preparing the cement-based nanoporous material may include the steps of:
mixing bentonite and water in a mass ratio of 1: 2-1: 50, and uniformly stirring to obtain bentonite slurry, as shown in step S01 in figure 1. The particle size of the bentonite may be 150 μm or less, for example, 0.03 to 70 μm, and further, for example, 0.5 to 10 μm. The pore size of the product can be effectively controlled by the concentration of the bentonite slurry and the particle size of the bentonite, if the particle size of the bentonite is small, the lamella is small, and the space formed by the overlap joint of the dissociated lamella is small, so that the pores of the obtained product are smaller, for example, a nano-pore material with the nano-pore diameter of 70nm and the porosity of more than 70 percent can be prepared by the general bentonite with the particle size of 1 micron. The stirring time and the stirring speed are not particularly required, and the stirring time is uniform, and can be 0.8-1.5 h, such as 1 h.
Mixing and stirring water and cement in a mass ratio of 0-2: 1 to obtain cement paste, as shown in step S02 in FIG. 1. In other words, the cement may be mixed with water to obtain cement paste, or only cement; in the case of cement alone, the cement paste is cement. Further, the mass ratio of water to cement may be 0.12 to 2.0, for example 0.8. The stirring time and speed are not particularly required, as long as the stirring time and speed are uniform, for example, the stirring time can be 50-70 s, and the stirring speed can be 350-450 r/min.
Mixing the bentonite slurry and the cement slurry (or cement) in any volume ratio, and uniformly stirring to obtain an intermediate slurry, as shown in step S03 in FIG. 1. For example, bentonite slurry and cement slurry with the volume ratio of 0.001-99.999: 99.999-0.001 can be mixed; further, the volume ratio of the bentonite slurry to the cement slurry can be 10-99: 1-90, and further can be 40-80: 20-60. Wherein, the stirring time and the stirring speed have no special requirements as long as blockless homogeneous cement slurry can be obtained; for example, the stirring time may be 90s and the stirring rate may be 400 r/min. The volume ratio of the bentonite slurry to the cement slurry is the most main influence factor for pore structure construction, so that the volume ratio of the bentonite slurry to the cement slurry is controlled within the range, so that the cement material can fully construct nano micropores.
Curing the intermediate slurry, and then drying to obtain the cement-based nanoporous material, as shown in step S04 in fig. 1. Wherein, the curing can enable the hardening and the strength of the material to be increased, the curing temperature can be 16-28 ℃, and the relative humidity can be 85-95%; further, the temperature can be 20 +/-2 ℃, and the relative humidity can be 90%, so that the strength and the hardness of the material can be better increased. The drying aims to remove water and make holes appear, and if the water cannot be removed without drying, the holes are filled with the water; the drying can comprise conventional drying, for example, drying at 30-120 ℃ until the sample quality is not changed; vacuum freeze drying or CO may also be used2Supercritical drying until the drying time is no longer changed by mass.
In this example, the bentonite may be composed of montmorillonite, quartz and illite. Wherein the mass fraction of the montmorillonite can be 5-100%, the mass fraction of the quartz can be below 95%, and the mass fraction of the illite can be below 95%.
Further, the mass ratio of Si/(Al + Mg) in the bentonite may be 1.6 to 1.8, for example, 1.69.
The bentonite may be a modified bentonite such as sodium bentonite, organic bentonite, aerogel slurry, as long as it is capable of being converted into a gel, i.e., it may be initially in a solution state and may be converted into a gel state later.
In the embodiment, after the bentonite slurry is obtained, standing for 20-28 h, for example, 24h, can be selected to completely hydrate and expand the bentonite.
In this example, any cement can be used as the cement raw material of the present invention, and the raw material range is wide. For example, ordinary portland cement can be used; for another example, the cement may have a particle size of less than 100 μm, such as 50 ± 40 μm.
In the process of preparing the cement paste, the temperature of the environment can be room temperature, for example, 18-26 ℃.
In this embodiment, the curing method may include curing in an environment with a humidity of at least 95% at 20 ℃, air curing (in air), autoclave curing (0.1 to 1.1MPa), or steam curing (in a steam environment at 30 to 90 ℃).
The curing time can be carried out according to actual conditions, such as 24h, 7 days, 28 days, 56 days, 120 days and the like. The longer the curing time, the more the pore structure is increased, i.e. the volume fraction of the nano-pores in the material and the volume of the nano-pores are increased. FIG. 2 shows a microscopic scanning electron microscope image of a cement-based nanoporous material cured for 24 hours; figure 3 shows a microscopic scanning electron micrograph of the cement-based nanoporous material after 28 days of curing. It can be seen from FIG. 2 that the cement hydration product rarely grows on the smectite sheet, and from FIG. 3 it can be seen that the cement hydration product grows on the smectite sheet more in 28 days, and this hydration product grows on the smectite sheet and more prevents the smectite from returning to its original state when dried, thereby preserving the pore structure.
In this embodiment, the curing can be divided into two stages, wherein in the first stage, the intermediate slurry is placed in a mold, covered with a preservative film to prevent the water from evaporating too fast, and cured for a period of time; the curing time can be 60-80 h, for example 72 h. In the second stage, the sample is removed from the grinding tool and then maintained.
The invention provides a cement-based nano porous material. The material may include a material prepared by the above-described method.
In another exemplary embodiment of the present invention, the cement-based nanoporous material may consist of a solid phase and pores, which are uniformly distributed in the material.
In this embodiment, the solid phase may be cement or concrete.
The solid phase mineral phase may include calcium hydroxide, calcium carbonate, C-S-H, C-A-S-H, montmorillonite, and the like. The solid phase may have various shapes, such as needle, sheet, and coiled foil, and each shape has different sizes.
In this embodiment, the volume ratio of the pores in the cement-based nanoporous material can be less than 90%. The cement-based nano-porous material can comprise pores with the pore diameter of more than 100nm and pores with the pore diameter of less than 100nm, wherein the volume of the pores with the pore diameter of less than 100nm accounts for more than 70 percent of the volume of the total pores. The pore diameter of the pores of the cement-based nano porous material can be controlled below 100nm, such as 10-80 nm.
Compared with the traditional visible hole material, the cement-based nano material has smaller hole diameter, and the thinning of the hole diameter is beneficial to reducing the uneven stress under the load condition. Fig. 4 shows a comparison graph of a cement-based nanoporous material and a prior cement material, wherein A, B and C represent the surface of the prior cement material, a represents the surface of foam concrete, B represents a cement-based nanoporous material with an air pore-micro/nano composite pore structure, C represents the surface of EPS foam concrete, and D represents the surface of the cement-based nanoporous material of the present invention, and the pore diameter of the cement-based nanoporous material of the present invention is very small by comparison. The pore diameter is actually the evolution from harmful pores to harmless pores from visible pores to nano pores, most of the current common pore materials are visible pore materials, and the mechanical property is lower than that of a cement-based nano pore material.
In this example, the thermal conductivity of the cement-based nanoporous material was 0.55W/mK or less, and further 0.3W/mK or less. The pore diameter of the cement-based nano porous material is smaller than the free path of air molecules, so that the air heat conductivity coefficient is greatly reduced, and the introduction of the nano porous structure greatly increases the heat transfer path, so that the cement-based nano material has lower heat conductivity coefficient.
The strength of the cement-based nano porous material can be 0.1-120 MPa.
The cement-based nano porous material can be applied to multiple fields, such as heat preservation and insulation, road and waste pipeline backfilling, heavy metal and nuclide adsorption, catalyst carriers, wastewater treatment, explosion resistance, buffering and energy absorption, penetration resistance and the like.
The application can be cast in situ, and various shapes can be formed to meet the application requirements. The general heat preservation and insulation is a wall body and a heat preservation plate; the road energy absorption and shock absorption can also use a prefabricated plate, and can also be integrally cast in place; backfilling is cast-in-place and pouring is carried out; the adsorbent is generally made into spherical or columnar blocks for adsorption, and the pipeline requirement of liquid passing is met; the waste water treatment is generally a product, placed in the waste water, or the product is placed in a pipeline, the latter being granulated and filled in the pipeline; the anti-explosion, buffering, energy absorption and penetration resistance can be cast in place into any shape, and can also be prefabricated into any shape and spliced in blocks.
The above-mentioned application can be added into fibre, ceramsite and zeolite, etc., and also can be used alone.
In summary, the cement-based nanoporous material and the preparation method thereof of the invention have the advantages that:
(1) the preparation method is simple and convenient, the cost is low, and the material source is wide.
(2) Under the condition of the same density of the existing cement-based material, the strength of the cement-based nano porous material is higher.
(3) Under the condition of the same density of the existing cement-based material, the cement-based nano porous material has low heat conductivity coefficient and excellent heat preservation and insulation capacity.
(4) The cement-based nano porous material has large pore volume, small pore diameter and large specific surface area, and the pore-forming agent (i.e. montmorillonite) has a certain humidity regulating function, so that the cement-based nano porous material has a better humidity regulating effect compared with other materials.
(5) The cement-based nano porous material is an inorganic non-metallic material, the pore-forming agent can contain water, and the cement-based material can also contain water, so that the cement-based nano porous material has the properties of fire prevention and flame retardance.
(6) The cement-based nano-porous material has small and many pore diameters, and more energy is dissipated through the material, so that the material has shock resistance and energy absorption capacity. The efficiency of the reference foam concrete and the aerated concrete is more than 50 percent higher than that of the reference foam concrete and the aerated concrete.
(7) The pore diameter of the cement-based nano-porous material can be adjusted according to practical application.
(8) When the method is applied to backfill, compared with the existing air entraining process (bubbles are in a thermodynamically unstable state and change all the time, so that the final material design and performance are influenced), the backfill can be a cast-in-place process, and the backfill is only performed after the final material design and performance are fully poured, so that the method is more stable and simple.
Although the present invention has been described above in connection with exemplary embodiments, it will be apparent to those skilled in the art that various modifications and changes may be made to the exemplary embodiments of the present invention without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (7)
1. The preparation method of the cement-based nano porous material is characterized by comprising the following steps of:
mixing bentonite and water in a mass ratio of 1: 2-50, and uniformly stirring to obtain bentonite slurry, wherein the particle size of the bentonite is below 150 microns;
mixing cement and water in a mass ratio of 1: x, and uniformly stirring to obtain cement paste, wherein x is more than 0.12 and less than or equal to 0.8;
mixing bentonite slurry and cement slurry in a volume ratio of 40-80: 20-60, and uniformly stirring to obtain intermediate slurry;
and curing the intermediate slurry, and then drying to obtain the cement-based nano porous material.
2. The preparation method of the cement-based nano porous material is characterized by comprising the following steps of:
mixing bentonite and water in a mass ratio of 1: 2-50, and uniformly stirring to obtain bentonite slurry, wherein the particle size of the bentonite is below 150 microns;
mixing bentonite slurry and cement in a volume ratio of 40-80: 20-60, and uniformly stirring to obtain intermediate slurry;
and curing the intermediate slurry, and then drying to obtain the cement-based nano porous material.
3. The method for the preparation of cement-based nanoporous material according to claim 1 or 2, wherein the bentonite comprises a modified bentonite capable of being transformed into a gel.
4. The method for preparing a cement-based nanoporous material according to claim 1 or 2, wherein the method further comprises the steps of:
after the bentonite slurry is obtained, standing to fully hydrate or expand the bentonite.
5. A cement-based nanoporous material, characterized in that the cement-based nanoporous material comprises a material prepared by the method of preparation of a cement-based nanoporous material according to claim 1 or 2.
6. The cement-based nanoporous material according to claim 5, wherein the cement-based nanoporous material comprises a solid phase and pores, wherein the volume fraction of the pores is below 90%, and the pores are uniformly distributed in the material.
7. The cement-based nanoporous material according to claim 5, wherein the volume of the pores having a pore diameter of 100nm or less accounts for more than 70% of the total pore volume.
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| CN112456955B (en) * | 2020-12-01 | 2022-06-03 | 西南科技大学 | Basic magnesium sulfate cement-based lightweight porous material and preparation method thereof |
| CN113603410A (en) * | 2021-05-21 | 2021-11-05 | 西南科技大学 | Modified bentonite ultra-low shrinkage cement-based nano porous material and preparation method thereof |
| CN115140987B (en) * | 2022-05-13 | 2023-06-27 | 西南科技大学 | Porous material based on construction waste slurry and preparation method thereof |
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