CN113149540A - Grouting material based on industrial graphene oxide and preparation method thereof - Google Patents
Grouting material based on industrial graphene oxide and preparation method thereof Download PDFInfo
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- CN113149540A CN113149540A CN202110048532.2A CN202110048532A CN113149540A CN 113149540 A CN113149540 A CN 113149540A CN 202110048532 A CN202110048532 A CN 202110048532A CN 113149540 A CN113149540 A CN 113149540A
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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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- 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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/70—Grouts, e.g. injection mixtures for cables for prestressed concrete
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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
- 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
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Abstract
The invention discloses a grouting material based on industrial graphene oxide and a preparation method thereof, belongs to the technical field of building materials, and is suitable for underground grouting engineering. Comprises the following components: the ratio of the superfine portland cement to the fly ash to the dispersion liquid is 4:1: 3; the dispersion liquid is prepared by mixing industrial-grade graphene oxide and a polycarboxylic acid water reducing agent. The invention reduces the cost of grouting materials and improves the fluidity of the slurry by adding the fly ash. The growth of a hydration product in slurry is promoted and a pore structure is optimized by means of industrial-grade graphene oxide, so that the mechanical loss of a grouting material caused by replacement of part of cement powder by fly ash is reinforced. Thereby preparing the grouting material with higher flow property, stronger mechanical property and lower price. Compared with cement paste, the fluidity of the grouting material disclosed by the invention is improved by 8.50% -8.64%; the mechanical property is improved by 11.40-29.50% in 28 days.
Description
Technical Field
The invention belongs to the technical field of building materials, is suitable for underground grouting engineering, and particularly relates to a grouting material based on industrial graphene oxide and a preparation method thereof.
Background
The grouting material is a main substance playing a role in consolidation and filling in the fractured rock mass, and plays a role in enhancing the mechanical strength and the impermeability of the fractured rock mass. The commonly used grouting materials include silicate cement grouting materials and chemical grouting materials. The chemical grouting material has low viscosity and good groutability, can be injected into micro-pore cracks, but has higher cost, lower strength, poorer durability and larger environmental pollution; the ordinary portland cement grouting material has the advantages of high strength, good durability, no toxicity, no odor, convenient material source and low price, but has the defects of high energy consumption, great carbon dioxide emission, more generated building wastes, larger particle size of ordinary cement, more coarse particles, poor stability of grout, incapability of injecting tiny cracks and the like in the preparation process; the superfine portland cement as one kind of portland cement has small cement grain fineness and excellent permeability, and may be injected into small crack of rock. The development of a grouting material with high strength and low cost is urgently needed.
Disclosure of Invention
The invention provides a graphene oxide-based grouting material and a preparation method thereof, and aims to solve the problem of economic cost caused by poor fluidity and high consumption of the existing superfine portland cement grouting material.
In order to solve the problems of the prior art, the invention adopts the technical scheme that:
a graphene oxide-based grouting material comprises the following components: the ratio of the superfine portland cement to the fly ash to the dispersion liquid is 4:1: 3; the dispersion liquid is prepared by mixing industrial-grade graphene oxide and a polycarboxylic acid water reducing agent.
The improved composition is characterized in that the dispersion liquid is prepared by mixing 2500 parts by weight of water, 2 parts by weight of industrial-grade graphene oxide and 16 parts by weight of polycarboxylic acid water reducing agent.
The improvement is that the polycarboxylic acid water reducing agent dispersion liquid is formed by mixing 2500 parts by weight of water and 16 parts by weight of polycarboxylic acid water reducing agent.
The improvement is that the average grain diameter of the superfine portland cement is 6-18.6 microns, and the average grain diameter of the fly ash is 38-48 microns.
The preparation method of the graphene oxide-based grouting material comprises the following steps:
step 1, weighing the components in parts by weight, and uniformly stirring and mixing the superfine portland cement and the fly ash to prepare dry powder;
dissolving industrial-grade graphene oxide and a polycarboxylate superplasticizer in water to prepare a solution, and performing ultrasonic dispersion in an ice water environment in an ultrasonic cell disruption instrument to obtain an industrial-grade graphene oxide dispersion liquid; the graphene oxide dispersion liquid is placed in an ice-water mixture environment in the ultrasonic process, so that the dispersion liquid is prevented from being overheated by energy generated in the ultrasonic process, and the property of the graphene oxide after ultrasonic dispersion is ensured;
and 3, mixing and stirring the dry powder and the industrial-grade graphene oxide dispersion liquid uniformly to obtain the grouting material.
The improvement is that the ultrasonic time of the ultrasonic crusher used for ultrasonic dispersion in the step 2 is 10min, and the power is 150W.
As a refinement, the water-cement ratio of the injected material in step 3 is 0.6.
The industrial graphene oxide and the fly ash cooperate to play roles in reducing the cost and enhancing the fluidity and the strength of the superfine cement-based grouting material under the dispersion action of the polycarboxylic acid water reducing agent.
Among these, with regard to the effect of reducing costs and enhancing flowability: on one hand, the fly ash replaces part of the superfine portland cement with extremely low cost, so that the problem of high cost caused by high consumption of the superfine portland cement is reduced; on the other hand, the fly ash particles are in a smooth spherical shape on a microscopic scale, and after the fly ash particles are mixed into cement slurry, the fly ash particles can play a role in lubrication in the slurry, so that the mechanical friction effect among cement particles is reduced, and the fluidity of the slurry is improved. In addition, the use of fly ash relieves the pressure of industrial waste on the ecological environment.
The underground grouting engineering has the following requirements on materials: high fluidity, i.e., a relatively large water-cement ratio is required so that the grouting material can be filled into rock fractures of a certain depth. Secondly, the cost is low, and the price control is very important because the engineering quantity of grouting is huge. Therefore, with respect to enhancing the strength of the grouting material: (1) the industrial graphene oxide has excellent mechanical properties and bears stress in a grouting material; (2) the industrial graphene oxide has active functional groups and high specific surface area, can be used as nucleation sites of hydration products, and promotes hydration reaction; (3) industrial graphene oxide is used as a nano material to fill pores and compact the pore structure; (4) the industrial graphene oxide is bonded with the grouting material to form a compact structure, so that crack propagation is hindered.
Has the advantages that:
according to the high-strength and high-economy grouting material based on the industrial graphene oxide, the strength and the fluidity of the grouting material can be effectively improved and the cost of the grouting material is reduced under the synergistic effect of the dispersion effect of the industrial graphene oxide in the polycarboxylic acid water reducing agent and the fly ash. Compared with cement paste, the fluidity of the grouting material is improved by 8.50-8.64%; the 28-day compressive strength is improved by 14.96-29.50 percent; the tensile strength is improved by 22.61-27.56%; the cohesive force is improved by 12.57 to 14.65 percent; the internal friction angle is improved by 11.40 to 13.40 percent.
Drawings
FIGS. 1(a) and 1(b) are electron microscope scanning images of the 28-day-old micro-topography of the pure cement slurry;
FIGS. 1(c) and 1(d) are electron microscope scanning images of 28-day-age micro-morphology of composite cement slurry containing 20% of fly ash;
FIGS. 2(a) and 2(b) are electron microscope scanning images of 28-day-age micro-morphology of fly ash composite cement slurry without graphene oxide;
and FIGS. 2(c) and 2(d) are 28-day-age microscopic morphology electron microscope scanning images of fly ash composite cement slurry containing 0.08 wt% of graphene oxide.
Detailed Description
The principles and features of this invention are described below in conjunction with embodiments, which are included to explain the invention and not to limit the scope of the invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1 (control without fly ash)
The graphene oxide-based grouting material comprises, by weight, 5 parts of superfine portland cement and 3 parts of a dispersion liquid. The dispersion liquid is prepared by mixing 2500 parts of water, 2 parts of industrial graphene oxide and 16 parts of a polycarboxylic acid water reducing agent.
(1) Dissolving the industrial graphene oxide and the polycarboxylate superplasticizer in water to prepare a solution, and performing ultrasonic dispersion in an ultrasonic cell disruptor to prepare an industrial graphene oxide dispersion liquid;
(2) uniformly stirring and mixing the industrial graphene oxide dispersion liquid and superfine portland cement to prepare a grouting material; wherein the water-cement ratio in the grouting material slurry is 0.6;
(3) and curing the grouting material in a curing box for 28 days, wherein the temperature of the standard curing box is 20 +/-5 ℃, and the relative humidity is 95%.
Example 2 (control group with graphene oxide and fly ash added simultaneously)
A graphene oxide-based grouting material comprises, by weight, 4 parts of superfine portland cement, 1 part of fly ash and 3 parts of a dispersion liquid. The dispersion liquid is prepared by mixing 2500 parts of water, 2 parts of industrial graphene oxide and 16 parts of a polycarboxylic acid water reducing agent.
The preparation method of the graphene oxide-based grouting material comprises the following steps:
(1) stirring and mixing the superfine portland cement and the fly ash uniformly to prepare dry powder;
(2) dissolving the industrial graphene oxide and the polycarboxylate superplasticizer in water to prepare a solution, and performing ultrasonic dispersion in an ultrasonic cell disruptor to prepare an industrial graphene oxide dispersion liquid;
(3) uniformly stirring and mixing the dry powder and the industrial graphene oxide dispersion liquid to prepare a grouting material; wherein the water-cement ratio in the grouting material is 0.6;
(4) maintaining the slurry of the grouting material in a maintenance box for 28d of age; wherein the standard curing box temperature is 20 + -5 deg.C and the relative humidity is 95%.
Comparative example 1 (control group without graphene oxide and fly ash)
The grouting material comprises, by weight, 5 parts of superfine portland cement and 3 parts of polycarboxylic acid water reducer dispersion liquid. The polycarboxylic acid water reducing agent dispersion liquid is formed by mixing 2500 parts by weight of water and 16 parts by weight of a polycarboxylic acid water reducing agent.
The preparation method of the grouting material comprises the following steps:
(1) dissolving the polycarboxylic acid water reducer in water to prepare a solution, and stirring the solution in a magnetic stirrer to prepare a polycarboxylic acid water reducer dispersion liquid;
(2) uniformly stirring and mixing the polycarboxylic acid water reducer dispersion liquid and the superfine portland cement to prepare a grouting material; wherein the water-cement ratio in the grouting material is 0.6.
(3) Maintaining the slurry of the grouting material in a maintenance box for 28d of age; wherein the standard curing box temperature is 20 + -5 deg.C and the relative humidity is 95%.
Comparative example 2 (control group without graphene oxide)
The grouting material comprises, by weight, 4 parts of superfine portland cement, 1 part of fly ash and 3 parts of polycarboxylic acid water reducer dispersion liquid. The average grain diameter of the superfine portland cement is 6-18.6 microns, and the average grain diameter of the fly ash is 38-48 microns.
The preparation method of the grouting material comprises the following steps:
(1) stirring and mixing the superfine portland cement and the fly ash uniformly to prepare dry powder;
(2) dissolving the polycarboxylic acid water reducer in water to prepare a solution, and stirring the solution in a magnetic stirrer to prepare a polycarboxylic acid water reducer dispersion liquid;
(3) uniformly stirring and mixing the dry powder and the polycarboxylic acid water reducing agent dispersion liquid to prepare a grouting material; wherein the water cement ratio of the grouting material slurry is 0.6.
(4) The slip of grouted material was cured in a curing box for 28 days of age. Wherein the standard curing box temperature is 20 + -5 deg.C and the relative humidity is 95%.
The grouting materials of examples 1 to 2 and comparative examples 1 to 2 were subjected to strength, fluidity and test, and the results are shown in table 1. Wherein, the strength test: (1) and (3) testing the compressive strength: the test model is a standard cylinder of 50 multiplied by 100mm, the 28d compressive strength is measured on a cylinder sample by using a universal material testing machine, and the displacement rate is 0.1 mm/min. Each batch was tested in parallel for 3 times and the average intensity value was recorded; (2) brazilian split test: the test specimen is a standard 50X 25mm disc, and the 28d tensile strength is measured on a disc sample by using a universal material tester, and the displacement rate is 0.1 mm/min. Each batch was tested in parallel for 3 times and the average intensity value was recorded; (3) angle-variable shear test: the test model is a standard cylinder of 50 multiplied by 50mm, the 28d shear strength is measured on a cylinder sample by using a universal material testing machine, and the displacement rate is 0.1 mm/min. Each batch was subjected to 3 parallel tests at angles of 45 °, 50 ° and 60 °, and the average intensity values were recorded; testing the fluidity; during the test, the mold is filled without tamping, the truncated cone circular mold is lifted to allow slurry to naturally flow, the slurry diffusion radius is measured once in the direction of 45 degrees, and the average value of the diffusion radius is taken.
As shown in FIG. 1, the scanning electron microscope result of the cured surface of the grouting material after 28 days of curing shows that when the slurry does not contain fly ash, the surface structure of the slurry is compact and uniform, and no large holes are generated, as shown in FIG. 1 (a). With the addition of fly ash, the surface of the slurry gradually becomes porous and microcracks increase, as shown in FIG. 1 (b). The method is consistent with the test result of a mechanical test, and proves that the pore structure of the cement-based grouting material is changed along with the doping of the fly ash, the porosity of the grouting material is increased, and the mechanical property of the material is further reduced. The fly ash causes the grouting material to become loose and porous, and the reasons are as follows: the fly ash can generate a large amount of Al after being dissolved3+When the fly ash is mixed into the cement-based material, the fly ash is dissolved during hydration reaction, so that a large amount of Al is generated3+Released in cement paste solution, Al3+Will preferentially react with Ca2+Reaction to generate calciumVanadium stone, Ca in cement paste solution at this time2+The content is reduced, so that the hydration reaction is inhibited to a certain extent, and the generation of calcium silicate hydrate (C-S-H) is prevented; in addition, because of the low activity of the fly ash, the fly ash is doped into the cement slurry and is difficult to react with other substances to form an integral structure, so that the contact surface between the fly ash and hydration products becomes extremely fragile, the integral material becomes broken, the mechanical strength is reduced, and the existence of the fly ash causes the connection between the hydration products to be damaged, and the integrity of the hydration products is influenced.
Fig. 2 is a microscopic representation diagram of a grouting material containing 20% of fly ash after no graphene oxide is doped and after graphene oxide is doped. As shown in fig. 2 (a): when the slurry does not contain graphene oxide, the pores on the surface of the slurry are more, the shapes of hydration products mainly show needle shapes and flower shapes, and the needle-shaped hydration products have more content and are interwoven together. After the graphene oxide is mixed, the shape of the hydration product is changed into a polyhedral shape, which shows that the graphene oxide can promote the formation of the hydration product, the shape of the hydration product is changed, so that the hydration product forms a regular and ordered polyhedral shape, the polyhedral hydration products are stacked together, holes of the slurry are filled, a compact structure is formed, and the porosity of the slurry is reduced, as shown in fig. 2 (b).
TABLE 1 mechanical Properties test Table for grouting materials of examples 1-2 and comparative examples 1-2
Table 2 shows the fluidity of the grouting materials obtained according to different formulations
As can be seen from tables 1 and 2, the strength and the fluidity of the grouting material can be effectively improved and the cost of the grouting material is reduced under the dispersion effect of the industrial graphene oxide in the polycarboxylate water reducing agent and the synergistic effect of the fly ash. Compared with cement paste, the fluidity of the grouting material is improved by 8.50-8.64%; the 28-day compressive strength is improved by 14.96-29.50 percent; the tensile strength is improved by 22.61-27.56%; the cohesive force is improved by 12.57 to 14.65 percent; the internal friction angle is improved by 11.40 to 13.40 percent. Of note are two groups of comparative examples 2-3: 20% of cement is replaced by fly ash, and industrial graphene oxide is added to make up for the loss of the strength of a sample caused by the fly ash, so that the difference between the compressive strength and the cohesive force of a grouting material is not more than 1%, the tensile strength and the internal friction angle can be improved by nearly 10%, and the fluidity is improved by 6.9%. The fact that a small amount of fly ash and industrial graphene oxide are added in a certain proportion can not only replace cement to be used as a grouting material and not influence the final reinforcing performance of slurry, but also can further improve the fluidity of the slurry.
Although the present invention has been described with reference to the specific embodiments, it should be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
Claims (7)
1. The graphene oxide-based grouting material is characterized by comprising the following components in parts by weight: the ratio of the superfine portland cement to the fly ash to the dispersion liquid is 4:1: 3; the dispersion liquid is prepared by mixing industrial-grade graphene oxide and a polycarboxylic acid water reducing agent.
2. The graphene oxide-based grouting material as claimed in claim 1, wherein the dispersion is prepared by mixing 2500 parts by weight of water, 2 parts by weight of industrial graphene oxide and 16 parts by weight of polycarboxylic acid water reducer.
3. The graphene oxide-based grouting material of claim 1, wherein the polycarboxylic acid water reducer dispersion is prepared by mixing 2500 parts by weight of water and 16 parts by weight of polycarboxylic acid water reducer.
4. The graphene oxide-based grouting material according to claim 1, wherein the average particle size of the superfine portland cement is 6-18.6 μm, and the average particle size of the fly ash is 38-48 μm.
5. The preparation method of the graphene oxide-based grouting material based on claim 1 is characterized by comprising the following steps:
step 1, weighing the components in parts by weight, and uniformly stirring and mixing the superfine portland cement and the fly ash to prepare dry powder;
dissolving industrial-grade graphene oxide and a polycarboxylate superplasticizer in water to prepare a solution, and performing ultrasonic dispersion in an ice water environment in an ultrasonic cell disruption instrument to obtain an industrial-grade graphene oxide dispersion liquid;
and 3, mixing and stirring the dry powder and the industrial-grade graphene oxide dispersion liquid uniformly to obtain the grouting material.
6. The method for preparing the graphene oxide-based grouting material according to claim 5, wherein the ultrasonic time of the ultrasonic crusher used in the ultrasonic dispersion in the step 2 is 10min, and the power is 150W.
7. The method for preparing the graphene oxide-based grouting material according to claim 5, wherein the water-cement ratio of the grouting material in step 3 is 0.6.
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| CN116217173A (en) * | 2023-03-07 | 2023-06-06 | 北京交通大学 | Novel high-performance green grouting water-blocking material, preparation method and application thereof |
| CN116789406A (en) * | 2023-03-11 | 2023-09-22 | 南通大学 | Grouting material based on modified cement of fly ash coated by carbon nano tube and preparation method thereof |
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| CN115368076A (en) * | 2022-08-24 | 2022-11-22 | 广州市岩土勘测设计有限公司 | Novel grouting material for water-rich fractured zone stratum and preparation method thereof |
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| CN115745558B (en) * | 2022-11-10 | 2023-09-08 | 煤炭科学研究总院 | Graphene oxide clay cement grouting material and preparation method thereof |
| CN116217173A (en) * | 2023-03-07 | 2023-06-06 | 北京交通大学 | Novel high-performance green grouting water-blocking material, preparation method and application thereof |
| CN116789406A (en) * | 2023-03-11 | 2023-09-22 | 南通大学 | Grouting material based on modified cement of fly ash coated by carbon nano tube and preparation method thereof |
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