Preparation method of cement mineral-sodium silicate composite grouting material

By using graphene oxide and nano-silica to coat glassy calcium silicate particles in cement-water glass dual-liquid grouting material, hydrated calcium silicate gel is generated, which solves the problem of unstable performance caused by uneven dispersion of water glass and improves the strength and bonding force of the grouting material.

CN119349957BActive Publication Date: 2025-10-10ZAOZHUANG MINING GRP ZHONGXING JIANAN ENG CO LTD
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Patent Information

Application Number
CN202411560052.4
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-11-04
Publication Date
2025-10-10
Estimated Expiration
2044-11-04

AI Technical Summary

Technical Problem

The performance of traditional cement-water glass two-liquid grouting material is unstable due to the uneven dispersion of water glass, which affects the strength and application range of the grouting material.

Method used

Graphene oxide and nano-silica are used to coat glassy calcium silicate particles to form a graphene oxide-glassy calcium silicate structure, and sodium silicate or potassium is generated in an alkaline solution and loaded on the surface of the glassy calcium silicate particles to form a hydrated calcium silicate gel, thereby improving the mechanical strength and bonding force of the composite grouting material.

Benefits of technology

It effectively avoids the dissociation of water glass, improves the early and late strength of the grouting material, enhances the bonding strength with the matrix, and improves the toughness and crack resistance of the grouting material.

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Abstract

The application discloses a preparation method of a cement mineral-water glass composite grouting material, and comprises the following steps: (1) dispersing graphene oxide in isopropyl alcohol, then adding glassy calcium silicate particles, stirring to uniformly coat the graphene oxide on the surface of the glassy calcium silicate particles, adding nano silicon dioxide after mixing, and then performing solid-liquid separation to obtain a solid product for standby; (2) adding the solid product into a saturated sodium hydroxide and / or potassium hydroxide solution, then heating and keeping warm, performing solid-liquid separation after completion, and obtaining sodium and / or potassium silicate-graphene oxide-glassy calcium silicate; (3) mixing the sodium and / or potassium silicate-graphene oxide-glassy calcium silicate with cement mineral tricalcium silicate, dicalcium silicate and water, and then uniformly mixing to obtain the composite grouting material. The application effectively avoids the problems of traditional cement-water glass double-liquid grouting materials, such as easy dissociation of water glass, unstable performance of the grouting material and strength deterioration.
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Description

Technical Field

[0001] The invention belongs to the technical field of cement grouting material preparation, and in particular relates to a method for preparing a cement mineral-water glass composite grouting material. Background Art

[0002] The information disclosed in this background technology section is only intended to enhance understanding of the overall background of the invention and should not necessarily be regarded as an admission or any form of suggestion that the information constitutes the prior art already known to those skilled in the art.

[0003] With the acceleration of urbanization and the continuous increase in infrastructure construction, issues such as soil and rock stability, bearing capacity, and waterproofing have become increasingly prominent, leading to the emergence of grouting technology. Grouting technology is not only used in traditional civil engineering fields, but has also gradually expanded to various fields such as underground engineering, mining, and environmental governance, promoting diversified development.

[0004] Traditionally, the main types of grouting used in engineering projects include polyurethane organic grouting and single-liquid cement grouting. Single-liquid grouting is limited in its application due to factors such as poor stability, uncontrollable gel time, susceptibility to stratification and segregation, and environmental pollution. Advances in modern materials science, particularly the application of new materials such as organic polymers and nanomaterials, have significantly improved the performance of composite grouting materials. Cement-waterglass dual-liquid grouting technology, with its advantages of controllable gel time and high early strength, is increasingly gaining widespread attention, adapting to more complex engineering requirements.

[0005] The combination of cement and water glass produces high compressive and tensile strengths, possesses excellent bonding properties, and can effectively bond with soil or rock, enhancing reinforcement effectiveness. However, cement-water glass two-liquid grouting materials suffer from localized excessive concentrations due to uneven water glass dispersion, which in turn causes water glass dissociation, leading to unstable performance and deteriorating strength development in the grouting material. This has significantly restricted the widespread application of cement-water glass two-liquid grouting materials. Summary of the Invention

[0006] To address the above problems, the present invention provides a method for preparing a cement mineral-water glass composite grouting material, which effectively solves the problem of easy dissociation and unstable performance of traditional water glass. Specifically, the technical solution of the present invention is as follows.

[0007] A method for preparing a cement mineral-water glass composite grouting material comprises the following steps:

[0008] (1) Graphene oxide is dispersed in isopropanol, and then glassy calcium silicate particles are added and stirred continuously to coat the graphene oxide on the surface of the glassy calcium silicate particles. After completion, nano-silicon dioxide is added and mixed, and solid-liquid separation is performed to obtain a solid product for use.

[0009] (2) adding the solid product to a saturated sodium hydroxide and / or potassium hydroxide solution, then heating and keeping the temperature, and performing solid-liquid separation after completion to obtain sodium silicate and / or potassium-graphene oxide-glassy calcium silicate, wherein: the graphene oxide is coated on the surface of the glassy calcium silicate particles, and the sodium silicate and / or potassium are formed by the in-situ reaction of the nano-silicon dioxide adsorbed on the surface of the graphene oxide and the surface of the glassy calcium silicate with the sodium hydroxide and / or potassium hydroxide.

[0010] (3) The sodium silicate and / or potassium-graphene oxide-glassy calcium silicate is mixed with cement mineral tricalcium silicate, dicalcium silicate and water to obtain the cement mineral-water glass composite grouting material.

[0011] Furthermore, in step (1), the graphene oxide is dispersed in isopropanol by ultrasonic dispersion. Optionally, the power of the ultrasonic dispersion is 100-300W, and the dispersion time is 30-60min.

[0012] Furthermore, in step (1), the glassy calcium silicate is obtained by mixing calcium carbonate and silicon dioxide in a molar ratio of 0.8 to 1.2:1, sintering, performing a solid-phase reaction, and then grinding. Optionally, the sintering temperature is 1650 to 1750°C, and the sintering time is 2 to 3 hours.

[0013] Furthermore, in step (1), the particle size of the glassy calcium silicate particles is 20-40 μm.

[0014] Furthermore, in step (1), when the liquid phase system is continuously stirred until it changes from light yellow to colorless and transparent, it indicates that the graphene oxide is coated on the surface of the glassy calcium silicate particles, and then the nano-silicon dioxide is added.

[0015] Furthermore, in step (1), the mass ratio of the graphene oxide, glassy calcium silicate, and nano-silicon dioxide is 1:1-3:10-25. Optionally, the particle size of the nano-silicon dioxide is 20-50 nm.

[0016] Furthermore, in step (1), the solid-liquid ratio of the graphene oxide, glassy calcium silicate, nano-silicon dioxide and isopropyl alcohol is 1 g: 5-10 ml.

[0017] Furthermore, in step (1), the solid-liquid ratio of the solid product to the saturated sodium hydroxide and / or potassium hydroxide solution is 1 g: 5-15 ml.

[0018] Furthermore, in step (2), the heating temperature is 40-60° C., and the holding time is 1-3 hours. Optionally, slow stirring is performed at a rate of 30-50 r / min during the holding process.

[0019] Furthermore, in step (3), the mass ratio of the sodium silicate and / or potassium-graphene oxide-glassy calcium silicate, tricalcium silicate, dicalcium silicate, and water is 1:0.5~0.8:0.2~0.5:0.3~0.5.

[0020] Compared with the prior art, the technical solution of the present invention has at least the following beneficial effects:

[0021] First, the present invention uniformly disperses graphene oxide and glassy calcium silicate in an isopropyl alcohol solution. Leveraging its large specific surface area, rich surface functional groups, and structural defects, graphene oxide is adsorbed onto the roughened surfaces of ground glassy calcium silicate particles, forming a graphene oxide-coated glassy calcium silicate structure. Nano-silicon dioxide is then added and adsorbed onto the defective surfaces of the graphene oxide. Some nano-silicon dioxide particles also adsorb onto the surfaces of the glassy calcium silicate particles, resulting in a layered nano-silicon dioxide-graphene oxide-glassy calcium silicate coating. This product is then added to a saturated sodium hydroxide and / or potassium hydroxide solution (alkaline solution). The silicon dioxide on the graphene oxide and glassy calcium silicate particles reacts with the alkaline solution to form sodium and / or potassium silicate (i.e., water glass), which is then loaded onto the surfaces of the corresponding carriers. Since the graphene oxide is now loaded onto the surfaces of the calcium silicate particles, the steric hindrance of the particles prevents the graphene oxide from flocculating and precipitating when exposed to the alkaline solution. When the sodium silicate and / or potassium-graphene oxide-glassy calcium silicate obtained through the above treatment is combined with the cement minerals tricalcium silicate, dicalcium silicate, and water to form a grouting material, the tricalcium silicate reacts with water to form a calcium silicate hydrate (CSH) gel and calcium hydroxide. The sodium silicate and / or potassium further react with the calcium hydroxide to form calcium silicate hydrate (Ca(OH)2 + Na2O·SiO2 / K2O·SiO2 + mH2O → CaO·SiO2·mH2O + 2NaOH / KOH). These calcium silicate hydrates help further enhance the mechanical strength of the composite grouting material. As the above reaction continues, the hydration product calcium hydroxide is continuously consumed and its concentration continuously decreases, promoting the continuous hydration of the tricalcium silicate, increasing its hydration degree, and improving the early mechanical strength of the composite grouting material. In addition, since the water glass component of the present invention is directly or indirectly loaded on the surface of the glassy calcium silicate particles, the problem of local excessive concentration caused by uneven dispersion of water glass in traditional cement-water glass two-liquid grouting materials is effectively avoided, which in turn causes the water glass to be easily dissociated, resulting in unstable performance of the grouting material and causing strength degradation.

[0022] Secondly, the NaOH / KOH formed by the above reaction can also excite the surface of the glassy calcium silicate particles to depolymerize the inert glassy silicon-oxygen tetrahedral structure on the surface to form Si(OH)3 - 、SiO2(OH)2 2- The plasma monomer can undergo a secondary reaction with the hydration product calcium hydroxide formed by the dicalcium silicate with a slow hydration start to form a calcium silicate hydrate (CSH) gel, thereby improving the later strength of the grouting material and improving the bonding force between the glassy calcium silicate particles and the grouting material matrix.

[0023] Furthermore, the graphene oxide dispersed in the grouting material provides nucleation sites for the formation of the CSH gel, thereby promoting hydration and improving the mechanical strength of the grouting material. Furthermore, the graphene oxide also increases the toughness of the grouting material, hinders crack propagation, and enhances the grouting's crack resistance. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] It should be noted that the drawings in the specification, which constitute a part of the present invention, are used to provide a further understanding of the present invention and do not constitute an improper limitation of the present invention.

[0025] Figure 1 This is a scanning electron microscope image of the cement mineral-water glass composite grouting material prepared in the following Example 1.

[0026] Figure 2 This is a compressive strength test diagram of the specimen prepared in the following Example 1.

[0027] Figure 3 This is a compressive strength test diagram of the specimen prepared in the following Example 4. DETAILED DESCRIPTION

[0028] The present invention will be further described below in conjunction with specific examples. It should be understood that these examples are intended to illustrate the present invention and are not intended to limit the scope of the invention. Unless otherwise defined, all professional and scientific terms used in the present invention are identical in meaning to those skilled in the art. The preferred implementation methods and materials described in the present invention are for demonstration purposes only. The reagents or raw materials used in the invention can be purchased and obtained through conventional means. Unless otherwise specified, the reagents or raw materials used in the present invention are used in a conventional manner in this area or according to the product specifications. Now, in conjunction with specific embodiments, the technical scheme of the present invention will be further described.

[0029] Example 1

[0030] A method for preparing a cement mineral-water glass composite grouting material comprises the following steps:

[0031] (1) Calcium oxide and silicon dioxide are mixed in a molar ratio of 1:1 and stirred evenly, and then heated to 1650°C and sintered for 3 hours. After completion, the mixture is cooled to room temperature, and the sintered product is ball-milled and sieved to obtain glassy calcium silicate particles with a particle size distribution between 20 and 40 μm, which are set aside.

[0032] (2) Graphene oxide (with a diameter distribution between 2 and 8 μm, a thickness distribution between 1 and 3 nm, and an oxygen content of 44.7%) was ultrasonically dispersed in isopropanol for 40 minutes at an ultrasonic power of 200 W. Then, the glassy calcium silicate particles were added and stirred continuously until the liquid phase system changed from light yellow to colorless and transparent. Then, nano-silicon dioxide with a particle size of 20 to 50 nm was added. The mass ratio of the graphene oxide, glassy calcium silicate, and nano-silicon dioxide was 1:2:15, and the solid-liquid ratio of the total mass of the graphene oxide, glassy calcium silicate, and nano-silicon dioxide to isopropanol was 1 g:8 ml. After stirring for 10 minutes, the mixture was filtered for solid-liquid separation. The obtained solid product was set aside.

[0033] (3) Add the solid product to a saturated sodium hydroxide solution at a ratio of 1 g:10 ml, then heat to 50°C and maintain for 2 hours while stirring continuously at a rate of 40 r / min. After completion, filter to separate the solid and liquid to obtain sodium silicate and / or potassium-graphene oxide-glassy calcium silicate for later use.

[0034] (4) The sodium silicate and / or potassium-graphene oxide-glassy calcium silicate is mixed with cement mineral tricalcium silicate, dicalcium silicate and water in a mass ratio of 1:0.6:0.35:0.4 and stirred evenly to obtain a composite grouting material.

[0035] Performance test: The composite grouting material prepared in this embodiment was prepared into a test piece (microscopic scanning electron microscope image as shown in FIG. Figure 1 Then, the early and late mechanical strength of the specimens were tested according to the Standard for Test Methods of Physical and Mechanical Properties of Concrete (GBT 50081-2019). The results are shown in Figure 2 and the following table:

[0036] .

[0037] Example 2

[0038] A method for preparing a cement mineral-water glass composite grouting material comprises the following steps:

[0039] (1) Calcium oxide and silicon dioxide are mixed in a molar ratio of 0.8:1 and stirred evenly, and then heated to 1750°C and sintered for 2 hours. After completion, the mixture is cooled to room temperature, and the sintered product is ball-milled and sieved to obtain glassy calcium silicate particles with a particle size distribution between 30 and 40 μm, which are set aside.

[0040] (2) Graphene oxide (with a diameter distribution between 2 and 8 μm, a thickness distribution between 1 and 3 nm, and an oxygen content of 44.7%) was ultrasonically dispersed in isopropanol for 60 min at an ultrasonic power of 100 W. Then, the glassy calcium silicate particles were added and stirred continuously until the liquid phase system changed from light yellow to colorless and transparent. Then, nano-silicon dioxide with a particle size of 20 to 50 nm was added. The mass ratio of the graphene oxide, glassy calcium silicate, and nano-silicon dioxide was 1:1:10, and the solid-liquid ratio of the total mass of the graphene oxide, glassy calcium silicate, and nano-silicon dioxide to isopropanol was 1 g:5 ml. After stirring for 10 min, the mixture was filtered for solid-liquid separation. The obtained solid product was set aside.

[0041] (3) Add the solid product to a saturated sodium hydroxide solution at a ratio of 1 g:5 ml, then heat to 40°C and maintain for 3 hours while stirring continuously at a rate of 50 r / min. After completion, filter to separate the solid and liquid to obtain sodium silicate and / or potassium-graphene oxide-glassy calcium silicate for later use.

[0042] (4) The sodium silicate and / or potassium-graphene oxide-glassy calcium silicate is mixed with cement mineral tricalcium silicate, dicalcium silicate and water in a mass ratio of 1:0.5:0.2:0.3 and stirred evenly to obtain a composite grouting material.

[0043] Performance test: The composite grouting material prepared in this example was prepared into test specimens, and then the early and late mechanical strength of the test specimens were tested according to the "Standard for Test Methods of Physical and Mechanical Properties of Concrete" (GBT 50081-2019). The results are shown in the following table:

[0044] .

[0045] Example 3

[0046] A method for preparing a cement mineral-water glass composite grouting material comprises the following steps:

[0047] (1) Calcium oxide and silicon dioxide are mixed in a molar ratio of 1.2:1 and stirred evenly, and then heated to 1680°C and sintered for 3 hours. After completion, the mixture is cooled to room temperature, and the sintered product is ball-milled and sieved to obtain glassy calcium silicate particles with a particle size distribution between 20 and 40 μm, which are set aside.

[0048] (2) Put the graphene oxide (diameter distribution between 2-8 pm, thickness distribution between 1-3 nm, oxygen content of 44.7%) into isopropyl alcohol and ultrasonic dispersion for 30 min, ultrasonic power of 300 W. Then add the glassy calcium silicate particles, continuously stir until the liquid phase system changes from light yellow to colorless and transparent, then add nano-silicon dioxide with a particle size of 20-50 nm, the mass ratio of graphene oxide, glassy calcium silicate, and nano-silicon dioxide = 1:3:25, and the solid-liquid ratio of the total mass of graphene oxide, glassy calcium silicate, and nano-silicon dioxide to isopropyl alcohol is 1 g:10 ml, stir for 10 min, then filter for solid-liquid separation, and the obtained solid product is ready for use.

[0049] (3) Add the solid product to the saturated sodium hydroxide solution according to the ratio of 1 g:15 ml, then heat to 60°C and keep for 1 hour, and continuously stir at a speed of 30 r / min during the incubation. After completion, filter for solid-liquid separation, and obtain sodium and / or potassium-silicate-graphene oxide-glassy calcium silicate ready for use.

[0050] (4) Mix the sodium and / or potassium-silicate-graphene oxide-glassy calcium silicate with cement minerals tricalcium silicate, dicalcium silicate, and water according to the mass ratio of 1:0.8:0.5:0.5, and stir uniformly to obtain a composite grouting material.

[0051] Performance test: prepare the composite grouting material prepared in this example into test pieces, and then test the early and late mechanical strength of the test pieces according to the “Standard Test Methods for Physical and Mechanical Properties of Concrete” (GBT 50081-2019), and the results are shown in the following table:

[0052] .

[0053] Example 4

[0054] A preparation method of a traditional cement-sodium silicate double-liquid grouting material, comprising the following steps:

[0055] (1) Mix 42.5 ordinary portland cement with water according to the water-cement ratio, and stir uniformly to form a cement slurry (A liquid).

[0056] (2) Use water glass solution (modulus 2.3, Baume degree 30°Bé) as B liquid. When in use, mix the A liquid with the B liquid according to the volume ratio of 1:1 to obtain a traditional cement-sodium silicate double-liquid grouting material.

[0057] Performance test: prepare the grouting material prepared in this example into test pieces, and then test the early and late mechanical strength of the test pieces according to the “Standard Test Methods for Physical and Mechanical Properties of Concrete” (GBT 50081-2019), and the results are shown in the following table: Figure 3As shown in the table below, it can be seen that the mechanical strength of the traditional cement-water glass two-liquid grouting material of this embodiment is significantly lower than the mechanical strength of the composite grouting material proposed in the present invention in the above-mentioned embodiments 1 to 3:

[0058] .

[0059] Example 5

[0060] A method for preparing a cement mineral-water glass composite grouting material comprises the following steps:

[0061] (1) Calcium oxide and silicon dioxide are mixed in a molar ratio of 1:1 and stirred evenly, and then heated to 1650°C and sintered for 3 hours. After completion, the mixture is cooled to room temperature, and the sintered product is ball-milled and sieved to obtain glassy calcium silicate particles with a particle size distribution between 20 and 40 μm, which are set aside.

[0062] (2) Graphene oxide (diameter distribution between 2 and 8 μm, thickness distribution between 1 and 3 nm, oxygen content of 44.7%) was ultrasonically dispersed in isopropanol for 40 minutes at an ultrasonic power of 200 W. Then, the glassy calcium silicate particles were added and stirred continuously until the liquid phase system changed from light yellow to colorless and transparent. The mass ratio of the graphene oxide to the glassy calcium silicate was 1:2, and the solid-liquid ratio of the total mass of the graphene oxide and the glassy calcium silicate to the isopropanol was 1 g:8 ml. After stirring for 10 minutes, the mixture was filtered for solid-liquid separation, and the obtained solid product was set aside.

[0063] (3) The solid product was added to a saturated sodium hydroxide solution at a ratio of 1 g:10 ml, and then heated to 50°C for 2 hours while continuously stirring at a rate of 40 r / min. After completion, the solid-liquid separation was performed by filtration to obtain graphene oxide-glassy calcium silicate for use.

[0064] (4) The graphene oxide-glassy calcium silicate is mixed with cement minerals tricalcium silicate, dicalcium silicate and water in a mass ratio of 1:0.6:0.35:0.4 and stirred evenly to obtain a composite grouting material.

[0065] Performance test: The composite grouting material prepared in this example was prepared into test specimens, and then the early and late mechanical strength of the test specimens were tested according to the "Standard for Test Methods of Physical and Mechanical Properties of Concrete" (GBT 50081-2019). The results are shown in the following table:

[0066] .

[0067] Example 6

[0068] A preparation method of a cement mineral-sodium silicate composite grouting material, comprising the following steps:

[0069] (1) The solid product (prepared by the same method as in Example 3) is added to water in a ratio of 1 g:15 ml, and then heated to 60°C for 1 hour, and stirring is continuously carried out at a speed of 30 r / min during the incubation. After completion, filtration is carried out for solid-liquid separation, and graphene oxide-glassy calcium silicate is obtained for standby.

[0070] (2) The graphene oxide-glassy calcium silicate is mixed with cement minerals tricalcium silicate, dicalcium silicate, and water in a mass ratio of 1:0.8:0.5:0.5, and then uniformly stirred to obtain the composite grouting material.

[0071] Performance test: The composite grouting material prepared in this example is prepared into a test piece, and then the early and late mechanical strengths of the test piece are tested according to the Standard Test Methods for Physical and Mechanical Properties of Concrete (GBT 50081-2019), and the results are shown in the following table:

[0072] .

[0073] Example 7

[0074] A preparation method of a cement mineral-sodium silicate composite grouting material, comprising the following steps:

[0075] (1) Graphene oxide (diameter distribution between 2-8 μm, thickness distribution between 1-3 nm, and oxygen content of 44.7%) is placed in isopropanol and ultrasonically dispersed for 60 min, and the ultrasonic power is 100 W. Then ordinary calcium silicate particles (formed by reaction of sodium silicate solution and calcium chloride) with a particle size distribution between 30-40 μm are added, continuous stirring is carried out until the liquid phase system changes from light yellow to colorless and transparent, then nano-silicon dioxide with a particle size of 20-50 nm is added, the mass ratio of graphene oxide, calcium silicate, and nano-silicon dioxide is 1:1:10, and the solid-liquid ratio of the total mass of graphene oxide, calcium silicate, and nano-silicon dioxide to isopropanol is 1 g:5 ml. After stirring for 10 min, filtration is carried out for solid-liquid separation, and the obtained solid product is reserved for standby.

[0076] (2) The solid product is added to saturated sodium hydroxide solution in a ratio of 1 g:5 ml, and then heated to 40°C for 3 hours, and stirring is continuously carried out at a speed of 50 r / min during the incubation. After completion, filtration is carried out for solid-liquid separation, and sodium and / or potassium silicate-graphene oxide-calcium silicate is obtained for standby.

[0077] (3) The sodium silicate and / or potassium-graphene oxide-calcium silicate is mixed with cement mineral tricalcium silicate, dicalcium silicate and water in a mass ratio of 1:0.5:0.2:0.3 and stirred evenly to obtain a composite grouting material.

[0078] Performance test: The composite grouting material prepared in this example was prepared into test specimens, and then the early and late mechanical strength of the test specimens were tested according to the "Standard for Test Methods of Physical and Mechanical Properties of Concrete" (GBT 50081-2019). The results are shown in the following table:

[0079] .

[0080] Example 8

[0081] A method for preparing a cement mineral-water glass composite grouting material comprises the following steps:

[0082] (1) Glassy calcium silicate particles (prepared as in Example 3) and nano-silicon dioxide with a particle size of 20 to 50 nm were ultrasonically dispersed in isopropyl alcohol for 30 minutes at an ultrasonic power of 300 W. The mass ratio of the glassy calcium silicate to the nano-silicon dioxide was 3:25, and the solid-liquid ratio of the total mass of the glassy calcium silicate and nano-silicon dioxide to the isopropyl alcohol was 1 g:10 ml. The solid-liquid separation was then performed by filtration, and the resulting solid product was set aside.

[0083] (2) Add the solid product to a saturated sodium hydroxide solution at a ratio of 1 g:15 ml, then heat to 60°C and keep warm for 1 hour. Stir continuously at a rate of 30 r / min during the holding period. After completion, filter to separate the solid and liquid to obtain a solid product for use.

[0084] (3) The solid product of step (2) is mixed with cement mineral tricalcium silicate, dicalcium silicate and water in a mass ratio of 1:0.8:0.5:0.5 and stirred evenly to obtain a composite grouting material.

[0085] Performance test: The composite grouting material prepared in this example was prepared into test specimens, and then the early and late mechanical strength of the test specimens were tested according to the "Standard for Test Methods of Physical and Mechanical Properties of Concrete" (GBT 50081-2019). The results are shown in the following table:

[0086] .

[0087] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art will be able to modify the technical solutions described in the aforementioned embodiments or replace some of the technical features therein with equivalents. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention shall be included within the scope of protection of the present invention.

Claims

1. A method for preparing a cement mineral-water glass composite grouting material, characterized in that: The steps include: (1) dispersing graphene oxide in isopropanol, then adding glassy calcium silicate particles, stirring continuously to coat the graphene oxide on the surface of the glassy calcium silicate particles, adding nano-silicon dioxide and mixing, and then performing solid-liquid separation to obtain a solid product for use; (2) adding the solid product to a saturated sodium hydroxide and / or potassium hydroxide solution, then heating and keeping the temperature, and performing solid-liquid separation after completion to obtain sodium silicate and / or potassium-graphene oxide-glassy calcium silicate, wherein: the graphene oxide is coated on the surface of the glassy calcium silicate particles, and the sodium silicate and / or potassium are formed by the in-situ reaction of the nano-silicon dioxide adsorbed on the surface of the graphene oxide and the surface of the glassy calcium silicate with the sodium hydroxide and / or potassium hydroxide; (3) The sodium silicate and / or potassium-graphene oxide-glassy calcium silicate is mixed with cement mineral tricalcium silicate, dicalcium silicate and water to obtain the cement mineral-water glass composite grouting material.

2. The preparation method of cement mineral-water glass composite grouting material according to claim 1, characterized in that: In step (1), the graphene oxide is dispersed in isopropanol by ultrasonic dispersion.

3. The preparation method of cement mineral-water glass composite grouting material according to claim 2, characterized in that: The power of the ultrasonic dispersion is 100-300W, and the dispersion time is 30-60min.

4. The method for preparing the cement mineral-water glass composite grouting material according to claim 1, wherein: In step (1), the glassy calcium silicate is obtained by mixing calcium oxide and silicon dioxide in a molar ratio of 0.8 to 1.2:1, sintering, performing solid-phase reaction, and then grinding.

5. The method for preparing the cement mineral-water glass composite grouting material according to claim 4, wherein: The sintering temperature is 1650-1750° C., and the sintering time is 2-3 hours.

6. The method for preparing the cement mineral-water glass composite grouting material according to claim 1, wherein: In step (1), the particle size of the glassy calcium silicate particles is 20-40 μm.

7. The method for preparing the cement mineral-water glass composite grouting material according to claim 1, wherein: In step (1), the nano-silica is added when the liquid phase system changes from light yellow to colorless and transparent during continuous stirring.

8. The method for preparing the cement mineral-water glass composite grouting material according to claim 1, wherein: In step (1), the mass ratio of graphene oxide, glassy calcium silicate, and nano-silicon dioxide is 1:1~3:10~25.

9. The method for preparing the cement mineral-water glass composite grouting material according to claim 1, wherein: In step (1), the particle size of the nano-silica is 20-50 nm.

10. The method for preparing the cement mineral-water glass composite grouting material according to claim 1, characterized in that: In step (1), the solid-liquid ratio of the graphene oxide, glassy calcium silicate, nano-silicon dioxide and isopropyl alcohol is 1 g: 5-10 ml.

11. The method for preparing the cement mineral-water glass composite grouting material according to claim 1, characterized in that: In step (2), the solid-liquid ratio of the solid product to the saturated sodium hydroxide and / or potassium hydroxide solution is 1 g: 5-15 ml.

12. The method for preparing the cement mineral-water glass composite grouting material according to claim 1, characterized in that: In step (2), the heating temperature is 40-60° C., and the insulation time is 1-3 hours.

13. The method for preparing the cement mineral-water glass composite grouting material according to claim 1, characterized in that: During the heat preservation process, slow stirring is performed at a rate of 30-50 r / min.

14. The method for preparing the cement mineral-water glass composite grouting material according to any one of claims 1 to 13, characterized in that: In step (3), the mass ratio of the sodium silicate and / or potassium silicate-graphene oxide-glassy calcium silicate, tricalcium silicate, dicalcium silicate, and water is 1:0.5~0.8:0.2~0.5:0.3~0.5.

Citation Information

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