An inorganic two-liquid slurry and its preparation method

Abstract

This application relates to the technical field of inorganic two-component slurries, specifically disclosing an inorganic two-component slurry and its preparation method. The inorganic two-component slurry disclosed in this application consists of component A and component B. Component A includes: 30-40 parts cement powder, 5-10 parts silicon-based material, 2-8 parts ethylene / vinyl acetate copolymer powder, and 2-10 parts modified montmorillonite. The modified montmorillonite is prepared by reacting montmorillonite, sodium carboxymethyl cellulose, water, and phosphonic acid substances at a temperature of 50-60°C in the dark for 2-3 hours. Component B includes: 50-60 parts water, 0.5-1.0 parts polycarboxylate superplasticizer, 0.2-0.5 parts defoamer, and 0.5-1.5 parts film-forming aid. This application also provides a method for preparing the above-mentioned inorganic two-component slurry. The inorganic two-component slurry material obtained using the technical solution of this application has good setting properties, compressive strength, and impermeability.

Description

Technical Field

[0001] This application relates to the technical field of inorganic two-liquid slurries, specifically to an inorganic two-liquid slurry and its preparation method. Background Technology

[0002] Inorganic two-component grouts are important engineering materials with wide applications in construction fields such as buildings, tunnels, and subways. Traditional methods for preparing inorganic two-component grouts typically employ a single chemical reaction system, making it difficult to achieve precise control over material properties. Furthermore, commercially available inorganic two-component grouts often suffer from long setting times, low early strength, and unstable later-stage strength. Therefore, traditional inorganic two-component grouts have significant performance limitations and cannot meet the complex and ever-changing requirements of engineering construction.

[0003] Therefore, a novel inorganic two-liquid slurry is needed to solve these problems. Summary of the Invention

[0004] In order to shorten the setting time of inorganic two-liquid slurry and improve its early strength, this application provides an inorganic two-liquid slurry and its preparation method.

[0005] This application provides an inorganic two-component slurry, which is composed of component A and component B in a volume ratio of 8.5-9.5:1; The A component specifically includes the following components by weight: 90-110 parts water, 30-40 parts cement powder, 5-10 parts silicon-based material, 12-18 parts ethylene / vinyl acetate copolymer powder, and 2-10 parts modified montmorillonite. The preparation method of the modified montmorillonite is as follows: by weight, 15-20 parts of montmorillonite and 2-5 parts of sodium carboxymethyl cellulose are dispersed in 45-55 parts of water, 5-10 parts of phosphonic acid substances are added, and the mixture is stirred thoroughly to carry out the reaction at a temperature of 50-60℃ for 2-3 hours in the dark. After filtration, drying, and pulverization, the modified montmorillonite is obtained. The phosphonic acid is selected from one or more of aminotrimethylenephosphonic acid, 2-hydroxyphosphonoacetic acid, sodium hexametaphosphate, and sodium tripolyphosphate; The B component specifically includes the following components in parts by weight: 50-60 parts water, 0.5-1.0 parts polycarboxylate superplasticizer, 0.2-0.5 parts defoamer, and 0.5-1.5 parts additives.

[0006] In the technical solution provided in this application, montmorillonite is modified using phosphonic acid substances with abundant phosphate functional groups and sodium carboxymethyl cellulose, which has adhesive and filling effects. This can generate hydroxyl and phosphate active groups on the surface of inorganic nanoparticles, reducing the viscosity of the montmorillonite structure itself. This results in good bonding between the modified montmorillonite and the cement powder, silicon-based materials, and ethylene / vinyl acetate copolymer powder components in the slurry system. At the same time, the synergistic effect of the phosphonic acid substances and sodium carboxymethyl cellulose makes the generated active groups stable, thereby effectively shortening the setting time of the inorganic two-liquid slurry and improving the early strength of the inorganic two-liquid slurry. In order to improve the stability of the coupling effect between montmorillonite particles and phosphonic acid substances and carboxymethyl cellulose, this application needs to control the amount of each component within the above-mentioned range.

[0007] The inorganic two-component slurry prepared in this application has strong surface bonding between component A and component B. When the two are mixed, a dense curing film can be formed quickly. Furthermore, the modified montmorillonite can block the capillary channels of the slurry, isolating its surface from the air. During application, it has high bonding strength and, through the effects of embedding and interfacial barrier, enables the material sample to have high impermeability.

[0008] Preferably, component A specifically includes the following components in parts by weight: 32-38 parts cement powder, 6-8 parts silicon-based material, 14-17 parts ethylene / vinyl acetate copolymer powder, and 4-8 parts modified montmorillonite.

[0009] Preferably, the viscosity of the sodium carboxymethyl cellulose is 800-1200 mPa·s.

[0010] Preferably, the average particle size of the montmorillonite is 100-500 nm.

[0011] Preferably, the phosphonic acid substance is composed of a mixture of aminotrimethylenephosphonic acid and sodium hexametaphosphate in a weight ratio of 17:1-5.

[0012] Experimental analysis shows that the present application selects aminotrimethylene phosphonic acid and sodium hexametaphosphate in a weight ratio of 17:1-5 to form phosphonic acid substances, and then prepares modified montmorillonite, which can further improve the compressive strength and impermeability of the material.

[0013] Preferably, the silicon-based material is selected from one or more of SH-9501 silicone resin, SH-9602 silicone resin, and SH-5202S silicone resin.

[0014] Preferably, in component B, the auxiliary agent is selected from one or more of turpentine oil, diacetone alcohol, ethylene glycol, and ethylene glycol butyl ether.

[0015] Furthermore, in component B, the additive is composed of a mixture of turpentine oil and ethylene glycol in a weight ratio of 1-5:20.

[0016] In some specific implementations, the weight ratio of turpentine oil to ethylene glycol in the additive is 1-2:20, 1-3:20, 1-4:20, 2-3:20, 2-4:20, 2-5:20, 3-4:20, 3-5:20, or 4-5:20.

[0017] In one specific implementation, the weight ratio of turpentine oil to ethylene glycol in the additive can also be 1:20, 2:20, 3:20, 4:20, or 5:20.

[0018] Experimental analysis shows that by adding an additive composed of turpentine and ethylene glycol in the above weight ratio to component B, the compressive strength and impermeability of the inorganic two-liquid slurry material obtained in this application are further improved.

[0019] Preferably, in component B, the defoamer is selected from one or more of P803, SPA-102, SPA-202, and 201 methyl silicone oil.

[0020] Secondly, this application provides a method for preparing the above-mentioned inorganic two-liquid slurry, specifically including the following steps: Mix all the raw materials of component A, stir with a stirrer until they are evenly mixed, and then add water to obtain component A; Add polycarboxylate superplasticizer and defoamer to water, keep the temperature at 20-30℃ for 10-20 minutes, then add the additives and continue the reaction for 20-40 minutes to end the reaction and obtain component B; Mix component A and component B at a volume ratio of 8.5-9.5:1 to obtain the finished product.

[0021] In summary, the technical solution of this application has the following effects: The inorganic two-liquid slurry material obtained using the technical solution provided in this application, after mixing component A and component B, reaches initial setting (i.e., loss of fluidity) within 130-158 seconds and final setting (i.e., internal hardening) within 249-290 seconds. The mixed material exhibits a compressive strength of not less than 14.2 MPa at 1 hour, not less than 20.3 MPa at 7 days, and not less than 24.8 MPa at 28 days; and a permeability resistance of not less than 0.85 MPa. These test results demonstrate that the inorganic two-liquid slurry material obtained using the technical solution provided in this application possesses excellent setting properties, compressive strength, and permeability resistance.

[0022] The inorganic two-component slurry prepared in this application is used as a reinforcement material in construction fields such as buildings, tunnels, and subways. Due to its strong fluidity, the inorganic two-component slurry can effectively enter cracks for sealing. It also has a short setting time and fast hardening speed after use, resulting in good reinforcement effect. Furthermore, the early compressive strength of the material after solidification is high, and the reinforced construction material is complete and hard, which can better bond to form an integral structure and meet the usage requirements.

[0023] In the process of preparing modified montmorillonite, this application further improves the performance of inorganic two-liquid slurry materials by screening and optimizing the types of carboxymethyl cellulose and phosphonic acid substances, and using the prepared modified montmorillonite as raw material.

[0024] In the preparation of component B, this application further improves the performance of inorganic two-liquid slurry materials by screening and optimizing the types of additives. Detailed Implementation

[0025] The cement powder used in this application is PO42.5 silicate cement with a fineness of 800 mesh; the silicon-based material was purchased from Hubei Longsheng Sihai New Material Co., Ltd.; the ethylene / vinyl acetate copolymer powder and ethylene tert-carbonate / vinyl acetate / ethylene copolymer homopolymer powder were purchased from Guangzhou Yuanye Industrial Co., Ltd.; and sodium carboxymethyl cellulose was purchased from Shanghai Yuanye Biotechnology Co., Ltd.

[0026] All other raw materials and reagents can be obtained commercially.

[0027] The present application will be further described in detail below with reference to embodiments, comparative examples and performance test results. These embodiments should not be construed as limiting the scope of protection claimed in this application. Example

[0028] Examples 1-3 Examples 1-3 each provide an inorganic two-liquid slurry.

[0029] The difference in the above embodiments is that the amount of each raw material component in the inorganic two-liquid slurry is different, as shown in Table 1.

[0030] The specific preparation process of the inorganic two-liquid slurry in the above embodiments is as follows: According to the formula requirements shown in Table 1, weigh out the corresponding weight parts of each raw material component; Preparation of modified montmorillonite: 17g of montmorillonite (average particle size 300±50nm) and 3g of sodium carboxymethyl cellulose (model C104985, viscosity 800-1200mpa.s) were dispersed in 50g of water. 8g of phosphonic acid (composed of aminotrimethylene phosphonic acid and sodium hexametaphosphate in a weight ratio of 17:3) were added. The mixture was stirred thoroughly to carry out the reaction at 55℃ for 2.5h in the dark. After filtration, drying, and pulverization, modified montmorillonite with a particle size of 50±10μm was obtained. Mix all the raw materials of component A and stir with a stirrer until they are evenly mixed. Then add 100g of water to obtain component A. Control the speed at 1000±200r / min and the stirring time at 20±5min. Add 0.75g of polycarboxylate superplasticizer and 0.3g of defoamer to water, keep the mixture at 25℃ for 15 minutes, then add 1g of additive (the additive is composed of turpentine oil and ethylene glycol in a weight ratio of 3:20) and continue to keep the mixture at 25℃ for 30 minutes. The reaction is then stopped to obtain component B. Mix component A and component B at a volume ratio of 9:1 to obtain the finished product.

[0031] Table 1. Dosage of each raw material component in component A of inorganic two-liquid slurry Example 4-12 Examples 4-12 each provide an inorganic two-liquid slurry.

[0032] The difference between the above embodiments and Embodiment 1 is that the preparation method of modified montmorillonite in inorganic two-liquid slurry is different, as detailed below.

[0033] In Example 4: 15g of montmorillonite and 2g of sodium carboxymethyl cellulose (model C104985, viscosity 800-1200 mPa·s) were dispersed in 50g of water, and 10g of phosphonic acid (composed of aminotrimethylene phosphonic acid and sodium hexametaphosphate in a weight ratio of 17:3) were added. The mixture was stirred thoroughly to carry out the reaction at 55℃ for 2.5h in the dark. After filtration, drying, and pulverization, modified montmorillonite with a particle size of 50±10μm was obtained.

[0034] In Example 5: 20g of montmorillonite and 5g of sodium carboxymethyl cellulose (model C104985, viscosity 800-1200 mPa·s) were dispersed in 50g of water, and 5g of phosphonic acid (composed of aminotrimethylene phosphonic acid and sodium hexametaphosphate in a weight ratio of 17:3) were added. The mixture was stirred thoroughly to carry out the reaction at 55℃ for 2.5h in the dark. After filtration, drying, and pulverization, modified montmorillonite with a particle size of 50±10μm was obtained.

[0035] In Example 6: Sodium carboxymethyl cellulose (model C104984, viscosity 300-800 mPa·s) was used instead of sodium carboxymethyl cellulose (model C104985, viscosity 800-1200 mPa·s).

[0036] In Example 7: an equal amount of sodium carboxymethyl cellulose (model C104978, MW250000, viscosity 1500-3100 mPa.s) was used.

[0037] In Example 8, an equal amount of 2-hydroxyphosphonoacetic acid was used as a phosphonic acid.

[0038] In Example 9: a phosphonic acid substance was composed of a mixture of 2-hydroxyphosphonoacetic acid and sodium hexametaphosphate in a weight ratio of 17:3.

[0039] In Example 10: a phosphonic acid substance was composed of aminotrimethylene phosphonic acid and sodium hexametaphosphate in a weight ratio of 17:7.

[0040] In Example 11: a phosphonic acid substance was composed of aminotrimethylene phosphonic acid and sodium hexametaphosphate in a weight ratio of 17:5.

[0041] In Example 12: a phosphonic acid substance was composed of aminotrimethylene phosphonic acid and sodium hexametaphosphate in a weight ratio of 17:1.

[0042] The remaining components, the amounts of each component, and the preparation method of the inorganic two-liquid slurry are the same as those in Example 1 in the above embodiments.

[0043] Examples 13-16 Examples 13-16 each provide an inorganic two-liquid slurry.

[0044] The difference between the above embodiments and Embodiment 1 is that the types of adjuvants in component B are different, as detailed below.

[0045] In Example 13: the additive is composed of a mixture of diacetone alcohol and ethylene glycol in a weight ratio of 3:20.

[0046] In Example 14: the additive was composed of turpentine oil and ethylene glycol butyl ether in a weight ratio of 3:20. In Example 15: the additive is composed of turpentine oil and ethylene glycol in a weight ratio of 7:20.

[0047] In Example 16: the additive is composed of turpentine oil and ethylene glycol in a weight ratio of 5:20.

[0048] The remaining components, the amounts of each component, and the preparation method of the inorganic two-liquid slurry are the same as those in Example 1 in the above embodiments.

[0049] Comparative Example Comparative Example 1 This comparative example provides an inorganic two-liquid slurry.

[0050] The difference between this comparative example and Example 2 is that the amount of each raw material component in the inorganic two-liquid slurry is different, as shown in Table 1.

[0051] In this comparative example, the remaining components, the amounts of each component, and the preparation method of the inorganic two-liquid slurry are all the same as in Example 1.

[0052] Comparative Examples 2-5 Comparative Examples 2-5 each provide an inorganic two-liquid slurry.

[0053] The differences between the above comparative examples and Example 1 are as follows.

[0054] In Comparative Example 2: an equal amount of ethylene carbonate / vinyl acetate / ethylene copolymer powder was used instead of ethylene / vinyl acetate copolymer powder.

[0055] In Comparative Example 3, an equal amount of unmodified montmorillonite (average particle size of 300±50nm) was used to replace modified montmorillonite.

[0056] In Comparative Example 4: The modified montmorillonite was prepared as follows: 17g of montmorillonite (average particle size of 300±50nm) and 3g of sodium carboxymethyl cellulose (model C104985, viscosity of 800-1200mpa.s) were dispersed in 50g of water, 8g of phosphonic acid was added, and the mixture was stirred thoroughly to carry out the reaction at 55℃ for 2.5h in the dark. After filtration, drying, and pulverization, modified montmorillonite with a particle size of 50±10μm was obtained. In Comparative Example 5: The modified montmorillonite was prepared as follows: 25g of montmorillonite (average particle size of 300±50nm) and 1g of sodium carboxymethyl cellulose (model C104985, viscosity of 800-1200mpa.s) were dispersed in 50g of water, and 15g of phosphonic acid (composed of aminotrimethylene phosphonic acid and sodium hexametaphosphate in a weight ratio of 17:3) were added. The mixture was stirred thoroughly to carry out the reaction at 55℃ for 2.5h in the dark. After filtration, drying, and pulverization, modified montmorillonite with a particle size of 50±10μm was obtained.

[0057] The remaining components, amounts of each component, and preparation methods of the inorganic two-liquid slurry in the above comparative examples are the same as those in Example 1.

[0058] Performance testing (1) Condensation time Mix 300g of reference cement (P.I.42.5 silicate cement), 6g of admixture and 87g of water until homogeneous to obtain cement paste; then test according to the method disclosed in standard GB / T1346-2011.

[0059] In this test, the initial spread of cement paste was controlled at (260±10) mm.

[0060] The tests were conducted according to the methods published in standard GB / 8076-2008.

[0061] (2) Compressive strength The tests were conducted according to the methods published in standard GB / T50081-2019.

[0062] (3) The performance of the above materials shall be tested in accordance with the standards specified in GB / T23445 "Polymer Cement Waterproof Coating" and JG 26 "Exterior Wall Inorganic Building Coating".

[0063] Test results are shown in Table 2.

[0064] Table 2 Performance test results of inorganic two-liquid slurries in Examples 1-16 and Comparative Examples 1-6 Referring to Table 2, by comparing the test results of Examples 1-16 and Comparative Examples 1-5, the inorganic two-liquid slurry material obtained using the technical solution provided in this application, after mixing component A and component B, reaches initial setting (i.e., loses fluidity) within 130-158 seconds and final setting (i.e., internal hardening) within 249-290 seconds. The mixed material exhibits a compressive strength of not less than 14.2 MPa at 1 hour, not less than 20.3 MPa at 7 days, and not less than 24.8 MPa at 28 days; and a permeability resistance of not less than 0.85 MPa. The above test results indicate that the inorganic two-liquid slurry material obtained using the technical solution of this application possesses excellent setting performance, compressive strength, and permeability resistance.

[0065] By comparing the test results of Examples 1-3 with Comparative Example 1, it was found that the amount of each raw material has a significant impact on the performance of the inorganic two-liquid slurry material. This application optimizes the amount of each component to prepare a material with excellent performance.

[0066] In Comparative Example 2, the inorganic two-liquid slurry material obtained by replacing the ethylene / vinyl acetate copolymer powder with an equal amount of tert-vinyl carbonate / vinyl acetate / ethylene copolymer powder had poor performance; while the inorganic two-liquid slurry material obtained in this application by using ethylene / vinyl acetate copolymer powder as raw material has excellent performance.

[0067] By comparing the test results of Examples 2, 4-12 and Comparative Examples 3-5, it was found that in Comparative Example 3, an equal amount of unmodified montmorillonite was used instead of modified montmorillonite; in Comparative Example 4, phosphonic acid was used as a phosphonic acid substance to prepare modified montmorillonite; and in Comparative Example 5, the proportions of each component were not optimized during the preparation of modified montmorillonite, resulting in a poor-performing inorganic two-liquid slurry material. In contrast, the embodiments of this application, through screening and optimization of the types of carboxymethyl cellulose and phosphonic acid substances, and using the prepared modified montmorillonite as raw material, yielded an inorganic two-liquid slurry material with excellent performance. Furthermore, this application selects sodium carboxymethyl cellulose with a viscosity of 800-1200 mPa·s as a raw material, which can further improve the coagulation performance of the material; this application selects a mixture of aminotrimethylene phosphonic acid and sodium hexametaphosphate in a weight ratio of 17:1-5 to form a phosphonic acid substance, which can further improve the compressive strength and impermeability of the material.

[0068] By comparing the test results of Examples 2 and 13-16, this application selected a mixture of turpentine and ethylene glycol in a weight ratio of 1-5:20 as an additive to be added to Component B, which further improved the compressive strength and impermeability of the inorganic two-liquid slurry material.

[0069] Although the present invention has been described in detail above with general descriptions and specific embodiments, modifications or improvements can be made to it, which will be obvious to those skilled in the art. Therefore, all such modifications or improvements made without departing from the spirit of the present invention fall within the scope of protection claimed by the present invention.

Claims

1. An inorganic two-liquid slurry, characterized in that, The inorganic two-component slurry is composed of component A and component B with a volume ratio of 8.5-9.5:1; The A component specifically includes the following components by weight: 90-110 parts water, 30-40 parts cement powder, 5-10 parts silicon-based material, 12-18 parts ethylene / vinyl acetate copolymer powder, and 2-10 parts modified montmorillonite. The preparation method of the modified montmorillonite is as follows: by weight, 15-20 parts of montmorillonite and 2-5 parts of sodium carboxymethyl cellulose are dispersed in 45-55 parts of water, 5-10 parts of phosphonic acid substances are added, and the mixture is stirred thoroughly to carry out the reaction at a temperature of 50-60℃ for 2-3 hours in the dark. After filtration, drying, and pulverization, the modified montmorillonite is obtained. The phosphonic acid substance is selected from 2-hydroxyphosphonoacetic acid or is composed of a mixture of aminotrimethylenephosphonic acid and sodium hexametaphosphate in a weight ratio of 17:1-5 or a mixture of 2-hydroxyphosphonoacetic acid and sodium hexametaphosphate in a weight ratio of 17:

3. Component B specifically includes the following components in parts by weight: 50-60 parts water, 0.5-1.0 parts polycarboxylate superplasticizer, 0.2-0.5 parts defoamer, and 0.5-1.5 parts additives; In component B, the auxiliary agent is selected from one or more of turpentine oil, diacetone alcohol, ethylene glycol, and ethylene glycol butyl ether. The silicon-based material is selected from one or more of SH-9501 silicone resin, SH-9602 silicone resin, and SH-5202S silicone resin.

2. The inorganic two-liquid slurry according to claim 1, characterized in that, Component A specifically includes the following components by weight: 32-38 parts cement powder, 6-8 parts silicon-based material, 14-17 parts ethylene / vinyl acetate copolymer powder, and 4-8 parts modified montmorillonite.

3. The inorganic two-liquid slurry according to claim 1, characterized in that, The viscosity of the sodium carboxymethyl cellulose is 800-1200 mPa·s.

4. The inorganic two-liquid slurry according to claim 1, characterized in that, The average particle size of the montmorillonite is 100-500 nm.

5. The inorganic two-liquid slurry according to claim 1, characterized in that, In component B, the additive is composed of turpentine oil and ethylene glycol in a weight ratio of 1-5:

20.

6. The inorganic two-liquid slurry according to claim 1, characterized in that, In component B, the defoamer is selected from one or more of P803, SPA-102, SPA-202, and 201 methyl silicone oil.

7. The method for preparing the inorganic biliquid slurry according to any one of claims 1-6, characterized in that, Specifically, the following steps are included: Mix all the raw materials of component A, stir with a stirrer until they are evenly mixed, and then add water to obtain component A; Add polycarboxylate superplasticizer and defoamer to water, keep the temperature at 20-30℃ for 10-20 minutes, then add the additives and continue the reaction for 20-40 minutes to end the reaction and obtain component B. Mix component A and component B at a volume ratio of 8.5-9.5:1 to obtain the finished product.

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