A large-sized anti-detachment rock slab adhesive and its preparation method

Abstract

A large-sized anti-detachment rock slab adhesive and its preparation method according to the present invention. The rock slab adhesive comprises the following raw materials in parts by weight: 50-60 parts of portland cement, 35-40 parts of river sand with a particle size of 0.2 mm, 5-8 parts of silica fume, 6-9 parts of anti-detachment functional agent, 5-8 parts of basalt fiber agent blended based on coal gangue, 4-7 parts of yttrium conditioner, 2-5 parts of water-reducing agent, and 40-50 parts of water. In the present invention, portland cement and river sand with a particle size of 0.2 mm are used as matrix materials. By adding a water-reducing agent as a functional auxiliary agent, and the added silica fume has an active addition effect, and the added anti-detachment functional agent and basalt fiber agent blended based on coal gangue are coordinated together, further enhancing the performance effect of the system.

Description

Technical Field

[0001] The present invention relates to the technical field of rock slab adhesives, and particularly relates to a large-sized anti-detachment rock slab adhesive and a preparation method thereof. Background Art

[0002] Rock slabs are made from natural raw materials through special processes, pressed by presses with a capacity of over ten thousand tons, and fired at high temperatures. They can be processed such as cutting, drilling, and grinding, and belong to a new type of super-large-sized porcelain material.

[0003] Existing large-sized rock slabs need to be bonded to the wall surface. Due to the large size and heavy weight of the rock slabs, the anti-detachment bonding performance of the adhesives used is poor. At the same time, it is difficult to coordinately improve the shrinkage rate and compressive strength of the products, and the products have poor thermal-freeze cycle resistance and immersion stability, which easily affect the use efficiency of the rock slabs. Based on this, the present invention makes further improvements. Summary of the Invention

[0004] Aiming at the defects of the existing technology, the purpose of the present invention is to provide a large-sized anti-detachment rock slab adhesive and a preparation method thereof to solve the problems raised in the above background art.

[0005] The present invention adopts the following technical solutions to solve the technical problems:

[0006] The present invention provides a large-sized anti-detachment rock slab adhesive, and the rock slab adhesive comprises the following raw materials in parts by weight:

[0007] 50 - 60 parts of portland cement, 35 - 40 parts of river sand with a particle size of 0.2 mm, 5 - 8 parts of silica fume, 6 - 9 parts of anti-detachment functional agent, 5 - 8 parts of basalt fiber agent based on coal gangue blending, 4 - 7 parts of yttrium modifier, 2 - 5 parts of water-reducing agent, 40 - 50 parts of water;

[0008] The preparation method of the yttrium modifier is as follows:

[0009] 3 - 5 parts of a yttrium nitrate solution with a mass fraction of 2 - 5% and 1 - 3 parts of nano-silica sol are blended and added to 6 - 10 parts of a sodium dodecylbenzenesulfonate solution with a mass fraction of 5%, and stirred and mixed evenly to obtain the yttrium modifier.

[0010] Preferably, the water-reducing agent is a polycarboxylate water-reducing agent; the particle size of the silica fume is 10 - 20 nm.

[0011] Preferably, the preparation method of the anti-detachment functional agent is as follows:

[0012] S01: 2 - 5 parts of silane coupling agent KH560, 4 - 6 parts of a sodium citrate solution with a mass fraction of 5%, and 1 - 3 parts of ethanol are blended and mixed evenly to obtain a coupling modification liquid;

[0013] S02: Mix 4 - 7 parts of flaky boron nitride and 2 - 5 parts of silicon carbide into the coupling modification liquid and stir evenly to obtain a composite modification agent.

[0014] S03: Add a 5% chitosan solution with a mass fraction of 10 - 15% of the total amount of the composite modification agent to the composite modification agent and stir. After stirring, wash with water, filter by suction, and dry to obtain an anti - shedding functional agent.

[0015] Preferably, in S03, the stirring temperature of the stirring treatment is 50 - 55°C, the stirring speed is 350 - 400 r / min, and the stirring time is 20 - 30 min.

[0016] Preferably, the preparation method of the basalt fiber agent based on coal gangue blending is as follows:

[0017] S11: First, mix coal gangue evenly in a sufficient amount of potassium permanganate solution with a mass fraction of 2 - 5%, then wash with water, filter by suction, and dry.

[0018] S12: Immerse the dried coal gangue in an ethanol / water solution 3 - 5 times the total amount of the dried coal gangue, and stir evenly during immersion. The ethanol / water solution is prepared by mixing ethanol and water in a weight ratio of 7:3.

[0019] Then add 5 - 8% of the silane coupling agent KH550 based on the total amount of coal gangue to the coal gangue in S12, continue to stir evenly, and finally wash with water and dry to obtain pre - adjusted coal gangue.

[0020] S13: Mix the pre - adjusted coal gangue and the basalt fiber blending agent in a weight ratio of 5:(2 - 3) and perform ball - milling treatment. After ball - milling, wash with water, filter by suction, and dry to obtain the basalt fiber agent based on coal gangue blending.

[0021] Preferably, the ball - milling speed of the mixing and ball - milling treatment in S13 is 550 - 750 r / min, and the ball - milling time is 2 h.

[0022] Preferably, the preparation method of the basalt fiber blending agent is as follows:

[0023] Mix 3 - 5 parts of basalt fiber, 1 - 3 parts of a 5% sodium silicate solution, and 2 - 4 parts of a 3 - 4% lanthanum chloride solution and perform ball - milling treatment. The ball - milling speed is 1000 r / min, and the ball - milling time is 1 h. After ball - milling, obtain the basalt fiber modifier.

[0024] Add 1 - 3 parts of calcium dodecylbenzenesulfonate to 2 - 5 parts of hydrochloric acid dopamine solution and mix evenly to obtain a treatment agent; continue to mix the halloysite powder and the treatment agent in a weight ratio of 2:5 evenly, then wash with water, filter by suction, and dry to obtain the halloysite agent.

[0025] The halloysite agent and the basalt fiber modifier are subjected to ultrasonic modification treatment in a weight ratio of 2:5, and after the ultrasonic treatment is completed, a basalt fiber admixture is obtained.

[0026] Preferably, the mass fraction of the dopamine hydrochloride solution is 10-15%; the length of the halloysite powder is 2-5 um.

[0027] Preferably, the ultrasonic power of the ultrasonic modification treatment is 350-400 W, and the ultrasonic time is 20-30 min.

[0028] The present invention also provides a method for preparing a large-scale anti-falling rock plate adhesive, comprising the following steps:

[0029] Adding silicon powder, anti-shedding functional agent, and basalt fiber agent based on coal gangue into yttrium blending agent, stirring sufficiently, and then filtering and drying to obtain additives;

[0030] The additive, silicate cement, river sand with a particle size of 0.2 mm, a water reducer and water are further mixed to obtain the large-scale anti-falling rock slab adhesive of the present invention.

[0031] Compared with the prior art, the present invention has the following beneficial effects:

[0032] The present invention uses portland cement and river sand with a particle size of 0.2 mm as the matrix material. By adding a water reducer as a functional auxiliary agent and adding silica fume with an active addition effect to the system, the active connectivity between the raw materials is enhanced, and the compactness of the system is improved. However, the silica fume with a nanostructure is prone to agglomeration. Therefore, it is first treated with a yttrium modifier. The yttrium nitrate solution, nano-silica sol, and sodium dodecylbenzenesulfonate solution in the yttrium modifier are co-formulated and synergistic. The yttrium nitrate solution in the yttrium modifier co-formulates to enhance the activity of the system, and the nano-silica sol and sodium dodecylbenzenesulfonate solution co-formulate to enhance the dispersion, enabling the silica fume to further play a role in the system. In addition, the added anti-detachment functional agent and the basalt fiber agent doped with coal gangue are co-formulated and coordinated to improve the anti-detachment property and performance stability of the product, and further enhance the performance effect of the system; the anti-detachment functional agent is obtained by fully blending a silane coupling agent with a sodium citrate solution and ethanol to obtain a coupling modified liquid. At the same time, flaky boron nitride and silicon carbide are blended and added to the coupling modified liquid and stirred evenly. Then, it is coordinated with a chitosan solution. With the co-effect and co-formulation of flaky boron nitride and silicon carbide, and through the coordination of the coupling modified liquid, the obtained anti-detachment functional agent enhances the tensile bonding strength of the product in the system, improves the anti-detachment stability and shrinkage rate performance of the system; the basalt fiber agent doped with coal gangue is obtained by treating coal gangue with a potassium permanganate solution, and then fully stirring and immersing it in an ethanol / water solution and a silane coupling agent KH550 to optimize the active effect of coal gangue in the system and better fill it into the system. At the same time, the basalt fiber doping agent uses basalt fiber through the matrix material, reinforced by a needle-like structure, and ball-milled by blending a sodium silicate solution with a mass fraction of 5% and a lanthanum chloride solution with a mass fraction of 3 - 4%. Through the coordination of the raw materials, and then adding calcium dodecylbenzenesulfonate to a dopamine hydrochloride solution and fully blending to obtain a treatment agent. The halloysite agent obtained by improving halloysite powder with the treatment agent further improves the basalt fiber modifier, so that the obtained basalt fiber doping agent can better coordinate with coal gangue, and the performance is further improved. Detailed Embodiments

[0033] The following combines specific embodiments to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative work fall within the scope of protection of the present invention.

[0034] A large-size anti-detachment rock slab adhesive in this embodiment, the rock slab adhesive includes the following raw materials in parts by weight:

[0035] 50 - 60 parts of portland cement, 35 - 40 parts of river sand with a particle size of 0.2 mm, 5 - 8 parts of silica fume, 6 - 9 parts of anti - shedding functional agent, 5 - 8 parts of basalt fiber agent based on coal gangue blending, 4 - 7 parts of yttrium conditioner, 2 - 5 parts of water - reducing agent, 40 - 50 parts of water;

[0036] The preparation method of the yttrium conditioner is as follows:

[0037] Mix 3 - 5 parts of yttrium nitrate solution with a mass fraction of 2 - 5% and 1 - 3 parts of nano - silica sol and add them into 6 - 10 parts of sodium dodecyl benzene sulfonate solution with a mass fraction of 5% and stir well to obtain the yttrium conditioner.

[0038] The water - reducing agent in this example is a polycarboxylate water - reducing agent; the particle size of the silica fume is 10 - 20 nm.

[0039] The preparation method of the anti - shedding functional agent in this example is as follows:

[0040] S01: Mix 2 - 5 parts of silane coupling agent KH560, 4 - 6 parts of sodium citrate solution with a mass fraction of 5% and 1 - 3 parts of ethanol to obtain the coupling modification liquid;

[0041] S02: Mix 4 - 7 parts of flaky boron nitride and 2 - 5 parts of silicon carbide and add them into the coupling modification liquid and stir well to obtain the composite modifier;

[0042] S03: Add a chitosan solution with a mass fraction of 5% accounting for 10 - 15% of the total amount of the composite modifier to the composite modifier and stir. After stirring, wash with water, filter by suction, and dry to obtain the anti - shedding functional agent.

[0043] In S03 of this example, the stirring temperature of the stirring treatment is 50 - 55 °C, the stirring speed is 350 - 400 r / min, and the stirring time is 20 - 30 min.

[0044] The preparation method of the basalt fiber agent based on coal gangue blending in this example is as follows:

[0045] S11: First, stir and mix coal gangue in a sufficient amount of potassium permanganate solution with a mass fraction of 2 - 5%, then wash with water, filter by suction, and dry;

[0046] S12: Immerse the dried coal gangue in an ethanol / water solution that is 3 - 5 times the total amount of the dried coal gangue, and stir well during immersion. The ethanol / water solution is prepared by mixing ethanol and water according to a weight ratio of 7:3;

[0047] Then add 5 - 8% of silane coupling agent KH550 based on the total amount of coal gangue to the coal gangue in S12, continue to stir well, and finally wash with water and dry to obtain the pre - adjusted coal gangue;

[0048] S13: Mix the pre-adjusted coal gangue and basalt fiber admixture in a weight ratio of 5:(2 - 3), conduct ball milling treatment, and after the ball milling is completed, wash with water, filter by suction, and dry to obtain the basalt fiber agent based on coal gangue admixture.

[0049] In S13 of this embodiment, the ball milling speed for the mixing ball milling treatment is 550 - 750 r / min, and the ball milling lasts for 2 h.

[0050] The preparation method of the basalt fiber admixture in this embodiment is as follows:

[0051] Mix 3 - 5 parts of basalt fiber, 1 - 3 parts of sodium silicate solution with a mass fraction of 5%, and 2 - 4 parts of lanthanum chloride solution with a mass fraction of 3 - 4% for ball milling treatment. The ball milling speed is 1000 r / min, and the ball milling lasts for 1 h. After the ball milling is completed, obtain the basalt fiber modifier;

[0052] Add 1 - 3 parts of calcium dodecylbenzenesulfonate to 2 - 5 parts of hydrochloric acid dopamine solution and mix well to obtain the treatment agent; continue to mix the halloysite powder and the treatment agent in a weight ratio of 2:5 until well - mixed, then wash with water, filter by suction, and dry to obtain the halloysite agent;

[0053] Conduct ultrasonic modification treatment on the halloysite agent and the basalt fiber modifier in a weight ratio of 2:5. After the ultrasonic treatment is completed, obtain the basalt fiber admixture.

[0054] In this embodiment, the mass fraction of the hydrochloric acid dopamine solution is 10 - 15%; the length dimension of the halloysite powder is 2 - 5 μm.

[0055] In this embodiment, the ultrasonic power for the ultrasonic modification treatment is 350 - 400 W, and the ultrasonic time is 20 - 30 min.

[0056] The preparation method of a large - size anti - shedding rock slab adhesive in this embodiment includes the following steps:

[0057] Add silicon powder, anti - shedding functional agent, and the basalt fiber agent based on coal gangue admixture to the yttrium conditioner and stir well, then filter by suction and dry to obtain the additive;

[0058] Continue to mix the additive, portland cement, river sand with a particle size of 0.2 mm, water - reducing agent, and water until well - mixed to obtain the large - size anti - shedding rock slab adhesive of the present invention.

[0059] Example 1.

[0060] For a large - size anti - shedding rock slab adhesive in this embodiment, the rock slab adhesive comprises the following raw materials in parts by weight:

[0061] 50 parts of portland cement, 35 parts of river sand with a particle size of 0.2 mm, 5 parts of silica fume, 6 parts of anti-shedding functional agent, 5 parts of basalt fiber agent based on coal gangue blending, 4 parts of yttrium modifier, 2 parts of water reducer, and 40 parts of water;

[0062] The preparation method of the yttrium modifier is as follows:

[0063] 3 parts of yttrium nitrate solution with a mass fraction of 2% and 1 part of nano-silica sol are blended and added to 6 parts of sodium dodecylbenzenesulfonate solution with a mass fraction of 5%, and stirred and mixed thoroughly to obtain the yttrium modifier.

[0064] The water reducer in this example is a polycarboxylate water reducer; the particle size of the silica fume is 10 nm.

[0065] The preparation method of the anti-shedding functional agent in this example is as follows:

[0066] S01: 2 parts of silane coupling agent KH560, 4 parts of sodium citrate solution with a mass fraction of 5% and 1 part of ethanol are blended and mixed thoroughly to obtain the coupling modification liquid;

[0067] S02: 4 parts of flaky boron nitride and 2 parts of silicon carbide are blended and added to the coupling modification liquid, and stirred and mixed thoroughly to obtain the composite modification agent;

[0068] S03: Add a chitosan solution with a mass fraction of 5% accounting for 10% of the total amount of the composite modification agent to the composite modification agent for stirring treatment. After the stirring ends, wash with water, filter by suction, and dry to obtain the anti-shedding functional agent.

[0069] In S03 of this example, the stirring temperature of the stirring treatment is 50 °C, the stirring speed is 350 r / min, and the stirring time is 20 min.

[0070] The preparation method of the basalt fiber agent based on coal gangue blending in this example is as follows:

[0071] S11: First, stir and mix coal gangue thoroughly in a sufficient amount of potassium permanganate solution with a mass fraction of 2%, and then wash with water, filter by suction, and dry;

[0072] S12: Immerse the dried coal gangue in an ethanol / water solution that is 3 times the total amount of the dried coal gangue, and immerse and stir thoroughly, where the ethanol / water solution is prepared by mixing ethanol and water in a weight ratio of 7:3;

[0073] Then add 5% of silane coupling agent KH550 based on the total amount of coal gangue to the coal gangue in S12, continue to stir thoroughly, and finally wash with water and dry to obtain the pre-adjusted coal gangue;

[0074] S13: Mix the pre-adjusted coal gangue and the basalt fiber blending agent in a weight ratio of 5:2, perform ball milling treatment. After the ball milling ends, wash with water, filter by suction, and dry to obtain the basalt fiber agent based on coal gangue blending.

[0075] In S13 of this embodiment, the ball milling speed for the mixing and ball milling treatment is 5500 r / min, and the ball milling is carried out for 2 h.

[0076] The preparation method of the basalt fiber admixture in this embodiment is as follows:

[0077] Mix 3 parts of basalt fiber, 1 part of sodium silicate solution with a mass fraction of 5%, and 2 parts of lanthanum chloride solution with a mass fraction of 3% and carry out ball milling treatment. The ball milling speed is 1000 r / min, and the ball milling is carried out for 1 h. After the ball milling is completed, a basalt fiber modifier is obtained;

[0078] Add 1 part of calcium dodecylbenzenesulfonate to 2 parts of hydrochloric acid dopamine solution and mix well to obtain a treatment agent; continue to mix well the halloysite powder and the treatment agent according to a weight ratio of 2:5, then wash with water, filter by suction, and dry to obtain a halloysite agent;

[0079] Carry out ultrasonic modification treatment on the halloysite agent and the basalt fiber modifier according to a weight ratio of 2:5. After the ultrasonic treatment is completed, a basalt fiber admixture is obtained.

[0080] In this embodiment, the mass fraction of the hydrochloric acid dopamine solution is 10%; the length dimension of the halloysite powder is 2 μm.

[0081] In this embodiment, the ultrasonic power for the ultrasonic modification treatment is 350 W, and the ultrasonic time is 20 min.

[0082] The preparation method of a large-size anti-detachment rock slab adhesive in this embodiment includes the following steps:

[0083] Add silicon powder, an anti-detachment functional agent, and a basalt fiber agent based on coal gangue admixture to a yttrium conditioner and stir well, then filter by suction and dry to obtain an additive;

[0084] Continue to mix the additive, portland cement, river sand with a particle size of 0.2 mm, a water reducing agent, and water well to obtain the large-size anti-detachment rock slab adhesive of the present invention.

[0085] Example 2.

[0086] A large-size anti-detachment rock slab adhesive in this embodiment, the rock slab adhesive includes the following raw materials in parts by weight:

[0087] 60 parts of portland cement, 40 parts of river sand with a particle size of 0.2 mm, 8 parts of silicon powder, 9 parts of anti-detachment functional agent, 8 parts of basalt fiber agent based on coal gangue admixture, 7 parts of yttrium conditioner, 5 parts of water reducing agent, 50 parts of water;

[0088] The preparation method of the yttrium conditioner is as follows:

[0089] Add 5 parts of a yttrium nitrate solution with a mass fraction of 5% and 3 parts of nano-silica sol into 10 parts of a sodium dodecylbenzenesulfonate solution with a mass fraction of 5%, and stir and mix well to obtain a yttrium conditioner.

[0090] The water reducer in this example is a polycarboxylate water reducer; the particle size of the silica fume is 20 nm.

[0091] The preparation method of the anti-shedding functional agent in this example is as follows:

[0092] S01: Mix 5 parts of silane coupling agent KH560, 6 parts of a sodium citrate solution with a mass fraction of 5% and 3 parts of ethanol well to obtain a coupling modification solution;

[0093] S02: Add 7 parts of flaky boron nitride and 5 parts of silicon carbide into the coupling modification solution, stir and mix well to obtain a composite modifier;

[0094] S03: Add a chitosan solution with a mass fraction of 5% accounting for 15% of the total amount of the composite modifier to the composite modifier, stir, wash with water, filter by suction, and dry to obtain the anti-shedding functional agent.

[0095] In S03 of this example, the stirring temperature of the stirring treatment is 55 °C, the stirring speed is 400 r / min, and the stirring time is 30 min.

[0096] The preparation method of the basalt fiber agent based on coal gangue blending in this example is as follows:

[0097] S11: First, mix coal gangue well in a sufficient amount of potassium permanganate solution with a mass fraction of 5%, and then wash with water, filter by suction, and dry;

[0098] S12: Immerse the dried coal gangue in an ethanol / water solution 5 times the total amount of the dried coal gangue, immerse and stir well, where the ethanol / water solution is prepared by mixing ethanol and water in a weight ratio of 7:3;

[0099] Then add 8% of the silane coupling agent KH550 based on the total amount of coal gangue to the coal gangue in S12, continue to stir well, and finally wash with water and dry to obtain pre-adjusted coal gangue;

[0100] S13: Mix the pre-adjusted coal gangue and the basalt fiber blending agent in a weight ratio of 5:3, perform ball milling, wash with water, filter by suction, and dry to obtain the basalt fiber agent based on coal gangue blending.

[0101] In S13 of this example, the ball milling speed of the mixing and ball milling treatment is 750 r / min, and the ball milling time is 2 h.

[0102] The preparation method of the basalt fiber blending agent in this example is as follows:

[0103] Mix 5 parts of basalt fiber, 3 parts of a 5% sodium silicate solution by mass fraction, and 4 parts of a 4% lanthanum chloride solution by mass fraction, and conduct ball milling treatment at a ball milling speed of 1000 r / min for 1 h. After the ball milling is completed, a basalt fiber modifier is obtained;

[0104] Add 3 parts of calcium dodecylbenzenesulfonate to 5 parts of dopamine hydrochloride solution and mix well to obtain a treatment agent; continue to mix well the halloysite powder and the treatment agent according to a weight ratio of 2:5, then wash with water, filter by suction, and dry to obtain a halloysite agent;

[0105] Conduct ultrasonic modification treatment on the halloysite agent and the basalt fiber modifier according to a weight ratio of 2:5. After the ultrasonic treatment is completed, a basalt fiber admixture is obtained.

[0106] In this example, the mass fraction of the dopamine hydrochloride solution is 15%; the length dimension of the halloysite powder is 5 μm.

[0107] In this example, the ultrasonic power of the ultrasonic modification treatment is 400 W, and the ultrasonic time is 30 min.

[0108] A preparation method of a large-size anti-detachment rock slab adhesive in this example includes the following steps:

[0109] Add silicon powder, an anti-detachment functional agent, and a basalt fiber agent based on coal gangue admixture to a yttrium conditioner and stir well, then filter by suction and dry to obtain an additive;

[0110] Continue to mix well the additive, portland cement, river sand with a particle size of 0.2 mm, a water reducing agent, and water to obtain the large-size anti-detachment rock slab adhesive of the present invention.

[0111] Example 3.

[0112] A large-size anti-detachment rock slab adhesive in this example, the rock slab adhesive includes the following raw materials in parts by weight:

[0113] 55 parts of portland cement, 37.5 parts of river sand with a particle size of 0.2 mm, 6.5 parts of silicon powder, 7.5 parts of anti-detachment functional agent, 6.5 parts of basalt fiber agent based on coal gangue admixture, 5.5 parts of yttrium conditioner, 3.5 parts of water reducing agent, 45 parts of water;

[0114] The preparation method of the yttrium conditioner is:

[0115] Mix 4 parts of a 3.5% yttrium nitrate solution by mass fraction and 2 parts of nano-silica sol, and add them to 8 parts of a 5% sodium dodecylbenzenesulfonate solution and stir well to obtain a yttrium conditioner.

[0116] In this example, the water reducing agent is a polycarboxylate water reducing agent; the particle size of the silicon powder is 15 nm.

[0117] The preparation method of the anti - shedding functional agent in this embodiment is as follows:

[0118] S01: Blend 3.5 parts of silane coupling agent KH560, 5 parts of 5% sodium citrate solution by mass, and 2 parts of ethanol thoroughly to obtain a coupling modification solution;

[0119] S02: Blend 5.5 parts of flaky boron nitride and 3.5 parts of silicon carbide, add them to the coupling modification solution, and stir evenly to obtain a composite modification agent;

[0120] S03: Add a 5% chitosan solution with a mass fraction of 12.5% of the total amount of the composite modification agent to the composite modification agent, stir, wash with water, filter by suction, and dry to obtain the anti - shedding functional agent.

[0121] In S03 of this embodiment, the stirring temperature of the stirring treatment is 52 °C, the stirring speed is 370 r / min, and the stirring time is 25 min.

[0122] The preparation method of the basalt fiber agent based on coal gangue blending in this embodiment is as follows:

[0123] S11: First, stir and mix coal gangue thoroughly in a sufficient amount of 3.5% potassium permanganate solution by mass, then wash with water, filter by suction, and dry;

[0124] S12: Immerse the dried coal gangue in an ethanol / water solution that is 4 times the total amount of the dried coal gangue, immerse and stir thoroughly, where the ethanol / water solution is prepared by mixing ethanol and water in a weight ratio of 7:3;

[0125] Then add 5 - 8% of silane coupling agent KH550 based on the total amount of coal gangue to the coal gangue in S12, continue to stir thoroughly, and finally wash with water and dry to obtain pre - adjusted coal gangue;

[0126] S13: Mix the pre - adjusted coal gangue and the basalt fiber blending agent in a weight ratio of 2:1, perform ball - milling treatment, after ball - milling, wash with water, filter by suction, and dry to obtain the basalt fiber agent based on coal gangue blending.

[0127] In S13 of this embodiment, the ball - milling speed of the mixing and ball - milling treatment is 600 r / min, and the ball - milling time is 2 h.

[0128] The preparation method of the basalt fiber blending agent in this embodiment is as follows:

[0129] Mix 4 parts of basalt fiber, 2 parts of 5% sodium silicate solution by mass, and 3 parts of 3.5% lanthanum chloride solution by mass, perform ball - milling treatment, with a ball - milling speed of 1000 r / min and a ball - milling time of 1 h. After ball - milling, obtain the basalt fiber modifier;

[0130] Add 2 parts of calcium dodecylbenzenesulfonate to 3.5 parts of dopamine hydrochloride solution and mix well to obtain a treatment agent; continue to mix halloysite powder and the treatment agent in a weight ratio of 2:5 until well mixed, then wash with water, filter by suction, and dry to obtain a halloysite agent;

[0131] The halloysite agent and the basalt fiber modifier are ultrasonically modified in a weight ratio of 2:5. After the ultrasonic treatment is completed, a basalt fiber admixture is obtained.

[0132] In this example, the mass fraction of the dopamine hydrochloride solution is 12.5%; the length dimension of the halloysite powder is 3.5 μm.

[0133] In this example, the ultrasonic power of the ultrasonic modification treatment is 370 W, and the ultrasonic time is 25 min.

[0134] A preparation method of a large-size anti-detachment rock slab adhesive in this example includes the following steps:

[0135] Add silicon powder, anti-detachment functional agent, and basalt fiber agent based on coal gangue admixture to the yttrium conditioner and stir well, then filter by suction and dry to obtain an additive;

[0136] Continue to mix the additive, portland cement, river sand with a particle size of 0.2 mm, water reducing agent, and water until well mixed to obtain the large-size anti-detachment rock slab adhesive of the present invention.

[0137] Comparative Example 1.

[0138] The difference from Example 3 is that the anti-detachment functional agent is not added.

[0139] Comparative Example 2.

[0140] The difference from Example 3 is that the S03 step treatment is not adopted in the preparation of the anti-detachment functional agent.

[0141] Comparative Example 3.

[0142] The difference from Example 3 is that the coupling modification liquid treatment is not adopted in the preparation of the anti-detachment functional agent.

[0143] Comparative Example 4.

[0144] The difference from Example 3 is that silicon carbide is not added in the preparation of the anti-detachment functional agent.

[0145] Comparative Example 5.

[0146] The difference from Example 3 is that the basalt fiber agent based on coal gangue admixture is not added.

[0147] Comparative Example 6.

[0148] The difference from Example 3 is that the pre-adjusted coal gangue in the preparation of the basalt fiber agent based on coal gangue admixture is replaced with coal gangue.

[0149] Comparative Example 7

[0150] Different from Example 3, in the preparation of the basalt fiber agent blended with coal gangue, the basalt fiber blending agent treatment was not used.

[0151] Comparative Example 8

[0152] Different from Example 3, the yttrium conditioner treatment was not used.

[0153] Comparative Example 9

[0154] Different from Example 3, yttrium nitrate solution and nano-silica sol were not added to the yttrium conditioner.

[0155] For the conventional tests, the compressive strength, tensile bond original strength and shrinkage rate performance of Examples 1 - 3 and Comparative Examples 1 - 9 were tested according to the JC / T547 - 2017 standard;

[0156]

[0157] It can be seen from Comparative Examples 1 - 9 and Examples 1 - 3 that;

[0158] The product of Example 3 has excellent 28d compressive strength. At the same time, the effects of the tensile bond original strength and shrinkage rate performance of the product are remarkable. The compressive strength, tensile bond original strength and shrinkage rate performance of the product can be improved in a coordinated manner;

[0159] The products of Examples 1 - 3 and Comparative Examples 1 - 9 were coated on large - sized rock slabs of 1m×1m. Two rock slabs were bonded together, and the coating thickness was 2mm for the bonding treatment of the rock slabs. Then, after curing at room temperature for 72h, the water immersion stability of the tensile bond original strength of the product was tested (the rock slab was immersed in water for 72h, and the immersion temperature was 60℃), the thermal - freeze stability cycle test (the rock slab was placed at - 5℃ for 24h and then at 65℃ for 12h, and the above was taken as one cycle and repeated 10 times), and the stability of the compressive strength performance of the product was tested. For this performance stability test, the product was only immersed in water for 72h at a temperature of 60℃, taken out and dried. At the same time, the product was placed at - 5℃ for 24h and then at 65℃ for 12h. The above was taken as one cycle and repeated 10 times to test the freeze - thermal stability and water immersion stability of the compressive strength respectively;

[0160]

[0161] It can be seen from Comparative Examples 1 - 9 and Example 3 that without adding the anti - shedding functional agent, without adding the basalt fiber agent blended with coal gangue, and without using the yttrium conditioner treatment, the performance stability of the product shows an obvious trend of deterioration. When the three raw materials are coordinated and combined, the product performance effect is the most remarkable;

[0162] When the anti - shedding functional agent is prepared without the S03 step treatment, without the treatment with the coupling modification liquid, and without adding silicon carbide, the performance of the product also shows a deteriorating trend to varying degrees. At the same time, when preparing the basalt fiber agent blended with gangue, the pre - adjusted gangue is replaced with gangue, and without the treatment with the basalt fiber blending agent, the performance of the product also shows a deteriorating trend. Moreover, without the treatment with the basalt fiber blending agent, the deterioration of the product performance is more obvious; when the yttrium conditioner does not add yttrium nitrate solution and nano - silica sol, the performance of the product shows a deteriorating trend. Only the raw material products obtained by the specific method of the present invention have the most significant product performance effect.

[0163] Since the basalt fiber blending agent has a more obvious impact on the deterioration of product performance, the present invention further explores and processes it:

[0164] Experimental Example 1.

[0165] The only difference from Example 3 is that halloysite agent is not added in the preparation of the basalt fiber blending agent.

[0166] Experimental Example 2.

[0167] The only difference from Example 3 is that the halloysite agent is not treated with the treatment agent during its preparation.

[0168] Experimental Example 3.

[0169] The only difference from Example 3 is that calcium dodecylbenzenesulfonate is not added to the treatment agent.

[0170] Experimental Example 4.

[0171] The only difference from Example 3 is that water is used to replace the hydrochloric acid dopamine solution in the treatment agent.

[0172] Experimental Example 5.

[0173] The only difference from Example 3 is that the basalt fiber modifier treatment is not used.

[0174] Experimental Example 6.

[0175] The only difference from Example 3 is that basalt fiber is not added in the preparation of the basalt fiber modifier.

[0176] Experimental Example 7.

[0177] The only difference from Example 3 is that sodium silicate solution is not added in the preparation of the basalt fiber modifier.

[0178] Experimental Example 8.

[0179] The only difference from Example 3 is that lanthanum chloride solution was not added during the preparation of the basalt fiber modifier. Taking the freeze - heat stability and immersion stability tests as examples, the performance tests of Experimental Examples 1 - 8 are as follows:

[0180]

[0181] It can be seen from Experimental Examples 1 - 8 that without adding halloysite agent and without using basalt fiber modifier treatment during the preparation of the basalt fiber admixture, the performance of the product shows an obvious downward trend. Also, when basalt fiber is not added during the preparation of the basalt fiber modifier, sodium silicate solution is not added during the preparation of the basalt fiber modifier, or lanthanum chloride solution is not added during the preparation of the basalt fiber modifier, the performance of the product shows a downward trend to varying degrees;

[0182] When the halloysite agent is not treated with a treatment agent during its preparation, calcium dodecylbenzenesulfonate is not added to the treatment agent, or water is used instead of dopamine hydrochloride solution in the treatment agent, the performance of the product also shows a downward trend. The performance effect of the product is the most significant when the halloysite agent treated with the treatment agent obtained by the specific method of the present invention is combined with the basalt fiber modifier obtained from the specific raw materials of the present invention;

[0183] Only the basalt fiber admixture obtained by combining the specific raw materials of the present invention has the most significant performance effect, and the technical effect of the present invention cannot be achieved by using other raw materials instead.

[0184] For those skilled in the art, it is obvious that the present invention is not limited to the details of the above - mentioned exemplary embodiments, and without departing from the spirit or basic characteristics of the present invention, the present invention can be implemented in other specific forms. Therefore, from any point of view, the embodiments should be regarded as exemplary and non - restrictive. The scope of the present invention is defined by the appended claims rather than the above description. Therefore, all changes falling within the meaning and scope of the equivalent elements of the claims are intended to be embraced within the present invention.

[0185] In addition, it should be understood that although this specification is described according to embodiments, not every embodiment only contains an independent technical solution. This narrative way of the specification is only for clarity. Those skilled in the art should regard the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.

Claims

1. A large-sized anti-detachment rock slab adhesive, characterized in that, The slate adhesive comprises the following raw materials in parts by weight: 50 - 60 parts of portland cement, 35 - 40 parts of river sand with a particle size of 0.2 mm, 5 - 8 parts of silica fume, 6 - 9 parts of anti - shedding functional agent, 5 - 8 parts of basalt fiber agent based on coal gangue blending, 4 - 7 parts of yttrium conditioner, 2 - 5 parts of water - reducing agent, 40 - 50 parts of water; The preparation method of the yttrium conditioner is as follows: 3 - 5 parts of yttrium nitrate solution with a mass fraction of 2 - 5% and 1 - 3 parts of nano - silica sol are blended and added to 6 - 10 parts of sodium dodecylbenzenesulfonate solution with a mass fraction of 5%, and stirred evenly to obtain the yttrium conditioner; The preparation method of the anti - shedding functional agent is as follows: S01: 2 - 5 parts of silane coupling agent KH560, 4 - 6 parts of sodium citrate solution with a mass fraction of 5% and 1 - 3 parts of ethanol are blended evenly to obtain the coupling modification liquid; S02: 4 - 7 parts of flaky boron nitride and 2 - 5 parts of silicon carbide are blended and added to the coupling modification liquid, and stirred evenly to obtain the composite modification agent; S03: Add 5% chitosan solution with a mass fraction of 10 - 15% of the total amount of the composite modification agent to the composite modification agent, stir, wash with water, filter by suction, and dry to obtain the anti - shedding functional agent; The preparation method of the basalt fiber agent based on coal gangue blending is as follows: S11: First, stir coal gangue evenly in a sufficient amount of potassium permanganate solution with a mass fraction of 2 - 5%, then wash with water, filter by suction, and dry; S12: Immerse the dried coal gangue in an ethanol / water solution 3 - 5 times the total amount of the dried coal gangue, stir evenly during immersion, and the ethanol / water solution is prepared by mixing ethanol and water according to a weight ratio of 7:3; Then add 5 - 8% of silane coupling agent KH550 based on the total amount of coal gangue to the coal gangue in S12, continue to stir evenly, and finally wash with water and dry to obtain the pre - adjusted coal gangue; S13: The pre - adjusted coal gangue and basalt fiber blending agent are mixed and ball - milled according to a weight ratio of 5:(2 - 3). After ball - milling, wash with water, filter by suction, and dry to obtain the basalt fiber agent based on coal gangue blending. The preparation method of the basalt fiber blending agent is as follows: 3 - 5 parts of basalt fiber, 1 - 3 parts of sodium silicate solution with a mass fraction of 5% and 2 - 4 parts of lanthanum chloride solution with a mass fraction of 3 - 4% are blended and ball - milled. The ball - milling speed is 1000 r / min, and the ball - milling time is 1 h. After ball - milling, obtain the basalt fiber modifier; Add 1 - 3 parts of calcium dodecylbenzenesulfonate to 2 - 5 parts of hydrochloric acid dopamine solution and blend evenly to obtain the treatment agent; Halloysite powder and the treatment agent are continuously blended evenly according to a weight ratio of 2:5, then washed with water, filtered by suction, and dried to obtain the halloysite agent; The halloysite agent and the basalt fiber modifier are ultrasonically modified according to a weight ratio of 2:

5. After ultrasonic treatment, obtain the basalt fiber blending agent.

2. The large-sized anti-detachment rock slab adhesive as claimed in claim 1, wherein The water - reducing agent is a polycarboxylate water - reducing agent; the particle size of the silica fume is 10 - 20 nm.

3. A large-sized anti-detachment rock slab adhesive according to claim 1, characterized in that, In S03, the stirring temperature of the stirring treatment is 50 - 55 °C, the stirring speed is 350 - 400 r / min, and the stirring time is 20 - 30 min.

4. A large-sized anti-detachment rock slab adhesive according to claim 1, characterized in that, In S13, the ball - milling speed of the mixing and ball - milling treatment is 550 - 750 r / min, and the ball - milling time is 2 h.

5. A large-sized anti-detachment rock slab adhesive according to claim 1, characterized in that, The mass fraction of the dopamine hydrochloride solution is 10-15%; the length of the halloysite powder is 2-5 um.

6. A large-sized anti-detachment rock slab adhesive according to claim 1, characterized in that, The ultrasonic power of the ultrasonic modification treatment is 350-400W, and the ultrasonic time is 20-30min.

7. The preparation method of a large-size anti-detachment rock slab adhesive according to any one of claims 1 to 6, characterized in that The following steps are involved: Adding silicon powder, anti-shedding functional agent, and basalt fiber agent based on coal gangue into yttrium blending agent, stirring sufficiently, and then filtering and drying to obtain additives; The additive, silicate cement, river sand with a particle size of 0.2 mm, water reducer and water are further mixed to obtain an anti-shedding rock slab adhesive.

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