A crack-resistant, super-strong, and highly flexible diamond sand carbon fiber tile adhesive and its preparation method

Abstract

The present invention relates to the technical field of tile adhesives and discloses a crack-resistant, super-strong, and highly flexible diamond grit carbon fiber tile adhesive and a preparation method thereof. The tile adhesive comprises 35-40 parts by weight of cement, 60-65 parts by weight of sand, 0.1-0.8 parts by weight of nano-silicon dioxide-modified carbon fibers, and 1.5-4 parts by weight of diamond grit. The carbon fibers of the present invention are surface-grafted with nano-silicon dioxide and have excellent compatibility with cement and sand, allowing for uniform dispersion in the tile adhesive matrix. This significantly improves the mechanical properties of the tile adhesive, exhibiting high tensile adhesive strength, compressive strength, and flexural strength, thereby improving the crack resistance and flexibility of the tile adhesive.

Description

Technical Field

[0001] The invention relates to the technical field of tile adhesives, in particular to a crack-resistant, super-strong, high-flexibility diamond sand carbon fiber tile adhesive and a preparation method thereof. Background Art

[0002] The main components of tile adhesive are cement, sand, cellulose, redispersible latex powder, etc., which are mainly used in pasting ceramic tiles, facing tiles, floor tiles and other decorative materials. Improving the bonding performance and mechanical strength of tile adhesive has important applications. Carbon fiber is a functional inorganic fiber material with high strength, high modulus, and good high temperature resistance. It is widely used in adhesives, concrete and other building materials. The patent with publication number CN117417156A discloses a carbon fiber tile pasting material, tile adhesive and its application. The tile adhesive obtained with raw materials such as cement, metakaolin, hollow glass microspheres, and carbon fiber has the advantages of good bonding and good thermal conductivity. However, the patent did not improve the dispersibility of carbon fiber in tile adhesive, and the tile adhesive did not show good mechanical properties such as flexural strength and compressive strength. Summary of the Invention

[0003] The technical problem solved by the invention is to provide a corundum carbon fiber tile adhesive with good mechanical properties and high flexibility.

[0004] The technical solution provided by the present invention is: a crack-resistant, super-strong and highly flexible corundum carbon fiber tile adhesive, comprising 35-40 parts by weight of cement, 60-65 parts by weight of sand, 0.3-0.4 parts by weight of cellulose ether, 1-1.6 parts by weight of redispersible latex powder, 0.1-0.8 parts by weight of nano-silica modified carbon fiber, and 1.5-4 parts by weight of corundum.

[0005] The preparation method of nano-silica modified carbon fiber comprises the following steps:

[0006] Step (1), washing the carbon fiber with ethanol and water in sequence, drying, adding it into concentrated nitric acid for oxidation, filtering and then washing with water to obtain oxidized carbon fiber.

[0007] Step (2), adding oxidized carbon fiber to N,N-dimethylformamide, stirring, adding styrene-TM I copolymer and dibutyltin dilaurate, heating to 75-85° C. in a nitrogen atmosphere, stirring and reacting for 12-18 hours, then adding nano-silica, stirring and reacting for 24-36 hours, filtering, and washing with N,N-dimethylformamide and water in sequence to obtain nano-silica modified carbon fiber.

[0008] Preferably, the sand is composed of medium sand and fine sand in a mass ratio of (34-42): (58-66); the particle size of the medium sand is 30-70 mesh, and the particle size of the fine sand is 70-150 mesh.

[0009] Preferably, in step (2), the mass ratio of oxidized carbon fiber, styrene-TM I copolymer, dibutyltin dilaurate, and nano-silicon dioxide is 100:(20-60):(0.5-1.8):(5-30).

[0010] Preferably, the average particle size of nano-silicon dioxide is 10-30 nm.

[0011] Preferably, the preparation method of the styrene-TM I copolymer is as follows: styrene, 3-isopropenyl-α,α-dimethylbenzyl isocyanate TMI, and dibenzoyl peroxide are added to toluene, and the mixture is heated at 75-80° C. in a nitrogen atmosphere, stirred and reacted for 24-30 hours. After cooling, the solution is poured into methanol for precipitation, filtered, and washed with methanol to obtain the styrene-TM I copolymer.

[0012] Preferably, the mass ratio of styrene, 3-isopropenyl-α,α-dimethylbenzyl isocyanate TM I, and dibenzoyl peroxide is 100:(2-8):(2.2-3).

[0013] Preferably, the preparation method of the crack-resistant, super-strong, and highly flexible diamond sand carbon fiber tile adhesive is as follows: water, cement, sand, cellulose ether, redispersible latex powder, nano-silica modified carbon fiber, and diamond sand are added to a mixer, stirred and mixed, and vibrated to degas to obtain the crack-resistant, super-strong, and highly flexible diamond sand carbon fiber tile adhesive.

[0014] The technical effect of the present invention is as follows: the present invention uses silicate cement and sand as the matrix of tile adhesive, and compounded with nano-silica-modified carbon fiber, corundum, cellulose ether and redispersible latex powder to obtain a crack-resistant, super-strong, and highly flexible diamond sand carbon fiber tile adhesive. A styrene-TM I copolymer containing an isocyanate group is used as a bridge to react sequentially with the hydroxyl groups on the surface of the oxidized carbon fiber and the hydroxyl groups on the surface of the nano-silica, thereby grafting the nano-silica onto the surface of the carbon fiber. Due to the good compatibility between nano-silica and cement and sand, the carbon fiber grafted with nano-silica also has good compatibility with cement and sand, and can be uniformly dispersed in the tile adhesive matrix, significantly improving the mechanical properties of the tile adhesive, exhibiting high tensile adhesive strength, compressive strength, and flexural strength, which is beneficial to improving the crack resistance and flexibility of the tile adhesive. At the same time, the carbon fiber grafted polystyrene copolymer has certain hydrophobicity and mechanical properties. Adding it to the tile adhesive matrix is ​​beneficial to improving water resistance and mechanical properties. The tile adhesive specimens still maintained a high tensile adhesive strength after being immersed in water for 7 days. DETAILED DESCRIPTION

[0015] The following description sets forth numerous specific details to facilitate a thorough understanding of the present invention. However, the present invention can be implemented in many other ways than those described herein, and those skilled in the art may make similar modifications without departing from the scope of the present invention. Therefore, the present invention is not limited to the specific implementations disclosed below.

[0016] The cement of the present invention is P.O42.5 silicate cement; the particle size of the medium sand is 30-70 mesh; the particle size of the fine sand is 70-150 mesh; the specification of the carbon fiber is 3 mm; and the average particle size of the corundum is 200 mesh.

[0017] Redispersible latex powder, Shandong Yade Waterproof Materials Co., Ltd.

[0018] Example 1

[0019] (1) Wash the carbon fiber with ethanol and water in turn, weigh 1 g of it and add it to 40 mL of 68% concentrated nitric acid after drying, stir and oxidize it for 6 h, filter it and wash it with water to obtain oxidized carbon fiber.

[0020] (2) Add 5 g of styrene, 0.2 g of 3-isopropenyl-α,α-dimethylbenzyl isocyanate TMI, and 0.12 g of dibenzoyl peroxide to 50 mL of toluene, heat to 80 ° C in a nitrogen atmosphere, stir and react for 24 hours, and after cooling, pour the solution into methanol for precipitation. After filtering, wash with methanol to obtain a styrene-TMI copolymer.

[0021] (3) Add 1 g of oxidized carbon fiber to 80 mL of N,N-dimethylformamide, stir, add 0.2 g of styrene-TMI copolymer and 5 mg of dibutyltin dilaurate, heat to 80 ° C in a nitrogen atmosphere, stir and react for 12 hours, then add 0.05 g of nano-silica with an average particle size of 30 nm, stir and react for 24 hours, filter, and wash with N,N-dimethylformamide and water in turn to obtain nano-silica modified carbon fiber.

[0022] (4) Add 2.5 kg of water, 3.8 kg of cement, 6.2 kg of sand (the sand is composed of medium sand and fine sand with a mass ratio of 35:65), 36 g of cellulose ether, 0.14 kg of redispersible latex powder, 10 g of nano-silica modified carbon fiber, and 0.15 kg of corundum into the mixer, stir and mix, and vibrate to degas to obtain crack-resistant, super-strong, and highly flexible corundum carbon fiber tile adhesive.

[0023] Example 2

[0024] (1) Add 5 g of styrene, 0.1 g of 3-isopropenyl-α,α-dimethylbenzyl isocyanate TMI, and 0.11 g of dibenzoyl peroxide to 50 mL of toluene, heat to 80 ° C in a nitrogen atmosphere, stir and react for 24 hours, cool the solution, pour it into methanol for precipitation, filter it, and wash it with methanol to obtain a styrene-TM I copolymer.

[0025] (2) Add 1 g of oxidized carbon fiber (prepared in Example 1) to 100 mL of N,N-dimethylformamide, stir, add 0.5 g of styrene-TM I copolymer and 14 mg of dibutyltin dilaurate, heat to 85 ° C in a nitrogen atmosphere, stir and react for 12 hours, then add 0.25 g of nano-silica with an average particle size of 10 nm, stir and react for 36 hours, filter, and wash with N,N-dimethylformamide and water in turn to obtain nano-silica modified carbon fiber.

[0026] (3) Add 2.2 kg of water, 3.5 kg of cement, 6.5 kg of sand (the sand is composed of medium sand and fine sand with a mass ratio of 40:60), 40 g of cellulose ether, 0.1 kg of redispersible latex powder, 30 g of nano-silica modified carbon fiber, and 0.22 kg of corundum into the mixer, stir and mix, and vibrate to degas to obtain crack-resistant, super-strong, and highly flexible corundum carbon fiber tile adhesive.

[0027] Example 3

[0028] (1) Add 5 g of styrene, 0.4 g of 3-isopropenyl-α,α-dimethylbenzyl isocyanate TMI, and 0.15 g of dibenzoyl peroxide to 60 mL of toluene, add 75 ° C in a nitrogen atmosphere, stir and react for 30 h, cool and pour the solution into methanol for precipitation, filter and wash with methanol to obtain styrene-TM I copolymer.

[0029] (2) Add 1 g of oxidized carbon fiber (prepared in Example 1) to 100 mL of N,N-dimethylformamide, stir, add 0.4 g of styrene-TM I copolymer and 10 mg of dibutyltin dilaurate, heat to 85 ° C in a nitrogen atmosphere, stir and react for 12 hours, then add 0.18 g of nano-silica with an average particle size of 10 nm, stir and react for 24 hours, filter, and wash with N,N-dimethylformamide and water in turn to obtain nano-silica modified carbon fiber.

[0030] (3) Add 3 kg of water, 4.0 kg of cement, 6.0 kg of sand (the sand is composed of medium sand and fine sand with a mass ratio of 42:58), 40 g of cellulose ether, 0.1 kg of redispersible latex powder, 50 g of nano-silica modified carbon fiber, and 0.28 kg of corundum into the mixer, stir and mix, and vibrate to degas to obtain crack-resistant, super-strong, and highly flexible corundum carbon fiber tile adhesive.

[0031] Example 4

[0032] (1) Add 5 g of styrene, 0.3 g of 3-isopropenyl-α,α-dimethylbenzyl isocyanate TMI, and 0.14 g of dibenzoyl peroxide to 60 mL of toluene, heat to 80 ° C in a nitrogen atmosphere, stir and react for 24 hours, cool the solution, pour it into methanol for precipitation, filter it, and wash it with methanol to obtain a styrene-TM I copolymer.

[0033] (2) Add 1 g of oxidized carbon fiber (prepared in Example 1) to 100 mL of N,N-dimethylformamide, stir, add 0.3 g of styrene-TM I copolymer and 8 mg of dibutyltin dilaurate, heat to 75 ° C in a nitrogen atmosphere, stir and react for 18 hours, then add 0.12 g of nano-silica with an average particle size of 10 nm, stir and react for 30 hours, filter, and wash with N,N-dimethylformamide and water in turn to obtain nano-silica modified carbon fiber.

[0034] (3) Add 2.8 kg of water, 3.5 kg of cement, 6.5 kg of sand (the sand is composed of medium sand and fine sand with a mass ratio of 34:66), 30 g of cellulose ether, 0.16 kg of redispersible latex powder, 65 g of nano-silica modified carbon fiber, and 0.34 kg of corundum into the mixer, stir and mix, and vibrate to degas to obtain crack-resistant, super-strong, and highly flexible corundum carbon fiber tile adhesive.

[0035] Example 5

[0036] (1) Add 5 g of styrene, 0.4 g of 3-isopropenyl-α,α-dimethylbenzyl isocyanate TMI, and 0.15 g of dibenzoyl peroxide to 60 mL of toluene, heat to 80 ° C in a nitrogen atmosphere, and stir to react for 30 hours. After cooling, pour the solution into methanol for precipitation, filter, and wash with methanol to obtain a styrene-TM I copolymer.

[0037] (2) Add 1 g of oxidized carbon fiber (prepared in Example 1) to 100 mL of N,N-dimethylformamide, stir, add 0.6 g of styrene-TM I copolymer and 18 mg of dibutyltin dilaurate, heat to 75 ° C in a nitrogen atmosphere, stir and react for 18 hours, then add 0.3 g of nano-silica with an average particle size of 10 nm, stir and react for 36 hours, filter, and wash with N,N-dimethylformamide and water in turn to obtain nano-silica modified carbon fiber.

[0038] (3) Add 2.2 kg of water, 3.5 kg of cement, 6.5 kg of sand (the sand is composed of medium sand and fine sand with a mass ratio of 40:60), 38 g of cellulose ether, 0.13 kg of redispersible latex powder, 80 g of nano-silica modified carbon fiber, and 0.4 kg of corundum into the mixer, stir and mix, and vibrate to degas to obtain crack-resistant, super-strong, and highly flexible corundum carbon fiber tile adhesive.

[0039] Comparative Example 1

[0040] (1) Add 2.5 kg of water, 3.8 kg of cement, 6.2 kg of sand (the sand is composed of medium sand and fine sand with a mass ratio of 35:65), 36 g of cellulose ether, 0.14 kg of redispersible latex powder, and 0.15 kg of corundum into a mixer, stir and mix, and vibrate to degas to obtain crack-resistant, super-strong, and highly flexible corundum carbon fiber tile adhesive.

[0041] Comparative Example 2

[0042] (1) Add 2.5 kg of water, 3.8 kg of cement, 6.2 kg of sand (the sand is composed of medium sand and fine sand with a mass ratio of 35:65), 36 g of cellulose ether, 0.14 kg of redispersible latex powder, 10 g of oxidized carbon fiber, and 0.15 kg of corundum into a mixer, stir and mix, and vibrate to degas to obtain crack-resistant, super-strong, and highly flexible corundum carbon fiber tile adhesive.

[0043] Comparative Example 3

[0044] (1) 1 g of oxidized carbon fiber was added to 80 mL of N,N-dimethylformamide, stirred, and then 0.2 g of styrene-TMI copolymer (prepared in Example 1) and 5 mg of dibutyltin dilaurate were added. The mixture was heated to 80 ° C in a nitrogen atmosphere, stirred for 12 h, filtered, and washed with N,N-dimethylformamide and water in turn to obtain modified carbon fiber.

[0045] (2) Add 2.5 kg of water, 3.8 kg of cement, 6.2 kg of sand (the sand is composed of medium sand and fine sand with a mass ratio of 35:65), 36 g of cellulose ether, 0.14 kg of redispersible latex powder, 10 g of modified carbon fiber, and 0.15 kg of corundum into a mixer, stir and mix, and vibrate to degas to obtain crack-resistant, super-strong, and highly flexible corundum carbon fiber tile adhesive.

[0046] Comparative Example 4

[0047] (1) Add 1 g of oxidized carbon fiber to 80 mL of N,N-dimethylformamide, stir, then add 0.05 g of nano-silica with an average particle size of 30 nm, stir, and filter to obtain nano-silica-carbon fiber.

[0048] (2) Add 2.5 kg of water, 3.8 kg of cement, 6.2 kg of sand (the sand is composed of medium sand and fine sand with a mass ratio of 35:65), 36 g of cellulose ether, 0.14 kg of redispersible latex powder, 10 g of nano-silica-carbon fiber, and 0.15 kg of corundum into the mixer, stir and mix, and vibrate to degas to obtain crack-resistant, super-strong, and highly flexible corundum carbon fiber tile adhesive.

[0049] Tile adhesive specimens were formed and cured according to JC / T 547-2017 for 28 days, and the tensile adhesive strength M was tested. After curing for 21 days, the tile adhesive specimens were immersed in water for 7 days, dried, and then tested for tensile adhesive strength M1.

[0050] Tile adhesive specimens were formed and cured for 28 days according to JC / T 1004-2017. Compressive and flexural strengths were then tested. The test results are shown in Table 1.

[0051] Table 1: Test results

[0052]

[0053]

[0054] After testing, the crack-resistant, super-strong, high-flexibility diamond sand carbon fiber tile adhesives of Examples 1-5 have higher tensile adhesive strength, compressive strength, and flexural strength. This is mainly because the styrene-TMI copolymer containing an isocyanate group is used as a bridge connection to react with the hydroxyl groups on the surface of the oxidized carbon fiber and the hydroxyl groups on the surface of the nano-silica in sequence, thereby grafting the nano-silica on the surface of the carbon fiber. Since the compatibility between nano-silica and cement (main component silicate) and sand (main component silica) is very good, the carbon fiber with nano-silica grafted on the surface is also very compatible with cement and sand, and can be evenly dispersed in the tile adhesive matrix, significantly improving the mechanical properties of the tile adhesive, which is beneficial to improving the crack resistance and flexibility of the tile adhesive. At the same time, the carbon fiber grafted polystyrene copolymer has certain hydrophobicity and mechanical properties. Adding it to the tile adhesive matrix is ​​beneficial to improving water resistance and mechanical properties. The tile adhesive specimen still maintains a high tensile adhesive strength after being immersed in water for 7 days.

[0055] Compared with Example 1, in Comparative Example 1, nano-silica-modified carbon fibers were not added, and the tensile adhesion strength, compressive strength, and flexural strength of the tile adhesive specimens were lower.

[0056] Compared with Example 1, Comparative Example 2 adds oxidized carbon fiber, which has poor compatibility with cement and sand, poor dispersion in the tile adhesive matrix, and poor carbon fiber reinforcement effect, resulting in low tensile adhesion strength, compressive strength and flexural strength of the tile adhesive specimen.

[0057] In Comparative Example 3, the surface of the modified carbon fiber is not grafted with nano-silica. In Comparative Example 4, the oxidized carbon fiber is physically blended with nano-silica, and nano-silica is not grafted onto the surface of the carbon fiber. The dispersion of the carbon fiber in the tile adhesive matrix is ​​poor, and the reinforcement effect is poor, resulting in low tensile adhesion strength, compressive strength and flexural strength of the tile adhesive specimens.

[0058] The above-described embodiments merely illustrate several implementations of the present invention, and while their descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the patent. It should be noted that a person skilled in the art would be able to make numerous variations and improvements without departing from the spirit of the present invention, all of which fall within the scope of protection of the present invention. Therefore, the scope of protection of the patent for this invention shall be determined by the appended claims.

Claims

1. A crack-resistant, super-strong, and highly flexible diamond sand carbon fiber tile adhesive, characterized in that: The crack-resistant, super-strong, and highly flexible diamond sand carbon fiber tile adhesive comprises 35-40 parts by weight of cement, 60-65 parts by weight of sand, 0.3-0.4 parts by weight of cellulose ether, 1-1.6 parts by weight of redispersible latex powder, 0.1-0.8 parts by weight of nano-silica modified carbon fiber, and 1.5-4 parts by weight of diamond sand; The preparation method of the nano-silica modified carbon fiber comprises the following steps: Step (1), washing the carbon fiber with ethanol and water in sequence, drying, adding it to concentrated nitric acid for oxidation, filtering, and then washing with water to obtain oxidized carbon fiber; Step (2): adding oxidized carbon fiber to N,N-dimethylformamide, stirring, adding styrene-TMI copolymer and dibutyltin dilaurate, carrying out a primary reaction in a nitrogen atmosphere, then adding nano-silica, carrying out a secondary reaction, filtering, and washing with N,N-dimethylformamide and water in turn to obtain nano-silica modified carbon fiber.

2. The crack-resistant, super-strong, high-flexibility diamond sand carbon fiber tile adhesive according to claim 1, characterized in that: The sand is composed of medium sand and fine sand in a mass ratio of (34-42): (58-66); the particle size of the medium sand is 30-70 meshes, and the particle size of the fine sand is 70-150 meshes.

3. The crack-resistant, super-strong, and highly flexible diamond sand carbon fiber tile adhesive according to claim 1, characterized in that: In the step (2), the mass ratio of oxidized carbon fiber, styrene-TMI copolymer, dibutyltin dilaurate, and nano-silicon dioxide is 100:(20-60):(0.5-1.8):(5-30).

4. The crack-resistant, super-strong, and highly flexible diamond sand carbon fiber tile adhesive according to claim 1, characterized in that: The average particle size of the nano-silicon dioxide is 10-30 nm.

5. The crack-resistant, super-strong, and highly flexible diamond sand carbon fiber tile adhesive according to claim 1, characterized in that: In step (2), the temperature of the primary reaction is 75-85° C., and the reaction time is 12-18 h; the time of the secondary reaction is 24-36 h.

6. The crack-resistant, super-strong, and highly flexible diamond sand carbon fiber tile adhesive according to claim 3, characterized in that: The preparation method of the styrene-TMI copolymer comprises the following steps: adding styrene, 3-isopropenyl-α,α-dimethylbenzyl isocyanate TMI, and dibenzoyl peroxide to toluene; heating the mixture to 75-80° C. in a nitrogen atmosphere; stirring the mixture for reaction for 24-30 hours; cooling the mixture; pouring the solution into methanol for precipitation; filtering the mixture; and washing the mixture with methanol to obtain the styrene-TMI copolymer.

7. The crack-resistant, super-strong, and highly flexible diamond sand carbon fiber tile adhesive according to claim 6, characterized in that: The mass ratio of styrene, 3-isopropenyl-α,α-dimethylbenzyl isocyanate TMI, and dibenzoyl peroxide is 100:(2-8):(2.2-3).

8. A method for preparing the crack-resistant, super-strong, and highly flexible diamond grit carbon fiber tile adhesive according to any one of claims 1 to 7, characterized in that: The preparation method comprises the following steps: adding water, cement, sand, cellulose ether, redispersible latex powder, nano-silicon dioxide modified carbon fiber and corundum into a mixer, stirring and mixing, and vibrating to degas, so as to obtain crack-resistant, super-strong and highly flexible corundum carbon fiber tile adhesive.

9. Use of the crack-resistant, super-strong, and highly flexible diamond grit carbon fiber tile adhesive as claimed in any one of claims 1 to 7 in tile products.

10. Use of the crack-resistant, super-strong, and highly flexible diamond grit carbon fiber tile adhesive prepared by the preparation method according to claim 8 in tile products.

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