High-adhesion elastic tile adhesive and preparation method thereof
Through the combination of modified glue powder and reinforcement, the bonding and mechanical strength of tiles are improved, and the problem of tiles being susceptible to falling off by the substrate is solved, and the high bonding and vibration resistance of tiles are achieved.
Patent Information
- Application Number
- CN202311287939.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-09-28
- Publication Date
- 2025-09-02
- Estimated Expiration
- 2043-09-28
AI Technical Summary
The adhesiveness of existing ceramic tile glue is insufficient and is easily damaged by the influence of the substrate, causing the tile to fall off.
Using a combination of modified gel powder and reinforcement, the modified gel powder is polymerized by polymerizing γ-glycidyl etheroxypropylmethyldimethoxysilane with 1,1,3,3-tetramethyldisiloxane to form a dihydrogen-terminal polysiloxane. After the intermediate reacts, it reacts with dopamine and dicyclohexylcarbodiimide to form a polyurethane prepolymer, and KH550 ends; the reinforcement is hydrolyzed by KH550 and treated with glutaraldehyde to form an aminolated silsesquioxane. The modifier and the modified matrix form a core-shell structure under alkaline conditions, and triethylenetetramine crosslinks.
Improve the adhesion and mechanical strength of ceramic tile adhesive, enhance the vibration and shrinkage resistance to the substrate, and prevent the tile from falling off.
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Figure BDA0004480366830000111
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of tile adhesive preparation, and in particular to an elastic tile adhesive with high adhesion and a preparation method thereof. Background Art
[0002] Currently, with the rapid development of the building decoration industry, ceramic tiles have garnered significant attention for their decorative properties in both indoor and outdoor settings, as well as their ease of implementation. As the use and decorative applications of ceramic tiles continue to grow, so too has the demand for tile adhesives. When it comes to adhering these tiles to the substrate wall, the traditional method of using sand-cement grouting suffers from insufficient bonding strength, leading to tile hollowing and detachment. Tile adhesives formulated with the addition of redispersible polymer powders and other cementitious ingredients effectively address this issue, leading to their widespread use in interior home tile installations. However, existing tile adhesives lack sufficient mechanical and adhesive properties. Vibration or shrinkage of the substrate significantly reduces the adhesive's adhesion, leading to tile detachment. Consequently, a stable tile adhesive is urgently needed to address this issue. Summary of the Invention
[0003] The purpose of the present invention is to provide a high-adhesion elastic tile adhesive and a preparation method, which solves the problem that the adhesion of current tile adhesives is insufficient and is easily affected by the substrate, thereby damaging the adhesion of tiles.
[0004] The purpose of the present invention can be achieved through the following technical solutions:
[0005] A method for preparing a high-adhesion elastic tile adhesive comprises the following steps:
[0006] The following raw materials are weighed in parts by weight: 300-350 parts of cement, 650-700 parts of sand, 3-5 parts of hydroxypropyl methylcellulose, 2-4 parts of calcium formate, 10-13 parts of a strengthening agent, 20-30 parts of modified rubber powder and 1.5-3 parts of triethylenetetramine, and the above raw materials are mixed evenly to prepare a high-adhesion elastic tile adhesive.
[0007] Furthermore, the modified rubber powder is prepared by the following steps:
[0008] Step A1: γ-glycidoxypropylmethyldimethoxysilane and deionized water are mixed and stirred at a speed of 200-300 r / min and a temperature of 60-70° C. for 10-15 minutes. Concentrated sulfuric acid and 1,1,3,3-tetramethyldisiloxane are then added and reacted for 4-6 hours. The pH is then adjusted to neutral to obtain a dihydrogen-terminated polysiloxane.
[0009] Step A2: Mix dihydrogen-terminated polysiloxane, propylene alcohol, and DMF, stir at a speed of 120-150 r / min and a temperature of 50-55°C, add chloroplatinic acid, raise the temperature to 60-65°C, and react for 3-4 hours to obtain intermediate 1. Dopamine, 2,2-dimethylpropionic acid, dicyclohexylcarbodiimide, and DMF are mixed uniformly, and react at a speed of 200-300 r / min and a temperature of 40-50°C for 3-5 hours to obtain intermediate 2.
[0010] Step A3: Intermediate 1, intermediate 2, hexamethylene diisocyanate, polytetrahydrofuran diol and 2,2-dimethylpropionic acid are mixed, nitrogen protection is introduced, and the reaction is carried out at a speed of 150-200 r / min and a temperature of 80-85°C for 6-8 hours. After cooling to 60-65°C, KH550 and triethylamine are added, and the reaction is continued for 1-1.5 hours to obtain a modified rubber powder.
[0011] Furthermore, the ratio of γ-glycidyloxypropylmethyldimethoxysilane, deionized water and 1,1,3,3-tetramethyldisiloxane used in step A1 is 2mmol:10mL:5mmol, and the amount of concentrated sulfuric acid used is 5-8% of the total mass of 3-glycidyloxypropylmethyldiethoxysilane and 1,1,3,3-tetramethyldisiloxane.
[0012] Furthermore, the molar ratio of the dihydrogen-terminated polysiloxane and 2,3-dihydroxy-1-butene described in step A2 is 1:2, the concentration of chloroplatinic acid in the mixture of dihydrogen-terminated polysiloxane and 2,3-dihydroxy-1-butene is 15-20 ppm, and the molar ratio of dopamine, 2,2-dimethylpropionic acid and dicyclohexylcarbodiimide is 1:1:1.1.
[0013] Furthermore, the mass ratio of the intermediate 1, intermediate 2, hexamethylene diisocyanate, polytetrahydrofuran diol, 2,2-dimethylpropionic acid, KH550 and triethylamine described in step A3 is 5.6:2.8:25:50:3.5:1.4:3.6.
[0014] Furthermore, the enhancer is prepared by the following steps:
[0015] Step B1: KH550, ethanol, deionized water, and tetramethylammonium hydroxide are uniformly mixed, reacted at a speed of 200-300 r / min and a temperature of 20-25° C. for 3-5 hours, then heated to 70-80° C. and continued to react for 10-15 hours. The reaction solution is added to petroleum ether, and the filtrate is filtered to remove the filtrate to obtain amino silsesquioxane. The amino silsesquioxane is dissolved in tetrahydrofuran, stirred at a speed of 150-200 r / min and a temperature of 40-50° C., and glutaraldehyde is added and reacted for 4-6 hours to obtain a modified matrix;
[0016] Step B2: Add polyvinyl alcohol to deionized water, stir for 1-1.5 hours at a speed of 60-80 r / min and a temperature of 20-25°C, then raise the temperature to 90-95°C, add epichlorohydrin and sodium hydroxide solution, maintain the pH value at 10, and react for 5-7 hours to obtain a modifier. The modified substrate, modifier and DMF are evenly mixed, and reacted for 6-8 hours at a speed of 150-200 r / min, a temperature of 30-40°C and a pH value of 10-11 to obtain a strengthener.
[0017] Furthermore, the mass ratio of KH550, ethanol and deionized water in step B1 is 1:80:8, the amount of tetramethylammonium hydroxide is 3% of the mass of KH550, and the amount of glutaraldehyde is 10% of the mass of KH550.
[0018] Furthermore, the amount of epichlorohydrin used in step B2 is 1-1.5% of the mass of polyvinyl alcohol, the mass fraction of sodium hydroxide solution is 15%, the molecular weight of polyvinyl alcohol is 600, and the mass ratio of modified matrix to modifier is 1:8-10.
[0019] The beneficial effects of the present invention are as follows: a high-adhesion elastic tile adhesive prepared by the present invention comprises the following raw materials: cement, sand, hydroxypropyl methylcellulose, calcium formate, a strengthening agent, modified rubber powder and triethylenetetramine, wherein the modified rubber powder is hydrolyzed with γ-glycidyloxypropylmethyldimethoxysilane as a raw material, and then polymerized with 1,1,3,3-tetramethyldisiloxane to form a dihydrogen-terminated polysiloxane, and the dihydrogen-terminated polysiloxane and allyl alcohol are reacted under the action of chloroplatinic acid, so that the Si-H bond on the dihydrogen-terminated polysiloxane reacts with the double bond on the allyl alcohol to prepare an intermediate 1, and dopamine and 2,2-dimethylpropionic acid are reacted in a dicyclopentadiene silane. The reaction is carried out under the action of hexylcarbodiimide, so that the amino group on dopamine and the carboxyl group on 2,2-dimethylpropionic acid undergo dehydration condensation to obtain intermediate 2. Intermediate 1, intermediate 2, hexamethylene diisocyanate, polytetramethylene glycol and 2,2-dimethylpropionic acid are reacted to form a polyurethane prepolymer, KH550 and triethylamine are added, KH550 is capped, and triethylamine reacts with the side chain carboxyl group to obtain a modified rubber powder. The modified rubber powder contains an organic silicon segment on the molecular chain, which can increase the waterproof performance of the tile adhesive, and the bisphenol structure of the side chain can increase the adhesion of the tile adhesive. At the same time, the siloxane group is capped, and the siloxane will hydrate when it encounters water. The hydrolysis generates silanol groups, which are then grafted with the hydroxyl groups on the surface of cement and sand particles, thereby enhancing the coordination between the modified rubber powder and the inorganic particles, thereby enhancing the strength of the tile adhesive. The strengthening agent is prepared by hydrolysis and polymerization of KH550 as a raw material to obtain amino silsesquioxane, which is treated with glutaraldehyde to react the aldehyde group on the glutaraldehyde with part of the amino group on the amino silsesquioxane, and the adjacent amino silsesquioxanes are connected to obtain a modified matrix. Polyvinyl alcohol and epichlorohydrin are reacted to open the ring of epichlorohydrin and react with the hydroxyl groups on the polypropylene alcohol, and then close the ring under alkaline conditions to form an epoxy group to obtain a modifier. The modifier and the modified matrix are mixed under alkaline conditions, so that the epoxy group on the side chain of the modifier reacts with the amino group on the modified matrix, thereby forming a core-shell structure of the modifier coating the modified matrix to prepare a reinforcing agent. The reinforcing agent has a core-shell structure and can increase the mechanical strength of the tile adhesive. In the process of mixing with the modified adhesive powder and triethylenetetramine, the triethylenetetramine can react and cross-link with the epoxy group on the reinforcing agent and the epoxy group on the modified adhesive powder, and the modified adhesive powder molecules are coated on the reinforcing agent to form a multi-layer core-shell structure. At the same time, the modified adhesive powder molecules are an elastomeric structure, so that the tile adhesive can absorb and weaken the substrate due to vibration and expansion and contraction, which damages the adhesion of the tiles. DETAILED DESCRIPTION
[0020] The following is a clear and complete description of the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative efforts are within the scope of protection of the present invention.
[0021] Example 1
[0022] A method for preparing a high-adhesion elastic tile adhesive comprises the following steps:
[0023] The following raw materials were weighed in parts by weight: 300 parts of cement, 650 parts of sand, 3 parts of hydroxypropyl methylcellulose, 2 parts of calcium formate, 10 parts of a strengthening agent, 20 parts of modified rubber powder, and 1.5 parts of triethylenetetramine. The raw materials were mixed evenly to prepare a high-adhesion elastic tile adhesive.
[0024] The cement is Portland cement No. 42.5, the fineness of the sand is 0.3 mm, and the model of the hydroxypropyl methylcellulose is 30011C.
[0025] The modified rubber powder is prepared by the following steps:
[0026] Step A1: γ-glycidoxypropylmethyldimethoxysilane and deionized water were mixed and stirred at a speed of 200 r / min and a temperature of 60° C. for 10 minutes. Concentrated sulfuric acid and 1,1,3,3-tetramethyldisiloxane were then added and reacted for 4 hours. The pH was then adjusted to neutral to obtain a dihydrogen-terminated polysiloxane.
[0027] Step A2: Dihydrogen-terminated polysiloxane, propylene alcohol, and DMF were mixed, stirred at a speed of 120 r / min and a temperature of 50°C, and chloroplatinic acid was added. The temperature was raised to 60°C, and the reaction was carried out for 3 hours to obtain Intermediate 1. Dopamine, 2,2-dimethylpropionic acid, dicyclohexylcarbodiimide, and DMF were mixed uniformly, and the reaction was carried out at a speed of 200 r / min and a temperature of 40°C for 3 hours to obtain Intermediate 2.
[0028] Step A3: Intermediate 1, intermediate 2, hexamethylene diisocyanate, polytetrahydrofuran diol and 2,2-dimethylpropionic acid were mixed, nitrogen protection was introduced, and the reaction was carried out at a speed of 150 r / min and a temperature of 80°C for 6 hours. After cooling to 60°C, KH550 and triethylamine were added, and the reaction was continued for 1 hour to obtain a modified rubber powder.
[0029] The amount ratio of γ-glycidyloxypropylmethyldimethoxysilane, deionized water and 1,1,3,3-tetramethyldisiloxane described in step A1 is 2mmol:10mL:5mmol, and the amount of concentrated sulfuric acid used is 5% of the total mass of 3-glycidyloxypropylmethyldiethoxysilane and 1,1,3,3-tetramethyldisiloxane.
[0030] The molar ratio of the dihydrogen-terminated polysiloxane and 2,3-dihydroxy-1-butene described in step A2 is 1:2, the concentration of chloroplatinic acid in the mixture of dihydrogen-terminated polysiloxane and 2,3-dihydroxy-1-butene is 15 ppm, and the molar ratio of dopamine, 2,2-dimethylpropionic acid and dicyclohexylcarbodiimide is 1:1:1.1.
[0031] The mass ratio of intermediate 1, intermediate 2, hexamethylene diisocyanate, polytetrahydrofuran diol, 2,2-dimethylpropionic acid, KH550 and triethylamine described in step A3 is 5.6:2.8:25:50:3.5:1.4:3.6, and the molecular weight of polytetrahydrofuran diol is 1000.
[0032] The enhancer is prepared by the following steps:
[0033] Step B1: KH550, ethanol, deionized water, and tetramethylammonium hydroxide were uniformly mixed, reacted at a speed of 200 r / min and a temperature of 20° C. for 3 hours, then heated to 70° C. and continued to react for 10 hours. The reaction solution was added to petroleum ether, and the filtrate was filtered to remove the filtrate to obtain amino silsesquioxane. The amino silsesquioxane was dissolved in tetrahydrofuran, stirred at a speed of 150 r / min and a temperature of 40° C., and glutaraldehyde was added and reacted for 4 hours to obtain a modified matrix;
[0034] Step B2: Add polyvinyl alcohol to deionized water, stir for 1 hour at a speed of 60 r / min and a temperature of 20°C, then heat to 90°C, add epichlorohydrin and sodium hydroxide solution, maintain the pH value at 10, and react for 5 hours to obtain a modifier. The modified substrate, modifier and DMF are evenly mixed, and reacted for 6 hours at a speed of 150 r / min, a temperature of 30°C and a pH value of 10 to obtain a strengthener.
[0035] The mass ratio of KH550, ethanol and deionized water in step B1 is 1:80:8, the amount of tetramethylammonium hydroxide used is 3% of the mass of KH550, and the amount of glutaraldehyde used is 10% of the mass of KH550.
[0036] The amount of epichlorohydrin used in step B2 is 1% by mass of polyvinyl alcohol, the mass fraction of sodium hydroxide solution is 15%, the molecular weight of polyvinyl alcohol is 600, and the mass ratio of modified matrix to modifier is 1:8.
[0037] Example 2
[0038] A method for preparing a high-adhesion elastic tile adhesive comprises the following steps:
[0039] The following raw materials were weighed in parts by weight: 330 parts of cement, 680 parts of sand, 4 parts of hydroxypropyl methylcellulose, 3 parts of calcium formate, 12 parts of a strengthening agent, 25 parts of modified rubber powder, and 2.3 parts of triethylenetetramine. The raw materials were mixed evenly to prepare a high-adhesion elastic tile adhesive.
[0040] The cement is Portland cement No. 42.5, the fineness of the sand is 0.4 mm, and the model of the hydroxypropyl methylcellulose is 30011C.
[0041] The modified rubber powder is prepared by the following steps:
[0042] Step A1: γ-glycidoxypropylmethyldimethoxysilane and deionized water were mixed and stirred at a speed of 200 r / min and a temperature of 65° C. for 13 minutes. Concentrated sulfuric acid and 1,1,3,3-tetramethyldisiloxane were then added and reacted for 5 hours. The pH was then adjusted to neutral to obtain a dihydrogen-terminated polysiloxane.
[0043] Step A2: Dihydrogen-terminated polysiloxane, propylene alcohol, and DMF were mixed, stirred at a speed of 120 r / min and a temperature of 53°C, and chloroplatinic acid was added. The temperature was raised to 63°C, and the reaction was carried out for 3.5 hours to obtain Intermediate 1. Dopamine, 2,2-dimethylpropionic acid, dicyclohexylcarbodiimide, and DMF were mixed uniformly, and the reaction was carried out at a speed of 200 r / min and a temperature of 45°C for 4 hours to obtain Intermediate 2.
[0044] Step A3: Intermediate 1, intermediate 2, hexamethylene diisocyanate, polytetrahydrofuran diol and 2,2-dimethylpropionic acid were mixed, nitrogen protection was introduced, and the reaction was carried out at a speed of 150 r / min and a temperature of 83°C for 7 hours. After cooling to 63°C, KH550 and triethylamine were added, and the reaction was continued for 1.3 hours to obtain a modified rubber powder.
[0045] The amount ratio of γ-glycidyloxypropylmethyldimethoxysilane, deionized water and 1,1,3,3-tetramethyldisiloxane described in step A1 is 2mmol:10mL:5mmol, and the amount of concentrated sulfuric acid used is 6% of the total mass of 3-glycidyloxypropylmethyldiethoxysilane and 1,1,3,3-tetramethyldisiloxane.
[0046] The molar ratio of the dihydrogen-terminated polysiloxane and 2,3-dihydroxy-1-butene described in step A2 is 1:2, the concentration of chloroplatinic acid in the mixture of dihydrogen-terminated polysiloxane and 2,3-dihydroxy-1-butene is 18 ppm, and the molar ratio of dopamine, 2,2-dimethylpropionic acid and dicyclohexylcarbodiimide is 1:1:1.1.
[0047] The mass ratio of intermediate 1, intermediate 2, hexamethylene diisocyanate, polytetrahydrofuran diol, 2,2-dimethylpropionic acid, KH550 and triethylamine described in step A3 is 5.6:2.8:25:50:3.5:1.4:3.6, and the molecular weight of polytetrahydrofuran diol is 1000.
[0048] The enhancer is prepared by the following steps:
[0049] Step B1: KH550, ethanol, deionized water, and tetramethylammonium hydroxide were uniformly mixed, reacted at a speed of 200 r / min and a temperature of 23° C. for 4 hours, then heated to 75° C. and continued to react for 13 hours. The reaction solution was added to petroleum ether, and the filtrate was filtered to remove the filtrate to obtain amino silsesquioxane. The amino silsesquioxane was dissolved in tetrahydrofuran, stirred at a speed of 150 r / min and a temperature of 45° C., and glutaraldehyde was added and reacted for 5 hours to obtain a modified matrix;
[0050] Step B2: Add polyvinyl alcohol to deionized water, stir for 1.3 hours at a speed of 60 r / min and a temperature of 23°C, then heat to 93°C, add epichlorohydrin and sodium hydroxide solution, maintain the pH value at 10, and react for 6 hours to obtain a modifier. The modified substrate, modifier and DMF are evenly mixed, and reacted at a speed of 150 r / min, a temperature of 35°C and a pH value of 11 for 6-8 hours to obtain a strengthener.
[0051] The mass ratio of KH550, ethanol and deionized water in step B1 is 1:80:8, the amount of tetramethylammonium hydroxide used is 3% of the mass of KH550, and the amount of glutaraldehyde used is 10% of the mass of KH550.
[0052] The amount of epichlorohydrin used in step B2 is 1.3% of the mass of polyvinyl alcohol, the mass fraction of sodium hydroxide solution is 15%, the molecular weight of polyvinyl alcohol is 600, and the mass ratio of modified matrix to modifier is 1:9.
[0053] Example 3
[0054] A method for preparing a high-adhesion elastic tile adhesive comprises the following steps:
[0055] The following raw materials were weighed in parts by weight: 350 parts of cement, 700 parts of sand, 5 parts of hydroxypropyl methylcellulose, 4 parts of calcium formate, 13 parts of a strengthening agent, 30 parts of modified rubber powder, and 3 parts of triethylenetetramine. The raw materials were mixed evenly to prepare a high-adhesion elastic tile adhesive.
[0056] The cement is Portland cement No. 42.5R, the fineness of the sand is 0.5 mm, and the model of the hydroxypropyl methylcellulose is 30011C.
[0057] The modified rubber powder is prepared by the following steps:
[0058] Step A1: γ-glycidoxypropylmethyldimethoxysilane and deionized water were mixed and stirred at a speed of 300 r / min and a temperature of 70°C for 15 minutes. Concentrated sulfuric acid and 1,1,3,3-tetramethyldisiloxane were then added and reacted for 6 hours. The pH was then adjusted to neutral to obtain a dihydrogen-terminated polysiloxane.
[0059] Step A2: Dihydrogen-terminated polysiloxane, propylene alcohol, and DMF were mixed, stirred at a speed of 150 r / min and a temperature of 55°C, and chloroplatinic acid was added. The temperature was raised to 65°C, and the reaction was carried out for 4 hours to obtain Intermediate 1. Dopamine, 2,2-dimethylpropionic acid, dicyclohexylcarbodiimide, and DMF were mixed uniformly, and the reaction was carried out at a speed of 300 r / min and a temperature of 50°C for 5 hours to obtain Intermediate 2.
[0060] Step A3: Intermediate 1, intermediate 2, hexamethylene diisocyanate, polytetrahydrofuran diol and 2,2-dimethylpropionic acid were mixed, nitrogen protection was introduced, and the reaction was carried out at a speed of 200 r / min and a temperature of 85°C for 8 hours. After cooling to 65°C, KH550 and triethylamine were added, and the reaction was continued for 1.5 hours to obtain a modified rubber powder.
[0061] The amount ratio of γ-glycidyloxypropylmethyldimethoxysilane, deionized water and 1,1,3,3-tetramethyldisiloxane described in step A1 is 2mmol:10mL:5mmol, and the amount of concentrated sulfuric acid used is 8% of the total mass of 3-glycidyloxypropylmethyldiethoxysilane and 1,1,3,3-tetramethyldisiloxane.
[0062] The molar ratio of the dihydrogen-terminated polysiloxane and 2,3-dihydroxy-1-butene described in step A2 is 1:2, the concentration of chloroplatinic acid in the mixture of dihydrogen-terminated polysiloxane and 2,3-dihydroxy-1-butene is 20 ppm, and the molar ratio of dopamine, 2,2-dimethylpropionic acid and dicyclohexylcarbodiimide is 1:1:1.1.
[0063] The mass ratio of intermediate 1, intermediate 2, hexamethylene diisocyanate, polytetrahydrofuran diol, 2,2-dimethylpropionic acid, KH550 and triethylamine described in step A3 is 5.6:2.8:25:50:3.5:1.4:3.6, and the molecular weight of polytetrahydrofuran diol is 1000.
[0064] The enhancer is prepared by the following steps:
[0065] Step B1: KH550, ethanol, deionized water, and tetramethylammonium hydroxide were uniformly mixed, reacted at a speed of 300 r / min and a temperature of 25° C. for 5 hours, then heated to 80° C. and continued to react for 15 hours. The reaction solution was added to petroleum ether, and the filtrate was filtered to remove the filtrate to obtain amino silsesquioxane. The amino silsesquioxane was dissolved in tetrahydrofuran, stirred at a speed of 200 r / min and a temperature of 50° C., and glutaraldehyde was added and reacted for 6 hours to obtain a modified matrix;
[0066] Step B2: Add polyvinyl alcohol to deionized water, stir for 1.5 hours at a speed of 80 r / min and a temperature of 25°C, then heat to 95°C, add epichlorohydrin and sodium hydroxide solution, maintain the pH value at 10, and react for 7 hours to obtain a modifier. The modified substrate, modifier and DMF are evenly mixed, and reacted for 8 hours at a speed of 200 r / min, a temperature of 40°C and a pH value of 11 to obtain a strengthener.
[0067] The mass ratio of KH550, ethanol and deionized water in step B1 is 1:80:8, the amount of tetramethylammonium hydroxide used is 3% of the mass of KH550, and the amount of glutaraldehyde used is 10% of the mass of KH550.
[0068] The amount of epichlorohydrin used in step B2 is 1.5% by mass of polyvinyl alcohol, the mass fraction of sodium hydroxide solution is 15%, the molecular weight of polyvinyl alcohol is 600, and the mass ratio of modified matrix to modifier is 1:10.
[0069] Comparative Example 1
[0070] Compared with Example 1, no enhancer was added in this comparative example, and the remaining steps were the same.
[0071] Comparative Example 2
[0072] Compared with Example 1, this comparative example did not add intermediate 1, and the remaining steps were the same.
[0073] Comparative Example 3
[0074] Compared with Example 1, this comparative example did not add intermediate 2, and the remaining steps were the same.
[0075] The tile adhesives prepared in Examples 1-3 and Comparative Examples 1-3 were tested according to the JC / T547-2005 standard. The test results are shown in the following table.
[0076]
[0077]
[0078] It can be seen from the above table that this application has a good bonding effect and can ensure the normal bonding of tiles.
[0079] The above content is merely an example and explanation of the concept of the present invention. Those skilled in the art may make various modifications or additions to the described specific embodiments or replace them in a similar manner. As long as they do not deviate from the concept of the invention or exceed the scope defined by the claims, they should all fall within the scope of protection of the present invention.
Claims
1. A method for preparing a high-adhesion elastic tile adhesive, characterized by: The specific steps include: Weigh the following raw materials in parts by weight: 300-350 parts of cement, 650-700 parts of sand, 3-5 parts of hydroxypropyl methylcellulose, 2-4 parts of calcium formate, 10-13 parts of a strengthening agent, 20-30 parts of modified rubber powder, and 1.5-3 parts of triethylenetetramine, and mix the above raw materials evenly to prepare a high-adhesion elastic tile adhesive; The modified rubber powder is prepared by the following steps: Step A1: After mixing γ-glycidyloxypropylmethyldimethoxysilane and deionized water, concentrated sulfuric acid and 1,1,3,3-tetramethyldisiloxane are added, reacted, and the pH is adjusted to neutral to prepare a dihydrogen-terminated polysiloxane; Step A2: Mixing dihydrogen-terminated polysiloxane, propylene alcohol, and DMF, adding chloroplatinic acid, and heating to react to obtain intermediate 1; mixing dopamine, 2,2-dimethylpropionic acid, dicyclohexylcarbodiimide, and DMF to react to obtain intermediate 2; Step A3: Intermediate 1, intermediate 2, hexamethylene diisocyanate, polytetrahydrofuran diol, and 2,2-dimethylpropionic acid are mixed, nitrogen is introduced for protection, and the mixture is reacted. The mixture is then cooled and KH550 and triethylamine are added to continue the reaction to obtain a modified rubber powder. The reinforcing agent is prepared by the following steps: Step B1: KH550, ethanol, deionized water, and tetramethylammonium hydroxide are mixed and reacted, and the temperature is increased to continue the reaction. The reaction solution is added to petroleum ether, and the filtrate is filtered to remove the filtrate to obtain amino silsesquioxane. The amino silsesquioxane is dissolved in tetrahydrofuran, stirred, and glutaraldehyde is added to react to obtain a modified matrix; Step B2: Add polyvinyl alcohol to deionized water and stir, then heat it and add epichlorohydrin and sodium hydroxide solution, keep the pH value alkaline, and react to obtain a modifier, and mix the modified substrate, modifier and DMF to obtain a strengthening agent.
2. The method for preparing a high-adhesion elastic tile adhesive according to claim 1, characterized in that: The amount ratio of γ-glycidyloxypropylmethyldimethoxysilane, deionized water and 1,1,3,3-tetramethyldisiloxane described in step A1 is 2mmol:10mL:5mmol, and the amount of concentrated sulfuric acid used is 5-8% of the total mass of 3-glycidyloxypropylmethyldiethoxysilane and 1,1,3,3-tetramethyldisiloxane.
3. The method for preparing a high-adhesion elastic tile adhesive according to claim 1, characterized in that: The molar ratio of dopamine, 2,2-dimethylpropionic acid and dicyclohexylcarbodiimide in step A2 is 1:1:1.
1.
4. The method for preparing a high-adhesion elastic tile adhesive according to claim 1, characterized in that: The mass ratio of intermediate 1, intermediate 2, hexamethylene diisocyanate, polytetrahydrofuran diol, 2,2-dimethylpropionic acid, KH550 and triethylamine described in step A3 is 5.6:2.8:25:50:3.5:1.4:3.
6.
5. The method for preparing a high-adhesion elastic tile adhesive according to claim 1, characterized in that: The mass ratio of KH550, ethanol and deionized water in step B1 is 1:80:8, the amount of tetramethylammonium hydroxide is 3% of the mass of KH550, and the amount of glutaraldehyde is 10% of the mass of KH550.
6. The method for preparing a high-adhesion elastic tile adhesive according to claim 1, characterized in that: The amount of epichlorohydrin used in step B2 is 1-1.5% by mass of polyvinyl alcohol, the mass fraction of sodium hydroxide solution is 15%, and the mass ratio of modified substrate to modifier is 1:8-10.
7. A high-adhesion elastic tile adhesive, characterized by: Prepared according to any one of claims 1 to 6.
Citation Information
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Ceramic tile adhesive special for saltpetering-resistant super-soft rock board and preparation method of ceramic tile adhesive
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