An adhesive for building ceramic tiles and a method for preparing the same

Abstract

The application relates to the technical field of adhesives, and particularly discloses a building ceramic tile adhesive and a preparation method thereof. The building ceramic tile adhesive is mainly prepared from the following raw materials in parts by weight: cement 90-100 parts, machine-made sand 125-145 parts, fly ash 30-40 parts, microsilica 10-20 parts, modified redispersible latex powder 5-7 parts, attapulgite 2-4 parts and water reducing agent 0.5-2 parts. The modified redispersible latex powder is obtained by treating redispersible latex powder with sodium hydroxide, 4-chloroacetyl acetic acid, 3-aminopropyl trimethoxysilane, 3-butene-1-amine and dimethylpropyl sulfonic acid amine ethyl methacrylate. The adhesive has the advantages of strong adhesion, good water resistance and good frost resistance, and meets the market demand.

Description

Technical Field

[0001] This application relates to the field of adhesive technology, and more specifically, to an adhesive for building ceramic tiles and a method for preparing the same. Background Technology

[0002] Tiles are a crucial decorative material in home improvement, widely accepted and used. During tile installation, adhesives are inevitably needed, providing excellent bonding to ensure tiles adhere firmly to the wall surface. Common adhesives on the market typically consist of cement, sand, fly ash, and water-reducing agents, mixed together to form the adhesive. To use, water is added to the adhesive to create a slurry, which is then applied to the wall surface. The tiles are then adhered to the slurry, and after the water evaporates, a stable bond is achieved between the tile and the wall. To further improve the adhesive's bonding strength, some researchers have added redispersible latex powder to the raw materials. This has been verified to increase the tensile bond strength of the adhesive to 1.9 MPa, although further improvements in bonding performance are needed. Summary of the Invention

[0003] To improve the adhesion of adhesives, this application provides an adhesive for building ceramic tiles and a method for preparing the same.

[0004] In a first aspect, this application provides an adhesive for building ceramic tiles, employing the following technical solution: An adhesive for building ceramic tiles is mainly composed of the following raw materials in parts by weight: 90-100 parts cement, 125-145 parts manufactured sand, 30-40 parts fly ash, 10-20 parts silica fume, 5-7 parts modified redispersible latex powder, 2-4 parts attapulgite, and 0.5-2 parts water-reducing agent; wherein the modified redispersible latex powder is obtained by treating redispersible latex powder with sodium hydroxide, 4-chloroacetoacetic acid, 3-aminopropyltrimethoxysilane, 3-butene-1-amine, and dimethylpropylsulfonate ethyl methacrylate.

[0005] The adhesive of this application incorporates redispersible latex powder and attapulgite in its raw materials, utilizing their synergistic effect to improve the tensile bond strength, post-immersion tensile bond strength, and post-freeze-thaw cycle tensile bond strength. Furthermore, the redispersible latex powder is treated with sodium hydroxide, 4-chloroacetoacetic acid, 3-aminopropyltrimethoxysilane, 3-butene-1-amine, and dimethylpropyl sulfonate ethyl methacrylate. This introduces carbonyl, amide, siloxy, quaternary ammonium, and sulfonic acid groups onto the surface of the redispersible latex powder, increasing bonding strength and overall integrity. This results in an adhesive exhibiting high adhesion, good water resistance, and good freeze-thaw resistance, with a 28-day tensile bond strength >3 MPa, a post-immersion tensile bond strength >2 MPa, a post-immersion tensile bond strength loss rate <35%, and a post-freeze-thaw cycle tensile bond strength >2 MPa, with a post-freeze-thaw cycle tensile bond strength loss rate <35%, meeting market demands.

[0006] Optionally, the modified redispersible latex powder is prepared using the following method: S1. Add redispersible latex powder to water and mix, then add sodium hydroxide, stir for 3-5 hours, spray dry to obtain hydrolyzed powder; S2. At a temperature of 80-90℃, add hydrolyzed powder to water and mix. Then adjust the pH to 13-14, add 4-chloroacetoacetic acid, and stir for 7-9 hours. Then adjust the pH to 5-6, add 3-aminopropyltrimethoxysilane and 3-buten-1-amine, and stir for 3-5 hours. Then add dimethylpropyl sulfonamide ethyl methacrylate and initiator, and stir for 3-5 hours. Spray dry to obtain modified redispersible latex powder.

[0007] Optionally, the weight ratio of the hydrolyzed powder, 4-chloroacetoacetic acid, 3-aminopropyltrimethoxysilane, 3-butene-1-amine, and dimethylpropyl sulfonate ethyl methacrylate is 10:(1-3):(0.6-2):(0.3-0.8):(1-2).

[0008] First, sodium hydroxide is used to hydrolyze the ester groups in the redispersible latex powder, resulting in a higher concentration of hydroxyl groups on the surface of the hydrolyzed powder. Then, chlorine from 4-chloroacetoacetic acid reacts with the hydroxyl groups on the surface of the hydrolyzed powder to achieve grafting, introducing carboxyl groups. Next, primary amine groups from 3-aminopropyltrimethoxysilane and 3-buten-1-amine react with the carboxyl groups on the surface of the hydrolyzed powder to achieve grafting, introducing amide groups, siloxy groups, and carbon-carbon double bonds. Finally, carbon-carbon double bonds from dimethylpropyl sulfonamide ethyl methacrylate react with the carbon-carbon double bonds on the surface of the hydrolyzed powder to achieve grafting, introducing quaternary ammonium groups and sulfonic acid groups, thus obtaining a modified redispersible latex powder. The modified redispersible latex powder of this application contains a higher concentration of carbonyl groups, amide groups, siloxy groups, quaternary ammonium groups, and sulfonic acid groups on its surface, increasing the bonding strength and overall integrity between raw materials, improving the performance of the redispersible latex powder, and enhancing the adhesive's adhesion, water resistance, and freeze resistance.

[0009] Optionally, the weight ratio of dimethylpropyl sulfonamide ethyl methacrylate to the initiator is (0.3-0.8):(0.01-0.03). For example, weight ratios of 0.3:0.01, 0.3:0.02, 0.3:0.03, 0.6:0.01, 0.6:0.02, 0.6:0.03, 0.8:0.01, 0.8:0.02, and 0.8:0.03 are possible, but not limited to the listed values; other unlisted values ​​within this range are also applicable. Optimizing the amount of initiator facilitates the polymerization reaction of the monomer.

[0010] Optionally, the initiator is one or more of ammonium persulfate, sodium persulfate, potassium persulfate, and hydrogen peroxide. Optimizing the initiator facilitates its selection, and ammonium persulfate, sodium persulfate, potassium persulfate, and hydrogen peroxide can all promote the polymerization reaction of monomers, enhance the grafting stability of dimethylpropyl sulfonamide ethyl methacrylate, and ensure the effectiveness of the modified redispersible latex powder.

[0011] Optionally, the weight ratio of the redispersible latex powder to sodium hydroxide is (15-25):(4-6). For example, weight ratios of 15:4, 3:1, 5:2, 5:1, 4:1, 10:3, 25:4, 5:1, and 25:6 are possible, but not limited to the listed values; other unlisted values ​​within this range are also applicable. Limiting the weight ratio of redispersible latex powder to sodium hydroxide facilitates the hydrolysis of ester groups in the redispersible latex powder, increases the grafting of 4-chloroacetoacetic acid, and ensures the stability and effectiveness of the modified redispersible latex powder preparation.

[0012] Optionally, the redispersible latex powder is one or more of vinyl acetate copolymer powder, vinyl acetate-ethylene copolymer powder, vinyl acetate-higher fatty acid vinyl ester copolymer powder, and vinyl acetate-acrylate-higher fatty acid vinyl ester terpolymer powder. Preferably, the redispersible latex powder is one or more of vinyl acetate-ethylene copolymer powder, vinyl acetate-higher fatty acid vinyl ester copolymer powder, and vinyl acetate-acrylate-higher fatty acid vinyl ester terpolymer powder. More preferably, the redispersible latex powder is vinyl acetate-ethylene copolymer powder.

[0013] Optionally, the cement is silicate cement; the water-reducing agent is a polycarboxylate superplasticizer. Preferably, the silicate cement is silicate cement P.O42.5R; the polycarboxylate superplasticizer is polycarboxylate superplasticizer MELFLUX®4930F.

[0014] Optionally, the manufactured sand is either medium sand with a continuous gradation of 0.35-0.5mm or coarse sand with a continuous gradation of 0.5-2mm, and the weight ratio of medium sand to coarse sand is (1-3):(2-4). For example, the weight ratios are 1:2, 1:3, 1:4, 1:1, 2:3, 3:2, and 3:4, but are not limited to the listed values; other unlisted values ​​within this range are also applicable. Limiting the particle size of the manufactured sand facilitates its preparation and ensures that the adhesive maintains good flowability and density, guaranteeing the quality and stability of the adhesive during use.

[0015] Secondly, this application provides a method for preparing the adhesive for building ceramic tiles, which adopts the following technical solution: A method for preparing the adhesive for building ceramic tiles includes the following steps: mixing cement, manufactured sand, fly ash, silica fume, modified redispersible latex powder, attapulgite clay, and water-reducing agent to obtain the adhesive.

[0016] In summary, this application has at least the following beneficial effects: The adhesive of this application incorporates redispersible latex powder and attapulgite in its raw materials, leveraging the synergistic effect between the two to increase the tensile bond strength, post-immersion tensile bond strength, and post-freeze-thaw cycle tensile bond strength of the adhesive. Further modification of the redispersible latex powder enhances the interaction between it and the attapulgite, improving the performance of the redispersible latex powder. This results in an adhesive with a 28-day tensile bond strength >3 MPa, a post-immersion tensile bond strength >2 MPa, a post-immersion tensile bond strength loss rate <35%, and a post-freeze-thaw cycle tensile bond strength >2 MPa, with a post-freeze-thaw cycle tensile bond strength loss rate <35%. This gives the adhesive advantages of strong adhesion, good water resistance, and good freeze-thaw resistance, meeting market demands. Detailed Implementation

[0017] The present application will be further described in detail below with reference to the embodiments.

[0018] Preparation Example Preparation Example 1 A modified redispersible latex powder is prepared by the following method: S1. At a rotation speed of 350 r / min, add 20 g of redispersible latex powder to 200 g of water and stir for 5 min. Then add 5 g of sodium hydroxide and stir for 4 h. After that, spray dry to obtain hydrolyzed powder.

[0019] Among them, the redispersible latex powder is vinyl acetate-ethylene copolymer powder; the vinyl acetate-ethylene copolymer powder is selected from redispersible latex powder DA1100.

[0020] S2. At a rotation speed of 350 r / min and a temperature of 80℃, 10 g of the hydrolyzed powder obtained in step S1 was added to 100 g of water and stirred for 5 min. Then, the pH was adjusted to 13 using a 20% sodium hydroxide aqueous solution, and 1 g of 4-chloroacetoacetic acid was added, and the mixture was stirred for 8 h. Next, the pH was adjusted to 6 using a 20% hydrochloric acid aqueous solution, and 0.6 g of 3-aminopropyltrimethoxysilane and 0.8 g of 3-buten-1-amine were added, and the mixture was stirred for 4 h. Then, 2 g of dimethylpropyl sulfonamide ethyl methacrylate and 0.02 g of initiator sodium persulfate were added, and the mixture was stirred for 4 h. Finally, the mixture was spray-dried to obtain the modified redispersible latex powder.

[0021] Preparation Example 2 A modified redispersible latex powder differs from Preparation Example 1 in that, in step T2, the amounts of 4-chloroacetoacetic acid, 3-aminopropyltrimethoxysilane, 3-buten-1-amine, and dimethylpropylsulfonate ethyl methacrylate are different, and the amounts of 4-chloroacetoacetic acid added are 2g, 3-aminopropyltrimethoxysilane added are 1.3g, 3-buten-1-amine added are 0.5g, and dimethylpropylsulfonate ethyl methacrylate added are 1.5g.

[0022] Preparation Example 3 A modified redispersible latex powder differs from Preparation Example 1 in that, in step T2, the amounts of 4-chloroacetoacetic acid, 3-aminopropyltrimethoxysilane, 3-buten-1-amine, and dimethylpropylsulfonate ethyl methacrylate are different, and the amounts of 4-chloroacetoacetic acid added are 3g, 3-aminopropyltrimethoxysilane added are 2g, 3-buten-1-amine added are 0.3g, and dimethylpropylsulfonate ethyl methacrylate added are 1g. Example

[0023] Table 1. Amount of each raw material in the adhesive (unit: g) Example 1

[0024] An adhesive for building ceramic tiles, the raw materials and their proportions are shown in Table 1.

[0025] The cement used was silicate cement, specifically silicate cement P.O42.5R; the manufactured sand was quartz manufactured sand, consisting of two types: medium sand with a continuous gradation of 0.35-0.5mm and coarse sand with a continuous gradation of 0.5-2mm, with a weight ratio of 2:3 between the medium and coarse sand; the fly ash was Grade I fly ash; the average particle size of the silica fume was 0.1μm; the attapulgite clay had a mesh size of 325 mesh and a density of 2.4g / cm³, and was selected from Lingshou County Chengnuo Mineral Products Co., Ltd.; the water-reducing agent was a polycarboxylate superplasticizer, specifically polycarboxylate superplasticizer MELFLUX®4930F; and the modified redispersible latex powder was prepared using the method described in Preparation Example 1.

[0026] A method for preparing an adhesive for building ceramic tiles includes the following steps: Add manufactured sand, fly ash, microsilica, modified redispersible latex powder, attapulgite clay, and water-reducing agent to silicate cement, stir for 10 minutes, and obtain an adhesive. Example 2

[0027] An adhesive for building ceramic tiles differs from that in Example 1 in that the raw material ratios of the adhesive are different, and the raw material ratios are shown in Table 1. Example 3

[0028] An adhesive for building ceramic tiles differs from that in Example 1 in that the raw material ratios of the adhesive are different, and the raw material ratios are shown in Table 1. Example 4

[0029] An adhesive for building ceramic tiles differs from that of Example 2 in that the modified redispersible latex powder in the raw materials of the adhesive has a different source, and the modified redispersible latex powder is prepared by the method of Preparation Example 2. Example 5

[0030] An adhesive for building ceramic tiles differs from Example 2 in that the modified redispersible latex powder in the adhesive has a different source, and the modified redispersible latex powder is prepared using the method of Preparation Example 3.

[0031] Comparative Example Comparative Example 1 An adhesive for building ceramic tiles differs from Example 4 in that, in the adhesive raw materials, an equal amount of redispersible latex powder replaces the modified redispersible latex powder and attapulgite clay, and the redispersible latex powder is vinyl acetate-ethylene copolymer powder; the vinyl acetate-ethylene copolymer powder is selected from redispersible latex powder DA1100.

[0032] Comparative Example 2 An adhesive for building ceramic tiles differs from Example 4 in that an equal amount of attapulgite clay is used to replace the modified redispersible latex powder in the adhesive raw materials, and the attapulgite clay has a mesh size of 325 mesh, a density of 2.4 g / cm³, and is selected from Lingshou County Chengnuo Mineral Products Co., Ltd.

[0033] Comparative Example 3 An adhesive for building ceramic tiles differs from Example 4 in that an equal amount of redispersible latex powder is used to replace the modified redispersible latex powder in the raw materials of the adhesive, and the redispersible latex powder is vinyl acetate-ethylene copolymer powder; the vinyl acetate-ethylene copolymer powder is selected from redispersible latex powder DA1100.

[0034] Comparative Example 4 An adhesive for building ceramic tiles differs from that in Example 4 in that, in the method for preparing modified redispersible latex powder of the adhesive raw material, in step S2, an equal amount of 3-aminopropyltrimethoxysilane is used to replace 3-butene-1-amine.

[0035] Comparative Example 5 An adhesive for building ceramic tiles differs from that in Example 4 in that, in the method for preparing modified redispersible latex powder of the adhesive raw material, in step S2, 3-aminopropyltrimethoxysilane is replaced with an equal amount of 3-butene-1-amine.

[0036] Comparative Example 6 An adhesive for building ceramic tiles differs from that in Example 4 in that, in the method for preparing modified redispersible latex powder of the adhesive raw material, in step S2, an equal amount of 3-butene-1-amine is used to replace dimethylpropyl sulfonate ethyl methacrylate.

[0037] Performance testing The adhesives obtained in Examples 1-5 and Comparative Examples 1-6 were taken respectively, and water was added. The amount of water added was 20 wt% of the total amount of adhesive. The mixture was stirred for 5 minutes to obtain a slurry. The slurry was then subjected to the following performance tests, and the test results are shown in Table 2.

[0038] In accordance with JC / T547-2017 "Ceramic Tile Adhesives", the 28-day tensile bond strength, the tensile bond strength after immersion in water, and the tensile bond strength after freeze-thaw cycles of the slurry were tested, and the tensile bond strength loss rate after immersion in water and the tensile bond strength loss rate after freeze-thaw cycles were calculated.

[0039] Table 2 Test Results

[0040] As can be seen from Table 2, the adhesive of this application has a 28-day tensile bond strength of 3.12-3.65 MPa, a tensile bond strength after immersion in water of 2.04-2.61 MPa, a tensile bond strength loss rate after immersion in water of 28.49-34.62%, a tensile bond strength after freeze-thaw cycles of 2.18-2.76 MPa, and a tensile bond strength loss rate after freeze-thaw cycles of 24.38-30.13%, which makes it exhibit the advantages of high adhesion, good water resistance, and good freeze resistance, thus meeting market demand.

[0041] Comparing Comparative Examples 1-3, Comparative Example 1 added redispersible latex powder to the adhesive raw material; Comparative Example 2 added attapulgite clay to the adhesive raw material; and Comparative Example 3 added both redispersible latex powder and attapulgite clay to the adhesive raw material. This shows that simultaneously adding redispersible latex powder and attapulgite clay to the raw material, and utilizing their synergistic effect, can improve tensile bond strength, tensile bond strength after immersion in water, and tensile bond strength after freeze-thaw cycles. Furthermore, in Example 4, modified redispersible latex powder and attapulgite clay were added to the adhesive raw material. This shows that modifying the redispersible latex powder can improve the interaction between the redispersible latex powder and attapulgite clay, enhance the performance of the redispersible latex powder, and make the adhesive exhibit superior overall performance.

[0042] Comparing Example 4 and Comparative Examples 4-6, in Comparative Example 4, the modified redispersible latex powder in the adhesive raw material was not treated with 3-buten-1-amine; in Comparative Example 5, the modified redispersible latex powder in the adhesive raw material was not treated with 3-aminopropyltrimethoxysilane; and in Comparative Example 6, the modified redispersible latex powder in the adhesive raw material was not treated with dimethylpropylsulfonamide ethyl methacrylate. This demonstrates that, based on the treatment of redispersible latex powder with sodium hydroxide and 4-chloroacetoacetic acid, further treatment with 3-butene-1-amine, 3-aminopropyltrimethoxysilane, and dimethylpropyl sulfonate ethyl methacrylate can introduce quaternary ammonium groups, sulfonic acid groups, and siloxy groups onto the surface. This effectively increases the bonding strength, crosslinking density, and overall integrity of the adhesive, enhancing its adhesion, water resistance, and freeze resistance, resulting in superior overall performance.

[0043] This specific embodiment is merely an explanation of this application and is not intended to limit it. After reading this specification, those skilled in the art can make modifications to this embodiment without contributing any inventive step, but such modifications are protected by patent law as long as they fall within the scope of the claims of this application.

Claims

1. An adhesive for building ceramic tiles, characterized in that: It is mainly made of the following raw materials in parts by weight: 90-100 parts cement, 125-145 parts manufactured sand, 30-40 parts fly ash, 10-20 parts silica fume, 5-7 parts modified redispersible latex powder, 2-4 parts attapulgite, and 0.5-2 parts water-reducing agent; the modified redispersible latex powder is obtained by treating redispersible latex powder with sodium hydroxide, 4-chloroacetoacetic acid, 3-aminopropyltrimethoxysilane, 3-butene-1-amine, and dimethylpropylsulfonate ethyl methacrylate. The modified redispersible latex powder is prepared by the following method: S1. Add redispersible latex powder to water and mix, then add sodium hydroxide, stir for 3-5 hours, and spray dry to obtain hydrolyzed powder; S2. Add hydrolyzed powder to water at a temperature of 80-90℃, then adjust the pH to 13-14, add 4-chloroacetoacetic acid, stir for 7-9 hours, then adjust the pH to 5-6, add 3-aminopropyltrimethoxysilane and 3-buten-1-amine, stir for 3-5 hours, then add dimethylpropylsulfonamide ethyl methacrylate and initiator, stir for 3-5 hours, and spray dry to obtain modified redispersible latex powder.

2. The adhesive for building ceramic tiles according to claim 1, characterized in that: The weight ratio of the hydrolyzed powder, 4-chloroacetoacetic acid, 3-aminopropyltrimethoxysilane, 3-butene-1-amine, and dimethylpropyl sulfonamide ethyl methacrylate is 10:(1-3):(0.6-2):(0.3-0.8):(1-2).

3. The adhesive for building ceramic tiles according to claim 1, characterized in that: The weight ratio of dimethylpropyl sulfonamide ethyl methacrylate to the initiator is (0.3-0.8):(0.01-0.03).

4. The adhesive for building ceramic tiles according to claim 1, characterized in that: The initiator is one or more of ammonium persulfate, sodium persulfate, potassium persulfate, and hydrogen peroxide.

5. The adhesive for building ceramic tiles according to claim 1, characterized in that: The weight ratio of the redispersible latex powder and sodium hydroxide is (15-25):(4-6).

6. The adhesive for building ceramic tiles according to claim 1, characterized in that: The redispersible latex powder is one or more of the following: vinyl acetate copolymer powder, vinyl acetate-ethylene copolymer powder, vinyl acetate-higher fatty acid ethylene copolymer powder, and vinyl acetate-acrylate-higher fatty acid ethylene terpolymer powder.

7. The adhesive for building ceramic tiles according to claim 1, characterized in that: The cement is silicate cement; the water-reducing agent is a polycarboxylate water-reducing agent.

8. The adhesive for building ceramic tiles according to claim 1, characterized in that: The manufactured sand is of two types: medium sand with a continuous gradation of 0.35-0.5mm and coarse sand with a continuous gradation of 0.5-2mm, and the weight ratio of medium sand to coarse sand is (1-3):(2-4).

9. A method for preparing an adhesive for building ceramic tiles as described in any one of claims 1-8, characterized in that: The process includes the following steps: mixing cement, manufactured sand, fly ash, silica fume, modified redispersible latex powder, attapulgite clay, and water-reducing agent to obtain an adhesive.

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