Special glue for rock plate large plate, preparation method and construction method

Abstract

The application belongs to the technical field of ceramic tile glue, and discloses a special glue for rock plate large plates, a preparation method and a construction method.The special glue for rock plate large plates comprises 36-45 parts by weight of cement, 54-62 parts by weight of quartz sand, 0.6-1.6 parts by weight of silane modified polyether, 4-8 parts by weight of filler, 1-3.5 parts by weight of imidazole-based polyvinyl alcohol, 0.7-2.5 parts by weight of epoxy resin and the like.The active imidazole structure is introduced into the side chain of polyvinyl alcohol, so that the curing reaction with epoxy resin occurs at room temperature, the cohesion of the ceramic tile glue is enhanced, the tensile bonding strength of the ceramic tile glue is improved, the performance of the ceramic tile glue is further improved in cooperation with a composite system of silane modified polyether polymer, inorganic filler and the like, the special glue does not contain formaldehyde and meets the indoor decoration environmental protection standard;after curing, the special glue can be matched with brushing of acrylate resin paint, epoxy paint and the like.

Description

Technical Field

[0001] The present invention relates to the technical field of tile adhesives, and in particular to a special adhesive for large rock slabs, a preparation method and a construction method. Background Art

[0002] Tile adhesives, primarily composed of cement, polymer additives, fillers, and additives, are crucial for bonding decorative ceramic tiles such as rock slabs and slabs. Traditional tile adhesives have poor bonding properties, and their bond strength decreases significantly after immersion in water, resulting in poor water resistance. Polyvinyl alcohol (PVA) exhibits excellent bonding properties and can enhance bond strength when added to tile adhesives. However, its addition does not improve the adhesive's water resistance.

[0003] Epoxy resins have excellent bonding strength, water resistance, and heat resistance, making them widely used in adhesives and floor mortars. Patent application CN116120019A discloses a two-component tile adhesive and its preparation method. Using a waterproof emulsion, epoxy resin-modified polyvinyl alcohol adhesive, cement, fine sand powder, and a water-retaining agent, the resulting tile adhesive exhibits excellent flexibility, bonding, and vibration resistance. However, the patented product exhibits low tensile bond strength before and after immersion, hindering its practical application. Summary of the Invention

[0004] The technical problem solved by the present invention is to solve the problem of low tensile bonding strength of tile adhesive.

[0005] The technical solution of the present invention is: a special glue for large slabs of rock slabs, comprising the following components: 36-45 parts by weight of cement, 54-62 parts by weight of quartz sand, 4-8 parts by weight of filler, 1-3.5 parts by weight of imidazole polyvinyl alcohol, 0.7-2.5 parts by weight of epoxy resin, 0.2-0.4 parts by weight of hydroxypropyl methylcellulose, 0.6-1.6 parts by weight of silane-modified polyether, 0.3-0.6 parts by weight of water reducer, 2-4 parts by weight of redispersible latex powder, and 23-28 parts by weight of water; wherein the preparation method of imidazole polyvinyl alcohol is as follows: polyvinyl alcohol is added to the reaction solvent, heated and stirred, and then cooled, 2-ethyl-1H-imidazole-5-carboxylic acid, 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride, and 4-dimethylaminopyridine are added, and after the reaction, the solution is poured into ethanol, filtered, and the precipitate is washed with water and ethanol, and dried to obtain imidazole polyvinyl alcohol. The preparation reaction formula is as follows:

[0006] .

[0007] Preferably, the reaction solvent is dimethyl sulfoxide or N,N-dimethylformamide.

[0008] Preferably, in the preparation method of imidazole polyvinyl alcohol, the heating and stirring temperature is 90-100° C. and the time is 30-40 minutes.

[0009] Preferably, the amount of polyvinyl alcohol is 100 parts by weight, the amount of 2-ethyl-1H-imidazole-5-carboxylic acid is 3-12 parts by weight, the amount of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride is 4.2-17.3 parts by weight, and the amount of 4-dimethylaminopyridine is 2.8-11.6 parts by weight.

[0010] Preferably, in the preparation method of imidazole polyvinyl alcohol, the reaction temperature is 20-30° C. and the reaction time is 18-36 hours.

[0011] Preferably, the filler is heavy calcium carbonate, metakaolin or slag powder.

[0012] Preferably, the quartz sand is composed of fine quartz sand and coarse quartz sand in a mass ratio of (20-35): (65-80).

[0013] Preferably, the particle size of the fine quartz sand is 150-300 mesh; the particle size of the coarse quartz sand is 20-60 mesh.

[0014] Preferably, the preparation method of the special glue for large slabs of rock slabs is: stir and mix cement, quartz sand, filler, imidazole polyvinyl alcohol, hydroxypropyl methylcellulose, silane-modified polyether, water reducer, redispersible latex powder, and water, and finally add epoxy resin, stir and mix well to obtain the special glue for large slabs of rock slabs.

[0015] Preferably, the special glue for rock slabs or large panels can be applied to the rock slabs or large panels in a spot-sticking manner.

[0016] The technical effect of the present invention is as follows: 2-ethyl-1H-imidazole-5-carboxylic acid is used to react with polyvinyl alcohol for esterification to obtain imidazole-based polyvinyl alcohol, which is then compounded with cement, quartz sand, filler, hydroxypropyl methylcellulose, silane-modified polyether, epoxy resin, etc. to obtain a special adhesive for large rock slabs. By introducing an active imidazole structure into the side chain of polyvinyl alcohol, a curing reaction with epoxy resin is achieved at room temperature, thereby enhancing the cohesive force of the tile adhesive and improving the tensile bonding strength of the tile adhesive. The performance of the tile adhesive is further improved by synergistically combining a composite system of silane-modified polyether polymers, inorganic fillers, etc., and the addition of epoxy resin is beneficial to reducing the water absorption of the tile adhesive specimen, thereby improving the tensile bonding strength of the specimen after immersion in water, and exhibiting good water resistance. The special adhesive does not contain formaldehyde and meets the environmental protection standards for interior decoration; after curing, it can be applied with acrylic resin paint, epoxy paint, etc. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 This is the infrared spectrum of imidazolyl polyvinyl alcohol. DETAILED DESCRIPTION

[0018] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative efforts shall fall within the scope of protection of the present invention.

[0019] The particle size of the fine quartz sand is between 150-300 mesh; the particle size of the coarse quartz sand is between 20-60 mesh. The cement is P.O42.5 Portland cement. The polyvinyl alcohol is PVA2488. The redispersible polymer powder is Wacker 5010N. The silane-modified polyether is ACG S5830E. The water reducer is Sika 530P polycarboxylate superplasticizer.

[0020] Example 1

[0021] (1) Add 200 g of polyvinyl alcohol to 2 L of dimethyl sulfoxide, heat to 90 ° C, stir for 40 min, cool, add 12 g of 2-ethyl-1H-imidazole-5-carboxylic acid (CAS No. 84255-21-0), 17.1 g of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride, and 11.5 g of 4-dimethylaminopyridine, and stir at 25 ° C for 18 h. Pour the solution into ethanol, filter, wash the precipitate with water and ethanol, and dry to obtain imidazole-based polyvinyl alcohol. Figure 1 In the infrared spectrum, 3378 cm -1 is the absorption peak of hydroxyl group, 1734 cm -1 It is the vibration absorption peak of ester group C=O, 1641cm -1 It is the vibration absorption peak of C=N in the imidazole ring.

[0022] (2) 3.9 kg cement, 5.8 kg quartz sand, 0.5 kg filler heavy calcium carbonate, 0.1 kg imidazole polyvinyl alcohol, 26 g hydroxypropyl methylcellulose, 90 g silane modified polyether, 30 g water reducer, 0.25 kg redispersible latex powder, and 2.3 kg water were stirred and mixed, wherein the quartz sand consisted of fine quartz sand and coarse quartz sand with a mass ratio of 25:75; finally, 70 g epoxy resin E51 was added and stirred to obtain a special adhesive for large stone slabs.

[0023] Example 2

[0024] (1) Add 200 g of polyvinyl alcohol to 2 L of dimethyl sulfoxide, heat to 100 °C, stir for 30 min, cool, add 6 g of 2-ethyl-1H-imidazole-5-carboxylic acid, 8.4 g of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride, and 5.6 g of 4-dimethylaminopyridine, and stir at 20 °C for 24 h. Pour the solution into ethanol, filter, wash the precipitate with water and ethanol, and dry to obtain imidazole-based polyvinyl alcohol.

[0025] (2) 4.5 kg of cement, 6.2 kg of quartz sand, 0.4 kg of slag powder, 0.18 kg of imidazole polyvinyl alcohol, 20 g of hydroxypropyl methylcellulose, 160 g of silane-modified polyether, 60 g of water reducer, 0.3 kg of redispersible latex powder, and 2.8 kg of water were stirred and mixed, wherein the quartz sand consisted of fine quartz sand and coarse quartz sand in a mass ratio of 20:80; finally, 130 g of epoxy resin E51 was added and stirred to obtain a special adhesive for large stone slabs.

[0026] Example 3

[0027] (1) Add 200 g of polyvinyl alcohol to 2.5 L of N,N-dimethylformamide, heat to 100 °C, stir for 30 min, cool, add 24 g of 2-ethyl-1H-imidazole-5-carboxylic acid, 34.6 g of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride, and 23.2 g of 4-dimethylaminopyridine, and stir at 20 °C for 36 h. Pour the solution into ethanol, filter, wash the precipitate with water and ethanol, and dry to obtain imidazolyl polyvinyl alcohol.

[0028] (2) 3.6 kg of cement, 5.4 kg of quartz sand, 0.6 kg of heavy calcium carbonate, 0.27 kg of imidazole polyvinyl alcohol, 40 g of hydroxypropyl methylcellulose, 60 g of silane-modified polyether, 42 g of water reducer, 0.2 kg of redispersible latex powder, and 2.3 kg of water were stirred and mixed, wherein the quartz sand consisted of fine quartz sand and coarse quartz sand in a mass ratio of 35:65; finally, 190 g of epoxy resin E51 was added and stirred to obtain a special adhesive for large stone slabs.

[0029] Example 4

[0030] (1) Add 200 g of polyvinyl alcohol to 2.5 L of dimethyl sulfoxide, heat to 100 °C, stir for 30 min, cool, add 18 g of 2-ethyl-1H-imidazole-5-carboxylic acid, 25.5 g of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride, and 17.3 g of 4-dimethylaminopyridine, and stir at 30 °C for 24 h. Pour the solution into ethanol, filter, wash the precipitate with water and ethanol, and dry to obtain imidazole-based polyvinyl alcohol.

[0031] (2) 4.2 kg of cement, 5.9 kg of quartz sand, 0.8 kg of metakaolin, 0.35 kg of imidazole polyvinyl alcohol, 33 g of hydroxypropyl methylcellulose, 110 g of silane-modified polyether, 47 g of water reducer, 0.4 kg of redispersible latex powder, and 2.6 kg of water were stirred and mixed, wherein the quartz sand consisted of fine quartz sand and coarse quartz sand in a mass ratio of 25:75; finally, 250 g of epoxy resin E51 was added and stirred to obtain a special adhesive for large stone slabs.

[0032] Comparative Example 1

[0033] (1) 3.9 kg of cement, 5.8 kg of quartz sand, 0.5 kg of filler heavy calcium carbonate, 0.1 kg of polyvinyl alcohol, 26 g of hydroxypropyl methylcellulose, 90 g of silane-modified polyether, 30 g of water reducer, 0.25 kg of redispersible latex powder, and 2.3 kg of water were stirred and mixed, wherein the quartz sand consisted of fine quartz sand and coarse quartz sand in a mass ratio of 25:75, to obtain a special adhesive for large stone slabs.

[0034] Comparative Example 2

[0035] (1) Imidazole-based polyvinyl alcohol was prepared according to the method of Example 1.

[0036] (2) 3.9 kg of cement, 5.8 kg of quartz sand, 0.5 kg of filler heavy calcium carbonate, 0.1 kg of imidazole polyvinyl alcohol, 26 g of hydroxypropyl methylcellulose, 90 g of silane-modified polyether, 30 g of water reducer, 0.25 kg of redispersible latex powder, and 2.3 kg of water were stirred and mixed, wherein the quartz sand consisted of fine quartz sand and coarse quartz sand in a mass ratio of 25:75, to obtain a special adhesive for large stone slabs.

[0037] Comparative Example 3

[0038] (1) 3.9 kg cement, 5.8 kg quartz sand, 0.5 kg heavy calcium carbonate filler, 0.1 kg polyvinyl alcohol, 26 g hydroxypropyl methylcellulose, 90 g silane-modified polyether, 30 g water reducer, 0.25 kg redispersible latex powder, and 2.3 kg water were stirred and mixed, wherein the quartz sand consisted of fine quartz sand and coarse quartz sand with a mass ratio of 25:75; finally, 70 g epoxy resin E51 was added and stirred to obtain a special adhesive for large stone slabs.

[0039] Comparative Example 4

[0040] (1) Add 200 g of polyvinyl alcohol to 2 L of dimethyl sulfoxide, heat to 90 ° C, stir for 40 min, cool, add 12 g of 1H-imidazole-4-carboxylic acid (CAS No. 1072-84-0), 17.1 g of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride, and 11.5 g of 4-dimethylaminopyridine, and stir at 25 ° C for 18 h. Pour the solution into ethanol, filter, wash the precipitate with water and ethanol, and dry it to obtain imidazole-based polyvinyl alcohol.

[0041] (2) 3.9 kg cement, 5.8 kg quartz sand, 0.5 kg filler heavy calcium carbonate, 0.1 kg imidazole polyvinyl alcohol, 26 g hydroxypropyl methylcellulose, 90 g silane modified polyether, 30 g water reducer, 0.25 kg redispersible latex powder, and 2.3 kg water were stirred and mixed, wherein the quartz sand consisted of fine quartz sand and coarse quartz sand with a mass ratio of 25:75; finally, 70 g epoxy resin E51 was added and stirred to obtain a special adhesive for large stone slabs.

[0042] The rock slab was used as the ceramic tile sample. The special adhesive for rock slab was used to form and cure the specimens according to the JC / T 547-2017 method. The curing time was 28 days at a temperature of 25°C. The tensile bond strength of the specimens was then tested.

[0043] The specimens were immersed in deionized water for 14 days, and then the tensile bond strength of the specimens after immersion in water was tested.

[0044] Table 1 Performance test of special adhesive for large rock slabs

[0045]

[0046] After testing, the tensile strength of Examples 1 to 4 before and after immersion in water is very high, and the bonding performance is excellent. This is mainly because imidazole-based polyvinyl alcohol and epoxy resin are added, and an active imidazole structure is introduced into the side chain of polyvinyl alcohol, which undergoes a curing reaction with the epoxy resin at room temperature. It is speculated that the introduction of an ethyl group at position 2 and an ester group at position 5 of the imidazole structure enhances the electron delocalization effect of the imidazole group and improves the activity of the imidazole and its NH bond, thereby achieving room temperature curing of the epoxy resin, enhancing the cohesion of the tile adhesive, and improving the tensile bonding strength of the tile adhesive. In addition, the cured epoxy resin has the characteristic of low water absorption, which is beneficial to reducing the water absorption of the tile adhesive specimen, thereby improving the tensile bonding strength of the specimen after immersion in water, and showing good water resistance.

[0047] In Comparative Example 1, only polyvinyl alcohol was added without epoxy resin, and the cohesive force and bonding performance of the tile adhesive were poor, and the tensile bonding strength before and after immersion in water was low.

[0048] In Comparative Example 2, only imidazole-based polyvinyl alcohol was added without epoxy resin. The cohesive force and bonding performance of the tile adhesive were poor, and the tensile bonding strength before and after immersion in water was low.

[0049] Comparative Example 3 added polyvinyl alcohol and epoxy resin. Polyvinyl alcohol does not contain an active imidazole structure and cannot undergo a curing reaction with the epoxy resin. The cohesion and bonding properties of the tile adhesive are poor, and the tensile bonding strength before and after immersion in water is low.

[0050] Comparative Example 4 uses 1H-imidazole-4-carboxylic acid to react with polyvinyl alcohol to obtain imidazolyl polyvinyl alcohol, the imidazole group of its side chain has low activity and poor room temperature curing reaction with epoxy resin, resulting in low tensile bonding strength of the tile adhesive before and after immersion in water.

[0051] The above embodiments are intended only to illustrate the technical concepts and features of the present invention. Their purpose is to enable those skilled in the art to understand the contents of the present invention and implement them accordingly. They are not intended to limit the scope of protection of the present invention. Any equivalent changes or modifications made in accordance with the spirit of the present invention are intended to be covered by the scope of protection of the present invention.

Claims

1. A special glue for large rock slabs, characterized by: The special adhesive for large rock slabs includes the following components: 36-45 parts by weight of cement, 54-62 parts by weight of quartz sand, 4-8 parts by weight of filler, 1-3.5 parts by weight of imidazole polyvinyl alcohol, 0.7-2.5 parts by weight of epoxy resin, 0.6-1.6 parts by weight of silane-modified polyether, 0.2-0.4 parts by weight of hydroxypropyl methylcellulose, 0.3-0.6 parts by weight of water reducer, 2-4 parts by weight of redispersible latex powder, and 23-28 parts by weight of water; The preparation method of the imidazole-based polyvinyl alcohol comprises the following steps: adding polyvinyl alcohol to a reaction solvent, heating and stirring, and then cooling; adding 2-ethyl-1H-imidazole-5-carboxylic acid, 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride, and 4-dimethylaminopyridine; after the reaction, pouring the solution into ethanol; filtering, washing the precipitate, and drying to obtain the imidazole-based polyvinyl alcohol.

2. The special adhesive for rock slabs according to claim 1, characterized in that: The filler is heavy calcium carbonate, metakaolin or slag powder.

3. The special adhesive for rock slabs according to claim 1, characterized in that: The quartz sand consists of fine quartz sand and coarse quartz sand in a mass ratio of (20-35): (65-80).

4. The special adhesive for rock slabs according to claim 3, characterized in that: The particle size of the fine quartz sand is 150-300 meshes; the particle size of the coarse quartz sand is 20-60 meshes.

5. The special adhesive for rock slabs according to claim 1, characterized in that: The heating and stirring temperature is 90-100° C., and the time is 30-40 minutes.

6. The special adhesive for rock slabs according to claim 1, characterized in that: The reaction solvent is dimethyl sulfoxide or N,N-dimethylformamide.

7. The special adhesive for rock slabs according to claim 1, characterized in that: The amount of polyvinyl alcohol used is 100 parts by weight, the amount of 2-ethyl-1H-imidazole-5-carboxylic acid used is 3-12 parts by weight, the amount of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride used is 4.2-17.3 parts by weight, and the amount of 4-dimethylaminopyridine used is 2.8-11.6 parts by weight.

8. The special adhesive for rock slabs according to claim 1, characterized in that: The reaction temperature is 20-30° C., and the reaction time is 18-36 hours.

9. A method for preparing a special adhesive for rock slabs according to any one of claims 1 to 8, characterized in that: The preparation method comprises the following steps: mixing cement, quartz sand, filler, imidazole-based polyvinyl alcohol, hydroxypropyl methylcellulose, silane-modified polyether, water reducer, redispersible latex powder and water, and finally adding epoxy resin and stirring to obtain a special adhesive for large rock slabs.

10. A construction method for the special adhesive for rock slabs obtained by the preparation method according to claim 9, characterized in that: The construction method is: use the special glue for rock slabs and large panels to construct the rock slabs or large panels in a spot-stick manner.

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