CN118290098A - Ceramic tile adhesive and preparation method thereof - Google Patents
Ceramic tile adhesive and preparation method thereof Download PDFInfo
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- CN118290098A CN118290098A CN202410409468.XA CN202410409468A CN118290098A CN 118290098 A CN118290098 A CN 118290098A CN 202410409468 A CN202410409468 A CN 202410409468A CN 118290098 A CN118290098 A CN 118290098A
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- 239000000853 adhesive Substances 0.000 title claims abstract description 217
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- 238000002360 preparation method Methods 0.000 title abstract description 19
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- 239000006004 Quartz sand Substances 0.000 claims abstract description 63
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 55
- 239000012744 reinforcing agent Substances 0.000 claims abstract description 53
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- 239000004816 latex Substances 0.000 claims abstract description 18
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- 239000000463 material Substances 0.000 claims abstract description 15
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 43
- 239000002244 precipitate Substances 0.000 claims description 22
- 239000003292 glue Substances 0.000 claims description 21
- -1 carboxypropyl methyl Chemical group 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 19
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- 238000006243 chemical reaction Methods 0.000 claims description 17
- 238000005406 washing Methods 0.000 claims description 17
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- MGNCLNQXLYJVJD-UHFFFAOYSA-N cyanuric chloride Chemical compound ClC1=NC(Cl)=NC(Cl)=N1 MGNCLNQXLYJVJD-UHFFFAOYSA-N 0.000 claims description 15
- 239000006185 dispersion Substances 0.000 claims description 15
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- 239000012043 crude product Substances 0.000 claims description 13
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- AEQDJSLRWYMAQI-UHFFFAOYSA-N 2,3,9,10-tetramethoxy-6,8,13,13a-tetrahydro-5H-isoquinolino[2,1-b]isoquinoline Chemical compound C1CN2CC(C(=C(OC)C=C3)OC)=C3CC2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-UHFFFAOYSA-N 0.000 claims description 8
- 238000004108 freeze drying Methods 0.000 claims description 8
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- 229940005574 sodium gluconate Drugs 0.000 claims description 8
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- CBOCVOKPQGJKKJ-UHFFFAOYSA-L Calcium formate Chemical group [Ca+2].[O-]C=O.[O-]C=O CBOCVOKPQGJKKJ-UHFFFAOYSA-L 0.000 claims description 7
- 239000004281 calcium formate Substances 0.000 claims description 7
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- YLGXILFCIXHCMC-JHGZEJCSSA-N methyl cellulose Chemical compound COC1C(OC)C(OC)C(COC)O[C@H]1O[C@H]1C(OC)C(OC)C(OC)OC1COC YLGXILFCIXHCMC-JHGZEJCSSA-N 0.000 claims description 7
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- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 3
- VJHCJDRQFCCTHL-UHFFFAOYSA-N acetic acid 2,3,4,5,6-pentahydroxyhexanal Chemical compound CC(O)=O.OCC(O)C(O)C(O)C(O)C=O VJHCJDRQFCCTHL-UHFFFAOYSA-N 0.000 claims description 3
- 239000001110 calcium chloride Substances 0.000 claims description 3
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- CREXVNNSNOKDHW-UHFFFAOYSA-N azaniumylideneazanide Chemical group N[N] CREXVNNSNOKDHW-UHFFFAOYSA-N 0.000 description 1
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Landscapes
- Adhesives Or Adhesive Processes (AREA)
Abstract
The application provides a tile adhesive and a preparation method thereof, wherein the tile adhesive comprises the following components in parts by weight: 50-60 parts of quartz sand, 38-42 parts of ordinary Portland cement, 1.5-2.5 parts of fly ash, 0.8-1.2 parts of workability reinforcing agent, 0.5-0.8 part of early strength agent, 0.2-0.8 part of cellulose ether, 0.04-0.1 part of magnesium aluminum silicate, 0.04-0.06 part of starch ether and 0.03-0.07 part of adhesion reinforcing agent. The adhesion enhancer comprises the following components in percentage by weight: 0.5-0.8:0.3-0.6 of latex powder, 3-amino-2, 2-dimethyl propionamide and porous nanometer materials. The preparation method of the tile adhesive comprises the following steps: obtaining porous nano material, obtaining adhesive reinforcing agent and obtaining ceramic tile adhesive. The ceramic tile adhesive produced by the application can keep better bonding strength under different temperature change environments.
Description
Technical Field
The application relates to the technical field of building materials, in particular to a tile adhesive and a preparation method thereof.
Background
The tile glue is a new modern decoration material for pasting decorative materials such as tiles, face bricks, floor tiles and the like, and is widely applicable to decorative surfaces of buildings such as inner and outer walls, floors, bathrooms, kitchens and the like. In recent years, with the great development of the building decoration industry, the use and decoration amount of ceramic tiles are larger and larger, and the ceramic tile glue market has a steadily increasing trend.
The currently used tile adhesive has lower heat-resistant adhesive strength, namely when the tile is subjected to thermal expansion and cold shrinkage in different temperature fields (especially in winter and summer), the internal stress generated by the thermal expansion and condensation of the tile cannot be well released due to the lack of enough adhesive strength of the tile adhesive, small cracks appear between the tile adhesive and the tile after the tile adhesive is used for several years, the cracks gradually form hollows after accumulating to a certain amount, the final falling is caused, and great hidden danger is caused to normal use.
Disclosure of Invention
The application provides a tile adhesive and a preparation method thereof, which are used for solving the problems mentioned in the background art.
On the one hand, the application provides a tile adhesive, which comprises the following components in parts by weight:
50-60 parts of quartz sand, 38-42 parts of ordinary Portland cement, 1.5-2.5 parts of fly ash, 0.8-1.2 parts of workability reinforcing agent, 0.5-0.8 part of early strength agent, 0.2-0.8 part of cellulose ether, 0.04-0.1 part of magnesium aluminum silicate, 0.04-0.06 part of starch ether and 0.03-0.07 part of adhesive reinforcing agent.
The adhesion enhancer comprises the following components in percentage by weight: 0.5-0.8:0.3-0.6 of latex powder, 3-amino-2, 2-dimethyl propionamide and porous nanometer materials.
Optionally, the quartz sand comprises 30-50 mesh quartz sand and 60-80 mesh quartz sand, wherein the weight ratio of the 30-50 mesh quartz sand to the 60-80 mesh quartz sand is 0.75-1:1.
Alternatively, the Portland cement is 42.5R Portland cement.
Optionally, the cellulose ether is one or more of methyl cellulose ether, carboxymethyl cellulose ether, carboxypropyl methyl cellulose ether or carboxyethyl cellulose ether.
Optionally, the workability enhancer comprises a weight ratio of 1:0.7-1 wood fiber and sodium gluconate.
Optionally, the early strength agent is calcium formate, calcium chloride or triethanolamine.
On the other hand, the application provides a preparation method of the tile adhesive, which comprises the following steps:
(1) Obtaining a porous nanomaterial: adding 2, 5-diamino-benzo-dithiazole into a reaction kettle, adding N, N-dimethylformamide and triethanolamine into the reaction kettle successively under a stirring state to form a dispersion liquid, carrying out ultrasonic treatment on the dispersion liquid for 10-15min, adding cyanuric chloride, carrying out ultrasonic treatment again for 10-20min to obtain slurry to be reacted, reacting the slurry to be reacted at the temperature of 90-130 ℃ for 10-14h to obtain a porous nano material crude product, and washing the porous nano material crude product for multiple times to obtain the porous nano material.
(2) Obtaining an adhesion enhancer: mixing the porous nano material, the latex powder and the 3-amino-2, 2-dimethyl propionamide according to the weight ratio to obtain the adhesive reinforcing agent.
(3) Obtaining ceramic tile adhesive: and mixing quartz sand, ordinary Portland cement, fly ash, an easy reinforcing agent, an early strength agent, cellulose ether, magnesium aluminum silicate, starch ether and an adhesive reinforcing agent according to the weight parts for 5-10min to obtain the tile adhesive.
Optionally, the weight ratio of cyanuric chloride, 2, 5-diamino-benzo-dithiazole, triethanolamine and N, N-dimethylformamide is 1:2.5-3:2.0-2.5:50-80.
Optionally, in the step of preparing the porous nanomaterial, washing the crude porous nanomaterial multiple times includes:
And (3) centrifugally separating the crude porous nano material to obtain a precipitate, alternately washing the precipitate with deionized water and ethanol, centrifuging for 3-5 times, and freeze-drying the washed precipitate to obtain the porous nano material.
Optionally, the average particle size of the emulsion powder is 0.2-0.4 μm.
The tile adhesive and the preparation method thereof realize the production of the tile adhesive, and compared with the prior art, the tile adhesive has the following beneficial effects:
(1) By adding ordinary silicate cement and quartz sand into the tile adhesive as main aggregate components of the tile adhesive, the viscosity and the cohesive force of the tile adhesive are increased, so that the tile adhesive is more easily and tightly adhered to a base layer. The quartz sand makes the paved ceramic tile more firm and durable. Fly ash is added to improve the binding force and the adhesive force between the ceramic tile and the base layer. The flexibility of the tile glue is increased, and the tile is prevented from cracking. The cellulose ether is added to further improve the bonding performance of the tile adhesive and improve the anti-slip performance and the bonding firmness of the tile adhesive. The magnesium aluminum silicate can improve the construction smoothness of the tile adhesive in use. The starch ether can play a role in quick thickening, so that the adhesion between the ceramic tile and the base material is firmer, and meanwhile, the fluidity of the ceramic tile adhesive is improved, and the ceramic tile adhesive is better smeared on a wall surface. Meanwhile, the adhesive reinforcing agent is added, so that the adhesiveness of the tile adhesive is further improved, meanwhile, the adhesive strength of the tile adhesive when the tile adhesive expands with heat and contracts with cold at different temperatures can be obviously improved, the addition of the porous nano material disperses the stress generated by the expansion with heat and contraction with cold of the tile adhesive, the buffer effect is achieved among components with different coefficients of thermal expansion, and the cracking and even falling of the tile adhesive caused by the different stresses generated by the expansion with heat and contraction with cold of different components are avoided.
(2) By adding the early strength agent, the hydration speed of the ordinary Portland cement is accelerated, the early strength of the tile adhesive is promoted, the adhesive force and cohesive force of the tile adhesive are obviously improved, and the construction speed is accelerated. And the triethanolamine not only has the early strength function, but also has a certain water reducing and enhancing function.
(3) The porous nano material is synthesized by adopting a solvothermal method, the porous nano material is freeze-dried, the porosity of the porous nano material is kept as much as possible, the porous nano material is added into the ceramic tile adhesive, the adhesive property of the ceramic tile adhesive is improved, meanwhile, the stress generated by the expansion and contraction of the ceramic tile adhesive is dispersed, the buffer effect is realized between components with different coefficients of thermal expansion, the adhesive strength of the ceramic tile adhesive when the expansion and contraction of the ceramic tile adhesive occur at different temperatures can be obviously improved, and the cracking and even the falling of the ceramic tile adhesive caused by the different stresses generated by the expansion and contraction of the different components are avoided.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present application more clear, the technical solutions in the embodiments of the present application will be clearly and completely described below, and it is apparent that the described embodiments are some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are also within the scope of the application.
On the one hand, the application provides a tile adhesive, which comprises the following components in parts by weight:
50-60 parts of quartz sand, 38-42 parts of ordinary Portland cement, 1.5-2.5 parts of fly ash, 0.8-1.2 parts of workability reinforcing agent, 0.5-0.8 part of early strength agent, 0.2-0.8 part of cellulose ether, 0.04-0.1 part of magnesium aluminum silicate, 0.04-0.06 part of starch ether and 0.03-0.07 part of adhesive reinforcing agent.
The adhesion enhancer comprises the following components in percentage by weight: 0.5-0.8:0.3-0.6 of latex powder, 3-amino-2, 2-dimethyl propionamide and porous nanometer materials.
Specifically, the tile glue is a new material for adhering decorative materials such as tiles, face bricks, floor tiles and the like. The ordinary silicate cement is generally used for bonding building materials in buildings, is a main component in the tile adhesive, takes quartz sand as aggregate, avoids phenomena such as hollowness and cracking in the laying process, and can also increase the viscosity and the bonding force of the tile adhesive, so that the tile adhesive is more easily and tightly adhered to a base layer. And quartz sand is taken from nature, natural, pollution-free and harmless to human health, has excellent mechanical strength and wear performance, and has long service life, so that the paved ceramic tile is firmer and more durable.
The ordinary Portland cement is a hydraulic cementing material which is prepared by grinding Portland cement clinker, 5-20% of mixed materials and a proper amount of gypsum and meets the national standard GB 175-2007.
The fly ash is a solid residual substance after filtration and dust removal in the coal-fired emission of a power plant, and the main components of the fly ash are silicic acid, alumina, calcium oxide and the like, so that the fly ash has good activity and self-adhesion. The proper amount of fly ash is added to effectively improve the performance of the tile adhesive and improve the binding force and the adhesive force between the tile and the base layer. The fly ash also has a slight expansion effect, so that the flexibility of the tile adhesive is increased, and the tile is prevented from cracking. And because the fly ash has fine expansibility, the use amount of the fly ash is controlled when the ceramic tile is used, and the ceramic tile is easy to fall off or crack due to excessive use.
The workability reinforcing agent can improve the construction operability of each process, including fluidity, cohesiveness and water retention, and is convenient for operators to operate when using the tile glue to lay tiles. The early strength agent is used for improving the early mechanical property of the tile adhesive, is convenient for the early adhesion of the tile adhesive to the substrate and the tile, and accelerates the construction progress. The cellulose ether can further improve the bonding performance of the tile adhesive, and improve the anti-slip performance and the bonding firmness of the tile adhesive. The magnesium aluminum silicate can improve the construction smoothness of the tile adhesive in use. The starch ether can play a role in quick thickening, so that the adhesion between the ceramic tile and the base material is firmer, meanwhile, the fluidity of the ceramic tile adhesive is improved, the ceramic tile adhesive is better smeared on a wall surface, the lubricity of the ceramic tile adhesive is improved, and the operation is smoother and easier to construct. Meanwhile, the consumption of the starch ether is controlled to be 0.04-0.06 weight part, and the excessively high consumption of the starch ether can increase the viscosity of the tile adhesive, thereby being not beneficial to construction and delay of drying time; if the usage amount is too small, the binding force and ductility of the tile adhesive can be reduced, and the quality of the tile is affected.
The adhesive reinforcing agent can further improve the cohesiveness of the tile adhesive, and can obviously improve the cohesive strength of the tile adhesive when the tile adhesive expands with heat and contracts with cold at different temperatures, wherein the latex powder is redispersible, has better viscosity when being dispersed in water, and can be dispersed into gaps between the ordinary Portland cement and the quartz sand skeleton in the use process, so that the ordinary Portland cement, the quartz sand aggregate and the fly ash are further bonded together, and the integral cohesive strength of the tile adhesive is improved. Meanwhile, porous nano materials are added, the inside of the porous nano materials is provided with a regularly arranged porous structure, the porous structure has stronger adsorptivity, so that ordinary Portland cement, quartz sand aggregate, fly ash and emulsion powder in the ceramic tile adhesive can be adsorbed in and on the inside and the surface of pores in the ceramic tile adhesive in the use process of the ceramic tile adhesive, so that the particles are filled in the pores of the porous nano materials, meanwhile, the porous nano materials are uniformly dispersed in the ceramic tile adhesive to form a mutually staggered reticular structure, so that the components in the ceramic tile adhesive are mutually bonded, and the porous nano materials further have cohesive action on the components of the ceramic tile adhesive, so that the components in the ceramic tile adhesive form integral cohesive force, and the cohesiveness of the ceramic tile adhesive is improved.
And the ceramic tile adhesive is applied to environments at various different temperatures, when the environmental temperature is too high, the stress generated by expansion with heat and contraction with cold under the temperature change of each component in the ceramic tile adhesive is different, and the ordinary silicate cement in the ceramic tile adhesive, quartz sand aggregate, fly ash and molecular bonds in emulsion powder can be broken, so that the structural fracture and cross linkage fracture in the ceramic tile adhesive components are caused, the cracking or mechanical property of the ceramic tile adhesive is reduced, and the cohesive force is further reduced. After the porous nano material is added, each component in the ceramic tile adhesive enters the pores of the porous nano material, and the mutually staggered reticular structure plays a role in connecting and gathering each component in the ceramic tile adhesive, so that each component forms a whole, when the external environment temperature changes, the ceramic tile adhesive expands and contracts with heat due to the change of the environment temperature, a large number of pores have good inclusion on the components with large thermal expansion coefficients in the components, and meanwhile, the mutually staggered reticular structure of the porous nano material can disperse the stress generated by the expansion and contraction with heat, plays a role in buffering among the components with different thermal expansion coefficients, and avoids the cracking and even falling of the ceramic tile adhesive caused by the different stress generated by the expansion and contraction of different components. The addition of the porous nano material can disperse and buffer the stress generated by each component when the temperature changes, improve the adhesion of the tile adhesive and the adaptability of the tile adhesive in different temperature environments, and also can lead the tile adhesive to have wide applicability.
Meanwhile, 3-amino-2, 2-dimethyl propionamide and 3-amino-2, 2-dimethyl propionamide are added into the adhesive reinforcing agent to provide amido and amino, wherein nitrogen atoms have better activity and can react with active groups in porous nano materials, common silicate cement, quartz sand aggregate, fly ash and latex powder respectively, so that the connection between the common silicate cement, quartz sand aggregate, fly ash and latex powder and the porous nano materials can be further improved, each component can enter the pores of the porous nano materials and be adsorbed on the surfaces of the porous nano materials, the connection effect between the components of the ceramic tile adhesive is improved, the overall cohesiveness of the ceramic tile adhesive is further improved, the dispersion and buffering of internal stress generated by the porous nano materials on the components of the ceramic tile adhesive during temperature transformation are improved, and cracking or falling of the ceramic tile adhesive is further avoided.
Wherein the emulsion powder is redispersible emulsion powder, and concretely is ethylene/vinyl acetate copolymer, vinyl acetate/tertiary ethylene carbonate copolymer or acrylic acid copolymer.
According to the scheme, the production of the ceramic tile adhesive is realized. By adding ordinary silicate cement and quartz sand into the tile adhesive as main aggregate components of the tile adhesive, the viscosity and the cohesive force of the tile adhesive are increased, so that the tile adhesive is more easily and tightly adhered to a base layer. The quartz sand makes the paved ceramic tile more firm and durable. Fly ash is added to improve the binding force and the adhesive force between the ceramic tile and the base layer. The flexibility of the tile glue is increased, and the tile is prevented from cracking. The cellulose ether is added to further improve the bonding performance of the tile adhesive and improve the anti-slip performance and the bonding firmness of the tile adhesive. The magnesium aluminum silicate can improve the construction smoothness of the tile adhesive in use. The starch ether can play a role in quick thickening, so that the adhesion between the ceramic tile and the base material is firmer, and meanwhile, the fluidity of the ceramic tile adhesive is improved, and the ceramic tile adhesive is better smeared on a wall surface. Meanwhile, the adhesive reinforcing agent is added, so that the adhesiveness of the tile adhesive is further improved, meanwhile, the adhesive strength of the tile adhesive when the tile adhesive expands with heat and contracts with cold at different temperatures can be obviously improved, the addition of the porous nano material disperses the stress generated by the expansion with heat and contraction with cold of the tile adhesive, the buffer effect is achieved between components with different thermal expansion coefficients, the cracking and even the falling of the tile adhesive caused by the different stress generated by the expansion with heat and contraction with cold of different components are avoided, and the blank formation of the tile adhesive is further avoided.
Optionally, the quartz sand comprises 30-50 mesh quartz sand and 60-80 mesh quartz sand, wherein the weight ratio of the 30-50 mesh quartz sand to the 60-80 mesh quartz sand is 0.75-1:1.
Specifically, the quartz sand can increase the viscosity and the binding force of the tile adhesive, and meanwhile, the strength of the tile adhesive is improved, wherein the strength of the tile adhesive is better through the quartz sand with thicker fineness, and the promotion effect of the binding property of the tile adhesive through the quartz sand with thinner fineness is better, so that the quartz sand with different fineness is mixed for use, and the strength and the binding property of the tile adhesive are jointly promoted.
Alternatively, the Portland cement is 42.5R Portland cement.
Specifically, the ordinary Portland cement is used as a basic component of the adhesive, provides main bonding strength, is beneficial to the bonding property of the tile adhesive, and is convenient for operators to construct in use.
Optionally, the cellulose ether is one or more of methyl cellulose ether, carboxymethyl cellulose ether, carboxypropyl methyl cellulose ether or carboxyethyl cellulose ether.
In particular, the cellulose ether can improve the adhesion of the tile glue. The cellulose ether molecules have stronger adsorptivity and adhesiveness, and can form a uniform adsorption layer on the surface of the tile adhesive, thereby increasing the adhesiveness between the tile and the base layer. And the cellulose ether can improve the rheological property of the tile adhesive, increase the ductility of the tile adhesive, reduce shrinkage deformation, and improve the stability and the adhesion firmness of the tile adhesive.
Optionally, the workability enhancer comprises a weight ratio of 1:0.7-1 wood fiber and sodium gluconate.
In particular, wood fibers belong to natural fibers, differing from synthetic fibers in fiber structure and chemical composition. The bonding property and the flexibility of the ceramic tile adhesive can be effectively enhanced by adding proper wood fiber, and meanwhile, the tensile strength and the shear strength of the ceramic tile adhesive can be improved, the mechanical strength of the ceramic tile adhesive can be improved, and the durability and the reliability of the ceramic tile adhesive can be enhanced. Sodium gluconate is used as a high-efficiency retarder and a high-efficiency water reducing agent in the concrete industry, so that the workability of concrete is greatly improved, the slump loss is reduced, and the later strength of the tile adhesive is improved.
Optionally, the early strength agent is calcium formate, calcium chloride or triethanolamine.
Specifically, the early strength agent has the main effects of accelerating the hydration speed of the ordinary Portland cement, promoting the formation of the early strength of the tile adhesive, obviously improving the cohesive force and cohesive force of the tile adhesive and accelerating the construction speed. And the triethanolamine not only has the early strength function, but also has a certain water reducing and enhancing function.
On the other hand, the application provides a preparation method of the tile adhesive, which comprises the following steps:
(1) Obtaining a porous nanomaterial: adding 2, 5-diamino-benzo-dithiazole into a reaction kettle, adding N, N-dimethylformamide and triethanolamine into the reaction kettle successively under a stirring state to form a dispersion liquid, carrying out ultrasonic treatment on the dispersion liquid for 10-15min, adding cyanuric chloride, carrying out ultrasonic treatment again for 10-20min to obtain slurry to be reacted, reacting the slurry to be reacted at the temperature of 90-130 ℃ for 10-14h to obtain a porous nano material crude product, and washing the porous nano material crude product for multiple times to obtain the porous nano material.
(2) Obtaining an adhesion enhancer: mixing porous nano material, emulsion powder and 3-amino-2, 2-dimethyl propionamide according to the weight ratio to obtain the adhesive reinforcing agent.
(3) Obtaining ceramic tile adhesive: and mixing quartz sand, ordinary Portland cement, fly ash, an easy reinforcing agent, an early strength agent, cellulose ether, magnesium aluminum silicate, starch ether and an adhesive reinforcing agent according to the weight parts for 5-10min to obtain the tile adhesive.
Specifically, N-dimethylformamide is used as a solvent, and a solvothermal method is adopted to synthesize the porous nano material. Firstly, stirring and mixing 2, 5-diamino-benzo-dithiazole and N, N-dimethylformamide, adding triethanolamine as a catalyst, then adding cyanuric chloride, simultaneously adopting ultrasonic treatment to ensure that the dispersibility of reactants is better, mixing the reactants to obtain slurry to be reacted, sealing the slurry to be reacted in a reaction kettle, and reacting for 10-14 hours at the temperature of 90-130 ℃ to obtain a porous nano material crude product. The slurry to be reacted is sealed because high pressure is generated in the reaction process in a high temperature state, and if the reaction raw materials are not sealed, the reaction can be smoothly and safely carried out due to the sealing. And washing the crude porous nano material for multiple times to remove residual raw materials and other impurities, and drying to obtain the porous nano material. And mixing the porous nano material, the latex powder and the 3-amino-2, 2-dimethyl propionamide in a weight ratio to obtain the adhesive reinforcing agent. And finally, mixing quartz sand, ordinary Portland cement, fly ash, an easy reinforcing agent, an early strength agent, cellulose ether, magnesium aluminum silicate, starch ether and an adhesive reinforcing agent according to the weight parts for 5-10min to obtain the tile adhesive.
Optionally, the weight ratio of cyanuric chloride, 2, 5-diamino-benzo-dithiazole, triethanolamine and N, N-dimethylformamide is 1:2.5-3:2.0-2.5:50-80.
Specifically, the N, N-dimethylformamide is taken as a solvent, the addition amount is used for fully dispersing the reaction raw materials, and the weight ratio of the 2, 5-diamino-benzo-dithiazole to the cyanuric chloride can ensure that the 2, 5-diamino-benzo-dithiazole is grafted on the cyanuric chloride, and can avoid waste caused by excessive use amount and subsequent washing procedures.
Optionally, in the step of preparing the porous nanomaterial, washing the crude porous nanomaterial multiple times includes:
And (3) centrifugally separating the crude porous nano material to obtain a precipitate, alternately washing the precipitate with deionized water and ethanol, centrifuging for 3-5 times, and freeze-drying the washed precipitate to obtain the porous nano material.
Specifically, washing impurities in the crude porous nano material by deionized water and ethanol, centrifuging once for each washing, and washing the precipitate again for 3-5 times to obtain the porous nano material. Wherein freeze-drying can maintain the structure of the porous nanomaterial as much as possible and maintain the porosity of the porous nanomaterial.
Optionally, the average particle size of the emulsion powder is 0.2-0.4 μm.
Specifically, the emulsion powder has better viscosity, and meanwhile, in the use process, the emulsion powder can be dispersed into gaps between the ordinary Portland cement and the quartz sand skeleton, so that the ordinary Portland cement, the quartz sand aggregate and the fly ash are further bonded together, the overall bonding strength of the tile adhesive is improved, the stability and the water resistance of the tile adhesive can be improved, the tile is ensured to be completely fixed on a base layer after being paved, and the long-term service life of the tile is ensured.
The technical scheme of the application is illustrated in detail by specific examples.
Example 1
A tile adhesive and a preparation method thereof comprise the following steps:
(1) Obtaining a porous nanomaterial: adding 2, 5-diamino-benzo-dithiazole into a reaction kettle, sequentially adding N, N-dimethylformamide and triethanolamine into the reaction kettle under a stirring state to form a dispersion liquid, carrying out ultrasonic treatment on the dispersion liquid for 10min, adding cyanuric chloride, carrying out ultrasonic treatment again for 10min to obtain slurry to be reacted, reacting the slurry to be reacted at 90 ℃ for 10h to obtain a porous nano material crude product, carrying out centrifugal separation on the porous nano material crude product to obtain a precipitate, alternately washing the precipitate with deionized water and ethanol for 3-5 times, dispersing the washed precipitate into the deionized water, freezing, and carrying out freeze drying on the precipitate and a frozen matter of the deionized water to obtain the porous nano material. Wherein, when the washed precipitate is dispersed into deionized water, the volume ratio of the precipitate to the deionized water is 1:2-3, the freeze drying condition is-40-50 ℃ and the pressure is 5-10Pa.
Wherein, the weight ratio of cyanuric chloride to 2, 5-diamino-benzo-dithiazole to triethanolamine to N, N-dimethylformamide is 1:2.5:2.0:50.
(2) Obtaining an adhesion enhancer: the weight ratio of the porous nano material to the latex powder to the 3-amino-2, 2-dimethyl propionamide is 1:0.5: mixing the components according to the proportion of 0.3 to obtain the adhesive reinforcing agent.
The latex powder is acrylic acid copolymer, and the average grain diameter is 0.3 mu m.
(3) Obtaining ceramic tile adhesive: and mixing quartz sand, ordinary Portland cement, fly ash, an easy reinforcing agent, an early strength agent, cellulose ether, magnesium aluminum silicate, starch ether and an adhesive reinforcing agent according to weight parts for 5 minutes to obtain the tile adhesive.
Wherein the dosage of each component is as follows: 50 parts of quartz sand, 38 parts of 42.5R ordinary Portland cement, 1.5 parts of fly ash, 0.8 part of workability reinforcing agent, 0.5 part of early strength agent, 0.2 part of cellulose ether, 0.04 part of magnesium aluminum silicate, 0.04 part of starch ether and 0.03 part of adhesive reinforcing agent.
The weight ratio of 30-50 mesh quartz sand to 60-80 mesh quartz sand is 0.75:1, the workability enhancer comprises the components in a weight ratio of 1:0.7 of wood fiber and sodium gluconate, wherein the cellulose ether is methyl cellulose ether, and the early strength agent is calcium formate.
Example 2
A tile adhesive and a preparation method thereof comprise the following steps:
The difference from example 1 is that:
(3) Obtaining ceramic tile adhesive: and mixing quartz sand, ordinary Portland cement, fly ash, an easy reinforcing agent, an early strength agent, cellulose ether, magnesium aluminum silicate, starch ether and an adhesive reinforcing agent according to parts by weight for 7 minutes to obtain the ceramic tile adhesive.
Wherein the dosage of each component is as follows: 53 parts of quartz sand, 39.5 parts of 42.5R ordinary Portland cement, 1.8 parts of fly ash, 0.98 part of workability reinforcing agent, 0.6 part of early strength agent, 0.4 part of cellulose ether, 0.06 part of magnesium aluminum silicate, 0.05 part of starch ether and 0.04 part of adhesion reinforcing agent.
The weight ratio of 30-50 mesh quartz sand to 60-80 mesh quartz sand is 0.8:1, the workability enhancer comprises the components in a weight ratio of 1:0.8 of wood fiber and sodium gluconate, wherein the cellulose ether is methyl cellulose ether, and the early strength agent is calcium formate.
Example 3
A tile adhesive and a preparation method thereof comprise the following steps:
The difference from example 1 is that:
(3) Obtaining ceramic tile adhesive: and mixing quartz sand, ordinary Portland cement, fly ash, an easy reinforcing agent, an early strength agent, cellulose ether, magnesium aluminum silicate, starch ether and an adhesive reinforcing agent according to parts by weight for 10 minutes to obtain the ceramic tile adhesive.
Wherein the dosage of each component is as follows: 57 parts of quartz sand, 41 parts of 42.5R ordinary Portland cement, 2.2 parts of fly ash, 1 part of workability reinforcing agent, 0.7 part of early strength agent, 0.6 part of cellulose ether, 0.08 part of magnesium aluminum silicate, 0.06 part of starch ether and 0.06 part of adhesive reinforcing agent.
The weight ratio of 30-50 mesh quartz sand to 60-80 mesh quartz sand is 0.9:1, the workability enhancer comprises the components in a weight ratio of 1:0.9 of wood fiber and sodium gluconate, wherein the cellulose ether is methyl cellulose ether, and the early strength agent is calcium formate.
Example 4
A tile adhesive and a preparation method thereof comprise the following steps:
The difference from example 1 is that:
(3) Obtaining ceramic tile adhesive: and mixing quartz sand, ordinary Portland cement, fly ash, an easy reinforcing agent, an early strength agent, cellulose ether, magnesium aluminum silicate, starch ether and an adhesive reinforcing agent according to parts by weight for 10 minutes to obtain the ceramic tile adhesive.
Wherein the dosage of each component is as follows: 60 parts of quartz sand, 42.5 parts of 42.5R ordinary Portland cement, 2.5 parts of fly ash, 1.2 parts of workability reinforcing agent, 0.8 part of early strength agent, 0.8 part of cellulose ether, 0.1 part of magnesium aluminum silicate, 0.06 part of starch ether and 0.07 part of adhesive reinforcing agent.
The weight ratio of 30-50 mesh quartz sand to 60-80 mesh quartz sand is 1:1, the workability enhancer comprises the components in a weight ratio of 1:1, wood fiber and sodium gluconate, wherein the cellulose ether is methyl cellulose ether, and the early strength agent is calcium formate.
Example 5
A tile adhesive and a preparation method thereof comprise the following steps:
the difference from example 3 is that:
(1) Obtaining a porous nanomaterial: adding 2, 5-diamino-benzo-dithiazole into a reaction kettle, sequentially adding N, N-dimethylformamide and triethanolamine into the reaction kettle under a stirring state to form a dispersion liquid, carrying out ultrasonic treatment on the dispersion liquid for 15min, adding cyanuric chloride, carrying out ultrasonic treatment again for 20min to obtain a slurry to be reacted, reacting the slurry to be reacted at 110 ℃ for 12h to obtain a porous nano material crude product, carrying out centrifugal separation on the porous nano material crude product to obtain a precipitate, alternately washing the precipitate with deionized water and ethanol, centrifuging for 3-5 times, and freeze-drying the washed precipitate to obtain the porous nano material.
Wherein, the weight ratio of cyanuric chloride to 2, 5-diamino-benzo-dithiazole to triethanolamine to N, N-dimethylformamide is 1:2.7:2.2:65.
(2) Obtaining an adhesion enhancer: the weight ratio of the porous nano material to the latex powder to the 3-amino-2, 2-dimethyl propionamide is 1:0.65: mixing the components according to the proportion of 0.4 to obtain the adhesive reinforcing agent.
The latex powder is acrylic acid copolymer, and the average grain diameter is 0.3 mu m.
Example 6
A tile adhesive and a preparation method thereof comprise the following steps:
the difference from example 3 is that:
(1) Obtaining a porous nanomaterial: adding 2, 5-diamino-benzo-dithiazole into a reaction kettle, sequentially adding N, N-dimethylformamide and triethanolamine into the reaction kettle under a stirring state to form a dispersion liquid, carrying out ultrasonic treatment on the dispersion liquid for 15min, adding cyanuric chloride, carrying out ultrasonic treatment again for 20min to obtain a slurry to be reacted, reacting the slurry to be reacted at 130 ℃ for 14h to obtain a porous nano material crude product, carrying out centrifugal separation on the porous nano material crude product to obtain a precipitate, alternately washing the precipitate with deionized water and ethanol, centrifuging for 3-5 times, and freeze-drying the washed precipitate to obtain the porous nano material.
Wherein, the weight ratio of cyanuric chloride to 2, 5-diamino-benzo-dithiazole to triethanolamine to N, N-dimethylformamide is 1:3:2.5:80.
(2) Obtaining an adhesion enhancer: the weight ratio of the porous nano material to the latex powder to the 3-amino-2, 2-dimethyl propionamide is 1:0.8: mixing the components according to the proportion of 0.6 to obtain the adhesive reinforcing agent.
The latex powder is acrylic acid copolymer, and the average grain diameter is 0.4 mu m.
Comparative example 1
A tile adhesive and a preparation method thereof comprise the following steps:
The difference from example 5 is that:
(3) Obtaining ceramic tile adhesive: the dosage of each component is as follows: 57 parts of quartz sand, 41 parts of 42.5R ordinary Portland cement, 2.2 parts of fly ash, 1 part of workability reinforcing agent, 0.7 part of early strength agent, 0.6 part of cellulose ether, 0.08 part of magnesium aluminum silicate, 0.06 part of starch ether and 0.02 part of adhesive reinforcing agent.
Comparative example 2
A tile adhesive and a preparation method thereof comprise the following steps:
The difference from example 5 is that:
(3) Obtaining ceramic tile adhesive: the dosage of each component is as follows: 57 parts of quartz sand, 41 parts of 42.5R ordinary Portland cement, 2.2 parts of fly ash, 1 part of workability reinforcing agent, 0.7 part of early strength agent, 0.6 part of cellulose ether, 0.08 part of magnesium aluminum silicate, 0.06 part of starch ether and 0.08 part of adhesive reinforcing agent.
Comparative example 3
A tile adhesive and a preparation method thereof comprise the following steps:
The difference from example 5 is that:
(2) Obtaining an adhesion enhancer: the weight ratio of the latex powder to the 3-amino-2, 2-dimethyl propionamide is 0.65: mixing the components according to the proportion of 0.4 to obtain the adhesive reinforcing agent. The adhesion enhancer does not contain porous nanomaterial.
Comparative example 4
A tile adhesive and a preparation method thereof comprise the following steps:
The difference from example 5 is that:
(2) Obtaining an adhesion enhancer: the porous nano material and the emulsion powder are mixed according to the weight ratio of 1: mixing the components according to the proportion of 0.65 to obtain the adhesive reinforcing agent. The adhesion enhancer does not contain 3-amino-2, 2-dimethylpropionamide.
Experimental example 1
The tensile bond strength, tensile bond strength after immersion, tensile bond strength after heat aging, tensile bond strength after freeze thawing cycle, and tensile bond strength for open time of 20min or more of tile adhesives prepared using the above-described schemes provided in examples 1 to 6 and comparative examples 1 to 4 were examined, at least 3 parallel experiments were set for each group, and the average was taken to obtain the results shown in table one.
The test standard is JC/T547-2017 of ceramic wall and floor tile adhesive.
List one
As can be seen from table one, the adhesive strength of the tile adhesives produced in examples 1 to 6 was significantly improved compared to comparative examples 1 to 4. In examples 1 to 6, the tile adhesive contains the aggregates of ordinary portland cement, quartz sand aggregate and fly ash, provides main adhesive components, and is added with an early strength agent for improving the early mechanical properties of the tile adhesive, so that the early adhesion of the tile adhesive to a substrate and tiles is facilitated, and the construction progress is accelerated. Cellulose ether is also added to further improve the adhesive property of the tile adhesive. As can be seen from table one, the tensile bond strength after heat aging and the tensile bond strength after freeze thawing cycle in examples 1 to 6 are both significantly higher than those in examples 1 to 4, because the adhesion of the tile glue is further improved by adding the adhesion enhancer to the tile glue, and the bond strength of the tile glue when heat expansion and cold contraction occur at different temperatures can be significantly improved. The adhesive reinforcing agent comprises latex powder, 3-amino-2, 2-dimethyl propionamide and a porous nanomaterial, after the porous nanomaterial is added, each component in the tile adhesive enters the pores of the porous nanomaterial, and the mutually staggered reticular structure plays a role in connecting and gathering each component in the tile adhesive, so that each component forms a whole, when the external environment temperature changes, the tile adhesive can expand with heat and contract with cold due to the change of the external environment temperature, a large number of pores have good inclusion for the components with large thermal expansion coefficients in the components, and meanwhile, the mutually staggered reticular structure of the porous nanomaterial can disperse the stress generated by the expansion with cold, plays a role in buffering among the components with different thermal expansion coefficients, and avoids cracking or even falling of the tile adhesive caused by the different stress generated by the expansion with the contraction with different components. The addition of the porous nano material can disperse and buffer the stress generated by each component when the temperature changes, improve the adhesion of the tile adhesive and the adaptability of the tile adhesive in different temperature environments, and also can lead the tile adhesive to have wide applicability. The 3-amino-2, 2-dimethylpropionamide provides amido and amino, nitrogen atoms in the amido and amino have better activity, and the amido and amino can react with active groups in porous nano materials, common silicate cement, quartz sand aggregate, fly ash and emulsion powder respectively, so that the connection between the common silicate cement, the quartz sand aggregate, the fly ash and the emulsion powder and the porous nano materials can be further improved, the components can be adsorbed on the surface of the porous nano materials while entering the pores of the porous nano materials, the connection effect between the components of the ceramic tile adhesive is improved, the overall cohesiveness of the ceramic tile adhesive is further improved, and the dispersion and buffering of internal stress generated by the porous nano materials to the components of the ceramic tile adhesive during temperature transformation are further avoided.
Examples 1 to 6, compared with comparative examples 1 and 2, demonstrate that although the addition of the adhesion enhancer is advantageous for improving the tensile bond strength after heat aging and the tensile bond strength after freeze-thawing cycle of the tile glue, the addition amount of the adhesion enhancer should be within a proper range, and that neither too much nor too little addition has a significant effect on improving the bond strength of the tile glue at different temperatures. The adhesive reinforcing agent of the present application is preferably added in an amount.
In addition, in the embodiments 1 to 6, compared with the embodiments 3 and 4, the porous nano material and 3-amino-2, 2-dimethyl propionamide added in the adhesion enhancer are mutually synergistic, the porous structure has stronger adsorptivity, the common silicate cement and quartz sand aggregate, the fly ash and the emulsion powder in the tile adhesive are adsorbed in the pores and on the surfaces, so that the particles are filled in the pores of the porous nano material, the porous nano material further plays a cohesive role on each component of the porous nano material while the components in the tile adhesive are mutually adhered, and the 3-amino-2, 2-dimethyl propionamide respectively reacts with the porous nano material, the common silicate cement and the quartz sand aggregate, the fly ash and the active groups in the emulsion powder, so that the connection of the common silicate cement and the quartz sand aggregate, the fly ash and the emulsion powder with the porous nano material can be further improved, the components can be adsorbed on the surfaces of the porous nano material while entering the pores of the porous nano material, the connection effect between the components of the tile adhesive is improved, the overall adhesion of the tile adhesive is further improved, the dispersion of the components of the porous nano material to the tile adhesive is improved, and the internal stress of the tile adhesive is further avoided when the components of the porous nano material are dispersed and the tile adhesive is further dispersed.
Experimental example 2
Toxicity of tile adhesives prepared using the protocol provided in example 5 above was tested, at least 3 replicates were set for each group, and averaged.
The test criteria were: radionuclide detection (including internal and external illumination indices): "A-type decorative finishing Material" GB 6566-2010;
Free formaldehyde detection: "quantity of harmful substances in interior Material adhesive" GB 18583-2008
Hexavalent chromium content: determination of six limiting substances (lead, mercury, cadmium, hexavalent chromium, polybrominated biphenyls and polybrominated diphenyl ethers) for electronic and electric products, GB/T26125-2011
The detection result is as follows: in radionuclide detection, the internal irradiation index I Ra is 0.1 which is far lower than 1.0 specified in the standard, the external irradiation index I r is 0.2 which is lower than 1.3 specified in the standard, and free formaldehyde and hexavalent chromium are not detected, so that the tile glue provided by the application is environment-friendly and nontoxic, and can be applied to more places.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solution of the present application, and not limiting thereof; although the application has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art will appreciate that; the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the application.
Claims (10)
1. The ceramic tile adhesive is characterized by comprising the following components in parts by weight:
50-60 parts of quartz sand, 38-42 parts of ordinary Portland cement, 1.5-2.5 parts of fly ash, 0.8-1.2 parts of workability reinforcing agent, 0.5-0.8 part of early strength agent, 0.2-0.8 part of cellulose ether, 0.04-0.1 part of magnesium aluminum silicate, 0.04-0.06 part of starch ether and 0.03-0.07 part of adhesion reinforcing agent;
The adhesion enhancer comprises the following components in percentage by weight: 0.5-0.8:0.3-0.6 of latex powder, 3-amino-2, 2-dimethyl propionamide and porous nanometer materials.
2. The tile glue of claim 1, wherein the quartz sand comprises 30-50 mesh quartz sand and 60-80 mesh quartz sand, and the weight ratio of the 30-50 mesh quartz sand to the 60-80 mesh quartz sand is 0.75-1:1.
3. The tile glue of claim 1, wherein the portland cement is 42.5R portland cement.
4. The tile glue of claim 1, wherein the cellulose ether is one or more of methyl cellulose ether, carboxymethyl cellulose ether, carboxypropyl methyl cellulose ether, or carboxyethyl cellulose ether.
5. The tile glue of any one of claims 1-4, wherein the workability enhancing agent comprises a weight ratio of 1:0.7-1 wood fiber and sodium gluconate.
6. The tile glue of claim 5, wherein the early strength agent is calcium formate, calcium chloride or triethanolamine.
7. A method for preparing a tile glue according to any one of claims 1 to 6, comprising the steps of:
(1) Obtaining a porous nanomaterial: adding 2, 5-diamino-benzo-dithiazole into a reaction kettle, sequentially adding N, N-dimethylformamide and triethanolamine into the reaction kettle in a stirring state to form a dispersion liquid, ultrasonically treating the dispersion liquid for 10-15min, adding cyanuric chloride, ultrasonically treating for 10-20min again to obtain slurry to be reacted, reacting the slurry to be reacted for 10-14h at the temperature of 90-130 ℃ to obtain a porous nano material crude product, and washing the porous nano material crude product for multiple times to obtain the porous nano material;
(2) Obtaining an adhesion enhancer: mixing the porous nano material, the latex powder and the 3-amino-2, 2-dimethylpropionamide according to the weight ratio to obtain the adhesive reinforcing agent;
(3) Obtaining ceramic tile adhesive: and mixing the quartz sand, the ordinary portland cement, the fly ash, the easy reinforcing agent, the early strength agent, the cellulose ether, the magnesium aluminum silicate, the starch ether and the adhesion reinforcing agent according to parts by weight for 5-10min to obtain the tile adhesive.
8. The method for preparing ceramic tile glue according to claim 7, wherein the weight ratio of cyanuric chloride, 2, 5-diamino-benzo-dithiazole, triethanolamine and N, N-dimethylformamide is 1:2.5-3:2.0-2.5:50-80.
9. The method of preparing a tile glue according to claim 8, wherein in the step of preparing the porous nanomaterial, washing the crude porous nanomaterial a plurality of times comprises:
And (3) centrifugally separating the crude porous nano material to obtain a precipitate, alternately washing the precipitate with deionized water and ethanol, centrifuging for 3-5 times, and freeze-drying the washed precipitate to obtain the porous nano material.
10. The method for preparing tile adhesive according to claim 9, wherein the average particle size of the emulsion powder is 0.2-0.4 μm.
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