A composition for tile adhesive, tile adhesive and a method of preparing the same

Abstract

The present application relates to the technical field of building materials, in particular to a composition for ceramic tile glue, ceramic tile glue and a preparation method thereof. The composition for ceramic tile glue contains a main agent and an auxiliary agent; the main agent contains Portland cement, redispersible latex powder, cellulose ether and fluorosilicone oil-starch sol. The ceramic tile glue provided by the present application contains fluorosilicone oil-starch sol, can realize dust suppression in the whole cycle of the construction stage and the maintenance period, and has a long-lasting effect. Meanwhile, the ceramic tile glue has strong environmental adaptability and shear resistance, can keep stable performance in a humid environment, and still has a high elastic network retention rate and a low dynamic construction dust dispersion rate under high shear.

Description

Technical Field

[0001] This invention relates to the field of building materials technology, and specifically to a composition for tile adhesive, tile adhesive and its preparation method. Background Technology

[0002] Tile adhesive is a modern decorative material with high adhesion, high waterproof and impermeable properties, as well as crack resistance and aging resistance. It is widely used for bonding indoor and outdoor ceramic wall and floor tiles, and for waterproofing the interior and exterior walls of various buildings.

[0003] The dust generated during the production and use of traditional tile adhesives can cause environmental pollution and harm the health of those involved. Therefore, there is an urgent need to find effective measures to solve the dust problem caused by tile adhesives.

[0004] CN118580022A discloses a composition for dust-free tile adhesive and its application, as well as dust-free tile adhesive. The composition for dust-free tile adhesive includes: a solid dust suppressant, phospholipids, a dispersant, nano-silica, and nano-modified bentonite. It can suppress dust from tile adhesive, reduce the mixing difficulty of dust-free tile adhesive, and take into account the cohesive strength of dust-free tile adhesive. However, phospholipids are easily hydrolyzed in alkaline cement environments, and the dust suppression network is easily damaged under shear force during dynamic construction.

[0005] CN118851658A discloses a dust-free tile adhesive composition, its preparation method, and the tile adhesive itself. The method involves mixing a dust-reducing agent with sand, then mixing the resulting mixture with a powder composition containing cement to obtain the dust-free tile adhesive composition. This dust-free tile adhesive composition significantly reduces dust generation, and the tile adhesive exhibits good tensile bond strength. However, this method relies on physical coating, resulting in a short dust suppression time (≤7 days), and a 50% decrease in effectiveness in humid environments.

[0006] Dust-free tile adhesive is a new type of tile bonding material with low dust emissions. By optimizing particle size distribution and formula design, it reduces dust emission during construction, meeting the indoor air quality requirements of green buildings. However, ordinary dust-free tile adhesives suffer from poor dust suppression, poor adaptability to humid environments, and unstable bonding strength. Therefore, there is an urgent need to develop a tile adhesive dust suppressant with good dust suppression, strong environmental adaptability, and high bonding strength. Summary of the Invention

[0007] The purpose of this invention is to overcome the problems of poor dust suppression effect, poor adaptability to humid environments, and insufficient dynamic stability of dust suppression networks in existing tile adhesive dust suppressants.

[0008] To achieve the above objectives, a first aspect of the present invention provides a composition for tile adhesive, the composition comprising a main agent and an additive; said main agent comprising silicate cement, redispersible latex powder, cellulose ether, and fluorosilicone oil-starch sol; Based on the total weight of the composition, the content of the silicate cement is 35-50 wt%, the content of the redispersible latex powder is 1-3 wt%, the content of the cellulose ether is 0.2-0.4 wt%, and the content of the fluorosilicone oil-starch sol is 8-12 wt%. The fluorosilicone oil-starch sol contains fluorosilicone oil, maleic anhydride-modified starch, and nano-titanium dioxide; Based on the total weight of the fluorosilicone oil-starch sol, the content of the fluorosilicone oil is 10-20 wt%, the content of the maleic anhydride modified starch is 30-80 wt%, and the content of the nano titanium dioxide is 20-60 wt%.

[0009] A second aspect of the present invention provides a method for preparing tile adhesive, the method comprising using the components of the composition described in the first aspect of the present invention, including: (1) Silicate cement, aggregate, filler, cellulose ether and redispersible latex powder are first mixed to obtain intermediate I; (2) The intermediate I is mixed with fluorosilicone oil-starch sol for a second time to obtain an encapsulated powder; (3) The encapsulated powder is mixed with water in a third mixing process to obtain the tile adhesive.

[0010] A third aspect of the present invention provides a tile adhesive prepared by the method described in the second aspect.

[0011] Through the above technical solution, the present invention has at least the following advantages: (1) The tile adhesive provided by the present invention contains fluorosilicone oil-starch sol as a dust suppressant, which can achieve dust suppression throughout the construction and curing periods and has a long-lasting effect.

[0012] (2) The tile adhesive provided by this invention has strong environmental adaptability and shear resistance. It can maintain stable performance in humid environments and still has a high elastic network retention rate and a low dynamic construction dust emission rate under high shear.

[0013] (3) The tile adhesive provided by the present invention can balance the dust suppression effect with the physical properties of the tile adhesive such as bonding strength and water retention. Detailed Implementation

[0014] The endpoints and any values ​​of the ranges disclosed herein are not limited to the precise ranges or values, and these ranges or values ​​should be understood to include values ​​close to these ranges or values. For numerical ranges, the endpoint values ​​of the various ranges, the endpoint values ​​of the various ranges and individual point values, and individual point values ​​can be combined with each other to obtain one or more new numerical ranges, which should be considered as specifically disclosed herein.

[0015] As previously described, a first aspect of the present invention provides a composition for tile adhesive, the composition comprising a main agent and an additive; said main agent comprising silicate cement, redispersible latex powder, cellulose ether and fluorosilicone oil-starch sol; Based on the total weight of the composition, the content of the silicate cement is 35-50 wt%, the content of the redispersible latex powder is 1-3 wt%, the content of the cellulose ether is 0.2-0.4 wt%, and the content of the fluorosilicone oil-starch sol is 8-12 wt%. The fluorosilicone oil-starch sol contains fluorosilicone oil, maleic anhydride-modified starch, and nano-titanium dioxide; Based on the total weight of the fluorosilicone oil-starch sol, the content of the fluorosilicone oil is 10-20 wt%, the content of the maleic anhydride modified starch is 30-80 wt%, and the content of the nano titanium dioxide is 20-60 wt%.

[0016] Preferably, the fluorosilicone oil-starch sol is prepared by a method comprising the following steps: (1) In the presence of a solvent, fluorosilicone oil is contacted with maleic anhydride modified starch to carry out an esterification reaction to obtain a crosslinked prepolymer; the kinematic viscosity of the fluorosilicone oil at 25°C is 500-10000cSt and the surface tension at 25°C is ≤30mN / m. (2) The cross-linked prepolymer is mixed with nano-titanium dioxide to obtain the fluorosilicone oil-starch sol.

[0017] Preferably, the fluorosilicone oil is selected from at least one of trifluoropropylmethyl silicone oil and alkyl polyether modified fluorosilicone oil.

[0018] Preferably, the maleic anhydride modified starch is selected from at least one of maleic anhydride corn starch and maleic anhydride potato starch.

[0019] Preferably, in step (1), the solvent is a mixture of ethanol and water.

[0020] More preferably, in step (1), the volume ratio of ethanol to water in the mixture is 1:1-5.

[0021] Preferably, in step (1), the weight ratio of the fluorosilicone oil to the maleic anhydride-modified starch is 1:1.5-5. The inventors have found that, under this preferred condition, the fluorosilicone oil-starch sol provided by the present invention possesses stronger alkali resistance and shear resistance.

[0022] More preferably, the amount of solvent used is 1250-2500 mL relative to 100 g of the fluorosilicone oil.

[0023] In a preferred embodiment, in step (1), the conditions for the esterification reaction include: a temperature of 50-70°C and a time of 1-3 hours.

[0024] Preferably, in step (2), the weight ratio of the crosslinked prepolymer to the nano-titanium dioxide is 1:0.2-0.6.

[0025] More preferably, the weight-average diameter of the nano-titanium dioxide is 50-100 nm. The inventors have found that, under this preferred condition, the fluorosilicone oil-starch sol provided by the present invention has a more significant effect on the photocatalytic decomposition of organic dust, while also possessing stronger shear resistance.

[0026] More preferably, the nano-titanium dioxide is selected from at least one of rutile nano-titanium dioxide and anatase titanium dioxide.

[0027] In a preferred embodiment, the conditions for the mixing reaction include: a temperature of 50-60°C and a time of 5-60 min.

[0028] Preferably, the mixing reaction is carried out by ultrasonic dispersion. The present invention does not impose any particular requirements on the specific operation of the ultrasonic dispersion; those skilled in the art can use methods known in the art.

[0029] Preferably, the additive contains aggregates and fillers.

[0030] More preferably, based on the total weight of the composition, the content of the aggregate is 35-45 wt% and the content of the filler is 5-10 wt%.

[0031] Preferably, the silicate cement is selected from at least one of P·O42.5 grade, P·O42.5R grade, P·O52.5 grade, and P·O52.5R grade.

[0032] Preferably, the redispersible latex powder is a water-soluble redispersible powder; the water-soluble redispersible powder is selected from at least one of ethylene / vinyl acetate copolymer redispersible powder, vinyl acetate / ethylene tert-carbonate copolymer redispersible powder, acrylic copolymer redispersible powder, acrylate / styrene copolymer redispersible powder, and styrene / butadiene copolymer redispersible powder.

[0033] Preferably, the cellulose ether is selected from at least one of hydroxyethyl methyl cellulose ether and hydroxypropyl methyl cellulose ether.

[0034] Preferably, the hydroxypropyl methylcellulose ether is selected from at least one of low-viscosity hydroxypropyl methylcellulose ether, medium-viscosity hydroxypropyl methylcellulose ether, and high-viscosity hydroxypropyl methylcellulose ether.

[0035] More preferably, the low-viscosity hydroxypropyl methylcellulose ether has a kinematic viscosity of 50-500 mPa·s at 25°C; the medium-viscosity hydroxypropyl methylcellulose ether has a kinematic viscosity of 1000-5000 mPa·s at 25°C; and the high-viscosity hydroxypropyl methylcellulose ether has a kinematic viscosity of 10,000-100,000 mPa·s at 25°C.

[0036] Preferably, the average particle size of the aggregate is 0.1-0.3 mm.

[0037] More preferably, the aggregate is selected from at least one of quartz sand, river sand, and limestone sand.

[0038] Preferably, the average particle size of the filler is 60-100 μm.

[0039] More preferably, the filler is selected from at least one of calcium powder and stone powder.

[0040] As previously described, a second aspect of the present invention provides a method for preparing tile adhesive, the method comprising using the components of the composition described in the first aspect, including: (1) Silicate cement, aggregate, filler, cellulose ether and redispersible latex powder are first mixed to obtain intermediate I; (2) The intermediate I is mixed with fluorosilicone oil-starch sol for a second time to obtain an encapsulated powder; (3) The encapsulated powder is mixed with water in a third mixing process to obtain the tile adhesive.

[0041] Preferably, in step (1), the first mixing time is 1-20 min.

[0042] Preferably, in step (2), the operation of performing the second mixing includes: introducing the fluorosilicone oil-starch sol in the form of a spray to contact the intermediate I.

[0043] More preferably, in step (2), the introduction flow rate of the fluorosilicone oil-starch sol is 1-2 g / min relative to 1 kg of the intermediate I.

[0044] Preferably, in step (3), the mixing conditions for the third mixing are: stirring speed 300-500 rpm, time 3-5 min.

[0045] More preferably, in step (3), the weight ratio of the encapsulated powder to the water is 1:0.25-0.30. The inventors have found that, under this preferred condition, the tile adhesive provided by the present invention possesses a higher shear viscosity.

[0046] As previously stated, a third aspect of the present invention provides a tile adhesive prepared by the method described in the second aspect.

[0047] Preferably, the tile adhesive has a bonding strength ≥0.6MPa, a 28d friction dust suppression efficiency ≥70wt%, a shear dust emission rate ≤15wt%, and a high humidity dust suppression tolerance coefficient ≥90wt% in an environment with a relative humidity of 90%RT.

[0048] The present invention will be described in detail below through examples. In the following examples, the reagents and raw materials involved are all commercially available products, and the reagents are all analytical grade products.

[0049] Fluorosilicone oil: Trifluoropropylmethyl silicone oil, with a kinematic viscosity of 5000 cSt at 25°C and a surface tension of 25 mN / m at 25°C, was purchased from Wuhan Hongde Yuexin Pharmaceutical Technology Co., Ltd. Alkyl polyether modified fluorosilicone oil, with a kinematic viscosity of 600 cSt at 25°C and a surface tension of 20 mN / m at 25°C, was purchased from Shenzhen Jipeng Silicon Fluorine Materials Co., Ltd. Maleic anhydride modified starch: Maleic anhydride corn starch was purchased from Foshan Gaofeng Starch Technology Co., Ltd. Maleic anhydride potato starch was purchased from Guangxi Mingyang Biochemical Technology Co., Ltd. Nano titanium dioxide: Rutile nano-titanium dioxide, with an average diameter of 60 nm, was purchased from Xuancheng Jingrui New Materials Co., Ltd. Anatase titanium dioxide: with an average diameter of 60 nm, purchased from Lomon Billions Group Co., Ltd. Cellulose ether: Hydroxypropyl methylcellulose ether, brand name HD110, is a high-viscosity hydroxypropyl methylcellulose ether with a kinematic viscosity of 20000 Pa·s at 25°C, purchased from Shandong Heda Co., Ltd. Silicate cement: strength grade P·O42.5, purchased from Yangchun Conch Cement Co., Ltd.; Aggregate: Quartz sand, with an average particle size of 0.2 mm, purchased from Guangdong Aosheng New Materials Co., Ltd.; Filler: calcium powder, with an average particle size of 75μm, purchased from Zhongshan Xiongding Environmental Building Materials Co., Ltd. Redispersible latex powder: average particle size 150μm, grade 5010N, purchased from Wacker Chemie (China) Co., Ltd.

[0050] Unless otherwise specified, the total mass of the fluorosilicone oil-starch sol prepared in the following examples is 10g, and the total mass of the tile adhesive prepared is 1000g.

[0051] Example 1 Fluorosilicone oil-starch sol is prepared using the following steps: (1) Using a mixture of 2500 mL of ethanol and water in a volume ratio of 1:2 as a solvent, add fluorosilicone oil in a weight ratio of 1:3 and maleic anhydride modified starch (of which the mass of fluorosilicone oil is 150 g) to the solvent to carry out an esterification reaction to obtain a crosslinked prepolymer; the conditions for the esterification reaction include: a temperature of 60 °C and a time of 2 h.

[0052] (2) The crosslinked prepolymer with a weight ratio of 1:0.4 and nano-titanium dioxide are mixed and reacted by ultrasonic dispersion to obtain the fluorosilicone oil-starch sol; the conditions for the mixing reaction include: temperature of 60°C and time of 15 min.

[0053] Tile adhesive is prepared using the following steps: (1) Silicate cement, aggregate, filler, cellulose ether and redispersible latex powder are mixed for the first time (the mass of silicate cement is 400g) for 5min to obtain intermediate I; (2) Relative to 1 kg of the intermediate I, the fluorosilicone oil-starch sol is introduced in the form of spray at a flow rate of 1.5 g / min to perform a second mixing with the intermediate I to obtain an encapsulated powder; (3) The coated powder is mixed with water in a third mixing process to obtain the tile adhesive. The mixing conditions for the third mixing are as follows: the weight ratio of the coated powder to the water is 1:0.28, the stirring speed is 500 rpm, and the mixing time is 5 min.

[0054] The remaining specific process parameters of this embodiment are shown in Table 1. In Table 1, the content of fluorosilicone oil refers to the proportion of the mass of fluorosilicone oil to the total mass of fluorosilicone oil-starch sol; the content of maleic anhydride modified starch refers to the proportion of the mass of maleic anhydride modified starch to the total mass of fluorosilicone oil-starch sol; the content of nano titanium dioxide refers to the proportion of the mass of nano titanium dioxide to the total mass of fluorosilicone oil-starch sol; the content of silicate cement refers to the proportion of the mass of silicate cement to the total mass of the tile adhesive composition; the content of aggregate refers to the proportion of the mass of aggregate to the total mass of the tile adhesive composition; the content of filler refers to the proportion of the mass of filler to the total mass of the tile adhesive composition; the content of redispersible latex powder refers to the proportion of the mass of redispersible latex powder to the total mass of the tile adhesive composition; the content of fluorosilicone oil-starch sol refers to the proportion of the mass of fluorosilicone oil-starch sol to the total mass of the tile adhesive composition; and the content of cellulose ether refers to the proportion of the mass of cellulose ether to the total mass of the tile adhesive composition.

[0055] Examples 2-13 Examples 2-13 all used the same process as Example 1, with the differences listed in Table 1.

[0056] Comparative Examples 1-9 Comparative Examples 1-9 all used the same process as Example 1, with the differences listed in Table 1.

[0057] Table 1

[0058] Table 1 (continued)

[0059] Test case The physical performance test data of the examples and comparative examples are shown in Table 2.

[0060] The test methods for tensile bond strength, tensile bond strength after immersion in water, and tensile bond strength after heat aging shall refer to the section on "Determination of Tensile Bond Strength" in JC / T547-2017 "Ceramic Tile Adhesives".

[0061] The test method for shear dust emission rate is as follows: Referencing ASTM D2983, "Determination of Plastic Viscosity and Yield Value," coupled with dust emission testing; the experimental setup includes a rheometer (equipped with parallel plate clamps, 25mm in diameter, 1mm gap) and a dust emission monitoring system (laser particle size analyzer + PM2.5 sensor); the test steps include: preparing tile adhesive mortar, and in the rheometer, at a speed of 10-1000 s⁻¹... -1 The shear rate gradient was scanned, and the viscosity-shear rate curve was recorded. During the shearing process, the dust emission rate on the slurry surface was monitored simultaneously (PM2.5 concentration was collected every 10 seconds). The shear dust emission rate can be calculated using formula (1). [PM2.5] max [PM2.5]0 refers to the peak value of PM2.5 concentration during the shearing process; [PM2.5]0 refers to the initial value of PM2.5 concentration.

[0062]

[0063] The test method for the high humidity dust suppression tolerance coefficient is as follows: Referencing the improved environmental control module of ISO 11925-2 "Test for flammability of building materials"; the experimental setup includes a constant temperature and humidity chamber (humidity control range 30%-90%) and a dust emission test chamber (with real-time humidity adjustment function); the test steps include: placing the dust-free ceramic tile adhesive powder and the control sample without dust suppressant in environments with 50% and 90% humidity for 24 hours respectively; after removal (adding water at a water-to-powder ratio of 1:0.28), stirring at 200 rpm for 3 minutes in the dust emission test chamber, and recording the PM2.5 concentration at different humidity levels. The dust suppression efficiency is calculated using formula (2), and the high humidity dust suppression tolerance coefficient can be calculated using formula (3). In formula (2), [PM2.5] CK [PM2.5]1 refers to the PM2.5 concentration of the control sample; [PM2.5]1 refers to the PM2.5 concentration of the dust-free ceramic tile adhesive powder; in formula (3), the dust suppression efficiency (90%RT) refers to the dust suppression efficiency when the humidity is 90%RT; the dust suppression efficiency (50%RT) refers to the dust suppression efficiency when the humidity is 50%RT.

[0064]

[0065] The test method for the 28-day friction dust suppression efficiency is a modified version of GB / T16157 "Methods for Determination of Particulate Matter and Sampling of Gaseous Pollutants in Exhaust Gas from Stationary Sources". The experimental setup includes a sealed mixing chamber (1 m³, with a dust concentration sensor) and a constant temperature and humidity curing chamber (temperature controlled at 23 ± 2 ℃, humidity at 50 ± 5%). The test steps include: weighing 500 g each of the tile adhesive and the control sample without dust suppressant, adding water at a water-to-powder ratio of 1:0.28 and stirring, stirring at 300 r / min for 5 min in the mixing chamber, and recording the initial PM2.5 concentration in real time; making 100 mm × 100 mm test blocks from the stirred slurry, curing for 28 days, scraping the surface of the test blocks with a scraper, simulating construction dust in the mixing chamber, and recording the PM2.5 concentration during scraping. The 28-day friction dust suppression efficiency can be calculated using formula (4). In formula (4), [PM2.5] CK [PM2.5]1 refers to the PM2.5 concentration when the control sample is scraped; [PM2.5]1 refers to the PM2.5 concentration when the tile adhesive in this scheme is scraped.

[0066]

[0067] Table 2

[0068] As can be seen from the results in the table above, the tile adhesive provided by this invention has significant advantages such as long-lasting dust suppression effect, strong adaptability to humid environments, and high bonding strength. Its dust suppression efficiency remains at a high level, and it has high practical application value.

[0069] The preferred embodiments of the present invention have been described in detail above; however, the present invention is not limited thereto. Within the scope of the inventive concept, various simple modifications can be made to the technical solutions of the present invention, including combinations of various technical features in any other suitable manner. These simple modifications and combinations should also be considered as the content disclosed in the present invention and are all within the protection scope of the present invention.

Claims

1. A composition for tile adhesive, characterized by, The composition contains a main agent and an auxiliary agent; the main agent contains silicate cement, redispersible latex powder, cellulose ether, and fluorosilicone oil-starch sol; Based on the total weight of the composition, the content of the silicate cement is 35-50 wt%, the content of the redispersible latex powder is 1-3 wt%, the content of the cellulose ether is 0.2-0.4 wt%, and the content of the fluorosilicone oil-starch sol is 8-12 wt%. The fluorosilicone oil-starch sol contains fluorosilicone oil, maleic anhydride-modified starch, and nano-titanium dioxide; Based on the total weight of the fluorosilicone oil-starch sol, the content of the fluorosilicone oil is 10-20 wt%, the content of the maleic anhydride-modified starch is 30-80 wt%, and the content of the nano-titanium dioxide is 20-60 wt%; the total weight of the fluorosilicone oil-starch sol is 100 wt%. The fluorosilicone oil-starch sol was prepared by a method comprising the following steps: (1) In the presence of a solvent, fluorosilicone oil is contacted with maleic anhydride modified starch to carry out an esterification reaction to obtain a crosslinked prepolymer; the kinematic viscosity of the fluorosilicone oil at 25°C is 500-10000cSt and the surface tension at 25°C is ≤30mN / m. (2) The cross-linked prepolymer is mixed with nano-titanium dioxide to obtain the fluorosilicone oil-starch sol.

2. The composition according to claim 1, characterized in that, In step (1), the solvent is a mixture of ethanol and water.

3. The composition according to claim 2, characterized in that, In step (1), the volume ratio of ethanol to water in the mixture is 1:1-5.

4. The composition according to claim 1, characterized in that, In step (1), the weight ratio of the fluorosilicone oil to the maleic anhydride modified starch is 1:1.5-5.

5. The composition according to claim 1, characterized in that, In step (1), the conditions for the esterification reaction include: a temperature of 50-70°C and a time of 1-3 hours.

6. The composition according to any one of claims 1-5, characterized in that, In step (2), the weight ratio of the crosslinked prepolymer to the nano-titanium dioxide is 1:0.2-0.

6.

7. The composition according to any one of claims 1-5, characterized in that, The average diameter of the nano-titanium dioxide is 50-100 nm.

8. The composition according to any one of claims 1-5, characterized in that, In step (2), the conditions for the mixing reaction include: a temperature of 50-60°C and a time of 5-60 min.

9. The composition according to any one of claims 1-5, characterized in that, The additives contain aggregates and fillers.

10. The composition according to claim 9, characterized in that, Based on the total weight of the composition, the content of the aggregate is 35-45 wt% and the content of the filler is 5-10 wt%.

11. The composition according to any one of claims 1-5, characterized in that, The cellulose ether is selected from at least one of hydroxyethyl methyl cellulose ether and hydroxypropyl methyl cellulose ether.

12. The composition according to claim 11, characterized in that, The hydroxypropyl methylcellulose ether is selected from at least one of low-viscosity hydroxypropyl methylcellulose ether, medium-viscosity hydroxypropyl methylcellulose ether, and high-viscosity hydroxypropyl methylcellulose ether.

13. A method for preparing tile adhesive, characterized in that, This method is carried out using any of the components in the composition according to any one of claims 1-12, comprising: Step 1: Silicate cement, aggregate, filler, cellulose ether and redispersible latex powder are mixed for the first time to obtain intermediate I; Step 2: Mix the intermediate I with the fluorosilicone oil-starch sol for the second time to obtain the encapsulated powder; Step 3: Mix the encapsulated powder with water to obtain the tile adhesive.

14. The method according to claim 13, characterized in that, In step one, the first mixing time is 1-20 minutes.

15. The method according to claim 13, characterized in that, In step two, the second mixing operation includes introducing the fluorosilicone oil-starch sol in the form of a spray to contact the intermediate I.

16. The method according to claim 13, characterized in that, In step two, the introduction flow rate of the fluorosilicone oil-starch sol is 1-2 g / min relative to 1 kg of intermediate I.

17. The tile adhesive prepared by the method according to any one of claims 13-16.

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