Double-effect waterproof tiling coating and preparation method thereof

Abstract

The invention discloses a double-effect waterproof tiling coating and a preparation method thereof, and belongs to the technical field of tiling coating preparation. The double-effect waterproof tiling coating is prepared from the following components in parts by weight: 30 to 40 parts of Portland cement, 20 to 30 parts of quartz sand, 8 to 15 parts of a modified waterproof agent, 1 to 2 parts of nano silicon dioxide, 5 to 12 parts of a tackifier, 0.3 to 0.6 part of hydroxypropyl methyl cellulose, 0.2 to 0.5 part of a water reducing agent, 0.1 to 0.3 part of a de-foaming agent and 0.1 to 0.2 part of a preservative. The coating prepared by the method has excellent waterproofness and adhesiveness.

Description

Technical Field

[0001] The invention belongs to the technical field of coating preparation, and particularly relates to a dual-effect waterproof tile coating and a preparation method thereof. Background Art

[0002] In the field of modern architectural decoration and renovation, tile laying is widely used for the decoration of indoor and outdoor walls, floors, and various special scenes. In traditional tile laying, the attachment of tiles mainly relies on basic materials such as cement mortar. However, with the development of the construction industry and the continuous improvement of people's requirements for building quality, traditional tile laying methods have gradually exposed many problems. On the one hand, the increasingly complex building environment, such as basements, bathrooms, kitchens, etc. in a long-term humid environment, and the need for outdoor walls to withstand the erosion of natural factors such as rain, wind and frost, has put higher requirements on the waterproof performance of tile materials. On the other hand, the continuous increase in tile specifications and the increasing diversity of materials have made the stability and durability of tiles after attachment greater challenges, and also put forward more stringent standards for the adhesion of tile materials. Therefore, dual-effect waterproof tile coatings have come into being, aiming to simultaneously solve the two key problems of waterproofing and adhesion to meet the high-quality needs of modern architectural decoration and renovation.

[0003] Patent CN111087860A discloses a flexible, multifunctional polymer cement waterproof coating and its preparation method. The waterproof coating comprises the following components: (1) liquid material: aqueous polymer benzoic acid emulsion, modified vinyl acetate-ethylene copolymer emulsion, aqueous pure acrylic emulsion, wetting dispersant, preservative, defoamer, functional thickener, and water; (2) powder material: cement. The coating prepared by this invention can improve bonding strength, prevent hollowing, and improve brick lifting. However, the waterproofness and adhesion of the coating prepared by this method still need to be improved. Summary of the Invention

[0004] The purpose of the present invention is to provide a dual-effect waterproof tile coating and a preparation method thereof, so as to solve the technical problems of poor waterproof performance and poor adhesion performance of coatings in the prior art.

[0005] In order to achieve the above object, the present invention adopts the following technical solutions: The invention provides a dual-effect waterproof tile coating, which consists of the following components in parts by weight: 30-40 parts of Portland cement, 20-30 parts of quartz sand, 8-15 parts of a modified waterproofing agent, 1-2 parts of nano-silicon dioxide, 5-12 parts of a tackifier, 0.3-0.6 parts of hydroxypropyl methylcellulose, 0.2-0.5 parts of a water reducer, 0.1-0.3 parts of a defoamer, and 0.1-0.2 parts of a preservative. The modified waterproofing agent is prepared from eugenol, epichlorohydrin, 1,1,5,5-tetramethyl-3,3-diphenyltrisiloxane, tetrafluorodibromoethane, and zinc powder as main raw materials, and the tackifier is prepared from 1,3-bis(1-isocyanato-1-methylethyl)benzene, 3-amino-1-propanol, diphenylmethane diisocyanate, polypropylene glycol, and hydroxyethyl acrylate as main raw materials.

[0006] Preferably, the preparation method of the modified waterproofing agent comprises the following steps: Q1: Eugenol was added to a container containing epichlorohydrin, followed by benzyltriethylammonium chloride. The mixture was heated and stirred under a nitrogen atmosphere. After the reaction was completed, the temperature was lowered, and then an aqueous sodium hydroxide solution was added to continue the reaction. After the reaction was completed, the reactant was added to ethyl acetate, washed, separated, and the organic phase was dried, filtered, and rotary evaporated to obtain intermediate 1. Q2: Add intermediate 1, toluene and Custer's catalyst to a container, heat under a nitrogen atmosphere, then add 1,1,5,5-tetramethyl-3,3-diphenyltrisiloxane dropwise and continue the reaction. After the reaction is complete, rotary evaporation is performed to obtain intermediate 2; Q3: Add intermediate 2, potassium hydroxide, dimethyl sulfoxide, and m-xylene to a container, heat and stir to react, reduce the vacuum, cool, then add tetrafluorodibromoethane dropwise, control the addition time, stir to react, then heat and continue to react, then add distilled water to quench the reaction, extract, wash, dry, rotary evaporate, and purify to obtain intermediate 3; Q4: Wash the zinc powder, filter it, and dry it to obtain treated zinc powder. Add anhydrous acetonitrile and the treated zinc powder into a container, then slowly dropwise add the intermediate 3, heat and reflux to react. After the reaction is completed, cool it, rotary evaporate it, and purify it to obtain a modified waterproofing agent.

[0007] In the above process, eugenol and epichlorohydrin undergo a substitution reaction under the condition of benzyltriethylammonium chloride as a catalyst to obtain intermediate 1, and then intermediate 1 undergoes an addition reaction with 1,1,5,5-tetramethyl-3,3-diphenyltrisiloxane under the condition of Custer's catalyst to obtain intermediate 2, and then intermediate 2 undergoes a ring-opening reaction and a substitution reaction with tetrafluorodibromoethane under alkaline conditions to obtain intermediate 3, and then the intermediate undergoes an elimination reaction in the presence of treated zinc powder to obtain a modified waterproofing agent.

[0008] Preferably, in Q1, the amount ratio of eugenol, epichlorohydrin, benzyltriethylammonium chloride and sodium hydroxide aqueous solution is (30-50) g: (25.36-37.94) g: (3-4.2) g: (40-60) mL, the heating and stirring reaction temperature is 100-120°C, the reaction time is 3-5 h, the temperature is lowered to 60-65°C, the mass fraction of sodium hydroxide aqueous solution is 20 wt%, the reaction time is continued for 5-7 h, the reaction is washed with saturated sodium chloride solution, and the organic phase is dried with anhydrous magnesium sulfate.

[0009] Preferably, in Q2, the amount ratio of intermediate 1, toluene, Custer's catalyst and 1,1,5,5-tetramethyl-3,3-diphenyltrisiloxane is (22.01-33.03) g: (20-30) mL: (0.46-0.53) g: (16.62-24.54) g, the temperature is raised to 100-105°C, and the reaction is continued for 20-24 hours.

[0010] Preferably, in Q3, the amount ratio of intermediate 2, potassium hydroxide, dimethyl sulfoxide, m-xylene and tetrafluorodibromoethane is (120-200) g: (40-62.3) g: (320-430) mL: (80-100) mL: (200.11-240.32) g, the temperature is raised and the stirring reaction time is 80-90 ° C, the reaction time is 70-74h, the dropwise addition time is controlled to be 4-6h, the stirring reaction time is 2-3h, the temperature is raised and the stirring reaction time is 2-3h. to 50-55°C and continue the reaction for 10-12 hours; in Q4, first wash with 20vt% hydrochloric acid 3-5 times, then wash with distilled water 3-5 times, wash with anhydrous acetone 3-5 times, and finally wash with anhydrous ether 3-5 times. The dosage ratio of anhydrous acetonitrile, treated zinc powder and intermediate 3 is (100-120) mL: (5-5.7) g: (20-23) g. The heating reflux reaction temperature is 80-90°C, and the reflux reaction time is 15-20 hours.

[0011] Preferably, the preparation method of the tackifier comprises the following steps: S1: 1,3-bis(1-isocyanato-1-methylethyl)benzene was added to N,N-dimethylformamide, and 3-amino-1-propanol was slowly added in an ice bath, and the reaction was carried out at low temperature. After the reaction was completed, the mixture was added to ethyl acetate, and a solid was precipitated, washed, and vacuum dried to obtain monomer A; S2: Add diphenylmethane diisocyanate and dibutyltin dilaurate to a container filled with ethyl acetate, heat and stir, then add polypropylene glycol dropwise, then add monomer A, heat and continue the reaction, finally add hydroxyethyl acrylate and hydroquinone monomethyl ether dropwise, continue stirring and reacting, after the reaction is completed, rotary evaporate to obtain a thickener.

[0012] In the above process, 1,3-bis(1-isocyanato-1-methylethyl)benzene reacts with 3-amino-1-propanol to synthesize monomer A containing two urea groups, diphenylmethane diisocyanate reacts with polypropylene glycol under the condition of dibutyltin dilaurate as a catalyst, monomer A serves as a chain extender, and hydroxyethyl acrylate serves as a capping agent. The monomers are added to the container and the reaction is continued to obtain a tackifier.

[0013] Preferably, in S1, the amount ratio of 1,3-bis(1-isocyanato-1-methylethyl)benzene, N,N-dimethylformamide and 3-amino-1-propanol is (10.3-14.6) g: (45-55) mL: (8.94-11.23) g, the low-temperature reaction temperature is 2-6°C, the reaction time is 6-10 h, and washing is performed with ethyl acetate.

[0014] Preferably, in S2, the usage ratio of diphenylmethane diisocyanate, dibutyltin dilaurate, ethyl acetate, polypropylene glycol, monomer A, hydroxyethyl acrylate and hydroquinone monomethyl ether is (15.23-19.12) g: (0.01-0.03) g: (30-42) mL: (13.42-16.78) g: (8.12-10.36) g: (4.12-5.34) g: (0.01-0.02) g, the heating and stirring temperature is 40-45°C, and the heating and reaction temperature is 80-85°C.

[0015] Preferably, the preparation method of the dual-effect waterproof tile coating comprises the following steps: Step 1: Stir and mix silicate cement, quartz sand, modified waterproofing agent, nano silicon dioxide, tackifier and distilled water to obtain a mixture; Step 2: While the mixture is being stirred, hydroxypropyl methylcellulose, a water reducer, a defoaming agent and a preservative are added, the mixture is continued to be mixed, and the mixture is filtered to obtain a dual-effect waterproof tile coating.

[0016] In summary, due to the adoption of the above technical solution, the beneficial effects of the present invention are: 1. The present invention first prepares a modified waterproofing agent using eugenol, epichlorohydrin, 1,1,5,5-tetramethyl-3,3-diphenyltrisiloxane, tetrafluorodibromoethane and zinc powder as main raw materials, and then prepares a tackifier using 1,3-bis(1-isocyanato-1-methylethyl)benzene, 3-amino-1-propanol, diphenylmethane diisocyanate, polypropylene glycol and hydroxyethyl acrylate as main raw materials. The modified waterproofing agent and the tackifier are added to the preparation process of the tile coating, which can effectively improve the waterproofing performance, adhesion performance and chemical corrosion resistance of the coating.

[0017] 2. The modified waterproofing agent prepared in the present invention is applied to tile coatings, which can effectively improve the waterproofness and weather resistance of the coating. The presence of silicone segments and fluorocarbon groups can significantly reduce its surface tension, increase the water contact angle, and improve the waterproofness. At the same time, silicone can resist ultraviolet degradation and temperature changes, and the chemical inertness of the fluorocarbon chain makes its coating highly tolerant to corrosive substances, thereby improving the weather resistance and chemical corrosion resistance of the coating.

[0018] 3. The present invention adds the prepared tackifier to the preparation of tile coating, which can effectively improve the adhesion of the coating. The urea group in the tackifier, as a strong polar group, can form double hydrogen bonds with the hydroxyl groups on the surface of the tile, thereby enhancing the interfacial bonding force. The tackifier interacts with the inorganic minerals through the electron cloud, generating van der Waals forces to consolidate adhesion and further enhance the adhesion ability. DETAILED DESCRIPTION

[0019] The following is a clear and complete description of the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0020] Example 1: This example discloses a method for preparing a modified waterproofing agent, comprising the following steps: Q1: 40 g of eugenol was added to a container containing 31.28 g of epichlorohydrin, followed by the addition of 3.6 g of benzyltriethylammonium chloride. The mixture was heated and stirred at 110°C under a nitrogen atmosphere for 5 h. After the reaction, the temperature was lowered to 60°C, and 50 mL of a 20 wt% aqueous sodium hydroxide solution was added. The reaction was continued for 6 h. After the reaction, the reactant was added to ethyl acetate, washed with a saturated sodium chloride solution, separated, and the organic phase was dried over anhydrous magnesium sulfate, filtered, and rotary evaporated to obtain intermediate 1. Q2: 26.13 g of intermediate 1, 25 mL of toluene, and 0.49 g of Custer's catalyst were added to a container, and the temperature was raised to 100°C under a nitrogen atmosphere. Then, 20.12 g of 1,1,5,5-tetramethyl-3,3-diphenyltrisiloxane was added dropwise. The reaction was continued for 24 h. After the reaction was completed, the mixture was rotary evaporated to obtain intermediate 2. Q3: 160 g of intermediate 2, 51.1 g of potassium hydroxide, 375 mL of dimethyl sulfoxide, and 90 mL of m-xylene were added to a container, heated to 85°C with stirring for 72 h, the vacuum degree was reduced, and the mixture was cooled. 220.24 g of tetrafluorodibromoethane was then added dropwise at a time of 4 h. The mixture was stirred for 2 h, and the temperature was then raised to 50°C and the reaction was continued for 12 h. Distilled water was then added to quench the reaction, and the mixture was extracted, washed, dried, rotary evaporated, and purified to obtain intermediate 3. Q4: Wash the zinc powder, first with 20vt% hydrochloric acid for 3 times, then with distilled water for 3 times, with anhydrous acetone for 3 times, and finally with anhydrous ether for 3 times, filter and dry to obtain treated zinc powder, add 110mL of anhydrous acetonitrile and 5.3g of treated zinc powder into the container, then slowly add 21.5g of intermediate 3 dropwise, heat under reflux at 85℃ for 16h, cool, rotary evaporate and purify to obtain the modified waterproofing agent.

[0021] This embodiment discloses a method for preparing a tackifier, comprising the following steps: S1: 12.4 g of 1,3-bis(1-isocyanato-1-methylethyl)benzene was added to 50 mL of N,N-dimethylformamide, and 10.11 g of 3-amino-1-propanol was slowly added in an ice bath. The mixture was reacted at 4°C for 8 h. After the reaction, the mixture was added to ethyl acetate, and a solid was precipitated. The solid was washed with ethyl acetate and dried in vacuo to obtain monomer A. S2: Add 17.18 g of diphenylmethane diisocyanate and 0.02 g of dibutyltin dilaurate to a container containing 36 mL of ethyl acetate, heat to 45°C and stir, then add 14.78 g of polypropylene glycol dropwise, followed by adding 9.27 g of monomer A, and continue the reaction by heating at 85°C. Finally, add 4.83 g of hydroxyethyl acrylate and 0.01 g of hydroquinone monomethyl ether dropwise, continue stirring to react, and after the reaction is completed, rotary evaporate to obtain a tackifier.

[0022] This embodiment discloses a dual-effect waterproof tile coating, which is composed of the following ingredients in parts by weight: 35 parts of Portland cement, 25 parts of quartz sand, 11.5 parts of modified waterproofing agent, 1.5 parts of nano-silicon dioxide, 8.5 parts of tackifier, 0.45 parts of hydroxypropyl methylcellulose, 0.35 parts of water reducer, 0.2 parts of defoaming agent, and 0.15 parts of preservative.

[0023] This embodiment discloses a method for preparing a dual-effect waterproof tile coating, comprising the following steps: Step 1: Stir and mix silicate cement, quartz sand, modified waterproofing agent, nano silicon dioxide, tackifier and distilled water to obtain a mixture; Step 2: While the mixture is being stirred, hydroxypropyl methylcellulose, a water reducer, a defoaming agent and a preservative are added, the mixture is continued to be mixed, and the mixture is filtered to obtain a dual-effect waterproof tile coating.

[0024] Example 2: This example discloses a method for preparing a modified waterproofing agent, comprising the following steps: Q1: 30 g of eugenol was added to a container containing 25.36 g of epichlorohydrin, followed by the addition of 4.2 g of benzyltriethylammonium chloride. The mixture was heated and stirred at 110°C under a nitrogen atmosphere for 5 h. After the reaction, the temperature was lowered to 60°C, and 40 mL of a 20 wt% aqueous sodium hydroxide solution was added. The reaction was continued for 6 h. After the reaction, the reactant was added to ethyl acetate, washed with a saturated sodium chloride solution, separated, and the organic phase was dried over anhydrous magnesium sulfate, filtered, and rotary evaporated to obtain intermediate 1. Q2: 22.01 g of intermediate 1, 30 mL of toluene, and 0.46 g of Custer's catalyst were added to a container, and the temperature was raised to 100°C under a nitrogen atmosphere. Then, 16.62 g of 1,1,5,5-tetramethyl-3,3-diphenyltrisiloxane was added dropwise. The reaction was continued for 24 h. After the reaction was completed, the mixture was rotary evaporated to obtain intermediate 2. Q3: 120 g of intermediate 2, 40.3 g of potassium hydroxide, 320 mL of dimethyl sulfoxide, and 80 mL of m-xylene were added to a container, heated to 85°C with stirring for 72 h, the vacuum degree was reduced, and the mixture was cooled. Then, 200.11 g of tetrafluorodibromoethane was added dropwise at a time of 4 h, and the mixture was stirred for 2 h. The mixture was then heated to 50°C and the reaction was continued for 12 h. Distilled water was then added to quench the reaction, and the mixture was extracted, washed, dried, rotary evaporated, and purified to obtain intermediate 3. Q4: Wash the zinc powder, first with 20vt% hydrochloric acid for 3 times, then with distilled water for 3 times, with anhydrous acetone for 3 times, and finally with anhydrous ether for 3 times, filter and dry to obtain treated zinc powder, add 100mL of anhydrous acetonitrile and 5.7g of treated zinc powder into the container, then slowly add 20g of intermediate 3 dropwise, heat under reflux at 85℃ for 16h, cool, rotary evaporate and purify to obtain the modified waterproofing agent.

[0025] This embodiment discloses a method for preparing a tackifier, comprising the following steps: S1: 10.3 g of 1,3-bis(1-isocyanato-1-methylethyl)benzene was added to 45 mL of N,N-dimethylformamide, and 8.94 g of 3-amino-1-propanol was slowly added in an ice bath. The mixture was reacted at 4°C for 8 h. After the reaction, the mixture was added to ethyl acetate, and a solid was precipitated. The solid was washed with ethyl acetate and dried in vacuo to obtain monomer A. S2: Add 15.23 g of diphenylmethane diisocyanate and 0.01 g of dibutyltin dilaurate to a container containing 30 mL of ethyl acetate, heat to 45°C and stir, then add 13.42 g of polypropylene glycol dropwise, followed by 8.12 g of monomer A, heat at 85°C and continue the reaction, finally add 4.12 g of hydroxyethyl acrylate and 0.02 g of hydroquinone monomethyl ether dropwise, continue stirring to react, and after the reaction is completed, rotary evaporate to obtain a thickener.

[0026] This embodiment discloses a dual-effect waterproof tile coating, which is composed of the following ingredients in parts by weight: 30 parts of Portland cement, 20 parts of quartz sand, 8 parts of modified waterproofing agent, 1 part of nano-silicon dioxide, 5 parts of viscosity enhancer, 0.3 parts of hydroxypropyl methylcellulose, 0.2 parts of water reducer, 0.1 parts of defoaming agent, and 0.1 parts of preservative.

[0027] This embodiment discloses a method for preparing a dual-effect waterproof tile coating, comprising the following steps: Step 1: Stir and mix silicate cement, quartz sand, modified waterproofing agent, nano silicon dioxide, tackifier and distilled water to obtain a mixture; Step 2: While the mixture is being stirred, hydroxypropyl methylcellulose, a water reducer, a defoaming agent and a preservative are added, the mixture is continued to be mixed, and the mixture is filtered to obtain a dual-effect waterproof tile coating.

[0028] Example 3: This example discloses a method for preparing a modified waterproofing agent, comprising the following steps: Q1: 50 g of eugenol was added to a container containing 37.94 g of epichlorohydrin, followed by the addition of 3 g of benzyltriethylammonium chloride. The mixture was heated and stirred at 110°C under a nitrogen atmosphere for 5 h. After the reaction, the temperature was lowered to 60°C, and 60 mL of a 20 wt% aqueous sodium hydroxide solution was added. The reaction was continued for 6 h. After the reaction, the reactant was added to ethyl acetate, washed with a saturated sodium chloride solution, separated, and the organic phase was dried over anhydrous magnesium sulfate, filtered, and rotary evaporated to obtain intermediate 1. Q2: 33.03 g of intermediate 1, 20 mL of toluene, and 0.53 g of Custer's catalyst were added to a container, and the temperature was raised to 100°C under a nitrogen atmosphere. Then, 24.54 g of 1,1,5,5-tetramethyl-3,3-diphenyltrisiloxane was added dropwise. The reaction was continued for 24 h. After the reaction was completed, the mixture was rotary evaporated to obtain intermediate 2. Q3: 200 g of intermediate 2, 62.3 g of potassium hydroxide, 430 mL of dimethyl sulfoxide, and 100 mL of m-xylene were added to a container, heated to 85°C with stirring for 72 h, the vacuum degree was reduced, and the mixture was cooled. Then, 240.32 g of tetrafluorodibromoethane was added dropwise at a time of 4 h. The mixture was stirred for 2 h, and then the temperature was raised to 50°C and the reaction was continued for 12 h. Then, distilled water was added to quench the reaction, and the mixture was extracted, washed, dried, rotary evaporated, and purified to obtain intermediate 3. Q4: Wash the zinc powder, first with 20vt% hydrochloric acid for 3 times, then with distilled water for 3 times, with anhydrous acetone for 3 times, and finally with anhydrous ether for 3 times, filter and dry to obtain treated zinc powder, add 120mL of anhydrous acetonitrile and 5g of treated zinc powder into the container, then slowly add 23g of intermediate 3 dropwise, heat under reflux at 85℃ for 16h, cool, rotary evaporate and purify to obtain the modified waterproofing agent.

[0029] This embodiment discloses a method for preparing a tackifier, comprising the following steps: S1: 14.6 g of 1,3-bis(1-isocyanato-1-methylethyl)benzene was added to 55 mL of N,N-dimethylformamide, and 11.23 g of 3-amino-1-propanol was slowly added in an ice bath. The mixture was reacted at 4°C for 8 h. After the reaction, the mixture was added to ethyl acetate, and a solid was precipitated. The solid was washed with ethyl acetate and dried in vacuo to obtain monomer A. S2: Add 19.12 g of diphenylmethane diisocyanate and 0.03 g of dibutyltin dilaurate to a container containing 42 mL of ethyl acetate, heat to 45°C and stir, then add 16.78 g of polypropylene glycol dropwise, followed by 10.36 g of monomer A, heat at 85°C and continue the reaction, finally add 5.34 g of hydroxyethyl acrylate and 0.01 g of hydroquinone monomethyl ether dropwise, continue stirring to react, and after the reaction is completed, rotary evaporate to obtain a tackifier.

[0030] This embodiment discloses a dual-effect waterproof tile coating, which is composed of the following ingredients in parts by weight: 40 parts of Portland cement, 30 parts of quartz sand, 15 parts of modified waterproofing agent, 2 parts of nano-silicon dioxide, 12 parts of viscosity enhancer, 0.6 parts of hydroxypropyl methylcellulose, 0.5 parts of water reducer, 0.3 parts of defoaming agent, and 0.2 parts of preservative.

[0031] This embodiment discloses a method for preparing a dual-effect waterproof tile coating, comprising the following steps: Step 1: Stir and mix silicate cement, quartz sand, modified waterproofing agent, nano silicon dioxide, tackifier and distilled water to obtain a mixture; Step 2: While the mixture is being stirred, hydroxypropyl methylcellulose, a water reducer, a defoaming agent and a preservative are added, the mixture is continued to be mixed, and the mixture is filtered to obtain a dual-effect waterproof tile coating.

[0032] Example 4: This example discloses a method for preparing a modified waterproofing agent, comprising the following steps: Q1: 35 g of eugenol was added to a container containing 37.12 g of epichlorohydrin, followed by the addition of 3.3 g of benzyltriethylammonium chloride. The mixture was heated and stirred at 110°C under a nitrogen atmosphere for 5 h. After the reaction, the temperature was lowered to 60°C, and 45 mL of a 20 wt% aqueous sodium hydroxide solution was added. The reaction was continued for 6 h. After the reaction, the reactant was added to ethyl acetate, washed with a saturated sodium chloride solution, separated, and the organic phase was dried over anhydrous magnesium sulfate, filtered, and rotary evaporated to obtain intermediate 1. Q2: 24.87 g of intermediate 1, 22 mL of toluene, and 0.47 g of Custer's catalyst were added to a container, and the temperature was raised to 100°C under a nitrogen atmosphere. Then, 18.23 g of 1,1,5,5-tetramethyl-3,3-diphenyltrisiloxane was added dropwise. The reaction was continued for 24 h. After the reaction was completed, the mixture was rotary evaporated to obtain intermediate 2. Q3: 140 g of intermediate 2, 45.7 g of potassium hydroxide, 350 mL of dimethyl sulfoxide, and 85 mL of m-xylene were added to a container, heated to 85°C with stirring for 72 h, the vacuum degree was reduced, and the mixture was cooled. Then, 210.17 g of tetrafluorodibromoethane was added dropwise at a time of 4 h. The mixture was stirred for 2 h, and the temperature was then raised to 50°C and the reaction was continued for 12 h. Distilled water was then added to quench the reaction, and the mixture was extracted, washed, dried, rotary evaporated, and purified to obtain intermediate 3. Q4: Wash the zinc powder, first with 20vt% hydrochloric acid for 3 times, then with distilled water for 3 times, with anhydrous acetone for 3 times, and finally with anhydrous ether for 3 times, filter and dry to obtain treated zinc powder, add 105mL of anhydrous acetonitrile and 5.1g of treated zinc powder into the container, then slowly add 21g of intermediate 3 dropwise, heat under reflux at 85℃ for 16h, cool, rotary evaporate and purify to obtain the modified waterproofing agent.

[0033] This embodiment discloses a method for preparing a tackifier, comprising the following steps: S1: 11.7 g of 1,3-bis(1-isocyanato-1-methylethyl)benzene was added to 48 mL of N,N-dimethylformamide, and 9.27 g of 3-amino-1-propanol was slowly added in an ice bath. The mixture was reacted at 4°C for 8 h. After the reaction, the mixture was added to ethyl acetate, and a solid was precipitated. The solid was washed with ethyl acetate and dried in vacuo to obtain monomer A. S2: Add 16.17 g of diphenylmethane diisocyanate and 0.02 g of dibutyltin dilaurate to a container containing 33 mL of ethyl acetate, heat to 45°C and stir, then add 13.97 g of polypropylene glycol dropwise, followed by 8.97 g of monomer A, heat at 85°C and continue the reaction, finally add 4.47 g of hydroxyethyl acrylate and 0.02 g of hydroquinone monomethyl ether dropwise, continue stirring to react, and after the reaction is completed, rotary evaporate to obtain a tackifier.

[0034] This embodiment discloses a dual-effect waterproof tile coating, which is composed of the following ingredients in parts by weight: 32 parts of Portland cement, 22 parts of quartz sand, 11 parts of modified waterproofing agent, 1.1 parts of nano-silicon dioxide, 6 parts of tackifier, 0.4 parts of hydroxypropyl methylcellulose, 0.3 parts of water reducer, 0.11 parts of defoaming agent, and 0.17 parts of preservative.

[0035] This embodiment discloses a method for preparing a dual-effect waterproof tile coating, comprising the following steps: Step 1: Stir and mix silicate cement, quartz sand, modified waterproofing agent, nano silicon dioxide, tackifier and distilled water to obtain a mixture; Step 2: While the mixture is being stirred, hydroxypropyl methylcellulose, a water reducer, a defoaming agent and a preservative are added, the mixture is continued to be mixed, and the mixture is filtered to obtain a dual-effect waterproof tile coating.

[0036] Comparative Example 1: Compared with Example 1, in the process of preparing the dual-effect waterproof tile coating in Comparative Example 1, no modified waterproofing agent is added, and other conditions remain unchanged.

[0037] Comparative Example 2: Compared with Example 1, in the process of preparing the dual-effect waterproof tile coating in Comparative Example 2, no tackifier is added, and other conditions remain unchanged.

[0038] Experimental Example: The performance of the dual-effect waterproof tile coatings prepared in Examples 1-4 and Comparative Examples 1-2 was tested. The waterproof performance, chemical corrosion resistance, and adhesion performance of the samples were tested in accordance with GB / T 23445-2009. The test results are shown in Table 1: Table 1 The test results in Table 1 show that the coatings prepared in Examples 1-4 of the present invention have excellent water resistance, chemical corrosion resistance, and adhesion properties. A comparison between Comparative Example 1 and Examples 1-4 shows that the addition of a modified water repellent can effectively improve the water resistance and chemical corrosion resistance of the coatings; a comparison between Comparative Example 2 and Examples 1-4 shows that the addition of a tackifier can effectively improve the adhesion of the coatings.

[0039] The above description is only a preferred specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any technician familiar with the technical field, within the technical scope disclosed by the present invention, who makes equivalent replacements or changes based on the technical solution and inventive concept of the present invention, should be covered by the scope of protection of the present invention.

[0040] The preferred embodiments of the present invention disclosed above are intended only to help illustrate the present invention. These preferred embodiments do not exhaustively describe all details, nor do they limit the present invention to specific embodiments. Obviously, many modifications and variations are possible based on the contents of this specification. These embodiments are selected and described in detail in this specification to better explain the principles and practical applications of the present invention, thereby enabling those skilled in the art to better understand and utilize the present invention. The present invention is limited only by the claims and their full scope and equivalents.

Claims

1. A dual-effect waterproof tile coating, characterized in that: The invention is composed of the following ingredients in parts by weight: 30-40 parts of silicate cement, 20-30 parts of quartz sand, 8-15 parts of modified waterproofing agent, 1-2 parts of nano silicon dioxide, 5-12 parts of viscosity enhancer, 0.3-0.6 parts of hydroxypropyl methylcellulose, 0.2-0.5 parts of water reducer, 0.1-0.3 parts of defoaming agent, and 0.1-0.2 parts of preservative. The modified waterproofing agent is prepared from eugenol, epichlorohydrin, 1,1,5,5-tetramethyl-3,3-diphenyltrisiloxane, tetrafluorodibromoethane and zinc powder as main raw materials, and the viscosity enhancer is prepared from 1,3-bis(1-isocyanato-1-methylethyl)benzene, 3-amino-1-propanol, diphenylmethane diisocyanate, polypropylene glycol and hydroxyethyl acrylate as main raw materials.

2. The dual-effect waterproof tile coating according to claim 1, characterized in that: The preparation method of the modified waterproofing agent comprises the following steps: Q1: Eugenol was added to a container containing epichlorohydrin, followed by benzyltriethylammonium chloride. The mixture was heated and stirred under a nitrogen atmosphere. After the reaction was completed, the temperature was lowered, and then an aqueous sodium hydroxide solution was added to continue the reaction. After the reaction was completed, the reactant was added to ethyl acetate, washed, separated, and the organic phase was dried, filtered, and rotary evaporated to obtain intermediate 1. Q2: Add intermediate 1, toluene and Custer's catalyst to a container, heat under a nitrogen atmosphere, then add 1,1,5,5-tetramethyl-3,3-diphenyltrisiloxane dropwise and continue the reaction. After the reaction is complete, rotary evaporation is performed to obtain intermediate 2; Q3: Add intermediate 2, potassium hydroxide, dimethyl sulfoxide, and m-xylene to a container, heat and stir to react, reduce the vacuum, cool, then add tetrafluorodibromoethane dropwise, control the addition time, stir to react, then heat and continue to react, then add distilled water to quench the reaction, extract, wash, dry, rotary evaporate, and purify to obtain intermediate 3; Q4: Wash the zinc powder, filter it, and dry it to obtain treated zinc powder. Add anhydrous acetonitrile and the treated zinc powder into a container, then slowly dropwise add the intermediate 3, heat and reflux to react. After the reaction is completed, cool it, rotary evaporate it, and purify it to obtain a modified waterproofing agent.

3. The dual-effect waterproof tile coating according to claim 2, characterized in that: In the Q1, the usage ratio of eugenol, epichlorohydrin, benzyltriethylammonium chloride and sodium hydroxide aqueous solution is (30-50) g: (25.36-37.94) g: (3-4.2) g: (40-60) mL.

4. The dual-effect waterproof tile coating according to claim 2, characterized in that: In Q2, the usage ratio of the intermediate 1, toluene, Custer's catalyst and 1,1,5,5-tetramethyl-3,3-diphenyltrisiloxane is (22.01-33.03) g: (20-30) mL: (0.46-0.53) g: (16.62-24.54) g.

5. The dual-effect waterproof tile coating according to claim 2, characterized in that: In the Q3, the usage ratio of intermediate 2, potassium hydroxide, dimethyl sulfoxide, m-xylene and tetrafluorodibromoethane is (120-200) g: (40-62.3) g: (320-430) mL: (80-100) mL: (200.11-240.32) g; in the Q4, the usage ratio of anhydrous acetonitrile, treated zinc powder and intermediate 3 is (100-120) mL: (5-5.7) g: (20-23) g.

6. The dual-effect waterproof tile coating according to claim 1, characterized in that: The preparation method of the tackifier comprises the following steps: S1: 1,3-bis(1-isocyanato-1-methylethyl)benzene was added to N,N-dimethylformamide, and 3-amino-1-propanol was slowly added in an ice bath, and the reaction was carried out at low temperature. After the reaction was completed, the mixture was added to ethyl acetate, and a solid was precipitated, washed, and vacuum dried to obtain monomer A; S2: Add diphenylmethane diisocyanate and dibutyltin dilaurate to a container filled with ethyl acetate, heat and stir, then add polypropylene glycol dropwise, then add monomer A, heat and continue the reaction, finally add hydroxyethyl acrylate and hydroquinone monomethyl ether dropwise, continue stirring and reacting, after the reaction is completed, rotary evaporate to obtain a thickener.

7. The dual-effect waterproof tile coating according to claim 6, characterized in that: In S1, the usage ratio of 1,3-bis(1-isocyanato-1-methylethyl)benzene, N,N-dimethylformamide and 3-amino-1-propanol is (10.3-14.6) g: (45-55) mL: (8.94-11.23) g.

8. The dual-effect waterproof tile coating according to claim 6, characterized in that: In S2, the usage ratio of diphenylmethane diisocyanate, dibutyltin dilaurate, ethyl acetate, polypropylene glycol, monomer A, hydroxyethyl acrylate and hydroquinone monomethyl ether is (15.23-19.12) g: (0.01-0.03) g: (30-42) mL: (13.42-16.78) g: (8.12-10.36) g: (4.12-5.34) g: (0.01-0.02) g.

9. A method for preparing the dual-effect waterproof tile coating according to any one of claims 1 to 8, characterized in that: The following steps are involved: Step 1: Stir and mix silicate cement, quartz sand, modified waterproofing agent, nano silicon dioxide, tackifier and distilled water to obtain a mixture; Step 2: While the mixture is being stirred, hydroxypropyl methylcellulose, a water reducer, a defoaming agent and a preservative are added, the mixture is continued to be mixed, and the mixture is filtered to obtain a dual-effect waterproof tile coating.

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