High-temperature-resistant and corrosion-resistant emulsion pool ceramic tile and preparation method thereof

Abstract

The invention discloses a high-temperature-resistant and corrosion-resistant emulsion pool ceramic tile and a preparation method thereof, and belongs to the technical field of ceramic tile preparation. The preparation method of the high-temperature-resistant and corrosion-resistant emulsion pool ceramic tile comprises the following steps: 1, mixing quartz sand, calcined kaolin, potassium feldspar powder, iron oxide red, titanium dioxide and a carboxymethyl cellulose aqueous solution, then adding distilled water, and carrying out granulation, compression molding and sintering to obtain a green body; 2, Portland cement and quartz sand are mixed, a silane coupling agent, a water reducing agent, lithium carbonate, a modified high-temperature-resistant additive, a composite corrosion-resistant agent and distilled water serve as raw materials, and slurry is prepared; 3, the slurry is evenly sprayed to the surface of a green body, high-temperature curing treatment is conducted, and the high-temperature-resistant and corrosion-resistant emulsion pool ceramic tile is obtained. The emulsion pool ceramic tile prepared by the method has excellent high temperature resistance and corrosion resistance.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of ceramic tile preparation, and particularly relates to a high-temperature-resistant and corrosion-resistant emulsion pool ceramic tile and a preparation method thereof. BACKGROUND

[0002] In the field of industrial production, emulsion as a high-performance metal processing fluid is widely used in the processing link of aluminum metal and its alloy. The deployment and storage of emulsion have extremely high requirements for environmental stability. However, the building materials of traditional emulsion pools often have problems such as structural failure, leakage and shortened service life when they are exposed to high temperature, strong acid and strong base and chemical corrosive media. For example, ordinary ceramic tiles are easily corroded by penetrating acid when they are in contact with warm chloride salt water, hydrochloric acid, sulfuric acid and other corrosive media, and metal materials are at risk of oxidation and contamination of the medium, especially in a high-temperature environment, the corrosion resistance of the metal material decreases significantly, and it is difficult to meet the long-term stable operation requirements of the emulsion pool. Among the existing corrosion-resistant materials, acid-resistant and temperature-resistant bricks have certain acid resistance, but their loose texture and high water absorption limit their application in high-wear and high-pressure scenarios; silicon carbide ceramics are known for their high hardness and high temperature resistance, but the high manufacturing cost and complex processing process make it difficult to be widely used in civil industrial facilities. In addition, the traditional ceramic tile back adhesive material has shortcomings in weather resistance, water resistance and bonding strength, and cannot effectively solve the problems of ceramic tile hollowing and falling off, further increasing the maintenance cost and safety hazards of the emulsion pool.

[0003] Patent CN116640007B discloses a high-temperature-resistant and corrosion-resistant flexible curved marble ceramic tile and a preparation method thereof. The curved marble ceramic tile comprises a surface glaze layer and a curved glaze layer attached to a body in sequence. The surface glaze layer comprises the following raw materials in weight parts: potassium feldspar 32-55 parts, quartz 10-15 parts, kaolin 6-10 parts, limestone 10-13 parts, wollastonite 5-10 parts, zinc oxide 1-5 parts, zirconium silicate 10-15 parts, methyl cellulose 0.15-0.25 parts, and sodium tripolyphosphate 0.25-0.45 parts. The ceramic tile prepared by the method has the advantages of high-temperature resistance, corrosion resistance, good ductility, and the glaze layer pattern texture effect changes with the bending of the ceramic tile without cracking. In the current method, the raw material ratio is optimized, but the synergistic effect of each component is not sufficient in extreme conditions. For example, some raw materials are prone to chemical reaction in high temperature or corrosive environment, which changes the original structure and weakens the overall high-temperature resistance and corrosion resistance of the ceramic tile. Therefore, it is necessary to further improve the raw material system or process to improve its performance. SUMMARY

[0004] The present application aims to provide a high-temperature-resistant and corrosion-resistant emulsion pool tile and a preparation method thereof, and aims to solve the technical problem of poor high-temperature resistance and corrosion resistance of emulsion tiles in the prior art.

[0005] In order to achieve the above-mentioned purpose, the present application adopts the following technical solutions:

[0006] The present application provides a preparation method of a high-temperature-resistant and corrosion-resistant emulsion pool tile, comprising the following steps:

[0007] Step one: mix quartz sand, calcined kaolin, potassium feldspar powder, iron oxide red, titanium dioxide and carboxymethyl cellulose aqueous solution, then add distilled water for granulation, press into shape, sinter to obtain a body;

[0008] Step two: mix Portland cement and quartz sand to obtain dry mixture, then mix and stir silane coupling agent, water reducing agent, lithium carbonate, modified high-temperature-resistant additive, composite corrosion-resistant agent and distilled water to obtain wet mixture, then add the wet mixture to the dry mixture, stir and mix, then stand for aging, then continue to stir to obtain slurry;

[0009] Step three: uniformly spray the slurry onto the surface of the body, and perform high-temperature curing treatment to obtain a high-temperature-resistant and corrosion-resistant emulsion pool tile.

[0010] As a preferred, the preparation method of the modified high-temperature-resistant additive comprises the following steps:

[0011] Q1: add 4-nitro-1,2-phenylenediamine and acetic acid to a container, add 2,2,2-trichloroacetic acid methyl ester under ice bath environment, after the addition is completed, react at room temperature, after the reaction is completed, precipitate, wash, filter, and vacuum dry to obtain intermediate 1;

[0012] Q2: add 2-amino-4-nitrophenol, intermediate 1, ethanol and triethylamine to a container, heat and stir to react, after the reaction is completed, filter, wash, recrystallize, wash, filter, and vacuum dry to obtain intermediate 2;

[0013] Q3: add intermediate 2, Pd / C and 1,4-dioxane to a container, heat and stir, then add hydrazine hydrate, after the addition is completed, incubate to react, then add N,N-dimethylformamide, heat to react, filter, wash, and vacuum dry to obtain intermediate 3;

[0014] Q4: add intermediate 3 and N-methylpyrrolidone to a container, stir at room temperature, then add diphenyl sulfide dianhydride, react under ice bath, then react at room temperature, after the reaction is completed, obtain the modified high-temperature-resistant additive.

[0015] In the above process, the synthesis reaction formula of the modified high-temperature-resistant additive is as follows:

[0016]

[0017] The results of mass spectrometric analysis of intermediate 1 are: m / z: 280.95 (100.0%), 282.95 (96.0%), 284.95 (31.1%), 283.95 (9.4%), 281.96 (8.8%), 286.94 (3.3%), 285.95 (2.7%), 281.95 (1.1%); the results of mass spectrometric analysis of intermediate 2 are: m / z: 325.04 (100.0%), 326.05 (15.4%), 327.05 (2.4%), 326.04 (1.8%); the results of mass spectrometric analysis of intermediate 3 are: m / z: 265.10 (100.0%), 266.10 (15.3%), 266.09 (1.8%), 267.10 (1.6%).

[0018] As preferred, in the Q1, the amount ratio of 4-nitro-1,2-phenylenediamine, acetic acid and methyl 2,2,2-trichloroacetimidate is (8.82-12.23) g:(100-120) mL:(11.15-13.58) g, the reaction time at room temperature is 20-24 h; in the Q2, the amount ratio of 2-amino-4-nitrophenol, intermediate 1, ethanol and triethylamine is (8.88-9.46) g:(14.38-18.86) g:(150-180) mL:(10.12-13.48) g, the heating and stirring temperature is 78-82℃, and the time is 42-50 h.

[0019] As preferred, in the Q3, the amount ratio of intermediate 2, Pd / C, 1,4-dioxane, hydrazine hydrate and N,N-dimethylformamide is (4.8-7.3) g:(0.38-0.86) g:(50-70) mL:(8.88-9.58) g:(2.6-4.2) mL, the heating and stirring temperature is 80-83℃, the time is 10-15 min, the incubation reaction temperature is 80-83℃, the time is 8-10 h, and the temperature is raised to 100-102℃ for 2-4 h; in the Q4, the amount ratio of intermediate 3, N-methylpyrrolidone and diphenyl sulfide dianhydride is (0.238-0.322) g:(1.187-1.346) g:(0.271-0.298) g, the ice bath reaction is 6-8 h, and the room temperature reaction is 10-12 h.

[0020] As preferred, the preparation method of the composite corrosion inhibitor comprises the following steps:

[0021] S1: furoin, benzaldehyde, ammonium acetate and silica gel are added into a container, after mixing, microwave treatment is carried out, after the treatment, cooling is carried out, separation and purification are carried out, rotary evaporation is carried out, drying is carried out, and organic matter a is obtained;

[0022] S2: the organic matter a is added into a container containing anhydrous tetrahydrofuran, then sodium hydroxide and chloropropene are added, and after warming and stirring, reaction is carried out, after the reaction, cooling to room temperature is carried out, washing is carried out, extraction is carried out, drying is carried out, rotary evaporation is carried out, separation and purification are carried out, rotary evaporation is carried out, drying is carried out, and organic matter b is obtained;

[0023] S3: polymethylhydrogen siloxane, organic matter b and isopropyl alcohol are added into a container, after heating and stirring, isopropyl alcohol solution of chloroplatinic acid is added, and after heating and keeping, reaction is carried out, cooling is carried out, sodium hydroxide aqueous solution is added, and rotary evaporation is carried out, and a composite corrosion inhibitor is obtained.

[0024] In the above process, the synthesis reaction formula of the composite corrosion inhibitor is as follows:

[0025]

[0026] The mass spectrum analysis result of the organic matter a is: m / z: 276.09 (100.0%), 277.09 (19.2%), 278.10 (1.6%); and the mass spectrum analysis result of the organic matter b is: m / z: 316.12 (100.0%), 317.12 (22.4%), 318.13 (2.7%).

[0027] As preferred, in the S1, the molar ratio of furoin and benzaldehyde is (0.98-1.08):(0.95-1.14), the microwave treatment temperature is 120-130℃, and the time is 5-10min; in the S2, the molar ratio of the organic matter a and chloropropene is (0.92-1.08):(0.88-1.09), the warming and stirring reaction temperature is 60-65℃, and the time is 10-12h.

[0028] As preferred, in the S3, the dosage ratio of polymethylhydrogen siloxane, organic matter b, isopropyl alcohol, isopropyl alcohol solution of chloroplatinic acid and sodium hydroxide aqueous solution is (1.42-1.58)g:(0.268-0.305)g:(20-25)mL:(0.12-0.17)mL:(0.1-0.12)mL, the heating and stirring temperature is 70-75℃, the time is 10-20min, the concentration of the isopropyl alcohol solution of chloroplatinic acid is 0.5g / L, heating to 88-90℃ for keeping for 6-8h, and the concentration of the sodium hydroxide aqueous solution is 0.002mol / L.

[0029] As preferred, in the step one, the mass ratio of the quartz sand, calcined kaolin, potassium feldspar powder, iron oxide red, titanium dioxide, carboxymethyl cellulose aqueous solution and distilled water is (50-66):(24-36):(3-9):(0.8-1.8):(0.1-0.5):(0.4-1.5):(6-12), the particle size of the quartz sand is ≤45 μm, the mass fraction of the carboxymethyl cellulose aqueous solution is 5 wt%, granulation is performed to the particle size of 0.5-1 mm, the pressure applied in the process of compression molding is 160-180 MPa, the pressure maintaining time is 30-45 s, and the sintering process is as follows:

[0030] The temperature is raised from room temperature to 300℃ at a rate of 3℃ / min, kept at 300℃ for 30 min, then raised from 300℃ to 950℃ at a rate of 5℃ / min, then raised from 950℃ to 1240℃ at a rate of 2℃ / min, kept at 1240℃ for 45 min, and then reduced to 800℃ at a rate of 5℃ / min.

[0031] As preferred, in the step two, the mass ratio of the Portland cement, quartz sand, silane coupling agent, water reducing agent, lithium carbonate, modified high-temperature-resistant additive, composite corrosion-resistant agent and distilled water is (30-35):(22-28):(1-2):(0.6-1.1):(0.5-0.9):(10-14):(12-19):(10-20); and in the step three, the high-temperature curing treatment process is as follows: maintaining at 100℃, 200℃, 300℃ and 400℃ for 1 h respectively, and the temperature rising rate is 3-5℃ / min.

[0032] A high-temperature-resistant and corrosion-resistant emulsion pool ceramic tile is prepared by the above preparation method.

[0033] As described above, due to the adoption of the above technical solutions, the present application has the following beneficial effects:

[0034] 1. The modified high-temperature-resistant additive and the composite corrosion-resistant agent prepared in the present application are added to the preparation process of the emulsion pool ceramic tile, so that the high-temperature-resistant and corrosion-resistant properties of the emulsion pool ceramic tile can be effectively improved.

[0035] 2. The modified high-temperature-resistant additive prepared in the present application is applied to the emulsion pool ceramic tile, so that the high-temperature-resistant and corrosion-resistant properties of the emulsion pool ceramic tile can be effectively improved. The high resonance energy of the rigid skeleton of the aromatic heterocyclic ring in the modified high-temperature-resistant additive can inhibit the thermal motion of the molecular chain, the flexible unit of the sulfide bond can relieve the pyrolysis stress, and the intermolecular hydrogen bond network can further improve the thermal stability. At the same time, the structure formed by the dense stacking of the aromatic ring can physically block the penetration of water molecules, the benzimidazole hydrophobic skeleton can inhibit the adsorption of the emulsion, the imidazole nitrogen atom can chelate metal ions to form a passivation layer, and the electrochemical corrosion is blocked, so that the corrosion-resistant property can be effectively improved.

[0036] 3. The prepared composite corrosion-resistant agent is applied to the emulsion pool tile, so that the corrosion resistance and thermal stability of the tile can be effectively improved. The aromatic ring structure and the siloxane network structure contained in the composite corrosion-resistant agent can effectively reduce the contact between the corrosion medium and the tile base material, thereby improving the corrosion resistance of the tile. Meanwhile, the bond energy of the polysiloxane main chain is higher than that of the carbon-carbon bond, and the three-dimensional cross-linked structure formed can effectively improve the thermal stability of the tile. DETAILED DESCRIPTION

[0037] The technical solutions in the embodiments of the present application will be described below in a clear and complete manner. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the present application.

[0038] Embodiment 1: The present embodiment discloses a preparation method of a modified high-temperature-resistant additive, comprising the following steps:

[0039] Q1: 10.52g 4-nitro-1,2-phenylenediamine and 110mL acetic acid are added to a container, 12.31g 2,2,2-trichloroacetic acid methyl ester is added under ice bath environment, after the addition is completed, room temperature reaction is carried out for 24h, after the reaction is completed, it is added to ultrapure water for precipitation, washed with ethanol, suction filtered, and vacuum dried to obtain intermediate 1;

[0040] Q2: 9.12g 2-amino-4-nitrophenol, 16.52g intermediate 1, 165mL ethanol and 11.58g triethylamine are added to a container, 80℃ heating and stirring reaction is carried out for 48h, after the reaction is completed, filtration, washing, recrystallization, washing, filtration and vacuum drying are carried out to obtain intermediate 2;

[0041] Q3: 5.8g intermediate 2, 0.52g Pd / C and 60mL 1,4-dioxane are added to a container, 80℃ heating and stirring is carried out for 15min, then 9.28g hydrazine hydrate is added, after the addition is completed, 83℃ incubation reaction is carried out for 8h, then 3.4mL N,N-dimethylformamide is added, and 100℃ reaction is carried out for 4h, filtration, washing and vacuum drying are carried out to obtain intermediate 3;

[0042] Q4: 0.275g intermediate 3 and 1.226g N-methylpyrrolidone are added to a container, after room temperature stirring, 0.285g diphenyl sulfide dianhydride is added, ice bath reaction is carried out for 6h, then room temperature reaction is carried out for 12h, after the reaction is completed, the modified high-temperature-resistant additive is obtained.

[0043] The present embodiment discloses a preparation method of a composite corrosion-resistant agent, comprising the following steps:

[0044] S1: 1.95 g of furil, 1.11 g of benzaldehyde, 4.98 g of ammonium acetate and 0.46 g of silica gel were added into a container, mixed and then subjected to microwave treatment at 130°C for 10 min, after the treatment, the mixture was cooled, separated, purified, rotary evaporated and dried to obtain organic matter a;

[0045] S2: 2.755 g of organic matter a was added into a container containing 20 mL of anhydrous tetrahydrofuran, followed by adding 0.521 g of sodium hydroxide and 0.753 g of chloropropene, and the mixture was stirred at 60°C for 12 h, after the reaction, the mixture was cooled to room temperature, washed, extracted, dried, rotary evaporated, separated and purified to obtain organic matter b;

[0046] S3: 1.5 g of polymethylhydrogenosiloxane, 0.285 g of organic matter b and 22.5 mL of isopropyl alcohol were added into a container, after stirring at 70°C for 15 min, 0.15 mL of chloroplatinic acid isopropyl alcohol solution with a concentration of 0.5 g / L was added, the mixture was heated to 90°C and reacted for 6 h, then cooled, 0.11 mL of sodium hydroxide aqueous solution with a concentration of 0.002 mol / L was added, and rotary evaporation was performed to obtain a composite corrosion-resistant agent.

[0047] The embodiment discloses a preparation method of a high-temperature-resistant and corrosion-resistant emulsion pool ceramic tile, and comprises the following steps:

[0048] Step one: 58 kg of quartz sand (particle size ≤45 μm), 30 kg of calcined kaolin, 6 kg of potassium feldspar powder, 1.3 kg of red iron oxide, 0.3 kg of titanium white powder and 0.89 kg of a carboxymethyl cellulose aqueous solution with a mass fraction of 5 wt% were mixed, then 9 kg of distilled water was added for granulation, the granulation was performed to a particle size of 1 mm, and the granulation was formed by compression at 180 MPa for 45 s, and then sintering was performed, the sintering process was as follows: the temperature was increased from room temperature to 300°C at a rate of 3°C / min, the temperature was kept at 300°C for 30 min, then the temperature was increased from 300°C to 950°C at a rate of 5°C / min, then the temperature was increased from 950°C to 1240°C at a rate of 2°C / min, the temperature was kept at 1240°C for 45 min, then the temperature was decreased to 800°C at a rate of 5°C / min, and a green body was obtained;

[0049] Step two: 32.5 kg of Portland cement and 25 kg of quartz sand were mixed to obtain dry mixture, then 1.5 kg of silane coupling agent, 0.85 kg of water reducing agent, 0.7 kg of lithium carbonate, 12 kg of modified high-temperature-resistant additive, 15.5 kg of composite corrosion-resistant agent and 15 kg of distilled water were mixed and stirred to obtain wet mixture, then the wet mixture was added into the dry mixture, after stirring and mixing, the mixture was left to stand and age, then the stirring was continued, and a slurry was obtained;

[0050] Step three: the slurry is uniformly sprayed on the surface of the body, and high-temperature curing treatment is carried out, that is, 1 h is maintained at 100℃, 200℃, 300℃ and 400℃ respectively, the temperature rising rate is 3-5℃ / min, and the emulsion pool ceramic tile with high-temperature resistance and corrosion resistance is obtained.

[0051] Example 2: The present embodiment discloses a preparation method of a modified high-temperature-resistant additive, comprising the following steps:

[0052] Q1: 8.82g 4-nitro-1,2-phenylenediamine and 120mL acetic acid are added to a container, 11.15g methyl 2,2,2-trichloroacetimidate is added under ice bath environment, after the addition is completed, room temperature reaction is carried out for 24h, after the reaction is completed, it is added to ultrapure water for precipitation, washed with ethanol, suction filtered, and vacuum dried to obtain intermediate 1;

[0053] Q2: 8.88g 2-amino-4-nitrophenol, 14.38g intermediate 1, 150mL ethanol and 10.12g triethylamine are added to a container, 80℃ heating and stirring reaction is carried out for 48h, after the reaction is completed, it is filtered, washed, recrystallized, washed, filtered and vacuum dried to obtain intermediate 2;

[0054] Q3: 4.8g intermediate 2, 0.38g Pd / C and 50mL 1,4-dioxane are added to a container, 80℃ heating and stirring is carried out for 15min, then 8.88g hydrazine hydrate is added, after the addition is completed, 83℃ incubation reaction is carried out for 8h, then 2.6mL N,N-dimethylformamide is added, the temperature is raised to 100℃ and reaction is carried out for 4h, it is filtered, washed and vacuum dried to obtain intermediate 3;

[0055] Q4: 0.238g intermediate 3 and 1.187g N-methylpyrrolidone are added to a container, after stirring at room temperature, 0.271g diphenyl sulfide dianhydride is added, ice bath reaction is carried out for 6h, then room temperature reaction is carried out for 12h, after the reaction is completed, the modified high-temperature-resistant additive is obtained.

[0056] The present embodiment discloses a preparation method of a composite corrosion-resistant agent, comprising the following steps:

[0057] S1: 1.86g furfuryl, 1.01g benzaldehyde, 4.98g ammonium acetate and 0.46g silica gel are added to a container, after mixing, 130℃ microwave treatment is carried out for 10min, after the treatment is completed, it is cooled, separated and purified, rotary evaporated and dried to obtain organic matter a;

[0058] S2: 2.539g of organic matter a was added to a container containing 20mL of anhydrous tetrahydrofuran, followed by the addition of 0.521g of sodium hydroxide and 0.673g of chloropropene, and the reaction was stirred at 60°C for 12h. After the reaction was completed, it was cooled to room temperature, washed, extracted, dried, rotary evaporated, separated and purified, rotary evaporated, and dried to obtain organic matter b;

[0059] S3: 1.42g of polymethylhydrogenosiloxane, 0.268g of organic matter b and 20mL of isopropyl alcohol were added to a container, heated and stirred at 70°C for 15min, then 0.12mL of 0.5g / L chloroplatinic acid isopropyl alcohol solution was added, heated to 90°C and reacted for 6h, cooled, added 0.1mL of 0.002mol / L sodium hydroxide aqueous solution, and rotary evaporated to obtain a composite corrosion inhibitor.

[0060] The embodiment discloses a preparation method of a high-temperature-resistant and corrosion-resistant emulsion pool ceramic tile, comprising the following steps:

[0061] Step one: 50kg of quartz sand (particle size ≤45μm), 24kg of calcined kaolin, 3kg of potassium feldspar powder, 0.8kg of red iron oxide, 0.1kg of titanium white powder and 0.4kg of 5wt% carboxymethyl cellulose aqueous solution were mixed, then 12kg of distilled water was added for granulation, the granulation was performed to a particle size of 1mm, and the granulation was pressed at 180MPa for 45s to form a body, and the body was sintered by the following process: the temperature was raised from room temperature to 300°C at a rate of 3°C / min, kept at 300°C for 30min, then the temperature was raised from 300°C to 950°C at a rate of 5°C / min, then the temperature was raised from 950°C to 1240°C at a rate of 2°C / min, kept at 1240°C for 45min, then the temperature was lowered to 800°C at a rate of 5°C / min to obtain the body;

[0062] Step two: 30kg of portland cement and 22kg of quartz sand were mixed to obtain dry mixture, then 1kg of silane coupling agent, 0.6kg of water reducing agent, 0.5kg of lithium carbonate, 10kg of modified high-temperature-resistant additive, 12kg of composite corrosion inhibitor and 10kg of distilled water were mixed and stirred to obtain wet mixture, then the wet mixture was added to the dry mixture, and after stirring and mixing, the mixture was left to stand and age, then the stirring was continued to obtain slurry;

[0063] Step three: the slurry was uniformly sprayed on the surface of the body, and high-temperature solidification treatment was performed by the following process: the temperature was maintained at 100°C, 200°C, 300°C and 400°C for 1h respectively, and the temperature raising rate was 3-5°C / min to obtain the high-temperature-resistant and corrosion-resistant emulsion pool ceramic tile.

[0064] Embodiment 3: The embodiment discloses a preparation method of a modified high-temperature-resistant additive, comprising the following steps:

[0065] Q1: 12.23g 4-nitro-1,2-phenylenediamine and 100mL acetic acid were added to a container, 13.58g methyl 2,2,2-trichloroacetimidate was added under ice bath environment, after the addition was completed, it was reacted at room temperature for 24h, after the reaction was completed, it was precipitated into ultrapure water, washed with ethanol, suction filtered, and vacuum dried to obtain intermediate 1;

[0066] Q2: 9.46g 2-amino-4-nitrophenol, 18.86g intermediate 1, 180mL ethanol and 13.48g triethylamine were added to a container, heated and stirred at 80℃ for 48h, after the reaction was completed, it was filtered, washed, recrystallized, washed, filtered, and vacuum dried to obtain intermediate 2;

[0067] Q3: 7.3g intermediate 2, 0.86g Pd / C and 70mL 1,4-dioxane were added to a container, heated and stirred at 80℃ for 15min, then 9.58g hydrazine hydrate was added, after the addition was completed, it was reacted at 83℃ for 8h, then 4.2mL N,N-dimethylformamide was added, and it was reacted at 100℃ for 4h, filtered, washed, and vacuum dried to obtain intermediate 3;

[0068] Q4: 0.322g intermediate 3 and 1.346g N-methylpyrrolidone were added to a container, after stirring at room temperature, 0.298g diphenyl sulfide dianhydride was added, it was reacted at an ice bath for 6h, and then at room temperature for 12h, after the reaction was completed, a modified high-temperature resistant additive was obtained.

[0069] The embodiment discloses a preparation method of a composite corrosion-resistant agent, comprising the following steps:

[0070] S1: 2.05g furfuryl, 1.21g benzaldehyde, 4.98g ammonium acetate and 0.46g silica gel were added to a container, mixed, treated with microwave at 130℃ for 10min, after the treatment was completed, it was cooled, separated and purified, rotary evaporated, and dried to obtain organic matter a;

[0071] S2: 2.981g organic matter a was added to a container containing 20mL anhydrous tetrahydrofuran, then 0.521g sodium hydroxide and 0.834g chloropropene were added, and it was stirred and reacted at 60℃ for 12h, after the reaction was completed, it was cooled to room temperature, washed, extracted, dried, rotary evaporated, separated and purified, rotary evaporated, and dried to obtain organic matter b;

[0072] S3: 1.58 g of polymethylhydrogen siloxane, 0.305 g of organic matter b and 25 mL of isopropyl alcohol were added into a container, after stirring at 70°C for 15 min, 0.17 mL of chloroplatinic acid isopropyl alcohol solution with a concentration of 0.5 g / L was added, heated to 90°C for 6 h, cooled, 0.12 mL of sodium hydroxide aqueous solution with a concentration of 0.002 mol / L was added, rotary evaporation was performed, and a composite corrosion inhibitor was obtained.

[0073] The embodiment discloses a preparation method of a high-temperature-resistant and corrosion-resistant emulsion pool ceramic tile, and comprises the following steps:

[0074] Step one: 66 kg of quartz sand (particle size ≤45 μm), 36 kg of calcined kaolin, 9 kg of potassium feldspar powder, 1.8 kg of red iron oxide, 0.5 kg of titanium white powder and 1.5 kg of a carboxymethyl cellulose aqueous solution with a mass fraction of 5 wt% were mixed, then 6 kg of distilled water was added for granulation, the granulation was performed to a particle size of 1 mm, and the granulation was formed by pressing at 180 MPa for 45 s, and then sintering was performed, and the sintering process was as follows: the temperature was increased from room temperature to 300°C at a temperature increasing rate of 3°C / min, the temperature was kept at 300°C for 30 min, then the temperature was increased from 300°C to 950°C at a temperature increasing rate of 5°C / min, then the temperature was increased from 950°C to 1240°C at a temperature increasing rate of 2°C / min, the temperature was kept at 1240°C for 45 min, and then the temperature was decreased to 800°C at a temperature decreasing rate of 5°C / min, and a green body was obtained;

[0075] Step two: 35 kg of silicate cement and 28 kg of quartz sand were mixed to obtain dry mixture, then 2 kg of silane coupling agent, 1.1 kg of water reducing agent, 0.9 kg of lithium carbonate, 14 kg of modified high-temperature-resistant additive, 19 kg of composite corrosion-resistant agent and 20 kg of distilled water were mixed and stirred to obtain wet mixture, then the wet mixture was added into the dry mixture, and after stirring and mixing, standing and aging were performed, and then continuous stirring was performed to obtain slurry;

[0076] Step three: the slurry was uniformly sprayed on the surface of the green body, and high-temperature curing treatment was performed, and the process was as follows: the temperature was kept at 100°C, 200°C, 300°C and 400°C for 1 h respectively, and the temperature increasing rate was 3-5°C / min, and a high-temperature-resistant and corrosion-resistant emulsion pool ceramic tile was obtained.

[0077] Embodiment 4: The embodiment discloses a preparation method of a modified high-temperature-resistant additive, and comprises the following steps:

[0078] Q1: 9.38 g of 4-nitro-1,2-phenylenediamine and 105 mL of acetic acid were added into a container, 11.87 g of 2,2,2-trichloroacetimidate was added under ice bath environment, after the addition was completed, room temperature reaction was performed for 24 h, after the reaction was completed, precipitation was performed in ultrapure water, washing was performed with ethanol, suction filtration was performed, and vacuum drying was performed to obtain intermediate 1;

[0079] Q2: 9.08g 2-amino-4-nitrophenol, 15.45g intermediate 1, 160mL ethanol and 10.97g triethylamine were added into a container, heated and stirred at 80℃ for 48h, after the reaction was completed, filtered, washed, recrystallized, washed, filtered and vacuum dried to obtain intermediate 2;

[0080] Q3: 5.2g intermediate 2, 0.47g Pd / C and 65mL 1,4-dioxane were added into a container, heated and stirred at 80℃ for 15min, then 8.99g hydrazine hydrate was added, after the addition was completed, the reaction was carried out at 83℃ for 8h, then 3.1mL N,N-dimethylformamide was added, the temperature was raised to 100℃ and the reaction was carried out for 4h, filtered, washed and vacuum dried to obtain intermediate 3;

[0081] Q4: 0.258g intermediate 3 and 1.219g N-methylpyrrolidone were added into a container, after stirring at room temperature, 0.279g diphenyl sulfide dianhydride was added, the reaction was carried out in an ice bath for 6h, then the reaction was carried out at room temperature for 12h, after the reaction was completed, the modified high-temperature resistant additive was obtained.

[0082] The embodiment discloses a preparation method of a composite corrosion-resistant agent, comprising the following steps:

[0083] S1: 1.89g furfuryl, 1.06g benzaldehyde, 4.98g ammonium acetate and 0.46g silica gel were added into a container, mixed, treated by microwave at 130℃ for 10min, after the treatment was completed, cooled, separated and purified, rotary evaporated, and dried to obtain an organic matter a;

[0084] S2: 2.687g organic matter a was added into a container containing 20mL anhydrous tetrahydrofuran, then 0.521g sodium hydroxide and 0.721g chloropropene were added, the temperature was raised to 60℃ and the reaction was carried out for 12h, after the reaction was completed, cooled to room temperature, washed, extracted, dried, rotary evaporated, separated and purified, rotary evaporated and dried to obtain an organic matter b;

[0085] S3: 1.46g polymethylhydrogenosiloxane, 0.271g organic matter b and 21mL isopropyl alcohol were added into a container, heated and stirred at 70℃ for 15min, then 0.13mL chloroplatinic acid isopropyl alcohol solution with a concentration of 0.5g / L was added, heated to 90℃ and the reaction was carried out for 6h, cooled, 0.11mL sodium hydroxide aqueous solution with a concentration of 0.002mol / L was added, and rotary evaporated to obtain a composite corrosion-resistant agent.

[0086] The embodiment discloses a preparation method of a high-temperature resistant and corrosion-resistant emulsion pool ceramic tile, comprising the following steps:

[0087] Step one: 54 kg of quartz sand (particle size ≤ 45 μm), 28 kg of calcined kaolin, 4 kg of potassium feldspar powder, 0.5 kg of red iron oxide, 0.2 kg of titanium dioxide, and 0.8 kg of a 5 wt% carboxymethyl cellulose aqueous solution were mixed, then 7 kg of distilled water was added for granulation, the particle size was 1 mm, and the granules were pressed at 180 MPa for 45 s to form, sintered, the process was: heated from room temperature to 300°C at a rate of 3°C / min, kept at 300°C for 30 min, then heated from 300°C to 950°C at a rate of 5°C / min, then heated from 950°C to 1240°C at a rate of 2°C / min, kept at 1240°C for 45 min, then cooled to 800°C at a rate of 5°C / min, to obtain a green body;

[0088] Step two: 31 kg of Portland cement and 23 kg of quartz sand were mixed to obtain a dry mixture, then 1.2 kg of silane coupling agent, 0.7 kg of water reducing agent, 0.6 kg of lithium carbonate, 11 kg of modified high-temperature resistant additive, 13 kg of composite corrosion resistant agent, and 12 kg of distilled water were mixed and stirred to obtain a wet mixture, then the wet mixture was added to the dry mixture, stirred and mixed, then allowed to stand and age, then continued to stir to obtain a slurry;

[0089] Step three: the slurry was uniformly sprayed onto the surface of the green body and high-temperature solidification treatment was performed, the process was: maintaining at 100°C, 200°C, 300°C and 400°C for 1 h respectively, the heating rate was 3-5°C / min, to obtain a high-temperature resistant and corrosion resistant emulsion pool ceramic tile.

[0090] Comparative Example 1: Comparative Example 1 is compared with Example 1, in the process of preparing the emulsion pool ceramic tile, no modified high-temperature resistant additive is added, and other conditions remain unchanged.

[0091] Comparative Example 2: Comparative Example 2 is compared with Example 1, in the process of preparing the emulsion pool ceramic tile, no composite corrosion resistant agent is added, and other conditions remain unchanged.

[0092] Performance test:

[0093] The emulsion pool ceramic tiles prepared in Examples 1-4 and Comparative Examples 1-2 were tested for performance, the heat resistance of the samples was tested according to GB / T1735-2009, and the corrosion resistance of the samples was tested according to GB / T 10125-2021, and the test results are shown in Table 1:

[0094] Table 1

[0095]

[0096] From the test results in Table 1, it can be seen that by using the method of Examples 1-4, the emulsion pool tiles prepared have excellent high-temperature resistance and corrosion resistance. From the comparison of Comparative Example 1 and Examples 1-4, it can be found that the addition of the modified high-temperature resistant additive can effectively improve the high-temperature resistance and corrosion resistance of the emulsion pool tiles. From the comparison of Comparative Example 2 and Examples 1-4, it can be found that the addition of the composite corrosion resistant agent can effectively improve the corrosion resistance and high-temperature resistance of the emulsion pool tiles.

[0097] The above description is merely preferred embodiments of the present application. The protection scope of the present application is not limited to this, and any modification or change made by those skilled in the art within the technical scope disclosed by the present application and the inventive concept should be covered within the protection scope of the present application.

[0098] The preferred embodiments of the present application disclosed above are only used to help explain the present application. The preferred embodiments do not describe all the details and do not limit the present application to the specific embodiments. Obviously, many modifications and changes can be made according to the content of the present application. The present application selects and describes these embodiments in order to better explain the principles and practical applications of the present application, so that those skilled in the art can well understand and use the present application. The present application is limited by the claims and their full scope and equivalents.

Claims

1. A method for preparing a high-temperature and corrosion-resistant emulsion pool ceramic tile, characterized in that, Includes the following steps: Step 1: Mix quartz sand, calcined kaolin, potassium feldspar powder, iron oxide red, titanium dioxide and carboxymethyl cellulose aqueous solution, then add distilled water to granulate, press into shape, sinter to obtain green body; Step 2: Mix silicate cement and quartz sand to obtain a dry mixture. Then mix and stir silane coupling agent, water-reducing agent, lithium carbonate, modified high-temperature resistant additive, composite corrosion resistant agent and distilled water to obtain a wet mixture. Then add the wet mixture to the dry mixture, stir and mix, let stand and age, and then continue stirring to obtain a slurry. Step 3: Spray the slurry evenly onto the surface of the ceramic body and cure it at high temperature to obtain high-temperature and corrosion-resistant emulsion pool ceramic tiles.

2. The method for preparing a high-temperature and corrosion-resistant emulsion pool ceramic tile according to claim 1, characterized in that, The preparation method of the modified high-temperature resistant additive, Includes the following steps: Q1: Add 4-nitro-1,2-phenylenediamine and acetic acid to a container, add methyl 2,2,2-trichloroacetylimine under ice bath conditions, and react at room temperature after the addition is complete. After the reaction is complete, precipitate, wash, filter, and vacuum dry to obtain intermediate 1. Q2: Add 2-amino-4-nitrophenol, intermediate 1, ethanol and triethylamine to a container, heat and stir to react. After the reaction is complete, filter, wash, recrystallize, wash, filter, and vacuum dry to obtain intermediate 2. Q3: Add intermediate 2, Pd / C and 1,4-dioxane to a container, heat and stir, then add hydrazine hydrate. After the addition is complete, keep the reaction at the temperature, then add N,N-dimethylformamide, heat the reaction, filter, wash, and vacuum dry to obtain intermediate 3. Q4: Add intermediate 3 and N-methylpyrrolidone to a container, stir at room temperature, add diphenyl sulfide dianhydride, react in an ice bath, then react at room temperature. After the reaction is complete, the modified high-temperature resistant additive is obtained.

3. The method for preparing a high-temperature and corrosion-resistant emulsion pool ceramic tile according to claim 2, characterized in that, In Q1, the ratio of 4-nitro-1,2-phenylenediamine, acetic acid, and methyl 2,2,2-trichloroacetylimine is (8.82-12.23) g : (100-120) mL : (11.15-13.58) g; in Q2, the ratio of 2-amino-4-nitrophenol, intermediate 1, ethanol, and triethylamine is (8.88-9.46) g : (14.38-18.86) g : (150-180) mL : (10.12-13.48) g.

4. The method for preparing a high-temperature and corrosion-resistant emulsion pool ceramic tile according to claim 2, characterized in that, In Q3, the ratio of intermediate 2, Pd / C, 1,4-dioxane, hydrazine hydrate, and N,N-dimethylformamide is (4.8-7.3) g : (0.38-0.86) g : (50-70) mL : (8.88-9.58) g : (2.6-4.2) mL; in Q4, the ratio of intermediate 3, N-methylpyrrolidone, and diphenyl sulfide dianhydride is (0.238-0.322) g : (1.187-1.346) g : (0.271-0.298) g.

5. The method for preparing a high-temperature and corrosion-resistant emulsion pool ceramic tile according to claim 1, characterized in that, The preparation method of the composite corrosion resistant agent includes the following steps: S1: Add furoyl ether, benzaldehyde, ammonium acetate and silica gel to a container, mix and microwave. After treatment, cool, separate and purify, rotary evaporate and dry to obtain organic compound a. S2: Add organic compound a to a container containing anhydrous tetrahydrofuran, then add sodium hydroxide and allyl chloride, heat and stir to react. After the reaction is complete, cool to room temperature, wash, extract, dry, rotary evaporate, separate and purify, rotary evaporate, dry to obtain organic compound b; S3: Add polymethylhydrosiloxane, organic compound b and isopropanol to a container, heat and stir, then add isopropanol chloroplatinic acid solution, heat and keep the reaction at the temperature, cool, add sodium hydroxide aqueous solution, and rotary evaporate to obtain composite corrosion resistant agent.

6. The method for preparing a high-temperature and corrosion-resistant emulsion pool ceramic tile according to claim 5, characterized in that, In S1, the molar ratio of furoyl to benzaldehyde is (0.98-1.08):(0.95-1.14); in S2, the molar ratio of organic compound a to allyl chloride is (0.92-1.08):(0.88-1.09).

7. The method for preparing a high-temperature and corrosion-resistant emulsion pool ceramic tile according to claim 5, characterized in that, In S3, the ratio of polymethylhydrosiloxane, organic compound b, isopropanol, isopropanol chloroplatinate solution, and sodium hydroxide aqueous solution is (1.42-1.58)g:(0.268-0.305)g:(20-25)mL:(0.12-0.17)mL:(0.1-0.12)mL.

8. The method for preparing a high-temperature and corrosion-resistant emulsion pool ceramic tile according to claim 1, characterized in that, In step one, the mass ratio of quartz sand, calcined kaolin, potassium feldspar powder, iron oxide red, titanium dioxide, carboxymethyl cellulose aqueous solution and distilled water is (50-66):(24-36):(3-9):(0.8-1.8):(0.1-0.5):(0.4-1.5):(6-12).

9. The method for preparing a high-temperature and corrosion-resistant emulsion pool ceramic tile according to claim 1, characterized in that, In step two, the mass ratio of silicate cement, quartz sand, silane coupling agent, water-reducing agent, lithium carbonate, modified high-temperature resistant additive, composite corrosion resistant agent and distilled water is (30-35):(22-28):(1-2):(0.6-1.1):(0.5-0.9):(10-14):(12-19):(10-20).

10. A high-temperature and corrosion-resistant ceramic tile for emulsion tanks, characterized in that, It is prepared by the preparation method according to any one of claims 1-9.

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