A lightweight, thermal insulation self-leveling floor coating
By combining modified hollow glass microspheres and heavy calcium carbonate with titanate coupling agent and dicyclohexylphosphinoethyltriethoxysilane modifier, a lightweight heat-insulating self-leveling floor coating was prepared. This solved the problem of floor coatings being prone to condensation and slipping in wet and cold seasons, improved flame retardancy and wear resistance, and enhanced heat insulation performance.
Patent Information
- Application Number
- CN202311614173.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-11-29
- Publication Date
- 2025-12-16
- Estimated Expiration
- 2043-11-29
AI Technical Summary
Existing floor coatings are prone to condensation and slipping in wet and cold seasons, have poor flame retardancy and wear resistance, and insufficient heat insulation performance.
Lightweight, heat-insulating, self-leveling floor coatings were prepared by using modified hollow glass microspheres and heavy calcium carbonate, combined with titanate coupling agents and dicyclohexylphosphinoethyltriethoxysilane modifiers. The coatings' fluidity, leveling properties, heat insulation performance, and flame retardancy were improved by optimizing the component ratio and mixing process.
It improves the anti-slip and wear resistance of floor coatings in wet and cold seasons, while also enhancing the heat insulation and flame retardancy of the coatings and reducing the thermal conductivity.
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Figure SMS_1
Abstract
Description
Technical Field
[0001] This invention relates to the field of coating technology, specifically to a lightweight, heat-insulating, self-leveling floor coating. Background Technology
[0002] Epoxy floor coatings are base decoration materials made primarily of epoxy resin, with added pigments, solvents, additives, and curing agents. They are mainly used for floor decoration and protection in factories, warehouses, underground parking lots, and other places, creating a clean and beautiful indoor environment. The material consumption of epoxy self-leveling surface coatings is generally 2 kg / mm / ㎡. In humid seasons, condensation easily forms on the surface, making the floor slippery and posing safety risks to vehicles and pedestrians.
[0003] Currently, lightweight, heat-insulating, high-temperature resistant, and airflow-resistant pigments and fillers, such as hollow glass microspheres, are often introduced to give coatings excellent flow and leveling properties, avoiding the problem of condensation and slippage on the surface of the floor coating in the wet and cold season. However, there are significant differences in the coefficient of thermal expansion and surface polarity between hollow glass microspheres and organic matrix resins, which leads to a decrease in the flame retardancy and wear resistance of floor coatings. Summary of the Invention
[0004] This invention proposes a lightweight, heat-insulating, self-leveling floor coating that solves the problems of poor flame retardancy, wear resistance, and heat insulation performance of floor coatings in related technologies.
[0005] The technical solution of the present invention is as follows:
[0006] A lightweight, heat-insulating, self-leveling floor coating, comprising component A and component B, wherein component A comprises the following components by weight: 25-30 parts epoxy resin, 3-5 parts reactive diluent, 1.5-2 parts additives, 2-5 parts pigment, 10-15 parts modified hollow glass microspheres, 20-25 parts heavy calcium carbonate, and 30-35 parts quartz powder; component B comprises an amine curing agent and an epoxy resin curing accelerator; the modified hollow glass microspheres are obtained by modification with a modifier, wherein the modifier is a titanate coupling agent and / or dicyclohexylphosphine ethyltriethoxysilane.
[0007] As a further technical solution, component B consists of 90-95 parts of amine curing agent and 5-10 parts of epoxy resin curing accelerator.
[0008] As a further technical solution, the pigment includes one or more of carbon black, phthalocyanine blue, and graphite.
[0009] As a further technical solution, the active diluent is polypropylene glycol diglycidyl ether, tripropylene glycol diacrylate, or trimethylolpropane triacrylate.
[0010] As a further technical solution, the additives include one or more of dispersants, defoamers, and leveling agents.
[0011] As a further technical solution, the mass ratio of component A to component B is 100:(15-17).
[0012] As a further technical solution, the hollow glass microspheres are composed of coarse-sized hollow glass microspheres and fine-sized hollow glass microspheres; the coarse-sized hollow glass microspheres have a particle size of 400 mesh, and the fine-sized hollow glass microspheres have a particle size of 1000 mesh.
[0013] As a further technical solution, the mass ratio of the coarse-sized hollow glass microspheres to the fine-sized hollow glass microspheres is 1-2:10.
[0014] As a further technical solution, the mass ratio of the coarse-sized hollow glass microspheres to the fine-sized hollow glass microspheres is 1.5:10.
[0015] As a further technical solution, the modifier is 2%-4% of the mass of hollow glass microspheres.
[0016] As a further technical solution, the modifier is composed of a titanate coupling agent and a dicyclohexylphosphine ethyltriethoxysilane; the mass ratio of the titanate coupling agent to the dicyclohexylphosphine ethyltriethoxysilane is 1-4:1.
[0017] As a further technical solution, the mass ratio of the titanate coupling agent to dicyclohexylphosphine ethyltriethoxysilane is 3:1.
[0018] This invention has found that when the mass ratio of titanate coupling agent to dicyclohexylphosphinoethyltriethoxysilane is 3:1, the floor coating exhibits the best oxygen index and abrasion resistance, and the lowest thermal conductivity.
[0019] As a further technical solution, the titanate coupling agent is a chelating titanate coupling agent.
[0020] As a further technical solution, the chelating titanate coupling agent is one of QX-311W titanate coupling agent and LD-311 titanate coupling agent.
[0021] As a further technical solution, the chelating titanate coupling agent is QX-311W titanate coupling agent.
[0022] As a further technical solution, the preparation method of the modified hollow glass microspheres includes the following steps:
[0023] A1. Add hollow glass microspheres to an ethanol solution and mix thoroughly to obtain a mixture;
[0024] A2. After adding a modifier to the mixture, modified hollow glass microspheres are obtained.
[0025] As a further technical solution, A1 involves adding hollow glass microspheres to an ethanol solution, mixing them thoroughly, and adjusting the pH of the solution to 3.5-4.5 to obtain a mixture.
[0026] As a further technical solution, the hollow glass microspheres in A1 are dried at 120°C for 2 hours before use.
[0027] As a further technical solution, the modification temperature in A2 is 50-60℃, and the modification time is 30-60min.
[0028] This invention also includes a method for preparing a lightweight, heat-insulating, self-leveling floor coating, comprising the following steps:
[0029] S1. Mix all components in component A thoroughly to obtain component A;
[0030] S2. After mixing all the components in component B evenly, component B is obtained;
[0031] S3. After mixing components A and B evenly, a lightweight heat-insulating self-leveling floor coating is obtained.
[0032] As a further technical solution, S1 involves mixing epoxy resin and reactive diluent for the first time, adding additives for the second mixing, then adding pigments and quartz powder for the third mixing, and finally adding modified hollow glass microspheres and heavy calcium carbonate for the fourth mixing to obtain component A.
[0033] As a further technical solution, the rotation speed of the first mixing is 500-800 rpm, and the mixing time is 5-10 min.
[0034] As a further technical solution, the rotation speed of the second mixing is 500-800 rpm, and the mixing time is 5-10 min.
[0035] As a further technical solution, the rotation speed of the third mixing is 1500-2000 rpm, and the mixing time is 30-50 min.
[0036] As a further technical solution, the rotation speed of the fourth mixing is 300-500 rpm, and the mixing time is 5-10 min.
[0037] As a further technical solution, the mixing speed in S2 is 600-800 rpm, and the mixing time is 5-10 min.
[0038] As a further technical solution, the mixing speed in S3 is 600 rpm, and the mixing time is 2-4 min.
[0039] The working principle and beneficial effects of this invention are as follows:
[0040] 1. In this invention, modified hollow glass microspheres and heavy calcium carbonate are added to the floor coating, which can give the floor coating excellent fluidity and leveling properties, achieve self-leveling at high viscosity, and give the coating heat insulation and wear resistance. It can effectively avoid the problem of condensation and slippage on the surface of the floor coating in the cold and humid season. Furthermore, the hollow glass microspheres modified by titanate coupling agent and dicyclohexylphosphine ethyltriethoxysilane can further improve the heat insulation and wear resistance of the coating and increase the flame retardancy of the coating.
[0041] 2. In this invention, the hollow glass microspheres are composed of coarse-diameter hollow glass microspheres and fine-diameter hollow glass microspheres. By using large-diameter particles, the surface area of the filler is reduced, the resin content is lowered, and a low-density floor coating is obtained, resulting in a significant increase in the coating rate. The combination of coarse-diameter hollow glass microspheres and fine-diameter hollow glass microspheres can further improve the heat insulation performance, wear resistance, and flame retardant performance of the coating. Detailed Implementation
[0042] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.
[0043] In the following embodiments and comparative examples:
[0044] The ethanol solution consists of anhydrous ethanol and distilled water in a mass ratio of 9:1.
[0045] Epoxy resin, model NPEL128, manufacturer: Nan Ya Electronic Materials (Kunshan) Co., Ltd.
[0046] Quartz powder, product number HY-G, 800 mesh, manufactured by Shenzhen Haiyang Powder Technology Co., Ltd.
[0047] Heavy calcium carbonate, 800 mesh, manufactured by Jiangxi Guangyuan Chemical Co., Ltd.
[0048] BYK-163 dispersant, manufactured by Shanghai Guangbai New Materials Co., Ltd.
[0049] BYK-A530 defoamer, manufactured by Huizhou Aike New Materials Co., Ltd.
[0050] Leveling agent 837, manufactured by Shanghai Puhao Chemical Co., Ltd.
[0051] The amine curing agent is 8125 epoxy curing agent, manufactured by Guangzhou Huabang Chemical Technology Co., Ltd.
[0052] DMP-30 epoxy resin curing accelerator was purchased from Shandong Baihong New Materials Co., Ltd.
[0053] Example 1
[0054] A lightweight, heat-insulating, self-leveling floor coating includes the following steps:
[0055] S1. After stirring 25 parts of epoxy resin and 3 parts of tripropylene glycol diacrylate at 500 rpm for 10 min, add 1.5 parts of additives and stir at 500 rpm for 10 min. Then, add 2 parts of carbon black and 30 parts of quartz powder and stir at 1500 rpm for 30 min. Finally, add 10 parts of modified hollow glass microspheres and 20 parts of heavy calcium carbonate and stir at 300 rpm for 10 min to obtain component A. The additives consist of BYK-163 dispersant, BYK-A530 defoamer and leveling agent 837 in a mass ratio of 1:1:1.
[0056] S2. Stir 95 parts of amine curing agent and 5 parts of DMP-30 epoxy resin curing accelerator at 600 rpm for 10 min to obtain component B;
[0057] S3. Mix component A and component B at 600 rpm for 5 minutes at a mass ratio of 100:15 to obtain a lightweight heat-insulating self-leveling floor coating.
[0058] The preparation method of modified hollow glass microspheres includes the following steps:
[0059] A1. Add 40g of hollow glass microspheres to 500mL of ethanol solution and mix well. Adjust the pH value to 3.5 with acetic acid to obtain a mixture. The hollow glass microspheres are dried at 120℃ for 2h before use. The hollow glass microspheres are composed of coarse-sized hollow glass microspheres (400 mesh) and fine-sized hollow glass microspheres (1000 mesh) in a mass ratio of 1:10.
[0060] A2. Add 0.4g of QX-311W titanate coupling agent and 0.4g of dicyclohexylphosphine ethyltriethoxysilane to the mixture, modify at 50℃ for 60min, filter, and dry to obtain modified hollow glass microspheres.
[0061] Example 2
[0062] S1. After stirring 25 parts of epoxy resin and 4 parts of trimethylolpropane triacrylate at 600 rpm for 8 min, add 1.8 parts of additives and stir at 600 rpm for 8 min. Then, add 3 parts of carbon black and 32 parts of quartz powder and stir at 1800 rpm for 40 min. Finally, add 13 parts of modified hollow glass microspheres and 23 parts of heavy calcium carbonate and stir at 400 rpm for 8 min to obtain component A. The additives consist of BYK-163 dispersant, BYK-A530 defoamer and leveling agent 837 in a mass ratio of 1:1:1.
[0063] S2. Stir 95 parts of amine curing agent and 5 parts of DMP-30 epoxy resin curing accelerator at 700 rpm for 8 min to obtain component B;
[0064] S3. Mix component A and component B at 600 rpm for 5 minutes at a mass ratio of 100:16 to obtain a lightweight heat-insulating self-leveling floor coating.
[0065] The preparation method of modified hollow glass microspheres includes the following steps:
[0066] A1. Add 40g of hollow glass microspheres to 500mL of ethanol solution and mix well. Adjust the pH value to 4 with acetic acid to obtain a mixture. The hollow glass microspheres are dried at 120℃ for 2h before use. The hollow glass microspheres are composed of coarse-sized hollow glass microspheres (400 mesh) and fine-sized hollow glass microspheres (1000 mesh) in a mass ratio of 1:10.
[0067] A2. Add 0.6g of QX-311W titanate coupling agent and 0.6g of dicyclohexylphosphine ethyltriethoxysilane to the mixture, modify at 55℃ for 40min, filter, and dry to obtain modified hollow glass microspheres.
[0068] Example 3
[0069] S1. After stirring 30 parts of epoxy resin and 5 parts of trimethylolpropane triacrylate at 800 rpm for 5 min, add 2 parts of additives and stir at 800 rpm for 5 min. Then, add 5 parts of carbon black and 35 parts of quartz powder and stir at 2000 rpm for 30 min. Finally, add 15 parts of modified hollow glass microspheres and 25 parts of heavy calcium carbonate and stir at 500 rpm for 5 min to obtain component A. The additives consist of BYK-163 dispersant, BYK-A530 defoamer and leveling agent 837 in a mass ratio of 1:1:1.
[0070] S2. Stir 90 parts of amine curing agent and 10 parts of DMP-30 epoxy resin curing accelerator at 800 rpm for 5 min to obtain component B;
[0071] S3. Mix component A and component B at 600 rpm for 5 minutes at a mass ratio of 100:17 to obtain a lightweight heat-insulating self-leveling floor coating.
[0072] The preparation method of modified hollow glass microspheres includes the following steps:
[0073] A1. Add 40g of hollow glass microspheres to 500mL of ethanol solution and mix well. Adjust the pH value to 4.5 with acetic acid to obtain a mixture. The hollow glass microspheres are dried at 120℃ for 2h before use. The hollow glass microspheres are composed of coarse-sized hollow glass microspheres (400 mesh) and fine-sized hollow glass microspheres (1000 mesh) in a mass ratio of 1:10.
[0074] A2. Add 0.8g of QX-311W titanate coupling agent and 0.8g of dicyclohexylphosphine ethyltriethoxysilane to the mixture, modify at 60℃ for 30min, filter, and dry to obtain modified hollow glass microspheres.
[0075] Example 4
[0076] The difference between this embodiment and Example 1 is that dicyclohexylphosphine ethyltriethoxysilane is not added.
[0077] Example 5
[0078] The difference between this embodiment and Example 1 is that QX-311W titanate coupling agent is not added.
[0079] Example 6
[0080] The difference between this embodiment and Example 1 is that 0.6g of QX-311W titanate coupling agent and 0.2g of dicyclohexylphosphine ethyltriethoxysilane are used.
[0081] Example 7
[0082] The difference between this embodiment and Example 1 is that 0.64 g of QX-311W titanate coupling agent and 0.16 g of dicyclohexylphosphine ethyltriethoxysilane are used.
[0083] Example 8
[0084] The difference between this embodiment and Embodiment 1 is that the hollow glass microspheres are composed of coarse-sized hollow glass microspheres (400 mesh) and fine-sized hollow glass microspheres (1000 mesh) with a mass ratio of 1.5:10.
[0085] Example 9
[0086] The difference between this embodiment and Embodiment 1 is that the hollow glass microspheres are composed of coarse-sized hollow glass microspheres (400 mesh) and fine-sized hollow glass microspheres (1000 mesh) in a mass ratio of 2:10.
[0087] Example 10
[0088] The difference between this embodiment and embodiment 8 is that the particle size of the fine-particle hollow glass microspheres is 1250 mesh.
[0089] Example 11
[0090] The difference between this embodiment and Example 1 is that the QX-311W titanate coupling agent is replaced with an equal amount of LD-311 titanate coupling agent.
[0091] Example 12
[0092] The difference between this embodiment and Example 1 is that the QX-311W titanate coupling agent is replaced with an equal amount of titanate coupling agent CS-101.
[0093] Comparative Example 1
[0094] A lightweight, heat-insulating, self-leveling floor coating includes the following steps:
[0095] S1. After stirring 25 parts of epoxy resin and 3 parts of tripropylene glycol diacrylate at 500 rpm for 10 min, add 1.5 parts of additives and stir at 500 rpm for 10 min. Then, add 2 parts of pigment and 30 parts of quartz powder and stir at 1500 rpm for 30 min. Finally, add 10 parts of modified hollow glass microspheres and 20 parts of heavy calcium carbonate and stir at 300 rpm for 10 min to obtain component A. The hollow glass microspheres are composed of coarse-sized hollow glass microspheres (400 mesh) and fine-sized hollow glass microspheres (1000 mesh) in a mass ratio of 1:10. The additives are composed of BYK-163 dispersant, BYK-A530 defoamer, and leveling agent 837 in a mass ratio of 1:1:1.
[0096] S2. Stir 95 parts of amine curing agent and 5 parts of DMP-30 epoxy resin curing accelerator at 600 rpm for 10 min to obtain component B;
[0097] S3. Mix component A and component B at 600 rpm for 5 minutes at a mass ratio of 100:15 to obtain a lightweight heat-insulating self-leveling floor coating.
[0098] Test case
[0099] The performance of the floor coatings in Examples 1-12 and Comparative Example 1 was determined using the following methods:
[0100] Abrasion resistance: The abrasion resistance of floor coatings was determined according to the test method in GB / T 1768-2006 "Determination of abrasion resistance of paints and varnishes - Rotating rubber grinding wheel method";
[0101] Flame retardancy: The oxygen index of the floor coating was determined according to the test method in GB / T 2406.2-2009 "Determination of flammability of plastics by oxygen index method - Part 2: Room temperature test";
[0102] Thermal insulation: The thermal conductivity of the floor coating was tested using a thermal conductivity meter at an ambient temperature of 25°C and a humidity of 55%.
[0103] The measurement results are shown in Table 1.
[0104] Table 1. Performance test results of floor coatings in Examples 1-12 and Comparative Example 1
[0105]
[0106] Compared with Example 1, the hollow glass microspheres in Comparative Example 1 were not modified. As a result, the wear resistance and oxygen index of the floor coating in Comparative Example 1 were lower than those in Example 1, while the thermal conductivity was higher than that in Example 1. This indicates that modifying the hollow glass microspheres with titanate coupling agent and / or dicyclohexylphosphine ethyltriethoxysilane can improve the wear resistance and oxygen index of the floor coating and reduce the thermal conductivity.
[0107] Compared with Example 1, Example 4 did not add dicyclohexylphosphinoethyltriethoxysilane, and Example 5 did not add titanate coupling agent. As a result, the wear resistance and oxygen index of the floor coatings in Examples 4-5 were lower than those in Example 1, while the thermal conductivity was higher than that in Example 1. This indicates that the present invention, by simultaneously adding dicyclohexylphosphinoethyltriethoxysilane and titanate coupling agent to modify hollow glass microspheres, can improve the wear resistance and oxygen index of the floor coating and reduce the thermal conductivity.
[0108] Compared with Example 1, Examples 6-7 changed the mass ratio of dicyclohexylphosphinoethyltriethoxysilane and titanate coupling agent. The results showed that the oxygen index and abrasion resistance of the floor coating in Example 6 were higher than those in Examples 1 and 7, while the thermal conductivity was lower than that in Examples 1 and 7. This indicates that when the mass ratio of titanate coupling agent to dicyclohexylphosphinoethyltriethoxysilane is 3:1, the oxygen index and abrasion resistance of the floor coating can be further improved, and the thermal conductivity can be reduced.
[0109] Compared with Example 1, Examples 8-9 changed the mass ratio of coarse-sized hollow glass microspheres to fine-sized hollow microspheres, and Example 10 changed the particle size of the fine-sized hollow microspheres. The results showed that the oxygen index and abrasion resistance of the floor coatings in Examples 1 and 10 were lower than those in Example 8, while the thermal conductivity was higher than that in Example 8. This indicates that when the mass ratio of coarse-sized hollow glass microspheres to fine-sized hollow microspheres is 1.5:10, the oxygen index and abrasion resistance of the floor coating can be further improved, and the thermal conductivity can be reduced.
[0110] Compared with Example 1, Example 11 replaced QX-311W titanate coupling agent with an equal amount of LD-311 titanate coupling agent, and Example 12 replaced QX-311W titanate coupling agent with an equal amount of titanate coupling agent CS-101. The results showed that the oxygen index and abrasion resistance of the floor coatings in Examples 11-12 were lower than those in Example 1, while the thermal conductivity was higher than that in Example 1. This indicates that adding QX-311W titanate coupling agent can further improve the oxygen index and abrasion resistance of the floor coatings and reduce the thermal conductivity.
[0111] The above are merely preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.
Claims
1. A lightweight, heat-insulating, self-leveling floor coating, characterized in that, The coating is composed of component A and component B. Component A includes the following components by weight: 25-30 parts epoxy resin, 3-5 parts reactive diluent, 1.5-2 parts additives, 2-5 parts pigment, 10-15 parts modified hollow glass microspheres, 20-25 parts heavy calcium carbonate, and 30-35 parts quartz powder. Component B is composed of an amine curing agent and an epoxy resin curing accelerator. The modified hollow glass microspheres are obtained by modification with a modifier. The hollow glass microspheres are composed of coarse-sized hollow glass microspheres and fine-sized hollow glass microspheres; the coarse-sized hollow glass microspheres have a particle size of 400 mesh, and the fine-sized hollow glass microspheres have a particle size of 1000 mesh. The mass ratio of the coarse-sized hollow glass microspheres to the fine-sized hollow glass microspheres is 1.5:10; The modifier is composed of QX-311W titanate coupling agent and dicyclohexylphosphine ethyltriethoxysilane in a mass ratio of 3:
1. The additives consist of BYK-163 dispersant, BYK-A530 defoamer, and leveling agent 837 in a mass ratio of 1:1:
1.
2. The lightweight, heat-insulating, self-leveling floor coating according to claim 1, characterized in that, The modifier is 2%-4% of the mass of the hollow glass microspheres.
3. The lightweight, heat-insulating, self-leveling floor coating according to claim 1, characterized in that, The method for preparing the modified hollow glass microspheres includes the following steps: A1. Add hollow glass microspheres to an ethanol solution and mix thoroughly to obtain a mixture; A2. After adding a modifier to the mixture, modified hollow glass microspheres are obtained.
4. The lightweight, heat-insulating, self-leveling floor coating according to claim 3, characterized in that, The modification temperature in A2 is 50-60℃, and the modification time is 30-60min.
5. The method for preparing a lightweight, heat-insulating, self-leveling floor coating according to claim 1, characterized in that, Includes the following steps: S1. Mix all components in component A thoroughly to obtain component A; S2. After mixing all the components in component B evenly, component B is obtained; S3. After mixing components A and B evenly, a lightweight heat-insulating self-leveling floor coating is obtained.
Citation Information
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Epoxy self-leveling floor coating and preparation method thereof
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