Super-hydrophobic flame-retardant insulation board and preparation method thereof

By using water-based green and environmentally friendly flame retardants and superhydrophobic aluminum trioxide nanoparticles in building insulation materials, the problems of flammable and poor fire resistance of existing building insulation materials are solved, and efficient hydrophobic, water-resistant and flame retardant properties are achieved, with the characteristics of green and environmental protection and superior performance.

CN120098519APending Publication Date: 2025-06-06QILU UNIVERSITY OF TECHNOLOGY (SHANDONG ACADEMY OF SCIENCES)
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Patent Information

Application Number
CN202411823788.6
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-12
Publication Date
2025-06-06

AI Technical Summary

Technical Problem

Existing building insulation materials have problems such as flammability, low fire safety, flame retardants pollute the environment and poor performance, especially the water resistance and mechanical properties of organic insulation materials are affected.

Method used

A superhydrophobic flame retardant insulation board is prepared by mixing and combining with aqueous resin. The method includes preparing aqueous green environmentally friendly flame retardant and superhydrophobic aluminum trioxide nanoparticles, which are then coated and sprayed onto the surface of the plate, and obtaining a functionalized thermal insulation sheet by drying.

Benefits of technology

It realizes superhydrophobic performance, excellent water resistance, self-cleaning performance and excellent flame retardant performance, making the insulation board have the characteristics of green and environmentally friendly and superior performance.

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Abstract

A preparation method of the super-hydrophobic flame-retardant insulation board comprises the following steps: preparing a water-based green environment-friendly flame-retardant coating and a super-hydrophobic coating, roll-coating the surface of the board with the flame-retardant coating, drying, spraying the surface of the board with the super-hydrophobic coating, and drying by a hot air drying furnace to obtain the green environment-friendly flame-retardant super-hydrophobic functional insulation board. The super-hydrophobic flame-retardant insulation board provided by the invention has super-hydrophobic performance, excellent water resistance and self-cleaning performance; the flame retardant property is excellent; the method takes water as a medium, and is green and environment-friendly.
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Description

Technical Field

[0001] The invention relates to a super-hydrophobic flame-retardant thermal insulation board and a preparation method thereof, and belongs to the field of functional polymers. Background Art

[0002] At present, building energy-saving technology is recognized by the international community as an important way to solve energy loss and improve environmental problems.

[0003] Building insulation materials can be divided into inorganic insulation materials and organic insulation materials. Although inorganic insulation materials have excellent fire resistance, their insulation effect is average and their bulk density is large, which increases the load on the exterior wall and has high construction requirements. In comparison, organic insulation materials have low density, light weight, good insulation effect and simple construction.

[0004] However, organic thermal insulation materials are extremely flammable, have low fire safety, and poor long-term use. In order to improve the flame retardant performance, flame retardants are added to thermal insulation materials, mainly including brominated flame retardants and melamine intumescent flame retardants. However, there are problems such as brominated flame retardants polluting the environment; melamine intumescent flame retardants are added in large amounts, are easy to absorb water, and have poor compatibility with matrix materials, which seriously affect the water resistance and mechanical properties of the materials.

[0005] Patent "202210649816.1" discloses a method for preparing a self-hydrophobic insulation board surface layer, which uses nanocellulose powder to make a nanocellulose suspension and uses a solid-gas phase separation method to provide a super-hydrophobic structure. It has the advantages of being green and environmentally friendly, highly hydrophobic, durable, and low energy consumption. However, nanocellulose is flammable, which affects the flame retardant properties of the insulation board.

[0006] Patent "202410496734.7" discloses a method for preparing a high-strength heat-insulating and fire-proof composite insulation board, which relates to the technical field of composite insulation boards, specifically a method for preparing a high-strength heat-insulating and fire-proof composite insulation board, including a main insulation board and a covering material. The high-strength heat-insulating and fire-proof composite insulation board preparation method produces a composite building insulation board with high compressive strength and good thermal insulation performance, and the original insulation board has ultra-low thermal conductivity, flame retardant and good insulation effect. However, the insulation board has poor waterproof ability. Summary of the invention

[0007] In view of the above problems, the present invention provides a super hydrophobic flame retardant thermal insulation board and a preparation method thereof.

[0008] The technical solution of the present invention is as follows:

[0009] (1) Preparation of water-based green flame retardant

[0010] 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO), ethanol and silane coupling agent are mixed, washed and dried to obtain a transparent yellow viscous product, ammonium polyphosphate is added, nitrogen is passed, the temperature is raised to react, and a solid product is dried. The solid product is dissolved in water to obtain a water-based green flame retardant.

[0011] (2) Preparation of super hydrophobic coating

[0012] Nano-aluminum oxide is dispersed in a mixture of ethanol, water and a fluorine-containing silane coupling agent to obtain super-hydrophobic aluminum oxide nanoparticles, which are then dispersed in a water-based resin to obtain a water-based super-hydrophobic coating.

[0013] (3) Preparation of super hydrophobic flame retardant insulation board

[0014] The flame retardant coating of step (1) is rolled on the surface of the board, and after drying, the super hydrophobic coating of step (2) is sprayed on the surface of the board, and dried in a hot air drying furnace to obtain a green and environmentally friendly flame retardant super hydrophobic functional insulation board.

[0015] Preferably, in step (1), the mass ratio of DOPO, ethanol and silane coupling agent is (1-200): (1-200): 1; the mass ratio of DOPO: ammonium polyphosphate is 1: (0.01-100).

[0016] Preferably, according to the present invention, in step (1), the reaction temperature is 70 to 200° C., the reaction time is 1 to 12 hours, and the drying time is 1 to 24 hours.

[0017] Preferably according to the present invention, in step (1), the mass ratio of solid product: water is (0.01-1):1.

[0018] Preferably, according to the present invention, in step (2), the mass ratio of ethanol, water and fluorine-containing silane coupling agent is (1-200): (1-200): 1; the mass ratio of aluminum oxide to the mixed liquid is 1: (1-500); and the mass ratio of superhydrophobic aluminum oxide nanoparticles to the emulsion is 1: (1-500).

[0019] Preferably according to the present invention, in step (2), the water-based resin is epoxy resin, amino resin, polyurethane or the like.

[0020] Preferably according to the present invention, in step (3), the drying temperature after spraying the super-hydrophobic coating is 60-200°C.

[0021] Compared with the prior art, the present invention has the following beneficial effects: the super-hydrophobic flame-retardant insulation board provided by the present invention has super-hydrophobic properties, excellent water resistance, and self-cleaning properties; the super-hydrophobic aluminum oxide nanoparticles not only play a super-hydrophobic role, but also have a synergistic effect with water-based green and environmentally friendly flame retardants, so that the insulation board has outstanding flame retardant properties; water-based, green, and environmentally friendly. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 Contact angle of super hydrophobic flame retardant insulation board DETAILED DESCRIPTION

[0023] Hereinafter, the present invention will be described in detail. Before describing, it should be understood that the terms used in this specification and the appended claims should not be interpreted as being limited to the general meaning and dictionary meaning, but should be interpreted according to the meaning and concept corresponding to the technical aspects of the present invention on the basis of the principle that the inventor is allowed to appropriately define the terms for the best interpretation. Therefore, the descriptions presented here are only preferred examples for illustrative purposes and are not intended to limit the scope of the present invention, so that it should be understood that other equivalents or improvements can be obtained therefrom without departing from the spirit and scope of the present invention.

[0024] The following examples are only listed as examples of embodiments of the present invention and do not constitute any limitation to the present invention. It can be understood by those skilled in the art that modifications within the scope of the essence and concept of the present invention fall within the scope of protection of the present invention. Unless otherwise specified, the reagents and instruments used in the following examples are all commercially available products.

[0025] Example 1

[0026] A super hydrophobic flame retardant insulation board, the preparation method of which is as follows:

[0027] (1) Preparation of water-based green flame retardant

[0028] 2g 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO), 1g ethanol and 1g silane coupling agent were mixed for 12h, washed and dried to obtain a transparent yellow viscous product. 2g ammonium polyphosphate was mixed with the above product, nitrogen was passed through, 120℃ for 4h, and dried at 130℃ for 4h to obtain a solid product. 1g of the solid product was dissolved in 10g water to obtain a nitrogen-silicon-phosphorus environmentally friendly flame retardant.

[0029] (2) Preparation of superhydrophobic materials

[0030] 5g of nano-aluminum trioxide was dispersed in a solution of 30g of ethanol, 20g of water and 1g of a fluorinated silane coupling agent, and reacted at 80°C for 24h to obtain super-hydrophobic aluminum trioxide nanoparticles. 1g of super-hydrophobic aluminum trioxide nanoparticles was dispersed in 10g of waterborne polyurethane to obtain a waterborne super-hydrophobic coating.

[0031] (3) Preparation of super hydrophobic flame retardant insulation board

[0032] The coating machine rolls the flame retardant coating on the surface of the board once, and then dries it in a folding furnace at 100°C. Then the super hydrophobic coating is sprayed on the surface of the board once, and then dried in a hot air drying furnace at 100°C to obtain a green, flame retardant, super hydrophobic functional insulation board.

[0033] Example 2

[0034] A super hydrophobic flame retardant insulation board, the preparation method of which is as follows:

[0035] (1) Preparation of water-based green flame retardant

[0036] 2g 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO), 1g ethanol and 1g silane coupling agent were mixed for 12h, washed and dried to obtain a transparent yellow viscous product. 2g ammonium polyphosphate was mixed with the above product, nitrogen was passed through, 110℃ for 4h, and dried at 140℃ for 4h to obtain a solid product. 1g of the solid product was dissolved in 10g water to obtain a nitrogen-silicon-phosphorus environmentally friendly flame retardant.

[0037] (2) Preparation of superhydrophobic materials

[0038] 5g of nano-aluminum oxide was dispersed in a solution of 30g of ethanol, 20g of water and 1g of a fluorinated silane coupling agent, and reacted at 80°C for 24h to obtain super-hydrophobic aluminum oxide nanoparticles. 1.5g of super-hydrophobic aluminum oxide nanoparticles was dispersed in 10g of waterborne polyurethane to obtain a waterborne super-hydrophobic coating.

[0039] (3) Preparation of super hydrophobic flame retardant insulation board

[0040] The coating machine rolls the flame retardant coating on the surface of the board once, and then dries it in a folding furnace at 100°C. Then the super hydrophobic coating is sprayed on the surface of the board once, and then dried in a hot air drying furnace at 100°C to obtain a green, flame retardant, super hydrophobic functional insulation board.

[0041] Example 3

[0042] A super hydrophobic flame retardant insulation board, the preparation method of which is as follows:

[0043] (1) Preparation of water-based green flame retardant

[0044] 2.5g 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO), 1g ethanol and 1g silane coupling agent were mixed for 12h, washed and dried to obtain a transparent yellow viscous product. 2g ammonium polyphosphate was mixed with the above product, nitrogen was passed through, 120℃ for 4h, and dried at 130℃ for 4h to obtain a solid product. The 2g solid product was dissolved in 10g water to obtain a nitrogen-silicon-phosphorus environmentally friendly flame retardant.

[0045] (2) Preparation of superhydrophobic materials

[0046] 4g of nano-aluminum trioxide was dispersed in a solution of 30g of ethanol, 20g of water and 1g of a fluorinated silane coupling agent, and reacted at 80°C for 24h to obtain super-hydrophobic aluminum trioxide nanoparticles. 1g of super-hydrophobic aluminum trioxide nanoparticles was dispersed in 10g of waterborne polyurethane to obtain a waterborne super-hydrophobic coating.

[0047] (3) Preparation of super hydrophobic flame retardant insulation board

[0048] The coating machine rolls the flame retardant coating on the surface of the board once, and then dries it in a folding furnace at 100°C. Then the super hydrophobic coating is sprayed on the surface of the board once, and then dried in a hot air drying furnace at 100°C to obtain a green, flame retardant, super hydrophobic functional insulation board.

[0049] Comparative Example 1

[0050] A flame retardant heat-insulating board, which differs from Example 1 in that no super-hydrophobic aluminum oxide nanoparticles are added, and the preparation method thereof is as follows:

[0051] (1) Preparation of water-based green flame retardant

[0052] 2g 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO), 1g ethanol and 1g silane coupling agent were mixed for 12h, washed and dried to obtain a transparent yellow viscous product. 2g ammonium polyphosphate was mixed with the above product, nitrogen was passed through, 120℃ for 4h, and dried at 130℃ for 4h to obtain a solid product. 1g of the solid product was dissolved in 10g water to obtain a nitrogen-silicon-phosphorus environmentally friendly flame retardant.

[0053] (2) Preparation of flame retardant insulation board

[0054] The coating machine rolls the flame retardant coating on the surface of the board once, and then dries it in a folding furnace at 100°C. It is dried in a hot air drying furnace at 100°C to obtain a green, environmentally friendly, flame retardant functional insulation board.

[0055] Comparative Example 2

[0056] A super hydrophobic flame retardant insulation board, the preparation method of which is as follows:

[0057] (1) Preparation of superhydrophobic materials

[0058] 5g of nano-aluminum trioxide was dispersed in a solution of 30g of ethanol, 20g of water and 1g of a fluorinated silane coupling agent, and reacted at 80°C for 24h to obtain super-hydrophobic aluminum trioxide nanoparticles. 1g of super-hydrophobic aluminum trioxide nanoparticles was dispersed in 10g of waterborne polyurethane to obtain a waterborne super-hydrophobic coating.

[0059] (2) Preparation of super hydrophobic flame retardant insulation board

[0060] The surface of the board is sprayed with a super-hydrophobic coating once, and then dried in a hot air drying furnace at 100° C. to obtain a green, flame-retardant, super-hydrophobic functional insulation board.

[0061] Results test:

[0062] 1. Test of thermal insulation effect

[0063] The thermal conductivity coefficients of Examples 1, 2, and 3 are 0.032, 0.041, and 0.033 W / (m·K), respectively, and have good thermal insulation properties.

[0064] 2. Test of hydrophobic effect

[0065] The contact angle of the insulation board in Example 1 is 151°, the contact angle in Example 2 is 152°, and the contact angle in Example 3 is 150°, which has good hydrophobicity. The contact angle in Comparative Example 1 is 90°, and the contact angle in Comparative Example 2 is 150°.

[0066] 3. Flame retardant effect test

[0067] The flame retardant grade of the insulation board of Example 1 is A2, the flame retardant grade of the insulation board of Example 2 is A2, and the flame retardant grade of the insulation board of Example 3 is A2. The flame retardant grade of the insulation board of Comparative Example 1 is B1, and the flame retardant grade of the insulation board of Comparative Example 2 is B2, indicating that the super-hydrophobic aluminum oxide nanoparticles not only play a hydrophobic role, but also have a synergistic flame retardant effect with the water-based environmentally friendly flame retardant.

Claims

1. A method for preparing a super hydrophobic flame retardant thermal insulation board, comprising the following steps: (1) Preparation of water-based green flame retardant 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO), ethanol and silane coupling agent are mixed, washed and dried to obtain a transparent yellow viscous product, ammonium polyphosphate is added, nitrogen is passed, the temperature is raised to react, and a solid product is dried. The solid product is dissolved in water to obtain a water-based green flame retardant. (2) Preparation of super hydrophobic coating Nano-aluminum oxide is dispersed in a mixture of ethanol, water and a silane coupling agent to react and obtain super-hydrophobic aluminum oxide nanoparticles, which are then dispersed in a water-based resin to obtain a water-based super-hydrophobic coating. (3) Preparation of super hydrophobic flame retardant insulation board The flame retardant coating of step (1) is rolled on the surface of the board, and after drying, the super hydrophobic coating of step (2) is sprayed on the surface of the board, and dried in a hot air drying furnace to obtain a green and environmentally friendly flame retardant super hydrophobic functional insulation board.

2. The method according to claim 1, characterized in that In step (1), the mass ratio of DOPO, ethanol and silane coupling agent is (1-200): (1-200): 1; The mass ratio of DOPO: ammonium polyphosphate is 1:(0.01-100).

3. The method according to claim 1, characterized in that In step (1), the reaction temperature is 70 to 200° C., the reaction time is 1 to 12 hours, and the drying time is 1 to 24 hours.

4. The method according to claim 1, characterized in that In step (1), the mass ratio of solid product to water is (0.01-1):

1.

5. The method according to claim 1, characterized in that In step (2), the mass ratio of ethanol, water and silane coupling agent is (1-200): (1-200): 1; the mass ratio of aluminum oxide to the mixed solution is 1: (1-500); and the mass ratio of superhydrophobic aluminum oxide nanoparticles to the emulsion is 1: (1-500).

6. The method according to claim 1, characterized in that In step (2), the water-based resin is epoxy resin, amino resin, polyurethane, etc.

7. The method according to claim 1, characterized in that In step (3), the drying temperature after spraying the flame retardant coating is 60-200°C.

Citation Information

Patent Citations

  • Preparation method of self-hydrophobic insulation board surface layer

    CN114989690A

  • Preparation method of high-strength heat-insulation fireproof composite insulation board

    CN118342862A