Production method of polymer aerogel thermal insulation aluminum-based decorative plate

Abstract

The application provides a production method of a high-molecular aerogel heat-insulating aluminum-based decorative plate, and belongs to the technical field of heat-insulating decorative plates.The disclosed production method of the high-molecular aerogel heat-insulating aluminum-based decorative plate adopts pre-crosslinking epoxy resin gel for crosslinking and foaming, mixes with polyurethane emulsion to obtain a milky gel material, fills silica aerogel, and then adopts aluminum-based decorative plate composite molding to trim the aluminum plate, naturally air-dries the aluminum plate to constant weight, and finally obtains the high-molecular aerogel heat-insulating aluminum-based decorative plate.The prepared aerogel heat-insulating aluminum-based decorative plate has improved mechanical properties, a relatively short preparation period, can maintain the integrity of the aerogel skeleton structure, improves the high brittleness of the aerogel, and finally obtains a decorative plate material with low thermal conductivity and A2-grade fireproof property.

Description

Technical Field

[0001] This invention belongs to the technical field of thermal insulation decorative panels, specifically relating to a production method of a polymer aerogel thermal insulation aluminum-based decorative panel. Background Technology

[0002] With the continuous expansion and deepening of research on aerogel materials, the structure and types of aerogels have been continuously improved. Based on their composition, aerogel materials can be broadly classified into: oxide aerogels, carbide aerogels, nitride aerogels, organic aerogels, and composite aerogels. For example, organic aerogels include formaldehyde, polyurethane, and polystyrene; carbon aerogels include carbon, carbon nanotubes, and graphene; semiconductor chalcogenide aerogels include CdS, PbTe, and CdSe; and natural gas aerogels include cellulose and other polysaccharide compounds and proteins. CN201610214851.5 discloses an aerogel thermal insulation and fireproof board with a decorative surface and its preparation method. Aerogel is a solid material with excellent thermal insulation properties, possessing a unique microstructure such as high specific surface area, nanoscale pores, and low density. Therefore, it exhibits excellent performance in thermal insulation, adsorption separation, biomedicine, photocatalysis, energy storage and conversion, and sound absorption and insulation. Aerogel is a nanomaterial with a unique structure and many special physical and chemical properties, showing promising applications in numerous fields and possessing great development potential and research value. The preparation of polymeric aerogels involves the use of many toxic solvents, and the resulting pollution makes large-scale production of polymeric organic aerogels difficult. However, the social and economic impact of aerogels has become increasingly apparent in recent years. Despite breakthroughs, aerogels suffer from low strength and fragility, and their processing, molding, and application still face challenges. Current research on aerogel materials mainly focuses on upgrading preparation processes, with insufficient in-depth research into the synthesis mechanisms. Therefore, it is necessary to strengthen the in-depth study of the formation mechanisms of aerogel materials at the molecular and atomic levels to further optimize and control their properties. However, aerogels have poor mechanical properties, making pure aerogel materials unsuitable for use as wall materials or for use alone on the inner and outer surfaces of walls. Furthermore, the high cost and difficult construction of aerogels currently limit their large-scale application. Research is needed to develop lower-cost precursors, combined with lower-cost drying processes, to further reduce the preparation cost of aerogel materials, promote large-scale production, and enable aerogel materials to be more widely used in more fields, creating greater social and economic value. Composite aerogels refer to aerogels that use other materials to combine with a certain aerogel matrix, overcoming some of the shortcomings of the aerogel matrix to obtain aerogels with enhanced performance and specific functions. Therefore, those skilled in the art urgently need to develop a production method for polymer aerogel thermal insulation aluminum-based decorative panels to overcome the deficiencies of existing technologies and thus meet current market demands and performance requirements. Summary of the Invention

[0003] In view of the shortcomings of the prior art, the main objective of the present invention is to provide a method for producing a polymer aerogel thermal insulation aluminum-based decorative panel.

[0004] To achieve the above objectives, the present invention adopts the following technical solution:

[0005] A method for producing a polymer aerogel thermal insulation aluminum-based decorative panel includes the following steps: Step 1, preparation of pre-crosslinked epoxy resin gel: 100-110 parts of 0.2 mol / L sodium hydroxide solution, 3-5 parts of diethylenetriamine, 45-53 parts of epoxy resin, and 0.2-0.3 parts of sodium stearate are added to a reactor equipped with a stirrer and a reflux condenser. The mixture is stirred at 500-600 rpm and reacted at 90-110℃ for 10-15 minutes, followed by filtration to obtain the pre-crosslinked epoxy resin gel; Step 2, emulsion gel-sol reaction: The crosslinking foaming agent, the pre-crosslinked epoxy resin gel, and the polyurethane emulsion are mixed in a certain proportion, and then 5-15% (by weight of epoxy resin) of carbon dioxide is added. The silica aerogel is stirred at 1000-1500 rpm for 5-10 minutes and then at 2000-3000 rpm for 10-15 minutes to obtain an emulsion gel material. The third step is the composite molding of the aluminum-based decorative panel: a flat vulcanizing machine is used. An aluminum substrate is placed on the lower heating plate of the machine, and a shim frame is placed on top. The emulsion gel material is injected into the shim frame, and then another aluminum substrate is covered on top of the emulsion foam material. The composite molding process conditions are: pressure 0.2-0.6 MPa, temperature 120-135℃, and time 5-10 minutes. After this, the aluminum plate is removed, trimmed, and naturally air-dried to a constant weight to obtain the polymer aerogel thermal insulation aluminum-based decorative panel.

[0006] Furthermore, the mass ratio of the crosslinking foaming agent, the pre-crosslinked epoxy resin gel, and the polyurethane emulsion is 1~2:11~13:15~17.

[0007] Furthermore, the crosslinking foaming agent is N-aminoethylpiperazine dissolved in anhydrous ethanol to prepare a solution with a mass fraction of 10-15%, which is placed in a reaction vessel. Then, carbon dioxide gas is introduced into the reaction vessel at a flow rate of 25-30 mL / min. After reacting for 10-15 min, the precipitate is obtained by filtration.

[0008] Furthermore, the polyurethane emulsion in the second step is a blocked anionic polyurethane emulsion with an NCO content of 3.5%~5% and a solid content of 15%~20%.

[0009] Furthermore, the silica aerogel in the second step is an amino-modified silica aerogel.

[0010] Furthermore, the aluminum substrate in the third step is one of the aluminum alloy plates selected from 1100, 3003, 3004, and 5052.

[0011] This invention discloses a method for producing polymer aerogel insulated aluminum-based decorative panels. The method involves cross-linking and foaming a pre-crosslinked epoxy resin gel, mixing it with a polyurethane emulsion to obtain an emulsion-like gel material, filling it with silica aerogel, and then molding it using an aluminum-based decorative panel. The aluminum panel is then trimmed and naturally air-dried to a constant weight to obtain the polymer aerogel insulated aluminum-based decorative panel. Using epoxy resin polymer cross-linked foamed gel as a framework, the mechanical properties of the prepared aerogel insulated aluminum-based decorative panel are improved, and the preparation cycle is relatively short. It maintains the integrity of the aerogel framework structure, overcomes the high brittleness of aerogel, and yields a decorative panel with low thermal conductivity and A2 fire resistance. Detailed Implementation

[0012] The present invention will be further described in detail below with reference to embodiments, but the implementation of the present invention is not limited thereto. Example 1

[0013] Raw materials: silica aerogel TLS-F04, Jiaxing Zhengda E-51 epoxy resin, Deyang 99.9% carbon dioxide, Linghu Xinwang sodium stearate, 1100 aluminum alloy H16 0.4mm thick plate from Liuan Qianghuang Aluminum Company, and CNOOC Changzhou polyurethane emulsion, which is a closed anionic polyurethane emulsion with an NCO content of 3.5%.

[0014] The production method of polymer aerogel thermal insulation aluminum-based decorative panel includes the following steps: Step 1, preparation of pre-crosslinked epoxy resin gel: 110 parts of 0.2 mol / L sodium hydroxide solution, 5 parts of diethylenetriamine, 53 parts of epoxy resin and 0.3 parts of sodium stearate are added to a reactor equipped with a stirrer and a reflux condenser. The mixture is stirred at 600 rpm and reacted at 110℃ for 15 min. After filtration, the pre-crosslinked epoxy resin gel is obtained. Step 2, emulsion gel-sol reaction: The silica aerogel is an amino-modified silica aerogel. The silica aerogel is added to xylene with a volume of 3 times its volume, and then transferred to a reactor. 3% KH550 by weight of the silica aerogel is added. The mixture is heated to reflux at 60℃ for 24 h under a nitrogen atmosphere, centrifuged, washed with xylene and ethanol, and dried to constant weight. The mass ratio of crosslinking foaming agent, pre-crosslinked epoxy resin gel and polyurethane emulsion is 2:13:17. The crosslinking foaming agent and pre-crosslinked epoxy resin gel are mixed and then... The adhesive and polyurethane emulsion are mixed, and then 15% (by weight) of epoxy resin and silica aerogel are added. The mixture is stirred at 1500 rpm for 10 min and then at 3000 rpm for 5 min to obtain an emulsion gel material. The crosslinking foaming agent is N-aminoethylpiperazine dissolved in anhydrous ethanol to prepare a 15% (by weight) solution, which is placed in a reaction vessel. Then, carbon dioxide gas is introduced into the reaction vessel at a flow rate of 30 mL / min. After reacting for 15 min, the mixture is filtered and precipitated to obtain the final product. The third step is the composite molding of aluminum-based decorative panels: a flat vulcanizing machine is used for the composite molding. An aluminum substrate is placed on the lower heating plate of the flat vulcanizing machine, and a shim frame is placed on the aluminum substrate. The emulsion gel material is injected into the shim frame, and another aluminum substrate is covered on the emulsion foam material. The composite molding process conditions are: pressure 0.6 MPa, temperature 135℃, time 10 min. After that, the aluminum plate is removed, trimmed, and naturally air-dried to constant weight to obtain a polymer aerogel thermal insulation aluminum-based decorative panel. Example 2

[0015] Raw materials: Silica aerogel (multi-dimensional type A), Kleis E-52-D epoxy resin, Aoke Chemical Industry carbon dioxide, Linzi Luwei sodium stearate, Qianghuang 3003 aluminum alloy H44 1mm thick plate, and Haiyou Changzhou polyurethane emulsion, which is a closed anionic polyurethane emulsion with an NCO content of 3.5%.

[0016] The production method of polymer aerogel thermal insulation aluminum-based decorative panel includes the following steps: Step 1, preparation of pre-crosslinked epoxy resin gel: 100 parts of 0.2 mol / L sodium hydroxide solution, 3 parts of diethylenetriamine, 45 parts of epoxy resin and 0.2 parts of sodium stearate are added to a reactor equipped with a stirrer and a reflux condenser. The mixture is stirred at 600 rpm and reacted at 90℃ for 10 min. After filtration, the pre-crosslinked epoxy resin gel is obtained. Step 2, emulsion gel-sol reaction: The silica aerogel is an amino-modified silica aerogel. The silica aerogel is added to xylene with a volume of 3 times its volume, and then transferred to a reactor. 3% KH550 by weight of the silica aerogel is added. The mixture is heated to reflux at 60℃ for 24 h under a nitrogen atmosphere, centrifuged, washed with xylene and ethanol, and dried to constant weight. The mass ratio of crosslinking foaming agent, pre-crosslinked epoxy resin gel and polyurethane emulsion is 1:11:15. The crosslinking foaming agent and pre-crosslinked epoxy resin gel are mixed... The mixture is made by mixing polyurethane emulsion with epoxy resin and adding 5% (by weight) silica aerogel. The mixture is stirred at 1000 rpm for 5 minutes and then at 2000 rpm for 10 minutes to obtain an emulsion gel. The crosslinking foaming agent is N-aminoethylpiperazine dissolved in anhydrous ethanol to prepare a 10% (by weight) solution, which is placed in a reaction vessel. Carbon dioxide gas is then introduced into the reaction vessel at a flow rate of 25-30 mL / min. After reacting for 10 minutes, the mixture is filtered to obtain the precipitate. The third step is the composite molding of aluminum-based decorative panels: A flat vulcanizing machine is used for composite molding. An aluminum substrate is placed on the lower heating plate of the flat vulcanizing machine, and a shim frame is placed on top of the aluminum substrate. Emulsion gel is injected into the shim frame, and another aluminum substrate is covered on top of the emulsion foam. The composite molding process conditions are: pressure 0.2 MPa, temperature 120℃, time 5 minutes. After this, the aluminum plate is removed, trimmed, and naturally air-dried to a constant weight to obtain a polymer aerogel thermal insulation aluminum-based decorative panel. Example 3

[0017] Raw materials: Zhongning Technology AG-D silica aerogel, Shanghai Resin E-51 epoxy resin, Kaimete 99.9% carbon dioxide, Xinjiang Debang ZZ-23 sodium stearate, Yongjie Aluminum 5052 aluminum alloy H32 2mm thick plate, and Haiyou Changzhou polyurethane emulsion, which is a closed anionic polyurethane emulsion with 5% NCO content.

[0018] The production method of polymer aerogel thermal insulation aluminum-based decorative panel includes the following steps: Step 1, preparation of pre-crosslinked epoxy resin gel: 105 parts of 0.2 mol / L sodium hydroxide solution, 4 parts of diethylenetriamine, 48 parts of epoxy resin and 0.25 parts of sodium stearate are added to a reactor equipped with a stirrer and a reflux condenser. The mixture is stirred at 550 rpm and reacted at 95°C for 12 min. After filtration, the pre-crosslinked epoxy resin gel is obtained. Step 2, emulsion gel-sol reaction: The silica aerogel is an amino-modified silica aerogel. The silica aerogel is added to xylene with a volume of 3 times its volume, and then transferred to a reactor. 3% KH550 by weight of the silica aerogel is added, and the mixture is heated to reflux at 60°C under a nitrogen atmosphere. After 124 h, it is centrifuged, washed with xylene and ethanol, and dried to constant weight. The mass ratio of crosslinking foaming agent, pre-crosslinked epoxy resin gel and polyurethane emulsion is 1.5:12:15. The mixture of lipogel and polyurethane emulsion is followed by the addition of 10% (by weight) of epoxy resin and silica aerogel. The mixture is stirred at 1200 rpm for 6 minutes and then at 25000 rpm for 12 minutes to obtain an emulsion gel. The crosslinking foaming agent is N-aminoethylpiperazine dissolved in anhydrous ethanol to prepare a 12% (by weight) solution, which is placed in a reaction vessel. Carbon dioxide gas is then introduced into the reaction vessel at a flow rate of 28 mL / min. After reacting for 12 minutes, the mixture is filtered to obtain the precipitate. The third step is the composite molding of aluminum-based decorative panels: a flat vulcanizing machine is used. An aluminum substrate is placed on the lower heating plate of the flat vulcanizing machine, and a shim frame is placed on top of the aluminum substrate. Emulsion gel is injected into the shim frame, and another aluminum substrate is covered on top of the emulsion foam. The composite molding process conditions are: pressure 0.4 MPa, temperature 125℃, and time 8 minutes. After this, the aluminum plate is removed, trimmed, and naturally air-dried to a constant weight to obtain the polymer aerogel thermal insulation aluminum-based decorative panel.

[0019] The performance of the polymer aerogel thermal insulation aluminum-based decorative panels prepared in Examples 1-3 was tested. The test results are shown in Table 1.

[0020] Table 1 Performance test results of polymer aerogel thermal insulation aluminum-based decorative panels in Examples 1-3

[0021]

[0022] Note: The standard laboratory test environment conditions are a temperature of 23℃ and a relative humidity of 50%. Visual inspection is conducted at a distance of 0.5m to 1.0m from the sample to check for surface flatness and visible defects such as bulging, cracks, and warping. Density is determined according to the method specified in GB / T5486, with sample dimensions of 300mm × 300mm × plate thickness. After drying to constant weight, the sample is placed under standard test conditions for 24 hours, and the density is measured as the arithmetic mean of three sample data. Thermal conductivity is determined according to the method specified in GB / T10294 or GB / T10295, with sample dimensions of 300mm × 300mm × 30mm. The sample should be taken from a sample whose density has been determined, with an average sample temperature of 23℃. The test result is the arithmetic mean of three sample test data. Tensile strength perpendicular to the plate surface is measured according to JG / T536-2017. Compressive strength shall be tested according to the method specified in GB / T 5486. If the specimen does not break under 10% compression deformation, the load at which the specimen undergoes 10% compression deformation is considered the breaking load. The test result is the arithmetic mean of test data from 10 specimens. Volumetric water absorption shall be tested according to the method specified in GB / T 5486. The test result is the arithmetic mean of test data from 10 specimens. Flexural strength shall be tested according to the method specified in GB / T 5486. The test result is the arithmetic mean of test data from 10 specimens. Flammability rating shall be tested using samples with determined density, and the flammability rating shall be determined according to the method specified in GB 8624.

Claims

1. A method for producing a polymer aerogel thermal insulation aluminum-based decorative panel, characterized in that, Includes the following steps: Step 1: Preparation of pre-crosslinked epoxy resin gel: Add 100-110 parts of 0.2 mol / L sodium hydroxide solution, 3-5 parts of diethylenetriamine, 45-53 parts of epoxy resin, and 0.2-0.3 parts of sodium stearate to a reactor equipped with a stirrer and reflux condenser. React at 90-110℃ for 10-15 minutes with stirring at 500-600 rpm, then filter to obtain the pre-crosslinked epoxy resin gel. Step 2: Emulsion gel sol reaction: Mix the crosslinking foaming agent, pre-crosslinked epoxy resin gel, and polyurethane emulsion in a certain proportion, then add 5%-15% (by weight of epoxy resin) of silica aerogel. Stir at 1000-1500 rpm for 5-10 minutes, then at 2000-3000 rpm for 10-15 minutes to obtain an emulsion gel. Step 2: Preparation of pre-crosslinked epoxy resin gel and polyurethane emulsion... The mass ratio is 1~2∶11~13∶15~17; the second step crosslinking foaming agent is N-aminoethylpiperazine dissolved in anhydrous ethanol to prepare a solution with a mass fraction of 10~15%, placed in a reaction vessel, and then carbon dioxide gas is introduced into the reaction vessel at a flow rate of 25~30mL / min. After reacting for 10~15min, the mixture is filtered and precipitated; the third step, aluminum-based decorative panel composite molding: composite molding is carried out using a flat vulcanizing machine. A layer of aluminum substrate is placed on the lower heating plate of the flat vulcanizing machine, and a pad frame is placed on the aluminum substrate. Emulsion gel material is injected into the pad frame, and another layer of aluminum substrate is covered on the emulsion foam material. The composite molding process conditions are: pressure 0.2~0.6MPa, temperature 120~135℃, time 5~10min. After that, the aluminum plate is taken out, trimmed, and naturally air-dried to constant weight to obtain a polymer aerogel thermal insulation aluminum-based decorative panel.

2. The method for producing a polymer aerogel thermal insulation aluminum-based decorative panel according to claim 1, characterized in that, The second step involves a closed-cell anionic polyurethane emulsion with an NCO content of 3.5% to 5% and a solid content of 15% to 20%.

3. The method for producing a polymer aerogel thermal insulation aluminum-based decorative panel according to claim 1, characterized in that, The second step involves using an amino-modified silica aerogel.

4. The method for producing a polymer aerogel thermal insulation aluminum-based decorative panel according to claim 1, characterized in that, The aluminum substrate in the third step is one of the aluminum alloy plates selected from 1100, 3003, 3004, and 5052.

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