Preparation method of inorganic active and passive A-level fireproof thermal insulation integrated board
Patent Information
- Application Number
- CN202410350937.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-03-26
- Publication Date
- 2026-10-30
- Estimated Expiration
- 2044-03-26
AI Technical Summary
[0005]本发明要解决现有防火保温一体化板防火性能很难达到A级不燃,防火性能不足,而且燃烧释放有毒有害气体的问题,进而提供一种无机的主被动A级防火保温一体化板的制备方法
[0025](1)本发明的一种主被动A级防火保温一体板,为无机A级防火材料,通过协同发挥主动防火层(石膏)在火灾条件下的化学反应吸收热量释放水蒸气的主动防火原理和被动防火层(多孔无机纤维保温板)的低热导率隔绝热量的被动防火原理,显著提升了围护体系(一体板)的耐火极限。三层结构的一种无机主被动A级防火保温一体板较单层同厚度的石膏板的防火极限提高了20%以上,在主动防火期间,背火面温升曲线平台期的温度降低了0~30℃。
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Figure CN118255567B_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of building materials. Background Technology
[0002] The emergence of fireproof and thermal insulation integrated panels has brought about technological updates to building materials and their engineering applications, shifting the traditional method of on-site discrete construction to factory completion. This has advantages such as more stable quality, increased production capacity, and less susceptibility to construction environment, providing an effective way to achieve building industrialization.
[0003] However, current fireproof and thermal insulation integrated panels still have two significant drawbacks: 1. Because organic adhesives are used to bond the functional layers, the fire resistance of integrated panels is difficult to reach Class A non-combustible, and they release toxic and harmful gases when burning; 2. The thermal insulation materials in integrated panels are still mainly polystyrene boards, polystyrene, etc., which have insufficient fire resistance and pose a huge fire safety hazard.
[0004] With the development of the times, people's requirements for green fireproof and thermal insulation materials are becoming increasingly stringent, and researchers are paying more and more attention to the upgrading and transformation of integrated fireproof and thermal insulation panels. Developing a new type of inorganic fireproof and thermal insulation integrated panel that can achieve both Class A fire resistance and excellent thermal insulation performance is of great significance. Summary of the Invention
[0005] This invention aims to address the problems of existing fireproof and heat-insulating integrated panels having insufficient fire resistance and releasing toxic and harmful gases during combustion, and to provide a method for preparing an inorganic active and passive Class A fireproof and heat-insulating integrated panel.
[0006] A method for preparing an inorganic active and passive Class A fireproof and thermal insulation integrated board, comprising the following steps:
[0007] I. Pouring the first active fireproof layer:
[0008] ① Weigh out 0.25 to 2.5 parts of retarder, 0.25 to 2.5 parts of water-reducing agent, 0.125 to 1.25 parts of hydroxypropyl methylcellulose, 150 to 250 parts of water, 250 to 1000 parts of calcined gypsum powder, 0.1 to 50 parts of graphite powder, and 2.5 to 25 parts of chopped inorganic fibers according to the following mass percentages;
[0009] ② Mix and dissolve 0.25 to 2.5 parts of retarder, 0.25 to 2.5 parts of water-reducing agent, 0.125 to 1.25 parts of hydroxypropyl methylcellulose and 150 to 250 parts of water to obtain solution I;
[0010] ③ Stir 250 to 1000 parts of calcined gypsum powder, 0.1 to 50 parts of graphite powder and 2.5 to 25 parts of chopped inorganic fibers at low speed to obtain gypsum dry mixture I;
[0011] ④ Pour the solution I into the gypsum dry mix I, stir at low speed first, then stir at high speed to obtain gypsum slurry I;
[0012] ⑤ Pour gypsum slurry I into the mold to obtain a mold with a first active fireproof layer;
[0013] II. Laying a passive fireproof layer:
[0014] ① A hydrophobic agent is sprayed onto the surface of the porous inorganic fiber insulation board to obtain a hydrophobic insulation board;
[0015] ② Lay a hydrophobically treated insulation board on the surface of the first active fireproof layer to obtain a mold with a first active fireproof layer / passive fireproof layer;
[0016] III. Pouring the second active fireproof layer:
[0017] ① Weigh out 0.25 to 2.5 parts of retarder, 0.25 to 2.5 parts of water-reducing agent, 0.125 to 1.25 parts of hydroxypropyl methylcellulose, 150 to 250 parts of water, 250 to 1000 parts of calcined gypsum powder, 0.1 to 50 parts of gaseous silica, and 2.5 to 25 parts of chopped inorganic fibers according to the following mass percentages;
[0018] ② Mix and dissolve 0.25 to 2.5 parts of retarder, 0.25 to 2.5 parts of water-reducing agent, 0.125 to 1.25 parts of hydroxypropyl methylcellulose and 150 to 250 parts of water to obtain solution II;
[0019] ③ Stir 250 to 1000 parts of calcined gypsum powder, 0.1 to 50 parts of gaseous silica and 2.5 to 25 parts of chopped inorganic fibers at low speed to obtain gypsum dry mix II;
[0020] ④ Pour the solution II into the gypsum dry mix II, stir at low speed first, then stir at high speed to obtain gypsum slurry II;
[0021] ⑤ Pour gypsum slurry II onto the surface of the insulation board after it has been treated with hydrophobicity to obtain a mold with a first active fireproof layer / passive fireproof layer / second active fireproof layer;
[0022] IV. Maintenance:
[0023] A plastic film is laid on the surface of the mold with the first active fireproof layer / passive fireproof layer / second active fireproof layer, then the top cover is placed on and pressure is applied for curing. Finally, the mold is removed and the plastic film is removed to obtain an inorganic active and passive Class A fireproof and heat-insulating integrated board.
[0024] The beneficial effects of this invention are:
[0025] (1) The present invention provides an integrated active and passive Class A fireproof and thermal insulation panel, which is an inorganic Class A fireproof material. By synergistically utilizing the active fireproof layer (gypsum) to absorb heat and release water vapor through chemical reaction under fire conditions and the passive fireproof layer (porous inorganic fiber insulation board) to insulate heat through low thermal conductivity, the fire resistance limit of the enclosure system (integrated panel) is significantly improved. The three-layer inorganic active and passive Class A fireproof and thermal insulation integrated panel has a fire resistance limit that is more than 20% higher than that of a single-layer gypsum board of the same thickness. During active fire protection, the temperature of the plateau period of the temperature rise curve on the unexposed side is reduced by 0-30℃.
[0026] (2) The active and passive Class A fireproof and thermal insulation integrated panel of the present invention has excellent thermal insulation performance. The equivalent thermal conductivity is as low as 0.1W / (mK), which is more than 50% lower than that of a single-layer gypsum board of the same thickness.
[0027] (3) This invention achieves the integrated composite of gypsum and porous inorganic fiber insulation board through an integrated casting process. The entire preparation process does not use starch, gypsum facing paper or other materials, and does not use organic adhesives, thus eliminating the release of toxic and harmful gases in case of fire, making it green and environmentally friendly.
[0028] (4) The active and passive Class A fireproof and heat-insulating integrated board of the present invention is more than 30% lighter than a single layer of gypsum board of the same thickness.
[0029] (5) The active and passive Class A fireproof and heat-insulating integrated board of the present invention maintains structural integrity after combustion testing. Compared with single-layer gypsum board of the same thickness, the modification method of adding gaseous silica can significantly reduce the thermal stress of the board, reduce the width and length of single cracks, and effectively prevent the board from cracking after annealing (fire suppression), thus improving safety.
[0030] (6) This invention can improve building energy efficiency and reduce the use of heating equipment. This reduces energy consumption and carbon emissions during building operation, improves green energy conservation, and promotes the green and sustainable development of the construction industry, thus having good economic, environmental and social benefits.
[0031] This invention relates to a method for preparing an inorganic active and passive Class A fireproof and heat-insulating integrated panel. Attached Figure Description
[0032] Figure 1 A schematic diagram and a physical image of the gypsum board prepared for Comparative Example 1;
[0033] Figure 2 A schematic diagram and a physical image of the graphite-modified gypsum board prepared in Comparative Example 2;
[0034] Figure 3A schematic diagram and a physical image of the fumed silica-modified gypsum board prepared in Comparative Example 3;
[0035] Figure 4 A schematic diagram and a physical image of the double-layer fireproof and heat-insulating integrated panel prepared in Comparative Example 4;
[0036] Figure 5 A schematic diagram and a physical image of the double-layer graphite-modified fireproof and heat-insulating integrated board prepared in Comparative Example 5;
[0037] Figure 6 A schematic diagram and a physical image of the double-layer fumed silica modified fireproof and heat-insulating integrated board prepared in Comparative Example 6;
[0038] Figure 7 A schematic diagram and a physical image of the inorganic active and passive Class A fireproof and heat-insulating integrated panel prepared in Example 1;
[0039] Figure 8 A schematic diagram and physical image of the unmodified inorganic active and passive Class A fireproof and thermal insulation integrated board prepared for Comparative Example 7;
[0040] Figure 9 A schematic diagram and a physical image of the graphite-modified inorganic active and passive Class A fireproof and thermal insulation integrated panel prepared for Comparative Example 8;
[0041] Figure 10 A schematic diagram and a physical image of the inorganic active and passive Class A fireproof and thermal insulation integrated board modified with silica powder prepared in Comparative Example 9.
[0042] Figure 11 For comparison, the average temperature curve of the central region of the unexposed side during the combustion test;
[0043] Figure 12 The average temperature curves of the central region of the unexposed side during combustion tests are shown for the examples and comparative examples.
[0044] Figure 13 The image shows the morphology of the central region of the flame-exposed surface of the specimen after natural cooling following the combustion test. Detailed Implementation
[0045] The technical solution of the present invention is not limited to the specific embodiments listed below, but also includes any combination of the specific embodiments.
[0046] Specific Implementation Method 1: This implementation method describes a method for preparing an inorganic active and passive Class A fireproof and thermal insulation integrated board, which is carried out according to the following steps:
[0047] I. Pouring the first active fireproof layer:
[0048] ① Weigh out 0.25 to 2.5 parts of retarder, 0.25 to 2.5 parts of water-reducing agent, 0.125 to 1.25 parts of hydroxypropyl methylcellulose, 150 to 250 parts of water, 250 to 1000 parts of calcined gypsum powder, 0.1 to 50 parts of graphite powder, and 2.5 to 25 parts of chopped inorganic fibers according to the following mass percentages;
[0049] ② Mix and dissolve 0.25 to 2.5 parts of retarder, 0.25 to 2.5 parts of water-reducing agent, 0.125 to 1.25 parts of hydroxypropyl methylcellulose and 150 to 250 parts of water to obtain solution I;
[0050] ③ Stir 250 to 1000 parts of calcined gypsum powder, 0.1 to 50 parts of graphite powder and 2.5 to 25 parts of chopped inorganic fibers at low speed to obtain gypsum dry mixture I;
[0051] ④ Pour the solution I into the gypsum dry mix I, stir at low speed first, then stir at high speed to obtain gypsum slurry I;
[0052] ⑤ Pour gypsum slurry I into the mold to obtain a mold with a first active fireproof layer;
[0053] II. Laying a passive fireproof layer:
[0054] ① A hydrophobic agent is sprayed onto the surface of the porous inorganic fiber insulation board to obtain a hydrophobic insulation board;
[0055] ② Lay a hydrophobically treated insulation board on the surface of the first active fireproof layer to obtain a mold with a first active fireproof layer / passive fireproof layer;
[0056] III. Pouring the second active fireproof layer:
[0057] ① Weigh out 0.25 to 2.5 parts of retarder, 0.25 to 2.5 parts of water-reducing agent, 0.125 to 1.25 parts of hydroxypropyl methylcellulose, 150 to 250 parts of water, 250 to 1000 parts of calcined gypsum powder, 0.1 to 50 parts of gaseous silica, and 2.5 to 25 parts of chopped inorganic fibers according to the following mass percentages;
[0058] ② Mix and dissolve 0.25 to 2.5 parts of retarder, 0.25 to 2.5 parts of water-reducing agent, 0.125 to 1.25 parts of hydroxypropyl methylcellulose and 150 to 250 parts of water to obtain solution II;
[0059] ③ Stir 250 to 1000 parts of calcined gypsum powder, 0.1 to 50 parts of gaseous silica and 2.5 to 25 parts of chopped inorganic fibers at low speed to obtain gypsum dry mix II;
[0060] ④ Pour the solution II into the gypsum dry mix II, stir at low speed first, then stir at high speed to obtain gypsum slurry II;
[0061] ⑤ Pour gypsum slurry II onto the surface of the insulation board after it has been treated with hydrophobicity to obtain a mold with a first active fireproof layer / passive fireproof layer / second active fireproof layer;
[0062] IV. Maintenance:
[0063] A plastic film is laid on the surface of the mold with the first active fireproof layer / passive fireproof layer / second active fireproof layer, then the top cover is placed on and pressure is applied for curing. Finally, the mold is removed and the plastic film is removed to obtain an inorganic active and passive Class A fireproof and heat-insulating integrated board.
[0064] This specific embodiment is based on the active fireproofing principle of gypsum (a type of cementing material) decomposing, consuming energy, and releasing water vapor when exposed to fire, and the passive fireproofing principle of porous inorganic fiber insulation board with low thermal conductivity and high heat insulation. It proposes an integrated inorganic active and passive Class A fireproof and heat-insulating board, comprising a first active fireproof layer, a passive fireproof layer, and a second active fireproof layer. The integrated board is formed in one piece, eliminating the need for adhesives between the layers. The active fireproof layer is a graphite-modified gypsum layer or a gaseous silica-modified gypsum layer; the passive fireproof layer is a hydrophobic porous inorganic fiber insulation board. By synergistically leveraging the fireproofing effects of the active and passive fireproofing materials, and through optimized structural design and differentiated modifications, the three-layer inorganic active and passive Class A fireproof and heat-insulating integrated board of this invention significantly improves fire resistance, insulation performance, and reduces weight compared to a single-layer gypsum board of the same thickness or a double-layer active and passive fireproof and heat-insulating integrated board.
[0065] In this specific embodiment, the first active fireproof layer is modified with high thermal conductivity inorganic powder (graphite), which has high thermal conductivity, allowing heat to be quickly transferred from the fire point to other areas in the event of a fire, allowing more gypsum-based cementitious materials to play an active fireproof role. In addition, due to the presence of the passive fireproof layer, heat does not quickly penetrate the board.
[0066] The purpose of the hydrophobic treatment in this specific embodiment is to prevent the high porosity of the passive fireproof layer from siphoning away the water in the gypsum slurry of the active fireproof layer during the pouring of the first and second active fireproof layers, thereby changing the material ratio of the fireproof layer and forming a weak interface transition zone.
[0067] In this specific embodiment, the second active fireproof layer is modified with low thermal conductivity inorganic powder fumed silica, resulting in lower thermal conductivity and enhanced insulation capacity, serving as the final fire barrier for the panel. The uniform distribution of fumed silica increases the heat and water vapor transport paths, further extending the fire resistance limit and reducing the temperature rise on the unexposed surface.
[0068] In this specific embodiment, the plastic film serves to isolate the second active fireproof layer from the mold cover, facilitating demolding and preventing the second active fireproof layer from sticking to the mold.
[0069] The beneficial effects of this embodiment are:
[0070] (1) The active and passive Class A fireproof and thermal insulation integrated panel of this embodiment is an inorganic Class A fireproof material. By synergistically utilizing the active fireproof layer (gypsum) to absorb heat and release water vapor through chemical reaction under fire conditions and the passive fireproof layer (porous inorganic fiber insulation board) to insulate heat through low thermal conductivity, the fire resistance limit of the enclosure system (integrated panel) is significantly improved. The fire resistance limit of the three-layer inorganic active and passive Class A fireproof and thermal insulation integrated panel is more than 20% higher than that of a single-layer gypsum board of the same thickness. During active fire protection, the temperature of the plateau period of the temperature rise curve on the unexposed side is reduced by 0-30℃.
[0071] (2) The active and passive Class A fireproof and thermal insulation integrated panel of this embodiment has excellent thermal insulation performance. The equivalent thermal conductivity is as low as 0.1W / (mK), which is more than 50% lower than that of a single-layer gypsum board of the same thickness.
[0072] (3) This embodiment realizes the integrated composite of gypsum and porous inorganic fiber insulation board through integrated casting process. The entire preparation process does not use starch, gypsum facing paper and other materials, and does not use organic adhesives, thus eliminating the release of toxic and harmful gases in case of fire, making it green and environmentally friendly.
[0073] (4) The active and passive Class A fireproof and heat-insulating integrated board of this embodiment is more than 30% lighter than a single layer of gypsum board of the same thickness.
[0074] (5) The active and passive Class A fireproof and heat-insulating integrated panel of this embodiment maintains structural integrity after combustion testing. Compared with single-layer gypsum board of the same thickness, the modification method of adding gaseous silica can significantly reduce the thermal stress of the board, reduce the width and length of single cracks, and effectively prevent the board from cracking after annealing (fire suppression), thus improving safety.
[0075] (6) This implementation method can improve building energy efficiency and reduce the use of heating equipment. This reduces energy consumption and carbon emissions during building operation, improves green energy conservation, promotes the green and sustainable development of the construction industry, and has good economic, environmental and social benefits.
[0076] Specific Implementation Method Two: This implementation method differs from Specific Implementation Method One in that: the retarder mentioned in steps one ① and three ① is sodium tripolyphosphate; the water-reducing agent mentioned in steps one ① and three ① is polycarboxylic acid, and the molecular weight of the polycarboxylic acid is 30,000 to 50,000; the chopped inorganic fibers mentioned in steps one ① and three ① are chopped glass fibers, aluminosilicate fibers, mullite fibers, or alumina fibers; and the length of the chopped inorganic fibers is 3 mm to 12 mm. Everything else is the same as in Specific Implementation Method One.
[0077] Specific Implementation Method Three: This implementation method differs from Specific Implementation Method One or Two in that: the graphite powder mentioned in step one ① is high-purity flake graphite powder; the particle size of the graphite powder is 3.4μm to 6.5μm; the fumed silica powder mentioned in step three ① is hydrophilic fumed silica powder, with a particle size of 200nm to 500nm and a specific surface area of 200m². 2 / g~500m 2 / g, the mass percentage of silicon dioxide is not less than 99.8%. Other aspects are the same as in specific embodiments one or two.
[0078] Specific Implementation Method Four: This implementation method differs from Specific Implementation Methods One to Three in that the low-speed stirring described in Step One ③ and Step Three ③ is specifically performed at a rotation speed of 500 r / min to 800 r / min for 2 to 5 minutes. Everything else is the same as in Specific Implementation Methods One to Three.
[0079] Specific Implementation Method Five: This implementation method differs from Specific Implementation Methods One to Four in that: the process of first stirring at low speed and then stirring at high speed in steps One ④ and Three ④ specifically involves first stirring at low speed for 1 to 2 minutes at a speed of 500 r / min to 800 r / min, and then stirring at high speed for 1 to 2 minutes at a speed of 1500 r / min to 2000 r / min. Everything else is the same as in Specific Implementation Method Four.
[0080] Specific Implementation Method Six: This implementation method differs from Specific Implementation Methods One to Five in that: the porous inorganic fiber insulation board mentioned in step two① is an aerogel-alumina silicate fiber board, aerogel-glass fiber board, aerogel-alumina fiber board, aerogel-mullite fiber board, inorganic alumina silicate fiber board, inorganic glass fiber board, inorganic mullite fiber board, or rock wool board; the thickness of the porous inorganic fiber insulation board mentioned in step two① is 2mm to 25mm. Everything else is the same as in Specific Implementation Methods One to Five.
[0081] Specific Implementation Method Seven: This implementation method differs from Specific Implementation Methods One to Six in that the hydrophobic agent mentioned in step two① is an organosilicon hydrophobic agent, polysiloxane, potassium methylsilicate, water-based paraffin emulsion, or nanomaterial-modified fluorocarbon polymer. Everything else is the same as in Specific Implementation Methods One to Six.
[0082] Specific Implementation Method Eight: This implementation method differs from Specific Implementation Methods One to Seven in that the spraying described in step two① is carried out as follows: The surface of the porous inorganic fiber insulation board is blown clean to remove surface delamination and easily detachable aerogel powder. Then, the porous inorganic fiber insulation board is preheated for 10 to 30 minutes at a temperature of 45–60°C. Next, at room temperature, the hydrophobic agent is evenly sprayed onto the surface of the porous inorganic fiber insulation board using a spray bottle with a nozzle diameter of 0.2 mm to 0.5 mm. Finally, it is cured at room temperature. Everything else is the same as in Specific Implementation Methods One to Seven.
[0083] Specific Implementation Method Nine: This implementation method differs from Specific Implementation Methods One to Eight in that: in step one (⑤), gypsum slurry I is poured into the mold to a thickness of 2mm to 10mm; in step three (⑤), gypsum slurry II is poured onto the surface of the hydrophobic treated insulation board to a thickness of 2mm to 10mm. Everything else is the same as in Specific Implementation Methods One to Eight.
[0084] Specific Implementation Method Ten: This implementation method differs from Specific Implementation Methods One to Nine in that the pressure curing described in step four is specifically carried out under conditions of a temperature of 40℃~60℃, a humidity of 30%RH~60%RH, and a pressure of 1MPa~5MPa for 12h~24h. Everything else is the same as in Specific Implementation Methods One to Nine.
[0085] The beneficial effects of the present invention are verified using the following embodiments:
[0086] Example 1:
[0087] A method for preparing an inorganic active and passive Class A fireproof and thermal insulation integrated board, comprising the following steps:
[0088] I. Pouring the first active fireproof layer:
[0089] ① Weigh out 0.25 parts of retarder, 0.25 parts of water-reducing agent, 0.125 parts of hydroxypropyl methylcellulose, 150 parts of water, 250 parts of calcined gypsum powder, 12.5 parts of graphite powder and 2.5 parts of chopped inorganic fiber according to the following mass proportions;
[0090] ② Mix and dissolve 0.25 parts of retarder, 0.25 parts of water-reducing agent, 0.125 parts of hydroxypropyl methylcellulose and 150 parts of water to obtain solution I;
[0091] ③ Stir 250 parts of calcined gypsum powder, 12.5 parts of graphite powder and 2.5 parts of chopped inorganic fibers at low speed to obtain gypsum dry mixture I;
[0092] ④ Pour the solution I into the gypsum dry mix I, stir at low speed first, then stir at high speed to obtain gypsum slurry I;
[0093] ⑤ Pour gypsum slurry I into the mold to obtain a mold with a first active fireproof layer;
[0094] II. Laying a passive fireproof layer:
[0095] ① A hydrophobic agent is sprayed onto the surface of the porous inorganic fiber insulation board to obtain a hydrophobic insulation board;
[0096] ② Lay a hydrophobically treated insulation board on the surface of the first active fireproof layer to obtain a mold with a first active fireproof layer / passive fireproof layer;
[0097] III. Pouring the second active fireproof layer:
[0098] ① Weigh out 0.25 parts of retarder, 0.25 parts of water-reducing agent, 0.125 parts of hydroxypropyl methylcellulose, 150 parts of water, 250 parts of calcined gypsum powder, 12.5 parts of gaseous silica and 2.5 parts of chopped inorganic fiber by weight.
[0099] ② Mix and dissolve 0.25 parts of retarder, 0.25 parts of water-reducing agent, 0.125 parts of hydroxypropyl methylcellulose and 150 parts of water to obtain solution II;
[0100] ③ Stir 250 parts of calcined gypsum powder, 12.5 parts of gaseous silica and 2.5 parts of chopped inorganic fibers at low speed to obtain gypsum dry mix II;
[0101] ④ Pour the solution II into the gypsum dry mix II, stir at low speed first, then stir at high speed to obtain gypsum slurry II;
[0102] ⑤ Pour gypsum slurry II onto the surface of the insulation board after it has been treated with hydrophobicity to obtain a mold with a first active fireproof layer / passive fireproof layer / second active fireproof layer;
[0103] IV. Maintenance:
[0104] A plastic film is laid on the surface of the mold with the first active fireproof layer / passive fireproof layer / second active fireproof layer, then the top cover is placed on and pressure is applied for curing. Finally, the mold is removed and the plastic film is removed to obtain an inorganic active and passive Class A fireproof and heat-insulating integrated board.
[0105] The retarder mentioned in Step 1① and Step 3① is sodium tripolyphosphate; the water-reducing agent mentioned in Step 1① and Step 3① is polycarboxylic acid, and the molecular weight of the polycarboxylic acid is 40,000; the chopped inorganic fiber mentioned in Step 1① and Step 3① is chopped glass fiber; and the length of the chopped inorganic fiber is 6 mm.
[0106] The graphite powder mentioned in step one ① is high-purity flake graphite powder; the particle size of the graphite powder is 3000 mesh; the fumed silica powder mentioned in step three ① is hydrophilic fumed silica powder, with a particle size of 300 nm and a specific surface area of 300 m². 2 / g, the mass percentage of silicon dioxide is not less than 99.8%.
[0107] The low-speed stirring mentioned in steps 1.③ and 3.③ specifically refers to stirring at a speed of 500 r / min for 2 minutes.
[0108] The steps 1. ③ and 3. ④ mentioned above, which involve stirring at low speed first and then at high speed, specifically mean stirring at low speed for 1 minute at a speed of 500 r / min and then stirring at high speed for 1 minute at a speed of 1500 r / min.
[0109] The porous inorganic fiber insulation board mentioned in step 2① is the HY-1000 aluminum silicate inorganic fiber board of Deqing Hongye Crystal Fiber Co., Ltd., with a thickness of 10mm;
[0110] The hydrophobic agent mentioned in step 2① is a 3% (w / w) aqueous solution of potassium methylsilicate.
[0111] The spraying process described in step 2① is carried out as follows: blow away the surface of the porous inorganic fiber insulation board to remove surface delamination and easily detachable aerogel powder, preheat the porous inorganic fiber insulation board for 15 minutes at a temperature of 60℃, and then spray the hydrophobic agent evenly onto the surface of the porous inorganic fiber insulation board using a spray bottle with a nozzle diameter of 0.3mm at room temperature, and finally cure at room temperature.
[0112] Step 1, ⑤: Pour gypsum slurry I into the mold to a thickness of 5mm; Step 3, ⑤: Pour gypsum slurry II onto the surface of the hydrophobic insulation board to a thickness of 5mm.
[0113] The pressure curing described in step four is specifically carried out under the conditions of a temperature of 45±2℃, a humidity of 50±5%RH, and a pressure of 2MPa for 24 hours.
[0114] Example 2: The proportions and preparation process of Example 1 were repeated, except that the exposed and unexposed sides were reversed during the combustion test.
[0115] Comparative Example 1: This comparative example differs from Example 1 in that: in step 1①, 1 part retarder, 1 part water-reducing agent, 0.5 parts hydroxypropyl methylcellulose, 600 parts water, 1000 parts calcined gypsum powder, and 10 parts chopped inorganic fibers are weighed according to the following mass proportions; steps 2 and 3 are omitted; in step 4, a gypsum board with a thickness of 20 mm is obtained. Everything else is the same as in Example 1.
[0116] Comparative Example 2: This comparative example differs from Example 1 in that: in step 1①, 1 part retarder, 1 part water-reducing agent, 0.5 parts hydroxypropyl methylcellulose, 600 parts water, 1000 parts calcined gypsum powder, 50 parts graphite powder, and 10 parts chopped inorganic fibers are weighed according to the following mass proportions; steps 2 and 3 are omitted; in step 4, graphite-modified gypsum board with a thickness of 20 mm is obtained. Everything else is the same as in Example 1.
[0117] Comparative Example 3: This comparative example differs from Example 1 in that: in step 1①, 1 part retarder, 1 part water-reducing agent, 0.5 parts hydroxypropyl methylcellulose, 600 parts water, 1000 parts calcined gypsum powder, 50 parts fumed silica powder, and 10 parts chopped inorganic fibers are weighed according to the following mass proportions; steps 2 and 3 are omitted; in step 4, fumed silica-modified gypsum board with a thickness of 20 mm is obtained. Everything else is the same as in Example 1.
[0118] Comparative Example 4: This comparative example differs from Example 1 in the following ways: In step 1①, 0.5 parts by weight of retarder, 0.5 parts by weight of water-reducing agent, 0.25 parts by weight of hydroxypropyl methylcellulose, 300 parts by weight of water, 500 parts by weight of calcined gypsum powder, and 5 parts by weight of chopped inorganic fibers are weighed; in step 1⑤, gypsum slurry I is poured into a mold to a thickness of 10 mm; step 3 is omitted; in step 4, a double-layer fireproof and heat-insulating integrated board is obtained. Everything else is the same as in Example 1.
[0119] Comparative Example 5: This comparative example differs from Example 1 in the following ways: In step 1①, 0.5 parts by weight of retarder, 0.5 parts by weight of water-reducing agent, 0.25 parts by weight of hydroxypropyl methylcellulose, 300 parts by weight of water, 500 parts by weight of calcined gypsum powder, 25 parts by weight of graphite powder, and 5 parts by weight of chopped inorganic fibers are weighed; in step 1⑤, gypsum slurry I is poured into a mold to a thickness of 10 mm; step 3 is omitted; in step 4, a double-layer graphite-modified fireproof and heat-insulating integrated board is obtained. Everything else is the same as in Example 1.
[0120] Comparative Example 6: This comparative example differs from Example 1 in the following ways: In step 1①, 0.5 parts by weight of retarder, 0.5 parts by weight of water-reducing agent, 0.25 parts by weight of hydroxypropyl methylcellulose, 300 parts by weight of water, 500 parts by weight of calcined gypsum powder, 25 parts by weight of fumed silica powder, and 5 parts by weight of chopped inorganic fibers are weighed; in step 1⑤, gypsum slurry I is poured into a mold to a thickness of 10 mm; step 3 is omitted; in step 4, a double-layer fumed silica-modified fireproof and heat-insulating integrated board is obtained. Everything else is the same as in Example 1.
[0121] Comparative Example 7: This comparative example differs from Example 1 in that: step 1 ③ omits the addition of graphite powder; step 3 ③ omits fumed silica powder. Everything else is the same as Example 1.
[0122] Comparative Example 8: This comparative example differs from Example 1 in that: step 3.③ fumed silica powder was omitted; 12.5 parts of graphite powder were added to both the first and second active fireproof layers. Everything else is the same as in Example 2.
[0123] Comparative Example 9: This comparative example differs from Example 1 in that: step 1.③ Graphite powder was omitted; 12.5 parts of silica powder were added to both the first and second active fireproof layers. Everything else was the same as in Example 2.
[0124] Performance testing:
[0125] 1. The product weight and dimensions were measured, and the equivalent density was calculated, as shown in Table 1.
[0126] 2. Conduct BS 476-4 non-flammability test and BS 476-7 flame spread test.
[0127] 3. Combustion tests were conducted using a propane flame. During the test, the temperature of the flame-exposed surface of the specimen was raised from room temperature to 1000℃ within one minute and maintained stable. The flame-exposed surface of the test specimen is the side in contact with the outer flame of the propane flame, while the unflamed surface is the side in contact with room temperature air, i.e., the side unaffected by the flame. Comparative Examples 1 to 3 were single-layer boards; Comparative Examples 4 to 9, Examples 1 and 2 were double-layer or triple-layer fireproof and heat-insulating integrated boards. Comparative Examples 4 and 7 used a gypsum layer as the flame-exposed surface; Comparative Examples 5, 8, and 1 all used a graphite-modified gypsum layer as the flame-exposed surface; and Comparative Examples 6, 9, and 2 all used gaseous silica as the flame-exposed surface. The other side of the corresponding specimen was the unflamed surface.
[0128] 4. The thermal conductivity was measured using a thermal constant analyzer, as shown in Table 1.
[0129] 5. The tensile bond strength of comparative examples four to nine and examples one to two was tested in accordance with JGJ144-2019 "Technical Standard for External Thermal Insulation Engineering" and JGJ / T110-2017 "Standard for Testing Bond Strength of Facing Bricks in Building Engineering", and the results are shown in Table 1.
[0130] Table 1 summarizes the weight, thickness, time for the average temperature of the central region of the unexposed surface to reach 160°C, room temperature thermal conductivity, and tensile bond strength of the finished products in each comparative example and embodiment. The inorganic active-passive Class A fire-resistant and thermally insulating integrated panel of this embodiment is more than 30% lighter than a single-layer gypsum board of the same thickness. This inorganic active-passive Class A fire-resistant and thermally insulating integrated panel significantly improves the fire resistance limit of the enclosure system (integrated panel) by synergistically utilizing the active fire-resistant layer (gypsum) to absorb heat and release water vapor through chemical reaction under fire conditions and the passive fire-resistant layer to insulate heat through low thermal conductivity. In Example 1, the three-layer inorganic active-passive Class A fire-resistant and thermally insulating integrated panel has a fire resistance limit that is more than 20% higher than a single-layer gypsum board of the same thickness. Figure 11 and 12 The comparison shows that during active fire protection, the temperature of the first plateau period of the temperature rise curve of the three-layer inorganic active-passive Class A fireproof and thermal insulation integrated panel on the unexposed side is 0℃~30℃ lower than that of a single-layer gypsum board. The inorganic active-passive Class A fireproof and thermal insulation integrated panel of this embodiment has excellent thermal insulation performance, with a thermal conductivity as low as approximately 0.11W / (mK), which is more than 50% lower than that of a single-layer gypsum board of the same thickness. As shown in Table 1, the tensile bond strength of the inorganic active-passive Class A fireproof and thermal insulation integrated panel of this embodiment is all above 0.2MPa, and the material failure occurs only in the aerogel fiber board passive fireproof layer (thermal insulation layer), and not at the active fireproof layer or its interface with the passive fireproof layer, thus meeting the standard requirement of tensile bond strength ≥0.15MPa.
[0131] Table 1 Performance parameters of comparative examples and embodiments
[0132]
[0133] All comparative examples and embodiments passed the BS 476-4 non-combustibility test; according to the BS 476-7 test, the flame spread reached the highest safety level Class 1, which meets the corresponding requirements for Class A1 non-combustible materials in the national standard "Classification of Combustion Performance of Building Materials and Products" (GB8624).
[0134] Figure 1 The diagram and physical image show the gypsum board prepared for Comparative Example 1.
[0135] Figure 2 The diagram and physical image show the graphite-modified gypsum board prepared in Comparative Example 2.
[0136] Figure 3 The diagram and physical image show the gypsum board modified with fumed silica prepared in Comparative Example 3.
[0137] Figure 4The diagram and physical image show the double-layer fireproof and heat-insulating integrated panel prepared for Comparative Example 4.
[0138] Figure 5 The diagram and physical image show the double-layer graphite-modified fireproof and heat-insulating integrated board prepared for Comparative Example 5.
[0139] Figure 6 The diagram and physical image show the double-layer structure of the fumed silica-modified fireproof and heat-insulating integrated board prepared for Comparative Example 6.
[0140] Figure 7 The diagram and physical image show the inorganic active and passive Class A fireproof and heat-insulating integrated board prepared in Example 1.
[0141] Figure 8 A schematic diagram and a physical image of the unmodified inorganic active and passive Class A fireproof and thermal insulation integrated board prepared for Comparative Example 7.
[0142] Figure 9 Schematic diagram and physical image of the graphite-modified inorganic active and passive Class A fireproof and thermal insulation integrated board prepared for Comparative Example 8.
[0143] Figure 10 Schematic diagram and physical image of the inorganic active and passive Class A fireproof and heat-insulating integrated board modified with silica powder prepared for Comparative Example 9.
[0144] Figure 11 For comparison, the average temperature curve of the central region of the unexposed side during the combustion test; Figure 12 The following are the average temperature curves of the central region of the unexposed side during the combustion test for the examples and comparative examples; the average temperature of the central region of the unexposed side during the combustion test for all comparative examples and examples is shown below. Figure 11 and Figure 12 As shown in the figure, both single-layer gypsum board and double-layer integrated active-passive composite board exhibit a three-stage temperature rise pattern with a plateau period, while the three-layer integrated active-passive composite board exhibits a multi-stage, multi-plateau temperature rise pattern and significantly delays the temperature rise on the unexposed side.
[0145] Figure 13 The image shows the morphology of the central region of the flame-exposed surface of the specimen after natural cooling following the combustion test. After cooling to room temperature, the unexposed surfaces of all comparative examples and embodiments remained structurally intact without cracks. Cracks of varying degrees appeared on the flame-exposed surfaces, such as... Figure 13 As shown. By Figure 13 It is known that the modification method of adding gaseous silica can significantly reduce the thermal stress of the board, reduce the width and length of single cracks, effectively prevent the board from cracking after annealing (fire suppression), and improve safety.
Claims
1. A method for preparing an inorganic active and passive Class A fireproof and thermal insulation integrated panel, characterized in that... It is done in the following steps: I. Pouring the first active fireproof layer: ① Weigh out 0.25 to 2.5 parts of retarder, 0.25 to 2.5 parts of water-reducing agent, 0.125 to 1.25 parts of hydroxypropyl methylcellulose, 150 to 250 parts of water, 250 to 1000 parts of calcined gypsum powder, 0.1 to 50 parts of graphite powder, and 2.5 to 25 parts of chopped inorganic fibers according to the following mass percentages; ② Mix and dissolve 0.25 to 2.5 parts of retarder, 0.25 to 2.5 parts of water-reducing agent, 0.125 to 1.25 parts of hydroxypropyl methylcellulose and 150 to 250 parts of water to obtain solution I; ③ Stir 250 to 1000 parts of calcined gypsum powder, 0.1 to 50 parts of graphite powder and 2.5 to 25 parts of chopped inorganic fibers at low speed to obtain gypsum dry mixture I; ④ Pour the solution I into the gypsum dry mix I, stir at low speed first, then stir at high speed to obtain gypsum slurry I; ⑤ Pour gypsum slurry I into the mold to obtain a mold with a first active fireproof layer; II. Laying a passive fireproof layer: ① A hydrophobic agent is sprayed onto the surface of the porous inorganic fiber insulation board to obtain a hydrophobic insulation board; ② Lay a hydrophobically treated insulation board on the surface of the first active fireproof layer to obtain a mold with a first active fireproof layer / passive fireproof layer; III. Pouring the second active fireproof layer: ① Weigh out 0.25 to 2.5 parts of retarder, 0.25 to 2.5 parts of water-reducing agent, 0.125 to 1.25 parts of hydroxypropyl methylcellulose, 150 to 250 parts of water, 250 to 1000 parts of calcined gypsum powder, 0.1 to 50 parts of fumed silica powder, and 2.5 to 25 parts of chopped inorganic fibers according to the following mass percentages; ② Mix and dissolve 0.25 to 2.5 parts of retarder, 0.25 to 2.5 parts of water-reducing agent, 0.125 to 1.25 parts of hydroxypropyl methylcellulose and 150 to 250 parts of water to obtain solution II; ③ Stir 250 to 1000 parts of calcined gypsum powder, 0.1 to 50 parts of fumed silica powder and 2.5 to 25 parts of chopped inorganic fibers at low speed to obtain gypsum dry mix II; ④ Pour the solution II into the gypsum dry mix II, stir at low speed first, then stir at high speed to obtain gypsum slurry II; ⑤ Pour gypsum slurry II onto the surface of the insulation board after it has been treated with hydrophobicity to obtain a mold with a first active fireproof layer / passive fireproof layer / second active fireproof layer; IV. Maintenance: A plastic film is laid on the surface of the mold with the first active fireproof layer / passive fireproof layer / second active fireproof layer, then the top cover is placed on and pressure is applied for curing. Finally, the mold is removed and the plastic film is removed to obtain an inorganic active and passive Class A fireproof and heat-insulating integrated board.
2. The method for preparing an inorganic active and passive Class A fireproof and heat-insulating integrated panel according to claim 1, characterized in that... The retarder mentioned in Step 1① and Step 3① is sodium tripolyphosphate; the water-reducing agent mentioned in Step 1① and Step 3① is polycarboxylic acid, and the molecular weight of the polycarboxylic acid is 30,000~50,000; the chopped inorganic fibers mentioned in Step 1① and Step 3① are chopped glass fibers, aluminosilicate fibers, mullite fibers or alumina fibers; the length of the chopped inorganic fibers is 3mm~12mm.
3. The method for preparing an inorganic active and passive Class A fireproof and heat-insulating integrated panel according to claim 1, characterized in that... The graphite powder mentioned in step one ① is high-purity flake graphite powder; the particle size of the graphite powder is 3.4μm~6.5μm; the fumed silica powder mentioned in step three ① is hydrophilic fumed silica powder, with a particle size of 200nm~500nm and a specific surface area of 200m². 2 / g~500m 2 / g, the mass percentage of silicon dioxide is not less than 99.8%.
4. The method for preparing an inorganic active and passive Class A fireproof and heat-insulating integrated panel according to claim 1, characterized in that... The low-speed stirring mentioned in steps 1.3 and 3.3 specifically refers to stirring at a speed of 500 r / min to 800 r / min for 2 min to 5 min.
5. The method for preparing an inorganic active and passive Class A fireproof and heat-insulating integrated panel according to claim 1, characterized in that... The steps described in Step 1, Step 4 and Step 3, Step 4, specifically "stirring at low speed first and then at high speed," involve stirring at low speed for 1 to 2 minutes at a speed of 500 to 800 r / min, followed by stirring at high speed for 1 to 2 minutes at a speed of 1500 to 2000 r / min.
6. The method for preparing an inorganic active and passive Class A fireproof and heat-insulating integrated panel according to claim 1, characterized in that... The porous inorganic fiber insulation board mentioned in step 2① is an aerogel-alumina silicate fiber board, an aerogel-glass fiber board, an aerogel-alumina fiber board, an aerogel-mullite fiber board, an inorganic alumina silicate fiber board, an inorganic glass fiber board, an inorganic mullite fiber board, or a rock wool board; the thickness of the porous inorganic fiber insulation board mentioned in step 2① is 2mm~25mm.
7. The method for preparing an inorganic active and passive Class A fireproof and heat-insulating integrated panel according to claim 1, characterized in that... The hydrophobic agent mentioned in step 2① is an organosilicon hydrophobic agent, polysiloxane, potassium methylsilicate, water-based paraffin emulsion, or nanomaterial-modified fluorocarbon polymer.
8. The method for preparing an inorganic active and passive Class A fireproof and heat-insulating integrated panel according to claim 1, characterized in that... The spraying process described in step 2① is carried out as follows: blow away the surface of the porous inorganic fiber insulation board to remove surface delamination and easily detachable aerogel powder; preheat the porous inorganic fiber insulation board for 10 to 30 minutes at a temperature of 45 to 60°C; then, at room temperature, use a spray bottle with a nozzle diameter of 0.2 mm to 0.5 mm to evenly spray the hydrophobic agent onto the surface of the porous inorganic fiber insulation board in an atomizing spraying manner; finally, cure at room temperature.
9. The method for preparing an inorganic active and passive Class A fireproof and heat-insulating integrated panel according to claim 1, characterized in that... Step 1, ⑤: Pour gypsum slurry I into the mold to a thickness of 2mm~10mm; Step 3, ⑤: Pour gypsum slurry II onto the surface of the hydrophobic insulation board to a thickness of 2mm~10mm.
10. The method for preparing an inorganic active and passive Class A fireproof and heat-insulating integrated panel according to claim 1, characterized in that... The pressure curing described in step four is specifically carried out under the conditions of temperature of 40℃~60℃, humidity of 30%RH~60%RH and pressure of 1MPa~5MPa for 12h~24h.
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