Ultra-light flame-retardant sound absorption and insulation board and preparation method thereof

By optimizing raw material selection and process, combined with the characteristics of closed-cell hollow foamed microbead particles and glass fiber mesh cloth, an ultra-lightweight flame-retardant sound-absorbing and sound-absorbing plate was prepared, solving the problem that existing sound-absorbing and insulation materials are difficult to achieve light weight, and achieving ultra-lightweight and excellent acoustic and fire-resistant properties of the plate.

CN119974592APending Publication Date: 2025-05-13HUAYAN SPACE (BEIJING) INTERNATIONAL ARCHITECTURAL DESIGN CO LTD
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Patent Information

Application Number
CN202510158056.8
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-02-13
Publication Date
2025-05-13

AI Technical Summary

Technical Problem

While ensuring acoustic performance and fire-retardant flame retardant properties, existing sound insulation materials are difficult to achieve light weight, especially on the ceiling decoration surfaces of large public buildings and large-span structures, which increases transportation and installation costs and poses a great burden on the building structure.

Method used

By optimizing raw material selection and process, the lightweight properties of closed-cell hollow foamed microbead particles are maximized, and combined with the enhancement effect of glass fiber mesh cloth, an ultra-lightweight flame retardant sound insulation plate is prepared. The plate consists of closed-cell hollow foamed microbead particles, modified epoxy resin, nanosilica aerogel, flame retardant, surface modifier and additive. Through specific proportions and process treatment, the plate is ultra-lightweight.

Benefits of technology

The ultra-lightweight properties of the sound-absorbing insulation board are achieved, and the weight can be reduced by 50% to 70%, while maintaining excellent sound absorption, sound insulation and fire-retardant flame retardant performance. The noise reduction coefficient can reach 0.8~0.95, and the average sound insulation volume can reach 30~40dB. It meets various acoustic environment needs and has Class A fire resistance and good mechanical properties.

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Abstract

The invention discloses an ultra-light flame-retardant sound absorption and insulation board which is sequentially composed of a first glass fiber gridding cloth layer, an ultra-light flame-retardant sound absorption and insulation board layer and a second glass fiber gridding cloth layer from inside to outside. Wherein the ultra-light flame-retardant sound absorption and insulation board layer is formed by uniformly stirring 65-80 parts of closed-cell hollow foaming microbead particles, 10-15 parts of modified epoxy resin, 3-6 parts of nano silicon dioxide aerogel, 2-4 parts of a flame retardant, 1-2 parts of a surface modifier and 0.3-1 part of an auxiliary agent. The invention further discloses a preparation method of the ultra-light flame-retardant sound absorption and insulation board. The preparation method comprises the following steps: (1) raw material pretreatment; (2) mixing the ingredients; (3) forming; and (4) post-treatment. The invention has the following beneficial effects: 1, the light weight is ultra-light; 2, the sound absorption and insulation performance is excellent; 3, high-efficiency fireproof and flame-retardant properties are realized; 4, high strength and high stability; and 5, the environment-friendly and weather-resistant properties are good.
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Description

Technical Field

[0001] The invention relates to the fields of acoustic materials and building fireproof materials, and in particular to an ultra-light flame-retardant sound-absorbing and insulating board using specific closed-cell hollow foamed microbead particles as aggregate and reinforced with glass fiber mesh cloth, and a preparation method thereof. Background Art

[0002] With the development of construction and industry, the requirements for sound-absorbing and sound-insulating materials are constantly increasing. Chinese invention patent application CN104177114A discloses a microporous rock sound-absorbing and sound-insulating board, the board body of which is composed of rock particles and polyester silicon adhesive in a weight ratio of 1: (0.01-0.3); the polyester silicon adhesive is composed of methyl silane 2.5-3.5%, sodium silicate 25-27%, calcium silicate 3.5-4.5%, fumed silica 7.5-8.5%, dibutyl tin dilaurate 0.003-0.005%, triethanolamine 5.5-6.5%, epoxy resin 8.5-9.5%, feldspar powder 5.5-6.5%, glyceride 3.5-4.5%, dimethylformamide 2.5-3.5%, and the balance is silicon tripolyphosphate; the board body is provided with reinforcement. Although the above-mentioned materials must have good acoustic properties and fire retardant properties, how to achieve lightweight while ensuring the acoustic properties and fire retardant properties has also become a key requirement.

[0003] Traditional sound-absorbing and insulating materials (such as the microporous rock sound-absorbing and insulating board disclosed in the above-mentioned Chinese invention patent application CN104177114A) often have a great disadvantage in weight, especially for ceiling decoration surfaces of large public buildings and large-span structures, which not only increases transportation and installation costs, but also imposes a heavy burden on the building structure.

[0004] Closed-cell hollow foamed microspheres have the potential to be lightweight, but how to further reduce the weight of the board while ensuring acoustic performance and fire retardant properties and achieve lightweight flame retardant sound-absorbing and sound-insulating boards has become a technical problem that needs to be solved urgently. Summary of the invention

[0005] Purpose of the invention: In view of the above-mentioned deficiencies in the prior art, the present invention discloses an ultra-lightweight flame-retardant sound-absorbing and insulating board and a preparation method thereof.

[0006] The present invention optimizes the selection of raw materials and processes to maximize the lightweight characteristics of closed-cell hollow foamed microsphere particles, and combines the reinforcing effect of glass fiber mesh cloth to enable the board to be ultra-lightweight while having excellent sound absorption, sound insulation and fire retardant properties.

[0007] Technical solution: An ultra-light flame-retardant sound-absorbing and insulating board, which is composed of a first glass fiber mesh cloth layer, an ultra-light flame-retardant sound-absorbing and insulating board layer and a second glass fiber mesh cloth layer from the inside to the outside, wherein:

[0008] The ultra-light flame-retardant sound-absorbing and insulating board layer is prepared by uniformly mixing 65-80 parts of closed-cell hollow foamed microbead particles, 10-15 parts of modified epoxy resin, 3-6 parts of nano-silicon dioxide aerogel, 2-4 parts of flame retardant, 1-2 parts of surface modifier and 0.3-1 part of auxiliary agent.

[0009] Furthermore, the particle size of the closed-cell hollow foamed microsphere particles is 30 to 60 meshes. The closed-cell hollow foamed microsphere particles with low density are selected, and their unique structure provides an excellent lightweight foundation for the board, while having certain sound insulation and sound absorption properties.

[0010] Modified epoxy resin is used because it has good bonding properties and high temperature resistance, can maintain structural stability in high temperature environments, and ensure the overall performance of the board.

[0011] Furthermore, the first glass fiber mesh cloth layer and the second glass fiber mesh cloth layer are both made of the same light-weight and high-strength glass fiber mesh cloth. The main function of the first glass fiber mesh cloth layer and the second glass fiber mesh cloth layer is to significantly enhance the tensile strength and overall stability of the board without significantly increasing the weight of the board, and prevent the board from cracking during use.

[0012] Furthermore, the performance parameters of the lightweight and high-strength glass fiber mesh cloth are as follows:

[0013] The weight is 80-100 g / m2; the mesh size is 20×20 mm; the alkali-resistant breaking strength is 3000-5000 N / 50 mm.

[0014] Nano-silica aerogel is used because it has an extremely high specific surface area and a special pore structure, which can effectively improve the sound absorption performance of the sound-absorbing panel and optimize the acoustic effect.

[0015] Furthermore, the flame retardant is an intumescent environmentally friendly flame retardant, and the intumescent environmentally friendly flame retardant is one of ammonium polyphosphate (APP) and phosphate ester. The intumescent environmentally friendly flame retardant can form an intumescent heat-insulating layer when heated, enhance the flame retardant performance of the board, and is environmentally friendly.

[0016] Furthermore, the phosphate ester is one or more of tricresyl phosphate, triethyl phosphate or triphenyl phosphate.

[0017] Furthermore, the surface modifier is one of a silane coupling agent and a titanate coupling agent. The surface modifier is used to improve the interface bonding force between the closed-cell hollow foamed microsphere particles and the modified epoxy resin, thereby improving the comprehensive performance of the board.

[0018] Furthermore, the auxiliary agent is composed of a high-efficiency dispersant and a defoamer, and the mass ratio of the high-efficiency dispersant to the defoamer is (3-5): 1. The auxiliary agent ensures that the raw materials are evenly dispersed during the mixing process, improves the processing performance and use performance, and ensures the stability of the board quality.

[0019] Furthermore, the high-efficiency dispersant is one of polycarboxylate and phosphate.

[0020] Furthermore, the polycarboxylate is one of sodium polyacrylate, polyacrylic acid amine, polyepoxysuccinic acid, and sodium dodecyl sulfate.

[0021] Furthermore, the phosphate ester is one of fatty alcohol polyoxyethylene ether phosphate and alkylphenol polyoxyethylene ether phosphate.

[0022] Furthermore, the defoamer is a commercially available high-efficiency silicone defoamer, which is one of BYK-016 defoamer, BYK-024 defoamer, and BASF DF-2800 defoamer.

[0023] Furthermore, the thickness of the ultra-light flame-retardant sound-absorbing and insulating board layer is 0.8 to 1.5 cm.

[0024] The method for preparing the ultra-light flame-retardant sound-absorbing and sound-insulating board described in any one of the above items comprises the following steps:

[0025] (1) Raw material pretreatment:

[0026] (11) drying the closed-cell hollow foamed microsphere particles at at least 70° C., preferably 70 to 90° C., for at least 1 hour, preferably 1 to 2 hours, to remove moisture and impurities on the surface of the closed-cell hollow foamed microsphere particles and improve the bonding effect between the closed-cell hollow foamed microsphere particles and the modified epoxy resin;

[0027] (12) Cutting the lightweight and high-strength glass fiber mesh cloth to make its size match the size of the mold to obtain the first / second glass fiber mesh cloth layer, and cleaning its surface to remove oil and dust to ensure good combination with other raw materials;

[0028] (2) Mixing ingredients:

[0029] (21) First, add a formulated amount of modified epoxy resin, a formulated amount of surface modifier, and a formulated amount of auxiliary agent into a high-speed mixer, and stir evenly to form a uniform binder system;

[0030] (22) slowly adding the closed-cell hollow foamed microsphere particles dried in step (11) into a high-speed mixer, keeping the stirring speed constant, and continuing to stir with the binder system for at least 6 minutes, preferably 6 to 8 minutes, to form a uniform first mixture;

[0031] (23) adding a formulated amount of nano-silica aerogel and a formulated amount of flame retardant into a high-speed mixer, and stirring evenly to obtain a second mixture;

[0032] (3) Molding:

[0033] (31) Laying a first glass fiber mesh cloth layer on the bottom of the mold, pouring an appropriate amount of the second mixed material obtained in step (2) into the mold and placing it above the first glass fiber mesh cloth layer, laying it flat, and then laying a second glass fiber mesh cloth layer on the surface;

[0034] (32), placing the mold processed in step (31) on a vibration table, vibrating it at a certain frequency for a period of time, and then proceeding to step (33);

[0035] (33), placing the mold processed in step (32) on a press, and compacting it under a certain pressure for a period of time;

[0036] (4) Post-processing:

[0037] The mold treated in step (3) is dried at a certain temperature for a period of time to set the shape, and then demoulded and polished to obtain an ultra-light flame-retardant sound-absorbing and insulating board.

[0038] Furthermore, the rotation speed of the high-speed stirrer in step (21) is at least 800 rpm, preferably 800-1000 rpm; and the stirring time is at least 2 minutes, preferably 2-4 minutes.

[0039] Furthermore, the rotation speed of the high-speed stirrer in step (22) is at least 400 rpm, preferably 400-600 rpm; and the stirring time is at least 3 minutes, preferably 3-5 minutes.

[0040] Furthermore, in step (32), the vibration frequency of the vibration table is at least 30 Hz, preferably 30 to 50 Hz;

[0041] The vibration time of the vibration table in step (32) is at least 2 minutes, preferably 2 to 4 minutes. The vibration makes the material in the mold more compact and uniform.

[0042] Furthermore, in step (33), the mold is compacted and formed by a press machine at a pressure of at least 1 MPa, preferably 1-3 MPa, and the pressure holding time is at least 3 minutes, preferably 3-6 minutes, to ensure that the first / second glass fiber mesh cloth layer is tightly combined with the second mixed material to enhance the structural strength of the board.

[0043] Furthermore, in step (4), hot air circulation drying equipment is used for drying;

[0044] In step (4), hot air at a temperature of at least 90° C., preferably 90 to 110° C., is used for drying and shaping, and the drying time is at least 60 minutes, preferably 60 to 80 minutes. Under the action of hot air, the modified epoxy resin is further cured, the structure of the board is more stable, and the mechanical properties and fire resistance are improved.

[0045] Beneficial effects: The ultra-light flame-retardant sound-absorbing and insulating board and its preparation method disclosed in the present invention have the following advantages:

[0046] Beneficial effects:

[0047] 1. Super light weight characteristics - the optimized closed-cell hollow foamed microspheres have increased particle size and density (controlled at 200Kg / m 3 ) is more suitable, which greatly reduces the weight of the sound-absorbing and sound-insulating panels compared to traditional products, and can reduce the weight by 50% to 70%, which greatly facilitates transportation and installation and reduces the load on the building structure;

[0048] 2. Excellent sound absorption and sound insulation performance - the addition of nano-silica aerogel and reasonable structural design make the sound absorption and insulation board have excellent sound absorption performance in the medium, low and high frequency ranges, and the noise reduction coefficient (NRC) can reach 0.8 to 0.95; good sound insulation performance can effectively block the propagation of sound, and the average sound insulation can reach 30 to 40dB, meeting the needs of various acoustic environments;

[0049] 3. Highly effective fire retardant performance - the synergistic effect of modified epoxy resin and flame retardant, as well as the stable structure of glass fiber mesh cloth at high temperature, make the fire resistance of the board reach Class A standard, which can effectively prevent the spread of flames and reduce fire losses when a fire occurs;

[0050] 4. High strength and high stability - the reinforcing effect of the glass fiber mesh cloth ensures that the sound-absorbing and insulating board has good tensile strength, compressive strength and impact resistance. It is not easy to deform or damage during use, and can maintain stable performance for a long time, thus improving the service life and reliability of the product;

[0051] 5. Environmental protection and good weather resistance - Environmentally friendly raw materials are used in the preparation process to reduce pollution to the environment. At the same time, the board has good weather resistance after post-processing, and can resist the influence of natural factors such as ultraviolet rays, temperature changes, humidity, etc., and maintain its stable performance for a long time. BRIEF DESCRIPTION OF THE DRAWINGS

[0052] Figure 1 The present invention is a flow chart of a method for preparing an ultra-light flame-retardant sound-absorbing and sound-insulating board. DETAILED DESCRIPTION

[0053] The specific embodiments of the present invention are described in detail below.

[0054] The "range" disclosed in the present invention is defined in the form of a lower limit and an upper limit, and a given range is defined by selecting a lower limit and an upper limit, and the selected lower limit and upper limit define the boundaries of the particular range. The range defined in this way can be inclusive or exclusive of the end values, and can be arbitrarily combined, that is, any lower limit can be combined with any upper limit to form a range. For example, if a range of 10 to 50 is listed for a specific parameter, it is understood that the range of 10 to 40 and 20 to 50 is also expected. In addition, if the minimum range values ​​1 and 2 are listed, and if the maximum range values ​​3, 4 and 5 are listed, the following ranges can all be expected: 1 to 3, 1 to 4, 1 to 5, 2 to 3, 2 to 4 and 2 to 5. In this application, unless otherwise specified, the range of values ​​"a to b" represents an abbreviation of any real number combination between a and b, where a and b are both real numbers. For example, the range of values ​​"0 to 5" means that all real numbers between "0 to 5" have been fully listed in this article, and "0 to 5" is only an abbreviation of these numerical combinations.

[0055] Unless otherwise specified, all embodiments and optional embodiments of the present application can be combined with each other to form a new technical solution.

[0056] Unless otherwise specified, all technical features and optional technical features of this application can be combined with each other to form a new technical solution.

[0057] If there is no special explanation, all steps of the present application can be performed sequentially or randomly, preferably sequentially. For example, the method includes steps (a) and (b), which means that the method may include steps (a) and (b) performed sequentially, or may include steps (b) and (a) performed sequentially. For example, the method may further include step (c), which means that step (c) may be added to the method in any order. For example, the method may include steps (a), (b) and (c), or may include steps (a), (c) and (b), or may include steps (c), (a) and (b), etc.

[0058] If there is no special explanation, the "include" and "comprising" mentioned in this application are open-ended or closed-ended. For example, the "include" and "comprising" may mean that other components not listed may also be included or only the listed components may be included or only the listed components may be included.

[0059] Unless otherwise specified, the reaction is carried out at room temperature and pressure.

[0060] Unless otherwise specified, all parts or percentages are by weight.

[0061] In the present invention, all substances used are known substances and can be purchased or synthesized by known methods.

[0062] In the present invention, the devices or equipment used are all conventional devices or equipment known in the art and are commercially available.

[0063] An ultra-light flame-retardant sound-absorbing and insulating board is composed of a first glass fiber mesh cloth layer, an ultra-light flame-retardant sound-absorbing and insulating board layer, and a second glass fiber mesh cloth layer from the inside to the outside, wherein:

[0064] The ultra-light flame-retardant sound-absorbing and insulating board layer is prepared by uniformly mixing 65-80 parts of closed-cell hollow foamed microbead particles, 10-15 parts of modified epoxy resin, 3-6 parts of nano-silicon dioxide aerogel, 2-4 parts of flame retardant, 1-2 parts of surface modifier and 0.3-1 part of auxiliary agent.

[0065] Furthermore, the particle size of the closed-cell hollow foamed microsphere particles is 30 to 60 meshes.

[0066] Furthermore, the first glass fiber mesh cloth layer and the second glass fiber mesh cloth layer are both made of the same light-weight and high-strength glass fiber mesh cloth.

[0067] Furthermore, the performance parameters of the lightweight and high-strength glass fiber mesh cloth are as follows:

[0068] The weight is 80-100 g / m2; the mesh size is 20×20 mm; the alkali-resistant breaking strength is 3000-5000 N / 50 mm.

[0069] Furthermore, the flame retardant is an intumescent environmentally friendly flame retardant, and the intumescent environmentally friendly flame retardant is one of ammonium polyphosphate and phosphate ester.

[0070] Furthermore, the phosphate ester is one of tricresyl phosphate, triethyl phosphate or triphenyl phosphate.

[0071] Furthermore, the surface modifier is one of a silane coupling agent and a titanate coupling agent.

[0072] Furthermore, the auxiliary agent is composed of a high-efficiency dispersant and a defoaming agent, and the mass ratio of the high-efficiency dispersant to the defoaming agent is (3-5):1.

[0073] Furthermore, the high-efficiency dispersant is one of polycarboxylate and phosphate.

[0074] Furthermore, the polycarboxylate is one of sodium polyacrylate, polyacrylic acid amine, polyepoxysuccinic acid, and sodium dodecyl sulfate.

[0075] Furthermore, the phosphate ester is one of fatty alcohol polyoxyethylene ether phosphate and alkylphenol polyoxyethylene ether phosphate.

[0076] Furthermore, the defoamer is a commercially available high-efficiency silicone defoamer, which is one of BYK-016 defoamer, BYK-024 defoamer, and BASF DF-2800 defoamer.

[0077] Furthermore, the thickness of the ultra-light flame-retardant sound-absorbing and insulating board layer is 0.8 to 1.5 cm.

[0078] The method for preparing the ultra-light flame-retardant sound-absorbing and sound-insulating board described in any one of the above items comprises the following steps:

[0079] (1) Raw material pretreatment:

[0080] (11) drying the closed-cell hollow foamed microsphere particles at at least 70° C., preferably 70 to 90° C., for at least 1 hour, preferably 1 to 2 hours;

[0081] (12) cutting the lightweight and high-strength glass fiber mesh cloth to make its size match the size of the mold to obtain the first / second glass fiber mesh cloth layer, and performing surface cleaning treatment on the same;

[0082] (2) Mixing ingredients:

[0083] (21) First, add a formulated amount of modified epoxy resin, a formulated amount of surface modifier, and a formulated amount of auxiliary agent into a high-speed mixer, and stir evenly to form a uniform binder system;

[0084] (22) slowly adding the closed-cell hollow foamed microsphere particles dried in step (11) into a high-speed mixer, keeping the stirring speed constant, and continuing to stir with the binder system for at least 6 minutes, preferably 6 to 8 minutes, to form a uniform first mixture;

[0085] (23) adding a formulated amount of nano-silica aerogel and a formulated amount of flame retardant into a high-speed mixer, and stirring evenly to obtain a second mixture;

[0086] (3) Molding:

[0087] (31) Laying a first glass fiber mesh cloth layer on the bottom of the mold, pouring an appropriate amount of the second mixed material obtained in step (2) into the mold and placing it above the first glass fiber mesh cloth layer, laying it flat, and then laying a second glass fiber mesh cloth layer on the surface;

[0088] (32), placing the mold processed in step (31) on a vibration table, vibrating it at a certain frequency for a period of time, and then proceeding to step (33);

[0089] (33), placing the mold processed in step (32) on a press, and compacting it under a certain pressure for a period of time;

[0090] (4) Post-processing:

[0091] The mold treated in step (3) is dried at a certain temperature for a period of time to set the shape, and then demoulded and polished to obtain an ultra-light flame-retardant sound-absorbing and insulating board.

[0092] Furthermore, the rotation speed of the high-speed stirrer in step (21) is at least 800 rpm, preferably 800-1000 rpm; and the stirring time is at least 2 minutes, preferably 2-4 minutes.

[0093] Furthermore, the rotation speed of the high-speed stirrer in step (22) is at least 400 rpm, preferably 400-600 rpm; and the stirring time is at least 3 minutes, preferably 3-5 minutes.

[0094] Furthermore, in step (32), the vibration frequency of the vibration table is at least 30 Hz, preferably 30 to 50 Hz;

[0095] The vibration time of the vibration table in step (32) is at least 2 minutes, preferably 2 to 4 minutes.

[0096] Furthermore, in step (33), the mold is compacted and molded by a press machine at a pressure of at least 1 MPa, preferably 1 to 3 MPa, and the holding time is at least 3 minutes, preferably 3 to 6 minutes.

[0097] Furthermore, in step (4), hot air circulation drying equipment is used for drying;

[0098] In step (4), hot air at a temperature of at least 90° C., preferably 90 to 110° C., is used for drying and shaping, and the drying time is at least 60 minutes, preferably 60 to 80 minutes.

[0099] In one embodiment:

[0100] An ultra-light flame-retardant sound-absorbing and insulating board is composed of a first glass fiber mesh cloth layer, an ultra-light flame-retardant sound-absorbing and insulating board layer, and a second glass fiber mesh cloth layer from the inside to the outside, wherein:

[0101] The ultra-light flame-retardant sound-absorbing and insulating board layer is prepared by uniformly mixing 65 parts of closed-cell hollow foamed microsphere particles, 10 parts of modified epoxy resin, 3 parts of nano-silicon dioxide aerogel, 2 parts of flame retardant, 1 part of surface modifier and 0.3 parts of auxiliary agent.

[0102] Furthermore, the particle size of the closed-cell hollow foamed microsphere particles is 30 meshes.

[0103] Furthermore, the first glass fiber mesh cloth layer and the second glass fiber mesh cloth layer are both made of the same light-weight and high-strength glass fiber mesh cloth.

[0104] Furthermore, the performance parameters of the lightweight and high-strength glass fiber mesh cloth are as follows:

[0105] Weight: 80g / m2; mesh size: 20×20mm; alkali-resistant breaking strength: 3000N / 50mm.

[0106] Furthermore, the flame retardant is an intumescent environmentally friendly flame retardant, and the intumescent environmentally friendly flame retardant is ammonium polyphosphate.

[0107] Furthermore, the surface modifier is a silane coupling agent.

[0108] Furthermore, the auxiliary agent consists of a high-efficiency dispersant and a defoamer, and the mass ratio of the high-efficiency dispersant to the defoamer is 3:1.

[0109] Furthermore, the high-efficiency dispersant is a polycarboxylate.

[0110] Furthermore, the polycarboxylate is sodium polyacrylate. In other embodiments, the polycarboxylate is polyacrylic acid amine. In other embodiments, the polycarboxylate is polyepoxysuccinic acid. In other embodiments, the polycarboxylate is sodium dodecyl sulfate.

[0111] Furthermore, the defoamer is a commercially available high-efficiency silicone defoamer, which is BYK-016 defoamer.

[0112] Furthermore, the thickness of the ultra-light flame-retardant sound-absorbing and insulating board layer is 0.8 cm.

[0113] The method for preparing the ultra-light flame-retardant sound-absorbing and sound-insulating board described in any one of the above items comprises the following steps:

[0114] (1) Raw material pretreatment:

[0115] (11) drying the closed-cell hollow foamed microsphere particles at 70° C. for 2 hours;

[0116] (12) cutting the lightweight and high-strength glass fiber mesh cloth to make its size match the size of the mold to obtain the first / second glass fiber mesh cloth layer, and performing surface cleaning treatment on the same;

[0117] (2) Mixing ingredients:

[0118] (21) First, add a formulated amount of modified epoxy resin, a formulated amount of surface modifier, and a formulated amount of auxiliary agent into a high-speed mixer, and stir evenly to form a uniform binder system;

[0119] (22) slowly adding the closed-cell hollow foamed microsphere particles dried in step (11) into a high-speed mixer, keeping the stirring speed constant, and continue stirring with the binder system for 6 minutes to form a uniform first mixture;

[0120] (23) adding a formulated amount of nano-silica aerogel and a formulated amount of flame retardant into a high-speed mixer, and stirring evenly to obtain a second mixture;

[0121] (3) Molding:

[0122] (31) Laying a first glass fiber mesh cloth layer on the bottom of the mold, pouring an appropriate amount of the second mixed material obtained in step (2) into the mold and placing it above the first glass fiber mesh cloth layer, laying it flat, and then laying a second glass fiber mesh cloth layer on the surface;

[0123] (32), placing the mold processed in step (31) on a vibration table, vibrating it at a certain frequency for a period of time, and then proceeding to step (33);

[0124] (33), placing the mold processed in step (32) on a press, and compacting it under a certain pressure for a period of time;

[0125] (4) Post-processing:

[0126] The mold treated in step (3) is dried at a certain temperature for a period of time to set the shape, and then demoulded and polished to obtain an ultra-light flame-retardant sound-absorbing and insulating board.

[0127] Furthermore, the rotation speed of the high-speed stirrer in step (21) is 800 rpm; and the stirring time is 4 minutes.

[0128] Furthermore, the rotation speed of the high-speed stirrer in step (22) is 400 rpm; and the stirring time is 5 minutes.

[0129] Furthermore, in step (32), the vibration frequency of the vibration table is 30 Hz;

[0130] The vibration time of the vibration table in step (32) is 4 minutes.

[0131] Furthermore, in step (33), the mold is compacted and formed by a press machine at a pressure of 1 MPa, and the holding time is 6 minutes.

[0132] Furthermore, in step (4), hot air circulation drying equipment is used for drying; in step (4), hot air at 90° C. is used for drying and shaping, and the drying time is 80 minutes.

[0133] In another embodiment:

[0134] An ultra-light flame-retardant sound-absorbing and insulating board is composed of a first glass fiber mesh cloth layer, an ultra-light flame-retardant sound-absorbing and insulating board layer, and a second glass fiber mesh cloth layer from the inside to the outside, wherein:

[0135] The ultra-light flame-retardant sound-absorbing and insulating board layer is prepared by uniformly mixing 80 parts of closed-cell hollow foamed microbead particles, 15 parts of modified epoxy resin, 6 parts of nano-silicon dioxide aerogel, 4 parts of flame retardant, 2 parts of surface modifier and 1 part of auxiliary agent.

[0136] Furthermore, the particle size of the closed-cell hollow foamed microsphere particles is 60 meshes.

[0137] Furthermore, the first glass fiber mesh cloth layer and the second glass fiber mesh cloth layer are both made of the same light-weight and high-strength glass fiber mesh cloth.

[0138] Furthermore, the performance parameters of the lightweight and high-strength glass fiber mesh cloth are as follows:

[0139] Weight: 100 g / m2; mesh size: 20×20 mm; alkali-resistant breaking strength: 5000 N / 50 mm.

[0140] Furthermore, the flame retardant is an intumescent environmentally friendly flame retardant, and the intumescent environmentally friendly flame retardant is a phosphate ester.

[0141] Furthermore, the phosphate ester is tricresyl phosphate. In other embodiments, the phosphate ester is triethyl phosphate. In other embodiments, the phosphate ester is triphenyl phosphate.

[0142] Furthermore, the surface modifier is a titanate coupling agent.

[0143] Furthermore, the auxiliary agent consists of a high-efficiency dispersant and a defoaming agent, and the mass ratio of the high-efficiency dispersant to the defoaming agent is 5:1.

[0144] Furthermore, the high-efficiency dispersant is a phosphate ester.

[0145] Furthermore, the phosphate ester is fatty alcohol polyoxyethylene ether phosphate. In other embodiments, the phosphate ester is alkylphenol polyoxyethylene ether phosphate.

[0146] Furthermore, the defoamer is a commercially available high-efficiency silicone defoamer, which is BYK-024 defoamer.

[0147] Furthermore, the thickness of the ultra-light flame-retardant sound-absorbing and insulating board layer is 1.5 cm.

[0148] The method for preparing the ultra-light flame-retardant sound-absorbing and sound-insulating board described in any one of the above items comprises the following steps:

[0149] (1) Raw material pretreatment:

[0150] (11) drying the closed-cell hollow foamed microsphere particles at 90° C. for 1 hour;

[0151] (12) cutting the lightweight and high-strength glass fiber mesh cloth to make its size match the size of the mold to obtain the first / second glass fiber mesh cloth layer, and performing surface cleaning treatment on the same;

[0152] (2) Mixing ingredients:

[0153] (21) First, add a formulated amount of modified epoxy resin, a formulated amount of surface modifier, and a formulated amount of auxiliary agent into a high-speed mixer, and stir evenly to form a uniform binder system;

[0154] (22) slowly adding the closed-cell hollow foamed microsphere particles dried in step (11) into a high-speed mixer, keeping the stirring speed constant, and continue stirring with the binder system for 8 minutes to form a uniform first mixture;

[0155] (23) adding a formulated amount of nano-silica aerogel and a formulated amount of flame retardant into a high-speed mixer, and stirring evenly to obtain a second mixture;

[0156] (3) Molding:

[0157] (31) Laying a first glass fiber mesh cloth layer on the bottom of the mold, pouring an appropriate amount of the second mixed material obtained in step (2) into the mold and placing it above the first glass fiber mesh cloth layer, laying it flat, and then laying a second glass fiber mesh cloth layer on the surface;

[0158] (32), placing the mold processed in step (31) on a vibration table, vibrating it at a certain frequency for a period of time, and then proceeding to step (33);

[0159] (33), placing the mold processed in step (32) on a press, and compacting it under a certain pressure for a period of time;

[0160] (4) Post-processing:

[0161] The mold treated in step (3) is dried at a certain temperature for a period of time to set the shape, and then demoulded and polished to obtain an ultra-light flame-retardant sound-absorbing and insulating board.

[0162] Furthermore, the rotation speed of the high-speed stirrer in step (21) is 1000 rpm; and the stirring time is 2 minutes.

[0163] Furthermore, the rotation speed of the high-speed stirrer in step (22) is 600 rpm; and the stirring time is 3 minutes.

[0164] Furthermore, in step (32), the vibration frequency of the vibration table is 50 Hz;

[0165] The vibration time of the vibration table in step (32) is 2 minutes.

[0166] Furthermore, in step (33), the mold is compacted and formed by a press machine at a pressure of 3 MPa, and the holding time is 3 minutes.

[0167] Furthermore, in step (4), hot air circulation drying equipment is used for drying; in step (4), hot air at 110° C. is used for drying and shaping, and the drying time is 60 minutes.

[0168] In yet another embodiment:

[0169] An ultra-light flame-retardant sound-absorbing and insulating board is composed of a first glass fiber mesh cloth layer, an ultra-light flame-retardant sound-absorbing and insulating board layer, and a second glass fiber mesh cloth layer from the inside to the outside, wherein:

[0170] The ultra-light flame-retardant sound-absorbing and insulating board layer is prepared by uniformly mixing 70 parts of closed-cell hollow foamed microsphere particles, 12 parts of modified epoxy resin, 4 parts of nano-silicon dioxide aerogel, 3 parts of flame retardant, 1.5 parts of surface modifier and 0.5 parts of auxiliary agent.

[0171] Furthermore, the particle size of the closed-cell hollow foamed microsphere particles is 40 meshes.

[0172] Furthermore, the first glass fiber mesh cloth layer and the second glass fiber mesh cloth layer are both made of the same light-weight and high-strength glass fiber mesh cloth.

[0173] Furthermore, the performance parameters of the lightweight and high-strength glass fiber mesh cloth are as follows:

[0174] Weight: 90g / m2; mesh size: 20×20mm; alkali-resistant breaking strength: 4000N / 50mm.

[0175] Furthermore, the flame retardant is an intumescent environmentally friendly flame retardant, and the intumescent environmentally friendly flame retardant is ammonium polyphosphate.

[0176] Furthermore, the phosphate ester is triphenyl phosphate.

[0177] Furthermore, the auxiliary agent consists of a high-efficiency dispersant and a defoaming agent, and the mass ratio of the high-efficiency dispersant to the defoaming agent is 4:1.

[0178] Furthermore, the high-efficiency dispersant is a polycarboxylate.

[0179] Furthermore, the polycarboxylate is polyepoxysuccinic acid.

[0180] Furthermore, the defoamer is a commercially available high-efficiency silicone defoamer, which is BASF DF-2800 defoamer.

[0181] Furthermore, the thickness of the ultra-light flame-retardant sound-absorbing and insulating board layer is 1 cm.

[0182] The method for preparing the ultra-light flame-retardant sound-absorbing and sound-insulating board described in any one of the above items comprises the following steps:

[0183] (1) Raw material pretreatment:

[0184] (11) drying the closed-cell hollow foamed microsphere particles at 80° C. for 1.5 hours;

[0185] (12) cutting the lightweight and high-strength glass fiber mesh cloth to make its size match the size of the mold to obtain the first / second glass fiber mesh cloth layer, and performing surface cleaning treatment on the same;

[0186] (2) Mixing ingredients:

[0187] (21) First, add a formulated amount of modified epoxy resin, a formulated amount of surface modifier, and a formulated amount of auxiliary agent into a high-speed mixer, and stir evenly to form a uniform binder system;

[0188] (22) slowly adding the closed-cell hollow foamed microsphere particles dried in step (11) into a high-speed mixer, keeping the stirring speed constant, and continue stirring with the binder system for 7 minutes to form a uniform first mixture;

[0189] (23) adding a formulated amount of nano-silica aerogel and a formulated amount of flame retardant into a high-speed mixer, and stirring evenly to obtain a second mixture;

[0190] (3) Molding:

[0191] (31) Laying a first glass fiber mesh cloth layer on the bottom of the mold, pouring an appropriate amount of the second mixed material obtained in step (2) into the mold and placing it above the first glass fiber mesh cloth layer, laying it flat, and then laying a second glass fiber mesh cloth layer on the surface;

[0192] (32), placing the mold processed in step (31) on a vibration table, vibrating it at a certain frequency for a period of time, and then proceeding to step (33);

[0193] (33), placing the mold processed in step (32) on a press, and compacting it under a certain pressure for a period of time;

[0194] (4) Post-processing:

[0195] The mold treated in step (3) is dried at a certain temperature for a period of time to set the shape, and then demoulded and polished to obtain an ultra-light flame-retardant sound-absorbing and insulating board.

[0196] Furthermore, the rotation speed of the high-speed stirrer in step (21) is 900 rpm; and the stirring time is 3 minutes.

[0197] Furthermore, the rotation speed of the high-speed stirrer in step (22) is 500 rpm; and the stirring time is 4 minutes.

[0198] Further, in step (32), the vibration frequency of the vibration table is 40 Hz;

[0199] The vibration time of the vibration table in step (32) is 3 minutes.

[0200] Furthermore, in step (33), the mold is compacted and formed by a press machine at a pressure of 2 MPa, and the holding time is 4 minutes.

[0201] Furthermore, in step (4), hot air circulation drying equipment is used for drying; in step (4), hot air at 100° C. is used for drying and shaping, and the drying time is 70 minutes.

[0202] Example 1

[0203] A method for preparing an ultra-light flame-retardant sound-absorbing and sound-insulating board, the steps are as follows:

[0204] 1. Raw material preparation

[0205] Weigh 65 parts of 30-40 mesh closed-cell hollow foamed microsphere particles and dry them at 80° C. for 1.5 hours.

[0206] Prepare 10 parts of modified epoxy resin, 3 parts of lightweight and high-strength glass fiber mesh cloth (specifications can be cut as needed), 3 parts of nano-silica aerogel, 2 parts of flame retardant (ammonium polyphosphate), 1 part of surface modifier (silane coupling agent), 0.3 parts of high-efficiency dispersant (polycarboxylate), and 0.2 parts of defoaming agent (BYK-016 defoaming agent).

[0207] 2. Mesh cloth processing

[0208] Cut the lightweight and high-strength fiberglass mesh into suitable sizes and clean the surface.

[0209] 3. Mixing ingredients

[0210] Add the modified epoxy resin, surface modifier, high-efficiency dispersant and defoamer in the formula amount into a high-speed mixer and stir at 900 rpm for 3 minutes.

[0211] Slowly add the dried formula amount of closed-cell hollow foamed microsphere particles and continue stirring for 7 minutes.

[0212] Add the formulated amount of nano-silica aerogel and flame retardant, stir at 500 rpm for 4 minutes to obtain a mixture.

[0213] 4. Molding

[0214] Lay the first glass fiber mesh cloth layer at the bottom of the mold, pour the mixture, lay the second glass fiber mesh cloth layer on the surface after leveling. Vibrate at 40Hz for 3 minutes on the vibration table, then compact and shape at 2MPa pressure, and keep the pressure for 4 minutes.

[0215] 5. Post-processing

[0216] The formed board was placed in a hot air circulation drying device and dried at 100°C for 70 minutes.

[0217] The dried sound-absorbing and sound-insulating panels are cut and polished to achieve a dimensional accuracy of ±1.5mm and a surface flatness of ±0.4mm.

[0218] Example 2

[0219] A method for preparing an ultra-light flame-retardant sound-absorbing and sound-insulating board, the steps are as follows:

[0220] 1. Raw material preparation

[0221] Take 70 parts of 40-50 mesh closed-cell hollow foamed microsphere particles and dry them at 70°C for 2 hours.

[0222] Prepare 12 parts of modified epoxy resin, 4 parts of lightweight and high-strength glass fiber mesh cloth (specifications cut as needed), 4 parts of nano-silica aerogel, 3 parts of flame retardant (tricresyl phosphate), 1.5 parts of surface modifier (silane coupling agent), 0.5 parts of high-efficiency dispersant (polyacrylic acid amine), and 0.3 parts of defoaming agent (BYK-024 defoaming agent).

[0223] 2. Mesh cloth processing

[0224] Cut the lightweight and high-strength fiberglass mesh into suitable sizes and clean the surface.

[0225] 3. Mixing ingredients

[0226] Add the modified epoxy resin, surface modifier (silane coupling agent), high-efficiency dispersant and defoamer in the formula amount into a high-speed mixer and stir at 800 rpm for 4 minutes.

[0227] Slowly add the dried closed-cell hollow foamed microsphere particles and continue stirring for 8 minutes.

[0228] Nano-silica aerogel and flame retardant were added, and the mixture was stirred at 400 rpm for 5 minutes to obtain a mixture.

[0229] 4. Molding

[0230] Lay the first glass fiber mesh cloth layer at the bottom of the mold, pour the mixture, lay the second glass fiber mesh cloth layer on the surface after leveling. Vibrate at 35Hz for 2 minutes on the vibration table, then compact and shape at 1.5MPa pressure, and keep the pressure for 6 minutes.

[0231] 5. Post-processing

[0232] The formed board was placed in a hot air circulation drying device and dried at 90°C for 80 minutes.

[0233] The dried sound-absorbing and sound-insulating panels are cut and polished to achieve a dimensional accuracy of ±2mm and a surface flatness of ±0.5mm.

[0234] Example 3

[0235] A method for preparing an ultra-light flame-retardant sound-absorbing and sound-insulating board, the steps are as follows:

[0236] 1. Raw material preparation

[0237] Take 75 parts of 50-60 mesh closed-cell hollow foamed microsphere particles and dry them at 90°C for 1 hour.

[0238] Prepare 14 parts of modified epoxy resin, 5 parts of lightweight and high-strength glass fiber mesh cloth (specifications can be cut as needed), 5 parts of nano-silica aerogel, 4 parts of flame retardant (tricresyl phosphate), 2 parts of surface modifier (titanate coupling agent), 0.8 parts of high-efficiency dispersant (polyepoxysuccinic acid), and 0.4 parts of defoaming agent (BASF DF-2800).

[0239] 2. Mesh cloth processing

[0240] Cut the lightweight and high-strength fiberglass mesh into suitable sizes and clean the surface.

[0241] 3. Mixing ingredients

[0242] Add the modified epoxy resin, surface modifier (titanium ester coupling agent), high-efficiency dispersant and defoaming agent in the formula amount into a high-speed mixer and stir at 1000 rpm for 2 minutes.

[0243] Slowly add the dried closed-cell hollow foamed microsphere particles and continue stirring for 6 minutes.

[0244] Nano-silica aerogel and flame retardant were added, and the mixture was stirred at 600 rpm for 3 minutes to obtain a mixture.

[0245] 4. Molding

[0246] Lay the first glass fiber mesh cloth layer at the bottom of the mold, pour the mixture in, lay the second glass fiber mesh cloth layer on the surface after leveling. Vibrate on the vibration table at a frequency of 50Hz for 4 minutes, then compact and shape at a pressure of 3MPa, and maintain the pressure for 3 minutes.

[0247] 5. Post-processing

[0248] The formed board was placed in a hot air circulation drying device and dried at 110°C for 60 minutes.

[0249] The dried sound-absorbing and sound-insulating panels are cut and polished to achieve a dimensional accuracy of ±1mm and a surface flatness of ±0.3mm.

[0250] Performance Testing

[0251] The sound absorption coefficient test is carried out in accordance with GB / T 20247-2006 "Acoustic Reverberation Chamber Sound Absorption Measurement" standard.

[0252] The test of average sound insulation is carried out in accordance with GB / T 19889.4-2005 "Acoustic sound insulation measurement of buildings and building elements Part 4: Field measurement of airborne sound insulation between rooms".

[0253] The test of moisture expansion rate shall comply with GB / T7019-20141 "Test Methods for Fiber Cement Products" standard.

[0254] The flexural strength test is carried out in accordance with GB / T7019-20141 "Test methods for fiber cement products".

[0255] The fire resistance test is carried out in accordance with GB8624-2012 "Classification of Combustion Performance of Building Materials and Products".

[0256] The performance of the ultra-light flame-retardant sound-absorbing and insulating panels prepared in Examples 1 to 3 was tested, and a particle rock board was used as a control group. The results are shown in the following table:

[0257]

[0258] It can be seen from the test results that the ultra-light flame-retardant sound-absorbing and sound-insulating board prepared by the present invention maintains good sound absorption, sound insulation, fire resistance and mechanical properties while achieving ultra-lightweight, and has broad application prospects.

[0259] The above describes the embodiments of the present invention in detail. However, the present invention is not limited to the above embodiments, and various changes can be made within the knowledge of ordinary technicians in the relevant technical field without departing from the purpose of the present invention.

Claims

1. An ultra-light flame-retardant sound-absorbing and sound-insulating board, characterized in that: From the inside to the outside, it is composed of the first glass fiber mesh cloth layer, the ultra-light flame retardant sound absorbing and insulating board layer and the second glass fiber mesh cloth layer, of which: The ultra-light flame-retardant sound-absorbing and insulating board layer is prepared by uniformly mixing 65-80 parts of closed-cell hollow foamed microbead particles, 10-15 parts of modified epoxy resin, 3-6 parts of nano-silicon dioxide aerogel, 2-4 parts of flame retardant, 1-2 parts of surface modifier and 0.3-1 part of auxiliary agent.

2. The ultra-light flame-retardant sound-absorbing and sound-insulating board according to claim 1, characterized in that: The particle size of the closed-cell hollow foamed microsphere particles is 30 to 60 meshes, and / or The thickness of the ultra-light flame-retardant sound-absorbing and insulating board layer is 0.8 to 1.5 cm, and / or The surface modifier is one of a silane coupling agent and a titanate coupling agent.

3. The ultra-light flame-retardant sound-absorbing and insulating board according to claim 1, characterized in that: The first fiberglass mesh cloth layer and the second fiberglass mesh cloth layer are made of the same light-weight and high-strength fiberglass mesh cloth; The performance parameters of the lightweight and high-strength glass fiber mesh cloth are as follows: The weight is 80-100 g / m2; the mesh size is 20×20 mm; the alkali-resistant breaking strength is 3000-5000 N / 50 mm.

4. The ultra-light flame-retardant sound-absorbing and insulating board according to claim 1, characterized in that: The flame retardant is an intumescent environmentally friendly flame retardant, and the intumescent environmentally friendly flame retardant is one of ammonium polyphosphate and phosphate ester, wherein: The phosphate ester is one or more of tricresyl phosphate, triethyl phosphate or triphenyl phosphate.

5. The ultra-light flame-retardant sound-absorbing and insulating board according to claim 1, characterized in that: The auxiliary agent is composed of a high-efficiency dispersant and a defoamer, and the mass ratio of the high-efficiency dispersant to the defoamer is (3-5):1, wherein: The high-efficiency dispersant is one of polycarboxylate and phosphate; The defoamer is a commercially available high-efficiency silicone defoamer, which is one of BYK-016 defoamer, BYK-024 defoamer, and BASF DF-2800 defoamer.

6. The ultra-light flame-retardant sound-absorbing and insulating board according to claim 5, characterized in that: The polycarboxylate is one of sodium polyacrylate, polyacrylic acid amine, polyepoxysuccinic acid, and sodium dodecyl sulfonate; The phosphate ester is one of fatty alcohol polyoxyethylene ether phosphate and alkylphenol polyoxyethylene ether phosphate.

7. The method for preparing the ultra-light flame-retardant sound-absorbing and sound-insulating board according to any one of claims 1 to 6, characterized in that: Here are the steps: (1) Raw material pretreatment: (11) drying the closed-cell hollow foamed microsphere particles at at least 70° C., preferably 70 to 90° C., for at least 1 hour, preferably 1 to 2 hours; (12) cutting the lightweight and high-strength glass fiber mesh cloth to make its size match the size of the mold to obtain the first / second glass fiber mesh cloth layer, and performing surface cleaning treatment on the same; (2) Mixing ingredients: (21) First, add a formulated amount of modified epoxy resin, a formulated amount of surface modifier, and a formulated amount of auxiliary agent into a high-speed mixer, and stir evenly to form a uniform binder system; (22) slowly adding the closed-cell hollow foamed microsphere particles dried in step (11) into a high-speed mixer, keeping the stirring speed constant, and continuing to stir with the binder system for at least 6 minutes, preferably 6 to 8 minutes, to form a uniform first mixture; (23) adding a formulated amount of nano-silica aerogel and a formulated amount of flame retardant into a high-speed mixer, and stirring evenly to obtain a second mixture; (3) Molding: (31) Laying a first glass fiber mesh cloth layer on the bottom of the mold, pouring an appropriate amount of the second mixed material obtained in step (2) into the mold and placing it above the first glass fiber mesh cloth layer, laying it flat, and then laying a second glass fiber mesh cloth layer on the surface; (32), placing the mold processed in step (31) on a vibration table, vibrating it at a certain frequency for a period of time, and then proceeding to step (33); (33), placing the mold processed in step (32) on a press, and compacting it under a certain pressure for a period of time; (4) Post-processing: The mold treated in step (3) is dried at a certain temperature for a period of time to set the shape, and then demoulded and polished to obtain an ultra-light flame-retardant sound-absorbing and insulating board.

8. The method for preparing the ultra-light flame-retardant sound-absorbing and sound-insulating board according to claim 7, characterized in that: The speed of the high-speed stirrer in step (21) is at least 800 rpm, preferably 800-1000 rpm; the stirring time is at least 2 minutes, preferably 2-4 minutes, and / or The rotation speed of the high-speed stirrer in step (22) is at least 400 rpm, preferably 400-600 rpm; the stirring time is at least 3 minutes, preferably 3-5 minutes.

9. The method for preparing the ultra-light flame-retardant sound-absorbing and sound-insulating board according to claim 7, characterized in that: The vibration frequency of the vibration table in step (32) is at least 30 Hz, preferably 30 to 50 Hz, and / or The vibration time of the vibration table in step (32) is at least 2 minutes, preferably 2 to 4 minutes, and / or In step (33), the mold is compacted and formed by a press machine at a pressure of at least 1 MPa, preferably 1 to 3 MPa, and the holding time is at least 3 minutes, preferably 3 to 6 minutes.

10. The method for preparing the ultra-light flame-retardant sound-absorbing and sound-insulating board according to claim 7, characterized in that: In step (4), hot air circulation drying equipment is used for drying; In step (4), hot air at a temperature of at least 90° C., preferably 90 to 110° C., is used for drying and shaping, and the drying time is at least 60 minutes, preferably 60 to 80 minutes.

Citation Information

Patent Citations

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    CN104177114A