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CN115262788A - Composite sound absorption plate with multi-scale hole structure and preparation method thereof - Google Patents

Composite sound absorption plate with multi-scale hole structure and preparation method thereof Download PDF

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Publication number
CN115262788A
CN115262788A CN202210908845.5A CN202210908845A CN115262788A CN 115262788 A CN115262788 A CN 115262788A CN 202210908845 A CN202210908845 A CN 202210908845A CN 115262788 A CN115262788 A CN 115262788A
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porous
volume weight
holes
sound absorption
particles
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CN202210908845.5A
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CN115262788B (en
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李常胜
曹海琳
翁履谦
李丹
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Shenzhen Aerospace New Material Technology Co ltd
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Shenzhen Aerospace New Material Technology Co ltd
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    • EFIXED CONSTRUCTIONS
    • E04BUILDING
    • E04BGENERAL BUILDING CONSTRUCTIONS; WALLS, e.g. PARTITIONS; ROOFS; FLOORS; CEILINGS; INSULATION OR OTHER PROTECTION OF BUILDINGS
    • E04B1/00Constructions in general; Structures which are not restricted either to walls, e.g. partitions, or floors or ceilings or roofs
    • E04B1/62Insulation or other protection; Elements or use of specified material therefor
    • E04B1/74Heat, sound or noise insulation, absorption, or reflection; Other building methods affording favourable thermal or acoustical conditions, e.g. accumulating of heat within walls
    • E04B1/82Heat, sound or noise insulation, absorption, or reflection; Other building methods affording favourable thermal or acoustical conditions, e.g. accumulating of heat within walls specifically with respect to sound only
    • E04B1/84Sound-absorbing elements
    • E04B1/86Sound-absorbing elements slab-shaped
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29DPRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
    • B29D7/00Producing flat articles, e.g. films or sheets
    • EFIXED CONSTRUCTIONS
    • E04BUILDING
    • E04BGENERAL BUILDING CONSTRUCTIONS; WALLS, e.g. PARTITIONS; ROOFS; FLOORS; CEILINGS; INSULATION OR OTHER PROTECTION OF BUILDINGS
    • E04B1/00Constructions in general; Structures which are not restricted either to walls, e.g. partitions, or floors or ceilings or roofs
    • E04B1/62Insulation or other protection; Elements or use of specified material therefor
    • E04B1/74Heat, sound or noise insulation, absorption, or reflection; Other building methods affording favourable thermal or acoustical conditions, e.g. accumulating of heat within walls
    • E04B1/82Heat, sound or noise insulation, absorption, or reflection; Other building methods affording favourable thermal or acoustical conditions, e.g. accumulating of heat within walls specifically with respect to sound only
    • E04B1/84Sound-absorbing elements
    • E04B1/8409Sound-absorbing elements sheet-shaped
    • EFIXED CONSTRUCTIONS
    • E04BUILDING
    • E04BGENERAL BUILDING CONSTRUCTIONS; WALLS, e.g. PARTITIONS; ROOFS; FLOORS; CEILINGS; INSULATION OR OTHER PROTECTION OF BUILDINGS
    • E04B1/00Constructions in general; Structures which are not restricted either to walls, e.g. partitions, or floors or ceilings or roofs
    • E04B1/62Insulation or other protection; Elements or use of specified material therefor
    • E04B1/74Heat, sound or noise insulation, absorption, or reflection; Other building methods affording favourable thermal or acoustical conditions, e.g. accumulating of heat within walls
    • E04B1/82Heat, sound or noise insulation, absorption, or reflection; Other building methods affording favourable thermal or acoustical conditions, e.g. accumulating of heat within walls specifically with respect to sound only
    • E04B1/84Sound-absorbing elements
    • E04B2001/8457Solid slabs or blocks
    • E04B2001/8476Solid slabs or blocks with acoustical cavities, with or without acoustical filling
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/91Use of waste materials as fillers for mortars or concrete

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  • Physics & Mathematics (AREA)
  • Acoustics & Sound (AREA)
  • Engineering & Computer Science (AREA)
  • Architecture (AREA)
  • Electromagnetism (AREA)
  • Civil Engineering (AREA)
  • Structural Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)

Abstract

The composite sound absorption plate comprises a composite sound absorption material, wherein the composite sound absorption material comprises a first-stage hole with the diameter smaller than 2nm, a second-stage hole with the diameter of 0.5-3 mu m and a third-stage hole with the diameter of 0.1-3 mm; wherein, the volume weight of the first-stage holes accounts for 5-50% of the total volume weight of the holes, the volume weight of the second-stage holes accounts for 20-60% of the total volume weight of the holes, the volume weight of the third-stage holes accounts for 30-60% of the total volume weight of the holes, and the volume weight of the holes with other scales accounts for 0-10% of the total volume weight of the holes. The composite sound absorption plate can effectively avoid the problem that the sound absorption performance is attenuated because the pore channel of the porous material is blocked by the resin matrix in the preparation and forming process, can accurately control the size and the range of the micron-sized hole according to the difference of sound absorption characteristics of sound waves in different pore diameters, ensures that the porous sound absorption material has better low-frequency sound absorption performance, and shows better sound absorption performance in a wider frequency range.

Description

Composite sound absorption plate with multi-scale hole structure and preparation method thereof
Technical Field
The application relates to the technical field of environmental protection materials, in particular to a composite sound absorption plate with a multi-scale hole structure and a preparation method thereof.
Background
The porous fibers such as organic fibers, glass fiber cotton and the like have low density, have good sound absorption characteristics above 500Hz, and are commonly used as sound absorption materials for adjusting indoor reverberation. The particle porous materials, such as zeolite, molecular sieve, MOFS (metal organic framework compound) and the like, have nanoscale pores with single dimension, the size of the pores is more than 1nm, and the porous materials are used as an adsorption material, a catalyst carrier and a filter material besides a sound absorption material due to high specific surface area and large pore volume.
Patent No. CN113041993A describes a zeolite ball-type porous sound-absorbing particle for increasing the virtual volume of a loudspeaker. Compared with other porous materials, the zeolite molecular sieve has smaller specific surface area and pore volume, and small gas adsorption and desorption amount, and has limited application as a filling material for improving the low-frequency performance of a loudspeaker. Patent No. CN111362272A introduces a mesoporous silica material, which contains a large amount of 2-50nm mesoporous silica material and exhibits strong adsorption property, and as a filler, can improve the low frequency characteristics of a speaker. Compared with porous fiber, the particle-based porous material has better low-frequency sound absorption performance, but is limited by pore scale characteristics or quantity limitation, and the low-frequency sound absorption performance is still lower than expected. Air molecules show different gas/fluid characteristics in pores with different scales, and air shows the characteristics of transition fluid in micro-nano pores equivalent to the free path of the air molecules; in voids much smaller than the free path of the air molecules, air exhibits free-fluid behavior. Therefore, in the process of sound transmission, the energy absorption modes of different types of holes are obviously different, and the sound absorption material containing multiple holes has higher sound absorption characteristics in a low-frequency area through the synergistic coupling effect of the holes.
Bio-based materials contain natural nanopores such as coconut shells, animal bones, loofah capsules, bamboo hemp. During physical and chemical activation, these nanopores can be opened up to form nanopores with the micropores. Due to the limited number of micropores, the low-frequency sound absorption performance of some bio-based materials is not ideal, i.e. the synergistic effect of micropores and nanopores is poor.
Disclosure of Invention
In view of the problems, the present application is proposed to provide a multi-scale pore structured composite sound-absorbing panel and a method for manufacturing the same, which overcome or at least partially solve the problems, comprising:
a composite sound absorption plate with a multi-scale hole structure comprises a composite sound absorption material, wherein the composite sound absorption material comprises a first-stage hole with the diameter less than 2nm, a second-stage hole with the diameter of 0.5-3 mu m and a third-stage hole with the diameter of 0.1-3 mm; wherein, the volume weight of the first-stage holes accounts for 5-50% of the total volume weight of the holes, the volume weight of the second-stage holes accounts for 20-60% of the total volume weight of the holes, the volume weight of the third-stage holes accounts for 30-60% of the total volume weight of the holes, and the volume weight of the holes with other scales accounts for 0-10% of the total volume weight of the holes.
Preferably, the diameter of the primary pores is less than 1.5nm; the diameter of the second-stage hole is 0.8-2 μm; the diameter of the third-stage hole is 0.5mm-2 mm.
The application also provides a preparation method of the composite sound absorption plate with the multi-scale hole structure, which comprises the following steps:
mixing an adhesive, an auxiliary agent and a microporous template material with a preset shape with an alkaline solution or an acidic solution to obtain an inorganic dispersion liquid;
carbonizing the bio-based material at a first specified temperature for a first specified time, and mixing the bio-based material with the inorganic dispersion liquid to solidify at a second specified temperature for a second specified time to obtain a porous solidified material;
activating the porous solidified material at a third specified temperature for a third specified time, and cooling, neutralizing, cleaning, drying and crushing to obtain porous particles;
mixing the porous particles and the porous material according to a first preset mass ratio, and mixing and hot-pressing the porous particles and the organic resin particles to obtain the composite sound-absorbing board; or mixing the porous particles and the porous material according to a second preset mass ratio, and mixing the porous particles and the porous material with a foaming material to obtain the composite sound-absorbing board.
Preferably, the step of activating the porous solidified material at a third specified temperature for a third specified time to obtain porous particles after cooling, neutralizing, washing, drying and pulverizing comprises:
thermally oxidizing the porous cured material at a fourth specified temperature for a fourth specified time to obtain the porous cured material with micron-sized pores;
and activating the porous solidified material with the micron-sized pores at a third specified temperature for a third specified time, and cooling, neutralizing, washing, drying and crushing to obtain the porous particles with the micron-sized pores and the nanometer-sized pores.
Preferably, the microporous template material is an organic fiber or microsphere;
the organic fiber comprises one or more of polyester fiber, polyvinyl alcohol fiber, polyvinyl butyral, polyacrylonitrile fiber and polyvinylpyrrolidone fiber, and the microsphere comprises one or more of polystyrene microsphere, polypropylene microsphere, polyethylene microsphere, polylactic acid microsphere and polyacrylonitrile microsphere.
Preferably, the adhesive comprises one or more of metakaolin, fly ash, mineral powder, silica sol and coal tar.
Preferably, the bio-based material comprises one or more of coconut shell, bamboo, walnut shell and straw.
Preferably, the porous material is one or more of carbon nanotubes, zeolites, molecular sieves and graphene.
Preferably, the foaming material is an aqueous polyurethane emulsion, and the preparation method of the aqueous polyurethane emulsion comprises the following steps:
preheating polyurethane prepolymer containing 1-3% of isocyanate groups at a fifth specified temperature for a fifth specified time to obtain the 1-5% aqueous polyurethane emulsion.
Preferably, the organic resin particles include one or more of phenol resin particles, melamine resin particles, polyvinyl formal particles, polyvinyl butyral particles, and polymethyl methacrylate particles.
The application has the following advantages:
in an embodiment of the present application, the composite sound absorption panel comprises a composite sound absorption material comprising first-stage holes having a diameter of less than 2nm, second-stage holes having a diameter of 0.5 to 3 μm, and third-stage holes having a diameter of 0.1 to 3 mm; wherein, the volume weight of the first-stage holes accounts for 5-50% of the total volume weight of the holes, the volume weight of the second-stage holes accounts for 20-60% of the total volume weight of the holes, the volume weight of the third-stage holes accounts for 30-60% of the total volume weight of the holes, and the volume weight of the holes with other scales accounts for 0-10% of the total volume weight of the holes. The composite sound absorption plate can effectively avoid the problem that the sound absorption performance is attenuated due to the fact that the pore channel of the porous material is blocked, the size and the range of the micron-sized hole can be accurately controlled according to the difference of sound absorption characteristics of sound waves in different pore diameters, the porous sound absorption material is guaranteed to have better low-frequency sound absorption performance, and better sound absorption performance is shown in a wider frequency range.
Drawings
In order to more clearly illustrate the technical solutions of the present application, the drawings required to be used in the description of the present application will be briefly described below, and it is apparent that the drawings in the following description are only some embodiments of the present application, and it is obvious for those skilled in the art that other drawings may be obtained according to these drawings without inventive labor.
Fig. 1 is a flowchart illustrating steps of a method for manufacturing a composite sound absorbing panel with a multi-scale pore structure according to an embodiment of the present disclosure.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present application more comprehensible, the present application is described in further detail with reference to the accompanying drawings and the detailed description. It is to be understood that the embodiments described are only a few embodiments of the present application and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
In one embodiment of the application, the composite sound absorption plate with the multi-scale hole structure comprises a composite sound absorption material, wherein the composite sound absorption material comprises a first-stage hole with the diameter less than 2nm, a second-stage hole with the diameter of 0.5-3 μm and a third-stage hole with the diameter of 0.1-3 mm; wherein, the volume weight of the first-stage holes accounts for 5-50% of the total volume weight of the holes, the volume weight of the second-stage holes accounts for 20-60% of the total volume weight of the holes, the volume weight of the third-stage holes accounts for 30-60% of the total volume weight of the holes, and the volume weight of the holes with other scales accounts for 0-10% of the total volume weight of the holes.
In an embodiment of the present application, the composite sound absorption panel comprises a composite sound absorption material comprising first-stage holes having a diameter of less than 2nm, second-stage holes having a diameter of 0.5 to 3 μm, and third-stage holes having a diameter of 0.1 to 3 mm; wherein, the volume weight of the first-stage holes accounts for 5-50% of the total volume weight of the holes, the volume weight of the second-stage holes accounts for 20-60% of the total volume weight of the holes, the volume weight of the third-stage holes accounts for 30-60% of the total volume weight of the holes, and the volume weight of the holes with other scales accounts for 0-10% of the total volume weight of the holes. The composite sound absorption plate can effectively avoid the problem that the sound absorption performance is attenuated because the pore channel of the porous material is blocked by the resin matrix in the preparation and forming process, can accurately control the size and the range of the micron-sized hole according to the difference of sound absorption characteristics of sound waves in different pore diameters, ensures that the porous sound absorption material has better low-frequency sound absorption performance, and shows better sound absorption performance in a wider frequency range.
Hereinafter, a composite sound-absorbing panel of a multi-scale hole structure in the present exemplary embodiment will be further described.
It should be noted that the pore volume weight is pv and is abbreviated as pore volume, and is pore volume, or the like. Pore volume weight is also known as pore volume. The total pore volume per unit mass of the porous solid is referred to as the pore volume or specific pore volume Vg. This is one of the characteristic values of the porous structure adsorbent or catalyst.
As an example, the composite sound absorbing panel is a composite sound absorbing particle panel or a composite sound absorbing foam panel.
In one embodiment of the present application, the first-order pores have a diameter of less than 1.5nm.
As an example, the first-stage pores are formed by two parts, one part is introduced by porous materials such as carbon nanotubes with nanometer-scale pores, molecular sieves and the like, and the other part is generated by activation of bio-based materials in the preparation process of the composite sound absorption material, wherein the content of the activated pores exceeds 50% of the first-stage pores, and preferably exceeds 70%.
As an example, the first-order pore diameter may be 1.5nm, 1.2nm, 1nm, 0.8nm, 0.5nm, and 0.3nm, which may be selected according to actual circumstances; the first-stage pore volume weight ratio is 5% to 50%, and may be 5%, 10%, 15%, 20%, 25%, 30%, 40%, and 50%, which may be selected according to the actual situation.
In one embodiment of the present application, the diameter of the second-stage pores is 0.8 μm to 2 μm.
As an example, the second-level pores are formed by degrading an organic fiber dispersion or a microsphere dispersion by an alkaline or acidic solution and then thermally oxidizing and ablating at high temperature, and have uniform sizes, and the diameters of the second-level pores can be 0.8 μm, 1 μm, 1.2 μm, 1.5 μm, 1.8 μm and 2 μm, and can be selected according to actual situations; the second-stage pore volume ratio is 20-60%, and can be 20%, 25%, 30%, 35%, 40%, 45%, 50% and 60%, and can be selected according to actual conditions.
In an embodiment of the present application, the diameter of the third stage hole is 0.5mm to 2mm.
As an example, the diameter of the third stage hole may be 0.5mm, 0.8mm, 1mm, 1.2mm, 1.5mm, 1.8mm and 2mm, which may be selected according to actual conditions; the volume weight ratio of the third-stage hole is 30% -60%, and the volume weight ratio can be 30%, 35%, 40%, 45%, 50%, 55% and 60%, and can be selected according to actual conditions.
As an example, the third stage holes are formed by stacking porous particles obtained after high-temperature activation, cleaning and crushing, and the diameter of the porous particles is 0.5mm-2mm, preferably 0.8mm-1.5mm.
As an example, the volume-to-weight ratio of the pores of other scales is 0% -10%, which can be 0%, 1%, 3%, 5%, 7%, 9% and 10%, and can be selected according to practical situations.
Referring to fig. 1, there is shown a method for manufacturing a composite sound-absorbing panel with a multi-scale pore structure according to an embodiment of the present application,
the method comprises the following steps:
s110, mixing an adhesive, an auxiliary agent and a microporous template material with a preset shape with an alkaline solution or an acidic solution to obtain an inorganic dispersion liquid;
s120, carbonizing the bio-based material at a first specified temperature for a first specified time, and mixing the bio-based material with the inorganic dispersion liquid to be cured at a second specified temperature for a second specified time to obtain a porous cured material;
s130, activating the porous solidified material at a third specified temperature for a third specified time, and cooling, neutralizing, cleaning, drying and crushing to obtain porous particles;
s140, mixing the porous particles and the porous material according to a first preset mass ratio, and mixing and hot-pressing the mixture with organic resin particles to obtain the composite sound absorption board; or mixing the porous particles and the porous material according to a second preset mass ratio, and mixing the porous particles and the porous material with a foaming material to obtain the composite sound-absorbing board.
Next, a method for manufacturing a composite sound-absorbing panel having a multi-scale pore structure in the present exemplary embodiment will be further described.
And step S110, mixing the adhesive, the auxiliary agent, and the microporous template material having the predetermined shape with an alkaline solution or an acidic solution to obtain an inorganic dispersion.
In an embodiment of the present invention, the specific process of "mixing the adhesive, the auxiliary agent, and the microporous template material with a predetermined shape with the alkaline solution or the acidic solution to obtain the inorganic dispersion liquid" in step S110 may be further described with reference to the following description.
As an example, the inorganic dispersion is prepared by mixing and stirring an auxiliary agent, the microporous template material, the adhesive, and an alkaline solution or an acidic solution. Specifically, the auxiliary agent is an emulsifier and is used for forming stable emulsion by a mixed liquid of two or more immiscible components; in this embodiment, the emulsifier can be selected from OP-10 (polyoxyethylene octyl phenol ether-10) or sodium dodecyl sulfate; the alkaline solution is strong alkali solution such as potassium hydroxide or sodium hydroxide; the acidic solution is a phosphoric acid solution.
In this embodiment, the microporous template material is an organic fiber or microsphere dispersion;
the organic fiber comprises one or more of polyester fiber, polyvinyl alcohol fiber, polyvinyl butyral, polyacrylonitrile fiber and polyvinylpyrrolidone fiber, and the microsphere comprises one or more of polystyrene microsphere, polypropylene microsphere, polyethylene microsphere, polylactic acid microsphere and polyacrylonitrile microsphere.
As an example, the microporous template material has a specific shape, which provides a microporous template, wherein the micron-sized pores are formed by high-temperature ablation of organic fibers or microspheres after degradation by a strong alkaline solution or a phosphoric acid solution, and are uniformly-sized pores formed by thermal oxidation of the organic material micron-sized template.
In this embodiment, the adhesive includes one or more of metakaolin, fly ash, mineral powder, silica sol, and coal tar.
As an example, the inorganic dispersion liquid is rich in a large amount of activated carbon active agents such as phosphoric acid, sodium hydroxide, sodium bicarbonate and the like, and inorganic adhesives such as metakaolin, fly ash, mineral powder, coal tar and the like, and during the preparation of the inorganic dispersion liquid, nucleating agents such as nano zirconium dioxide, aluminum oxide and the like can be optionally added to accelerate the crystallization rate.
Carbonizing the bio-based material at a first specified temperature for a first specified time and mixing with the inorganic dispersion liquid at a second specified temperature for a second specified time to obtain a porous solidified material as described in step S120.
In an embodiment of the present invention, the specific process of "carbonizing the bio-based material at a first designated temperature for a first designated time and mixing with the inorganic dispersion liquid at a second designated temperature for a second designated time to obtain a porous solidified material" in step S120 can be further described with reference to the following description.
In this embodiment, the bio-based material includes one or more of coconut shell, bamboo, walnut shell, and coal tar.
As an example, biological base materials such as coconut shells, bamboos, walnut shells or straws are carbonized for 1 to 3 hours at the temperature of between 400 and 600 ℃ and ground into powder according to the weight ratio of 100:300, soaking the bio-based powder in the inorganic dispersion liquid, and curing for 2-8h at 80-150 ℃ to obtain the porous cured material; wherein, the first appointed temperature of carbonization can be 400 ℃, 450 ℃, 500 ℃, 550 ℃ or 600 ℃, and can be selected according to the actual situation; the first designated time of carbonization can be 1h, 1.5h, 2h, 2.5h or 3h, and can be selected according to the actual situation; the second designated temperature for curing can be 80 ℃,90 ℃, 100 ℃, 120 ℃ or 150 ℃, and can be selected according to actual conditions; the second designated time for curing can be 2h, 3h, 5h, 6h or 8h, and can be selected according to actual conditions.
It should be noted that the curing times can be adjusted according to the state of the porous cured material after curing until the curing state of the material meets the requirements.
As stated in step S130, the porous solidified material is activated at a third specified temperature for a third specified time, and is pulverized to obtain porous particles.
In an embodiment of the present invention, the specific process of "activating the porous solidified material at a third specified temperature for a third specified time, cooling, neutralizing, washing, drying and pulverizing to obtain porous particles" in step S130 can be further described with reference to the following description.
Carrying out thermal oxidation on the porous solidified material at a fourth specified temperature for a fourth specified time to obtain the porous solidified material with micron-sized pores;
and (3) activating the porous solidified material with the micron-sized pores at a third specified temperature for a third specified time, and cooling, neutralizing, washing, drying and crushing to obtain the porous particles with the micron-sized pores and the nanometer-sized pores.
As an example, the porous solidified material obtained by degrading organic fibers or microspheres by using a strong alkali solution or a phosphoric acid solution is subjected to thermal oxidation at 400-600 ℃ for 0.5-2h to form micron-sized pores with uniform sizes; wherein, the fourth designated temperature can be 400 ℃, 450 ℃, 500 ℃, 550 ℃ or 600 ℃, and can be selected according to the actual situation; the fourth designated time may be 0.5h, 1h, 1.5h or 2h, and may be specifically selected according to the actual situation.
As an example, the porous solidified material with micron-scale pores is activated at 700-900 ℃ for 3-5h, cooled to room temperature, neutralized, washed and dried, and finally crushed to obtain the porous particles with nano-scale and micron-scale pores; specifically, if activated with phosphoric acid, it is neutralized with an alkali solution, and if activated with a strong alkali, it is neutralized with a dilute acid; the temperature of the third designated temperature can be 700 ℃, 750 ℃,800 ℃, 850 ℃ and 900 ℃, and can be specifically selected according to actual conditions; the third designated time may be 3h, 3.5h, 4h, 4.5h or 5h, and may be specifically selected according to the actual situation.
The nanometer-scale pores come from two parts, one part is generated by carbonizing and activating a bio-based material, and the other part is introduced by a porous material such as carbon nanotubes, molecular sieves and the like.
Mixing the porous particles and the porous material according to a first preset mass ratio, and mixing and hot-pressing the mixture with organic resin particles to obtain the composite sound absorbing panel according to the step S140; or mixing the porous particles and the porous material according to a second preset mass ratio, and mixing the porous particles and the porous material with a foaming material to obtain the composite sound-absorbing board.
In an embodiment of the present invention, the step S140 "mixing the porous particles and the porous material according to the first predetermined mass ratio, and mixing and hot-pressing the mixture with the organic resin particles to obtain the composite sound absorbing panel; or, mixing the porous particles and the porous material according to a second preset mass ratio, and mixing the porous particles and the porous material with the foaming material to obtain the composite sound-absorbing board.
As an example, the composite sound absorbing panel is prepared by hot-pressing and compounding the porous particles containing the nano-scale and micron-scale holes and organic resin particles at a mass ratio of 1 to 20, wherein the porous particles are prepared by hot-pressing at 100 to 200 ℃, and the composite sound absorbing panel is a composite sound absorbing particle panel with the density of 0.2 to 0.7g/cm3
As an example, the hot pressing temperature can be 100 ℃, 120 ℃, 150 ℃, 180 ℃ and 200 ℃, and can be selected according to practical situations.
In this embodiment, the porous material is one or more of carbon nanotubes, zeolites, molecular sieves, and graphene.
In this embodiment, the organic resin particles include one or more of phenol resin particles, melamine resin particles, polyvinyl formal particles, polyvinyl butyral particles, and polymethyl methacrylate particles.
In this embodiment, the foaming material is an aqueous polyurethane emulsion, and the preparation method of the aqueous polyurethane emulsion includes:
preheating polyurethane prepolymer containing 1-3% of isocyanate groups at a fifth specified temperature for a fifth specified time to obtain the 1-5% aqueous polyurethane emulsion.
As an example, the composite sound absorbing panel is obtained by compounding porous particles containing nano-sized and micro-sized pores with a foam material at a mass ratio of 1 to 20. The foaming material is aqueous polyurethane emulsion with the tail end containing NCO (weight content of isocyanate group), wherein the resin matrix is polyurethane prepolymer, the content of NCO is 1-3%, the polyurethane prepolymer is emulsified and dispersed into emulsion with the concentration of 1-5% after being preheated for 0.2-1h at the temperature of 20-50 ℃, the porous particles and the aqueous polyurethane emulsion are mixed and foamed for 12h to obtain the composite sound absorbing plate, and the composite sound absorbing plate is prepared by the steps ofThe sound board is a composite sound absorption foam board with the density of 0.05-0.3g/cm3. Specifically, the fifth designated time may be 20 ℃, 30 ℃, 40 ℃ or 50 ℃, preferably 30 ℃; the fifth designated time may be 0.2h, 0.4h, 0.5h, 0.8h or 1h, preferably 0.5h.
The following are specific examples:
example 1
(1) And preparing micro-nano fiber solution. Preparing PVA spinning solution (polyvinyl alcohol fiber) with the concentration of 5 percent, and hot water as a solvent; a home-made electrostatic spinning device is adopted, under the conditions that the spinning voltage is 15kV and the distance is 20cm, an injector is added, the spinning solution is directly sprayed into the water solution which is continuously stirred through a nozzle, the electrostatic spinning solution with the concentration of 0.5% is obtained, and the diameter of the PVB fiber is measured to be 0.6 mu m through a scanning electron microscope.
(2) An inorganic dispersion is prepared. Weighing 200g of the micro-nanofiber solution, adding a proper amount of 1% emulsifier OP-10 into the solution, stirring and uniformly stirring, and then adding 10g of coal tar, 5g of fly ash, 10g of 50% alkaline silica sol and 100g of potassium hydroxide.
(3) Carbonization of coconut shells: weighing 500g of coconut shell, carbonizing at 550 ℃ for 1.5h to obtain coconut shell carbon, crushing the coconut shell carbon, and sieving with a 200-mesh sieve to obtain 100g of coconut shell carbon powder.
(4) Activating coconut shell carbon: coconut shell carbon powder and inorganic dispersion are blended, cured for 8 hours at 80 ℃ and then cured for 2 hours at 100 ℃. After high-temperature heat treatment at 400 ℃ for 2h, activating at 800 ℃ for 4h in a nitrogen atmosphere, and cooling, neutralizing, cleaning, drying, crushing and sieving to obtain the porous particles with the micro-nano holes of 40 x 70 meshes. The volume weight of the micron-sized pores is analyzed by a mercury intrusion method, and the volume weight of the nanometer-sized pores is measured by a specific surface tester.
(5) And (4) preparing the composite sound absorption board. Compounding micro-nano-pore porous particles with polyurethane thermoplastic resin according to the proportion of 100:15 compounding, hot pressing at 150 deg.C to obtain the composite sound absorption particle board with thickness of 3.0cm and density of 0.53g/cm3. The volume weight of the millimeter-level hole is measured by adopting a flow resistance method, and the sound absorption performance of the composite sound absorption particle board is measured by adopting the impedance tube.
Example 2
(1) And preparing micro-nano fiber solution. Preparing PVA spinning solution with the concentration of 5 percent, and hot water as a solvent; adopting self-made electrostatic spinning equipment, adding an injector to directly spray spinning solution into the continuously stirred aqueous solution through a nozzle under the conditions that the spinning voltage is 15kV and the distance is 20cm, obtaining the electrostatic spinning solution with the concentration of 2%, and measuring the diameter of the PVB fiber to be 0.6 mu m through a scanning electron microscope.
(2) An inorganic dispersion was prepared. Weighing 200g of the micro-nanofiber solution, adding a proper amount of 1% emulsifier OP-10 into the solution, stirring and uniformly stirring, and then adding 10g of coal tar, 5g of fly ash, 10g of 50% alkaline silica sol and 100g of sodium hydroxide.
(3) Carbonization of coconut shells: weighing 500g of coconut shell, carbonizing at 500 ℃ for 2.0h to obtain coconut shell carbon, crushing the coconut shell carbon, and sieving with a 200-mesh sieve to obtain 100g of coconut shell carbon powder.
(4) Activating coconut shell carbon: coconut shell carbon powder and inorganic dispersion are blended, cured for 8 hours at 80 ℃ and then cured for 1.5 hours at 150 ℃. After being subjected to high-temperature heat treatment at 550 ℃ for 1h, the porous particles are activated at 700 ℃ for 5h in a nitrogen atmosphere, and are cooled, neutralized, cleaned, dried, crushed and sieved to obtain the micro-nano hole composite porous particles of 40 x 70 meshes. And (3) analyzing the volume weight of the second-stage hole by a mercury intrusion method, and measuring the volume weight of the nano-scale hole by a specific surface tester.
(5) And (4) preparing the composite sound absorption board. Mixing the micro-nano-pore compounded activated carbon particles and self-prepared waterborne polyurethane emulsion (the residual content of NCO% is 0.5%) according to the proportion of 100:100, adding 1 percent of silicone oil, pouring into a mold, and foaming at room temperature for 4 hours to obtain a mixture with the thickness of 3.0cm and the density of 0.15g/cm3The composite sound absorbing foam panel. The volume weight of the millimeter-level hole is measured by adopting a flow resistance method, and the sound absorption performance of the composite sound absorption foam board is measured by adopting an impedance tube.
Example 3
(1) And preparing micro-nano fiber solution. Preparing PVA spinning solution with the concentration of 5 percent, and hot water as a solvent; a home-made electrostatic spinning device is adopted, under the conditions that the spinning voltage is 15kV and the distance is 20cm, an injector is added, the spinning solution is directly sprayed into the water solution which is continuously stirred through a nozzle, the electrostatic spinning solution with the concentration of 2% is obtained, and the diameter of the PVB fiber is measured to be 1.0 mu m through a scanning electron microscope.
(2) An inorganic dispersion is prepared. Weighing 200g of the micro-nanofiber solution, adding a proper amount of 1% emulsifier OP-10 into the solution, stirring and uniformly stirring, and then adding 10g of coal tar, 5g of fly ash, 10g of 50% alkaline silica sol and 100g of potassium hydroxide.
(3) Carbonization of coconut shells: weighing 500g of coconut shell, carbonizing at 550 ℃ for 1.5h to obtain coconut shell carbon, crushing the coconut shell carbon, and sieving with a 200-mesh sieve to obtain 100g of coconut shell carbon powder.
(4) Activating coconut shell carbon: coconut shell carbon powder and inorganic dispersion are blended, cured for 7 hours at 90 ℃, and then cured for 2 hours at 120 ℃. After high-temperature heat treatment at 600 ℃ for 0.5h, activating at 900 ℃ for 3h in nitrogen atmosphere, and cooling, neutralizing, cleaning, drying, crushing and sieving to obtain the 1mm micro-nano hole composite activated carbon particles. And (3) analyzing the volume weight of the second-stage hole by a mercury intrusion method, and measuring the volume weight of the nano-scale hole by a specific surface tester.
(5) And (4) preparing the composite sound absorption board. Compounding micro-nano hole activated carbon particles and polyvinyl butyral resin according to the proportion of 100:15 compounding, hot pressing at 150 ℃ to form the composite sound absorption particle board with the thickness of 3.0cm and the multiple holes, wherein the density is 0.45g/cm3. The flow resistance method is adopted to measure the volume weight of the millimeter-sized hole, and the impedance tube is adopted to measure the sound absorption performance of the composite sound absorption particle board.
Example 4
(1) And (4) preparing a micro-nano fiber solution. Preparing PAN spinning solution (polyacrylonitrile microspheres) with the concentration of 5 percent, wherein the solvent is DMF (dimethyl formyl); adopting self-made electrostatic spinning equipment, adding an injector to directly spray spinning solution into continuously stirred aqueous solution through a nozzle under the conditions that the spinning voltage is 15kV and the distance is 20cm, obtaining the electrostatic spinning solution with the concentration of 1%, and measuring the diameter of the PAN fiber to be 0.8 mu m through a scanning electron microscope.
(2) An inorganic dispersion is prepared. Weighing 300g of the micro-nanofiber solution, adding a proper amount of 1% emulsifier OP-10 into the solution, stirring and uniformly stirring, and then adding 10g of coal tar, 5g of fly ash, 10g of 50% alkaline silica sol and 100g of potassium hydroxide.
(3) Carbonization of coconut shells: weighing 500g of coconut shell, carbonizing at 550 ℃ for 1.5h to obtain coconut shell carbon, crushing the coconut shell carbon, and sieving with a 200-mesh sieve to obtain 100g of coconut shell carbon powder.
(4) Activating coconut shell carbon: coconut shell carbon powder and inorganic dispersion are blended, cured for 8 hours at 80 ℃, and cured for 2 hours at 100 ℃. After high-temperature heat treatment at 500 ℃ for 1h, activating at 800 ℃ for 4h in a nitrogen atmosphere, and cooling, neutralizing, cleaning, drying, crushing and sieving to obtain the 0.8mm micro-nano hole composite activated carbon particles. And (3) analyzing the volume weight of the second-stage hole by a mercury intrusion method, and measuring the volume weight of the nano-scale hole by a specific surface tester.
(5) And (4) preparing the composite sound absorption board. Compounding the micro-nano hole activated carbon particles with polyvinyl butyral resin according to the proportion of 100:15 compounding, hot pressing at 200 deg.C to obtain the composite sound-absorbing board with thickness of 3.0cm and multiple holes and density of 0.40g/cm3. The volume weight of the millimeter-level hole is measured by adopting a flow resistance method, and the sound absorption performance of the composite sound absorption plate is measured by adopting an impedance tube.
Comparative example 1
Using commercially available activated carbon granules (BET 1115 cm)2Per g, pore volume weight of 0.5g/cm3) Compounding with polyvinyl butyral resin according to a ratio of 1003
Comparative example 2
Using commercially available activated carbon granules (BET 2500 cm)2Per g, pore volume weight of 1.5g/cm3) Compounding with polyvinyl butyral resin according to a ratio of 1003
Comparative example 3
The activated carbon particles were prepared according to the method of comparative example 1 without adding any microfiber as a micron pore forming agent during the preparation, and then compounded with a polyurethane thermoplastic resin according to a ratio of 1003
The low frequency performance versus ratio of examples 1-4 and comparative examples 1-3 is shown in table one:
Figure BDA0003773406360000131
Figure BDA0003773406360000141
watch 1
As can be seen from the first table, the composite sound absorbing panel of the present embodiment exhibits higher low frequency sound absorbing performance, particularly sound absorbing performance of 250Hz and 500 Hz; the low-frequency sound absorption performance of the commercially available glass wool is lower, and the low-frequency sound absorption performance of the glass wool with the thickness of about more than 10cm is equivalent to that of the composite sound absorption plate of the embodiment.
While preferred embodiments of the present application have been described, additional variations and modifications of these embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including the preferred embodiment and all such alterations and modifications as fall within the true scope of the embodiments of the application.
Finally, it should also be noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or terminal that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or terminal. Without further limitation, an element defined by the phrases "comprising one of \ 8230; \8230;" does not exclude the presence of additional like elements in a process, method, article, or terminal device that comprises the element.
The composite sound absorbing panel with a multi-scale hole structure and the preparation method thereof provided by the application are introduced in detail, and specific examples are applied to explain the principle and the implementation mode of the application, and the description of the examples is only used for helping to understand the method and the core idea of the application; meanwhile, for a person skilled in the art, according to the idea of the present application, the specific implementation manner and the application scope may be changed, and in summary, the content of the present specification should not be construed as a limitation to the present application.

Claims (10)

1. The composite sound absorption plate with the multi-scale hole structure is characterized by comprising a composite sound absorption material, wherein the composite sound absorption material comprises a first-stage hole with the diameter of less than 2nm, a second-stage hole with the diameter of 0.5-3 mu m and a third-stage hole with the diameter of 0.1-3 mm; wherein, the volume weight of the first-stage holes accounts for 5-50% of the total volume weight of the holes, the volume weight of the second-stage holes accounts for 20-60% of the total volume weight of the holes, the volume weight of the third-stage holes accounts for 30-60% of the total volume weight of the holes, and the volume weight of the holes with other scales accounts for 0-10% of the total volume weight of the holes.
2. The composite acoustical panel of claim 1 wherein the primary pores have a diameter of less than 1.5nm; the diameter of the second-stage hole is 0.8-2 μm; the diameter of the third-stage hole is 0.5mm-2 mm.
3. A method of making a composite acoustical panel of a multi-scale pore structure as defined in any one of claims 1-2, comprising the steps of:
mixing an adhesive, an auxiliary agent and a microporous template material with a preset shape with an alkaline solution or an acidic solution to obtain an inorganic dispersion liquid;
carbonizing the bio-based material at a first specified temperature for a first specified time, and mixing the bio-based material with the inorganic dispersion liquid to solidify at a second specified temperature for a second specified time to obtain a porous solidified material;
activating the porous solidified material at a third specified temperature for a third specified time, and cooling, neutralizing, cleaning, drying and crushing to obtain porous particles;
mixing the porous particles and the porous material according to a first preset mass ratio, and mixing and hot-pressing the porous particles and the organic resin particles to obtain the composite sound-absorbing board; or mixing the porous particles and the porous material according to a second preset mass ratio, and mixing the porous particles and the porous material with a foaming material to obtain the composite sound-absorbing board.
4. The method of claim 3, wherein the step of activating the porous solidified material at a third specified temperature for a third specified time to obtain porous particles after cooling, neutralizing, washing, drying and pulverizing comprises:
carrying out thermal oxidation on the porous cured material at a fourth specified temperature for a fourth specified time to obtain the porous cured material with micron-sized pores;
and activating the porous solidified material with the micron-sized pores at a third specified temperature for a third specified time, and cooling, neutralizing, washing, drying and crushing to obtain the porous particles with the micron-sized pores and the nanometer-sized pores.
5. The method of claim 3, wherein the microporous template material is an organic fiber or microsphere;
the organic fiber comprises one or more of polyester fiber, polyvinyl alcohol fiber, polyvinyl butyral, polyacrylonitrile fiber and polyvinylpyrrolidone fiber, and the microsphere comprises one or more of polystyrene microsphere, polypropylene microsphere, polyethylene microsphere, polylactic acid microsphere and polyacrylonitrile microsphere.
6. The method of claim 3, wherein the adhesive comprises one or more of metakaolin, fly ash, mineral fines, silica sol, and coal tar.
7. The method of claim 3, wherein the bio-based material comprises one or more of coconut shells, bamboo, walnut shells, and straw.
8. The method of claim 3, wherein the porous material is one or more of carbon nanotubes, zeolites, molecular sieves, and graphene.
9. The method according to claim 3, wherein the foaming material is an aqueous polyurethane emulsion, and the preparation method of the aqueous polyurethane emulsion comprises the following steps:
preheating polyurethane prepolymer containing 1-3% of isocyanate groups at a fifth specified temperature for a fifth specified time to obtain the 1-5% aqueous polyurethane emulsion.
10. The method of claim 3, wherein the organic resin particles comprise one or more of phenolic resin particles, melamine resin particles, polyvinyl formal particles, polyvinyl butyral particles, and polymethyl methacrylate particles.
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