CN113816765A - Zeolite sound absorbing material and preparation method and application thereof - Google Patents

Zeolite sound absorbing material and preparation method and application thereof Download PDF

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CN113816765A
CN113816765A CN202111132422.0A CN202111132422A CN113816765A CN 113816765 A CN113816765 A CN 113816765A CN 202111132422 A CN202111132422 A CN 202111132422A CN 113816765 A CN113816765 A CN 113816765A
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zeolite
absorbing material
precursor
parts
sound
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滕超
黄天龙
郑俊文
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Shenzhen Polytechnic
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Abstract

The invention provides a zeolite sound absorbing material, wherein the macro morphology of the zeolite sound absorbing material is granular, the micro morphology of the zeolite sound absorbing material is characterized under SEM, the zeolite sound absorbing material is provided with first granules, second granules are piled and grown on the surfaces of the first granules, the grain diameter of the first granules is 15-55 mu m, and the grain diameter of the second granules is 25-545 nm. The prepared zeolite sound-absorbing material keeps complete macro-morphology and has a microstructure in which first particles are grown in an interlaced mode and the surfaces of the first particles are closely packed and grown by second smaller particles, so that the product has a rich pore structure, a larger specific surface area, a wider pore size range and higher mechanical strength.

Description

Zeolite sound absorbing material and preparation method and application thereof
Technical Field
The invention relates to a zeolite sound-absorbing material and a preparation method and application thereof.
Background
In recent years, with the increasingly thinner and lighter wearable electronic products, the traditional sound-absorbing material cannot meet the requirements of the micro-speaker for acoustic performance debugging and correction, and new sound-absorbing materials are continuously developed and tried. Through verification, the porous sound-absorbing material is placed in the rear cavity of the loudspeaker device and used for increasing the virtual volume of the rear cavity, so that the acoustic performance of the loudspeaker device can be effectively improved. At present, the novel sound-absorbing material with better application effect comprises natural zeolite, active carbon, white carbon black, zeolite powder with the silicon-aluminum ratio of more than 200, and the like, or a mixture of the materials. In speaker application, the sound-absorbing material in powder state is prepared into particles for the quantifiability and the process filling feasibility.
In order to obtain molecular sieves with proper shape and size, commercially synthesized zeolite molecular sieves in powder or granular form generally need to be prepared into monolithic structures by adding a binder, but the addition of the binder can cover the active sites of the zeolite molecular sieves, block part of the cell channels, and even cause a series of side reactions.
Compared with the traditional powder or granular zeolite, the integral zeolite sound-absorbing material without the adhesive has better mass transfer performance, higher mechanical strength and larger specific surface area.
The addition of the binder can block the pore channels of the zeolite molecular sieve, reduce the specific surface area and porosity, and finally lead to the deterioration of the low-frequency effect of the zeolite improved loudspeaker. Meanwhile, the surface modified active substances are covered, the content of active components is limited, and in addition, the combination of the adhesive and oxygen is easy to cause side reaction, so that an integral zeolite sound absorbing material without the adhesive is urgently needed to effectively solve the problems.
Disclosure of Invention
In order to solve the above-mentioned drawbacks of the prior art, the present invention provides a sound absorbing material made of zeolite, wherein the sound absorbing material has a granular macro-morphology, and the micro-morphology of the sound absorbing material is characterized by SEM, and the sound absorbing material has first particles, wherein second particles are grown on the surface of the first particles, the first particles have a particle size of 0.9 to 55 μm, and the second particles have a particle size of 5 to 545 nm.
Furthermore, the macroscopic morphology of the zeolite sound absorbing material is one or more of a cylinder type, an olive type and a regular sphere type.
Furthermore, the zeolite sound absorbing material has a pore structure, and the pore diameter of the pore structure is 0.05-56 μm.
Further, the raw materials for preparing the zeolite sound absorbing material comprise: 9-10 parts of white carbon black, 40-45 parts of siliceous pseudo-boehmite powder, 26-30 parts of silica sol, 1-4 parts of zeolite powder and 18-21 parts of deionized water.
The preparation method of the zeolite sound absorbing material comprises the following steps:
the method comprises the following steps: mixing and kneading white carbon black, siliceous pseudo-boehmite, silica sol, zeolite powder and deionized water to prepare a mixture;
step two: kneading and extruding the mixture prepared in the step one into regular particles with uniform size, and drying to prepare a preformed roasted precursor;
step three: roasting the roasted precursor prepared in the second step in an air atmosphere, and crystallizing to prepare a roasted precursor;
step four: and (3) carrying out hydrothermal crystallization treatment on the calcined precursor prepared in the third step to prepare the zeolite sound-absorbing material.
Further, the zeolite powder in the first step accounts for 12-15 wt% of the roasting precursor by mass.
Further, the calcination temperature in the third step is 450-850 ℃.
Furthermore, the roasting time in the third step is 5-16 h.
Further, the calcined precursor in the fourth step is subjected to hydrothermal crystallization, and the hydrothermal crystallization comprises the following steps: and (2) treating the roasted precursor in a solution containing NaOH and TPABr at the temperature of 130-250 ℃ for 2-5 days, filtering, washing and drying the prepared product, and roasting the product in an air atmosphere at the temperature of 300-600 ℃ for 2-8 hours to prepare the zeolite sound-absorbing material.
The zeolite sound absorbing material is used in a loudspeaker rear cavity and used for increasing the virtual volume of the rear cavity.
The zeolite sound-absorbing material prepared by the invention keeps complete macro-morphology, the micro-morphology is characterized by SEM, samples prepared by a hydrothermal crystallization method all have a structure that first particles are grown in an interlaced mode, the surfaces of the first particles are tightly stacked and grown by second particles, and the product has rich hole structures, larger specific surface area, wider aperture range and higher mechanical strength.
Drawings
FIG. 1 is a schematic structural view of the microstructure of a zeolitic acoustical absorbent;
1. a first particle; 2. a second particle.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
The present invention will be described in detail below with reference to the accompanying drawings and examples.
The technical solution of the invention is as follows:
a preparation method of a zeolite sound absorbing material comprises the following steps:
the method comprises the following steps: mixing and kneading white carbon black, siliceous pseudo-boehmite, silica sol, zeolite powder and deionized water to prepare a mixture;
according to the mass parts, 9-10 parts of white carbon black, 40-45 parts of siliceous pseudo-boehmite powder, 26-30 parts of silica sol, 1-4 parts of zeolite powder and 18-21 parts of deionized water are mixed and kneaded to prepare a mixture. The granular form is one or more of a cylinder form, an olive form and a regular sphere form, and is preferably a cylinder form.
Wherein the white carbon black is 10279-57-9, the siliceous pseudo-boehmite powder is YN-102D, the silica sol is GTS-9728, and the zeolite powder is: HZSM-5 zeolite powder, 100 mesh powder, special premix.
SiO in the silicon-containing pseudo-boehmite in the step one2Is 26 weight percent, the weight percent of water is 30 weight percent, and SiO in the silica sol2The mass percentage of the zeolite is 40 wt%, the zeolite powder is HZSM-5 zeolite powder, and the mass percentage of the zeolite powder in the roasting precursor is 12-15 wt%.
Step two, kneading and extruding the mixture prepared in the step one into ellipsoidal particles with the size of 1-3.5mm, and drying to prepare a preformed roasted precursor;
and drying the prepared mixture in an oven at the temperature of 45-85 ℃ for 15-64h to obtain the precursor before roasting.
Step three, roasting the roasted precursor prepared in the step two in an air atmosphere, and crystallizing to prepare a roasted precursor;
and placing the preformed roasting precursor into a high-temperature reaction kettle, and roasting for 5-16h at the temperature of 850 ℃ and 450 ℃ in an air atmosphere to obtain the roasted precursor.
Step four, carrying out hydrothermal crystallization treatment on the calcined precursor prepared in the step three to prepare the zeolite sound-absorbing material;
and (2) converting the roasted precursor, treating the roasted precursor for 2-5 days at the temperature of 130-600 ℃ in a solution containing NaOH and TPABr by a hydrothermal crystallization method, filtering, washing and drying the prepared product, placing the product into a high-temperature reaction kettle, and roasting the product for 2-8 hours at the temperature of 300-600 ℃ in an air atmosphere to obtain the final product, namely the zeolite sound-absorbing material.
The final product was obtained, which was measured macroscopically as a cylinder of 0.2 to 0.5mm in the above-mentioned zeolite sound-absorbing material.
Further, the microstructure of the above-mentioned zeolite sound absorbing material is characterized under SEM, and the schematic diagram of the microstructure of the above-mentioned zeolite sound absorbing material is shown in fig. 1, and it can be seen that the first particles 1, the second particles 2 piled and grown on the surface of the first particles 1, the particle size of the above-mentioned first particles 1 is 15-55 μm, and the particle size of the above-mentioned second particles 2 is 25-545 nm. Specifically, the precursor of the zeolite sound absorbing material is roasted and subjected to hydrothermal crystallization to form first particles 1 with a large particle size and second particles 2 with a small particle size, and the second particles 2 with the small particle size are attached to the surfaces of the first particles 1 with the large particle size to form a special stacking structure. In practice, the adjacent first particles 1 are in a staggered growth position relationship, the second particles 2 are attached to the surfaces of the first particles 1 in a close-packed state, or the second particles 2 act as bridges to act like adhesive bonds, and the adjacent first particles 1 are connected to form a monolithic material, and in fig. 1, in order to describe the position and size relationship between the first particles 1 and the second particles 2, the position relationship between the first particles 1 and the close-packed relationship of the second particles 2 are not shown.
Further, when the particle size of the first particles 1 is less than 15 μm, the growth attachment points of the second particles 2 are reduced, and thus the space with small pore size is reduced, when the particle size of the first particles 1 exceeds 55 μm, the occupied volume is larger, the specific surface area is smaller, so that the sound absorption coefficient of the sound absorption material is reduced, when the particle size of the second particles 2 is less than 25nm, the lower particle size affects the mechanical properties of the sound absorption material, when the particle size of the second particles 2 exceeds 545nm, the size is close to the size of the first particles 1, so that the growth sites of the first particles 1 are reduced, so that the relationship of staggered growth between the first particles 1 is difficult to form, and the second particles 2 are difficult to attach to the first particles 1, so that the sound absorption performance is reduced, and when the particle size is too large, the sound absorption performance of the sound absorption material is affected, so that a certain range of particle size is required.
Different first particles 1, different second particles 2, and the first particles 1 and the second particles 2 are connected with each other to form a rich pore structure, the porosity of the zeolite sound-absorbing material is 30-55%, further, the rich pore structure has a wide pore size range, the pore size of the zeolite sound-absorbing material is 0.05-56 μm, and further, the rich pore structure enables the zeolite sound-absorbing material to have a large specific surface area which is 230-850m2g-1. Furthermore, the zeolite sound absorbing material has high mechanical strength, and the mechanical strength is 430-840 kPa.
The zeolite sound-absorbing material with high specific surface area and without the adhesive prepared by the method is used as the rear cavity filler of the loudspeaker, so that the specific surface area and the porosity of the zeolite sound-absorbing material are increased, and the low-frequency effect of the loudspeaker is increased. Through hydrothermal crystallization recrystallization treatment on the zeolite sound-absorbing material, the polarity defect is eliminated, the mechanical strength is increased, and the adsorption of zeolite sound-absorbing material particles on heterogeneous molecules in the application process of a loudspeaker product is reduced, so that the sound-absorbing effect of the zeolite particles is controlled. By controlling the roasting temperature, the graded porous zeolite without the adhesive can be obtained, and the graded porous zeolite has better adsorption and desorption effects on air, so that the low-frequency sound effect of the loudspeaker is better.
Therefore, the zeolite sound-absorbing material with the morphology can be successfully prepared by adopting a hydrothermal crystallization method, and the zeolite sound-absorbing material has a rich pore structure, a larger specific surface area, a wider range and higher mechanical strength.
Further illustrated by specific examples:
example 1:
according to the mass parts, 9.9 parts of white carbon black, 40.1 parts of siliceous pseudo-boehmite powder, 27.8 parts of silica sol, 2.4 parts of HZSM-5 zeolite powder and 19.8 parts of deionized water are mixed, kneaded and extruded to prepare a 2mm cylindrical mixture, the cylindrical mixture is put into a drying oven to be dried for 24 hours at the temperature of 76 ℃ to prepare a cylindrical precursor with the diameter of 1.5mm, namely the precursor before roasting, the prepared precursor before roasting is roasted for 5 hours at the temperature of 450 ℃ in the air atmosphere to prepare the roasted precursor, the roasted precursor is converted by a hydrothermal crystallization method, the precursor is treated for 3 days at the temperature of 160 ℃ in a solution containing NaOH and TPABr, and the prepared product is washed, dried and then roasted for 4 hours at the temperature of 450 ℃ in the air atmosphere to prepare the final product which is marked as a zeolite sound-absorbing material A1.
Example 2:
according to the mass parts, 9.9 parts of white carbon black, 40.1 parts of siliceous pseudo-boehmite powder, 27.8 parts of silica sol, 2.4 parts of HZSM-5 zeolite powder and 19.8 parts of deionized water are mixed, kneaded and extruded to prepare a 2mm cylindrical mixture, the cylindrical mixture is put into a drying oven to be dried for 24 hours at the temperature of 76 ℃ to prepare a cylindrical precursor with the diameter of 1.5mm, namely the precursor before roasting, the prepared precursor before roasting is roasted for 5 hours at the temperature of 650 ℃ in the air atmosphere to prepare the roasted precursor, the roasted precursor is converted by a hydrothermal crystallization method, the precursor is treated for 3 days at the temperature of 160 ℃ in a solution containing NaOH and TPABr, and the prepared product is washed, dried and then roasted for 4 hours at the temperature of 450 ℃ in the air atmosphere to prepare the final product which is marked as a zeolite sound-absorbing material A2.
Example 3:
according to the mass parts, 9.9 parts of white carbon black, 40.1 parts of siliceous pseudo-boehmite powder, 30 wt% of water, 27.8 parts of silica sol, 2.4 parts of HZSM-5 zeolite powder and 19.8 parts of deionized water are mixed, kneaded and extruded to prepare a 2mm cylindrical mixture, the cylindrical mixture is put into an oven to be dried for 24 hours at 76 ℃ to prepare a cylindrical precursor with the diameter of 1.5mm, namely the precursor before roasting, the prepared precursor before roasting is roasted for 5 hours at 850 ℃ in the air atmosphere to prepare the roasted precursor, the roasted precursor is converted by a hydrothermal crystallization method, the cylindrical precursor is treated for 3 days at 160 ℃ in a solution containing NaOH and TPABr, and the prepared product is washed, dried and then roasted for 4 hours at 450 ℃ in the air atmosphere to prepare the final product which is marked as the sound-absorbing zeolite material A3.
Example 4:
according to the mass parts, 9.9 parts of white carbon black, 40.1 parts of siliceous pseudo-boehmite powder, 27.8 parts of silica sol, 1.4 parts of HZSM-5 zeolite powder and 20.8 parts of deionized water are mixed, kneaded and extruded to prepare a 2mm cylindrical mixture, the cylindrical mixture is put into a drying oven to be dried for 24 hours at the temperature of 76 ℃ to prepare a cylindrical precursor with the diameter of 1.5mm, namely the precursor before roasting, the prepared precursor before roasting is roasted for 5 hours at the temperature of 650 ℃ in the air atmosphere to prepare the roasted precursor, the roasted precursor is converted by a hydrothermal crystallization method, the precursor is treated for 3 days at the temperature of 160 ℃ in a solution containing NaOH and TPABr, and the prepared product is washed, dried and then roasted for 4 hours at the temperature of 450 ℃ in the air atmosphere to prepare the final product which is marked as the sound-absorbing zeolite material A4.
Example 5:
according to the mass parts, 9.9 parts of white carbon black, 40.1 parts of siliceous pseudo-boehmite powder, 27.8 parts of silica sol, 3.4 parts of HZSM-5 zeolite powder and 18.8 parts of deionized water are mixed, kneaded and extruded to prepare a 2mm cylindrical mixture, the cylindrical mixture is put into a drying oven to be dried for 24 hours at the temperature of 76 ℃ to prepare a cylindrical precursor with the diameter of 1.5mm, namely the precursor before roasting, the prepared precursor before roasting is roasted for 5 hours at the temperature of 650 ℃ in the air atmosphere to prepare the roasted precursor, the roasted precursor is converted by a hydrothermal crystallization method, the precursor is treated for 3 days at the temperature of 160 ℃ in a solution containing NaOH and TPABr, and the prepared product is washed, dried and then roasted for 4 hours at the temperature of 450 ℃ in the air atmosphere to prepare the final product which is marked as a zeolite sound-absorbing material A5.
Example 6:
according to the mass parts, 9 parts of white carbon black, 40.1 parts of siliceous pseudo-boehmite powder, 27.8 parts of silica sol, 2.4 parts of HZSM-5 zeolite powder and 19.7 parts of deionized water are mixed, kneaded and extruded to prepare a 2mm cylindrical mixture, the cylindrical mixture is put into a drying oven to be dried for 24 hours at the temperature of 76 ℃ to prepare a cylindrical precursor with the diameter of 1.5mm, namely the precursor before roasting, the prepared precursor before roasting is roasted for 5 hours at the temperature of 650 ℃ in the air atmosphere to prepare the roasted precursor, the roasted precursor is converted by a hydrothermal crystallization method, the precursor is treated for 3 days at the temperature of 160 ℃ in a solution containing NaOH and TPABr, and the prepared product is washed, dried and then roasted for 4 hours at the temperature of 450 ℃ in the air atmosphere to prepare the final product which is marked as the sound-absorbing zeolite material A6.
Example 7:
according to the mass parts, 9 parts of white carbon black, 45 parts of silicon-containing pseudo-boehmite powder, 26 parts of silica sol, 2 parts of HZSM-5 zeolite powder and 18 parts of deionized water are mixed, kneaded and extruded to prepare a 2mm cylindrical mixture, the cylindrical mixture is placed in a drying oven to be dried for 24 hours at the temperature of 76 ℃ to prepare a cylindrical precursor with the diameter of 1.5mm, namely the precursor before roasting, the prepared precursor before roasting is roasted for 5 hours at the temperature of 650 ℃ in the air atmosphere to prepare a roasted precursor, the roasted precursor is converted by a hydrothermal crystallization method, the precursor is treated for 3 days at the temperature of 160 ℃ in a solution containing NaOH and TPABr, and the prepared product is washed and dried and then roasted for 4 hours at the temperature of 450 ℃ in the air atmosphere to prepare a final product which is marked as a zeolite sound-absorbing material A7.
Example 8:
according to the mass parts, 9 parts of white carbon black, 40.6 parts of siliceous pseudo-boehmite powder, 30 parts of silica sol, 2.4 parts of HZSM-5 zeolite powder and 18 parts of deionized water are kneaded and extruded to prepare a 2mm cylindrical mixture, the cylindrical mixture is put into a baking oven to be dried for 24 hours at the temperature of 76 ℃ to prepare a cylindrical precursor with the diameter of 1.5mm, namely the precursor before baking, the prepared precursor is baked for 5 hours at the temperature of 650 ℃ in the air atmosphere to prepare a baked precursor, the baked precursor is converted by a hydrothermal crystallization method, the precursor is treated for 3 days at the temperature of 160 ℃ in a solution containing NaOH and TPABr, and the prepared product is washed, dried and then baked for 4 hours at the temperature of 450 ℃ in the air atmosphere to prepare a final product which is marked as a zeolite sound-absorbing material A8.
Example 9:
according to the mass parts, 9.1 parts of white carbon black, 40.1 parts of siliceous pseudo-boehmite powder, 27.8 parts of silica sol, 4 parts of HZSM-5 zeolite powder and 19 parts of deionized water are mixed, kneaded and extruded to prepare a 2mm cylindrical mixture, the cylindrical mixture is put into a baking oven to be dried for 24 hours at the temperature of 76 ℃ to prepare a cylindrical precursor with the diameter of 1.5mm, namely the precursor before baking, the prepared precursor is baked for 5 hours at the temperature of 450 ℃ in the air atmosphere to prepare a baked precursor, the baked precursor is converted by a hydrothermal crystallization method, the precursor is treated for 3 days at the temperature of 160 ℃ in a solution containing NaOH and TPABr, and the prepared product is washed, dried and then baked for 4 hours at the temperature of 450 ℃ in the air atmosphere to prepare a final product which is marked as a zeolite sound-absorbing material A9.
Comparative example 1:
according to the mass parts, 9.9 parts of white carbon black, 40.1 parts of siliceous pseudo-boehmite powder, 27.8 parts of silica sol, 2.4 parts of HZSM-5 zeolite powder and 19.8 parts of deionized water are mixed, kneaded and extruded to prepare a 2mm cylindrical mixture, the cylindrical mixture is put into a drying oven to be dried for 24 hours at the temperature of 76 ℃ to prepare a cylindrical precursor with the diameter of 1.5mm, namely the precursor before roasting, the prepared precursor before roasting is roasted for 5 hours at the temperature of 450 ℃ in the air atmosphere to prepare the roasted precursor, the roasted precursor is converted by a hydrothermal crystallization method, the precursor is treated for 3 days at the temperature of 160 ℃ in a solution containing NaOH and TPABr, and the prepared product is washed, dried and then roasted for 4 hours at the temperature of 450 ℃ in the air atmosphere to prepare the final product which is marked as the zeolite sound-absorbing material B1.
Comparative example 2:
according to the mass parts, 9.9 parts of white carbon black, 40.1 parts of siliceous pseudo-boehmite powder, 27.8 parts of silica sol, 2.4 parts of HZSM-5 zeolite powder and 19.8 parts of deionized water are mixed, kneaded and extruded to prepare a 2mm cylindrical mixture, the cylindrical mixture is put into a drying oven to be dried for 24 hours at the temperature of 76 ℃ to prepare a cylindrical precursor with the diameter of 1.5mm, namely the precursor before roasting, the prepared precursor before roasting is roasted for 5 hours at the temperature of 200 ℃ in the air atmosphere to prepare the roasted precursor, the roasted precursor is converted by a hydrothermal crystallization method, the precursor is treated for 3 days at the temperature of 160 ℃ in a solution containing NaOH and TPABr, and the prepared product is washed, dried and then roasted for 4 hours at the temperature of 450 ℃ in the air atmosphere to prepare the final product which is marked as the zeolite sound-absorbing material B2.
Comparative example 3:
according to the mass parts, 9.9 parts of white carbon black, 40.1 parts of siliceous pseudo-boehmite powder, 27.8 parts of silica sol, 2.4 parts of HZSM-5 zeolite powder and 19.8 parts of deionized water are mixed, kneaded and extruded to prepare a 2mm cylindrical mixture, the cylindrical mixture is put into a drying oven to be dried for 24 hours at the temperature of 76 ℃ to prepare a cylindrical precursor with the diameter of 1.5mm, namely the precursor before roasting, the prepared precursor before roasting is roasted for 5 hours at the temperature of 1000 ℃ in the air atmosphere to prepare the roasted precursor, the roasted precursor is converted by a hydrothermal crystallization method, the precursor is treated for 3 days at the temperature of 160 ℃ in a solution containing NaOH and TPABr, and the prepared product is washed, dried and then roasted for 4 hours at the temperature of 450 ℃ in the air atmosphere to prepare the final product which is marked as the zeolite sound-absorbing material B3.
Comparative example 4:
according to the mass parts, 9.9 parts of white carbon black, 40.1 parts of siliceous pseudo-boehmite powder, 27.8 parts of silica sol, 3 parts of adhesive, 2.4 parts of HZSM-5 zeolite powder and 16.8 parts of polyurethane suspension are used as adhesive, the mixture is kneaded and extruded to prepare a 2mm cylindrical mixture, the cylindrical mixture is put into a drying oven at 76 ℃ for drying for 24h to prepare a cylindrical precursor with the diameter of 1.5mm, namely the precursor before roasting, the prepared precursor before roasting is roasted at 450 ℃ for 5h in the air atmosphere to prepare a roasted precursor, the roasted precursor is converted by a hydrothermal crystallization method, the cylindrical precursor is treated in a solution containing NaOH and TPABr at 160 ℃ for 3 days, the prepared product is washed and dried, and then the prepared product is roasted at 450 ℃ for 4h in the air atmosphere to prepare the final product, which is marked as zeolite sound-absorbing material B4.
Comparative example 5:
according to the mass parts, 11.3 parts of white carbon black, 40.1 parts of siliceous pseudo-boehmite powder, 27.8 parts of silica sol, 1 part of HZSM-5 zeolite powder and 19.8 parts of deionized water are mixed, kneaded and extruded to prepare a 2mm cylindrical mixture, the cylindrical mixture is put into a drying oven to be dried for 24 hours at the temperature of 76 ℃ to prepare a cylindrical precursor with the diameter of 1.5mm, namely the precursor before roasting, the prepared precursor before roasting is roasted for 5 hours at the temperature of 450 ℃ in the air atmosphere to prepare the roasted precursor, the roasted precursor is converted by a hydrothermal crystallization method, the precursor is treated for 3 days at the temperature of 160 ℃ in a solution containing NaOH and TPABr, and the prepared product is washed, dried and then roasted for 4 hours at the temperature of 450 ℃ in the air atmosphere to prepare the final product which is marked as the sound-absorbing zeolite material B5.
Comparative example 6:
according to the mass parts, 6.3 parts of white carbon black, 40.1 parts of siliceous pseudo-boehmite powder, 27.8 parts of silica sol, 6 parts of HZSM-5 zeolite powder and 19.8 parts of deionized water are mixed, kneaded and extruded to prepare a 2mm cylindrical mixture, the cylindrical mixture is put into a drying oven to be dried for 24 hours at the temperature of 76 ℃ to prepare a cylindrical precursor with the diameter of 1.5mm, namely the precursor before roasting, the prepared precursor before roasting is roasted for 5 hours at the temperature of 450 ℃ in the air atmosphere to prepare the roasted precursor, the roasted precursor is converted by a hydrothermal crystallization method, the precursor is treated for 3 days at the temperature of 160 ℃ in a solution containing NaOH and TPABr, and the prepared product is washed, dried and then roasted for 4 hours at the temperature of 450 ℃ in the air atmosphere to prepare the final product which is marked as the sound-absorbing zeolite material B6.
Comparative example 7:
according to the mass parts, 9.9 parts of white carbon black, 30 parts of siliceous pseudo-boehmite powder, 37.9 parts of silica sol, 2.4 parts of HZSM-5 zeolite powder and 19.8 parts of deionized water are mixed, kneaded and extruded to prepare a 2mm cylindrical mixture, the cylindrical mixture is put into a drying oven to be dried for 24 hours at the temperature of 76 ℃ to prepare a cylindrical precursor with the diameter of 1.5mm, namely the precursor before roasting, the prepared precursor before roasting is roasted for 5 hours at the temperature of 450 ℃ in the air atmosphere to prepare the roasted precursor, the roasted precursor is converted by a hydrothermal crystallization method, the precursor is treated for 3 days at the temperature of 160 ℃ in a solution containing NaOH and TPABr, and the prepared product is washed, dried and then roasted for 4 hours at the temperature of 450 ℃ in the air atmosphere to prepare the final product which is marked as the sound-absorbing zeolite material B7.
Comparative example 8:
according to the mass parts, 9.9 parts of white carbon black, 50 parts of siliceous pseudo-boehmite powder, 17.9 parts of silica sol, 2.4 parts of HZSM-5 zeolite powder and 19.8 parts of deionized water are mixed, kneaded and extruded to prepare a 2mm cylindrical mixture, the cylindrical mixture is put into a drying oven to be dried for 24 hours at the temperature of 76 ℃ to prepare a cylindrical precursor with the diameter of 1.5mm, namely the precursor before roasting, the prepared precursor before roasting is roasted for 5 hours at the temperature of 450 ℃ in the air atmosphere to prepare the roasted precursor, the roasted precursor is converted by a hydrothermal crystallization method, the precursor is treated for 3 days at the temperature of 160 ℃ in a solution containing NaOH and TPABr, and the prepared product is washed, dried and then roasted for 4 hours at the temperature of 450 ℃ in the air atmosphere to prepare the final product which is marked as the sound-absorbing zeolite material B8.
The test method comprises the following steps:
1. observing the microstructure, namely observing the particle size of the particles through SEM;
2. specific surface area measurement using a SORPTOMATIC type specific surface area tester;
3. the mechanical strength is measured by using an XP nano indentation hardness tester;
4. the pore size was measured using a SORPTOMATIC pore size analyzer;
5. macroscopic morphology, and observing whether the final product has intact morphology:
and (3) excellent: more than 95% of the product keeps a complete cylinder structure;
the method comprises the following steps: over 75% of the product keeps a complete cylinder structure;
difference: more than 50% of the product keeps a complete cylinder structure;
6. sound absorption performance:
in the experiment, a SW series impedance tube test system of Beijing prestige company is adopted for testing the sound absorption performance of the sample, and the types of the impedance tubes adopted in the experiment are SW422 and SW 477.
The sound absorption capacity of a certain material or structure is expressed by a sound absorption coefficient alpha. The sound absorption coefficient alpha is equal to the ratio of the sound energy absorbed by the material (including transmitted sound energy) to the total sound energy incident on the material, i.e. the sound absorption coefficient alpha is equal to the ratio of the sound energy absorbed by the material (including transmitted sound energy) to the total sound energy incident on the material
Figure BDA0003278601020000091
E-total acoustic energy (J) incident to the material; ea-acoustic energy (J) absorbed by the material; Et-Acoustic energy (J) transmitted through the material. The larger the sound absorption coefficient, the stronger the sound absorption ability.
The experimental results are shown in table 1:
TABLE 1
Figure BDA0003278601020000092
Figure BDA0003278601020000101
According to the above experimental data, the zeolite sound absorbing materials prepared by the present invention, as described in examples 1-9, all maintain complete macro-morphology, and the micro-morphology is characterized by SEM, and for the samples prepared by hydrothermal crystallization, the samples have a structure in which first particles are grown by being interlaced with each other and the surfaces of the first particles are grown by being closely packed by smaller second particles, such that the product has a rich pore structure, a larger specific surface area and a wider pore size range, and a higher mechanical strength. Comparative example No sample prepared by hydrothermal crystallization method has corresponding structure, but the first particle has smaller particle size and lower mechanical strength, resulting in poorer sound absorption performance, comparative examples 2-3 show that too low or too high calcination temperature can cause narrower particle size distribution and can not maintain rich pore size structure, resulting in poorer sound absorption performance, comparative example 4 is a scheme using adhesive, although having excellent macro particles, too large particle size can not form a structure of stacking small particles to form large particles, and the use of adhesive can cause the pore channel on the particle surface to be blocked, porosity and specific surface area to be reduced, thereby reducing sound absorption performance, in comparative example 6, the content of white carbon black is too low, the content of zeolite powder is more, resulting in smaller final particle size, and also can not form a structure of stacking small particles to form large particles, thus having insufficient sound absorption performance, meanwhile, the mechanical property is poor, in comparative examples 7 to 8, the content of the silicon-containing pseudo-boehmite powder and the content of the silica sol are too low or too high, and finally, good macroscopic morphology can not be maintained, and the sound absorption performance can not meet the requirement.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. The zeolite sound absorption material is characterized in that the macro morphology of the zeolite sound absorption material is granular, the micro morphology of the zeolite sound absorption material is characterized under SEM, first particles are visible, second particles are piled and grown on the surfaces of the first particles, the particle size of the first particles is 15-55 mu m, and the particle size of the second particles is 25-545 nm.
2. A zeolite sound absorbing material as claimed in claim 1, wherein the zeolite sound absorbing material has a macro morphology in one or more of a cylinder type, an olive type, and a regular sphere type.
3. A zeolite sound-absorbing material as claimed in claim 1, wherein the zeolite sound-absorbing material has a pore structure having a pore diameter of 0.05 to 56 μm.
4. The sound absorbing material of claim 1, wherein the sound absorbing material is prepared from the following raw materials: 9-10 parts of white carbon black, 40-45 parts of siliceous pseudo-boehmite powder, 26-30 parts of silica sol, 1-4 parts of zeolite powder and 18-21 parts of deionized water.
5. The method for preparing a sound absorbing material of zeolite according to any of claims 1 to 4, comprising the steps of:
the method comprises the following steps: mixing and kneading white carbon black, siliceous pseudo-boehmite, silica sol, zeolite powder and deionized water to prepare a mixture;
step two: kneading and extruding the mixture prepared in the step one into regular particles with uniform size, and drying to prepare a preformed roasted precursor;
step three: roasting the roasted precursor prepared in the second step in an air atmosphere, and crystallizing to prepare a roasted precursor;
step four: and (3) carrying out hydrothermal crystallization treatment on the calcined precursor prepared in the third step to prepare the zeolite sound-absorbing material.
6. The method for preparing the sound absorbing material of zeolite according to claim 5, wherein the zeolite powder in the first step accounts for 12-15 wt% of the mass of the calcination precursor.
7. The method for preparing the sound absorbing material of zeolite as claimed in claim 5, wherein the calcination temperature in the third step is 450-850 ℃.
8. The method for preparing the sound absorbing material of zeolite according to claim 5, wherein the calcination time in the third step is 5-16 h.
9. The method for preparing the sound absorbing material of zeolite according to claim 5, wherein the calcined precursor in the fourth step is subjected to hydrothermal crystallization, and the hydrothermal crystallization comprises the following steps: and (2) treating the roasted precursor in a solution containing NaOH and TPABr at the temperature of 130-250 ℃ for 2-5 days, filtering, washing and drying the prepared product, and roasting the product in an air atmosphere at the temperature of 300-600 ℃ for 2-8 hours to obtain the zeolite sound-absorbing material.
10. Use of a zeolitic acoustic material according to any of claims 1 to 4, characterized in that it is used in the rear cavity of a loudspeaker for increasing the virtual volume of the rear cavity.
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CN105731848A (en) * 2016-01-28 2016-07-06 歌尔声学股份有限公司 Preparation method of sound absorbing material particles and sound absorbing material particles
CN107708040A (en) * 2016-08-31 2018-02-16 歌尔股份有限公司 Loudspeaker module

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CN115570850A (en) * 2022-05-24 2023-01-06 珠海格力新材料有限公司 Sound absorption and insulation cotton and preparation process thereof

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Application publication date: 20211221