CN115725111A - Composite aerogel with broadband low-frequency sound absorption and heat insulation functions and preparation and application thereof - Google Patents
Composite aerogel with broadband low-frequency sound absorption and heat insulation functions and preparation and application thereof Download PDFInfo
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Abstract
The invention discloses a composite aerogel with broadband low-frequency sound absorption and heat insulation and a preparation method and application thereof, wherein the preparation method comprises the following steps: s1: preparing a spinning solution: dissolving a polymer in a solvent to obtain a solution with the concentration of 10-20 wt%, adding a metal-organic framework material after stirring, uniformly stirring to obtain a spinning solution, and performing electrostatic spinning to obtain a nanofiber membrane; s2: preparing the composite aerogel: crushing the nanofiber membrane obtained in the step S1 under mechanical stirring, adding the crushed nanofiber membrane into a solvent, uniformly stirring, adding Kevlar fibers and an aziridine crosslinking agent, pre-freezing the mixed solution, and freeze-drying the frozen sample to obtain an uncrosslinked aerogel; s3: and (3) crosslinking the obtained uncrosslinked aerogel at 70-80 ℃ to obtain the crosslinked composite aerogel. The composite aerogel disclosed by the invention has the characteristics of excellent heat insulation performance and capability of absorbing broadband low-frequency sound.
Description
Technical Field
The invention relates to the technical field of sound absorption and heat insulation of composite materials, in particular to a composite aerogel with broadband low-frequency sound absorption and heat insulation as well as preparation and application thereof.
Background
Noise pollution from transportation vehicles, buildings and social activities severely interferes with people's daily life and may lead to health risks such as insomnia, dysphoria and cardiac insufficiency. Generally, porous materials have good sound absorption performance at high frequencies, but noise in daily life exhibits broadband distribution, and most of the noise is distributed in a low frequency range (< 1000 Hz), which is not the dominant range of the commonly used porous materials, so that sound absorption materials with better performance are required.
Attenuation of low frequency sound has been a challenging task. The common micropore plate sound absorber has a good sound absorption effect under low frequency through a local vibration resonance effect. They are resonant materials that absorb very low frequency acoustic energy depending on the designed resonant frequency. However, their effective absorption bands are usually relatively narrow, typically only 100-300Hz. Therefore, a broadband low-frequency sound absorption material is urgently needed, and a more suitable living and working environment is created for people.
In recent years, further introduction of nano-level porosity substances into conventional microporous or mesoporous materials is becoming a useful strategy for improving sound absorption and heat insulation performance of the overall materials. Since the hierarchical pore structure provides sufficient reaction area and more complex path for the sound wave, it greatly increases the consumption of the sound energy and strongly scatters the sound wave. Also, the abundance of micropores in the material can suppress gas movement and reduce the mean free path to a few nanometers, and the mixed structure is also beneficial for reducing heat conduction, resulting in low thermal conductivity.
Currently, the most common method for preparing hierarchical pore structures includes: MOF particles (acsappl. Mater. Interfaces,2020, 12, 55316-55323, cellulose,2022, 29, 355-365) are grown in situ on the surface of a porous fabric, or the MOF is grown in situ on cellulose nanocrystals and then the composite is freeze-dried to prepare aerogel (Nano-microlett. 2020, 12,9). In both methods, MOF particles are introduced into the original porous material by an in-situ growth method so as to endow the material with a multi-level pore structure, the preparation time is long, the specific surface area is small, and the content and the particle size of porous nano particles are difficult to control, so that the sound absorption range cannot be effectively covered below 1000 Hz.
Therefore, it is necessary to design a method for preparing aerogel having excellent heat insulation property and absorbing broadband low frequency sound.
Disclosure of Invention
The invention aims to provide a composite aerogel with broadband low-frequency sound absorption and heat insulation as well as preparation and application thereof, and the existing preparation method has the advantages of long preparation time, small specific surface area in the aerogel and difficulty in controlling the content and particle size of porous nanoparticles, so that the sound absorption range cannot be effectively covered below 1000 Hz.
In order to achieve the above purpose, the present invention provides a composite aerogel with broadband low-frequency sound absorption and thermal insulation, and a preparation method and an application thereof, wherein the preparation method comprises the following steps:
s1: preparing electrostatic spinning solution: dissolving polymer powder in a solvent to obtain a solution with the concentration of 10-20 wt%, stirring and defoaming, adding a metal-organic framework material, uniformly stirring to obtain a spinning solution, and performing electrostatic spinning to obtain a nanofiber membrane; wherein the polymer is selected from a polymer containing a benzene ring or a polar group; the solvent is a solvent capable of dissolving the polymer but not the metal-organic framework material;
s2: preparing the composite aerogel: crushing the nanofiber membrane obtained in the step S1 under mechanical stirring, adding the crushed nanofiber membrane into an alcohol solvent, uniformly stirring, adding Kevlar fibers and an aziridine crosslinking agent, pre-freezing the mixed solution, and freeze-drying the frozen sample to obtain an uncrosslinked aerogel;
s3: and (3) crosslinking the obtained uncrosslinked aerogel at 70-80 ℃ to obtain the crosslinked composite aerogel.
Preferably, the nanofiber membrane in the step S2 is broken into short fibers with mechanical agitation, and the average length thereof is 15 to 30 μm.
Preferably, the polymer in step S1 is a polymer containing benzene rings or polar groups, comprising: any one of polyacrylonitrile, polyurethane, polystyrene and polyvinyl alcohol; the solvent in step S1 includes: n, N-dimethylformamide or water; the weight ratio of the polymer to the metal organic framework material in the step S1 is 1 (0.1-0.6), and the concentration of the polymer in the solvent is 5-20 wt%.
Preferably, the metal-organic framework material in step S1 includes: ZIF-8, ZIF-67, HKUST-1, UIO66-NH 2 And MIL-101 (Cr).
Preferably, the electrospinning time in the step S1 is 1 to 10 hours, and the voltage used is 18 to 25KV.
Preferably, the mass ratio of the nano fiber and the Kevlar fiber after being crushed in the step S2 is 1:3-3:1; the alcohol solvent in the step S2 is a mixed solvent of tertiary butanol and water, and the mixing ratio of the tertiary butanol and the water is 1:9-9:1.
Preferably, the temperature of the freeze drying in the step S2 is-45 to-55 ℃, the pressure is 5 to 15Pa, and the freezing time is 12 to 72 hours.
Preferably, the crosslinking time in the step S3 is 1 to 3 hours; the crosslinking agent comprises: any one of GY-225, XR-100 and CX-300; the dosage of the cross-linking agent is 1-10%.
Preferably, the composite aerogel material has a large specific surface area which is more than 700m 2 /g。
Preferably, the composite aerogel material with broadband low-frequency sound absorption and thermal insulation is applied to a place with noise less than 1000 Hz.
The composite aerogel material and the method solve the problems that the existing aerogel does not have broadband low-frequency sound absorption characteristics and has insignificant heat insulation performance, and have the following advantages:
1. the high-performance low-frequency sound absorption and heat insulation aerogel is obtained by utilizing commercial products through a simple preparation process, all raw materials are industrialized, the preparation process is simple, the time consumption is very small, and the large-scale production is facilitated.
2. The MOF (metal-organic framework material) is blended with a polymer at a high loading of 10-60 wt% by a direct blending method, and then is electrospun into fibers together, and is further prepared into the aerogel through freeze drying, so that the function of the electrospun fiber aerogel is combined with the MOF (metal-organic framework material), the composite aerogel is endowed with a high specific surface area, and has an abundant hierarchical pore structure and an extremely low density. Due to the large specific surface area in the aerogel and the self-contained nanoscale interconnected pore structure in the MOF (metal-organic framework material) rich on the surface of the nano fibers, the nano-porous structure can concentrate low-frequency sound energy in pores, increase the contact area between the material and an air domain, increase viscous dissipation due to the movement of air in the porous structure, and increase the dissipation and absorption of the sound energy due to the repeated propagation of the sound waves among the materials; therefore, the composite aerogel not only has higher sound absorption coefficient (0.99 at 500 Hz) at low frequency, but also has broadband low-frequency sound absorption characteristic (the sound absorption coefficient is more than 0.6 between 250 and 900 Hz); in addition, the composite nanofiber aerogel has excellent thermal insulation performance (the thermal conductivity coefficient is less than 0.026W/mK); the addition of Kevlar fibers in the system endows the composite nanofiber aerogel with strong structural stability, and the materials can still maintain structural integrity after cyclic compression.
Drawings
FIG. 1 is a microstructure (A) and a specific surface area map (B) of the PAN @ ZIF8-Kevlar nanofiber aerogel in example 1 of the present invention.
FIG. 2 is a graph of the sound absorption properties of the PAN @ ZIF8-Kevlar nanofiber aerogel in example 1 of the present invention and the PAN-Kevlar nanofiber aerogel in comparative example 1.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, 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 invention.
Example 1
A PAN @ ZIF8-Kevlar nanofiber aerogel is prepared by the following steps:
(1) Preparation of PAN @ ZIF-8 electrostatic spinning solution: dissolving PAN (polyacrylonitrile) powder (with the molecular weight of 15 ten thousand) in N, N-Dimethylformamide (DMF) solution to obtain a solution with the concentration of 13wt%, stirring for 20 hours, dispersing ZIF-8 powder in DMF, stirring uniformly, mixing the PAN solution and the ZIF-8 dispersion solution to obtain a spinning solution, spraying the prepared spinning solution onto silicone oil paper through an electrostatic spinning machine, and removing the silicone oil paper from a roller after 2 hours to obtain a nanofiber membrane;
(2) Crushing and cutting the obtained PAN @ ZIF-8 electrospun fiber membrane into small blocks by using a high-speed homogenizer to obtain a uniform nanofiber dispersion, wherein the length of most fibers is about 20 mu m, then dispersing the fibers in a tert-butyl alcohol-water mixed solvent with the volume ratio of 5:5, then adding Kevlar short fibers, stirring and mixing the two fibers, adding a crosslinking agent aziridine crosslinking agent XR-100, wherein the content of the crosslinking agent is 5wt% of the weight of the two fibers (the nano electrospun fibers and the Kevlar short fibers), freezing the dispersion at-20 ℃ for 12 hours, and freeze-drying at 5Pa for 72 hours;
(3) And placing the obtained uncrosslinked aerogel in an oven at 70 ℃ for 1h to obtain the crosslinked PAN @ ZIF8-Kevlar nanofiber aerogel.
Example 2
PAN @ UIO66-NH 2 -Kevlar nanofibrous aerogel, prepared substantially in the same way as in example 1, with the difference that:
this example uses UIO66-NH 2 Powder;
in the step (1), the concentration of the obtained solution is 15wt%, the stirring time is 24 hours, and the spinning solution is kept stand on silicone oil paper for 3 hours;
in the step (2), the length of most of the broken fibers is about 27 microns, the cross-linking agent is aziridine cross-linking agent CX-300 with the content of 6wt% of the two fibers, the dispersion is frozen for 10 hours and freeze-dried for 48 hours at 5Pa, and the volume ratio of the tertiary butanol-water mixed solvent is 6:4;
in step (3), the obtained uncrosslinked aerogel was placed in an oven at 80 ℃ for 2h.
Example 3
A PU @ ZIF-67-Kevlar nanofiber aerogel is prepared by the method which is basically the same as that of the embodiment 1, and the differences are as follows:
the present example used ZIF-67 powder and PU (polyurethane) powder;
in the step (1), taking PU powder (with the molecular weight of 20 ten thousand) and keeping the solution concentration at 10wt%, and standing the spinning solution on silicone oil paper for 3 hours;
in step (2), the length of most of the fibers after crushing is about 24 μm and the content of the cross-linking agent is 6wt%, freezing the dispersion for 16 hours and lyophilizing at 5Pa for 60 hours;
in step (3), the obtained uncrosslinked aerogel was placed in an oven for 2h.
Example 4
A PS @ HKUST-1-Kevlar nanofiber aerogel, the preparation method is basically the same as that of example 1, except that:
this example used HKUST-1 powder and PS (polystyrene) powder;
in the step (1), PS powder (with the molecular weight of 20 ten thousand) is taken, the solution concentration is 15wt%, and the stirring is carried out for 22 hours;
in the step (2), most of the fibers after crushing have a length of about 29 μm, the solvent used is a tert-butanol/water mixed solvent, the crosslinking agent used is an aziridine crosslinking agent CX-300, the content of the crosslinking agent is 7wt%, and the dispersion is lyophilized at 5Pa for 60 hours;
in step (3), the obtained uncrosslinked aerogel was placed in an oven at 80 ℃ for 3h.
Example 5
A PVA @ MIL-101 (Cr) -Kevlar nanofiber aerogel, the preparation method of which is basically the same as that of the example 1, except that:
this example used MIL-101 (Cr) powder and PVA (polyvinyl alcohol) powder;
in the step (1), PVA1799 powder is dissolved in water, and the concentration of the solution is 11wt%;
in step (2), most of the fibers after the crushing had a length of about 28 μm, a mixed solvent of t-butanol and water was used as a solvent, an aziridine-based crosslinking agent CX-300 was used as a crosslinking agent, and the content of the crosslinking agent was 6wt%, and the dispersion was lyophilized at 5Pa for 50 hours.
Comparative example 1
Preparation of PAN-Kevlar nanofiber aerogel
(1) Preparing PAN electrostatic spinning solution: dissolving PAN powder (with the molecular weight of 15 ten thousand) in N, N-Dimethylformamide (DMF) solution to obtain a solution with the concentration of 13wt%, stirring for 24 hours, defoaming to obtain a spinning solution, spraying the prepared spinning solution onto silicone oil paper through an electrostatic spinning machine, and removing the silicone oil paper from a roller after 3 hours to obtain a nanofiber membrane;
(2) Crushing and cutting the obtained PAN electrospun fiber membrane into small pieces by using a high-speed homogenizer to obtain a uniform nanofiber dispersion, wherein the length of most fibers is about 26 mu m, then dispersing the fibers in a solvent, adding Kevlar short fibers, stirring and mixing the two fibers, adding a crosslinking agent of aziridine, namely CX-300, wherein the content of the crosslinking agent is 5wt% of the weight of the fibers, freezing the dispersion at-20 ℃ for 12 hours, and freeze-drying the dispersion at 5Pa for 60 hours;
(3) And placing the obtained uncrosslinked aerogel in an oven at 70 ℃ for 1h to obtain the crosslinked PAN-Kevlar nanofiber aerogel.
Comparative example 2
Preparation of PS nanofiber aerogel
(1) Preparing a PS electrostatic spinning solution: dissolving PS powder (with the molecular weight of 20 ten thousand) in N, N-Dimethylformamide (DMF) solution, stirring for 24 hours, defoaming to obtain spinning solution, spraying the prepared spinning solution onto silicone oil paper through an electrostatic spinning machine, and removing the silicone oil paper from a roller after 3 hours to obtain a nanofiber membrane;
(2) Crushing and cutting the obtained electrospun fiber membrane into small pieces by using a high-speed homogenizer to obtain a uniform nanofiber dispersion, wherein the length of most fibers is about 25 mu m, then dispersing the fibers in a solvent, adding Kevlar short fibers, stirring and mixing the two fibers, adding a crosslinking agent of aziridine, namely CX-300, wherein the content of the crosslinking agent is 6wt% of the weight of the two fibers, freezing the dispersion at-20 ℃ for 12 hours, and freeze-drying the dispersion at 5Pa for 60 hours;
(3) And placing the obtained uncrosslinked aerogel in an oven at 80 ℃ for 1h to obtain the crosslinked PS-Kevlar nanofiber aerogel.
Test example 1
The microscopic morphology and the specific surface area of the composite aerogel
1. Test method
The aerogel prepared in example 1 was used, the surface morphology of the aerogel was observed by a scanning electron microscope, and the aerogel was subjected to a gold-spraying treatment before the observation. Specific surface area was calculated using an isothermal adsorption apparatus and measured at 273K on Micromeritics a sap 2020 (Micromeritics Instruments corp., USA) after degassing the sample at 120 ℃ for 6 hours.
2. Test results
The SEM picture of the composite aerogel is shown in A of figure 1, and micron-scale pore structures can be formed inside the aerogel prepared by slow freezing, and the micropore volume is more than 0.4cm 3 G, as shown in B of FIG. 1, the electrospun nanofibers are loaded with high content of MOF nanoparticles, so that the aerogel contains a large amount of microporous structures, thereby bringing about high specific surface area which is more than 700m 2 /g。
Test example 2
Thermal conductivity of composite aerogels of the invention and comparative examples
1. Test method
The thermal conductivity of the aerogels prepared in example 1 and comparative examples 1 and 2 was measured using a thermal conductivity tester in accordance with the international standard ASTM-D5470. At the instantAnd completing the test of the heat conductivity coefficient in a state isotropy and heat capacity mode. Thermal conductivity lambda (unit is W.m) -1 ·K -1 ) Is the thermal diffusion coefficient Cp (in mm) 2 ·s -1 ) Heat capacity α (unit is J.g) -1 ·K -1 ) And a density ρ (in g · cm) -3 ) The test results are shown in table 1.
2. Test results
TABLE 1 thermal conductivity of aerogels in the examples of the invention
Test example 3
Low frequency sound absorption Properties of composite aerogels of the invention and comparative examples
1. Test method
The sound absorption properties of the samples of example 1 and comparative example 1 were tested with reference to the ISO 10534-2 1998 standard for the sound absorption characteristics of the samples; impedance tubes (SW 422 and SW477, bswatechnologyco., ltd) were used to detect samples at 100-1600 Hz.
2. Test results
As shown in fig. 2, the aerogel of comparative example 1 has a very low sound absorption coefficient at low frequencies, and the sound absorption coefficient is only 0.15 even at 1100Hz, indicating that it has a relatively poor sound absorption effect in the low frequency range. However, the novel aerogel of example 1 has not only a high sound absorption coefficient at low frequencies (0.99 at 500 Hz), but also broad-band low-frequency sound absorption characteristics (sound absorption coefficient of 250-900Hz is greater than 0.6).
While the present invention has been described in detail with reference to the preferred embodiments, it should be understood that the above description should not be taken as limiting the invention. Various modifications and alterations to this invention will become apparent to those skilled in the art upon reading the foregoing description. Accordingly, the scope of the invention should be determined from the following claims.
Claims (10)
1. The preparation method of the composite aerogel material with broadband low-frequency sound absorption and heat insulation is characterized by comprising the following steps of:
s1: preparing an electrostatic spinning solution: dissolving polymer powder in a solvent to obtain a solution with the concentration of 10-20 wt%, stirring and defoaming, adding a metal-organic framework material, uniformly stirring to obtain a spinning solution, and performing electrostatic spinning to obtain a nanofiber membrane; wherein the polymer is selected from a polymer containing a benzene ring or a polar group; the solvent is a solvent capable of dissolving the polymer but not the metal-organic framework material;
s2: preparing the composite aerogel: crushing the nanofiber membrane obtained in the step S1 under mechanical stirring, adding the crushed nanofiber membrane into an alcohol solvent, uniformly stirring, adding Kevlar fibers and an aziridine crosslinking agent, pre-freezing the mixed solution, and freeze-drying the frozen sample to obtain an uncrosslinked aerogel;
s3: and (3) crosslinking the obtained uncrosslinked aerogel at 70-80 ℃ to obtain the crosslinked composite aerogel.
2. The method for preparing a composite aerogel material having both broadband and low frequency sound absorption and thermal insulation functions as claimed in claim 1, wherein the nanofiber membrane in step S2 is broken into short fibers with an average length of 15-30 μm under mechanical stirring.
3. The method for preparing a composite aerogel material having both broadband and low frequency sound absorption and thermal insulation functions as claimed in claim 1, wherein the polymer in step S1 is a polymer containing benzene ring or polar group, and comprises: any one of polyacrylonitrile, polyurethane, polystyrene and polyvinyl alcohol; the solvent in step S1 includes: n, N-dimethylformamide or water; the weight ratio of the polymer to the metal organic framework material in the step S1 is 1 (0.1-0.6), and the concentration of the polymer in the solvent is 5-20 wt%.
4. The method for preparing a composite aerogel material having both broadband low frequency sound absorption and thermal insulation properties as claimed in claim 1, whereinIn step S1, the metal-organic framework material includes: ZIF-8, ZIF-67, HKUST-1, UIO66-NH 2 And MIL-101 (Cr).
5. The method for preparing the composite aerogel material with the functions of broadband low-frequency sound absorption and heat insulation according to claim 1, wherein the electrostatic spinning time in the step S1 is 1-10 hours, and the applied voltage is 18-25 KV.
6. The preparation method of the composite aerogel material with broadband low-frequency sound absorption and heat insulation functions as claimed in claim 1, wherein the mass ratio of the nano fibers and the Kevlar fibers crushed in the step S2 is 1:3-3:1; the alcohol solvent in the step S2 is a mixed solvent of tertiary butanol and water, and the mixing ratio of the tertiary butanol to the water is 1:9-9:1.
7. The preparation method of the composite aerogel material with broadband low-frequency sound absorption and heat insulation functions as claimed in claim 1, wherein the temperature of the freeze drying in the step S2 is-45 to-55 ℃, the pressure is 5 to 15Pa, and the freezing time is 12 to 72 hours.
8. The method for preparing the composite aerogel material with broadband low-frequency sound absorption and thermal insulation functions as claimed in claim 1, wherein the crosslinking time in the step S3 is 1-3 hours; the crosslinking agent comprises: any one of GY-225, XR-100 and CX-300; the dosage of the cross-linking agent is 1-10 wt% of the total weight of the polymer and the metal-organic framework material.
9. The composite aerogel material prepared by the preparation method of any one of claims 1 to 8 and having both broadband low-frequency sound absorption and heat insulation functions, wherein the composite aerogel material has a large specific surface area which is more than 700m 2 /g。
10. Use of the composite aerogel material of claim 9 having both broadband low frequency sound absorption and thermal insulation in locations with noise less than 1000 Hz.
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