CN112126110B - Polyimide sound absorption foam with spherical pit microstructure and preparation method thereof - Google Patents
Polyimide sound absorption foam with spherical pit microstructure and preparation method thereof Download PDFInfo
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- CN112126110B CN112126110B CN202010898286.5A CN202010898286A CN112126110B CN 112126110 B CN112126110 B CN 112126110B CN 202010898286 A CN202010898286 A CN 202010898286A CN 112126110 B CN112126110 B CN 112126110B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/30—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by mixing gases into liquid compositions or plastisols, e.g. frothing with air
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1003—Preparatory processes
- C08G73/1035—Preparatory processes from tetracarboxylic acids or derivatives and diisocyanates
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- G—PHYSICS
- G10—MUSICAL INSTRUMENTS; ACOUSTICS
- G10K—SOUND-PRODUCING DEVICES; METHODS OR DEVICES FOR PROTECTING AGAINST, OR FOR DAMPING, NOISE OR OTHER ACOUSTIC WAVES IN GENERAL; ACOUSTICS NOT OTHERWISE PROVIDED FOR
- G10K11/00—Methods or devices for transmitting, conducting or directing sound in general; Methods or devices for protecting against, or for damping, noise or other acoustic waves in general
- G10K11/16—Methods or devices for protecting against, or for damping, noise or other acoustic waves in general
- G10K11/162—Selection of materials
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
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Abstract
The invention discloses polyimide sound absorption foam with a spherical pit microstructure and a preparation method thereof, wherein the preparation method comprises the following steps of S1, preparing a foaming white material containing a nonionic surfactant, wherein the total part of the foaming white material is 250-450 parts by weight, and the dosage of the nonionic surfactant for preparing the foaming white material is 75-125 parts by weight; the nonionic surfactant is composed of a polyol polymer and a polysiloxane-polyether copolymer, and the mass ratio is 0.8; s2, uniformly mixing a foaming white material containing a nonionic surfactant with a foaming black material, and foaming and forming to obtain a polyimide foam intermediate; and S3, demolding the foam intermediate, and placing the foam intermediate in a forced air drying box for curing to finally obtain the polyimide sound absorption foam with the spherical pit microstructure. The prepared polyimide sound absorption foam can improve the reflection and absorption effects of sound waves in the foam holes so as to enhance the consumption capacity of the material to the sound waves.
Description
Technical Field
The invention relates to a polyimide foam material and a preparation method thereof, in particular to polyimide sound absorption foam with a spherical pit microstructure and a preparation method thereof.
Background
There are three main mechanisms for sound absorption of foams: the first is that air molecules in the porous sound absorption material rub with the hole wall to convert sound energy into heat energy for dissipation; the second is that when longitudinal sound waves penetrate through the porous material, air in pores is periodically compressed and released, so that energy consumption in the energy conversion process is caused; the third is that the acoustic energy is converted into mechanical energy and thermal energy by the resonance of the hole wall. It follows that the surface microstructure of the cell walls has a non-negligible effect on the dissipation of acoustic energy by the sound-absorbing material. The surface roughness and the specific surface area of the foam wall with the surface microstructure are further improved, the viscous absorption effect of the foam wall on noise can be effectively enhanced, and the sound absorption performance of the foam material is further improved.
In current research, the resin skeleton of the foam material matrix and the surface of the window are basically smooth surfaces. Although it has been studied to increase the roughness by loading a nanomaterial on the surface of the foam skeleton.
For example, chinese patent document CN110975932A discloses a method for preparing a photocatalytic carrier by combining nano-scale inorganic catalyst powder and the surface of an organic high molecular polymer, wherein nano-scale TiO is used 2 Loaded on polyurethane foam, lays a foundation for realizing ICPB technology in photocatalysis.
Chinese patent document CN110124748A discloses a preparation method and application of a melamine formaldehyde foam loaded nano manganese dioxide material, and the generated manganese dioxide is deposited on the inner wall of the foam, thereby being beneficial to the absorption and decomposition of formaldehyde and relating to the field of air purification and catalytic materials.
Chinese patent document CN110102271a provides a porous section containing nano-adsorbent for VOCs treatment, and a method and an apparatus thereof, the nano-adsorbent is loaded on a porous substrate in a self-assembly manner, the increased specific surface area can promote the rapid proceeding of surface adsorption, the adsorption efficiency is improved, and the method and the apparatus are applied to the field of VOCs waste gas treatment.
However, with some post-treatment added rough surfaces, the firmness is not long lasting. There are also many studies to apply biomimetic surface microstructures to material design today.
For example, chinese patent document CN108955784a discloses a V-cone flowmeter with a bionic microstructure on the surface, which effectively achieves the purposes of drag reduction, energy saving and emission reduction by arranging the bionic microstructures such as ribs, grooves, convex hulls, pits and the like on the surface of a cone.
Chinese patent document CN109822950A introduces a polymer integrated forming method with an anti-icing function, and an anti-icing microstructure is designed on the surface of a polymer-based material, so that the polymer integrated forming method has important significance for the development of an airplane anti-icing technology.
For the polymer sound absorption foam material, the research on the microstructure design on the matrix resin framework and the window surface and the influence of the microstructure on the sound absorption performance of the material is still in a blank state at present.
Disclosure of Invention
In view of the above, the present invention provides a polyimide sound absorption foam having a spherical pit microstructure, which can improve the reflection and absorption of sound waves inside the cells to enhance the consumption of sound waves by the material, and a preparation method thereof.
The adopted technical scheme is as follows:
a preparation method of polyimide sound absorption foam with a spherical pit microstructure comprises the following steps:
s1, preparing a foaming white material containing a nonionic surfactant, wherein the total part of the foaming white material is 250-450 parts by weight, and the dosage of the nonionic surfactant for preparing the foaming white material is 75-125 parts by weight; the nonionic surfactant is composed of a polymeric polyol and a polysiloxane-polyether copolymer, and the mass ratio of the polymeric polyol to the polysiloxane-polyether copolymer is 0.8;
s2, uniformly mixing a foaming white material containing a nonionic surfactant with a foaming black material, and foaming and forming to obtain a polyimide foam intermediate;
and S3, demolding the foam intermediate, and placing the foam intermediate in a forced air drying box for curing to finally obtain the polyimide sound absorption foam with the spherical pit microstructure.
Further, in S1, the polyhydric alcohol is a mixture of one or more of polyethylene glycol 200, polyethylene glycol 400, polyethylene glycol 600, polyethylene glycol 800, polyethylene glycol 1000, polyethylene glycol 2000, polytetrahydrofuran ether glycol 1000, polytetrahydrofuran ether glycol 18000, polytetrahydrofuran ether glycol 2000 and polytetrahydrofuran ether glycol 3000.
Further, in S1, the polysiloxane-polyether copolymer is a mixture of one or more of AK8805, AK5000, AK10000, AK60000, L580, L560, DC193, OFX-0193, PMX200 and DC 556.
Further, in S1, the foaming white material is prepared by compounding a carboxylic ester solution dissolved by a polar solvent, the nonionic surfactant, a catalyst and water.
In S2, the foaming black material is polyisocyanate, and the mass ratio of the foaming black material to the foaming white material is 0.8.
Polyimide sound absorption foam with spherical pit microstructure is prepared according to the preparation method.
Further, the matrix resin framework and the window surface of the polyimide sound absorption foam are provided with spherical pit structures with the diameter size of 1-10 mu m, and wrinkles appear on part of pit surfaces.
Further, the polyimide sound absorption foam has a density of 8 to 25kg/m 3 (ii) a The slope of the sound absorption coefficient curve at 100-600Hz is as high as 1.3-1.5kHz -1 The normalized average sound absorption coefficient is up to 0.6-0.7; the sound absorption coefficient is kept between 0.80 and 0.85 at the frequency band of 500 to 600 Hz.
The invention has the beneficial effects that:
the invention provides polyimide sound absorption foam with spherical pit microstructures and a preparation method thereof, and the polyimide sound absorption foam is based on a water foaming technology of polyimide foam, and introduces the spherical pit inner surface microstructures on a foam wall by simply adjusting the proportion of a surfactant, so that the reflection of the inner wall of a material and the consumption of sound waves are increased, the sound absorption performance of a porous material is improved, and the aim of the invention is achieved.
Compared with the prior art, the polyimide foam matrix resin framework and the window surface prepared by the invention have spherical pit inner surface microstructures, so that more reflection paths can be provided for sound wave energy, the vibration energy dissipation and the conversion degree to heat energy are improved, the sound absorption performance of the foam material is improved, and the improvement degree of the absorption effect on sound waves in low-frequency and medium-frequency bands of 60-1000Hz is obvious.
The invention has simple operation process, does not add other fillers, designs the pore structure of the foam material, and obtains better noise reduction effect under the condition of not adding additional components.
Drawings
FIG. 1 is a scanning electron micrograph of a first product of polyimide acoustic foam having a microstructure of spherical dimple inner surfaces prepared in example 1 of the present invention.
FIG. 2 is a scanning electron micrograph of a second product of the polyimide acoustic foam having a microstructure of a spherical dimple inner surface prepared in example 1 of the present invention.
Fig. 3 is a graph showing sound absorption curves of the polyimide sound absorption foam having a microstructure of a spherical dimple inner surface prepared in embodiment 1 of the present invention and the polyimide foam prepared in comparative example 1, wherein Frequency is plotted on the abscissa and Abs. Is a sound absorption coefficient.
Detailed Description
The present invention will be described in detail with reference to specific examples, but the use and purpose of these exemplary embodiments are only to exemplify the present invention, and do not limit the actual scope of the present invention in any way, and the scope of the present invention is not limited thereto.
Example 1
In a disposable plastic cup, 40g of 45 mass percent N, N-dimethylformamide solution of 3,3',4,4' -benzophenone dimethyl tetraacetate, 3.2g of catalyst prepared from T12, dabco33 and triethanolamine according to the mass ratio of 1; weighing 60g of polyisocyanate, and adding the polyisocyanate into a disposable plastic cup to be used as a foaming black material; uniformly mixing the foaming white material and the foaming black material, and foaming and molding to obtain a polyimide foam intermediate; and (3) demolding the foam intermediate, and placing the demolded foam intermediate in a forced air drying oven at 180 ℃ for 2 hours to finally obtain the polyimide sound absorption foam with the spherical pit inner surface microstructure. Referring to fig. 1 and fig. 2, the diameter of the spherical pit structure on the resin skeleton of the foam matrix and the surface of the window is 6-8 μm, and the surface of part of the pit is wrinkled.
The polyimide sound absorption foam material prepared in the above way is tested, and the density of the polyimide sound absorption foam material is 20kg/m 3 (ii) a Referring to FIG. 3, the slope of the sound absorption coefficient curve at 100-600Hz is as high as 1.4kHz -1 The normalized average sound absorption coefficient is 0.66; absorbing at 500-600Hz frequency rangeThe acoustic coefficient is kept between 0.82 and 0.84.
Example 2
In a disposable plastic cup, 44g of 47 mass percent N, N-dimethylacetamide solution of 3,3',4,4' -diethyl biphenyltetraacetate, 3.2g of catalyst prepared from T12, dabco33 and triethanolamine according to the mass ratio of 1; weighing 60g of polyisocyanate, and adding the polyisocyanate into a disposable plastic cup to be used as a foaming black material; uniformly mixing the foaming white material and the foaming black material, and foaming and molding to obtain a polyimide foam intermediate; and (3) demolding the foam intermediate, and placing the demolded foam intermediate in a forced air drying oven at 180 ℃ for 2 hours to finally obtain the polyimide sound absorption foam with the spherical pit inner surface microstructure. The diameter of the foam matrix resin framework and the spherical pit structure on the surface of the window is 8-10 mu m, and wrinkles appear on the surface of part of pits.
The polyimide sound absorption foam material prepared in the above way is tested to obtain the polyimide sound absorption foam material with the density of 24kg/m 3 (ii) a The slope of the sound absorption coefficient curve at 100-600Hz is as high as 1.3kHz -1 The normalized average sound absorption coefficient is 0.62; the sound absorption coefficient is kept between 0.80 and 0.82 at the frequency band of 500 to 600 Hz.
Example 3
In a disposable plastic cup, 25g of N-methylpyrrolidone solution of diisopropyl pyromellitate with the mass fraction of 77%, 3.2g of a catalyst prepared from T12, dabco33 and triethanolamine according to the mass ratio of about 1; weighing 60g of polyisocyanate, and adding the polyisocyanate into a disposable plastic cup to serve as a foaming black material; uniformly mixing the foaming white material and the foaming black material, and foaming and molding to obtain a polyimide foam intermediate; and (3) demolding the foam intermediate, and placing the demolded foam intermediate in a forced air drying oven at 180 ℃ for 2 hours to finally obtain the polyimide sound absorption foam with the spherical pit inner surface microstructure. The diameter of the spherical pit structure on the resin skeleton of the foam matrix and the surface of the window is 5-7 mu m, and wrinkles appear on the surface of part of pits.
The polyimide sound absorption foam material prepared in the above way is tested, and the density of the polyimide sound absorption foam material is 15kg/m 3 (ii) a The slope of the sound absorption coefficient curve at 100-600Hz is as high as 1.4kHz -1 The normalized average sound absorption coefficient is 0.64; the sound absorption coefficient is kept between 0.8 and 0.81 at the frequency band of 500 to 600 Hz.
Comparative example 1
This comparative example differs from example 1 in that 8g of a surfactant formulated from AK8805 and PEG600 at a mass ratio of 1:1 was added. Finally, the matrix resin framework and the window surface of the polyimide sound absorption foam are smooth and have no spherical pit structure.
A polyimide foam obtained in the above comparative example was tested to give a density of 15kg/m 3 (ii) a The slope of the sound absorption curve at 100-600Hz is 0.49kHz -1 The normalized average sound absorption coefficient is 0.29; the sound absorption coefficient is kept between 0.37 and 0.43 at the frequency band of 500 to 600 Hz.
The above-listed detailed description is only a specific description of a possible embodiment of the present invention, and they are not intended to limit the scope of the present invention, and equivalent embodiments or modifications made without departing from the technical spirit of the present invention should be included in the scope of the present invention.
Claims (4)
1. A preparation method of polyimide sound absorption foam with a spherical pit microstructure is characterized by comprising the following steps:
s1, in a disposable plastic cup, uniformly mixing 40g of N, N-dimethylformamide solution of 3,3',4,4' -benzophenone dimethyl tetraacetate with the mass fraction of 45%, 3.2g of catalyst prepared from T12, dabco33 and triethanolamine according to the mass ratio of 1; weighing 60g of polyisocyanate, and adding the polyisocyanate into a disposable plastic cup to be used as a foaming black material;
s2, uniformly mixing the foaming white material and the foaming black material, and foaming and forming to obtain a polyimide foam intermediate;
and S3, demolding the foam intermediate, and placing the foam intermediate in a forced air drying oven at 180 ℃ for 2 hours to finally obtain the polyimide sound absorption foam with the spherical pit inner surface microstructure.
2. A preparation method of polyimide sound absorption foam with a spherical pit microstructure is characterized by comprising the following steps:
s1, in a disposable plastic cup, uniformly mixing 44g of 47 mass percent N, N-dimethylacetamide solution of 3,3',4,4' -diethyl biphenyltetraacetate, 3.2g of a catalyst prepared from T12, dabco33 and triethanolamine according to a mass ratio of 1; weighing 60g of polyisocyanate, and adding the polyisocyanate into a disposable plastic cup to be used as a foaming black material;
s2, uniformly mixing the foaming white material and the foaming black material, and foaming and forming to obtain a polyimide foam intermediate;
and S3, demolding the foam intermediate, and placing the foam intermediate in a forced air drying oven at 180 ℃ for 2 hours to finally obtain the polyimide sound absorption foam with the spherical pit inner surface microstructure.
3. A preparation method of polyimide sound absorption foam with a spherical pit microstructure is characterized by comprising the following steps:
s1, in a disposable plastic cup, uniformly mixing 25g of N-methylpyrrolidone solution containing 77% of diisopropyl pyromellitate, 3.2g of a catalyst prepared from T12, dabco33 and triethanolamine according to a mass ratio of 1; weighing 60g of polyisocyanate, and adding the polyisocyanate into a disposable plastic cup to be used as a foaming black material;
s2, uniformly mixing the foaming white material and the foaming black material, and foaming and forming to obtain a polyimide foam intermediate;
and S3, demolding the foam intermediate, and placing the foam intermediate in a forced air drying oven at 180 ℃ for 2 hours to finally obtain the polyimide sound absorption foam with the spherical pit inner surface microstructure.
4. A polyimide sound absorption foam with a spherical pit microstructure is characterized by being prepared according to the preparation method of any one of claims 1 to 3, wherein a matrix resin framework and a window surface of the polyimide sound absorption foam are provided with spherical pit structures with the diameter size of 1-10 microns, and wrinkles appear on partial pit surfaces, and the density of the polyimide sound absorption foam is 8-25kg/m 3 (ii) a The slope of the sound absorption coefficient curve at 100-600Hz is as high as 1.3-1.5kHz -1 The normalized average sound absorption coefficient is up to 0.6-0.7; the sound absorption coefficient is kept between 0.80 and 0.85 at the frequency band of 500 to 600 Hz.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US4081410A (en) * | 1975-01-13 | 1978-03-28 | General Electric Company | Polysiloxane surfactants useful for foaming polyurethane foams |
| EP1281727A4 (en) * | 1999-11-10 | 2004-08-04 | Kaneka Corp | Soluble polyimide and composition comprising the same, bonding sheet, adhesive laminated film for covering accelerator beam tube, and adhesive laminated film for covering conductor wire for accelerator quench heater |
| JP2007262282A (en) * | 2006-03-29 | 2007-10-11 | Toshiba Corp | Acoustic material, method for producing the same and method for regenerating acoustic material |
| CN101407594B (en) * | 2008-11-25 | 2012-03-21 | 北京市射线应用研究中心 | Modified polyimides foam and preparation thereof |
| CN103012793A (en) * | 2012-12-28 | 2013-04-03 | 青岛海洋新材料科技有限公司 | Novel mould-pressing polyimide foamed plastic and preparation method thereof |
| WO2015000067A1 (en) * | 2013-07-05 | 2015-01-08 | Proprietect L.P. | Foam composite product and process for production thereof |
| JP2016180077A (en) * | 2015-03-25 | 2016-10-13 | 宇部興産株式会社 | Method for producing polyimide foam |
| CN105175724A (en) * | 2015-11-02 | 2015-12-23 | 哈尔滨工程大学 | Preparation method of ultralow-density polyimide porous material by one-step process |
| CN107540839B (en) * | 2016-06-27 | 2021-04-23 | 上海康达化工新材料集团股份有限公司 | Light sound-absorbing heat-insulating polyimide foam material and preparation method thereof |
| CN106280451A (en) * | 2016-09-14 | 2017-01-04 | 郑州峰泰纳米材料有限公司 | The preparation method of hard polyimide foaming |
| CN109929107B (en) * | 2019-04-04 | 2021-06-01 | 哈尔滨工程大学 | Polyimide sound absorption foam material containing wedge cavity structure and preparation method thereof |
| CN110734645B (en) * | 2019-09-24 | 2022-03-22 | 哈尔滨工程大学 | Heat-insulation sound-absorption honeycomb core material and preparation method thereof |
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