CN109929107B - Polyimide sound absorption foam material containing wedge cavity structure and preparation method thereof - Google Patents
Polyimide sound absorption foam material containing wedge cavity structure and preparation method thereof Download PDFInfo
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Abstract
The invention provides a polyimide sound absorption foam material containing a wedge cavity structure and a preparation method thereof, wherein diacid diester polar solvent solution, a foam stabilizer, a compound catalyst and deionized water are quickly and uniformly mixed at room temperature, then isocyanate is added, the mixture is stirred at a high speed to form mixed foaming slurry, and then the mixed foaming slurry is poured into an open mold coated with a release agent; carrying out mould closing operation by using a mould cover with a wedge structure, carrying out foaming molding on the mixed foaming slurry in the mould after mould closing, and finishing the dense filling of the residual space in the mould to obtain a polyimide foam intermediate body with a wedge cavity structure; and placing the obtained mold containing the polyimide foam intermediate in an oven for high-temperature curing to complete the conversion of the polyimide intermediate into polyimide, and demolding to obtain the polyimide sound absorption foam material containing the wedge cavity structure. The invention realizes effective improvement of acoustic performance of the polyimide foam material.
Description
Technical Field
The invention relates to a sound absorption foam material and a preparation method thereof, in particular to a polyimide sound absorption foam material containing a wedge cavity structure and a preparation method thereof, and belongs to the technical field of polymer foam sound absorption performance improvement.
Background
The porous sound absorption material has a large number of through hole structures inside, and thus is one of the sound absorption and noise reduction materials commonly used at present. Polymer-based porous sound-absorbing materials such as melamine foam, polyurethane foam and the like have been widely used as main sound-absorbing and noise-reducing materials in the fields of architectural decoration, transportation vehicles, ships, aerospace and the like because of the advantages of light weight, low cost, excellent sound-absorbing performance and the like. However, due to the restriction of the molecular structure of the matrix resin, the heat resistance, flame retardancy and safety in use of the polymer sound-absorbing foam material are generally poor, and meanwhile, the toxicity of combustion flue gas is high, so that great potential safety hazards exist, and many serious fire accidents are caused.
Polyimide foam is one of polymer-based porous materials with the best use safety, the limited oxygen index is greater than 32%, the maximum use temperature for a long time can reach more than 300 ℃, the release amount of combustion smoke is almost zero, and the polyimide foam also has excellent chemical stability, irradiation resistance, low temperature resistance and the like. However, under the influence of the foaming and forming process, melt viscosity and rheological behavior during forming, the foam cell structure is mainly closed-cell or semi-closed-cell structure, and the open-cell mode is mainly in a crack form, so that the internal air flow resistance is large, and therefore, the sound absorption performance of the polyimide foam material is poorer than that of foam materials such as melamine, and the polyimide foam material is mainly used as a heat insulation material of special parts in the tip technical field such as aerospace, ships and the like at present.
Currently, there are few reports on the application of polyimide foam as a sound absorbing material or on the research of an acoustic performance improvement technique thereof. Most of the reported patents and literature only slightly mention the average sound absorption coefficient when describing the comprehensive properties of the materials, and do not carry out deep serial research on the acoustic properties of the polyimide foam. CN 101402743 discloses a polyimide foam and a preparation method thereof, wherein the octave average sound absorption coefficient of the prepared polyimide foam material is between 0.38 and 0.5. CN101407594 discloses a modified polyimide foam and a preparation method thereof, wherein the patent mentions that the octave average sound absorption coefficient of the prepared polyimide foam material is between 0.42 and 0.51. CN 104086995A discloses a hollow microbead-reinforced polyimide-based composite foam material and a preparation method thereof, and the average sound absorption coefficient of the prepared foam material is between 0.4 and 0.51. From the data reported in the above data, it can be further seen that the octave average sound absorption coefficient of the polyimide foam material is far from the octave average sound absorption coefficient of 0.6-0.8 of the polymer-based porous sound absorption materials such as polyurethane foam and melamine foam. In the article of research on influence of additive amount and slurry temperature on isocyanate-based polyimide foam cell structure and sound absorption performance, Wang Lei super et al realize that the polyimide foam micro cell structure is mainly the adjustment of the opening and closing porosity to a certain extent by adjusting the amount of a surfactant in a formula, and prepare polyimide foam materials with different micro cell structures so as to hopefully improve the acoustic performance of the polyimide foam materials. However, the method for simply adjusting the proportion of the auxiliary agents such as the surfactant and the like only realizes the slight change of the cellular structure, physical parameters such as a hole opening mode, flow resistance and the like which have a large relation with the acoustic performance of the foam material are not effectively regulated, the acoustic performance of the material is not greatly improved, and the octave average sound absorption coefficient is generally between 0.5 and 0.55.
Disclosure of Invention
The invention aims to provide a polyimide sound absorption foam material containing a wedge cavity structure and a preparation method thereof, aiming at improving the sound absorption performance of the polyimide foam material.
The purpose of the invention is realized as follows:
a polyimide sound absorption foam material containing a wedge cavity structure is prepared by the following method:
the method comprises the following steps: quickly and uniformly mixing diacid diester polar solvent solution with a foam stabilizer, a compound catalyst and deionized water at room temperature, adding isocyanate, stirring at a high speed to form mixed foaming slurry, and pouring the mixed foaming slurry into an open mold coated with a release agent;
step two: carrying out mould closing operation by using a mould cover with a wedge structure, carrying out foaming molding on the mixed foaming slurry in the mould after mould closing, and finishing the dense filling of the residual space in the mould to obtain a polyimide foam intermediate body with a wedge cavity structure;
step three: and (4) placing the mold containing the polyimide foam intermediate obtained in the step two in an oven for high-temperature curing to complete the conversion of the polyimide intermediate into polyimide, and demolding to obtain the polyimide sound absorption foam material containing the wedge cavity structure.
The invention also includes such features:
1. 150-300 parts of diacid diester polar solvent solution, 200-350 parts of isocyanate, 10-50 parts of foam stabilizer, 10-20 parts of compound catalyst and 15-30 parts of deionized water; the release agent comprises the following components in parts by weight: 5-50 parts; the solid content of the diacid diester polar solvent solution is as follows: 30-75 wt%;
2. the wedge structure material that the mould lid was taken is metal and the parameter is: the ratio of the height of the cone to the height of the inner cavity of the die is 1: 7-9: 10, the ratio of the height to the diameter of the cone is 0.5-3, and the number of wedges in a circular surface with the diameter of 10cm is 5-10;
3. the diacid diester comprises: dimethyl pyromellitate, dimethyl 3,3',4,4' -benzophenone tetraacetate, diethyl 3,3',4,4' -biphenyl tetraacetate, dimethyl 3,3',4,4' -diphenyl ether tetraacetate and the like are prepared by the reaction of dibasic acid anhydride and micromolecular monoalcohol according to the molar ratio of 1: 1.9-1: 2.1; the foam stabilizer comprises one or more of foam stabilizers or surfactants such as non-hydrolytic water-soluble polyether siloxane, nonionic fluorocarbon surfactant, polyoxyethylene nonionic surfactant and the like; the compound catalyst is composed of one or more of triethanolamine, triethylene diamine, dibutyltin dilaurate, stannous octoate, Dabco-33 and other catalysts; the release agent comprises: fatty acids, paraffin, vaseline, silicone oil or low molecular weight polyethylene;
4. the temperature of the mixed foaming slurry is kept at-10-30 ℃, and the high-temperature curing temperature is 150-210 ℃.
A preparation method of polyimide sound absorption foam material containing wedge cavity structure comprises the following steps:
the method comprises the following steps: quickly and uniformly mixing diacid diester polar solvent solution with a foam stabilizer, a compound catalyst and deionized water at room temperature, adding isocyanate, stirring at a high speed to form mixed foaming slurry, and pouring the mixed foaming slurry into an open mold coated with a release agent;
step two: carrying out mould closing operation by using a mould cover with a wedge structure, carrying out foaming molding on the mixed foaming slurry in the mould after mould closing, and finishing the dense filling of the residual space in the mould to obtain a polyimide foam intermediate body with a wedge cavity structure;
step three: and (4) placing the mold containing the polyimide foam intermediate obtained in the step two in an oven for high-temperature curing to complete the conversion of the polyimide intermediate into polyimide, and demolding to obtain the polyimide sound absorption foam material containing the wedge cavity structure.
150-300 parts of diacid diester polar solvent solution, 200-350 parts of isocyanate, 10-50 parts of foam stabilizer, 10-20 parts of compound catalyst and 15-30 parts of deionized water; the release agent comprises the following components in parts by weight: 5-50 parts; the solid content of the diacid diester polar solvent solution is as follows: 30-75 wt%;
the wedge structure material that the mould lid was taken is metal and the parameter is: the ratio of the height of the cone to the height of the inner cavity of the die is 1: 7-9: 10, the ratio of the height to the diameter of the cone is 0.5-3, and the number of wedges in a circular surface with the diameter of 10cm is 5-10;
the diacid diester comprises: dimethyl pyromellitate, dimethyl 3,3',4,4' -benzophenone tetraacetate, diethyl 3,3',4,4' -biphenyl tetraacetate, dimethyl 3,3',4,4' -diphenyl ether tetraacetate and the like are prepared by the reaction of dibasic acid anhydride and micromolecular monoalcohol according to the molar ratio of 1: 1.9-1: 2.1; the foam stabilizer comprises one or more of foam stabilizers or surfactants such as non-hydrolytic water-soluble polyether siloxane, nonionic fluorocarbon surfactant, polyoxyethylene nonionic surfactant and the like; the compound catalyst is composed of one or more of triethanolamine, triethylene diamine, dibutyltin dilaurate, stannous octoate, Dabco-33 and other catalysts; the release agent comprises: fatty acids, paraffin, vaseline, silicone oil or low molecular weight polyethylene;
the temperature of the mixed foaming slurry is kept at-10-30 ℃, and the high-temperature curing temperature is 150-210 ℃.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a method for preparing a polyimide foam material with excellent sound absorption performance by introducing a wedge cavity structure and simultaneously greatly regulating and controlling a foam hole structure so as to improve the acoustic performance of the polyimide foam material. According to the invention, based on the water foaming technology and the mold closing forming control technology of the polyimide foam, the introduction of the wedge-shaped cavity sound absorption structure and even the back cavity sound absorption structure is completed in a free foaming forming filling mode, and the incidence of sound waves and the gradual dissipation degree of the sound waves in the cavity structure are effectively increased. Meanwhile, the foam can be limited in growth and expansion by a closed die foaming mode, and the independent adjustment of the material density and the large-scale adjustment and control of the cell size and the cell structure are realized. Finally, the double-frequency average sound absorption coefficient of the polyimide foam material is improved to be more than 0.6 by means of the dual functions of introduction of the wedge cavity sound absorption structure and automatic regulation and control of the microscopic cell structure, the sound absorption performance of the polyimide foam material is effectively improved, and the purpose of the invention is achieved.
Compared with the prior art, the wedge cavity structure and the polyimide foam are combined in a specific mould casting and mould closing forming mode, the independent adjustment of the cell structure and the material density is realized, and the polyimide sound absorption foam material with the wedge cavity structure and the adjustable and controllable cell structure is prepared. The original molecular structure of the matrix resin is maintained, the large-scale regulation and control of the cell structure and the introduction of an effective acoustic structure are realized simultaneously, and the effective improvement of the acoustic performance of the polyimide foam material is realized through a simple technology. Compared with the existing polyimide foam material, the sound absorption coefficient of the high-efficiency sound absorption type polyimide foam material prepared by the invention, especially the sound absorption coefficient in a low-frequency range, is remarkably improved, and the sound absorption coefficient in a high-frequency range is effectively maintained, so that the integral octave average sound absorption coefficient of the material is effectively improved. The polyimide sound absorption foam material with the wedge-shaped cavity structure and the adjustable and controllable foam cell structure has the advantages of simple preparation process, simple and easy introduction of the cavity structure into the process flow, simple and feasible adjustment and control technology of the foam cell structure, excellent sound absorption performance of the material, and contribution to further widening the wide application of the polyimide foam material as the sound absorption material in the fields of aerospace, ships, rail transit, buildings and the like.
Drawings
FIG. 1 is a digital photo of polyimide acoustic foam with adjustable and controllable cell structure and wedge-shaped cavity structure prepared by the embodiment of the present invention;
FIG. 2 is a scanning electron micrograph of polyimide acoustic foam with a controllable cell structure and a wedge-shaped cavity structure prepared according to an embodiment of the present invention;
FIG. 3 is a sound absorption coefficient curve diagram of the polyimide sound absorption foam material with the adjustable and controllable cellular structure and the wedge-shaped cavity structure, which is prepared by the embodiment of the invention, at 0-6300 Hz.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
The invention aims to provide a method for effectively improving the sound absorption performance of a polyimide foam material by introducing a wedge cavity or a cavity structure through specific mould casting molding, limiting the growth and expansion of a foam body by a closed mould, realizing the autonomous adjustment of material density and the large-scale regulation and control of the size and the structure of a foam hole, and finally realizing the effective improvement of the sound absorption performance of the polyimide foam material through the combined action of the two, thereby providing a new thought for the improvement of the sound absorption performance of the polyimide foam material. The polyimide sound absorption foam material containing the wedge cavity structure and the preparation method thereof are as follows: (1) quickly and uniformly mixing a polar solvent solution of diester diacid with a foam stabilizer, a compound catalyst and deionized water at room temperature, then adding isocyanate, stirring at a high speed to form mixed foaming slurry, then quickly pouring the mixed slurry into an open mold coated with a release agent, and simultaneously ensuring that the slurry is uniformly distributed at the bottom of the mold in a scraper leveling mode; (2) rapidly closing the mold by using a prefabricated mold cover with a wedge structure, foaming and molding the foaming slurry in the mold after the mold is closed, and compactly filling the residual space in the mold to obtain a polyimide foam intermediate body with a wedge cavity structure; (3) and (3) placing the mold containing the polyimide foam intermediate obtained in the step (2) in an oven for high-temperature curing to complete the conversion of the polyimide intermediate into polyimide, and obtaining the polyimide sound absorption foam material with the adjustable and controllable cellular structure and the wedge cavity structure through post-treatment processes such as cutting after demolding and the like. The mixed foaming slurry comprises the following components in parts by weight: 150-300 parts of diacid diester polar solvent solution, 200-350 parts of isocyanate, 10-50 parts of foam stabilizer, 10-20 parts of compound catalyst and 15-30 parts of deionized water; the release agent comprises the following components in parts by weight: 5-50 parts; the solid content of the diacid diester polar solvent solution is as follows: 30 to 75 wt%. The diacid diester comprises: dimethyl pyromellitate, dimethyl 3,3',4,4' -benzophenone tetraacetate, diethyl 3,3',4,4' -biphenyl tetraacetate, dimethyl 3,3',4,4' -diphenyl ether tetraacetate and the like are prepared by the reaction of dibasic acid anhydride and micromolecular monoalcohol according to the molar ratio of 1: 1.9-1: 2.1. The polar solvent described above includes: aprotic highly polar solvents such as N-methylpyrrolidone, N-dimethylformamide, N-dimethylacetamide, and dimethylsulfoxide. The foam stabilizer comprises one or more of foam stabilizers or surfactants such as non-hydrolytic water-soluble polyether siloxane, nonionic fluorocarbon surfactant, polyoxyethylene nonionic surfactant and the like. The compound catalyst is composed of one or more of triethanolamine, triethylene diamine, dibutyltin dilaurate, stannous octoate, Dabco-33 and the like. The isocyanate comprises: polyfunctional isocyanates such as polymethylenepolyphenyl polyisocyanate (PAPI), diphenylmethane diisocyanate (MDI), Toluene Diisocyanate (TDI), and Hexamethylene Diisocyanate (HDI). The release agent comprises: fatty acids, paraffin, petrolatum, silicone oil, low molecular weight polyethylene, and the like. The wedge structure carried by the mould cover is mainly a metal wedge structure; the general parameters of the wedge structure are as follows: the ratio of the height of the cone to the height of the inner cavity of the mold is 1: 7-9: 10, the ratio of the height to the diameter of the cone is 0.5-3, and the number of wedges in a circular surface with the diameter of 10cm is 5-10. The temperature of the mixed slurry is controlled to be-10-30 ℃, and the required environment temperature is-15-35 ℃. The high-temperature curing temperature is 150-210 DEG C
Examples 1
31g of N, N-dimethylformamide solution of dimethyl 3,3',4,4' -benzophenonetetracarboxylate with a solid content of about 45%, 2.4g of a complex catalyst prepared from T12, Dabco33 and triethanolamine in a mass ratio of about 1:2:5, 7.4g of a foam stabilizer prepared from AK8805 and PEG600 in a mass ratio of 1:1 and 3.6g of deionized water were sequentially added into a disposable plastic cup at 20 ℃, and after stirring and mixing uniformly with a glass rod, 44.4g of polymethylene polyphenyl polyisocyanate (PAPI) with a temperature of 20 ℃ was continuously added. Stirring the mixture at high speed for 30s by a stirring paddle at the temperature to be uniformly mixed to form mixed foaming slurry. Pouring the slurry into an open mold coated with silicone oil within 10s, wherein the height of the inner cavity of the mold is 6cm, and simultaneously, the slurry is ensured to be uniformly distributed at the bottom of the mold in a scraper leveling mode. Then, a mold cover coated with silicone oil and provided with a steel wedge structure with a cone height of 5cm, a cone height-diameter ratio of 3 and a wedge number of 7 in a circular surface with a diameter of 10cm is used for rapidly closing the mold. And after the mold is closed, foaming and molding the foaming slurry in the mold to complete the dense filling of the residual space in the mold, so as to obtain the polyimide foam intermediate containing the wedge cavity structure. And finally, placing the obtained mold containing the polyimide foam intermediate in a drying oven at 180 ℃ for high-temperature curing, demolding, and then performing post-treatment processes such as cutting to obtain the polyimide sound absorption foam material with the wedge cavity structure and the adjustable and controllable cellular structure.
The prepared polyimide sound absorption foam material with the adjustable and controllable cellular structure and the wedge-shaped cavity structure is tested to obtain the polyimide sound absorption foam material with the density of 78kg/m3The average cell size is 0.15mm, and the standing wave tube test result shows that the octave average sound absorption coefficient is 0.63.
EXAMPLES example 2
41.5g of N, N-dimethylformamide solution of dimethyl 3,3',4,4' -benzophenonetetracarboxylate with a solid content of about 45%, 3.2g of a complex catalyst prepared from T12, Dabco33 and triethanolamine in a mass ratio of about 1:2:5, 9.0g of a foam stabilizer prepared from AK8805 and PEG600 in a mass ratio of 1:1 and 4.8g of deionized water are sequentially added into a disposable plastic cup at 20 ℃, and after the mixture is uniformly stirred by a glass rod, 59.2g of polymethylene polyphenyl polyisocyanate (PAPI) with a temperature of 20 ℃ is continuously added. Stirring the mixture at high speed for 30s by a stirring paddle at the temperature to be uniformly mixed to form mixed foaming slurry. Pouring the slurry into an open mold coated with silicone oil within 10s, wherein the height of the inner cavity of the mold is 6cm, and simultaneously, the slurry is ensured to be uniformly distributed at the bottom of the mold in a scraper leveling mode. Then, a mold cover coated with silicone oil and provided with a steel wedge structure with a cone height of 5cm, a cone height-diameter ratio of 3 and a wedge number of 7 in a circular surface with a diameter of 10cm is used for rapidly closing the mold. And after the mold is closed, foaming and molding the foaming slurry in the mold to complete the dense filling of the residual space in the mold, so as to obtain the polyimide foam intermediate containing the wedge cavity structure. And finally, placing the obtained mold containing the polyimide foam intermediate in a drying oven at 180 ℃ for high-temperature curing, demolding, and then performing post-treatment processes such as cutting to obtain the polyimide sound absorption foam material with the wedge cavity structure and the adjustable and controllable cellular structure.
The prepared polyimide sound absorption foam material with the adjustable and controllable cellular structure and the wedge-shaped cavity structure is tested to obtain the polyimide sound absorption foam material with the density of 103kg/m3And the average cell size is 0.12mm, and the standing wave tube test result shows that the octave average sound absorption coefficient is 0.62.
EXAMPLE 3
51.8g of N, N-dimethylformamide solution of 3,3',4,4' -benzophenone dimethyl tetraacetate with a solid content of about 45%, 4.0g of compound catalyst prepared from T12, Dabco33 and triethanolamine according to a mass ratio of about 1:2:5, 12.3g of foam stabilizer prepared from AK8805 and PEG600 according to a mass ratio of 1:1 and 5.6g of deionized water are sequentially added into a disposable plastic cup at the temperature of 20 ℃, and after the mixture is stirred and mixed uniformly by a glass rod, 74.0g of polymethylene polyphenyl polyisocyanate (PAPI) with the temperature of 20 ℃ is continuously added. Stirring the mixture at high speed for 30s by a stirring paddle at the temperature to be uniformly mixed to form mixed foaming slurry. Pouring the slurry into an open mold coated with silicone oil within 10s, wherein the height of the inner cavity of the mold is 6cm, and simultaneously, the slurry is ensured to be uniformly distributed at the bottom of the mold in a scraper leveling mode. Then, a mold cover coated with silicone oil and provided with a steel wedge structure with a cone height of 5cm, a cone height-diameter ratio of 3 and a wedge number of 7 in a circular surface with a diameter of 10cm is used for rapidly closing the mold. And after the mold is closed, foaming and molding the foaming slurry in the mold to complete the dense filling of the residual space in the mold, so as to obtain the polyimide foam intermediate containing the wedge cavity structure. And finally, placing the obtained mold containing the polyimide foam intermediate in a drying oven at 180 ℃ for high-temperature curing, demolding, and then performing post-treatment processes such as cutting to obtain the polyimide sound absorption foam material with the wedge cavity structure and the adjustable and controllable cellular structure.
The prepared polyimide sound absorption foam material with the adjustable and controllable cellular structure and the wedge-shaped hollow structure is tested to obtain the polyimide sound absorption foam material with the density of 129kg/m3The average cell size is 0.08mm, and the standing wave tube test result shows that the octave average sound absorption coefficient is 0.63.
In summary, the following steps:
the invention provides a method for preparing polyimide sound absorption foam material by introducing a sound absorption wedge cavity structure. (1) Preparing polyimide foam foaming slurry at room temperature, quickly pouring the polyimide foam foaming slurry into an open mold coated with a release agent, and ensuring that the slurry is uniformly distributed at the bottom of the mold in a scraper leveling mode; (2) rapidly closing the mold by using a prefabricated mold cover with a wedge structure, foaming and molding the foaming slurry in the mold after the mold is closed, and compactly filling the residual space in the mold to obtain a polyimide foam intermediate body with a wedge cavity structure; (3) and (3) placing the mould in a high-temperature oven to complete the conversion of the polyimide intermediate into polyimide, and obtaining the high-efficiency sound absorption type polyimide foam material containing the wedge cavity structure through post-treatment processes such as cutting after demoulding. The wedge cavity sound absorption structure and even the back cavity sound absorption structure are introduced in a free foaming forming filling mode based on a water foaming technology and a closed die forming control technology of polyimide foam, and the preparation process is simple, convenient and easy to implement. Meanwhile, the foam can be limited in growth and expansion by a closed die in a foaming mode, the density of the material can be automatically adjusted, and the large-scale regulation and control of the size and the structure of the foam holes are realized. Finally, the sound absorption performance of the polyimide foam material is effectively improved by means of dual functions of wedge cavity sound absorption structure introduction and automatic control of a micro-cellular structure, and the purpose of the invention is achieved.
Claims (6)
1. A polyimide sound absorption foam material containing a wedge cavity structure is characterized by being prepared by the following method:
the method comprises the following steps: quickly and uniformly mixing diacid diester polar solvent solution with a foam stabilizer, a compound catalyst and deionized water at room temperature, adding isocyanate, stirring at a high speed to form mixed foaming slurry, and pouring the mixed foaming slurry into an open mold coated with a release agent; the mixed foaming slurry comprises the following components in parts by weight: 150-300 parts of diacid diester polar solvent solution, 200-350 parts of isocyanate, 10-50 parts of foam stabilizer, 10-20 parts of compound catalyst and 15-30 parts of deionized water; the release agent comprises the following components in parts by weight: 5-50 parts; the solid content of the diacid diester polar solvent solution is as follows: 30-75 wt%;
step two: carrying out mould closing operation by using a mould cover with a wedge structure, carrying out foaming molding on the mixed foaming slurry in the mould after mould closing, and finishing the dense filling of the residual space in the mould to obtain a polyimide foam intermediate body with a wedge cavity structure; the wedge structure material that the mould lid was taken is metal and the parameter is: the ratio of the height of the cone to the height of the inner cavity of the die is 1: 7-9: 10, the ratio of the height to the diameter of the cone is 0.5-3, and the number of wedges in a circular surface with the diameter of 10cm is 5-10;
step three: placing the mold containing the polyimide foam intermediate obtained in the step two in an oven for high-temperature curing to complete the conversion of the polyimide intermediate into polyimide, and obtaining the polyimide sound absorption foam material containing the wedge cavity structure after demolding; the frequency octave average sound absorption coefficient of the polyimide sound absorption foam material is more than 0.6.
2. The wedge void structure containing polyimide acoustic foam material as set forth in claim 1, wherein said diacid diester comprises: dimethyl pyromellitate, dimethyl 3,3',4,4' -benzophenone tetraacetate, diethyl 3,3',4,4' -biphenyl tetraacetate or dimethyl 3,3',4,4' -diphenyl ether tetraacetate are prepared by the reaction of dibasic acid anhydride and micromolecular monoalcohol according to the molar ratio of 1: 1.9-1: 2.1; the foam stabilizer consists of one or more of non-hydrolytic water-soluble polyether siloxane, a nonionic fluorocarbon surfactant and a polyoxyethylene nonionic surfactant; the compound catalyst consists of a plurality of catalysts of triethanolamine, triethylene diamine, dibutyltin dilaurate, stannous octoate and Dabco-33; the release agent comprises: fatty acids, paraffin, vaseline, silicone oil or low molecular weight polyethylene.
3. The polyimide sound absorption foam material containing the wedge cavity structure as claimed in claim 1, wherein the temperature of the mixed foaming slurry is maintained at-10 to 30 ℃, and the high-temperature curing temperature is 150 to 210 ℃.
4. A preparation method of polyimide sound absorption foam material containing wedge cavity structure is characterized by comprising the following steps:
the method comprises the following steps: quickly and uniformly mixing diacid diester polar solvent solution with a foam stabilizer, a compound catalyst and deionized water at room temperature, adding isocyanate, stirring at a high speed to form mixed foaming slurry, and pouring the mixed foaming slurry into an open mold coated with a release agent; the mixed foaming slurry comprises the following components in parts by weight: 150-300 parts of diacid diester polar solvent solution, 200-350 parts of isocyanate, 10-50 parts of foam stabilizer, 10-20 parts of compound catalyst and 15-30 parts of deionized water; the release agent comprises the following components in parts by weight: 5-50 parts; the solid content of the diacid diester polar solvent solution is as follows: 30-75 wt%;
step two: carrying out mould closing operation by using a mould cover with a wedge structure, carrying out foaming molding on the mixed foaming slurry in the mould after mould closing, and finishing the dense filling of the residual space in the mould to obtain a polyimide foam intermediate body with a wedge cavity structure; the wedge structure material that the mould lid was taken is metal and the parameter is: the ratio of the height of the cone to the height of the inner cavity of the die is 1: 7-9: 10, the ratio of the height to the diameter of the cone is 0.5-3, and the number of wedges in a circular surface with the diameter of 10cm is 5-10;
step three: and (4) placing the mold containing the polyimide foam intermediate obtained in the step two in an oven for high-temperature curing to complete the conversion of the polyimide intermediate into polyimide, and demolding to obtain the polyimide sound absorption foam material containing the wedge cavity structure.
5. The method for preparing polyimide acoustic foam material containing wedge cavity structure according to claim 4, wherein the diacid diester comprises: dimethyl pyromellitate, dimethyl 3,3',4,4' -benzophenone tetraacetate, diethyl 3,3',4,4' -biphenyl tetraacetate or dimethyl 3,3',4,4' -diphenyl ether tetraacetate are prepared by the reaction of dibasic acid anhydride and micromolecular monoalcohol according to the molar ratio of 1: 1.9-1: 2.1; the foam stabilizer consists of one or more of non-hydrolytic water-soluble polyether siloxane, a nonionic fluorocarbon surfactant and a polyoxyethylene nonionic surfactant; the compound catalyst consists of a plurality of catalysts of triethanolamine, triethylene diamine, dibutyltin dilaurate, stannous octoate and Dabco-33; the release agent comprises: fatty acids, paraffin, vaseline, silicone oil or low molecular weight polyethylene.
6. The method for preparing polyimide sound absorption foam material containing wedge cavity structure as claimed in claim 4, wherein the temperature of the mixed foaming slurry is kept between-10 ℃ and 30 ℃, and the high temperature curing temperature is 150 ℃ to 210 ℃.
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| 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 |
| CN111087618B (en) * | 2019-12-30 | 2022-10-14 | 江苏中科聚合新材料产业技术研究院有限公司 | Sound absorption and noise reduction type polyimide foam, sound absorption and noise reduction type high-speed train cold-proof material and application |
| CN111619183B (en) * | 2020-05-20 | 2021-11-19 | 哈尔滨工程大学 | Composite polyimide foam with synergistic sound absorption effect and preparation method thereof |
| CN111635551B (en) * | 2020-06-23 | 2022-04-22 | 哈尔滨工程大学 | Method for preparing polyimide open-cell foam by one-step method and product |
| CN112126110B (en) * | 2020-08-31 | 2022-11-08 | 哈尔滨工程大学 | Polyimide sound absorption foam with spherical pit microstructure and preparation method thereof |
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