CN115353698B - Polyvinylidene fluoride composite foam sound absorption material and preparation method and application thereof - Google Patents
Polyvinylidene fluoride composite foam sound absorption material and preparation method and application thereof Download PDFInfo
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- CN115353698B CN115353698B CN202210945823.6A CN202210945823A CN115353698B CN 115353698 B CN115353698 B CN 115353698B CN 202210945823 A CN202210945823 A CN 202210945823A CN 115353698 B CN115353698 B CN 115353698B
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- 239000002033 PVDF binder Substances 0.000 title claims abstract description 134
- 229920002981 polyvinylidene fluoride Polymers 0.000 title claims abstract description 134
- 239000006260 foam Substances 0.000 title claims abstract description 90
- 239000002131 composite material Substances 0.000 title claims abstract description 82
- 238000010521 absorption reaction Methods 0.000 title claims abstract description 73
- 239000000463 material Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 30
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 20
- 235000021552 granulated sugar Nutrition 0.000 claims abstract description 20
- 239000006185 dispersion Substances 0.000 claims abstract description 18
- 239000011358 absorbing material Substances 0.000 claims abstract description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 14
- 239000011148 porous material Substances 0.000 claims abstract description 13
- 239000002657 fibrous material Substances 0.000 claims abstract description 11
- 239000003365 glass fiber Substances 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract description 9
- 229920001046 Nanocellulose Polymers 0.000 claims abstract description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 54
- 238000003756 stirring Methods 0.000 claims description 46
- 239000011259 mixed solution Substances 0.000 claims description 41
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 34
- 239000000243 solution Substances 0.000 claims description 32
- 230000001112 coagulating effect Effects 0.000 claims description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 239000000843 powder Substances 0.000 claims description 25
- 239000003960 organic solvent Substances 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 14
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 11
- 229920007859 Kynar® HSV 900 Polymers 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 229920007485 Kynar® 761 Polymers 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000009210 therapy by ultrasound Methods 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 239000000945 filler Substances 0.000 abstract description 6
- 239000002245 particle Substances 0.000 abstract description 6
- 238000002386 leaching Methods 0.000 abstract description 5
- 238000005191 phase separation Methods 0.000 abstract description 4
- 239000011159 matrix material Substances 0.000 abstract description 3
- 239000011157 advanced composite material Substances 0.000 abstract description 2
- 230000008569 process Effects 0.000 description 14
- 238000010586 diagram Methods 0.000 description 13
- 238000005187 foaming Methods 0.000 description 7
- 230000008901 benefit Effects 0.000 description 5
- 239000002134 carbon nanofiber Substances 0.000 description 5
- 210000004027 cell Anatomy 0.000 description 5
- 238000001000 micrograph Methods 0.000 description 4
- 238000004364 calculation method Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000012814 acoustic material Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000004566 building material Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 210000000497 foam cell Anatomy 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 229920005830 Polyurethane Foam Polymers 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000004378 air conditioning Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000006261 foam material Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920006327 polystyrene foam Polymers 0.000 description 1
- 239000011496 polyurethane foam Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- 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
- C08J9/26—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a solid phase from a macromolecular composition or article, e.g. leaching out
-
- 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
- C08J9/0066—Use of inorganic compounding ingredients
- C08J9/0071—Nanosized fillers, i.e. having at least one dimension below 100 nanometers
-
- 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
- C08J9/0085—Use of fibrous compounding ingredients
-
- 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
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/042—Elimination of an organic solid phase
- C08J2201/0422—Elimination of an organic solid phase containing oxygen atoms, e.g. saccharose
-
- 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
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2327/16—Homopolymers or copolymers of vinylidene fluoride
-
- 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
- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/02—Cellulose; Modified cellulose
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/041—Carbon nanotubes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
Abstract
The invention belongs to the field of advanced composite materials, and discloses a polyvinylidene fluoride composite foam sound absorption material, a preparation method and application thereof. The preparation method of the polyvinylidene fluoride composite foam sound absorbing material comprises the following steps: PVDF is used as a matrix, fiber materials (carbon nano tubes, nanocellulose and glass fibers) are used as fillers, commercial white granulated sugar is used as a leached particle template, and a non-solvent induced phase separation (NIPS) method and a particle leaching method are combined to prepare the polyvinylidene fluoride composite foam sound absorbing material which is light and thin in thickness, uniform in pore size, uniform in filler dispersion, mutually communicated in pores and provided with holes in foam pore walls. The sound absorption material prepared by the invention has sound absorption coefficient alpha more than 0.2 in the frequency range of 1000-6400Hz and more than 0.5 in the frequency range of 1800-6400Hz, has excellent overall sound absorption performance and has good application prospect in the field of broadband sound absorption materials.
Description
Technical Field
The invention belongs to the field of advanced composite materials, and particularly relates to a polyvinylidene fluoride composite foam sound absorption material, a preparation method and application thereof.
Background
In recent years, with the deep integration of information technology and manufacturing industry, more and more intelligent devices enter the life of people, and the intelligent mechanical devices bring convenience to the life of people and generate more kinds of noise, such as air conditioning noise, automobile driving noise, sweeping robot noise and the like; moreover, along with the continuous improvement of the life quality of people, the demands for culture and art are also continuously increasing, and more people can choose to go to libraries, theatres, concert halls and the like when leisure. In these scenarios, in order to enhance the acoustic experience of people, improve the acoustic environment, people have placed higher demands on the sound absorption properties of acoustic materials. The sound absorbing material refers to a material that performs noise blocking during sound propagation, and is intended to absorb sound, reduce reflection of sound inside a space, and propagate outside the space. Therefore, the sound absorbing material is generally used in space interior to control the reverberation of sound, eliminate echo and absorb noise.
Currently, many porous sound absorbing materials are emerging on the market for urban living noise. The sound absorption mechanism of the porous sound absorption material is that sound energy is converted into heat energy to be dissipated through viscosity, thermal effect and material damping. More common porous sound absorbing materials are polyurethane foam, melamine foam, polystyrene foam, polypropylene foam, and the like. These foams are inexpensive and easy to process, but suffer from drawbacks in terms of broadband sound absorption, and generally only an increase in the thickness of the material is an option in order to achieve the desired sound absorption; moreover, the existing porous sound absorption material has certain defects in ageing resistance and flame retardant property, and has certain potential safety hazards as a building material.
Polyvinylidene fluoride (PVDF) is a fluororesin with good wear resistance, weather resistance and corrosion resistance, and simultaneously, PVDF also has excellent flame retardance, thereby meeting the requirements of being used as a building material. Furthermore, because the PVDF matrix has unique piezoelectricity, the acoustic-electric conversion can be realized on the basis of the traditional acoustic-thermal conversion, and the acoustic energy is converted into electric energy; the interconnected cells in the foam enable sound waves to be reflected in the material for multiple times, so that the sound energy is converted into heat energy; the fiber filler increases the bending degree of the foam material, which is beneficial to the improvement of the sound absorption performance of the low frequency band; small holes in the walls of the foam cells also provide an advantage for the dissipation of acoustic energy. Therefore, polyvinylidene fluoride composite foam applied to the field of acoustic materials is worthy of exploration. However, no patent publication of polyvinylidene fluoride composite foam sound absorbing materials and preparation methods related to the same exists at present.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the primary purpose of the invention is to provide a preparation method of a polyvinylidene fluoride composite foam sound absorbing material.
The invention also aims to provide the polyvinylidene fluoride composite foam sound-absorbing material prepared by the preparation method; the polyvinylidene fluoride composite foam sound absorption material is light and thin in thickness, uniform in pore size, uniform in filler dispersion, mutually communicated in pores and provided with holes in foam pore walls, and the preparation method of the polyvinylidene fluoride composite foam sound absorption material can realize good broadband sound absorption under the thickness of 10mm, so that the sound absorption requirement of people on a complex acoustic environment is met.
It is still another object of the present invention to provide an application of the above polyvinylidene fluoride composite foam sound absorbing material.
The aim of the invention is achieved by the following technical scheme:
the preparation method of the polyvinylidene fluoride composite foam sound absorption material comprises the following operation steps:
(1) Dissolving polyvinylidene fluoride powder serving as a raw material in an organic solvent, and fully stirring at 50-80 ℃ for 0.5-2h to obtain a polyvinylidene fluoride solution;
(2) Dispersing a fiber material in an organic solvent, carrying out ultrasonic treatment for 0.5-2h to obtain a fiber material solution with uniform dispersion, adding the fiber material solution into the polyvinylidene fluoride solution obtained in the step (1), and fully stirring at 50-80 ℃ for 0.5-2h to obtain a mixed solution;
(3) Adding white granulated sugar into the mixed solution obtained in the step (2), and fully stirring for 0.5-2h at the temperature of 50-80 ℃ to obtain a mixed system;
(4) Stopping stirring, adding a coagulating bath into the mixed system obtained in the step (3), repeatedly replacing the coagulating bath, washing with water, and drying to obtain polyvinylidene fluoride composite foam;
(5) And (3) cutting off the upper and lower compact skin layers of the polyvinylidene fluoride composite foam obtained in the step (4) to obtain the polyvinylidene fluoride composite foam sound absorption material.
The polyvinylidene fluoride powder in the step (1) is one or two of polyvinylidene fluoride powder with MW=600000 and KYNAR761 and polyvinylidene fluoride powder with MW=800000 and KYNAR HSV 900.
The organic solvents in the step (1) and the step (2) are one or two of N, N-Dimethylformamide (DMF), N-dimethylacetamide (DMAc) and acetone.
The mass ratio of the polyvinylidene fluoride powder in the step (1) to the fiber material in the step (2) is 50:1-300:1; the mass ratio of the polyvinylidene fluoride powder in the step (1) to the white granulated sugar in the step (3) is 1:11-1:5.
The fiber material in the step (2) is one or more of Carbon Nanotubes (CNTs), nanocellulose (CNFs) and glass fibers.
The white granulated sugar in the step (3) is commercial white granulated sugar.
The coagulating bath in the step (4) is one or more of water, an alcohol solvent, N-Dimethylformamide (DMF) and N, N-dimethylacetamide (DMAc).
The thickness of the polyvinylidene fluoride composite foam sound absorption material in the step (5) is 10mm.
The stirring rates in steps (1) to (3) were 500rpm.
The polyvinylidene fluoride composite foam sound absorption material prepared by the method has the thickness of 10mm, the sound absorption coefficient alpha is larger than 0.2 in the frequency range of 1000-6400Hz, and the sound absorption coefficient alpha is larger than 0.5 in the frequency range of 1800-6400 Hz.
The polyvinylidene fluoride composite foam sound absorbing material prepared by the method can effectively absorb building noise, audio noise and traffic noise in modern life, control the transmission of the noise and reduce the trouble brought by the noise to life and health of people. In addition, the research of the broadband sound absorbing material has important application value in the military field. Such as how to cancel sound from a submarine engine, thereby avoiding detection by enemy sonar.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) The preparation method provided by the invention has the advantages of simple conditions and novel method, and can be used for foaming the polyvinylidene fluoride composite material at the temperature of below 80 ℃, so that the technical blank of foaming by combining a non-solvent induced phase separation method with a particle leaching method is filled.
(2) The invention provides a precise and controllable foaming method for a cell structure, and the prepared polyvinylidene fluoride composite foam has the advantages of uniform pore size, uniform filler dispersion, interconnected cells and holes on the wall of the foam.
(3) The polyvinylidene fluoride composite foam sound absorption material prepared by the invention has the performance of broadband sound absorption, when the thickness is only 10mm, the sound absorption coefficient alpha is larger than 0.2 in the frequency range of 1000-6400Hz, and the sound absorption coefficient alpha is larger than 0.5 in the frequency range of 1800-6400Hz, and the excellent sound absorption performance can meet the sound absorption requirements of different acoustic environments.
Drawings
FIG. 1 is a diagram of a process for preparing a polyvinylidene fluoride composite foam;
FIG. 2 is a scanning electron microscope image of the walls of the holes of the polyvinylidene fluoride composite foam 5 prepared in example 5;
FIG. 3 is a scanning electron microscope image of the polyvinylidene fluoride composite foam 8 prepared in example 8;
FIG. 4 is a photograph of polyvinylidene fluoride composite foam 9 prepared in example 9;
fig. 5 is a graph showing the relationship between the sound absorption coefficient and the frequency of the polyvinylidene fluoride composite foam sound absorption material 10 prepared in example 10.
Detailed Description
The invention is described in further detail below with reference to examples and figures, but embodiments of the invention are not limited to the specific embodiments of the invention, involving non-solvent induced phase separation (NIPS) process curing of a substrate and physical foaming in combination with particle leaching. The NIPS method utilizes an organic solvent and a coagulating bath to carry out mass transfer exchange of the solvent and the non-solvent to form a two-phase structure which takes a polymer as a continuous phase and the solvent as a disperse phase, thereby solidifying a matrix material and forming small holes on the wall of a foam hole; the particle leaching method is to take commercially available white granulated sugar with controllable shape and low cost as a pore-forming agent, add the pore-forming agent into a mixed solution to form a mixed system by a blending method, and finally wash out the pore-forming agent to obtain the porous material with uniform foaming and mutually communicated cells.
The polyvinylidene fluoride powders referred to in the examples were all purchased from ARKEMA, france.
Example 1
As shown in fig. 1, a process diagram of the preparation of polyvinylidene fluoride composite foam is shown. 3g of polyvinylidene fluoride powder (KYNAR HSV 900, MW= 800 000) was dissolved in N, N-Dimethylformamide (DMF), and stirred at 50℃for 2 hours to obtain a polyvinylidene fluoride solution. Dispersing 0.01g of Carbon Nano Tube (CNT) in acetone, carrying out ultrasonic treatment for 0.5h, adding the obtained CNT/acetone dispersion liquid into polyvinylidene fluoride solution, and fully stirring for 1h at 50 ℃ to obtain a mixed solution. 15g of commercial white granulated sugar is added into the mixed solution, stirring is continued for 1h at 50 ℃, and a mixed system is obtained when the viscosity of the mixed solution is proper. Stopping stirring, adding water into the mixed system as a coagulating bath, repeatedly replacing the coagulating bath, washing with water after 24 hours, and drying to obtain the polyvinylidene fluoride composite foam 1.
Example 2
As shown in fig. 1, a process diagram of the preparation of polyvinylidene fluoride composite foam is shown. 3g of polyvinylidene fluoride powder (KYNAR HSV 900, MW= 800 000) was dissolved in an organic solvent of 1:1 acetone/DMF and stirred at 80℃for 0.5h to give a polyvinylidene fluoride solution. 0.01g of Carbon Nanotubes (CNTs) was dispersed in acetone and sonicated for 1h. The obtained CNT/acetone dispersion is added into polyvinylidene fluoride solution, and stirring is continued for 2 hours at 80 ℃ to obtain mixed solution. 15g of commercial white granulated sugar is added into the mixed solution, stirring is continued for 0.5h at 80 ℃, and a mixed system is obtained when the viscosity of the mixed solution is proper. Stopping stirring, adding water into the mixed system as a coagulating bath, repeatedly replacing the coagulating bath, washing with water after 24 hours, and drying to obtain the polyvinylidene fluoride composite foam 2.
Example 3
As shown in fig. 1, a process diagram of the preparation of polyvinylidene fluoride composite foam is shown. 3g of polyvinylidene fluoride powder (KYNAR 761, MW= 600 000) was dissolved in an organic solvent of 1:1 acetone: DMAc and stirred at 50℃for 1 hour to give a polyvinylidene fluoride solution. 0.01g of Carbon Nanotubes (CNT) was dispersed in acetone: dmac=1:1, sonicated for 2h. The obtained CNT/acetone/DMAc dispersion is added into polyvinylidene fluoride solution, and stirring is continued for 0.5h at 50 ℃ to obtain mixed solution. 15g of commercial white granulated sugar is added into the mixed solution, stirring is continued for 1h at 50 ℃, and a mixed system is obtained when the viscosity of the mixed solution is proper. Stopping stirring, adding water into the mixed system as a coagulating bath, repeatedly replacing the coagulating bath, washing with water after 24 hours, and drying to obtain the polyvinylidene fluoride composite foam 3.
Example 4
As shown in fig. 1, a process diagram of the preparation of polyvinylidene fluoride composite foam is shown. 3g of polyvinylidene fluoride powder (KYNAR 761, MW= 600 000) was dissolved in an organic solvent of 1:1 acetone/DMF and stirred at 80℃for 1h to give a polyvinylidene fluoride solution. 0.01g of Carbon Nanotubes (CNT) was dispersed in acetone dmf=1:1 and sonicated for 2h. The obtained CNT/acetone/DMF dispersion is added into polyvinylidene fluoride solution, and stirring is continued for 1h at 60 ℃ to obtain mixed solution. Adding 20g of commercial white granulated sugar into the mixed solution, and continuously stirring at 60 ℃ until the viscosity of the mixed solution is proper, thus obtaining a mixed system. Stopping stirring, adding water into the mixed system as a coagulating bath, repeatedly replacing the coagulating bath, washing with water after 24 hours, and drying to obtain the polyvinylidene fluoride composite foam 4.
Example 5
As shown in fig. 1, a process diagram of the preparation of polyvinylidene fluoride composite foam is shown. 3g of polyvinylidene fluoride powder (KYNAR HSV 900, MW= 800 000) was dissolved in an organic solvent of 1:1 acetone/DMF and stirred at 80℃for 1h to give a polyvinylidene fluoride solution. 0.01g of Carbon Nanotubes (CNTs) was dispersed in DMF and sonicated for 2h. The obtained CNF/DMF dispersion is added into polyvinylidene fluoride solution, and stirring is continued for 2 hours at 50 ℃ to obtain mixed solution. 27g of commercial white granulated sugar is added into the mixed solution, stirring is continued for 1h at 60 ℃, and a mixed system is obtained when the viscosity of the mixed solution is proper. Stopping stirring, adding water into the mixed system as a coagulating bath, repeatedly replacing the coagulating bath, washing with water after 24 hours, and drying to obtain the polyvinylidene fluoride composite foam 5.
As shown in fig. 2, a scanning electron microscope image of the wall of the hole of the polyvinylidene fluoride composite foam 5 is shown. From fig. 2, it is clear that micron-sized holes are distributed on the walls of the pores of the polyvinylidene fluoride composite foam 5, and that the small holes on the walls of the pores of the foam provide favorable conditions for the dissipation of acoustic energy, thereby improving the sound absorption performance of the polyvinylidene fluoride composite foam.
Example 6
As shown in fig. 1, a process diagram of the preparation of polyvinylidene fluoride composite foam is shown. 3g of polyvinylidene fluoride powder (KYNAR HSV 900, MW= 800 000) was dissolved in an organic solvent of 1:1 acetone/DMF and stirred at 80℃for 1h to give a polyvinylidene fluoride solution. 0.01g of Carbon Nanotubes (CNTs) was dispersed in DMF and sonicated for 2h. The obtained CNF/DMF dispersion is added into polyvinylidene fluoride solution, and stirring is continued for 2 hours at 70 ℃ to obtain mixed solution. 33g of commercial white granulated sugar is added into the mixed solution, stirring is continued for 1h at 70 ℃, and a mixed system is obtained when the viscosity of the mixed solution is proper. Stopping stirring, adding water into the mixed system as a coagulating bath, repeatedly replacing the coagulating bath, washing with water after 24 hours, and drying to obtain the polyvinylidene fluoride composite foam 6.
Example 7
As shown in fig. 1, a process diagram of the preparation of polyvinylidene fluoride composite foam is shown. 3g of polyvinylidene fluoride powder (KYNAR HSV 900, MW= 800 000) was dissolved in an organic solvent of 1:1 acetone/DMF and stirred at 80℃for 1h to give a polyvinylidene fluoride solution. 0.01g of glass fibers was dispersed in DMF and sonicated for 2h. The obtained glass fiber/DMF dispersion was added to polyvinylidene fluoride solution, and stirring was continued at 80℃for 2 hours to obtain a mixed solution. 33g of commercial white granulated sugar is added into the mixed solution, and stirring is continued for 0.5h at 70 ℃ until the viscosity of the mixed solution is proper, so as to obtain a mixed system. Stopping stirring, adding water into the mixed system as a coagulating bath, repeatedly replacing the coagulating bath, washing with water after 24 hours, and drying to obtain the polyvinylidene fluoride composite foam 7.
Example 8
As shown in fig. 1, a process diagram of the preparation of polyvinylidene fluoride composite foam is shown. 3g of polyvinylidene fluoride powder (KYNAR 761, MW= 600 000) was dissolved in an organic solvent of 1:1 acetone/DMF and stirred at 80℃for 1h to give a polyvinylidene fluoride solution. 0.06g of Carbon Nanotubes (CNTs) were dispersed in acetone and sonicated for 2h. The obtained CNT/acetone dispersion is added into polyvinylidene fluoride solution, and stirring is continued for 2 hours at 70 ℃ to obtain mixed solution. 30g of commercial white granulated sugar is added into the mixed solution, stirring is continued for 1h at 70 ℃, and a mixed system is obtained when the viscosity of the mixed solution is proper. Stopping stirring, adding water into the mixed system as a coagulating bath, repeatedly replacing the coagulating bath, washing with water after 24 hours, and drying to obtain the polyvinylidene fluoride composite foam 8.
As shown in fig. 3, a scanning electron microscope image of the polyvinylidene fluoride composite foam 8 is shown. From fig. 3, it can be seen that the prepared polyvinylidene fluoride composite foam 8 has uniform pore size, uniform filler dispersion, interconnected cells and foam pore walls. The foam cell structure is accurate and controllable, the requirement of regulating and controlling the optimal sound absorption frequency of the material is met, and the possibility is provided for targeted application of the material in complex scenes.
Example 9
As shown in fig. 1, a process diagram of the preparation of polyvinylidene fluoride composite foam is shown. 3g of polyvinylidene fluoride powder (KYNAR 761, MW= 600 000) was dissolved in an organic solvent of 1:1 acetone/DMF and stirred at 80℃for 1h to give a polyvinylidene fluoride solution. 0.03g of glass fibers was dispersed in DMF and sonicated for 2h. The obtained glass fiber/DMF dispersion was added to polyvinylidene fluoride solution, and stirring was continued at 50℃for 2 hours to obtain a mixed solution. 30g of commercial white granulated sugar is added into the mixed solution, stirring is continued for 1.5 hours at 60 ℃, and a mixed system is obtained when the viscosity of the mixed solution is proper. Stopping stirring, adding water with DMF ratio of 5:1 as coagulating bath into the mixed system, repeatedly replacing the coagulating bath, washing with water after 24 hours, and drying to obtain polyvinylidene fluoride composite foam 9.
As shown in fig. 4, a photograph of the polyvinylidene fluoride composite foam 9 is shown. As can be seen from the photographs, the material prepared by the method provided by the patent is uniform and bubble-free. Compared with the prior preparation method, the method has great advantages, realizes the foaming of the polyvinylidene fluoride composite material below 80 ℃ and fills the technical blank of the foaming of a non-solvent induced phase separation method combined with a particle leaching method.
Example 10
As shown in fig. 1, a process diagram of the preparation of polyvinylidene fluoride composite foam is shown. 3g of polyvinylidene fluoride powder (KYNAR 761, MW= 600 000) was dissolved in an organic solvent of 1:1 acetone/DMF and stirred at 80℃for 1h to give a polyvinylidene fluoride solution. 0.02g of Carbon Nanotubes (CNTs) were dispersed in acetone and sonicated for 2h. The obtained CNT/acetone dispersion is added into polyvinylidene fluoride solution, and stirring is continued for 2 hours at 80 ℃ to obtain mixed solution. 30g of commercial white granulated sugar is added into the mixed solution, stirring is continued for 1h at 70 ℃, and a mixed system is obtained when the viscosity of the mixed solution is proper. Stopping stirring, adding water into the mixed system as a coagulating bath, repeatedly replacing the coagulating bath, washing with water after 24 hours, and drying to obtain the polyvinylidene fluoride composite foam 10.
The upper and lower dense skin layers of the composite foam 10 are cut off to prepare a polyvinylidene fluoride composite foam sound absorption material 10 with the diameter of 29mm and the thickness of 10mm, and the polyvinylidene fluoride composite foam sound absorption material 10 is placed in an acoustic impedance tube for acoustic testing, so that a curve of the relation between the sound absorption coefficient and the frequency is obtained.
As shown in fig. 5, the sound absorption coefficient versus frequency curve of the polyvinylidene fluoride composite foam sound absorbing material 10 is shown. As can be seen from fig. 5, the polyvinylidene fluoride composite foam sound absorbing material prepared by the invention has the performance of wide-band sound absorption. Through calculation, when the thickness of the composite foam sound absorption material 10 is only 10mm, the average sound absorption coefficient is 0.71 in the frequency range of 500-6400Hz, and the average sound absorption coefficient is 0.85 in the frequency range of 2000-6400 Hz; the sound absorption coefficient alpha in the frequency range of 1000-6400Hz is larger than 0.2, and the sound absorption coefficient alpha in the frequency range of 1800-6400Hz is larger than 0.5, and the excellent sound absorption performance can meet the sound absorption requirements of different acoustic environments.
Example 11
As shown in fig. 1, a process diagram of the preparation of polyvinylidene fluoride composite foam is shown. 3g of polyvinylidene fluoride powder (KYNAR HSV 900, MW= 800 000) was dissolved in an organic solvent of 1:1 acetone/DMF and stirred at 80℃for 1h to give a polyvinylidene fluoride solution. 0.03g of nanocellulose (CNF) was dispersed in DMAc and sonicated for 2h. The obtained CNF/DMAc dispersion is added into polyvinylidene fluoride solution, and stirring is continued for 2 hours at 70 ℃ to obtain mixed solution. 33g of commercial white granulated sugar is added into the mixed solution, stirring is continued for 2 hours at 70 ℃, and a mixed system is obtained when the viscosity of the mixed solution is proper. Stopping stirring, adding water with DMAc of 5:1 as coagulating bath into the mixed system, repeatedly replacing the coagulating bath, washing with water after 24 hours, and drying to obtain the polyvinylidene fluoride composite foam 11.
The upper and lower dense skin layers of the composite foam 11 are cut off to prepare a polyvinylidene fluoride composite foam sound absorption material 11 with the diameter of 29mm and the thickness of 10mm, and the polyvinylidene fluoride composite foam sound absorption material 11 is placed in an acoustic impedance tube for acoustic testing, so that a curve of the relation between the sound absorption coefficient and the frequency is obtained.
Through calculation, when the thickness of the composite foam sound absorption material 11 is only 10mm, the average sound absorption coefficient is 0.73 in the frequency range of 500-6400Hz, and the average sound absorption coefficient is 0.87 in the frequency range of 2000-6400 Hz; the sound absorption coefficient alpha in the frequency range of 1000-6400Hz is larger than 0.2, and the sound absorption coefficient alpha in the frequency range of 1800-6400Hz is larger than 0.5, and the excellent sound absorption performance can meet the sound absorption requirements of different acoustic environments.
Example 12
As shown in fig. 1, a process diagram of the preparation of polyvinylidene fluoride composite foam is shown. 3g of polyvinylidene fluoride powder (KYNAR HSV 900, MW= 800 000) was dissolved in an organic solvent of 1:1 acetone/DMF and stirred at 80℃for 1h to give a polyvinylidene fluoride solution. 0.03g of glass fibers was dispersed in acetone and sonicated for 2h. The obtained glass fiber/acetone dispersion liquid is added into polyvinylidene fluoride solution, and stirring is continued for 2 hours at 80 ℃ to obtain mixed solution. Adding 33g of commercial white granulated sugar into the mixed solution, continuously stirring, and obtaining a mixed system when the viscosity of the mixed solution is proper. Stopping stirring, adding water and ethanol at a ratio of 5:1 as coagulating bath, repeatedly replacing the coagulating bath, washing with water after 24 hours, and drying to obtain the polyvinylidene fluoride composite foam 12.
The upper and lower dense skin layers of the composite foam 12 are cut off to prepare a polyvinylidene fluoride composite foam sound absorption material 12 with the diameter of 29mm and the thickness of 10mm, and the polyvinylidene fluoride composite foam sound absorption material 12 is placed in an acoustic impedance tube for acoustic testing, so that a curve of the relation between the sound absorption coefficient and the frequency is obtained.
Through calculation, when the thickness of the composite foam sound absorption material 12 is only 10mm, the average sound absorption coefficient is 0.70 in the frequency range of 500-6400Hz, and the average sound absorption coefficient is 0.82 in the frequency range of 2000-6400 Hz; the sound absorption coefficient alpha in the frequency range of 1000-6400Hz is larger than 0.2, and the sound absorption coefficient alpha in the frequency range of 1800-6400Hz is larger than 0.5, and the excellent sound absorption performance can meet the sound absorption requirements of different acoustic environments.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (10)
1. The preparation method of the polyvinylidene fluoride composite foam sound absorption material is characterized by comprising the following operation steps:
(1) Dissolving polyvinylidene fluoride powder serving as a raw material in an organic solvent, and fully stirring at 50-80 ℃ for 0.5-2h to obtain a polyvinylidene fluoride solution;
(2) Dispersing a fiber material in an organic solvent, carrying out ultrasonic treatment for 0.5-2h to obtain a fiber material solution with uniform dispersion, adding the fiber material solution into the polyvinylidene fluoride solution obtained in the step (1), and fully stirring at 50-80 ℃ for 0.5-2h to obtain a mixed solution;
(3) Adding white granulated sugar into the mixed solution obtained in the step (2), and fully stirring for 0.5-2h at the temperature of 50-80 ℃ to obtain a mixed system;
(4) Stopping stirring, adding a coagulating bath into the mixed system obtained in the step (3), repeatedly replacing the coagulating bath, washing with water, and drying to obtain polyvinylidene fluoride composite foam; the aperture of the obtained polyvinylidene fluoride composite foam is uniform and controllable, and the pore wall is distributed with micro-scale small holes;
(5) And (3) cutting off the upper and lower compact skin layers of the polyvinylidene fluoride composite foam obtained in the step (4) to obtain the polyvinylidene fluoride composite foam sound absorption material.
2. The method of manufacturing according to claim 1, characterized in that: the polyvinylidene fluoride powder in the step (1) is one or two of polyvinylidene fluoride powder with MW=600000 and KYNAR761 and polyvinylidene fluoride powder with MW=800000 and KYNAR HSV 900.
3. The method of manufacturing according to claim 1, characterized in that: the organic solvents in the step (1) and the step (2) are one or two of N, N-dimethylformamide, N-dimethylacetamide and acetone.
4. The method of manufacturing according to claim 1, characterized in that: the mass ratio of the polyvinylidene fluoride powder in the step (1) to the fiber material in the step (2) is 50:1-300:1;
the mass ratio of the polyvinylidene fluoride powder in the step (1) to the white granulated sugar in the step (3) is 1:11-1:5.
5. The method of manufacturing according to claim 1, characterized in that: the fiber material in the step (2) is one or more of carbon nano tubes, nano cellulose and glass fibers.
6. The method of manufacturing according to claim 1, characterized in that: the coagulating bath in the step (4) is one or more of water, an alcohol solvent, N-dimethylformamide and N, N-dimethylacetamide.
7. The method of manufacturing according to claim 1, characterized in that: the thickness of the polyvinylidene fluoride composite foam sound absorption material in the step (5) is 10mm.
8. The method of manufacturing according to claim 1, characterized in that: the stirring rates in steps (1) to (3) were 500rpm.
9. A polyvinylidene fluoride composite foam sound absorbing material prepared by the method of any one of claims 1 to 8, characterized in that: the thickness of the polyvinylidene fluoride composite foam sound absorption material is 10mm, the sound absorption coefficient alpha is larger than 0.2 in the frequency range of 1000-6400Hz, and the sound absorption coefficient alpha is larger than 0.5 in the frequency range of 1800-6400 Hz.
10. Use of the polyvinylidene fluoride composite foam sound absorbing material according to claim 9 in the field of broadband sound absorbing materials.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005316353A (en) * | 2004-03-29 | 2005-11-10 | Cci Corp | Sound absorbing structure |
| CN104530614A (en) * | 2014-12-25 | 2015-04-22 | 武汉工程大学 | Porous polyvinylidene fluoride-carbon nanotube composite material and preparation method thereof |
| JP2021043388A (en) * | 2019-09-13 | 2021-03-18 | Jnc株式会社 | Sound absorbing and insulating material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| TWI614386B (en) * | 2015-03-11 | 2018-02-11 | National Taiwan University Of Science And Technology | Acoustic absorbing material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005316353A (en) * | 2004-03-29 | 2005-11-10 | Cci Corp | Sound absorbing structure |
| CN104530614A (en) * | 2014-12-25 | 2015-04-22 | 武汉工程大学 | Porous polyvinylidene fluoride-carbon nanotube composite material and preparation method thereof |
| JP2021043388A (en) * | 2019-09-13 | 2021-03-18 | Jnc株式会社 | Sound absorbing and insulating material |
Non-Patent Citations (3)
| Title |
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| Enhanced airborne sound absorption effect in poly(vinylidene fluoride)/(K0.5Na0.5)NbO3‐nanofiber composite foams;Ayman M.Mohamed等;《Jounal of Applied Polymer Science》;第1-10页 * |
| Hybrid local piezoelectric and conductive functions for high performance airborne sound absorption;Mojtaba Rahimababy等;《Applied Physics Letters》;第111卷(第24期);第1-6页 * |
| Open-Cell Poly(vinylidene fluoride) Foams with Polar Phase for Enhanced Airbone Sound Absorption;Ayman Mahmound Mohamed等;《Applied Physice Letters》;第113卷(第8期);第1-4页 * |
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