CN104464712B - A kind of preparation method of nanofiber foam-based sound-absorbing material - Google Patents
A kind of preparation method of nanofiber foam-based sound-absorbing material Download PDFInfo
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Abstract
The invention provides a kind of preparation method of nanofiber foam-based sound-absorbing material, it is characterised in that specific steps include：The first step：Activation process is carried out to nanofiber foam surface；Second step：It it is 32 DEG C~35 DEG C in temperature, pressure is 7.39 × 106Pa~8.0 × 106Under conditions of Pa, the nanofiber foam obtained by previous step is handled with the mixture of adhesion agent and surface roughness modified particles using supercritical carbon dioxide fluid, then pressure is reduced, nanofiber foam is desorbed supercritical carbon dioxide fluid, make adhesion agent and surface roughness modified particles dispersed to fiber surface；3rd step：Adhesion agent solidification crosslinking is made using heat cross-linking method, surface roughness modified particles is incorporated in fiber surface, obtains nanofiber foam-based sound-absorbing material.The present invention has more excellent sound absorption qualities.
Description
Technical field
The invention belongs to noise pollution Treatment process field, more particularly to a kind of nanofiber foam-based sound-absorbing material and its
Preparation method.
Background technology
Noise pollution produces greatly harm to people's physiology, mental health, effectively prevents noise pollution, reduces noise
Harm be ensure people's normal work and life requisite measure.Sound-absorbing material can from source caused by noise, be propagated through
Journey and the aspect of terminal victim protection three set about administering noise pollution, are to apply the hand maximally efficient to noise pollution
Section.Sound-absorbing material can be divided into porous sound absorbing material, resonance acoustical absorption material and special construction sound-absorbing material by its sound absorption characteristics, its
Middle porous material sound-absorbing material has the characteristics of in light weight, sound-absorbing effect is good, is one of current most widely used sound-absorbing material,
It is widely used in the vehicles, performs in a radio or TV programme the places such as hall, theater.With the fast development of sound-absorbing material industry, only possess good
Good sound-absorbing effect can not fully meet the demand of existing market, and people propose higher requirement to sound-absorbing material, material
Not only want sound absorption qualities good, and require in light weight.Therefore, Ultralight high-efficiency sound-absorbing material becomes global evolution in recent years
One of focus.
Efficient and light weight sound-absorbing material is mainly traditional non-woven fabrics acoustical cotton at present, and scientific research personnel have also been made phase in this regard
The research work answered simultaneously develops a series of sound-absorbing material.Domestic patent CN101471070A discloses a kind of high-performance sound-absorbing
Material and preparation method thereof, the preparation method are first by 1D, 15D terylene short fiber and 1.5D hot melt terylene short fiber by certain
Ratio mixing is standby into the solid netted short fine layer of mixing through hot pressing, then uses 10g/cm2Polypropylene spunbond cloth clamping multilayer it is above-mentioned
The solid netted short fine layer of mixing prepares sound-absorbing material.The TAI-2047 series acoustical cotton products of 3M companies production are current whole world tools
Representational absorptive product, the product be it is compound by a diameter of 25 μm of polyester fiber and a diameter of 2 μm of polypropylene fiber and
Into nonwoven cloth material, bulk density 20mg/cm3, thickness 10mm.Domestic patent CN101903434A discloses one kind and subtracted
Shake sound-absorbing material and its manufacture method, sound-absorbing material described in the patent is obtained by the foamed processing of polyurethane.Above-mentioned patent institute
The material of offer and interiors of products aperture are big and pore-size distribution is narrower, it is impossible to effectively realize the absorption to low frequency noise, Er Qiecai
The bulk density of material is generally bigger than normal.For this big problem of sound-absorbing material bulk density, domestic patent CN101807394Y is disclosed
A kind of micro nanometer fiber compound layered sound-absorbing material, the invention be by it is one or more simultaneously containing 50~900nm and 2~
The sound absorbing layer of 800 μm of fiber composition is overlapped mutually combination, by adjust the micro nanometer fiber components of different layer materials, thickness,
Bulk density and feature filler adjust the sound-absorbing of integral material and the performance such as fire-retardant, although the patent introduces Nanowire
The light components as material are tieed up, but the bulk density of material is still larger, and internal filler only rises including powder split filler
To single filling-modified effect, can not tight bond improve the pore structure of material to fiber surface, therefore material
Sound absorption qualities particularly low frequency sound absorption qualities are poor.In summary, there are sound absorption qualities and be particularly in above-mentioned patent and product
The deficiency that low-frequency range sound absorption qualities are poor and bulk density is excessive, sound-absorbing material is seriously limited in Aero-Space, superior automobile
Deng the extensive application in field.
The content of the invention
The invention aims to solve the problems, such as that above-mentioned material is present to propose a kind of nanofiber foam-based sound absorber
The preparation method of material.
In order to achieve the above object, the invention provides a kind of preparation method of nanofiber foam-based sound-absorbing material, its
It is characterised by, specific steps include：
The first step：Activation process is carried out to nanofiber foam surface；
Second step：It it is 32 DEG C~35 DEG C in temperature, pressure is 7.39 × 106Pa~8.0 × 106Under conditions of Pa, using super
Critical carbon dioxide fluid steeps with the mixture of adhesion agent and surface roughness modified particles to the nanofiber obtained by previous step
Foam is handled, and then reduces pressure, nanofiber foam is desorbed supercritical carbon dioxide fluid, is made adhesion agent thick with surface
Rugosity modified particles are dispersed to fiber surface；
3rd step：Adhesion agent solidification crosslinking is made using heat cross-linking method, surface roughness modified particles is incorporated in fiber table
Face, obtain nanofiber foam-based sound-absorbing material.
Preferably, described nanofiber foam is nanofiber mutually through the three-dimensional network shape frame body sectional material being staggered to form
Material.
Preferably, the bulk density of described nanofiber foam is 0.1~50mg/cm3, aperture is 0.01~10 μm,
Specific surface area is 10~2000m2/g。
Preferably, described nanofiber foam is the uniform nanofiber foamed material of global density, or density
The nanofiber bubble of the nanofiber foamed material of through-thickness even variation either density through-thickness graded
Foam material.
Preferably, described activating treatment method is：Alkali reduction method, solvent extraction, hydrothermal growth process, vapor growth method
With one or more combinations in induced by magnetic field self-assembly method.
Preferably, described adhesion agent is benzoxazine monomer, described supercritical carbon dioxide fluid and adhesion agent and
The mass fraction of adhesion agent is 0.01~10% in the mixture of surface roughness modified particles.
Preferably, described surface roughness modified particles are metallic particles, metal oxide particle, inorganic non-metallic oxygen
One or more combinations of compound particle, organic nanocrystalline particle, graphene sheet layer and graphene oxide layer；The surface
The average grain diameter of roughness modified particles is 0.002~100 μm, described supercritical carbon dioxide fluid and adhesion agent and surface
The mass fraction of surface roughness modified particles is 0.1~20% in the mixture of roughness modified particles.
Preferably, described heat cross-linking is the segmented heat cross-linking mode of temperature programming.
Preferably, the bulk density of described nanofiber foam-based sound-absorbing material is 0.2~60mg/cm3。
Described nanofiber foam-based sound-absorbing material is the suction obtained after modified by three-dimensional manometer fibrous foam material
Sound material, mutually constructed and obtained through surface two level coarse structure through three-dimensional network shape bulk material staggeredly by nanofiber
, surface roughness modified particles are dispersed in fibrous material surface and effective cementation are presented between fiber, construct two
Level coarse structure, increase the reflection loss area of sound wave.
Compared with prior art, the beneficial effects of the invention are as follows：
(1) the nanofiber open celled foam that the present invention uses is different from conventional foam, and its frame structure is by nanometer
Fiber forms so that material has higher specific surface area, high porosity, high pore communication and excellent mechanical property.
By the two level coarse structure of modified fiber surface, the reflection-absorption area to sound wave and the resonance to low frequency noise are added
Decay, assign material more excellent sound absorption qualities.
(2) the characteristics of present invention utilizes nano-fiber material category wide, has widened the raw material type of sound-absorbing material, and
And preparation technology can be regulated and controled in material preparation process, one-step shaping prepares the sound-absorbing material of density gradient structure, improves
The sound absorption qualities of material.
(3) preparation technology of nanofiber foam-based sound-absorbing material provided by the invention is simple, and design on material structure is strong,
Small product size density is small, and thickness is small, and cost is cheap, administers field in noise pollution and is particularly led in light materials such as Aero-Space
Domain has great application prospect and commercial value.
Embodiment
The invention will be further elucidated with reference to specific embodiments.It should be understood that these embodiments are merely to illustrate this hair
Bright rather than limitation the scope of the present invention.In addition, it is to be understood that after the content of the invention lectured has been read, art technology
Personnel can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Fixed scope.Nanofiber foam in following examples is nanofiber mutually through the three-dimensional network shape build being staggered to form
Material, it can be bought in Shanghai Dong Xiang nanosecond science and technology Co., Ltd, high-purity carbon dioxide gas (purity 99.99%) can be with
In Shanghai, Jia Ya Chemical Co., Ltd.s buy, and the air-cooled carbon-dioxide gas compressors of VW-6/2-6 can be in Anhui Ju Feng compressors
Manufacturing Co., Ltd buys.
Embodiment 1
A kind of preparation method of nanofiber foam-based sound-absorbing material, is concretely comprised the following steps：
The first step：Activation process is carried out to nanofiber foam surface using Alkali reduction method, wherein aqueous slkali is quality point
Number is 2% sodium hydroxide solution, and nanofiber foam impregnation is taken out after 2% sodium hydroxide solution, 1 hour and is washed to
Neutrality, it is then placed in convection oven and dries；The nanofiber foam volume density is 0.1mg/cm3, average pore size be
0.01 μm, specific surface area 10m2/g；The nanofiber foam is the uniform nanofiber foam of global density；
Second step：Temperature be 32 DEG C, pressure be 7.39 × 106Under conditions of Pa, using supercritical carbon dioxide fluid
The nanofiber foam obtained by previous step is handled with the mixture of adhesion agent and surface roughness modified particles, then subtracted
Small pressure is 1.01 × 105Pa, nanofiber foam is desorbed supercritical carbon dioxide fluid, make adhesion agent and surface roughness
Modified particles are dispersed to fiber surface；Described supercritical carbon dioxide fluid is by the air-cooled carbon dioxide of VW-6/2-6
Ultrapure carbon dioxide is compressed to 7.39 × 10 by compressor6Pa, temperature are increased to 32 DEG C of gained；Described adhesion agent is benzene
Bing oxazine monomers, described supercritical carbon dioxide fluid and adhesion in the mixture of adhesion agent and surface roughness modified particles
The mass fraction of agent is 0.01%；Described surface roughness modified particles are Al2O3Nano particle, average grain diameter are 0.002 μ
M, described supercritical carbon dioxide fluid change with surface roughness in the mixture of adhesion agent and surface roughness modified particles
Property particle mass fraction be 0.1%：
3rd step：Adhesion agent solidification crosslinking is made using heat cross-linking method, surface roughness modified particles is combined closely in fibre
Dimension table face, two level coarse structure is constructed, obtain the nanofiber-based foam sound-absorbing material of complex three-dimensional with excellent sound absorption qualities；
Described temperature programming segmented heat cross-linking mode be with 5 DEG C/min heating rate temperature programming, respectively 80 DEG C, 100 DEG C,
120 DEG C, 160 DEG C, 180 DEG C, 200 DEG C, 220 DEG C of insulation 10min, the nanofiber foam-based sound-absorbing material bulk density of gained are
0.2mg/cm3。
It is the 5mm sound-absorbing material as test specimen to use thickness, described in ISO10534-2《Acoustic impedance
The measurement part 2 of acoustic absorptivity and acoustic impedance in pipe：Transfer function method》Assay method, given birth to Beijing popularity sound Co., Ltd
The SW260 type impedance tubes of production measure the low-frequency sound-absorbing coefficient of the sample more than 0.20, and maximum sound-absorption coefficient is more than 0.90.It is real
Apply example 2
A kind of preparation method of nanofiber foam-based sound-absorbing material, is concretely comprised the following steps：
The first step：Activation process is carried out to nanofiber foam surface using solvent extraction, wherein extractant is two
Chloromethanes, extraction time 30min, extraction times are 3 times, soluble surface functional group is removed by dichloromethane, are formed and lived
Property site；The nanofiber foam volume density is 50mg/cm3, average pore size be 10 μm, specific surface area 2000m2/g；Institute
It is the nanofiber foamed material that global density through-thickness uniformly changes to state nanofiber foam；
Second step：Temperature be 35 DEG C, pressure be 7.4 × 106Under conditions of Pa, using supercritical carbon dioxide fluid with
The mixture of adhesion agent and surface roughness modified particles is handled the nanofiber foam obtained by previous step, is then reduced
Pressure is to 1.01 × 105Pa, nanofiber foam is desorbed supercritical carbon dioxide fluid, adhesion agent is changed with surface roughness
Property even particulate dispersion is to fiber surface；Described supercritical carbon dioxide fluid is by the air-cooled pressurized carbon dioxides of VW-6/2-6
Ultrapure carbon dioxide is compressed to 7.39 × 10 by contracting machine6Pa, temperature are increased to 32 DEG C of gained；Described adhesion agent is benzo
Oxazine monomer, described supercritical carbon dioxide fluid and adhesion agent in the mixture of adhesion agent and surface roughness modified particles
Mass fraction be 10%；Described surface roughness modified particles are iron particle, and average grain diameter is 100 μm, described super to face
The quality of boundary's CO 2 fluid and surface roughness modified particles in the mixture of adhesion agent and surface roughness modified particles
Fraction is 20%；
3rd step：Adhesion agent solidification crosslinking is made using heat cross-linking method, surface roughness modified particles is firmly incorporated in
Fiber surface, two level coarse structure is constructed, obtain the nanofiber-based foam sound absorber of complex three-dimensional with excellent sound absorption qualities
Material；Described temperature programming segmented heat cross-linking mode be with 5 DEG C/min heating rate temperature programming, respectively 80 DEG C, 100
DEG C, 120 DEG C, 160 DEG C, 180 DEG C, 200 DEG C, 220 DEG C of insulation 10min, the nanofiber foam-based sound-absorbing material volume of gained is close
Spend for 60mg/cm3.It is the 5mm sound-absorbing material as test specimen to use thickness, described in ISO10534-2《Sound
Learn the measurement part 2 of Sound Absorption Coefficient in Impedance Tubes and acoustic impedance：Transfer function method》Assay method, it is limited with Beijing popularity sound
The SW260 type impedance tubes of company's production measure the low-frequency sound-absorbing coefficient of the sample more than 0.4, maximum sound-absorption coefficient be 0.99 with
On.
Embodiment 3
A kind of preparation method of nanofiber foam-based sound-absorbing material, is concretely comprised the following steps：
The first step：Activation process, wherein hydrothermal growth process institute are carried out to nanofiber foam surface using hydrothermal growth process
It is that mass fraction is 5% glucose solution with solution, heating-up temperature is 200 DEG C, pressure 10MPa, and processing time is 2 hours；
The nanofiber foam volume density is 5mg/cm3, average pore size be 1 μm, specific surface area 1000m2/g；The Nanowire
Tie up the nanofiber foamed material that foam is global density through-thickness gradient change.
Second step：Temperature be 34 DEG C, pressure be 7.5 × 106Under conditions of Pa, using supercritical carbon dioxide fluid with
The mixture of adhesion agent and surface roughness modified particles is handled the nanofiber foam obtained by previous step, is then reduced
Pressure is 1.01 × 105Pa, nanofiber foam is desorbed supercritical carbon dioxide fluid, adhesion agent is changed with surface roughness
Property even particulate dispersion is to fiber surface；Described supercritical carbon dioxide fluid is by the air-cooled pressurized carbon dioxides of VW-6/2-6
Ultrapure carbon dioxide is compressed to 7.39 × 10 by contracting machine6Pa, temperature are increased to 32 DEG C of gained；Described adhesion agent is benzo
Oxazine monomer, described supercritical carbon dioxide fluid and adhesion agent in the mixture of adhesion agent and surface roughness modified particles
Mass fraction be 5%；Described surface roughness modified particles are SiO2Particle, average grain diameter are 5 μm, and described is overcritical
The quality point of CO 2 fluid and surface roughness modified particles in the mixture of adhesion agent and surface roughness modified particles
Number is 5%；
3rd step：Adhesion agent solidification crosslinking is made using heat cross-linking method, surface roughness modified particles is combined closely in fibre
Dimension table face, two level coarse structure is constructed, obtain the nanofiber-based foam sound-absorbing material of complex three-dimensional with excellent sound absorption qualities；
Described temperature programming segmented heat cross-linking mode be with 5 DEG C/min heating rate temperature programming, respectively 80 DEG C, 100 DEG C,
120 DEG C, 160 DEG C, 180 DEG C, 200 DEG C, 220 DEG C of insulation 10min, the nanofiber foam-based sound-absorbing material bulk density of gained are
6mg/cm3。
It is the 5mm sound-absorbing material as test specimen to use thickness, described in ISO10534-2《Acoustic impedance
The measurement part 2 of acoustic absorptivity and acoustic impedance in pipe：Transfer function method》Assay method, given birth to Beijing popularity sound Co., Ltd
The SW260 type impedance tubes of production measure the low-frequency sound-absorbing coefficient of the sample more than 0.26, and maximum sound-absorption coefficient is more than 0.93.
Embodiment 4
A kind of preparation method of nanofiber foam-based sound-absorbing material, is concretely comprised the following steps：
The first step：Activation process is carried out to nanofiber foam surface using vapor growth method, wherein using ethene as carbon source,
Ferrocene is catalyst, and high pure nitrogen is protective gas, and treatment temperature is 250 DEG C, and processing time is 1 hour；The Nanowire
It is 15mg/cm to tie up foam volume density3, average pore size be 5 μm, specific surface area 1500m2/g；The nanofiber foam is whole
The uniform nanofiber foam of volume density.
Second step：Temperature be 34 DEG C, pressure be 7.6 × 106Under conditions of Pa using supercritical carbon dioxide fluid with
The mixture of adhesion agent and surface roughness modified particles is handled the nanofiber foam obtained by previous step, is then reduced
Pressure is 1.01 × 105Pa, nanofiber foam is desorbed supercritical carbon dioxide fluid, adhesion agent is changed with surface roughness
Property even particulate dispersion is to fiber surface；Described supercritical carbon dioxide fluid is by the air-cooled pressurized carbon dioxides of VW-6/2-6
Ultrapure carbon dioxide is compressed to 7.39 × 10 by contracting machine6Pa, temperature are increased to 32 DEG C of gained；Described adhesion agent is benzo
Oxazine monomer, described supercritical carbon dioxide fluid and adhesion agent in the mixture of adhesion agent and surface roughness modified particles
Mass fraction be 10%；Described surface roughness modified particles are organic silica gel particle, and average grain diameter is 10 μm, described
Supercritical carbon dioxide fluid and surface roughness modified particles in the mixture of adhesion agent and surface roughness modified particles
Mass fraction is 10%；
3rd step：Adhesion agent solidification crosslinking is made using heat cross-linking method, surface roughness modified particles is combined closely in fibre
Dimension table face, two level coarse structure is constructed, obtain the nanofiber-based foam sound-absorbing material of complex three-dimensional with excellent sound absorption qualities；
Described temperature programming segmented heat cross-linking mode be with 5 DEG C/min heating rate temperature programming, respectively 80 DEG C, 100 DEG C,
120 DEG C, 160 DEG C, 180 DEG C, 200 DEG C, 220 DEG C of insulation 10min, the nanofiber foam-based sound-absorbing material bulk density of gained are
20mg/cm3。
It is the 5mm sound-absorbing material as test specimen to use thickness, described in ISO10534-2《Acoustic impedance
The measurement part 2 of acoustic absorptivity and acoustic impedance in pipe：Transfer function method》Assay method, given birth to Beijing popularity sound Co., Ltd
The SW260 type impedance tubes of production measure the low-frequency sound-absorbing coefficient of the sample more than 0.32, and maximum sound-absorption coefficient is more than 0.97.
Embodiment 5
A kind of preparation method of nanofiber foam-based sound-absorbing material, is concretely comprised the following steps：
The first step：Activation process is carried out to nanofiber foam surface using induced by magnetic field self-assembly method, the magnetic field lures
It is permanent for the PEM-80AC that Mianyang City Li Tian magnetoelectricities Science and Technology Ltd. of Sichuan Province produces to lead the magnetic field generator that self-assembly method uses
Steady magnetic field generator, magnetic field intensity 1.5T, activation modifier Fe3O4Nano particle, a diameter of 20~200nm；It is described from group
Dress method is that magnetized nanofiber is impregnated in into Fe3O440min in nano granule suspension；The nanofiber foam volume
Density is 25mg/cm3, average pore size be 10 μm, specific surface area 1000m2/g；The nanofiber foam is that global density is equal
Even nanofiber foam.
Second step：Temperature be 33 DEG C, pressure be 8 × 106Under conditions of Pa, using supercritical carbon dioxide fluid with gluing
Even the mixture of agent and surface roughness modified particles is handled the nanofiber foam obtained by previous step, then reduces pressure
By force to 1.01 × 105Pa, nanofiber foam is desorbed supercritical carbon dioxide fluid, adhesion agent is modified with surface roughness
Even particulate dispersion is to fiber surface；Described supercritical carbon dioxide fluid is by the air-cooled carbon dioxide compressions of VW-6/2-6
Ultrapure carbon dioxide is compressed to 7.39 × 10 by machine6Pa, temperature are increased to 32 DEG C of gained；Described adhesion agent is Ben Bing Evil
Piperazine monomer, described supercritical carbon dioxide fluid and adhesion agent in the mixture of adhesion agent and surface roughness modified particles
Mass fraction is 10%；Described surface roughness modified particles are graphene sheet layer, and average grain diameter is 10 μm, described super to face
The quality of boundary's CO 2 fluid and surface roughness modified particles in the mixture of adhesion agent and surface roughness modified particles
Fraction is 20%；
3rd step：Adhesion agent solidification crosslinking is made using heat cross-linking method, surface roughness modified particles is combined closely in fibre
Dimension table face, two level coarse structure is constructed, obtain the nanofiber-based foam sound-absorbing material of complex three-dimensional with excellent sound absorption qualities；
Described temperature programming segmented heat cross-linking mode be with 5 DEG C/min heating rate temperature programming, respectively 80 DEG C, 100 DEG C,
120 DEG C, 160 DEG C, 180 DEG C, 200 DEG C, 220 DEG C of insulation 10min, the nanofiber foam-based sound-absorbing material bulk density of gained are
30mg/cm3。
It is the 5mm sound-absorbing material as test specimen to use thickness, described in ISO10534-2《Acoustic impedance
The measurement part 2 of acoustic absorptivity and acoustic impedance in pipe：Transfer function method》Assay method, given birth to Beijing popularity sound Co., Ltd
The SW260 type impedance tubes of production measure the low-frequency sound-absorbing coefficient of the sample more than 0.34, and maximum sound-absorption coefficient is more than 0.98.
Embodiment 6
A kind of preparation method of nanofiber foam-based sound-absorbing material, is concretely comprised the following steps：
The first step：Activation process is carried out to nanofiber foam surface using induced by magnetic field self-assembly method, the magnetic field lures
It is permanent for the PEM-80AC that Mianyang City Li Tian magnetoelectricities Science and Technology Ltd. of Sichuan Province produces to lead the magnetic field generator that self-assembly method uses
Steady magnetic field generator, magnetic field intensity 1.5T, activation modifier Fe3O4Nano particle, a diameter of 20~200nm；It is described from group
Dress method is that magnetized nanofiber is impregnated in into Fe3O430min in nano granule suspension；The nanofiber foam volume
Density is 35mg/cm3, average pore size be 10 μm, specific surface area 2000m2/g；The nanofiber foam is that global density is equal
Even nanofiber foam；
Second step：Temperature be 34 DEG C, pressure be 7.9 × 106Under conditions of Pa, using supercritical carbon dioxide fluid with
The mixture of adhesion agent and surface roughness modified particles is handled the nanofiber foam obtained by previous step, is then reduced
Pressure is to 1.01 × 105Pa, nanofiber foam is desorbed supercritical carbon dioxide fluid, adhesion agent is changed with surface roughness
Property even particulate dispersion is to fiber surface；Described supercritical carbon dioxide fluid is by the air-cooled pressurized carbon dioxides of VW-6/2-6
Ultrapure carbon dioxide is compressed to 7.39 × 10 by contracting machine6Pa, temperature are increased to 32 DEG C of gained；Described adhesion agent is benzo
Oxazine monomer, described supercritical carbon dioxide fluid and adhesion agent in the mixture of adhesion agent and surface roughness modified particles
Mass fraction be 1%；Described surface roughness modified particles are graphene oxide layer, and average grain diameter is 10 μm, described
Supercritical carbon dioxide fluid and adhesion agent and surface roughness modified particles mixture in surface roughness modified particles
Mass fraction be 20%；
3rd step：Adhesion agent solidification crosslinking is made using heat cross-linking method, surface roughness modified particles is combined closely in fibre
Dimension table face, two level coarse structure is constructed, obtain the nanofiber-based foam sound-absorbing material of complex three-dimensional with excellent sound absorption qualities；
Described temperature programming segmented heat cross-linking mode be with 5 DEG C/min heating rate temperature programming, respectively 80 DEG C, 100 DEG C,
120 DEG C, 160 DEG C, 180 DEG C, 200 DEG C, 220 DEG C of insulation 10min, the nanofiber foam-based sound-absorbing material bulk density of gained are
40mg/cm3。
It is the 5mm sound-absorbing material as test specimen to use thickness, described in ISO10534-2《Acoustic impedance
The measurement part 2 of acoustic absorptivity and acoustic impedance in pipe：Transfer function method》Assay method, given birth to Beijing popularity sound Co., Ltd
The SW260 type impedance tubes of production measure the low-frequency sound-absorbing coefficient of the sample more than 0.34, and maximum sound-absorption coefficient is more than 0.99.
Embodiment 7
A kind of preparation method of nanofiber foam-based sound-absorbing material, is concretely comprised the following steps：
The first step：Nanofiber foam surface is entered using the solvent extraction method compound with induced by magnetic field self-assembly method
Row activation process, activation process is carried out to nanofiber foam surface using solvent extraction first, wherein extractant is two
Chloromethanes, extraction time 30min, extraction times are that 3 Ci Shi soluble surfaces functional groups are removed by dichloromethane, form activity
Site；Then the nanofiber foam of above-mentioned gained is handled using induced by magnetic field self-assembly method, the induced by magnetic field is certainly
The magnetic field generator that construction from part uses is the permanent steady magnetic of the PEM-80AC that Mianyang City Li Tian magnetoelectricities Science and Technology Ltd. of Sichuan Province produces
Field generator, magnetic field intensity 1.5T, activation modifier Fe3O4Nano particle, a diameter of 20~200nm；The self assembly side
Method is that magnetized nanofiber is impregnated in into Fe3O430min in nano granule suspension；The nanofiber foam volume density
For 18mg/cm3, average pore size be 10 μm, specific surface area 2000m2/g；The nanofiber foam is that global density is uniform
Nanofiber foam；
Second step：Temperature be 33 DEG C, pressure be 8 × 106Under conditions of Pa, using supercritical carbon dioxide fluid with gluing
Even the mixture of agent and surface roughness modified particles is handled the nanofiber foam obtained by previous step, then reduces pressure
By force to 1.01 × 105Pa, nanofiber foam is desorbed supercritical carbon dioxide fluid, adhesion agent is modified with surface roughness
Even particulate dispersion is to fiber surface；Described supercritical carbon dioxide fluid is by the air-cooled carbon dioxide compressions of VW-6/2-6
Ultrapure carbon dioxide is compressed to 7.39 × 10 by machine6Pa, temperature are increased to 32 DEG C of gained；Described adhesion agent is Ben Bing Evil
Piperazine monomer, described supercritical carbon dioxide fluid and adhesion agent in the mixture of adhesion agent and surface roughness modified particles
Mass fraction is 6%；Described surface roughness modified particles are graphene oxide layer and Al2O3The mixture of particle, it is described
Supercritical carbon dioxide fluid be averaged with graphene oxide layer in the mixture of adhesion agent and surface roughness modified particles
Particle diameter is 10 μm, mass fraction 5%, described supercritical carbon dioxide fluid and adhesion agent and surface roughness modified particles
Mixture in Al2O3Particle, particle diameter are 5 μm, mass fraction 10%,
3rd step：Adhesion agent solidification crosslinking is made using heat cross-linking method, surface roughness modified particles is combined closely in fibre
Dimension table face, two level coarse structure is constructed, obtain the nanofiber-based foam sound-absorbing material of complex three-dimensional with excellent sound absorption qualities；
Described temperature programming segmented heat cross-linking mode be with 5 DEG C/min heating rate temperature programming, respectively 80 DEG C, 100 DEG C,
120 DEG C, 160 DEG C, 180 DEG C, 200 DEG C, 220 DEG C of insulation 10min, the nanofiber foam-based sound-absorbing material bulk density of gained are
20mg/cm3。
It is the 5mm sound-absorbing material as test specimen to use thickness, described in ISO10534-2《Acoustic impedance
The measurement part 2 of acoustic absorptivity and acoustic impedance in pipe：Transfer function method》Assay method, given birth to Beijing popularity sound Co., Ltd
The SW260 type impedance tubes of production measure the low-frequency sound-absorbing coefficient of the sample more than 0.32, and maximum sound-absorption coefficient is more than 0.97.
Embodiment 8
A kind of preparation method of nanofiber foam-based sound-absorbing material, is concretely comprised the following steps：
The first step：Using vapor growth method and induced by magnetic field self-assembly method composite modifying method to nanofiber foam surface
Activation process is carried out, activation process is carried out to nanofiber foam surface using vapor growth method first, wherein using ethene as carbon
Source, ferrocene are catalyst, and high pure nitrogen is protective gas, and treatment temperature is 250 DEG C, and processing time is 1 hour；Then use
Induced by magnetic field self-assembly method is handled the nanofiber foam of above-mentioned gained, the magnetic that the induced by magnetic field self-assembly method uses
Field generator is the PEM-80AC constant magnetic field generators of Mianyang City Li Tian magnetoelectricities Science and Technology Ltd. of Sichuan Province production, and magnetic field is strong
Spend for 1.5T, activation modifier Fe3O4Nano particle, a diameter of 20~200nm；The self-assembling method is to be received magnetized
Rice fiber impregnation is in Fe3O430min in nano granule suspension；The nanofiber foam volume density is 8mg/cm3, it is average
Aperture is 10 μm, specific surface area 2000m2/g；The nanofiber foam is the uniform nanofiber foam of global density；
Second step：Temperature be 34 DEG C, pressure be 7.8 × 106Under conditions of Pa, using supercritical carbon dioxide fluid with
The mixture of adhesion agent and surface roughness modified particles is handled the nanofiber foam obtained by previous step, is then reduced
Pressure is to 1.01 × 105Pa, nanofiber foam is desorbed supercritical carbon dioxide fluid, adhesion agent is changed with surface roughness
Property even particulate dispersion is to fiber surface；Described supercritical carbon dioxide fluid is by the air-cooled pressurized carbon dioxides of VW-6/2-6
Ultrapure carbon dioxide is compressed to 7.39 × 10 by contracting machine6Pa, temperature are increased to 32 DEG C of gained；Described adhesion agent is benzo
Oxazine monomer, described supercritical carbon dioxide fluid and adhesion agent in the mixture of adhesion agent and surface roughness modified particles
Mass fraction be 7%；Described surface roughness modified particles are graphene oxide layer and Fe3O4The mixing of nano particle
Thing, described supercritical carbon dioxide fluid and graphene oxide sheet in the mixture of adhesion agent and surface roughness modified particles
Layer average grain diameter is 10 μm, mass fraction 10%, described supercritical carbon dioxide fluid and adhesion agent and surface roughness
Al in the mixture of modified particles2O3Particle, particle diameter are 5 μm, mass fraction 5%；
3rd step：Adhesion agent solidification crosslinking is made using heat cross-linking method, surface roughness modified particles is combined closely in fibre
Dimension table face, two level coarse structure is constructed, obtain the nanofiber-based foam sound-absorbing material of complex three-dimensional with excellent sound absorption qualities；
Described temperature programming segmented heat cross-linking mode be with 5 DEG C/min heating rate temperature programming, respectively 80 DEG C, 100 DEG C,
120 DEG C, 160 DEG C, 180 DEG C, 200 DEG C, 220 DEG C of insulation 10min, the nanofiber foam-based sound-absorbing material bulk density of gained are
10mg/cm3。
Bulk density is used as 10mg/cm3, thickness be 5mm sound-absorbing material as test specimen, based on ISO10534-2
Described in《The measurement part 2 of acoustic absorptivity and acoustic impedance in acoustic impedance pipe：Transfer function method》Assay method, use Beijing
The SW260 type impedance tubes of popularity sound Co., Ltd production measure the low-frequency sound-absorbing coefficient of the sample more than 0.3, maximum sound-absorbing system
Number is more than 0.95.
Embodiment 9
A kind of preparation method of nanofiber foam-based sound-absorbing material, is concretely comprised the following steps：
The first step：Using vapor growth method and induced by magnetic field self-assembly method composite modifying method to nanofiber foam surface
Activation process is carried out, activation process is carried out to nanofiber foam surface using vapor growth method first, wherein using ethene as carbon
Source, ferrocene are catalyst, and high pure nitrogen is protective gas, and treatment temperature is 250 DEG C, and processing time is 1 hour；Then use
Induced by magnetic field self-assembly method is handled the nanofiber foam of above-mentioned gained, the magnetic that the induced by magnetic field self-assembly method uses
Field generator is the PEM-80AC constant magnetic field generators of Mianyang City Li Tian magnetoelectricities Science and Technology Ltd. of Sichuan Province production, and magnetic field is strong
Spend for 1.5T, activation modifier Fe3O4Nano particle, a diameter of 20~200nm；The self-assembling method is to be received magnetized
Rice fiber impregnation is in Fe3O430min in nano granule suspension；The nanofiber foam volume density is 30mg/cm3, it is average
Aperture is 10 μm, specific surface area 2000m2/g；The nanofiber foam is the uniform nanofiber foam of global density；
Second step：Temperature be 33 DEG C, pressure be 7.7 × 106Under conditions of Pa, using supercritical carbon dioxide fluid with
The mixture of adhesion agent and surface roughness modified particles is handled the nanofiber foam obtained by previous step, is then reduced
Pressure is to 1.01 × 105Pa, nanofiber foam is desorbed supercritical carbon dioxide fluid, adhesion agent is changed with surface roughness
Property even particulate dispersion is to fiber surface；Described supercritical carbon dioxide fluid is by the air-cooled pressurized carbon dioxides of VW-6/2-6
Ultrapure carbon dioxide is compressed to 7.39 × 10 by contracting machine6Pa, temperature are increased to 32 DEG C of gained；Described adhesion agent is benzo
Oxazine monomer, described supercritical carbon dioxide fluid and adhesion agent in the mixture of adhesion agent and surface roughness modified particles
Mass fraction be 6%；Described surface roughness modified particles are iron particle, graphene oxide layer and Al2O3Particle mixes
Compound, described supercritical carbon dioxide fluid with the mixture of adhesion agent and surface roughness modified particles iron particle it is straight
Footpath is 5 μm, mass fraction 4%, and graphene oxide layer average grain diameter is 10 μm, mass fraction 5%, Al2O3Particle, grain
Footpath is 5 μm, mass fraction 10%；
3rd step：Adhesion agent solidification crosslinking is made using heat cross-linking method, surface roughness modified particles is combined closely in fibre
Dimension table face, two level coarse structure is constructed, obtain the nanofiber-based foam sound-absorbing material of complex three-dimensional with excellent sound absorption qualities；
Described temperature programming segmented heat cross-linking mode be with 5 DEG C/min heating rate temperature programming, respectively 80 DEG C, 100 DEG C,
120 DEG C, 160 DEG C, 180 DEG C, 200 DEG C, 220 DEG C of insulation 10min, the nanofiber foam-based sound-absorbing material bulk density of gained are
40mg/cm3。
It is the 5mm sound-absorbing material as test specimen to use thickness, described in ISO10534-2《Acoustic impedance
The measurement part 2 of acoustic absorptivity and acoustic impedance in pipe：Transfer function method》Assay method, given birth to Beijing popularity sound Co., Ltd
The SW260 type impedance tubes of production measure the low-frequency sound-absorbing coefficient of the sample more than 0.34, and maximum sound-absorption coefficient is more than 0.99.
Embodiment 10
A kind of preparation method of nanofiber foam-based sound-absorbing material, is concretely comprised the following steps：
The first step：Using vapor growth method, induced by magnetic field self-assembly method and hydrothermal growth process composite modifying method to nanometer
Fibrous foam surface carries out activation process, carries out activation process to nanofiber foam surface using vapor growth method first, its
In using ethene as carbon source, ferrocene is catalyst, and high pure nitrogen is protective gas, and treatment temperature is 250 DEG C, processing time 1
Hour；Then the nanofiber foam obtained by previous step is handled using induced by magnetic field self-assembly method, the induced by magnetic field
The magnetic field generator that self-assembly method uses is permanent steady for the PEM-80AC that Mianyang City Li Tian magnetoelectricities Science and Technology Ltd. of Sichuan Province produces
Magnetic field generator, magnetic field intensity 1.5T, activation modifier Fe3O4Nano particle, a diameter of 20~200nm；The self assembly
Method is that magnetized nanofiber is impregnated in into Fe3O430min in nano granule suspension；Finally using hydrothermal growth process to upper
Nanofiber foam obtained by one step is handled, and wherein solution used in hydrothermal growth process is that mass fraction is 5% glucose solution,
Heating-up temperature is 200 DEG C, pressure 10MPa, and processing time is 2 hours；The nanofiber foam volume density is 4mg/
cm3, average pore size be 20 μm, specific surface area 2000m2/g；The nanofiber foam is global density through-thickness gradient
The nanofiber foamed material of change；
Second step：Temperature be 32 DEG C, pressure be 7.5 × 106Under conditions of Pa, using supercritical carbon dioxide fluid with
The mixture of adhesion agent and surface roughness modified particles is handled the nanofiber foam obtained by previous step, is then reduced
Pressure is 1.01 × 105Pa, nanofiber foam is desorbed supercritical carbon dioxide fluid, adhesion agent is changed with surface roughness
Property even particulate dispersion is to fiber surface；Described supercritical carbon dioxide fluid is by the air-cooled pressurized carbon dioxides of VW-6/2-6
Ultrapure carbon dioxide is compressed to 7.39 × 10 by contracting machine6Pa, temperature are increased to 32 DEG C of gained；Described adhesion agent is benzo
Oxazine monomer, described supercritical carbon dioxide fluid and adhesion agent in the mixture of adhesion agent and surface roughness modified particles
Mass fraction be 6%；Described surface roughness modified particles are iron particle, graphene oxide layer and Al2O3Particle mixes
Compound, described supercritical carbon dioxide fluid with the mixture of adhesion agent and surface roughness modified particles iron particle it is straight
Footpath is 5 μm, mass fraction 4%, and graphene oxide layer average grain diameter is 10 μm, mass fraction 5%, Al2O3Grain diameter
For 5 μm, mass fraction 10%；
3rd step：Adhesion agent solidification crosslinking is made using heat cross-linking method, surface roughness modified particles is combined closely in fibre
Dimension table face, two level coarse structure is constructed, obtain the nanofiber-based foam sound-absorbing material of complex three-dimensional with excellent sound absorption qualities；
Described temperature programming segmented heat cross-linking mode be with 5 DEG C/min heating rate temperature programming, respectively 80 DEG C, 100 DEG C,
120 DEG C, 160 DEG C, 180 DEG C, 200 DEG C, 220 DEG C of insulation 10min, the nanofiber foam-based sound-absorbing material bulk density of gained are
5mg/cm3。
It is the 5mm sound-absorbing material as test specimen to use thickness, described in ISO10534-2《Acoustic impedance
The measurement part 2 of acoustic absorptivity and acoustic impedance in pipe：Transfer function method》Assay method, given birth to Beijing popularity sound Co., Ltd
The SW260 type impedance tubes of production measure the low-frequency sound-absorbing coefficient of the sample more than 0.25, and maximum sound-absorption coefficient is more than 0.92.
Claims (8)
1. a kind of preparation method of nanofiber foam-based sound-absorbing material, it is characterised in that specific steps include：
The first step：Activation process is carried out to nanofiber foam surface；
Second step：It it is 32 DEG C ~ 35 DEG C in temperature, pressure is 7.39 × 106Pa~8.0 × 106Under conditions of Pa, use is overcritical
CO 2 fluid enters with the mixture of adhesion agent and surface roughness modified particles to the nanofiber foam obtained by previous step
Row processing, then reduces pressure, nanofiber foam is desorbed supercritical carbon dioxide fluid, makes adhesion agent and surface roughness
Modified particles are dispersed to fiber surface；Described surface roughness modified particles be metallic particles, metal oxide particle,
Inorganic non-metallic oxide particle, organic nanocrystalline particle, graphene sheet layer and graphene oxide layer it is one or more
Combination；The average grain diameter of the surface roughness modified particles be 0.002 ~ 100 μm, described supercritical carbon dioxide fluid with
The mass fraction of surface roughness modified particles is 0.1 ~ 20% in the mixture of adhesion agent and surface roughness modified particles；
3rd step：Adhesion agent solidification crosslinking is made using heat cross-linking method, surface roughness modified particles is incorporated in fiber surface, obtains
Obtain nanofiber foam-based sound-absorbing material.
2. the preparation method of nanofiber foam-based sound-absorbing material as claimed in claim 1, it is characterised in that described nanometer
Fibrous foam is nanofiber mutually through the three-dimensional network shape bulk material being staggered to form.
3. the preparation method of nanofiber foam-based sound-absorbing material as claimed in claim 1, it is characterised in that described nanometer
The bulk density of fibrous foam is 0.1 ~ 50mg/cm3, aperture is 0.01 ~ 10 μm, and specific surface area is 10 ~ 2000m2/g。
4. the preparation method of nanofiber foam-based sound-absorbing material as claimed in claim 1, it is characterised in that described nanometer
Fibrous foam is the uniform nanofiber foamed material of global density, or the Nanowire of density through-thickness even variation
Tie up the nanofiber foamed material of foamed material either density through-thickness graded.
5. the preparation method of nanofiber foam-based sound-absorbing material as claimed in claim 1, it is characterised in that described activation
Processing method is：One in Alkali reduction method, solvent extraction, hydrothermal growth process, vapor growth method and induced by magnetic field self-assembly method
Kind or a variety of combinations.
6. the preparation method of nanofiber foam-based sound-absorbing material as claimed in claim 1, it is characterised in that described adhesion
Agent is benzoxazine monomer, described supercritical carbon dioxide fluid and adhesion agent and the mixture of surface roughness modified particles
The mass fraction of middle adhesion agent is 0.01 ~ 10%.
7. the preparation method of nanofiber foam-based sound-absorbing material as claimed in claim 1, it is characterised in that described heat friendship
Join the segmented heat cross-linking mode for temperature programming.
8. the preparation method of nanofiber foam-based sound-absorbing material as claimed in claim 1, it is characterised in that described nanometer
The bulk density of fibrous foam base sound-absorbing material is 0.2 ~ 60mg/cm3。
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| CN106782476A (en) * | 2016-11-17 | 2017-05-31 | 无锡明盛纺织机械有限公司 | A kind of sound-absorbing material and preparation method thereof |
| US11738116B2 (en) | 2017-06-09 | 2023-08-29 | Board Of Regents Of The University Of Nebraska | Expanded nanofiber structures comprising electrospun nanofibers and a plurality of holes and methods of making and use thereof |
| CN107142557B (en) * | 2017-06-29 | 2019-09-13 | 苏州夸克新材料科技有限公司 | A method of Zeolite-carbon composite fibre sound-absorbing material is prepared using method of electrostatic spinning |
| WO2019060393A1 (en) | 2017-09-19 | 2019-03-28 | Board Of Regents Of The University Of Nebraska | Nanofiber structures and methods of use thereof |
| CN108442099B (en) * | 2018-03-28 | 2020-06-02 | 南通大学 | Anti-ultraviolet nano zinc oxide composite textile fabric and preparation method thereof |
| CN115960586B (en) * | 2022-12-09 | 2023-11-28 | 中国石油大学(北京) | Foam drilling fluid and preparation method and application thereof |
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