CN108395637A - A kind of sound-absorbing micro-sphere material and preparation method thereof - Google Patents
A kind of sound-absorbing micro-sphere material and preparation method thereof Download PDFInfo
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- CN108395637A CN108395637A CN201810131978.XA CN201810131978A CN108395637A CN 108395637 A CN108395637 A CN 108395637A CN 201810131978 A CN201810131978 A CN 201810131978A CN 108395637 A CN108395637 A CN 108395637A
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- 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
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
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- 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
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- C08K3/36—Silica
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- 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
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Abstract
The present invention relates to speaker technology fields, more particularly to a kind of sound-absorbing micro-sphere material and preparation method thereof.The preparation method includes the following steps：By zeolite particles, elastomer powder, adhesive and aqueous solvent stirring to obtain mix suspending solution, wherein the addition quality of elastomer powder is the 2%~4% of the mix suspending solution gross mass；Mix suspending solution is granulated, sieves the sound absorption micro-sphere material for obtaining target grain size.The present invention is on the basis of conventional loudspeakers porous zeolite absorbs sound micro-sphere material bonding preparation; by the elastomer powder for introducing certain content; without increasing gluing agent content; it can be solved the low impact flexibility problem of sound absorption micro-sphere material generally existing; and can prepare conveniently and scale that anti-aging property is excellent, have the zeolite sound-absorbing micro-sphere material of more long life.
Description
【Technical field】
The present invention relates to speaker technology fields, more particularly to a kind of sound-absorbing micro-sphere material and preparation method thereof.
【Background technology】
Current speaker sound-absorbing micro-sphere material, is mainly obtained by multiple zeolite particles by way of bonding forming.
After sound-absorbing micro-sphere material is prepared with which, which can be packed into speaker chamber.It raises one's voice
At work, cavity will produce judder to device, if things go on like this sound-absorbing micro-sphere material will appear outer layer zeolite particle fall off or even
The broken situation of whole ball, influences the sound absorption effect and service life of loud speaker.Existing settling mode is usually：By increasing glue
The mode of glutinous agent content or the adhesive for selecting lower glass transition temperatures is effectively to solve made sound-absorbing micro-sphere material in routine
Shock resistance problem under operating temperature, frequency.
Inventor has found in the implementation of the present invention：In order to increase the impact resistance of sound-absorbing micro-sphere material, and select
The mode for increasing gluing agent content or the adhesive of lower glass transition temperatures, can lead to such as adhesive plug-hole, sound-absorbing microballoon
The problems such as material at high temperature weatherability is poor, material hole holds and specific surface area reduces, which also will greatly reduce micro-sphere material
Whole sound absorption effect.
【Invention content】
One purpose of the embodiment of the present invention is to provide a kind of sound-absorbing micro-sphere material and preparation method thereof, aims to solve the problem that existing
There is sound-absorbing micro-sphere material to be difficult on the basis of keeping high acoustic absorption performance, have the problem of high impact resistance.
In order to solve the above-mentioned technical problem, the embodiment of the present invention provides following technical scheme：
In a first aspect, the embodiment of the present invention provides a kind of preparation method of sound-absorbing micro-sphere material,
Include the following steps：Zeolite particles, elastomer powder, adhesive and aqueous solvent stirring to obtain mix suspending is molten
Liquid, wherein the addition quality of the elastomer powder is the 2%~4% of the mix suspending solution gross mass；By the mixing
Aaerosol solution is granulated, sieves the sound absorption micro-sphere material for obtaining target grain size.
It is optionally, described that the mix suspending solution is granulated, sieves the sound absorption micro-sphere material for obtaining target grain size,
It specifically includes：The mix suspending solution is subjected to spray-drying process, obtains preliminary shaped granule；By the just one-step forming
For grain at 100~150 DEG C, dry 1~3h obtains dry particle；The dry particle is obtained into target grain size using sieve screening
Sound absorption micro-sphere material.
Optionally, the target grain size is 150~380 μm.
Optionally, the addition quality of the elastomer powder be the mix suspending solution gross mass 2.5%~
3.5%.
Optionally, the particle diameter range of the zeolite particles raw material is 0.5~5 μm.
Optionally, the particle diameter range of the zeolite particles raw material is 1~3 μm.
Optionally, the elastomer powder is made of following one or more kinds of crosslinking-type rubbers：Cross-linking type natural rubber,
Cross-linking type butadiene-styrene rubber, cross-linking type carboxylic styrene-butadiene rubber, cross-linking type polybutadiene rubber, crosslinking butadiene nitrile rubber, cross-linking type carboxylic
Base nitrile rubber, cross-linking type neoprene, crosslinking acrylate rubber, cross-linking type silicon rubber and cross-linking type butadiene-vinylpyridine rubber.
Optionally, the particle diameter of the elastomer powder is 20nm~2 μm.
Optionally, the particle diameter of the elastomer powder is 50nm~500nm.
In second aspect, the embodiment of the present invention provides a kind of preparation method using above-mentioned sound-absorbing micro-sphere material and is prepared
Sound-absorbing micro-sphere material.
The present invention is specific by introducing on the basis of conventional loudspeakers porous zeolite absorbs sound micro-sphere material bonding preparation
The elastomer powder of content, without increasing gluing agent content, you can solve the low impact flexibility of sound absorption micro-sphere material generally existing
Problem, and can prepare conveniently and scale that anti-aging property is excellent, have the zeolite sound-absorbing micro-sphere material of more long life.
【Description of the drawings】
Fig. 1 is a kind of flow diagram of the preparation method of sound-absorbing micro-sphere material provided in an embodiment of the present invention.
【Specific implementation mode】
In order to make the purpose of the present invention, scheme and advantage be more clearly understood, with reference to the accompanying drawings and embodiments, to this hair
It is bright to be further elaborated.It should be appreciated that described herein, specific examples are only used to explain the present invention, is not used to
Limit the present invention.In addition, as long as technical characteristic involved in invention described below different embodiments is each other
Not constituting conflict can be combined with each other.
The embodiment of the present invention is mainly used in the sound-absorbing material in loud speaker, for the ease of those skilled in the art to this hair
The understanding of bright embodiment, inventor applied to the mechanism of action of the sound-absorbing material in loud speaker to being described below：
Loud speaker converting electrical signals to voice signal energy converter as one kind, is widely used in a variety of electronics devices
In part.The shell inner cavity of loud speaker module can be divided into former and later two operatic tunes from structure, wherein it is most important to influence loudspeaker tonequality
Factor be back cavity sound-absorbing effect.Microspeaker of new generation mostly uses porous sound absorbing material to realize sound-absorbing, and zeolite
Sound absorption microballoon is one kind in granular porous sound-absorbing material, and microsphere surface is mutually communicated and deep between duct rich in pore
Enter to inside microballoon.Sound wave can cause air vibration, due to the vibration as a kind of mechanical energy after entering porous sound absorbing material
Stopped by tortuous pore wall, with pore wall friction, which occurs, for air will cause energy loss.Simultaneously, sound wave can be in hole
Multiple reflections and refraction are undergone between gap wall, so that most of energy is become in heat energy dissipation to environment, are reached noise reduction.This
Outside, porous sound absorbing material compares the gentle body quick adsorption-desorption property of high surface area, and operatic tunes resonance space may make virtually to increase
Greatly, to effectively reduce the middle low-frequency resonance frequency F0 of loud speaker module.
As recorded in background technology, at work, cavity will produce judder to loud speaker, if things go on like this sound absorber
Material will appear the situation that outer layer zeolite particle falls off or even whole ball is broken, influence the sound absorption effect and service life of loud speaker.
Based on this, the embodiment of the present invention provide a kind of convenience, can prepare with scale sound-absorbing micro-sphere material, by inhaling
Sound micro-sphere material adds elastomer powder during preparing and buffers filler as structural mechanics, is deposited to solve existing sound-absorbing material
Low impact sex chromosome mosaicism.Sound-absorbing micro-sphere material provided in an embodiment of the present invention has good acoustical behavior and application advantage.
The preparation method of sound-absorbing micro-sphere material provided in an embodiment of the present invention is illustrated first below.
Referring to Fig. 1, Fig. 1 is a kind of flow signal of the preparation method of sound-absorbing micro-sphere material provided in an embodiment of the present invention
Figure, as shown in Figure 1, this method 100 includes：
Step 10, by zeolite particles, elastomer powder, adhesive and aqueous solvent stirring to obtain aaerosol solution.
Wherein, the zeolite particles can select the zeolite particles of following one or more kinds of structures：FER zeolites, MFI boilings
Stone, MEL zeolites, CHA zeolites, IHW zeolites, IWV zeolites, ITE zeolites, UTL zeolites, VET zeolites, MTW zeolites and FAU zeolites.
Preferably, the silica alumina ratio of the zeolite particles raw material is more than 200, higher silica alumina ratio can increase the hydrophobicity of zeolite particles,
The hygroscopicity for reducing sound absorption micro-sphere material, to increase its ageing resistance.
Zeolite type selected by the application, the solid porose diameter range of zeolite particles raw material be 0.38nm extremely
0.74nm.Preferably, a diameter of 0.4nm~0.6nm of zeolite particles.The present embodiment is simultaneous in the case where ensureing that raw material aperture is small
It is pliable to care for gas, a diameter of 0.4nm~0.6nm of preferred zeolite particle.The particle diameter of the zeolite particles raw material is 0.5~5 μ
M, preferably 1~3 μm.
In the present embodiment, the addition quality of zeolite particles is the 20%~40% of mix suspending solution gross mass, preferably
It is 25%~35%；Wherein, the calculation of aaerosol solution gross mass is zeolite particles, elastomer powder, adhesive and solvent
The sum of water gross mass.
Wherein, the elastomer powder can be made by following one or more kinds of crosslinking-type rubbers after dusting：
Cross-linking type natural rubber, cross-linking type butadiene-styrene rubber, cross-linking type carboxylic styrene-butadiene rubber, cross-linking type polybutadiene rubber,
Crosslinking butadiene nitrile rubber, cross-linking type carboxy nitrile rubber, cross-linking type neoprene, crosslinking acrylate rubber, cross-linking type silicon
Rubber, cross-linking type butadiene-vinylpyridine rubber etc.；
It can be following various ways that above-mentioned crosslinking-type rubber is obtained the dusting mode of elastomer powder by dusting：Machine
Tool comminuting method, spray drying process, expansion drying method, freezing dusting method, co-agglomeration etc..Preferably, in view of making in the present invention
Elastomer powder granular size, preferred method are spray drying process.In the present embodiment, elastomer powder obtained
A diameter of 20nm~2 μm of grain, preferably, the elastomer powder particle diameter is preferably 50nm~500nm.This is because：
Rubber powder is too small, can block the surface duct of zeolite materials particle, and the specific surface area for reducing micro-sphere material entirety is gentle pliable,
It is unfavorable to sound absorption qualities.2, rubber powder particle is bigger, is just more difficult to be filled into the gap of zeolite particles, to micro-sphere material
Bulk density promotion is smaller, and the present embodiment is based on above-mentioned consideration, the preferably elastomer powder of 50nm~500nm.
In some embodiments, the elastomer powder can also be made by crosslinking-type rubber and plastic blend system, i.e.,
It is made by sulfuration thermoplastic elastomer.
The crosslinking-type rubber is as described above, the plastics can be following one or more：Polyamide, polypropylene,
Polyethylene, polyvinyl chloride, polyurethane, epoxy resin, polyester, makrolon, polyformaldehyde, polystyrene, polyphenylene oxide, polyphenylene sulfide
Ether, polyimides or polysulfones.The preparation method of above-mentioned elastomer powder is preparation method commonly used in the art, this field skill
Art personnel can be prepared, details are not described herein according to existing elastomer powder preparation method.
In the present embodiment, elastomer powder quality accounts for the 2%~4% of aaerosol solution gross mass, preferably 2.5%~
3.5%；Wherein, the calculation of aaerosol solution gross mass is zeolite particles, elastomer powder and the total matter of gluing agent emulsion three
The sum of amount.
Wherein, the adhesive can be inorganic adhesive and/or polymer adhesive；The inorganic adhesive packet
It includes：One or more of Ludox, Aluminum sol and kaolin；The polymer adhesive includes：Polyacrylate, poly- ammonia
One or more of esters, epoxy resin.
The adhesive and the zeolite particles and the elastomer powder are at normal temperatures, fully mixed by aqueous solvent stirring
It closes, obtains mix suspending solution.
In the present embodiment, churned mechanically 250~1000rpm of rate, 1~4h of mixing time.Those skilled in the art
The suitable adjustment of suitable agitation rate and mixing time can also be carried out according to practical stirring state, wherein stir speed (S.S.) is slower
Then mixing time is longer, and correspondingly, the more fast then mixing time of stir speed (S.S.) is shorter.
In the present embodiment, adhesive quality accounts for the 1%~10% of aaerosol solution gross mass, preferably 2%~5%；Its
In, the calculation of aaerosol solution gross mass be zeolite particles, elastomer powder, adhesive and aqueous solvent gross mass it
With.
Preferably, when being stirred mixing, aqueous solvent can be added, so that in mix suspending solution obtained, is added
The gross mass of the zeolite particles, elastomer powder and the adhesive that add is suspension gross mass：25~50%, preferably 30~
40%.
Above-mentioned aaerosol solution is granulated, sieves the sound absorption micro-sphere material for obtaining target size by step 20.
Following methods can be selected to be granulated in this embodiment：Spray-drying process squeezes granulation, melt granulation, turns
Dynamic granulation or vulcanization bed granulation.Preferably, after spray drying being selected to be pelletized, carries out screening and obtain target size
Absorb sound micro-sphere material.
The process described in detail below pelletized using spray drying, the process include：
1, mix suspending solution under nitrogen atmosphere or air atmosphere is subjected to spray-drying process, obtains just one-step forming
Particle；
2, by the preliminary shaped granule at 100~150 DEG C, dry 1~3h obtains dry particle；
3, the dry particle is obtained to the sound absorption micro-sphere material of target grain size using the screening of 40~100 mesh screens.
Wherein, those skilled in the art are easy to obtain, drying temperature more low then drying time is longer, correspondingly, do
Dry temperature more high then drying time is shorter.
In some embodiments, it is also an option that non-crosslinked type rubber powder or adhesive use rubber latex, with system
It is standby go out similar grain size porous zeolite absorb sound micro-sphere material, then similar material of the present invention is obtained by sulfidation.
The preparation method of sound-absorbing micro-sphere material provided in an embodiment of the present invention introduces elastomer powder work in preparation process
Filler is buffered for structural mechanics.There is no need to increase gluing agent content, you can solve the low punching of sound absorption micro-sphere material generally existing
Hit tough sex chromosome mosaicism.Further, zeolite particles and elastomer powder can select the discarded molecule of the condition of satisfaction in this method
Sieve and industrial rubber, which are used as, to process raw material, therefore has certain environmentally friendly foreground.
Below in conjunction with specific embodiment, embodiment that the present invention will be described in detail provide sound-absorbing micro-sphere material preparation method and
The shock resistance of sound-absorbing micro-sphere material.
1, sound-absorbing micro-sphere material (embodiment 1-5) is prepared
Embodiment 1
1) by dry zeolite materials particle, (zeolite structured is FER, and micropore average pore size is about 0.49nm, particle diameter
About 2 μm) and full vulcanization butadiene-styrene rubber powder (particle diameter is about 400nm), Polystyrene-acrylate (adhesive) addition
Into aqueous solvent, at 500 rpm, mechanical agitation 2h obtains evenly dispersed mix suspending solution (also known as slurry).
Wherein, the addition quality of zeolite particles is the 25% of above-mentioned mix suspending solution gross mass；Full vulcanization butadiene-styrene rubber
The addition quality of powder particle is the 2.5% of above-mentioned mix suspending solution gross mass；The addition quality of Polystyrene-acrylate
It is the 2.5% of above-mentioned mix suspending solution gross mass.In aaerosol solution, solid masses is above-mentioned mix suspending solution gross mass
30%.
2) evenly dispersed mix suspending solution is added into spray-drying pelleting machine, spray-drying pelleting machine is set
Granulation is dried in 140~160 DEG C of inlet temperature, 100~110 DEG C of outlet temperature, atomisation pressure 0.5MPa, obtain tentatively at
Type particle.
3) above-mentioned preliminary shaped granule is heating and curing dry 1.5h in 120 DEG C of baking oven, obtains dry particle.
4) above-mentioned dry particle is sieved with 80~100 mesh screens and obtains the sound absorption microballoon material that grain size is about 150~180 μm
Material.
Embodiment 2：
1) by dry zeolite materials particle, (zeolite structured is FER, and micropore average pore size is about 0.49nm, particle diameter
About 2 μm) and full vulcanized acrylate rubber powder (particle diameter is about 250nm), Polystyrene-acrylate (adhesive)
It is added into aqueous solvent, at 500 rpm, mechanical agitation 2h obtains evenly dispersed mix suspending solution (also known as slurry).
Wherein, the addition quality of zeolite particles is the 30% of above-mentioned mix suspending solution gross mass；Full vulcanized acrylate
The addition quality of rubber powder particle is the 3% of above-mentioned mix suspending solution gross mass；The addition matter of Polystyrene-acrylate
Amount is the 3% of above-mentioned mix suspending solution gross mass.In aaerosol solution, solid masses is above-mentioned mix suspending solution gross mass
36%.
2) evenly dispersed mix suspending solution is added into spray-drying pelleting machine, spray-drying pelleting machine is set
Granulation is dried in 140~160 DEG C of inlet temperature, 100~110 DEG C of outlet temperature, atomisation pressure 0.4MPa, obtain tentatively at
Type particle.
3) above-mentioned preliminary shaped granule is heating and curing dry 1.5h in 120 DEG C of baking oven, obtains dry particle.
4) above-mentioned dry particle is sieved with 60~70 mesh screens and obtains the sound absorption microballoon material that grain size is about 220~250 μm
Material.
Embodiment 3：
1) by dry zeolite materials particle, (zeolite structured is MFI, and micropore average pore size is about 0.55nm, particle diameter
About 2 μm) and full-sulfurized nitrile rubber powder (particle diameter is about 350nm), polyurethane (adhesive) be added in aqueous solvent,
At 250rpm, mechanical agitation 4h obtains evenly dispersed mix suspending solution (also known as slurry).
Wherein, the addition quality of zeolite particles is the 35% of above-mentioned mix suspending solution gross mass；Full-sulfurized nitrile rubber
The addition quality of powder particle is the 2.5% of above-mentioned mix suspending solution gross mass；The addition quality of Polystyrene-acrylate
It is the 2.5% of above-mentioned mix suspending solution gross mass.In aaerosol solution, solid masses is above-mentioned mix suspending solution gross mass
40%.
2) evenly dispersed mix suspending solution is added into spray-drying pelleting machine, spray-drying pelleting machine is set
Granulation is dried in 140~160 DEG C of inlet temperature, 100~110 DEG C of outlet temperature, atomisation pressure 0.3MPa, obtain tentatively at
Type particle.
3) above-mentioned preliminary shaped granule is heating and curing dry 1h in 150 DEG C of baking oven, obtains dry particle.
4) above-mentioned dry particle is sieved with 40~45 mesh screens and obtains the sound absorption microballoon material that grain size is about 325~380 μm
Material.
Embodiment 4：
1) by dry zeolite materials particle, (zeolite structured is MFI, and micropore average pore size is about 0.55nm, particle diameter
About 3 μm) and vulcanization carboxyl acrylonitrile-butadiene rubber powder last (particle diameter is about 300nm), epoxy resin (adhesive) are added to molten entirely
In agent water, at 250rpm, mechanical agitation 4h obtains evenly dispersed mix suspending solution (also known as slurry).
Wherein, the addition quality of zeolite particles is the 30% of above-mentioned mix suspending solution gross mass；Full vulcanization carboxyl butyronitrile
The addition quality of rubber grain is the 3% of above-mentioned mix suspending solution gross mass；The addition quality of Polystyrene-acrylate is
The 2% of above-mentioned mix suspending solution gross mass.In aaerosol solution, solid masses is above-mentioned mix suspending solution gross mass 35%.
2) evenly dispersed mix suspending solution is added into spray-drying pelleting machine, spray-drying pelleting machine is set
Granulation is dried in 140~160 DEG C of inlet temperature, 100~110 DEG C of outlet temperature, atomisation pressure 0.35MPa, obtain tentatively at
Type particle.
3) above-mentioned preliminary shaped granule is heating and curing dry 1h in 150 DEG C of baking oven, obtains dry particle.
4) above-mentioned dry particle is sieved with 40~50 mesh screens and obtains the sound absorption microballoon material that grain size is about 270~325 μm
Material.
Embodiment 5：
1) by dry zeolite materials particle, (zeolite structured is MEL, and micropore average pore size is about 0.55nm, particle diameter
About 3 μm) and vulcanization butadiene rubber powder (particle diameter is about 250nm) Ludox (adhesive) is added to aqueous solvent entirely
In, at 500 rpm, mechanical agitation 2h obtains evenly dispersed mix suspending solution (also known as slurry).
Wherein, the addition quality of zeolite particles is the 25% of above-mentioned mix suspending solution gross mass；Full vulcanization butadiene rubber
The addition quality of glue particle is the 3.5% of above-mentioned mix suspending solution gross mass；The addition quality of Polystyrene-acrylate is
The 4.5% of above-mentioned mix suspending solution gross mass.In aaerosol solution, solid masses is above-mentioned mix suspending solution gross mass
33%.
2) evenly dispersed mix suspending solution is added into spray-drying pelleting machine, spray-drying pelleting machine is set
Granulation is dried in 140~160 DEG C of inlet temperature, 100~110 DEG C of outlet temperature, atomisation pressure 0.4MPa, obtain tentatively at
Type particle.
3) above-mentioned preliminary shaped granule is heating and curing dry 2h in 120 DEG C of baking oven, obtains dry particle.
4) above-mentioned dry particle is sieved with 60~70 mesh screens and obtains the sound absorption microballoon material that grain size is about 220~250 μm
Material.
2, control group embodiment
By embodiment 1-5 under identical preparation condition, rubber powder (elastomer powder) particle is not only added, is made respectively
It is standby to obtain 1 sound-absorbing micro-sphere material of comparative example corresponding with embodiment 1, comparative example 2 corresponding with embodiment 2 suction
Sound micro-sphere material, 3 sound-absorbing micro-sphere material of comparative example corresponding with embodiment 3, comparison corresponding with embodiment 4 are implemented
4 sound-absorbing micro-sphere material of example, 5 sound-absorbing micro-sphere material of comparative example corresponding with embodiment 5.
3, the comparative example 1-1 and 1-2 of embodiment 1
By embodiment 1 under identical preparation condition, change the addition quality and mix suspending solution of zeolite particles raw material
The proportioning of gross mass；Change the proportioning of the addition quality and mix suspending solution gross mass of full-sulfurized nitrile rubber powder particle；
The proportioning for changing the addition quality and mix suspending solution gross mass of Polystyrene-acrylate, obtains embodiment 1-1 and implementation
Example 1-2.
Wherein, in comparative example 1-1, the addition quality of zeolite particles is above-mentioned mix suspending solution gross mass
50%；The addition quality of full-sulfurized nitrile rubber powder particle is the 5% of above-mentioned mix suspending solution gross mass；Polystyrene-
The addition quality of acrylate is the 5% of above-mentioned mix suspending solution gross mass.In aaerosol solution, solid masses is above-mentioned mixing
Aaerosol solution gross mass 60%.
Wherein, in comparative example 1-2, the addition quality of zeolite particles is above-mentioned mix suspending solution gross mass
15%；The addition quality of full-sulfurized nitrile rubber powder particle is the 1.5% of above-mentioned mix suspending solution gross mass；Polyphenyl second
The addition quality of alkene-acrylate is the 1.5% of above-mentioned mix suspending solution gross mass.In aaerosol solution, solid masses is upper
State mix suspending solution gross mass 18%.
4, embodiment 1-5 shock resistances are tested
The sound absorption micro-sphere material that above-described embodiment 1-5 is prepared carries out fall-down test.The fall-down test is specific as follows：
1) the sound absorption micro-sphere material that 0.1g embodiments 1-5 is prepared is packed into Microspeaker back cavity as test specimen
In, wherein loud speaker back cavity volume is 1.0 cubic centimetres.
2) loud speaker is assembled in an aluminium alloy box, the size of aluminium alloy box is 150 × 75 × 10mm (to simulate
Use environment of the sound-absorbing granular materials in mobile phone)；The laboratory sample counterweight 150g fallen for each.
3) lift test specimen to 1500mm falling height (falling height refer to prepare release when sample minimum point with
Impact the distance between table top) position, and supported by predetermined state.Wherein, lift height and the difference of predetermined altitude
It must not exceed ± the 2% of predetermined altitude.
4) select the longest edge and the largest face of aluminium alloy box for drop test object；By one jiao, trigone and six faces it is predetermined
State is first fallen angle, then falls rib, after fall face and fall (angle, rib, face fall survey respectively be once one group of experiment), wherein falling
It is necessary to meet following condition when falling：
(a) when angle is fallen, the angle error on test specimen between predetermined surface and impact table top is not more than ± 5 ° or this folder
10% (be subject to bigger numerical) at angle, so that the gravity vertical of test specimen passes through the angle fallen；
(b) when rib falls, angle maximum between the rib and horizontal plane that fall is no more than 2 °, on test specimen predetermined surface with
The error of impact table top angle no more than ± 5 ° or this angle 10% (be subject to bigger numerical) so that the gravity of test specimen
Line passes through the rib that is fallen；
(c) when face is fallen, the angle maximum of test specimen fallen between face and horizontal plane is made to be no more than 2 °；So that experiment
The gravity vertical of sample passes through the face fallen；
(d) ± 1% when the difference of real impact speed and impact velocity when free-electron model is no more than free-electron model.
5, the shock resistance test of rubber powder particle control group is not added
Rubber powder particle comparative example will not be added, carries out shock resistance survey according to the method for above-mentioned steps respectively
Examination.
6, embodiment 1-5 resonant frequencies are tested
It is 1.0 vertical with loudspeaker enclosure tooling back cavity volume when the manufactured zeolite granular is applied in loudspeaker enclosure
For square centimetre, the zeolite granular size after molding and resonant frequency decreasing value.
7, the resonant frequency test of rubber powder particle control group is not added
By comparative example 1, comparative example 2, comparative example 3, comparative example 4 and comparative example 5, respectively
Resonant frequency test is carried out according to the method for above-mentioned steps.
8, to the resonance of each embodiment group sample and the control sample for not adding rubber powder particle after falling
Frequency decreasing value and the experimental result fallen are recorded, the record result table 1.
Table 1
9, sound-absorbing micro-sphere material made from embodiment 1 and its comparative example 1-1, comparative example 1-2 is carried out respectively
Morphology analysis, and resonant frequency decreasing value is carried out to it and drop test result records, the analysis and record result are as follows
Table.
Table 2
Based on test result shown in above table 1 and table 2, inventor is in the mistake developed to sound-absorbing micro-sphere material
It is found in journey：
In drop test, relative to comparative example 1-5, embodiment 1-5 can obtain complete microballoon, even if microballoon has
Institute is damaged also to only have a small amount of powder, not a large amount of broken, this explanation：Elastomer powder is introduced in preparation process as structural capacity
Buffering filler is learned, can solve the problems, such as low impact flexibility existing for sound absorption micro-sphere material.
In embodiment 1, when preparing mixing suspension (also known as slurry), to zeolite particles raw material, vulcanize butadiene-styrene rubber entirely
The additive amount of powder particle and Polystyrene-acrylate adhesive is optimized, and obtains the preferable sound absorber of microballoon pattern
Material, when which is applied to resonant frequency decreasing value and drop test analysis, relative contrast's embodiment 1-1 and comparison are implemented
Example 1-2 obtains preferable experimental result, this is because suspension mixed solid content asks that drying-granulating method obtains by spray is influenced
The microballoon pattern and microsphere particle heap density obtained.
Further, solid gross mass zeolite particles, elastomer powder and adhesive added in the present embodiment into
Row is preferred, and the solid gross mass that zeolite particles, elastomer powder and adhesive are added is suspension gross mass：25~
50%, this is because, it is contemplated that the granulating process of sound-absorbing microballoon, such as the preferred spray-drying process method of the present embodiment.Work as spray
When the atomizer part dimension of mist equipment has been fixed, solid content is bigger in suspension, then the viscosity of suspension is also bigger, mist
Change device to be more difficult to be atomized, made micro-sphere material particle will become inhomogenous, and product yield declines；In addition, containing admittedly in suspension
Amount is bigger, and the granular pile density of made micro-sphere material is bigger, although mechanical strength is promoted, specific surface area declines, acoustic efficiency
Decline.And suspension solid content is smaller, the granular pile density of made micro-sphere material is too small, and microballoon shape loosely has breakage, particle
It is less than normal, influence its mechanics impact resistance.
The present invention has carried out preferably the solid porose diameter of zeolite particles raw material, preferred zeolite particles it is a diameter of
0.4nm~0.6nm, why carry out preferably because, it is however generally that, Gu porose diameter is smaller, sound-absorbing efficiency is better.Due to
Sound is propagated by air vibration, and air main component is nitrogen, therefore the lower limit of the intrinsic bore dia of selected zeolite is by nitrogen
The kinetic diameter (about 0.36nm) of qi leel provides.Further, the gas of material is pliable also directly affects its sound absorption qualities, example
Such as the sound absorption qualities of the DDR zeolites of the bore dia with 0.44nm × 0.36nm since the pliable problem of gas is poor instead.Cause
This selects suitable channel diameter extremely important, is preferably 0.4nm~0.6nm in the present embodiment according to experimental result.
The present invention carries out preferably the stronger particle diameter of crosslinking-type rubber elasticity, and the particle of preferred crosslinking-type rubber is straight
Diameter be 50nm~500nm, why carry out preferably because：1, since crosslinking-type rubber elasticity is stronger, the smaller internal stress of particle
It is bigger, little particle rubber powder be easy to itself rupture cannot keep it is spherical, itself be difficult to synthesize and process.This outer rubber
Powder is too small, can also block the surface duct of zeolite materials particle, and the specific surface area for reducing micro-sphere material entirety is gentle pliable, right
Sound absorption qualities are unfavorable.2, rubber powder particle is bigger, and being just more difficult to be filled into zeolite particles, (particle diameter of zeolite particles raw material is
0.5~5 μm, preferably 1~3 μm.) gap in, the bulk density of micro-sphere material is promoted it is smaller, according to experimental result,
The mechanics impact resilience that its made micro-sphere material reflects is promoted also not notable.
Obviously, above-described embodiment is only intended to clearly illustrate example, and does not limit the embodiments.For
For those of ordinary skill in the art, other various forms of variations or change can also be made on the basis of the above description
It is dynamic.There is no necessity and possibility to exhaust all the enbodiments.And obvious variation extended from this or change
It is dynamic still within the protection scope of the invention.
Claims (10)
1. a kind of preparation method of sound-absorbing micro-sphere material, which is characterized in that include the following steps：
By zeolite particles, elastomer powder, adhesive and aqueous solvent stirring to obtain mix suspending solution, wherein the elastomer
The addition quality of powder is the 2%~4% of the mix suspending solution gross mass；
The mix suspending solution is granulated, sieves the sound absorption micro-sphere material for obtaining target grain size.
2. preparation method according to claim 1, which is characterized in that it is described the mix suspending solution is granulated,
Screening obtains the sound absorption micro-sphere material of target grain size, specifically includes：
The mix suspending solution is subjected to spray-drying process, obtains preliminary shaped granule；
By the preliminary shaped granule at 100~150 DEG C, dry 1~3h obtains dry particle；
The dry particle is obtained to the sound absorption micro-sphere material of target grain size using sieve screening.
3. preparation method according to claim 2, which is characterized in that the target grain size is 150~380 μm.
4. preparation method according to claim 1, which is characterized in that the addition quality of the elastomer powder is described mixed
Close the 2.5%~3.5% of aaerosol solution gross mass.
5. preparation method according to claim 1, which is characterized in that the particle diameter range of the zeolite particles raw material is
0.5~5 μm.
6. preparation method according to claim 5, which is characterized in that the particle diameter range of the zeolite particles raw material is
1~3 μm.
7. preparation method according to claim 1, which is characterized in that the elastomer powder is by following one or more
Crosslinking-type rubber is made：
Cross-linking type natural rubber, cross-linking type butadiene-styrene rubber, cross-linking type carboxylic styrene-butadiene rubber, cross-linking type polybutadiene rubber, crosslinking
Type nitrile rubber, cross-linking type carboxy nitrile rubber, cross-linking type neoprene, crosslinking acrylate rubber, cross-linking type silicon rubber
With cross-linking type butadiene-vinylpyridine rubber.
8. preparation method according to claim 1, which is characterized in that the particle diameter of the elastomer powder be 20nm~
2μm。
9. preparation method according to claim 8, which is characterized in that the particle diameter of the elastomer powder be 50nm~
500nm。
10. the sound-absorbing that a kind of preparation method of sound-absorbing micro-sphere material of application as described in claim 1-9 is any is prepared is micro-
Ball material.
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