CN106750386B - A kind of noise reduction particle and the preparation method and application thereof - Google Patents

A kind of noise reduction particle and the preparation method and application thereof Download PDF

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Publication number
CN106750386B
CN106750386B CN201611190724.2A CN201611190724A CN106750386B CN 106750386 B CN106750386 B CN 106750386B CN 201611190724 A CN201611190724 A CN 201611190724A CN 106750386 B CN106750386 B CN 106750386B
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reagent
particle
reagent solution
noise reduction
photoinitiator
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CN106750386A (en
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王焱华
贺晓宁
冯玉林
张丽
于法猛
杨波
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Shenzhen Mofang Materials Technology Co.,Ltd.
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Shenzhen Mopha Mstar Technology Ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/12—Powdering or granulating
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/20—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the epoxy compounds used
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/20—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the epoxy compounds used
    • C08G59/22—Di-epoxy compounds
    • C08G59/24—Di-epoxy compounds carbocyclic
    • 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
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/28—Treatment by wave energy or particle radiation
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D127/00—Coating compositions based on 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; Coating compositions based on derivatives of such polymers
    • C09D127/02—Coating compositions based on 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; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
    • C09D127/04—Coating compositions based on 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; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
    • C09D127/06—Homopolymers or copolymers of vinyl chloride
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D133/00—Coating compositions based on 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 only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
    • C09D175/04—Polyurethanes
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D195/00—Coating compositions based on bituminous materials, e.g. asphalt, tar, pitch
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/65—Additives macromolecular
    • 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
    • C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins

Abstract

The present invention provides a kind of noise reduction particle and the preparation method and application thereof, including one of or several in reagent A, reagent B and reagent C, by weight percentage, the reagent A, reagent B and reagent C include 94-99% epoxy resin quasi-oligomer, 0.5-3% photoinitiator, 0.5-4% defoaming agent.The preparation method of noise reduction particle provided by the invention can be by the size (10-500um) of the diameter control of particle to very little, and particle size is uniform.The magnitude that the density of noise reduction particle can control very little (is less than 0.5g/cm3), compared to antidrumming compound functional stuffing traditional at present, noise reduction particle of the invention can achieve light-weighted feature.

Description

A kind of noise reduction particle and the preparation method and application thereof
Technical field
The invention belongs to technical field of function materials, and in particular to a kind of noise reduction particle and the preparation method and application thereof.
Background technique
At present in antidrumming compound and damping vibration attenuation coating application field, the main component of general coating includes matrix, filling Material, coupling agent and some adjuvants.At present in automobile and rail traffic noise reduction application aspect, the material of matrix is generally comprised Pitch, PVC, acrylic acid, polyurethane etc..Packing material has a significant impact to the performance of damping antidrumming compound, including improves damping Value improves sound-absorbing effect, changes glass transition temperature, reduces cost etc..Current packing material generally comprises mica, titanium dioxide Titanium, glass microballoon, carbon fiber, glass fibre, carbon nanotube etc..
For packing material, currently used inorganic filling material has the following problems or defect: 1, the shape of filler Shape and partial size are uneven, and noise reduction or damping vibration attenuation effect is caused to be difficult to reach optimum efficiency.2, preparation cost is high, current filler Chemical synthesis or other forming methods are generally used, process flow is complicated.3, the general density of current filler is larger, it is difficult to meet Automobile, the light-weighted growth requirement of rail traffic.
Summary of the invention
To solve the above problem existing for packing material, the present invention proposes a kind of noise reduction particle as packing material, this disappears Sound particle has accurate size controllable, the whole erasure effect effect of being greatly improved to antidrumming compound, while the noise reduction grain Sub- preparation method is simple, and manufacturing cost is low, can be widely applied in automobile or the antidrumming compound of field of track traffic.
Specifically, a kind of noise reduction particle, including reagent solution, the reagent solution is using in reagent A, reagent B and reagent C One of or several, by weight percentage, the reagent A, reagent B and reagent C include that 94-99% epoxy resin is low Polymers, 0.5-3% photoinitiator, 0.5-4% defoaming agent.
As shown in Figure 1, noise reduction particle: the research mechanism of antidrumming compound or quieter material shows to improve antidrumming compound Or the sound absorption qualities of quieter material, particle (medicine ball, spiral shape particle, the solid wall sky of suitable shape can be added in the material Bulbus cordis, column shell) composite material that is formed, particle has the contribution of sound attenuating: a. Particles Moving under the action of sound wave generates Spilehole makes material deformation generate heat, thus the sound energy for the particle that dissipates.B. KPT Scatter, when the diameter and sound wave of particle In the same order of magnitude, Mie scattering occurs wavelength for sound wave, and when the diameter of particle is much smaller than the wavelength of sound wave, sound wave occurs Rayleigh scattering, due to the effect of scattering, thus it is possible to vary acoustic wave propagation path enables reflection direction sound to weaken.C. KPT Scatter makes to damage Low wave mode (longitudinal wave) is consumed to high wave mode (shear wave) conversion is lost, and is improved the modulus of shearing of material, is reinforced to acoustic wave energy Decaying.
Preferably, the epoxy resin quasi-oligomer uses 3,4- epoxycyclohexyl-methyl -3,4- epoxycyclohexyl carbonic acid One of rouge, bisphenol A epoxide resin, bis- (7- oxabicyclo (4.1.0) 3- methyl in heptan) adipate esters are several.
Preferably, the photoinitiator uses sulfosalt photoinitiator Omnicat432, sulfosalt photoinitiator One of Omnicat320 and sulfosalt photoinitiator Omnicat550 are several.
Preferably, the defoaming agent is using one of BYK088, BYK307 and BYK501.
Specific formula is as follows, by weight percentage:
Reagent A: (1) epoxy resin quasi-oligomer: 3,4- epoxycyclohexyl-methyl -3,4- epoxycyclohexyl carbonic ether (95- 99%)
(2) photoinitiator: sulfosalt photoinitiator Omnicat432 (0.5-2.5%)
(3) defoaming agent: BYK088 (0.5-2.5%)
Reagent B:(1) epoxy resin quasi-oligomer: bisphenol A epoxide resin (95-99%)
(2) photoinitiator: sulfosalt photoinitiator Omnicat320 (0.5-3%)
(3) defoaming agent: BYK307 (0.5-2%)
Reagent C: (1) epoxy resin quasi-oligomer: bis- (7- oxabicyclo (4.1.0) 3- methyl in heptan) adipate ester (94- 99%)
(2) photoinitiator: sulfosalt photoinitiator Omnicat550 (0.5-2%)
(3) defoaming agent: BYK501 (0.5-4%)
The present invention also provides a kind of method for preparing the noise reduction particle, including the following steps:
Step (1): reagent preparation: epoxy resin quasi-oligomer, photoinitiator and defoaming agent are poured into beaker, and stirring is equal It is even；
Step (2): reagent solution push is flowed out into container and forms drop, illumination simultaneously solidifies；
Step (3): after particle former, the particle after dispersion is gone out by air-flow, is ejected into the structure for needing sprayed coating Fixing on part and on structural member after basis material mixing becomes muffle coating.
Preferably, in the step (2), the pressure of push is 0.01-0.6MPa；The flow of reagent solution is 0.001- 0.1mL/s。
Preferably, in the step (2), it is 0.01-15mj/ that when illumination, which launches the energy density range of radiation energy, cm2, light source exposure time range is 0.1-5s；Optical source wavelength range is 355-445nm；
The invention adopts the above technical scheme, the advantage is that, flows out to container by the pressure push of air pressure and forms liquid Drop, the Pressure generator are air compressor, and pressure limit is 0.01-0.6MPa, while light source irradiates droplet formation grain The sequencing of son, the ratio and outflow that change reagent can form the functional particles of different core-shell structures.The size of particle (optical source wavelength range is 365-445nm) is controlled by changing reagent A, the flow of B, C and light source irradiation time, flow is big Small range is 0.001-0.1mL/s, and light application time range is 0.1-5s.After the completion of particle morphology, in the left side of shown container Particle transfer to commitment positions and substrate are subjected to fusion by air-flow, antidrumming compound is made, the container is particle formation The place of reaction, generally circle test tube made of glass are provided.The commitment positions are after particle as shown in Figure 2 generates Placement or storage location.The particle that the present invention produces preparation, which is added to inside substrate, improves erasure effect.
Preferably, in the step (2), the container in the step (2) uses round tubular, diameter 0.01mm- 1mm, there is water and ethyl alcohol in container, and the volume ratio of water and ethyl alcohol is 1:1, the weight ratio range of the total amount and reagent of water and ethyl alcohol It is 3:1~6:1.
Preferably, in the step (2), in the step (3), described matrix material using pitch, PVC, acrylic acid and At least one of polyurethane.
The present invention also provides application of the noise reduction particle on quieter material.
The present invention further uses the above technical characteristic, the advantage is that, works as reagent A, and B, one or more of C are flowed into After container, the size of outlet is controlled, exports to be round tubular that (radius r), diameter 2*r magnitude range is 0.01mm-1mm.Make The solution of outflow forms drop, and drop becomes spherical under the action of surface tension, and such spherical drop is dispersed in a reservoir, It is full of ethyl alcohol or water in container, floats drop in a reservoir, and the liquid (water or ethyl alcohol) in container of getting along well occurs It chemically reacts or dissolves each other.After droplet formation, light source launches the radiation energy of some strength, makes the surface cure of drop, shape At the spheroidal particle of core-shell structure, energy density range is 0-15mj/cm2.The mechanism of action of light source irradiation is to make drop Gelation or liquid-solid phase transformation.Since the size of the particle of formation can be controlled by controlling flow velocity and the outlet size of reagent, The cured thickness of droplet surface can be controlled by controlling intensity and the time of illumination, so noise reduction particle provided by the invention Preparation method can be by the size (10-500um) of the diameter control of particle to very little.The density of noise reduction particle can control The magnitude of very little (is less than 0.5g/cm3), compared to antidrumming compound functional stuffing traditional at present, noise reduction particle of the invention can To reach light-weighted feature.
Detailed description of the invention
Fig. 1 is the structure chart of noise reduction particle.
Fig. 2 is the preparation technology flow chart of noise reduction particle.
Fig. 3 is the sound transmission loss test effect of embodiment 4 from the damping paint piece of various different fillers.
Fig. 4 is that noise reduction particle prepared by embodiment 4 tests its grain size distribution using dynamic light scattering method (DLS).
Specific embodiment
Preferably embodiment of the invention is described in further detail below:
Embodiment 1
(1) prepared by reagent, carries out sample preparation to reagent A, sample preparation step be at room temperature first by epoxy resin quasi-oligomer 3, 4- epoxycyclohexyl-methyl -3,4- epoxycyclohexyl carbonic ether (95%), photoinitiator Omnicat432 (2.5%), defoaming agent BYK088 (2.5%) is poured into beaker, and mechanical stirring 5 minutes.
(2) reagent droplet is expressed into container by 0.5MPa pressure, modulates the flow of reagent A for 0.001mL/s, in container There are water and ethyl alcohol, the volume ratio of water and ethyl alcohol is 1:1, and the weight ratio of the total amount and reagent A of water and ethyl alcohol is 3:1.
(3) select the radiation of light source time for 3s, radiation of light source energy density 3mj/cm2。
(4) it is dispersed in solution after particle a molding.
(5) particle after dispersing is gone out by air-flow, is ejected on the structural member for needing sprayed coating and basis material mixes It is fixed on structural member afterwards to become muffle coating.
Embodiment 2
(1) prepared by reagent, carries out sample preparation to reagent B, sample preparation step is first that epoxy resin quasi-oligomer is double at room temperature Phenol A epoxy resin (95%), photoinitiator Omnicat320 (3%), defoaming agent BYK307 (2%) are poured into beaker, mechanical stirring 5 Minute.
(2) reagent droplet is expressed into container by 0.6MPa pressure, and the flow of modulation reagent B is 0.002mL/s；In container There are water and ethyl alcohol, the volume ratio of water and ethyl alcohol is 1:1, and the weight ratio of the total amount and reagent of water and ethyl alcohol is 6:1.
(3) select the radiation of light source time for 2s, radiation of light source energy density 7mj/cm2。
(4) it is dispersed in solution after particle b molding.
(5) particle after dispersing is gone out by air-flow, is ejected on the structural member for needing sprayed coating and basis material mixes It is fixed on structural member afterwards to become muffle coating.
Embodiment 3
(1) prepared by reagent, carries out sample preparation to reagent C, sample preparation step is first that epoxy resin quasi-oligomer is double at room temperature (7- oxabicyclo (4.1.0) 3- methyl in heptan) adipate ester (94%), photoinitiator Omnicat550 (2%), defoaming agent BYK501 (4%) it pours into beaker, mechanical stirring 5 minutes.
(2) reagent droplet is expressed into container by 0.01MPa pressure, modulates the flow of reagent B for 0.1mL/s, in container There are water and ethyl alcohol, the volume ratio of water and ethyl alcohol is 1:1, and the weight ratio of the total amount and reagent of water and ethyl alcohol is 4:1.
(3) select the radiation of light source time for 5s, radiation of light source energy density 15mj/cm2。
(4) it is dispersed in solution after particle c molding.
(5) particle after dispersing is gone out by air-flow, is ejected on the structural member for needing sprayed coating and basis material mixes It is fixed on structural member afterwards to become muffle coating.
Embodiment 4
(1) prepared by reagent, and to A, two kinds of reagents of B carry out sample preparation, and by weight percentage, reagent A is low using epoxy resin Polymers 3,4- epoxycyclohexyl-methyl -3,4- epoxycyclohexyl carbonic ether (99%), photoinitiator Omnicat432 (0.5%) disappear Infusion BYK088 (0.5%)；Reagent B uses epoxy resin quasi-oligomer bisphenol A epoxide resin (99%), photoinitiator Omnicat320 (0.5%), the ratio of defoaming agent BYK307 (0.5%), sample preparation step are first that epoxy resin is low at room temperature Polymers, photoinitiator, defoaming agent pour into beaker, mechanical stirring 5 minutes, prepare reagent A and reagent B respectively.
(2) reagent droplet is expressed into container by 0.2MPa pressure, and the flow for modulating reagent A is 0.005mL/s；In container There are water and ethyl alcohol, the volume ratio of water and ethyl alcohol is 1:1, and the weight ratio of the total amount and reagent of water and ethyl alcohol is 5:1.
(3) select the radiation of light source time for 0.1s, radiation of light source energy density 10mj/cm2。
(4) it is dispersed in solution after particle a molding.
(5) flow for modulating reagent B is 0.002mL/s, and the radiation of light source time is 0.05s, and radiation of light source energy density is 12mj/cm2
(6) it is dispersed in solution after particle d molding, particle d is core-shell structure, and core is particle a, and shell is reagent B solidification The shell formed afterwards.
(7) particle after dispersing is gone out by air-flow, is ejected on the structural member for needing sprayed coating and basis material mixes It is fixed on structural member afterwards to become muffle coating.
Step 4 is the arrangement for other two kinds of reagents the step of forming core-shell structure particle using two kinds of reagents of A, B It is similar to combine the step of (BA, AC, CA, BC, CB etc.) forms core-shell structure particle, can also prepare the core-shell structure grain of corresponding construction Son.
Embodiment 5
(1) prepared by reagent, and to A, tri- kinds of reagents of B, C carry out sample preparation, and by weight percentage, reagent A uses epoxy resin Oligomer 3,4- epoxycyclohexyl-methyl -3,4- epoxycyclohexyl carbonic ether (98%), photoinitiator Omnicat432 (1.5%), Defoaming agent BYK088 (1.5%)；Reagent B uses epoxy resin quasi-oligomer bisphenol A epoxide resin (97%), photoinitiator Omnicat320 (2%), defoaming agent BYK307 (1%)；Reagent C uses bis- (the 7- oxabicyclos (4.1.0) of epoxy resin quasi-oligomer 3- methyl in heptan) adipate ester (99%), photoinitiator Omnicat550 (0.5%), defoaming agent BYK501 (0.5%), sample preparation step is At room temperature first by epoxy resin quasi-oligomer, photoinitiator, defoaming agent is poured into beaker, mechanical stirring 5 minutes, is prepared respectively Reagent A, reagent B and reagent C out.
(2) reagent droplet is expressed into container by 0.4MPa pressure, modulates the flow of reagent A for 0.003mL/s, in container There are water and ethyl alcohol, the volume ratio of water and ethyl alcohol is 1:1, and the weight ratio of the total amount and reagent of water and ethyl alcohol is 6:1.
(3) select the radiation of light source time for 0.1s, radiation of light source energy density 4mj/cm2。
(4) it is dispersed in solution after particle a molding.
(5) flow for modulating reagent B is 0.008mL/s, and the radiation of light source time is 0.05s, and radiation of light source energy density is 7mj/cm2
(6) it is dispersed in solution after particle d molding, particle d is core-shell structure, and core is particle a, and shell is reagent B solidification The shell formed afterwards.
(7) flow for modulating reagent C is 0.006mL/s, and the radiation of light source time is 0.05s, and radiation of light source energy density is 5mj/cm2；
(8) it is dispersed in solution after particle e molding, particle e is three-layer nuclear shell structure, and core is the d of particle core-shell structure Particle, shell are the shell formed after reagent C solidifies.
(9) particle after dispersing is gone out by air-flow, is ejected on the structural member for needing sprayed coating and basis material mixes It is fixed on structural member afterwards to become muffle coating.
Step 5 is the step of forming core-shell structure particle using tri- kinds of reagents of A, B, C, for the row of other three kinds of reagents The step of column combination (ACB, BAC, BCA, CAB, CBA etc.) formation core-shell structure particle, is similar, can also prepare the core of corresponding construction Shell structure particle.
Embodiment 6
It is in noise reduction and noise reduction application field, noise reduction prepared by embodiment 1-5 is particle-filled to inside coating matrix, disappear Sound particle specific gravity by weight is 10%, and sheet coating is made and tests its soundproof effect.The ingredient at paint-based bottom is by weight percentage Are as follows: 1. 25% styrene acrylic emulsion, 2. 25% silicone acrylic emulsion, 3. 30% acrylic emulsion, 4. 10% water.
The preparation step of coating are as follows:
(1) by coating base material 1. -4. with noise reduction particle at room temperature, mixed in beaker, stirring 5min make its It is even.
(2) by the coating spray gun spraying mixed on aluminum base plate, spraying with a thickness of 2mm.
(3) sample is placed and is toasted 2 hours in an oven, temperature is 60 DEG C.
(4) coating sample is solidified into damping fin.
(5) step (1)-(4) are repeated, by same amount of glass microballoon, mica sheet, glass fibre is filled into paint-based respectively Body, and prepare corresponding damping paint piece.
Test sound insulation value step:
(1) the various damping paint pieces of above-mentioned preparation are cut into the disk that diameter is 30mm.
(2) disk that above-mentioned diameter is 30mm is placed in B & K4206 type impedance tube, using four microphones, is used Transfer function method tests its sound transmission loss, and test frequency range is 500-6400Hz.
(3) after the completion of testing, data comparison, analysis are carried out.
As shown in figure 3, testing the sound transmission loss number of the damping paint piece of various different fillers within the scope of 500-6400Hz The particle-filled damping paint piece of the noise reduction prepared according to four that, 3# is step of the present invention, in dosage (chymoplasm under the same conditions It measures ratio 10%), is filled into the antidrumming compound substrate of same thickness (2mm), with other types of filler, 2# glass microballoon, 1# cloud Master slice, 4# glass fibre etc. are compared, and sound transmission loss significantly improves.
In order to characterize the feature of uniform size of noise reduction particle, the noise reduction particle of four preparations of step is dissipated using dynamic optical Shooting method (DLS) tests its grain size distribution, as shown in figure 4, from the point of view of DLS grain size distribution, the noise reduction particle diameter of preparation It is substantially distributed in 23-27 μm, and particle distribution is uniform.
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that Specific implementation of the invention is only limited to these instructions.For those of ordinary skill in the art to which the present invention belongs, exist Under the premise of not departing from present inventive concept, a number of simple deductions or replacements can also be made, all shall be regarded as belonging to of the invention Protection scope.

Claims (5)

1. a kind of method for preparing noise reduction particle, which is characterized in that the raw material of the noise reduction particle includes reagent solution A, reagent solution B With it is one of or several in reagent solution C, by weight percentage, the reagent solution A, reagent solution B and reagent solution C include 94-99% epoxy resin quasi-oligomer, 0.5-3% photoinitiator, 0.5-4% defoaming agent；
The method includes following steps:
Step (1): reagent solution preparation: epoxy resin quasi-oligomer, photoinitiator and defoaming agent are poured into beaker, and stirring is equal It is even, form reagent solution A, reagent solution B and reagent solution C；
Step (2): reagent solution push is flowed out into container and forms drop, illumination simultaneously solidifies；
In the step (2), the pressure of push is 0.01-0.6MPa；The flow of reagent solution is 0.001-0.1mL/s；When illumination The energy density range for launching radiation energy is 0-15mj/cm2, light source exposure time range is 0-5s；Optical source wavelength range It is 355-445nm；Container uses round tubular, diameter 0.01mm-1mm, has at least one of water or ethyl alcohol in container.
2. the method as described in claim 1, which is characterized in that the epoxy resin quasi-oligomer uses 3,4- epoxycyclohexyl Methyl -3,4- epoxycyclohexyl carbonic ether, bisphenol A epoxide resin, bis- (7- oxabicyclo (4.1.0) 3- methyl in heptan) adipate esters One of or it is several.
3. the method as described in claim 1, which is characterized in that the photoinitiator uses sulfosalt photoinitiator One of Omnicat432, sulfosalt photoinitiator Omnicat320 and sulfosalt photoinitiator Omnicat550 or Person is several.
4. the method as described in claim 1, which is characterized in that the defoaming agent is using in BYK088, BYK307 and BYK501 One kind.
5. noise reduction particle as described in claim 1 is preparing the application on quieter material.
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EP0407157A2 (en) * 1989-07-03 1991-01-09 Mitsui Petrochemical Industries, Ltd. Vibration-damping material
WO1999016840A1 (en) * 1997-09-26 1999-04-08 The Dow Chemical Company Flexible epoxy sound damping coatings
EP1500690A1 (en) * 2003-07-24 2005-01-26 PPG Industries Ohio, Inc. Composition having sealing and sound dampening properties and methods related thereto
CN101253243A (en) * 2005-10-28 2008-08-27 赢创罗姆有限责任公司 Sprayable acoustic compositions
CN102134412A (en) * 2011-03-02 2011-07-27 武汉理工大学 Damping vibration-attenuating noise-reducing coating material used under hot environment
CN103806552A (en) * 2013-12-31 2014-05-21 李�杰 Method for producing sound absorbing plates
CN105199322A (en) * 2015-10-10 2015-12-30 苏州大学 Epoxy resin microsphere and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0407157A2 (en) * 1989-07-03 1991-01-09 Mitsui Petrochemical Industries, Ltd. Vibration-damping material
WO1999016840A1 (en) * 1997-09-26 1999-04-08 The Dow Chemical Company Flexible epoxy sound damping coatings
EP1500690A1 (en) * 2003-07-24 2005-01-26 PPG Industries Ohio, Inc. Composition having sealing and sound dampening properties and methods related thereto
CN101253243A (en) * 2005-10-28 2008-08-27 赢创罗姆有限责任公司 Sprayable acoustic compositions
CN102134412A (en) * 2011-03-02 2011-07-27 武汉理工大学 Damping vibration-attenuating noise-reducing coating material used under hot environment
CN103806552A (en) * 2013-12-31 2014-05-21 李�杰 Method for producing sound absorbing plates
CN105199322A (en) * 2015-10-10 2015-12-30 苏州大学 Epoxy resin microsphere and preparation method thereof

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