WO2017092243A1 - 介孔吸音材料颗粒的制备方法和介孔吸音材料颗粒 - Google Patents

介孔吸音材料颗粒的制备方法和介孔吸音材料颗粒 Download PDF

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WO2017092243A1
WO2017092243A1 PCT/CN2016/082475 CN2016082475W WO2017092243A1 WO 2017092243 A1 WO2017092243 A1 WO 2017092243A1 CN 2016082475 W CN2016082475 W CN 2016082475W WO 2017092243 A1 WO2017092243 A1 WO 2017092243A1
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absorbing material
sound absorbing
mesoporous
material particles
particles
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English (en)
French (fr)
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曹晓东
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Goertek Inc
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Goertek Inc
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Priority to US15/781,297 priority Critical patent/US11028023B2/en
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
    • C04B38/063—Preparing or treating the raw materials individually or as batches
    • C04B38/0635—Compounding ingredients
    • C04B38/0645—Burnable, meltable, sublimable materials
    • C04B38/067—Macromolecular compounds
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/0045—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by a process involving the formation of a sol or a gel, e.g. sol-gel or precipitation processes
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/0051—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof characterised by the pore size, pore shape or kind of porosity
    • C04B38/0054—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof characterised by the pore size, pore shape or kind of porosity the pores being microsized or nanosized
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/0067—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof characterised by the density of the end product
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/007—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof characterised by the pore distribution, e.g. inhomogeneous distribution of pores
    • C04B38/0074—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof characterised by the pore distribution, e.g. inhomogeneous distribution of pores expressed as porosity percentage
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/009—Porous or hollow ceramic granular materials, e.g. microballoons
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
    • C04B38/0615—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances the burned-out substance being a monolitic element having approximately the same dimensions as the final article, e.g. a porous polyurethane sheet or a prepreg obtained by bonding together resin particles
    • C04B38/062—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances the burned-out substance being a monolitic element having approximately the same dimensions as the final article, e.g. a porous polyurethane sheet or a prepreg obtained by bonding together resin particles the burned-out substance being formed in situ, e.g. by polymerisation of a prepolymer composition containing ceramic powder
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
    • C04B38/063—Preparing or treating the raw materials individually or as batches
    • C04B38/0635—Compounding ingredients
    • C04B38/0645—Burnable, meltable, sublimable materials
    • G—PHYSICS
    • G10—MUSICAL INSTRUMENTS; ACOUSTICS
    • G10K—SOUND-PRODUCING DEVICES; METHODS OR DEVICES FOR PROTECTING AGAINST, OR FOR DAMPING, NOISE OR OTHER ACOUSTIC WAVES IN GENERAL; ACOUSTICS NOT OTHERWISE PROVIDED FOR
    • G10K11/00—Methods or devices for transmitting, conducting or directing sound in general; Methods or devices for protecting against, or for damping, noise or other acoustic waves in general
    • G10K11/16—Methods or devices for protecting against, or for damping, noise or other acoustic waves in general
    • G10K11/162—Selection of materials
    • G—PHYSICS
    • G10—MUSICAL INSTRUMENTS; ACOUSTICS
    • G10K—SOUND-PRODUCING DEVICES; METHODS OR DEVICES FOR PROTECTING AGAINST, OR FOR DAMPING, NOISE OR OTHER ACOUSTIC WAVES IN GENERAL; ACOUSTICS NOT OTHERWISE PROVIDED FOR
    • G10K11/00—Methods or devices for transmitting, conducting or directing sound in general; Methods or devices for protecting against, or for damping, noise or other acoustic waves in general
    • G10K11/16—Methods or devices for protecting against, or for damping, noise or other acoustic waves in general
    • G10K11/162—Selection of materials
    • G10K11/165—Particles in a matrix
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/52—Sound-insulating materials
    • H—ELECTRICITY
    • H04—ELECTRIC COMMUNICATION TECHNIQUE
    • H04R—LOUDSPEAKERS, MICROPHONES, GRAMOPHONE PICK-UPS OR LIKE ACOUSTIC ELECTROMECHANICAL TRANSDUCERS; ELECTRIC HEARING AIDS; PUBLIC ADDRESS SYSTEMS
    • H04R1/00—Details of transducers, loudspeakers or microphones
    • H04R1/20—Arrangements for obtaining desired frequency or directional characteristics
    • H04R1/22—Arrangements for obtaining desired frequency or directional characteristics for obtaining desired frequency characteristic only 
    • H04R1/28—Transducer mountings or enclosures modified by provision of mechanical or acoustic impedances, e.g. resonator, damping means
    • H04R1/2869—Reduction of undesired resonances, i.e. standing waves within enclosure, or of undesired vibrations, i.e. of the enclosure itself
    • H04R1/2876—Reduction of undesired resonances, i.e. standing waves within enclosure, or of undesired vibrations, i.e. of the enclosure itself by means of damping material, e.g. as cladding
    • H04R1/288—Reduction of undesired resonances, i.e. standing waves within enclosure, or of undesired vibrations, i.e. of the enclosure itself by means of damping material, e.g. as cladding for loudspeaker transducers

Definitions

  • the invention belongs to the technical field of material processing, and in particular to a method for preparing mesoporous sound absorbing material particles and a mesoporous sound absorbing material particle.
  • the granulation method usually employed does not fully exert the performance of such non-foaming sound absorbing materials.
  • the preparation methods used by those skilled in the art include extrusion, boiling granulation, rolling into a ball, and the like.
  • the inventors of the present invention have found through actual use and testing that the strength of the particles obtained by the extrusion method, the boiling granulation method, and the rolling ball method is relatively poor, the surface is not smooth, the particle size is uneven, and the physical structure and properties are limited.
  • the limitation of the resulting sound absorbing material particles has a limited sound absorption effect and affects the flow of air in the rear cavity of the speaker.
  • the particles formed by the spray drying method are relatively small, and the particle size distribution is uneven, and the sound absorbing effect is not as expected. Therefore, the inventors of the present invention believe that the existing sound absorbing material particles are filled into the rear acoustic cavity of the speaker structure, causing two problems. First, the air flow in the rear cavity is hindered, so that the sensitivity of the speaker is lowered, and the cavity is lowered. The generated negative pressure affects the normal operation of the speaker diaphragm. Second, the sound absorbing material particles have limited sound absorption and room for improvement.
  • the structure is improved, the number of holes is increased, the sound absorption effect of the material is improved, and the sound absorbing material particles are prevented from reducing the smoothness of the air in and out of the rear cavity of the speaker.
  • a method of preparing a mesoporous sound absorbing material particle comprising:
  • Step 1 mixing the sound absorbing material powder, the templating agent with the binder and water to form a sol slurry, the templating agent is an organic monomer or a linear polymer, the templating agent has a purity greater than 95%;
  • Step 2 the sol slurry is dropped into a molding oil, and droplets of the sol slurry are aged in the molding oil to form gel particles;
  • Step 3 taking the gel particles from the molding oil, drying the gel particles to form mesoporous sound absorbing material particles;
  • Step 4 Roasting the mesoporous sound absorbing material particles.
  • the templating agent is added in an amount of 1% to 35% of the total mass of the sol slurry.
  • the binder is added in an amount of 1% to 35% by weight of the total mass of the sol slurry, and the binder is a silicone sol or a fibrous resin.
  • an auxiliary agent is added to the sol slurry, and the auxiliary agent is added in an amount of 0.02% to 10% by mass of the total mass of the sol slurry, and the auxiliary agent is Defoamer, accelerator or homogenizer.
  • the temperature of the molding oil ranges from 40 to 120 ° C, and the molding oil is white lubricating oil, stator oil, machine tool oil or vacuum pump oil.
  • the gel particles are dried in an inert gas having a temperature in the range of 40 to 150 °C.
  • the temperature during calcination ranges from 120 to 850 ° C
  • the heating rate of calcination ranges from 20 to 120 ° C/h
  • the calcination time ranges from 0.5 to 96 h.
  • the content of oxygen in the firing atmosphere is from 0.1% to 21%.
  • the present invention also provides a mesoporous sound absorbing material particle having a specific surface area in the range of 250-650 m 2 /g and a pore volume of 0.2-2.0 ml/g in the mesoporous sound absorbing material particle.
  • the mesoporous pore volume having a pore diameter of 0.5 to 35 ⁇ m accounts for 15% to 85% of the total pore volume.
  • the mesoporous sound absorbing material particles have a diameter ranging from 0.05 to 1.0 mm and a bulk density ranging from 0.25 to 0.95 g/ml.
  • the inventors of the present invention have found that those skilled in the art will generally prepare the sound absorbing material particles by the prior art methods described in the background art, and directly use the particles produced by these means, without exploring new molding processes or improving the particles. Structural characteristics. That is to say, those skilled in the art are not aware of the problems existing in the prior non-foaming sound absorbing material particles during use. Therefore, the technical task to be achieved by the present invention or the technical problem to be solved is not thought of or expected by those skilled in the art, so the present invention is a new technical solution.
  • FIG. 1 is a block diagram showing the steps of a method for preparing mesoporous sound absorbing material particles provided by the present invention.
  • the invention provides a preparation method of mesoporous sound absorbing material particles, which comprises:
  • Step 1 mixing the sound absorbing material powder, the templating agent with the binder and water to form a sol slurry, the templating agent is an organic monomer or a linear polymer, the templating agent has a purity greater than 95%;
  • the sol slurry is dropped into a molding oil, and droplets of the sol slurry are aged in the molding oil to form gel particles; and step 3, the gel particles are taken out from the molding oil, The gel particles are dried to form mesoporous sound absorbing material particles; and step 4, the mesoporous sound absorbing material particles are calcined.
  • the preparation method provided by the present invention is an oil column molding method.
  • step 1 the sound absorbing material powder is mixed with a binder and water to form a sol-like sol slurry.
  • the templating agent serves to provide a structural framework for the body crystallization of the sound absorbing material powder to perform structural guiding.
  • the sound absorbing material can be directed to form a different crystal structure.
  • the templating agent Since it is finally required to form mesoporous sound absorbing material particles, the templating agent needs to be able to fabricate a large number of mesoporous structures in the mesoporous sound absorbing material particles to improve the sound absorbing effect and air fluency.
  • the templating agent is an organic monomer or a linear polymer, and the purity is greater than 95%, so that the templating agent can function in a subsequent step to form a large amount of mesoporous structure when the sound absorbing material is recrystallized. .
  • the templating agent is added in a ratio of between 1% and 35% of the total mass of the sol slurry, and if the amount of the templating agent is too high, the prepared mesopores may be caused.
  • the structure of the sound absorbing material is unstable and the strength is low. If the amount of the templating agent is too low, the mesoporous sound absorbing material particles may have a small pore structure and a small number of micropores, and the sound absorbing effect is poor.
  • a person skilled in the art can appropriately adjust the amount of the template agent according to actual conditions, so that the prepared mesopores can be made.
  • the sound absorbing material particles are matched to the speaker structure to maximize the sound absorbing effect.
  • the mass ratio of the binder in the sol slurry should be between 1% and 35%, and if the proportion of the binder is too high, The prepared mesoporous sound absorbing material has a too tight grain structure, resulting in poor sound absorbing effect. Conversely, if the proportion of the binder is too low, the mesoporous sound absorbing material particles eventually fail to solidify into a ball.
  • the mass ratio of the binder in the sol slurry should be matched to the mass ratio of the templating agent, and those skilled in the art can formulate according to actual conditions.
  • the binder may be a material such as silica, organosol, inorganic silicon powder or fiber resin, which is not limited in the present invention.
  • an auxiliary agent may be incorporated, and the auxiliary agent may be an antifoaming agent, a coagulant, a homogenizing agent and the like.
  • the auxiliary agent assists the auxiliary binder and the templating agent to promote the formation of mesoporous sound absorbing material particles by the sound absorbing material powder.
  • the adjuvant will comprise from 0.02% to 10% of the total mass of the sol slurry.
  • the sound absorbing material powder may be natural zeolite powder, activated silica, white carbon black, activated carbon, molecular sieve, or the like, and may be a mixture of different or different zeolite-based sound absorbing material powders in a specific ratio.
  • the invention does not limit the material of the sound absorbing material powder, and those skilled in the art can perform the formulation according to actual needs.
  • the sol slurry prepared above is dropped into a molding oil to gradually age and solidify the sol droplets to form gel particles, which are mesoporous sound absorbing material particles are not prepared. Shape.
  • the size of the sol slurry droplets dropped into the forming oil directly affects the size of the mesoporous sound absorbing material particles.
  • the sol slurry droplets The diameter is usually between 100 and 400 microns.
  • the temperature of the molding oil is higher than normal temperature.
  • the temperature of the molding oil may be between 40 and 120 ° C.
  • the molding oil may be white lubricating oil, stator oil, machine tool oil, vacuum pump oil, Edible oil, or a mixture of lubricating oil and aliphatic hydrocarbons.
  • the present invention does not specifically limit the type of the molding oil. Those skilled in the art can select different oils as the molding oil according to the pore condition, the outer shape and the smoothness of the surface of the mesoporous sound absorbing material particles which are actually required.
  • the well-dissolved solution prepared in the step 1 can be prepared.
  • the glue slurry is placed in the forming oil by titration, atomization, or the like. Under the action of the temperature and liquid properties of the forming oil, the droplets of the sol slurry will react, and the powder of the sound absorbing material in the droplets of the sol slurry will start to age, aggregate, and gradually solidify and crystallize under the action of the binder.
  • the templating agent in the droplet occupies a part of the space in the droplet, which constitutes a large number of mesoporous structures, and can also cut large bubbles formed during the aging process of the droplet to form a plurality of small bubbles, thereby gradually crystallization.
  • the solidified gel particles have a large number of ordered mesoporous structures.
  • the gel particles eventually form a substantially solidified form, and in step 3, the substantially shaped gel particles are removed from the forming oil and dried to form mesoporous sound absorbing material particles.
  • an inert gas may be used as a medium to prevent polar defect points in the microstructure of the gel particles from reacting with active molecules in the air.
  • the inert gas may be nitrogen.
  • the gel particles may be dried at a constant temperature.
  • the gel particles may be placed in an inert gas having a temperature between 40 and 150 °C. This can more effectively discharge the liquid and the molding oil in the gel particles.
  • the time of the drying process is allowed between 0.5-96 hours, and those skilled in the art can adjust the parameters in the drying process according to the actual application to the speaker structure and the acoustic properties of the mesoporous sound absorbing material particles, corresponding settings Specific temperature profiles and drying media.
  • step 3 the liquid in the mesoporous sound absorbing material particles has been substantially discharged, but the mesoporous sound absorbing material particles are also doped with the addition of the binder and the templating agent preparation in the processing step. Impurities.
  • step 4 it is also necessary to calcine the mesoporous sound absorbing material particles to remove impurities therein and discharge the remaining liquid molecules.
  • the temperature and time of calcination may affect the microstructure of the mesoporous sound absorbing material particles.
  • the temperature range of the calcination process should be between 120 and 850 ° C, and the calcination time should be between 0.5 and 96 hours.
  • the rate of temperature rise during calcination should not be too fast, and if the rate of temperature rise is too fast, the microstructure of the mesoporous sound absorbing material particles is severely damaged.
  • the heating rate of the calcination ranges from 20 to 120 ° C / h.
  • the calcination rate can be selected at a heating rate of 45 ° C / h, and the calcination time is 30 hours.
  • liquid molecules in the mesoporous sound absorbing material particles can be removed, and impurities such as a template agent and a binder can be eliminated.
  • the mesoporous structure of the mesoporous sound absorbing material particles can be activated to ensure the mesoporous structure of the mesoporous sound absorbing material particles without causing damage to the microstructure.
  • the temperature of the calcination process may be between 280 and 550 ° C, the calcination time is between 20 and 65 hours, and the rate of temperature rise of the calcination is between 25 and 65 ° C / h.
  • the above temperature and time range generally do not cause damage to the microstructure of the mesoporous sound absorbing material particles, and can substantially remove liquid molecules and impurities.
  • the present invention does not accurately limit the temperature, time, and temperature increase rate of calcination, and those skilled in the art can adjust these parameters according to actual conditions.
  • the wide range of temperatures, times, and rate of temperature increase illustrated by the present invention encompasses situations that may be employed in special circumstances.
  • the content of oxygen in the furnace gas atmosphere during the calcination may be between 0.1 and 21%.
  • the presence of oxygen can activate the mesoporous structure in the mesoporous sound absorbing material particles to some extent, eliminate impurities in the mesoporous structure, make the mesoporous sound absorbing material particles have good sound absorbing effect, and the air circulation is smooth.
  • a person skilled in the art may select the oxygen content according to the actual situation, or may add a small amount of other active atmosphere in the atmosphere of the roasting furnace, which is not limited by the present invention.
  • the preparation method provided by the invention introduces the mesoporous structure into the particles of the sound absorbing material by the action of the templating agent, wherein the mesoporous structure is uniform and orderly, and the air molecular velocity in the rear cavity of the speaker can be greatly improved, and the mesoporous sound absorbing material is made.
  • the particles are matched with the millisecond-level reaction level of the applied speaker structure. Under the negative pressure condition, the effective instantaneous adsorption-desorption completion degree is significantly increased, and the optimized debugging effect on the acoustic performance of the speaker structure is greatly improved.
  • the mesoporous structure can also effectively enhance the sound absorbing effect of the sound absorbing material particles.
  • the present invention also provides a mesoporous sound absorbing material particle which can be directly obtained by the above method.
  • the mesoporous sound absorbing material particles have a specific surface area ranging from 250 to 650 m 2 /g, a pore volume of 0.2 to 2.0 ml/g, and a mesoporous pore volume having a pore diameter of 0.5 to 35 ⁇ m in the mesoporous sound absorbing material particles. It accounts for 15%-85% of the total pore volume.
  • the mesoporous sound absorbing material particles have a diameter ranging from 0.05 to 1.0 mm, and the mesoporous sound absorbing material particles having a diameter within this range are generally applicable to the back cavity of most of the speaker structures, and the bulk density is usually in the range of 0.25-0.95 g/ml.
  • the diameter of the mesoporous sound absorbing material particles is affected by the diameter of the droplet of the sol slurry which is dropped into the forming oil in the step 2 of the above method, and those skilled in the art can debug the parameters of the sound absorbing material particles according to the speaker of various rear acoustic cavity structures. .

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Abstract

一种介孔吸音材料颗粒的制备方法和介孔吸音材料颗粒。该制备方法包括：步骤1、将吸音材料粉体、模板剂与粘结剂和水混合形成溶胶浆料，模板剂为有机物单体或线性聚合物，纯度大于95%；步骤2、将溶胶浆料滴入成型油中，溶胶浆料的液滴在所述成型油中老化形成凝胶粒；步骤3、将凝胶粒从成型油中取出，干燥形成介孔吸音材料颗粒；步骤4、对介孔吸音材料颗粒进行焙烧。

Description

介孔吸音材料颗粒的制备方法和介孔吸音材料颗粒 技术领域
本发明属于材料加工技术领域，具体地，涉及一种介孔吸音材料颗粒的制备方法和一种介孔吸音材料颗粒。
背景技术
近年，随着穿戴式电子产品的日益轻薄化，传统发泡吸音材料已不能满足微型扬声器行业的声学性能调试校正需求，本领域技术人员不断开发、尝试新型吸音材料，经过验证后发现，在扬声器装置后腔中放置多孔性吸音材料可以有效的改善其声学性能，目前应用效果较好的该类新型吸音材料包括天然沸石、活性炭、白炭黑、硅铝比200以上的沸石粉等非发泡吸音材料。在应用过程中，需先将以上粉末态非发泡吸音材料制备成颗粒，后将吸音材料颗粒填充到扬声器后腔中。
但是，在现有的制备工艺中，通常采用的制粒方式并没有完全发挥这类非发泡吸音材料的性能。通常，本领域技术人员使用的制备方法包括挤压法、沸腾制粒法、滚动成球法等。但是，本发明发明人经过实际使用和测试发现，挤压法、沸腾制粒法、滚动成球法制得的颗粒强度相对较差，表面不光滑且颗粒大小不均，物理结构和性能受到了一定的限制，制成的吸音材料颗粒的吸音效果有限，且会影响扬声器后腔中空气的流动。而喷雾干燥法成型的颗粒比较小，而且粒径分布不均，吸音效果并没有达到预期程度。所以，本发明的发明人认为，现有的吸音材料颗粒填充到扬声器结构的后声腔后造成了两个问题，第一，阻碍了后腔中的空气流动，使得扬声器的灵敏度降低，后腔中产生的负压影响了扬声器振膜的正常工作；第二，吸音材料颗粒的吸音效果有限，还有提升空间。
综上所述，有必要对吸音材料颗粒的制备方法或吸音材料颗粒的结 构进行改进，增加孔道数量，提高材料的吸音效果，避免吸音材料颗粒降低扬声器后腔的空气进出的顺畅性。
发明内容
本发明的一个目的是提供一种制备吸音材料颗粒的新技术方案。
根据本发明的第一方面，提供了一种介孔吸音材料颗粒的制备方法，其中包括：
步骤1、将吸音材料粉体、模板剂与粘结剂和水混合形成溶胶浆料，所述模板剂为有机物单体或线性聚合物，所述模板剂的纯度大于95％；
步骤2、将所述溶胶浆料滴入成型油中，所述溶胶浆料的液滴在所述成型油中老化形成凝胶粒；
步骤3、将所述凝胶粒从所述成型油中取出，对所述凝胶粒进行干燥形成介孔吸音材料颗粒；
步骤4、对所述介孔吸音材料颗粒进行焙烧。
可选地，在所述步骤1中，所述模板剂的添加比例占所述溶胶浆料的总质量的1％-35％。
可选地，在所述步骤1中，粘结剂的添加比例占所述溶胶浆料的总质量的1％-35％，所述粘结剂为有机硅溶胶或纤维状树脂。
可选地，在所述步骤1中，在所述溶胶浆料中添加助剂，所述助剂的添加比例占所述溶胶浆料的总质量的0.02％-10％，所述助剂为消泡剂、促凝剂或均匀性剂。
可选地，在所述步骤2中，所述成型油的温度范围为40-120℃，所述成型油为白润滑油、定子油、机床油或真空泵油。
可选地，在所述步骤3中，将所述凝胶粒置于惰性气体中干燥，所述惰性气体的温度范围为40-150℃。
可选地，在所述步骤4中，焙烧时的温度范围为120-850℃，焙烧的升温速率的范围为20-120℃/h，焙烧的时间范围为0.5-96h。更优地，在所述步骤4中，焙烧气氛中氧气的含量为0.1％-21％。
本发明还提供了一种介孔吸音材料颗粒，所述介孔吸音材料颗粒的比表面积范围为250-650m2/g，孔体积为0.2-2.0ml/g，在所述介孔吸音材料颗粒中，孔径为0.5-35微米的介孔孔体积占孔容总量的15％-85％。
可选地，所述介孔吸音材料颗粒的直径范围为0.05-1.0mm，堆积密度的范围为0.25-0.95g/ml。
本发明的发明人发现，本领域技术人员通常会采用背景技术中介绍的现有技术手段制备吸音材料颗粒，并直接使用通过这些手段制成的颗粒，并未探索新的成型工艺或改进颗粒的结构特性。也就是说，本领域技术人员还未意识到现有的非发泡吸音材料颗粒在使用过程中存在的问题。因此，本发明所要实现的技术任务或者所要解决的技术问题是本领域技术人员从未想到的或者没有预期到的，故本发明是一种新的技术方案。
通过以下参照附图对本发明的示例性实施例的详细描述，本发明的其它特征及其优点将会变得清楚。
附图说明
被结合在说明书中并构成说明书的一部分的附图示出了本发明的实施例，并且连同其说明一起用于解释本发明的原理。
图1是本发明提供的介孔吸音材料颗粒的制备方法的步骤框图。
具体实施方式
现在将参照附图来详细描述本发明的各种示例性实施例。应注意到：除非另外具体说明，否则在这些实施例中阐述的部件和步骤的相对布置、数字表达式和数值不限制本发明的范围。
以下对至少一个示例性实施例的描述实际上仅仅是说明性的，决不作为对本发明及其应用或使用的任何限制。
对于相关领域普通技术人员已知的技术、方法和设备可能不作详细讨论，但在适当情况下，所述技术、方法和设备应当被视为说明书的一部分。
在这里示出和讨论的所有例子中，任何具体值应被解释为仅仅是示例性的，而不是作为限制。因此，示例性实施例的其它例子可以具有不同的值。
应注意到：相似的标号和字母在下面的附图中表示类似项，因此，一旦某一项在一个附图中被定义，则在随后的附图中不需要对其进行进一步讨论。
本发明提供了一种介孔吸音材料颗粒的制备方法，其中包括：
步骤1、将吸音材料粉体、模板剂与粘结剂和水混合形成溶胶浆料，所述模板剂为有机物单体或线性聚合物，所述模板剂的纯度大于95％；步骤2、将所述溶胶浆料滴入成型油中，所述溶胶浆料的液滴在所述成型油中老化形成凝胶粒；步骤3、将所述凝胶粒从所述成型油中取出，对所述凝胶粒进行干燥形成介孔吸音材料颗粒；步骤4、对所述介孔吸音材料颗粒进行焙烧。
本发明提供的制备方法是一种油柱成型法。在步骤1中，将吸音材料粉体与粘结剂和水混合形成溶胶状的溶胶浆料。特别地，在步骤1中需要向溶胶浆料中添加具有结构导向功能的模板剂，所述模板剂的作用在于为吸音材料粉体重结晶时提供结构框架，起到结构导向作用。根据模板剂的性质不同，可以引导吸音材料形成不同的晶体结构。由于最终需要形成的是介孔吸音材料颗粒，所以，所述模板剂需要能够在介孔吸音材料颗粒制造大量的介孔结构，以提高吸音效果和空气流畅性。在本发明的步骤1中，所述模板剂为有机物单体或线性聚合物，且纯度大于95％，这样，模板剂在后续步骤中能够发挥作用，使吸音材料重结晶时形成大量介孔结构。
特别地，在所述步骤1中，所述模板剂的添加比例在所述溶胶浆料总质量的1％-35％之间，如果模板剂添加量过高，则可能造成制成的介孔吸音材料颗粒结构不稳定，强度较低，如果模板剂添加量过低，则可能造成制成的介孔吸音材料颗粒中介孔结构和微孔过少，吸音效果差。本领域技术人员可以根据实际情况适当调整所述模板剂的用量，以使制成的介孔 吸音材料颗粒与扬声器结构相匹配，最大程度地发挥吸音效果。
优选地，在所述步骤1中，所述粘结剂在所述溶胶浆料中所占的质量比例应在1％-35％之间，如果粘结剂所占比例过高，则会使制成的介孔吸音材料颗粒结构过于紧实，造成吸音效果差，相反地，如果粘结剂所占比例过低，则会使介孔吸音材料颗粒最终无法凝固成球。所述粘结剂在所述溶胶浆料中的质量比例应于所述模板剂的质量比例相配合，本领域技术人员可以根据实际情况进行调配。所述粘结剂可以为氧化硅、有机溶胶、无机硅粉末或纤维树脂等材料，本发明不对此进行限制。
更优地，在所述步骤1中，还可以掺入助剂，所述助剂可以为消泡剂、促凝剂和均匀性剂等。所述助剂对辅助粘结剂和模板剂起辅助作用，促进吸音材料粉体形成介孔吸音材料颗粒。通常，所述助剂在所诉溶胶浆料总质量中占0.02％-10％。
另外，所述吸音材料粉体可以为天然沸石粉、活性二氧化硅、白炭黑、活性炭、分子筛等，并且，可以是不同以上沸石类吸音材料粉体的按照特定比例组成的混合物。本发明并不限制所述吸音材料粉体的材料，本领域技术人员可以根据实际需要进行调配。
在本发明的步骤2中，将上述制备的溶胶浆料滴入成型油中，以使溶胶液滴逐渐老化凝固，形成凝胶粒，所述凝胶粒即为介孔吸音材料颗粒未制备完成的形态。滴入成型油的溶胶浆料液滴的尺寸直接影响了介孔吸音材料颗粒的尺寸，为了使介孔吸音材料颗粒的尺寸达到正常使用与扬声器后腔的尺寸，所述溶胶浆料液滴的直径通常在100-400微米之间。
通常，成型油的温度要高于常温，可选地，所述成型油的温度范围可以在40-120℃之间，所述成型油可以为白润滑油、定子油、机床油、真空泵油、食用油，或者润滑油与脂肪烃的混合物等。本发明并不具体限制所述成型油的种类，本领域技术人员可以根据实际需要生成的介孔吸音材料颗粒的孔道情况、外形大小以及表面光滑程度要求选择不同的油类作为成型油使用。
在所述步骤2中，可以将步骤1中调配的、经过充分均匀处理的溶 胶浆料通过滴定、雾化加入等方式置于成型油中。在所述成型油的温度、液体性质的作用下，溶胶浆料液滴会产生反应，溶胶浆料液滴中的吸音材料粉体会在粘结剂的作用下开始老化、聚集、逐渐凝固结晶，此时，液滴中的模板剂会占据液滴中的一部分空间，构成大量介孔结构，而且还可以对液滴老化过程中形成的大气泡进行切割形成若干个小气泡，从而使得逐渐结晶凝固的凝胶粒中具备大量的有序介孔结构。
凝胶粒最终会形成基本凝固的形态，在所述步骤3中，将基本成型的凝胶粒从所述成型油中取出，并进行干燥，形成介孔吸音材料颗粒。特别地，在所述干燥过程中，可以使用惰性气体作为介质，防止凝胶粒的微观结构中的极性缺陷点与空气中的活性分子发生反应。所述惰性气体可以是氮气。另外，也可以使凝胶粒在一定温度下进行干燥。可选地，可以将所述凝胶粒置于惰性气体中，所述惰性气体的温度在40-150℃之间。这样可以更有效地将凝胶粒中的液体、成型油排出。所述干燥过程的时间在0.5-96小时之间都是允许的，本领域技术人员可以根据实际应用于扬声器结构的情况，以及介孔吸音材料颗粒的声学性能调整干燥过程中的参数，对应设置特定温度曲线和干燥介质。
进一步地，经过步骤3，介孔吸音材料颗粒中的液体已基本排出，但是，由于在加工步骤中添加了粘结剂、模板剂的制剂，所以所述介孔吸音材料颗粒中还掺杂有杂质。在本发明步骤4中，还需要对介孔吸音材料颗粒进行焙烧处理，去除其中的杂质，并排出剩余的液体分子。但是，焙烧的温度和时间会对介孔吸音材料颗粒的微观结构造成影响，在控制得当的情况下，能够使晶化程度有所提升，提高晶格的结构稳定性，但是如果控制不当，则会对晶体结构造成破坏，这直接影响了介孔吸音材料颗粒的吸音效果。所以，通常情况下，焙烧加工的温度范围应在120-850℃之间，焙烧的时间应在0.5-96小时之间。特别地，焙烧时的升温速率也不能过快，如果升温速度过快则会严重破坏介孔吸音材料颗粒的微观结构。通常，焙烧的升温速率范围为20-120℃/h，当焙烧温度选择适中，例如为350℃时，可以选择45℃/h的升温速率进行焙烧，焙烧时间为30小时。这样， 基本可以将介孔吸音材料颗粒中的液体分子去除，并将模板剂、粘结剂等杂质排除。杂质排除后，能够活化介孔吸音材料颗粒的介孔结构，保证该介孔吸音材料颗粒的介孔结构的畅通性，不会对微观结构造成破坏。优选地，焙烧加工的温度范围可以在280-550℃之间，焙烧时间则在20-65小时之间，而焙烧的升温速度则在25-65℃/h之间。以上温度和时间范围通常不会对介孔吸音材料颗粒的微观结构造成损坏，能够基本去除液体分子和杂质。本发明并不对焙烧是的温度、时间以及升温速度准确的限制，本领域技术人员可以根据实际情况对这些参数进行调整。本发明说明的较宽的温度、时间以及升温速率范围包含了一些特殊情况下可以采用的情况。
更优地，在所述步骤4中，所述焙烧时的炉气气氛中氧气的含量可以在0.1-21％之间。氧气的存在能够一定程度上活化介孔吸音材料颗粒中的介孔结构，排除介孔结构中的杂质，使介孔吸音材料颗粒具有良好的吸音效果，并且空气流通顺畅。本领域技术人员可以根据实际情况对氧气的含量进行选择，或者也可以在焙烧炉气气氛中加入少量其他活性气氛，本发明不对此进行限制。
本发明提供的制备方法通过模板剂的作用，将介孔结构引入到吸音材料颗粒中，其中的介孔结构均匀有序，能够大幅提高扬声器后腔中空气分子流动速度，使该介孔吸音材料颗粒与应用的扬声器结构的毫秒级反应级相匹配，在负压条件下，有效的瞬时吸附-脱附完成度明显增加，大大提高其对扬声器结构的声学性能的优化调试效果。并且，介孔结构也能够有效提升吸音材料颗粒的吸音效果。
进一步地，本发明还提供了一种介孔吸音材料颗粒，这种颗粒可以直接由上述方法制备得到。所述介孔吸音材料颗粒的比表面积范围为250-650m2/g，孔体积为0.2-2.0ml/g，在所述介孔吸音材料颗粒中，孔径为0.5-35微米的介孔孔体积占孔容总量的15％-85％。优选地，所述介孔吸音材料颗粒的直径范围为0.05-1.0mm，直径在这个范围内的介孔吸音材料颗粒通常能够适用于大部分扬声器结构的后腔，其堆积密度的范围通常为为0.25-0.95g/ml。介孔吸音材料颗粒的直径受上述方法步骤2中滴 入成型油的溶胶浆料液滴的直径大小的影响，本领域技术人员可根据各种后声腔结构的扬声器对吸音材料颗粒的参数进行调试。
虽然已经通过例子对本发明的一些特定实施例进行了详细说明，但是本领域的技术人员应该理解，以上例子仅是为了进行说明，而不是为了限制本发明的范围。本领域的技术人员应该理解，可在不脱离本发明的范围和精神的情况下，对以上实施例进行修改。本发明的范围由所附权利要求来限定。

Claims (10)

  1. 一种介孔吸音材料颗粒的制备方法，包括：
    步骤1、将吸音材料粉体、模板剂与粘结剂和水混合形成溶胶浆料，所述模板剂为有机物单体或线性聚合物，所述模板剂的纯度大于95％；
    步骤2、将所述溶胶浆料滴入成型油中，所述溶胶浆料的液滴在所述成型油中老化形成凝胶粒；
    步骤3、将所述凝胶粒从所述成型油中取出，对所述凝胶粒进行干燥形成介孔吸音材料颗粒；
    步骤4、对所述介孔吸音材料颗粒进行焙烧。
  2. 根据权利要求1所述的制备方法，其特征在于，在所述步骤1中，所述模板剂的添加比例占所述溶胶浆料的总质量的1％-35％。
  3. 根据权利要求1或2所述的制备方法，其特征在于，在所述步骤1中，粘结剂的添加比例占所述溶胶浆料的总质量的1％-35％，所述粘结剂为有机硅溶胶或纤维状树脂。
  4. 根据权利要求1-3任意之一所述的制备方法，其特征在于，在所述步骤1中，在所述溶胶浆料中添加助剂，所述助剂的添加比例占所述溶胶浆料的总质量的0.02％-10％，所述助剂为消泡剂、促凝剂或均匀性剂。
  5. 根据权利要求1-4任意之一所述的制备方法，其特征在于，在所述步骤2中，所述成型油的温度范围为40-120℃，所述成型油为白润滑油、定子油、机床油或真空泵油。
  6. 根据权利要求1-5任意之一所述的制备方法，其特征在于，在所述步骤3中，将所述凝胶粒置于惰性气体中干燥，所述惰性气体的温度范围为40-150℃。
  7. 根据权利要求1-6任意之一所述的制备方法，其特征在于，在所述步骤4中，焙烧时的温度范围为120-850℃，焙烧的升温速率的范围为20-120℃/h，焙烧的时间范围为0.5-96h。
  8. 根据权利要求1-7任意之一所述的制备方法，其特征在于，在所 述步骤4中，焙烧气氛中氧气的含量为0.1％-21％。
  9. 一种介孔吸音材料颗粒，其特征在于，所述介孔吸音材料颗粒的比表面积范围为250-650m2/g，孔体积为0.2-2.0ml/g，在所述介孔吸音材料颗粒中，孔径为0.5-35微米的介孔孔体积占孔容总量的15％-85％。
  10. 根据权利要求9所述的介孔吸音材料颗粒，其特征在于，所述介孔吸音材料颗粒的直径范围为0.05-1.0mm，堆积密度的范围为0.25-0.95g/ml。
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