CN112080024A - Composite diaphragm and preparation method thereof - Google Patents
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/26—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a solid phase from a macromolecular composition or article, e.g. leaching out
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- C08J9/36—After-treatment
- C08J9/40—Impregnation
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- H—ELECTRICITY
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- H04R—LOUDSPEAKERS, MICROPHONES, GRAMOPHONE PICK-UPS OR LIKE ACOUSTIC ELECTROMECHANICAL TRANSDUCERS; DEAF-AID SETS; PUBLIC ADDRESS SYSTEMS
- H04R31/00—Apparatus or processes specially adapted for the manufacture of transducers or diaphragms therefor
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- H—ELECTRICITY
- H04—ELECTRIC COMMUNICATION TECHNIQUE
- H04R—LOUDSPEAKERS, MICROPHONES, GRAMOPHONE PICK-UPS OR LIKE ACOUSTIC ELECTROMECHANICAL TRANSDUCERS; DEAF-AID SETS; PUBLIC ADDRESS SYSTEMS
- H04R7/00—Diaphragms for electromechanical transducers; Cones
- H04R7/02—Diaphragms for electromechanical transducers; Cones characterised by the construction
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- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/046—Elimination of a polymeric phase
- C08J2201/0462—Elimination of a polymeric phase using organic solvents
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- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/02—Cellulose; Modified cellulose
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- C08J2397/00—Characterised by the use of lignin-containing materials
- C08J2397/02—Lignocellulosic material, e.g. wood, straw or bagasse
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- 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
- C08J2429/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2429/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2429/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2471/02—Polyalkylene oxides
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
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- H—ELECTRICITY
- H04—ELECTRIC COMMUNICATION TECHNIQUE
- H04R—LOUDSPEAKERS, MICROPHONES, GRAMOPHONE PICK-UPS OR LIKE ACOUSTIC ELECTROMECHANICAL TRANSDUCERS; DEAF-AID SETS; PUBLIC ADDRESS SYSTEMS
- H04R2307/00—Details of diaphragms or cones for electromechanical transducers, their suspension or their manufacture covered by H04R7/00 or H04R31/003, not provided for in any of its subgroups
- H04R2307/021—Diaphragms comprising cellulose-like materials, e.g. wood, paper, linen
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Abstract
The invention discloses a composite diaphragm and a preparation method thereof, wherein the composite diaphragm is prepared from the following raw materials in parts by weight: 5-15 parts of microcrystalline cellulose, 100-120 parts of cellulose dispersion liquid, 5-15 parts of pore-foaming agent, 150-200 parts of displacing agent, 5-30 parts of nano reinforcing material, 100-150 parts of dispersion liquid and 5-10 parts of surfactant. Microcrystalline cellulose and a nano-reinforcing material are used as raw materials for preparing the vibrating diaphragm, and after the cellulose membrane adsorbs the nano-reinforcing material, the strength of the vibrating diaphragm can be greatly improved. The preparation process of the composite diaphragm is simple and the cost is low.
Description
Technical Field
The invention relates to the technical field of diaphragms, in particular to a composite diaphragm and a preparation method thereof.
Background
With the increasing pace of social life, consumers are more interested in small and portable in-ear headphones rather than traditional headsets. In-ear earphones are smaller and therefore have more stringent requirements on the earphone material, including the diaphragm material. Due to the volume limitation of the earphone, and the earphone is mainly pushed by a mobile phone or mobile phone Bluetooth, the vibrating diaphragm of the in-ear earphone is required to be as light and thin as possible on the premise of keeping the rigidity. In recent years, how to prepare a diaphragm with a high elastic ratio has been a research focus in the field of earphones.
At present, the vibrating diaphragms made of materials such as diamond, graphene and beryllium which can be used practically are available on the market, and the vibrating diaphragms have super-strong rigidity and low density and are excellent materials for preparing the vibrating diaphragms. However, since these materials are difficult to process and expensive in cost, and cannot be popularized on a large scale in a short time, research and development personnel shift research centers to composite diaphragms. The high-performance film is prepared by selecting nano materials such as graphene and carbon nano tubes to dope and modify a high-molecular material with high damping and low density, or directly spraying a graphene coating and compounding a carbon fiber film. However, these several approaches have their drawbacks: the nanometer materials including graphene, carbon nanotubes, carbon nanofibers, gas-phase silica and the like are easy to agglomerate when being directly doped and stirred to form agglomerated particles with different sizes, so that the modification enhancement effect cannot be achieved, the uniformity of the film is reduced, and the properties of the film can be influenced if a large amount of dispersing agent is added; the methods of directly spraying graphene or weaving carbon nanofibers and the like also face the problems of high processing difficulty and high cost.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the composite vibrating diaphragm and the preparation method thereof are provided, and the composite vibrating diaphragm is high in mechanical strength, simple in preparation process and low in cost.
In order to solve the technical problems, the invention adopts the technical scheme that:
a composite diaphragm is prepared from the following raw materials in parts by weight: 5-15 parts of microcrystalline cellulose, 100-120 parts of cellulose dispersion liquid, 5-15 parts of pore-foaming agent, 150-200 parts of displacing agent, 5-30 parts of nano reinforcing material, 100-150 parts of dispersion liquid and 5-10 parts of surfactant.
The invention adopts another technical scheme that:
the preparation method of the composite diaphragm comprises the steps of mixing microcrystalline cellulose, cellulose dispersion liquid and pore-foaming agent to obtain first mixed liquid; leveling the first mixed solution in a mold to obtain a cellulose wet film; placing the cellulose wet film into a displacing agent for displacement to obtain a porous cellulose wet film; carrying out first drying treatment on the porous cellulose wet film to obtain a porous cellulose film; mixing the nano reinforcing material, the dispersion liquid and the surfactant to obtain nano dispersion liquid; immersing the porous cellulose membrane into the nano dispersion liquid, and then carrying out ultrasonic oscillation treatment to obtain a composite cellulose membrane intermediate; sequentially carrying out second drying treatment and compaction treatment on the composite cellulose membrane intermediate to obtain a composite cellulose membrane; and carrying out air pressure forming on the composite cellulose membrane to obtain the composite diaphragm.
The invention has the beneficial effects that:
1. microcrystalline cellulose and a nano-reinforcing material are used as raw materials for preparing the vibrating diaphragm, and after the cellulose membrane adsorbs the nano-reinforcing material, the mechanical strength of the vibrating diaphragm can be greatly improved.
2. When the diaphragm is prepared, microcrystalline cellulose is processed into a porous structure, so that the nano reinforced material can be effectively adsorbed; in the preparation process, the pore diameter of the material can be controlled by adopting the displacing agents with different polarities, and composite films with different proportions and forms can be prepared by matching the nano-dispersion liquid with different concentrations, so that different use requirements are met; the nano reinforced material can perform self-growth adsorption on the porous cellulose membrane, and the continuous ultrasonic oscillation can ensure that the nano reinforced material cannot agglomerate and can perform uniform adsorption, so that the strength of the cellulose membrane is greatly improved; the nano dispersion liquid can be used for multiple times, the utilization rate is high, the adsorption process is simple, and the cost can be effectively reduced; the cellulose membrane has biodegradability, and is more environment-friendly compared with a plastic diaphragm and a metal diaphragm.
Detailed Description
In order to explain the technical content, the objects and the effects of the present invention in detail, the following description will be given with reference to the embodiments.
The most key concept of the invention is as follows: microcrystalline cellulose and a nano-reinforcing material are used as raw materials for preparing the vibrating diaphragm, and after the cellulose membrane adsorbs the nano-reinforcing material, the strength of the vibrating diaphragm can be greatly improved.
A composite diaphragm is prepared from the following raw materials in parts by weight: 5-15 parts of microcrystalline cellulose, 100-120 parts of cellulose dispersion liquid, 5-15 parts of pore-foaming agent, 150-200 parts of displacing agent, 5-30 parts of nano reinforcing material, 100-150 parts of dispersion liquid and 5-10 parts of surfactant.
From the above description, the beneficial effects of the present invention are: microcrystalline cellulose and a nano-reinforcing material are used as raw materials for preparing the vibrating diaphragm, and after the cellulose membrane adsorbs the nano-reinforcing material, the mechanical strength of the vibrating diaphragm can be greatly improved.
Further, the microcrystalline cellulose is at least one of lignocellulose and bacterial cellulose.
Further, the cellulose dispersion liquid is at least one of water, methanol, ethanol, isopropanol, acetone, tert-butanol and octane.
Further, the pore-foaming agent is at least one of polyethylene glycol, polyvinyl alcohol, hydrogen peroxide and hydroxy cellulose.
Further, the displacer is at least one of ethanol, acetone, tert-butyl alcohol and potassium hydroxide solution.
Further, the nano reinforcing material is at least one of graphene powder, graphene nanosheets, single-walled carbon nanotubes, multi-walled carbon nanotubes, carbon nanofibers and fumed silica.
Further, the dispersion liquid is at least one of deionized water, NMP, DMF and ethanol.
Further, the surfactant is at least one of sodium dodecyl benzene sulfonate, quaternary ammonium compound and fatty glyceride.
As apparent from the above description, the kinds of microcrystalline cellulose, cellulose dispersion, pore-forming agent, substitution agent, nano-reinforcing material, dispersion, and surfactant may be selected as necessary.
The invention relates to another technical scheme which is as follows:
the preparation method of the composite diaphragm comprises the steps of mixing microcrystalline cellulose, cellulose dispersion liquid and pore-foaming agent to obtain first mixed liquid; leveling the first mixed solution in a mold to obtain a cellulose wet film; placing the cellulose wet film into a displacing agent for displacement to obtain a porous cellulose wet film; carrying out first drying treatment on the porous cellulose wet film to obtain a porous cellulose film; mixing the nano reinforcing material, the dispersion liquid and the surfactant to obtain nano dispersion liquid; immersing the porous cellulose membrane into the nano dispersion liquid, and then carrying out ultrasonic oscillation treatment to obtain a composite cellulose membrane intermediate; sequentially carrying out second drying treatment and compaction treatment on the composite cellulose membrane intermediate to obtain a composite cellulose membrane; and carrying out air pressure forming on the composite cellulose membrane to obtain the composite diaphragm.
From the above description, firstly, the microcrystalline cellulose is processed into a porous structure, which is beneficial to effectively adsorbing the nano reinforced material; in the preparation process, the pore diameter of the material can be controlled by adopting the displacing agents with different polarities, and composite films with different proportions and forms can be prepared by matching the nano-dispersion liquid with different concentrations, so that different use requirements are met; the nano reinforced material can perform self-growth adsorption on the porous cellulose membrane, and the continuous ultrasonic oscillation can ensure that the nano reinforced material cannot agglomerate and can perform uniform adsorption, so that the strength of the cellulose membrane is greatly improved; the nano dispersion liquid can be used for multiple times, the utilization rate is high, the adsorption process is simple, and the cost can be effectively reduced; the cellulose membrane has biodegradability, and is more environment-friendly compared with a plastic diaphragm and a metal diaphragm.
Further, the second drying treatment is carried out in a vacuum drying oven at the temperature of 50-100 ℃ for 6-12 hours.
Example one
The first embodiment of the invention is as follows:
a composite diaphragm is prepared from the following raw materials in parts by weight: 5-15 parts of microcrystalline cellulose, 100-120 parts of cellulose dispersion liquid, 5-15 parts of pore-foaming agent, 150-200 parts of displacing agent, 5-30 parts of nano reinforcing material, 100-150 parts of dispersion liquid and 5-10 parts of surfactant. The microcrystalline cellulose is at least one of lignocellulose and bacterial cellulose. The cellulose dispersion is at least one of water, methanol, ethanol, isopropanol, acetone, tert-butanol and octane. The pore-foaming agent is at least one of polyethylene glycol, polyvinyl alcohol, hydrogen peroxide and hydroxy cellulose. The displacer is at least one of ethanol, acetone, tert-butyl alcohol and potassium hydroxide solution. The nano reinforcing material is at least one of graphene powder, graphene nanosheets, single-walled carbon nanotubes, multi-walled carbon nanotubes, carbon nanofibers and gas-phase silica. The dispersion liquid is at least one of deionized water, NMP, DMF and ethanol. The surfactant is at least one of sodium dodecyl benzene sulfonate, quaternary ammonium compound and fatty glyceride.
The preparation method of the composite diaphragm comprises the following steps:
1. and mixing the microcrystalline cellulose, the cellulose dispersion liquid and the pore-foaming agent to obtain a first mixed liquid.
During mixing, microcrystalline cellulose, cellulose dispersion liquid and pore-forming agent can be added into a mixing container for mixing, and after the first mixed liquid is obtained, filtering and defoaming treatment can be sequentially carried out, wherein impurities can be removed through filtering, and bubbles can be removed through defoaming.
2. And leveling the first mixed solution in a mold to obtain a cellulose wet film.
In this embodiment, the first mixed liquid may be dried to some extent after being leveled, and may be left to stand and dried at room temperature.
3. And (3) placing the cellulose wet film into a displacing agent for displacement to obtain the porous cellulose wet film.
4. And carrying out first drying treatment on the porous cellulose wet film to obtain the porous cellulose film.
The first drying treatment may be performed by room temperature drying, freeze drying, vacuum heat drying, or the like.
5. Mixing the nano reinforcing material, the dispersion liquid and the surfactant to obtain the nano dispersion liquid.
6. And immersing the porous cellulose membrane into the nano dispersion liquid, and then carrying out ultrasonic oscillation treatment to obtain a composite cellulose membrane intermediate.
In this embodiment, the time of the ultrasonic oscillation treatment is 12-24 hours, and the nano-reinforcing material can perform self-growth adsorption.
7. And sequentially carrying out second drying treatment and compaction treatment on the composite cellulose membrane intermediate to obtain the composite cellulose membrane.
In the embodiment, the second drying treatment is performed in a vacuum drying oven at a temperature of 50-100 ℃ for 6-12 hours. The compaction treatment can be realized by a tablet press, and the pressure of the compaction treatment is 0.2-0.5 MPa.
8. And carrying out air pressure forming on the composite cellulose membrane to obtain the composite diaphragm.
In this embodiment, the air pressure forming can be realized by an air compressor, and the pressure of the air pressure forming is 0.3-0.8 MPa.
Example two
The second embodiment of the present invention is a composite diaphragm, which is different from the first embodiment in that:
the composite diaphragm is prepared from the following raw materials in parts by weight: 10 parts of microcrystalline cellulose, 100 parts of cellulose dispersion liquid, 5 parts of pore-foaming agent, 150 parts of displacing agent, 5 parts of nano reinforcing material, 120 parts of dispersion liquid and 5 parts of surfactant. The microcrystalline cellulose is lignocellulose, the cellulose dispersion liquid is water, the pore-forming agent is polyethylene glycol, the displacing agent is acetone, the nano-reinforcing material is graphene powder, the dispersion liquid is ethanol, and the surfactant is sodium dodecyl benzene sulfonate.
In the step 3, the replacement time is 6 hours when the composite diaphragm is prepared. In the step 4, the first drying treatment is to place the mixture into an oven and dry the mixture under the protection of nitrogen, wherein the temperature is 60 ℃ and the time is 6 hours. In step 6, the time of ultrasonic oscillation treatment is 12 hours. In the step 7, the temperature of the second drying treatment is 60 ℃, and the time is 6 hours; the pressure of the compacting treatment was 0.2 MPa. In step 8, the pressure of the air pressure forming is 0.4 MPa.
EXAMPLE III
The third embodiment of the present invention is a composite diaphragm, which is different from the first embodiment in that:
the composite diaphragm is prepared from the following raw materials in parts by weight: 5 parts of microcrystalline cellulose, 110 parts of cellulose dispersion liquid, 10 parts of pore-foaming agent, 180 parts of displacing agent, 8 parts of nano reinforcing material, 100 parts of dispersion liquid and 8 parts of surfactant. The microcrystalline cellulose is bacterial cellulose, the cellulose dispersion liquid is ethanol, the pore-foaming agent is polyvinyl alcohol, the displacing agent is ethanol, the nano-reinforcing material is carbon nano-fiber, the dispersion liquid is water, and the surfactant is fatty glyceride.
In the step 3, the replacement time is 6 hours when the composite diaphragm is prepared. In the step 4, the first drying treatment is to place the mixture into an oven and dry the mixture under the protection of nitrogen, wherein the temperature is 60 ℃ and the time is 6 hours. In step 6, the time of ultrasonic oscillation treatment is 18 h. In the step 7, the temperature of the second drying treatment is 50 ℃, and the time is 8 hours; the pressure of the compacting treatment was 0.3 MPa. In step 8, the pressure of the air pressure forming is 0.3 MPa.
Example four
The fourth embodiment of the present invention is a composite diaphragm, which is different from the first embodiment in that:
the composite diaphragm is prepared from the following raw materials in parts by weight: 15 parts of microcrystalline cellulose, 120 parts of cellulose dispersion liquid, 15 parts of pore-foaming agent, 200 parts of displacing agent, 30 parts of nano reinforcing material, 150 parts of dispersion liquid and 10 parts of surfactant. The microcrystalline cellulose is bacterial cellulose, the cellulose dispersion liquid is ethanol, the pore-foaming agent is polyvinyl alcohol, the displacing agent is ethanol, the nano-reinforcing material is graphene nanosheet, the dispersion liquid is water, and the surfactant is fatty glyceride.
In the step 3, the replacement time is 6 hours when the composite diaphragm is prepared. In the step 4, the first drying treatment is to place the mixture into an oven and dry the mixture under the protection of nitrogen, wherein the temperature is 60 ℃ and the time is 6 hours. In the step 6, the time of ultrasonic oscillation treatment is 24 hours. In the step 7, the temperature of the second drying treatment is 100 ℃, and the time is 12 hours; the pressure of the compacting treatment was 0.5 MPa. In step 8, the pressure of the air pressure molding is 0.8 MPa.
Performance testing
Tensile mechanical property tests are carried out on the composite diaphragms of the second embodiment to the fourth embodiment, the PET diaphragms are used as a control group, test samples are standard sample bars of 15mm multiplied by 80mm, test equipment is a new three-Si brand universal tester, and test results are shown in table 1,
TABLE 1 tensile mechanical Properties test results Table
As can be seen from table 1, the composite diaphragms of the second embodiment to the fourth embodiment have better mechanical properties than PET diaphragms.
In conclusion, the composite diaphragm and the preparation method thereof provided by the invention have the advantages of simple preparation process and low cost, and the obtained composite diaphragm has good mechanical property and can meet the use requirement.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all equivalent modifications made by the present invention in the specification or directly or indirectly applied to the related technical field are included in the scope of the present invention.
Claims (10)
1. The composite diaphragm is characterized by being prepared from the following raw materials in parts by weight: 5-15 parts of microcrystalline cellulose, 100-120 parts of cellulose dispersion liquid, 5-15 parts of pore-foaming agent, 150-200 parts of displacing agent, 5-30 parts of nano reinforcing material, 100-150 parts of dispersion liquid and 5-10 parts of surfactant.
2. The composite diaphragm of claim 1, wherein the microcrystalline cellulose is at least one of lignocellulose and bacterial cellulose.
3. The composite diaphragm of claim 1, wherein the cellulose dispersion is at least one of water, methanol, ethanol, isopropanol, acetone, tert-butanol, and octane.
4. The composite diaphragm of claim 1, wherein the pore-forming agent is at least one of polyethylene glycol, polyvinyl alcohol, hydrogen peroxide, and hydroxy cellulose.
5. The composite diaphragm of claim 1, wherein the displacing agent is at least one of ethanol, acetone, tert-butyl alcohol and potassium hydroxide solution.
6. The composite diaphragm of claim 1, wherein the nano reinforcing material is at least one of graphene powder, graphene nanoplatelets, single-walled carbon nanotubes, multi-walled carbon nanotubes, carbon nanofibers, and fumed silica.
7. The composite diaphragm of claim 1, wherein the dispersion is at least one of deionized water, NMP, DMF, and ethanol.
8. The composite diaphragm of claim 1, wherein the surfactant is at least one of sodium dodecyl benzene sulfonate, a quaternary ammonium compound and fatty glyceride.
9. The method for preparing a composite diaphragm according to any one of claims 1 to 8, wherein microcrystalline cellulose, a cellulose dispersion liquid and a pore-forming agent are mixed to obtain a first mixed liquid; leveling the first mixed solution in a mold to obtain a cellulose wet film; placing the cellulose wet film into a displacing agent for displacement to obtain a porous cellulose wet film; carrying out first drying treatment on the porous cellulose wet film to obtain a porous cellulose film; mixing the nano reinforcing material, the dispersion liquid and the surfactant to obtain nano dispersion liquid; immersing the porous cellulose membrane into the nano dispersion liquid, and then carrying out ultrasonic oscillation treatment to obtain a composite cellulose membrane intermediate; sequentially carrying out second drying treatment and compaction treatment on the composite cellulose membrane intermediate to obtain a composite cellulose membrane; and carrying out air pressure forming on the composite cellulose membrane to obtain the composite diaphragm.
10. The method for preparing a composite diaphragm according to claim 9, wherein the second drying treatment is performed in a vacuum drying oven at a temperature of 50-100 ℃ for 6-12 hours.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010854652.7A CN112080024A (en) | 2020-08-24 | 2020-08-24 | Composite diaphragm and preparation method thereof |
| PCT/CN2021/113442 WO2022042410A1 (en) | 2020-08-24 | 2021-08-19 | Composite diaphragm and preparation method therefor |
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| CN202010854652.7A CN112080024A (en) | 2020-08-24 | 2020-08-24 | Composite diaphragm and preparation method thereof |
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| CN112080024A true CN112080024A (en) | 2020-12-15 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022042410A1 (en) * | 2020-08-24 | 2022-03-03 | 深圳市信维通信股份有限公司 | Composite diaphragm and preparation method therefor |
| CN116836596A (en) * | 2023-06-30 | 2023-10-03 | 常州第六元素材料科技股份有限公司 | Modified graphene oxide vibrating diaphragm and preparation method thereof |
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| CN116836596B (en) * | 2023-06-30 | 2024-04-02 | 常州第六元素材料科技股份有限公司 | Modified graphene oxide vibrating diaphragm and preparation method thereof |
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| WO2022042410A1 (en) | 2022-03-03 |
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