CN116177559A - Silicon-aluminum-titanium molecular sieve, acoustic reinforcing material, preparation method of silicon-aluminum-titanium molecular sieve, loudspeaker and electronic equipment - Google Patents

Silicon-aluminum-titanium molecular sieve, acoustic reinforcing material, preparation method of silicon-aluminum-titanium molecular sieve, loudspeaker and electronic equipment Download PDF

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CN116177559A
CN116177559A CN202111425964.7A CN202111425964A CN116177559A CN 116177559 A CN116177559 A CN 116177559A CN 202111425964 A CN202111425964 A CN 202111425964A CN 116177559 A CN116177559 A CN 116177559A
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molecular sieve
aluminum
silicon
titanium
acoustic
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王义君
张磊
郭明波
马院红
龚畅
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Shanghai Runshi Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
    • C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
    • C01B39/06—Preparation of isomorphous zeolites characterised by measures to replace the aluminium or silicon atoms in the lattice framework by atoms of other elements, i.e. by direct or secondary synthesis
    • C01B39/065—Galloaluminosilicates; Group IVB- metalloaluminosilicates; Ferroaluminosilicates
    • H—ELECTRICITY
    • H04—ELECTRIC COMMUNICATION TECHNIQUE
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • H—ELECTRICITY
    • H04—ELECTRIC COMMUNICATION TECHNIQUE
    • H04R—LOUDSPEAKERS, MICROPHONES, GRAMOPHONE PICK-UPS OR LIKE ACOUSTIC ELECTROMECHANICAL TRANSDUCERS; DEAF-AID SETS; PUBLIC ADDRESS SYSTEMS
    • H04R2499/00—Aspects covered by H04R or H04S not otherwise provided for in their subgroups
    • H04R2499/10—General applications
    • H04R2499/11—Transducers incorporated or for use in hand-held devices, e.g. mobile phones, PDA's, camera's
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts

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  • General Life Sciences & Earth Sciences (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
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  • Acoustics & Sound (AREA)
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  • Silicates, Zeolites, And Molecular Sieves (AREA)

Abstract

The invention provides a silicon-aluminum-titanium molecular sieve, an acoustic enhancement material, a preparation method thereof, a loudspeaker and electronic equipment, wherein the skeleton of the silicon-aluminum-titanium molecular sieve contains silicon, aluminum and titanium elements, the mass ratio of the silicon to the aluminum elements is 1-500:1, and the mass ratio of the silicon to the titanium elements is 10-50:1. Compared with the traditional high-silicon aluminum molecular sieve, the silicon aluminum titanium molecular sieve provided by the invention has heavier bulk density, and can obtain heavier vibration quality under the same filling volume, so that the acoustic performance is better, and the delta F0 of the molecular sieve is 20-30% higher than the delta F0 of the traditional high-silicon aluminum molecular sieve under the same conditions. Compared with the traditional titanium-silicon molecular sieve, the silicon-aluminum-titanium molecular sieve provided by the invention has the advantages that because the framework contains aluminum element, uniform slurry is easy to form in the slurry forming process, so that the sphericity of the prepared finished product acoustic enhancement material microsphere is higher.

Description

Silicon-aluminum-titanium molecular sieve, acoustic reinforcing material, preparation method of silicon-aluminum-titanium molecular sieve, loudspeaker and electronic equipment
Technical Field
The invention relates to a silicon-aluminum-titanium molecular sieve, an acoustic enhancement material, a preparation method thereof, a loudspeaker and electronic equipment, and belongs to the technical field of electronic acoustic materials.
Background
With the development of social economy and the improvement of consumption level, people have higher and higher requirements on life quality, and mobile phones as the most important electronic consumer products play a very important role in life, and the quality of the speaker as an important part of the mobile phones is also more and more important.
In particular, for a mobile phone speaker, it is required to provide excellent acoustic performance while being as small as possible. The tone quality and design of the loudspeaker are closely related to the manufacturing process, especially the size design of the rear cavity of the loudspeaker. In general, the smaller the rear cavity of the speaker is, the worse the acoustic response in the low frequency band is, and the worse the acoustic performance such as sound quality is, so it is necessary to try to enlarge the rear cavity of the speaker to improve the acoustic response in the low frequency band. In the prior art, the virtual volume of the rear cavity is increased by filling sound absorbing materials such as active carbon, silicon dioxide, molecular sieve, high-phosphorus soil and the like into the rear cavity, and the gas acoustic compliance of the rear cavity is improved, so that the low-frequency response is improved, and the traditional acoustic enhancement material for the loudspeaker is obtained by using a silicon-aluminum molecular sieve or a titanium-silicon molecular sieve with an MFI structure as a main component and assisting with a binder and an auxiliary agent for molding. Because the loudspeaker is mainly oriented to the consumer market, besides the acoustic performance, stability and reliability are important considerations, the silicon-aluminum ratio of the molecular sieve has to be improved, and even the molecular sieve is made into an all-silicon molecular sieve so as to improve the bulk density and the vibration quality and optimize the acoustic performance, but the bulk density, the vibration quality, the acoustic performance and the like of the molecular sieve materials currently used still cannot meet the requirements of people.
Based on such problems, there is a need to develop new molecular sieves and acoustic enhancing materials that have higher bulk density, vibration mass, and more excellent acoustic properties.
Disclosure of Invention
In order to solve the above-mentioned disadvantages and shortcomings, an object of the present invention is to provide a silicon-aluminum-titanium molecular sieve.
The invention also aims to provide a preparation method of the silicon-aluminum-titanium molecular sieve.
The invention also aims to provide an acoustic reinforcing material which is prepared by uniformly mixing the silicon-aluminum-titanium molecular sieve, the binder, the dispersing agent and/or the auxiliary agent and then molding.
It is also an object of the present invention to provide a method of preparing the above-described acoustic enhancement material.
It is also an object of the invention to provide a loudspeaker with a rear chamber fitted with an acoustic enhancement material as described above.
It is also a final object of the invention to provide an electronic device with a speaker rear cavity fitted with the above-mentioned acoustic enhancement material.
In order to achieve the above purpose, in one aspect, the invention provides a silicon-aluminum-titanium molecular sieve, wherein the skeleton of the silicon-aluminum-titanium molecular sieve contains silicon, aluminum and titanium elements, the mass ratio of the silicon to the aluminum elements is 1-500:1, and the mass ratio of the silicon to the titanium elements is 10-50:1.
As a specific embodiment of the silicon aluminum titanium molecular sieve, the structure of the silicon aluminum titanium molecular sieve comprises any one of MFI, CHA, FER, MOR, AFI, BEA, MWW, and the grain size of the silicon aluminum titanium molecular sieve is 20-1000nm.
As a specific embodiment of the silicon-aluminum-titanium molecular sieve, the silicon-aluminum-titanium molecular sieve is prepared by uniformly mixing raw materials and water, crystallizing the obtained mixed solution at the temperature of 100-200 ℃, and centrifugally separating, washing, drying and roasting;
wherein the raw materials comprise a silicon source, an aluminum source, a titanium source, a template agent, an alkali source and an auxiliary agent, and the use amount of the auxiliary agent is 0-5% based on 100% of the total weight of the silicon-aluminum-titanium molecular sieve.
As a specific embodiment of the silicon-aluminum-titanium molecular sieve, the silicon source comprises one or a mixture of more of silica sol, white carbon black, silica gel, ethyl orthosilicate and water glass.
As a specific embodiment of the aluminosilicate-titanium molecular sieve according to the present invention, the aluminum source includes one or a mixture of several aluminum salts such as aluminum isopropoxide, aluminum nitrate, aluminum sulfate, pseudo-boehmite, aluminum chloride, aluminum sol, and the like.
As a specific embodiment of the silicon aluminum titanium molecular sieve, the titanium source comprises one or a mixture of a plurality of titanium salts such as tetrabutyl titanate, titanium tetrachloride, titanium sulfate and the like.
As a specific embodiment of the silicon aluminum titanium molecular sieve, the template agent comprises one or a mixture of several of tetrapropylammonium hydroxide, tetrapropylammonium bromide, n-butylamine, ethylamine, tetraethylammonium hydroxide, triethylamine and diethylamine.
As a specific embodiment of the above-mentioned aluminosilicate molecular sieve according to the present invention, the alkali source includes one or a mixture of two of sodium hydroxide and potassium hydroxide.
As a specific embodiment of the above-mentioned si-al-ti molecular sieve according to the present invention, the auxiliary agent includes a molecular sieve having any one of structures MFI, CHA, FER, MOR, AFI, BEA, MWW. Wherein, the auxiliary agent added in the preparation of the silicon aluminum titanium molecular sieve is used as seed crystal, which can accelerate the crystallization reaction speed and shorten the crystallization time.
In another aspect, the invention also provides a preparation method of the silicon-aluminum-titanium molecular sieve, wherein the preparation method comprises the following steps:
uniformly mixing raw materials and water, carrying out crystallization reaction on the obtained mixed solution at the temperature of 100-200 ℃ by a hydrothermal synthesis method, carrying out centrifugal separation on the obtained slurry after the reaction is finished, continuously washing the separated dry base until the pH value of the washing solution is 8-9, drying the separated dry base to ensure that the water content of the dried dry base is less than 2%, and finally roasting the dried dry base at the temperature of 400-650 ℃ to obtain the silicon-aluminum-titanium molecular sieve;
wherein the raw materials comprise a silicon source, an aluminum source, a titanium source, a template agent, an alkali source and an auxiliary agent, and the use amount of the auxiliary agent is 0-5% based on 100% of the total weight of the silicon-aluminum-titanium molecular sieve.
In some embodiments of the invention, the adjuvant may be used, for example, in an amount of 0.61%, 1.09%, 1.32%, 2.80%, 3.82%, etc., based on 100% by weight of the total weight of the aluminosilicate molecular sieve.
In still another aspect, the invention further provides an acoustic enhancement material, wherein the acoustic enhancement material is prepared by uniformly mixing the silicon-aluminum-titanium molecular sieve, the binder, the dispersant and/or the auxiliary agent, and then molding, and the content of the silicon-aluminum-titanium molecular sieve is not less than 70% based on 100% of the total weight of the acoustic enhancement material.
As a specific embodiment of the above-described acoustic enhancement material of the present invention, wherein the shape of the acoustic enhancement material includes microspheres (i.e., particles), blocks, or flakes; wherein the size of the microsphere is between 50 and 300 mu m.
As an embodiment of the above-mentioned acoustic reinforcement material of the present invention, wherein the content of the binder is 1 to 15% based on 100% of the total weight of the acoustic reinforcement material; wherein the content of the binder is calculated by the content of the solid component in the binder, namely the dry basis of the binder.
As a specific embodiment of the above acoustic reinforcement material of the present invention, wherein the binder includes an inorganic binder and/or an organic binder;
wherein the inorganic binder comprises one or a mixture of a plurality of silica sol, alumina sol, water glass and pseudo-boehmite; the organic binder comprises one or a mixture of a plurality of acrylic ester, epoxy and polyurethane organic binders.
As a specific embodiment of the above-mentioned acoustic enhancement material of the present invention, the dry content of the dispersant is 0 to 1% based on 100% of the total weight of the acoustic enhancement material.
In some embodiments of the invention, the dispersant may be present at, for example, 0.43%, 0.44%, 0.88%, 0.90%, 0.96% dry basis, and the like, based on 100% by weight of the acoustic enhancement material.
As a specific embodiment of the above-mentioned acoustic enhancement material of the present invention, the dispersing agent includes a mixture of one or more of glycerin, HPMA, and liquid paraffin.
As a specific embodiment of the above-mentioned acoustic enhancement material of the present invention, the dry content of the auxiliary agent is 0-15% based on 100% of the total weight of the acoustic enhancement material.
In some embodiments of the invention, the auxiliary agent may be present in a dry basis of, for example, 1.62%, 3.64%, 3.70%, 5.84%, 14.33%, 3.80%, etc., based on 100% by weight of the acoustic enhancement material.
As a specific embodiment of the above acoustic enhancement material of the present invention, the auxiliary agent includes one or more of kaolin, diatomaceous earth, silica fume, bentonite, and montmorillonite.
In still another aspect, the present invention further provides a method for preparing the above-mentioned acoustic enhancement material, wherein the preparation method includes:
uniformly mixing the silicon-aluminum-titanium molecular sieve, the binder, the dispersing agent and/or the auxiliary agent to obtain a suspension, and forming the suspension to obtain the acoustic enhancement material, wherein the content of the silicon-aluminum-titanium molecular sieve is not less than 70 percent based on 100 percent of the total weight of the acoustic enhancement material.
The method for molding is not particularly required, and a person skilled in the art can reasonably select the method for molding according to actual operation needs, so long as the purpose of the invention can be realized. For example, when the acoustic enhancement material microspheres are to be prepared, the molding method may be spray drying, freeze molding, oil column molding, rolling ball method molding, or the like; when the acoustic reinforcement material block or the acoustic reinforcement material sheet is to be produced, molding may be performed by a hot air drying method.
In yet another aspect, the present invention also provides a speaker comprising one or more acoustic sensors, one or more housings, the one or more acoustic sensors in combination with the one or more housings forming the speaker rear cavity, wherein the speaker rear cavity is fitted with an acoustic enhancement material as described above.
In a final aspect, the invention also provides an electronic device, wherein the acoustic enhancement material described above is mounted in a speaker rear cavity of the electronic device.
As a specific embodiment of the electronic device according to the present invention, the electronic device includes a smart phone, a TWS headset, a pair of smart glasses, a smart watch, a VR device, an AR device, a tablet computer, or a light and thin notebook computer.
Compared with the traditional high-silicon aluminum molecular sieve, the silicon aluminum titanium molecular sieve provided by the invention has heavier bulk density, and can obtain heavier vibration quality under the same filling volume, so that the silicon aluminum titanium molecular sieve has better acoustic performance, and under the same condition, the delta F0 of the silicon aluminum titanium molecular sieve is 20-30 percent higher than the delta F0 of the traditional high-silicon aluminum molecular sieve. Compared with the traditional titanium-silicon molecular sieve, the silicon-aluminum-titanium molecular sieve provided by the invention has the advantages that because the framework contains aluminum element, uniform slurry is easy to form in the slurry forming process, so that the sphericity of the prepared finished product acoustic enhancement material microsphere is higher.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for the description of the embodiments will be briefly described, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings may be obtained according to the drawings without inventive effort for a person skilled in the art.
Fig. 1 is a scanning electron microscope image of molecular sieve 1# provided in example 1 of the present invention.
Fig. 2 is a scanning electron microscope image of molecular sieve 2# provided in example 2 of the present invention.
FIG. 3 is a scanning electron microscope image of sample No. 1 provided in example 1-1 of the present invention.
FIG. 4 is a scanning electron microscope image of sample No. 2 provided in example 2-1 of the present invention.
FIG. 5 is a scanning electron microscope image of reference sample # 2 provided in comparative example 2.
FIG. 6 is a scanning electron microscope image of reference sample 3# provided in comparative example 3.
Detailed Description
The "range" disclosed herein is given in the form of a lower limit and an upper limit. There may be one or more lower limits and one or more upper limits, respectively. The given range is defined by selecting a lower limit and an upper limit. The selected lower and upper limits define the boundaries of the particular ranges. All ranges defined in this way are combinable, i.e. any lower limit can be combined with any upper limit to form a range. For example, ranges of 60-120 and 80-110 are listed for specific parameters, with the understanding that ranges of 60-110 and 80-120 are also contemplated. Furthermore, if the minimum range values listed are 1 and 2 and the maximum range values listed are 3,4 and 5, then the following ranges are all contemplated: 1-3, 1-4, 1-5, 2-3, 2-4 and 2-5.
In the present invention, unless otherwise indicated, the numerical range "a-b" represents a shorthand representation of any combination of real numbers between a and b, where a and b are both real numbers. For example, the numerical range "0-5" means that all real numbers between "0-5" have been listed throughout this disclosure, and "0-5" is only a shorthand representation of a combination of these values.
The term "two" as used in the present specification means "at least two" unless specifically indicated otherwise.
In the present invention, all the embodiments and preferred embodiments mentioned in the present invention may be combined with each other to form new technical solutions, unless otherwise specified.
In the present invention, all technical features mentioned in the present invention and preferred features may be combined with each other to form a new technical solution unless specifically stated otherwise.
In the present invention, all the steps mentioned herein may be performed sequentially or randomly, but are preferably performed sequentially, unless otherwise specified. For example, the method comprises steps (a) and (b), meaning that the method may comprise steps (a) and (b) performed sequentially, or may comprise steps (b) and (a) performed sequentially. For example, the method may further include step (c), which means that step (c) may be added to the method in any order, for example, the method may include steps (a), (b) and (c), may include steps (a), (c) and (b), may include steps (c), (a) and (b), and the like.
In the present invention, the term "comprising" as referred to herein means open or closed unless otherwise specified. For example, the term "comprising" may mean that other elements not listed may be included or that only listed elements may be included.
The ZSM-5 molecular sieve with high silica-alumina ratio is a molecular sieve material known in the art, can be directly purchased in the market, and can also be synthesized according to a literature method. The ZSM-5 molecular sieves used in the examples of the present invention had silica alumina ratios of 200 and 400.
All of the starting materials used in the present invention are commercially available or can be prepared by methods known in the art.
The present invention will be described in further detail with reference to the accompanying drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. The following described embodiments are some, but not all, examples of the present invention and are merely illustrative of the present invention and should not be construed as limiting the scope of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Silicon aluminum titanium molecular sieve examples
Example 1
The embodiment provides a silicon-aluminum-titanium molecular sieve which is prepared by a method comprising the following steps:
sequentially adding 500g of 30wt% silica sol, 89g of aluminum stearyl sulfate, 50g of tetrabutyl titanate, 200g of tetrapropyl ammonium bromide, 30g of sodium hydroxide and 600g of water into a 2L reaction kettle, sealing the reaction kettle, heating to 150 ℃ for crystallization for 96 hours according to the heating rate of 2 ℃/min, taking out slurry after crystallization, centrifugally separating the slurry, continuously washing the separated dry base until the pH value of the washing liquid is 8-9, stopping washing, drying the separated dry base at 110 ℃, enabling the water content of the dried dry base to be less than 2%, placing the dried dry base in a muffle furnace after drying, and roasting for 4 hours at 500 ℃ to obtain the silicon aluminum titanium molecular sieve, and marking the silicon aluminum titanium molecular sieve as molecular sieve No. 1.
In the molecular sieve 1# prepared in the embodiment, the mass ratio of silicon to aluminum elements is 10:1, and the mass ratio of silicon to titanium elements is 10:1.
Example 2
The embodiment provides a silicon-aluminum-titanium molecular sieve which is prepared by a method comprising the following steps:
513g of 30wt% silica sol, 2g of aluminum nonanitrate, 5.7g of titanium tetrachloride, 400g of 25wt% tetrapropylammonium hydroxide, 40g of sodium hydroxide, 7.8g of seed crystal (ZSM-5 molecular sieve) and 600g of water are sequentially added into a 2L reaction kettle, the reaction kettle is closed, the temperature is increased to 200 ℃ according to the heating rate of 2 ℃/min for crystallization for 12 hours, slurry is taken out after crystallization, centrifugal separation is carried out on the slurry, the separated dry base is continuously washed until the washing solution stops at a pH value of the washing solution is between 8 and 9, the separated dry base is dried at 110 ℃, the water content of the dried dry base is less than 2%, the dried dry base is placed in a muffle furnace for roasting for 4 hours at 550 ℃ to obtain the silicon aluminum titanium molecular sieve, and the molecular sieve is marked as molecular sieve No. 2.
In the molecular sieve 2# prepared in the embodiment, the mass ratio of silicon to aluminum elements is 500:1, the mass ratio of silicon to titanium elements is 50:1, and the addition amount of the auxiliary agent is 2.80%.
Example 3
The embodiment provides a silicon-aluminum-titanium molecular sieve which is prepared by a method comprising the following steps:
adding 500g of tetraethoxysilane, 3.2g of aluminum isopropoxide, 18.5g of titanyl sulfate, 50g of n-butylamine, 15g of sodium hydroxide, 2g of seed crystal (CHA structure, SSZ-13 molecular sieve) and 900g of water into a 2L reaction kettle in sequence, sealing the reaction kettle, heating to 100 ℃ according to the heating rate of 2 ℃/min for crystallization for 72 hours, taking out slurry after crystallization, carrying out centrifugal separation on the slurry, continuously washing the separated dry base until the pH value of the washing solution is between 8 and 9, stopping washing, separating the dry base, drying the dry base at 110 ℃, placing the dried dry base with the water content of <2 percent in a muffle furnace for roasting for 4 hours at 550 ℃ after drying, and obtaining the silicon-aluminum-titanium molecular sieve marked as molecular sieve 3#.
In the molecular sieve 3# prepared in the embodiment, the mass ratio of silicon to aluminum elements is 160:1, the mass ratio of silicon to titanium elements is 18.4:1, and the addition amount of the auxiliary agent is 1.32%.
Example 4
The embodiment provides a silicon-aluminum-titanium molecular sieve which is prepared by a method comprising the following steps:
sequentially adding 300g of white carbon black, 10g of pseudo-boehmite, 80g of tetrabutyl titanate, 300g of ethylamine, 80g of sodium hydroxide, 2g of seed crystal (MOR structure, mordenite) and 800g of water into a 2L reaction kettle, sealing the reaction kettle, heating to 140 ℃ for crystallization for 48 hours according to the heating rate of 2 ℃/min, taking out slurry after crystallization, centrifugally separating the slurry, continuously washing separated dry bases until the pH value of a washing solution is 8-9, stopping washing until the separated dry bases are dried at 110 ℃, drying the dried dry bases until the water content of the dried dry bases is less than 2%, and placing the dried dry bases in a muffle furnace for roasting for 4 hours at 500 ℃ to obtain a silicon aluminum titanium molecular sieve, wherein the molecular sieve is marked as a molecular sieve No. 4.
In the molecular sieve 4# prepared in the embodiment, the mass ratio of silicon to aluminum elements is 38:1, the mass ratio of silicon to titanium elements is 12.7:1, and the addition amount of the auxiliary agent is 0.61%.
Example 5
The embodiment provides a silicon-aluminum-titanium molecular sieve which is prepared by a method comprising the following steps:
500g of water glass with the silicon oxide content of 25wt%, 3.2g of aluminum chloride, 20g of tetrabutyl titanate, 200g of 25wt% of tetraethylammonium hydroxide, 30g of sodium hydroxide, 5g of seed crystal (FER structure, ferrierite) and 600g of water are sequentially added into a 2L reaction kettle, the reaction kettle is closed, the temperature is increased to 180 ℃ according to the heating rate of 2 ℃/min for crystallization for 32h, after the crystallization is finished, slurry is taken out, centrifugal separation is carried out on the slurry, continuous washing is carried out on separated dry base until the washing is stopped until the pH value of washing liquid is between 8 and 9, the separated dry base is dried at 110 ℃, the water content of the dried dry base is less than 2%, the dry base is baked for 4h in a muffle furnace at 550 ℃ after drying, and the molecular sieve 5# molecular sieve is obtained.
In the molecular sieve 5# prepared in the embodiment, the mass ratio of silicon to aluminum elements is 90:1, the mass ratio of silicon to titanium elements is 22.5:1, and the addition amount of the auxiliary agent is 3.82%.
Example 6
The embodiment provides a silicon-aluminum-titanium molecular sieve which is prepared by a method comprising the following steps:
600g of 30wt% silica sol, 3g of 20wt% aluminum sol, 15g of tetrabutyl titanate, 300g of triethylamine, 30g of potassium hydroxide, 2g of seed crystal (AFI structure, aluminum phosphate molecular sieve) and 600g of water are sequentially added into a 2L reaction kettle, the reaction kettle is closed, the temperature is increased to 150 ℃ according to the heating rate of 2 ℃/min for crystallization for 48 hours, slurry is taken out after the crystallization is finished, centrifugal separation is carried out on the slurry, the washing is stopped until the pH value of the washing liquid is between 8 and 9, the separated dry base is dried under the condition of 110 ℃, the water content of the dried dry base is less than 2%, and the dry base is placed in a muffle furnace for roasting for 4 hours under the condition of 550 ℃ after the drying, so that the silicon aluminum titanium molecular sieve is marked as molecular sieve 6#.
In the molecular sieve 6# prepared in the embodiment, the mass ratio of silicon to aluminum elements is 265:1, the mass ratio of silicon to titanium elements is 40.2:1, and the addition amount of the auxiliary agent is 1.09%.
Example 7
The embodiment provides a silicon-aluminum-titanium molecular sieve which is prepared by a method comprising the following steps:
sequentially adding 600g of 30wt% silica sol, 5g of aluminum stearyl sulfate, 15g of tetrabutyl titanate, 300g of diethylamine, 30g of sodium hydroxide, 2g of seed crystal (MWW structure, MCM-22 molecular sieve) and 600g of water into a 2L reaction kettle, sealing the reaction kettle, heating to 150 ℃ according to the heating rate of 2 ℃/min for crystallization for 48 hours, taking out slurry after crystallization, carrying out centrifugal separation on the slurry, continuously washing the separated dry base until the pH value of the washing liquid is between 8 and 9, stopping washing, drying the separated dry base at 110 ℃, roasting the dried dry base with the water content of <2%, and placing the dried dry base in a muffle furnace for 4 hours at 550 ℃ after drying to obtain the silicon aluminum titanium molecular sieve, and marking the molecular sieve as 7#.
In the molecular sieve 7# prepared in the embodiment, the mass ratio of silicon to aluminum elements is 207.25:1, the mass ratio of silicon to titanium elements is 39.78:1, and the addition amount of the auxiliary agent is 1.09%.
Acoustic enhancement material embodiments
Example 1-1
The present embodiment provides an acoustic enhancement material, which is manufactured by a method comprising the steps of:
100g of molecular sieve No. 1, 30g of water-based acrylate adhesive with the dry basis (solid component) content of 40wt%, 1g of glycerol and 100g of water are taken and mixed, fully stirred for 1h, and formed by a spray drying method, thus obtaining the granular acoustic enhancement material, namely the acoustic enhancement material microsphere, wherein the median diameter D50 of the sample is 359 mu m, and the sample is marked as sample No. 1.
In the acoustic reinforcing material prepared in this example, the mass content of the molecular sieve was 88.50%, the mass content of the binder was 10.62%, the mass content of the dispersant on a dry basis was 0.88%, and the mass content of the auxiliary agent on a dry basis was 0%, wherein the content of the binder was based on the content of the solid component in the binder.
Example 2-1
The present embodiment provides an acoustic enhancement material, which is manufactured by a method comprising the steps of:
100g of molecular sieve No. 2, 70g of 30wt% silica sol, 24g of kaolin and 120g of water are taken, fully stirred for 1h, and molded by an oil column molding method to obtain a granular acoustic reinforcing material, namely an acoustic reinforcing material microsphere, wherein the median diameter D50 of the sample is 342 mu m, and the sample is marked as sample No. 2.
In the acoustic reinforcing material prepared in this example, the mass content of the molecular sieve was 70.92%, the mass content of the binder was 14.75%, the mass content of the dispersant on a dry basis was 0.00%, and the mass content of the auxiliary agent on a dry basis was 14.33%, wherein the content of the binder was based on the content of the solid component in the binder.
Example 3-1
The present embodiment provides an acoustic enhancement material, which is manufactured by a method comprising the steps of:
taking 100g of molecular sieve 3#, 10g of aluminum sol with 20wt% content (aluminum oxide), 1g of glycerin, 2g of diatomite and 100g of water, fully stirring for 1h, and forming by a spray drying method to obtain a granular acoustic reinforcing material, namely an acoustic reinforcing material microsphere, wherein the median diameter D50 of the sample is 98 mu m, and the sample is marked as sample 3#.
In the acoustic reinforcing material prepared in this example, the mass content of the molecular sieve was 95.51%, the mass content of the binder was 1.91%, the mass content of the dispersant on a dry basis was 0.96%, and the mass content of the auxiliary agent on a dry basis was 1.62%, wherein the content of the binder was based on the content of the solid component in the binder.
Example 4-1
The present embodiment provides an acoustic enhancement material, which is manufactured by a method comprising the steps of:
100g of molecular sieve 4#, 25g of water glass with the silicon oxide content of 25%, 1g of liquid paraffin, 5g of silica fume and 100g of water are taken, fully stirred for 1h, and formed by a spray drying method, so that a granular acoustic reinforcing material, namely an acoustic reinforcing material microsphere, is obtained, the median diameter D50 of the sample is 111 mu m, and the sample is marked as sample 4#.
In the acoustic reinforcing material prepared in this example, the mass content of the molecular sieve was 89.69%, the mass content of the binder was 5.61%, the mass content of the dispersant on a dry basis was 0.90%, and the mass content of the auxiliary agent on a dry basis was 3.80%, wherein the content of the binder was based on the content of the solid component in the binder.
Example 5-1
The present embodiment provides an acoustic enhancement material, which is manufactured by a method comprising the steps of:
taking 100g of molecular sieve No. 5, 10g of epoxy binder, 0.5g of HPMA, 5g of bentonite and 100g of water, fully stirring for 1h, and forming by a rolling ball method to obtain a granular acoustic reinforcing material, namely an acoustic reinforcing material microsphere, wherein the median diameter D50 of the sample is 312 mu m, and the sample is marked as sample No. 5.
In the acoustic reinforcing material prepared in this example, the mass content of the molecular sieve was 87.15%, the mass content of the binder was 8.71%, the mass content of the dry basis of the dispersant was 0.44%, and the mass content of the dry basis of the auxiliary agent was 3.70%, wherein the content of the binder was calculated as the content of the solid component in the binder.
Example 6-1
The present embodiment provides an acoustic enhancement material, which is manufactured by a method comprising the steps of:
taking 100g of molecular sieve 6#, 12g of polyurethane binder, 0.5g of glycerol, 5g of bentonite and 100g of water, fully stirring for 1h, placing in a block mold, and forming by a hot air drying method to obtain a block-shaped acoustic reinforcing material, namely an acoustic reinforcing material block, wherein the size of the sample is 2mm multiplied by 4mm multiplied by 6mm, and the sample is marked as sample 6#.
In the acoustic reinforcing material prepared in this example, the mass content of the molecular sieve was 85.65%, the mass content of the binder was 10.28%, the mass content of the dry basis of the dispersant was 0.43%, and the mass content of the dry basis of the auxiliary agent was 3.64%, wherein the content of the binder was calculated as the content of the solid component in the binder.
Example 7-1
The present embodiment provides an acoustic enhancement material, which is manufactured by a method comprising the steps of:
taking 100g of molecular sieve 7#, 13g of pseudo-boehmite, 0.5g of glycerol, 8g of montmorillonite and 100g of water, fully stirring for 1h, pouring into a plane mould, forming by a hot air drying method, cutting the formed sheet into a plurality of samples of 2mm multiplied by 4mm multiplied by 0.2mm, namely the acoustic enhancement material sheet, and marking the acoustic enhancement material sheet as sample 7#.
In the acoustic reinforcing material prepared in this example, the mass content of the molecular sieve was 85.91%, the mass content of the binder was 7.82%, the mass content of the dispersant on a dry basis was 0.43%, and the mass content of the auxiliary agent on a dry basis was 5.84%, wherein the content of the binder was based on the content of the solid component in the binder.
Comparative example 1
The present comparative example provides an acoustic enhancement material made by a process comprising the steps of:
mixing 100g of ZSM-5 molecular sieve with a silicon-aluminum mass ratio of 400, 30g of water-based acrylate adhesive with a dry content of 40%, 1g of glycerol and 100g of water, fully stirring for 1h, and forming by a spray drying method to obtain a granular acoustic enhancement material, namely an acoustic enhancement material microsphere, wherein the median diameter D50 of the sample is 370 mu m, and the sample is marked as reference sample No. 1.
Comparative example 2
The present comparative example provides an acoustic enhancement material made by a process comprising the steps of:
100g of ZSM-5 molecular sieve with the silicon-aluminum mass ratio of 200, 10g of aluminum sol with the content of 20 percent (aluminum oxide), 1g of glycerol, 2g of kieselguhr and 100g of water are taken, fully stirred for 1h, and formed by a spray drying method, thus obtaining the granular acoustic enhancement material, namely the acoustic enhancement material microsphere, wherein the median diameter D50 of the sample is 95 mu m and marked as reference sample No. 2.
Comparative example 3
The present comparative example provides an acoustic enhancement material made by a process comprising the steps of:
preparation of molecular sieves:
adding 513g of 30wt% silica sol, 1g of aluminum nonanitrate, 3g of titanium tetrachloride, 400g of 25wt% tetrapropylammonium hydroxide, 40g of sodium hydroxide, 7.8g of seed crystal (ZSM-5 molecular sieve) and 600g of water into a 2L reaction kettle in sequence, sealing the reaction kettle, heating to 200 ℃ at the speed of 2 ℃/min for crystallization for 12 hours, taking out slurry after crystallization, centrifuging the slurry, continuously washing the separated dry base until the pH value of the washing solution is between 8 and 9, stopping washing, drying the separated dry base at 110 ℃, roasting the dried dry base at the temperature of <2%, placing the dried dry base in a muffle furnace at the temperature of 550 ℃ after drying for 4 hours to obtain a molecular sieve, marking as reference molecular sieve 1#, wherein the mass ratio of silicon to aluminum element in the reference molecular sieve 1# is 665:1 and the mass ratio of silicon to titanium element is 56:1 according to the feeding amount.
Preparation of acoustic enhancement materials:
mixing 100g of reference molecular sieve No. 1, 10g of 20wt% silica sol, 1g of glycerol and 100g of water, fully stirring for 1h, and forming by a spray drying method to obtain a granular acoustic enhancement material, namely an acoustic enhancement material microsphere, wherein the median diameter D50 of the sample is 99um, and the sample is marked as reference sample No. 3.
Test example 1
Respectively taking 0.14g of sample 1# -sample 7# (wherein sample 1# -sample 5# is microsphere, sample 6# is block material and sample 7# is sheet material) and reference sample 1# -reference sample 3#, performing acoustic performance test on sample 1# -sample 7# -and reference sample 1# -reference sample 3#, and testing delta F0 of sample 1# -sample 7# and reference sample 1# -reference sample 3# -by using a surface resistance tester. Wherein the tests are all carried out by the conventional method in the art, for example, the acoustic performance test can be carried out by referring to the method of measuring electrical impedance shown in paragraphs 0049-0054 of Chinese patent CN 105049997A. In this test example, the test environment is: the cavity is a 0.2cc speaker module.
Reliability test of samples: the sample was first placed in an oven at 85 c with 85% humidity for 72 hours, then removed and tested for acoustic performance according to the method described above.
The test result data obtained in this test example are shown in table 1 below.
TABLE 1
Figure BDA0003378455460000121
Figure BDA0003378455460000131
As can be seen from the test results shown in table 1 above, compared with the microspheres of comparative examples 1-2, which are the microspheres of the acoustic enhancement materials prepared by using ZSM-5 molecular sieve conventionally used in the art as the main component, i.e., reference sample 1# and reference sample 2#, the microspheres of examples 1-5 of the present invention, which are the microspheres of sample 1, sample 5#, which are prepared by using the sialyltitanium molecular sieve as the main component, have more excellent acoustic properties; after the microspheres are treated under the high-temperature and high-humidity conditions, the acoustic performance of a sample 1, a sample 5, is lower than that of a reference sample 1 and a reference sample 2, which shows that the reliability of the microspheres prepared by using the silicon-aluminum-titanium molecular sieve as a main component in the embodiment of the invention is better than that of the microspheres prepared by using the reference sample 1 and the reference sample 2 under the high-temperature and high-humidity conditions.
Test example 2
And respectively carrying out scanning electron microscope analysis on the molecular sieve 1# and the molecular sieve 2# to obtain scanning electron microscope images respectively shown in fig. 1 and 2.
Scanning electron microscope analyses were performed on sample 1# provided in example 1-1 of the present invention, sample 2# provided in example 2-1 of the present invention, and reference sample 2# provided in comparative example 2, and reference sample 3# provided in comparative example 3, respectively, and the resulting scanning electron microscope graphs are shown in fig. 3 to 6, respectively.
As can be seen from the sem images shown in fig. 3 to 6, the sphericity of the microspheres of the acoustic enhancement material prepared using ZSM-5 molecular sieve in comparative example 2 and reference molecular sieve 1# in comparative example 3 (i.e., conventional titanium silicalite molecular sieve) is poor compared to sample 1# provided in example 1-1 of the present invention and sample 2# provided in example 2-1 of the present invention.
The foregoing description of the embodiments of the invention is not intended to limit the scope of the invention, so that the substitution of equivalent elements or equivalent variations and modifications within the scope of the invention shall fall within the scope of the patent. In addition, the technical features and the technical features, the technical features and the technical invention can be freely combined for use.

Claims (22)

1. The silicon-aluminum-titanium molecular sieve is characterized in that the skeleton of the silicon-aluminum-titanium molecular sieve contains silicon, aluminum and titanium elements, the mass ratio of the silicon to the aluminum elements is 1-500:1, and the mass ratio of the silicon to the titanium elements is 10-50:1.
2. The molecular sieve according to claim 1, wherein the molecular sieve comprises any one of MFI, CHA, FER, MOR, AFI, BEA, MWW, and has a grain size of 20-1000nm.
3. The molecular sieve according to claim 1 or 2, wherein the molecular sieve is prepared by uniformly mixing raw materials and water, crystallizing the obtained mixture at 100-200 ℃, centrifuging, washing, drying and roasting;
wherein the raw materials comprise a silicon source, an aluminum source, a titanium source, a template agent, an alkali source and an auxiliary agent, and the use amount of the auxiliary agent is 0-5% based on 100% of the total weight of the silicon-aluminum-titanium molecular sieve.
4. The molecular sieve of claim 3, wherein the silicon source comprises one or more of silica sol, white carbon black, silica gel, ethyl orthosilicate, water glass.
5. The molecular sieve according to claim 3, wherein the aluminum source comprises one or more of aluminum isopropoxide, aluminum nitrate, aluminum sulfate, pseudo-boehmite, aluminum chloride, aluminum sol.
6. A silicoaluminotitanium molecular sieve according to claim 3, wherein the titanium source comprises one or a mixture of several of tetrabutyl titanate, titanium tetrachloride, titanyl sulfate.
7. A silicoaluminotitanium molecular sieve according to claim 3 wherein the templating agent comprises one or a mixture of several of tetrapropylammonium hydroxide, tetrapropylammonium bromide, n-butylamine, ethylamine, tetraethylammonium hydroxide, triethylamine, diethylamine.
8. A silicoaluminotitanium molecular sieve according to claim 3, wherein the alkali source comprises one or a mixture of two of sodium hydroxide and potassium hydroxide.
9. A silicoaluminotitanium molecular sieve according to claim 3, wherein the adjunct comprises a molecular sieve having any one of the structures MFI, CHA, FER, MOR, AFI, BEA, MWW.
10. The method for preparing the silicon-aluminum-titanium molecular sieve according to any one of claims 1 to 9, comprising:
uniformly mixing raw materials and water, carrying out crystallization reaction on the obtained mixed solution at the temperature of 100-200 ℃, centrifuging the obtained slurry after the reaction is finished, continuously washing the separated dry base until the pH value of the washing solution is 8-9, stopping washing, drying the separated dry base to ensure that the water content of the dried dry base is less than 2%, and finally roasting the dried dry base at the temperature of 400-650 ℃ to obtain the silicon-aluminum-titanium molecular sieve;
wherein the raw materials comprise a silicon source, an aluminum source, a titanium source, a template agent, an alkali source and an auxiliary agent, and the use amount of the auxiliary agent is 0-5% based on 100% of the total weight of the silicon-aluminum-titanium molecular sieve.
11. An acoustic enhancement material, characterized in that the acoustic enhancement material is prepared by uniformly mixing the silicon-aluminum-titanium molecular sieve, the binder, the dispersing agent and/or the auxiliary agent according to any one of claims 1-9, and then molding, wherein the content of the silicon-aluminum-titanium molecular sieve is not less than 70 percent based on the total weight of the acoustic enhancement material being 100 percent.
12. The acoustic enhancement material of claim 11, wherein the shape of the acoustic enhancement material comprises microspheres, blocks, or flakes; wherein the size of the microsphere is between 50 and 300 mu m.
13. The acoustic reinforcement material according to claim 11 or 12, wherein the content of the binder is 1-15% based on 100% of the total weight of the acoustic reinforcement material; wherein the content of the binder is calculated by the content of the solid component in the binder.
14. The acoustic reinforcement material of claim 13, wherein the binder comprises an inorganic binder and/or an organic binder;
wherein the inorganic binder comprises one or a mixture of a plurality of silica sol, alumina sol, water glass and pseudo-boehmite; the organic binder comprises one or a mixture of a plurality of acrylic acid esters, epoxy compounds and polyurethane organic binders.
15. Acoustic reinforcement material according to claim 11 or 12, characterized in that the dry content of the dispersant is 0-1% based on 100% of the total weight of the acoustic reinforcement material.
16. The acoustic enhancement material of claim 15, wherein the dispersant comprises a mixture of one or more of glycerin, HPMA, liquid paraffin.
17. Acoustic reinforcement material according to claim 11 or 12, characterized in that the dry content of the auxiliary agent is 0-15% based on 100% of the total weight of the acoustic reinforcement material.
18. The acoustic reinforcement material of claim 17, wherein the auxiliary agent comprises a mixture of one or more of kaolin, diatomaceous earth, silica fume, bentonite, montmorillonite.
19. A method of producing an acoustic enhancement material according to any one of claims 11 to 18, comprising:
uniformly mixing the silicon-aluminum-titanium molecular sieve, the binder, the dispersing agent and/or the auxiliary agent according to any one of claims 1-9 to obtain a suspension, and forming the suspension to obtain the acoustic enhancement material, wherein the content of the silicon-aluminum-titanium molecular sieve is not less than 70 percent based on 100 percent of the total weight of the acoustic enhancement material.
20. A loudspeaker comprising one or more acoustic sensors, one or more housings, the one or more acoustic sensors in combination with the one or more housings forming the loudspeaker rear cavity, wherein the loudspeaker rear cavity is fitted with an acoustic enhancement material as claimed in any one of claims 11 to 18.
21. An electronic device, characterized in that an acoustic enhancement material according to any of claims 11-18 is fitted in a speaker rear cavity of the electronic device.
22. The electronic device of claim 21, wherein the electronic device comprises a smart phone, a TWS headset, a smart glasses, a smart watch, a VR device, an AR device, a tablet computer, or a lightweight notebook computer.
CN202111425964.7A 2021-11-26 2021-11-26 Silicon-aluminum-titanium molecular sieve, acoustic reinforcing material, preparation method of silicon-aluminum-titanium molecular sieve, loudspeaker and electronic equipment Pending CN116177559A (en)

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