Organosilicon light-cured resin, high-damping horn UV center glue containing same, and preparation method and application of organosilicon light-cured resin

By preparing silicone photocuring resin with interpenetrating network structure and polyurethane acrylic resin, a high-damping UV center glue is formed, which solves the problems of poor compatibility and complex processes in the prior art, and achieves high damping performance and rapid curing effects.

CN119859158APending Publication Date: 2025-04-22GUOGUANG ELECTRIC COMPANY LIMITED
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Patent Information

Application Number
CN202510166710.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-02-14
Publication Date
2025-04-22

AI Technical Summary

Technical Problem

In the prior art, acoustic damping glues prepared using silicone and acrylic resin compound have poor compatibility and complex hot press coating processes, which are difficult to meet the needs of single-layer sound films and rapid curing production.

Method used

By preparing silicone photocuring resin with an interpenetrating network structure, and combining it with polyurethane acrylic resin, reactive diluents, photoinitiators, etc., a high-damping UV central glue is formed, and the UV curing process is used to improve production efficiency.

Benefits of technology

It significantly improves the damping performance and temperature domain of the glue, meets the high damping effect of the single-layer diaphragm, and greatly improves the production efficiency through the UV curing process, far exceeding the traditional solvent-based damping glue.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention provides organic silicon light-cured resin, high-damping horn UV center glue containing the organic silicon light-cured resin and a preparation method and application of the high-damping horn UV center glue. Diethoxydimethylsilane, phenyltriethoxysilane and vinyltriethoxysilane are subjected to a hydrolytic condensation reaction, and the organic silicon light-cured resin is obtained; the high-damping horn UV center glue comprises the following components in percentage by weight: 10%-40% of the organic silicon light-cured resin, 25%-30% of acrylic prepolymer resin, 30%-45% of a reactive diluent, 3%-7% of a photoinitiator and 2%-8% of an adhesion promoter. The high-damping horn UV center glue has a high damping value and a wide damping temperature range, can be cured by UV, has the characteristic of rapid curing, and can greatly improve the production efficiency of factories.
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Description

Technical Field

[0001] The invention belongs to the technical field of ultraviolet light curing adhesives, and relates to an organosilicon light curing resin, a high damping speaker UV center glue containing the organosilicon resin, and a preparation method and application thereof. Background Art

[0002] With the rapid development of electronic products such as VR and AR, customers have higher and higher requirements for the sound quality experience of these products. They not only need to have high reliability, but also require the speakers to have low distortion and support multi-scene 3D sound fields. Related research shows that adding wide temperature range and high damping glue to the vibration system can significantly reduce the distortion of micro speakers and improve the acoustic performance of the speakers.

[0003] CN118325574A discloses an acoustic damping glue prepared by compounding organic silicon and acrylic resin. The glue is applied to a composite sound film after physical blending and hot pressing to improve the damping effect of the sound film. However, there are two problems in this process. First, pure organic silicon itself has poor compatibility with acrylate when simply physically blended. After simple stirring and blending, stratification will occur after a period of storage. Second, the glue is used in a composite sound film and is not applicable to a single-layer sound film. In addition, the hot pressing coating process is complicated and requires high-temperature baking at 105°C, which can easily cause deformation of the sound film.

[0004] CN102911634A discloses a core glue prepared by silicone-modified polyurethane, which mainly improves the temperature resistance of the glue but does not improve the damping effect. In addition, the glue is moisture-cured and requires a long curing time, which makes it difficult to meet the needs of rapid curing production in factories.

[0005] The speaker center glue in the micro speaker is mainly used as glue to bond the sound membrane and the voice coil. It not only fixes the voice coil and the sound membrane, but also has a high damping center glue which can greatly improve the electroacoustic performance of the speaker, reduce the distortion of the micro speaker, and improve the acoustic performance of the speaker. Summary of the invention

[0006] In view of the deficiencies of the prior art, the purpose of the present invention is to provide an organosilicon photocurable resin and a high-damping speaker UV center glue containing the same and a preparation method and application thereof. The organosilicon photocurable resin of the present invention is combined with a polyurethane acrylic resin, a polar group- and large side chain active diluent, a photoinitiator, etc. to prepare a high-damping UV glue with an interpenetrating network (IPN), and at the same time, through the synergistic effects of strong hydrogen bonds, high steric hindrance, and microphase separation, the damping of the glue is significantly improved. It is applied to the center glue part of the speaker, which can not only meet the high damping effect of a single-layer diaphragm, but also use a UV curing process to greatly improve the production efficiency of the factory.

[0007] In order to achieve the purpose of the invention, the present invention adopts the following technical solutions:

[0008] In one aspect, the present invention provides an organosilicon photocurable resin having the following structure:

[0009]

[0010] wherein x=0-1.66 (e.g., 0, 0.2, 0.4, 0.6, 0.8, 1.2, 1.4, 1.6 or 1.66), y=0-1.39 (e.g., 0, 0.2, 0.4, 0.6, 0.8, 1.2 or 1.39), and n=an integer from 1 to 5 (e.g., 1, 2, 3, 4 or 5).

[0011] On the other hand, the present invention provides a method for preparing the above-mentioned organosilicon photocurable resin, the preparation method comprising the following steps:

[0012] Diethoxydimethylsilane, phenyltriethoxysilane and vinyltriethoxysilane undergo hydrolysis condensation reaction to obtain the organosilicon photocurable resin.

[0013] In the present invention, the reaction formula for preparing the organosilicon photocurable resin is as follows:

[0014]

[0015] Preferably, the molar ratio of diethoxydimethylsilane, phenyltriethoxysilane and vinyltriethoxysilane is 1:(1-2):(1-3), for example 1:1:1, 1:1:1.5, 1:1:1.8, 1:1:2, 1:1:2.2, 1:1:2.5, 1:1:2.8, 1:1:3, 1:1.2:1, 1:1.2:1.2, 1:1.2:1.5, 1:1.2:1.8, 1:1.2:2, 1:1.2:2.2, 1:1.2:2.4, 1:1.2:2.6, 1:1.2:2.8, 1:1.2:3, 1:1.5:1, 1:1.5:1.2, 1:1.5:1.5, 1:1.5:1. :1.5:1.8, 1:1.5:2, 1:1.5:2.2, 1:1.5:2.4, 1:1.5:2.6, 1:1.5:2.8, 1:1.5:3, 1:1.8:1, 1:1.8:1.2, 1:1.8:1.5, 1:1.8:1.8, 1:1.8:2, 1:1.8:2.2, 1:1.8:2.4, 1:1.8:2.6, 1:1.8:2.8, 1:1.8:3, 1:2:1, 1:2:1.2, 1:2:1.5, 1:2:1.8, 1:2:2, 1:2:2.2, 1:2:2.4, 1:2:2.6, 1:2:2.8, 1:2:3, etc.

[0016] Preferably, the hydrolysis condensation reaction is carried out under nitrogen protection.

[0017] Preferably, the hydrolysis condensation reaction is carried out in the presence of an acidic catalyst.

[0018] Preferably, the acidic catalyst is a hydrochloric acid solution.

[0019] Preferably, the hydrolysis condensation reaction is carried out at room temperature (20-35°C, such as 20°C, 25°C, 28°C, 30°C, 33°C or 35°C), and the reaction time is 48-72 hours, such as 48 hours, 50 hours, 54 hours, 56 hours, 60 hours, 64 hours, 66 hours, 70 hours or 72 hours.

[0020] On the other hand, the present invention provides a high damping speaker UV center glue, wherein the high damping speaker UV center glue comprises the following components in weight percentage:

[0021]

[0022] In the present invention, the organosilicon photocurable resin contains carbon-carbon double bonds on the side chain, which can react with acrylic prepolymer resin, reactive diluent, etc. through cross-linking. At the same time, the side chain contains polar hydroxyl groups and relatively large phenyl groups. The more polar groups can generate strong hydrogen bonds with reactive diluents, etc., reducing the movement of the molecular chain. The large phenyl groups can reduce the flexibility of the molecular chain due to the volume steric effect, increase the friction resistance of the molecular chain movement, improve energy dissipation, and thus improve the damping performance of the glue.

[0023] The content of the organosilicon light-curable resin in the high damping speaker UV center glue of the present invention can be 10%, 13%, 15%, 18%, 20%, 23%, 25%, 28%, 30%, 33%, 35%, 38% or 40%, and more preferably 15% to 30%.

[0024] The content of the acrylic prepolymer resin in the high damping speaker UV center glue of the present invention can be 25%, 26%, 27%, 28%, 29% or 30%.

[0025] The content of the active diluent in the high damping speaker UV center glue of the present invention can be 30%, 33%, 35%, 38%, 40%, 42%, 44% or 45%, preferably 30% to 40%.

[0026] The content of the photoinitiator in the high damping speaker UV center glue of the present invention can be 3%, 3.5%, 4%, 4.5%, 5%, 5.5%, 6%, 6.5% or 7%, preferably 3% to 5%.

[0027] The content of the adhesion promoter in the high damping speaker UV center glue of the present invention can be 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, 5.5%, 6%, 6.5%, 7%, 7.5% or 8%.

[0028] Preferably, the acrylic prepolymer resin is selected from polyurethane acrylic resin.

[0029] Preferably, the polyurethane acrylic resin includes one or a combination of at least two of Taiwan Changxing Materials 61363, Taiwan Changxing Materials 61396, Songda SD810, Songda SD871, Sartomer CN9001 or Sartomer CN8003.

[0030] Preferably, the reactive diluent is selected from any one or a combination of at least two of monomers containing oxygen heterocycles, monomers containing polar groups or monomers containing long-chain structures.

[0031] Preferably, the monomer containing oxygen heterocycle is selected from any one of isobornyl acrylate, acryloyl morpholine or tetrahydrofurfuryl acrylate, or a combination of at least two thereof.

[0032] Preferably, the monomer containing a polar group is selected from any one of 2-hydroxyethyl acrylate, acrylic acid, 4-hydroxybutyl acrylate or 2-hydroxypropyl acrylate, or a combination of at least two thereof.

[0033] Preferably, the monomer containing a long-chain structure is selected from any one or a combination of at least two of isooctyl acrylate, butyl acrylate, lauric acrylate, isodecyl acrylate or isononyl acrylate.

[0034] Preferably, the photoinitiator is a free radical photoinitiator.

[0035] Preferably, the photoinitiator is selected from any one or a combination of at least two of (2,4,6-trimethylbenzoyl)di(p-tolyl)phosphine oxide, diphenyl(2,4,6-trimethylbenzoyl)phosphine oxide, 1-hydroxycyclohexylphenyl ketone, 2-hydroxy-2-methyl-1-phenylacetone, benzoin methyl ether, and ethyl 2,4,6-trimethylbenzoylphosphonate. When it is a combination of the initiators, it can be a mixture in any proportion.

[0036] Preferably, the adhesion promoter is selected from any one or a combination of at least two of 2-hydroxyethyl methacrylate phosphate, acrylic acid, γ-aminopropyltrimethoxysilane, and β-acryloxypropionic acid. When it is a combination of the adhesion promoters, it can be a mixture in any proportion.

[0037] On the other hand, the present invention provides a method for preparing the high damping speaker UV center glue as described above, the preparation method comprising the following steps:

[0038] The photocurable silicone resin, acrylic prepolymer, reactive diluent, photoinitiator and adhesion promoter are mixed evenly to obtain the high damping speaker UV center glue.

[0039] Preferably, the mixing is carried out under stirring at 20-70°C (e.g., 20°C, 25°C, 28°C, 30°C, 33°C, 35°C, 40°C, 45°C, 50°C, 55°C, 60°C, 65°C or 70°C).

[0040] Preferably, the mixing time is 30 min-3 h, for example 30 min, 40 min, 50 min, 1 h, 1.3 h, 1.5 h, 1.8 h, 2 h, 2.5 h, 2.8 h or 3 h.

[0041] Preferably, the stirring speed is 800-1000 rpm, for example, 800 rpm, 830 rpm, 850 rpm, 880 rpm, 900 rpm, 930 rpm, 950 rpm, 980 rpm or 1000 rpm.

[0042] Preferably, the preparation method is carried out in a reactor.

[0043] Preferably, the preparation method specifically includes the following steps: first, add silicone photocurable resin, acrylic prepolymer resin, and active diluent into a reaction kettle, heat to 40-70°C and stir for 20-50 minutes, control the stirring speed at 800-1000 rpm, add photoinitiator and adhesion promoter after the acrylic prepolymer resin is dissolved, continue stirring for 2 hours until the liquid is evenly mixed, and finally vacuum degas and stir for 10-30 minutes to obtain the high damping speaker UV center glue.

[0044] On the other hand, the present invention provides the use of the high damping speaker UV center glue in the speaker, for example, as described above.

[0045] In the present invention, the high damping refers to a damping value tanδ>0.3, for example, 0.35, 0.38, 0.4, 0.42, 0.45, 0.5, 0.6, 0.7, 0.8, 0.9, etc.

[0046] Compared with the prior art, the present invention has the following beneficial effects:

[0047] The organosilicon photocurable resin of the present invention contains carbon-carbon double bonds on the side chain, which can react with UV acrylic resin, reactive diluent, etc. through cross-linking. At the same time, the side chain contains polar hydroxyl groups and relatively large phenyl groups. The more polar groups can generate strong hydrogen bonds with acrylate monomers, etc., reducing the movement of the molecular chain. The large phenyl groups can reduce the flexibility of the molecular chain due to the volume steric effect, increase the friction resistance of the molecular chain movement, improve energy dissipation, and thus improve the damping performance of the glue.

[0048] In the high-damping speaker UV center glue of the present invention, the weak compatibility of the silicone photocurable resin and the acrylic prepolymer resin enables the glue to have microphase separation after curing. At the same time, the hydroxyl and phenyl groups of the silicone photocurable resin further increase the molecular chain force of the glue, thereby significantly improving the damping temperature range and the maximum damping value of the glue. The test results show that the maximum damping value of the glue can reach 0.98, and the damping temperature range (damping value>0.3) can be from -50°C to 120°C; at the same time, the glue introduces carbon-carbon double bonds into the silicone, so that the glue has the characteristic of rapid curing, which can greatly improve the efficiency of actual use, far exceeding the solvent damping glue currently on the market. BRIEF DESCRIPTION OF THE DRAWINGS

[0049] Figure 1 This is the infrared spectrum of the organosilicon photocurable resin PSI prepared in Preparation Example 1.

[0050] Figure 2 The organic silicon photocurable resin PSI prepared in Preparation Example 1 1 H-NMR spectrum.

[0051] Figure 3 The damping test results of Example 1, Comparative Example 1, Comparative Example 3 and Comparative Example 4 are shown. DETAILED DESCRIPTION

[0052] The technical solution of the present invention is further described below by specific implementation methods. It should be understood by those skilled in the art that the embodiments are only to help understand the present invention and should not be regarded as specific limitations of the present invention.

[0053] Preparation Example 1

[0054] A photocurable silicone resin, the preparation method of which comprises the following steps:

[0055] (1) At room temperature, under nitrogen protection, 100 g of diethoxydimethylsilane, phenyltriethoxysilane, and vinyltriethoxysilane in a molar ratio of 1:1:3 and 10 ml of a 37% mass concentration hydrochloric acid solution were added to a reactor containing 20 ml of distilled water.

[0056] (2) The mixture was stirred for 48 hours to complete the hydrolysis condensation reaction. The mixture was then filtered using a Buchner funnel to remove the gel in the mixture. The remaining solution was poured into a separatory funnel, diluted with distilled water, and then added dropwise to a large amount of cold methanol to obtain a precipitate. The precipitate was filtered and separated, washed three times with methanol, and then dried in a vacuum at 45°C for 24 hours to obtain a silicone photocurable resin PSI.

[0057] The prepared organosilicon photocurable resin PSI was characterized by Fourier transform infrared spectrometer (Nicolet6700, Thermo Fisher Scientific, USA). Figure 1 As shown, 3300cm -1 It is the -OH vibration absorption peak, 3030~2860cm -1 It is the absorption peak of -CH3 and -CH2, 1600cm -1 It is the characteristic absorption peak of benzene ring, 1018cm -1 It is the characteristic absorption peak of -Si-O-Si, and 810cm-1 is the infrared absorption peak of -C=C-.

[0058] The prepared organic silicon photocurable resin PSI was analyzed by using the German Bruker nuclear magnetic resonance spectrometer AV400. 1 H-NMR characterization, measured using CDCl3 as solvent 1 H-NMR (400MHz) spectrum Figure 2 As shown, 0.2ppm is the C-H3 absorption peak at methyl hydrogen 1, 5.8-6.1ppm is the absorption peak displayed at CH=CH22,3 position on vinyl, and 7.1-7.8ppm is the absorption peak at 4,5,6 shown in the phenyl hydrogen diagram. 1 H-NMR integration can obtain the signal intensity ratio of vinyl hydrogen to methyl hydrogen and phenyl hydrogen in the polymer as 1:1.44:2.00, respectively. From this, it can be obtained that the ratio of polydimethylsiloxane, phenylsiloxane and vinylsiloxane is 1:1.66:1.39, so the range of x is 0-1.66, and the range of y is 0-1.39.

[0059] Preparation Example 2

[0060] The difference from Preparation Example 1 is that the molar ratio of diethoxydimethylsilane, phenyltriethoxysilane and vinyltriethoxysilane is 1:1:1.

[0061] Preparation Example 3

[0062] The difference from Preparation Example 1 is that the molar ratio of diethoxydimethylsilane, phenyltriethoxysilane and vinyltriethoxysilane is 1:2:2.

[0063] Comparative Preparation Example 1

[0064] (1) At room temperature and under nitrogen protection, diethoxydimethylsilane, phenyltriethoxysilane in a 1:1 molar ratio and an appropriate amount of hydrochloric acid solution are added to a reaction kettle containing an appropriate amount of distilled water.

[0065] (2) The mixture was stirred for 48 hours to complete the hydrolysis condensation reaction. The mixture was then filtered using a Buchner funnel to remove the gel in the mixture. The remaining solution was poured into a separatory funnel, diluted with distilled water, and then added dropwise to a large amount of cold methanol to obtain a precipitate. The precipitate was filtered and separated, washed three times with methanol, and then dried in a vacuum at 45°C for 24 hours to obtain silicone resin A.

[0066] Example 1

[0067] This embodiment provides a high damping speaker UV center glue, which includes the following components in weight percentage:

[0068]

[0069] The preparation method comprises the following steps: adding the organosilicon light-curing resin prepared in Example 1 and the polyurethane acrylic resin SD871 into a stirring container of a non-intrusive homogenizer, then adding a reactive diluent (including 10% of 2-hydroxyethyl acrylate, 10% of isooctyl acrylate, and 20% of isobornyl acrylate), then adding a photoinitiator (2,4,6-trimethylbenzoyl) di(p-tolyl) phosphine oxide and an adhesion promoter β-acryloxy propionic acid, stirring at a temperature of 25° C., stirring in a vacuum environment, setting a stirring speed of revolution: rotation = 1000: 600, and stirring for 10 minutes. Finally, a UV adhesive is obtained.

[0070] Example 2

[0071] This embodiment provides a high damping speaker UV center glue, which includes the following components in weight percentage:

[0072]

[0073] The preparation method comprises the following steps: adding the organosilicon photocurable resin prepared in Preparation Example 1 and the polyurethane acrylic resin SD871 into a stirring container of a non-intrusive homogenizer, then adding a reactive diluent (including 10% 2-hydroxyethyl acrylate and 30% butyl acrylate), then adding a photoinitiator (2,4,6-trimethylbenzoyl) di(p-tolyl) phosphine oxide and an adhesion promoter acrylic acid, stirring at a temperature of 25°C, in a vacuum environment, setting a stirring speed of revolution: rotation = 1000: 600, and stirring for 10 minutes. Finally, a UV adhesive is obtained.

[0074] Example 3

[0075] This embodiment provides a high damping speaker UV center glue, which includes the following components in weight percentage:

[0076]

[0077] The preparation method comprises the following steps: adding the organosilicon photocurable resin prepared in Preparation Example 1 and polyurethane acrylic resin 61363 into a stirring container of a non-intrusive homogenizer, then adding a reactive diluent (including 20% ​​of 4-hydroxybutyl acrylate and 20% of acryloylmorpholine), then adding a photoinitiator (2,4,6-trimethylbenzoyl) di(p-tolyl) phosphine oxide and an adhesion promoter β-acryloxy propionic acid, stirring at a temperature of 25°C, in a vacuum environment, setting a stirring speed of revolution: rotation = 1000: 600, and stirring for 10 minutes. Finally, a UV adhesive is obtained.

[0078] Example 4

[0079] This embodiment provides a high damping speaker UV center glue, which includes the following components in weight percentage:

[0080]

[0081] The preparation method comprises the following steps: adding the organosilicon photocurable resin prepared in Preparation Example 1 and the polyurethane acrylic resin CN9001 into a stirring container of a non-intrusive homogenizer, then adding the reactive diluent isobornyl acrylate, then adding the photoinitiator (2,4,6-trimethylbenzoyl) di(p-tolyl) phosphine oxide and the adhesion promoter β-acryloxy propionic acid, stirring at 40°C, stirring in a vacuum environment, setting the stirring speed to revolution: rotation = 1000: 600, and stirring for 10 minutes. Finally, a UV adhesive is obtained.

[0082] Example 5

[0083] This embodiment provides a high damping speaker UV center glue, which includes the following components in weight percentage:

[0084]

[0085] The preparation method comprises the following steps: adding the organosilicon photocurable resin prepared in Preparation Example 1 and the polyurethane acrylic resin SD810 into a stirring container of a non-intrusive homogenizer, then adding the reactive diluent 4-hydroxybutyl acrylate, then adding the photoinitiator (2,4,6-trimethylbenzoyl) di(p-tolyl) phosphine oxide and the adhesion promoter β-acryloxy propionic acid, stirring at 70°C, stirring in a vacuum environment, setting the stirring speed to revolution: rotation = 1000: 600, and stirring for 10 minutes. Finally, a UV adhesive is obtained.

[0086] Example 6

[0087] This embodiment provides a high damping speaker UV center glue, which includes the following components in weight percentage:

[0088]

[0089]

[0090] The preparation method comprises the following steps: adding the organosilicon light-curing resin prepared in Preparation Example 2 and the polyurethane acrylic resin CN8003 into a stirring container of a non-intrusive homogenizer, then adding the reactive diluent isodecyl acrylate, then adding the photoinitiator diphenyl (2,4,6-trimethylbenzoyl) phosphine oxide and the adhesion promoter 2-hydroxyethyl methacrylate phosphate, stirring at a temperature of 50° C., stirring in a vacuum environment, setting the stirring speed to revolution: rotation = 1000: 600, and stirring for 10 minutes. Finally, a UV adhesive is obtained.

[0091] Example 7

[0092] This embodiment provides a high damping speaker UV center glue, which includes the following components in weight percentage:

[0093]

[0094] The preparation method comprises the following steps: adding the organosilicon light-curing resin prepared in Preparation Example 3 and the polyurethane acrylic resin CN8003 into a stirring container of a non-intrusive homogenizer, then adding the reactive diluent isodecyl acrylate, then adding the photoinitiator diphenyl (2,4,6-trimethylbenzoyl) phosphine oxide and the adhesion promoter 2-hydroxyethyl methacrylate phosphate, stirring at a temperature of 30° C., stirring in a vacuum environment, setting the stirring speed to revolution: rotation = 1000: 600, and stirring for 10 minutes. Finally, a UV adhesive is obtained.

[0095] Comparative Example 1

[0096] Commercially available UV glue 1, German DELO 4086 UV glue, is specially used as the center glue of micro speaker sound membrane. The MSDS (Material Safety Data Sheet) shows that the UV glue contains polyurethane acrylic resin, N,N-dimethylacrylamide, 3,3,5-trimethylcyclohexyl acrylate, ethoxyethoxyethyl acrylate, acrylic acid, etc.

[0097] Comparative Example 2

[0098] Commercially available UV glue 2, 5305R UV glue product of Kyoritsu Chemical Company of Japan, is specially used for the center glue of the speaker cone within 10 watts. MSDS (Material Safety Data Sheet) shows that the UV glue contains polyurethane acrylic resin, isobornyl acrylate, N,N-dimethylacrylamide, hydroxyethyl methacrylate, etc.

[0099] Comparative Example 3

[0100] The only difference from Example 1 is that the organosilicon photocurable resin is replaced by phenyl vinyl silicone oil AM-3050 (Clarmar).

[0101] Comparative Example 4

[0102] The only difference from Example 1 is that the organosilicon photocurable resin is replaced by the organosilicon resin A prepared in Comparative Example 1.

[0103] The comprehensive performance comparison parameters of the above Examples 1-6 and Comparative Examples 1-4 are shown in Tables 1 and 2.

[0104] Tg, modulus, damping coefficient, and damping temperature domain tests are all tested using METTLER TOLED0 DMA equipment. The test conditions are tensile mode, sample size: 10.000mm×2.660mm×4.020mm, temperature range: -40℃~110℃, heating rate: 5K / min, vibration frequency: 1Hz, amplitude: 5μm, dynamic force: 10.00N, static force: 0.02N, atmosphere: air.

[0105] Table 1

[0106]

[0107] Table 2

[0108] Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Tg / ℃ 74 49.8 45.9 57.2 Modulus / MPa@25℃ 190 13.76 210 185 Maximum damping coefficient tanδmax 0.678 1.25 0.73 0.74 tanδ>0.3 Damping temperature / ℃ 44.5~92 17.7~103.4 24.9~70.3 32.1~92.9 Damping temperature range / ℃ 47.5 85.7 45.4 60.7

[0109] It can be seen from the data in Table 1 that the maximum damping coefficient tanδmax of Examples 1 to 6 exceeds 0.95, and the damping coefficients in Examples 4 and 5 even show over-damping phenomena of 1.192 and 1.339; at the same time, the damping temperature range of Examples 1 to 4 exceeds 100°C, among which Example 1 even has a high damping tanδ>0.3 temperature range in the entire working area of ​​167°C, while the maximum damping coefficient tanδmax of Comparative Examples 1 to 4 exceeds 0.75 (except Comparative Example 2), and the maximum damping temperature range is only 85.7°C, which is much smaller than the damping effect in the embodiments.

[0110] In particular, by comparing Example 1 with Comparative Example 3 and Comparative Example 4, it can be seen that the damping temperature range of the glue added with the prepared silicone photocurable resin and the glue added with other silicone or vinyl silicone resins after curing is significantly increased, and the maximum damping coefficient is significantly improved, indicating that the prepared photocurable silicone and other monomers and resins have a synergistic effect. Example 1 shows double peaks at -9.9°C and 71.3°C, which is caused by the phase separation structure of the photocurable silicone and polyurethane acrylate.

[0111] Figure 3 It is a damping test result diagram of Example 1 and Comparative Examples 1, 3 and 4.

[0112] The applicant declares that the present invention uses the above-mentioned embodiments to illustrate the organosilicon photocurable resin of the present invention and the high damping speaker UV center glue containing the same and the preparation method and application thereof, but the present invention is not limited to the above-mentioned embodiments, that is, it does not mean that the present invention must rely on the above-mentioned embodiments to be implemented. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of the raw materials selected by the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

Claims

1. A silicone photocurable resin, characterized in that: The organosilicon photocurable resin has the following structure: Wherein x=0~1.66, y=0~1.39 natural numbers, and n=1~5 integers.

2. The method for preparing the organosilicon photocurable resin according to claim 1, characterized in that: The preparation method comprises the following steps: Diethoxydimethylsilane, phenyltriethoxysilane and vinyltriethoxysilane undergo hydrolysis condensation reaction to obtain the organosilicon photocurable resin.

3. The preparation method according to claim 2, characterized in that: The molar ratio of diethoxydimethylsilane, phenyltriethoxysilane and vinyltriethoxysilane is 1:(1-2):(1-3); Preferably, the hydrolysis condensation reaction is carried out under nitrogen protection; Preferably, the hydrolysis condensation reaction is carried out in the presence of an acidic catalyst; Preferably, the acidic catalyst is a hydrochloric acid solution; Preferably, the hydrolysis condensation reaction is carried out at room temperature, and the reaction time is 48-72 hours.

4. A high damping speaker UV center glue, characterized in that: The high damping speaker UV center glue includes the following components in weight percentage:

5. The high damping speaker UV center glue according to claim 4 is characterized in that: The content of the organosilicon photocurable resin is 15% to 30%; Preferably, the content of the active diluent is 30% to 40%; Preferably, the content of the photoinitiator is 3% to 5%.

6. The high damping speaker UV center glue according to claim 4 or 5, characterized in that: The acrylic prepolymer resin is selected from polyurethane acrylic resin; Preferably, the polyurethane acrylic resin includes one or a combination of at least two of China Taiwan Changxing Materials 61363, China Taiwan Changxing Materials 61396, Songda SD810, Songda SD871, Sartomer CN9001 or Sartomer CN8003.

7. The high damping speaker UV center glue according to any one of claims 4-6, characterized in that: The active diluent is selected from any one or a combination of at least two of monomers containing oxygen heterocycles, monomers containing polar groups or monomers containing long chain structures; Preferably, the monomer containing oxygen heterocycle is selected from any one or a combination of at least two of isobornyl acrylate, acryloyl morpholine or tetrahydrofurfuryl acrylate; Preferably, the monomer containing a polar group is selected from any one or a combination of at least two of 2-hydroxyethyl acrylate, acrylic acid, 4-hydroxybutyl acrylate or 2-hydroxypropyl acrylate; Preferably, the monomer containing a long chain structure is selected from any one or a combination of at least two of isooctyl acrylate, butyl acrylate, lauric acrylate, isodecyl acrylate or isononyl acrylate; Preferably, the photoinitiator is a free radical photoinitiator; Preferably, the photoinitiator is selected from any one or a combination of at least two of (2,4,6-trimethylbenzoyl)di(p-tolyl)phosphine oxide, diphenyl(2,4,6-trimethylbenzoyl)phosphine oxide, 1-hydroxycyclohexylphenyl ketone, 2-hydroxy-2-methyl-1-phenylpropanone, benzoin methyl ether, and ethyl 2,4,6-trimethylbenzoylphosphonate; Preferably, the adhesion promoter is selected from any one of 2-hydroxyethyl methacrylate phosphate, acrylic acid, γ-aminopropyltrimethoxysilane, β-acryloxypropionic acid, or a combination of at least two thereof.

8. The method for preparing the high damping speaker UV center glue according to any one of claims 4 to 7, characterized in that: The preparation method comprises the following steps: The light-curable silicone resin, acrylic prepolymer, reactive diluent, photoinitiator and adhesion promoter are mixed evenly to obtain the high-damping speaker UV center glue.

9. The preparation method according to claim 8, characterized in that: The mixing is carried out under stirring at 20-70°C; Preferably, the mixing time is 30min-3h; Preferably, the revolution speed of the stirring is 800 to 1000 rpm, and the rotation speed is 600 to 800 rpm; Preferably, the preparation method is carried out in a reaction vessel; Preferably, the preparation method specifically includes the following steps: first, add silicone photocurable resin, acrylic prepolymer resin, and active diluent into a reaction kettle, heat to 40-70°C and stir for 20-50 minutes, control the stirring speed at 800-1000 rpm, add photoinitiator and adhesion promoter after the acrylic prepolymer resin is dissolved, continue stirring for 2 hours until the liquid is evenly mixed, and finally vacuum degas and stir for 10-30 minutes to obtain the high damping speaker UV center glue.

10. Application of the high damping speaker UV center glue according to any one of claims 4 to 7 in speakers.

Citation Information

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