Liquid light-cured acrylate pressure-sensitive adhesive and preparation method thereof
By introducing deep curing accelerator into the pressure-sensitive adhesive and synergistically interact with nanotitanium dioxide, the curing depth of the pressure-sensitive adhesive is significantly improved, solving the problem of insufficient curing depth of traditional pressure-sensitive adhesives, and achieving better workpiece bonding effect and material safety.
Patent Information
- Application Number
- CN202510153792.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-12
- Publication Date
- 2025-05-06
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
Traditional pressure-sensitive adhesives have problems with insufficient curing depth in practical applications, especially in electronic component packaging, which leads to unstable product performance. The existing solutions are costly and inefficient, and are prone to overheating of materials, making it difficult to meet actual needs.
Liquid photocuring acrylate pressure-sensitive adhesive is used to significantly enhance the curing depth of the pressure-sensitive adhesive by introducing independently developed deep curing accelerators and nanotitanium dioxide. The deep curing accelerator is replaced by diethanolamine and methylvinyldichlorosilane to form a silicon-doped small-molecular-weight chain compound, and through the double-bonded side chain link addition of mercaptoethanol and the silicon-modified matrix, an active thiool hydroxyl group is introduced to the side chain, and finally an active thiool hydroxyl esterification is introduced to the side chain through the side chain of methacryloyl chloride and the hydroxylation intermediate, and a methacrylate structure is introduced to the side chain.
The deep curing of pressure-sensitive adhesive is achieved, the bonding effect and tensile shear strength of the workpiece are improved, the problem of insufficient curing depth is solved, and the process does not escape toxic and harmful substances, which has little impact on the environment and personnel health.
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Figure CN119931583A_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of adhesives, and in particular relates to a liquid light-curing acrylate pressure-sensitive adhesive and a preparation method thereof. Background Art
[0002] Pressure-sensitive adhesive is a material with unique adhesive properties, which is widely used in various fields, including labels, tapes, medical dressings, electronic component fixation, etc. Traditional pressure-sensitive adhesives usually adopt solution form or hot-melt system, which has disadvantages in application and storage. For example, solution-type pressure-sensitive adhesives have high volatile organic compound content, which pollutes the environment, and hot-melt pressure-sensitive adhesives need to be heated to melt, and the use process is relatively cumbersome. Acrylic resin is one of the photocurable materials currently widely used in industry. Using it as the base material of pressure-sensitive adhesive can achieve rapid curing of the adhesive material, effectively improving production efficiency.
[0003] However, in practical applications, the problem of insufficient curing depth of acrylic glue often occurs. For example, when packaging electronic components, the packaging surface of high-density components is large, and it is very easy to produce incomplete curing during the curing process, resulting in unstable product performance. To solve the problem of insufficient curing depth, existing technologies mainly include using higher-power light sources, increasing the number of curing times, and adjusting the light curing curve. However, these methods are usually costly, inefficient, and prone to overheating of materials, making it difficult to meet practical application needs. Summary of the invention
[0004] In order to solve the technical problems mentioned in the background technology, the purpose of the present invention is to provide a liquid light-curing acrylate pressure-sensitive adhesive and a preparation method thereof.
[0005] The purpose of the present invention can be achieved by the following technical solutions: A liquid light-curing acrylate pressure-sensitive adhesive, comprising, by weight: 100 parts of low-viscosity acrylate prepolymer, 15-20 parts of active diluent, 8-12 parts of deep curing accelerator, 2.7-3.4 parts of photoinitiator, 3.2-3.9 parts of nano titanium dioxide, 1.3-1.7 parts of wetting agent, 1.2-1.5 parts of defoaming agent and 0.8-1.1 parts of leveling agent.
[0006] The deep curing accelerator is prepared by the following method: Step A1: premix diethanolamine and anhydrous acetone, pass dry gas protection, then add methylvinyldichlorosilane, apply rapid stirring at 180-240 rpm at room temperature to react for 15-20 minutes, then add methanol and mix, heat to 40-50°C and continue to react for 1-1.5 hours, and after the reaction is completed, remove acetone by rotary evaporation to obtain a silicon-modified matrix; Furthermore, the feed ratio of methylvinyldichlorosilane, diethanolamine, methanol and anhydrous acetone is 0.1 mol: 70-90 mmol: 25-50 mmol: 40-55 mL, and diethanolamine and methylvinyldichlorosilane are substituted to form a silicon-doped small molecular weight chain compound, which is then capped with methanol.
[0007] Step A2: Mix the silicon-modified substrate, mercaptoethanol, dimethylphenylphosphine and dimethyl sulfoxide, raise the temperature to 45-60°C, and apply 150-200W / m 2 UV irradiation and stirring at 60-90 rpm for 2.5-3.5 h, after the reaction is completed, dimethyl sulfoxide is removed by vacuum rotary evaporation to obtain a hydroxylated intermediate; Furthermore, the feed ratio of the silicon-modified substrate, mercaptoethanol, dimethylphenylphosphine and dimethyl sulfoxide is 10g:50-60mmol:10-15mg:25-40mL, and mercaptoethanol is subjected to click addition to the double bond of the side chain of the silicon-modified substrate to introduce active thiol hydroxyl groups into the side chain.
[0008] Step A3: the hydroxylated intermediate, triethylamine and tetrahydrofuran are mixed, dry gas protection is introduced, stirring is applied at 120-180 rpm at room temperature, methacryloyl chloride is slowly added to react for 2-3 hours, tetrahydrofuran is removed by rotary evaporation after the reaction is completed, the substrate is washed with water, the aqueous phase is separated and dried in vacuo to obtain a deep curing accelerator; Furthermore, the feed ratio of the hydroxylated intermediate, methacryloyl chloride, triethylamine and tetrahydrofuran is 10 g: 20-30 mmol: 3-5 mL: 30-40 mL, and the methacryloyl chloride is esterified with the active thiol hydroxyl group introduced into the side chain of the hydroxylated intermediate to introduce a methacrylate structure into the side chain.
[0009] Furthermore, the low-viscosity acrylic prepolymer is a bifunctional prepolymer with a room temperature viscosity of no more than 300 cps, good processability, and meets the construction environments of coating and dispensing, and the mechanical properties of the adhesive layer are uniform.
[0010] Furthermore, the active diluent is a multifunctional acrylate monomer having good diluting ability and cross-linking activity.
[0011] Furthermore, the photoinitiator is selected from benzophenone photoinitiators, which have good storage stability and have a high curing effect on the acrylate system.
[0012] A preparation method of a liquid light-curing acrylic pressure-sensitive adhesive comprises the following steps: premixing an active diluent, a deep curing accelerator, a wetting agent and nano titanium dioxide, adding a photoinitiator, a defoaming agent and a leveling agent, and finally adding a low-viscosity acrylic prepolymer, mixing, and vacuum degassing to obtain the liquid light-curing acrylic pressure-sensitive adhesive.
[0013] Beneficial effects of the present invention: The invention is based on an acrylate photocuring system and discloses a liquid solvent-free pressure-sensitive adhesive. No toxic or harmful substances escape during the curing process, and the impact on the environment and personnel health is small. The liquid is in a low-viscosity liquid state, and the adhesive is applied accurately, so the pressure-sensitive adhesive is suitable for bonding workpieces with complex structures. The curing depth of the pressure-sensitive adhesive is significantly improved by introducing a self-developed deep curing accelerator and synergizing with nano titanium dioxide, which is beneficial to the effective bonding of the workpieces. The deep curing accelerator is substituted by diethanolamine and methylvinyldichlorosilane to form a silicon-doped small molecular weight chain compound, which is then capped by methanol to form a silicon-modified matrix, and then mercaptoethanol is click-added to the double bonds of the side chains of the silicon-modified matrix to introduce active thiol hydroxyl groups to the side chains to prepare a hydroxylated intermediate, and finally methacryloyl chloride is esterified with the active thiol hydroxyl groups introduced in the side chains of the hydroxylated intermediate to introduce methyl Acrylate structure is made into deep curing accelerator; in the compounding process, the nitrogen oxygen structure introduced by the diethanolamine block on the main chain of the deep curing accelerator and the sulfur oxygen structure introduced by the mercaptoethanol on the side chain form a complexing effect, which is easy to be coated on the surface of nano titanium dioxide to form a uniform silicon doping layer. During the ultraviolet curing process, the nano titanium dioxide particles reflect ultraviolet rays, which promotes the preferential polymerization of the acrylate structure of the side chain of the deep curing accelerator with the low-viscosity acrylate prepolymer and the active diluent to form an initial curing layer, and then in the double-layer coating layer of the nano titanium dioxide particles with different media, the scattering degree of ultraviolet rays is greatly increased, so that the ultraviolet rays are effectively introduced into the deep of the adhesive layer, promoting the deep curing of the adhesive layer. In addition, the deep curing accelerator enhances the bonding strength between nano titanium dioxide and the acrylate macromolecular chain, and effectively enhances the tensile shear strength of the pressure-sensitive adhesive. BRIEF DESCRIPTION OF THE DRAWINGS
[0014] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for describing the embodiments are briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without creative work.
[0015] Figure 1 It is a graph showing the light curing time and curing depth of the present invention. DETAILED DESCRIPTION
[0016] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0017] Example 1, preparing a liquid light-curable acrylate pressure-sensitive adhesive, as follows: (1) Preparation of deep curing accelerator Step A1: Take diethanolamine and anhydrous acetone as feed materials and premix them, pass dry nitrogen for protection, then add methylvinyldichlorosilane, and rapidly stir at 180rpm for reaction at room temperature for 20min, then add methanol and mix, heat to 40°C and continue to react for 1.5h, wherein the feed ratio of methylvinyldichlorosilane, diethanolamine, methanol and anhydrous acetone is 0.1mol:70mmol:50mmol:40mL. After the reaction, remove acetone and take out excess methanol by rotary evaporation to obtain a silicon-modified matrix.
[0018] Step A2: Take the silicon-modified substrate, mercaptoethanol, dimethylphenylphosphine and dimethyl sulfoxide, mix them, heat them to 45°C, and apply 150W / m 2 The reaction was stirred at 60 rpm and ultraviolet irradiation for 3.5 h, wherein the feed ratio of the silicon-modified substrate, mercaptoethanol, dimethylphenylphosphine and dimethyl sulfoxide was 10 g: 50 mmol: 10 mg: 25 mL. After the reaction was completed, dimethyl sulfoxide and low-boiling substances were removed by vacuum rotary evaporation to obtain a hydroxylated intermediate.
[0019] Step A3: Take the hydroxylated intermediate, triethylamine and tetrahydrofuran, mix them, introduce dry nitrogen protection, apply stirring at 120rpm at room temperature, slowly add methacryloyl chloride to react for 3h, wherein the feed ratio of hydroxylated intermediate, methacryloyl chloride, triethylamine and tetrahydrofuran is 10g:20mmol:3mL:30mL. After the reaction, remove tetrahydrofuran by rotary evaporation, wash the substrate with water, separate the liquid to remove the water phase and dry in vacuo to obtain a deep curing accelerator.
[0020] (2) Preparation of acrylic pressure-sensitive adhesive Ingredients: according to weight parts, 100 parts of low-viscosity acrylate prepolymer, U-CURE® 9110 type difunctional prepolymer is selected, and the room temperature viscosity is 260cps; 15 parts of reactive diluent, BM3232 type trifunctional acrylate monomer is selected; 8 parts of deep curing accelerator, which is self-made in this embodiment; 3 parts of photoinitiator, Lencolo 5006D type benzophenone derivative photoinitiator is selected; 3.2 parts of nano titanium dioxide, NT-50 type nanomaterial is selected; 1.3 parts of wetting agent, Lencolo 1113 type raw material is selected; 1.2 parts of defoaming agent, Lencolo 2108 type raw material is selected; 1.1 parts of leveling agent, Lencolo 3137 type raw material is selected.
[0021] Glue preparation: premix the active diluent, deep curing accelerator, wetting agent and nano titanium dioxide at 600 rpm for 3 minutes, then add the photoinitiator, defoamer and leveling agent and mix at 120 rpm for 10 minutes, finally slowly add the low-viscosity acrylate prepolymer to the mixture at 30 rpm and stir for 20 minutes, and vacuum degas for 5 minutes to obtain a liquid light-curing acrylate pressure-sensitive adhesive.
[0022] Example 2, preparing a liquid light-curable acrylate pressure-sensitive adhesive, as follows: (1) Preparation of deep curing accelerator Step A1: Take diethanolamine and anhydrous acetone as feed materials and premix them, pass dry nitrogen for protection, then add methylvinyldichlorosilane, and rapidly stir at 240rpm for reaction at room temperature for 15 minutes, then add methanol and mix, heat to 50°C and continue to react for 1 hour, wherein the feed ratio of methylvinyldichlorosilane, diethanolamine, methanol and anhydrous acetone is 0.1mol:90mmol:25mmol:55mL. After the reaction, remove acetone and take out excess methanol by rotary evaporation to obtain a silicon-modified matrix.
[0023] Step A2: Take the silicon-modified substrate, mercaptoethanol, dimethylphenylphosphine and dimethyl sulfoxide, mix them, heat them to 60°C, and apply 200W / m 2 The reaction was stirred at 90 rpm and subjected to ultraviolet irradiation for 2.5 h, wherein the feed ratio of the silicon-modified substrate, mercaptoethanol, dimethylphenylphosphine and dimethyl sulfoxide was 10 g: 60 mmol: 15 mg: 40 mL. After the reaction was completed, dimethyl sulfoxide and low-boiling substances were removed by vacuum rotary evaporation to obtain a hydroxylated intermediate.
[0024] Step A3: Take the hydroxylated intermediate, triethylamine and tetrahydrofuran, mix them, introduce dry nitrogen protection, apply stirring at 180 rpm at room temperature, slowly add methacryloyl chloride to react for 2 hours, wherein the feed ratio of hydroxylated intermediate, methacryloyl chloride, triethylamine and tetrahydrofuran is 10g:30mmol:5mL:40mL. After the reaction, remove tetrahydrofuran by rotary evaporation, wash the substrate with water, separate the liquid to remove the water phase and dry in vacuo to obtain a deep curing accelerator.
[0025] (2) Preparation of acrylic pressure-sensitive adhesive Ingredients: according to weight parts, 100 parts of low-viscosity acrylate prepolymer, U-CURE® 9110 type difunctional prepolymer is selected, and the room temperature viscosity is 260cps; 20 parts of reactive diluent, BM3232 type trifunctional acrylate monomer is selected; 12 parts of deep curing accelerator, which is self-made in this embodiment; 3.4 parts of photoinitiator, Lencolo 5006D type benzophenone derivative photoinitiator is selected; 3.9 parts of nano titanium dioxide, NT-50 type nanomaterial is selected; 1.7 parts of wetting agent, Lencolo 1113 type raw material is selected; 1.5 parts of defoaming agent, Lencolo 2108 type raw material is selected; 0.8 parts of leveling agent, Lencolo 3137 type raw material is selected.
[0026] Glue preparation: premix the active diluent, deep curing accelerator, wetting agent and nano titanium dioxide at 600 rpm for 3 minutes, then add the photoinitiator, defoamer and leveling agent and mix at 120 rpm for 10 minutes, finally slowly add the low-viscosity acrylate prepolymer to the mixture at 30 rpm and stir for 20 minutes, and vacuum degas for 5 minutes to obtain a liquid light-curing acrylate pressure-sensitive adhesive.
[0027] Example 3, preparing a liquid light-curable acrylate pressure-sensitive adhesive, as follows: (1) Preparation of deep curing accelerator Step A1: Take diethanolamine and anhydrous acetone as feed materials and premix them, pass dry nitrogen for protection, then add methylvinyldichlorosilane, and rapidly stir at 240rpm for reaction at room temperature for 15 minutes, then add methanol and mix, heat to 45°C and continue to react for 1.2 hours, wherein the feed ratio of methylvinyldichlorosilane, diethanolamine, methanol and anhydrous acetone is 0.1mol:80mmol:35mmol:45mL. After the reaction is completed, the acetone is removed by rotary evaporation and excess methanol is taken out to obtain a silicon-modified matrix.
[0028] Step A2: Take the silicon-modified substrate, mercaptoethanol, dimethylphenylphosphine and dimethyl sulfoxide, mix them, heat them to 55°C, and apply 150W / m 2 The reaction was carried out under ultraviolet irradiation and stirred at 90 rpm for 3 hours, wherein the feed ratio of the silicon-modified substrate, mercaptoethanol, dimethylphenylphosphine and dimethyl sulfoxide was 10 g:50 mmol:12 mg:30 mL. After the reaction was completed, dimethyl sulfoxide and low-boiling substances were removed by vacuum rotary evaporation to obtain a hydroxylated intermediate.
[0029] Step A3: Take the hydroxylated intermediate, triethylamine and tetrahydrofuran, mix them, introduce dry nitrogen protection, apply stirring at 120rpm at room temperature, slowly add methacryloyl chloride to react for 2.5h, wherein the feed ratio of hydroxylated intermediate, methacryloyl chloride, triethylamine and tetrahydrofuran is 10g:25mmol:4mL:40mL. After the reaction, remove tetrahydrofuran by rotary evaporation, wash the substrate with water, separate the liquid to remove the water phase and dry in vacuo to obtain a deep curing accelerator.
[0030] (2) Preparation of acrylic pressure-sensitive adhesive Ingredients: according to weight parts, 100 parts of low-viscosity acrylate prepolymer, U-CURE® 9110 type difunctional prepolymer is selected, and the room temperature viscosity is 260cps; 18 parts of reactive diluent, BM3232 type trifunctional acrylate monomer is selected; 10 parts of deep curing accelerator, which is self-made in this embodiment; 2.7 parts of photoinitiator, Lencolo 5006D type benzophenone derivative photoinitiator is selected; 3.4 parts of nano titanium dioxide, NT-50 type nanomaterial is selected; 1.5 parts of wetting agent, Lencolo 1113 type raw material is selected; 1.4 parts of defoaming agent, Lencolo 2108 type raw material is selected; 0.9 parts of leveling agent, Lencolo 3137 type raw material is selected.
[0031] Glue preparation: premix the active diluent, deep curing accelerator, wetting agent and nano titanium dioxide at 600 rpm for 3 minutes, then add the photoinitiator, defoamer and leveling agent and mix at 120 rpm for 10 minutes, finally slowly add the low-viscosity acrylate prepolymer to the mixture at 30 rpm and stir for 20 minutes, and vacuum degas for 5 minutes to obtain a liquid light-curing acrylate pressure-sensitive adhesive.
[0032] Example 4, preparing a liquid light-curable acrylate pressure-sensitive adhesive, as follows: (1) Preparation of deep curing accelerator Step A1: Take diethanolamine and anhydrous acetone as feed materials and premix them, pass dry nitrogen for protection, then add methylvinyldichlorosilane, and rapidly stir at 240rpm for reaction at room temperature for 20min, then add methanol and mix, heat to 45°C and continue to react for 1.2h, wherein the feed ratio of methylvinyldichlorosilane, diethanolamine, methanol and anhydrous acetone is 0.1mol:75mmol:40mmol:50mL. After the reaction, remove acetone by rotary evaporation and take out excess methanol to obtain a silicon-modified matrix.
[0033] Step A2: Take the silicon-modified substrate, mercaptoethanol, dimethylphenylphosphine and dimethyl sulfoxide, mix them, heat them to 50°C, and apply 180W / m 2The reaction was stirred at 90 rpm and subjected to ultraviolet irradiation for 3.2 h, wherein the feed ratio of the silicon-modified substrate, mercaptoethanol, dimethylphenylphosphine and dimethyl sulfoxide was 10 g:55 mmol:12 mg:35 mL. After the reaction was completed, dimethyl sulfoxide and low-boiling substances were removed by vacuum rotary evaporation to obtain a hydroxylated intermediate.
[0034] Step A3: Take the hydroxylated intermediate, triethylamine and tetrahydrofuran, mix them, introduce dry nitrogen protection, apply stirring at 180 rpm at room temperature, slowly add methacryloyl chloride to react for 2.5 hours, wherein the feed ratio of the hydroxylated intermediate, methacryloyl chloride, triethylamine and tetrahydrofuran is 10 g: 25 mmol: 5 mL: 40 mL. After the reaction, remove tetrahydrofuran by rotary evaporation, wash the substrate with water, separate the liquid to remove the water phase and dry in vacuo to obtain a deep curing accelerator.
[0035] (2) Preparation of acrylic pressure-sensitive adhesive Ingredients: according to weight parts, 100 parts of low-viscosity acrylate prepolymer, U-CURE® 9110 type difunctional prepolymer is selected, and the room temperature viscosity is 260cps; 17 parts of reactive diluent, BM3232 type trifunctional acrylate monomer is selected; 10 parts of deep curing accelerator, which is self-made in this embodiment; 2.9 parts of photoinitiator, Lencolo 5006D type benzophenone derivative photoinitiator is selected; 3.6 parts of nano titanium dioxide, NT-50 type nanomaterial is selected; 1.5 parts of wetting agent, Lencolo 1113 type raw material is selected; 1.3 parts of defoaming agent, Lencolo 2108 type raw material is selected; 1 part of leveling agent, Lencolo 3137 type raw material is selected.
[0036] Glue preparation: premix the active diluent, deep curing accelerator, wetting agent and nano titanium dioxide at 600 rpm for 3 minutes, then add the photoinitiator, defoamer and leveling agent and mix at 120 rpm for 10 minutes, finally slowly add the low-viscosity acrylate prepolymer to the mixture at 30 rpm and stir for 20 minutes, and vacuum degas for 5 minutes to obtain a liquid light-curing acrylate pressure-sensitive adhesive.
[0037] Comparative Example 1: This comparative example refers to Example 4, except that the deep-layer curing accelerator is replaced with 8 parts of low-viscosity acrylate prepolymer and 2 parts of reactive diluent, and the rest of the implementation process is exactly the same.
[0038] Comparative Example 2: This comparative example refers to Example 4, except that the deep curing accelerator is replaced with 4 parts of low-viscosity acrylate prepolymer, 4 parts of reactive diluent and 2 parts of acryloxypropyltrimethoxysilane, and the rest of the implementation process is exactly the same.
[0039] The pressure-sensitive adhesive prepared above was injected into the inclined groove mold with a groove width of 2 mm, a groove length of 200 mm, and a maximum groove depth of 10 mm. It was placed in a UV curing machine with an ultraviolet wavelength of 365 nm and an ultraviolet irradiation intensity of 500 mW / cm 2 After a certain period of curing, remove the glue layer and slice to detect the curing depth. The specific test results are as follows: Figure 1 As shown; Depend on Figure 1 It can be seen that the embodiment and the comparative example almost complete the curing within 30s of curing time, and the curing depth is higher than that of the comparative example under the same curing conditions. Among them, the curing depth of the embodiment shows obvious secondary rapid rising fluctuations over time within the range of 10-20s.
[0040] Glass sheet, copper sheet and epoxy resin sheet were respectively used as bonding objects. The surfaces were cleaned with ethanol and dried. 1 mL of glue was applied by a glue dispenser. After bonding, they were placed in a UV curing machine for curing for 30 seconds. Then, the tensile shear strength test was carried out according to GB / T 7124-2008 standard. The specific test results are shown in Table 1:
[0041] It can be seen from the test results in Table 1 that the pressure-sensitive adhesives of the embodiments and comparative examples have good bonding ability to glass, copper and epoxy resin, and have a broad-spectrum bonding effect.
[0042] In the description of the specification, the description with reference to the terms "one embodiment", "example", "specific example", etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.
[0043] The above contents are merely examples and explanations of the concept of the present invention. Those skilled in the art may make various modifications or additions to the specific embodiments described or replace them in a similar manner. As long as they do not deviate from the concept of the invention or exceed the scope defined by the claims, they shall all fall within the protection scope of the present invention.
Claims
1. A liquid light-curing acrylate pressure-sensitive adhesive, characterized in that: The composition comprises, by weight: 100 parts of low-viscosity acrylate prepolymer, 15-20 parts of reactive diluent, 8-12 parts of deep curing accelerator, 2.7-3.4 parts of photoinitiator, 3.2-3.9 parts of nano titanium dioxide, 1.3-1.7 parts of wetting agent, 1.2-1.5 parts of defoamer and 0.8-1.1 parts of leveling agent; The deep layer curing accelerator is prepared by the following method: Step A1: premix diethanolamine and anhydrous acetone, introduce dry gas protection, then add methylvinyldichlorosilane, stir and react at room temperature for 15-20 minutes, then add methanol and mix, heat to 40-50°C and continue to react for 1-1.5 hours to obtain a silicon-modified matrix; Step A2: Mix the silicon-modified substrate, mercaptoethanol, dimethylphenylphosphine and dimethyl sulfoxide, raise the temperature to 45-60°C, and apply 150-200W / m 2 The mixture was stirred and reacted under ultraviolet irradiation for 2.5-3.5 hours to obtain a hydroxylated intermediate; Step A3: Mix the hydroxylated intermediate, triethylamine and tetrahydrofuran, introduce dry gas protection, stir at room temperature and slowly add methacryloyl chloride to react for 2-3 hours to obtain a deep curing accelerator.
2. The liquid light-curable acrylate pressure-sensitive adhesive according to claim 1, characterized in that: The feed ratio of methylvinyldichlorosilane, diethanolamine, methanol and anhydrous acetone is 0.1 mol: 70-90 mmol: 25-50 mmol: 40-55 mL.
3. A liquid light-curable acrylate pressure-sensitive adhesive according to claim 2, characterized in that: The feed ratio of the silicon-modified matrix, mercaptoethanol, dimethylphenylphosphine and dimethyl sulfoxide is 10 g: 50-60 mmol: 10-15 mg: 25-40 mL.
4. The liquid light-curable acrylate pressure-sensitive adhesive according to claim 3, characterized in that: The feed ratio of the hydroxylated intermediate, methacryloyl chloride, triethylamine and tetrahydrofuran is 10 g: 20-30 mmol: 3-5 mL: 30-40 mL.
5. The liquid light-curable acrylate pressure-sensitive adhesive according to claim 1, characterized in that: The low viscosity acrylic prepolymer is a bifunctional prepolymer.
6. The liquid light-curable acrylate pressure-sensitive adhesive according to claim 1, characterized in that: The active diluent is a multifunctional acrylate monomer.
7. The liquid light-curable acrylate pressure-sensitive adhesive according to claim 1, characterized in that: The photoinitiator is a benzophenone photoinitiator.
8. A method for preparing a liquid light-curable acrylate pressure-sensitive adhesive according to any one of claims 1 to 7, characterized in that: Specifically, active diluent, deep curing accelerator, wetting agent and nano titanium dioxide are premixed, photoinitiator, defoamer and leveling agent are added and mixed, and finally low-viscosity acrylate prepolymer is added and mixed, vacuum degassing is performed to obtain liquid light-curing acrylate pressure-sensitive adhesive.