Preparation method of rapidly-cured UV blue gel

Abstract

The invention provides a preparation method of rapidly-cured UV blue gel. The preparation method comprises the steps of material preparation, premixing dispersion, main agent mixing, ultrasonic dispersion, viscosity adjustment, filtration, defoaming and the like. The nano silicon dioxide and the acrylate monomer are premixed, so that the nano silicon dioxide is ensured to be uniformly dispersed in a system, the curing speed of the UV blue gel is finally accelerated, meanwhile, the good and uniform cohesiveness of the UV blue gel produced by the preparation method is ensured, and the quality and the reliability of a product are effectively improved.

Description

[0001] The invention belongs to the technical field of chemical industry, and in particular relates to a method for preparing fast-curing UV blue glue. Background Art

[0002] As a traditional material for electrical insulation and physical protection of power batteries, blue film tape has weak adhesion and low surface energy, so its viscosity strength on the surface can only reach 2-3MPa. In this case, when the battery pack is impacted by external force, the following situations are likely to occur: (1) The structural adhesive undergoes interfacial damage and falls off the blue film tape.

[0003] (2) The PSA adhesive backing of the blue film tape undergoes cohesive failure, causing the blue film to fall off and peel off from the battery cell casing.

[0004] With the development of new energy vehicles, major manufacturers have begun to further improve the driving range and charging speed, resulting in the voltage platform of many new vehicles jumping from no more than 400V to 800V. Still using blue film tape is tantamount to planting a time bomb for the safety of power batteries.

[0005] UV curing adhesives are widely used in electronic packaging, optical component bonding, medical device manufacturing and other fields due to their advantages such as fast curing, easy operation, low volatility and environmental protection. However, traditional UV curing adhesives have some limitations in the application process. Due to the limited penetration of ultraviolet rays, the overall curing time is prolonged, affecting production efficiency and final product quality.

[0006] According to the relevant public technology, the Chinese patent with the announcement number CN104479436B discloses a method for preparing a peelable adhesive coating, but the method only simply configures the components of the composition in the peelable adhesive coating composition, and does not consider the possible impact of the order of adding the components. In the Chinese patent application with the publication number CN104497660A, the various raw materials are simply mixed and then ground. In the Chinese patent application with the publication number CN119432307A, the order of the components is set in the preparation method of the high-temperature resistant and high-toughness organosilicon-modified peelable blue glue disclosed therein, but the invention lies in the introduction of organosilicon compounds such as organosilicon polyols into the polyurethane acrylate adhesive to pre-form a prepolymer, and there is a situation where the components added subsequently cannot be guaranteed to be completely mixed with the prepolymer, which leads to the blue glue prepared by the method being applied to the surface of a power battery shell, and the various parts of the formed glue coating cannot determine the isotropic uniformity, and there is a risk of the glue coating falling off and peeling off from the surface of the battery shell.

[0007] In summary, for the preparation of UV blue glue, while achieving rapid curing, the isotropic homogeneity of the colloid must still be ensured to ensure that it can be used as a power battery adhesive. More optimization solutions need to be proposed. Summary of the invention

[0008] The object of the present invention is to provide a method for preparing a fast-curing UV blue glue. The preparation method comprises the following steps: S1 material preparation: drying nano silicon dioxide; S2 premixing and dispersing: premixing and dispersing the nano-silicon dioxide and the acrylate monomer under low-speed stirring, wherein the low-speed stirring state is stirring for 20-25 minutes at a mixture temperature of 40-50°C and a stirring speed of 200-500 rpm; S3 main agent mixing: adding a photoinitiator and an auxiliary agent to the premixed dispersion obtained in step S2, and continuing to stir at a low speed; the initiating light source of the photoinitiator is ultraviolet light, and the auxiliary agent includes a defoaming agent; The auxiliary agent may also include one or a combination of two or more of a leveling agent, a temperature stabilizer or a polymerization inhibitor; S4 ultrasonic dispersion: using ultrasonic dispersion to treat the mixture obtained in step S3 to ensure that no agglomeration occurs, wherein the ultrasonic dispersion treatment is performed at 20-40 kHz for 15-30 minutes; S5: adjusting viscosity: cooling the mixture obtained in step S4 to 25° C., adding a diluent, and adjusting the viscosity of the mixture to 900-1200 mPa·s; S6 Filtration and defoaming: For the mixture whose viscosity has been adjusted in step S5, filter to remove undispersed particles therein, and after standing to defoam, store it in a sealed light-proof container.

[0009] Preferably, the acrylate monomer may be one or a combination of two or more of methyl methacrylate, ethylene glycol diacrylate, butyl acrylate, and hydroxyethyl acrylate.

[0010] Preferably, the photoinitiator is selected from 2,4,6-(trimethylbenzoyl)-diphenylphosphine oxide, 2-methyl-1-(4-methylthiophenyl)-2-morpholinyl-1-propanone, or a combination of two thereof; more preferably, when the photoinitiator is a combination of 2,4,6-(trimethylbenzoyl)-diphenylphosphine oxide and 2-methyl-1-(4-methylthiophenyl)-2-morpholinyl-1-propanone, the molar ratio of the two, n[2,4,6-(trimethylbenzoyl)-diphenylphosphine oxide]:n[2-methyl-1-(4-methylthiophenyl)-2-morpholinyl-1-propanone], is 3:1.

[0011] Preferably, if the nano-silica used is hydrophobic nano-silica, it needs to be surface-modified by a silane coupling agent before step S1; more preferably, the silane coupling agent is KH-570.

[0012] Preferably, by weight, the UV blue glue has: Nano silicon dioxide: 5-15 parts Acrylate monomer: 125-150 parts Photoinitiator: 3-7 parts Additives: 5-10 parts Diluent: 60-80 parts.

[0013] The beneficial effects achieved by the present invention are as follows: in the preparation method of the UV blue glue of the technical solution, nano-silicon dioxide is used to improve the dispersion efficiency of the photoinitiator. In order to avoid premature contact of the nano-silicon dioxide with the photoinitiator and thus initiation of agglomeration, the inventor premixes the nano-silicon dioxide with the acrylate monomer, thereby ensuring that the nano-silicon dioxide is evenly dispersed in the system, and ultimately accelerating the curing speed of the UV blue glue. At the same time, it ensures that the UV blue glue produced by the preparation method has good and uniform adhesion, and effectively improves the quality and reliability of the product. DETAILED DESCRIPTION

[0014] In order to make the purpose, technical solutions and advantages of the present invention clearer, the present invention is further described in detail below in conjunction with its embodiments; it should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention. For those skilled in the art, after reviewing the following detailed description, other systems, methods and / or features of the present embodiment will become apparent. It is intended that all such additional systems, methods, features and advantages are included in this specification. Included within the scope of the present invention and protected by the appended claims. Additional features of the disclosed embodiments are described in the following detailed description, and these features will be apparent from the following detailed description.

[0015] The present invention provides a method for preparing a fast-curing UV blue glue, the preparation method comprising the following steps: S1 Material preparation: Drying the nano-silicon dioxide.

[0016] S2 premixing and dispersing: premixing and dispersing the nano-silica and the acrylate monomer under low-speed stirring, wherein the low-speed stirring state is stirring at a mixture temperature of 40-50° C. and a stirring speed of 200-500 rpm for 20-25 minutes.

[0017] By premixing the nano-silica with the acrylate monomer, it is ensured that the nano-silica is evenly dispersed in the system and avoids premature contact with the photoinitiator to cause agglomeration.

[0018] S3 main agent mixing: adding a photoinitiator and an auxiliary agent to the premixed dispersion obtained in step S2, and continuing to stir at a low speed to obtain a main agent mixture, wherein the low-speed stirring state is at a mixture temperature of 40-50°C, a stirring speed of 200-500 rpm, and stirring for 20-30 minutes; the initiating light source of the photoinitiator is ultraviolet light, and the auxiliary agent includes a defoaming agent; S4 ultrasonic dispersion: using ultrasonic dispersion to treat the mixture obtained in step S3 to ensure that no agglomeration occurs, wherein the ultrasonic dispersion treatment is performed at 20-40 kHz for 15-30 minutes; S5: adjusting viscosity: cooling the mixture obtained in step S4 to 25° C., adding a diluent, and adjusting the viscosity of the mixture to 900-1200 mPa·s; S6 Filtration and defoaming: For the mixture whose viscosity is adjusted in step S5, filter to remove the undispersed particles therein, and after standing and defoaming, obtain the blue glue to be solidified, which is stored in a sealed light-proof container.

[0019] Preferably, the acrylate monomer is one or a combination of ethylene glycol diacrylate and butyl acrylate.

[0020] Preferably, the auxiliary agent may further include one or a combination of two or more of commonly used leveling agents, temperature stabilizers or polymerization inhibitors.

[0021] The diluent involved in the present invention is a commonly used diluent in the field, and typical examples include: ethyl acetate, butyl acetate, methanol, ethanol, propanol, isopropanol, isobutanol, n-butanol, methyl isobutyl ketone, isophorone, acetone, butanone, cyclohexanone, toluene, xylene, propylene glycol methyl ether and dipropylene glycol methyl ether.

[0022] The leveling agent involved in the present invention is a commonly used diluent in the field, and typical examples include: acrylic leveling agent, silicone leveling agent, etc.

[0023] The temperature stabilizer involved in the present invention is a commonly used temperature stabilizer in the art, and typical examples include: hindered phenol temperature stabilizers (such as BASF Irgastab® HT-3025), ionic liquid temperature stabilizers (such as Merck Luvatec® IL-TS88), etc.

[0024] The polymerization inhibitor involved in the present invention is a commonly used polymerization inhibitor in the art, and typical examples include: N-nitroso-N-phenylhydroxylamine aluminum (inhibitor 510) and the like.

[0025] Preferably, the photoinitiator is selected from one of 2,4,6-(trimethylbenzoyl)-diphenylphosphine oxide, 2-methyl-1-(4-methylthiophenyl)-2-morpholinyl-1-propanone, or a combination of two thereof; more preferably, when the photoinitiator is a combination of 2,4,6-(trimethylbenzoyl)-diphenylphosphine oxide and 2-methyl-1-(4-methylthiophenyl)-2-morpholinyl-1-propanone, the molar ratio of the two, n[2,4,6-(trimethylbenzoyl)-diphenylphosphine oxide]:n[2-methyl-1-(4-methylthiophenyl)-2-morpholinyl-1-propanone], is 3:1.

[0026] Preferably, by weight, the UV blue glue has: Nano silicon dioxide: 5-15 parts Acrylate monomer: 125-150 parts Photoinitiator: 3-7 parts Additives: 5-10 parts Diluent: 60-80 parts.

[0027] The diluent involved in the present invention is a commonly used diluent in the field, and typical examples include: ethyl acetate, butyl acetate, methanol, ethanol, propanol, isopropanol, isobutanol, n-butanol, methyl isobutyl ketone, isophorone, acetone, butanone, cyclohexanone, toluene, xylene, propylene glycol methyl ether and dipropylene glycol methyl ether.

[0028] The inventors have found that when the addition amount of nano-silicon dioxide (parts by weight) is 5 to 15 parts, the dispersion efficiency of the photoinitiator can be effectively improved, thereby accelerating the curing speed of the UV blue glue. When the addition amount of nano-silicon dioxide is less than 5 parts, the improvement of the dispersion efficiency of the photoinitiator is not obvious, and the viscosity of the mixture will be lower than 900mPa·s, which cannot meet the bonding performance requirements of UV blue glue used in electronic packaging, optical component manufacturing and other fields; when the addition amount of nano-silicon dioxide is greater than 15 parts, the viscosity of the mixture will be too high, and the mixture will easily agglomerate, which is not conducive to the uniform mixing of the various substances.

[0029] In addition, the inventors also found that when hydrophobic nano-silica is pre-mixed with acrylate monomers (especially ethylene glycol diacrylate or butyl acrylate, etc.), the effect is not as good as the pre-mixing effect when hydrophilic nano-silica is used. Therefore, the present invention preferably performs surface modification on the hydrophobic nano-silica before pre-mixing with the acrylate monomers.

[0030] More preferably, if the nano-silica used is hydrophobic nano-silica, then before step S1, the surface of the nano-silica is first modified by a silane coupling agent; further preferably, the silane coupling agent is KH-570.

[0031] (Example 1) 9g of dried nano-silica and 130g of ethylene glycol diacrylate were pre-mixed and dispersed at 40°C and 300rpm for 25min to obtain a pre-mixed dispersion; 5g of 2,4,6-(trimethylbenzoyl)-diphenylphosphine oxide and 1g of defoamer were added to the pre-mixed dispersion, and the mixture was stirred at 40°C and 300rpm for 25min to obtain a main agent mixture. After the main agent mixture was subjected to ultrasonic dispersion treatment (20-40 kHz) for 20 minutes, 75g of ethanol was added to adjust the viscosity of the mixture to 1050mPa·s, and the undispersed particles therein were removed by filtration, and the target product UV blue glue was obtained after standing and defoaming.

[0032] The obtained UV blue glue is sprayed onto the surface of the aluminum alloy plate by 3D printing or using a piezoelectric valve, with a spray thickness of 30-150μm, and then 365-405nm energy and 800mW / cm 2 The UV light source was used for irradiation, and the curing time at 25°C was recorded.

[0033] Examples 2-3 and Comparative Example 1 The adjusted parameters were set as shown in Table 1, and the unadjusted parameters were the same as Example 1, to obtain Examples 2-3, Comparative Example 1 without the addition of nano-silicon dioxide, and Comparative Example 2 with an addition amount of 20 g of nano-silicon dioxide. The viscosity values ​​(mPa·s) of each Example and Comparative Example at 25°C were measured and recorded in Table 1.

[0034] Table 1 The UV blue glue of Examples 1-3 and Comparative Examples 1-2 were first subjected to a 6kV breakdown voltage test, and then subjected to a high-temperature residual glue test at 260°C for ten minutes. The test results are listed in Table 2.

[0035] Table 2 The UV blue glue prepared in Examples 1 to 3 of the present invention has good rapid curing and high-voltage breakdown resistance performance, and can meet the bonding requirements of power batteries on high-voltage platforms.

Claims

1. A method for preparing a fast-curing UV blue glue, characterized in that: The preparation method comprises the following steps: S1 material preparation: drying nano silicon dioxide; S2 premixing and dispersing: premixing and dispersing the nano-silicon dioxide and the acrylate monomer under low-speed stirring to obtain a premixed dispersion, wherein the low-speed stirring state is at a mixture temperature of 40-50° C. and a stirring speed of 200-500 rpm for 20-25 minutes; S3 main agent mixing: adding a photoinitiator and an auxiliary agent to the premixed dispersion obtained in step S2, and continuing to stir at a low speed to obtain a main agent mixture, wherein the low-speed stirring state is stirring for 20-30 minutes at a mixture temperature of 40-50°C and a stirring speed of 200-500rpm; the initiating light source of the photoinitiator is ultraviolet light, and the auxiliary agent includes a defoaming agent; S4 ultrasonic dispersion: using ultrasonic dispersion to treat the mixture obtained in step S3 to ensure that no agglomeration occurs, wherein the ultrasonic dispersion treatment is performed at 20-40 kHz for 15-30 minutes; S5: adjusting viscosity: cooling the mixture obtained in step S4 to 25° C., adding a diluent, and adjusting the viscosity of the mixture to 900-1200 mPa·s; S6 Filtration and defoaming: For the mixture obtained after adjusting the viscosity in step S5, filter to remove the undispersed particles therein, and after standing and defoaming, obtain the blue glue to be solidified, which is stored in a sealed light-proof container.

2. The method for preparing the fast-curing UV blue glue according to claim 1, characterized in that: The acrylate monomer is one of ethylene glycol diacrylate and butyl acrylate or a combination of both.

3. The method for preparing the fast-curing UV blue glue as claimed in claim 1, characterized in that: The photoinitiator is selected from one or a combination of 2,4,6-(trimethylbenzoyl)-diphenylphosphine oxide and 2-methyl-1-(4-methylthiophenyl)-2-morpholinyl-1-propanone.

4. The method for preparing the fast-curing UV blue glue according to claim 3, characterized in that: When the photoinitiator is a combination of 2,4,6-(trimethylbenzoyl)-diphenylphosphine oxide and 2-methyl-1-(4-methylthiophenyl)-2-morpholinyl-1-propanone, the molar ratio of the two, n[2,4,6-(trimethylbenzoyl)-diphenylphosphine oxide]:n[2-methyl-1-(4-methylthiophenyl)-2-morpholinyl-1-propanone], is 3:

1.

5. The method for preparing the fast-curing UV blue glue as claimed in claim 1, characterized in that: The auxiliary agent may further include one or a combination of two or more of a leveling agent, a defoaming agent, a temperature stabilizer or a polymerization inhibitor.

6. The method for preparing the fast-curing UV blue glue as claimed in claim 1 or 2, characterized in that: If the nano-silica used is hydrophobic nano-silica, before step S1, the surface of the nano-silica is first modified by a silane coupling agent.

7. The method for preparing the fast-curing UV blue glue as claimed in claim 6, characterized in that: The silane coupling agent is KH-570.

8. The method for preparing the fast-curing UV blue glue according to any one of claims 1 to 7, characterized in that: By weight, the UV blue glue has: Nano silicon dioxide: 5-15 parts Acrylate monomer: 125-150 parts Photoinitiator: 3-7 parts Additives: 5-10 parts Diluent: 60-80 parts.