Acrylate adhesive for sealing energy storage aerogel pad and preparation method thereof
By combining monomers such as bismaleimide and initiators with specific ratios, the cross-linking density and heat resistance of the adhesive are improved, and the peel strength is solved The problem of insufficient is that adhesives with high peel strength and moisture resistance are achieved, suitable for sealing purposes and have industrial production value.
Patent Information
- Application Number
- CN202411632968.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-15
- Publication Date
- 2025-01-03
AI Technical Summary
The peel strength of existing adhesives is insufficient, making it difficult to meet certain high-demand application needs.
Using acrylic adhesive components A and B with specific ratios, the reaction conditions and time are controlled to improve the cross-linking density and heat resistance of the resin by adding monomers such as bismaleimide and initiators. Enhance peel strength.
Acrylate adhesive with high peel strength and good moisture and heat resistance is achieved, which is suitable for sealing purposes and the preparation method is suitable for industrial production.
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Abstract
Description
Technical Field
[0001] The invention relates to the technical field of adhesives, and in particular to an acrylic adhesive for sealing an energy storage aerogel pad and a preparation method thereof. Background Art
[0002] Adhesives, as a commonly used adhesive, can tightly bond two or more substances together and have been widely used in aircraft, automobiles, construction, electronic products and other fields.
[0003] Chinese patent CN112812718A discloses a high-performance polyurethane adhesive preparation process, and the high-performance polyurethane adhesive produced has good use effect, strong high temperature resistance, adaptable viscosity, safety and reliability; Chinese patent CN116814184B discloses a method for preparing a low residual adhesive pressure-sensitive adhesive, which not only promotes the cross-linking density of the main adhesive, but also introduces N-containing heterocycles and -Si-O-Si- chains into the adhesive, thereby effectively improving the adhesive's stickiness and heat resistance, improving the adhesive's flame retardant properties, and making it difficult for the adhesive to leave residue on the adherend, effectively reducing the residual adhesive phenomenon. However, the peel strength of the adhesive in the above-mentioned prior art still needs to be improved. Summary of the invention
[0004] In order to solve the problems in the prior art, the first aspect of the present invention provides an acrylic adhesive for sealing an energy storage aerogel pad, wherein the raw materials for preparing the acrylic adhesive include: component A and component B; the raw materials for preparing component A include a first mixed monomer, a first initiator and a first solvent; the raw materials for preparing component B include a second mixed monomer, a second initiator and a second solvent.
[0005] In one embodiment, the mass ratio of component A to component B is (5-15):1.
[0006] In one embodiment, the mass ratio of component A to component B is (10-15):1.
[0007] In one embodiment, the first mixed monomer includes one or both of an acrylate monomer and an acrylonitrile monomer.
[0008] In one embodiment, the first mixed monomer includes an acrylate monomer and an acrylonitrile monomer.
[0009] In one embodiment, the acrylic acid ester monomer includes one or more of butyl methacrylate, ethyl acrylate, and glycidyl methacrylate.
[0010] In one embodiment, the acrylate monomers include butyl methacrylate, ethyl acrylate, and glycidyl methacrylate.
[0011] In one embodiment, ethyl acrylate in the first mixed monomer accounts for 12-17% of the total mass of component A.
[0012] In one embodiment, the second mixed monomer includes a bismaleimide monomer.
[0013] In one embodiment, the bismaleimide monomer accounts for 8-10% of the total mass of component B.
[0014] In one embodiment, the second mixed monomer further comprises butyl methacrylate, hydroxyethyl acrylate, ethyl acrylate and acrylic acid.
[0015] In one embodiment, the first initiator and the second initiator both include at least one of azobisisovaleronitrile, benzoyl peroxide, and azobisisobutyronitrile.
[0016] In one embodiment, the first initiator and the second initiator are both benzoyl peroxide.
[0017] In one embodiment, the first solvent and the second solvent are both ethyl acetate.
[0018] In one embodiment, the raw materials for preparing component A include, by weight, 16-65 parts of a first mixed monomer, 0.1-2 parts of a first initiator, and 50-65 parts of a first solvent; the raw materials for preparing component B include, by weight, 41-85 parts of a second mixed monomer, 0.1-2 parts of a second initiator, and 20-40 parts of a second solvent.
[0019] In one embodiment, the raw materials for preparing component A include, by weight, 5-20 parts of butyl methacrylate, 5-20 parts of ethyl acrylate, 5-20 parts of acrylonitrile, 1-5 parts of glycidyl methacrylate, 50-65 parts of ethyl acetate and 0.1-2 parts of benzoyl peroxide.
[0020] In one embodiment, the raw materials for preparing component B include, by weight, 10-20 parts of butyl methacrylate, 5-15 parts of hydroxyethyl acrylate, 15-20 parts of ethyl acrylate, 10-20 parts of acrylic acid, 1-10 parts of bismaleimide, 20-40 parts of ethyl acetate and 0.1-2 parts of benzoyl peroxide.
[0021] The second aspect of the present invention provides a method for preparing an acrylic adhesive for sealing an energy storage aerogel pad, comprising the following steps: adding component A and component B in proportion to a reactor, heating to 40-50° C. and stirring evenly, and cooling to obtain the acrylic adhesive for sealing an energy storage aerogel pad.
[0022] In one embodiment, the preparation method of component A comprises the following steps: S1: Add 10-50wt% of the total amount of the first mixed monomer, 20-30wt% of the total amount of the first initiator and 25-35wt% of the total amount of the first solvent into the reactor, stir and heat, control the speed at 160-200r / min, and control the temperature at 80-88°C for 1-2h; S2: 20-30wt% of the total amount of the first initiator, 10-20wt% of the total amount of the first solvent and the remaining first mixed monomer are mixed evenly and added into a dropping funnel; S3: After the reaction of S1 is completed, the temperature is maintained at 80-88°C, and the mixture of S2 is added dropwise for 2-3 hours. After the addition is completed, the mixture is kept warm for 1-2 hours, and then 10-20wt% of the total amount of the first initiator is added. The mixture is kept warm for another 1-2 hours. Then, the remaining first initiator is added, and the reaction is continued for 1-2 hours. Then, the remaining first solvent is added and stirred for 5-10 minutes, and then cooled to obtain component A.
[0023] In one embodiment, the preparation method of component A comprises the following steps: S1: Add 30wt% of the total amount of the first mixed monomer, 25wt% of the total amount of the first initiator and 30wt% of the total amount of the first solvent into the reactor, stir and heat, control the speed at 180r / min, and control the temperature at 84°C for 1.5h; S2: 25 wt% of the total amount of the first initiator, 15 wt% of the total amount of the first solvent and the remaining first mixed monomer are mixed evenly and added into a dropping funnel; S3: After the reaction of S1 is completed, the temperature is maintained at 84°C, and the mixture of S2 is added dropwise for 2.5 hours. After the addition is completed, the mixture is kept warm for reaction for 1.5 hours. Then, 15 wt% of the total amount of the first initiator is added, and the mixture is kept warm for reaction again for 1.5 hours. Then, the remaining first initiator is added, and the mixture is kept warm for reaction for 1.5 hours. Then, the remaining first solvent is added, stirred for 8 minutes, and cooled to obtain component A.
[0024] In one embodiment, the preparation method of component B comprises the following steps: adding 20-30wt% of the total amount of the second initiator, a second mixed monomer, and a second solvent, heating while stirring, controlling the speed at 160-200r / min, controlling the temperature at 70-80°C, and reacting for 6-10h; adding 20-30wt% of the total amount of the second initiator, keeping the temperature for reaction again for 1-2h, then adding the remaining second initiator, continuing the keeping temperature for reaction for 1-2h, and cooling to obtain component B.
[0025] In one embodiment, the preparation method of component B comprises the following steps: adding 25wt% of the total amount of the second initiator, a second mixed monomer, and a second solvent, heating while stirring, controlling the speed at 180r / min, the temperature at 75°C, and reacting for 8h; adding 25wt% of the total amount of the second initiator, keeping the temperature for reaction again for 1.5h, then adding the remaining second initiator, continuing the keeping temperature for reaction for 1.5h, and cooling to obtain component B.
[0026] Beneficial Effects 1. The acrylate adhesive for energy storage aerogel pad sealing provided by the present invention is composed of a specific amount of component A and component B. By controlling the ratio of the raw materials and the addition of bismaleimide, the obtained acrylate adhesive has a suitable viscosity, excellent heat resistance, high peel strength, good moisture and heat resistance, and fast low-temperature curing rate.
[0027] 2. Component A in the present invention is composed of a specific acrylate monomer, an initiator system and an additive, and benzoyl peroxide is selected as the initiator. At a lower reaction temperature, a shorter dropwise addition time and a method of keeping warm again after adding the initiator make the resin have a high conversion rate. The lower reaction temperature and the shorter dropwise addition time make the resin molecular weight controlled at a higher level without affecting the film-forming performance of the resin.
[0028] 3. The present invention controls the amount of acrylonitrile monomer and glycidyl methacrylate in component A so that the resin has a better crosslinking density during the film-forming process, and at the same time makes the peel strength and heat resistance of the system better.
[0029] 4. Component B of the present invention is prepared by polymerization reaction of butyl methacrylate, hydroxyethyl acrylate, ethyl acrylate, acrylic acid, bismaleimide and initiator, and bismaleimide is introduced into the acrylic adhesive resin. Since it contains benzene rings and imide heterocycles, it has a higher cross-linking density, thereby improving the heat resistance, moisture and heat resistance and peel strength of the acrylic adhesive resin.
[0030] 5. The preparation method provided by the present invention can be applied to industrial production and has higher practical value. DETAILED DESCRIPTION
[0031] In order to make the purpose, technical scheme and advantages of the present invention clearer, the present invention is further described in detail below in conjunction with the examples. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not intended to limit the present invention. The experimental methods in the examples without specifying specific conditions are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used without specifying the manufacturer are all conventional products that can be purchased commercially.
[0032] Examples 1-9, Comparative Examples 1-8 Embodiments 1-9 and Comparative Examples 1-8 of the present invention provide, in a first aspect, an acrylic adhesive for sealing an energy storage aerogel pad. The raw materials for preparation are shown in Table 1 and Table 2, respectively, in parts by weight.
[0033] Embodiments 1-9 and comparative examples 1-8 of the present invention provide a second aspect of a method for preparing an acrylic adhesive for sealing an energy storage aerogel pad, comprising the following steps: adding component A and component B in proportion to a reactor, heating to 45° C. and stirring evenly, and cooling to obtain the acrylic adhesive for sealing an energy storage aerogel pad.
[0034] The preparation method of component A comprises the following steps: S1: Add 30wt% of the total amount of the first mixed monomer, 25wt% of the total amount of the first initiator and 30wt% of the total amount of the first solvent into the reactor, stir and heat, control the speed at 180r / min, and control the temperature at 84°C for 1.5h; S2: 25 wt% of the total amount of the first initiator, 15 wt% of the total amount of the first solvent and the remaining first mixed monomer are mixed evenly and added into a dropping funnel; S3: After the reaction of S1 is completed, the temperature is maintained at 84°C, and the mixture of S2 is added dropwise for 2.5 hours. After the addition is completed, the mixture is kept warm for reaction for 1.5 hours. Then, 15 wt% of the total amount of the first initiator is added, and the mixture is kept warm for reaction again for 1.5 hours. Then, the remaining first initiator is added, and the mixture is kept warm for reaction for 1.5 hours. Then, the remaining first solvent is added, stirred for 8 minutes, and cooled to obtain component A.
[0035] The preparation method of component B comprises the following steps: adding 25wt% of the total amount of the second initiator, a second mixed monomer, and a second solvent, heating while stirring, controlling the rotation speed at 180r / min, the temperature at 75°C, and reacting for 8h; adding 25wt% of the total amount of the second initiator, keeping the temperature for reaction again for 1.5h, then adding the remaining second initiator, continuing the keeping temperature for reaction for 1.5h, and cooling to obtain component B.
[0036] Performance Testing 1. Peel strength test: The adhesives prepared in Examples 1-9 and Comparative Examples 1-8 were coated on polyimide films, and samples were prepared at 80° C. The samples were tested according to IPC-TM-650. The test results are shown in Tables 1 and 2.
[0037] 2. Moisture and heat stability test: The adhesives of Examples 1-9 and Comparative Examples 1-8 were coated on polyimide films, and samples were made at 80°C. After being placed in an environment of 85°C / 85%RH for 72 hours, peel strength tests were performed. The test results are shown in Tables 1 and 2.
[0038] In Table 2, “ / ” means that the viscosity is too high to be coated.
[0039] Table 1
[0040] Table 2
Claims
1. An acrylic adhesive for sealing an energy storage aerogel pad, characterized in that: The raw materials for preparing the composition include: component A and component B; the raw materials for preparing component A include a first mixed monomer, a first initiator and a first solvent; the raw materials for preparing component B include a second mixed monomer, a second initiator and a second solvent.
2. The acrylic adhesive for sealing the energy storage aerogel pad according to claim 1, characterized in that: The mass ratio of component A to component B is (5-15):
1.
3. The acrylic adhesive for sealing the energy storage aerogel pad according to claim 1, characterized in that: The first mixed monomer includes one or both of acrylate monomer and acrylonitrile monomer.
4. The acrylic adhesive for sealing the energy storage aerogel pad according to claim 3, characterized in that: The acrylic acid ester monomer includes one or more of butyl methacrylate, ethyl acrylate, and glycidyl methacrylate.
5. The acrylic adhesive for sealing the energy storage aerogel pad according to claim 1, characterized in that: The second mixed monomer includes a bismaleimide monomer.
6. The acrylic adhesive for sealing the energy storage aerogel pad according to claim 1, characterized in that: The first initiator and the second initiator both include at least one of azobisisovaleronitrile, benzoyl peroxide, and azobisisobutyronitrile.
7. The acrylic adhesive for sealing the energy storage aerogel pad according to claim 1, characterized in that: The raw materials for preparing component A include, by weight, 16-65 parts of a first mixed monomer, 0.1-2 parts of a first initiator and 50-65 parts of a first solvent; the raw materials for preparing component B include, by weight, 41-85 parts of a second mixed monomer, 0.1-2 parts of a second initiator and 20-40 parts of a second solvent.
8. A method for preparing the acrylic adhesive for sealing the energy storage aerogel pad according to any one of claims 1 to 7, characterized in that: The method comprises the following steps: adding component A and component B in a proportion into a reactor, heating to 40-50° C. and stirring evenly, and cooling to obtain the acrylic adhesive for sealing the energy storage aerogel pad.
9. The method for preparing the acrylic adhesive for sealing the energy storage aerogel pad according to claim 8, characterized in that: The preparation method of component A comprises the following steps: S1: Add 10-50wt% of the total amount of the first mixed monomer, 20-30wt% of the total amount of the first initiator and 25-35wt% of the total amount of the first solvent into the reactor, stir and heat, control the speed at 160-200r / min, and control the temperature at 80-88°C for 1-2h; S2: 20-30wt% of the total amount of the first initiator, 10-20wt% of the total amount of the first solvent and the remaining first mixed monomer are mixed evenly and added into a dropping funnel; S3: After the reaction of S1 is completed, the temperature is maintained at 80-88°C, and the mixture of S2 is added dropwise for 2-3 hours. After the addition is completed, the mixture is kept warm for 1-2 hours, and then 10-20wt% of the total amount of the first initiator is added. The mixture is kept warm for another 1-2 hours. Then, the remaining first initiator is added, and the reaction is continued for 1-2 hours. Then, the remaining first solvent is added and stirred for 5-10 minutes, and then cooled to obtain component A.
10. The method for preparing the acrylic adhesive for sealing the energy storage aerogel pad according to claim 8, characterized in that: The preparation method of component B comprises the following steps: adding 20-30wt% of the total amount of the second initiator, a second mixed monomer, and a second solvent, heating while stirring, controlling the rotation speed at 160-200r / min, controlling the temperature at 70-80°C, and reacting for 6-10h; adding 20-30wt% of the total amount of the second initiator, keeping the temperature for reaction again for 1-2h, then adding the remaining second initiator, continuing the keeping temperature for reaction for 1-2h, and cooling to obtain component B.
