Preparation method of adhesive with high adhesive property

Abstract

The invention relates to the technical field of adhesive production, in particular to a preparation method of an adhesive with high adhesive property. The adhesive with the high adhesive property is prepared from the following raw materials in parts by weight: 30 to 40 parts of bisphenol A epoxy resin, 3 to 6 parts of a functional additive, 3 to 5 parts of a synergistic additive, 2 to 4 parts of a surfactant, 2 to 4 parts of a curing agent, 1 to 3 parts of dibutyltin dilaurate, 2 to 4 parts of bis (3-ethyl-5-methyl-4-maleimidophenyl) methane and 1 to 3 parts of zinc naphthenate, the high-bonding-property adhesive prepared by the invention not only has better mechanical properties, but also has excellent flame retardance and aging resistance, and the quality of the high-bonding-property adhesive is effectively ensured.

Description

Technical Field

[0001] The present invention relates to the technical field of adhesive production, and specifically to a preparation method of an adhesive with high bonding performance. Background Art

[0002] In modern industrial production and daily life, adhesives, as an important functional material that can firmly connect different materials together, are widely used in many fields such as construction, automobile manufacturing, electronic appliances, and aerospace. With the continuous development and progress of various industries, the performance requirements for adhesives are also increasing day by day. The commonly used adhesives in the market are mostly water-based polyurethane adhesives, which use water as a solvent. Although they have good environmental protection performance, they have problems such as a narrow range of use and low bonding strength.

[0003] Based on this, the present invention provides a preparation method of an adhesive with high bonding performance to solve the above-mentioned technical problems. Summary of the Invention

[0004] The purpose of the present invention is to provide a preparation method of an adhesive with high bonding performance. The prepared adhesive with high bonding performance not only has good mechanical properties, but also has excellent flame retardant and anti-aging properties, effectively ensuring its quality and quality.

[0005] To achieve the above purpose, the present invention provides the following technical solutions:

[0006] The present invention provides a preparation method of an adhesive with high bonding performance. The adhesive is composed of the following raw materials in parts by weight: 30-40 parts of bisphenol A epoxy resin, 3-6 parts of functional additives, 3-5 parts of synergistic additives, 2-4 parts of surfactants, 2-4 parts of curing agents, 1-3 parts of dibutyltin dilaurate, 2-4 parts of bis(3-ethyl-5-methyl-4-maleimidophenyl)methane, and 1-3 parts of zinc naphthenate;

[0007] The preparation process of the adhesive with high bonding performance is as follows:

[0008] Step 1: Accurately weigh bisphenol A epoxy resin, functional additives, synergistic additives, surfactants, curing agents, dibutyltin dilaurate, bis(3-ethyl-5-methyl-4-maleimidophenyl)methane, and zinc naphthenate, and set aside;

[0009] Step 2: Stir and mix bisphenol A epoxy resin, functional additives, synergistic additives, surfactants, and bis(3-ethyl-5-methyl-4-maleimidophenyl)methane;

[0010] Step 3: After heating up, add curing agents, dibutyltin dilaurate, and zinc naphthenate and stir well. After cooling, the finished product of the adhesive with high bonding performance is prepared.

[0011] A further setting of the present invention is as follows: The preparation process of the functional auxiliary is as follows:

[0012] Triphenyl phosphate is placed in absolute ethanol at a dosage ratio of 0.05 - 0.1 g / mL, and stirred for 15 - 20 min under the condition of 120 - 150 r / min. Mica powder pretreated with 120 - 200% of the mass of triphenyl phosphate is added thereto. Under a nitrogen atmosphere, the temperature is raised to 100 °C and treated for 8 - 10 h under the condition of 300 - 350 r / min. After cooling to room temperature, centrifugation is carried out at 5000 - 6000 r / min for 10 - 15 min. The obtained centrifuged product is washed 2 - 4 times with deionized water, and then dried at 70 - 80 °C for 12 - 14 h to obtain the first material;

[0013] Graphene oxide is placed in deionized water at a dosage ratio of 0.12 - 0.22 g / mL and ultrasonically treated for 15 - 20 min. The first material with 150 - 200% of the mass of graphene oxide is added thereto. At room temperature, it is treated for 120 - 150 min under the condition of 200 - 300 r / min. After suction filtration, it is dried to constant weight at a temperature of 50 - 60 °C to obtain the second material;

[0014] The second material is placed in the compound solution at a dosage ratio of 0.08 - 0.14 g / mL, and treated for 20 - 30 min under the conditions of 50 - 60 °C and 150 - 200 r / min. After suction filtration, it is dried to constant weight at a temperature of 50 - 60 °C to obtain the functional auxiliary.

[0015] A further setting of the present invention is as follows: The preparation process of the pretreated mica powder is as follows:

[0016] Mica powder is placed in an aqueous sodium hydroxide solution with a mass concentration of 1.5 - 3% at a dosage ratio of 0.01 - 0.08 g / mL, and stirred for 30 - 40 min under the conditions of 50 - 60 °C and 50 - 100 r / min;

[0017] After suction filtration, it is washed 2 - 4 times with deionized water and dried to constant weight at a temperature of 50 - 60 °C to obtain the pretreated mica powder.

[0018] A further setting of the present invention is as follows: The compound solution is prepared by compounding γ - aminopropyltriethoxysilane and absolute ethanol at a mass ratio of 0.12 - 0.22:1.

[0019] A further setting of the present invention is as follows: The preparation process of the synergistic auxiliary is as follows:

[0020] The nano-clay is placed in a γ-aminopropyltriethoxysilane ethanol solution with a mass concentration of 0.5-1.2% according to a dosage ratio of 0.05-0.1 g / mL, and is treated at 50-70 °C and 200-400 r / min for 120-150 min, centrifuged at 4000-6000 r / min for 10-15 min, the obtained centrifuged product is washed with absolute ethanol 2-4 times, and is placed under the condition of 60-80 °C for vacuum drying for 20-24 h to obtain the pretreated nano-clay;

[0021] Tetraethyl orthosilicate is placed in the mixed solution according to a mass ratio of 0.15-0.25:1, and is treated at 100-120 r / min for 5-10 min, then the pH is adjusted to 8-9 with ammonia water, 25-45% of the pretreated nano-clay based on the mass of tetraethyl orthosilicate is added thereto, and is treated at 30-60 °C and 300-400 r / min for 20-24 h, centrifuged at 4000-6000 r / min for 10-15 min, the obtained centrifuged product is washed with absolute ethanol 2-4 times, and is placed under the condition of 60-80 °C for vacuum drying for 20-24 h to obtain the pretreated nano-clay.

[0022] The present invention is further arranged such that: the mixed solution is formed by mixing absolute ethanol and deionized water according to a mass ratio of 0.12-0.22:1.

[0023] The present invention is further arranged such that: the surfactant is selected from any one of sodium lignosulfonate and sodium dodecylbenzenesulfonate.

[0024] The present invention is further arranged such that: the curing agent is selected from any one of phthalic anhydride and maleic anhydride.

[0025] The present invention is further arranged such that: in the third step, the temperature for heating up is 45-65 °C.

[0026] Compared with the prior art, the beneficial effect of the present invention is:

[0027] In the present invention, bisphenol A epoxy resin, functional additives, synergistic additives, surfactants, curing agents, dibutyltin dilaurate, bis(3-ethyl-5-methyl-4-maleimidophenyl)methane, zinc naphthenate, etc. are used as raw materials. By stirring and mixing bisphenol A epoxy resin, functional additives, synergistic additives, surfactants and bis(3-ethyl-5-methyl-4-maleimidophenyl)methane, heating up, adding curing agents, dibutyltin dilaurate and zinc naphthenate and fully stirring, and then cooling, an adhesive finished product with high bonding performance is prepared. The adhesive with high bonding performance prepared by the present invention not only has good mechanical properties, but also has excellent flame retardant and aging resistance properties, effectively ensuring its quality and quality. The preparation method of the adhesive with high bonding performance provided by the present invention has a broader market prospect and is more suitable for popularization. Detailed Embodiments

[0028] The following will combine 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 a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments in the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts belong to the scope of protection of the present invention.

[0029] Example 1

[0030] This example provides a preparation method of an adhesive with high bonding performance. The adhesive is composed of the following raw materials in parts by weight: 30 parts of bisphenol A epoxy resin, 3 parts of functional additives, 3 parts of synergistic additives, 2 parts of surfactants, 2 parts of curing agents, 1 part of dibutyltin dilaurate, 2 parts of bis(3-ethyl-5-methyl-4-maleimidophenyl)methane and 1 part of zinc naphthenate.

[0031] In this example, it should be noted that the bisphenol A epoxy resin is purchased from Guangzhou Taili Chemical Co., Ltd.

[0032] Among them, the preparation process of the functional additives is as follows:

[0033] Triphenyl phosphate is placed in absolute ethanol at a dosage ratio of 0.05 g / mL, stirred for 15 min under the condition of 120 r / min, mica powder pretreated with 120% of the mass of triphenyl phosphate is added thereto, heated to 100 °C under a nitrogen atmosphere, treated for 8 h under the condition of 300 r / min, cooled to room temperature, centrifuged at 5000 r / min for 10 min, the obtained centrifuged product is washed 2 times with deionized water, and then dried at 70 °C for 12 h to obtain the first material;

[0034] Graphene oxide was placed in deionized water and ultrasonically treated for 15 min at a dosage ratio of 0.12 g / mL. The first material, which was 150% of the mass of graphene oxide, was added thereto. At room temperature, it was treated for 120 min under the condition of 200 r / min. After suction filtration, it was dried to a constant weight at a temperature of 50 °C to obtain the second material;

[0035] The second material was placed in the compound solution at a dosage ratio of 0.08 g / mL and treated for 20 min at 50 °C and 150 r / min. After suction filtration, it was dried to a constant weight at a temperature of 50 °C to obtain the functional additive.

[0036] Furthermore, the preparation process of the pretreated mica powder is as follows:

[0037] Mica powder was placed in an aqueous sodium hydroxide solution with a mass concentration of 1.5% at a dosage ratio of 0.01 g / mL and stirred at 50 °C and 50 r / min for 30 min;

[0038] After suction filtration, it was washed twice with deionized water and dried to a constant weight at a temperature of 50 °C to obtain the pretreated mica powder.

[0039] The compound solution was prepared by compounding γ-aminopropyltriethoxysilane and absolute ethanol at a mass ratio of 0.12:1.

[0040] In this example, it should be noted that the mica powder was purchased from Hebei Huayuan Mining Co., Ltd., and the graphene oxide was purchased from Wuhan Lanaibai Pharmaceutical Chemical Co., Ltd.

[0041] Among them, the preparation process of the synergistic additive is as follows:

[0042] Nanoclay was placed in a γ-aminopropyltriethoxysilane ethanol solution with a mass concentration of 0.5% at a dosage ratio of 0.05 g / mL and treated for 120 min at 50 °C and 200 r / min. It was centrifuged for 10 min at 4000 r / min. The obtained centrifuged product was washed twice with absolute ethanol and vacuum dried at 60 °C for 20 h to obtain the pretreated nanoclay;

[0043] Ethyl orthosilicate was placed in the mixed solution at a mass ratio of 0.15:1 and treated for 5 min at 100 r / min. Then the pH was adjusted to 8 with ammonia water. 25% of the pretreated nanoclay based on the mass of ethyl orthosilicate was added thereto and treated for 20 h at 30 °C and 300 r / min. It was centrifuged for 10 min at 4000 r / min. The obtained centrifuged product was washed twice with absolute ethanol and vacuum dried at 60 °C for 20 h to obtain the pretreated nanoclay.

[0044] Further, the mixed solution is formed by mixing absolute ethanol and deionized water in a mass ratio of 0.12:1.

[0045] In this embodiment, it should be noted that the nano-clay is purchased from Shijiazhuang Fengming Mineral Products Co., Ltd.

[0046] Among them, the surfactant is selected as sodium lignosulfonate.

[0047] The curing agent is selected as phthalic anhydride.

[0048] In addition, this embodiment also provides the preparation process of the above-mentioned adhesive with high bonding performance as follows:

[0049] Step 1: Accurately weigh bisphenol A epoxy resin, functional additives, synergistic additives, surfactant, curing agent, dibutyltin dilaurate, bis(3-ethyl-5-methyl-4-maleimidophenyl)methane and zinc naphthenate, and set aside;

[0050] Step 2: Stir and mix bisphenol A epoxy resin, functional additives, synergistic additives, surfactant and bis(3-ethyl-5-methyl-4-maleimidophenyl)methane;

[0051] Step 3: After heating up, add the curing agent, dibutyltin dilaurate and zinc naphthenate and stir well. After cooling, the finished adhesive with high bonding performance is prepared.

[0052] Among them, the temperature for heating up is 45°C.

[0053] Example 2

[0054] The preparation method of the adhesive with high bonding performance provided in this embodiment is basically the same as that in Example 1, except that: the specific raw material composition and the specific preparation method of the adhesive with high bonding performance in this embodiment are different; the specific raw material composition and the specific preparation method of the adhesive with high bonding performance in this embodiment are as follows:

[0055] A preparation method of an adhesive with high bonding performance, and the adhesive is composed of the following raw materials in parts by weight: 35 parts of bisphenol A epoxy resin, 4 parts of functional additives, 4 parts of synergistic additives, 3 parts of surfactant, 3 parts of curing agent, 2 parts of dibutyltin dilaurate, 3 parts of bis(3-ethyl-5-methyl-4-maleimidophenyl)methane and 2 parts of zinc naphthenate.

[0056] In this embodiment, it should be noted that the bisphenol A epoxy resin is purchased from Guangzhou Taili Chemical Industry Co., Ltd.

[0057] Among them, the preparation process of the functional additives is as follows:

[0058] Triphenyl phosphate was placed in absolute ethanol at a dosage ratio of 0.07 g / mL and stirred for 17 min under the condition of 135 r / min. Mica powder pretreated at 160% of the mass of triphenyl phosphate was added thereto. Under a nitrogen atmosphere, the temperature was raised to 100 °C and treated for 9 h under the condition of 325 r / min. After cooling to room temperature, it was centrifuged for 12 min under the condition of 5500 r / min. The obtained centrifuged product was washed 3 times with deionized water and then dried at 75 °C for 13 h to obtain the first material;

[0059] Graphene oxide was placed in deionized water and ultrasonically treated for 17 min at a dosage ratio of 0.17 g / mL. The first material at 175% of the mass of graphene oxide was added thereto. At room temperature, it was treated for 135 min under the condition of 250 r / min. After suction filtration, it was dried to constant weight at a temperature of 55 °C to obtain the second material;

[0060] The second material was placed in the compound solution at a dosage ratio of 0.11 g / mL and treated for 25 min under the conditions of 55 °C and 175 r / min. After suction filtration, it was dried to constant weight at a temperature of 55 °C to obtain the functional additive.

[0061] Furthermore, the preparation process of the pretreated mica powder is as follows:

[0062] Mica powder was placed in a 2% sodium hydroxide aqueous solution at a dosage ratio of 0.04 g / mL and stirred for 35 min under the conditions of 55 °C and 75 r / min;

[0063] After suction filtration, it was washed 3 times with deionized water and dried to constant weight at a temperature of 55 °C to obtain the pretreated mica powder.

[0064] The compound solution was prepared by compounding γ-aminopropyltriethoxysilane and absolute ethanol at a mass ratio of 0.17:1.

[0065] In this example, it should be noted that the mica powder was purchased from Hebei Huayuan Mining Co., Ltd., and the graphene oxide was purchased from Wuhan Lanaibai Pharmaceutical and Chemical Co., Ltd.

[0066] Among them, the preparation process of the synergistic additive is as follows:

[0067] Nanoclay was placed in a 1% γ-aminopropyltriethoxysilane ethanol solution at a dosage ratio of 0.07 g / mL and treated for 135 min under the conditions of 60 °C and 300 r / min. It was centrifuged for 12 min under the condition of 5000 r / min. The obtained centrifuged product was washed 3 times with absolute ethanol and vacuum dried at 70 °C for 22 h to obtain the pretreated nanoclay;

[0068] Tetraethyl orthosilicate was placed in the mixed solution at a mass ratio of 0.2:1, treated at 110 r / min for 7 minutes, then adjusted to pH 9 with ammonia water, and nanoclay pretreated with 35% by mass of tetraethyl orthosilicate was added thereto, treated at 45°C and 350 r / min for 22 hours, centrifuged at 5000 r / min for 12 minutes, and the centrifuged product was washed three times with anhydrous ethanol, and vacuum dried at 70°C for 22 hours to obtain pretreated nanoclay.

[0069] Furthermore, the mixed liquid is prepared by mixing anhydrous ethanol and deionized water in a mass ratio of 0.17:1.

[0070] In this embodiment, it should be noted that the nanoclay was purchased from Shijiazhuang Fengming Mineral Products Co., Ltd.

[0071] Wherein, sodium dodecylbenzene sulfonate is selected as the surfactant.

[0072] Maleic anhydride is selected as the curing agent.

[0073] In addition, this embodiment also provides the following preparation process of the adhesive with high bonding performance:

[0074] Step 1, accurately weigh bisphenol A epoxy resin, functional additives, synergistic additives, surfactants, curing agents, dibutyltin dilaurate, bis(3-ethyl-5-methyl-4-maleimidophenyl)methane and zinc naphthenate for later use;

[0075] Step 2, stirring and mixing bisphenol A epoxy resin, functional additives, synergistic additives, surfactants and bis(3-ethyl-5-methyl-4-maleimidophenyl)methane;

[0076] Step 3: After heating, add curing agent, dibutyltin dilaurate and zinc cyclohexaneate and stir thoroughly. After cooling, a finished adhesive with high bonding performance is prepared.

[0077] The heating temperature is 55°C.

[0078] Example 3

[0079] The preparation method of the adhesive with high bonding performance provided in this embodiment is basically the same as that in Embodiment 1, except that: the specific raw material composition and the specific preparation method of the adhesive with high bonding performance in this embodiment are different; the specific raw material composition and the specific preparation method of the adhesive with high bonding performance in this embodiment are as follows:

[0080] A preparation method of an adhesive with high bonding performance, the adhesive is composed of the following raw materials in parts by weight: 40 parts of bisphenol A epoxy resin, 6 parts of functional additives, 5 parts of synergistic additives, 4 parts of surfactant, 4 parts of curing agent, 3 parts of dibutyltin dilaurate, 4 parts of bis(3-ethyl-5-methyl-4-maleimidophenyl)methane and 3 parts of zinc naphthenate.

[0081] In this embodiment, it should be noted that the bisphenol A epoxy resin is purchased from Guangzhou Taili Chemical Industry Co., Ltd.

[0082] Among them, the preparation process of the functional additive is as follows:

[0083] Put triphenyl phosphate into absolute ethanol according to the dosage ratio of 0.1 g / mL, stir for 20 min under the condition of 150 r / min, add mica powder pretreated with 200% of the mass of triphenyl phosphate to it, under the nitrogen atmosphere, heat up to 100 °C, and treat for 10 h under the condition of 350 r / min. After cooling to room temperature, centrifuge for 15 min under the condition of 6000 r / min. The obtained centrifuged product is washed 4 times with deionized water, and then dried at 80 °C for 14 h to obtain the first material;

[0084] Put graphene oxide into deionized water according to the dosage ratio of 0.22 g / mL and ultrasonically treat for 20 min. Add the first material with 200% of the mass of graphene oxide to it. At room temperature, treat for 150 min under the condition of 300 r / min. After suction filtration, dry at 60 °C until constant weight to obtain the second material;

[0085] Put the second material into the compound solution according to the dosage ratio of 014 g / mL, treat at 60 °C and 200 r / min for 30 min. After suction filtration, dry at 60 °C until constant weight to obtain the functional additive.

[0086] Furthermore, the preparation process of the pretreated mica powder is as follows:

[0087] Put mica powder into an aqueous sodium hydroxide solution with a mass concentration of 3% according to the dosage ratio of 0.08 g / mL, and stir for 40 min under the conditions of 60 °C and 100 r / min;

[0088] After suction filtration, wash 4 times with deionized water, and dry at 60 °C until constant weight to obtain the pretreated mica powder.

[0089] The compound solution is prepared by compounding γ-aminopropyltriethoxysilane and absolute ethanol according to a mass ratio of 0.22:1.

[0090] In this embodiment, it should be noted that the mica powder is purchased from Hebei Huayuan Mining Co., Ltd., and the graphene oxide is purchased from Wuhan Lanabai Medical and Chemical Co., Ltd.

[0091] Among them, the preparation process of the synergistic auxiliary agent is as follows:

[0092] The nano-clay is placed in a γ-aminopropyltriethoxysilane ethanol solution with a mass concentration of 1.2% at a dosage ratio of 0.1 g / mL, treated under the conditions of 70 °C and 400 r / min for 150 min, centrifuged at 6000 r / min for 15 min, and the obtained centrifuged product is washed 4 times with absolute ethanol and vacuum dried at 80 °C for 24 h to obtain pretreated nano-clay;

[0093] Ethyl orthosilicate is placed in the mixed solution at a mass ratio of 0.25:1, treated under the conditions of 120 r / min for 10 min, then the pH is adjusted to 9 with ammonia water, 45% of the pretreated nano-clay by mass of ethyl orthosilicate is added thereto, treated under the conditions of 60 °C and 400 r / min for 24 h, centrifuged at 6000 r / min for 15 min, and the obtained centrifuged product is washed 4 times with absolute ethanol and vacuum dried at 80 °C for 24 h to obtain pretreated nano-clay.

[0094] Furthermore, the mixed solution is composed of absolute ethanol and deionized water mixed at a mass ratio of 0.22:1.

[0095] In this embodiment, it should be noted that the nano-clay is purchased from Shijiazhuang Fengming Mineral Products Co., Ltd.

[0096] Among them, the surfactant is selected as sodium lignosulfonate.

[0097] The curing agent is selected as phthalic anhydride.

[0098] In addition, this embodiment also provides the preparation process of the above-mentioned adhesive with high bonding performance as follows:

[0099] Step 1: Accurately weigh bisphenol A epoxy resin, functional auxiliary agent, synergistic auxiliary agent, surfactant, curing agent, dibutyltin dilaurate, bis(3-ethyl-5-methyl-4-maleimidophenyl)methane and zinc naphthenate, and set aside;

[0100] Step 2: Stir and mix bisphenol A epoxy resin, functional auxiliary agent, synergistic auxiliary agent, surfactant and bis(3-ethyl-5-methyl-4-maleimidophenyl)methane;

[0101] Step 3: After heating up, add the curing agent, dibutyltin dilaurate and zinc naphthenate and stir well. After cooling, the finished product of the adhesive with high bonding performance is prepared.

[0102] Among them, the temperature for heating up is 65 °C.

[0103] Comparative Example 1: The difference from Example 1 is that in this example, an equal amount of mica powder is used to replace the functional auxiliary agent.

[0104] Comparative Example 2: The difference from Example 1 is that in this example, an equal amount of nano-clay is used to replace the synergistic auxiliary agent.

[0105] Performance test: The adhesive samples with high bonding performance provided in Examples 1 to 3 and Comparative Examples 1 to 2 are respectively marked as Examples 1 to 3 and Comparative Examples 1 to 2; and the relevant performances of the adhesives with high bonding performance provided in Examples 1 to 3 and Comparative Examples 1 to 2 are tested as follows:

[0106] 1. Viscosity test: The test method is in accordance with the standard of GB / T22314-2008, and a rotational viscometer is used to test the viscosity.

[0107] 2. Flame retardancy test: The test method is to conduct the test in accordance with the vertical burning rating standard of UL94-2012 for materials.

[0108] 3. Aging resistance test: The test method is to take a glass product with a specification of 25×25×3mm as the bonding substrate, wipe the surface dry with acetone, scrape and coat an adhesive film with a thickness of 0.2mm, dry it in hot air at 50°C for 1h, then naturally stand still and cure for 24h, break the glass to take out the adhesive film, and conduct a tensile strength test in accordance with the standard of GB / T1040.1-2018, and conduct artificial accelerated aging in accordance with the standard of GB / T14522-2008. The parameter settings for one cycle are: UVB-313 ultraviolet irradiation + temperature of 60°C, treatment for 4h, ultraviolet irradiation + spray water, treatment for 4h, and the total cycle time is 168h.

[0109] The obtained test data are recorded in Tables 1 to 3 below:

[0110] Table 1 Viscosity performance test results of each group of adhesives

[0111] Group Viscosity (mPa*s) Example Group 1 1634 Example Group 2 1629 Example Group 3 1631 Control Group 1 1422 Control Group 2 1510

[0112] Table 2 Flame retardancy performance test results of each group of adhesives

[0113]

[0114]

[0115] Table 3 Aging resistance performance test results of each group of adhesives

[0116] Group Initial Tensile Strength (MPa) Tensile Strength after Aging (MPa) Example Group 1 51.8 26.5 Example Group 2 51.5 26.1 Example Group 3 51.7 26.3 Control Group 1 44.8 20.4 Control Group 2 45.6 20.8

[0117] By comparing and analyzing the relevant data in Tables 1 to 3, it can be seen that the adhesive with high bonding performance prepared by the present invention not only has good mechanical properties, but also has excellent flame retardant and aging resistance properties, effectively ensuring its quality and quality. This shows that the preparation method of the adhesive with high bonding performance provided by the present invention has a broader market prospect and is more suitable for popularization.

[0118] In the description of this specification, the description with reference to terms such as "one embodiment", "example", "specific example", etc. means that the specific features, structures, materials or characteristics described in connection 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 a suitable manner in any one or more embodiments or examples.

[0119] The preferred embodiments of the present invention disclosed above are only used to help explain the present invention. The preferred embodiments do not describe all the details in detail, nor do they limit the invention to the specific embodiments described. Obviously, according to the content of this specification, many modifications and changes can be made. This specification selects and specifically describes these embodiments in order to better explain the principle and practical application of the present invention, so that those skilled in the art can well understand and utilize the present invention. The present invention is only limited by the claims and their full scope and equivalents.

Claims

1. A method for preparing an adhesive with high bonding performance, characterized in that: The adhesive is composed of the following raw materials in parts by weight: 30 to 40 parts of bisphenol A epoxy resin, 3 to 6 parts of functional additives, 3 to 5 parts of synergistic additives, 2 to 4 parts of surfactants, 2 to 4 parts of curing agents, 1 to 3 parts of dibutyltin dilaurate, 2 to 4 parts of bis(3-ethyl-5-methyl-4-maleimidophenyl)methane and 1 to 3 parts of zinc naphthenate; The preparation process of the adhesive with high bonding performance is as follows: Step 1, accurately weigh bisphenol A epoxy resin, functional additives, synergistic additives, surfactants, curing agents, dibutyltin dilaurate, bis(3-ethyl-5-methyl-4-maleimidophenyl)methane and zinc naphthenate for later use; Step 2, stirring and mixing bisphenol A epoxy resin, functional additives, synergistic additives, surfactants and bis(3-ethyl-5-methyl-4-maleimidophenyl)methane; Step 3: After heating, add curing agent, dibutyltin dilaurate and zinc cyclohexaneate and stir thoroughly. After cooling, a finished adhesive with high bonding performance is prepared.

2. The method for preparing an adhesive with high bonding performance according to claim 1, characterized in that: The preparation process of the functional additive is as follows: Triphenyl phosphate is placed in anhydrous ethanol at a dosage ratio of 0.05 to 0.1 g / mL, stirred at 120 to 150 r / min for 15 to 20 min, and mica powder pretreated with 120 to 200% of the mass of triphenyl phosphate is added thereto, and the mixture is heated to 100° C. in a nitrogen atmosphere, and treated at 300 to 350 r / min for 8 to 10 h. After cooling to room temperature, the mixture is centrifuged at 5000 to 6000 r / min for 10 to 15 min, and the obtained centrifugal product is washed with deionized water 2 to 4 times, and then dried at 70 to 80° C. for 12 to 14 h to obtain a first material; The graphene oxide is placed in deionized water for ultrasonic treatment at a dosage ratio of 0.12 to 0.22 g / mL for 15 to 20 minutes, and the first material of 150 to 200% by mass of the graphene oxide is added thereto, and the treatment is carried out at room temperature at 200 to 300 r / min for 120 to 150 minutes, and after suction filtration, the second material is dried at a temperature of 50 to 60° C. to constant weight to obtain a second material; The second material is placed in the compound liquid at a dosage ratio of 0.08-014 g / mL, treated at 50-60° C. and 150-200 r / min for 20-30 min, filtered, and dried at 50-60° C. to constant weight to obtain a functional additive.

3. The method for preparing an adhesive with high bonding performance according to claim 2, characterized in that: The preparation process of the pretreated mica powder is as follows: The mica powder is placed in a sodium hydroxide aqueous solution with a mass concentration of 1.5-3% at a dosage ratio of 0.01-0.08 g / mL, and stirred at 50-60° C. and 50-100 r / min for 30-40 minutes; After suction filtration, the product is washed with deionized water for 2 to 4 times and dried at a temperature of 50 to 60° C. to a constant weight to obtain pretreated mica powder.

4. The method for preparing an adhesive with high bonding performance according to claim 2, characterized in that: The compound liquid is compounded by mixing gamma-aminopropyltriethoxysilane and anhydrous ethanol in a mass ratio of 0.12 to 0.22:

1.

5. The method for preparing an adhesive with high bonding performance according to claim 1, characterized in that: The preparation process of the synergistic aid is as follows: The nanoclay is placed in a γ-aminopropyltriethoxysilane ethanol solution with a mass concentration of 0.5-1.2% at a dosage ratio of 0.05-0.1 g / mL, treated at 50-70° C. and 200-400 r / min for 120-150 min, centrifuged at 4000-6000 r / min for 10-15 min, the obtained centrifugal product is washed 2-4 times with anhydrous ethanol, and vacuum dried at 60-80° C. for 20-24 h to obtain the pretreated nanoclay; Tetraethyl orthosilicate is placed in a mixed solution at a mass ratio of 0.15 to 0.25:1, treated at 100 to 120 r / min for 5 to 10 minutes, then adjusted to pH 8 to 9 with ammonia water, added with nanoclay pretreated with 25 to 45% by mass of tetraethyl orthosilicate, treated at 30 to 60°C and 300 to 400 r / min for 20 to 24 hours, centrifuged at 4000 to 6000 r / min for 10 to 15 minutes, washed the obtained centrifugal product with anhydrous ethanol for 2 to 4 times, and dried under vacuum at 60 to 80°C for 20 to 24 hours to obtain the pretreated nanoclay.

6. The method for preparing an adhesive with high bonding performance according to claim 5, characterized in that: The mixed liquid is prepared by mixing anhydrous ethanol and deionized water in a mass ratio of 0.12 to 0.22:

1.

7. The method for preparing an adhesive with high bonding performance according to claim 1, characterized in that: The surfactant is selected from any one of sodium lignin sulfonate and sodium dodecylbenzene sulfonate.

8. The method for preparing an adhesive with high bonding performance according to claim 1, characterized in that: The curing agent is selected from any one of phthalic anhydride and maleic anhydride.

9. The method for preparing an adhesive with high bonding performance according to claim 1, characterized in that: In the step three, the heating temperature is 45-65°C.

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