Preparation method of high-temperature-resistant water-based environment-friendly adhesive
By using modified polyurethane prepolymer and specific preparation methods, high-temperature-resistant water-based environmentally friendly glue is prepared, which solves the problem of the existing water-based glue reducing viscosity in a high-temperature environment, and achieves both high viscosity and environmental protection.
Patent Information
- Application Number
- CN202411797778.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-09
- Publication Date
- 2025-02-14
- Estimated Expiration
- 2044-12-09
AI Technical Summary
The viscosity of existing aqueous glues decreases in long-term exposure to the sun or high temperature environment, and the high temperature resistance of solvent-based glues is high and their volatile VOCs are difficult to take into account both environmental protection and high temperature stability.
Using modified polyurethane prepolymers, modified acrylic resins, polyvinylidene chloride, coupling agents, polyvinyl alcohol, heat-resistant monomers, silica powders and alumina powders, etc., through specific stirring and ultrasonic treatment methods , prepare high-temperature resistant water-based environmentally friendly glue.
The prepared water-based environmentally friendly glue not only has high viscosity, but also maintains a stable viscosity under long-term exposure to the sun or high temperature environment. Compared with solvent-based glue, it has fewer volatile harmful gases and is suitable for high-temperature environments such as solar photovoltaic modules and automotive headlight modules. .
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Figure BDA0005177227430000101
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of water-based adhesive preparation, and in particular to a method for preparing a high-temperature resistant water-based environmentally friendly adhesive. Background Art
[0002] Water-based adhesives, as the name implies, refer to adhesives with water as the main solvent. They usually contain natural or synthetic polymers and use water as a solvent or dispersant. Compared with traditional organic solvent adhesives, this type of adhesive has the advantages of being environmentally friendly, safe, easy to operate and highly efficient, and has therefore been widely used in many fields.
[0003] Water-based adhesives can be classified according to different standards. According to the source of the material, they can be divided into natural water-based adhesives and synthetic water-based adhesives. Natural water-based adhesives are mainly composed of natural substances such as plant collagen, natural gum and sodium alginate, while synthetic water-based adhesives are obtained through chemical synthesis, and the main components include polyester, polyurethane and synthetic collagen.
[0004] The viscosity of existing water-based glue decreases after long-term exposure to sunlight or high temperature environment. The high temperature resistance of solvent-based glue is higher than that of water-based glue, but its volatile VOCs are high. Therefore, a high temperature resistant and environmentally friendly water-based glue is needed. Summary of the invention
[0005] In order to solve the above technical problems, the present invention provides a method for preparing a high temperature resistant water-based environmentally friendly adhesive.
[0006] The technical solution of the present invention is: a method for preparing a high temperature resistant water-based environmentally friendly adhesive, comprising the following steps:
[0007] S1-1. Prepare the following ingredients in percentage by mass: 13-15% modified polyurethane prepolymer, 7.5-9.6% modified acrylic resin, 5-7% polyvinylidene chloride, 4-5% coupling agent, 3-5% polyvinyl alcohol, 7-12% heat-resistant monomer, 3-4% silicon dioxide powder, 1-3% aluminum oxide powder, and the balance is deionized water;
[0008] S1-2, adding the above deionized water to a reactor, and heating to 70-80°C to maintain a constant temperature, then adding modified polyurethane prepolymer, modified acrylic resin, and polyvinylidene chloride to the reactor and mixing and stirring; stirring speed 120r / min, stirring time 4-6h, stirring accompanied by ultrasonic treatment, after stirring is completed, adding heat-resistant monomer and polyvinyl alcohol according to the weight parts and continuing stirring for 2-4h to obtain a colloidal solution;
[0009] S1-3. Continue to add coupling agent, silica powder and alumina powder to the reaction kettle containing the colloidal solution, heat to 80-90°C, continue stirring for 2-3 hours, then cool to room temperature, perform vacuum degassing treatment, and then fill to obtain water-based environmentally friendly glue.
[0010] Furthermore, the heat-resistant monomer is vinyl pyrrolidone and / or methyl methacrylate.
[0011] Furthermore, the coupling agent is prepared by mixing 3-aminopropyltriethoxysilane and γ-glycidyloxypropyltrimethoxysilane in a mass ratio of 1:1.
[0012] Furthermore, the method for preparing the modified polyurethane prepolymer in step S1-1 comprises the following steps:
[0013] S2-1, adding polyester polyol dropwise to a reaction kettle containing isocyanate, stirring under nitrogen atmosphere protection, stirring at a speed of 80-100 r / min, a reaction temperature of 70-90° C., and a reaction time of 5-8 h to obtain a polyurethane prepolymer; the molar ratio of the polyester polyol to the isocyanate is 2:1;
[0014] S2-2, lowering the temperature of the reactor to 40-50°C, and then continuing to add the modifier to the reactor, the amount of the modifier added is 20-25% of the total mass of the polyurethane prepolymer, keeping the stirring speed unchanged, and continuing stirring for 4-6 hours. After the stirring is completed, add the chain extender to the reactor for chain extension reaction. The chain extender is diethylenetriamine, and the amount of the chain extender added is 10-15% of the total mass of the polyurethane prepolymer. Keep the stirring speed unchanged, and continue stirring for 2-5 hours to obtain a modified polyurethane prepolymer.
[0015] Furthermore, the preparation method of the modifier is: γ-aminopropyltriethoxysilane and nano-SiO2 are mixed and put into a reactor, the amount of γ-aminopropyltriethoxysilane is 1-5wt% of the nano-SiO2, the temperature of the reactor is 80-95°C, the reaction time is 5-8h, the product obtained after the reaction is washed to remove unreacted γ-aminopropyltriethoxysilane, and then vacuum dried to obtain the modifier.
[0016] Furthermore, the preparation method of the modified acrylic resin comprises the following steps:
[0017] S3-1, adding acrylate monomer, crosslinking agent and initiator into a reactor in a mass ratio of 87:5:3, using argon as a protective gas, to carry out polymerization reaction, the reactor pressure is 5-10Pa relative to the atmospheric pressure, the reactor temperature is 60-70°C, the reaction time is 5-10h, the stirring speed is 80-100r / min, and after the reaction is completed, an acrylic acid polymer is obtained;
[0018] S3-2. Heat the reactor to 80-90°C, then add a modifier and an emulsifier to the reactor, wherein the amount of the modifier added accounts for 5-10% of the total mass of the acrylic polymer, and the amount of the emulsifier added accounts for 3-7% of the total mass of the acrylic polymer. Continue stirring for 4-5 hours, evacuate the reactor to 7-15Pa, and maintain for 2-3 hours to obtain a modified acrylic resin.
[0019] Furthermore, the emulsifier is allyloxy nonylphenol polyoxyethylene ether diphosphoric acid, the crosslinking agent is glycerol acrylate, the initiator is azobisisobutyronitrile, and the modifier is epoxy resin.
[0020] The beneficial effects of the present invention are:
[0021] The water-based environmentally friendly glue prepared by the present invention not only has high viscosity, but also has good high temperature resistance. It can maintain stable viscosity under long-term exposure or high temperature environment. Compared with solvent-based glue, the water-based environmentally friendly glue of the present invention has less volatile harmful gases and can be used in high temperature environments such as solar photovoltaic components and automobile headlight components. DETAILED DESCRIPTION
[0022] Embodiment 1:
[0023] A method for preparing a high temperature resistant water-based environmentally friendly adhesive comprises the following steps:
[0024] S1-1. Prepare the following ingredients in percentage by mass: 13% modified polyurethane prepolymer, 7.5% modified acrylic resin, 5% polyvinylidene chloride, 4% coupling agent, 3% polyvinyl alcohol, 7% heat-resistant monomer, 3% silica powder, 1% alumina powder, and the balance is deionized water; the average particle size of silica powder and alumina powder is 10 μm; the heat-resistant monomer is vinyl pyrrolidone; the coupling agent is prepared by mixing 3-aminopropyltriethoxysilane and γ-glycidyloxypropyltrimethoxysilane in a mass ratio of 1:1;
[0025] S1-2, add the above deionized water to the reactor, heat it to 70°C and keep the constant temperature, then add the modified polyurethane prepolymer, modified acrylic resin and polyvinylidene chloride to the reactor and mix and stir; the stirring speed is 120r / min, the stirring time is 4h, and ultrasonic treatment is carried out while stirring, the ultrasonic frequency of the ultrasonic treatment is 20Hz, and the ultrasonic wavelength is 0.06mm; after the stirring is completed, add the heat-resistant monomer and polyvinyl alcohol according to the weight and continue stirring for 2h to obtain a colloidal solution;
[0026] S1-3. Continue to add coupling agent, silica powder and alumina powder to the reactor containing the colloidal solution, heat to 80°C, continue stirring for 2 hours, and then cool to room temperature 28°C and perform vacuum degassing. The vacuum degassing treatment is to evacuate the reactor to 4Pa and maintain it for 2 hours; then fill it to obtain a water-based environmentally friendly glue.
[0027] The method for preparing the modified polyurethane prepolymer in step S1-1 comprises the following steps:
[0028] S2-1, adding polyester polyol dropwise to a reaction kettle containing isocyanate, stirring under a nitrogen atmosphere, the stirring speed is 80 r / min, the reaction temperature is 70° C., the reaction time is 5 h, to obtain a polyurethane prepolymer; the molar ratio of polyester polyol to isocyanate is 2:1;
[0029] S2-2. Lower the temperature of the reactor to 40°C, and then continue to add the modifier to the reactor. The amount of the modifier added is 20% of the total mass of the polyurethane prepolymer. Keep the stirring speed unchanged and continue stirring for 4 hours. After the stirring is completed, add the chain extender to the reactor for chain extension reaction. The chain extender is diethylenetriamine. The amount of the chain extender added is 10% of the total mass of the polyurethane prepolymer. Keep the stirring speed unchanged and continue stirring for 2 hours to obtain a modified polyurethane prepolymer.
[0030] The preparation method of the modifier is as follows: γ-aminopropyltriethoxysilane is mixed with nano-SiO2 and put into a reactor, the amount of γ-aminopropyltriethoxysilane is 1wt% of the nano-SiO2, the reactor temperature is 80°C, the reaction time is 5h, the product obtained after the reaction is cleaned to remove unreacted γ-aminopropyltriethoxysilane, and then vacuum dried to obtain the modifier.
[0031] The preparation method of modified acrylic resin comprises the following steps:
[0032] S3-1, adding acrylate monomer, crosslinking agent and initiator into a reactor in a mass ratio of 87:5:3, using argon as a protective gas, to carry out polymerization reaction, the reactor pressure is 5Pa relative to the atmospheric pressure, the reactor temperature is 60°C, the reaction time is 5h, the stirring speed is 80r / min, and after the reaction is completed, an acrylic acid polymer is obtained;
[0033] S3-2. Heat the reactor to 80°C, then add a modifier and an emulsifier to the reactor, wherein the amount of the modifier added accounts for 5% of the total mass of the acrylic polymer, and the amount of the emulsifier added accounts for 3% of the total mass of the acrylic polymer. Continue stirring for 4 hours, evacuate the reactor to 7Pa, and maintain for 2 hours to obtain a modified acrylic resin.
[0034] The emulsifier is allyloxy nonylphenol polyoxyethylene ether diphosphoric acid, the crosslinking agent is glycerol acrylate, the initiator is azobisisobutyronitrile, and the modifier is epoxy resin.
[0035] Embodiment 2:
[0036] A method for preparing a high temperature resistant water-based environmentally friendly adhesive comprises the following steps:
[0037] S1-1. Prepare the following ingredients in percentage by mass: 13.5% modified polyurethane prepolymer, 8.6% modified acrylic resin, 5.5% polyvinylidene chloride, 4.5% coupling agent, 3.5% polyvinyl alcohol, 7.5% heat-resistant monomer, 3.2% silica powder, 1.5% alumina powder, and the balance is deionized water; the average particle size of silica powder and alumina powder is 13 μm; the heat-resistant monomer is methyl methacrylate; the coupling agent is prepared by mixing 3-aminopropyltriethoxysilane and γ-glycidyloxypropyltrimethoxysilane in a mass ratio of 1:1;
[0038] S1-2, add the above deionized water to the reactor, heat it to 77°C and keep the constant temperature, then add the modified polyurethane prepolymer, modified acrylic resin and polyvinylidene chloride to the reactor and mix and stir; the stirring speed is 120r / min, the stirring time is 5.5h, and ultrasonic treatment is carried out while stirring, the ultrasonic frequency of the ultrasonic treatment is 35Hz, and the ultrasonic wavelength is 0.3mm; after the stirring is completed, add the heat-resistant monomer and polyvinyl alcohol according to weight and continue stirring for 2.5h to obtain a colloidal solution;
[0039] S1-3. Continue to add coupling agent, silica powder and alumina powder to the reactor containing the colloidal solution, heat to 88°C, continue stirring for 2.5 hours, and then cool to room temperature 24°C and perform vacuum degassing. The vacuum degassing treatment is to evacuate the reactor to 5Pa and maintain it for 2.5 hours; then fill it to obtain a water-based environmentally friendly glue.
[0040] The method for preparing the modified polyurethane prepolymer in step S1-1 comprises the following steps:
[0041] S2-1, adding polyester polyol dropwise to a reaction kettle containing isocyanate, stirring under a nitrogen atmosphere, the stirring speed is 88 r / min, the reaction temperature is 75° C., the reaction time is 5.5 h, to obtain a polyurethane prepolymer; the molar ratio of polyester polyol to isocyanate is 2:1;
[0042] S2-2. Lower the temperature of the reactor to 45°C, and then continue to add the modifier to the reactor. The amount of the modifier added is 23% of the total mass of the polyurethane prepolymer. Keep the stirring speed unchanged and continue stirring for 4.5 hours. After the stirring is completed, add the chain extender to the reactor for chain extension reaction. The chain extender is diethylenetriamine. The amount of the chain extender added is 13% of the total mass of the polyurethane prepolymer. Keep the stirring speed unchanged and continue stirring for 3 hours to obtain a modified polyurethane prepolymer.
[0043] The preparation method of the modifier is as follows: γ-aminopropyltriethoxysilane is mixed with nano-SiO2 and put into a reactor, the amount of γ-aminopropyltriethoxysilane is 3wt% of nano-SiO2, the temperature of the reactor is 90°C, the reaction time is 6h, the product obtained after the reaction is washed to remove unreacted γ-aminopropyltriethoxysilane, and then vacuum dried to obtain the modifier.
[0044] The preparation method of modified acrylic resin comprises the following steps:
[0045] S3-1, adding acrylate monomer, crosslinking agent and initiator into a reactor in a mass ratio of 87:5:3, using argon as a protective gas, to carry out polymerization reaction, the reactor pressure is 6Pa relative to the atmospheric pressure, the reactor temperature is 65°C, the reaction time is 7h, the stirring speed is 90r / min, and after the reaction is completed, an acrylic acid polymer is obtained;
[0046] S3-2. Heat the reactor to 88°C, then add a modifier and an emulsifier to the reactor, wherein the amount of the modifier added accounts for 6% of the total mass of the acrylic polymer, and the amount of the emulsifier added accounts for 4% of the total mass of the acrylic polymer. Continue stirring for 4.5 hours, evacuate the reactor to 10Pa, and maintain for 1.5 hours to obtain a modified acrylic resin.
[0047] The emulsifier is allyloxy nonylphenol polyoxyethylene ether diphosphoric acid, the crosslinking agent is glycerol acrylate, the initiator is azobisisobutyronitrile, and the modifier is epoxy resin.
[0048] Embodiment 3:
[0049] A method for preparing a high temperature resistant water-based environmentally friendly adhesive comprises the following steps:
[0050] S1-1. Prepare the following ingredients in percentage by mass: 15% modified polyurethane prepolymer, 9.6% modified acrylic resin, 7% polyvinylidene chloride, 5% coupling agent, 5% polyvinyl alcohol, 12% heat-resistant monomer, 4% silica powder, 3% alumina powder, and the balance is deionized water; the average particle size of silica powder and alumina powder is 20 μm; the heat-resistant monomer is prepared by mixing vinyl pyrrolidone and methyl methacrylate in a mass ratio of 1:1; the coupling agent is prepared by mixing 3-aminopropyl triethoxysilane and γ-glycidyloxypropyl trimethoxysilane in a mass ratio of 1:1;
[0051] S1-2, add the above deionized water to the reactor, heat it to 80°C and keep the constant temperature, then add the modified polyurethane prepolymer, modified acrylic resin and polyvinylidene chloride to the reactor and mix and stir; the stirring speed is 120r / min, the stirring time is 6h, and ultrasonic treatment is carried out while stirring, the ultrasonic frequency of the ultrasonic treatment is 40Hz, and the ultrasonic wavelength is 0.5mm; after the stirring is completed, add the heat-resistant monomer and polyvinyl alcohol according to the weight and continue stirring for 4h to obtain a colloidal solution;
[0052] S1-3. Continue to add coupling agent, silica powder and alumina powder to the reactor containing the colloidal solution, heat to 90°C, continue stirring for 3 hours, and then cool to room temperature 30°C and perform vacuum degassing. The vacuum degassing treatment is to evacuate the reactor to 8Pa and maintain it for 3 hours; then fill it to obtain a water-based environmentally friendly glue.
[0053] The method for preparing the modified polyurethane prepolymer in step S1-1 comprises the following steps:
[0054] S2-1, adding polyester polyol dropwise to a reaction kettle containing isocyanate, stirring under a nitrogen atmosphere, the stirring speed is 100 r / min, the reaction temperature is 90° C., the reaction time is 8 h, to obtain a polyurethane prepolymer; the molar ratio of polyester polyol to isocyanate is 2:1;
[0055] S2-2. Lower the temperature of the reactor to 50°C, and then continue to add the modifier to the reactor. The amount of the modifier added is 25% of the total mass of the polyurethane prepolymer. Keep the stirring speed unchanged and continue stirring for 6 hours. After the stirring is completed, add the chain extender to the reactor for chain extension reaction. The chain extender is diethylenetriamine. The amount of the chain extender added is 15% of the total mass of the polyurethane prepolymer. Keep the stirring speed unchanged and continue stirring for 5 hours to obtain a modified polyurethane prepolymer.
[0056] The preparation method of the modifier is as follows: γ-aminopropyltriethoxysilane is mixed with nano-SiO2 and put into a reactor, the amount of γ-aminopropyltriethoxysilane is 5wt% of the nano-SiO2, the temperature of the reactor is 95°C, the reaction time is 8h, the product obtained after the reaction is washed to remove the unreacted γ-aminopropyltriethoxysilane, and then vacuum dried to obtain the modifier.
[0057] The preparation method of modified acrylic resin comprises the following steps:
[0058] S3-1, adding acrylate monomer, crosslinking agent and initiator into a reactor in a mass ratio of 87:5:3, using argon as a protective gas, to carry out polymerization reaction, the reactor pressure is 10Pa relative to the atmospheric pressure, the reactor temperature is 70°C, the reaction time is 10h, the stirring speed is 100r / min, and after the reaction is completed, an acrylic acid polymer is obtained;
[0059] S3-2. Heat the reactor to 90°C, then add a modifier and an emulsifier into the reactor, wherein the amount of the modifier added accounts for 10% of the total mass of the acrylic polymer, and the amount of the emulsifier added accounts for 7% of the total mass of the acrylic polymer. Continue stirring for 5 hours, evacuate the reactor to 15 Pa, and maintain for 3 hours to obtain a modified acrylic resin.
[0060] The emulsifier is allyloxy nonylphenol polyoxyethylene ether diphosphoric acid, the crosslinking agent is glycerol acrylate, the initiator is azobisisobutyronitrile, and the modifier is epoxy resin.
[0061] Comparing Examples 1 to 3, Example 3 has the highest viscosity and the best high temperature resistance, so Example 3 is the best example;
[0062] Embodiment 4:
[0063] Based on Example 3, Example 4 is different from Example 3 in that S1-1, materials are prepared according to the following mass percentages: 15% modified polyurethane prepolymer, 9.6% modified acrylic resin, 7% polyvinylidene chloride, 5% coupling agent, 5% polyvinyl alcohol, 10% heat-resistant monomer, 4% silicon dioxide powder, 3% aluminum oxide powder, and the balance is deionized water;
[0064] Comparing Example 3 with Example 4, in Example 4, since the content of the heat-resistant monomer is reduced, the high temperature resistance of the prepared water-based environmentally friendly adhesive is reduced.
[0065] Embodiment 5:
[0066] Based on Example 3, Example 5 is different from Example 3 in that the vacuum degassing treatment in Example 5 is to evacuate the reactor to 4 Pa and maintain it for 3 hours.
[0067] Comparing Examples 3 to 5, the water-based environmentally friendly adhesive prepared in Example 5 has the least internal bubble content, so Example 5 has a better effect.
[0068] Embodiment 6:
[0069] On the basis of Example 5, Example 6 differs from Example 5 in that, S2-2, the temperature of the reactor is lowered to 50°C, and then the modifier is continuously added to the reactor, the amount of the modifier added is 23% of the total mass of the polyurethane prepolymer, the stirring speed is kept unchanged, and stirring is continued for 6 hours. After the stirring is completed, a chain extender is added to the reactor for a chain extension reaction, the chain extender is diethylenetriamine, and the amount of the chain extender added is 15% of the total mass of the polyurethane prepolymer, the stirring speed is kept unchanged, and stirring is continued for 5 hours to obtain a modified polyurethane prepolymer.
[0070] Comparing Example 5 and Example 6, the amount of the modifier added was reduced when preparing the modified polyurethane prepolymer in Example 6, and the heat resistance and viscosity of the water-based environmentally friendly adhesive prepared in Example 6 were reduced.
[0071] Embodiment 7:
[0072] On the basis of Example 5, Example 7 differs from Example 5 in that, S2-2, the temperature of the reactor is lowered to 50°C, and then the modifier is continuously added to the reactor, the amount of the modifier added is 25% of the total mass of the polyurethane prepolymer, the stirring speed is kept unchanged, and stirring is continued for 6 hours. After the stirring is completed, a chain extender is added to the reactor for a chain extension reaction, and the amount of the chain extender added is 13% of the total mass of the polyurethane prepolymer. The stirring speed is kept unchanged, and stirring is continued for 5 hours to obtain a modified polyurethane prepolymer.
[0073] Comparing Example 5 and Example 7, Example 7 reduced the amount of chain extender added when preparing the modified polyurethane prepolymer. Comparing the water-based environmentally friendly adhesives prepared in Example 5 and Example 7, it was found that Example 5 had better viscosity.
[0074] Embodiment 8:
[0075] Based on Example 5, the difference between Example 8 and Example 13 is that, S3-2, the reactor is heated to 90°C, and then a modifier and an emulsifier are added to the reactor, the amount of the modifier added accounts for 8% of the total mass of the acrylic polymer, and the amount of the emulsifier added accounts for 7% of the total mass of the acrylic polymer. Stirring is continued for 5 hours, and the reactor is evacuated to 15 Pa. After maintaining for 3 hours, a modified acrylic resin is obtained.
[0076] Comparing Example 5 with Example 8, the amount of modifier added was reduced in the modified acrylic resin prepared by Example 8. Comparing the water-based environmentally friendly adhesive prepared by Example 5 with that prepared by Example 8, the viscosity of the water-based environmentally friendly adhesive prepared by Example 8 was reduced.
[0077] Embodiment 9:
[0078] Based on Example 5, Example 9 differs from Example 5 in that, S3-2, the reactor is heated to 90° C., and then a modifier and an emulsifier are added to the reactor, wherein the amount of the modifier added accounts for 10% of the total mass of the acrylic polymer, and the amount of the emulsifier added accounts for 7% of the total mass of the acrylic polymer. Stirring is continued for 5 hours, and the reactor is evacuated to 7 Pa. After maintaining for 3 hours, a modified acrylic resin is obtained.
[0079] Compared with the water-based environmentally friendly adhesive prepared in Example 5 and Example 9, the water-based environmentally friendly adhesive prepared in Example 9 has the least bubble content, so Example 9 is the best example.
[0080] The viscosity and high temperature resistance of the water-based environmentally friendly adhesives prepared in Examples 1 to 9 are shown in Table 1;
[0081] Table 1: Comparison of performance of water-based environmentally friendly adhesives in Examples 1 to 9:
[0082]
[0083] By comparing the data in Table 1, the water-based environmentally friendly glue prepared in Example 9 has the best viscosity and high temperature resistance, and the smallest bubble content. Therefore, the water-based environmentally friendly glue prepared in Example 9 has the best use effect.
Claims
1. A method for preparing a high temperature resistant water-based environmentally friendly adhesive, characterized in that: The following steps are involved: S1-1. Prepare the following ingredients in percentage by mass: 13-15% modified polyurethane prepolymer, 7.5-9.6% modified acrylic resin, 5-7% polyvinylidene chloride, 4-5% coupling agent, 3-5% polyvinyl alcohol, 7-12% heat-resistant monomer, 3-4% silicon dioxide powder, 1-3% aluminum oxide powder, and the balance is deionized water; S1-2, adding the above deionized water to a reactor, and heating to 70-80°C to maintain a constant temperature, then adding modified polyurethane prepolymer, modified acrylic resin, and polyvinylidene chloride to the reactor and mixing and stirring; stirring speed 120r / min, stirring time 4-6h, stirring accompanied by ultrasonic treatment, after stirring is completed, adding heat-resistant monomer and polyvinyl alcohol according to the weight parts and continuing stirring for 2-4h to obtain a colloidal solution; S1-3. Continue to add coupling agent, silica powder and alumina powder to the reaction kettle containing the colloidal solution, heat to 80-90°C, continue stirring for 2-3 hours, then cool to room temperature, perform vacuum degassing treatment, and then fill to obtain water-based environmentally friendly glue.
2. The method for preparing a high temperature resistant water-based environmentally friendly adhesive according to claim 1, characterized in that: The heat-resistant monomer is vinyl pyrrolidone and / or methyl methacrylate.
3. The method for preparing a high temperature resistant water-based environmentally friendly adhesive according to claim 1, characterized in that: The heat-resistant monomer is vinyl pyrrolidone.
4. The method for preparing a high temperature resistant water-based environmentally friendly adhesive according to claim 1, characterized in that: The method for preparing the modified polyurethane prepolymer in step S1-1 comprises the following steps: S2-1, adding polyester polyol dropwise to a reaction kettle containing isocyanate, stirring under nitrogen atmosphere protection, stirring at a speed of 80-100 r / min, a reaction temperature of 70-90° C., and a reaction time of 5-8 h to obtain a polyurethane prepolymer; the molar ratio of the polyester polyol to the isocyanate is 2:1; S2-2, lowering the temperature of the reactor to 40-50°C, and then continuing to add the modifier to the reactor, the amount of the modifier added is 20-25% of the total mass of the polyurethane prepolymer, keeping the stirring speed unchanged, and continuing stirring for 4-6 hours. After the stirring is completed, add the chain extender to the reactor for chain extension reaction, the amount of the chain extender added is 10-15% of the total mass of the polyurethane prepolymer, keeping the stirring speed unchanged, and continuing stirring for 2-5 hours to obtain a modified polyurethane prepolymer.
5. The method for preparing a high temperature resistant water-based environmentally friendly adhesive according to claim 4, characterized in that: The preparation method of the modifier is as follows: γ-aminopropyltriethoxysilane and nano-SiO2 are mixed and put into a reaction kettle, wherein the amount of γ-aminopropyltriethoxysilane used is 1-5wt% of the nano-SiO2, the temperature of the reaction kettle is 80-95°C, the reaction time is 5-8h, the product obtained after the reaction is washed to remove the unreacted γ-aminopropyltriethoxysilane, and then vacuum dried to obtain the modifier.
6. The method for preparing a high temperature resistant water-based environmentally friendly adhesive according to claim 1, characterized in that: The preparation method of the modified acrylic resin comprises the following steps: S3-1, adding acrylate monomer, crosslinking agent and initiator into a reactor in a mass ratio of 87:5:3, using argon as a protective gas, to carry out polymerization reaction, the reactor pressure is 5-10Pa relative to the atmospheric pressure, the reactor temperature is 60-70°C, the reaction time is 5-10h, the stirring speed is 80-100r / min, and after the reaction is completed, an acrylic acid polymer is obtained; S3-2. Heat the reactor to 80-90°C, then add a modifier and an emulsifier to the reactor, wherein the amount of the modifier added accounts for 5-10% of the total mass of the acrylic polymer, and the amount of the emulsifier added accounts for 3-7% of the total mass of the acrylic polymer. Continue stirring for 4-5 hours, evacuate the reactor to 7-15Pa, and maintain for 2-3 hours to obtain a modified acrylic resin.
7. The method for preparing a high temperature resistant water-based environmentally friendly adhesive according to claim 6, characterized in that: The emulsifier is allyloxy nonylphenol polyoxyethylene ether diphosphoric acid, the crosslinking agent is glycerol acrylate, the initiator is azobisisobutyronitrile, and the modifier is epoxy resin.
Citation Information
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