New energy heating film high-temperature-resistant glue formula and preparation method thereof

Abstract

The invention relates to the technical field of high-temperature glue, in particular to a new energy heating film high-temperature-resistant glue formula and a preparation method thereof. The new energy heating film high-temperature-resistant glue formula comprises the following raw materials in percentage by weight: 60-66% of polyurethane, 8-12% of a flame retardant, 6-8% of an additive, 0.6-1.2% of a diluent and the balance of epoxy resin. The epoxy resin is pretreated before preparation. According to the high-temperature-resistant glue for the new energy heating film, by using the additive in the formula of the high-temperature-resistant glue for the new energy heating film, nanoscale boron nitride is subjected to surface modification treatment through the KH-560 silane coupling agent and then forms a three-dimensional heat conduction network with polytetrafluoroethylene, the heat conduction efficiency of the material is effectively improved, and the polytetrafluoroethylene forms a low-surface-energy layer in the mixing process; the function of reducing the molecular chain migration rate in a high-temperature state can be achieved, meanwhile, particle filling is achieved by adding zirconium dioxide, and the thermal stability of the material is further improved.

Description

Technical Field

[0001] The present invention relates to the technical field of high-temperature adhesives, and specifically to a high-temperature resistant adhesive formula for a new energy heating film and a preparation method thereof. Background Art

[0002] The high-temperature resistant adhesive for new energy heating films is an adhesive specifically designed for heating film scenarios, which can adapt to complex environments such as high temperature and high humidity, and provide an efficient bonding solution for high-temperature scenarios in the new energy field.

[0003] In the prior art, the high-temperature resistance of adhesives for new energy heating films is poor, and delamination and bubbling usually occur at about 160°C, making it difficult to meet the performance requirements for bonding various materials. Based on this, the present invention provides a high-temperature resistant adhesive formula for a new energy heating film and a preparation method thereof. Summary of the Invention

[0004] The purpose of the present invention is to provide a high-temperature resistant adhesive formula for a new energy heating film and a preparation method thereof. The high-temperature resistant adhesive for new energy heating films prepared by the present invention not only has good high-temperature resistance but also excellent peel strength performance.

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

[0006] In the first aspect, the present invention provides a high-temperature resistant adhesive formula for a new energy heating film, which comprises the following raw materials in weight percentage: 60-66% polyurethane, 8-12% flame retardant, 6-8% additive, 0.6-1.2% diluent, and the balance is epoxy resin;

[0007] The epoxy resin is pretreated before preparation;

[0008] The additive is prepared by the following steps:

[0009] S1: Preparation of the base material;

[0010] S2: Treatment of the base material to obtain the additive.

[0011] Further, the pretreatment method of the epoxy resin is as follows: The epoxy resin is added to a reaction kettle, the temperature of the reaction kettle is set to 50-60°C, and it is kept at a constant temperature and static for 10-20 min. Then, a mixture is added to the reaction kettle, the temperature of the reaction kettle is set to rise to 80-120°C, the stirring speed is 200-300 r / min, and it is stirred at a constant temperature for 1-3 h. Then, the temperature of the reaction kettle is set to rise to 140-150°C, and it reacts at a constant temperature for 2-4 h. After the constant temperature reaction is completed, it is cooled to room temperature, and the obtained product is left standing for 4-6 h to complete the pretreatment of the epoxy resin.

[0012] Further, the mixture is prepared by the following method: Polyimide, biphenyl-type epoxy resin, and polybenzimidazole are added into a reaction kettle. The temperature of the reaction kettle is set to 40 - 50 °C, the stirring speed is 300 - 400 r / min, and it is stirred at a constant temperature for 20 - 30 min. Then, silica and KH-550 are added into the reaction kettle. After cooling to room temperature, the stirring speed is set to 400 - 500 r / min, and it is stirred for 20 - 30 min to obtain the mixture.

[0013] Further, the mass ratio of polyimide, biphenyl-type epoxy resin, and polybenzimidazole is 1:(0.1 - 0.3):(0.6 - 0.8). The mass of silica is 10 - 20% of the mass of polyimide, and the mass of KH-550 is 6 - 10% of the mass of polyimide. The silica is selected as powder with a particle size of 10 - 40 nm.

[0014] Further, the method for preparing the base material is as follows: Boron nitride is sent into an oven, and the oven is set to 80 - 100 °C for drying treatment for 2 - 4 h. Then, the dried boron nitride is added into a mixer, and KH-560 is added into the mixer. The mixer is set to stir at 400 - 500 r / min for 30 - 40 min. After the stirring treatment is completed, polytetrafluoroethylene, zirconia, and polyether-modified silicone oil are added into the mixer. The mixer is set to stir at 200 - 300 r / min for 50 - 60 min to obtain the base material.

[0015] Further, the mass of KH-560 is 4 - 6% of the mass of boron nitride, the mass of polytetrafluoroethylene is 6 - 8% of the mass of boron nitride, the mass of zirconia is 10 - 12% of the mass of boron nitride, and the mass of polyether-modified silicone oil is 1 - 3% of the mass of boron nitride. The boron nitride, polytetrafluoroethylene, and zirconia are all selected as powders. The particle size of boron nitride is 10 - 40 nm, and the particle sizes of polytetrafluoroethylene and zirconia are 20 - 60 nm.

[0016] Further, the method for treating the base material is as follows: The base material and the powder are added into a mixer, and the mixer is set to stir at 600 - 800 r / min for 10 - 20 min to complete the treatment of the base material and obtain the additive.

[0017] Further, the powder material is prepared by the following method: Montmorillonite and deionized water are added into a water bath pot, and the water bath pot is set to heat up to 50-60 °C. Meanwhile, a magnetic stirrer is connected, and the magnetic stirrer is set at 200-300 r / min for constant-temperature stirring treatment for 6-12 min. Then, cetyltrimethylammonium bromide and multi-walled carbon nanotubes are added, the temperature is set to 70-80 °C, and the magnetic stirrer is set at 400-500 r / min for constant-temperature stirring treatment for 2-4 h. After the constant-temperature stirring treatment is completed, wait for it to cool to room temperature, and the obtained product is centrifuged to obtain a precipitate. The precipitate is sent into an oven, and the oven is set at 50-60 °C for drying treatment for 2-4 h to prepare the powder material. Among them, the mass ratio of montmorillonite to deionized water is 1:(2-4), the mass of cetyltrimethylammonium bromide is 1-3% of the mass of montmorillonite, and the mass of multi-walled carbon nanotubes is 2-4% of the mass of montmorillonite.

[0018] Further, the diluent is prepared by mixing neopentyl glycol diglycidyl ether and phenyl glycidyl ether, and the mass ratio of neopentyl glycol diglycidyl ether to phenyl glycidyl ether is 1:(0.4-0.6). The flame retardant is selected as cage-type polyhedral oligomeric silsesquioxane.

[0019] In the second aspect, the present invention also provides a preparation method of a high-temperature resistant glue formula for a new energy heating film, including the following steps: Weigh polyurethane, flame retardant, additive, diluent and pretreated epoxy resin as required and add them into a reaction kettle, and carry out stirring treatment at 20-26 °C. The stirring speed is 300-500 r / min, and the treatment time is 40-60 min. After the stirring treatment is completed, let it stand for 6-10 h to prepare the high-temperature resistant glue for the new energy heating film.

[0020] Compared with the prior art, the beneficial effects of the present invention are:

[0021] 1. In the present invention, through the use of additives in the high-temperature resistant glue formula for the new energy heating film, after the nano-level boron nitride is surface-modified by KH-560 silane coupling agent, a three-dimensional heat conduction network is formed with polytetrafluoroethylene, effectively improving the heat conduction efficiency of the material. Polytetrafluoroethylene forms a low surface energy layer during the mixing process, which can play a role in reducing the molecular chain migration rate at high temperature. At the same time, the addition of zirconia realizes particle filling, further improving the thermal stability of the material.

[0022] 2. In the present invention, a gradient interface layer is formed by combining polyether-modified silicone oil with KH-560, effectively improving the wettability of the material. By pre-treating the epoxy resin, the internal stress generated during the storage of the epoxy resin can be eliminated, enabling the molecular chains to be initially stretched. After high-temperature treatment, the pre-polymerization reaction between the polyimide and the biphenyl-type epoxy resin can be promoted to form a branched structure. Montmorillonite and multi-walled carbon nanotubes can combine and lock with each other, enhancing the interfacial bonding force, and thus effectively improving the peel strength performance of the material. Detailed Embodiments

[0023] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

[0024] Among them, it should be noted that the raw materials used in the following embodiments are all commercially available raw materials.

[0025] Embodiment 1: It includes the following raw material components by weight percentage: 60% polyurethane, 8% flame retardant, 6% additive, 0.6% diluent, and the balance is epoxy resin;

[0026] The epoxy resin is pre-treated before preparation;

[0027] The additive is prepared by the following steps:

[0028] S1: Preparation of the base material;

[0029] S2: Treatment of the base material to obtain the additive.

[0030] The pre-treatment method of the epoxy resin is as follows: The epoxy resin is added to a reaction kettle, the temperature of the reaction kettle is set at 50°C, and it is kept at a constant temperature and left standing for 10 minutes. Then, a mixture is added to the reaction kettle, the temperature of the reaction kettle is set to rise to 80°C, the stirring speed is 200 r / min, and it is stirred at a constant temperature for 1 hour. Then, the temperature of the reaction kettle is set to rise to 140°C, and it is reacted at a constant temperature for 2 hours. After the constant-temperature reaction is completed, it is cooled to room temperature, and the obtained product is left standing for 4 hours to complete the pre-treatment of the epoxy resin.

[0031] The mixture is prepared by the following method: Polyimide, biphenyl-type epoxy resin, and polybenzimidazole are added to a reaction kettle, the temperature of the reaction kettle is set at 40°C, the stirring speed is 300 r / min, and it is stirred at a constant temperature for 20 minutes. Then, silicon dioxide and KH-550 are added to the reaction kettle. After cooling to room temperature, the stirring speed is set to 400 r / min, and it is stirred for 20 minutes to obtain the mixture.

[0032] The mass ratio of polyimide, biphenyl-type epoxy resin and polybenzimidazole is 1:0.1:0.6. The mass of silica is 10% of the mass of polyimide. The mass of KH-550 is 6% of the mass of polyimide. The silica selected is in powder form with a particle size of 10 nm.

[0033] The method for preparing the base material is as follows: Boron nitride is sent into an oven, the oven is set at 80 °C, and dried for 2 h. Then the dried boron nitride is added into a mixer, KH-560 is added into the mixer, the mixer is set to stir at 400 r / min for 30 min. After the stirring treatment is completed, polytetrafluoroethylene, zirconia and polyether-modified silicone oil are added into the mixer, and the mixer is set to stir at 200 r / min for 50 min to obtain the base material.

[0034] The mass of KH-560 is 4% of the mass of boron nitride. The mass of polytetrafluoroethylene is 6% of the mass of boron nitride. The mass of zirconia is 10% of the mass of boron nitride. The mass of polyether-modified silicone oil is 1% of the mass of boron nitride. Boron nitride, polytetrafluoroethylene and zirconia are all selected as powders. The particle size of boron nitride is 10 nm, and the particle sizes of polytetrafluoroethylene and zirconia are 20 nm.

[0035] The method for treating the base material is as follows: The base material and powder are added into a mixer, and the mixer is set to stir at 600 r / min for 10 min to complete the treatment of the base material and obtain the additive.

[0036] The powder is prepared by the following method: Montmorillonite and deionized water are added into a water bath pot. The water bath pot is set to heat up to 50 °C, and at the same time, a magnetic stirrer is connected. The magnetic stirrer is set to 200 r / min for constant-temperature stirring for 6 min. Then cetyltrimethylammonium bromide and multi-walled carbon nanotubes are added, the temperature is set to 70 °C, and the magnetic stirrer is set to 400 r / min for constant-temperature stirring for 2 h. After the constant-temperature stirring treatment is completed, after cooling to room temperature, the obtained product is centrifuged to obtain a precipitate. The precipitate is sent into an oven, and the oven is set at 50 °C for drying treatment for 2 h to obtain the powder. Among them, the mass ratio of montmorillonite to deionized water is 1:2, the mass of cetyltrimethylammonium bromide is 1% of the mass of montmorillonite, and the mass of multi-walled carbon nanotubes is 2% of the mass of montmorillonite.

[0037] The diluent is prepared by mixing neopentyl glycol diglycidyl ether and phenyl glycidyl ether. The mass ratio of neopentyl glycol diglycidyl ether to phenyl glycidyl ether is 1:0.4. The flame retardant selected is cage-type polyhedral oligomeric silsesquioxane.

[0038] A preparation method of a high-temperature resistant glue formula for a new energy heating film includes the following steps: Weigh polyurethane, a flame retardant, an additive, a diluent, and pretreated epoxy resin as required and add them to a reaction kettle. Stir at 20°C with a stirring speed of 300 r / min for 40 min. After the stirring treatment, let it stand for 6 h to obtain the high-temperature resistant glue for the new energy heating film.

[0039] Example two: It includes the following raw material components by weight percentage: 63% polyurethane, 10% flame retardant, 7% additive, 1% diluent, and the balance is epoxy resin;

[0040] Pre-treat the epoxy resin before preparation;

[0041] The additive is prepared by the following steps:

[0042] S1: Preparation of the base material;

[0043] S2: Treatment of the base material to obtain the additive.

[0044] The pre-treatment method of the epoxy resin is as follows: Add the epoxy resin to a reaction kettle, set the temperature of the reaction kettle to 55°C, keep it at a constant temperature and let it stand for 15 min. Then add a mixture to the reaction kettle, set the temperature of the reaction kettle to rise to 100°C, with a stirring speed of 250 r / min, and keep stirring at a constant temperature for 2 h. Then set the temperature of the reaction kettle to rise to 145°C and carry out a constant temperature reaction for 3 h. After the constant temperature reaction ends, wait for it to cool to room temperature, and let the obtained product stand for 5 h to complete the pre-treatment of the epoxy resin.

[0045] The mixture is prepared by the following method: Add polyimide, biphenyl-type epoxy resin, and polybenzimidazole to a reaction kettle, set the temperature of the reaction kettle to 45°C, with a stirring speed of 350 r / min, and keep stirring at a constant temperature for 25 min. Then add silicon dioxide and KH-550 to the reaction kettle. After cooling to room temperature, set the stirring speed to 450 r / min and stir for 25 min to obtain the mixture.

[0046] The mass ratio of polyimide, biphenyl-type epoxy resin, and polybenzimidazole is 1:0.2:0.7. The mass of silicon dioxide is 15% of the mass of polyimide, and the mass of KH-550 is 8% of the mass of polyimide. The silicon dioxide is selected as powder with a particle size of 20 nm.

[0047] The method for preparing the base material is as follows: Send boron nitride into an oven, set the oven temperature to 90°C, and carry out a drying treatment for 3 h. Then add the dried boron nitride to a mixer, add KH-560 to the mixer, set the mixer to stir at 450 r / min for 35 min. After the stirring treatment is completed, add polytetrafluoroethylene, zirconia, and polyether-modified silicone oil to the mixer, and set the mixer to stir at 250 r / min for 55 min to obtain the base material.

[0048] The mass of KH-560 is 5% of the mass of boron nitride, the mass of polytetrafluoroethylene is 7% of the mass of boron nitride, the mass of zirconia is 11% of the mass of boron nitride, the mass of polyether-modified silicone oil is 2% of the mass of boron nitride. Boron nitride, polytetrafluoroethylene and zirconia are all selected as powders. The particle size of boron nitride is 20 nm, and the particle sizes of polytetrafluoroethylene and zirconia are 40 nm.

[0049] The method for treating the base material is as follows: The base material and the powder are added into a mixer, and the mixer is set to stir at 700 r / min for 15 min to complete the treatment of the base material and obtain the additive.

[0050] The powder is prepared by the following method: Montmorillonite and deionized water are added into a water bath kettle, and the water bath kettle is set to heat up to 55 °C. At the same time, a magnetic stirrer is connected, and the magnetic stirrer is set to 250 r / min for constant-temperature stirring treatment for 9 min. Then cetyltrimethylammonium bromide and multi-walled carbon nanotubes are added, the temperature is set to 75 °C, and the magnetic stirrer is set to 450 r / min for constant-temperature stirring treatment for 3 h. After the constant-temperature stirring treatment is completed, wait for it to cool to room temperature, and the obtained product is centrifuged to obtain a precipitate. The precipitate is sent into an oven, and the oven is set to 55 °C for drying treatment for 3 h to obtain the powder. Among them, the mass ratio of montmorillonite to deionized water is 1:3, the mass of cetyltrimethylammonium bromide is 2% of the mass of montmorillonite, and the mass of multi-walled carbon nanotubes is 3% of the mass of montmorillonite.

[0051] The diluent is prepared by mixing neopentyl glycol diglycidyl ether and phenyl glycidyl ether, and the mass ratio of neopentyl glycol diglycidyl ether to phenyl glycidyl ether is 1:0.5. The flame retardant is selected as cage-type polyhedral oligomeric silsesquioxane.

[0052] A preparation method of a high-temperature resistant glue formula for a new energy heating film includes the following steps: Weigh polyurethane, flame retardant, additive, diluent and pretreated epoxy resin as required and add them into a reaction kettle, and carry out stirring treatment at 23 °C. The stirring speed is 40 r / min, and the treatment time is 50 min. After the stirring treatment is completed, let it stand for 8 h to obtain the high-temperature resistant glue for the new energy heating film.

[0053] Example 3: It includes the following raw material composition by weight percentage: 66% polyurethane, 12% flame retardant, 8% additive, 1.2% diluent, and the balance is epoxy resin;

[0054] The epoxy resin is pretreated before preparation;

[0055] The additive is prepared by the following steps:

[0056] S1: Preparation of the base material;

[0057] S2: Treatment of the base material to obtain the additive.

[0058] The pretreatment method of epoxy resin is as follows: Epoxy resin is added into a reaction kettle, the temperature of the reaction kettle is set at 60 °C, and it is kept still at a constant temperature for 20 min. Then, a mixture is added into the reaction kettle, the temperature of the reaction kettle is set to rise to 120 °C, the stirring speed is 300 r / min, and it is stirred at a constant temperature for 3 h. After that, the temperature of the reaction kettle is set to rise to 150 °C, and it reacts at a constant temperature for 4 h. After the constant-temperature reaction ends, it is cooled to room temperature, and the obtained product is allowed to stand for 6 h to complete the pretreatment of epoxy resin.

[0059] The mixture is prepared by the following method: Polyimide, biphenyl-type epoxy resin, and polybenzimidazole are added into a reaction kettle, the temperature of the reaction kettle is set at 50 °C, the stirring speed is 400 r / min, and it is stirred at a constant temperature for 30 min. Then, silicon dioxide and KH-550 are added into the reaction kettle. After cooling to room temperature, the stirring speed is set to 500 r / min, and it is stirred for 30 min to obtain the mixture.

[0060] The mass ratio of polyimide, biphenyl-type epoxy resin, and polybenzimidazole is 1:0.3:0.8. The mass of silicon dioxide is 20% of the mass of polyimide, and the mass of KH-550 is 10% of the mass of polyimide. Silicon dioxide is selected as powder with a particle size of 40 nm.

[0061] The method for preparing the base material is as follows: Boron nitride is sent into an oven, the oven is set at 100 °C, and it is dried for 4 h. Then, the dried boron nitride is added into a mixer, KH-560 is added into the mixer, and the mixer is set to stir at 500 r / min for 40 min. After the stirring treatment is completed, polytetrafluoroethylene, zirconia, and polyether-modified silicone oil are added into the mixer, and the mixer is set to stir at 300 r / min for 60 min to obtain the base material.

[0062] The mass of KH-560 is 6% of the mass of boron nitride, the mass of polytetrafluoroethylene is 8% of the mass of boron nitride, the mass of zirconia is 12% of the mass of boron nitride, and the mass of polyether-modified silicone oil is 3% of the mass of boron nitride. Boron nitride, polytetrafluoroethylene, and zirconia are all selected as powders. The particle size of boron nitride is 40 nm, and the particle sizes of polytetrafluoroethylene and zirconia are 60 nm.

[0063] The method for treating the base material is as follows: The base material and powder are added into a mixer, the mixer is set to stir at 800 r / min for 20 min to complete the treatment of the base material and obtain the additive.

[0064] The powder is prepared by the following method: Montmorillonite and deionized water are added to a water bath pot, and the water bath pot is set to heat up to 60°C. At the same time, a magnetic stirrer is connected, and the magnetic stirrer is set at 300 r / min for constant-temperature stirring treatment for 12 min. Then, cetyltrimethylammonium bromide and multi-walled carbon nanotubes are added, the temperature is set at 80°C, and the magnetic stirrer is set at 500 r / min for constant-temperature stirring treatment for 4 h. After the constant-temperature stirring treatment is completed, wait for it to cool to room temperature, and the obtained product is centrifuged to obtain a precipitate. The precipitate is sent into an oven, and the oven is set at 60°C for drying treatment for 4 h to obtain the powder. Among them, the mass ratio of montmorillonite to deionized water is 1:4, the mass of cetyltrimethylammonium bromide is 3% of the mass of montmorillonite, and the mass of multi-walled carbon nanotubes is 4% of the mass of montmorillonite.

[0065] The diluent is prepared by mixing neopentyl glycol diglycidyl ether and phenyl glycidyl ether, and the mass ratio of neopentyl glycol diglycidyl ether to phenyl glycidyl ether is 1:0.6. The flame retardant is selected as cage-type polyhedral oligomeric silsesquioxane.

[0066] A preparation method for a high-temperature resistant glue formula of a new energy heating film includes the following steps: Weigh polyurethane, flame retardant, additive, diluent and pretreated epoxy resin as required and add them to a reaction kettle, and carry out stirring treatment at 26°C. The stirring speed is 500 r / min, and the treatment time is 60 min. After the stirring treatment is completed, let it stand for 10 h to obtain the high-temperature resistant glue for the new energy heating film.

[0067] Comparative Example 1. The difference between this comparative example and Example 1 is that: This comparative example does not contain a diluent.

[0068] Comparative Example 2. The difference between this comparative example and Example 1 is that: This comparative example does not contain epoxy resin.

[0069] Comparative Example 3. The difference between this comparative example and Example 1 is that: In this comparative example, the epoxy resin was not pretreated.

[0070] Comparative Example 4. The difference between this comparative example and Example 1 is that: This comparative example does not contain an additive.

[0071] Performance test: Perform performance tests on the high-temperature resistant glues for new energy heating films prepared in Example 1, Example 2, Example 3, Comparative Example 1, Comparative Example 2, Comparative Example 3 and Comparative Example 4, and record the obtained test data in the following table:

[0072]

[0073] In the performance test, after the high-temperature resistant glue of the new energy heating film prepared in Example 1, Example 2, Example 3, Comparative Example 1, Comparative Example 2, Comparative Example 3, and Comparative Example 4 was coated, heat treatment was carried out to observe whether the glue showed delamination and bubbling phenomena; the peel strength performance test of the high-temperature resistant glue of the new energy heating film prepared in Example 1, Example 2, Example 3, Comparative Example 1, Comparative Example 2, Comparative Example 3, and Comparative Example 4 was carried out by using the test method in GB / T 2790-1995.

[0074] It can be seen that the high-temperature resistance performance and peel strength performance of the high-temperature resistant glue of the new energy heating film prepared in Comparative Examples 1, 2, 3, and 4 are lower than those in Examples 1, 2, and 3; this shows that: by using additives in the formula of the high-temperature resistant glue of the new energy heating film, after the nano-scale boron nitride is surface-modified by KH-560 silane coupling agent, a three-dimensional heat conduction network is formed with polytetrafluoroethylene, effectively improving the heat conduction efficiency of the material. Polytetrafluoroethylene forms a low surface energy layer during the mixing process, which can play a role in reducing the molecular chain mobility at high temperature. At the same time, the addition of zirconia realizes particle filling, further improving the thermal stability performance of the material;

[0075] The use of polyether-modified silicone oil combined with KH-560 forms a gradient interface layer, effectively improving the wettability of the material. By pre-treating the epoxy resin, it can play a role in eliminating the internal stress generated during the storage of the epoxy resin, making its molecular chain initially stretch. After high-temperature treatment, it can promote the pre-polymerization reaction of polyimide and biphenyl-type epoxy resin to form a branched structure. Montmorillonite and multi-walled carbon nanotubes can be combined and locked with each other to improve the interfacial bonding force, and thus effectively improve the peel strength performance of the material.

[0076] By comparing and analyzing the relevant data in the table, it can be known that the high-temperature resistant glue of the new energy heating film prepared by the present invention not only has good high-temperature resistance performance, but also has excellent peel strength performance. This shows that the formula of the high-temperature resistant glue of the new energy heating film provided by the present invention has a broader market prospect and is more suitable for popularization.

[0077] In the description of this specification, the description referring 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 representations of the above terms do 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.

[0078] The preferred embodiments of the present invention disclosed above are only used to help illustrate 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, many modifications and variations can be made according to the content of this specification. These embodiments are selected and specifically described in this specification to better explain the principles and practical applications 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 high-temperature resistant glue formula for a new energy heating film, characterized in that: It comprises the following raw materials by weight percentage: 60-66% polyurethane, 8-12% flame retardant, 6-8% additive, 0.6-1.2% diluent, and the balance is epoxy resin; The epoxy resin is pretreated before preparation; The additive is prepared by the following steps: S1: Preparation of base material; S2: Treatment of base material to obtain the additive.

2. The high-temperature resistant glue formula for the new energy heating film according to claim 1, wherein The pretreatment method of the epoxy resin is as follows: The epoxy resin is added into a reaction kettle, the set temperature of the reaction kettle is 50-60 °C, and it is kept still at a constant temperature for 10-20 min. Then, a mixture is added into the reaction kettle, the set temperature of the reaction kettle is raised to 80-120 °C, the stirring speed is 200-300 r / min, and it is stirred at a constant temperature for 1-3 h. Then, the set temperature of the reaction kettle is raised to 140-150 °C, and it reacts at a constant temperature for 2-4 h. After the constant-temperature reaction is completed, it is cooled to room temperature, and the obtained product is left standing for 4-6 h to complete the pretreatment of the epoxy resin.

3. The high-temperature resistant glue formula for the new energy heating film according to claim 2, characterized in that, The mixture is prepared by the following method: Polyimide, biphenyl-type epoxy resin, and polybenzimidazole are added into a reaction kettle, the set temperature of the reaction kettle is 40-50 °C, the stirring speed is 300-400 r / min, and it is stirred at a constant temperature for 20-30 min. Then, silica and KH-550 are added into the reaction kettle. After being cooled to room temperature, the stirring speed is set to 400-500 r / min, and it is stirred for 20-30 min to obtain the mixture.

4. The high-temperature resistant glue formulation for the new energy heating film according to claim 3, characterized in that, The mass ratio of polyimide, biphenyl-type epoxy resin, and polybenzimidazole is 1:(0.1-0.3):(0.6-0.8). The mass of silica is 10-20% of the mass of polyimide, the mass of KH-550 is 6-10% of the mass of polyimide, the silica is selected as powder with a particle size of 10-40 nm.

5. The high-temperature resistant glue formula for the new energy heating film according to claim 1, characterized in that, The method for preparing the base material is as follows: Boron nitride is sent into an oven, the set temperature of the oven is 80-100 °C, and it is dried for 2-4 h. Then, the dried boron nitride is added into a mixer, KH-560 is added into the mixer, and the mixer is set to stir at 400-500 r / min for 30-40 min. After the stirring treatment is completed, polytetrafluoroethylene, zirconia, and polyether-modified silicone oil are added into the mixer, and the mixer is set to stir at 200-300 r / min for 50-60 min to obtain the base material.

6. The high-temperature resistant glue formula for the new energy heating film according to claim 5, characterized in that, The mass of KH-560 is 4-6% of the mass of boron nitride, the mass of polytetrafluoroethylene is 6-8% of the mass of boron nitride, the mass of zirconia is 10-12% of the mass of boron nitride, the mass of polyether-modified silicone oil is 1-3% of the mass of boron nitride. Boron nitride, polytetrafluoroethylene, and zirconia are all selected as powders. The particle size of boron nitride is 10-40 nm, and the particle sizes of polytetrafluoroethylene and zirconia are 20-60 nm.

7. The high-temperature resistant glue formula for the new energy heating film according to claim 1, characterized in that, The method for treating the base material is as follows: The base material and powder are added into a mixer, and the mixer is set to stir at 600-800 r / min for 10-20 min to complete the treatment of the base material and obtain the additive.

8. The high-temperature resistant glue formula for the new energy heating film according to claim 7, characterized in that, The powder material is prepared by the following method: Montmorillonite and deionized water are added into a water bath kettle, and the water bath kettle is set to heat up to 50-60 °C. Meanwhile, a magnetic stirrer is connected, and the magnetic stirrer is set at 200-300 r / min for constant-temperature stirring treatment for 6-12 min. Then, cetyltrimethylammonium bromide and multi-walled carbon nanotubes are added, the temperature is set at 70-80 °C, the magnetic stirrer is set at 400-500 r / min, and the constant-temperature stirring treatment is carried out for 2-4 h. After the constant-temperature stirring treatment is completed, it is cooled to room temperature, and the obtained product is centrifuged to obtain a precipitate. The precipitate is sent into an oven, and the oven is set at 50-60 °C for drying treatment for 2-4 h to prepare the powder material. Among them, the mass ratio of montmorillonite to deionized water is 1:(2-4), the mass of cetyltrimethylammonium bromide is 1-3% of the mass of montmorillonite, and the mass of multi-walled carbon nanotubes is 2-4% of the mass of montmorillonite.

9. The high-temperature resistant glue formulation for a new energy heating film according to claim 1, wherein, The diluent is prepared by mixing neopentyl glycol diglycidyl ether and phenyl glycidyl ether, and the mass ratio of neopentyl glycol diglycidyl ether to phenyl glycidyl ether is 1:(0.4-0.6). The flame retardant is selected as cage-type polyhedral oligomeric silsesquioxane.

10. A preparation method of a high-temperature resistant glue formula for a new energy heating film according to any one of claims 1 to 9, characterized in that, It includes the following steps: Weigh polyurethane, flame retardant, additive, diluent and pretreated epoxy resin as required and add them into a reaction kettle, and carry out stirring treatment under the condition of 20-26 °C. The stirring speed is 300-500 r / min, and the treatment time is 40-60 min. After the stirring treatment is completed, it is left standing for 6-10 h to prepare the high-temperature resistant glue for the new energy heating film.

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