High-transparency weather-resistant epoxy resin pouring sealant and preparation method thereof
Through the combination of bisphenol A type epoxy resin and glycidyl ester type epoxy resin and the use of modified alicyclic amine curing agent, the problem of insufficient transparency and weather resistance of epoxy resin potting glue is solved, and high transparency is prepared Weather-resistant epoxy resin potting adhesive improves its mechanical properties and service life.
Patent Information
- Application Number
- CN202411556686.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-04
- Publication Date
- 2024-12-27
AI Technical Summary
The transparency and weather resistance of existing epoxy resin potting glues are insufficient, which leads to prone to cracking and turning yellowing during use, affecting the quality and safety and stability of electrical products.
Using the combination of bisphenol A type epoxy resin and glycidyl ester type epoxy resin, combined with modified alicyclic amine curing agent and toughening agent, high transparency and weather resistance epoxy resin filling sealing is prepared through mixing and mechanical stirring. glue forms a highly crosslinked three-dimensional network structure to improve its weather resistance and mechanical properties.
It significantly improves the transparency, weather resistance and mechanical properties of the potting glue, reduces brittleness and internal stress, enhances crack resistance and electrical insulation properties, and extends service life.
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Figure BDA0005116665590000161 
Figure BDA0005116665590000171
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of epoxy potting adhesives, and in particular relates to a highly transparent weather-resistant epoxy resin potting adhesive and a preparation method thereof. Background Art
[0002] In the electronics industry, it is necessary to potting electronic components or assembly parts to isolate them from the outside world, so as to improve the electronic components' ability to resist impact and vibration, harsh environment, dust, moisture and corrosion, as well as electrical insulation and thermal conductivity. Therefore, potting glue is widely used in the overall potting and sealing of electrical equipment such as dry-type transformers and mutual inductors. Potting glue can be divided into epoxy resin (EP) potting glue, silicone (SR) potting glue and polyurethane (PU) potting glue according to its main components. Among them, epoxy resin is applied to potting materials due to its excellent mechanical properties, electrical properties, corrosion resistance, bonding properties, small linear expansion coefficient, high Young's modulus, solvent resistance and other advantages. Epoxy resin is used as the packaging material of electronic components, which has high hardness and strength, and can effectively protect electronic components from external impact and vibration. Excellent electrical insulation and adhesion can form a firm bond with other materials to prevent leakage and interference of electrical signals. Excellent high temperature resistance, sealing and dielectric properties can avoid damage to electronic components and extend service life.
[0003] The Chinese patent document with publication number CN118185535A discloses an epoxy resin electronic potting glue and its preparation method and application. The specific formula includes component A and component B; component A includes epoxy resin, defoamer, leveling agent, epoxy diluent, color powder and filler; component B includes aromatic amine curing agent, benzyl alcohol, furfuryl alcohol and salicylic acid; in the preparation process, component A and component B are prepared separately and mixed in a specific ratio to obtain epoxy resin electronic potting glue. The specific formula and preparation process of the invention realize the optimization of the performance of epoxy resin potting glue at the molecular level, so that the formed potting glue has a strong and stable cross-linked network structure inside. This structure can provide good thermal stability and chemical stability, as well as excellent electrical insulation performance, so that the finished product has higher mechanical strength, especially greatly enhances the impact strength and tensile strength, and meets the needs of high-end electronic packaging materials.
[0004] With the rapid development of electronic communication technology, electronic components are becoming increasingly miniaturized, lighter, and more integrated, and the requirements for the use and performance of epoxy potting adhesives will become more and more stringent. The transparency and aging resistance of epoxy potting adhesives on the market are poor, that is, the cured product is easily affected by the environment and cracks, turns yellow, and has low transparency, which seriously affects the quality and safety stability of electrical products during use. At present, most epoxy resin potting adhesives have the disadvantages of insufficient transparency and weather resistance. Therefore, it is very important to study the improvement of the weather resistance and transparency of epoxy resin potting adhesives. Summary of the invention
[0005] The technical problem solved by the invention is to provide a highly transparent weather-resistant epoxy resin potting adhesive and a preparation method thereof, aiming to solve the problems of insufficient transparency and weather resistance of most epoxy resin potting adhesives.
[0006] In order to solve the above problems, the first aspect of the present invention provides a highly transparent weather-resistant epoxy resin potting glue:
[0007] Including component A and component B:
[0008] The component A comprises the following components in parts by mass: 100 parts of epoxy resin, 0-30 parts of toughening agent, 0.3-0.5 parts of antioxidant, 1-5 parts of diluent, and 0.1-1 parts of first defoaming agent; and the toughening agent is not 0; wherein the epoxy resin is a mixture of at least two of bisphenol A epoxy resin, hydrogenated bisphenol A epoxy resin and glycidyl ester epoxy resin;
[0009] The B component includes the following components in parts by mass: 100 parts of curing agent, 0-10 parts of curing accelerator, and 0.1-1 parts of second defoaming agent; and the curing accelerator is not 0;
[0010] The mass ratio of the component A to the component B is 100:30-80.
[0011] Preferably, the A component includes the following components in parts by mass: 100 parts of epoxy resin, 0-20 parts of toughening agent, 0.3-0.5 parts of antioxidant, 1-3 parts of diluent, 0.1-0.5 parts of first defoaming agent; and the toughening agent is not 0; the B component includes the following components in parts by mass: 100 parts of curing agent, 0-5 parts of curing accelerator, 0.1-0.5 parts of second defoaming agent; and the curing accelerator is not 0; the mass ratio of the A component to the B component is 100:40-60.
[0012] Preferably, the component A includes the following components in parts by mass: 100 parts of epoxy resin, 10 parts of toughening agent, 0.3 parts of antioxidant, 2 parts of diluent, and 0.3 parts of first defoaming agent; the component B includes the following components in parts by mass: 100 parts of curing agent, 2 parts of curing accelerator, and 0.3 parts of second defoaming agent; the mass ratio of the component A to the component B is 100:50.
[0013] Preferably, the epoxy resin is a mixture of bisphenol A epoxy resin and glycidyl ester epoxy resin or a mixture of bisphenol A epoxy resin, hydrogenated bisphenol A epoxy resin and glycidyl ester epoxy resin; the epoxy resin includes: 0-40 parts of bisphenol A epoxy resin; 0-60 parts of hydrogenated bisphenol A epoxy resin; 20-100 parts of glycidyl ester epoxy resin.
[0014] Preferably, the bisphenol A type epoxy resin is a mixture of one or more of epoxy resin E44, epoxy resin E51, and epoxy resin E54; the hydrogenated bisphenol A type epoxy resin is a mixture of one or more of epoxy resin AL3030, epoxy resin AL3040, and epoxy resin AL3050; the glycidyl ester type epoxy resin is a mixture of one or more of diglycidyl phthalate, diglycidyl hexahydrophthalate, diglycidyl terephthalate, diglycidyl isophthalate, diglycidyl tetrahydrophthalate, diglycidyl methyltetrahydrophthalate, diglycidyl endonucleate, and diglycidyl adipic acid.
[0015] Preferably, the curing agent is a modified alicyclic amine curing agent, and the modified alicyclic amine curing agent is a mixture of one or more of isophorone diamine, R-2263, R-2270, R-2282, R-9030B, R-3604, R-3328L, and R-5911-8; the curing accelerator is a mixture of one or more of triethanolamine, 1,3-cyclohexanedimethylamine, triethylamine, and benzyldimethylamine; the toughening agent is a mixture of one or more of a core-shell toughening agent, a polyurethane toughening agent, a carboxyl-terminated liquid nitrile rubber toughening agent, and an epoxy resin active toughening agent.
[0016] Preferably, the antioxidant is a mixture of one or more of a phosphite antioxidant, a hindered phenol antioxidant, a thioether antioxidant and a sulfur-containing antioxidant; the diluent is a mixture of one or more of 1,4-butanediol diglycidyl ether, 1,6-hexanediol diglycidyl ether, dipropylene glycol diacrylate and tripropylene glycol diacrylate.
[0017] Preferably, the first defoamer is one of BYK-A530, BYK-special, BYK-1790, P573, P990 or a mixture of several thereof; the second defoamer is one of BYK-A530, BYK-special, BYK-1790, P573, P990 or a mixture of several thereof.
[0018] The second aspect of the present invention provides a method for preparing the above-mentioned highly transparent weather-resistant epoxy resin potting adhesive, comprising the following steps:
[0019] S1: Mix epoxy resin, toughening agent, antioxidant, diluent and first defoaming agent in proportion to prepare component A;
[0020] S2: Mix the curing agent, curing accelerator and second defoaming agent in proportion to prepare component B;
[0021] S3: Mixing component A and component B to obtain the highly transparent weather-resistant epoxy resin potting adhesive.
[0022] Preferably, the step S1 specifically includes the following steps: adding the epoxy resin, the toughening agent, the antioxidant, the diluent, and the first defoaming agent into a reactor in proportion, mechanically stirring and dispersing at a speed of 400 r / min, and vacuuming during the stirring process; stirring for 60 minutes, degassing for 30 minutes after sufficient stirring, to obtain the component A; the step S2 specifically includes the following steps: adding the curing agent, the curing accelerator, and the second defoaming agent into a reactor in proportion, mechanically stirring and dispersing at a speed of 300 r / min, and vacuuming during the stirring process; stirring for 30 minutes, degassing for 10 minutes after sufficient stirring, to obtain the component B.
[0023] Compared with the prior art, the present invention has the following beneficial effects:
[0024] The highly transparent weather-resistant epoxy resin potting glue of the present invention is compounded by adding glycidyl ester epoxy resin and epoxy resin, thereby improving the weather resistance and heat resistance of the potting glue, and the added modified alicyclic amine curing agent significantly improves the weather resistance and mechanical properties of the potting glue; the toughening agent added to the potting glue improves the flexibility of the potting glue, reduces its brittleness and internal stress, and significantly improves the anti-cracking property and electrical insulation property of the potting glue; the prepared epoxy potting glue has no filler added, so that the potting glue has higher transparency and fluidity. DETAILED DESCRIPTION
[0025] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solution of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0026] A first aspect of an embodiment of the present invention provides a highly transparent weather-resistant epoxy resin potting adhesive:
[0027] Including component A and component B:
[0028] The component A comprises the following components in parts by mass: 100 parts of epoxy resin, 0-30 parts of toughening agent, 0.3-0.5 parts of antioxidant, 1-5 parts of diluent, and 0.1-1 parts of first defoaming agent; and the toughening agent is not 0; wherein the epoxy resin is a mixture of at least two of bisphenol A epoxy resin, hydrogenated bisphenol A epoxy resin and glycidyl ester epoxy resin;
[0029] The B component includes the following components in parts by mass: 100 parts of curing agent, 0-10 parts of curing accelerator, and 0.1-1 parts of second defoaming agent; and the curing accelerator is not 0;
[0030] The mass ratio of the component A to the component B is 100:30-80.
[0031] The highly transparent weather-resistant epoxy resin potting glue of the embodiment of the present invention is compounded by adding glycidyl ester epoxy resin and bisphenol A epoxy resin, thereby improving the weather resistance and heat resistance of the potting glue. The molecular structure of the hydrogenated epoxy resin is converted from a benzene ring to a saturated six-membered ring. The saturated bond is more stable to ultraviolet rays and oxidation, and is not easy to break, thereby improving the weather resistance of the material. Glycidyl ester epoxy resin is a saturated structure and contains multiple epoxy groups, and forms a highly cross-linked three-dimensional network structure during the curing process. This high cross-linking density structure helps to improve the heat resistance, chemical corrosion resistance and mechanical strength of the material, and also enhances weather resistance. The addition of a toughening agent can improve the flexibility of the potting glue, reduce brittleness and internal stress, and significantly improve the anti-cracking performance and electrical insulation performance of the potting glue. The prepared epoxy potting glue has no filler added, so that the potting glue has better transparency and fluidity.
[0032] The highly transparent weather-resistant epoxy resin potting glue of the embodiment of the present invention may be brittle without the addition of fillers, and cracks may easily form after being subjected to thermal shocks. Therefore, a toughening agent is added to improve the flexibility of the potting glue and reduce its brittleness. The molecule of diglycidyl hexahydrophthalate contains a saturated structure and has excellent mechanical properties and crack resistance at ultra-low temperatures.
[0033] In some embodiments, the A component includes the following components in parts by mass: 100 parts of epoxy resin, 0-20 parts of toughening agent, 0.3-0.5 parts of antioxidant, 1-3 parts of diluent, 0.1-0.5 parts of first defoaming agent; and the toughening agent is not 0; the B component includes the following components in parts by mass: 100 parts of curing agent, 0-5 parts of curing accelerator, 0.1-0.5 parts of second defoaming agent; and the curing accelerator is not 0; the mass ratio of the A component to the B component is 100:40-60.
[0034] In some embodiments, the A component includes the following components in parts by mass: 100 parts of epoxy resin, 10 parts of toughening agent, 0.3 parts of antioxidant, 2 parts of diluent, and 0.3 parts of first defoaming agent; the B component includes the following components in parts by mass: 100 parts of curing agent, 2 parts of curing accelerator, and 0.3 parts of second defoaming agent; the mass ratio of the A component to the B component is 100:50.
[0035] In some embodiments, the epoxy resin is a mixture of bisphenol A epoxy resin and glycidyl ester epoxy resin or a mixture of bisphenol A epoxy resin, hydrogenated bisphenol A epoxy resin and glycidyl ester epoxy resin; the epoxy resin includes: 0-40 parts of bisphenol A epoxy resin; 0-60 parts of hydrogenated bisphenol A epoxy resin; 20-100 parts of glycidyl ester epoxy resin. Glycidyl ester epoxy resin and hydrogenated bisphenol A epoxy resin have low viscosity, low chroma and high transparency. After mixed use, the transparency of the potting glue is higher and the weather resistance is good. The hydroxyl and ether bonds in the molecular chain of bisphenol A epoxy resin give it high bonding properties and excellent electrical insulation. Therefore, the compounding of epoxy resin and glycidyl resin makes the mechanical properties, heat resistance, bonding properties, and mechanical properties of the potting glue better and reduces viscosity and cost.
[0036] In some embodiments, the bisphenol A type epoxy resin is a mixture of one or more of epoxy resin E44, epoxy resin E51, and epoxy resin E54; the hydrogenated bisphenol A type epoxy resin is a mixture of one or more of epoxy resin AL3030, epoxy resin AL3040, and epoxy resin AL3050; the glycidyl ester type epoxy resin is a mixture of one or more of diglycidyl phthalate, diglycidyl hexahydrophthalate, diglycidyl terephthalate, diglycidyl isophthalate, diglycidyl tetrahydrophthalate, diglycidyl methyltetrahydrophthalate, diglycidyl endonucleate, and diglycidyl adipic acid.
[0037] In some embodiments, the curing agent is a modified alicyclic amine curing agent. The present invention further adds a modified alicyclic amine curing agent, which can significantly improve the weather resistance and mechanical properties of the potting glue. The alicyclic amine group in the curing agent reacts with the epoxy group in the epoxy resin to form a three-dimensional network structure, that is, an amine-amine cross-linked structure, thereby improving the mechanical properties of the material. The modified alicyclic amine curing agent is a mixture of one or more of isophorone diamine, R-2263, R-2270, R-2282, R-9030B, R-3604, R-3328L, and R-5911-8; the curing accelerator is a mixture of one or more of triethanolamine, 1,3-cyclohexanedimethylamine, triethylamine, and benzyldimethylamine; the toughening agent is a mixture of one or more of a core-shell toughening agent, a polyurethane toughening agent, a carboxyl-terminated liquid nitrile rubber toughening agent, and an epoxy resin active toughening agent.
[0038] In some embodiments, the antioxidant is a mixture of one or more of a phosphite antioxidant, a hindered phenol antioxidant, a thioether antioxidant and a sulfur-containing antioxidant; the diluent is a mixture of one or more of 1,4-butanediol diglycidyl ether, 1,6-hexanediol diglycidyl ether, dipropylene glycol diacrylate and tripropylene glycol diacrylate.
[0039] In some embodiments, the first defoamer is one of BYK-A530, BYK-special, BYK-1790, P573, P990 or a mixture of several thereof; the second defoamer is one of BYK-A530, BYK-special, BYK-1790, P573, P990 or a mixture of several thereof.
[0040] A second aspect of an embodiment of the present invention provides a method for preparing the above-mentioned highly transparent weather-resistant epoxy resin potting adhesive, comprising the following steps:
[0041] S1: Mix epoxy resin, toughening agent, antioxidant, diluent and first defoaming agent in proportion to prepare component A;
[0042] S2: Mix the curing agent, curing accelerator and second defoaming agent in proportion to prepare component B;
[0043] S3: Mixing component A and component B to obtain the highly transparent weather-resistant epoxy resin potting adhesive.
[0044] In some embodiments, the step S1 specifically includes the following steps: adding the epoxy resin, the toughening agent, the antioxidant, the diluent, and the first defoaming agent into the reactor in proportion, mechanically stirring and dispersing at a speed of 400 r / min, and vacuuming during the stirring process; stirring for 60 minutes, degassing for 30 minutes after sufficient stirring, to obtain the A component; the step S2 specifically includes the following steps: adding the curing agent, the curing accelerator, and the second defoaming agent into the reactor in proportion, mechanically stirring and dispersing at a speed of 300 r / min, and vacuuming during the stirring process; stirring for 30 minutes, degassing for 10 minutes after sufficient stirring, to obtain the B component.
[0045] Example 1
[0046] The highly transparent weather-resistant epoxy resin potting glue of this embodiment:
[0047] Including component A and component B:
[0048] The component A comprises the following components in parts by mass: 100 parts of epoxy resin, 10 parts of toughening agent, 0.3 parts of antioxidant, 2 parts of diluent, and 0.3 parts of first defoaming agent;
[0049] The B component includes the following components in parts by mass: 100 parts of curing agent, 1 part of curing accelerator, and 0.3 parts of second defoaming agent;
[0050] The mass ratio of the component A to the component B is 100:50.
[0051] The preparation method of the highly transparent weather-resistant epoxy resin potting glue of this embodiment comprises the following steps:
[0052] S1: 40 parts of epoxy resin E54, 60 parts of diglycidyl hexahydrophthalate, 10 parts of epoxy resin active toughening agent, 0.3 parts of phosphite antioxidant, 2 parts of 1,4-butanediol diglycidyl ether, and 0.3 parts of BYK-A530 were added to a reactor, and mechanically stirred and dispersed at a speed of 400 r / min at room temperature. Vacuuming was required during the stirring process. After stirring for 60 minutes, degassing was performed for 30 minutes to obtain component A;
[0053] S2: 100 parts of R-2263, 1 part of 1,3-cyclohexanedimethylamine, and 0.3 parts of BYK-A530 were mechanically stirred at a speed of 300 r / min and vacuumed, and then degassed after stirring for 30 minutes to obtain component B;
[0054] S3: After cleaning the polytetrafluoroethylene mold with anhydrous ethanol, wipe the polytetrafluoroethylene mold with a release agent and dry it; start pouring the glue, mix the A and B components at a mass ratio of 100:50 at room temperature, cure at room temperature, and then perform a performance test on the cured potting glue. The test results are shown in Table 1.
[0055] Example 2
[0056] The highly transparent weather-resistant epoxy resin potting glue of this embodiment:
[0057] Including component A and component B:
[0058] The component A comprises the following components in parts by mass: 100 parts of epoxy resin, 10 parts of toughening agent, 0.3 parts of antioxidant, 2 parts of diluent, and 0.3 parts of first defoaming agent;
[0059] The B component includes the following components in parts by mass: 100 parts of curing agent, 1 part of curing accelerator, and 0.3 parts of second defoaming agent;
[0060] The mass ratio of the component A to the component B is 100:50.
[0061] The preparation method of the highly transparent weather-resistant epoxy resin potting glue of this embodiment comprises the following steps:
[0062] S1: 40 parts of epoxy resin E54, 60 parts of diglycidyl hexahydrophthalate, 10 parts of epoxy resin active toughening agent, 0.3 parts of phosphite antioxidant, 2 parts of 1,4-butanediol diglycidyl ether, and 0.3 parts of BYK-A530 were added to a reactor, and mechanically stirred and dispersed at a speed of 400 r / min at room temperature. Vacuuming was required during the stirring process. After stirring for 60 minutes, degassing was performed for 30 minutes to obtain component A;
[0063] S2: 100 parts of R-3328L, 1 part of 1,3-cyclohexanedimethylamine, and 0.3 parts of BYK-A530 were mechanically stirred at a speed of 300 r / min and vacuumed, and degassed after stirring for 20 minutes to obtain component B;
[0064] S3: After cleaning the polytetrafluoroethylene mold with anhydrous ethanol, wipe the polytetrafluoroethylene mold with a release agent and dry it; start pouring the glue, mix the A and B components at a mass ratio of 100:50 at room temperature, cure at room temperature, and then perform a performance test on the cured potting glue. The test results are shown in Table 1.
[0065] Example 3
[0066] The highly transparent weather-resistant epoxy resin potting glue of this embodiment:
[0067] Including component A and component B:
[0068] The component A comprises the following components in parts by mass: 100 parts of epoxy resin, 10 parts of toughening agent, 0.3 parts of antioxidant, 2 parts of diluent, and 0.3 parts of first defoaming agent;
[0069] The B component includes the following components in parts by mass: 100 parts of curing agent, 2 parts of curing accelerator, and 0.3 parts of second defoaming agent;
[0070] The mass ratio of the component A to the component B is 100:50.
[0071] The preparation method of the highly transparent weather-resistant epoxy resin potting glue of this embodiment comprises the following steps:
[0072] S1: 40 parts of hydrogenated bisphenol A epoxy resin, 60 parts of diglycidyl hexahydrophthalate, 10 parts of epoxy resin active toughening agent, 0.3 parts of phosphite antioxidant, 2 parts of 1,4-butanediol diglycidyl ether, and 0.3 parts of BYK-A530 defoamer are added to a reactor, and mechanically stirred and dispersed at a speed of 400 r / min at room temperature. Vacuuming is required during the stirring process. After stirring for 60 minutes, degassing is performed for 30 minutes to obtain component A;
[0073] S2: 100 parts of R9030B, 2 parts of 1,3-cyclohexanedimethylamine, and 0.3 parts of BYK-A530 were mechanically stirred at a speed of 300 r / min and vacuumed, and degassed after stirring for 20 minutes to obtain component B;
[0074] S3: After cleaning the polytetrafluoroethylene mold with anhydrous ethanol, wipe the polytetrafluoroethylene mold with a release agent and dry it; start pouring the glue, mix the A and B components at a mass ratio of 100:50 at room temperature, cure at room temperature, and then perform a performance test on the cured potting glue. The test results are shown in Table 1.
[0075] Example 4
[0076] The highly transparent weather-resistant epoxy resin potting glue of this embodiment:
[0077] Including component A and component B:
[0078] The component A comprises the following components in parts by weight: 100 parts of epoxy resin, 15 parts of toughening agent, 0.3 parts of antioxidant, 2 parts of diluent, and 0.3 parts of first defoaming agent;
[0079] The B component includes the following components in parts by mass: 100 parts of curing agent, 2 parts of curing accelerator, and 0.3 parts of second defoaming agent;
[0080] The mass ratio of the component A to the component B is 100:80.
[0081] The preparation method of the highly transparent weather-resistant epoxy resin potting glue of this embodiment comprises the following steps:
[0082] S1: 40 parts of epoxy resin E54, 20 parts of hydrogenated bisphenol A epoxy resin, 40 parts of diglycidyl hexahydrophthalate, 15 parts of epoxy resin active toughening agent, 2 parts of 1,4-butanediol diglycidyl ether, 0.3 parts of phosphite antioxidant, and 0.3 parts of BYK-A530 defoamer are added to a reactor, and mechanically stirred and dispersed at a speed of 400 r / min at room temperature. Vacuuming is required during the stirring process. After stirring for 60 minutes, degassing is performed for 30 minutes to obtain component A;
[0083] S2: 100 parts of R9030B, 2 parts of 1,3-cyclohexanedimethylamine, and 0.3 parts of BYK-A530 were mechanically stirred at a speed of 300 r / min and vacuumed, and then stirred for 20 minutes and degassed to obtain component B;
[0084] S3: After cleaning the polytetrafluoroethylene mold with anhydrous ethanol, wipe the polytetrafluoroethylene mold with a release agent and dry it; start pouring the glue, mix the A and B components at a mass ratio of 100:80 at room temperature, cure at room temperature, and then perform a performance test on the cured potting glue. The test results are shown in Table 1.
[0085] Example 5
[0086] The highly transparent weather-resistant epoxy resin potting glue of this embodiment:
[0087] Including component A and component B:
[0088] The component A comprises the following components in parts by mass: 100 parts of epoxy resin, 20 parts of toughening agent, 0.3 parts of antioxidant, 2 parts of diluent, and 0.3 parts of first defoaming agent;
[0089] The B component includes the following components in parts by mass: 100 parts of curing agent, 4 parts of curing accelerator, and 0.3 parts of second defoaming agent;
[0090] The mass ratio of the component A to the component B is 100:80.
[0091] The preparation method of the highly transparent weather-resistant epoxy resin potting glue of this embodiment comprises the following steps:
[0092] S1: 20 parts of epoxy resin E54, 40 parts of hydrogenated bisphenol A epoxy resin, 40 parts of diglycidyl hexahydrophthalate, 20 parts of epoxy resin active toughening agent, 0.3 parts of phosphite antioxidant, 2 parts of 1,4-butanediol diglycidyl ether, and 0.3 parts of BYK-A530 defoamer are added to a reactor, and mechanically stirred and dispersed at a speed of 400 r / min at room temperature. Vacuuming is required during the stirring process. After stirring for 60 minutes, degassing is performed for 30 minutes to obtain component A;
[0093] S2: 100 parts of R9030B, 4 parts of 1,3-cyclohexanedimethylamine, and 0.3 parts of BYK-A530 were mechanically stirred at a speed of 300 r / min and vacuumed, and degassed after stirring for 20 minutes to obtain component B;
[0094] S3: After cleaning the polytetrafluoroethylene mold with anhydrous ethanol, wipe the polytetrafluoroethylene mold with a release agent and dry it; start pouring the glue, mix the A and B components at a mass ratio of 100:80 at room temperature, cure at room temperature, and then perform a performance test on the cured potting glue. The test results are shown in Table 1.
[0095] Example 6
[0096] The highly transparent weather-resistant epoxy resin potting glue of this embodiment:
[0097] Including component A and component B:
[0098] The component A comprises the following components in parts by weight: 100 parts of epoxy resin, 30 parts of toughening agent, 0.3 parts of antioxidant, 2 parts of diluent, and 0.3 parts of first defoaming agent;
[0099] The B component includes the following components in parts by mass: 100 parts of curing agent, 1 part of curing accelerator, and 0.3 parts of second defoaming agent;
[0100] The mass ratio of the component A to the component B is 100:50.
[0101] The preparation method of the highly transparent weather-resistant epoxy resin potting glue of this embodiment comprises the following steps:
[0102] S1: 40 parts of epoxy resin E54, 40 parts of hydrogenated bisphenol A epoxy resin, 20 parts of diglycidyl hexahydrophthalate, 30 parts of epoxy resin active toughening agent, 0.3 parts of phosphite antioxidant, 2 parts of 1,4-butanediol diglycidyl ether, and 0.3 parts of BYK-A530 defoamer are added to a reactor, and mechanically stirred and dispersed at a speed of 400 r / min at room temperature. Vacuuming is required during the stirring process. After stirring for 60 minutes, degassing is performed for 30 minutes to obtain component A;
[0103] S2: 50 parts of R3328L, 50 parts of R-2263, 1 part of 1,3-cyclohexanedimethylamine, and 0.3 parts of BYK-A530 were mechanically stirred at a speed of 300 r / min, vacuumed, stirred for 20 minutes, and then degassed to obtain component B;
[0104] S3: After cleaning the polytetrafluoroethylene mold with anhydrous ethanol, wipe the polytetrafluoroethylene mold with a release agent and dry it; start pouring the glue, mix the A and B components at a mass ratio of 100:50 at room temperature, cure at room temperature, and then perform a performance test on the cured potting glue. The test results are shown in Table 1.
[0105] Example 7
[0106] The highly transparent weather-resistant epoxy resin potting glue of this embodiment:
[0107] Including component A and component B:
[0108] The component A comprises the following components in parts by mass: 100 parts of epoxy resin, 10 parts of toughening agent, 0.5 parts of antioxidant, 5 parts of diluent, and 1 part of first defoaming agent;
[0109] The B component includes the following components in parts by mass: 100 parts of curing agent, 10 parts of curing accelerator, and 1 part of second defoaming agent;
[0110] The mass ratio of the component A to the component B is 100:80.
[0111] The preparation method of the highly transparent weather-resistant epoxy resin potting glue of this embodiment comprises the following steps:
[0112] S1: 40 parts of epoxy resin E54, 60 parts of diglycidyl hexahydrophthalate, 10 parts of epoxy resin active toughening agent, 0.5 parts of phosphite antioxidant, 5 parts of 1,4-butanediol diglycidyl ether, and 1 part of BYK-A530 were added to a reactor, and mechanically stirred and dispersed at a speed of 400 r / min at room temperature. Vacuum was required during the stirring process. After stirring for 60 minutes, degassing was performed for 30 minutes to obtain component A;
[0113] S2: 100 parts of R-9030B, 10 parts of 1,3-cyclohexanedimethylamine, and 1 part of BYK-A530 were mechanically stirred at a speed of 300 r / min and vacuumed, and then stirred for 30 minutes and degassed to obtain component B;
[0114] S3: After cleaning the polytetrafluoroethylene mold with anhydrous ethanol, wipe the polytetrafluoroethylene mold with a release agent and dry it; start pouring the glue, mix the A and B components at a mass ratio of 100:80 at room temperature, cure at room temperature, and then perform a performance test on the cured potting glue. The test results are shown in Table 1.
[0115] Example 8
[0116] The highly transparent weather-resistant epoxy resin potting glue of this embodiment:
[0117] Including component A and component B:
[0118] The component A comprises the following components in parts by mass: 100 parts of epoxy resin, 30 parts of toughening agent, 0.3 parts of antioxidant, 1 part of diluent, and 0.1 parts of first defoaming agent;
[0119] The B component includes the following components in parts by mass: 100 parts of curing agent, 1 part of curing accelerator, and 0.1 part of second defoaming agent;
[0120] The mass ratio of the component A to the component B is 100:30.
[0121] The preparation method of the highly transparent weather-resistant epoxy resin potting glue of this embodiment comprises the following steps:
[0122] S1: 40 parts of epoxy resin E54, 60 parts of diglycidyl hexahydrophthalate, 30 parts of epoxy resin active toughening agent, 0.3 parts of phosphite antioxidant, 1 part of 1,4-butanediol diglycidyl ether, and 0.1 parts of BYK-A530 were added to a reactor, and mechanically stirred and dispersed at a speed of 400 r / min at room temperature. Vacuuming was required during the stirring process. After stirring for 60 minutes, degassing was performed for 30 minutes to obtain component A;
[0123] S2: 100 parts of R-9030B, 1 part of 1,3-cyclohexanedimethylamine, and 0.1 part of BYK-A530 were mechanically stirred at a speed of 300 r / min and vacuumed, and then stirred for 30 minutes and degassed to obtain component B;
[0124] S3: After cleaning the polytetrafluoroethylene mold with anhydrous ethanol, wipe the polytetrafluoroethylene mold with a release agent and dry it; start pouring the glue, mix the A and B components at a mass ratio of 100:30 at room temperature, cure at room temperature, and then perform a performance test on the cured potting glue. The test results are shown in Table 1.
[0125] Example 9
[0126] The highly transparent weather-resistant epoxy resin potting glue of this embodiment:
[0127] Including component A and component B:
[0128] The component A comprises the following components in parts by mass: 100 parts of epoxy resin, 20 parts of toughening agent, 0.3 parts of antioxidant, 1 part of diluent, and 0.1 parts of first defoaming agent;
[0129] The B component includes the following components in parts by mass: 100 parts of curing agent, 1 part of curing accelerator, and 0.1 part of second defoaming agent;
[0130] The mass ratio of the component A to the component B is 100:60.
[0131] The preparation method of the highly transparent weather-resistant epoxy resin potting glue of this embodiment comprises the following steps:
[0132] S1: 40 parts of epoxy resin E54, 60 parts of diglycidyl hexahydrophthalate, 20 parts of epoxy resin active toughening agent, 0.3 parts of phosphite antioxidant, 1 part of 1,4-butanediol diglycidyl ether, and 0.1 parts of BYK-A530 were added to a reactor, and mechanically stirred and dispersed at a speed of 400 r / min at room temperature. Vacuuming was required during the stirring process. After stirring for 60 minutes, degassing was performed for 30 minutes to obtain component A;
[0133] S2: 100 parts of R-9030B, 1 part of 1,3-cyclohexanedimethylamine, and 0.1 part of BYK-A530 were mechanically stirred at a speed of 300 r / min and vacuumed, and then stirred for 30 minutes and degassed to obtain component B;
[0134] S3: After cleaning the polytetrafluoroethylene mold with anhydrous ethanol, wipe the polytetrafluoroethylene mold with a release agent and dry it; start pouring the glue, mix the A and B components at a mass ratio of 100:60 at room temperature, cure at room temperature, and then perform a performance test on the cured potting glue. The test results are shown in Table 1.
[0135] Example 10
[0136] The highly transparent weather-resistant epoxy resin potting glue of this embodiment:
[0137] Including component A and component B:
[0138] The component A comprises the following components in parts by mass: 100 parts of epoxy resin, 5 parts of toughening agent, 0.5 parts of antioxidant, 3 parts of diluent, and 0.5 parts of first defoaming agent;
[0139] The B component includes the following components in parts by mass: 100 parts of curing agent, 5 parts of curing accelerator, and 0.5 parts of second defoaming agent;
[0140] The mass ratio of the component A to the component B is 100:40.
[0141] The preparation method of the highly transparent weather-resistant epoxy resin potting glue of this embodiment comprises the following steps:
[0142] S1: 40 parts of epoxy resin E54, 60 parts of diglycidyl hexahydrophthalate, 5 parts of epoxy resin active toughening agent, 0.5 parts of phosphite antioxidant, 3 parts of 1,4-butanediol diglycidyl ether, and 0.5 parts of BYK-A530 were added to a reactor, and mechanically stirred and dispersed at a speed of 400 r / min at room temperature. Vacuuming was required during the stirring process. After stirring for 60 minutes, degassing was performed for 30 minutes to obtain component A;
[0143] S2: 100 parts of R-9030B, 5 parts of 1,3-cyclohexanedimethylamine, and 0.5 parts of BYK-A530 were mechanically stirred at a speed of 300 r / min and vacuumed, and then degassed after stirring for 30 minutes to obtain component B;
[0144] S3: After cleaning the polytetrafluoroethylene mold with anhydrous ethanol, wipe the polytetrafluoroethylene mold with a release agent and dry it; start pouring the glue, mix the A and B components at a mass ratio of 100:40 at room temperature, cure at room temperature, and then perform a performance test on the cured potting glue. The test results are shown in Table 1.
[0145] Embodiment 11
[0146] The highly transparent weather-resistant epoxy resin potting glue of this embodiment:
[0147] Including component A and component B:
[0148] The component A comprises the following components in parts by mass: 100 parts of epoxy resin, 5 parts of toughening agent, 0.3 parts of antioxidant, 2 parts of diluent, and 0.3 parts of first defoaming agent;
[0149] The B component includes the following components in parts by mass: 100 parts of curing agent, 3 parts of curing accelerator, and 0.3 parts of second defoaming agent;
[0150] The mass ratio of the component A to the component B is 100:30.
[0151] The preparation method of the highly transparent weather-resistant epoxy resin potting glue of this embodiment comprises the following steps:
[0152] S1: 40 parts of epoxy resin E54, 60 parts of diglycidyl hexahydrophthalate, 5 parts of epoxy resin active toughening agent, 0.3 parts of phosphite antioxidant, 5 parts of 1,4-butanediol diglycidyl ether, and 0.3 parts of BYK-A530 were added to a reactor, and mechanically stirred and dispersed at a speed of 400 r / min at room temperature. Vacuuming was required during the stirring process. After stirring for 60 minutes, degassing was performed for 30 minutes to obtain component A;
[0153] S2: 100 parts of R-9030B, 3 parts of 1,3-cyclohexanedimethylamine, and 0.3 parts of BYK-A530 were mechanically stirred at a speed of 300 r / min and vacuumed, and then stirred for 30 minutes and degassed to obtain component B;
[0154] S3: After cleaning the polytetrafluoroethylene mold with anhydrous ethanol, wipe the polytetrafluoroethylene mold with a release agent and dry it; start pouring the glue, mix the A and B components at a mass ratio of 100:30 at room temperature, cure at room temperature, and then perform a performance test on the cured potting glue. The test results are shown in Table 1.
[0155] Example 12
[0156] The highly transparent weather-resistant epoxy resin potting glue of this embodiment:
[0157] Including component A and component B:
[0158] The component A comprises the following components in parts by mass: 100 parts of epoxy resin, 5 parts of toughening agent, 0.5 parts of antioxidant, 3 parts of diluent, and 0.3 parts of first defoaming agent;
[0159] The B component includes the following components in parts by mass: 100 parts of curing agent, 3 parts of curing accelerator, and 0.3 parts of second defoaming agent;
[0160] The mass ratio of the component A to the component B is 100:20.
[0161] The preparation method of the highly transparent weather-resistant epoxy resin potting glue of this embodiment comprises the following steps:
[0162] S1: 40 parts of epoxy resin E54, 60 parts of diglycidyl hexahydrophthalate, 5 parts of epoxy resin active toughening agent, 0.5 parts of phosphite antioxidant, 5 parts of 1,4-butanediol diglycidyl ether, and 0.3 parts of BYK-A530 were added to a reactor, and mechanically stirred and dispersed at a speed of 400 r / min at room temperature. Vacuuming was required during the stirring process. After stirring for 60 minutes, degassing was performed for 30 minutes to obtain component A;
[0163] S2: 100 parts of R-9030B, 3 parts of 1,3-cyclohexanedimethylamine, and 0.3 parts of BYK-A530 were mechanically stirred at a speed of 300 r / min and vacuumed, and then stirred for 30 minutes and degassed to obtain component B;
[0164] S3: After cleaning the polytetrafluoroethylene mold with anhydrous ethanol, wipe the polytetrafluoroethylene mold with a release agent and dry it; start pouring the glue, mix the A and B components at a mass ratio of 100:20 at room temperature, cure at room temperature, and then perform a performance test on the cured potting glue. The test results are shown in Table 1.
[0165] Comparative Example 1
[0166] In this comparative example, bisphenol A epoxy resin, bisphenol F epoxy resin, diluent, toughening agent, dispersant, flame retardant, defoaming agent and filler are used as component A, and component B is acid anhydride as curing agent and aromatic tertiary amine as curing accelerator. Components A and B are mixed at room temperature in a mass ratio of 100:50.
[0167] The performance of the highly transparent weather-resistant epoxy resin potting adhesive prepared in Examples 1 to 12 of the present invention was tested, and the test results are shown in Table 1 below:
[0168] In the embodiments of the present invention, the mechanical properties are tested using a MTS universal tensile testing machine in accordance with GB / T2567-2008; the operating time is tested in accordance with GB / T 7123.1-2015; the viscosity is tested in accordance with GB / T 10247-2008 at a temperature of 25°C; the density is tested in accordance with GB / T13354-1992 at a temperature of 25°C; the water absorption is tested in accordance with the industry standard requirements of GB / T1034-2008; the thermal conductivity is tested in accordance with GB / T10297-2015 at a temperature of 25°C; the high and low temperature cycle is tested in accordance with GB / T 2423.22-2012 "Environmental testing Part 2: Test method Test N: Temperature change" test, -40℃ / 8h-85℃ / 8h, and then placed under 95% relative humidity and 85℃ for 24h for testing; aging resistance refers to GB / T2423.24-2022 "Environmental testing Part 2: Test method Test S: Simulated ground solar radiation and solar radiation test and climate aging test guidelines" using KK-SN-150 xenon lamp aging test chamber (85℃, relative humidity RH 85% under hot and humid conditions, irradiated with xenon lamp for 1000h).
[0169] Table 1 Performance test of high transparent weather-resistant epoxy resin potting glue
[0170]
[0171]
[0172] It can be seen from the data in Table 1 that the highly transparent weather-resistant epoxy resin potting adhesive prepared in the present invention has a longer operation time, lower viscosity, better fluidity, excellent thermal conductivity and excellent mechanical properties compared with the comparative example.
[0173] Obviously, the above embodiments are merely examples for the purpose of clear explanation, and are not intended to limit the implementation methods. For those skilled in the art, other different forms of changes or modifications can be made based on the above description. It is not necessary and impossible to list all the implementation methods here. The obvious changes or modifications derived therefrom are still within the scope of protection of the invention.
Claims
1. A highly transparent weather-resistant epoxy resin potting adhesive, characterized in that: Including component A and component B: The component A comprises the following components in parts by mass: 100 parts of epoxy resin, 0-30 parts of toughening agent, 0.3-0.5 parts of antioxidant, 1-5 parts of diluent, and 0.1-1 parts of first defoaming agent; and the toughening agent is not 0; wherein the epoxy resin is a mixture of at least two of bisphenol A epoxy resin, hydrogenated bisphenol A epoxy resin and glycidyl ester epoxy resin; The B component includes the following components in parts by mass: 100 parts of curing agent, 0-10 parts of curing accelerator, and 0.1-1 parts of second defoaming agent; and the curing accelerator is not 0; The mass ratio of the component A to the component B is 100:30-80.
2. The highly transparent weather-resistant epoxy resin potting adhesive according to claim 1, characterized in that: The A component includes the following components in parts by mass: 100 parts of epoxy resin, 0-20 parts of toughening agent, 0.3-0.5 parts of antioxidant, 1-3 parts of diluent, and 0.1-0.5 parts of first defoaming agent; and the toughening agent is not 0; The B component includes the following components in parts by mass: 100 parts of curing agent, 0-5 parts of curing accelerator, and 0.1-0.5 parts of second defoaming agent; and the curing accelerator is not 0; The mass ratio of the component A to the component B is 100:40-60.
3. The highly transparent weather-resistant epoxy resin potting adhesive according to claim 2, characterized in that: The component A comprises the following components in parts by mass: 100 parts of epoxy resin, 10 parts of toughening agent, 0.3 parts of antioxidant, 2 parts of diluent, and 0.3 parts of first defoaming agent; The B component includes the following components in parts by mass: 100 parts of curing agent, 2 parts of curing accelerator, and 0.3 parts of second defoaming agent; The mass ratio of the component A to the component B is 100:
50.
4. The highly transparent weather-resistant epoxy resin potting adhesive according to claim 1, characterized in that: The epoxy resin is a mixture of bisphenol A epoxy resin and glycidyl ester epoxy resin or a mixture of bisphenol A epoxy resin, hydrogenated bisphenol A epoxy resin and glycidyl ester epoxy resin; the epoxy resin comprises: 0-40 parts of bisphenol A epoxy resin; 0-60 parts of hydrogenated bisphenol A epoxy resin; and 20-100 parts of glycidyl ester epoxy resin.
5. The highly transparent weather-resistant epoxy resin potting adhesive according to claim 1, characterized in that: The bisphenol A type epoxy resin is one or a mixture of epoxy resin E44, epoxy resin E51, and epoxy resin E54; The hydrogenated bisphenol A type epoxy resin is one or a mixture of epoxy resin AL3030, epoxy resin AL3040, epoxy resin AL3050; The glycidyl ester epoxy resin is one of diglycidyl phthalate, diglycidyl hexahydrophthalate, diglycidyl terephthalate, diglycidyl isophthalate, diglycidyl tetrahydrophthalate, diglycidyl methyltetrahydrophthalate, diglycidyl endomethyltetrahydrophthalate, and diglycidyl adipic acid, or a mixture of several of them.
6. The highly transparent weather-resistant epoxy resin potting adhesive according to claim 1, characterized in that ; The curing agent is a modified curing agent of alicyclic amines, and the modified curing agent of alicyclic amines is one or a mixture of isophorone diamine, R-2263, R-2270, R-2282, R-9030B, R-3604, R-3328L, and R-5911-8; The curing accelerator is one or a mixture of triethanolamine, 1,3-cyclohexanedimethylamine, triethylamine, benzyldimethylamine, or several thereof; The toughening agent is one or a mixture of core-shell toughening agent, polyurethane toughening agent, carboxyl-terminated liquid nitrile rubber toughening agent and epoxy resin active toughening agent.
7. The highly transparent weather-resistant epoxy resin potting adhesive according to claim 1, characterized in that: The antioxidant is one or a mixture of phosphite antioxidants, hindered phenol antioxidants, thioether antioxidants and sulfur-containing antioxidants; The diluent is one or a mixture of 1,4-butanediol diglycidyl ether, 1,6-hexanediol diglycidyl ether, dipropylene glycol diacrylate and tripropylene glycol diacrylate.
8. The highly transparent weather-resistant epoxy resin potting adhesive according to claim 1, characterized in that: The first defoaming agent is one or a mixture of BYK-A530, BYK-special, BYK-1790, P573, and P990; The second defoamer is one of BYK-A530, BYK-special, BYK-1790, P573, and P990, or a mixture of several thereof.
9. A method for preparing a highly transparent weather-resistant epoxy resin potting adhesive as claimed in any one of claims 1 to 8, characterized in that: The steps include: S1: Mix epoxy resin, toughening agent, antioxidant, diluent and first defoaming agent in proportion to prepare component A; S2: Mix the curing agent, curing accelerator and second defoaming agent in proportion to prepare component B; S3: Mixing component A and component B to obtain the highly transparent weather-resistant epoxy resin potting adhesive.
10. The method for preparing the highly transparent weather-resistant epoxy resin potting adhesive according to claim 9, characterized in that: The step S1 specifically comprises the following steps: adding the epoxy resin, the toughening agent, the antioxidant, the diluent, and the first defoaming agent into a reaction kettle in proportion, mechanically stirring and dispersing at a speed of 400 r / min, and vacuuming during the stirring process; stirring for 60 minutes, and degassing for 30 minutes after sufficient stirring to obtain the component A; The step S2 specifically includes the following steps: adding the curing agent, the curing accelerator and the second defoaming agent into a reaction kettle in proportion, mechanically stirring and dispersing at a speed of 300 r / min, and vacuuming during the stirring process; stirring for 30 minutes, and degassing for 10 minutes after sufficient stirring to obtain the B component.
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