A low-viscosity, high and low temperature resistant epoxy potting adhesive and its preparation method

Abstract

The present invention relates to the technical field of epoxy potting adhesives, in particular to the IPC C09J163 field. Further, it relates to a low-viscosity, high and low temperature resistant epoxy potting adhesive and a preparation method thereof. It includes component A and component B; the component A, by weight, comprises the following raw materials: 60-120 parts of epoxy resin, 20-100 parts of filler, 5-10 parts of toughening agent, 1-5 parts of reactive diluent, 1-5 parts of thixotropic agent, 0-2 parts of coupling agent, 0-1 part of auxiliary agent; the component B, by weight, comprises the following raw materials: 80-100 parts of polyetheramine, 10-20 parts of aromatic amine, 10-20 parts of phenolic amine. The present invention selects specific epoxy resin to act together with polyetheramine, aromatic amine and phenolic amine to achieve the advantages of low viscosity, good bonding performance and excellent high and low temperature impact resistance of the epoxy potting adhesive.

Description

Technical Field

[0001] The present invention relates to the technical field of epoxy potting adhesives, in particular to the IPC C09J163 field. Further, it relates to a low-viscosity, high and low temperature resistant epoxy potting adhesive and a preparation method thereof. Background Art

[0002] Potting adhesives are used for bonding, sealing, potting and coating protection of electronic components. Since the cavities to be potted are sometimes narrow, the potting adhesive needs to fill all the gaps in the sandwich without bubbles and voids. Therefore, the potting adhesive must have very good fluidity. Potting adhesives can not only play the roles of moisture-proof, corrosion-proof and shock-proof, but also improve the performance and stability of electronic components. Epoxy resins have high strength and excellent adhesion performance. Epoxy potting adhesives prepared from epoxy resins have also been widely used. Epoxy potting adhesives have excellent high-temperature resistance and electrical insulation properties. However, the epoxy potting adhesives have poor resistance to thermal shock. Cracks are easily generated after being subjected to thermal shock, resulting in water vapor seeping into the electronic components from the cracks, poor moisture-proof ability, and the cured colloid has high hardness and brittleness, and is easy to strain the electronic components.

[0003] Chinese Patent CN 112694856B discloses a two-component epoxy potting adhesive, including A and B components. The A component includes a modified epoxy resin, a diluent and a thermal conductive filler. The B component includes a curing agent and a curing accelerator. The raw materials of the modified epoxy resin include an epoxy resin matrix, a vinyl monomer containing an ester group, and a hydrophobic hexagonal boron nitride nanosheet containing a vinyl group. The modified epoxy resin is prepared by a polymerization reaction of the epoxy resin matrix and the remaining raw materials, and the boron nitride nanosheet is prepared by a specific method: surface hydroxyl modification, freeze-thaw expansion treatment, and then combined with a one-pot method of a specific compound for exfoliation and

[0004] esterification modification catalysis; the potting adhesive of the invention can have the properties of low viscosity, good flow permeability, high thermal conductivity, low linear expansion coefficient, high heat resistance, etc. on the basis of excellent electrical and mechanical properties. However, this technical solution is relatively complex, and it is not clear how its high and low temperature shock resistance is. Summary of the Invention

[0005] To solve the above technical problems, the first aspect of the present invention provides a low-viscosity, high and low temperature resistant epoxy potting adhesive, including A component and B component; the A component, by weight, includes the following raw materials: 60-120 parts of epoxy resin, 20-100 parts of filler, 5-10 parts of toughening agent, 1-5 parts of active diluent, 1-5 parts of thixotropic agent, 0-2 parts of coupling agent, 0-1 part of auxiliary agent; the B component, by weight, includes the following raw materials: 80-100 parts of polyetheramine, 10-20 parts of aromatic amine, 10-20 parts of phenolic amine.

[0006] In some preferred embodiments, the weight ratio of component A to component B is (3 - 7):1.

[0007] In some preferred embodiments, the epoxy resin is selected from one or more combinations of bisphenol A epoxy resin, alicyclic epoxy resin, glycidyl ester epoxy resin, and glycidylamine epoxy resin.

[0008] Preferably, the epoxy resin is selected from the combination of bisphenol A epoxy resin and alicyclic epoxy resin.

[0009] Preferably, the weight ratio of bisphenol A epoxy resin to alicyclic epoxy resin is (4 - 8):1.

[0010] Preferably, the epoxy equivalent of the bisphenol A epoxy resin is 100 - 250 g / eq.

[0011] Preferably, the epoxy equivalent of the bisphenol A epoxy resin is 150 - 200 g / eq.

[0012] Preferably, the epoxy equivalent of the alicyclic epoxy resin is 80 - 150 g / eq.

[0013] Preferably, the epoxy equivalent of the alicyclic epoxy resin is 100 - 130 g / eq.

[0014] Preferably, the alicyclic epoxy resin is selected from one or more combinations of diglycidyl 4,5-epoxyhexane-1,2-dicarboxylate, diglycidyl cyclohexane-1,2-dicarboxylate, 3,4-epoxycyclohexylmethyl 3,4-epoxycyclohexanecarboxylate, bis(7-oxabicyclo[4.1.0]heptan-3-ylmethyl) adipate, and 1,4-cyclohexanedimethanol bis(3,4-epoxycyclohexanecarboxylate).

[0015] Preferably, the alicyclic epoxy resin is diglycidyl 4,5-epoxyhexane-1,2-dicarboxylate.

[0016] In the present invention, when the epoxy resin is selected from the combination of bisphenol A epoxy resin and alicyclic epoxy resin, and the weight ratio of bisphenol A epoxy resin to alicyclic epoxy resin is controlled to be (5-10):1, the bonding strength and mechanical properties of the epoxy potting adhesive can be effectively improved. Since the epoxy groups of the alicyclic epoxy resin are directly connected to the alicyclic ring, a tight rigid molecular structure can be formed. After introducing the alicyclic epoxy resin into the system, the crosslinking density of the cured epoxy potting adhesive is large, thereby improving the bonding strength and tensile strength of the epoxy potting adhesive. However, when the addition amount of the alicyclic epoxy resin exceeds this ratio, the introduction of excessive rigid molecules will cause the crosslinking density of the cured epoxy potting adhesive to be too large, increasing brittleness and reducing the bonding strength and mechanical properties. The inventor of the present invention found that when the epoxy equivalent of bisphenol A epoxy resin is 150-200 g / eq and the alicyclic epoxy resin is diglycidyl 4,5-epoxyhexane-1,2-dicarboxylate, the high and low temperature impact resistance of the epoxy potting adhesive can be significantly improved. The inventor of the present invention guesses that: due to the small viscosity of diglycidyl 4,5-epoxyhexane-1,2-dicarboxylate, and its molecular structure contains both alicyclic epoxy groups and glycidyl ester groups, having the dual characteristics of alicyclic epoxy and glycidyl ester. On the one hand, it has cyclohexyl groups that can absorb the impact energy, and on the other hand, it has a greater reactivity compared to other types of alicyclic epoxy resins, has a stronger interaction effect with bisphenol A epoxy resin with an epoxy equivalent of 150-200 g / eq, and also has good compatibility with the fillers in the system. When crosslinking occurs, it can reduce the curing shrinkage and the internal stress of shrinkage, thereby improving the high and low impact resistance.

[0017] In some preferred embodiments, the filler is selected from one or more combinations of barium sulfate fine powder, silica fine powder, alumina fine powder, and calcium carbonate fine powder.

[0018] Preferably, the filler is selected from the combination of barium sulfate fine powder, calcium carbonate fine powder, and silica fine powder.

[0019] Preferably, the weight ratio of barium sulfate fine powder, calcium carbonate fine powder, and silica fine powder is (1-3):(1-3):(1-3).

[0020] Preferably, the particle size of the barium sulfate fine powder is 1-4 μm.

[0021] Preferably, the mesh number of the calcium carbonate fine powder is 500-1000 mesh.

[0022] Preferably, the silica fine powder is irregular-shaped silica fine powder.

[0023] Preferably, the mesh number of the silica fine powder is 500-1000 mesh.

[0024] Preferably, the filler is modified, and the modification method of the filler is:

[0025] (1)Disperse silica powder in water, add hydroxymethyl cellulose, and perform ball milling for 3 - 5 h. Then filter and dry to obtain modified silica powder;

[0026] (2)Mix barium sulfate micropowder and calcium carbonate micropowder evenly with 50 wt% ethanol solution. Slowly drop silane coupling agent at 60 - 90 °C, control the dropping time to be 0.5 - 1 h. After dropping, continue stirring for 30 - 60 min, add the modified silica powder, and continue reacting for 1 - 3 h. Finally, obtain the modified filler through centrifugation and drying.

[0027] Preferably, the weight ratio of the silica powder, water, and hydroxymethyl cellulose is (10 - 15):(300 - 400):1.

[0028] Preferably, the weight parts of the barium sulfate micropowder, calcium carbonate micropowder, ethanol, and silane coupling agent are (1 - 3):(1 - 3):(5 - 10):(0.02 - 0.08).

[0029] Preferably, the silane coupling agent is vinyltrimethylsilane.

[0030] In the present invention, by selecting barium sulfate micropowder and barium carbonate micropowder with different particle sizes and silica powder with irregular shapes, and modifying the filler, while improving the high and low temperature resistance of the epoxy potting adhesive, the viscosity of the epoxy potting adhesive is significantly reduced. The inventor guesses that: the modified small - particle - size filler is more likely to fill the voids of the large - particle - size filler, and the irregular - shaped silica powder can combine more closely with barium sulfate micropowder and calcium carbonate micropowder, making the filler easier to disperse evenly in the system, improving the compatibility, thereby reducing the viscosity of the epoxy potting adhesive and improving the high and low temperature resistance of the epoxy potting adhesive; at the same time, by modifying the filler, the filler is not easy to settle and agglomerate, and the storage stability of the epoxy potting adhesive is good.

[0031] In some preferred embodiments, the toughening agent is selected from the Kane Ace MX series products of Japan's Kaneka Corporation.

[0032] In some preferred embodiments, the active diluent is selected from one or more combinations of C12 - 14 alkyl glycidyl ether, n - butyl glycidyl ether, ethylene glycol diglycidyl ether, benzyl glycidyl ether, 1,4 - butanediol diglycidyl ether.

[0033] In some preferred embodiments, the thixotropic agent is selected from one or more combinations of fumed silica, organic bentonite, and nanoscale calcium carbonate.

[0034] Preferably, the thixotropic agent is a combination of fumed silica and organic bentonite.

[0035] Preferably, the weight ratio of the fumed silica to the organobentonite is (1-3):(1-3).

[0036] Preferably, the specific surface area of the fumed silica is 200-500 m 2 / g.

[0037] Preferably, the organobentonite is any one of TY-118, TY-138, TY-108, and TY-188 produced by Anji Tianyu Bentonite Co., Ltd.

[0038] In some preferred embodiments, the coupling agent is selected from silane coupling agents or carbonate coupling agents.

[0039] In some preferred embodiments, the additives include a dispersant, an antifoaming agent, and an adhesion promoter.

[0040] In some preferred embodiments, the weight ratio of the dispersant, the antifoaming agent, and the adhesion promoter is (0.8-1.2):(0.8-1.2):(0.5-1).

[0041] Preferably, the dispersant is a modified siloxane dispersant.

[0042] Preferably, the antifoaming agent is an organosilicon antifoaming agent.

[0043] In some preferred embodiments, the weight ratio of the polyetheramine, the aromatic amine, and the phenolic amine is (5-7):1:1.

[0044] In some preferred embodiments, the polyetheramine is a binary polyetheramine.

[0045] Preferably, the number average molecular weight of the binary polyetheramine is 200-500.

[0046] In some preferred embodiments, the amine value of the aromatic amine is 200-300 mgKOH / g.

[0047] In some preferred embodiments, the viscosity of the phenolic amine is 3000-5000 cps (25°C).

[0048] In the present invention, by selecting a binary etheramine, an aromatic amine, and a phenolic amine compounded as a curing agent and controlling the weight ratio of the polyetheramine, the aromatic amine, and the phenolic amine to be (5-7):1:1, and acting together with the epoxy resin in the system, the advantages of the epoxy potting adhesive with low viscosity, good bonding performance, and excellent high and low temperature impact resistance are further realized.

[0049] On the other hand, the present invention provides a method for preparing a low-viscosity, high and low temperature resistant epoxy potting adhesive, comprising the following steps:

[0050] (1) Preparation of Component A: By weight, epoxy resin, filler, toughening agent, reactive diluent, thixotropic agent, coupling agent, and additives are stirred and mixed. After mixing evenly, vacuum degassing is carried out.

[0051] (2) Preparation of Component B: By weight, polyetheramine, aromatic amine, and phenolic amine are stirred and mixed evenly.

[0052] (3) Component A and Component B are stirred and mixed evenly to obtain the product.

[0053] Beneficial effects:

[0054] 1. In the present invention, a combination of bisphenol A epoxy resin and alicyclic epoxy resin is selected for the epoxy resin, and the weight ratio of bisphenol A epoxy resin to alicyclic epoxy resin is controlled to be (5 - 10):1. Since the epoxy groups of the alicyclic epoxy resin are directly connected to the alicyclic ring, a tight rigid molecular structure can be formed. After introducing the alicyclic epoxy resin into the system, the crosslinking density of the epoxy potting adhesive after curing is large, thereby improving the bonding strength and tensile strength of the epoxy potting adhesive.

[0055] 2. In the present invention, bisphenol A epoxy resin with an epoxy equivalent of 150 - 200 g / eq and 4,5-epoxyhexane-1,2-dicarboxylic acid diglycidyl ester are selected as the alicyclic epoxy resin. Since 4,5-epoxyhexane-1,2-dicarboxylic acid diglycidyl ester has a relatively low viscosity and contains both alicyclic epoxy groups and glycidyl ester groups in its molecular structure, having the dual characteristics of alicyclic epoxy and glycidyl ester. On the one hand, it has cyclohexyl groups that can absorb impact energy, and on the other hand, it has a greater reaction activity compared to other types of alicyclic epoxy resins, has a stronger interaction effect with bisphenol A epoxy resin with an epoxy equivalent of 150 - 200 g / eq, and also has good compatibility with the filler in the system. When crosslinking occurs, it can reduce the curing shrinkage and the internal stress of shrinkage, thereby improving the high and low impact resistance.

[0056] 3. In the present invention, a binary ether amine, aromatic amine, and phenolic amine are selected and compounded as the curing agent, and the weight ratio of polyetheramine, aromatic amine, and phenolic amine is controlled to be (5 - 7):1:1. Acting together with the epoxy resin in the system, it further realizes the advantages of the epoxy potting adhesive having low viscosity, good bonding performance, and excellent high and low temperature impact resistance.

[0057] 4. In the present invention, by selecting barium sulfate fine powder, barium carbonate fine powder with different particle sizes, and irregularly shaped silicon fine powder, and modifying the filler, the modified small particle size filler is more likely to fill the voids of the large particle size filler, and the irregularly shaped silicon fine powder can be combined more tightly with the barium sulfate fine powder and the barium carbonate fine powder, making it easier for the filler to be evenly dispersed in the system, improving the compatibility, and further reducing the viscosity of the epoxy potting adhesive and enhancing the high and low temperature resistance of the epoxy potting adhesive; at the same time, by modifying the filler, the filler is not prone to sedimentation and caking, and the storage stability of the epoxy potting adhesive is good. Detailed implementation mode

[0058] Example 1

[0059] Example 1 provides a low-viscosity, high and low temperature resistant epoxy potting adhesive, which includes component A and component B; the component A, by weight, includes the following raw materials: 100 parts of epoxy resin, 60 parts of filler, 8 parts of toughening agent, 4 parts of active diluent, 3 parts of thixotropic agent, 1 part of coupling agent, and 1 part of auxiliary agent; the component B, by weight, includes the following raw materials: 90 parts of polyetheramine, 15 parts of aromatic amine, and 15 parts of phenolic amine.

[0060] The weight ratio of the component A to the component B is 5:1.

[0061] The epoxy resin is selected from the combination of bisphenol A epoxy resin and alicyclic epoxy resin.

[0062] The weight ratio of the bisphenol A epoxy resin to the alicyclic epoxy resin is 6:1.

[0063] The epoxy equivalent of the bisphenol A epoxy resin is 182 - 192 g / eq, which is Dow DER331 epoxy resin.

[0064] The epoxy equivalent of the alicyclic epoxy resin is 100 - 111 g / eq.

[0065] The alicyclic epoxy resin is 4,5-epoxyhexane-1,2-dicarboxylic acid diglycidyl ester, model: MF-3286.

[0066] The filler is selected from the combination of barium sulfate fine powder, calcium carbonate fine powder, and silicon fine powder.

[0067] The weight ratio of the barium sulfate fine powder, calcium carbonate fine powder, and silicon fine powder is 2:1:1.

[0068] The particle size of the barium sulfate fine powder is 2.5 μm, purchased from Guizhou Haowei Powder Industry Co., Ltd., model: 10AB.

[0069] The mesh number of the calcium carbonate fine powder is 800 mesh, purchased from Guangxi Xincai Mining Co., Ltd.

[0070] The silica powder is irregularly shaped silica powder.

[0071] The silica powder has a mesh number of 800 mesh and is purchased from Anmi Micro-Nano New Materials Co., Ltd., model: H032.

[0072] Modify the filler. The modification method of the filler is as follows:

[0073] (1) Disperse the silica powder in water, add carboxymethyl cellulose, and perform ball milling for 4 hours. Filter and dry to obtain modified silica powder;

[0074] (2) Mix barium sulfate micropowder and calcium carbonate micropowder evenly with a 50 wt% ethanol solution. Slowly drop the silane coupling agent at 70 °C, control the dropping time to be 1 hour. After the dropping is completed, continue stirring for 40 minutes. Add the modified silica powder and continue to react for 2 hours. Finally, obtain the modified filler through centrifugation and drying.

[0075] The weight ratio of the silica powder, water, and carboxymethyl cellulose is 12:350:1.

[0076] The weight parts of the barium sulfate micropowder, calcium carbonate micropowder, ethanol, and silane coupling agent are 2:1:8:0.05.

[0077] The silane coupling agent is vinyltrimethylsilane.

[0078] The toughening agent is Kane Ace MX 154 from Kaneka Corporation, Japan.

[0079] The active diluent is C12-14 alkyl glycidyl ether.

[0080] The thixotropic agent is a combination of fumed silica and organobentonite.

[0081] The weight ratio of the fumed silica and organobentonite is 2:1.

[0082] The specific surface area of the fumed silica is 380 ± 30 m 2 / g, and it is Degussa fumed silica AEROSIL380.

[0083] The organobentonite is purchased from Anji Tianyu Bentonite Co., Ltd., model: TY-118.

[0084] The coupling agent is KH560.

[0085] The auxiliary agents include a dispersant, an antifoaming agent, and an adhesion promoter.

[0086] The weight ratio of the dispersant, antifoaming agent, and adhesion promoter is 1:1:0.8.

[0087] The dispersant is Evonik TEGOPREN 7008.

[0088] The defoamer is BYK-070 of BYK.

[0089] The adhesion promoter is BYK-4511 of BYK.

[0090] The polyetheramine is a binary polyetheramine.

[0091] The number-average molecular weight of the binary polyetheramine is 400, which is Huntsman D-400 from the United States.

[0092] The amine value of the aromatic amine is 280±20 mgKOH / g, purchased from Guangzhou Jiegao Chemical Trading Co., Ltd., model: J-3113.

[0093] The viscosity of the phenolic amine is 3350 cps (25°C).

[0094] A preparation method of a low-viscosity, high and low temperature resistant epoxy potting adhesive, comprising the following steps:

[0095] (1) Prepare component A: By weight, mix epoxy resin, filler, toughening agent, active diluent, thixotropic agent, coupling agent, and auxiliary agent, and after mixing evenly, carry out vacuum degassing;

[0096] (2) Prepare component B: By weight, mix polyetheramine, aromatic amine, and phenolic amine evenly;

[0097] (3) Stir and mix component A and component B evenly to obtain the product.

[0098] Example 2

[0099] Example 2 provides a low-viscosity, high and low temperature resistant epoxy potting adhesive as provided in Example 1, including component A and component B; the component A, by weight, includes the following raw materials: 90 parts of epoxy resin, 80 parts of filler, 7 parts of toughening agent, 4 parts of active diluent, 3 parts of thixotropic agent, 1 part of coupling agent, and 1 part of auxiliary agent; the component B, by weight, includes the following raw materials: 80 parts of polyetheramine, 16 parts of aromatic amine, and 16 parts of phenolic amine.

[0100] The weight ratio of component A and component B is 5:1.

[0101] The epoxy resin is selected from the combination of bisphenol A epoxy resin and alicyclic epoxy resin.

[0102] The weight ratio of bisphenol A epoxy resin and alicyclic epoxy resin is 6:1.

[0103] The epoxy equivalent of the bisphenol A epoxy resin is 182~192 g / eq, which is Dow DER331 epoxy resin.

[0104] The epoxy equivalent of the alicyclic epoxy resin is 100-111 g / eq.

[0105] The alicyclic epoxy resin is diglycidyl 4,5-epoxyhexane-1,2-dicarboxylate, model: MF-3286.

[0106] The filler is selected from the combination of barium sulfate fine powder, calcium carbonate fine powder and silicon fine powder.

[0107] The weight ratio of the barium sulfate fine powder, calcium carbonate fine powder and silicon fine powder is 2:1:1.

[0108] The particle size of the barium sulfate fine powder is 2.5 μm, purchased from Guizhou Nanometer Powder Industry Co., Ltd., model: 10AB.

[0109] The mesh number of the calcium carbonate fine powder is 800 mesh, purchased from Guangxi Xincai Mining Co., Ltd.

[0110] The silicon fine powder is irregularly shaped silicon fine powder.

[0111] The mesh number of the silicon fine powder is 800 mesh, purchased from Anmi Micro-Nano New Materials Co., Ltd., model: H032.

[0112] The filler is modified, and the modification method of the filler is as follows:

[0113] (1) Disperse the silicon fine powder in water, add carboxymethyl cellulose, carry out ball milling for 4 h, filter and dry to obtain modified silicon fine powder;

[0114] (2) Mix the barium sulfate fine powder and calcium carbonate fine powder evenly with a 50 wt% ethanol solution, slowly drop the silane coupling agent at 70 °C, control the dropping time to be 1 h, continue stirring for 40 min after dropping, add the modified silicon fine powder, continue to react for 2 h, and finally obtain the modified filler through centrifugation and drying.

[0115] The weight ratio of the silicon fine powder, water and carboxymethyl cellulose is 12:350:1.

[0116] The weight parts of the barium sulfate fine powder, calcium carbonate fine powder, ethanol and silane coupling agent are 2:1:8:0.05.

[0117] The silane coupling agent is vinyltrimethylsilane.

[0118] The toughening agent is Kane Ace MX 154 of Japan's Kaneka Corporation.

[0119] The active diluent is C12-14 alkyl glycidyl ether.

[0120] The thixotropic agent is a combination of fumed silica and organic bentonite.

[0121] The weight ratio of the fumed silica and the organobentonite is 2:1.

[0122] The specific surface area of the fumed silica is 380±30 m 2 / g, and it is Degussa fumed silica AEROSIL 380.

[0123] The organobentonite is purchased from Anji Tianyu Bentonite Co., Ltd., model: TY-118.

[0124] The coupling agent is KH560.

[0125] The auxiliary agents include a dispersant, an antifoaming agent and an adhesion promoter.

[0126] The weight ratio of the dispersant, the antifoaming agent and the adhesion promoter is 1:1:0.8.

[0127] The dispersant is Evonik TEGOPREN 7008.

[0128] The antifoaming agent is BYK-070 of BYK.

[0129] The adhesion promoter is BYK-4511 of BYK.

[0130] The polyetheramine is a binary polyetheramine.

[0131] The number-average molecular weight of the binary polyetheramine is 400, and it is Huntsman D-400 from the United States.

[0132] The amine value of the aromatic amine is 280±20 mgKOH / g, and it is purchased from Guangzhou Jiegao Chemical Trading Co., Ltd., model J-3113.

[0133] The viscosity of the phenolic amine is 3350 cps (25°C).

[0134] A preparation method of a low-viscosity, high and low temperature resistant epoxy potting adhesive comprises the following steps:

[0135] (1) Prepare component A: By weight, mix epoxy resin, filler, toughening agent, active diluent, thixotropic agent, coupling agent and auxiliary agent, and after mixing evenly, carry out vacuum degassing;

[0136] (2) Prepare component B: By weight, mix polyetheramine, aromatic amine and phenolic amine evenly;

[0137] (3) Mix component A and component B evenly to obtain the product.

[0138] Example 3

[0139] Example 3 provides a low-viscosity, high and low temperature resistant epoxy potting adhesive. Its specific implementation is the same as that of Example 1, except that the weight ratio of bisphenol A epoxy resin to alicyclic epoxy resin is 4:1.

[0140] Example 4

[0141] Example 4 provides a low-viscosity, high and low temperature resistant epoxy potting adhesive. Its specific implementation is the same as that of Example 1, except that Dow DER331 epoxy resin is replaced by Hexion EPIKOTE862.

[0142] Example 5

[0143] Example 5 provides a low-viscosity, high and low temperature resistant epoxy potting adhesive. Its specific implementation is the same as that of Example 1, except that 4,5-epoxyhexane-1,2-dicarboxylic acid diglycidyl ester is replaced by 3,4-epoxycyclohexylmethyl 3,4-epoxycyclohexanecarboxylate.

[0144] Example 6

[0145] Example 6 provides a low-viscosity, high and low temperature resistant epoxy potting adhesive. Its specific implementation is the same as that of Example 1, except that the B component includes the following raw materials by weight: 60 parts of aromatic amine and 60 parts of phenolic amine.

[0146] Example 7

[0147] Example 7 provides a low-viscosity, high and low temperature resistant epoxy potting adhesive. Its specific implementation is the same as that of Example 1, except that the filler is not modified.

[0148] Performance test:

[0149] Mix the A component and B component prepared in Examples 1-7 evenly, evacuate (vacuum degree ≤ -0.09 MPa) for 15 min, prepare corresponding specimens according to the test standard, and let them stand and cure at 23 °C for 7 d.

[0150] 1. Viscosity: Test according to the GB / T22235-2008 standard using a rotary digital viscometer NDJ 4S at 23 °C.

[0151] 2. Density: Test according to the drainage method in the GB / T1033.1-2008 standard at 23 °C.

[0152] 3. Steel-steel shear strength: Test according to the GB / T 7124-2008 standard using a universal tensile testing machine CMT4202 at 23 °C.

[0153] 4. Hardness: Refer to the GB / T 2411 standard and use a Type D durometer to test the surface hardness of the colloid.

[0154] 5. Surface flatness: Pour the glue solution into a disposable cup and check the surface flatness and the absence of bubbles after 24 hours of curing.

[0155] 6. High and low temperature shock performance: Pour the glue solution into a mold box (substrate galvanized sheet, cylinder with a diameter of 80 mm and a depth of 40 mm). After the glue solution is completely cured, conduct a high and low temperature shock performance test and observe whether there is delamination, cracking, color change at the contact surface between the colloid and the substrate box, and the change in hardness.

[0156] The test conditions are: high temperature 150 °C × 4 h + low temperature -45 °C × 4 h as one cycle, continuously cycle 125 times, for a total of 1000 h:

[0157] Test results:

[0158] Table 1

[0159]

Claims

1. A low-viscosity, high and low temperature resistant epoxy potting adhesive, characterized in that, It includes Component A and Component B; The Component A, by weight parts, includes the following raw materials: 60 - 120 parts of epoxy resin, 20 - 100 parts of filler, 5 - 10 parts of toughening agent, 1 - 5 parts of reactive diluent, 1 - 5 parts of thixotropic agent, 0 - 2 parts of coupling agent, 0 - 1 part of auxiliary agent; The Component B, by weight parts, includes the following raw materials: 80 - 100 parts of polyetheramine, 10 - 20 parts of aromatic amine, 10 - 20 parts of phenolic amine; The epoxy resin is bisphenol A epoxy resin and alicyclic epoxy resin, and the weight ratio of bisphenol A epoxy resin to alicyclic epoxy resin is (4 - 8):

1. The epoxy equivalent of bisphenol A epoxy resin is 100 - 250 g / eq, and the epoxy equivalent of alicyclic epoxy resin is 80 - 150 g / eq; The alicyclic epoxy resin is selected from one or a combination of more than one of diglycidyl 4,5-epoxyhexane-1,2-dicarboxylate, diglycidyl cyclohexane-1,2-dicarboxylate, 3,4-epoxycyclohexylmethyl 3,4-epoxycyclohexanecarboxylate, bis(7-oxabicyclo[4.1.0]hept-3-ylmethyl) adipate, 1,4-cyclohexanedimethanol bis(3,4-epoxycyclohexanecarboxylate); The filler includes barium sulfate fine powder, calcium carbonate fine powder and silicon fine powder, and the weight ratio of barium sulfate fine powder, calcium carbonate fine powder and silicon fine powder is (1 - 3):(1 - 3):(1 - 3); The modification method of the filler is as follows: (1) Disperse the silicon fine powder in water, add carboxymethyl cellulose, and carry out ball milling for 3 - 5 h, then filter and dry to obtain modified silicon fine powder; (2) Mix the barium sulfate fine powder and calcium carbonate fine powder evenly with 50 wt% ethanol solution, slowly dropwise add a silane coupling agent at 60 - 90 °C, control the dropping time to be 0.5 - 1 h, continue stirring for 30 - 60 min after dropping, add the modified silicon fine powder, continue to react for 1 - 3 h, and finally obtain the modified filler through centrifugation and drying; The weight ratio of the silicon fine powder, water and carboxymethyl cellulose is (10 - 15):(300 - 400):

1.

2. A low-viscosity, high and low temperature resistant epoxy potting adhesive according to claim 1, characterized in that, The weight ratio of the polyetheramine, aromatic amine and phenolic amine is (5 - 7):1:

1.

3. A preparation method of the low-viscosity, high and low temperature resistant epoxy potting adhesive according to any one of claims 1 to 2, characterized in that, It includes the following steps: (1) Prepare Component A: By weight parts, stir and mix the epoxy resin, filler, toughening agent, reactive diluent, thixotropic agent, coupling agent and auxiliary agent, and carry out vacuum degassing after mixing evenly; (2) Prepare Component B: By weight parts, stir and mix the polyetheramine, aromatic amine and phenolic amine evenly; (3) Stir and mix Component A and Component B evenly to obtain the product.

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