Type-C male connector epoxy pouring sealant and preparation method thereof

The organic fluorine modified epoxy derivatives prepared by reactions of sulfoxide chloride, fluorine-containing biphenyldicarboxylic acid and epoxy propyl alcohol were solved by combining other components. Epoxy filling in Type-C male connectors was solved The problem of poor high temperature resistance performance of glue has achieved improvements in high temperature stability and airtightness, preventing pollutants from entering.

CN119264851APending Publication Date: 2025-01-07QINGDAO DEJU BONDING TECH CO LTD
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Patent Information

Application Number
CN202411587002.5
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-11-08
Publication Date
2025-01-07

AI Technical Summary

Technical Problem

When dispensing and filling the Type-C male connector before and after the solder joint, the commonly used UV glue or epoxy glue has incomplete curing, poor high temperature resistance, and cracks, drumming, and poor airtightness after over-reflow soldering. The problem.

Method used

Using organic fluorine modified epoxy derivatives prepared by reaction with sulfoxide chloride, fluorine-containing biphenyl dicarboxylic acid and epoxy propyl alcohol as raw materials, the epoxy potting glue is improved by introducing fluorine atoms and biphenyl structures. Heat resistance, combined with toughening agent, diluent, coupling agent, curing accelerator and other components, an epoxy potting adhesive with excellent high temperature resistance is prepared.

Benefits of technology

It improves the heat resistance of epoxy potting glue, ensures the stability and airtightness of the connector under high temperature conditions, effectively prevents moisture, dust and other external pollutants from entering, and extends the service life.

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Abstract

The invention provides an epoxy pouring sealant for a Type-C male connector and a preparation method of the epoxy pouring sealant. The epoxy pouring sealant for the Type-C male connector comprises the following raw materials in parts by weight: 30-35 parts of epoxy resin, 10-20 parts of an organic fluorine modified epoxy derivative, 5-10 parts of a toughening agent, 5-10 parts of a reactive diluent, 0.5-3 parts of a coupling agent, 8-12 parts of a latent curing agent, 3-5 parts of a curing accelerator, 30-40 parts of filler and 1-3 parts of a thixotropic agent. The structural formula of the organic fluorine modified epoxy derivative is as shown in formula I in the specification. The raw materials of the epoxy pouring sealant for the Type-C male connector comprise the organic fluorine modified epoxy derivative prepared by reacting thionyl chloride, fluorine-containing biphenyl dicarboxylic acid and glycidol, and the organic fluorine modified epoxy derivative has excellent heat resistance by introducing fluorine atoms and biphenyl structures, so that the heat resistance of the epoxy pouring sealant is improved.
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Description

Technical Field

[0001] The present invention belongs to the technical field of epoxy potting adhesives, and in particular relates to an epoxy potting adhesive for a Type-C male connector and a preparation method thereof. Background Art

[0002] Type-C (USB Type-C, also known as USB-C) is a connection interface of the USB interface. It has the advantages of fast transmission speed (theoretical transmission speed can reach 10Gbps), no difference between forward and reverse insertion, slim body (8.3*2.5cm), strong power supply capacity, strong expandability (it can transmit audio and video signals and expand into a variety of audio and video output interfaces, such as HDMI, VGA, DVI interfaces), etc., and is being used in more and more electronic products.

[0003] The Type-C male connector can define up to 24 leads, which means that so many solder joints and wires need to be arranged in a small space. In the subsequent processing, solder joints are easily desoldered and wires are short-circuited. Therefore, glue potting before and after the solder joints becomes a necessary choice. The glue type usually chooses UV glue or epoxy glue, such as the one disclosed in patent CN115537128B for USB A high elastic sealing adhesive for Type-C connector and a preparation method thereof, which uses polyurethane modified acrylate oligomer as the main polymer and is supplemented with UV-curable components such as active diluent monomers; Patent CN115181523B discloses a low-temperature fast-curing adhesive for protecting the male head of a Type-C connector and a preparation method thereof, which includes the following components by mass fraction: 35%-45% epoxy resin, 5%-15% curing agent, 0.5%-4% accelerator, 28%-40% filler, 0.1%-0.8% color glue, and 10%-20% diluent; the epoxy resin includes: one or more of hydrogenated bisphenol A epoxy resin, p-aminophenol epoxy resin, diglycidyl ether of p-hydroxybenzoic acid, and dicyclopentadiene phenol type epoxy resin.

[0004] The above are common UV glue and epoxy glue that can be used for lead solder joint protection. Since there are a lot of narrow gaps between leads and between leads and shells, in order to prevent external pollutants such as moisture and dust from entering the connector, potting glue also needs to be used to pot these narrow gaps. However, some gaps cannot be irradiated by ultraviolet light. If UV glue is used, it will not be fully cured, and UV glue is not suitable. If epoxy glue is used, there are problems such as poor high temperature resistance, cracks and bulging after reflow soldering, and poor air tightness. Therefore, it is necessary to improve the epoxy glue to obtain an epoxy potting glue with excellent high temperature resistance and suitable for Type-C male connectors. Summary of the invention

[0005] In order to solve the above technical problems, the present invention provides a Type-C male connector epoxy potting glue and a preparation method thereof, which includes an organic fluorine-modified epoxy derivative prepared by reacting thionyl chloride, fluorinated biphenyl dicarboxylic acid, and glycidol as raw materials. By introducing fluorine atoms and biphenyl structures, the organic fluorine-modified epoxy derivative has excellent heat resistance, thereby improving the heat resistance of the epoxy potting glue.

[0006] In order to achieve the above purpose, the following technical solutions are adopted:

[0007] A Type-C male connector epoxy potting adhesive comprises the following raw materials in parts by weight: 30-35 parts of epoxy resin, 10-20 parts of organic fluorine-modified epoxy derivatives, 5-10 parts of toughening agents, 5-10 parts of active diluents, 0.5-3 parts of coupling agents, 8-12 parts of latent curing agents, 3-5 parts of curing accelerators, 30-40 parts of fillers, and 1-3 parts of thixotropic agents. The structural formula of the organic fluorine-modified epoxy derivative is shown in Formula I below:

[0008] Formula I:

[0009] wherein R1-R4 are independently F, CF3, H, and wherein at least one of R1-R4 is not H.

[0010] Furthermore, the organic fluorine-modified epoxy derivative is selected from one or a combination of two or more of Formulas I-1, I-2, I-3, I-4, and I-5.

[0011] Formula I-1:

[0012] Formula I-2

[0013] Formula I-3

[0014] Formula I-4

[0015] Formula I-5

[0016] Furthermore, the organic fluorine-modified epoxy derivative is of formula I-1

[0017] Formula I-1:

[0018] The organic fluorine-modified epoxy derivative is prepared by first chlorinating fluorinated biphenyl dicarboxylic acid with thionyl chloride to obtain a chlorinated product, and then reacting the chlorinated product with glycidol. The molar ratio of thionyl chloride, fluorinated biphenyl dicarboxylic acid and glycidol is 4-5:1:2.04-2.08.

[0019] The fluorine-containing biphenyl dicarboxylic acid is selected from one or a combination of two or more of 2,2'-bis(trifluoromethyl)-[1,1'-biphenyl]-4,4'-dicarboxylic acid, 3,3'-bis(trifluoromethyl)-[1,1'-biphenyl]-4,4'-dicarboxylic acid, 3,3',5,5'-tetrafluoro-[1,1'-biphenyl]-4,4'-dicarboxylic acid, 3,3-difluoro-[1,1-biphenyl]-4,4-dicarboxylic acid, and 4,4'-difluorobiphenyl-2,2'-dicarboxylic acid.

[0020] Furthermore, the fluorinated biphenyl dicarboxylic acid is selected from one or a combination of two or more of 3,3',5,5'-tetrafluoro-[1,1'-biphenyl]-4,4'-dicarboxylic acid, 2,2'-bis(trifluoromethyl)-[1,1'-biphenyl]-4,4'-dicarboxylic acid, and 3,3'-bis(trifluoromethyl)-[1,1'-biphenyl]-4,4'-dicarboxylic acid.

[0021] Furthermore, the fluorine-containing biphenyl dicarboxylic acid is 3,3',5,5'-tetrafluoro-[1,1'-biphenyl]-4,4'-dicarboxylic acid.

[0022] The organic fluorine-modified epoxy derivative is prepared by a method comprising the following steps:

[0023] 1) Add thionyl chloride and fluorinated biphenyl dicarboxylic acid to a dry distillation reactor, heat to reflux, wait until no gas is released, filter, and dry to obtain an acyl chloride product;

[0024] 2) dissolving the acyl chloride product, glycidol and catalyst in an organic solvent, controlling the temperature to react, adding water after the reaction until no precipitation is generated, filtering, washing and drying to obtain an organic fluorine-modified epoxy derivative.

[0025] The drying in step 1) is carried out at 80-100° C. to a constant weight.

[0026] Step 2) The organic solvent is selected from one or a combination of two or more of benzene, toluene, xylene and chloroform. The temperature control is to control the temperature at 20-30°C, and the reaction time is 1-2h. The catalyst is selected from one or a combination of two of N,N-dimethylaniline and triethylamine. The amount of the catalyst is 3-5% of the molar amount of propylene oxide. The washing is washing with water 1-3 times.

[0027] The toughening agent is selected from one or a combination of two or more of carboxyl-terminated liquid nitrile rubber, liquid nitrile rubber, liquid styrene butadiene rubber, liquid polybutadiene rubber, carboxyl-terminated liquid polybutadiene rubber, and hydroxyl-terminated liquid polybutadiene rubber, preferably carboxyl-terminated liquid nitrile rubber with an acid ester of 25-30 mgKOH / g.

[0028] The epoxy resin has an epoxy value of 0.41-0.54 and is selected from one or a combination of two or more of phenolic epoxy resin, alicyclic epoxy resin, bisphenol A epoxy resin, hydrogenated bisphenol A epoxy resin, bisphenol F epoxy resin and aliphatic epoxy resin.

[0029] The active diluent is selected from one or a combination of two or more of glycerol triglycidyl ether, 2-ethylhexyl glycidyl ether, neopentyl glycol diglycidyl ether, and trimethylolpropane triacrylate.

[0030] The coupling agent is selected from one or a combination of two or more of vinyl trimethoxy silane, 3-glycidyl propyl trimethoxy silane, 3-aminopropyl trimethoxy silane and 3-mercaptopropyl trimethoxy silane.

[0031] The latent curing agent is selected from one or a combination of dicyandiamide and dicyandiamide derivatives.

[0032] The curing accelerator is selected from one or a combination of two or more of 2-methylimidazole, 1-cyanoethyl substituted imidazole, 1-aminoethyl-2-methylimidazole, 1-benzyl-2-ethylimidazole, triethylamine, N,N-dimethylaniline, and nonylphenol.

[0033] The filler has an average particle size of 20-100 μm and is selected from one or a combination of two or more of talc, alumina, silica powder, hydrotalcite compound, aluminum hydroxide, nano calcium carbonate, and barium titanate.

[0034] The thixotropic agent is fumed silica.

[0035] The present invention also provides a method for preparing the epoxy potting adhesive of the Type-C male connector, comprising the following steps:

[0036] S1) mixing part of the organic fluorine-modified epoxy derivative and the toughening agent uniformly, heating to react, cooling to room temperature, adding the remaining organic fluorine-modified epoxy derivative to obtain a mixture for standby use;

[0037] S2) adding epoxy resin, the mixture of step S1, coupling agent, and thixotropic agent into a stirring kettle and mixing evenly, adding filler and mixing evenly, adding active diluent monomer and mixing evenly, adding latent curing agent and curing accelerator and mixing evenly, and obtaining the above-mentioned Type-C male connector epoxy potting glue.

[0038] In step S1), the temperature is raised to 100-140° C., and the reaction time is 1-3 hours. The remaining organic fluorine-modified epoxy derivative accounts for 3 / 4 to 4 / 5 of the total mass of the organic fluorine-modified epoxy derivative in step S1).

[0039] In step S2), the stirring tank is a vacuum double planetary stirring tank, and the mixing conditions are: high-speed dispersion stirring rate 1000-2000r / min, revolution stirring rate 100-150r / min, vacuum degree 0.001-0.01MPa, temperature control at 20-30°C, time 30-60min.

[0040] Compared with the prior art, the present invention has the following beneficial effects:

[0041] The raw materials of the epoxy potting glue of the Type-C male connector of the present invention include an organic fluorine-modified epoxy derivative prepared by reacting thionyl chloride, fluorinated biphenyl dicarboxylic acid, and glycidol as raw materials. By introducing fluorine atoms and biphenyl structures, the organic fluorine-modified epoxy derivative has excellent heat resistance, thereby improving the heat resistance of the epoxy potting glue.

[0042] The inventors found that the organic fluorine-modified epoxy derivative has the function of cooperating with the carboxyl-terminated liquid nitrile rubber toughening agent to improve the heat resistance. BRIEF DESCRIPTION OF THE DRAWINGS

[0043] Figure 1 The tensile shear strength test sample of the present invention;

[0044] Figure 2 The product to be tested is dispensed with epoxy potting glue of the Type-C male connector of Example 1 and cured. DETAILED DESCRIPTION

[0045] The present invention will be further described below in conjunction with specific embodiments, but is not limited to the contents of the specification. Unless otherwise specified, the "parts" described in the embodiments of the present invention are all parts by weight. The reagents used are all commercially available reagents in the art.

[0046] Liquid nitrile rubber LNBR 820N was purchased from Shanghai Jinju International Trade Co., Ltd., with an acrylonitrile content of 28 wt % and a number average molecular weight of 3,500.

[0047] Carboxyl-terminated liquid nitrile rubber CTBN1300×13, with an acid value of 32 mgKOH / g, an acrylonitrile content of 26 wt %, and a number average molecular weight of 3150, was purchased from Shenzhen Jiadida New Material Technology Co., Ltd.

[0048] Fumed silica AEROSIL R202 was purchased from EVONIK, Germany, with a specific surface area of ​​110 m 2 / g.

[0049] The average particle size of alumina was 100 μm and was purchased from Jinge New Materials.

[0050] The average particle size of silicon micropowder was 20 μm and it was purchased from Jiangsu Lianrui New Materials Co., Ltd.

[0051] The average particle size of hydrotalcite was 50 μm and it was purchased from Aidico Fine Chemical Co., Ltd.

[0052] Example 1

[0053] 1. Add 0.5 mol of thionyl chloride and 0.1 mol of 3,3',5,5'-tetrafluoro-[1,1'-biphenyl]-4,4'-dicarboxylic acid to a dry distillation reactor, heat to reflux, wait until no gas is released, filter, and dry at 100°C to constant weight to obtain the acyl chloride product;

[0054]

[0055] 2. The acyl chloride product obtained in step 1, 0.208 mol of glycidol and 0.01 mol of N,N-dimethylaniline were dissolved in 60 mL of chloroform, and the temperature was controlled at 30°C for reaction for 1 hour. After the reaction, water was added until no precipitation was produced, filtered, washed with water 3 times, and dried to obtain an organic fluorine-modified epoxy derivative;

[0056]

[0057] 3. Evenly mix 5g of organic fluorine-modified epoxy derivative and 10g of carboxyl-terminated liquid nitrile rubber CTBN1300×13, heat to 140°C for reaction for 3h, cool to room temperature, add the remaining 15g of organic fluorine-modified epoxy derivative to obtain a mixture, and set aside;

[0058] 4. Add 35g of bisphenol A epoxy resin E51, the mixture in step 3, 3g of 3-aminopropyltrimethoxysilane, and 3g of fumed silica into a stirring kettle and mix evenly. Add 20g of alumina, 10g of silicon powder, and 10g of hydrotalcite and mix evenly. Add 5g of propylene glycol triglycidyl ether and mix evenly. Add 12g of dicyandiamide and 3g of 2-methylimidazole and mix evenly to obtain the above-mentioned Type-C male connector epoxy potting glue.

[0059] Example 2

[0060] The rest is the same as Example 1, except that in step 1, an equal molar amount of 2,2'-bis(trifluoromethyl)-[1,1'-biphenyl]-4,4'-dicarboxylic acid is used to replace 3,3',5,5'-tetrafluoro-[1,1'-biphenyl]-4,4'-dicarboxylic acid.

[0061] Example 3

[0062] The rest is the same as Example 1, except that in step 1, an equal molar amount of 3,3-difluoro-[1,1-biphenyl]-4,4-dicarboxylic acid is used to replace 3,3',5,5'-tetrafluoro-[1,1'-biphenyl]-4,4'-dicarboxylic acid.

[0063] Example 4

[0064] The rest is the same as Example 1, except that step 3 is changed to: 2.5 g of the organic fluorine-modified epoxy derivative and 10 g of the terminal carboxyl liquid nitrile rubber CTBN1300×13 are mixed evenly, the temperature is raised to 140° C. to react for 3 h, the mixture is cooled to room temperature, and the remaining 7.5 g of the organic fluorine-modified epoxy derivative is added to obtain a mixture for use; that is, the total amount of the organic fluorine-modified epoxy derivative is 10 g.

[0065] Example 7

[0066] 1. Add 0.4 mol of thionyl chloride and 0.1 mol of 3,3',5,5'-tetrafluoro-[1,1'-biphenyl]-4,4'-dicarboxylic acid to a dry distillation reactor, heat to reflux, wait until no gas is released, filter, and dry at 100°C to constant weight to obtain the acyl chloride product;

[0067] 2. The acyl chloride product obtained in step 1, 0.204 mol of glycidol and 0.01 mol of N,N-dimethylaniline were dissolved in 60 mL of chloroform, and the reaction was carried out at 30°C for 1 hour. After the reaction, water was added until no precipitation was produced, filtered, washed with water 3 times, and dried to obtain an organic fluorine-modified epoxy derivative;

[0068] 3. Mix 2g of organic fluorine-modified epoxy derivative and 5g of carboxyl-terminated liquid nitrile rubber CTBN1300×13 evenly, heat to 140°C for reaction for 3h, cool to room temperature, add the remaining 8g of organic fluorine-modified epoxy derivative to obtain a mixture, and set aside;

[0069] 4. Add 30g bisphenol A epoxy resin E51, the mixture in step 3, 3g 3-aminopropyltrimethoxysilane, and 3g fumed silica into a stirring kettle and mix evenly. Add 20g alumina, 10g silica powder, and 10g hydrotalcite and mix evenly. Add 10g propylene glycol triglycidyl ether and mix evenly. Add 12g dicyandiamide and 3g 2-methylimidazole and mix evenly to obtain the above-mentioned Type-C male connector epoxy potting glue.

[0070] Example 8

[0071] The rest is the same as Example 1, except that in step 3, the carboxyl-terminated liquid nitrile rubber CTBN1300×13 is replaced by an equal mass of liquid nitrile rubber LNBR820N.

[0072] Example 9

[0073] 1. Add 0.5 mol of thionyl chloride and 0.1 mol of 3,3',5,5'-tetrafluoro-[1,1'-biphenyl]-4,4'-dicarboxylic acid to a dry distillation reactor, heat to reflux, wait until no gas is released, filter, and dry at 100°C to constant weight to obtain the acyl chloride product;

[0074] 2. The acyl chloride product obtained in step 1, 0.208 mol of glycidol and 0.01 mol of N,N-dimethylaniline were dissolved in 60 mL of chloroform, and the temperature was controlled at 30°C for reaction for 1 hour. After the reaction, water was added until no precipitation was produced, filtered, washed with water 3 times, and dried to obtain an organic fluorine-modified epoxy derivative;

[0075] 3. Add 35g of bisphenol A epoxy resin E51, 10g of terminal carboxyl liquid nitrile rubber CTBN1300×13, 20g of organic fluorine-modified epoxy derivative, 3g of 3-aminopropyltrimethoxysilane, and 3g of fumed silica into a stirring kettle and mix evenly. Add 20g of alumina, 10g of silica powder, and 10g of hydrotalcite and mix evenly. Add 5g of propylene triglycidyl ether and mix evenly. Add 12g of dicyandiamide and 3g of 2-methylimidazole and mix evenly to obtain the above-mentioned Type-C male connector epoxy potting glue.

[0076] Comparative Example 1

[0077] The rest is the same as Example 1, except that in step 1, an equal molar amount of 4,4'-biphenyldicarboxylic acid is used to replace 3,3',5,5'-tetrafluoro-[1,1'-biphenyl]-4,4'-dicarboxylic acid.

[0078] The epoxy potting adhesives prepared in the above examples and comparative examples were subjected to the following performance tests:

[0079] 1. Tg: Reference standard BS ISO 11359-1:2014, TMA method, compression mode, adhesive thickness 2mm, temperature range -20℃ to 200℃, 5℃ / min heating rate, heating-cooling-heating scan, pre-load 0.05N (take the data of the second heating process).

[0080] 2. Tensile shear strength: refer to standard ASTM D1002-10 tensile shear strength test, FR4 / FR4.

[0081] 3. Air tightness test: Prepare the Type-C product to be tested, the USB type-c / 3.1 interface male head (with version data AM) test piece of Dongguan Chengnan Technology Co., Ltd., and use the Nordson Asymtex S dispensing machine for dispensing and potting, the dispensing amount is 20mg, the glue line height is 2mm, and it is cured at 120℃ for 0.5h. The Type-C product to be tested is placed in the ES 602 model air tightness tester of Jiangsu Yixun Precision Technology Co., Ltd. for air tightness test, the test pressure is 15KPa (simulating the test pressure of the product at a water depth of 1m), and the upper limit of the allowable leakage is: 0.05KPa. The test process is air intake time 2s, pressure stabilization time 2s, test time 5s, exhaust time 1s, the whole test process 10s, read the pressure displayed on the display, and the indication is required to be unchanged. The Type-C product to be tested was subjected to reflow aging in the BT301N small desktop reflow oven. After reflowing at 265°C for 60 seconds, it was taken out and cooled to room temperature. This process was repeated three times. The previous air tightness test was repeated, and the air pressure loss rate was considered qualified if it was within 3%.

[0082] Figure 1 The tensile shear strength test sample of the present invention;

[0083] Figure 2 The product to be tested is dispensed with epoxy potting glue of the Type-C male connector of Example 1 and cured.

[0084] Table 1 Performance test results

[0085] project Tg℃ Tensile shear strength MPa Air pressure loss rate % Example 1 160.1 20.1 0 Example 2 157.8 20.0 0.4 Example 3 156.6 20.7 0.6 Example 4 159.2 18.5 0 Example 5 157.0 18.0 0.8 Example 6 155.2 19.4 0 Example 7 145.6 17.6 2.7 Comparative Example 1 133.7 21.1 6.9

[0086] It can be seen from Table 1 that the Type-C male connector epoxy potting adhesive prepared by the present invention has excellent high temperature resistance, good air tightness after reflow soldering aging, and can effectively prevent external pollutants such as moisture and dust from entering the interior of the connector.

[0087] The above detailed description is a specific description of one feasible embodiment of the present invention. The embodiment is not intended to limit the patent scope of the present invention. Any equivalent implementation or modification that does not deviate from the present invention should be included in the scope of the technical solution of the present invention.

Claims

1. A Type-C male connector epoxy potting adhesive, characterized in that: The raw materials include the following parts by weight: 30-35 parts of epoxy resin, 10-20 parts of organic fluorine-modified epoxy derivatives, 5-10 parts of toughening agents, 5-10 parts of reactive diluents, 0.5-3 parts of coupling agents, 8-12 parts of latent curing agents, 3-5 parts of curing accelerators, 30-40 parts of fillers, and 1-3 parts of thixotropic agents. The structural formula of the organic fluorine-modified epoxy derivatives is shown in the following formula I: Formula I: wherein R1-R4 are independently F, CF3, H, and wherein at least one of R1-R4 is not H.

2. The Type-C male connector epoxy potting adhesive according to claim 1, characterized in that: The organic fluorine-modified epoxy derivative is selected from one or a combination of two or more of Formulas I-1, I-2, I-3, I-4, and I-5, Formula I-1: Formula I-2 Formula I-3 Formula I-4 Formula I-5 3. The Type-C male connector epoxy potting adhesive according to claim 2, characterized in that: The organic fluorine-modified epoxy derivative is of formula I-1 Formula I-1:

4. The Type-C male connector epoxy potting adhesive according to claim 1, characterized in that: The organic fluorine-modified epoxy derivative is prepared by first chlorinating fluorinated biphenyl dicarboxylic acid with thionyl chloride to obtain a chlorinated product, and then reacting the chlorinated product with glycidol. The molar ratio of thionyl chloride, fluorinated biphenyl dicarboxylic acid and glycidol is 4-5:1:2.04-2.

08.

5. The Type-C male connector epoxy potting adhesive according to claim 4, characterized in that: The fluorine-containing biphenyl dicarboxylic acid is selected from one or a combination of two or more of 2,2'-bis(trifluoromethyl)-[1,1'-biphenyl]-4,4'-dicarboxylic acid, 3,3'-bis(trifluoromethyl)-[1,1'-biphenyl]-4,4'-dicarboxylic acid, 3,3',5,5'-tetrafluoro-[1,1'-biphenyl]-4,4'-dicarboxylic acid, 3,3-difluoro-[1,1-biphenyl]-4,4-dicarboxylic acid, and 4,4'-difluorobiphenyl-2,2'-dicarboxylic acid.

6. The Type-C male connector epoxy potting adhesive according to claim 5, characterized in that: The fluorinated biphenyl dicarboxylic acid is selected from one or a combination of two or more of 3,3',5,5'-tetrafluoro-[1,1'-biphenyl]-4,4'-dicarboxylic acid, 2,2'-bis(trifluoromethyl)-[1,1'-biphenyl]-4,4'-dicarboxylic acid, and 3,3'-bis(trifluoromethyl)-[1,1'-biphenyl]-4,4'-dicarboxylic acid.

7. The epoxy potting adhesive for Type-C male connector according to claim 6, characterized in that: The fluorine-containing biphenyl dicarboxylic acid is 3,3',5,5'-tetrafluoro-[1,1'-biphenyl]-4,4'-dicarboxylic acid.

8. The Type-C male connector epoxy potting adhesive according to claim 1, characterized in that: The organic fluorine-modified epoxy derivative is prepared by a method comprising the following steps: 1) Add thionyl chloride and fluorinated biphenyl dicarboxylic acid to a dry distillation reactor, heat to reflux, wait until no gas is released, filter, and dry to obtain an acyl chloride product; 2) dissolving the acyl chloride product, glycidol and catalyst in an organic solvent, controlling the temperature to react, adding water after the reaction until no precipitation is generated, filtering, washing and drying to obtain an organic fluorine-modified epoxy derivative.

9. The Type-C male connector epoxy potting adhesive according to claim 1, characterized in that: The toughening agent is selected from one or a combination of two or more of terminal carboxyl liquid nitrile rubber, liquid nitrile rubber, liquid styrene butadiene rubber, liquid polybutadiene rubber, terminal carboxyl liquid polybutadiene rubber, and terminal hydroxyl liquid polybutadiene rubber; preferably, the terminal carboxyl liquid nitrile rubber has an acid ester of 25-30 mgKOH / g; the epoxy value of the epoxy resin is 0.41-0.54, and is selected from one or a combination of two or more of phenolic epoxy resin, alicyclic epoxy resin, bisphenol A epoxy resin, hydrogenated bisphenol A epoxy resin, bisphenol F epoxy resin, and aliphatic epoxy resin.

10. The method for preparing the epoxy potting adhesive for the Type-C male connector according to any one of claims 1 to 9, characterized in that: The steps include: S1) mixing part of the organic fluorine-modified epoxy derivative and the toughening agent uniformly, heating to react, cooling to room temperature, adding the remaining organic fluorine-modified epoxy derivative to obtain a mixture for standby use; S2) adding epoxy resin, the mixture of step S1, coupling agent, and thixotropic agent into a stirring kettle, mixing evenly, adding filler and mixing evenly, adding active diluent monomer and mixing evenly, adding latent curing agent and curing accelerator and mixing evenly, to obtain the above-mentioned Type-C male connector epoxy potting glue; In step S1), the temperature is raised to 100-140° C., and the reaction time is 1-3 hours; the remaining organic fluorine-modified epoxy derivative accounts for 3 / 4 to 4 / 5 of the total mass of the organic fluorine-modified epoxy derivative in step S1); In step S2), the stirring tank is a vacuum double planetary stirring tank, and the mixing conditions are: high-speed dispersion stirring rate 1000-2000r / min, revolution stirring rate 100-150r / min, vacuum degree 0.001-0.01MPa, temperature control at 20-30°C, time 30-60min.

Citation Information

Patent Citations

  • A low-temperature fast-curing adhesive for protecting the male head of a Type-C connector and a preparation method thereof

    CN115181523B