A solvent-free epoxy potting adhesive and preparation method thereof

Abstract

The invention discloses a solvent-free epoxy potting glue, which comprises the following components by weight: 40-60 parts of solvent-free epoxy resin I, 0.5-0.7 parts of black slurry, 0.2-1.5 parts of defoamer and 10-20 parts of polyetheramine, wherein the raw material components of the black slurry comprise by weight: 70-90 parts of solvent-free epoxy resin II, 5-10 parts of active diluent, 5-30 parts of wetting dispersant and 15-30 parts of carbon black. The potting glue of the invention has no bubbles, good flatness, does not use solvents, and is environmentally friendly.

Description

Technical Field

[0001] The invention relates to the technical field of potting adhesives, in particular to a solvent-free epoxy potting adhesive and a preparation method thereof. Background Art

[0002] With the rapid development of electronic technology, high-tech fields such as electronic components, large integrated circuit boards, power circuit modules, etc. have further achieved high power, high performance, and miniaturization and density. At the same time, as the application fields of electronic components continue to expand, their use environment is becoming more and more demanding. Electronic components will be affected by factors such as mechanical external force, high temperature and high humidity environment, physical and chemical pollution, and electrical leakage during production, transportation, storage, and use. This requires that electronic potting materials not only need to have good high temperature resistance, mechanical properties, thermal conductivity, and electrical properties, but also put forward higher requirements on the adhesion between potting materials and components.

[0003] At present, the commonly used potting glues are mainly silicone potting glue, polyurethane potting glue and epoxy potting glue. Among them, silicone potting glue has excellent rework ability due to its low viscosity, and can quickly and conveniently remove the sealed components for repair and replacement; however, its high price, slightly poor adhesion, and easy to cause catalyst poisoning and non-curing problems limit its use. Polyurethane potting glue has excellent low temperature resistance. According to the principle that structure determines performance, polyurethane potting glue with different performance can be obtained by regulating the structure of polyurethane. Epoxy potting glue has excellent high temperature resistance and electrical insulation ability, simple operation, stable performance before and after curing, and excellent adhesion to a variety of metal substrates and porous substrates. However, epoxy potting glue has poor resistance to cold and hot shocks. It is easy to crack after being subjected to cold and hot shocks, causing water vapor to penetrate into electronic components from the cracks, resulting in poor moisture resistance; at the same time, the hardness of the colloid after curing is high and brittle, which is easy to damage electronic components.

[0004] Therefore, how to solve the above technical problems is the research direction that technicians in this field are committed to. Summary of the invention

[0005] The purpose of the present invention is to provide a solvent-free epoxy potting adhesive.

[0006] To achieve the above-mentioned purpose, the present invention provides the following technical scheme: a solvent-free epoxy potting glue, which comprises the following components in parts by weight: 40-60 parts of solvent-free epoxy resin I, 0.5-0.7 parts of black paste, 0.2-1.5 parts of defoaming agent and 10-20 parts of polyether amine, wherein the raw material components of the black paste comprise in parts by weight: 70-90 parts of solvent-free epoxy resin II, 5-10 parts of active diluent, 5-30 parts of wetting dispersant and 15-30 parts of carbon black.

[0007] As a specific implementation, the solvent-free epoxy resin I and the solvent-free epoxy resin II both use the solvent-free epoxy resin model BE188 produced by Taiwan Changchun Chemical Industry Group of China; the polyetheramine uses the polyetheramine brand C16 produced by Suzhou Hengst Industrial Co., Ltd. of China.

[0008] As a specific implementation manner, the defoamer used is the defoamer with the brand F-1301 or F-1501 produced by China's Aoshijia Material Technology (Shanghai) Co., Ltd.

[0009] As a specific implementation, the wetting and dispersing agent uses a dispersant with a brand name of DS-2002CRT or DS-8005 produced by China's Aoshijia Material Technology (Shanghai) Co., Ltd.

[0010] As a specific implementation manner, the active diluent used is a 748 active diluent produced by Evonik Degussa Specialty Chemicals (Shanghai) Co., Ltd. of China.

[0011] As a specific implementation manner, the carbon black uses carbon black with a brand number of MA100 produced by Mitsubishi Chemical Holdings Corporation of Japan.

[0012] As a specific implementation method, the preparation process of the black slurry is as follows: add solvent-free epoxy resin II, active diluent, wetting dispersant and carbon black into the reactor in sequence, mix them evenly, add an equal amount of glass beads and shake for 120 minutes.

[0013] Another object of the present invention is to provide a method for preparing the above-mentioned solvent-free epoxy potting glue, and the preparation process of the potting glue is as follows: solvent-free epoxy resin I, black slurry and defoaming agent are added to the reactor in sequence, stirred at a linear speed of 5 m / s for 5 minutes and then left overnight, and then polyetheramine is added, stirred at a speed of 1000 revolutions per minute with a 5 cm serrated turntable for 1 minute, left at room temperature for 30 minutes, and then baked in an oven at 60°C for 4-5 hours.

[0014] Compared with the prior art, the beneficial effects of the present invention are as follows: the solvent-free epoxy potting glue of the present invention adopts solvent-free epoxy resin, and is matched with corresponding wetting dispersant and defoaming agent. The product has no bubbles, good flatness, does not use solvent, and is environmentally friendly. DETAILED DESCRIPTION

[0015] Unless the context clearly dictates otherwise, unmodified nouns and nouns modified by "the" include singular and plural referents.

[0016] As used in the specification and claims, the terms "comprises," "comprising," "having," "may," "containing," and variations thereof as used herein refer to open transitional phrases, terms, or words that require the presence of specified ingredients / steps and allow for the presence of other ingredients / steps. However, such descriptions should be interpreted as also describing compositions or methods as "consisting of" and "consisting essentially of" the recited ingredients / steps, which allows for the presence of only the specified ingredients / steps and any unavoidable impurities that may result therefrom, and excludes other ingredients / steps.

[0017] Numerical values ​​in the specification and claims of this application should be understood to include the same numerical values ​​when reduced to the same number of significant figures and numerical values ​​that differ from the stated value by less than the experimental error of ordinary measurement techniques of the type described in this application for determining the stated value.

[0018] All ranges disclosed herein are inclusive of the indicated endpoints and are independently combinable (eg, the range of "2 grams to 10 grams" includes the endpoints 2 grams and 10 grams, and all intermediate values).

[0019] The terms "about" and "approximately" can be used to include any numerical value that can be varied without changing the basic function of the value. When used with a range, "about" and "approximately" also disclose the range defined by the absolute values ​​of the two endpoints, for example, "about 2 to about 4" also discloses a range of "2 to 4". Generally, the terms "about" and "approximately" can refer to ±10% of the indicated number. However, for temperature, the term "approximately" refers to ±1°C.

[0020] Unless expressly stated otherwise, the percentages of elements are to be considered as percentages by weight of the alloy in question.

[0021] The invention provides a solvent-free epoxy potting adhesive. The potting adhesive comprises the following components in parts by weight: 40-60 parts of solvent-free epoxy resin I, 0.5-0.7 parts of black paste, 0.5-1.5 parts of defoaming agent and 10-20 parts of polyether amine, wherein the raw material components of the black paste comprise in parts by weight: 70-90 parts of solvent-free epoxy resin II, 5-10 parts of active diluent, 5-30 parts of wetting dispersant and 15-30 parts of carbon black.

[0022] Here, solvent-free epoxy resin I and solvent-free epoxy resin II both use solvent-free epoxy resin model BE188 produced by Taiwan Changchun Chemical Industry Group of China; polyetheramine uses polyetheramine brand C16 produced by Suzhou HNSAT Industrial Co., Ltd. of China; defoamer uses defoamer brand F-1301 or F-1501 produced by Aoshijia Material Technology (Shanghai) Co., Ltd. of China; wetting dispersant uses dispersant brand DS-2002CRT or DS-8005 produced by Aoshijia Material Technology (Shanghai) Co., Ltd. of China; active diluent uses active diluent brand 748 produced by Evonik Degussa Specialty Chemicals (Shanghai) Co., Ltd. of China; carbon black uses carbon black brand MA100 produced by Mitsubishi Chemical Holdings Corporation of Japan.

[0023] 1. Selection of defoaming agent

[0024] 40 parts of BE188 and 1 part of defoamer were added to the reactor, and then stirred at a linear speed of 5 m / s for 5 minutes, left overnight, and then 10 parts of C16 polyetheramine were added, and stirred at a speed of 1000 rpm with a 5 cm serrated turntable for 1 minute, and then placed at room temperature for 30 minutes and placed in a 60°C oven for 4 hours. After drying, the bubble condition on the surface of the potting glue was evaluated visually and the glue was cut vertically with a paper cutter to evaluate the bubble condition of the cross section. The specific model of the defoamer and the performance of the potting glue are shown in Table 1.

[0025] Table 1

[0026]

[0027]

[0028] Among them, F-2020, F-136, F-1307, F-1501, F-1301 and F-2560 are all brands of defoaming agents produced by Aosjia Materials Technology (Shanghai) Co., Ltd.

[0029] The detection method is as follows:

[0030] Performance Testing method Substrate Drying conditions Color paste viscosity 6# rotor, 1000 1 / s Rubber state 5 m / s for 5 minutes with naked eye Surface condition of potting compound 5 m / s 1 minute pouring 7cm diameter cup lid Dry at room temperature Coating appearance and transparency 100 micron frame coating Polyester film Dry at room temperature

[0031] From Table 1, we can see that the defoamers with the best performance after screening are brands F-1501 and F-1301.

[0032] 2. Selection of wetting and dispersing agents

[0033] 1. Preparation of black pulp

[0034] 80 parts of BE188, 8 parts of Evonik Degussa 748, 30 parts of wetting and dispersing agent and 20 parts of Mitsubishi Carbon Black MA100 were added to the reactor in sequence, mixed evenly, and then an equal amount of glass beads were added and shaken for 120 minutes.

[0035] 2. Prepare potting glue

[0036] Add 40 parts of BE188, 0.5 parts of black pulp and 1 part of defoamer F-1301 to the reactor in sequence, stir at a linear speed of 5 m / s for 5 minutes and leave overnight, then add 10 parts of C16 polyetheramine, stir at 1000 rpm on a 5 cm serrated turntable for 1 minute, leave at room temperature for 30 minutes, and then bake in an oven at 60°C for 4-5 hours.

[0037] Among them, the specific models of wetting and dispersing agents and the properties of potting glue are shown in Table 2.

[0038] Table 2

[0039]

[0040]

[0041] Note: In transparency, 1 means the worst and 5 means the best.

[0042] DS-5010, DS-5207, DS-5244, DS-4276, DS-240, DS-210, DS-4063, DS-4061, DS-8005 and DS-2130H are all brands of wetting and dispersing agents produced by Aosjia Materials Technology (Shanghai) Co., Ltd.

[0043] It can be seen from Table 2 that after screening, the brands of wetting and dispersing agents with better performance are DS4276 and DS8005.

[0044] 3. Selection of the overall solution for potting glue

[0045] The two best performing defoamers F-1301 and F-1501, and wetting and dispersing agents DS-4276 and DS-8005, which were screened out in the first two steps, were combined for testing and evaluation.

[0046] 1. Preparation of black pulp

[0047] 80 parts of BE188, 8 parts of Evonik Degussa 748, 6 parts of wetting and dispersing agent and 20 parts of Mitsubishi Carbon Black MA100 were added to the reactor in sequence, mixed evenly, and then an equal amount of glass beads were added and shaken for 120 minutes.

[0048] 2. Prepare potting glue

[0049] Add 40 parts of BE188, 0.5 parts of black pulp and 1 part of defoamer into the reactor in sequence, stir at a linear speed of 5 m / s for 5 minutes and leave overnight, then add 10 parts of C16 polyetheramine, stir at 1000 rpm on a 5 cm serrated turntable for 1 minute, leave at room temperature for 30 minutes, and then bake in an oven at 60°C for 4-5 hours.

[0050] The selection of defoaming agent and wetting and dispersing agent and the performance of the prepared potting compound are shown in Table 3.

[0051] Table 3

[0052] Wetting and dispersing agents Defoaming agent Surface bubbles Section Bubble Appearance blank blank Lots of bubbles Lots of bubbles / DS-4276 F-1501 No bubbles A small amount of microbubbles smooth DS-8005 F-1501 No bubbles A small amount of microbubbles smooth DS-4276 F-1301 A small amount of microbubbles No bubbles smooth DS-8005 F-1301 No bubbles No bubbles smooth

[0053] Scanning electron microscopy (SEM) was used for degassing detection. It can be seen from Table 3 that the best overall solution for dispersing and degassing of solvent-free epoxy potting adhesive is: using a defoaming agent with a brand of F-1301 and a wetting and dispersing agent with a brand of DS-8005.

[0054] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A solvent-free epoxy potting adhesive, characterized in that: The potting compound comprises the following components in parts by weight: 40-60 parts of solvent-free epoxy resin I, 0.5-0.7 parts of black paste, 0.2-1.5 parts of defoaming agent and 10-20 parts of polyether amine, wherein the raw material components of the black paste comprise in parts by weight: 70-90 parts of solvent-free epoxy resin II, 5-10 parts of active diluent, 5-30 parts of wetting dispersant and 15-30 parts of carbon black.

2. A solvent-free epoxy potting adhesive according to claim 1, characterized in that: The solvent-free epoxy resin I and the solvent-free epoxy resin II both adopt the solvent-free epoxy resin of model BE188 produced by Taiwan Changchun Chemical Industry Group of China; the polyetheramine adopts the polyetheramine of brand C16 produced by Suzhou Hengst Industrial Co., Ltd. of China.

3. The solvent-free epoxy potting adhesive according to claim 1, characterized in that: The defoamer used is the defoamer with the brand F-1301 or F-1501 produced by China's Aoshijia Material Technology (Shanghai) Co., Ltd.

4. The solvent-free epoxy potting adhesive according to claim 1, characterized in that: The wetting and dispersing agent used is a dispersing agent with a brand name of DS-2002CRT or DS-8005 produced by China's Aoshijia Material Technology (Shanghai) Co., Ltd.

5. The solvent-free epoxy potting adhesive according to claim 1, characterized in that: The active diluent used was active diluent of brand 748 produced by Evonik Degussa Specialty Chemicals (Shanghai) Co., Ltd. of China.

6. The solvent-free epoxy potting adhesive according to claim 1, characterized in that: The carbon black used was carbon black with a brand number of MA100 produced by Mitsubishi Chemical Holdings Corporation of Japan.

7. The solvent-free epoxy potting adhesive according to claim 1, characterized in that: The preparation process of the black slurry is as follows: solvent-free epoxy resin II, active diluent, wetting dispersant and carbon black are added to the reactor in sequence, and after mixing evenly, an equal amount of glass beads are added and shaken for 120 minutes.

8. A method for preparing a solvent-free epoxy potting adhesive as claimed in any one of claims 1 to 7, characterized in that: The preparation process of the potting glue is as follows: solvent-free epoxy resin I, black paste and defoamer are added to the reactor in sequence, stirred at a linear speed of 5 m / s for 5 minutes and then left overnight, and then polyetheramine is added, stirred at a speed of 1000 revolutions per minute with a 5 cm serrated turntable for 1 minute, left at room temperature for 30 minutes, and then baked in an oven at 60°C for 4-5 hours.

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