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High-heat-resistance single-component adhesive and preparation method thereof

A one-component, adhesive technology, used in adhesives, adhesive additives, non-polymer adhesive additives, etc., can solve the problems of cracking and sealing, poor long-term reliability, large residual stress, etc., to achieve high resistance Improved low temperature impact performance, unaffected bond strength, and improved toughness of cured products

Pending Publication Date: 2021-12-03
艾蒙特成都新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Like two-component epoxy adhesives, one-component epoxy resin adhesives have problems such as insufficient heat resistance and high brittleness, which limit their application in the field of high heat resistance and high reliability.
At the same time, the curing time of the one-component epoxy adhesive is shorter, the residual stress is larger, and the cracking problem is more prone to occur
Although a variety of epoxy modification methods have been widely studied, the improvement effect is not obvious. One-component epoxy resin adhesives still have problems of insufficient heat resistance, high brittleness, and poor long-term reliability.
For example, in the sealing and bonding of automotive electronic components such as VVL (abbreviation for variable valve lift) actuators, there are long-term high temperature resistance requirements and harsh requirements for high and low temperature shocks in extreme environments. As a single-component packaging material Epoxy resin is prone to problems such as cracking and poor sealing, resulting in product failure
[0004] In order to solve the current problem of insufficient heat resistance and large thermal expansion coefficient of epoxy single-component adhesives, the prior art mostly uses multifunctional novolac epoxy resins to improve the heat resistance of the adhesive, for example: CN110655891A discloses "High temperature resistant adhesive", CN102391810A disclosed "a high temperature resistant variable color anti-counterfeit epoxy adhesive and its preparation method", CN105670542A disclosed "a low linear expansion coefficient medium and low temperature curing one-component epoxy adhesive and its preparation method", etc., because the heat resistance is improved by increasing the cross-linking density, the brittleness of the cured product will also increase simultaneously, and the reliability of use will decrease
There are many studies on the application of bismaleimide in adhesives, but most of them are limited to the introduction of bismaleimide to improve the overall heat resistance, and there are still obvious shortcomings in the performance balance of the entire composition

Method used

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Examples

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preparation example Construction

[0049] A preparation method of a high heat-resistant one-component adhesive, the steps are as follows:

[0050] The first part of the preparation of bismaleimide resin

Embodiment 1-1~1-5

[0051] Embodiment 1-1~1-5: Preparation of bismaleimide resin

[0052] Implementation steps:

[0053] (a) Add 0.1-0.15mol maleic anhydride and 200ml solvent into a round-bottomed flask equipped with a stirrer, thermometer and reflux condenser, stir to dissolve, then slowly add 0.1-0.15mol p-aminophenol, and react at room temperature 2 to 3 hours, then add 0.0001mol to 0.001mol of catalyst, heat up and reflux for 3 to 4 hours, then cool, water analysis, suction filtration, and recrystallization to obtain N-(4-hydroxyphenyl)maleimide;

[0054] (b) Add 0.1mol N-(4-hydroxyphenyl)maleimide and 100mL solvent to a round bottom flask A equipped with a stirrer, a thermometer and a reflux condenser, and stir to dissolve; in another vessel B Add 0.05mol chlorine-terminated polysiloxane, 50mL solvent, and 0.05-0.2mol alkaline substance to make a mixed solution C; slowly drop the mixed solution C into the round bottom through a constant pressure dropping funnel at 0-10°C In flask A, react...

Embodiment 2-1~2-7

[0063] Examples 2-1 to 2-7: Preparation of toughened modified bismaleimide resin

[0064] Implementation steps:

[0065] Add 0.1mol of bismaleimide resin into a three-necked flask, heat it to 100-140°C to melt it, then add 0.01-0.1mol of allyl compound, and stir at a constant temperature of 100-140°C for 10-60min to make it fully Prepolymerize, discharge and cool, grind into powder, and filter with a 2000-mesh sieve to obtain a resin powder with a particle size D50 within 20 μm.

[0066] The allyl compound is selected from 2,2'-diallyl bisphenol A or 2-allylphenol.

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Abstract

The invention discloses a high-heat-resistance single-component adhesive and a preparation method thereof. The high-heat-resistance single-component adhesive is characterized by being prepared by mixing the following components in parts by weight: 5 to 30 parts of toughening modified bismaleimide resin, 15 to 55 parts of epoxy resin, 0.1 to 5 parts of epoxy active diluent, 3 to 18 parts of a latent curing agent, 0.01 to 0.5 part of a defoaming agent, 0.01 to 0.5 part of a wetting dispersant, 0.1 to 5 parts of a catalyst and 5 to 60 parts of an inorganic filler. The preparation method comprises the following steps: preparing bismaleimide resin, carrying out toughening modification treatment, adding the toughening modified bismaleimide resin and other raw materials into a vacuum planetary mixer, and carrying out mixing. The high-heat-resistance single-component adhesive disclosed by the invention has the characteristics of gentle heat release in a curing process, high heat resistance of a cured product, high toughness, low thermal expansion coefficient, good high and low temperature impact resistance and the like, and is suitable for bonding and sealing of electronic and electric appliance elements and metal and nonmetal devices with heat resistance and environment temperature requirements.

Description

technical field [0001] The invention belongs to an adhesive and its preparation, and relates to a high heat-resistant one-component adhesive and a preparation method thereof. The high heat-resistant one-component adhesive of the present invention is suitable for the bonding of metal, non-metal and thermosetting polymer materials, etc., especially suitable for the bonding of electronic and electrical components, metal and non-metal devices that require heat resistance and ambient temperature and seal. Background technique [0002] Epoxy resin adhesives have good bonding properties to metals, non-metals and thermosetting polymer materials, etc., have strong adaptability, and are environmentally friendly. They occupy an important position in the adhesive industry and are widely used in machinery manufacturing, electronics, construction, etc. and aerospace industries. Compared with two-component epoxy resin adhesives, one-component epoxy resin adhesives have the advantages of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09J163/00C09J163/04C09J179/08C09J11/04C08G73/12
CPCC09J163/00C09J11/04C08G73/125C08L2205/03C08L2201/08C08L2203/206C08L2205/04C08L63/00C08L79/085C08K7/18C08L63/04
Inventor 易强宋贤锋陈立兴周友
Owner 艾蒙特成都新材料科技有限公司
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