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Difunctional epoxy resin-silicone rubber block interpenetrating network material and preparation method thereof

A technology of epoxy resin and interpenetrating network, which is applied in the field of bifunctional epoxy resin-silicone rubber block interpenetrating network material and its preparation, can solve the problem of poor heat resistance of epoxy resin, lower heat resistance of silicone rubber, Limit the application of silicone rubber and other problems to achieve the effect of excellent performance, wide application range and improved heat resistance

Active Publication Date: 2021-08-27
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the poor heat resistance of epoxy resin itself, adding it to the silicone rubber system usually reduces the heat resistance of silicone rubber, limiting its use.
[0005] Yishan Liu et al., "Self-adhesive epoxy modified silicone materials for light emitting diode encapsulation", DOI: 10.1002 / pat.4024 discloses the method of using epoxy resin to modify silicone rubber, which can effectively improve the bonding performance of materials , but its thermal residual weight at 800°C drops from 50% to less than 30%, which severely limits the application of silicone rubber

Method used

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  • Difunctional epoxy resin-silicone rubber block interpenetrating network material and preparation method thereof
  • Difunctional epoxy resin-silicone rubber block interpenetrating network material and preparation method thereof
  • Difunctional epoxy resin-silicone rubber block interpenetrating network material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] The synthesis of embodiment 1, difunctional epoxy resin DABPA

[0040]

[0041] DABPA

[0042] Solid alkali method: add epichlorohydrin (ECH, 1mol), diallyl bisphenol A (DADGEBA, 0.1mol), tetramethylammonium bromide (0.006mol) into a three-necked flask together, and stir at 100°C Reaction 2h. Then lower the temperature to 85°C, add 0.2mol sodium hydroxide solid, react at 85°C for 2h, and then use a rotary evaporator to distill off excess epichlorohydrin under reduced pressure. Pour the reaction solution into a separatory funnel, add an appropriate amount of 50mL xylene to dissolve the crude product, wash it with deionized water, remove the lower water layer, add 5% sodium hydroxide solution to the crude product, and react at 85°C for 2 hours. Hydrolyze chlorine, remove the water layer, check the acidity and alkalinity with ph test paper, then neutralize the organic phase with 2% sodium dihydrogen phosphate to neutrality, wash with water and remove the water layer, ...

Embodiment 2

[0043] Example 2. Preparation of bifunctional epoxy resin-silicone rubber block interpenetrating network material of the present invention

[0044] According to the feed ratio shown in Table 1, the invented bifunctional epoxy resin-silicone rubber block interpenetrating network materials DADGEBA-1p, DADGEBA-3p, DADGEBA-5p, DADGEBA-10p were prepared. Specific steps are as follows:

[0045]Add the difunctional epoxy resin DABPA prepared in Example 1 into the silicone rubber, stir at 80° C. for 1 h, and after cooling to room temperature, add hydrogen-containing silicone oil (HS) and methylnadic anhydride (MNA) successively, and epoxy cure Accelerator (DMP-30), catalyst (Pt) and catalytic retarder 2-methyl-3 butyn-2 alcohol (MBO), after stirring at room temperature for 15 minutes, remove air bubbles in vacuum for 10 minutes, then pour into the mold, press in order at 90 Cure at 2h at 120°C, 2h at 120°C, 2h at 140°C, and 2h at 180°C to obtain the invented bifunctional epoxy resin-...

experiment example 1

[0052] Experimental Example 1, Structural Characterization of Difunctional Epoxy Resin

[0053] (1) Experimental method

[0054] The bifunctional epoxy resin DABPA prepared in Example 1 was characterized by infrared, hydrogen nuclear magnetic spectrum and carbon nuclear magnetic spectrum respectively.

[0055] (2) Experimental results

[0056] The result is as Figure 1-3 shown. In the infrared spectrum ( figure 1 ), the hydroxyl peak of DADGEBA disappeared obviously, 850,914cm -1 The peak of the epoxy group at 723cm -1 The peak of carbon-chlorine bond disappeared, indicating that diallyl bisphenol A reacted with epichlorohydrin. In the H NMR and C NMR spectra ( figure 2 , image 3 ), the corresponding peaks of each hydrogen atom and carbon atom in DABPA can also be found respectively. The above results illustrate that the present invention has successfully prepared the difunctional epoxy resin DABPA.

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Abstract

The invention provides a block interpenetrating network epoxy resin-silicone rubber modified material with excellent heat resistance, which is prepared from the following raw materials in parts by weight: 100.00 parts of silicone rubber, difunctional epoxy resin 1.00-20.00 parts, 3.00-50.00 parts of hydrogen-containing silicone oil, 0.10-10.00 parts of epoxy curing agent, 0-1.00 parts of rubber additive, wherein the bifunctional epoxy resin contains both epoxy groups and vinyl groups. The epoxy-silicone rubber modified material prepared by the present invention has a block interpenetrating network structure, which has improved heat resistance, and the system can maintain long-term stability and excellent performance, and can be used in aerospace, electronic information, mechanical equipment and other fields High-temperature resistant coatings, adhesives, potting compounds, rubber and flexible ablation-resistant substrate materials. At the same time, the epoxy-silicone rubber modified material prepared by the present invention is a translucent material, which can be applied to fields with certain requirements for light transmission, and has a wider application range than ordinary opaque epoxy-silicone rubber modified materials. .

Description

technical field [0001] The invention belongs to the field of polymer modified materials, and in particular relates to a bifunctional epoxy resin-silicone rubber block interpenetrating network material and a preparation method thereof. Background technique [0002] Silicone rubber is a polymer elastic material with both inorganic and organic molecular chains. It has unique comprehensive properties, such as heat resistance, hydrophobicity, transparency, weather resistance, ozone aging resistance, etc., especially its heat resistance The properties make it widely used in aviation, aerospace, artificial intelligence, biomedicine, electrical and electronic, mechanical equipment and organic coating industries and other fields. However, due to the lack of polar groups in the silicone rubber matrix, the intermolecular force is low, the cohesive strength is low, and it is prone to deformation and failure under the action of external force, resulting in low tensile strength, which gre...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L83/07C08L63/00C08L83/05
CPCC08L83/04C08L2201/08C08L2205/025C08L2205/03C08L2205/04C08L63/00
Inventor 邹华维汪远陈洋梁梅
Owner SICHUAN UNIV
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