A kind of room temperature curing high temperature resistant epoxy resin adhesive and its preparation method and application
A technology of epoxy resin and epoxy resin matrix, which is applied in the direction of in-line phenolic epoxy resin adhesive, non-polymer adhesive additive, adhesive additive, etc. Effect
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[0068] Preparation of amino compounds containing meta-carborane in structure A: Add 1 part of meta-carborane to 2 parts of NaN under the protection of nitrogen flow 3 in toluene, stirred at 110°C and refluxed for 4h, filtered to remove excess NaN 3 And wash the filtrate with distilled water. Under the protection of nitrogen flow, the mixture was stirred and heated at 60°C for 2 hours. The reaction mixture was poured into ice water, the pH value of the mixture was adjusted to neutral with lye and extracted with ether, and anhydrous MgSO was added. 4 After removing the distilled water, the amino compound containing m-carborane with the structure shown in formula (A): diamino-m-carborane can be obtained.
[0069] The preparation of the amino compound containing m-carborane in structure B: (1) dissolve the m-carborane of 1 part of substance in the dry ethylene glycol dimethyl ether of 10 parts by volume, in an ice-water bath Under the protection of nitrogen atmosphere, add dropw...
Embodiment 1
[0072] Use novolac epoxy resin F51 as the epoxy resin matrix, add zinc oxide and sericite as heat-resistant fillers, the mass ratio of novolac epoxy resin F51 to zinc oxide and sericite is 100:10:20, and mix them evenly with a planetary mixer as A component.
[0073] Introduce the prepared diamine-based meta-carborane of the A structure into the 593 curing agent based on the adduct of diethylenetriamine and propylene oxide butyl ether, the 593 curing agent and the diamine-based meta-carborane The mass ratio of carborane is 100:60, and it is uniformly mixed by a planetary mixer as component B.
[0074] When in use, mix components A and B at a mass ratio of 100:100, and obtain a cured product of a high-temperature-resistant epoxy resin adhesive after 7 days at room temperature.
[0075] The cured product has a mass retention rate of 70% at 800°C in an air atmosphere ( figure 1 Curve b) in .
[0076] Using the cured product of the epoxy resin adhesive obtained in this example ...
Embodiment 2
[0078] Use novolac epoxy resin F44 as the epoxy resin matrix, add cerium oxide and sepiolite as heat-resistant fillers, the mass ratio of novolac epoxy resin F44 to cerium oxide and sepiolite is 100:20:10, and mix through a planetary mixer After homogenization, it will be used as A component.
[0079] Introduce the bis (m-aminophenyl) m-position carborane in the prepared B structure in the 590 curing agent based on the adduct of m-phenylenediamine and phenyl glycidyl ether, 590 curing agent and bis (m- The mass ratio of aminophenyl)-m-carborane is 100:10, and it is uniformly mixed as component B through a planetary mixer.
[0080] When in use, the mass ratio of component A and component B is mixed at a ratio of 100:50, and the cured product of the high temperature resistant epoxy resin adhesive is obtained after 3 days at room temperature.
[0081] The cured product has a mass retention rate of 65% at 800°C in an air atmosphere ( figure 1 Curve c) in .
[0082] Using the cu...
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