JP2020139169A5 - - Google Patents

Claims (16)

A method for producing an aluminum chelate-based latent curing agent in which the aluminum chelating agent is retained in a porous resin obtained by interfacial polymerization of a polyfunctional isocyanate compound, and the following steps (A) to (C)
(Step A: Particulate hardener preparation step)
The polyfunctional isocyanate compound is interfacially polymerized by heating and stirring the oil phase obtained by dissolving or dispersing the aluminum chelating agent and the polyfunctional isocyanate compound in a volatile organic solvent while putting it into the aqueous phase containing the dispersant. , A step of preparing a particulate curing agent by retaining an aluminum chelating agent in the resulting porous resin;
(Step B: Aluminum chelating agent additional filling step)
The particulate hardener obtained in step A is dispersed and mixed with an aluminum chelating agent solution in which an aluminum chelating agent is dissolved in a volatile organic solvent, and the obtained dispersion mixture is stirred to remove the volatile organic solvent. A step of additionally filling the particulate hardener with an aluminum chelating agent; and (step C: surface activity suppressing treatment step).
The particulate hardener additionally filled with the aluminum chelating agent is stirred in a hydrous alumina sol dispersion to obtain a massive hardener without forming gel-like aggregates, and then primary with the bulk hardener. By crushing into particles, an alumina film is formed on the surface of the particulate hardener to suppress the surface activity of the particulate hardener, thereby obtaining a latent aluminum chelate-based latent hardener. A manufacturing method characterized by having a process. The production method according to claim 1 , wherein the hydrous alumina sol dispersion liquid is a mixture of 1 to 70 parts by mass of an alumina sol and 30 to 99 parts by mass of a water-containing medium. The production method according to claim 2, wherein the alumina sol is obtained by dispersing alumina fibers having an average fiber length of 1 to 10000 nm and an aspect ratio (average fiber length / average fiber width) of 30 to 5000 in a water-containing medium. The production method according to claim 2 or 3 , wherein the alumina fiber content in the alumina sol is 1 to 30% by mass. The production method according to any one of claims 1 to 4 , wherein a silane compound is mixed in the oil phase in the step A. The production method according to claim 5 , wherein the silane compound is triphenylsilanol. The production method according to any one of claims 1 to 6 , wherein the removal of the volatile organic solvent in the step B is performed by heating the dispersed mixture to the boiling point or higher of the volatile organic solvent. The production method according to any one of claims 1 to 7 , wherein the radical polymerizable compound and the radical polymerization initiator are blended in the oil phase in the step A. The production method according to claim 8 , wherein the radically polymerizable compound contains a polyfunctional radically polymerizable compound. The production method according to claim 9 , wherein the radically polymerizable compound contains at least 50% by mass or more of the polyfunctional radically polymerizable compound. The production method according to claim 9 or 10 , wherein the polyfunctional radically polymerizable compound is a polyfunctional vinyl-based compound. The production method according to claim 11 , wherein the polyfunctional vinyl compound is divinylbenzene. The production method according to any one of claims 9 to 12 , wherein the polyfunctional radically polymerizable compound further contains a polyfunctional (meth) acrylate-based compound. The production method according to any one of claims 1 to 13 , wherein the content of the aluminum chelating agent in the oil phase in the step A is 10 to 500 parts by mass with respect to 100 parts by mass of the polyfunctional isocyanate compound. A thermosetting epoxy resin composition containing an aluminum chelate-based latent curing agent, an epoxy resin, and a silane-based compound produced by the production method according to any one of claims 1 to 14 . The thermosetting epoxy resin composition according to claim 15 , wherein the silane compound is triphenylsilanol.