Process for producing modified epoxy resin
View Patent ↗This invention provides a process for producing an epoxy resin composition having core/shell rubber particles (rubber-like polymer particles) dispersed in an epoxy resin, wherein an epoxy resin composition excellent in the dispersed state of rubber-like polymer particles in an epoxy resin with a reduced amount of contaminants is produced easily and efficiently. The epoxy resin composition having rubber-like polymer particles dispersed well in an epoxy resin with less contaminant is obtained by bringing an aqueous latex of rubber-like polymer particles (B) into contact with an organic medium (C) showing partial solubility in water, then bringing an organic medium (D) having lower partial solubility in water than that of the organic medium (C) into contact therewith to separate water substantially, to remove the rubber-like polymer particles as a dispersion (F) having the polymer particles dispersed in the organic medium, and mixing it with an epoxy resin (A), followed by distilling volatile components away.
1. A process for producing a curable epoxy resin composition comprising polymer particles (B) and a curable epoxy resin (A),
the polymer particles (B) comprising 5 to 50% by weight of a shell layer (B-2) and 50 to 95% by weight of a rubber particle core (B-1), and
the polymer particles (B) being in an independently dispersed state of substantially primary particles in the epoxy resin (A);
the process comprising the steps of
bringing an organic medium (C) showing partial solubility in water into contact with an aqueous latex of polymer particles (B),
then bringing an organic medium (D) having lower partial solubility in water than that of (C) into contact therewith to separate an aqueous layer substantially from the polymer particles (B),
discharging the aqueous layer to obtain a dispersion (F) consisting essentially of the polymer particles (B) and the mixed organic mediums (C) and (D), without isolating the polymer particles (B) as a coagulated material,
dissolving a curable epoxy resin (A) in the dispersion (F), and
removing volatile components; and
the polymer particles (B) being in an independently dispersed state of substantially primary particles in the dispersion (F).
2. The process for producing a curable epoxy resin composition according to claim 1 ,
wherein
after the organic medium (C) showing partial solubility in water is brought into contact with the aqueous latex of polymer particles (B) and then the organic medium (D) having lower partial solubility in water than that of (C) is brought into contact therewith to separate an aqueous layer substantially from the polymer particles (B), and
before the dispersion (F) is mixed with the curable epoxy resin (A), the dispersion (F) is washed by bringing it at least once into contact with water.
3. The process for producing a curable epoxy resin composition according to claim 1 , wherein the partial solubility of the organic medium (C) in water is defined as follows: a solubility of water in the organic medium (C) at 25° C. is 9 to 40% by weight.
4. The process for producing a curable epoxy resin composition according to claim 1 ,
wherein the organic mediums (C) and (D) are a combination not forming two-component azeotropic mixture.
5. The process for producing a curable epoxy resin composition according to claim 1 ,
wherein the polymer particles (B) are obtained by graft-polymerizing 5 to 50% by weight of the shell layer (B-2) comprising at least one monomer selected from the group consisting of (meth)acrylates, aromatic vinyls, vinyl cyanides, unsaturated acid derivatives, (meth)acrylamide derivatives and maleimide derivatives,
with 50 to 95% by weight of the rubber particle core (B-1)
comprising a rubber elastic body composed of
not less than 50% by weight of at least one monomer selected from the group consisting of diene monomers and (meth)acrylate monomers and
less than 50% by weight of another copolymerizable vinyl monomer, or a polysiloxane rubber elastic body, or a mixture thereof.
6. The process for producing a curable epoxy resin composition according to claim 5 ,
wherein the shell layer (B-2) in the polymer particle (B) comprises a monomer having reactivity with an epoxy resin or a curing agent.
7. A curable epoxy resin composition obtained by the process described in claim 1 .
8. A cured molded product comprising the curable epoxy resin composition of claim 7 cured with a curing agent.
9. A dispersion (F) consisting essentially of polymer particles (B) and mixed organic mediums (C) and (D),
the polymer particles (B) comprising 5 to 50% by weight of a shell layer (B-2) and 50 to 95% by weight of a rubber particle core (B-1), and
the polymer particles (B) being in an independently dispersed state of substantially primary particles in the dispersion (F);
wherein the dispersion (F) is obtained by bringing an organic medium (C) showing partial solubility in water into contact with an aqueous latex of polymer particles (B),
bringing an organic medium (D) having lower partial solubility in water than that of (C) into contact therewith to separate an aqueous layer substantially from the polymer particles (B), and
discharging the aqueous layer to obtain the dispersion (F) without isolating the polymer particles (B) as a coagulated material.