Powdery adhesive and process for preparation thereof

• US 4,959,398 A
• Filed: 02/13/1989
• Issued: 09/25/1990
• Est. Priority Date: 02/13/1989
• Status: Expired due to Fees

• Current Assignee: Toray Industries Incorporated
• Original Assignee: Toray Industries Incorporated
• Inventors: Hagiwara, Ikuo, Oka, Koichiro
• Primary Examiner(s): Kight, III, John
• Assistant Examiner(s): ACQUAH, SAMUEL A
• Application Number:
  US07/310,171
• Time in Patent Office: 589 Days
• Field of Search: 523/460, 523/407, 523/414, 523/420, 523/466, 428/403, 428/407, 528/88, 528/93, 528/111, 528/118, 528/119, 528/124
• US Class Current: 523/400
• CPC Class Codes: C08G 59/18 Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
• CPC Class Codes: C08L 2666/08 Homopolymers or copolymers according to C08L7/00 - C08L21/00; Derivatives thereof
• CPC Class Codes: C09J 163/00 Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
• CPC Class Codes: Y10T 428/2991 Coated
• CPC Class Codes: Y10T 428/2998 including synthetic resin or polymer

Abstract

A powdery adhesive comprised of spherical particles comprising 40 to 90 parts by weight of an epoxy resin component, 10 to 60 parts by weight of a rubber component and a latent curing agent contained inside the particles, the average particle size of the particles being from 0.1 to 500 μm. The powdery adhesive may be prepared by a process comprising a step of preparing a compatible mixture comprising an epoxy resin component, a rubber component and a common organic solvent, a step of emulsifying or suspending the compatible mixture in an aqueous medium to form spherical particles, and a step of causing a phase separation of the epoxy resin component and the rubber component in the spherical particles.

Claims

1. A powdery adhesive comprised of spherical particles comprising 40 to 90 parts by weight of an epoxy resin component and 10 to 60 parts by weight of a rubber component, said spherical particles containing up to about 15 parts by weight of a latent curing agent for the epoxy resin component per 100 parts of the total weight of the epoxy resin component and the rubber component, wherein the average particle size of the particles is from 0.1 to 500 μ

m.

2. A powdery adhesive as claimed in claim 1, wherein the epoxy resin component comprises 50 to 80% by weight and the rubber component comprises 20 to 50% by weight.

3. A powdery adhesive as claimed in claim 1, wherein the epoxy resin has at least 2 epoxy groups in the molecule.

4. A powdery adhesive as claimed in claim 1, wherein the rubber component is soluble in an organic solvent.

5. A powdery adhesive as claimed in claim 1, wherein the rubber component has a epoxy or glycidyl group.

6. A powdery adhesive as claimed in claim 1, wherein the latent curing agent is selected from bisphenols and condensates thereof.

7. A powdery adhesive as claimed in claim 1, wherein the amount of the latent curing agent is 0.05 to 1 equivalent per equivalent of the epoxy groups of the epoxy resin.

8. A powdery adhesive as claimed in claim 1, wherein the epoxy resin component and the rubber component are present in a phase-separated structure.

9. A powdery adhesive as claimed in claim 1, wherein the epoxy resin is partially cured.

10. A powdery adhesive as claimed in claim 1, wherein the particle size is 0.5 to 200 μ

m and the variation of the particle size is within 30%.

11. A process for the preparation of a powdery adhesive, which comprises a step of preparing a compatible mixture comprising an epoxy resin component, a rubber component and a common organic solvent for said epoxy resin and rubber components, wherein said epoxy resin component 40 to 90 parts by weight and said rubber components comprises 10 to 60 parts by weight, said mixture contains up to about 15 parts by weight of a latent curing agent for the epoxy resin component per 100 parts of the total weight of the epoxy resin component and the rubber component;

a step of emulsifying or suspending the compatible mixture in an aqueous medium, whereby spherical particles composed of said mixture being formed;

a step of removing the organic solvent from the mixture, whereby causing a phase separation of the epoxy resin component and the rubber component in the spherical particles; and

a step of collecting said spherical particles.

12. A process according to claim 11, wherein the organic solvent has a boiling point lower than 100°

C. and is water-insoluble.

13. A process according to claim 12, wherein the organic solvent is selected from chloroform, methylene chloride, carbon tetrachloride, ethyl ether, ethyl acetate and benzene.

14. A process according to claim 11, wherein the compatible mixture is emulsified or suspended by using a surface active agent.

15. A process according to claim 14, wherein the aqueous medium is gradually added to the compatible mixture while strongly stirred, or the compatible mixture is gradually added to the aqueous medium while strongly stirred.

16. A process according to claim 15, wherein a water-in-oil type emulsion is first formed and then converted to an oil-in-water type emulsion.

17. A process for the preparation of a powdery adhesive, which comprises a step of preparing a compatible mixture comprising an epoxy resin component, a rubber component and a common organic solvent for said epoxy resin and rubber components, wherein said epoxy resin component comprises 40 to 90 parts by weight and said rubber component comprises 10 to 60 parts by weight, a step of emulsifying or suspending the compatible mixture in an aqueous medium, whereby spherical particles composed of said mixture being formed, a step of removing the organic solvent from the mixture, whereby causing a phase separation of the epoxy resin component and the rubber component in the spherical particles, a step of adding an amine type curing agent to the emulsion or suspension, whereby partially curing the epoxy resin component in the spherical particles so that at least surface of the spherical particles loses stickiness, and a step of collecting said spherical particles.

18. A process according to claim 17, wherein the compatible mixture contains a latent curing agent for the epoxy resin component.

19. A process according to claim 17, wherein the organic solvent has a boiling point lower than 100°

C. and is water-insoluble.

20. A process according to claim 19, wherein the organic solvent is selected from chloroform, methylene chloride, carbon tetrachloride, ethyl ether, ethyl acetate and benzene.

21. A process according to claim 17, wherein the compatible mixture is emulsified or suspended by using a surface active agent.

22. A process according to claim 21, wherein the aqueous medium is gradually added to the compatible mixture while strongly stirred, or the compatible mixture is gradually added to the aqueous medium while strongly stirred.

23. A process according to claim 22, wherein a water-in-oil type emulsion is first formed and then converted to an oil-in-water type emulsion.