IP Library Granted Patent US 8,974,863
Granted Patent B2
US 8,974,863 · App. 13/499,800 · Granted Mar 10, 2015

Method for producing fiber-reinforced composite material, and heat-resistant mold material and heat-resistant structural material using the fiber-reinforced composite material

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Quick Facts
Patent No.
US 8,974,863
App. No.
13/499,800
Granted
Mar 10, 2015
Kind
B2
Abstract

A method for producing a fiber-reinforced composite material having high mechanical properties and high heat resistance, and allowing the use of a gypsum die in primary curing, wherein a fiber-reinforced prepreg, obtained by impregnating reinforcing fibers with an epoxy resin composition comprising a triphenylmethane-type epoxy resin, N,N,N′,N′-tetraglycidyldiaminodiphenylmethane (B) and diaminodiphenylsulfone (C), is subjected to primary curing at 110-130° C., and then to secondary curing at a temperature which is at least as high as the primary curing temperature.

Claims (31)

1. A method for producing a fiber-reinforced composite material, the method comprising:

(I) impregnating a fiber substrate comprising reinforcing fibers with an epoxy resin composition, to obtain a fiber-reinforced prepreg;

(II) curing the fiber-reinforced prepreg at a primary curing temperature in a range from 110-130° C., to obtain a primary fiber-reinforced composite material; and then

(III) curing the primary fiber-reinforced composite material at a secondary curing temperature, which is at least as high as the primary curing temperature, to obtain the fiber-reinforced composite material,

wherein the epoxy resin composition comprises:

(A) a triphenylmethane epoxy resin of formula 1:

(B) an N,N,N′,N′-tetraglycidyldiaminodiphenylmethane;

(C) a diaminodiphenylsulfone in an amount such that a ratio of amine equivalents to epoxy equivalents in the epoxy resin composition is from 0.8 to 1.2; and

(D) silica in an amount of 1 to 20 parts by mass with respect to 100 parts by mass of the sum of the triphenylmethane epoxy resin of formula 1 and the N,N,N′,N′-tetraglycidyldiaminodiphenylmethane.

2. The method of claim 1 , wherein the secondary curing temperature is 180° C. or higher.

3. The method of claim 2 , wherein the secondary curing temperature is no higher than 300° C.

4. The method of claim 1 , wherein the fiber substrate comprises carbon fibers.

5. The method of claim 1 , wherein the fiber substrate is a woven fabric.

6. The method of claim 1 , wherein the fiber substrate comprises a chopped material.

7. The method of claim 1 , wherein the curing (II) is carried out in a mother die, and

the method further comprises, after the curing (II), removing the primary fiber-reinforced composite material from the mother die,

wherein the curing (III) is carried out in a free standing state, thereby obtaining the fiber-reinforced composited material in the form of a heat-resistant mold material.

8. The method of claim 1 , wherein the curing (II) is carried out in a mother die, and

the method further comprises, after the curing (II), removing the primary fiber-reinforced composite material from the mother die,

wherein the curing (III) is carried out in a free standing state, thereby obtaining the fiber-reinforced composited material in the form of a heat-resistant structural material.

9. The method of claim 1 , wherein a mass ratio of (A) and (B) in the epoxy resin composition is in a range from 90:10 to 10:90.

10. The method of claim 1 , wherein a mass ratio of (A) and (B) in the epoxy resin composition is in a range from 90:10 to 30:70.

11. The method of claim 1 , wherein a mass ratio of (A) and (B) in the epoxy resin composition is in a range from 80:20 to 10:90.

12. The method of claim 1 , wherein the diaminodiphenylsulfone (C) is a 4,4′-diaminodiphenylsulfone or a 3,3′-diaminodiphenylsulfone.

13. The method of claim 1 , wherein the primary curing temperature is in a range from 110-120° C.

14. The method of claim 1 , wherein the secondary curing temperature is 200° C. or higher.

15. The method of claim 14 , wherein the secondary curing temperature is no higher than 300° C.

16. The method of claim 1 , wherein the secondary curing temperature is no higher than 300° C.

17. The method of claim 1 , wherein the fiber substrate comprises glass fibers.

18. The method of claim 1 , wherein the fiber substrate consists of carbon fibers.

19. The method of claim 1 , wherein (A) and (B) in the epoxy resin are in a mass ratio of 90:10 to 40:60.

Assignments (2)
CHANGE OF NAME Recorded Sep 5, 2017
From: MITSUBISHI RAYON CO., LTD.
To: MITSUBISHI CHEMICAL CORPORATION
Reel/Frame 043750/0834 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 13, 2012
From: MIURA, TEPPEI; KANEKO, MANABU
To: MITSUBISHI RAYON CO., LTD.
Reel/Frame 028367/0958 →