IP Library Granted Patent US 7,268,192
Granted Patent B2
US 7,268,192 · App. 10/511,553 · Granted Sep 11, 2007

Process for producing high-purity epoxy resin and epoxy resin composition

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Quick Facts
Patent No.
US 7,268,192
App. No.
10/511,553
Granted
Sep 11, 2007
Kind
B2
Abstract

A process for production a high purity epoxy compound with total chlorine content of 500 ppm or less is characterized in that alkali metal hydroxide is added to a bifunctional epoxy compound represented by the general formula (I), in which content of the component with n=0 is not less than 70% and less than 100%, and that reaction is caused to take place at a temperature of 95-150° C. to produce a multi-functional epoxy compound represented by the general formula (II)

Claims (31)

1. A process for production of a high-purity epoxy compound with total chlorine content of less than 500 ppm, said process comprising:

reacting an epoxy compound according to formula (I):

wherein,

R represents a dihydric phenol compound residue and/or a dihydric alcohol compound residue, and

n represents a numerical value with the average greater than 0 and not greater than 10, in which the proportion of the component having n equal to 0 is more than 70% and less than 100%,

in the presence of alkali metal hydroxide at temperature of 95° C.-150° C., to produce an epoxy compound according to formula (II):

wherein,

R represents a dihydric phenol compound residue and/or a dihydric alcohol compound residue,

n represents a numerical value with the average greater than 0 and not greater than 10, and

X is a hydrogen atom or a group according to formula (III):

wherein,

R has the above-described meaning in which the component with X represented by the-general formula (III) is always contained.

2. A process according to claim 1 , wherein the resultant epoxy compound obtained by the process contains the epoxy compound of formula (I) in the proportion of not less than 90% and less than 100%, and the epoxy compound of formula (II) in the proportion of greater than 0% and not greater than 10%.

3. A process according to claim 1 , wherein said alkali metal hydroxide is potassium hydroxide.

4. A process according claim 1 , wherein 5-100 g of potassium hydroxide is used per 1 kg of said epoxy compound of formula (I), and is used in the reaction in the form of aqueous solution of potassium hydroxide of 80% or higher in concentration.

5. A process according to claim 1 , wherein the reaction is conducted in the presence of a tertiary alcohol.

6. A process according to claim 1 , wherein said epoxy compound of formula (I) is an epoxy compound according to formula (IV):

wherein,

R 1 -R 8 may be same or different, and each of R 1 -R 8 is a hydrogen, alkyl, allyl, phenyl group or halogen atoms,

Y represents a direct bond, alkyl group with carbon number of 1-20, allyl, phenyl, aralkyl, biphenylaralkyl, oxygen, sulphur, sulfone, or carboxyl group; and

n is a numerical value with average greater than 0 and not greater than 10; and/or an epoxy compound according to formula (V):

wherein,

R 1 , R 2 , R 5 , and R 6 represent hydrogen, alkyl, allyl, phenyl group, or halogen atom, and may be same or different; and

n is a numerical value with average greater than 0 and not greater than 10.

7. A process for according to claim 6 , wherein said epoxy compound of formula (IV) is a tetramethyl bisphenol epoxy resin or a tetramethyl biphenyl epoxy resin.

8. A process according to claim 1 , wherein the resultant epoxy compound obtained by the process has a total chlorine content of less than 350 ppm.

9. A process according to claim 1 , wherein, for the epoxy of the compound of Formula (I) that is to be reacted, the proportion of the epoxy compound having n equal to 0 is 75%-99%.

10. A process according to claim 1 , wherein, for the epoxy of the compound of Formula (I) that is to be reacted, the proportion of the epoxy compound having n equal to 0 is 80%-99%.

11. A process according to claim 2 , wherein the resultant epoxy compound obtained by the process contains the epoxy compound of formula (II) in an amount of 1-10%.

12. A process according to claim 11 , wherein the resultant epoxy compound obtained by the process contains the epoxy compound of formula (II) in an amount of 1-6%.

13. A process according to claim 12 , wherein the resultant epoxy compound obtained by the process contains the epoxy compound of formula (II) in an amount of 2-5%.

Assignments (6)
CHANGE OF NAME Recorded Mar 20, 2013
From: NIPPON STEEL CHEMICAL CO., LTD.
To: NIPPON STEEL & SUMIKIN CHEMICAL CO., LTD.
Reel/Frame 030049/0771 →
CORRECTIVE ASSIGNMENT TO CORRECT THE ASSIGNOR'S NAME PREVIOUSLY RECORDED ON REEL 026370 FRAME 0302. ASSIGNOR(S) HEREBY CONFIRMS THE CORRECT ASSIGNOR SHOULD BE LISTED AS TOTO KASEI CO., LTD. (ALSO DESCRIBED AS TOHTO KASEI CO., LTD.). Recorded Jun 24, 2011
From: TOTO KASEI CO., LTD. (ALSO DESCRIBED AS TOHTO KASEI CO., LTD.)
To: NIPPON STEEL CHEMICAL CO., LTD.
Reel/Frame 026499/0604 →
CORRECTIVE ASSIGNMENT TO CORRECT THE TYPOGRAPHICAL ERROR IN NAME AND ADDRESS SPELLING OF ASSIGNEE PREVIOUSLY RECORDED ON REEL 024160 FRAME 0714. ASSIGNOR(S) HEREBY CONFIRMS THE CORRECT SPELLING AS NIPPON STEEL CHEMICAL CO., LTD. OF 14-1, SOTOKANDA 4-CHOME, CHIYODA-KU, TOKYO, JAPAN. Recorded Jun 1, 2011
From: TOTO KASEI CO. LTD.
To: NIPPON STEEL CHEMICAL CO., LTD.
Reel/Frame 026370/0302 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 31, 2010
From: TOTO KASEI CO., LTD.
To: NIPPON STEEL CHEMICALS CO., LTD.
Reel/Frame 024160/0714 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 3, 2007
From: TOHTO KASEI CO., LTD.
To: TOHTO KASEI CO., LTD.
Reel/Frame 019579/0874 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 18, 2004
From: ASAKAGE, HIDEYASU; SAITO, NOBUHISA; NAKAMURA, YUKIO
To: TOHTO KASEI CO., LTD.
Reel/Frame 016336/0858 →