# US 5,344,969 A · Process for purification of naphthalenedicarboxylic acid

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- Number: US 5,344,969 A
- Document ID: US5344969A
- Status: Granted
- Kind: A
- Application number: 07/983,411
- Filed: 1992-11-30
- Granted: 1994-09-06
- Earliest claimed: 1991-12-03
- Assignees: Mitsubishi Petrochemical Co., Ltd.
- Inventors: Hiroshi Iwane; Takahiro Sugawara; Miwa Shirasaki
- Web page: https://patentgrep.com/patent/US5344969A

## CPC

- C07C 51/43: by change of the physical state, e.g. crystallisation
- C07C: ACYCLIC OR CARBOCYCLIC COMPOUNDS

## Abstract

A process for purifying a crude naphthalenedicarboxylic acid containing impurities and coloring substances obtained by the oxidation of a di-substituted naphthalene, dispense with the use of a large amount of alkali or acid, and producing a naphthalenedicarboxylic acid having a high purity and good color effectively and in a high recovery is disclosed, which comprises dissolving the crude naphthalenedicarboxylic acid in a mixed solvent comprising an amine compound and an alcohol and conducting crystallization.

## Claims

### Claim 1

A process for producing a naphthalenedicarboxylic acid which comprises dissolving a crude naphthalenedicarboxylic acid in a mixed solvent comprising an amine compound and an alcohol and conducting crystallization, said crude naphthalenedicarboxylic acid being one obtained by the oxidation of a di-substituted naphthalene, wherein the proportion of the amine compound to the alcohol in the mixed solvent is in the range of from 1:99 to 99:1 by weight, and wherein the mixed solvent is used in an amount from 0.5 to 100 times by weight the amount of the crude naphthalenedicarboxylic acid.

### Claim 2 (depends on 1)

A process as claimed in claim 1, wherein said alcohol is an aliphatic monohydric alcohol.

### Claim 3 (depends on 1)

A process as claimed in claim 1, wherein the dissolution of the crude naphthalenedicarboxylic acid is conducted at a temperature of from 0.degree. to 350.degree. C.

### Claim 4 (depends on 1)

A process as claimed in claim 1, wherein the crystallization is conducted after the solution prepared by dissolving the crude naphthalenedicarboxylic acid is treated with active carbon.

### Claim 5 (depends on 1)

A process as claimed in claim 1, wherein the di-substituted naphthalene is a 2,6-substituted naphthalene or a 2,7-substituted naphthalene.

### Claim 6 (depends on 1)

A process as claimed in claim 1, wherein the amine compound is an alkylamine having up to 30 carbon atoms.

### Claim 7

A process for producing a high-purity naphthalenedicarboxylic acid which comprises dissolving a crude naphthalenedicarboxylic acid in a mixed solvent comprising an amine compound and an alcohol and then cooling the resulting solution to a temperature lower by at least 30.degree. C. than the temperature at which the crude naphthalenedicarboxylic acid was dissolved in the mixed solvent, thereby to precipitate an amine salt of the naphthalenedicarboxylic acid, wherein the proportion of the amine compound to the alcohol in the mixed solvent is in the range of from 1:99 to 99:1 by weight, and wherein the mixed solvent is used in an amount from 0.5 to 100 times by weight the amount of the crude naphthalenedicarboxylic acid.

### Claim 8 (depends on 7)

A process as claimed in claim 7, wherein the precipitation is conducted at a temperature of from -30.degree. to 100.degree. C.

### Claim 9 (depends on 7)

A process as claimed in claim 7, which further comprises heating the precipitated amine salt to a temperature not lower than the boiling point of the amine thereby to obtain the naphthalenedicarboxylic acid.

### Claim 10 (depends on 7)

A process as claimed in claim 7, which further comprises adding an acid to the precipitated amine salt thereby to obtain the naphthalenedicarboxylic acid.

### Claim 11 (depends on 10)

A process as claimed in claim 10, wherein the acid is added in an amount of from 0.1 to 10 mol per mol of the amine salt.

### Claim 12 (depends on 10)

A process as claimed in claim 10, wherein the acid to be added is an aliphatic carboxylic acid.

### Claim 13

A process for producing a high-purity naphthalenedicarboxylic acid which comprises dissolving a crude naphthalenedicarboxylic acid in a mixed solvent comprising an amine compound and an alcohol and then adding an acid to the resulting solution thereby to precipitate the naphthalenedicarboxylic acid.

### Claim 14 (depends on 13)

A process as claimed in claim 13, wherein the acid is added in an amount from 0.1 to 10 times by weight the amount of the amine contained in the solution.

### Claim 15 (depends on 13)

A process as claimed in claim 13, wherein the precipitation is conducted at a temperature of from 0.degree. to 40.degree. C.

### Claim 16 (depends on 13)

A process as claimed in claim 13, wherein the acid is an aliphatic carboxylic acid.