Process for the purification of a crude carboxylic acid slurry

• US 7,132,566 B2
• Filed: 09/22/2003
• Issued: 11/07/2006
• Est. Priority Date: 09/22/2003
• Status: Active Grant

• Current Assignee: Alpek Polyester SA de CV
• Original Assignee: Eastman Chemical Company
• Inventors: Arnold, Ernest William, Gibson, Philip Edward, Lin, Robert, Sumner, Charles Edwan Jr., Fugate, Eric Jackson
• Primary Examiner(s): OH, TAYLOR V
• Application Number:
  US10/667,744
• Publication Number:
  US 20050065373A1
• Time in Patent Office: 1,142 Days
• Field of Search: 562/416, 562/486, 562/485, 562/487
• US Class Current: 562/486
• CPC Class Codes: C07C 51/43 by change of the physical state, e.g. crystallisation
• CPC Class Codes: C07C 51/47 by solid-liquid treatment; by chemisorption
• CPC Class Codes: C07C 51/487 by treatment giving rise to chemical modification by chemisorption C07C51/47
• CPC Class Codes: C07C 63/26 1,4 - Benzenedicarboxylic acid

Abstract

Disclosed is a process to produce a purified carboxylic acid product. The process comprises removing impurities from a crude carboxylic acid slurry in a solid-liquid displacement zone to form a slurry product. The slurry product if further treated in a staged oxidation zone and a crystallization zone to from a crystallized product. The crystallized product is further cooled in a cooling zone and subsequently filtered and dried in a filtration and drying zone. The process produces purified carboxylic acid product having good color and low impurity levels without the use of purification steps like hydrogenation.

Claims

1. A process to produce a purified carboxylic acid composition comprising:

(a) oxidizing an aromatic feed stock in a primary oxidation zone at an oxidizing temperature to form a crude carboxylic acid slurry composition;

wherein said crude carboxylic acid slurry composition comprises at least one carboxylic acid;

wherein there is less than 5% by weight terephthalic acid and isophthalic acid in said crude carboxylic acid slurry composition;

(b) removing in a solid-liquid displacement zone impurities from said crude carboxylic acid slurry composition to form a slurry composition; and

wherein said

impurities comprise 4-carboxybenzaldehyde, trimellitic acid, or 2,6-dicarboxyfluorenone;

(c) oxidizing said slurry composition in a staged oxidation zone to form a staged oxidation composition;

wherein said oxidizing is conducted at an oxidizing temperature between about 190°

C. to about 280°

C.;

wherein said oxidizing temperature in said staged oxidation zone is higher than the oxidizing temperature in said primary oxidation zone;

(d) crystallizing said staged oxidation composition in a crystallization zone to form a crystallized composition;

(e) cooling said crystallized composition in a cooling zone to form a cooled purified carboxylic acid slurry composition; and

(f) filtering and optionally drying said cooled purified carboxylic slurry composition in a filtration and drying zone to produce said purified carboxylic acid composition.

2. The process according to claim 1 further comprising decolorizing in a reactor zone said purified carboxylic acid slurry composition or a carboxylic acid that has been esterified.

3. The process according to claim 2 wherein said decolorizing is accomplished by reacting said crude carboxylic acid slurry composition with hydrogen in the presence of a hydrogenation catalyst in said reactor zone to produce a decolorized carboxylic acid composition.

4. The process according to claim 1 wherein said solid-liquid displacement zone comprises a solid-liquid separator that is operated at a temperature between about 50°

C. to about 200°

C.

5. The process according to claim 1 wherein said purified carboxylic acid slurry composition has a b* of less than about 4.5.

6. The process according to claim 1 wherein said oxidizing in said primary oxidation zone is conducted in the presence of a catalyst that comprises cobalt, manganese and bromine compounds.

7. The process according to claim 6 wherein the cobalt and manganese are present in concentrations of about 1050 ppm to about 2700 ppm by weight in the crude carboxylic acid slurry composition and bromine is present at a concentration of about 1000 ppm to about 2500 ppm by weight in the crude carboxylic acid slurry composition.

8. A process to produce a purified carboxylic acid composition comprising:

(a) oxidizing an aromatic feed stock in a primary oxidation zone at an oxidizing temperature to form a crude carboxylic acid slurry composition;

wherein said crude carboxylic acid slurry composition comprises at least one carboxylic acid;

wherein said oxidizing is conducted at a temperature between about 120°

C. to about 200°

C.; and

wherein there is less than 5% by weight terephthalic acid and isophthalic acid in said crude carboxylic acid slurry composition;

(b) removing in a solid-liquid displacement zone impurities from said crude carboxylic acid slurry composition to form a slurry composition; and

wherein said impurities comprise 4-carboxybenzaldehyde, trimellitic acid, or 2,6-dicarboxyfluorenone;

(c) oxidizing said slurry composition in a staged oxidation zone to form a staged oxidation composition;

wherein said oxidizing is conducted at a temperature between about 190°

C. to about 280°

C.;

wherein said oxidizing temperature in said staged oxidation zone is higher than the oxidizing temperature in said primary oxidation zone;

(d) crystallizing said staged oxidation composition in a crystallization zone to form a crystallized composition;

(e) cooling said crystallized composition in a cooling zone to form a cooled purified carboxylic acid slurry composition; and

(f) filtering and optionally drying said cooled purified carboxylic acid slurry in a filtration and drying zone to produce said purified carboxylic acid composition.

9. The process according to claim 8 further comprising decolorizing in a reactor zone said purified carboxylic acid slurry composition or a carboxylic acid that has been esterified.

10. The process according to claim 9 wherein said decolorizing is accomplished by reacting said crude carboxylic acid slurry composition with hydrogen in the presence of a hydrogenation catalyst in said reactor zone to produce a decolorized carboxylic acid composition.

11. The process according to claim 8 wherein said solid-liquid displacement zone comprises a solid-liquid separator that is operated at a temperature between about 50°

C. to about 200°

C.

12. The process according to claim 8 wherein said purified carboxylic acid slurry composition has a b* of less than about 4.5.

13. The process according to claim 8 wherein said oxidizing in said primary oxidation zone is conducted in the presence of a catalyst that comprises cobalt, manganese and bromine compounds.

14. The process according to claim 13 wherein the cobalt and manganese are present in concentrations of about 1050 ppm to about 2700 ppm by weight in the crude carboxylic acid slurry composition and bromine is present at a concentration of about 1000 ppm to about 2500 ppm by weight in the crude carboxylic acid slurry composition.