Production of non-solid-stated polyester particles having solid-stated properties

• US 7,868,125 B2
• Filed: 02/27/2009
• Issued: 01/11/2011
• Est. Priority Date: 03/03/2008
• Status: Active Grant

• Current Assignee: Alpek Polyester SA de CV
• Original Assignee: Eastman Chemical Company
• Inventors: Wabshall, John Alan Jr., Stafford, Steven Lee, Wonders, Alan George, Estep, Robert Noah, Maddox, Tommy Ray II, Weinhold, Stephen, DeBruin, Bruce Roger, Jernigan, Mary Therese, Bellner, Steven Paul, Franjione, John Guy
• Primary Examiner(s): Boykin; Terressa M
• Application Number:
  US12/394,478
• Publication Number:
  US 20090221785A1
• Time in Patent Office: 683 Days
• Field of Search: 422/245.1, 422/255, 422/261, 528/481, 528/499, 528/502.R
• US Class Current: 528/274
• CPC Class Codes: B29B 2009/165 Crystallizing granules
• CPC Class Codes: B29B 9/065 under-water, e.g. underwater pelletizers
• CPC Class Codes: B29B 9/12 characterised by structure or composition
• CPC Class Codes: B29B 9/16 Auxiliary treatment of granules
• CPC Class Codes: C08G 63/90 Purification; Drying
• CPC Class Codes: C08J 2367/02 Polyesters derived from dicarboxylic acids and dihydroxy compounds; C08J2367/06 takes precedence
• CPC Class Codes: C08J 3/122 Pulverisation by spraying
• CPC Class Codes: F26B 17/24 with movement performed by shooting or throwing the materials , e.g. after which the materials are subject to impact F26B17/108 takes precedence
• CPC Class Codes: F26B 5/08 by centrifugal treatment
• CPC Class Codes: Y10T 428/2998 including synthetic resin or polymer

Abstract

A process for producing non-solid-stated polyester polymer particles having one or more properties similar to polyester polymer particles that have undergone solid-state processing. In one embodiment, the process comprises (a) forming polyester polymer particles from a polyester polymer melt; (b) quenching at least a portion of the particles, (c) drying at least a portion of the particles, (d) crystallizing at least a portion of the particles, (e) annealing at least a portion of the particles. At all points during and between steps (b) through (e), the average bulk temperature of the particles is maintained above 165° C.

Claims

1. A polyester polymer production process comprising:

(a) forming polyester polymer particles from a polyester polymer melt in a particle forming zone;

(b) subsequent to step (a), quenching at least a portion of said particles via contact with a quench liquid in a quenching zone;

(c) subsequent to step (b), drying at least a portion of said particles in a drying zone;

(d) subsequent to step (c), crystallizing at least a portion of said particles in a crystallizing zone; and

(e) subsequent to step (d), annealing at least a portion of said particles in an annealing zone wherein said particles have a residence time in said annealing zone of between 1 hour and 24 hours,

wherein at all points during and between steps (b) through (e) the average bulk temperature of said particles is maintained above 165°

C., wherein the It.V. of said particles produced from said particle forming zone is within about 5 percent of the It.V. of said particles produced from said annealing zone, and wherein said polyester polymer melt comprises a carboxylic acid component and a hydroxyl component, wherein said carboxylic acid component comprises at least 80 mole percent of the residues of terephthalic acid and/or derivatives thereof, wherein said hydroxyl component comprises at least 80 mole percent of residues of ethylene glycol.

2. The process of claim 1, wherein said polyester polymer melt has an intrinsic viscosity (It.V.) in the range of 0.70 dL/g to 1.20 dL/g when measured at 25°

C. in a 60/40 wt/wt phenol/tetrachloroethane solvent at a polymer concentration of 0.50 g/100 ml.

3. The process of claim 1, wherein said particles produced from said annealing zone, when measured on a first heating DSC scan, have a low melting peak temperature greater than 190°

C., and a melting endotherm area greater than the absolute value of 4 J/g.

4. The process of claim 1, wherein steps (b) and (c) are carried out in a period of time less than 1 minute, wherein said particles have a residence time in said crystallizing zone of less than 20 minutes.

5. The process of claim 1, wherein said particles introduced into said crystallizing zone have an average bulk temperature in the range of from 170°

C. to 210°

C. and wherein said particles produced from said crystallizing zone have an average bulk temperature in the range of from 180°

C. to 220°

C.

6. The process of claim 1, wherein the onset-of-melt temperature (T_om) of said particles introduced into said annealing zone is at least 10°

C. lower than the T_om of said particles produced from said annealing zone.

7. The process of claim 1, wherein said particles produced from said annealing zone have a degree of crystallinity less than 42 percent.

8. The process of claim 1, wherein less than 10 BTU of heat per pound of particles is added to said crystallizing zone, and wherein said particles produced from said crystallizing zone have an average bulk temperature that is at least 5°

C. higher than the average bulk temperature of said particles introduced into said crystallizing zone.

9. The process of claim 1, wherein the average bulk temperature of said particles produced from said annealing zone is in the range of from about 0.5°

C. to about 10°

C. lower than the average bulk temperature of said particles introduced into said annealing zone.

10. The process of claim 1, wherein at least a portion of said crystallizing zone is defined in a mechanically agitated crystallizer.

11. The process of claim 1, wherein said particles produced from said annealing zone comprise a shell and a core, wherein said shell substantially surrounds said core, wherein at least a portion of said core was formed via spherulitic crystallization, wherein at least a portion of said shell was formed via strain-induced crystallization, and wherein said particles produced from said annealing zone have a spheroidal shape.

12. The process of claim 1, wherein said particles produced from said annealing zone comprise less than 8 ppm of antimony catalyst.

13. The process of claim 2, wherein said polyester polymer production process is not a solid-stating process.

14. The process of claim 1, wherein the total thermal energy added to said polyester polymer production process between steps (a) and (d) is less than 100 BTU/lb of said particles produced from said annealing zone.

15. The process of claim 1, wherein said particles produced from said annealing zone, when measured on a first heating DSC scan, have an onset-of-melt temperature greater than 165°

C., and a melting endotherm area greater than the absolute value of 4 J/g.

16. The process of claim 1, wherein the low melting peak temperature of said particles introduced into said annealing zone is at least 10°

C. lower than the low melting peak temperature of said particles produced from said annealing zone.

17. A polyester polymer production process comprising:

(a) forming initial polyester polymer particles from a polymer melt having an intrinsic viscosity (It.V.) in the range of 0.70 dL/g to 1.2 dL/g when measured at 25°

C. in a 60/40 wt/wt phenol/tetrachloroethane solvent at a polymer concentration of 0.50 g/100 ml, wherein said initial particles comprise a shell and a core, wherein said shell is cooler and more crystalline than said core, wherein at least a portion of said shell exhibits strain-induced crystallinity;

(b) drying at least a portion of said initial particles to thereby provide dried particles;

(c) crystallizing at least a portion of said dried particles to thereby provide crystallized particles exhibiting both strain-induced crystallinity and spherulitic crystallinity; and

(d) annealing at least a portion of said crystallized particles to thereby provide annealed particles, wherein said annealing occurs in an annealing zone, wherein the average bulk temperature of said annealed particles exiting said annealing zone is in the range of 170°

C. to 205°

C., and wherein an average particle residence time in said annealing zone is in the range of 1 hour to 24 hours,

wherein the average bulk temperature of said initial particles and said dried particles is maintained above the onset-of-melting temperature (T_om) of said core, and wherein said polymer melt comprises a carboxylic acid component and a hydroxyl component, wherein said carboxylic acid component comprises at least 80 mole percent of the residues of terephthalic acid and/or derivatives thereof, wherein said hydroxyl component comprises at least 80 mole percent of residues of ethylene glycol, and wherein the It.V. of said initial particles is within about 5 percent of the It.V. of said annealed particles.

18. The process of claim 17, wherein the average bulk temperature of said initial particles, said dried particles, and said crystallized particles is maintained at a temperature greater than 165°

C.

19. The process of claim 17, wherein said annealed particles, when measured on a first heating DSC scan, have a low melting peak temperature greater than 190°

C., and a melting endotherm area greater than the absolute value of 4 J/g.

20. The process of claim 17, further comprising, prior to step (b), quenching at least a portion of said initial particles via contact with a quench liquid to thereby provide quenched particles, wherein said initial particles dried in step (b) comprise at least a portion of said quenched particles, and wherein said quenching is carried out in less than 30 seconds.

21. The process of claim 17, wherein said crystallized particles have an average bulk temperature greater than 180°

C., and wherein said particles have an average residence time in said crystallizing zone of less than 20 minutes.

22. The process of claim 17, wherein said annealed particles have an average bulk temperature that is in the range of from about 0.5°

C. to about 10°

C. less than the average bulk temperature of said crystallized particles.

23. The process of claim 17, wherein said annealed particles comprise less than 8 ppm of antimony catalyst.

24. The process of claim 17, wherein said annealed particles have an onset-of-melt temperature (T_om) that is at least 5°

C. higher than the T_om of said crystallized particles.

25. The process of claim 17, wherein said annealed particles have a degree of crystallinity in the range of from about 34 to about 42 percent.

26. The process of claim 17, wherein the total thermal energy added to said polyester polymer production process between steps (a) and (d) is less than 100 BTU/pound of said annealed particles.