Process for separating low molecular weight compounds from an impure thermoplastic polymer or mixture

• US 5,459,168 A
• Filed: 08/19/1994
• Issued: 10/17/1995
• Est. Priority Date: 08/20/1993
• Status: Expired due to Fees

• Current Assignee: Fried Krupp AG Hoesch-Krupp (Thyssenkrupp AG)
• Original Assignee: Fried Krupp AG Hoesch-Krupp (Thyssenkrupp AG)
• Inventors: Reimann, Klaus, Grabow, Manfred, Nasr, Hedi B.
• Primary Examiner(s): Foelak, Morton
• Application Number:
  US08/293,151
• Time in Patent Office: 424 Days
• Field of Search: 528/501, 528/481, 528/489, 528/323, 521/49.8
• US Class Current: 521/49.8
• CPC Class Codes: B29B 7/845 Venting, degassing or removing evaporated components in devices with rotary stirrers
• CPC Class Codes: B29B 7/86 for working at sub- or superatmospheric pressure B01F33/70 takes precedence
• CPC Class Codes: B29C 48/03 characterised by the shape of the extruded material at extrusion
• CPC Class Codes: B29C 48/76 Venting , drying means; Degassing means
• CPC Class Codes: B29C 48/762 Vapour stripping
• CPC Class Codes: B29K 2077/00 Use of PA, i.e. polyamides, e.g. polyesteramides or derivatives thereof, as moulding material
• CPC Class Codes: B29K 2105/26 Scrap or recycled material
• CPC Class Codes: C08G 69/16 Preparatory processes

Abstract

A process for treating an impure thermoplastic polymer, including raw and recycled polymers, during extrusion to separate low molecular weight compounds therefrom, including: introducing a separating agent into plasticized impure thermoplastic polymer passing through a first high pressure zone, the low molecular weight compounds of the plasticized polymer being at least partially soluble in the separating agent; extracting at least a part of the low molecular weight compounds from the plasticized polymer into the separation agent during passage of the plasticized polymer through an extraction zone; removing the separating agent charged with low molecular weight compounds from the extruder as the plasticized polymer passes through a low pressure zone having a residual pressure, P, which is lower the introductory pressure, P_e, and for which 1 bar≧P≧P_c ; collecting the charged separating agent as it is removed from the extruder; thermal vacuum treating the plasticized polymer as it passes through a last low pressure zone to vacuum degas the plasticized polymer at a pressure, P_v, for which P_v <0.5 bar and thereby further remove separating agent and low molecular weight compounds from the plasticized polymer; and passing the plasticized polymer through a last high pressure zone to an extruder head. The combination of solvent extraction in the extruder with subsequent vacuum degassing results in removal of large amounts of low molecular weight compounds with a relatively small expenditure of energy since energy-intensive vacuum degassing is needed only for removal of residuals.

Claims

1. A process for treating an impure thermoplastic polymer, including raw polymers and recycled polymers, during passage thereof through an extrusion apparatus to separate and remove low molecular weight compounds therefrom, the extrusion apparatus being comprised of a heated worm housing in which are defined, in the order recited, a heating zone, a first low pressure zone, an extraction zone, a first high pressure zone, a last low pressure zone, and a last high pressure zone, and an extruder head, the process comprising:

a. heating the impure thermoplastic polymer by passing the impure thermoplastic polymer through the heating zone of the extrusion apparatus to provide a plasticized polymer;

b. introducing a separating agent having a critical pressure, P_c, into the plasticized polymer passing through the first high pressure zone of the extrusion apparatus at an introduction pressure, P_e, the low molecular weight compounds of the plasticized polymer being at least partially soluble in the separating agent;

c. extracting at least a part of the low molecular weight compounds from the plasticized polymer into the separation agent during passage of the plasticized polymer through the extraction zone;

d. removing the separating agent charged with low molecular weight compounds from the extrusion apparatus as the plasticized polymer passes through a low pressure zone, which low pressure zone is one of upstream or downstream of the first high pressure zone and is upstream of the last low pressure zone, and which has a residual pressure, P, which is lower than the introduction pressure, P_e, in the first high pressure zone and which satisfies the requirement 1 bar≧

P≧

P_c ;

e. collecting the separating agent charged with low molecular weight compounds as it is removed from the extrusion apparatus;

f. thermal vacuum treating the plasticized polymer as it passes through the last low pressure zone to vacuum degas the plasticized polymer at a pressure, P_v, for which P_v <

0.5 bar and thereby further remove separating agent and low molecular weight compounds from the plasticized polymer; and

g. passing the plasticized polymer through the last high pressure zone to the extruder head from which purified thermoplastic polymer is recovered.

2. The process according to claim 1, wherein thermal vacuum treating the plasticized polymer as it passes through the last low pressure zone to vacuum degas the plasticized polymer is performed at a pressure, P_v, for which P_v <

0.05 bar.

3. The process according to claim 1, wherein the separating agent passes through the extrusion apparatus in a direction which is primarily counter to that of the passage of the plasticized polymer as a counterflow, and wherein the low pressure zone, from which the separating agent charged with low molecular weight compounds is removed as the plasticized polymer passes therethrough in the first low pressure zone, is upstream of the first high pressure zone.

4. The process according to claim 1, wherein thermal vacuum treating the plasticized polymer is performed only after the content of low molecular compounds therein has been lowered, by removal of low molecular compounds from the plasticized polymer, to <

10% of the original content of low molecular compounds within the impure thermoplastic polymer.

5. The process according to claim 1, wherein the residual pressure, (P), ranges between 1 and 8 bar, and wherein the introduction of separating agent takes place at an introduction pressure, P_e, which lies in a range which satisfies the requirement P<

P_e <

P_c.

6. The process according to claim 1,

wherein the extrusion apparatus further comprises a second high pressure zone into which additional separating agent is introduced at an introduction pressure, P_e, prior to passage of the plasticized polymer through the last high pressure zone;

and a second low pressure zone which has a residual pressure, P, which is lower than the introduction pressure, P_e and which satisfies the requirement 1 bar≧

P≧

P_c, and from which the additional separating agent charged with low molecular weight compounds is removed as the plasticized polymer passes therethrough, the second high pressure zone and the second low pressure zone being positioned downstream of the first low pressure zone and the first high pressure zone, and upstream of the last low pressure zone,

wherein the separating agent and additional separating agent pass through the extrusion apparatus in a direction which is primarily counter to the passage of the plasticized polymer as counterflows, and

wherein the low pressure zone from which the separating agent charged with low molecular weight compounds is removed as the plasticized polymer passes therethrough is the first low pressure zone having residual pressure, P, and the low pressure zone from which the additional separating agent charged with low molecular weight compounds is removed as the plasticized polymer passes therethrough is the second low pressure zone.

7. The process according to claim 6, wherein the separating agent is water, wherein more than 50 weight % of the water employed is introduced into the first high pressure zone, wherein less than 50 weight % of the water employed is introduced into the second high pressure zone, wherein the first low pressure zone has a residual pressure, p₁, and the second low pressure zone has a residual pressure, P₂, and wherein the residual pressure, P₁, is higher than the residual pressure, P₂, and P₁ -P₂ is at least 1 bar.

8. The process according to claim 1, wherein the removal of the separating agent takes place at a feed pressure, P_f, which satisfies the requirement for the residual pressure, P.

9. The process according to claim 1, wherein the separating agent is water.

10. The process according to claim 1, wherein the separating agent is water which is introduced into the plasticized polymer as steam and which is introduced in an amount which is at least 200% by weight based on the initial weight of low molecular compounds in the impure thermoplastic polymer.

11. The process according to claim 1, wherein the separating agent is one of CO₂ or N₂.

12. The process according to claim 1, wherein the separating agent is a mixture of a solvent which is liquid at 20°

C. and 1 bar abs. and one of CO₂ or N₂.

13. The process of separating low molecular weight compounds from one of a recycled plastic or a recycled plastic mixture, comprising:

treating the recycled plastic or recycled plastic mixture according to the process of claim 1.

14. The process of separating low molecular weight compounds from a raw plastic in the form of a mixture of substances, comprising:

treating the raw plastic according to the process of claim 1.

15. The process according to claim 14, wherein the raw plastic is polyamide-6 containing, as a low molecular weight compound, -caprolactam.

16. The process according to claim 1, wherein the impure thermoplastic polymer is a solid, wherein heating in step (a) is performed at a temperature effective to melt the impure thermoplastic polymer and provide a plasticized polymer which is a melt.

17. The process according to claim 1, wherein the impure thermoplastic polymer is introduced into the extrusion apparatus as a melt, and wherein heating in step (a) brings the melt to a temperature effective for extrusion thereof.

18. The process according to claim 1, wherein the impure thermoplastic polymer is introduced into the extrusion apparatus as a polymer paste, and wherein heating in step (a) brings the polymer paste to a temperature effective for extrusion thereof.

19. The process according to claim 1, wherein the impure thermoplastic polymer is introduced into the extrusion apparatus as a polymer solution, and wherein heating in step (a) brings the polymer solution to a temperature effective for extrusion thereof.