Method for producing aliphatic or partially aromatic polyamides, said method comprising a solid-phase polymerization process

Patent metadata

Field	Value
Publication number	US-9701790-B2
Application number	US-201414896456-A
Country	US
Kind code	B2
Filing date	Jun 11, 2014
Priority date	Jun 12, 2013
Publication date	Jul 11, 2017
Grant date	Jul 11, 2017

Abstract

The present invention relates to a process for preparing an aliphatic or semiaromatic polyamide, in which a polyamide prepolymer is subjected to a solid state polymerization.

First claim

The invention claimed is:

1. A process for preparing an aliphatic or semiaromatic polyamide comprising
a) providing a prepolymer of the aliphatic or semiaromatic polyamide,
b) subjecting the prepolymer provided in step a) to a solid state polymerization in a closed vessel at a temperature within a range from 200 to 290° C. and a pressure within a range from 1.5 to 20 bar in the presence of a gas which is inert under the treatment conditions.

2. The process according to claim 1 , wherein the prepolymer provided in step a) comprises polymerized components selected from the group consisting of
A) unsubstituted or substituted aromatic dicarboxylic acids and derivatives of unsubstituted or substituted aromatic dicarboxylic acids,
B) unsubstituted or substituted aromatic diamines,
C) aliphatic or cycloaliphatic dicarboxylic acids and derivatives thereof,
D) aliphatic or cycloaliphatic diamines,
E) monocarboxylic acids and derivatives thereof,
F) monoamines,
G) at least trifunctional amines,
H) lactams,
I) ω-amino acids, and
K) compounds different from A) to I) and that are cocondensable therewith.

3. The process according to claim 2 , wherein at least one of components A) and B) is present for providing the prepolymer in step a).

4. The process according to claim 1 , wherein the polyamide is selected from the group consisting of PA 6.T, PA 9.T, PA8.T, PA 10.T, PA 12.T, PA 6.I, PA 8I, PA 9I, PA 10I, PA 12I, PA 6.T/6, PA 6.T/10, PA 6.T/12, PA 6.T/6I, PA6.T/8.T, PA 6.T/9.T, PA 6.T/10T, PA 6.T/12.T, PA 12.T/6.T, PA 6.T/6.1/6, PA 6.T/6.I/12, PA 6.T/6.I/6.10, PA 6.T/6.I/6.12, PA 6.T/6.6, PA 6.T/6.10, PA 6.T/6.12, PA 10.T/6, PA 10.T/11, PA 10.T/12, PA 8.T/6.T, PA 8.T/66, PA 8.T/8.I, PA 8.T/8.6, PA 8.T/6.I, PA 10.T/6.T, PA 10.T/6.6, PA 10.T/10I, PA 10T/10.I/6.T, PA 10.T/6I, PA 4.T/4.I/46, PA 4.T/4.I/6.6, PA 5.T/5.I, PA 5.T/5.I/5.6, PA 5.T/5.I/6.6, PA 6.T/6.I/6.6, PA MXDA.6, PA IPDA.I, PA IPDA.T, PA MACM.I, PA MACM.T, PA PACM.I, PA PACM.T, PA MXDA.I, PA MXDA.T, PA 6.T/IPDA.T, PA 6.T/MACM.T, PA 6.T/PACM.T, PA 6.T/MXDA.T, PA 6.T/6.I/8.T/8.I, PA 6.T/6.I/10.T/10I, PA 6.T/6.I/IPDA.T/IPDA.I, PA 6.T/6.I/MXDA.T/MXDA.I, PA 6.T/6.I/MACM.T/MACM.I, PA 6.T/6.I/PACM.T/PACM.I, PA 6.T/10.T/IPDA.T, PA 6.T/12.T/IPDA.T, PA 6.T/10.T/PACM.T, PA 6.T/12.T/PACM.T, PA 10.T/IPDA.T, PA 12.T/IPDA.T, and copolymers and mixtures thereof.

5. The process according to claim 1 , wherein the prepolymer of step a) is PA 6.T/6.I or PA 6.T/6.I/IPDA.T/IPDA.I or PA 6.T/6.I/MXDA.T/MXDA.I.

6. The process according claim 1 , wherein the prepolymer of step a) has a number-average molecular weight of 500 to about 12,000 g/mol.

7. The process according to claim 6 , wherein the prepolymer of step a) has a number-average molecular weight of about 1000 to 4000 g/mol.

8. The process according to claim 1 , wherein the temperature in the closed vessel in the solid state polymerization in step b) is within a range from 250 to 280° C.

9. The process according to claim 1 , wherein the pressure in the closed vessel in the solid state polymerization in step b) is within a range from 2 to 15 bar.

10. The process according to claim 9 , wherein the pressure in the closed vessel in the solid state polymerization in step b) is within a range from 3 to 10 bar.

11. The process according to claim 1 , wherein the inert gas used in the solid state polymerization in step b) is nitrogen.

12. The process according to claim 1 , wherein the gas which is inert consists of an inert gas selected from the group consisting of nitrogen, carbon dioxide, helium, argon, neon, and mixtures thereof.

13. The process according to claim 1 , wherein there is no discharge of water from the closed vessel interior during the solid state polymerization.

14. The process according to claim 1 , wherein no gas stream is passed through the closed vessel during the solid state polymerization.

Assignees

• Basf Se

Inventors

• Schmidt Christian
• Richter Florian
• Clauss Joachim
• Wilms Axel
• Kory Gad
• Schneller Arnold
• Stammer Achim
• Rauschenberger Volker
• Schwiegk Stefan

Classifications

• C08G69/30 Primary

  Solid state polycondensation · CPC title

• C08L77/04

  Polyamides derived from alpha-amino carboxylic acids (C08L77/10 takes precedence) · CPC title

• C08G69/46

  Post-polymerisation treatment · CPC title

• C08G69/26

  derived from polyamines and polycarboxylic acids · CPC title