Production method for polyamide

Patent metadata

Field	Value
Publication number	US-9359477-B2
Application number	US-201314381182-A
Country	US
Kind code	B2
Filing date	Feb 25, 2013
Priority date	Feb 28, 2012
Publication date	Jun 7, 2016
Grant date	Jun 7, 2016

Abstract

The present invention is directed to a process for producing a polyamide, which process includes directly melt-polymerizing a diamine component including 70 mol % or more of p-xylylenediamine and a dicarboxylic acid component including 70 mol % or more of a C6 to C18 aliphatic dicarboxylic acid, in the absence of solvent in a batch-type reactor equipped with a stirring blade, the process including: (1) reacting the diamine component with the dicarboxylic acid component under a pressure condition of 0.2 to 0.5 MPa (Abs); (2) maintaining a vapor phase section of a reaction tank of the reactor at 200° C. or higher during reaction; (3) stirring the contents of the reaction tank, from the start of adding the diamine component until after completion of the addition and before the start of pressure falling, such that the stirring-related Froude number represented by a specific formula is adjusted to 0.0002 to 0.15; and (4) employing a stirring blade having no structural body in the horizontal direction or having a structural body in the horizontal direction, which body does not come into contact with the interface between the reaction mixture and the vapor phase section during stirring. In the polyamide production process, deposition of solid matter in the reaction tank vapor section and in a vapor pipe is suppressed, and incorporation into the product of unmelted solid matter originating from the deposits is reduced.

First claim

The invention claimed is:

1. A process for producing a polyamide, which process includes directly melt-polymerizing a diamine component including 70 mol % or more of p-xylylenediamine and a dicarboxylic acid component including 70 mol % or more of a C6 to C18 aliphatic dicarboxylic acid, in the absence of solvent in a batch-type reactor equipped with a stirring blade, the process being characterized by comprising:
(1) reacting the diamine component with the dicarboxylic acid component under a pressure condition of 0.2 to 0.5 MPa (Abs);
(2) maintaining a vapor phase section of a reaction tank of the reactor at 200° C. or higher during reaction by one or more steps selected from the group consisting of attaching a heater to a top plate of the reactor, controlling a reflux rate by controlling a temperature of a partial condenser on the reactor, and preventing heat dissipation at the top plate of the reactor;
(3) stirring the contents of the reaction tank, from the start of adding the diamine component until after completion of the addition and before the start of pressure falling, such that the stirring-related Froude number represented by Fr=(N/60) 2 ×d/g (N: stirring rate [rpm], d: diameter of stirring blade [m], and g: gravitational acceleration [m/s 2 ]) is adjusted to 0.0002 to 0.15; and
(4) employing a stirring blade having no structural body in the horizontal direction or having a structural body in the horizontal direction, which body does not come into contact with the interface between the reaction mixture and the vapor phase section during stirring.

2. A polyamide production process according to claim 1 , wherein the diamine component includes p-xylylenediamine and m-xylylenediamine.

3. A polyamide production process according to claim 1 , wherein the C6 to C18 aliphatic dicarboxylic acid is sebacic acid.

4. A polyamide production process according to claim 1 , wherein the stirring blade is a helical ribbon blade having a spiral ribbon blade.

5. A polyamide production process according to claim 1 , wherein the vapor phase section of the tank is maintained at 200° C. or higher during reaction by attaching a heater to a top plate of the reactor.

6. A polyamide production process according to claim 1 , wherein the vapor phase section of the tank is maintained at 200° C. or higher during reaction by controlling a reflux rate by controlling a temperature of the partial condenser on the reactor.

7. A polyamide production process according to claim 1 , wherein the vapor phase section of the tank is maintained at 200° C. or higher during reaction by preventing heat dissipation at the top plate of the reactor.

8. A polyamide production process according to claim 1 , wherein the diamine component includes 80 mol % or more of p-xylylenediamine.

9. A polyamide production process according to claim 1 , wherein the diamine component includes 90 mol % or more of p-xylylenediamine.

10. A polyamide production process according to claim 1 , further comprising discharging the produced polyamide from the reaction tank and performing steps (1) through (4) in a subsequent batch reaction to produce additional polyamide.

11. A polyamide production process according to claim 10 , wherein after the subsequent batch reaction, any solid matter deposited in the vapor phase section of the reaction tank has a mean thickness of less than 0.5 mm and no solid matter has been deposited having a thickness of greater than 3 mm.

12. A polyamide production process according to claim 4 , wherein the stirring blade rotates to create a downward flow on the contents of the reaction tank.

Assignees

• Mitsubishi Gas Chemical Co

Inventors

• Tochihara Tatsuya
• Shinohara Katsumi

Classifications

• C08L77/06

  Polyamides derived from polyamines and polycarboxylic acids (C08L77/10 takes precedence) · CPC title

• B01J19/18

  Stationary reactors having moving elements inside (B01J19/08, B01J19/26 take precedence) · CPC title

• B01F7/00291

  Operations & Transport · mapped topic

• B01J19/0066

  Stirrers (mixing per se B01F) · CPC title

• C08G69/265

  from at least two different diamines or at least two different dicarboxylic acids · CPC title