Method for preparing polyactic acid

Patent metadata

Field	Value
Publication number	US-10487174-B2
Application number	US-201615750862-A
Country	US
Kind code	B2
Filing date	Aug 10, 2016
Priority date	Aug 11, 2015
Publication date	Nov 26, 2019
Grant date	Nov 26, 2019

Abstract

The present invention relates to a method for preparing polylactic acid. According to the method for preparing polylactic acid, high quality polylactic acid can be provided by effectively removing residual monomers while minimizing property changes of the polylactic acid.

First claim

The invention claimed is:

1. A method for preparing polylactic acid, comprising:
a polymerization step wherein lactides or lactic acids are polymerized, and sterically hindered phenol is added when residual monomers are 1 to 8 mol % of the total monomers introduced and additionally reacted to obtain a polymer;
a cooling step wherein pellets are obtained from the polymer; and
a step of removing residual monomers wherein inert gas is introduced into a reactor containing the pellets at a velocity of 0.001 to 0.5 L/min while being heated,
wherein the inert gas is introduced while being heated from room temperature to a temperature of 100 to 130° C. at a first velocity of 1 to 10° C./min, and heated from a temperature of 100 to 130° C. to a temperature of 130 to 170° C. at a second velocity of 1 to 20° C./min,
wherein polylactic acid passing through the step of removing residual monomers exhibits a molecular weight decrease rate of 5% or less, compared to the polymer obtained in the polymerization step.

2. The method for preparing polylactic acid according to claim 1 , wherein in the polymerization step, L-lactide, D-lactide, DL-lactide, meso-lactide, L-lactic acid, D-lactic acid, DL-lactic acid, or mixtures thereof are polymerized.

3. The method for preparing polylactic acid according to claim 1 , wherein the polymerization step is conducted at a temperature of 170 to 210° C.

4. The method for preparing polylactic acid according to claim 1 , wherein in the polymerization step, sterically hindered phenol is added and then additionally reacted for 80 minutes to 180 minutes.

5. The method for preparing polylactic acid according to claim 1 , wherein as the sterically hindered phenol, 2′,3-bis-[3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionyl]propionohydrazide, pentaerythritol tetrakis(3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate), octadecyl-3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate, or a mixture thereof is used.

6. The method for preparing polylactic acid according to claim 1 , wherein the first velocity is slower than the second velocity.

7. The method for preparing polylactic acid according to claim 1 , wherein the inert gas is introduced while being heated from room temperature to 120° C. at a velocity of 2° C./min, and being heated from 120° C. to 160° C. at a velocity of 4° C./min.

8. The method for preparing polylactic acid according to claim 1 , wherein in the step of removing residual monomers, a time for which the inert gas is introduced is 1 hour to 30 hours.

Assignees

• Lotte Chemical Corp

Inventors

• Kim Hyun A
• Ko Myung Joo
• Kang Jong Won

Classifications

• C08G63/08 Primary

  Lactones or lactides · CPC title

• C08G63/78

  Preparation processes · CPC title

• C08G63/90

  Purification; Drying · CPC title