IP Library Granted Patent US 7,670,545
Granted Patent B2
US 7,670,545 · App. 12/163,466 · Granted Mar 2, 2010

Method for producing semicrystalline polylactic acid articles

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Quick Facts
Patent No.
US 7,670,545
App. No.
12/163,466
Granted
Mar 2, 2010
Kind
B2
Abstract

Amorphous sheets of PLA resins are thermoformed by heating the sheets until they become semicrystalline, and then forming the sheets on a relatively cold mold. Semicrystalline formed articles having improved heat resistance are made by the process.

Claims (22)

1. A method for making formed heat-resistant PLA articles, comprising softening and crystallizing a sheet of an amorphous, crystallizable PLA resin by heating the sheet until it has obtained a surface temperature from about 80 to about 155° C., adjusting the temperature of a male or female mold to a temperature below 80° C. and below the T g of the PLA resin, then positioning the softened and crystallized sheet over the mold and vacuum drawing the softened and crystallized sheet on the mold.

2. The method of claim 1 , wherein the sheet is heated under conditions such that the PLA resin attains a crystallinity of at least 15 Joules/gram.

3. The method of claim 2 , wherein the PLA resin is a homopolymer of L-lactic acid or D-lactic acid, a random copolymer of L-lactic acid and D-lactic acid, a block copolymer of L-lactic acid and D-lactic acid or a mixture of two or more of these.

4. The method of claim 3 wherein the PLA resin contains a nucleating agent, a plasticizer, or both.

5. The method of claim 4 wherein the PLA resin contains from about 1 to about 40 percent of a finely divided talc, based on the combined weight of the PLA resin and the talc.

6. The method of claim 3 wherein the PLA resin has a crystallization half-time at the temperature to which it is heated during the heating step of less than 3 minutes.

7. The method of claim 6 wherein the sheet is heated under conditions such that the PLA resin attains a crystallinity of at least 20 Joules/gram.

8. The method of claim 7 wherein the sheet is heated under conditions such that the PLA resin attains a crystallinity of at least 24 Joules/gram.

9. The method of claim 1 wherein the PLA sheet contains one or more additives selected from the group consisting of nucleants, other inorganic fillers, plasticizers, reinforcing agents, slip agents, lubricants, UV-stabilizers, thermal stabilizers, flame retardants, foaming agents, antistatic agents, antioxidants and colorants.

10. The method of claim 1 wherein the amorphous PLA sheet is cellular.

11. The method of claim 1 wherein the amorphous PLA sheet contains a foaming agent, and expands during the heating step to become cellular.

12. The method of claim 1 wherein the PLA resin contains a plasticizer.

13. The method of claim 1 wherein the sheet of amorphous PLA resin forms a layer of a multilayer structure having at least one other layer which is not a crystallizable PLA resin.

14. A thermoformed article made according to the process of claim 1 .

15. A method for making formed heat-resistant PLA articles, comprising softening a sheet of a semicrystalline PLA resin having a crystallinity of at least 10 Joules/gram by heating the sheet to a temperature at which the sheet can be thermoformed but at which the crystallinity of the sheet is not reduced below 10 Joules/gram, adjusting the temperature of a male or female mold to a temperature below 80° C. and below the T g of the PLA resin, and then positioning the softened sheet over the mold and vacuum drawing the softened sheet on the mold to produce a formed article of PLA resin having a crystallinity of at least 10 Joules/gram.

16. A method for making formed heat-resistant PLA articles, comprising heating softening and crystallizing a sheet of an amorphous, crystallizable PLA resin by heating the sheet to a temperature at which the PLA resin forms crystallites and for a time sufficient to impart a crystallinity of at least 10 Joules/gram to the PLA resin, adjusting the temperature of a male or female mold to a temperature below 80° C. and below the T g of the PLA resin, then positioning the softened and crystallized sheet over the mold and then vacuum drawing the softened sheet on the mold to produce a formed article of PLA resin with a crystallinity of at least 10 Joules/gram.

17. The method of claim 1 wherein the surface temperature of the heated sheet is below the melting temperature of the PLA resin.

18. The method of claim 17 wherein the mold temperature is adjusted to no greater than 50° C.

19. The method of claim 18 wherein the mold temperature is adjusted to no greater than 35° C.

20. The method of claim 1 wherein the sheet of amorphous PLA resin forms a layer of a multilayer structure containing at least one other layer.

21. The method of claim 20 wherein the at least one other layer of the multilayer structure is a layer of a crystallizable PLA resin.

22. The method of claim 21 wherein the sheet of amorphous PLA resin contains a nucleating agent.

Assignments (6)
RELEASE OF SECURITY INTEREST Recorded Aug 11, 2025
From: JPMORGAN CHASE BANK, N.A., AS ADMINISTRATIVE AGENT
To: NATUREWORKS, LLC
Reel/Frame 072412/0844 →
TERMINATION AND RELEASE OF SECURITY INTEREST IN PATENTS Recorded Oct 20, 2021
From: BANK OF AMERICA, N.A., AS ADMINISTRATIVE AGENT
To: NATUREWORKS LLC
Reel/Frame 057873/0985 →
SECURITY INTEREST Recorded Oct 20, 2021
From: NATUREWORKS LLC
To: JPMORGAN CHASE BANK, N.A., AS ADMINISTRATIVE AGENT
Reel/Frame 057879/0338 →
NOTICE OF GRANT OF SECURITY INTEREST IN PATENTS Recorded Jan 16, 2018
From: NATUREWORKS LLC
To: BANK OF AMERICA, N.A., AS ADMINISTRATIVE AGENT
Reel/Frame 045075/0556 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 15, 2010
From: BOPP, RICHARD C.; WHELAN, JASON
To: CARGILL DOW LLC
Reel/Frame 023795/0161 →
CHANGE OF NAME Recorded Jan 15, 2010
From: CARGILL DOW LLC
To: NATUREWORKS LLC
Reel/Frame 023799/0392 →