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Compositions of polyesters and sepiolite-type clays

a technology of sepiolite clay and polyester, which is applied in the field of polymer polyester and sepiolite clay compositions, can solve the problems of introducing the same thermal stability problems, sacrificing the performance and material toughness of low temperature impact, and only marginally successful attempts to generate nanocomposites or compositions containing nanosized particles dispersed in thermoplastic polyester matrix

Inactive Publication Date: 2006-09-14
EI DU PONT DE NEMOURS & CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This patent describes a process for making a thermoplastic polyester composition by mixing sepiolite-type clay with different types of polyester precursors. These precursors can include diacids, diesters, and diols, as well as linear and macrocyclic polyester oligomers. The mixture is then polymerized in the presence or absence of a solvent. The resulting composition has improved properties such as increased strength and flexibility. The patent also describes the use of this composition for making shaped parts and coatings.

Problems solved by technology

At these loading levels, however, low temperature impact performance and material toughness are usually sacrificed.
Attempts to generate nanocomposites, or compositions containing nanosized particles dispersed in a thermoplastic polyester matrix, have been only marginally successful.
Therefore, this process requires the use of an intercalating agent and as such introduces the same thermal stability issues described above.
This approach suffers from the requirement to use a large amount of solvent.
If the part is not solid and / or deforms easily upon ejection from the mold, it may be deformed and thereby rendered useless.
However, some semicrystalline polyesters crystallize very slowly, so they would have to be in the mold a long time to allow them to be demolded without significant deformation.
This would lead to long molding cycles, which is economically highly undesirable.
For example poly(ethylene terephthalate) (PET) is a slow crystallizing polyester, and by itself is usually unsuitable for injection molding because of the very long molding cycles and / or high mold temperatures needed.

Method used

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  • Compositions of polyesters and sepiolite-type clays
  • Compositions of polyesters and sepiolite-type clays
  • Compositions of polyesters and sepiolite-type clays

Examples

Experimental program
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example 1

[0143] BHET (300 g, 1.17 mol), sepiolite (Pangel® S9, 9 g), antimony oxide (96.5 mg, 321 ppm), and manganese acetate (102 mg, 340 ppm) were charged to a 500 mL three necked round-bottomed flask. An overhead stirrer was attached and a distillation condenser was attached. The reaction was heated to 180° C. under a light nitrogen flush. The reaction was held at 180° C. for 90 min. The reaction temperature was increased to 225° C. The reaction temperature was held at 225° C. for 30 min. The reaction temperature was increased to 295° C. at a rate of 1° C. / min. When the temperature reached 295° C., the reaction temperature was held constant for 30 min. The nitrogen flush was closed off and vacuum was slowly introduced. After 15 min, the vacuum was increased to a full vacuum eventually reaching a vacuum of 5 Pa. The reaction was maintained under vacuum for approximately 120 min. Mn=26000, PDI=1.81, % DEG=13 wt %, IV=0.9, Tg=65° C., Tm=228° C. The material so produced was characterized usin...

example 2

[0144] BHET (300 g, 1.17 mol), sepiolite (Pangel® B20, 9 g), antimony oxide (96.5 mg, 321 ppm), and manganese acetate (102 mg, 340 ppm) were charged to a 500 mL three necked round-bottomed flask. An overhead stirrer was attached and a distillation condenser was attached. The reaction was heated to 180° C. under a light nitrogen flush. The reaction was held at 180° C. for 90 min. The reaction temperature was increased to 225° C. The reaction temperature was held at 225° C. for 30 min. The reaction temperature was increased to 295° C. at a rate of 1° C. / min. When the temperature reached 295° C., the reaction temperature was held constant for 30 min. The nitrogen flush was closed off and vacuum was slowly introduced. After 15 min, the vacuum was increased to a full vacuum eventually reaching a vacuum of 5 Pa. The reaction was maintained under vacuum for approximately 120 min. Mn=26400, PDI=1.88, % DEG=6 wt %, IV=0.8, Tg=78° C., Tm=248° C. The material so produced was characterized usin...

example 3

[0149] BHET (300 g, 1.17 mol), sepiolite clay (Pangel® S9, 6g), antimony oxide (80 mg, 343 ppm), and sodium acetate (80 mg, 343 ppm) were charged to a 500 mL three necked round-bottomed flask. An overhead stirrer was attached and a distillation condenser was attached. The reaction was heated to 180° C. under a light nitrogen flush. The reaction was held at 180° C. for 90 min. The reaction temperature was increased to 225° C. The reaction temperature was held at 225° C. for 30 min. The reaction temperature was increased to 295° C. at a rate of 1° C. / min. When the temperature reached 295° C., the reaction temperature was held constant for 30 min. The nitrogen flush was closed off and vacuum was slowly introduced. After 15 min, the vacuum was increased to a full vacuum eventually reaching a vacuum of 5 Pa. The reaction was maintained under vacuum for approximately 120 min. The reaction was cooled under a nitrogen purge.

[0150] Tm and Tg were determined as described above, and t1 / 2 was ...

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Abstract

Compositions of thermoplastic polyesters and sepiolite-type clay in which the clay is dispersed in the polyester as often fibrous particles whose smallest dimension is less than 100 nm are made by polymerizing the polyester precursors in the presence of the clay. The compositions have good physical properties and can be melt molded into various articles. Many of these articles may be coated (painted) and are especially useful for appearance parts such as visible exterior automotive body parts.

Description

CROSS REFERENCE TO RELATED APPLICATIONS [0001] This application claims the benefit of priority of U.S. Provisional Application No. 60 / 638,225, filed Dec. 22, 2004, U.S. Provisional Application No. 60 / 686,675, filed Jun. 2, 2005, U.S. Provisional Application No. 60 / 686,728, filed Jun. 2, 2005, U.S. Provisional Application No. 60 / 686,847, filed Jun. 2, 2005, U.S. Provisional Application No. 60 / 686,689, filed Jun. 2, 2005, U.S. Provisional Application No. 60 / 686,707, filed Jun. 2, 2005, U.S. Provisional Application No. 60 / 686,708, filed Jun. 2, 2005.FIELD OF THE INVENTION [0002] This invention concerns compositions comprising thermoplastic polyesters and sepiolite-type clays, which are made by adding a sepiolite-type clay to a polyester polymerization, and forming the compositions into useful parts. TECHNICAL BACKGROUND OF THE INVENTION [0003] Nanocomposites are compositions that can address many of the challenges currently presented by automotive plastics and composites needs. These m...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): C08K9/04
CPCC08K3/0033C08K3/346C08K5/0016C08L63/00C08L67/02C09D167/02C08L2666/22C08K9/04C08K3/013Y10T428/31786
Inventor WILLIAMSON, DAVID T.
Owner EI DU PONT DE NEMOURS & CO
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