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Methods for preparation of macrocyclic polyester oligomer via heterogeneous catalysis

a technology of polyester oligomer and macrocyclic polyester, which is applied in the field of methods for preparing macrocyclic polyester oligomer, can solve the problems of longer time period in which column packing becomes spent, needs replacement or recycling, and the level of residual acids in the column is lower, so as to reduce the amount of residual oligomer, reduce catalyst concentration, and reduce the effect of filtration

Inactive Publication Date: 2014-12-25
LIQUID THERMO PLASTICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This approach results in a more efficient and cost-effective production of MPOs with higher purity, allowing for lower catalyst concentrations and reduced residual oligomers, leading to longer column life and easier removal of filtrate.

Problems solved by technology

This may result in a lower level of residual acids in the column, and the period of time in which column packing becomes spent and needs to be replaced or recycled is longer.

Method used

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  • Methods for preparation of macrocyclic polyester oligomer via heterogeneous catalysis
  • Methods for preparation of macrocyclic polyester oligomer via heterogeneous catalysis
  • Methods for preparation of macrocyclic polyester oligomer via heterogeneous catalysis

Examples

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experimental examples

MPO from DMT with a SiO2-Ti Solid Catalyst

[0040]Experiments were conducted to demonstrate preparation of cPBT directly from DMT and BDO via heterogeneous catalysis. The reaction set-up consisted of a 3 L three-necked flask fitted with an overhead stirrer, a sample port, a Dean Stark trap (boil up leg packed with stainless steel packing to assist separation), a vapor purge (a slow upward flow of N2 through the condenser to push volatiles out overhead [see FIG. 1]), just above the Dean Stark trap, a Vigreux column on top of the vapor purge (o-DCB reflux never reached beyond the very bottom of the Vigreux column), a water cooled condenser on top of the Vigreux column, and a nitrogen bubbler on the outlet of the condenser. The whole system was kept under a slight nitrogen pressure. Water and o-DCB were removed from the bottom of collection leg of the Dean Stark trap.

[0041]Initially the 3 L flask was charged with 2250 ml of o-DCB and 14.0 g of silica gel. The head space was purged with N...

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Abstract

The invention relates to methods and systems for preparing macrocyclic polyester oligomer (MPO) directly from monomer via heterogeneous catalysis, rather than by depolymerizing a polyester. For example, in an exemplary embodiment, cyclic poly(butylene terephthalate) (cPBT) is produced by reacting butanediol (BDO) and dimethylterephthalate (DMT) in an organic solvent—for example, ortho-dichlorobenzene (oDCB). The mixture flows over (or otherwise contacts) the catalyst-coated fiberglass or silica gel, e.g., which is packed in a column or bed. MPO is produced in the reaction mixture, while residual linears and catalyst residue remain in the column / bed.

Description

RELATED APPLICATION[0001]This application claims priority to and the benefit of U.S. provisional patent application Ser. No. 61 / 445,891, filed Feb. 23, 2011, the disclosure of which is incorporated herein by reference in its entirety.FIELD OF THE INVENTION[0002]This invention relates generally to methods for preparing macrocyclic polyester oligomer (MPO). More particularly, in certain embodiments, the invention relates to methods for preparing macrocyclic polyester oligomer using a solid catalyst.BACKGROUND OF THE INVENTION[0003]Macrocyclic polyester oligomers (MPOs) have unique properties that make them attractive as matrix-forming resins for engineering thermoplastic composites. MPOs lend valuable characteristics to polymerized products, for example, high strength, high gloss, and solvent resistance. Furthermore, because certain MPOs melt and polymerize at temperatures well below the melting point of the resulting polymer, polymerization and crystallization can occur virtually iso...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): C08G63/85C08G63/81
CPCC08G63/81C08G63/85B01J21/063B01J21/08B01J37/0209C08G63/183C08G2650/34
Inventor WEBB, JIMMY LYNNMIHALICH, JAMES
Owner LIQUID THERMO PLASTICS
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