Partially crystalline polyethyleneterephthalate
View Patent ↗The invention relates to a partially crystalline polyethylene terephthalate having a degree of polymerization which is greater than 80, particularly greater than 100, produced from a diol component and a dicarboxylic acid component, wherein according to the invention the DSC melting point, when measured with a heating rate of 10° C./Min during the first passage and second passage, is less than the melting temperature (Tm) of a comparable standard polyethylene terephthalate which is dependent upon the comonomer content. The inventive method for the production of a polyethylene terephthalate comprises a step for the production of a polycondensate prepolymer melt; a step for the formation of granules and the solidification of the polycondensate prepolymer melt; a step for increasing the degree of crystallization of the prepolymer granulates and a step for increasing the molecular weight of the granulates by means of solid phase polycondensation, wherein according to the invention a treatment temperature of 220° C. in step d) is not exceeded.
1. Partially crystalline polyethyleneterephthalate having a degree of polymerization larger than 80 manufactured from
(a) diol component which comprises up to 95 mol % to 100 mol % of ethylene glycol, and
(b) a dicarboxylic acid component which up to 95 mol % to 100 mol % comprises terephthalic acid,
wherein a total comonomer content of said polyethyleneterephthalate lies between 1 and 7%, and
wherein in a first step the diol component and dicarboxylic acid component are brought together in a liquid phase to obtain a low viscosity prepolymer having a degree of polymerization between 10 and 50,
said prepolymer is thereafter granulated into granules having an average granule size between 0.2 and 3 mm, and the granules subjected to a solid phase polycondensation at a temperature below 220° C. for from 6 to 30 hours to obtain a polyethyleneterephthalate, wherein a DSC melting point of said polyethyleneterephthalate measured at a heat-up rate of 10° C./min in a first run-through and in a second run-through, lies below a comonomer dependent melting temperature (Tm) of a polyethyleneterephthalate having been prepared via a solid state polycondensation from a prepolymer having a degree of polymerization between 65 and 80 which was formed into granulate having a mass of 10 to 30 mg and which was cooled with water below its glass transition temperature, as calculated with the equation
T 0 − 2 . 5 ° C.*% comonomer content (in mol %) with T 0 being equal to 260° C., wherein a comonomer proportion of the diol component is comprised mainly of diethyleneglycol,
or as calculated with the equation
T 0 − 3 . 0 ° C.*% comonomer content (in mol %) with T 0 being equal to 260° C.
2. Polyethyleneterephthalate in accordance with claim 1 manufactured from a diol component, which comprises up to 97 mol % to 99 mol % of ethylene glycol, and a dicarboxylic acid component, which up to 97 mol % to 100 mol % comprises terephthalic acid, wherein the total comonomer content lies between 1.5 and 5%.
3. Polyethyleneterephthalate in accordance with claim 2 , wherein the DSC melting point in the first run-through and in the second run-through lies under 245° C.
4. Polyethyleneterephthalate in accordance with claim 1 wherein the DSC melting point in the first run-through is larger than the DSC melting point in the second run-through.
5. A partially crystalline polyethyleneterephthalate in accordance with claim 1 having a thermally partially crystallized polyethyleneterephthalate therein.
6. A polyethyleneterephthalate in accordance with claim 1 having a linear polyethyleneterephthalate therein.
7. The polyethyleneterephthalate in accordance with claim 1 wherein the polyethyleneterephthalate has a DSC enthalpy of melting in the first run-through smaller than 65 J/g.
8. The polyethyleneterephthalate in accordance with claim 1 wherein the polyethyleneterephthalate exists as granulate and the average granulate size lies between 0.8 and 1.4 mm.
9. The polyethyleneterephthalate in accordance with claim 8 , wherein the granulate comprises massive particles, which have a defined shape selected from one of cylinder-shaped, spherically-shaped, ball-shaped, drop-shaped and ball-like.
10. The polyethyleneterephthalate in accordance with claim 1 wherein the degree of polymerization of the partially crystalline polyethyleneterephthalate lies between 145 and 180 and the comonomer content amounts to less than 3.5 mol %.
11. The polyethyleneterephthalate in accordance with claim 1 wherein the degree of polymerization of the partially crystalline polyethyleneterephthalate lies between 100 and 130.