Diblock polyester copolymer and process for making

A diblock copolymer and block technology, applied in the direction of one-component copolyester rayon, the structure of seat belts/slings, etc. , low fiber crystallinity and other problems

Inactive Publication Date: 2003-07-09
PERFORMANCE FIBERS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As a result, fibers spun from the above copolymers are undesirable because of the fibers' low crystallinity, low melting point, low ultimate tensile strength, and undesirable force / strain behavior
[0011] It would be desirable to have a diblock copolymer in which the starting aromatic polyester IV is high, the copolymer block length is long, the degree of transesterification is low, and the reaction time to prepare the copolymer is short (minutes, not hours) , without the use of polyfunctional acylating agents for chain extension, we attempted, using stirred reactors, to produce diblock copolymers from raw aromatic polyesters with higher IV and melt viscosities than described in the prior art, The above object was achieved; however, this attempt was not realized, as the following comparative example shows, because the autoclave cannot mix high IV PET and ε-caprolactone in an amount below 50% by weight to form a diblock copolymer based on weight

Method used

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  • Diblock polyester copolymer and process for making
  • Diblock polyester copolymer and process for making
  • Diblock polyester copolymer and process for making

Examples

Experimental program
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Effect test

example 1-9

[0059] The inventive examples illustrate the effect of catalyst concentration, polymerization temperature profile, and residence time on transesterification. Extruder zone temperatures, extruder screw speed, torque, polyester melt temperature and pressure, vacuum, throughput and residence time are shown in Table I below for all inventive examples. The obtained degree of transesterification is equal to transesterified caprolactone (expressed by σ=4.50ppm) / [caprolactone transesterified (expressed by σ=4.50ppm)+polycaprolactone (expressed by σ=4.24ppm)] . The transesterification in the diblock copolymer as reported in Table II was calculated by multiplying the percent caprolactone in the diblock copolymer by the transesterification.

example 1

[0061] see figure 1 , dry PET pellets (IV = 0.9, 280°C MV = 15000 poise) were fed into counter-rotating twin-screw extruder 10 (diameter = 27 mm, length = 1404 mm) at feed point 12 at 4.26 lbs / hr. The pellets begin to melt in first zone 14 and second zone 16 and are advanced by pumping element 20 in the direction of arrow 18 to a compression section at third zone 22 . Seal 24 acts as a dynamic seal at the end of the feed zone, tightly compressing the polymer melt and reducing back flow. Each zone is approximately 4 times the screw diameter in length.

[0062] A piston pump injected premixed ε-caprolactone and catalyst (tin octoate, 0.03% by weight of PET-caprolactone) into the extruder at injection point 26 at a rate of 0.75 lb / hr. The amount of ε-caprolactone in PET was 15% by weight. The injected liquid is rapidly mixed back and forth with the PET melt using a distributing and dispersing combing mixer 28 installed in the sprue area. ε-caprolactone solubilizes the PET me...

example 2

[0066] Dry PET pellets (IV = 0.9, 280°C MV = 15000 poise) were fed at feed point 12 at a rate of 7.7 lbs / hr figure 1 A twin-screw extruder 10 is shown. After PET is melted in zones 14 and 16, premixed ε-caprolactone and catalyst (tin octoate, 0.03% by weight of PET-caprolactone) are injected into the melt at injection point 26 at a rate of 2.7 lb / hr . The amount of ε-caprolactone in PET was 26% by weight. With the same extrusion profile as Inventive Example 1 above, the extrusion rate was increased (10.4 lbs / hr) to give an average residence time of 6 minutes. After venting at zone 60, the polymer (PET (74%)-polycaprolactone (26%)) was extruded through a three-hole die, quenched into water, and chopped into pellets. The diblock copolymer has a melting point of 219°C and IV=0.97, which proves that PET and ε-caprolactone have been copolymerized. The transesterification is reported in Table II below.

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Abstract

The present invention provides a diblock copolymer comprising: (a) a first block of polyester wherein said first block is made from aromatic polyester having: (i) an intrinsic viscosity which is measured in a 60 / 40 by weight mixture of phenol and tetrachloroethane and is at least about 0.6 deciliter / gram and (ii) a Newtonian melt viscosity which is measured by capillary rheometer and is at least about 7,000 poise at 280 DEG C; and (b) a second block of polyester wherein said second block is made from lactone monomer. The diblock copolymer is useful in engineered materials, films, and in spinning fibers for industrial applications such as seat belts. A process for making the diblock copolymer uses a twin screw extruder for melting the aromatic polyester and mixing it with monomer.

Description

[0001] This application is a continuation-in-part of co-pending Serial No. 08 / 788,895 filed January 22,1997. Background of the invention [0002] Known copolymers comprising aromatic polyesters and lactones are now limited to those formed from low intrinsic viscosity (IV) and low melt viscosity (MV) aromatic polyesters. Japanese Patent Publication 4115 (Publication 4115), published February 5, 1973, describes aromatic polyesters such as polyethylene terephthalate (PET) and polybutylene terephthalate (PBT) Applications. Publication 4115 contains examples of the use of PET in copolymers where the PET has a number average molecular weight ("Mn") of 500-5000 according to William L. Hergenrother and Charles Jay Nelson, "Classification of Polyethylene Terephthalate The relationship between diester viscosity and molecular weight" (Journal of Polymer Science (Journal of Polymer Science) 12, 2905-2915 (1974), measured in 60 / 40 (weight) phenol and tetrachloroethan...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/02C08G63/60C08G81/00D01F6/84
CPCC08G81/00D01F6/84C08G63/60C08L67/04B60R22/12C08L2203/12
Inventor W·唐F·马雷斯R·C·摩根
Owner PERFORMANCE FIBERS
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