NatureWorks PLAfibers

PLA Processing Guide for Bicomponent Staple Fibers
This information is intended for use only as a guide for the manufacture of PLA fibers. Because melt spinning and downstream processing of PLA fibers is complex, an experimental approach may be required to achieve desired results.
1.0 Safety and Handling Precautions

All safety precautions normally followed in the handling and processing of melted thermoplastics should be followed for NatureWorks PLA resins. As with most thermoplastics, melt processing and the variability of those conditions may result in minor decomposition. Lactide, a non-hazardous gaseous irritant, is a minor by-product of PLA melt processing. Appropriate air testing should be completed to ensure an acceptable Threshold Limit Value (TLV) of less than 5 mg/m3 is maintained. The use of process area point source remediation measures such as monomer fume hoods or exhausts near the spinneret are typically recommended. PLA is considered non-hazardous according to DOT shipping regulations. Care should be taken to avoid direct skin/eye contact along with conditions that promote dust formation. Product may cause eye/skin irritation. Product dust may be irritating to eyes, skin and respiratory system. Caused mild to moderate conjuctival irritation in eye irritation studies using rabbits. Caused very mild redness in dermal irritation studies using rabbits (slightly irritating). Ingestion may cause gastrointestinal irritation, nausea, vomiting and diarrhea. For further information, consult the appropriate MSDS for the PLA grade being processed.
2.0 Pellet Storage and Blending Recommendation

PLA resins should be stored in an environment designed to minimize moisture uptake. Product should also be stored in a cool place at temperatures below 50C (122oF). Product that is delivered in cartons or super sacks should be kept sealed until ready for loading into the blending and/or drying system. Bulk resin stored in silos, hoppers etc for extended periods (more than 6 hrs) should be kept purged with dry air or nitrogen to minimize moisture gain. In the case of outside storage, if the product is supplied in Boxes or other non-bulk containers, the unopened container should be brought into the fiber production area and allowed to equilibrate for a minimum of 24 hours before opening.
3.0 Resin Properties

Different grades of PLA have been designed for different types of bicomponent fibers
Resin Grade
6201D
Resin Use
High melt temperature, mid viscosity, lowshrink component used for cores in S/C, 1 side in S/S or segment in Pie/Wedge or as a component in Islands in the Sea Fibers High Melt temperature, low viscosity, low shrink component used for cores in S/C, 1 side in S/S or segment in Pie/Wedge or as a 1
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6251D
NatureWorks LLC Confidential
6301D
6350D
6400D
6800D
Other grades
component in Islands in the Sea Fibers Low Melt temperature, mid viscosity, higher shrink component for sheaths in S/C, 1 side in S/S or segment in Pie/Wedge or as a component in Islands in the Sea Low Melt temperature, low viscosity, higher shrink component for sheaths in S/C, 1 side in S/S or segment in Pie/Wedge or as a component in Islands in the Sea High melt temperature, high viscosity, low shrink component for cores in S/C, 1 side in S/S or segment in Pie/Wedge or as a component in Islands in the Sea High melt temperature, high viscosity, low shrink component for cores in S/C, 1 side in S/S or segment in Pie/Wedge or as a component in Islands in the Sea Grades normally intended for packaging have been evaluated in all applications mentioned above-S/C, S/S, P/W, IITS
Table of Resin Grades
Peak Fiber Crystalline MT vs. %D

180.0
160.0
140.0 Peak Crystalline Melt Temp (oC)
120.0
100.0
MT = -4.366%D + 174.78 R2 = 0.9758
80.0
60.0
40.0
20.0
0.0 0 2 4 6 %D 8 10 12
Relationship of Melt Tempature to %D
Typical PLA Resin Properties

The graph on the following page shows the melt density of PLA over a wide temperature range.
P L A M elt D en sity C u rve

1 .1 60 1 .1 50 1 .1 40 1 .1 30 Melt Density (g/cc) 1 .1 20 1 .1 10 1 .1 00 1 .0 90 1 .0 80 1 .0 70 1 .0 60 1 .0 50 1 40 150 160 17 0 1 80 190 20 0 21 0 2 20 230 24 0 25 0 T e m p (o C )
The rheology curves for several of these grades are shown in the following graph.
Fiber Grades Rheology Example, 230
1000
o
Sh ear Vis co sit y, Pa. 100 s
6251D, 2.4 RV 6201D, 3.1 RV 6201D, 3.1 RV 6201D, 3.1 RV 6350D, 2.6 RV
10 10 100 1000 Shear Rate, /sec. 10000 100000
Capillary Rheology, performed at 230oC
4.0 Materials of Construction

All metal parts in the extrusion process should be constructed of stainless steel to minimize corrosion. Furthermore, PLA should not be left in the extruder, polymer filter, polymer transfer lines, spin beam, spinnerets or any other part of the extrusion system at PLA melt temperatures or higher for extended periods. Below is a guideline for the recommended types of steel that should be used in the extrusion system.
Part
Melt pumps and bearings Pump blocks Transfer lines and spin beam
Steel Type
SUS440B SUS631 SUS440C
5.0 Drying
PLA resin can be successfully dried using most standard drying systems. Recommended conditions are provided for standard desiccant based column dryers. For other drying system designs, additional information can be provided upon request. To prevent equipment corrosion, it is not recommended to dry or store hot PLA resin in carbon steel vessels (see Section 2.0). In-line drying is essential for PLA resins. A moisture content of less than (50 PPM) is recommended to prevent viscosity degradation. Material is supplied in foil-lined containers dried to less than 400 PPM as
measured by NatureWorks LLC internal method. The resin should not be exposed to atmospheric conditions after drying. Keep the package sealed until ready to use and promptly dry and reseal any unused material. The drying table below can be used to estimate the drying time needed for PLA. Air or nitrogen based desiccant drying systems can be used at the recommended temperatures. Typical PLA drying conditions are shown in the table below. Typical Settings Amorphous Crystalline (6201D, (6301D, 6350D-Pellets 6251D, 6400D-Pellets that are clear) that are opaque) 4 2 50 100 - 40 - 40 > 0.031 > 0.031
Drying Parameter
Residence Time (hours) Air Temperature (oC) Air Dew Point (oC) Air Flow Rate (m3/min/kg resin)
Typical PLA Raw Material Drying Conditions

Typical desiccant dryer regeneration temperatures exceed the melt point of PLA resins. To prevent issues with pellet bridging, sticking or melting, the drying system should be verified to ensure temperature control is adequate during operation as well as during regeneration cycles since valve leakage is common in many systems.
6.0 Melt Spinning

Prior to introducing PLA into any melt spinning system, the system should be properly purged to prevent any polymer contamination and spinnability problems from occurring. The purging procedures below are recommended for optimal removal of other polymers.
6.1 PLA Purging Procedure Following PP in your systems (not degraded by cooling and re-heating system)
1. 2. 3. At normal PLA operating temperatures, run a high melt index PP (15- 40 MI) without spinneret in place. Purge for at least 3x average residence time. Let system empty as much as possible. Transition to purge PLA and purge following the same guidelines as step 1. Insert pre-heated spinneret and allow temperature to equilibrate. Purge with PLA grade to be used in extruder and evaluate flow from capillaries. As long as flow is even from each capillary and there is no evidence of contamination, begin spinning. Purge all PLA from the extrusion system, using a high melt index PP, immediately after completion of the production run
4.
Following PET, Nylon, or HDPE in your systems

1. 2. 3. 4. 5. 6. Purge with low MI (<1) PP at normal PET operating temperatures. Purge for at least 3x average residence time (~30 minutes). Let system empty as much as possible. Change to normal PLA operating temperatures and run a high melt index PP (15- 40 MI). Purge for at least 3x average residence time. Let system empty as much as possible. Transition to purge PLA and purge following the same guidelines as steps 1 and 2. Insert pre-heated spinneret and allow temperature to equilibrate. Purge with PLA grade to be used in extruder and evaluate flow from capillaries. As long as flow is even from each capillary and there is no evidence of contamination, begin spinning. Purge all PLA from the extrusion system, using a high melt index PP, immediately after completion of the production run
Important Notes:
1. It is critical that all drying and conveying/receiving systems be free of all PET or PP and is vacuumed to
2. 3.
4.
ensure that there is no remaining polymer dust, before adding PLA. PET will not melt at PLA operating temperatures and will block screens, if it is present in the system. Brand of PP used for purging is unimportant, as long as it does not thermally cross-link. It is important to purge all extruders being used shortly before running, preferably at the same time, just prior to spinning. Extruders that are left at temperature with any PLA can lead to degraded polymer that will cause problems in filtration/spinning. When handling PLA pellets, the generation of small particles or fines is possible. Conveying pellets slower, such as at a velocity of 25 m/s, will generate fewer fines than at 30 m/s when conveying in dilute phase. Please note that with dilute phase conveying, enough velocity must be maintained to prevent the pellets from plugging the line. Internal and external testing did not show plugging problems at 25 m/s.
6.2 Extrusion
A general-purpose single-screw extruder, 24 to 36:1 L/D with feed-throat cooling is acceptable for processing PLA. Effective feed-throat cooling is important to prevent the formation of a melt-block with amorphous gradess. A mixing tip is generally recommended along with static mixers in the product line to ensure temperature uniformity as well as optimum additive dispersion and melt polymer homogeneity. The following table shows a typical melt profile for PLA.
Extrusion Area
Melt Temperature Setting (oC) High Melting PLA Components

25 200 220 230 240 240
Melt Temperature Setting (oC) Low Melting PLA Components

25 200 200 170 240 240
Feed throat Zone 1 Zone 2 Zone 3 Melt pump Spin head
Typical PLA Extrusion Conditions

Note 1: Temperatures are only starting points and may need to be altered. Target PLA melt temperatures (after melt pump) should be in the range of 225-245C (437-473oF). Note 2: PLA resins should not be processed at temperatures above 250C (482F) due to excessive thermal degradation.
6.3 Additives
Delusterants such as TiO2 are best added as a masterbatch at 15-30 wt% in PLA resins and controlled dosing the required amount of dried masterbatch into the feed throat of the running extruder.
6.4 Filtration
PLA resin will be provided pre-filtered to a level of 20 microns. The following pack makeup is recommended: Loose media (optional - depending upon pack configuration) 200-350 micron shattered metal is recommended for an uncompressed pack cavity fill. Screens cascade configuration with appropriate support screens is recommended with finest filtration level of 325 mesh.
6.5 Heating Systems

To allow for the required temperatures to be obtained in spinning, typically vapor heat transfer system medium changes are required. Dowtherm J / Therminol LT or a comparable vapor HTM which has an atmospheric boiling point of 200C or less while remaining within specific system pressure design limits is generally recommended. Operation of the HTM system at a temperature as close as possible to the actual melt temperature (2355C) is recommended to provide an adiabatic spinning system. For vacuum assisted systems, typically heat transfer medium changes are not required as long as the system vacuum can be operated at a level to provide vaporization and uniform heating at the suggested temperatures (230240C). Prior to being placed into service, spin packs should be heated to 250oC to allow for some temperature loss during spin pack installation.
6.6 Spinnerets
Recommended capillary dimensions for a fiber with a solid round cross section range from 0.2-0.35 mm diameter, typically with a 2 to 3:1 L/D ratio. Larger capillaries may be necessary for fibers greater than 6 dpf. The following guide can be used to estimate spinneret requirements based on spun product dpf:
Spinneret Capillary Sizing
0.4 0.35 diameter mm 0.3 0.25 0.2 0.15 0 2 4 spun dpf 6 8 10 2 L/D 3 L/D
Capillary dimensions for modified cross sections will deviate greatly from solid round fibers. They should be designed to meet the desired fiber shape, while providing adequate pressure drop to ensure good denier uniformity and adequate draw down or stretch ratio to facilitate good spinning performance. Pack designs for production of bicomponent fibers vary greatly with type of fiber, equipment manufacturer and polymers intended to be process. Spinneret or extrusion system manufacturer should be consulted to ensure appropriate configuration is used. Improper pack set-up can lead to high pressure and pack leaks and should be avoided.
6.7 Quenching
Filaments should be quenched with air at controlled temperatures and velocities to ensure good denier and orientation uniformity. Typical quenching conditions are shown below, but quenching conditions need to be optimized by product depending upon the denier, spinneret design, and cross section. In some cases, special quenching conditions need to be used to avoid fibers sticking when condensing them, or to create some special effects in the fibers.
Quench parameter
Quench Air velocity (m/s) Quench Air Temperature (oC) Monomer Exhaust Velocity (m/s)
Typical Target
0.26 1.5 10 20 .26 2.0
Spacer or Shroud Length (mm)
50 100
Typical PLA Quenching Conditions A monomer exhaust system is preferred to prevent the buildup of residual lactide around the spinneret face and quench screen. 6.8 Take Up
PLA can be spun over a wide range of take up speeds, but typically runs between 1100 and 1850 m/min. Low or high viscosity components in bicomponent fibers can further limit the maximum take-up speed.
7.0 Drawing
A modern polyester type draw line equipped with accurate speed, temperature and tension controls is recommended for drawing PLA. Two-stage drawing is preferred to maximize tensile properties without stress whitening PLA. Fleissner and Neumag manufacture suitable draw lines for PLA. An illustration of a typical line is shown below: When running on older lines, draw ratios that can be achieved will depend on the degree of control over temperatures, both water and steam, the type of draw roll heating employed, the length of water baths and steam chests and the line speed. In short, uniform drawing depends on heat transfer rates from the equipment to the fibre and the degree of control over drawing temperatures and conditions. Several factors impact the heat transfer rate, including: Tow mass Initial tow temperature. Line speed Contact area of the rolls (diameter) and layout Number of rolls Method of heat application (immersion bath, sparge systems) Note, with bicomponent fibers, draw temperatures applied, especially by draw rolls, is limited by any lowmelting components. This can lead to limited draw ratios and limited ability to heat set fibers. Also, draw ratios can be limited by higher viscosity components in the bicomponent fiber. Draw ratios should be maximized to optimize tensile properties, without severe crazing (stress-whitening). Temperatures applied in drawing should be as high as possible to allow drawing without sticking on rolls and equipment.
7.1 Creeling and pre-tensioning

7.1.1 Creel Size Creel size is largely dependent upon the crimper size and the tension rating of the drawstands. PLA can be run at similar tow densities in crimping as PET, with typical densities ranging from 65 to 72 thousand dtex per cm of crimper width. Through experimentation, this can be optimised, along with crimp properties 7.1.2 Creel Tensioning Creels should be designed to provide a minimal tension level on each subtow in the creel. If the tension is too great, typically greater than 0.2 g/den, the tow could begin drawing before or during immersion in the pre draw bath, causing excessive denier variation along with the possibility of broken fibers and high wrap rates. In addition, the tension level between individual subtows in the creel should be uniform. An
adjustable pre tension stand is preferred prior to the pre draw bath to assist in equalising the tension between subtows.
7.2 Pre Draw Bath

Pre-draw baths should be sufficiently long to enable saturation of the tow with moisture and finish and to initially raise the tow temperature to 25-50oC. The tow should not be heated above PLAs Tg (58oC), other wise the tow could begin drawing, which would lead to the same types of problems described in the preceding section. Also nip rolls are recommended on the pre draw rolls to minimize tension on the towband before drawing.
7.3 Drawing
7.3.1 Temperatures The drawing occurs in the one draw stage, where the tow temperature should be maintained between 45 and 70oC. Roll cooling is recommended on the post draw stand to prevent the tow band from sticking to the rolls. To achieve the recommended tow temperatures, heating systems between the draw roll stands are required. Poor distribution of heat will lead to poor tow temperature uniformity, resulting in non uniform drawing and potentially broken fiber and/or undrawns. Immersion baths also provide good tension and drawing uniformity, provided that they have good temperature control and adequate circulation capabilities. 7.3.2 Draw Ratios PLA can be drawn over a wide range of draw ratios. The optimal draw ratio is dependent upon the type of polymer used, the type of bicomponent configuration used, the as spun orientation level, and the desired tensile properties for the product. PLA staple fiber is typically drawn in the 3:1 4:1 range. As mentioned earlier, two-stage drawing is recommended due to potential stress whitening concerns with single stage drawing. If stage 1 draw ratio is too high, the fiber will stress whiten, or craze. The % of the total draw ratio is typically split 70/30 between stage 1 and 2, but will require optimization by process and manufacturing line.
7.4 Finish application

Finish should be applied before entering the dryer or heat setter. Applying finish after the dryer will destabilize the tensile properties of the fiber with time. Finish should be selected based on planned downstream processing. Goulston Technologies, Inc or Takemoto Oil and Fat Company LTD can recommend and provide finishes for PLA that have been proven for a variety of applications. Depending on subsequent processing and finish types, application levels range from 0.35% up to 0.8% finish on fiber.
7.5 Crimping
7.5.1 Lamination, and Presentation Tow density, lamination and presentation upon entry into the crimper are critical to providing uniform crimp across the width of the tow band. Tow stackers and/or ply bars are recommended for achieving uniform tow density across the tow band. Dancer rolls are also recommended to maintain a constant tension on the tow entering the crimper. 7.5.2 Heating systems
Heating capabilities, preferably steam, are recommended prior to and during the crimper process. Pre heating the tow before entering the crimper allows the fiber to bend easily with minimal mechanical pressure. Heating the fiber during crimping provides greater crimp permanency. Typical tow temperatures before and during crimping are shown in the table below. These temperatures may need to be optimized for each process.
Process location Entering Crimper In the Crimper
Typical Temperatures o o F C 70-90 21 - 32 70-90 21 - 32
Typical Tow Temperatures in crimping

7.5.3 Crimping Minimal mechanical pressure should be used to crimp PLA to decrease the potential of fiber damage. The primary process variable for increasing crimp level should be the tow temperature entering the crimper. The flapper pressure should be used as a secondary control parameter to increase crimp level. Typical flapper and roll pressures for a bicomponent containing a low melting PLA component along with processes are shown below. Flapper and roll pressures will need to be adjusted for each process to achieve desired crimp levels. Product denier 4 (PLA/PET bico) Typical flapper pressure (bar) 1.0 2.0 Typical roll pressure (bar) 1.5 2.5
Typical mechanical pressures in crimping 7.6 Heatsetting

Hot through air dryers are recommended for drying and heatsetting. The dryers should have multiple zones with a cooling zone at the dryer exit. Temperature control is critical, as the objective is to expose the fiber to temperatures as close to the melt point as possible without actually melting the fiber. Recommended drying temperatures for PLA range from 120 to 140oC for high melting fibers only. If bicomponent lowmelting components are included, care must be taken at any temperature above the Tg of 55oC-57oC, to avoid blocking or melting of the low melting component. Depending on %D level of the PLA used, the temperature at which the fiber will melt and flow will vary from about 100oC to about 150oC. An experimental approach to determine the optimum heat setting dryer should be taken, to determine the maximum temperature that can be used without causing the fiber to block in processing or bale storage.
7.7 Cutting
The temperature of the tow should be maintained below 50oC to ensure that the crimp does not get pulled out due to the tension at cutting. Tension stands are recommended prior to cutting. Conventional rotary cutters are acceptable.
7.8 Baling
Conventional polyester balers are acceptable for baling PLA. The bale density required to produce stable bales will vary with denier and finish type. Bale densities range from 0.27 0.40 g/cm3 (17 25 lb/ft3). Typical pressures applied in baling range from 50 to 100 psi. Low melt point binder fibers require lower ram pressure to minimize the potential of fiber sticking together in the bale. For low-melt fibers, pressures of 50 psi or less are recommended.
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7.9 Fiber Storage

Baled fiber should be stored in cool, clean, dry location to prevent hydrolysis and contamination. Environmental conditions of 25oC, 55% RH are recommended.
8.0 Fiber Properties

The table below shows some typical PLA fiber properties. Fiber Property Denier CPI Tenacity (g/den) Elongation to break (%) Finish on Fiber (%) Hot air shrinkage (130oC, 10 mins) 4 dpf bicomponent PLA low Melt Sheath, PET Core 3.75-4.5 5-7 >2.5 70-110 0.25-0.35 < 15%*
* Note: Air temperature of 110C for 10 minutes
9.0 Attachments
9.1 Investigation of Bondability through bicomponent fibers with various D levels 9.2 Investigation of Shrinkage vs. Composition in Air Drawn Fibers 9.3 Fiber Properties in Crimping Experiment 9.4 Investigation of Spinning Speeds of Various Bicomponent Fibers 9.5 BCF and Bicomponent Trials 9.6 BCF and Bicomponent Follow-Up Trials 9.7 Comparison of Bicomponent Properties 9.8 Typical Staple Fiber Spinning System6 9.9 Typical PET Drawline Recommended for PLA Bicomponent Processing5
NatureWorks is a registered trademark of NatureWorks LLC
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9.1 Investigation of Bondability through bicomponent fibers with various D levels

NB96004 Date: January 24, 1996 From: Nancy Buehler Subject: Results from Fiber Experiment EXPERIMENT: FIX60100 OBJECTIVE: The aim of this experiment was to determine the crystalline melting temperature and thermal bondability ("tack") temperature of oriented PLA fibers at different D levels. BACKGROUND: It is useful to understand how D level influences the crystalline melting temperature and thermal bondability characteristics of PLA fibers. As stated in the experimental outline, the desirable attributes of bicomponent fibers is to (1.) have high heat resistance and (2.) low thermal bonding temperatures. The data generated from this experiment will be used to select grades of PLA to be screened in bicomponent fibers. MEASURES OF SUCCESS AGAINST STATED OBJECTIVES: Crystalline melt temperatures vs D level of as spun fibers Crystalline melting temperatures vs D level oriented 3:1 at 70C Crystalline melting temperatures vs D level after annealing at 100C, 120C and 140C, for 48 hours A plot of the Peak Melting Temperature vs Annealing Temperature to give equilibrium Tm vs D level MATERIALS: LOT # 389-2 386-1 372-3 416-2 418-2 423-3 MN 95,500 98,900 95,400 99,000 90,800 92,000 MW 218,000 226,000 203,000 230,000 210,000 234,000 PDI 2.28 2.28 2.13 2.30 2.30 2.55 LACTIDE 1.62 0.77 0.31 1.32 0.86 1.02 TOTAL % D 3 6.3 8.5 11.8 15.3 17.8
STEREOCHEMISTRY IDENTIFICATION LOT# 389-2 386-1 372-3 416-2 418-2 423-3 L-MER 97.0 95.7 91.5 89.7 85.90 83.80 D-MER 3.0 6.3 8.5 10.3 14.1 16.2 L-LACTIDE 96.80 93.56 91.40 87.09 82.13 79.05 D-LACTIDE 2.80 5.57 8.10 7.69 10.32 11.47 MESO LACTIDE 0.40 0.87 0.80 5.22 7.55 9.48
EXPLANATIONS OF DEVIATIONS FROM EXPERIMENTAL PLAN: Currently, there is no ASTM or industry standard method for determining "tack" temperature. "Tack" temperatures will not be reported here. DMA has a long lead time and samples are not long enough to fit in the grips of the fixtures
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Unable to get the "as spun" fibers down to 30 microns "As spun" fibers were oriented 3:1 at 70C, because fibers undergoing higher orientations at these temperatures spanned KEY LEARNINGS: Plotting the melting temperature by the Lot #, there is an apparent increase in melting temperature with decreasing meso and D content in the polymer. There is no statistical difference in melting temperatures among quiescent samples annealed at 100C, 120C and 140C. No evidence to support differences in the glass transition temperatures for quiescent samples annealed at 100C, 120C and 140C. Statistically, this experiment has shown that the mean glass transition temperature for oriented fiber is almost 10C higher than the as spun fibers Likewise, the onset of the glass transition is higher for the oriented fibers than for the as spun fibers The onset of the crystallization exotherm is lower in oriented fiber samples The as spun fibers have a higher crystallization exotherm peak than oriented samples There appears to be no apparent difference in peak melting temperatures between as spun and oriented fibers
TABLE 1. As Spun Fibers from Rheometer Lot # Tg onset Cryst. (C) (J/g) 48.23 3.96 51.22 1.31 50.79 50.53 49.62 50.27 Tg midpt (C) 52.85 54.53 53.58 52.88 51.29 51.94 Tc onset (C) 81.43 101.42 102.26 Tc peak (C) 96.62 120.2 119.13 Tm onset (C) 151.79 138.39 133.42 Tm peak (C) 163.64 148.83 139.04 0
389-2 386-1 372-3 416-2 418-2 423-3
TABLE 2. Oriented Fibers: 3:1 at 70C Lot # Tg onset Cryst. (C) (J/g) 62.9 27.77 62.90 27.05 62.73 16.4 61.15 10.3 Tg midpt (C) 66 65.90 65.95 64.28 Tc onset (C) 71.37 70.96 76.36 75.47 Tc peak (C) 77.76 76.93 89.44 89.32 Tm onset (C) 147.61 144.88 137.10 132.59 Tm peak (C) 161.05 160.40 148.55 147.38
389-2
386-1
13
372-3
416-2
418-2 423-3
61 10.92 59.9 4.62 58.7 2.53 57.98 1.61 54.97 52.28 53.85 50.96
64.65 60.80 60.88 59.61 57.89 54.53 57.28 55.18
80.08 89.20
100.4 108.44
127.6 129.19 103.73 105.45
137.76 137.05 120.17 120.15
TABLE 3. Annealed pellets: 100C for 48 hours Lot # Tg onset Cryst. (C) (J/g) 57.6 40.68 51.19 38.75 56.92 27.03 53.76 13.29 56.42 56.32 Tg midpt (C) 62 54.87 60.74 56.88 58.22 57.92 Tc onset (C) Tc peak (C) Tm onset (C) 149 138.62 127.99 109.14 Tm peak (C) 164.57 150.27 143.7 124.5
389-2 386-1 372-3 416-2 418-2 423-3
TABLE 4. Annealed pellets: 120C for 48 hours Lot # Tg onset Cryst. (C) (J/g) 54.9 46.59 54.43 39.91 53.02 26.3 55.09 52.04 54.87 Tg midpt (C) 60.02 57.99 56.44 59.82 55.71 57.1 Tc onset (C) Tc peak (C) Tm onset (C) 153.76 142.27 132.15 Tm (C) 170.53 158.07 147.85 peak
389-2 386-1 372-3 416-2 418-2 423-3
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TABLE 5. Annealed pellets: 140C for 48 hours Lot # Tg onset Cryst. (C) (J/g) 54.89 50.47 51.72 20.1 57.75 56.69 52.62 53.93 Tg midpt (C) 59.39 55.8 97.17 115.05 Tc onset (C) Tc peak (C) Tm onset (C) 161.23 132.63 159.17 372-3 416-2 418-2 423-3 60.6 59.05 56.14 57.19 Tm peak (C) 179.47 144.97 169.92
389-2 386-1*
A sample from Lot 3861 annealed at 140C for 48 hours displayed two melting endotherm peak. The onset temperature of the first endotherm is 132.63C with a peak temperature at 144.97C and a second endotherm onset at 159.17C and peak melting temperature at 169.92C. This trend is reproducible, see Lot 3861, annealed 140C duplicate. TABLE 6. Peak Width of Melting Endotherm As Spun Annealed Peak Width (C) 12.14 11.51 7.97 0 0 0 Oriented Peak Width (C) 14.29 11.83 11.91 15.6 0 0 Annealed 100C Peak Width 16.09 12.75 15.35 16.74 0 0 Annealed 120C Peak Width 15.41 15 15.39 0 0 0 140C Peak 16.96 11.34 0 0 0 0
Lot # Width 389-2 386-1 372-3 416-2 418-2 423-3
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9.2 Investigation of Shrinkage vs. Composition in Air Drawn Fibers

NB96005
NAF-649480 PART 1. The Relative Thermal Shrinkages of PET and PLA Filaments Location: Hills, Incorporated 7785 Ellis Road West Melbourne, FL 32904 Key Contact: Jerry Taylor Arthur Tally PH: (407) 724-2370 FAX: (407) 676-7635
Objective: Compare the relative shrinkages of PET and PLA as spun filaments spun at 1.0 g/min/hole with varying draw force. Key Observations: 1. Higher filament velocities reduce boil shrinkage for PET and PLA filaments. (Figures 1. and Figure 2.) 2. At moderate throughputs,1.0 g/min/hole, the critical filament velocity is slightly higher for PET filaments, Figure 1. (Critical filament velocity defined as the velocity at which filament shrinkage is reduced to 10% or below). 3. There appears to be an increase in boil shrinkage for PET filaments spun at speeds above 5300 m/mint A similar trend has been observed in PLA filaments produced at Alex James and Associates. (Figure 1.) 4. Critical filament velocity for PLA filaments is calculated to be 4526 m/min for the processing conditions disclosed. (Figure 2.) 5. Critical filament velocity for PET is 5314 m/min at comparable processing conditions. (Figure 1.) 6. PLA yields lower birefringence values at all filament velocities suggesting lower degrees of crystal and amorphous orientation. (Table 1.) Unexpected Occurrences: 1. Due to complications with the confidentiality agreement resulting in a one way nonanalysis agreement with Ason. Cargill, Inc. was not allowed to observe Ason technology or other filament processing using Hill's slot die. Procedure: 1. Air attenuated slot die located approximately 34 " from spinneret 2. 2 extruders, melt pumps and 144 hole pack purged with PP-35 MFR and then purged with PLA Lot 515-710. 3 Polymer was packaged in 10 lb bags and put into hoppers with nitrogen sparge. 4. Melt temperature set at 230C for both extruders. 5. Spinnability performance evaluated by Ason representatives; rating system: qualitative good or poor
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Equipment: 1. Pilot spinline utilizing (2) 1.25" single screw extruders 2. Slot die with air quench (designed and manufactured by Hill, Inc.) 3. Melt pumps (2): 6 cc/rev 4. Pack: 1 X 144 capillary with 0.35 mm diameter, 4:1 I/d 5. Air quench used Trial Outline: Throughputs: Air Draw Pressures: 1.0 g/min/hol 10-60 psi PLA with 10 psi increments 10-80 psi PET with 10 psi increments 20" for PLA (Location of Draw Unit)34" for PET Collected and recorded by Hills, Inc. Refer to Development Log Sheets 1 & 2 GPC DSC Filament boil shrinkage Birefringence Fiber diameter Calculated Filament Velocities
Distance from Spinneret:
Process Data:
Fiber Data:
Polymer Evaluated: Lot/Box 515-710 Mn 69,400 Mw 146,000 PDI 2.1 %R 1.2 % Lactide 0.4 % Olig. 0.1
Discussion: The objectives outlined for the scheduled December 913 trial at Hills, Incorporated were to (1) prepare a low shrinkage web using Ason technology and (2) make bicomponent (PP/PLA) filaments to characterize crimp and loft properties. There were some modifications made to the run plan because of complications with the confidentiality agreement with Ason/Hills. It was negotiated that a one way nonanalysis agreement be put into place. Filament Velocity and its Impact on Shrinkage: It appears, from process information shared by Ason, that the critical filament velocity for PET is slightly higher than for PLA filaments run under similar conditions, (refer to Table 1). Both cases ran comparable throughputs of 1.0 g/min/hol. Spin ratings were not measured using the S.Gessner 18 system. Birefringence values were indicative of low spinline stress during spinning (refer to Table 1). And higher filament velocities were required to increase spinline stress to achieve low shrinkage filaments, those with less than 15%. Polymer variables as well as processing parameters may be responsible for this trend. Molecular weight of Lot 515-710 was slightly lower than previously run at Alex James, Inc. GPC analyses performed on these filaments ranged from number average molecular weights of 63,000 to 66,000 and weight averages between 133,000 and 136,000. The lowest weight average run prior to this trial was approximately 155,000. Lower molecular weights may be partially responsible for reduced spinline stress compounded
17
with melt temperature effects. Residual lactide and oligomer values were both less than 0.5%; low enough not to influence melt flow character of the resin. As far as processing parameters are concerned, melt temperature was set at 230C, about 10 degrees cooler than previously run at other trials. Cooler melt temperatures would imply highly spinline stress. Throughputs were about 20% higher than normally run and more likely the reason for the shift to higher filament velocities. In addition to higher throughputs, the distance between the drawing unit and spinneret may also be responsible for low spinline stress. Generally, the stick point is a good indicator of how cool/hot filaments are before they are drawn. A stick point closer to the slot die will draw the filaments while they are still molten generating a lower degree of spinline stress affecting the overall degree of orientation and stressinduced crystallization. Although, utilizing Ason's technology with its adjustable draw unit may provide a process to control the amount and degree of orientation intoduced to the system, whether controlling spinline stress is advantageous or not is still in question. PLA filaments with low degrees of shrinkage have been made on conventional lines reducing the need for Ason technology to make bonded fabric with superior performance properties.
18
19
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21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
9.3 Fiber Properties in Crimping Experiment

Table 1: Sample Fiber Properties (Lot 440-719) % Break Fiber Modulus Crystallinity Elongation g/denier jg-1 72 24.6 28 16.4 37 29 18.7 25 19 30
Tenacity g/denier 1.54 320 dpf input multifil medium crimp 2 air entangled 1.74 self crimped 2.07
Figure 1: TechniService Texturizing (crimping) Process
Stuffer box Crimper Creel with 8 bobbins
Winders
Heated Draw 90C Rolls 75C
44
9.4 Investigation of Spinning Speeds of Various Bicomponent Fibers Trial Number: NWB12097BC Trial Description: Relative Spinning Speeds of Sheath-Core and Side-by-Side Bicomponents Containing PP/PP, PET/PP and PLA/PP. Trial Reference Number: TR-510D Location: Hills, Incorporated 7785 Ellis Road West Melbourne, FL 32904 Key Contact: Jerry Taylor Phone: (407) 724-2370 Fax: (407) 676-7635
Overview: The objectives of this trial were to compare the relative spinning behavior among PP/PP, PET/PP and PLA/PP sheath-core and side-by-side bicomponents and determine whether PLA/PP bicomponents offer any commercially valuable processing or property advantages to conventionally used materials. Trial results do in fact suggest that there are both processing and property advantages to using PLA with PP configured sideby-side, 50/50. The configuration mentioned above had the fastest calculated filament velocities over a large range of air draw forces and later these filaments proved to have more induced crimp behavior than PET/PP configured the same way. Objective(s): 1. Define the quench limitations of PP/PP, PLA/PP and PET/PP sheath-core bicomponents 2. Measure the relative speeds of spinning for sheath-core and side-by-side PP/PP, PET/PP and PLA/PP bicomponents. 3. Determine the relative crimp behavior of PET/PP and PLA/PP side-by-sides. Results: It appears that there is an inverse relationship among: Measured filament diameter, calculated filament velocity and applied air draw force variables for the sideby-side bicomponents. PLA/PP in a 50/50 weight ratio showed the most pronounced response to increasing air draw force. The results of this effect are illustrated in Graphs 1. and 2.
45
Graph 2.
For sheath-core configurations, fiber diameter did decrease with increasing air draw force as expected, however, it was without the same level of resolution as observed with the samples configured side-by side. PP/PP, PET/PP and PLA/PP in sheath-core configurations had similar filament velocities for a given air gun pressure. It is speculated that for sheath-core configurations, the PP core controls the quench rate of the filaments, ultimately controlling the final filament velocity. The rate at which different materials quench in the spin-line determines their relative spinning behavior. Under similar spinning conditions, relative spinning behavior may be represented by the
46
stick point. Stick point is the measured distance in the spin-line, in inches, from the spinneret to where filaments stick to a stainless steel rod. These measurements demonstrate that the spinning behavior of polypropylene can be dramatically improved under critical quench conditions by adding a sheath of PLA. PET on the sheath offers the same processing advantages as PLA under moderate spinning conditions. However, PET/PP is limited at low throughputs, and/or at high air draw forces due to filament breaks. It is thought that the fast quenching behavior of PET cools the filaments close to the spinneret decreasing the elasticity of the spin-line. Table 1. below displays the stick points for PP/PP, PLA/PP and PET/PP at three different quench conditions. From the table, it appears that sticking is the critical issue for monocomponent PP. Sticking can occur at higher throughputs or at insufficient air draw forces. PET/PP, on the other hand is ultra sensitive to quenching conditions and frequently breaks are experienced at lower throughputs or high air gun pressures. PLA/PP seems to be less sensitive to either of these extremes. Less sensitivity to quenching conditions may provide processing advantages to conventional materials used today. Less sensitivity may mean faster speeds of spinning which may lead to higher production rates overall.
Table 1. Spinning Behavior Measured as Stick Point for 50/50 Sheath-Core Bicomponents Throughput (g/min/hole) High Quench Medium Quench Low Quench PP/PP breaks 21 PLA/PP PET/P P 2 breaks 4 breaks
0.1 0.2
PP/PP PLA/P PET/P PP/PP PLA/P PET/P P P P P breaks breaks breaks breaks breaks breaks breaks 3 breaks 7 4 breaks 47
0.3 0.4 0.5 0.6 0.7 0.8 0.9 1 1.1 1.2
5 7 9 11 12 13 14 17 17 17
3 6 6 7 8 9 9 9 10 12
breaks breaks breaks breaks 3 5 6 6 7 7
11 13 13 20 sticking sticking sticking sticking sticking sticking
5 6 7 7 6 10 13 13 15 18
breaks breaks breaks 7 7 8 8 9 9 10
sticking sticking sticking sticking sticking sticking sticking sticking sticking sticking
5 7 8 10 10 12 13 17 17 20
breaks breaks breaks 6 7 8 8 9 11 11
Self-crimp is a behavior that is often observed with natural fibers, like cotton. However, this property can also be achieved with thermoplastics when there is a viscosity differential between the two polymers being used. Traditionally, PET has been used in combination with PP to achieve this type of behavior. Because PLA has greater shrinkage potential and shrinkage tension at lower temperatures, replacing PET with PLA would require less polymer to achieve the same crimping behavior. Or if an equivalent quantity of PLA were used, improved crimp would be possible. Shrinkage tension measurements are not complete yet, but Tables 2. and 3. below report crimp frequency for PLA/PP and PET/PP S/S at 50/50 and 30/70 weight basis ratios.
Table 2. Crimp Frequency (# crimps/inch) for PLA/PP and PET/PP Side-by-Side Bicomponents at 50/50
23C Temperature: Polymer Throughput (g/min/capillary) 0.3 0.4 0.5 0.6 0.7 PET/PP (crimp/in.) 2.7 3.8 4.8 4.9 5.3
50C
100C
PLA/PP PET/PP PLA/PP PET/PP PLA/PP (crimp/in.) (crimp/in.) (crimp/in.) (crimp/in.) (crimp/in.) 9.6 7 7.8 5 6.4 48 6.3 7.2 9.5 5.4 4.9 20.7 14.1 9.3 18.5 12 108.7 35.3 38.8 42.3 38.8 105.8 52.2 56.4 43.7 55
0.8 0.9 1 1.1 1.2
4.4 4.7 2.1 4.2 3.2
2.2 6.1 5.8 4.7 5.2
5.8 6.2 3.6 5.7
11.8 4.3 10.6 9 9.3
49.4 63.5 49.4 39.5 45.2
46.6 40.1 44.5 26.1 57.2
Table 3. Crimp Frequency (# crimps/inch) for PLA/PP and PET/PP Side-by-Side Bicomponents at 30/70
23C Temperature: Polymer Throughput (g/min/capillary) 0.3 0.4 0.5 0.6 0.7 0.8 0.9 PET/PP (crimp/in.) 7.9 1.9 5.8 4.4 9.7 5.3 5.4
50C
100C
PLA/PP PET/PP PLA/PP PET/PP PLA/PP (crimp/in.) (crimp/in.) (crimp/in.) (crimp/in.) (crimp/in.) 12.7 8.6 9.1 6.8 6.3 6.4 7.4 19.1 12.1 13.5 9.9 10.4 8.5 8.4 26.5 24 29.8 24 25.4 14.4 19.4 35.3 35.3 38.8 38.8 22.6 45.9 30.3 44.5 45.2 35.3 36.8 52.2 48.7 36.8
Materials: PLA Lot/Box 515-710 Mn 69,000 Mw 146,000 PP Montell polypropylene 35 MFI PDI 2.1 % lactide 0.4 %R 1.2
Discussion: Fiber structure development and property characteristics are strongly influenced by the thermal stress histories experienced by the polymer in the spin-line. Although two polymers are extruded at the exact melt temperature, as is the case when making bicomponent fibers, these materials can have substantially different thermal stress histories. Depending on these thermal histories and mutual interactions, the possibility of improving or controlling the structure and properties of high-speed spun bicomponents exists. High-speed spinning really addresses the rate at which the filaments can be drawn. Breaks or sticking during spinning are considered processing limitations. In the sheathcore configuration, PET/PP filaments are extrememly sensitive to low throughputs and NatureWorks LLC Confidential 49
high air pressures. PP/PP on the other hand, does not quench as quickly and therefore sticks and ropes at higher throughputs and/or low air gun pressures. It seems that PLA/PP filaments do not quench nearly as fast as PET/PP and therefore do not break at lower throughputs and high air draw forces. However, PLA/PP sheath-core bicomponents quench relatively fast when compared to PP. PLA/PP sheath-core bicomponents can be spun at a wider range of processing conditions where PET/PP and PP/PP have limitations. High-speed spinning for side-by-side bicomponents have a complexity of issues different from sheath-core filaments. The spinning behavior of the side-by-sides filaments cannot be captured by stick point as was done for the sheath-core filaments. Two polymer extruded at one melt temperature experience different quench rates. Both surfaces are exposed which make it difficult to determine a "true" stick point. Holding air pressure constant, and increasing the throughput, PET/PP and PP/PP both displayed roping behavior. At 100 psi gun pressure and a throughput of 1.2 g/min/capillary, evidence of roping was observed for the PET/PP bicomponents. At the same throughput and 50 psi, serious sticking was observed. On the otherhand, PLA/PP was not nearly as sensitive to roping or sticking. It is believed that roping and sticking exists in the PET/PP side-bysides because PP is being extruded at 295C. Typically, it is extruded at 230C or so. Because it is more than a 100 degrees above its true melting point, about 170 degrees or so, it increases the time required to quench the material. Between the PLA/PP and PP/PP bicomponents, it was difficult to determine a big difference in spinning behavior for side-by-sides. This was not the case in the sheath-core configurations. Filament diameters for PLA/PP side-by-sides revealed substantially higher calculated filament velocities. Not only did the 50/50 PLA/PP side-by-sides spin faster than any of the other combinations used, they also achieved more crimp than their as spun PET/PP counterparts. This trend was not observed in the 30/70 PLA/PP side-by-sides. It is postulated that as PP becomes more of the continuous phase spinning behavior and properties will most likely be representative of PP. Trial Outline: Part 1. Samples were collect for S/C bicomponents at increasing throughputs and constant pressure, 80 psi, for three different quench conditions. Stick point was the measured response variable for each of the combinations listed below. 50/50 PP/PP PLA/PP PET/PP Throughput (g/min/capillary) 0.1 0.2 High Quench (4" at 44F) 30/70 PP/PP PLA/PP PET/PP Medium Quench (2" at 44F) Low Quench (1" at 44F)
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0.3 0.4 0.5 0.6 0.7 0.8 0.9* 1 1.1 1.2 * Due to meter pump limitations, maximum throughput for the 30/70 bicomponents was 0.9 g/min/capillary Part 2. for the S/S bicomponents, samples were collected at each of the conditions listed below. Filament diameter and crimp tests were performed on these. 50/50 30/70 PP/PP PP/PP PLA/PP PLA/PP PET/PP PET/PP Throughput (g/min/capillary) 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9* 1 1.1 1.2 High Quench (4" at 44F)
Part 3. Throughput was held constant at 0.8 g/min/capillary, while air pressure varied from 20-110 psi. Samples were collected in 10 psi increments. Composition and configurations are listed below. Fiber diameter were collected on these samples. Composition PP/PP PLA/PP PET/PP sheath-core 50/50 30/70 side-by-side 50/50 30/70
51
Equipment/Processing: Extruders: 2 X 1 1/4" diameter screws with L/D 30:1 4 Zones, no screw cooling Drying capacity on extruder(s): Conair 110 lb capacity and Novatec with 250 lb capacity Meter pumps: 2 1X6 cc/rev Quench: One-sided with cross-flow air set up to deliver approximately 500-1000 fpm
Pack Build Pack Top: Standard Screen Sup Plate: Standard Meter V. Plate: 7696 Dist. Plate: 12605 Dist Plate: 11226 Dist Plate: 12229 Dist Plate: 12230 Spinneret: 288 Round, 0.35 mm
Polymer
Sheath PLA Lot 515-710
Core PP Montell 35 MFR
Extrusion Temperatures (C) zone1 zone 2 zone 3 zone 4 Melt Pressures Extruder Pack
187 209 219 229
187 209 219 229
750 see above
750 see above
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adjusted as a variable from 0.1 g/min/cap to 1.2 g/min/cap Meter Pump 6 size/rpm 24.6 Extruder Amps/ (%) 6 60
Speeds
adjusted as a variable from 0.1 g/min/cap to 1.2 g/min/cap 6 24.6 6 60
9.5 BCF and Bicomponent Trials NatureWorks LLC Confidential 53

TRIAL: BCF trial By: Donavon Kirschbaum

Dates:
Trial #BCF84320
October 19,20.21, 1998

Location: Hills Inc 7785 Ellis Road W. Melbourne, Fla Key Contact:
Donavon Kirschbaum (NatureWorks LLC)

Objective: Produce trilobal BCF 18-20 dpf at 1300 denier to be used for carpet fiber. Produce bicomponent side by side fibers consisting of the following: PLA/PLA 1.4%D/1.4%D different mws PLA/PLA 1.4%D/3.2%D PLA/PET 1.4%D/PET Measure of success against stated Approximately 200 lb of 1270/67 BCF trilobal fiber was produced. Bicomponent samples were produced. The samples will be tested and characterized for self-crimping properties.
1) Equipment Hills spin/draw line: bicomponent with 2-1.25 in. extruders. Spin pack: trilobal 67 holes for BCF Spin pack: 144 hole .35 mm (see figure below) 2) Materials: PLA lot # MF0628P104 MN 88.6k, Mw 179.4k, 1.4%D, MFI 8.1, color 29, %res. .17 GMID 112679 #M12328P103 MN 67.9 MW 137 3.2%D, MFI 30.9, %roes .14, GMID 111184
3) Explanation for deviations from the plan: none 4) Unexpected occurrences: Drawing between draw roll 1 and 2 and drawing between draw roll 3 and 4 had a significant effect on the max draw ratio. The only difference between the two is the distance between the draw rolls. The closer the draw rolls the higher the maximum draw ratio. 5) Key learnings: BCF PLA has improved drawability when drawing in water Trilobal fibers process easily 1% TIO2 masterbatch has a positive delustering effect. Bicomponent. PLA of the same D level with two different molecular weights worked well for self-crimping fiber. PLA/PET side by side had good adhesion under the microscope PLA/Pet side by side worked for a self-crimping fiber.
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6) Overall assessment: The drawing process needs further optimization to achieve the optimum fiber performance. However, until the fiber has been evaluated in a carper sample optimization will be put on hold. Process conditions:
Polymer Extrusion cond. Zone 1 Zone 2 Zone 3 Zone 4 Spin Head melt temp pressure extruder pack pump size cc/rev
1.4% D 3.2% D PET
200 210 220 230 230 230 750 1250 6
200 210 220 230 230 228 750 1150 6
280 290 290 290 280 274 750 1420 6
Samples:
BCF
Polymer was low %D 1.4% Reference # 15-36-2 15-36-5 15-36-9 15-36-13 15-36-17 15-36-21 15-36-25 15-36-30 15-36-33
All BCF samples were drawn at 4.2 draw ratio.
Bicomponent To be used for self crimp fibers
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Sample reference table Reference type polymer # 15-45-2 s/s 1.4%D pla/1.4%D PLA 15-45-5 s/s 1.4%D pla/1.4%D PLA 15-45-9 s/s 1.4%D pla/1.4%D PLA 15-47-2 s/s 1.4%D PLA/3.2%D PLA 1.4%D/PET 1.4%D/PET 1.4%D/PET
comments side by side, 1.4%DPLA high mw/1.4%D PLA low mw side by side, 1.4%DPLA high mw/1.4%D PLA low mw side by side, 1.4%DPLA high mw/1.4%D PLA low mw
15-48-1 15-48-2 15-48-3
s/s s/s s/s
4.6 draw ratio 4 draw ratio 3.5 draw ratio
BCF Process conditions

BCF samples
15-36-2 As spun dpf total denier denier /filament No. orifices Draw ratio spin finish Denier roll speed denier roll temp # wraps steam between denier and draw 1 Draw roll 1 m/min draw roll 1 temp # wraps steam between draw 1 and 2 BCF Draw roll 2 m/min draw roll 2 temp # wraps 660 130 17 660 130 17 660 130 17 660 130 17 660 130 17 660 130 17 660 130 17 660 130 17 660 130 17 75.2 1200 17.9 67 4.2 756A 156 amb. 3 yes 202 70 5 yes 15-36-5 75 1190 17.8 67 4.2 756A 156 amb. 3 yes 202 70 5 yes 15-36-9 80 1278 19 67 4.2 756A 156 amb. 3 yes 202 70 5 yes 15-36-13 79.8 1272 19 67 4.2 756A 156 amb. 3 yes 202 70 5 yes 15-36-17 80.4 1283 19.1 67 4.2 756A 156 amb. 3 yes 202 70 5 yes 15-36-21 80.6 1286 19.2 67 4.2 756A 156 amb. 3 yes 202 70 5 yes 15-36-25 81 1293 19.3 67 4.2 756A 156 amb. 3 yes 202 70 5 yes 15-36-30 79 1260 18.8 67 4.2 756A 156 amb. 3 yes 202 70 5 yes 15-36-33 79.8 1273 19 67 4.2 756A 156 amb. 3 yes 202 70 5 yes
Draw roll 3 m/min draw roll 3 temp
670 80
670 80
670 80
670 80
670 80
670 80
670 80
670 80
670 80
56
# wraps texture jet temp texture jet pressure interlacer pressure transvector pressure
10 80 50 35 50
10 80 50 35 50
10 80 50 35 50
10 80 50 35 50
10 80 50 35 50
10 80 50 35 50
10 80 50 35 50
10 80 50 35 50
10 80 50 35 50
testing at Hills tenacity elongation shrink (boiling water) 2.13 40 10 2.5 45 5 2.2 42 6 2.4 43 2.3 44 10 2.3 45 8 2.5 42 2.6 45 8 2.5 46 6
Bicomponent sample process conditions

BICOMPONENT 1.4%D PLA/1.4%D PLA 1.4%/3. 1.4%D 2% PLA/PET 15-45- 15-45- 15-45- 15-47-2 15-48-1 15-48-2 152 5 9 48-3 As spun dpf 18 18 19.3 19.2 18.55 total denier 829 829 750 600 697 760 denier /filament 5.7 5.7 5.2 4.16 4.8 5.3 No. orifices 144 144 144 144 144 144 144 Draw ratio 3.3 3.3 2.6 3.5 4.66 4 3.5 spin finish 756A 756A 756A 756A 756A 756A 756A 296 296 296 296 296 296 Denier roll speed 296 denier roll temp amb. amb. amb amb amb amb amb # wraps 3 3 3 3 3 3 3 298 298 298 298 298 298 298 Draw roll 1 (tension roll) tension roll temp amb. amb. 70 amb amb amb amb # wraps 4 4 4 4 5 5 5 Draw roll 2 300 300 790 57 300 300 300 300
m/min draw roll 2 temp # wraps Draw roll 3 m/min draw roll 3 temp # wraps Draw roll 4 m/min (relax) draw roll 4 temp # wraps testing at Hills tenacity elongation shrink (boiling water)
80 7 1000 100125 9 950 amb 7
80 7 1000 114 9 950 amb 7
120 7 790 34 9 890 amb 7
78 7 1050 119 9 1018 amb 7
77 7 1400 100 9 1335 amb 7
77 7 1200 100 9 1170 amb 7
77 7 1058 100 9 1040 amb 7
20
16
3.3 16 8
3 34 8
2.9 52
increased roll 3
Spin/draw line
Draw roll 1 Spin
Drawing
pac
Steam
Winder Draw roll 2 Cooling wheel
Stea Denier
Draw roll 3
Texturiz
58
ANALYTICAL--PLA values 48-(1-3)
DSC--PLA values
SHRINKAGE % H2O Shrink 100C
SINGLE FILAMENT TENACITY Ultimate Elongation Elongation at Peak
% Crystallinity
Peak Load (g)
Load (cm)
Std Dev
Std Dev
Tm
Mz
Mn
MP
Tg
015-45-02 015-45-05 015-45-09 015-47-02 015-48-01 015-48-02 015-48-03
75100 69057 69616 70445 77604 67880 71620
147979 143332 142598 135140 145622 145108 147076
133874 128980 121392 117250 126558 130550 132653
1.97 2.08 2.05 1.92 1.88 2.14 2.05
230219 227271 228991 211530 228177 233700 234408
1.56 1.59 1.61 1.57 1.57 1.61 1.59
317535 317596 325843 296285 318147 332552 332993
62.96 61.63 60.24 61.27
166.47 167.41 168.2 157.85 170 168.61 167.82
48 47.91 50.15 41.37 23.67 23.59 23.56
60.31 24.79 33.23 28.02 24.90 15.73 11.32
4.71 4.92 2.59 2.67 0.93 0.68 1.30
18.56 17.18 17.28 17.93 17.3 16.21 18.02
1.68 0.76 1.18 2.23 2.21 0.61 0.51
4.64 5.08 4.42 4.23 2.5 3.16 5.45
0.64 0.53 1.12 0.4 0.33 0.34 0.76
Boiling Water Shrinkage After Length After Length After Length After Length After Length Avg Shrink Sample# %Shrink %Shrink %Shrink %Shrink %Shrink StdDev 4.707711 4.921806 2.588495 2.665934 0.931695 0.679084 1.295702
015-45-02 015-45-05 015-45-09 015-47-02 015-48-01 015-48-02 015-48-03
4.6875 60.9375 9.875 17.70833 7.875 34.375 9 25 9 25 10.125 15.625 10.83333 9.722222
4 8.5 8.375 8.125 9 10.0625 10.5625
66.66667 29.16667 30.20833 32.29167 25 16.14583 11.97917
5.5625 9.25 8.3125 8.625 8.875 10.0625 10.625
53.64583 22.91667 30.72917 28.125 26.04167 16.14583 11.45833
4.9375 9.0625 7.6875 8.75 9.1875 10.0625 10.75
58.85417 24.47917 35.9375 27.08333 23.4375 16.14583 10.41667
4.625 8.4375 7.8125 8.6875 9 10.25 10.4375
61.45833 29.6875 34.89583 27.60417 25 14.58333 13.02083
60.3125 24.79167 33.22917 28.02083 24.89583 15.72917 11.31944
59
% 45.9 50.5 43.9 42.2 25.2 31.4 54.2
Sample
Std Dev
Mz/Mw
Mz+1
PDI
Mw
Material extrusion cond. Zone 1 Zone 2 Zone 3 Zone 4 Spin Head melt temp pressure extruder pack pump size cc/rev
1.4% D 200 210 220 230 230 230 750 1250 6
3.2% D 200 210 220 230 230 228 750 1150 6
PET 280 290 290 290 280 274 750 1420 6
Hills trial Oct. 1998 for BCF and bicomponent BCF samples 15-36-13 15-36-17 15-36-21 15-36-25 15-36-30 15-36-33 79.8 80.4 80.6 81 79 79.8 1272 1283 1286 1293 1260 1273 19 19.1 19.2 19.3 18.8 19 67 67 67 67 67 67 4.2 4.2 4.2 4.2 4.2 4.2 756A 756A 756A 756A 756A 756A 156 156 156 156 156 156 amb. amb. amb. amb. amb. amb. 3 3 3 3 3 3 yes yes yes yes yes yes 202 202 202 202 202 202 70 70 70 70 70 70 5 5 5 5 5 5 yes yes yes yes yes yes 660 130 17 670 80 10 80 50 35 50 660 130 17 670 80 10 80 50 35 50 660 130 17 670 80 10 80 50 35 50 660 130 17 670 80 10 80 50 35 50 660 130 17 670 80 10 80 50 35 50 660 130 17 670 80 10 80 50 35 50
As spun dpf total denier denier /filament No. orifices Draw ratio spin finish Denier roll speed denier roll temp # wraps steam between denier and draw 1 Draw roll 1 m/min draw roll 1 temp # wraps steam between draw 1 and 2 BCF Draw roll 2 m/min draw roll 2 temp # wraps Draw roll 3 m/min draw roll 3 temp # wraps texture jet temp texture jet pressure interlacer pressure transvector pressure testing at Hills tenacity elongation shrink (boiling water)
15-36-2 75.2 1200 17.9 67 4.2 756A 156 amb. 3 yes 202 70 5 yes 660 130 17 670 80 10 80 50 35 50
15-36-5 75 1190 17.8 67 4.2 756A 156 amb. 3 yes 202 70 5 yes 660 130 17 670 80 10 80 50 35 50
15-36-9 80 1278 19 67 4.2 756A 156 amb. 3 yes 202 70 5 yes 660 130 17 670 80 10 80 50 35 50
2.13 40 10
2.5 45 5
2.2 42 6
2.4 43
2.3 44 10
2.3 45 8
2.5 42
2.6 45 8
2.5 46 6
114 bobbins at 350 filiments each were used for the staple production
9.6 BCF and Bicomponent Follow-Up Trials
60
TRIAL: BCF Fiber By: Donavon Kirschbaum
Trial #BCF91220
Dates:
March 22-24, 1999
Location:
Hills Inc 7785 Ellis Road W. Melbourne, Fla
Key Contact:
Donavon Kirschbaum (NatureWorks LLC) Arthur Talley (Hills)
Objective: stated
Produce trilobal BCF 18-20 dpf at 1300 denier with 3.4%D PLA to be used for carpet fiber. Evaluate four spin finishes supplied by Goulston Pilot test to produce POY bicomponent trilobal fiber 72/36 self-bulking with 1.5%D/3.4%D PLA.
Measure of success against

Samples were produced having the same characteristics as the 1.5%D used in the past. Heat setting and draw conditions needed to be optimized. Samples were spun with the different finishes. Two looked ok two were poor. Testing underway Two samples were produced. One at 2000 m/min. and one at 3200 m/min. Tenacity was low (1g/denier) however, bulking looks good.
Reference: 15-62-67 Equipment

Hills spin/draw line: bicomponent with 2-1.25 in. extruders. Spin pack: trilobal 67 holes for BCF Spin pack: 144 hole .35 mm Barmag winder capable of high speed spinning (see figure below)
Materials:
PLA lot # NB1528P106 MN 88.5, Mw 173, PDI 1.96, Color 48.4, res. lactide .09%, Percent D 3.4 GMID 112681 # MF0128P105 MN88.9k, Mw 193.8, 1.5%D, MFI 6.6, color 38, %res .21, GMID 112679
Unexpected occurrences: NatureWorks LLC Confidential 61

POY samples had low tenacity (1 g/denier) the goal is 3. Process development is needed to increase the value.
Key learnings: BCF using 3.4%D PLA 3.4% D polymer behaved similar to the 1.5% D used in the past for BCF. The 1300/67 trilobal fiber had the following properties: 2-2.5 g tenacity 45-50% elongation 10% shrink in boiling water Heat setting the 3.4% D polymer requires longer residence time on heat set rolls. 25 wraps at 700 m/min. were needed to get 10% shrink vs. 15 wraps for 1.5%D. This may be a problem on commercial lines? Draw ratio increased from 4.2 (1.5%D) to 4.6 (3.4%D) TIO2 was not used to get the results. TIO2 improves fiber breakage thus with TIO2 the process should improve. Spin Finish Four finishes from Goulston Technologies and a silicone were tested. Lurol 7275- used in the past and works fairly well Lurol NF-6004 Lurol PP-8102GL-20 Lurol PP-3772-20 Formisil 45 from OSI chemicals lot# 23555D041095 Lurol 7275 and Lurol NF-6004 had the most favorable results. The other two inhibited fiber breakage and poor spinability. Goulston is doing a full evaluation of the spin finish along with a 756A (which translates into Lurol number PP5656) POY reference 15-67 Two samples were produced as a first step to evaluate the ability to produce bicomponent POY trilobal fiber for self-bulking low denier yarn. A 1.5%D PLA and a 3.4%D PLA were used. The idea is if the fiber is spun at high enough speed (~ 3,000 m/min) the low % D will inhibit low boiling water shrink whereas the 3.4% D will have high shrink thus creating self bulk. A Barmag winder was placed directly under the spin head. Samples were spun at 2,000 and 3,200 m/min. Process temperatures: Temperature zone 1 zone2 Zone 3 Melt Pressure Amp 180 220 230 225 1480 11 East 3.4 200 210 227 225 1970 8.5 West 1.5
Tenacity was low at around 1 g/denier
Next Step: Send Goulston the finish samples to evaluate.
62
Evaluate samples of BCF produced with 3.4% D and determine the feasibility of the product being produced commercially. Evaluate bicomponent POY samples and determine the feasibility of producing. (longer term) Guilford is planning a trial to produce a mono-component POY PLA continuous fiber.
Process conditions:
Polymer Extrusion cond. Zone 1 Zone 2 Zone 3 Zone 4 Spin Head melt temp Screen pack pressure extruder pack pump size cc/rev
3.4% D
200 210 220 230 230 228 150 750 1028 6
DRAWING
Notebook ref. 15-62-9 run # 9 156 Denier roll
63
Draw roll 1 speed temperature wraps Draw roll 2 speed temperature wraps aw roll 3 speed temperature wraps draw ratio spin finish spin finish setting denier tenacity elongation shrinkage boiling H20
162 70 15 740 100 10 735 80 14 4.7 lurol 7275 150 1170 2.3 47 10.8
For comprehensive details click on spread sheets below
Hills testing notebook ref. run # Denier roll Draw roll 1 speed temperature wraps
15-62-1 1 156 162 70 15
15-62-2 2 156
Developing conditions for 3.4%D PLA 15-62-3 15-62-4 15-62-5 15-62-6 3 4 5 6 156 156 156 156
64
A N A LYTICA L % Residual Lactide
Mz/Mw
S a m p le 0 1 5 -6 2 -0 1 0 1 5 -6 2 -0 2 0 1 5 -6 2 -0 3 0 1 5 -6 2 -0 4 0 1 5 -6 2 -0 5
3 .4
0 .0 5 0 .0 5 0 .0 5 0 .0 4 0 .0 4
86774 86732 85783 87060 85050
168290 169150 166970 166754 165194
148842 153133 152197 151727 144086
1 .9 4 1 .9 5 1 .9 5 1 .9 2 1 .9 4
258544 261495 257083 256026 254541
1 .5 4 1 .5 5 1 .5 4 1 .5 4 1 .5 4
355534 362388 353352 352775 351601
Boiling Water Shrinkage After Length After Length After Length After Length After Length 2.00 4.69 7.38 7.88 8.94 10.38 10.31 10.63 10.81 11.25 10.63 Sample# %Shrink %Shrink %Shrink %Shrink 83.33 64.06 47.92 38.02 39.06 11.98 15.63 7.81 10.94 8.85 12.50
015-62-01 015-62-02 015-62-03 015-62-04 015-62-05 015-62-06 015-62-07 015-62-08 015-62-09 015-65-10 015-65-11
1.75 5.81 6.31 8.13 7.88 10.69 10.00 10.88 10.69 11.19 10.56
85.42 51.56 47.40 32.29 34.38 10.94 16.67 9.38 10.94 6.77 11.98
11.06 4.31 6.63 6.56 7.25 10.75 9.88 10.88 10.88 11.13 10.00
7.81 64.06 44.79 45.31 39.58 10.42 17.71 9.38 9.38 7.29 16.67
1.94 4.19 7.13 7.88 8.63 10.75 10.19 10.81 10.75 11.25 10.25
83.85 65.10 40.63 34.38 28.13 10.42 15.10 9.90 10.42 6.25 14.58
2.00 4.31 6.25 7.44 7.31 10.56 10.13 11.06 10.69 10.94 10.50
65
Mz+1
PDI
Mw
%D
Mz
Mn
MP
Spin/draw line
Draw roll 1 Spin
Drawing
pac
Steam
Winder Draw roll 2 Cooling wheel
Stea Denier
Draw roll 3
Texturiz
66
Hills testing notebook ref. run # Denier roll Draw roll 1 speed temperature wraps
15-62-1 1 156 162 70 15
15-62-2 2 156
Developing conditions for 3.4%D PLA Evaluating spin finishes 15-62-3 15-62-4 15-62-5 15-62-6 15-62-7 15-62-8 15-62-9 15-62-10 15-62-11 15-62-12 15-62-13 15-62-14 15-62-15 3 4 5 6 7 8 9 10 11 12 13 14 15 156 156 156 156 156 156 156 156 156 156 156 156 156
Draw roll 2 speed 700 temperature 100 wraps 10 Draw roll 3 speed 685 temperature 80 wraps 14 draw ratio 4.5 spin finish lurol 7275 spin finish setting 150 1420 denier 2.3 tenacity elongation 29 80 shrinkage boiling H2
740 110 15 130 135 145 135 25 130 691 0.0 1429 1.8 31 70 0.0 1415 2 45 40 0.0 1425 2 49 35 0.0 1440 1.8 47 17 0.0 1440 2 50 8.7 0.0 1250 2.25 49 12.5 0.0 1258 1.95 46 11 135 735 4.7 1170 2.3 47.5 10.8 130
700 127 690
740 135 735 4.7 7275 1175 2.6 54 9
0.0 0.0 0.0 0.0 4.5 Lurol NF- Lurol PP- Lurol PP- silicone F no finish 1210 2.26 50.6 8 1187 2.4? 14 Problems with fiber breakage (poor) 1155 1.9 33 27
Ran very poor no sample taken
went back to original conditions
High fiber breakage
similat to 7275
New day
ANALYTICAL % Residual Lactide
Mz/Mw
Sample 015-62-01 015-62-02 015-62-03 015-62-04 015-62-05 015-62-06 015-62-07 015-62-08 015-62-09 015-65-10 015-65-11 015-65-12 015-65-15 015-67-01 015-67-02 015-67-03 015-67-04 015-69-01
3.4
bico bico purge purge 180.47
0.05 0.05 0.05 0.04 0.04 0.08 0.04 0.04 0.04 0.04 0.04 0.04 0.04 0.08 0.06 0.05 0.08 5.7
86774 86732 85783 87060 85050 80591 83715 84661 83696 85461 82387 84154 83518 77346 77098 83351 93754 3.34
168290 169150 166970 166754 165194 165124 166429 166598 165913 166746 164868 165847 165422 159246 158422 167526 192973 0.39
148842 153133 152197 151727 144086 150033 152024 155098 151320 150041 150594 148149 165422 159246 158422 167526 192973 13.5
1.94 1.95 1.95 1.92 1.94 2.05 1.99 1.97 1.98 1.95 2 1.97 1.98 2.06 2.05 2.01 2.06 1.6
258544 261495 257083 256026 254541 255402 259682 258222 257099 258047 258067 256318 255768 258118 253792 261358 315845 45.8
1.54 1.55 1.54 1.54 1.54 1.55 1.56 1.55 1.55 1.55 1.57 1.55 1.55 1.62 1.6 1.56 1.64 3.04
355534 362388 353352 352775 351601 351054 364709 358334 356307 358750 365810 354552 353850 385821 369522 366860 482782 1.83
67
Mz+1
PDI
Mw
%D
Mz
Mn
MP
DSC- 1st Upheat
DSC- 2nd Upheat
SHRINKAGE
% Crystallinity
% Crystallinity
% H2O Shrink
Tm
015-62-01 015-62-02 015-62-03 015-62-04 015-62-05 015-62-06 015-62-07 015-62-08 015-62-09 015-65-10 015-65-11 015-65-12 015-65-15 015-67-01 015-67-02 015-67-03 015-67-04 015-69-01
61.63 61.76 62.1 63.61 0.1
161.64 161.5 160.19 160.24 160.12 160.45 160.8 162.42 160.9 160.08 160.37 160.81 160.98 161.67 162.55 157.3 168.43 98.69
35.9 36.44 38.95 38.76 38.81 38.13 36.98 37.63 39.73 43.27 40.89 40.63 38.98 27.42 17.15 3.73 5.63
58.62 58.94 58.59 58.42 58.39 59.08 58.94 59.26 60.26 58.91 59.77 60.07 58.27 59.3 61.11 61.94
159.83 158.83 158.77 158.8 159.08 159.3 159.19 159.84 159.68 158.28 158.37 158.79 159.37 164.7 357.49 155.78 167.59
Tm
Tg
Tg
Sample
0.98 68.75 34.08 1.29 61.15 5.58 1.3 43.85 4.14 0.46 36.88 5.15 0.58 33.33 6.35 0.15 11.46 1.33 1.63 15.83 1.41 0 9.58 1.31 0 10.31 0.68 0.59 7.08 1.08 0.56 13.44 2.16 0.11 19.06 1.08 0 8.85 0.37 0 couldn't get off the roll 805.9j/g 84.79 1.74 1.73 3.86
MULTIFILAMENT TENACITY Ultimate Elongation Elongation at Peak
Fiber Tenacity
Fiber Modulus
Peak Load (g)
Load (cm)
Std Dev
Std Dev
Std Dev
Std Dev
1.77 1.5 1.45 1.28 1.05 0.95 1.8 1.89 1.64 2.28 1.99 1.18 2.44 1.39 1.12 0.14 0.12 0.26 0.13 0.08 0.14 0.14 0.25 0.18 0.12 0.31 0.22 0.05 0.01 0.05 Std Dev (g/den)
StdDev
015-62-01 015-62-02 015-62-03 015-62-04 015-62-05 015-62-06 015-62-07 015-62-08 015-62-09 015-65-10 015-65-11 015-65-12 015-65-15 015-67-01 015-67-02 015-67-03 015-67-04 015-69-01
2515.87 2140.07 2046.39 1855.14 1514.16 1368.13 2230 2380.21 1921.64 2764.41 2365.37 1365.49 2869.33 55.73 139.26
201.76 171.75 374.45 184.6 108.05 198.35 179.46 313.13 208.14 143.17 366.32 254.91 63.83 0.27 6.75
8.03 8.48 8.52 8.48 7.66 6.16 10.2 11.09 9.21 11.54 10.36 5.52 12.19 3.28 11.82
0.68 1.34 1.21 1.54 1.32 2.48 0.63 0.97 0.57 0.43 0.64 1.79 0.22 0.21 0.29
40.3 43.7 42.2 46.9 9.5 35.3 45.3 48.7 41.2 49 45.1 29.3 51.4 13.1 46.9
Sample
2.6 3.8 2.4 1.5 0.7 8.5 2.7 2 2.3 1.8 1.1 5.3 0.9 0.9 1.4
24.63 19.01 22.95 22.32 24.77 23.86 22.94 20.95 24.39 23.77 25.4 33.39 24.6 44.16 31.59
(g/den)
2.78 3.15 1.14 1.08 4.14 1.64 2.23 1.38 6.02 1.78 2.27 0.74 0.83 0.94 2.21
68
100C
SINGLE FILAMENT TENACITY Ultimate Elongation Elongation at Peak
FILAMENT PROP
Fiber Tenacity
Fiber Modulus
Peak Load (g)
Load (cm)
Std Dev
Std Dev
Std Dev
Std Dev
Std Dev
(g/den)
(g/den)
Denier
StdDev
015-62-01 68.01 12.03 4.47 1.44 015-62-02 58.5 5.11 3.37 0.31 015-62-03 69.34 9.59 3.63 0.27 015-62-04 59.48 10.9 4.09 0.53 015-62-05 55.27 12.42 4.34 0.26 015-62-06 61.1 10.04 4.47 0.65 015-62-07 55.57 11.81 4.56 0.64 015-62-08 53.56 4.02 4.47 0.31 015-62-09 50.9 7.82 4.13 0.42 015-65-10 54.21 3.87 4.65 0.26 015-65-11 54.23 10.76 3.99 0.25 015-65-12 47.08 8.14 3.37 0.59 015-65-15 50.56 2.81 4.58 0.24 015-67-01 unable to get one filament without breaking 015-67-02 3.93 0.27 0.7 0.69 015-67-03 015-67-04 015-69-01 180.47 5.7 3.34 0.39
44 33 36 40 43 44 45 44 41 46 39 33 45 42
Sample
Comment s
14.2 3.1 2.6 5.2 2.6 6.4 6.2 3.1 4.2 2.5 2.5 5.8 2.4 12.7
43.49 33.5 44.3 41.2 32.07 34.09 38.83 35.64 47.51 41.13 40.16 42.48 37.22 26.84
6.2 18 4 8 7.2 5.3 6.1 4.3 9.9 8 7.3 4 5.2 7.7
3.21 2.74 3.28 2.75 2.57 2.84 3 2.85 2.92 3.1 3 2.73 2.88 1.14
0.57 0.24 0.45 0.5 0.58 0.47 0.64 0.21 0.45 0.22 0.21 0.47 0.16 0.08
getting low 25 wraps at 25 wraps at lurol 7275 lurol NF-60 Lurol PP-81 lurol PP-37 lurol 7275 trilobal S/S trilobal S/S purge purge # sample 15-67-2
14
1.6
45.8
1.83
0.1
Boiling Water Shrinkage After Length After Length After Length After Length After Length Avg Shrink 84.37 61.15 43.85 36.88 33.33 11.46 15.83 9.58 10.31 7.08 13.44 19.06 8.85 84.79 Sample# %Shrink %Shrink %Shrink %Shrink %Shrink 83.33 60.94 38.54 34.38 25.52 13.54 14.06 11.46 9.90 6.25 11.46 18.23 8.85 87.50
015-62-01 015-62-02 015-62-03 015-62-04 015-62-05 015-62-06 015-62-07 015-62-08 015-62-09 015-65-10 015-65-11 015-65-12 015-65-15 015-67-01 015-67-02 015-67-03 015-67-04
1.75 5.81 6.31 8.13 7.88 10.69 10.00 10.88 10.69 11.19 10.56 9.50 10.94 2.00
85.42 51.56 47.40 32.29 34.38 10.94 16.67 9.38 10.94 6.77 11.98 20.83 8.85 83.33
1.69 4.31 6.63 6.56 7.25 10.75 9.88 10.88 10.88 11.13 10.00 9.81 11.00 2.00
85.92 64.06 44.79 45.31 39.58 10.42 17.71 9.38 9.38 7.29 16.67 18.23 8.33 83.33
1.94 4.19 7.13 7.88 8.63 10.75 10.19 10.81 10.75 11.25 10.25 9.75 10.94 1.88
83.85 65.10 40.63 34.38 28.13 10.42 15.10 9.90 10.42 6.25 14.58 18.75 8.85 84.38
2.00 4.31 6.25 7.44 7.31 10.56 10.13 11.06 10.69 10.94 10.50 9.69 10.88 1.75
83.33 64.06 47.92 38.02 39.06 11.98 15.63 7.81 10.94 8.85 12.50 19.27 9.38 85.42
2.00 4.69 7.38 7.88 8.94 10.38 10.31 10.63 10.81 11.25 10.63 9.81 10.94 1.50
getting low shrink 25 wraps at 133C ro 25 wraps at 130 C 25 wraps at 135C lurol 7275 lurol NF-6004 Lurol PP-8102GL-20 lurol PP-3772-20 lurol 7275 trilobal S/S 1.5/3.4 %D spun at 3200 m 1.74 trilobal S/S 1.5/3.4 %D spun at 2000 m purge purge
1.21 5.58 4.14 5.15 6.35 1.33 1.41 1.31 0.68 1.08 2.16 1.08 0.37
69
9.7 Comparison of Bicomponent Properties

BiComponent Fiber Property Comparison
Polymer Reference (for non CoPET (Sheath/Core) 110C / 260C 4.3 CoPET (Sheath/Core) 175C / 260C 4.75 PLA / PLA (Sheath/Core) PLA / PLA (Sheath/Core) PLA / PET (Sheath/Core) 1.4% D / PET 5.24 35.10% PLA / PET (Sheath/Core) 7.5% D / PET 5.51 36.40% PLA / PET (Sheath/Core) 5.2% D / PET 5.75 34.60%
Properties PLA Properties) strength-tenacity Wellman (g/den) Elongation @ Break Wellman (%) Specific Gravity Tm - melting point (C) softening sticking point (C) Tg (C) Wellman
5.2%D / 1.4% D 10.5% / 1.4% 3.92 3.98
60% 60% 31.20% 26.00% marginally lower marginally lower than PET than PET 1.25-1.28 1.25-1.28
Wellman Wellman Wellman
110 70 67
175 151.6 / 167.58
133.19 / 167.55
173.13 / 254.73
151.43 / 256.29
153.58 / 257.26
67
69.93 62.26 / 71.92 34.69 30.68 PLA=25.8 PLA=14.63 PLA=15.61
%Crystallinity (DSC) Wellman
no greater than 0 PET
Notes: Base Properties for sheath and core Bicomponent material, 50/50 A/B structure, 4-6 dpf.
70
9.8 Typical Staple Fiber Spinning System6
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9.9 Typical PET Drawline Recommended for PLA Bicomponent Processing5
Index for Drawing Equipment

ID I L M N O P Q Description Can Creel Tow reed Tension stand Pre dip bath Heated draw stand Hot air, steam or immersion bath Heatsetting calendar ID R S S2 T U V W Description Cold draw stand Finish applicator Dancer Rolls Ply bars Steam chest Crimper Dryer ID W1 W2 X Y Y2 Z Description Tow distribution system Tow take off system Cutter Staple transport system Condenser Baler
73

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PLA Processing Guide for Bicomponent Staple Fibers

1.0 Safety and Handling Precautions

2.0 Pellet Storage and Blending Recommendation

3.0 Resin Properties

NatureWorks LLC Confidential

Table of Resin Grades

Peak Fiber Crystalline MT vs. %D

140.0 Peak Crystalline Melt Temp (oC)

MT = -4.366%D + 174.78 R2 = 0.9758

Relationship of Melt Tempature to %D

NatureWorks LLC Confidential

Typical PLA Resin Properties

P L A M elt D en sity C u rve

NatureWorks LLC Confidential

Sh ear Vis co sit y, Pa. 100 s

10 10 100 1000 Shear Rate, /sec. 10000 100000

Capillary Rheology, performed at 230oC

4.0 Materials of Construction

NatureWorks LLC Confidential

Typical PLA Raw Material Drying Conditions

6.0 Melt Spinning

Following PET, Nylon, or HDPE in your systems

NatureWorks LLC Confidential

Melt Temperature Setting (oC) High Melting PLA Components

Melt Temperature Setting (oC) Low Melting PLA Components

Feed throat Zone 1 Zone 2 Zone 3 Melt pump Spin head

Typical PLA Extrusion Conditions

NatureWorks LLC Confidential

6.5 Heating Systems

NatureWorks LLC Confidential

Spacer or Shroud Length (mm)

7.1 Creeling and pre-tensioning

NatureWorks LLC Confidential

7.2 Pre Draw Bath

7.4 Finish application

NatureWorks LLC Confidential

Process location Entering Crimper In the Crimper

Typical Temperatures o o F C 70-90 21 - 32 70-90 21 - 32

Typical Tow Temperatures in crimping

Typical mechanical pressures in crimping 7.6 Heatsetting

NatureWorks LLC Confidential

7.9 Fiber Storage

8.0 Fiber Properties

* Note: Air temperature of 110C for 10 minutes

NatureWorks is a registered trademark of NatureWorks LLC

NatureWorks LLC Confidential

9.1 Investigation of Bondability through bicomponent fibers with various D levels

NatureWorks LLC Confidential

389-2 386-1 372-3 416-2 418-2 423-3

NatureWorks LLC Confidential

64.65 60.80 60.88 59.61 57.89 54.53 57.28 55.18

127.6 129.19 103.73 105.45

137.76 137.05 120.17 120.15

389-2 386-1 372-3 416-2 418-2 423-3

389-2 386-1 372-3 416-2 418-2 423-3

NatureWorks LLC Confidential

Lot # Width 389-2 386-1 372-3 416-2 418-2 423-3