PET Processing V4 - 2
PET Processing V4 - 2
Annexure I
Tm
Tg
The chart typically shows the thermal conditions undergone by the PET pellet before getting converted into the final bottle. Drying in Hopper: The pellets are heated to around 165 deg. C in the dryer, during the process of moisture removal. Plasticization: During this process the material undergoes the phase transformation from solid phase to liquid phase. The heat of fusion (58 J/g) is supplied to the polymer and plasticized into a homogeneous melt.
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IV of Preform / Bottle
The IV of the preform depends on various factors; 1. 2. 3. 4. IV of the resin. Efficiency of the Dryer. Residual moisture content of the resin, on entry to the extruder. Plasticizing conditions. a. Back pressure b. Screw speed c. Barrel temperature. d. Screw design 5. Melt residence conditions. a. Machine throughput utilized. b. Machine shot weight utilized. c. Barrel / Shooting pot cushion. d. Cycle time for the preform. e. Screw idle time. Thus the IV of the preform in simple sense will be
No. 1 2 3 4
Machine Type Single stage systems Two stage No Robot Two Stage Lower end systems Two stage Husky, Krauss Maffei, Nestal
(The curve is typical for PET preforms at 100 degC) The curve turns upward into region C, the strain-hardening region, where strain-induced crystallization takes place, and the highest tensile properties are achieved. The onset of strain hardening is in the transition region between regions B and C. According to a strict definition, the onset of strain-hardening is determined as follows: extend lines from regions B and C until it intersect; bisect the angle adjacent to the stress/strain curve; and extend that bisecting line to intersect the curve. The point at which that line and the curve intersect is the onset of strain hardening. (Refer Fig)
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Experience supports the need for a minimum of four effective flights in the feed section to avoid non-uniform feed and/or unwanted temperature rise in the rear zone. Hence the length of feed zone will be (4 D + maximum shot length of screw). Where, D is diameter of screw, which is equal to pitch. Typically flight depth is 12.50 to 18.75 mm for 112 mm extruder. A4.1.2: Transition (Compression) Section The transition (compression) section of full-flighted screws is designed to promote both the compression and heating of the plastic granules. This is achieved by a uniformly tapered, increasing root diameter that reduces the available volume between flights, compressing the granules. As granules are compressed, air is purged back through hopper. Material when compressed and moved forward, it is also heated, partly by conduction, but mainly by friction from rotary shear, it melts. Some screw designs achieve transition within a single flight. A transition section that is too short can promote overheating. Normally, the transition section is from one-fourth to one-third the entire screw length for PET. A4.1.3: Metering Section The metering section provides polymer melt stability and helps ensure a uniform delivery rate. Flight depth is at a minimum and is normally constant along the section length. The range for metering section 112 mm extruders is between 3.00 and 5.00 mm in depth, and five to twelve flights in length. On smaller 63 mm extruders, flight depth varies between 2.00 and 3.00 mm, and length runs from five to ten flights. Shallow screws have a short metering length to avoid undue compression and consequent high polymer temperatures. Deep screws have a longer metering length to provide added flow stability. Invariable low shear screws have barrier flights or a mixer added in the metering zone with a shorter length than normal. The mixer does the function of homogeneous melt, and the shorter metering zone reduces the effective shear on the melt. A4.1.4: Single-Stage Screw, Compression Ratio Screws are frequently referred to by their compression ratio. This factor is calculated from the relative volumes per flight of one revolution in the feed and metering. In practice, compression ratio is often considered to be the ratio between the relative flight depth in the feed and metering sections. A4.2: Two-Stage Screw The two-stage screws used in vented extruders can be considered as two separate screws in tandem as shown below. The first stage ordinarily comprises about 60 percent of the overall length, or about 17 flights in a 32:1 L/D ratio. The second stage is somewhat shorter, about 15 flights.
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Both stages are further subdivided into separate feed, transition (compression) and metering sections of varying length. For 112 mm diameter screws, flight depths in the feed sections range between 14.0 to 19 mm, with a greater depth in the second stage to provide a decompression zone at the vent. Metering section depths range between 3.80 to 6.40mm, with a greater depth in the second stage to ensure forward polymer flow and eliminate vent flooding. A4.3: Pump Ratio Pump ratio is the ratio of the flight depth in the second-stage metering section compared with the flight depth of the first-stage metering section. A factor greater than 1 is necessary to avoid having polymer flow out the vent. For Pump ratios of 1.6 to 1.7 commonly provide good performance. A4.4: Screw Cooling Some improvement in extrusion of plastic polymers is possible by circulating cooling water through the cored section(s) of the screw typically the feed section. The amount of cooling required is dependent on screw design and operating parameters. Cooling is more critical for larger diameter screws, because the larger volume of polymer flow requires more cooling. Superior extrusion may be achieved by optimized cooling, but reduced rates or surging may result unless proper processing temperatures are maintained. If screw cooling is used, it should be limited to the feed (hopper) section. A4.5: Key advantage of two stage / Vented barrel screws: 1. Ability to use material with lower bulk density. Less than 0.8 g/cc, basically for material with flakes and regrinds dosage greater than 10%, and still offer consistent melt quality and charging. 2. Ability to process with higher moisture, as the excess can be released through the vent at the middle of the barrel. 3. Low shear during plasticizing, as melting and homogeneous melt is one in two stages. Thus lower chance of shear degradation.
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A5.1: Final container Design: The final container design is based on the product packed, its shelf life requirements, and its characteristics. The final package also takes into consideration the product presentation requirements such as the aesthetic of the final container. The basic fact that needs to be frozen at this stage is the neck finish details, wall thickness and the shape of the container, based on the requirements discussed above. From the dimensional details we can also calculate the weight of the container. A5.2: Process: The PET container can be made with two processes, single stage and the two-stage process. Each of the process have a specific characteristics, i.e. the stretch ratio of the Single stage is lower than the two stage, similarly, single stage has more flexibility in terms of oblong shaped bottles compared to two stage process. A5.3: Basic Preform design: Once the container design is frozen and the process of manufacture determined, we have adequate details to decide on basic preform design. From the container wall thickness and the stretch ratio, we can determine the dimension of the preform, such as length, diameter and thickness.
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From the graph we understand that the wall thickness of the preform needs to be more as the length of the preform increase, and vise versa. And the maximum wall thickness is determined by the limitation of material; basically the 2 % IPA grades in the market can retain good clarity, till a wall thickness of 4 mm, beyond which the cooling the preform is slow, which results in higher crystallinity in the preform, and thus a hazy appearance. Also with higher wall thickness the cycle time increase drastically and process becomes less productive, as the cooling time is proportional to the square of the wall thickness. A5.5: Mold and Ejection requirements: Based on the mold design requirements and the scope for future increase and decrease of the preform weight one of the following preform designs can be selected.
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A5.5.2: Internal taper: In this design the neck ring surface is straight from the neck-holding diameter and matches the cavity. The core pins have a converging taper, which converges just below the neck finish to the nominal internal diameter of the preform. These preform design are used in high wall thickness preforms with neck diameters less than 28 mm & Large size water preforms. The advantage of this preform design is that we can have weight reduction of preforms with change of core pins
A5.5.3: Dual taper: There two type of dual taper preforms; 1) Converging core and diverging Neck finish. 2) Converging core and converging neck finish.
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A5.5.5: Converging core & Converging Neck finish: This design is normally used for low wall thickness water preforms, basically of 28mm & 30/25 mm neck finish, where the neck finish diameters are considerably higher. These preform designs provide possibilities for weight reduction & increase.
A5.5.6: Internal step relief design: Internal step relief are provided in high wall thickness and very long preforms, with length more than 150 mm, the relief in the internal core diameter helps in easy ejection of preforms with less force. As longer preforms will require higher ejection force due to higher sliding force required during the ejection of the preform.
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In case of three station single stage machines, it is difficult to eject the preform with surface temperature of o around 100 C (blowing temperature), and hence the ejection temperature is always lower. Thus, if extreme Blow ratios of 12 ~ 14 is used in these machines, it will lead to pearlescence or bursting. Two stage (Typical Values) Axial Hoop Blow Ratio Gate wall thickness, as % of Preform wall thickness Lower limit 2.2 4.4 9.6 70 Upper Limit 2.8 5.4 15 80 Typical Values 2.5 4.8 12
A6.2: Base Design Base of a PET bottle has a critical function of maintaining the bottle upright, it also takes the entire load of the package with the product, takes care of the drop load, maintain the pack in good condition. There are different types of bottle bases depending on the end use applications; following are some of the bases used, with their field of application; Flat Base: For mineral water, oil and other non-pressure applications. Champagne Base: originally used for Carbonated Beverages (High Pressure) application, it is one of the heaviest bases in PET containers, and it has been slowly phased of CSD, now there are few companies using for their beer application. The base is expensive and difficult to control the process. Petaloid Base: This base has widely accepted in the high-pressure carbonated beverages applications, due to its stability and lower weight. There other variants with six legs and eight legs, but these do not have the wide acceptance. Hot fill base: The hot fill base is also one of the heavy bases in PET container, due to inherent strength required to withstand the higher temperature and force encountered during the filling of the container with hot juice. The rugged internal ribs also prevent the base from warping outward and create rocking during the ejection of bottle at higher temperatures from hot fill blowing machine.
There are many base designs used in PET packages but they widely fall under these categories, and the functional aspects.
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ASPET 22CJ
ASPET 22CJ is a special grade, with lower rate of crystallization, to suit slow cooling high wall thickness preforms, used in 20 lts water containers with typical wall thickness of 8 ~ 10 mm. ASPET 22CJ has higher co-polymer content to ensure higher transparency and strength. Resin IV is 0.88 dl/g +/- 0.02. Injection Molding Machine - Setting Parameter 1 Dryer settings Significance Typical Values Process Temperature For Hot air dryers: To remove moisture from resin, to enable plasticization with minimum IV 170 deg C for 5hrs drop. 165 deg C for > 5 hrs (Max. 7hrs) Temperature required for Barrel: 275 +/- 10 deg C plasticization of the polymer. Nozzle: Barrel plus 5 deg C Plasticizing Parameters The screw rotation does the function of Shall be operated at minimum, so that feeding the pellets, melting, plasticizing. the idle time is kept low. Screw Idle time is waiting time after plasticization of melt, before injection. Set pre-charging delay to keep screw idle time low, ~ 10 sec. The backpressure aids in uniform Typically 10 ~ 15 bar. plasticizing of melt. Volume of melt held in front of screw at 10 ~ 15 mm the end of Injection. Injection Parameters Melt pressure for injecting the melt 300 ~ 400 bar (Melt pressure) into cavity. Low due to large cross sectional area. Typical speed: 35% ~ 45% The time required for filling the cavity High due to higher section wall thickness, with melt. typically 15g/s ~ 18 g/s Melt Pressure & time required for High as melt is packed for longer length packing the melt in cavity, to and cross sectional area. compensate shrinkage during Typical values: 500 ~ 650 bar solidification. Typical values: 12 ~ 16 sec. The time required to cool the Typical values: 30 ~ 40 sec (for 8.5 mm preforms. wall thickness) Total time required to process on shot Typical values: 110 ~ 120 sec. of preform
4 5
Back pressure Extruder Cushion Injection Pressure & Velocity Injection time Hold pressure & time
7 8
9 10
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Coloring of PET
Coloring of PET has become a important of aspect in PET packaging, with better understanding of packaging needs of products, like improvement in shelf life of product packed, and retaining the freshness of product through out its shelf life. Colorants have moved from just coloring the plastics to give aesthetic appearance to more product relevant needs such as protecting the product from radiations which harm the product such as UV, fluorescent light etc., Colorants such as green and blue are used in light dosages for product identification better appearance in water and soft drinks industry. With the fast growth of PET in drugs packaging, colorants have started taking additional roles as masking for UV and fluorescent light radiations, which decompose the organic molecules present in the drugs and reduce their efficiency. Amber color is generally used for this purpose, as they mask the high-energy radiations. It also protects the product colors from becoming pale, as in case of fruit juices and colored drugs. Coloring of plastics can be done by five methods; 1. Liquid color dosing (liquid) 2. Dry color dosing (Powder) 3. Wax concentrate dosing (Granular) 4. Master batches dosing (Pellet) 5. Pre-colored resin Pellets (Pellets) Liquid color dosing (liquid): Liquid color for thermoplastics has become the coloring system of choice because it offers lower cost, easier handling and higher-quality results than any other coloring system available today. What is liquid color? Liquid color is a dispersion of pigments or dyes in specialized liquid vehicles, which are compatible with PET, polyolefin, styrene and engineering resin systems. High letdown ratios are achieved by loading up to 75 percent pigment (by weight) into the liquid vehicle. Pigment agglomerates are then mechanically broken down into individual particles, which are wet-out in the resin vehicle to prevent agglomeration, increasing the uniformity, opacity and intensity of the original pigment by 50 to 80 percent. This high concentration of color results in high letdown ratios: for opaque colors, normally one part color to 100 parts resin; for transparent colors, as little as one part colorant to 1,000 parts resin. Functional additives such as anti-static agents, slip aids, chemical blowing agents and UV stabilizers and absorbers may be incorporated into the colorant. Such multi-additive packages enable the plastics processor to monitor all additives by monitoring only the color. A precision metering pump is used to inject small amounts of concentrated liquid color directly into the plasticizing screw of injection molding machine during screw recovery cycle. The pump is equipped with a three- or six-roller peristaltic head which compresses the outside of a flexible feed tube, forcing liquid color through the tube, and is capable of metering as little as one gram of material per cycle of viscosities up to 20,000 CPS. Output of the pump can be adjusted in milligram increments, permitting fine-tuning of color levels with no interruption in processing. Because the colorant is metered into the processing machine mechanically, the system requires little supervision or labor skill to obtain consistent color. Page 63
Solid colorants are mixed in tumbler mixers, with the resin pellets in the required dosing ratio and the mix is charged into the machine. The feeding of the resin dry color mix should be by gravity hopper and it cannot be loaded using vacuum hopper loader, since the fine color powder will be separated by the vacuum loader in filters. Hence requires considerable manual handling of the resin. Advantages of dry color: 1. Available in large or small quantities. 2. Economical to buy. 3. Less storage space. Disadvantages of dry color: 1. Dust is a health, housekeeping and cross-contamination problem. 2. Poor reproducibility, especially for critical colors. 3. No adequate metering system is available. 4. Resin to be mixed in batches to distribute the pigment. 5. Color changeover and/or clean up is very difficult. By comparison, dry colorant cost is the least to color per Kg of resin, However, the overall cost of liquid color is lower, as economies are achieved in the form of lower housekeeping costs, less downtime, reduced waste, reduced labor and reduced rejects. Dry color is not used in PET as it requires drying of pellets for 5 ~ 8 hrs, hence considerable quantity of resin is stored in the hopper, which makes the color change over a cumbersome process. The fine dry color powder settles on the hopper inner sides and is difficult to clean.
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