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Gel Formation in HDPE

Gel Formation in HDPE

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Published by Subhasish Mitra
This report focuses on various reasons behind ubiquitous problem of gel or fish eye formation in the pelletization section of low pressure HDPE slurry process.
This report focuses on various reasons behind ubiquitous problem of gel or fish eye formation in the pelletization section of low pressure HDPE slurry process.

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Published by: Subhasish Mitra on May 27, 2010
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01/07/2013

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Gel Formation in Low Pressure Slurry Process of HighDensity Polyethylene
Subhasish MitraManager (Process), HDPE plantReliance Industries Ltd, Gujarat, IndiaIntroduction:
Gel formation on the all types of polyethylene (PE) film i.e. HDPE, LDPEand LLDPE is reported to be a muchcommon phenomenon and experiencedalmost everywhere. The problem islearnt owing to various operationalfeatures of the concerned process. Originas well as probable measures toovercome this particular problem isdiscussed in this note based on theexperience in
 Low Pressure SlurryProcess of High Density Polyethylene
 (
 Licensor: M/s Basell Polyolefins,Germany
) engaged in production of blow molding grade, pipe grade and filmgrade product.
Brief description of Bassel Polyolefins- HDPE process:
Slurry process
(Fig1)
utilizes continuousstirred-tank reactors (CSTRs), themonomers, chain-transfer agent, solvent,and catalyst species enter the reactors forpolymerization. The vaporization of thesolvent removes a large portion of thehighly exothermic heat of polymerization. The resulting slurryundergoes separation, removingunreacted
 
monomer, solvent, andoligomeric species from the polymer.Solvent is separated from the oligomerand recycled to the reactor inlets, and theoligomer is processed and packaged.Meanwhile, the polymer undergoesmixing, pelletization, and packaging.
Gel formation:
Generically all types of polyethylene(PE) process has two distinguishedsections i.e.
Powder production(Polymer production)
and
Powder  processing (Additive dosing and  Extrusion)
and problem of gelsformation can be attributed to theoperating conditions in both sections.Polyethylene is very reactive beforestabilization. In presence of radical,Polyethylene generates macro-radicalshaving tendency to recombine generally- but not always - to branching and evengelling. With the influence of heat,shear, oxygen or light, the polymerbackbone can react via free radicalsreactions. These reactions are verycomplex and can lead to numerousspecies depending on the nature of theradicals and the polymer structure. Infilm extrusion, where optical propertiesare important, this phenomena is called"fish eyes" or unmelts.Gel particles in PE product may resultfrom several sources.
 
Unmelted particles that resultedfrom insufficient melting andmixing, such as undispersedadditives
 
 
Gels generated during extrusion,such as cross-linked particles
 
Recycled plastics
 
Carbonized resin on screw rootof extruder
 
Extruder-die foulingGels or unmelted particles may originatein the resin, due to the plasticizationtechnology and quality control. The gelsmay be in form of extremely highmolecular weight polymer chainsaggregated dispersed in the regularpolymeric matrix, or different grades ortypes of plastic (in recycling case andwide spec. resin) in a major plastic. Sucha system can be viewed as a smallpercentage of high molecular weightpolymers blended in a low molecularweight matrix, or a blend of twodifferent plastics.Origination of gels in polymerproduction section may be significant if the reactor is used for different grades of product and comparatively highermolecular weight polymer of previousrun mixes with lower molecular weight
Fig1. Block diagram of low pressureslurry HDPE process
polymer of next run as there is no scopefor reactor cleaning in between.Maintaining operating conditions of polymer reactor play a very crucial roleto prevent gel formation. Generically,reactor temperature, hydrogen flow andco monomer flow are the criticalparameters that govern the MFI of product. If MFI goes low than specifiedlimit due to fluctuation in theseoperating parameters, then highermolecular weight polymer may formwhich may not melt at extruder andappear as gels.In Powder Processing section, gelsformation is reported to occur due tooxidation and thermal deterioration of PE powder. When PE powder getsoxidized or thermally deteriorated,cross-linking takes place in between PEmolecules, which makes the resultantproduct very hard. This hard degradedoxidized polymer, which does not meltin extruder, comes out as “Gels”.Oxidation of PE powder may take placedue to ingression of air in powderstorage and subsequent processingsections or exposure to humidenvironment if adequate Nitrogenblanketing is not maintained. In thecontext of LDPE synthesis under two-phase conditions, the process has beenreported to be sensitive to gel formation,and this can be more easily seen whenthe melt index is low. Gel formation isalso found to increase with increasingmelt temperature and increasing mixingtime. The effect of mixing efficiency isminor. When the polymer containedBHT (Butylated Hydroxy Toluene -- antioxidant agent) there is a decrease in gelcontent. Based on the similar kind of experience in the above-mentionedHDPE process the following suggestionsmay be considered to avoid the problemof gel formation.
 
1.
 
Stable operating conditions inreactor are required to bemaintained ensuring no excessdosing of initiator in reactor.2.
 
Adequate nitrogen blanketing i.e.positive nitrogen pressure inpolyethylene powder storage andsubsequent processing units is tobe ensured. On line Oxygenanalyzer should be accurateenough to indicate the oxygenvolume%. If oxygen content inthe system (should be in theorder of 10 – 50 ppm) increasesthen nitrogen pressure in therespective system is to beincreased as well.3.
 
Non-exposure of PE powder todirect sunlight is to be ensured.4.
 
Proper dosing and mixing of master batch with PE powder isto be ensured if gel count is morethan usual.5.
 
If gels keep on coming in filmsample then Extruder barreltemperature controller’s setpoints may be increased by fewdegrees to ensure sufficienttemperature for melting alongwith reduction in Extruderthrottle valve opening to ensuremore residence time inside forbetter homogeneity.6.
 
During processing, deposits of low molecular weight polymer,additives and degradationproducts can build up on the dieand extruder surfaces. Suchdeposits when released can makedefects on the extrudate. Acommercially available processaid is able to reduce die build upbecause as the coating layerdevelops any degraded materialclinging to the die is displacedand also stagnation in theextrusion process is minimizedreducing the production of thermal degradation products.The low energy surface providedby the coating reduces internalbuild up and subsequentdegradation leading to cross-linked and oxidized gels.Reducing unmelted/unmixed gelseffects the prevention of solidbed break-up and the process aidmay prevent premature meltingin the feed section thus helping tomaintain a coherent solid bed.7.
 
Die plate temperature is to bemaintained to avoid over heatingof polymer.8.
 
Periodical cleaning/purging of extruder die plate holes may beplanned after planned shutdownto remove degraded polymers.9.
 
Fluoropolymer process aids havebeen widely reported to be quiteuseful to improve theprocessability of various types of polymers in a great range of extrusion processes. These aidscontribute to improve extrusionmelt stability, reduce meltfracture, increase extrusionthroughput, reduce die swell, ordie build-up. This process aidconcentrate is particularlyeffective in polymer systemscontaining silica & talcantiblocks, pigments and otheradditives. When used in LLDPE& HDPE films, it is reported

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