Product Application & Research Centre Mumbai

FIBRES AND FILAMENTS

Introduction Polypropylene (PP) is a popular material for fibre manufacture due to its properties like low density, easy processability, excellent orientation characteristics, superior tensile properties, good chemical resistance, hydrophobicity and resistance to micro-organisms. These properties have resulted in use of PP fibre in carpets, rugs, apparel, home furnishings, geotextiles, strappings, personal hygiene products, medical drapes and various other applications. Polypropylene filaments are produced by extrusion spinning process. Usually the product obtained from the spinning process is not directly suitable for commercial use. The post spinning operations involved are stretching and/or texturising and crimping. In stretching process, the spun filaments are stretched or drawn to several times its original length to increase molecular orientation and thus the tensile strength. These filaments may then be subjected to further operations, according to the final usage. Thermal setting and thermal relaxation processes provide dimensional stability; twisting and interlacing or intermingling provide interfilament cohesion; texturising and crimping provides a voluminuos yarn and cutting of continuous filaments into small pieces provide staple fibres.

Melt Spinning Process The principle method of manufacturing PP fibres is melt spinning. The melt spinning process is shown schematically in Fig 1. In this process, the polymer alongwith stabilizers, rheological modifiers or colourants is fed into an extruder through a hopper. The extruder is usually of single screw type. The molten polymer existing from the extruder is distributed through a manifold to various spinning positions under constant pressure. The design of manifold system must avoid dead spaces as well as provide equal residence time for the melt to reach at each spinning position. A spinning position usually consist of a melt pump eg. gear pump, a filter pack and set of spinnerets. A gear pump feeds metered quantity of melt to the filter pack. The polymer melt is then forced through a fine filtering assembly consisting of sand particles of 20-80 m size, a series of stainless steel wire gauges of different mesh sizes and a distributor plate. Filtration of the molten polymer before it enters the spinneret capillaries, homogenizes the melt and removes gels, and also eliminate gaseous bubbles. Efficient filtration brings down the breakage rate to almost below six breaks per 1000 kg filament production and also reduces the frequency of thick and thin places in the spun filaments. After filtration, the melt forced through spinneret capillaries. Spinnerets are metal plates containing holes. Each spinneret contains few to thousands of holes depending on the process or product type. It ranges from few for monofilaments, upto thirty to ninety for filament yarn and a few thousands for production of staple fibres. The capillary dia of holes usually ranges from 0.2 - 0.3 mm and their length ranges from 1 to 3 times the diameter. The cross-

section of spinneret capillary may be round, trilobal or of the shape that needs to be imparted to the filaments.

Fig 1. Schematic diagram of melt spinning process

The molten polymer filaments coming out of the spinneret in the form of fine stream of fluid are cooled by quench air to solidify over the first 80-100 centimeters of its length while being drawn off by the take-up device from the bottom of the spin line. The cooling of molten filaments is performed using purified chilled air at around 8-14 C and an air velocity of 0.6-0.8 m/sec. The filaments are then made to converge into a bundle with the help of ceramic guides. A spin finish is applied before the bundles are wound up on a package tube roll, which is often friction driven by a roller. Generally the yarn passes through two godets before reaching the package winder. In order to lay the filaments satisfactorily around the package, it is grasped by the forked thread guide and moved equally to the edges of the package by a traverse guide. F&F Spinning Equipments Used in India

Neumag, Germany Extrusion Systems Ltd., UK Plasticizers Engg, UK Toray Engg, Japan Fare, Italy Mackey, US Reifenhauser, Germany Starlinger, Austria Bukwang, Korea Tae Sung, Korea Dong Kwang, Korea

Resin Selection For polymer to perform well in filament spinning process, it has to meet certain basic requirements. These are :

Capability of being produced easily into fine filaments Good processing stability and melt strength to eliminate melt flow breaks and thus deteriorating physical properties of filaments Polymer cleanliness (very low filter index) to eliminate filter pack blockage Narrow molecular weight distribution resin ( olydispersity between 4-7) to ensure p consistent melt flow characteristics The capability of orient readily to eliminate filament breakages during post spinning operations Good end use properties, ie. dimensional stability, UV radiation and colour stability, gas fading stability, particularly for outdoor use products

Repol and competitor's grades for fibres and filaments Property Repol H200FG 20 3.0-3.2 34 11 1500 27 Montell VS6500H (A) 20 5.0 30 12 1400 29 Borealis HF435F (B) 20 4.7 33 11 1500 38 Repol H350FG 35 3.0-3.2 34 10 1600 22 Montell XS6500H (C) 40 5.0 32 10 1450 24 Solvay EltexP FHY681 (D) 35 4.2 32 10 1500 28

MFI (g/10min) Xylene solubles (%) Tensile yield strength (MPa) Elongation at yield (%) Flexural modulus (MPa) Izod impact (J/m)

Effect of Resin Variables on Fibre Properties There are mainly four resin variables that can significantly affect the properties of PP fibres 1. Molecular weight and molecular weight distribution 2. Additives 3. Catalyst Molecular weight and molecular weight distribution Molecular weight (MW) and molecular weight distribution (MWD) are important and can have a significant effect on processing in the melt and solid state and on the tensile properties of the fibre. The polydispersity (mol. wt. distribution index) of commercially available polymer ranges from 2 to 12. The narrower the molecular weight distribution, the easier the control of spinning; a molecular weight distribution of around 3-5 is considered ideal for high speed spinning. In general, changes in molecular weight have the following effects :

The degree of crystallinity in fibre increases as molecular weight decreases The nucleation rate increases as the molecular weight decreases The crystallisation rate increases with increase in polydispersity Optimum spinning temperature increases with increase in molecular weight and with the breadth of the molecular weight distribution. However, the effect of molecular weight distribution is less Broad molecular weight distribution demonstrates higher draw resonance and poor spinnability Polypropylene with a narrow molecular weight distribution shows higher birefringence (molecular orientation index) at higher spinning speeds, and consequently higher tenacity and lower elongation

The trend on influence of polymer characteristics on spinning parameters and mechanical properties of PP fibres are given in Table 1.

Influence of polymer characteristics on spinning parameters and properties of PP fibres Property Resins with same shape MWD. Trend as MW increases Increases Increases Decreases Decreases Increases Decreases Increases Decreases Decreases Decreases Increases Resin with same MW. Trend as MWD narrows Decreases Increases * Decreases --Increases Decreases Increases Decreases Increases Increases

Maximum obtainable draw ratio Maximum obtainable melt draw down * Draw resonance Ease of orientation Extrudability at the spinnerette Fibre strength Elongation at a given draw ratio Tenacity at a given draw ratio Modulus at a given draw ratio Orientation at a given draw ratio Processing speed

* It should be noted that in fibre spinning, elongational viscosity is more important than shear viscosity. Narrow MWD polymers show less shear thinning and therefore elongational viscosity increases at higher extrusion rates, leading to higher melt orientation. This results in higher orientation in the spun fibre leading to higher tenacity and lower extensibility. Whereas, broad MWD polypropylene tends to be more shear thinning. Therefore, necking can result and ultimately melt fracture occurs at high spinning speeds. The fibre is less oriented and shows higher elongation. Additives Additives are incorporated in PP, both to ease processing as well as to impart certain desired properties in the fibre with respect to end product. The types and amount of additives used determine how well the resin processes. If the additive level is insufficient, it can lead to melt flow break during extrusion, leading to deterioration in physical properties of the final product. Inappropriate addition of additives can lead to problems like yellowing, gas fading and pinking.

Catalyst The type of catalyst used during PP manufacturing process has a direct bearing on the resin characteristics. It affects the xylene soluble level, the molecular weight distribution and the level and type of catalyst residues. Catalyst residues can affect the colour of the resin and also have an effect on the final textile produced. The effect of oligomer level (xylene solubles) is reflected during processing as smoke or residue build up. It is also believed that a certain amount of oligomers content is beneficial during processing but their effect on textile properties is not fully understood. Other minor resin variables which affect either processing or final product properties are gels, filterability, pellet size and shape, pigmentation / masterbatches Effects of Processing Variables on Fibre Properties Besides the effect of resin properties, processing conditions like temperature and spinning speed also affect fibre properties. Some of the important processing variables are discussed below Throughput rate Throughput has a direct bearing on the phenomenon of melt fracture. The shear rate (or shear stress) that a polymer melt experiences during processing is determined by the throughput. Beyond a certain critical value of shear rate, the diameter of the extrudate varies considerably. This phenomenon is called melt fracture. Melt fracture is a die phenomenon and cannot be eliminated by decreasing spinning speed. It can be eliminated either by decreasing the throughput or by increasing the melt temperature. There is also a relationship between the throughput and spinning speed which can be explained as under. In the absence of a take-up force and for a given throughput, the melt exhibits swell as it exits the die. Polymer molecules are randomly coiled. When they traverse through the die, they are stretched and oriented which impart them with some energy. As the polymer molecules exit the die, this stored energy is released and manifests as die swell, where the diameter of the extrudate is larger than the diameter of the die exit. When throughput increases, die swell increases. Therefore, the polymer molecules require a longer process time to achieve a similar state of order as the molecules at a lower throughput. The relationship between throughput and take-up speed is illustrated in Figure 2.

For combinations of operating conditions of throughput and take-up speed below the curve in Figure 2, continuous fibre spinning will occur and for combinations above the curve, continuous spinning will not occur. Either the fibre will fail due to melt fracture or the take-up force will be higher than the capabilities of the fibre resulting in fibre breakage. It can therefore be said that for the fibre spinning the maximum spinning speed decreases with increasing throughput. Spinning speed Spinning speed affects the drawdown ratio. Drawdown ratio is the ratio of the fibre velocity at the take-up rolls to that at the die exit. Drawdown ratio is an expression of deformation that the melt undergoes before being taken up on cold rolls. For a given throughput, the drawdown ratio increases with increasing spinning speed.

Draw ratio Draw ratio is an expression of the amount of deformation a fibre undergoes in the solid state. It is expressed as the ratio of the speed of the draw rolls to the speed of the feed rolls. Orientation of the molecules occurs in both the melt and solid state processes. Draw ratio determines the solid state orientation. As draw ratio increases, tenacity increases and percent elongation decreases. Increasing the draw ratio increases the orientation of the chains and decreases the amount of unoriented amorphous material. The effect of draw ratio on the physical properties of the fibre are shown in Figure 3.

Percent relaxation It is defined as the ratio of the difference in the draw and relax roll speeds to the draw roll speed. This affects the residual shrinkage of a textile and decreases percent elongation. Relaxation is equivalent to an annealing process where the chains are allowed to form more perfect crystalline arrangements that are thermodynamically stable

Temperature Extrusion temperature, drying air temperature, draw temperature and relaxation temperature are all important parameters that eventually determine the physical properties of the fibre. The extrusion temperature affects the rheological behaviour of the melt and throughput. Temperature of the air for cooling determines the crystalline arrangements and the morphology of the fibre which ultimately affect the properties of the fibre. The

draw or orientation temperature and relaxation temperature decide the extent of orientation of the chains in the fibre axis direction and hence have a bearing on physical properties like tensile strength of the fibre. Generally the tenacity increases with increasing orientation. Colouration of Polypropylene Filaments Coloured PP filaments constitutes more than 55% share of the total PP fibre and filament production of India. The coloured PP filaments are usually made by mass colouration or pigmentation. The process involves intermixing of colourants with the polymer prior to extrusion. In order for the pigmentation of polypropylene to be successful, several important criteria have to be met. 1. 2. The pigment must be stable to the extrusion process The pigment must be dispersed evenly in the melt

The pigments differ in their ease of dispersion. Pigments such as titanium dioxide and cadmium or chrome pigments normally are among the easiest to disperse. Others, such as carbon black and iron oxides are the most difficult. Hydrophilic pigments aggregate severely whereas organophilic pigments have less tendency towards aggregation. Problems in Filament Spinning and Possible Causes 1. Non-uniformity of the spun filaments (i) Heterogenity of spinning fluid (polymer melt) (ii) High melt temperature than suitable for spinning (iii) Throughput variation (iv) Dirty and choked spinnerette capillaries (v) Variation in quench air velocity (vi) Variation in godet / take-up winder speeds (vii) Non-uniform dispersion of colourants in the melt Low tensile strength of spun filaments (i) Throughput variation (ii) Heterogenity of polymer melt (iii) Lower melt viscosity due to high MFI polymer (iv) High quench air velocity (v) Very low quench air temperature (vi) Low take-up velocity Low elongation in spun filaments (i) Heterogenity of polymer melt (ii) Lower melt temperature (iii) Low quench air velocity (iv) Higher quench air temperature (v) Higher take-up velocity

2.

3.

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Testing of Fibres, Filaments and Fabrics Depending on the end use, there is a whole range of properties that needs to be tested. A comprehensive list of tests for fibre and fabric is given below which applies for both wovens and non wovens. Physical Tensile Strength Elongation Burst strength Tear strength Seam strength Surface friction Air permeability Fluid porosity Water repellency Density Absorbency Sewability Weight / Mass Chemical Resistance to organics Resistance to inorganics UV resistance Thermal behaviour Flammability Durability Washability Hydrophobic / Philic nature Liquid repellency Sterilizability Biodegradability Static generation Aesthetics Soft/Stiff feel Odour Smooth/Coarse Colour Texture Fluffy/Hard nature Bouncy Reversible Textile/Papery appearance

Applications of Polypropylene Fibre and Filaments Fibre Type 1-4 Denier End Uses Filter and other industrial fabric. Non wovens fabrics for hygiene, medical nonwoven geotextiles Backing for pile fabric in carpets carpet pile Upholstery fabric Characteristics Excellent chemical resistance and strength, long life, lightest fibre Coverage Dimensional stability on washing strength Absorption resistance Excellent soil resistance Excellent ease of cleaning Excellent colour fastness Low specific gravity High bulk excellent thermal insulations. Dimensional stability on washing soft handle Excellent thermal insulations. High bulk resilience low moisture absorption

5-8 Denier

Blankets

Fibre fill and pile lining

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Fibre Type 15 Denier

End Uses Tufted and woven carpets Artificial grass

Non-woven fabrics Geotextiles Medical fabrics

Characteristics Excellent soil resistance Excellent ease of cleaning Low static build up Wear resistance pile Height retention Strength wear resistance Stain resistance coverage Long life

B - Filament Yarn Fibre Type 15 Denier 30-420 Denier End Uses Women's hosiery Knit wear Characteristics Snag resistance excellent feel. Easy care Dimensional stability on washing high bulk soft handle. Can be blended with rayon, cotton or wool Strength abrasion resistance coverage Coverage strength wear resistance Good abrasion resistance. Low moisture absorptions Easy drying characteristics Light weight Chemical resistance, abrasion resistance, dimensional stability High strength wet or dry light enough to float, lightest fibre. Low moisture pick up Highest resistance to weathering, microorganism etc. Dimensional stability on washing strength

Car Upholstery Socks, underwear and outerwear PP/Cotton & PP/Rayon Blend Fabrics

420-840 Denier

Laundry bags

Twines, ropes, cordage, fishnets, cargo handling, nets, straps for bags and ribbons

Backing for pile fabrics

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Fibre Type 840-3200 Denier

End Uses Tufted carpets

Carpet backing

Bag sewing thread

Window channel fabrics Woven geotextiles

Characteristics Coverage, wear resistance, pile height retention, excellent soil resistance, excellent ease of cleaning Excellent colour fastness with pigments. Strength Dimensional stability High covering fabric Rot and mildew resistance Strength high yield Chemical resistance Low moisture pick up Long wear high bulk Low moisture pick up High strength, excellent resistance to bacterial attack

Type of Yarn and Denier Range Produced in India # 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 Denier 65/24 65/24/2 90/24 90/24/2 150/40 210/40 210/80 300/70 420/70 840/80 840/140 400, 900, 1600, 2300 900/90 840/120 1260/120 1800/240 2600/240 Type Single crimped Crimped double twisted Single crimped Crimped double twisted Flat / twisted Flat / twisted Flat / twisted Fully drawn yarn Fully drawn yarn Flat / twisted Flat / twisted Air textured Flat / twisted Flat / twisted Flat / twisted Textured Textured

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