01B EVAL - Technical - EN

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EVAL™ EVOH Resins and Monolayer Film

www.evalevoh.com
EVAL™, a unique
Kuraray technology
EVAL™ EVOH combines the excellent gas barrier properties and resistance to organic solvents
of polyvinyl-alcohol with the easy processing and water resistance of polyethylene. EVAL™ is
commercially available as granules for coextrusion and coinjection, or as monolayer film for
lamination. EVAL™ is a crystalline copolymer with the following molecular structure:

Ethylene and Vinyl ALcohol

(CH2-CH2)m (CH2-CH)n

OH

Characteristics

2
High gas barrier properties out, EVAL™ also effectively blocks odours, of ­automotive fuel systems. EVOH is the
Extended freshness, less waste protecting product integrity. EVAL™ locks only conventional plastic that meets
Without an effective gas barrier, oxygen volatile fragrance and ingredients inside strict ­international emission standards.
may penetrate packaging and spoil the packaging without absorbing them, and
contents. EVAL™ keeps oxygen out and preserves aroma until it can be enjoyed Solvent resistance
safeguards quality, extending shelf life and by the consumer. Safe protection against permeation of
avoiding waste. This cost-saving f­ unction solvents and agricultural chemicals
is commonly added to food, medical, Transparency EVAL™ shows excellent physical resis-
pharmaceutical, cosmetic, agricultural A clear and reliable alternative to tance to solvents, and barrier against
and industrial packaging applications. aluminium foil their ­permeation into the environment.
All-plastic EVAL™ barrier layers have Because of its resistance to absorption
Migration barrier ­excellent flex crack and pinhole resis- and ­swelling, EVAL™ is typically used as
Improving food safety tance, even when flexed, folded and shak- the inner contact layer in UN-approved
EVAL™ provides excellent functional ­barrier en during processing and distribution. chemical bottles. A safe way to transport
against organic solvents, protecting food EVAL™ offers a reliable barrier alternative chemical concentrates.
against the ­migration of conta­mination to Al foil, with the addition of excellent
like MOSH/MOAH mineral oils that can transparency and safe and low-impact
compromise food safety. EVAL™ also resists energy recovery at end of life. Hydrophilic, anti-static and
permeation of hydrocarbons and grease, glossy appearance
maintaining packaging ­appearance. In Energy efficiency More than just a gas barrier layer
addition to protecting food, this property Extending service life EVAL ™ is a hydrophilic polar material
also protects the environment, locking EVAL™ barrier helps prolong performance with anti-static properties and a glossy
chemical substances inside safe and and service life in vacuum insulation and appearance when used as an outside
convenient plastic packaging. reliable all-plastic pipe heating/cooling ­layer. In addition to packaging, its un-
systems. usual mix of properties leads to use as a
Aroma barrier, no flavour technical plastic for industrial, electronic
scalping Fuel vapour barrier and medical components.
Assuring quality in new forms of Safety and environmental protection
distribution Light weight barrier plastic tanks and
While keeping oxygen and other gases lines improve the performance and ­safety
Function,
performance
and properties
"EVAL™ EVOH resins have outstanding
barrier properties, offering performance
far greater than any conventional polymer."

Typical coextrusion multilayer structure

Oxygen Odours

Outer layer
Regrind
Tie
EVAL™ EVOH
Tie
Inner layer

3
Freshness Flavour CO2
Table of contents

- EVAL™ resin grades 4


- EVAL™ monolayer film grades 6
- Gas barrier properties 6
Processability of EVAL™ resins can be coextruded with - Water vapour transmission and
EVAL™ resins many types of polyolefins, polyamides, ­moisture absorption of EVAL™ resins 12
EVAL™ resins are thermoplastic polymers, polystyrene and polyesters. Downstream - Mechanical properties 14
suitable for use on conventional processing such as thermoforming, - Thermal characteristics 15
converting equipment for the following ­vacuum and pressure moulding and - Processing EVAL™ resins 16
processes: printing can be normally done with - Typical temperature settings 21
flexible or sheet structures ­containing - Start-up, Purging and Shutdown 22
• monolayer film extrusion (blown or cast) EVAL™ resins, with special grades - Moisture absorption and drying 24
• multilayer film coextrusion available for even the most demanding - Adhesive resins 25
(blown or cast) conditions. - Utilisation of regrind 25
• sheet coextrusion - Environmental benefits 26
• coextrusion blow moulding Thin coextruded barrier film structures - Open innovation 27
• pipe coextrusion containing EVAL™ can be laminated to
• extrusion coating other substrates, adding barrier function
• coextrusion coating to paper, carton and other renewable
• pipe coextrusion coating resources.
• coinjection moulding
• lamination (EVAL™ monolayer film) Monolayer EVAL™ film can similarly be
laminated to virtually any substrate,
providing exceptional barrier properties For technical information
to demanding technical and industrial
applications, and as barrier sealant. Learn more and find your regional
contact at www.evalevoh.com
eval.eu@kuraray.com
EVAL™ resin grades

The widest range of grades


A variety of EVAL™ grades have been developed specifically for different methods of
production and secondary processing. The perfect balance of required properties is
achieved by using Kuraray technology to modify the ratio of ethylene to vinyl alcohol in
the copolymer. The result is the widest available range of EVOH grades.

M 24 mol%

EVAL™ M type 25
has the lowest ethylene content available, and provides the highest barrier for
26
automotive and flexible applications.
L 27 mol%
EVAL™ L type
28
has a very low ethylene content and is suitable as an ultra-high barrier grade in flexible,
bottle and sheet applications. 29

30
4
EVAL™ F type
offers superior barrier performance with long-term run stability, and is widely used 31
as the standard grade for flexible, automotive, bottle and tube applications.
Specific versions exist for coating and pipe applications.
F T J 32 mol%

33
EVAL™ T type 34
was specially developed to obtain reliable layer distribution in thermoforming,
and has become the industry standard for multilayer sheet and thermoformed C 35 mol%

flexible applications.
36

EVAL™ J type 37

offers thermoforming results even superior to those of T, and can be used for
unusually deep-draw or sensitive sheet-based applications.
H 38 mol%

39

EVAL™ C type 40
can be used for high-speed coextrusion coating and cast flexible applications.
41

EVAL™ H type 42
combines high-barrier properties and long-term run stability and thermoformability.
43
The higher ethylene content allows easier processing and longer running times on
older coextrusion equipment, especially for blown flexible structures.
E 44 mol%

45
EVAL™ E type
has a higher ethylene content that allows for greater flexibility and even 46
­easier ­processing.
47

EVAL™ G type G 48 mol%


has the highest ethylene content, making it the best candidate among standard EVAL™
49
grades for stretch and shrink film applications.
50
EVAL™ (EVOH) resin grades and typical characteristic values
The following is an overview of EVAL™ resin grades with their typical properties and a
­ pplications, distinguished by standard grades,
grades for specific processing and secondary processing, and special grades. EVAL™ SP grades have improved orientation properties,
taking EVOH where it could not go before.

Table 1a: Standard grades


Grade Et.Cont. Density*1 MFR*2 Tm Tg*3 OTR*4 Application
(mol%) (g/cm³) (g/10min) (°C) (°C) (cm³.20µm/m².day.atm)
L171B 27 1.21 4.0*5 190 63 0.1 ultra high-barrier
F101B 32 1.19 1.6 183 60 0.3 fuel tank, bottle
F171B 32 1.19 1.6 183 60 0.3 bottle, sheet, film, tube
H171B 38 1.17 1.7 172 56 0.7 bottle, sheet, film, tube
E105B 44 1.14 5.5 165 53 1.9 sheet, film, tube
G156B 48 1.12 6.4 157 50 3.7 oriented shrink film
*1 20°C *2 190°C, 2,160g *3 Dry *4 20°Cx65%RH, ISO 14663-2 annex C *5 210°C, 2,160g

Table 1b: Grades for specific processing conditions


Grade Et.Cont. Density*1 MFR*2 Tm Tg*3 OTR*4 Application
(mol%) (g/cm³) (g/10min) (°C) (°C) (cm³.20µm/m².day.atm)
F101A 32 1.19 1.6 183 60 0.3 F101 without external lubricant
F104B 32 1.19 4.4 183 60 0.3 high MFR F-type
FP101B 32 1.19 1.6 183 60 0.3 extended pipe service life
FP104B 32 1.18 4.4 183 60 0.3 extended pipe service life 5
T101B 32 1.17 2.0 183 55 0.4 thermoformed film, sheet
J102B 32 1.17 2.0 183 54 0.6 deep thermoforming, sheet
C109B 35 1.18 8.5 177 53 0.5 extrusion coating
E171B 44 1.14 1.7 165 53 1.9 low MFR E-type
*1 20°C *2 190°C, 2,160g *3 Dry *4 20°Cx65%RH, ISO 14663-2 annex C

Table 1c: Special grades


Characteristics Comparison to standard grades Grade

Thermoforming grade Improved EVAL™ layer distribution during deep thermoforming SP Series, LT Series, J171B
Soft grade Improved flex-crack resistance with similar barrier FS201B
High impact strength grade Improved impact strength LA170B
Fuel tank grade Ultra high barrier properties for automotive M100B
Pipe grade Provides extended service life at high temperature FP101B, FP104B, EP105B
Retort grade Retort flexible grade. Improved retort performance for thin transparent structures. FR101B, LR171B
Please contact us for more information concerning Special grades.

Table 1d: SP grades. Improved orientation and layer distribution during secondary processing
Grade Et.Cont. Density*1 MFR*2 Tm Tg*3 OTR*4 Application
(mol%) (g/cm³) (g/10min) (°C) (°C) (cm³.20µm/m.day.atm)
SP521B 27 1.19 4.1*5 190 63 0.2 improved layer distribution in forming
SP482B 32 1.16 2.0 183 60 0.6 improved film orientation
SP292B 44 1.13 1.9 165 48 3.0 improved film orientation

*1 20°C *2 190°C, 2,160g *3 Dry *4 20°Cx65%RH, ISO 14663-2 annex C *5 210°C, 2,160g

Processing agents for EVAL™ resin


We also offer the following processing agents, useful for specific EVAL™ resin applications and processing methods
• Recycling agent • Purging agent Please contact us for more information.
EVAL™ monolayer film grades
Table 2: EVAL™ EVOH monolayer film grades for lamination
Grade Type Thickness Ethylene Density OTR*1 Applications
(µm) Content (g/cm³) (cm³/m².day.atm)
(mol%) 20°C 65% RH
ISO 14663-2
EF-XL Biaxially oriented 12 32 1.20 0.4 high barrier

EF-F Non-oriented 12 32 1.20 0.6 high barrier, deep draw

EF-E Non-oriented 30 44 1.14 1.0 sealable, deep draw


Biaxially oriented,
VM-XL 15 32 1.20 <0.05 ultra-high barrier
Aluminium metalized.
HF-M Non-oriented 12 - 1.10 - matt for wallpaper use

Gas barrier properties


6
1. General information
EVAL™ resins have outstanding gas barrier properties that exceed those of all other plastics used today for barrier purposes.

Fig. 1: EVAL™ layer OTR (cm³/m².day.atm) at 20°C, 65%RH


thickness and Oxygen 100

­Transmission Rate
The Oxygen Transmission Rate of an
EVAL™ layer is inversely proportional
10
to its thickness. Put another way, by
doubling the thickness of the EVAL™ layer,
the oxygen transmission is reduced by
one half. 1

Packaging performance can be designed E105B

and optimised by selecting the appropri- H171B


0.1
ate EVAL™ layer thickness.
F101B

L171B
0.01
1 10 100 1000

Thickness (µm) of EVAL™ Layer


Table 3: Gas Transmission Rates of selected polymers
In addition to oxygen, EVAL™ resins offer outstanding barrier against other gases as well.
Data is provided below for helium and typical MAP gases like carbon dioxide and nitrogen.

Films Gas Transmission Rates at 0% RH (cm³.20 µm/m².day.atm)


H² N² CO² He Ar Ar Kr Kr
(20°C) (25°C) (25°C) (25°C) (35°C) (50°C) (35°C) (50°C)

F101B 30* 0.017 0.81 160 - 0.5 - 0.4

E105B 200 0.13 7.1 410 1.6 7.0 - 1.8

OPA - 12 205 2,000 - - - -

CPA - - - - 60 150 23 68

OPET - 8 110 3,100 - - - -

OPP 10,000 730 9,100 - 8,100 28,000 6,900 23,000

LDPE - 3,100 42,000 28,000 19,000 46,000 25,000 74,000


*F171B

"EVAL™ barrier properties work in both directions,


keeping unwanted gases and contamination out, 7
while maintaining inside gas mixes longer."
2. Effect of environmental conditions
EVAL™ resins, as indicated by the presence of hydroxyl groups in their molecular
­structure, are hygroscopic and readily absorb moisture. The amount of moisture that
will be absorbed and the speed of absorption will depend upon the environmental
­conditions encountered. Moisture absorption is dependent upon temperature and the
relative humidity of the environment.

Fig. 2: Oxygen Gas Transmission Rate at 20°C versus


­relative humidity in EVAL™ resins

OTR (cm³.20µm/m².day.atm) ISO14663-2 Annex C standard (65%RH)

100

10 G type (48% ethylene)

8
E type (44% ethylene)

H type (38% ethylene)


1

F type (32% ethylene)

0.10

L type (27% ethylene)

0.01
0% 20% 40% 60% 80% 100%

Relative humidity (%RH)


However, though the barrier properties of EVAL™ resins decrease with increasing
­humidity, even at high humidity, EVAL™ resins still maintain their superior barrier
­properties when compared with other materials as shown in figure 3.

Furthermore, by coextruding EVAL™ resin between layers of high moisture barrier resins
like polyethylene or polypropylene, the loss of oxygen barrier properties is greatly
diminished. Nevertheless, humidity should be considered in designing
high-barrier structures.

Fig. 3: Oxygen Transmission Rate of various polymers


­versus relative humidity at 20°C

OTR (cm³.20µm/m².day.atm) ISO14663-2 Annex C standard (65% RH)


10,000
LDPE

BOPP

1,000

9
PVC-U
100

OPET

OPA6
10 PAN
PVDC MXD-6

EVAL™ E type (44 mol% ethylene)


1

EVAL™ F type (32 mol% ethylene)

0.1

0% 20% 40% 60% 80% 100%

Relative humidity (%RH)


Adjusting structure design for optimal performance

Based on the application and typical conditions of use, it is possible to optimise barrier
performance. The equilibrium relative humidity of the EVAL™ layer can be lowered by
shifting its location or by carefully choosing the other materials in the structure.

liquid products dry products


Outside
liquid
Inside
products
Outside Inside Outside
dry products
Inside Outside
100%RH 100%RH
Outside Inside Outside Inside
91%RH Outside Inside Outside
84%RH 80%RH 80%RH
100%RH 100%RH
65%RH 91%RH 65%RH
84%RH 80%RH 80%RH
65%RH 65%RH
34%RH

34%RH
10%RH

OPP/EVAL™/LDPE OPP/EVAL™/LDPE OPP/EVAL™/LDPE10%RH OPP/EVAL


µm 20/15/50 µm 20/15/50 µm 20/15/50 µm 20/1
OPP/EVAL™/LDPE OPP/EVAL™/LDPE OPP/EVAL™/LDPE OPP/EVAL
µm 20/15/50 µm 20/15/50 µm 20/15/50 µm 20/1

Outside Inside Outside Inside Outside Inside Outside


100%RH 100%RH
Outside Inside Outside Inside Outside Inside Outside
80%RH 81%RH 80%RH
100%RH 100%RH
65%RH 66%RH 65%RH 63%RH
80%RH 81%RH 80%RH
65%RH 66%RH 65%RH 63%RH
10
10%RH

OPA/EVAL™/LDPE OPA/EVAL™/LDPE OPA/EVAL™/LDPE10%RH OPA/EVAL™


µm 15/15/50 µm 15/15/50 µm 15/15/50 µm 15/1
OPA/EVAL™/LDPE OPA/EVAL™/LDPE OPA/EVAL™/LDPE OPA/EVAL™
µm 15/15/50 µm 15/15/50 µm 15/15/50 µm 15/1

dry products
Outside
dry products
Inside Outside Inside

Outside Inside Outside Inside


80%RH
65%RH
80%RH
65%RH 40%RH
34%RH
40%RH
34%RH
10%RH 10%RH

OPP/EVAL™/LDPE10%RH OPP/EVAL™/LDPE10%RH
µm 20/15/50 µm 20/15/50
OPP/EVAL™/LDPE OPP/EVAL™/LDPE
µm 20/15/50 µm 20/15/50

Outside Inside Outside Inside

Outside Inside Outside Inside


80%RH 77%RH
65%RH 63%RH
80%RH 77%RH
65%RH 63%RH

10%RH 10%RH

OPA/EVAL™/LDPE10%RH OPA/EVAL™/LDPE10%RH
µm 15/15/50 µm 15/15/50
OPA/EVAL™/LDPE OPA/EVAL™/LDPE
µm 15/15/50 µm 15/15/50
Figure 4 shows that even in packaging wet foods, multilayered structures containing an EVAL™ resin
layer can be designed to give 10 times the oxygen barrier properties of PVDC.

Fig. 4: Changes in Oxygen Transmission Rate


for composite film structures

OTR (cm³/m².day.atm, 20°C)

100
50 Exterior 65% RH
PVDC (2 µm)
coated OPP (20 µm)
20 PE (60 µm)
Interior 100% RH
10

2
Exterior 65% RH
1 OPP (20 µm)
EVAL™ F101B (15 µm)
0.5 PE (60 µm)
Interior 100% RH

0.2

0 10 20 30 120
Days
11

With its exceptional barrier properties, at equal


thickness EVAL™ EVOH provides better barrier
performance than any other conventional polymer.
A well-designed team of different layers, each with its
own technical strengths, work together to make the
most efficient structures possible.

Regrind of multilayer structures is commonly used


on stream as a structural layer, and is proven
not to disrupt polyolefin recycling streams.

The excellent migration barrier of EVAL™ EVOH


ensures content integrity and opens new opportunities
for post consumer recycling in food packaging.
Water vapour transmission
and moisture absorption
of EVAL™ resins

As mentioned in the previous section, EVAL™ resins are hygroscopic and absorb
­moisture. The amount of moisture that will be absorbed and the speed of absorption
will depend upon the environmental conditions encountered. Moisture absorption is
dependent upon temperature and the relative humidity of the environment. For com-
parison, table 5 shows the water vapour transmission rate (WVTR) of monolayer EVAL™
films and films of other polymers. Figure 8 shows the speed of moisture absorption
of EVAL™ monolayer film, normally the EVAL™ is co-extruded/laminated with other
­materials, which will reduce this speed of moisture absorption in the EVAL™ greatly.

12
Table 4: WVTR of monolayer films

Films WVTR (ASTM E96-E). 40°C 0/90% RH (g.30µm/m².day)


EVAL™ L type (27% ethylene) 85
EVAL™ F type (32% ethylene) 52
EVAL™ T type (32% ethylene) 37
EVAL™ H type (38% ethylene) 32
EVAL™ E type (44% ethylene) 27
EVAL™ G type (48% ethylene) 23
EVAL™ F101 (bi-axially oriented) 20
Extrudable high barrier PVDC 3
Bi-axially oriented PP 5
HDPE 5
PP 9
LDPE 15
Bi-axially oriented PET 15
Rigid PVC 40
PAN 80
PS 112
Bi-axially oriented PA 6 134
Fig. 5: Moisture absorption of EVAL™
Moisture absorption (%)

12

10
EVAL™ F type 65% RH > 100% RH

6
EVAL™ E type 65% RH > 100% RH

EVAL™ F type 0% RH > 65% RH


4

EVAL™ E type 0% RH > 65% RH

2
13

0
0 1 2 3 4 5
Days

Fig. 6: Equilibrium moisture absorption Fig. 7: Moisture absorption of EVAL™


and relative humidity of EVAL™ multilayer film as a function of time
Equilibrium moisture absorption (%) at 20°C Moisture absorption of EVAL™ layer (%) at 20°C, 100% RH
12 12

10 10 OPA15µm / EVAL™ F101B15µm / PE60µm

8 8

OPP20µm / EVAL™ F101B15µm / PE60µm

6 EVAL™ F type 6

4 4

2 2
EVAL™ E type

0 0
0 20 40 60 80 100 0 10 20 30 120
Relative Humidity (%RH) Days
Mechanical properties

EVAL™ resins have high mechanical strength, elasticity and surface hardness plus excellent abrasion resistance.

Table 5: Typical mechanical properties of standard EVAL™ resin grades

EVAL™ Grade Name L171 F171 F101 F104 C109 T101 H171 E105

Ethylene content(%) mol% 27 32 32 32 35 32 38 44

Tensile stress at break MPa ISO 527 41 34 34 34 32 33 31 29

Tensile strain at break % ISO 527 12 14 15 14 14 16 16 18


Conditioning: 23°C, dry
Measurement: 23°C,
50%RH
Young's Modulus GPa ISO 527 4.9 4.5 4.5 4.5 4.3 4.3 4.0 3.5

Flexural Modulus GPa ISO 178 4.7 4.3 4.3 4.3 4.0 4.1 3.8 3.2
14
Charpy Impact Strength kJ/m² ISO 179-1 6 7 8 7 6 9 8 10

Conditioning: 23°C, dry


Rockwell Hardness HRM ISO 2039-2 Measurement: 23°C, 97 92 92 92 89 92 83 80
50%RH
Thermal characteristics

Table 6: Typical thermal properties of standard EVAL™ resin grades

EVAL™ Grade Name L171 F171 F101 F104 C109 T101 H171 E105

Melting Temperature °C ISO 11357 Measurement: 10°C/min 190 183 183 183 177 183 172 165

Crystalization
°C ISO 11357 Measurement: 10°C/min 164 158 158 158 155 158 151 145
Temperature

Glass Transition Point °C ISO 11357 Measurement: 20°C/min 63 60 60 60 58 60 56 53

Conditioning: 23°C, dry


Vicat Softening Point °C ISO 306 Measurement: 23°C, 50%RH 181 172 172 172 167 165 162 152

MFR g/10min ISO1133 190°C, 2160g 4.0 1.60 1.60 4.40 8.50 2.00 1.70 5.50
(210°C)
15
Density g/cm³ ISO1183-3 20°C 1.21 1.19 1.19 1.19 1.18 1.17 1.17 1.14
Processing EVAL™ resins

Cylinders
• Natural or shallow grooved is recommended.
• As steel type of cylinders, nitrided steel or special alloys are used for their superior
wear resistance with the inner surface honed.
• The outside of the cylinder should be divided into 4 to 5 zones for good extrusion
temperature control.
• The lower part of the hopper or the feed throat should be able to be cooled by water to
avoid premature melting of the surface of the pellets which might cause bridging and/
or blocking of the hopper.

Screws
Extruder properties such as output, resin temperature, consistency of extruded product,
output stability, power consumption, etc. are mainly determined by screw design.

16
•S
 crew type: single stage metering screw (full flight) is recommended.
•D
 esign L/D: screws with following length to diameter ratios are preferred:
- F grade (32 Et%) L/D ratios of at least 26 are desirable
- E grade (44 Et%) L/D ratios of 24 or larger are recommended
•C
 ompression ratio: a compression ratio of 3 is recommended (compression ratio
calculated as ratio of channel volume of feed and metering section of screw).
•Z
 one distribution: screws with constant pitch, relative long feed section and a
­gradually decreasing channel depth in the compression zone leading to a metering
zone are recommended; in particular, the following zone distributions will be best
suited for processing EVAL™ resins.

Table 7: Recommended zone distributions

L/D Feed zoned Zone distribution Metering zone


Compression zone
28 8D 10D 10D
26 8D 9D 9D
24 8D 8D 8D

Quick compression type screws, (4D or less for compression zone) as used for
­processing PA, should be avoided.

•M
 ixing zone: screws with mixing zones or heads may be used for extruding EVAL™
though this is generally not recommended. The use of a (high shear) mixing head can
restrict the flow of EVAL™ resin, causing degradation of the polymer under prolonged
heat and time.
•S
 crew tip: screw tip angle of 120° - 150° is recommended.
•F
 light: a constant flight width of 0.1D is recommended.
•S
 crew material: chromium molybdenum steel, normalised prior to plating is
­recommended as screw material. To help prevent the build-up of polymer on the
screw, surface hard chrome plating (30 - 50 μm) with buff finishing is recommended,
though in some cases nitration treatment can be applied as well.
•S
 crew clearance: instead of recommendation, following example is given for screw
clearance: inside diameter of cylinder is 60.02 - 60.05 mm in combination with screw
diameter of 59.87 - 59.89 mm. When, due to wear, the screw clearance becomes
too large, melt backflow can occur which can cause material degradation due to
high shear rates.

Fig. 8: Typical screw design for 60 mm single stage metering screw


Screw diameter Drive Shank Flight Channel Root Trailing Leading Screw Screw diameter
edge edge tip

17
Channel depth Pitch Channel depth

Feed section Compression section Metering section

Flight length

Note: screw drawing is not scaled to dimensions

Typical dimensions
Diameter 60 mm
Flight length 1 560 mm (26D)
Feed section length 480 mm (8D)
Compression section length 540 mm (9D)
Metering section length 540 mm (9D)
Compression ratio 3
Constant pitch (flight lead) 60 mm (1D)
Channel depth feed section 8.4 mm
Channel depth metering section 2.5 mm
Channel width 54 mm (0.9D)
Flight width 6 mm (0.1D)
Flight angle 17.65°
Screw tip angle 120° ~ 150°
Flight to root radius Feed section Compression section Metering section
• Leading edge radius 8.4 mm 8.4 - 2.5 mm 2.5 mm
• Trailing edge radius 5 mm 5-2 mm 2 mm
Typical output
•F or single flight metering screw, typical output can be calculated with following
­simplified method, where the drag flow, pressure flow, etc. are not considered.

Q = ½ • ρ • N • π • D • Hm • W • cos² φ • 60 • 10-6

where : Q = output (kg/hr)


ρ = melt density (g/cm3)
N = screw rotation (rpm)
D = screw diameter (mm)
Hm = channel depth in metering zone (mm)
W = channel width (mm)
φ = flight angle (deg)

­ hen the flight pitch (P) equals the screw diameter (P = π.D.tan φ
•W tan φ = φ = 17.65°)
and W = 0.9D, above equation becomes:

Q = 7.7 • 10-5 ρ • N • D² • Hm
18
which coincides with the experimental results given following conditions:
- back pressure from 0 - 20 MPa
- use of lubricated EVAL™
- ratio actual output / theoretical output =
˜ 0.8 - 1 : normal extrusion
- or ratio actual output / theoretical output > 1 : overpacking

•G
­ enerated shear rates can be calculated with γ= • (1/s)
and should be in the range of 50 - 100 (1/s)

Table 9 shows typical outputs, achieved using a metering screw with configuration as
recommended for EVAL™ resins.

Table 8: Calculated output for metering screw

Screw diameter (mm) 25 40 50 60 90


L/D 26 26 26 26 26
Constant pitch (mm) 25 40 50 60 90
Feeding zone, depth 8D, 4.9 mm 8D, 6.1 mm 8D, 6.6 mm 8D, 8.4 mm 8D, 11.6 mm
Compression zone 9D 9D 9D 9D 9D
Metering zone, depth 9D, 1.4 mm 9D, 1.8 mm 9D, 2.0 mm 9D, 2.5 mm 9D, 3.5 mm
Compression ratio* 3 3 3 3 3
Screen pack (mesh) 50/100/50/50 50/100/50/50 50/100/50/50 50/100/50/50 50/100/50/50
Motor capacity (kW) 2.2 ~ 3.7 7.5 ~ 11 11 ~ 15 15 ~ 22 37 ~ 55
Screw rotation (rpm)** 30 - 70 30 - 70 30 - 70 30 - 70 30 - 70
Output (kg/hr)** 2.1 - 5.0 7 - 16 12 - 29 22 - 51 69 - 162
Shear rate (1/s)*** 28 - 65 35 - 81 39 - 92 38 - 88 40 - 94

* volumetric compression ratio ** normal range *** theoretical values


Screen pack - breaker plate
A screen pack and breaker plate, placed between the extruder and die, is common
­practice in commercial polymer extrusion. The use of a screen pack is recommended
for extrusion of EVAL™ resins. The screen pack mesh should be based on commercial
polymer extrusion knowledge and common sense. Examples of typical combinations
of stainless steel meshes are: 50/100/50/50, 50/100/150/100 or 80/150/50/50.

Typical distance between screw tip and screen pack is 5 to 10 mm, longer distances
may cause unnecessary longer residence time. For the breaker plate it is recommended
that the holes have a diameter of approx. 5 mm and that the outermost array of holes
inscribes the inner surface of the cylinder.

Melt path (adapter, melt pipe)


EVAL™ resins are highly adhesive to metal surfaces. If the EVOH extrusion system consists
of concave or convex parts, acute angles, etc. EVAL™ resin can easily become r­ estricted
in these dead spot areas. Even in a passage of fixed diameter, retention can o
­ ccur on
the wall if the diameter is too large for the flow and therefore the shear rate is too low.
­Retained resin, exposed to heat at prolonged time, can deteriorate forming gels or oxi-
19
dised particles. The degraded resin will manifest itself as yellowish, brown or black gels.

When designing process equipment for EVAL™ resins, the following points are
­recommended for the EVAL™ melt path:
• Shear rate at wall: higher than 6 s-¹.
• Average flow rate: higher than 1 cm/s.
• Eliminate any concave, convex, or acute angles in the melt path.
• Minimise the diameter of all adapters.
• Chrome plate (and buff finish) the surfaces exposed to the EVAL™ melt path.

Following are examples recommendable, respectively not recommendable, for the


adapter direct after the breaker plate.

Fig. 9: Adapter design


Important part

long taper

straight
90°
120°

R30

Recommended Not recommended Not recommended


Dies
EVAL™ resins are suitable for normal feedblock type die designs. Special die designs are
not necessary, though care should be taken to streamline the flow channels as much as
possible, especially with complicated die designs (e.g. for blown film lines) which could have
increased number of dead spots and prolonged residence time. As with the adapter and
melt pipe, it is recommended to chrome plate the surfaces exposed to the EVAL™ melt.

Lubricant mixed EVAL™ resin


Use of lubricant mixed EVAL™ resin is recommended for improving the stability of the
resin flow at the feeding zone of the screw, resulting in a more constant output rate and
lower energy consumption of the extruder motor.

20
Extrusion temperature
In processing any polymer it is important that a homogeneous, completely melted and
well mixed mass at a uniform temperature is obtained. Also, the temperature must be
well controlled to minimise thermal decomposition of the polymer being processed.
EVAL™ resins are no exception to this rule. Upper and lower extrusion temperature limits
are as follows:

Table 9: Upper and lower extrusion temperature limits

EVAL™ resin grade L171 F171 F104 T101 H171 E105

Upper temperature °C 240 240 240 240 240 250


Lower temperature °C 210 200 200 200 200 185
Melting point °C 191 183 183 183 175 165

It should be remembered that when extruder temperature exceeds the recommended


upper limits, the polymer may decompose resulting in gels, voids, in the extrudate. On
the other hand, at low extrusion temperatures, the resin may only be partially melted,
the melt not mixed or heterogeneous, resulting in poor extrudate appearance, erratic
web gauge control or unmelted specs in the extrudate.

Coextrusion with polymers such as PET, PA, PC or PP may cause the EVAL™ resin to
come in contact with melt streams that are hotter than the recommended maximum
temperature. This contact is usually for a short period of time and adverse effects are
not encountered.
Table 11 shows typical extrusion temperature conditions for the different EVAL™ grades.

Table 10: Typical screw design characteristics

Extruder diameter 60 mm
L/D 26
Flight Full flight
Screw pitch 60 mm, constant
Feed zone, channel depth 8D, 8.4 mm
Compression zone 9D
Metering zone, channel depth 9D, 2.5 mm
Compression ratio 3.0
Motor capacity 22 kW
Screen structure 50/100/50/50 mesh

21

Table 11: Typical Temperature settings for extruding EVAL™ resins

EVAL™ resin grade M100 L171 F101 F171 F104 T101 C109 H171 E105 E171 G156
FP101 FP104 J102 EP105

Barrel temperature C1 °C 190 190 180 180 180 180 180 175 170 170 165

C2 °C 210 205 200 200 200 200 200 195 190 190 185

C3 °C 215 210 205 205 205 205 205 205 195 195 190

C4 °C 220 215 215 215 215 215 215 215 205 205 200

C5 °C 220 220 220 220 220 220 220 220 210 210 205

Adapter temperature AD1 °C 220 215 215 215 215 215 215 210 195 195 190

AD2 °C 220 215 215 215 215 215 215 210 195 195 190

Die temperature °C 215 215 215 215 215 215 215 210 195 195 190
Start-up, purging and shutdown procedures
Start-up
When starting up the extrusion of EVAL™ resins, the following procedure is
­recommended:
1. The extruder is filled with low MFR (0.7 - 1.0)(*) LDPE in order to avoid oxidisation of
residual material in the extruder.
2. Start the processing on a well-cleaned machine by raising the temperature to the
set point and introducing LDPE with an MFR of 0.7 – 1.0. Be careful not to start the
screw rotation before all LDPE material is heated up to processing conditions.
3. When the extrusion gets stable, directly switch over to EVAL™ without running the
extruder empty to avoid oxidisation of EVAL™ by the oxygen in the heated barrel.

Purging
When purging between production campaigns, the following procedure is recommended:
1. Remove EVAL™ from the hopper of the extruder.
2. Introduce LDPE with low MFR (0.7 - 1.0) and purge the EVAL™ out of the extruder
while keeping the same process temperature settings (or temperatures slightly
lowered). Adjust the processing conditions in case the extrusion becomes unstable.
Pressure in the extruder should be high enough to ensure proper cleaning.
3. Continue purging by low MFR LDPE until the residual EVAL™ is completely cleaned
out. If this cannot be determined by visually checking product appearance, set up
22
a specific purge test to determine the time or amount of purge material needed to
clean the extruder and die head.

Shutdown
1. Introduce LDPE with low MFR (0.7 - 1.0) and purge out EVAL™ from the extruder while
keeping the same process temperature settings (or temperatures slightly lowered).
Adjust the processing conditions in case the extrusion becomes unstable. Pressure in
the extruder should be high enough to ensure proper cleaning.
2. Continue purging by low MFR LDPE until EVAL™ is completely cleaned out by
­checking product appearance.
3. Screw revolution can be stopped when the extruder is completely filled with low MFR
LDPE followed by lowering the extruder temperatures. (In that way, the oxidisation of
residual EVOH in the extruder will be avoided).

It is strongly recommended not to use PA as a purge material, since PA will react/


bond with the residual EVAL™ and form numerous gels.

It is also recommended not to use PP, HDPE or adhesive resins as a purge material
because some PP and HDPE grades may contain some residual catalyst that can
very strongly deteriorate EVAL™.

(*) MFR: Melt Flow Rate mentioned in this section are data measured with a standard
melt indexer at 190°C, 2.16 kg (EVAL™ F101B: 1.6 g/10 min; EVAL™ H171B: 1.6 g/10
min; EVAL™ E105B: 5.5 g/10 min).
Kuraray's ETC-103 purging material
ETC-103 (MFR: 1.0) is a LDPE-based purge resin, developed by Kuraray for purging
­ex­truders running EVAL™ resins and for improved transitioning from EVAL™ extrusion
to PA or polyolefins. Because of its chemical properties (besides mechanical c­ leaning),
it is used to remove EVAL™ residues from the extruder and die head or to improve
­current purging procedure.

If time to start-up is critical, a LDPE with higher MFR (5 – 7) can be introduced after
purging with the low MFR (0.7 – 1.0) LDPE. The higher MFR (5 – 7) LDPE remains in the
extruder after shutdown and can be removed much faster by EVAL™ resin after start-up.

In case the application involves a regrind layer (incl. EVAL™), it is recommended also to
purge this extruder with the original material (LDPE, HDPE, PP).

Temporary extruder shutdown 23

When the extrusion operation has to be stopped temporarily, the following procedures
are given as an indication:

Shutdown time Procedure


Up to 30 minutes Maintain temperature settings, screw rotation can be stopped
Up to 3 hours Maintain or lower temperature settings by about 20°C and operate screw slowly
For more than 3 hours Purge out EVAL™ as recommended in extruder purging procedure

Please note that maximum shutdown times with EVAL™ in the extruder depend on the
design of the processing equipment, temperature settings and residence times.

Polymer change over


The table below lists the recommended purge sequences for change over involving EVAL™ resins.

Resin before change Resin after change Sequence


LLDPE, LDPE EVAL™ Direct
EVAL™ LLDPE, LDPE Direct
PA, HDPE, PP, PS EVAL™ PA, HDPE, PP, PS LDPE EVAL™
EVAL™ PA, HDPE, PP, PS EVAL™ LDPE PA, HDPE, PP, PS
Prevention of moisture absorption, drying
As mentioned in section 4, EVAL™ resins are hygroscopic and absorb moisture when
exposed to atmosphere. Depending upon the fabrication process being used, an increase
in the moisture content of EVAL™ resins can cause difficulties in processing; foaming,
voids and gels can occur at increased moisture levels (normally above 0.4 wt%).

After the production, EVAL™ resins are dried and packaged in moisture proof 25 kg bags
or 700 kg octabins. As packaged, the moisture content is controlled to less than 0.3%.
This means that EVAL™ resins do not need to be dried, when processed directly after
opening the package.

Precautions should be taken after opening a package to prevent against excessive


­moisture absorption especially in hot humid environments. These precautions include:
• Re-close the package tightly after use.
• If an air conveying system is used, prevent against excessive moisture in the
­conveying air by use of a moisture trap.
24
• When using octabins, it is not necessary to open the entire liner when inserting the
conveyer pipe; simply cut a hole in the liner and insert the conveyer pipe.

Under normal humidity conditions, packages may be left opened while being used for
several days, for more humid conditions see figure 10.

Fig. 10: Moisture regain vs. time


Moisture regain at 20°C
In the event the EVAL™ package has been
1.0
left open for a longer period and/or at higher
EVAL™ F type humidity conditions, re-drying process such
EVAL™ E type as 3 to 4 hours in hopper dryer or ­circulating
0.8
hot air dryer at 90 - 100°C is recommended.
Please make sure that dryer temperature
does not exceed 110°C to avoid discoloration
0.6
of the EVAL™ resin.
80% RH

0.4 65% RH

0.2

0
0 24 48 72 96 120 144
Time (hours)
Adhesive resins
To improve the properties of plastic packaging materials, two or more polymer layers
in a composite structure are typically employed. These multilayer structures can be
prepared by coating, laminating, or coextrusion. When different polymer layers are used
in multilayer structures, poor adhesion between the layers typically exists. In order to
overcome this deficiency, speciality adhesive resins have been developed. These tie
resins act as the glue substance between the non-adhering polymer layers.

With respect to EVAL™ resins, good adhesion can be achieved between EVAL™ resin and
PA without using an adhesive layer. In coextrusions with polyolefins, PET, PS, PC, etc.,
however, an adhesive layer is necessary between these polymers and EVAL™ resins.
Depending on the counter resin, different adhesive resins are available on the market.

25

Utilisation of regrind
One of the serious economic concerns in coextrusion is the loss of multilayer film
trim or flash. In monolayer film operations such trim is usually regrinded and recycled
with little economic loss to the processor. With thermally sensitive or vastly different
­polymers, however, multilayer films or structures cannot be reprocessed.

Such is not the case when using EVAL™ resins. Multilayer structures containing EVAL™
resin can be recovered and reused. For example, coextrusion trim containing EVAL™
resin can effectively be recycled when producing sheets, bottles and fuel tanks.

It should be remembered that if the regrind is stored unused for a prolonged period of
time, moisture absorption may occur in the EVAL™ component. The regrind then must
be dried prior to extrusion. If possible, it is recommended that regrind containing EVAL™
should be processed and reused as soon as possible to avoid potential processing
­difficulties due to high moisture content.

For several applications, special master batches for regrind are developed by Kuraray
to prevent processing troubles during extrusion of this regrind, increase the maximum
level of EVOH content in the regrind and enhance the properties of the final product.
Environmental benefits
of EVAL™ resins and monolayer film

Wasting food and commercial products generates its own environmental impact, but also wastes all
the resources used to produce, process, package and transport the goods as well. The trick to optimis-
ing packaging design is to find the perfect balance between protective function and minimum material
use. To be truly effective, a wide view of the entire product life cycle is necessary. Ideally, the materials
themselves should have low environmental footprints, but not solve problems at one life cycle stage
only to create different problems at another.

A one millimetre thickness of EVAL™


EVOH has about the same gas barrier
properties as ten metres of LDPE. With
such high performance, EVAL™ layers of
only a few microns can add real func-
tion to multilayer structures. Barrier
performance previously only available
from metal or glass can thus be added
to lightweight structures based on other
26
recyclable and energy recoverable plas-
tics, or renewable ­resources like PLA and
paperboard.

Protecting quality and


value ­decrease in the total amount of ­packaging
Although product development tends to materials used. Optimized portion size, Recyclable and recoverable
focus specifically on EVAL™’s functional lightweight and extended freshness EVAL™ EVOH is recyclable as post-con-
barrier properties, EVAL™ helps conserve help improve the efficiency of storage, sumer plastic waste, and will not disrupt
resources and avoid waste throughout a transport and display, s­ aving costs and polyolefin or PET recycling streams.
product’s life cycle. Reducing waste, and preserving resources.
thus avoiding the loss of all resources in- EVAL™ has excellent and safe energy
vested in the production and distribution Efficient energy use recovery properties, often reducing the
of fresh food, is the best way to reduce EVAL™ helps maintain the efficiency of amount of extra fuel necessary for energy
environmental impact. insulation and heating systems, saving generation from the thermal disposal of
money and resources by extending their sorted waste. Under perfect combustion,
When used in laminated structures for service life. EVAL™ barrier is effective the few microns of EVAL™ in the pack-
food packaging, very thin EVAL™ layers against new fuels, and blocks emissions age emit only small amounts of CO2 and
provide the valuable barrier function to from light weight plastic tank and line water vapour.
the entire structure, usually allowing a systems.
Open innovation
Application development with
the world’s barrier experts

Kuraray is a world leader in specialty chemicals and functional


materials. We are committed to developing products that ensure
quality and value while helping our business partners differentiate
themselves from their competition.

Kuraray Co. Ltd. was the first company in EVAL™ production began in Houston, with converters and end users, bringing
the world to produce and commercialise USA in 1986, and in Antwerp, Belgium in our expertise in barrier technology and
EVOH, starting in Okayama, Japan in 1999. structure optimisation.
1972. Today Kuraray is the world’s
largest producer of Vinyl Acetate Monomer Technical centres were established To learn more about our open
derivatives, and is still the leader in EVOH in Kurashiki, Japan, at the Houston innovation development, visit our
technology, production, structure analysis and Antwerp production sites, and in global website www.evalevoh.com
and technical development. Singapore. At each site we work together

27

HOUSTON, USA ANTWERP, BELGIUM

SINGAPORE KURASHIKI, JAPAN


1809-1410
Nizhny Novgorod
Antwerp
35,000T Kurashiki
Okayama
Houston 10 ,000T
58,000T Tokyo
Shanghai
New Delhi

Bangkok

Singapore

EVAL™ the world’s leading EVOH NOTICE


The information, specifications, procedures, methods and recommen-
Asia-Pacific dations herein are presented in good faith, are believed to be accurate
and reliable, but may well be incomplete and/or not applicable to all

Photos used in this brochure are representative of potential product applications only.
Kuraray Co., Ltd. (Okayama, Japan)
Capacity: 10,000 tons/year conditions or situations that may exist or occur. No r­ epresentation,
The world’s first EVOH production facility guarantee or warranty is made as to the completeness of said infor-
mation, specifications, procedures, methods and ­recommendations

EVAL TECH EN 1104/1809/200/1809 Copyright Kuraray Co., Ltd.


Americas or that the application or use of any of the same will avoid h
­ azards,
EVAL Company of America (Pasadena, Texas, USA) ­accidents, losses, damages or injury of any kind to persons or
Capacity: 58,000 tons/year property or that the same will not infringe patents of others or give
The world’s largest EVOH production facility desired results. Readers are cautioned to satisfy themselves as to the
­suitability of said information, specifications, procedures, methods
Europe and recommendations for the purpose intended prior to use.
EVAL Europe nv (Antwerp, Belgium)
Capacity: 35,000 tons/year
Europe’s first and largest EVOH production facility

www.evalevoh.com

Contact
KURARAY Co., Ltd. KURARAY Asia Pacific Pte. Ltd. KURARAY America Inc. EVAL Europe N.V.
Ote Center Bld., 1-1-3, 331 North Bridge Road 2625 Bay Area Bld. Suite 600 Keetberglaan 1B - Haven 1087
Otemachi, Chiyoda-Ku #18-02 odeon Towers Houston, TX 77058 9120 Melsele
Tokyo 100-8115, Japan Singapore 188720 USA Belgium

Tel: +81 3 6701 1489 Tel: +65 6337 0116 Tel: +1 800 423 9762 Tel: +32 3 250 9733
eval.jp@kuraray.com eval.jp@kuraray.com eval.us@kuraray.com eval.eu@kuraray.com

EVAL™ resins are produced worldwide under unified Kuraray product and quality specifications.

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