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1 Alejandra Reyna-Valencia, ARKEMA - Fine-tuned Adhesive for Extrusion-Coating and Lamination - 17th TAPPI European PLACE Conference 2019 Porto – Session 13 – Paper 1

Fine‐tuned Adhesive for Demanding Applications in Extrusion‐Coating and Lamination 

Presented by:Dr Alejandra REYNAResearch Scientist

ARKEMA

16TH TAPPI EUROPEAN PLACE CONFERENCE

17th TAPPI European PLACE Conference

20-22 May 2019Crown Plaza Hotel Porto

Portugal

2 Alejandra Reyna-Valencia, ARKEMA - Fine-tuned Adhesive for Extrusion-Coating and Lamination - 17th TAPPI European PLACE Conference 2019 Porto – Session 13 – Paper 1

OUTLINE OF THE PRESENTATION

1. The problem: performance issues related to the tie resin● Types of tie resins● Processing● Adhesion

2. The solution: fine-tuned resin● Performance results: laboratory and

industrial lines

3. Summary

Focus: coextrusion coatingCoextruded PO/tie on substrate‐ink

Die

Bi‐layer polymer melt

Chill roll

Nip roll

Substrate

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3 Alejandra Reyna-Valencia, ARKEMA - Fine-tuned Adhesive for Extrusion-Coating and Lamination - 17th TAPPI European PLACE Conference 2019 Porto – Session 13 – Paper 1

1.1. TIE RESINS FOR COEXTRUSION-COATING AND LAMINATIONE-AE-MAH are versatile adhesives for direct bonding in extrusion lamination without primer or liquid gluesRandom ethylene terpolymers produced by high pressure radical polymerizationFully compatible with PE

Ethylene – Acrylic Ester – MAH

--- (CH2 - CH2 -)x -- (CH2 - CH - )y --- (CH2 - CH2 -)z --- (CH - CH - )tI I I

C = O O = C C = OI \ /

O O I

R

Two synthesis routes: autoclave and tubular reactors different molecular architectures

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Ethylene acrylate copolymers: autoclave vs tubular● Different co-monomer distribution● Direct impact on polarity at the molecular scale

1.1. TIE RESINS FOR COEXTRUSION-COATING AND LAMINATION

Regular co-monomer (acrylate) distribution in the polymer chains

Autoclave Process

Lower Tm Better processability

Heterogeneous co-monomer (acrylate) distribution in the polymer chains: micro-domains

Rich in acrylate

Poor in acrylate

Tubular Process

Higher Tm Enhanced adhesion on inks

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5 Alejandra Reyna-Valencia, ARKEMA - Fine-tuned Adhesive for Extrusion-Coating and Lamination - 17th TAPPI European PLACE Conference 2019 Porto – Session 13 – Paper 1

1.1. TIE RESINS FOR COEXTRUSION-COATING AND LAMINATIONEthylene acrylate copolymers: autoclave vs tubular

● Effects on molecular weight distribution, rheological properties and processing behavior

Most LDPE grades used in extrusion coating are autoclave resins

Autoclave

Tubular

Log M

dW

(M)

/ d

(lo

g M

)

6 Alejandra Reyna-Valencia, ARKEMA - Fine-tuned Adhesive for Extrusion-Coating and Lamination - 17th TAPPI European PLACE Conference 2019 Porto – Session 13 – Paper 1

1.1. TIE RESINS FOR COEXTRUSION-COATING AND LAMINATION

Mechanism: 

Relaxation time controls the extent of neck‐in

● Extensional response

● Chain stretching and strain hardening

Extensive literature on the role of molecular architecture in processing behavior:● Example: LLDPE (linear, low polydispersity) shows greater neck-in than LDPE (containing

long-chain branching) and HDPE (high polydispersity)

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1.2. PERFORMANCE ISSUES IN COEXTRUSION-COATING AND LAMINATION

Autoclave Tubular

Drawability at high line speed Neck‐in Encapsulation Adhesion  Extrusiontemperature

8 Alejandra Reyna-Valencia, ARKEMA - Fine-tuned Adhesive for Extrusion-Coating and Lamination - 17th TAPPI European PLACE Conference 2019 Porto – Session 13 – Paper 1

2.1. FINE-TUNED TIE RESIN FOR COEXTRUSION-COATING AND LAMINATION

Requirements

•Good processability• Avoid common processing issues of tubular resins

• Processable at high line speeds

• Satisfactory adhesion• Wide range of substrates and inks

• No primer needed

• No high extrusion temperatures required

Push the limits of current tie resins

Need for high‐performance materials for an evolving application

Driver

Modified E‐MA‐MAH tubular resin

Work on the synthesis route in a tubular reactor

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9 Alejandra Reyna-Valencia, ARKEMA - Fine-tuned Adhesive for Extrusion-Coating and Lamination - 17th TAPPI European PLACE Conference 2019 Porto – Session 13 – Paper 1

2.2. PROCESSING PERFORMANCE: DRAWABILITYSingle-layer cast extrusion on Dr Collin laboratory line

Autoclave

Tubular

Meltbreak [m/m

in]

Melt instabilities [m/min]

T melt = 280°C 

New tubular resin

10 Alejandra Reyna-Valencia, ARKEMA - Fine-tuned Adhesive for Extrusion-Coating and Lamination - 17th TAPPI European PLACE Conference 2019 Porto – Session 13 – Paper 1

2.2. PROCESSING PERFORMANCE: ENCAPSULATIONCoextrusion-coating on Dr Collin laboratory lineStructure: bilayer cast film PP+PE/tie on Alu foil25m/min, die gap = 300µm

LPO

Ltie

% 100

Tubular

New tubular resin

Autoclave

PO blend 1 PO [15µm]/tie [10µm]

% Encapsulation

PO [10µm]/tie [5µm]PO blend 2

Effect of PO blendPO [15µm]/tie [10µm]/Alu foil

Effect of film thicknessPO blend 2

% Encapsulation

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11 Alejandra Reyna-Valencia, ARKEMA - Fine-tuned Adhesive for Extrusion-Coating and Lamination - 17th TAPPI European PLACE Conference 2019 Porto – Session 13 – Paper 1

2.2. PROCESSING PERFORMANCE: INDUSTRIAL SCALEEncapsulation: industrial line● Structure: PO [20g/m2]/tie [5g/m2] on woven PP

CASE 1o Line speed = 50m/mino Layer width difference measured on the melt curtain

CASE 2o Line speed = 150, 200, 220m/mino Layer width difference measured on the coatingLPO – Ltie

0

2

4

6

8

10

12

100 150 200 250L P

O–L tie[m

m]

Line speed [m/min]

L PO–L tie[m

m]

PO blend 1 PO blend 2

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2.3. ADHESION PERFORMANCE: INDUSTRIAL SCALE

150 200 220

Peel strength [N/15mm]

Line speed [m/min]

New tubular resin, method 1

New tubular resin, method 2

Tubular, method 1

Tubular, method 2

Peel strength as a function of line speed: industrial line● Structure: BOPET- ink [12µ]/tie [5g/m2]/PO [20g/m2]/woven PP● T melt = 290°C

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13 Alejandra Reyna-Valencia, ARKEMA - Fine-tuned Adhesive for Extrusion-Coating and Lamination - 17th TAPPI European PLACE Conference 2019 Porto – Session 13 – Paper 1

SUMMARY: LOTADER® 4513TFine-tuned tubular resin for specialty laminates including reverse-printed substrates, oriented substrates, primerless substrates ... Where adhesion is challenging with other resins (ex: LDPE + concentrate)

14 Alejandra Reyna-Valencia, ARKEMA - Fine-tuned Adhesive for Extrusion-Coating and Lamination - 17th TAPPI European PLACE Conference 2019 Porto – Session 13 – Paper 1

THANK YOUFOR YOUR ATTENTION

Contact:

Oceane LAMARZELLE, Ph.D.Extrusion-coating and lamination market developmentARKEMA - Functional PolyolefinsOceane.lamarzelle@arkema.com