49th Man-Made Fibre Congress Dornbirn

Dr. Roland Scholz,R&D, Kelheim Fibres GmbH

Ionic Activated

Viscose Fibres

Ionic Activated Viscose Fibres

Overview

1. Kelheim Fibres – a short introduction

2. Viscose fibres – process, properties, applications

3. Dye absorption characteristics of ionic activatedviscose fibres

4. Summary

2

Kelheim Fibres – Producer of Speciality Viscose Fibres

1930 1940 1950 1960 1970 1980 1990 2000 2010

1968

Hoechst AG

Acquisition of

a majority

shareholding

1974

Hoechst AG

Werk

Kelheim

1994

CourtauldsEuropean Fibres

Joint Venture

Hoechst

and Courtaulds

1999

AcordisKelheim GmbH

1936

Süddeutsche Zellwolle AG

Kelheim,

start-up of viscose

fibre production

(DANUFIL®)

3

2004:

KelheimFibres GmbH

Take-over by

EQUI-

Fibres GmbH

• Head Office Kelheim Germany

• Capacity ~ 75.000 to/year

• Staff ~ 500 people

• Turnover ~ 150 Mill €

• Accumulated R&D know how

from most of the historically leading

viscose producers

Cellulose – A very important Organic Polmyer

4

Cellulose provides structure to the world of plants

• the fibre component in the high-performance composite wood

• multi-functional molecule, polymorphic

• no synthetic polymer offers this spectrum of structures and properties

• renewable, ecologically worthwhile

Viscose Fibres – Chemistry made by Nature

Regeneration process:Conversion of inhomogeneous cellulosic fibres (pulp)to well-defined tailor-made cellulosic fibres (viscose)

5

O

+NaOH+ CS2

+ H2SO4

OH

CH2OH

OH

OH H

H

H

O

HH

CH2OH

OH

OH H

H

H

H

OCell. O C

S

SNa

OH

CH2OH

O

OH

OH H

H

H

O

HO

H

CH2OH

OH

OH H

H

H

O+ CS2+ Na2SO4

Cellulose XanthogenateCellulose

Regenerated Cellulose

Viscose Fibres – A Natural Cycle

6

beech trees

Viscose Fibres – Tailor-made Properties and Span of Application

7

Unrivalled properties

• physiologically neutral, skin-friendly

• superb next-to-skin comfort, soft to touch

• hydrophilic, perfect moisture management

• restricted growth of micro organisms

• chemical stability

• chemical reactivity

(dyeability, processability, adaptability)

• brilliant colours

• not-melting

Viscose Fibres – Ionic Modification

8

Ionic activation of viscose fibres

HO

CH2OH

CH2OH

O

OH

H

H H

OH

H H

HO

O

HO

HO

NMe3

⊕⊕⊕⊕

O

• Incorporation of ionic additives,

e.g. polyelectrolytes

• Covalent bonding

⊕⊕⊕⊕

NR3

⊕⊕⊕⊕

NR3

• Coating of fibres

Ionic Activated Viscose Fibres for Superior Dyeing

9

Cationic activated Deep Dye fibre for yarns and textiles

Test of new approach for cationised fibre

• Decolouration of aqueous media

• Attraction and capture of anionic substances

Competitive dyeing

in one bath

Standard

Viscose

StandardViscose

Deep Dye

• Originally devoloped for superior

dyeability of viscose fibres

• Differential dyeing

• Special dyeing effects and patterns

(e.g. melange)

• One bath dyeing with polyester fibres

• Saving of dye, salt, water, energy, time

and cost

• Less environmental impact

Dye Absorption Capacity and Kinetics – Direct Dyes

• Absorption trials with different direct dyes:

Direct Blue 71, Direct Red 80, Direct Yellow 162

Direct Blue 71(Formula: www.chemblink.com )

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Testing of dye adsorption / absorption properties

Test Parameters – Dye Absorption Capacity

• no classical dyeing conditions

→ no salt, no alkali

• analysis of remaining dye solution

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60 °C, 60 min

20 °C

2 °C

/min

X % dye / mass of fibre

- keep remaining dye solution

- rinse fibre

Dye Absorption Capacity Criteria

• colour intensity of fibre

• colour intensity of remaining

solution

Direct Blue 71

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Dye Absorption Curves

At a certain amount of dystuff → remaining solution not totally colourless

→ but fibre takes up additional dyestuff

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Dyestuff in Remaining Solution

Direct Blue 71

2. Visual rating of solution

→ clear appearance of solution

Judgement of colour intensity

1. Photometric measurement

Definition of threshold

→ 99,8 % of dystuff has to be absorbed

→ 0,02 % remaining dyestuff in solution allowed

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Distribution of Direct Dye in the Fibre

Direct Blue 71

Cationised

Viscose

Standard

Viscose

Low dye

concentration

High dye

concentration

• homogeneous distribution of dye stuff

• utilisation of total fibre cross-section

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Dyeing of Cationised Fibre with Cationic Dye

Cationised Viscose

Viscose

• Typical dyeing conditions (!)

• Cationised fibre absorbs

cationic dyesuff

• Catonised fibre absorbs even

more cationic dye than

standard viscose fibre

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Victoria Blue B

• Dye absorption capacity increases with level of cationic activation

(s-shaped curves)

Capacity – Dependency on the Level of Ionic Activation

Dye Pick up at 100 % Activation

Increase of dye concentrationat start of dye pick up test

Direct Blue 71

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No dependency on total fibre surface

→ consistent with a homogeneous distribution of dye in fibre volume

Capacity – Dependency on Total Fibre Surface

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Capacity – Different Direct Dyes

Remaining Solutions after Dye Pick-up withcationised fibre

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Trichromic solutions (reference):

Direct Red

Direct Blue

Trichromic

• Dye absorption

capacity similar for

different tested direct

dyes

• Trichromic test

shows a slightly

varying affinity to

different dyes →

colour of remaining

liquid is different to

original trichromic

solution

• Capacity depends on

specific dye- Direct Yellow 162- Direct Blue 71- Direct Red 80

• Unchanged dye absorption capacity → no wash outin spunlace process

• Improved absorption capacity with dimensional stable fabrics

Capacity – Dependency on Textile Making-Up of Fibres

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• Conversion of Deep Dye Fibre to nonwoven with standard equipment possilbe

Test Parameters – Dye Absorption Kinetics

• Basic parameters as used for capacity tests

• Analysis of remaining solution

time

Pre-Tests:

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X % dye / mass of fibre

no salt

no caustic soda

20 °C

2 °C

/min

60 °C

- keep remaining dye solution

- rinse fibre

10 min 20 min 30 min

• Increased dye absorption speed with increasing level of

cationic activation

• Almost complete absorption within 10 min

Kinetics – Dependency on the Level of Cationic Activation

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Kinetics – Dependency on tTextile Making-Up of Fibres

• Indication: increased dye absorption speed with increasing

dimensional stability of fabric23

Dye Transfer – Test Parameters

• Dye transfer test: Simulation of real conditions in laundry

⇒ bleeding of dye from textile fabric

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• Bleeding textile fabrics:

C.I.„ReactiveBlack 5“

on Cotton

C.I.„DirectOrange 39“

on Cotton

C.I.„AcidBlue 113“

on Polyamide

Dye Transfer – Test Parameters

• Components of Dye Transfer Test

→ Bleeding Fabric

→ Adjacent Fabric

→ Deep Dye Fibre

→ ECE-laundry detergent

→ Steel balls (6 mm diameter)

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• Parameter in accordance to DIN ISO 105-C06Test for colour fastness to domesticand commercial laundering“

Bleeding

Fabric

AdjacentFabric(segmented)

Wool

PAN

PES

PA 6.6

Cotton

2,5 Acetate

• 30 min, 60 °C

Test method and evaluation

• Staining of reference textile without Deep Dye fibre

• Use of a grey reference scale to judge level of staining26

AdjacentFabric

C.I „Direct Orange 39“

C.I. „Acid Blue 113“

C.I. „ReactiveBlack 5“

Wool

PAN

PES

PA 6.6

Cotton

2,5 Acetate

Dye transfer with {Cotton / Direct Orange 39}

Deep Dye fibresafter transfer test

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• Transfer inhibition with Deep Dye fibre

Adjacent Fabric

Reference DD (low) DD (medium) DD (high)

Wool

PAN

PES

PA 6.6

Cotton

2,5 Acetate

Dye Transfer with {Polyamide / Acid Blue 113}

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• Transfer inhibition with Deep Dye fibre

Deep Dye fibresafter transfer test

Adjacent Fabric

Reference DD (low) DD (medium) DD (high)

Wool

PAN

PES

PA 6.6

Cotton

2,5 Acetate

Dye Transfer with {Cotton / Reactive Black 5}

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• Transfer inhibition with Deep Dye fibre

Adjacent Fabric

Reference DD (medium) DD (high)

Wool

PAN

PES

PA 6.6

Cotton

2,5 Acetate

Deep Dye fibresafter transfer test

• Investigations prove the potential

of cationised Deep Dye fibre

to capture anionic substances andfor decolouring of aqueous media

→ Capacity, kinetics, colour transfer

→ Affinity to different dyes

• The level of cationic activation controls colour absorption

characteristics of Deep Dye fibre

• Homogeneous distribution of dye in the fibre cross section

→ No dependence of dye absorption capacity on total fibresurface

• Conversion of Deep Dye Fibre to nonwoven with standard

equipment possible, without loss of activity

Summary and conclusions

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StandardViscose

Deep Dye

Acknowledgements

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University of Applied Sciences Hof,

Faculty of Textile and Design

Hochschule für Angewandte Wissenschaften –

Fachhochschule Hof

• Dipl.-Ing. Dana DedinskiDiploma Thesis

• Prof. Michael RauchTextiltechnologie, Verfahrenstechnik der Textilveredlung

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THANK YOU

FOR

YOUR ATTENTION