How to identify Dyestuff mixtures?

Differentiation of Dyestuffs:
Some simple tests can be carried out to find out a dyestuff is a direct, acid or reactive or a
mixture of these things.

Wet filter paper blow test:

If you blow a pinch of dyestuff on dripping wet filter paper (from a short distance):
1. Acid dyes will create specks that do not spread.
2. Direct & reactive dyes will form a colored dispersion.
Dissolution Test:
1. Acid dyes will dissolve only in acid medium.
2. Direct & reactive will dissolve in soft water and form a uniformly colored solution.
Dyed fabric test:
1. Direct dyes weak hydrogen bond - in the presence 5 gpl soap @ 95', dye will strip out
and dye a fresh RFD fabric.
2. Acid dyes in the presence of soap, it will not strip/bleed
3. Reactive dye covalent bond color will not bleed and stain the adjacent rfd.
Pyridine test: P6H5N
1. Direct dye will strip completely.
2. Acid dye will not strip but will strip in acid medium with larger amount of leveling
agent.
3. Reactive dye will not bleed.
Dyeing Test:
1. Direct and reactive only dye cotton.

1. Direct dyes will dye weaker in the presence of higher dosage of soda ash. ( For
example a 3% depth of both, we can identify easily.)
2. Acid dyes will dye protein fibres and stain cotton.
Some More Methods:
1.

Polyester fibers were treated with 200 L of chlorobenzene at 100 C for 60 min. Complete
extraction indicated presence of a disperse dye.
2.
Acrylic fibers were treated with 50:50 formic acid:water (total volume 200 L) at 100 C for 60
min. Complete extraction after this step indicated that a basic dye is present.
3.
Nylon fibers were treated with equal parts of aqueous ammonia, pyridine, and water (66 L
each), heated at 100 C for 60 min.35 Complete extraction indicated presence of an acid dye.
4.
Cotton fibers may be dyed with direct, reactive or vat dyes. The first stage of cotton fiber
extraction used 60:40 pyridine:water using (120 L pyridine, 80 L water) at 100 C for 60 min;
complete extraction indicated a direct dye is present. If incomplete extraction occurred, 200 L
of 1.5% NaOH solution was added, and the plate heated at 100 C for 60 min. A complete
extraction signified that a reactive dye was present. If extraction was still incomplete, a vat dye
may be present. A 200 L volume of reducing agent solution (0.8 g sodium dithionite, 0.5 g of
NaOH, 5.0 mL H2O, 33.0 mL of 1,2-dimethoxy ethane, and 66.0 mL of H2O) was added to the
remaining fiber sample in a 96-well plate, and heated at 100 C for 30 min. When the plate was
placed in a fume hood without the cover, air oxidized the extracted vat dye to water insoluble
pigment with a corresponding color change.

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Saturday, September 24, 2011

Chemical Resist Process - Reactive Printing
Two Methods of Working with Two Different Families of Reactive Dyes

The chemical resist process allows you to control background coloring of printing (and other
methods of direct application) without the need for additional silkscreens and without color
overlays.

The process takes advantage of differing reactivity levels of Vinylsulphone based dyes
(Remazols) and Cibacron F reactive dyes (similar results can be obtained with Vinylsulphone
based dyes (Remazol) and DCT and MCT reactive dyes). Since some colors of dye work more
effectively with this process than others, thorough testing is necessary to achieve predictable
results.

Amount of Chemical Resist

The amount of Chemical Resist that needs to be added to the Cibacron F reactive dyes is
dependent upon the strength of Remazol dyes which will be applied over or under the reactive
dyes (see chart).

Dye Activator Options

The chemical resist process works best with soda ash as the activator in the Cibacron F
reactive dye pastes and Basilen Fixing Agent as the activator in the Remazol dye pastes. It will
work with baking soda as the activator for the Remazols, but not always reliably. (With baking
soda as the activator, it is critical for Remazol dyes to dry slowly; in mid-winter, it may be
necessary to prolong their dampness in the fabric by batching them in plastic for 24 hours).
Method One will also work with the soda soak/batching method for fixing the dyes.

Method One - Remazol Dyes Over Reactive Dyes

1. Mix Cibacron F reactive dye pastes, using the appropriate amount of Chemical Resist
(depending on the strength of the Remazols you intend to use) and soda ash (unless you have
soda soaked the fabric first). Refer to the chart for quantities of Chemical Resist and soda ash.
2. Apply Cibacron F reactive dyes and allow them to dry naturally. (Batch in plastic if using the
soda soak/batching method of activation.)
3. Mix thick Remazol dye pastes, using the appropriate amount of dye activator (see chart).
4. Roll or squeegee Remazol dye(s) over the dry Cibacron F dyes.
5. Allow dyes to dry naturally (unless using the soda soak/batching method for fixing the dyes).
6. Unless you have used Basilen Fixing Agent as the Remazol dye activator, you must
steam the fabric within 1 day of applying the Remazol dyes in order for the chemical
resist process to work. That timing is not necessary with Basilen Fixing Agent as the dye
activator, because it does not begin fixing the dye to the fabric until it is steamed.
7. Wrap fabric in paper, tie, and steam for 8-12 minutes.
8. Wash out excess dye and then boil the fabric for about ten minutes to achieve the full
chemical resist effect. Use a drop of synthrapol in the rinse water and also in the water to be
boiled.
9. The halos which occur around the Cibacron F reactive dye areas will be more or less
apparent, depending on the amount of Chemical Resist used as well as on the strength and
thickness of Remazol dyes you used.

Method Two - Remazol Dyes Under Reactive Dyes

1. Mix thin Remazol dye pastes with the appropriate amount of dye activator (see chart).
2. Apply Remazol dyes as desired. Allow them to dry naturally.
3. Mix Cibacron F reactive dye pastes with the appropriate amounts of Chemical Resist and
soda ash (see chart).
4. Apply Cibacron F reactive dyes. Allow them to dry naturally.
5. Wrap fabric in paper, tie, and steam for 8-12 minutes.
6. Wash out excess dye and then boil the fabric for a few minutes to achieve the full
chemical resist effect. Use a drop of synthrapol in the rinse water and also in the water
to be boiled.
7. Little or no halo effect should occur around reactive dye areas using this method.

Courtesy : patricia williams

Posted by nuchem at 12:22 PM No comments:
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Sunday, June 5, 2011

Nano and Micro Silicone softeners how to differentiate?
The processing of textiles to achieve a particular handle is one of the most important
aspects of finishing technology. Softeners are one of the main compounds in finishing
process and can improve some properties of textiles, depending on the chemical nature,
including soft handle, smoothness, elasticity, hydrophilic, antistatic and soil release
properties. They are classified according to their ionic character and the main classes are:
anionic, cationic, nonionic, amphoteric, reactive and silicone. Macro- and micro-emulsion
silicone softeners are commercial classes of softeners but nano-emulsions are new class of
softeners in textile industry. The purpose of this research was to study the effect of micro
and nano-silicone softeners on different properties of polyester fiber.

Polyester fabrics were first scoured with nonionic detergent and were then treated with three
concentrations (10, 20 and 30 gr/lit) of micro and nano-emulsions of silicones. The drape

length of treated samples with 10 gr/lit of solution was decreased and more decrease was
observed with increase in silicone concentration. Colorimetric properties of softener treated
fabrics were evaluated with a reflectance spectrophotometer. Nano-emulsion silicones
changed a little the surface reflectance of fibers compared to micro-silicone softener.
Increase in weight of all samples was observed which shows the coating of silicones on fiber
surface. Nano-emulsion silicones showed better results on samples treated compared to
micro-emulsion silicones.

1. The abrasion resistance of nano-silicone treated fabric will be more than that of
micro-silicone softener treated fabric.

2. Anti-pilling effect will also be more when compared against micro emulsion treated
fabrics.

3. Under powerful micro-scope one can see, micro emulsions will found to form surface
coating on fibre more than that of nano-emulsions, that will penetrate more to the
core of fibre than that of micro emulsions.
However, I do agree, that there should be some simple test to differentiate between nano
and micro silicone softeners. If anybody knows well, they can share the message in this plat
form.

Posted by nuchem at 12:12 PM No comments:

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Monday, May 9, 2011

Heat Setting
This operation is crucial for fabrics made of synthetic fibres (PE, PA, elastomers), for triacetate, and partly
for PAC fibres (setting), since it grants excellent dimensional stabilization and crease proof properties,
maintained till the fabric is exposed (by air blowing) to temperatures exceeding the heat setting one (after
being treated with water at a temperature above the second order glass transition temperature, i.e. 8085C for acrylics).

Heat setting is carried out on gray fabrics (scarcely applied), on scoured fabrics (frequently applied) and
on dyed fabrics (scarcely applied).

The process grants excellent dimensional stability and good crease-proof properties.

As far as operating conditions are concerned, the fabric must be treated in accurately controlled moisture
and temperature conditions.

Fibre

Min T. C

Max. T. C

Time (in seconds)

Polyester (PE)

170

210

15-50

Polyamide (PA) 6.6

170

210

15-40

Polyamide (PA) 6

160

180

15-40

Triacetate

160

180

15-40

Acrylic (PAC)

160

180-200

15-40

Elastomers

170

180-200

15-40

Machines used: stenters.

Fluctuating temperatures inside the stenter cause a consistent variation of crystallinity in the fibre
structure, which leads to different affinity for dyes.

The moisture in the fibre produces soft hand, but variable moisture percentages in the different fabric
sections create the above mentioned defect (variable crystallinity).

Too low temperatures do not allow a good setting while too high temperatures and too long setting times
cause yellowing (PA and elastic fibres), stiff hand (acrylics), and loss of elasticity (elastic fibres).

The presence of combustion gas (NOx) produces a yellowing of the elastomers.

The heat setting process carried out before scouring could fix the stains on the fabric or make the
scouring process more difficult due to the modification of the lubricating products (cracking with emission
of polluting gas).

Heat setting after dyeing could lead to the sublimation of disperse dyes (if not accurately selected).

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Friday, May 6, 2011

Testing of Vinyl sulphone/ Mono-chlorotriazine Dyestuffs by print strike off method

Although a comparative exhaust dyeing method is always recommended for comparing two
samples of dyestuffs, people in printing industry prefer to make strike off prints to compare the
standard and sample.
Print Paste preparation for strike off:
Materials used

Vinyl Sulphone dyes

H/P type of dyes

Dyestuff

40 grams

40 grams

3-4% Sodium Alginate gel

720 grams

720 grams

Sodium Bicarbonate

30 grams

20 grams

Soda Ash

---

15 grams

Resist Salt

10 grams

10 grams

Urea

100 grams

100 grams

Water

100 grams

95 grams

Total

1000 grams

1000 grams

Method of printing:
On a well mounted RFD fabric on printing table, using the above paste prepared separately for
standard and sample, two strikes off would be printed with the test screens.
After the print, gets dried properly, the fabric will be passed through saturated steam chamber (in
a Star Ager) at 1050C for 10-15 minutes or dry curing chamber at 1500C for 4 to 5 minutes. This
is followed by hot wash, cold wash, neutralization with acetic acid 2gpl and 2 soaping, hot and
cold washes.
Final pH is set at 6 by doing an acetic acid treatment at the end of all washings.

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Saturday, April 23, 2011

Application of disperse dyes on 100% Polyester and its blends with cotton and
viscose
General process sequence for PC blended fabric is:

Recipe:

Disperse dyestuff = x %

Nugen LFT = 0.5 %

Acetic Acid = 1.5 %

Carrier = 0.5%

If the recipe contains a Navy Blue dyestuff, then pH should 4.5 to 5.0 during dyeing,
otherwise navy will tend to exhaust partially and hence unlevel dyeing. (If Formic
Acid is available replace Acetic acid 1.5% with 1.0% of it, it is the most stable acid
at high temperatures rather than Acetic).
Nugen DFT concentration need not be increase more than 0.5%. It is in fact, leveling
and retarding agent; that will impair the depth and fastness.

Dyeing Procedure:

1. Pretreatment:
1. Acetic Acid = 1.5 g/l
2. Nugen DFT = 0.3 g/l
1. Treat at 500C for 10 minutes
2. Dyeing:
1. Add dissolved disperse dye solution at 500C = addition time = 10
minutes

2. Raise the temperature to 1150C @ 20C/minute; at 1150C hold for 10

minutes
3. Raise the temperature to 1350C @0.50C/minute; at 1350C hold for 30 to
45 minutes
4. Cool to 800C and drain
3. Reduction Clearing:
(Alkaline)
1. Caustic Soda = 2 gpl
2. Hydros = 2 gpl
3. Dispersol VLH = 1 gpl
1. Treat at 500C for 20 minutes
2. Cold wash Acetic acid wash with acetic acid 1 gpl 10 minutes.
(Acidic)
4. Cyclonon ECO = 2gpl
5. Acetic Acid = 2 gpl
1.

Treat at 800C for 20 minutes

2. Cold Wash 10 minutes; unload.

Please find below a general process sequence for Polyester Cotton blend:
Process Flow for PC and PV blends:

Some reasons for un-level dyeing:

Highly pH sensitive disperse dyes almost all navy's and blacks

Too much loading

Liquor Circulation problems

Improper heat setting/no heat setting

Too less quantity of Leveling /dispersing agent

Inadequate quantity of Acetic/Formic acid (please check acid concentrationacetic acid is being manufactured from different sources.) pH plays a major
role in disperse dyeing levelness take care.

Other Defects noticed in polyester dyeing:

Moire Effect on PC or PV woven/knitted:

A watered, clouded, or frosted wavy appearance produced upon either woven or
knitted textile fabrics is said to be moir effect.
The moir effect is caused mainly due to the differential shrinkage of polyester and
cotton or viscose at high temperature and high pressure dyeing. This problem can
be avoided by taking proper precautions before and after dyeing.

1. A perfect head setting on pins at a temperature of 200 to 210 0C for 30 to 45

seconds with an over feed of 6 to 8% may be done.
2. In case of PV blends, caustizisation with 10 to 12 0TW of caustic soda at room
temperature may minimize moir effect.
3. Moire effect after dyeing may be corrected either by caustizisation or treating
the fabric with 3 to 5 gpl of carrier at 1300C for 30 minutes in a jet or soft-flow
machine.
4. This can also be corrected by subjecting the fabric to high temperature at
2000C with an over feed of 6 to 7% and redye in HT + HP machine using 10%
of disperse dye recipe for 30 minutes.
Poor Sublimation Fastness:

Some of the disperse dyes tend to crystallize while cooling down the
exhausted bath from 1350C to 800C. 1000C is the most critical temperature at
which some of the red disperse dyes ( C.I.No. 53, 60, 131, 132 and 159) give
problem of crystallization when they are dyed at higher depths and especially
if the dyeing is carried out in hard water. The hardness of water should be
nil for disperse dyeing.

Some of the disperse dyes are very sensitive to metal ions and shade
changes considerably bluer to duller side. Spinning assistants, spinning oils,
alkaline residues and other factors cause crystallization of disperse dyes to
produce dye specks. This problem may be solved by proper pretreatment.

The chromophore of the azo based disperse dyes is reduced and become
soluble when an alkaline reducing agent (caustic & hydros) at 60C thus
promoting poor sublimation and rubbing fastness
Na2SO4 + 2 H2O ------- 2H + 2NaHSO3
(alkaline condition)
-N=N- + 4H -------- -NH2-NH2- (soluble disperse dye)

Azo dye

Use of non-ionic auxiliaries in the dye bath may also tend to aggregate some
of the disperse dyes causing poor sublimation and rubbing fastness.

These problems can be overcome by using the following recipe:

Disperse dye = x %

Acetic acid = 1.0 gpl

Sodium Acetate = 0.5 gpl

Anionic dispersing agent = 1.0 gpl

Disperse dye = x %

Formic acid = 0.35 to 0.5 gpl

Ammonium Sulphate = 1.0 gpl

Anionic dispersing agent = 1.0 gpl

Or

Dye Specks:
Dyeing auxiliaries like carrier, leveling agents (non-ionic) are liable to nullify the
effect and impair the solubilizing effect of dispersing agents thus promoting
aggregation and agglomeration of disperse dyes causing specks.
Also use of non-ionic silicones during final finishing tend to aggregate disperse dye
and reactive dyes; reduces the sublimation /rubbing fastness of the dyed fabric.
Non-ionic products in the form of wetting, leveling and finishing agents may be
curtailed to avoid these problems.

Pilling:
Factors responsible for pilling:
1. Fiber Characteristics such as morphological, chemical and fine structure of
the fiber, fiber length, fineness, strength etc.
2. Yarn Characteristics viz., blend, count, twist, hairiness
3. Fabric Characteristics such as weave, ends and picks etc.
4. Frictional and abrasive force such as linear or rotational rubbing forces
encountered during wear or processing.
Remedies:

Surface treatment: The protruding fibres from the yarn or fabric can be
removed mechanically/chemically or by burning out or cropping, surface
carbonizing, singeing, heat setting etc reduces pilling.

Steaming & cropping: the loose projecting fibres are removed mechanically
by sharp blades from the surface of the fabric to a certain extent and that
helps in reducing pilling.

Surface carbonizing: In this technique, the protruding fibres are burnt or

dissolved with suitable chemicals the nature and the amount of chemicals
used depends on the constituents of the blended fabrics. The fabric is thus
not only free from pilling but also gives surface feel.

Posted by nuchem at 2:09 PM No comments:

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Saturday, April 2, 2011

Disperse Dyes in Printing

Methods of printing with Disperse Dyes a practical over view

Nuchem Dyestuffs P Ltd., (NDPL), suggests the following 3 methods for printing with
disperse dyes. These methods can be used in flat-bed and rotary screen printing machines.

Method-1:
PRINTING - DRYING - BAKING - REDUCTION CLEARING - WASHING OFF

1.

PRINTING
Recipe

Full Thickening

Half
Thickening

Disperse Dyes

X - parts

X parts

Alginate thickener (10% conc)

600 - parts

450 parts

Emulsion thickener

Nil

150 parts

Anti-Reducing Agent (mild

5 parts

5 - parts

Citric Acid

2 parts

2 parts

Wetting Agent

20 parts

20 parts

Add water to make

1000 parts

1000 parts

Oxidizing agent)

2. DRYING on stenter at 100 105C

3. BAKING on Curing machine
-

Temperature

Time

210 0C
60

second

4. REDUCTION CLEARING (RC)

-

NaOH flake

gram / litre

Sodium hydrosulphite

gram / litre

Dispersing agent

gram / litre

Temperature

60 0C

Time

10 minutes

5. WASHING OFF

Method-2:
PRINTING - DRYING - HT STEAM - REDUCTION CLEARING - WASHING OFF
1.

PRINTING
Recipe

Full Thickening

Half
Thickening

Disperse Dyes

X - parts

X parts

Alginate thickener (10% conc)

600 - parts

450 parts

Emulsion thickener

Nil

150 parts

Anti-Reducing Agent (mild

5 parts

5 - parts

Citric Acid

2 parts

2 parts

Wetting Agent

20 parts

20 parts

Add water to make

1000 parts

1000 parts

Oxidizing agent)

2.

DRYING
3.

HIGH TEMPERATURE (HT) STEAM

Temperature

Time

4.

REDUCTION CLEARING (RC)

NaOH flake

gram / litre

Sodium hydrosulphite

gram / litre

Dispersing agent

Temperature

60 0C

Time

10 minutes

5.

WASHING OFF

170 0C
8 minutes

gram / litre

Method 3:
PRINTING
1.

- DRYING

- HP STEAM

- REDUCTION CLEARING

- WASHING OFF

PRINTING
Recipe

Full Thickening

Half
Thickening

Disperse Dyes

X - parts

X parts

Alginate thickener (10% conc)

500 - parts

250 parts

Emulsion thickener

Nil

450 parts

Anti-Reducing Agent (mild

2.5 parts

2.5- parts

Wetting Agent

10 parts

Nil

Add water to make

1000 parts

1000 parts

Oxidizing agent)

2.

DRYING

3.

HIGH PRESSURE (HP) STEAM

Temperature

Time

4.

REDUCTION CLEARING (RC)

NaOH flake

gram / litre

Sodium hydrosulphite

gram / litre

Dispersing agent

gram / litre

Temperature

60 0C

Time

10 minutes

5.

WASHING OFF

Notes:

130 0C
20 minutes

1.

Disperse Dyes

: Nusperse Dyes (Nuchem Disperse Dyes)

2.

Alginate thickener

: Manutex F , etc

3.

Emulsion thickener

: mixture from water , white spirit and emulsifier

4.

Anti reduction

: Matexil PAL , Ludigol , sodium chlorate , etc

5.

Wetting agent for print paste

6.

Dispersing agent

: Matexil WA-KBN , etc

: Matexil DN-VL , Solopol ZB , etc

How to identify Dyestuff mixtures?

Differentiation of Dyestuffs:
Some simple tests can be carried out to find out a dyestuff is a direct, acid or reactive or
a mixture of these things.
Wet filter paper blow test:
If you blow a pinch of dyestuff on dripping wet filter paper (from a short distance):
1. Acid dyes will create specks that do not spread.
2. Direct & reactive dyes will form a colored dispersion.
Dissolution Test:
1. Acid dyes will dissolve only in acid medium.
2. Direct & reactive will dissolve in soft water and form a uniformly colored
solution.
Dyed fabric test:
1. Direct dyes weak hydrogen bond - in the presence 5 gpl soap @ 95', dye will
strip out and dye a fresh RFD fabric.
2. Acid dyes in the presence of soap, it will not strip/bleed
3. Reactive dye covalent bond color will not bleed and stain the adjacent rfd.
Pyridine test: P6H5N
1. Direct dye will strip completely.

2. Acid dye will not strip but will strip in acid medium with larger amount of
leveling agent.
3. Reactive dye will not bleed.
Dyeing Test:
1. Direct and reactive only dye cotton.
1. Direct dyes will dye weaker in the presence of higher dosage of soda ash.
( For example a 3% depth of both, we can identify easily.)
2. Acid dyes will dye protein fibres and stain cotton.
Some More Methods:
1.

Polyester fibers were treated with 200 L of chlorobenzene at 100 C for 60 min.
Complete extraction indicated presence of a disperse dye.
2.
Acrylic fibers were treated with 50:50 formic acid:water (total volume 200 L) at 100
C for 60 min. Complete extraction after this step indicated that a basic dye is present.
3.
Nylon fibers were treated with equal parts of aqueous ammonia, pyridine, and water
(66 L each), heated at 100 C for 60 min.35 Complete extraction indicated presence of
an acid dye.
4.
Cotton fibers may be dyed with direct, reactive or vat dyes. The first stage of cotton
fiber extraction used 60:40 pyridine:water using (120 L pyridine, 80 L water) at 100 C
for 60 min; complete extraction indicated a direct dye is present. If incomplete
extraction occurred, 200 L of 1.5% NaOH solution was added, and the plate heated at
100 C for 60 min. A complete extraction signified that a reactive dye was present. If
extraction was still incomplete, a vat dye may be present. A 200 L volume of reducing
agent solution (0.8 g sodium dithionite, 0.5 g of NaOH, 5.0 mL H2O, 33.0 mL of 1,2dimethoxy ethane, and 66.0 mL of H2O) was added to the remaining fiber sample in a
96-well plate, and heated at 100 C for 30 min. When the plate was placed in a fume
hood without the cover, air oxidized the extracted vat dye to water insoluble pigment
with a corresponding color change.