Note: Descriptions are shown in the official language in which they were submitted.
CA 02049867 2004-07-02
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N-ALKYLPHTHALIMIDE MIXTURES FOR USE AS CARRIERS IN DYEING AND
OPTICAL BRIGHTENING
Low molecular N-alkylphthalimides are useful as carriers in the dyeing or
optical brightening of fibrous material with disperse dyes respectively
disperse optical brighteners and are advantageously employed in the form
of liquid compositions emulsifiable in water. For shipment and storage of
such compositions their stability under various temperature conditions is
of great significance. For their application it is desired that the con-
tent of active subtance in relation to any emulsifiers in the composition
be as high as possible.
It has now been found that certain N-alkylphthalimide mixtures, as defined
below, and which, in particular, are free of other (i.e. of lower and of
higher as well as of differently branched) N-alkylphthalimides are surpri-
singly well emulsifiable, there being obtainable therewith compositions
that remain stable in a very broad temperature range and that are distin-
guished by their outstanding efficiency as carriers.
The invention relates to the N-alkylphthalimide mixtures defined below,
compositions containing such mixtures and their use as carriers.
The invention thus provides an N-alkylphthalimide mixture (P) consisting
essentially of:
(a) N-(n-propyl)-phthalimide
(b) N-(sec.-C4_6-alkyl)-phthalimide
and (c) N-(n-C4-6-alkyl)-phthalimide
wherein the weight ratio (a)/(P) is in the range of 3/100 to 14/100,
the weight ratio (b)/(c) is in the range of 1/10 to 4/1, the
weight ratio (b)/(P) is in the range of 8/100 to 70/100, and the weight,
ratio of (c)/(P) is in the range of 55/100 to 80/100.
As components (b) come principally into consideration N-(butyl-2)-phthal-
imide, N-(pentyl-2)-phthalimide and N-(hexyl-2)-phthalimide, among which
N-(butyl-2)-phthalimide is preferred.
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As components (c) come into consideration N-(n-hexyl)-phthalimide,
N-(n-pentyl)-phthalimide and N-(n-butyl)-phthalimide among which the
latter are preferred, in particular N-(n-butyl)-phthalimide.
The weight ratio (a)/(P) is advantageously in the range of 3/100 to
12/100, in particular 5/100 to 11/100.
The weight ratio (b)/(c) is advantageously in the range of 1/10 to 4/1,
preferably below 2.5/1, more preferably below i/1, in particular in the
range of 1/4 to 1/1.3.
The weight ratio (b)/(P) is advantageously in the range of 8/100 to
70/100, preferably 15/100 to 42/100, most preferably 17/100 to 42/100.
The weight ratio (c)/(P) is advantageously in the range of 55/100 to
80/100, preferably 55/100 to 72/100.
These mixtures (P) may be produced by admixing the single components with
each other or also by synthesis of the imides in the presence of each
other in a manner known per se, e.g. starting from phthalic acid anhydride
or phthalic acid esters and the corresponding amines.
The phthalimides may optionally contain, e.g. due to an incomplete reac-
tion and/or to any secondary reactions, minor portions of carboxy groups
and/or (when starting from phthalic acid anhydride) optionally non-reacted
anhydride, mainly < 5 mole%, in particular < 2 mole% of the total of the
imides. The phthalimides indicated above as (a), (b) and (c) include any
such secondary products.
The mixtures (P) are, in particular, free of lower or higher N-alkylphtha-
limides as well as of differently branched N-alkylphthalimides. A content
of up to 2 % by weight, preferably < 1 % by weight of lower and/or higher
N-alkylphthalimides and/or of up to 5 Z by weight, preferably < 2.5 % by
weight, in particular < 1 % by weight, of differently branched N-alkyl-
phthalimides in each of (a), (b) and (c), eventually deriving from impuri-
ties in the respective starting materials, may still be tolerated and is
comprised in the definitions of (a), (b) and (c).
CA 02049867 2002-10-09
_ 3 _
The mixtures (P) of the invention find their use as carriers. For this
purpose they are advantageously combined with an emulsifier system (E), in
order to facilitate their distribution in water in emulsified form. The
invention thus further provides compositions (U) comprising (P) and (E)
but which are free of other phthalimides.
As emulsifier systems (E) are suitable in general emulsifiers (e) which
are preferably at least in part anionic and are optionally combined with
emulsifying assistants (h).
The emulsifier system (E) comprises preferably at least one emulsifier
(e); (e) preferably is
(el) at least one anionic emulsifier
optionally in admixture with
(e2) at least one non-ionic emulsifier.
As (el) come, in general, into consideration any anionic emulsifiers, e.g.
as named in the German Patent DE 29 41 763 C2 (~ USP 4 252 534) under (b)
or as described in the patents DE 23 06 104 C3 (a USP 3 874 891), DE
32 46 383 C2 (~ USP 4 516 979) and DE 32 47 400 C2 (a USP 4 464 180).
Preferably (el) is
(ell) an at least partially carboxymethylated, phosphated or sulphated
polyalkyleneglycolether of a hydrocarbon-mono- or -polyolcontaining
on average at least 10 carbon atoms per hydroxy group of the mono or
polyol,
(e12) a sulphate, phosphate or carboxymethylated derivative of a sorbitan
or glycerine fatty acid ester, wherein the fatty radical contains 12
to 24 carbon atoms or of a polyalkyleneglycolether thereof,
or
(e13) a C12_24-hydrocarbon sulphonic acid,
CA 02049867 2002-10-09
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the carboxy, phosphate or sulpho groups optionally being in salt form,
or a mixture of such surfactants.
As (e2) come, in general, into consideration any non-ionic emulsifiers,
e.g. oxyalkylation products as named in German Patent DE 29 41 763 C2
(a USP 4 252 534) under (e) or also oxyalkylation products of higher mole-
cular polyols, in particular oxyalkylated novolakes or mixed novolakes as
are described, e.g. in German Patents DE 23 06 104 C3 USP 3 874 891),
DE 32 46 383 C2 (a USP 4 516 979) and DE 32 47 400 C2 USP 4 464 180) as
intermediate products.
Preferably (e2) is
(eZl) a polyalkyleneglycolether of a hydrocarbon-mono- or -polyol, con-
taining on average at least 10 carbon atoms per hydroxy group of the
mono- or polyol
or
(e22) a sorbitan or glycerine fatty acid ester, in which the fatty radical
contains 12 to 24 carbon atoms, or a polyalkyleneglycolether thereof
or a mixture of such surfactants.
The polyalkyleneglycolethers in (ell), (e21), (el2) and (e22) are advan-
tageously polyethyleneglycolethers, which may optionally comprise a minor
proportion of propyleneoxy units and/or styreneoxy units; preferably the
polyalkyleneglycolethers are exclusively polyethyleneglycolethers.
As (e21) there may be mentioned, in particular, the following polyal-
kyleneglycolethers:
(ezll) polyalkyleneglycolethers of fatty alcohols with 12 to 24 carbon
atoms,
(e212) polyalkyleneglycolethers of mono- or dialkylphenols with 12 to 24,
2049867
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preferably 14 to 18 carbon atoms in the mono- or dialkylphenyl
radical
and
(e213) polyalkyleneglycolethers of simple or oligomeric methylene bridge-
-containing novolake condensates of mono- or dialkylphenols, that
contain each 10 to 24, preferably 12 to 18 carbon atoms per mole-
cule of mono- or dialkylphenol and optionally lower alkyl phenols
(e.g. cresols) with formaldehyde.
The degree of oxyethylation is advantageously in the range of 4 to 50,
preferably 4 to 20 moles of ethyleneoxide per val of alkylphenol and/or
fatty alcohol.
As (e22) come, in particular, into consideration the following:
(e221) mono- or diesters of sorbitan or glycerine, wherein the ester-for-
ming fatty acid radicals may be saturated or also unsaturated, in
particular monoethylenically unsaturated (e.g. lauroyl, palmitoyl,
myristoyl, oleoyl, stearoyl or arachidoyl), principally sorbitan
monooleate, sorbitan monostearate, sorbitan monolaurate and par-
tially hydrolyzed fatty acid triglycerides,
(e222) polyethyleneglycolethers of (e221) with 4 to 40 ethyleneoxy units,
on average, per hydroxy group of the starting material,
and
(e223) polyethylenglycolethers of ricinol group-containing fatty acid
glycerides, in particular triglycerides, preferably addition
products of 8 to 50 moles of ethyleneoxide to 1 mole of ricinol
group-containing triglyceride.
As (eli) come preferably into consideration the carboxymethylated, phos-
phated or sulphated derivatives of the corresponding surfactants named
under (eZl) above, in particular of (e211), (e212) and (e213)=
As (e12) come preferably into consideration the corresponding sulphated,
phosphated or carboxymethylated derivatives of the products named under
2049867
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(e22), in particular of (e221), (e222) and (e223).
As (e13) come preferably into consideration alkylbenzenesulphonic acids,
principally dodecylbenzene sulphonic acid.
Among the carboxymethylated, phosphated or sulphated derivatives in (ell)
and (e12) the sulphates are preferred.
The carboxy, sulpho and phosphato groups may be in the form of the free
acids or their salts, in particular as -COOM, -S03M respectively
-0P03(M)21 wherein M signifies hydrogen or a cation, preferably an alkali
metal cation (in particular lithium, sodium or potassium), an equivalent
of an alkaline earth metal cation (in particular magnesium or calcium) or
an ammonium cation [in particular unsubstituted ammonium, mono-, di- or
tri-(C2-3-alkanol)ammonium or C3-6-alkylammonium]. In the preferred
sulphates M is preferably NHq*.
The weight ratio (e2)/(el) advantageously is in the range of from 0/100 to
90/10, preferably 0/100 to 40/60. Where (e22) and/or a polyalkylene gly-
col ether of the monoalcohol (eZl) are employed in admixture with (e13),
(e12) or a carboxymethylated, phosphated or sulphated polyalkyleneglycol-
ether of a monoalcohol (ell), the weight ratio (eZ)/(el) is advantageously
in the range of 20/80 to 90/10.
According to a preferred feature of the invention there are employed such
surfactants (e) which are obtainable by sulphating, phosphating or carbo-
xymethylating the mentioned polyalkyleneglycolethers of the polyols, in
particular of the novolake kind condensates as indicated above under
(e213), preferably only in part, in particular to 10 to 70 mole%, most
preferably to 12 to 25 mole%. These partially anionically modified deri-
vatives of the products (e213) are indicatd in the following as (e3). The
particularly preferred addition products of 4 to 20 moles of ethyleneoxide
to 1 val of oligomeric, methylene bridge-containing condensation product
of alkylphenol and formaldehyde, sulphated to 12 to 25 mole% are indicatd
in the following as (e31).
Where as (e), (e3) or (e31) there are employed corresponding partially
anionically modified polyalkyleneglycolethers of hydrocarbon polyols, in
2049867
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particular of oligomeric condensates as described above, these are advan-
tageously such as shown in German Patents DE 23 06 104 C3 (=_ USP
3 874 891), DE 32 46 383 C2 (= USP 4 516 979) and DE 32 47 400 C2 (=_ USP
4 464 180), with the respective formulae (I) therein and as described in
their examples, whereby the partially anionically modified products - in
particular (e31) - due to the statistical distribution of the anionic
groups may optionally be present in admixture with non-anionically modi-
fied starting material (e213).
The emulsifier system (E) respectively the composition (U) of the inven-
tion, advantageously contains, along with emulsifier (e) respectively
along with (P) + (e),
(h) at least one lipophilic, non-ionic emulsifying assistant.
As (h) come advantageously into consideration oil-soluble polar products,
preferably oil-soluble fatty acid-(C1_4-alkyl)esters with 12 to 24 carbon
atoms, in the fatty acid radical or a mixture of such esters. As fatty
acid radicals in these esters come in particular into consideration those
mentioned above, as well as acyl radicals of technical fatty acids, in
particular of tallow fatty acid, of technical oleic acid, of coconut fatty
acid or of fisch-oil acids or refined technical fatty acids, preferably
such with 16 to 24 carbon atoms. As ester-forming C1_q-alkyl radicals in
(h) the lower molecular ones are preferred, in particular ethyl and,
before all, methyl.
The emulsifier system (E) may consist of (e) alone or preferably of a
mixture of (e) with (h); where (h) is present, the weight ratio (e)/(h) is
advantageously in the range of 95/5 to 40/60, preferably 80/20 to 40/60.
The weight ratio (B)/[(P) + (E)] is advantageously in the range of 3/100
to 20/100, preferably 5/100 to 20/100. If (E) resp. the composition (U)
of the invention contains no (h) the weight ratio of (e) to the total
composition advantageously is in the range of 6/100 to 20/100, preferably
10/100 to 20/100. If (h) is present [be it introduced in admixture with
(P) or with (e) or both or separately], the content of (e) may be consi-
derably reduced, advantageously so that the weight ratio (e)/[(P) + (E)]
in the compositions (U) containing (P), (e) and (h) is in the range of
2049867
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4/100 to 12/100, preferably - in particular at preferred ratios (e)/(h)
and in particular when employing the above-mentioned preferred surface-
-active derivatives (e31) of the novolake kind condensates - in the range
of 4/100 to 10/100 or even 4/100 to 9/100.
The compositions (U) of the invention comprise the mixtures (P) and the
emulsifier systems (E) and may be handled in this form. A base may be
added, if desired, in order to transform any carboxy groups and/or non-
-reacted anhydrides, at least in part, into the corresponding salt form,
so that the pH of the composition diluted with water to 1% by weight of
[(P) + (E) + optionally base] is advantageously in the range of 3 to 8,
preferably 4 to 7. As bases for the adjustment of this pH-values are
suitable, in general, conventional additives, in particular alkali metal
hydroxides, carbonates or bicarbonates or preferably aliphatic amines,
principally CZ-3-alkanolamines, in particular mono-, di- or triethanol-
amine or mono-, di- or triisopropanolamine and/or alkylamines, advan-
tageously C3_6-alkylamines, in particular, such in which the alkyl
radicals correspond to those of the employed N-alkylphthalimides.
The compositions (U) of the invention are, in particular, such that con-
sist essentially of (P) and (E) and optionally additional base, as indi-
cated above. They are, in general, free-flowing to viscous liquids and
are distinguished by their stability in shipment and storage, namely as
well under conditions of heat as of frost, e.g. at temperatures below
-10 C or above +40 C.
The phthalimide mixtures (P) of the inveniton, in particular in the form
of their (E)-containing compositions (U) as described above, serve as
assistants for the treatment of fibrous substrates with substances which
are in the form of aqueous dispersions; in particular, they serve as
carriers for the dyeing of fibrous material with disperse dyes or any
other dyes that are applied in the form of their aqueous dispersions or
for the optical brightening of fibrous material with disperse optical
brighteners. The compositions (U) of the invention are readily dilutable
with water; before use they may, if desired, be diluted with water to
stock emulsions [e.g. containing 5 to 40 % by weight, preferably 10 to
30 % by weight of (U)] or they may also be added into the dyestuff or
brightener stock dispersions or even directly into the liquors. The
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aqueous stock emulsions respectively dispersions are distinguished by
their storage stability and may be employed unchanged after several days;
if they should separate or sediment after longer storage they may readily
be emulsified or dispersed again by simple stirring. They are, in parti-
cular, suitable as carriers for the dyeing of synthetic or semi-synthetic
fibrous materials, principally fibrous material of polyester, polyamide or
cellulose acetates and their mixtures, as well as mixtures with natural
fibres (in particular cotton or wool), e.g. cotton/polyester or wool/poly-
ester, or with elastomeric fibres (e.g. polyurethanes). The substrates to
be treated may be in any form as conventionally employed for the dyeing or
optical brightening with the assistance of carriers, e.g. as loose fibres,
yarns, filaments, skeins, cross-wound spools, woven or knitted goods, non-
-wovens, felts, carpets, tuftings as well as half-ready-made or ready-made
goods. The application may take place according to methods known per se,
in particular from aqueous medium, advantageously at pH 3 to 8, e.g.
according to exhaust methods, under normal pressure advantageously at
temperatures > 95 C, or under superatmospheric pressure at temperatures
above 100 C, in particular in the temperature range from 102 to 140 C,
e.g. under HT-conditions advantageously at 102 to 110 C, or under rapid
dyeing conditions at higher temperatures (polyester fibres preferably at
temperatures in the range of 110 to 140 C, polyamide fibres preferably at
temperatures of 105 to 115 C, cellulose acetate fibres preferably at 105
to 125 C), or by impregnation methods, e.g. by padding, dipping, spraying,
foam application or printing (with printing pastes or printing inks) under
conventional impregnation conditions (e.g. at temperatures in the range of
15 to 50 C) and subsequent fixation, preferably at increased temperature,
in particular above 100 C, e.g. by steaming, preferably at 102 to 120 C,
or thermosoling (e.g. at temperatures in the range of 130 to 220 C; for
polyamides preferably in the range of 130 to 160 C and for polyester
preferably in the range of 150 to 220 C).
Due to the surprinsingly good emulsifiability of the mixtures (P) of the
invention in the presence of (E), there may be achieved, even employing
very small proportions of emulsifier systems (E), in particular of emulsi-
fier (e), before all emulsifiers (e31) of the above-mentioned novolake
surfactant kind, optimal effects, there taking place an outstanding and
very quick distribution of (P) in finest particles into the aqueous sys-
tem, so that its activity (in particular carrier activity) is immediately
2049867
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and best displayed and available in the dyeing process resp. brightening
process. If desired, other conventional dyeing assistants may be admixed
with the compositions (U) of the invention (in particular at latest in the
aqueous treatment liquor) e.g. further carriers (Q) that are compatible
with N-alkylphthalimides, in particular alkyl-substituted aromatics and
their mixtures, compounds of the aromatic or alkylaromatic carboxylic
ester series, halogen substituted aromatics, compounds of the optionally
alkyl- and/or hydroxy-substituted biphenyl, diphenylether or naphtholether
series. The additional use of other N-alkylphthalimides is here expressi-
vely not recommended. If (P) is employed together with (0) or blended
therewith, it is preferred that (P) outweighs. Further additives that may
be employed together with the carrier compositions (U) of the invention
are e.g. defoamers; if, as surfactants (E) in the compositions (U) of the
invention, there are employed the above-mentioned novolake kind surfac-
tants (e3), particularly (e31), the additional use of a defoamer is in
general not necessary, since these bestow to the composition already an
outstanding lack of foam, so that such compositions may be well employed,
even without addition of defoamers also for processes in which foam would
else appear in a disturbing amount (e.g. in dye-jet machines, for the
dyeing of cross-wound spools, in the jigger or in the winch-beck). For
the process of the invention there may be employed any conventional
disperse dyes and disperse brighteners as they are defined e.g. in the
"Colour Index" under the heading "Disperse Dyes" and, in part, under the
heading "Fluorescent Optical Brighteners" and which in their conventional
commercial forms usually contain formulation additions (mainly dispersing
agents), or also other dyes that, at least provisionally, contain no hy-
drosolubilizing substituents as e.g. sulphur dyes, vat dyes or developers.
With particular advantage the compositions (U) of the invention may be
employed also in aqueous printing pastes and inks (e.g. for the printing
of carpets or knitted goods) since they are capable or displaying their
optimal efficiency, even in relatively concentrated treatment
formulations.
By employing the carrier compositions (U) of the invention the properties
of the employed dyes and brighteners can be optimally displayed and there
can be obtained very regular dyeings in light to deep tones even with dye
mixtures (e.g. trichromatic mixtures) in good penetration of the substra-
2049867
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tes. There may be obtained dyeings with optimum fastnesses.
The required resp. optimum quantity of the composition (U) of the inven-
tion to be employed with respect to the substrate or to the liquor may
vary broadly, depending in the amount and kind of the dye or optical
brightener, on the kind and structure of the substrate, on the employed
treatment method and liquor-to-goods ratio and may be determined by means
of a few preliminary tests. Mainly the compositions (U) of the invention
are employed in concentrations of 0.3 to 25 g/l, referred to the aqueous
treatment liquor; at a liquor to goods ratio of 5:1 to 40:1, in particular
20:1, advantageously at concentrations of 0.4 to 12 g/l, preferably 0.5 to
4 g/1.
In the following examples the parts and percentages are by weight; the
temperatures are indicated in degrees Celsius. The dyes are employed in
commercial form and their concentration in percent is referred to the
substrates.
The employed N-alkylphthalimide mixtures (P) are listed in the following
Table 1.
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Table 1
Mixture Y by weight of N-R-phthalimide in (P)
(P)
R n-propyl (a) R sec.-butyl (b) R n-butyl (c)
P1 3 60 37
P2 3 55 42
P3 3 42 55
P4 3 17 80
P5 5 37 58
P6 6 31 63
P7 8 32 60
P8 8 27 65
P9 8 22 70
P10 10 32 58
Pil 10 30 60
P12 10 22 68
P13 12 60 28
P14 12 28 60
P15 12 18 70
P16 12 8 80
The employed emulsifier systems (E) are listed in the following Table 2,
wherein w, x and y are emulsifiers (e) and z is an emulsifier assistant
(h).
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Table 2
Emulsifier- % by weight in (E)
system
(E) w x y z
El 95 - - 5
E2 40 - - 60
E3 50 - - 50
E4 80 - - 20
E5 100 - - -
E6 - 90 10 -
E7 - 50 50 -
E8 - 20 80 -
E9 - 25 25 50
w novolake surfactant "compound 6" according to DE 32 46 383 C2 [i.e.
"compound 6" of Table (b) of USP 4 516 979)
x addition product of 32 moles of ethyleneoxide to 1 mole of castor oil
y = monoethanolammonium dodecylbenzenesulphonate
z s C16_2o-fatty acid methylester.
The employed carrier compositions (U) are set up in the following Table 3.
2049807
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Table 3
Carrier- Phthalimide mixture (P) Emulsifier system (E)
composition
(U)
U1 P1 (83) E3 (17)
U2 P2 (83) E3 (17)
U3 P3 (83) E3 (17)
U4 P4 (80) E2 (20)
U5 P4 (83) E3 (17)
U6 P4 (90) E6 (10)
U7 P4 (85) E7 (15)
U8 P5 (83) E3 (17)
U9 P6 (83) E3 (17)
U10 P7 (84) E3 (16)
Ull P7 (82) E4 (18)
U12 P7 (82) E5 (18)
U13 P7 (84) E9 (16)
U14 P8 (83) E3 (17)
U15 P9 (83) E3 (17)
U16 P10 (83) E3 (17)
U17 P11 (84) E3 (16)
U18 P11 (82) E4 (18)
U19 P11 (85) E5 (15)
U20 P11 (84) E9 (16)
U21 P12 (83) E3 (17)
U22 P13 (83) E3 (17)
U23 P13 (88) E8 (12)
U24 P14 (83) E3 (17)
U25 P15 (83) E3 (17)
U26 P16 (95) El (5)
U27 P16 (83) E3 (17)
If required monoethanolamime or diisopropanolamine is added to the above
carrier compositions (U) (pH of the aqueous diluted composition of 1 9;
concentration = 4 to 6).
204"9867
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Example 1
A texturized polyester (diolene loft) jersey is padded on a padding
machine at ambient temperature (= 20 C), to a pick-up of 80 Y with an
aqueous liquor containing per 1000 parts
25 parts of the dye C.I. Disperse Yellow 64 (structure no. 47023)
and 10 parts of the assistant U20.
The pH is set to 4.5 with acetic acid.
The textile material is intermediately dried on a pin stenter during 120
seconds at 110 C and then thermosoled during 90 seconds at 195 C. After
reduction clearance there is obtained a level, intense yellow dyeing of
good general fastnesses.
Example 2
A polyester/cotton blended fabric (blend ratio 67:33) is padded at ambient
temperature with an aqueous liquor (pick-up 60 X). The aqueous liquor
contains per 1000 parts:
25 parts of the red dye C.I. Vat Red 10 (structure no. 67000)
parts of the red dye C.I. Disperse Red 202
and 10 parts of the composition U16.
The pH is set to 4.5 with acetic acid.
The impregnated blended fabric is dried during 60 seconds at 110 C and
then treated with hot air at 210 C during 60 seconds. The vat dye is
developed at 60 C during 30 seconds using the following aqueous liquor
(liquor-to-goods ratio 5:1) that contains (per 1000 parts):
parts of 30 % sodium hydroxide solution
8 parts of sodium dithionite
and 3 parts of an anionic dispersing agent (sodium salt of a13-naphtha-
lene sulphonic acid/formaldehyde condensation product, commercially
204986r1
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available.
After soaping at the boil during 20 minutes rinsing and drying there is
obtained a fabric in which the polyester portion and the cotton portion
are dyed red nearly tone-in-tone. The dyeings have at a good colour depth
a level appearance and good general fastnesses.
Example 3
In an HT-dyeing machine a liquor of 130 C is flown through bobbins of tex-
turized polyester yarns at a liquor-to-goods ratio of 10:1. The liquor
contains demineralized water (set to pH 4.5 with acetic acid), 1.5 g/l of
the assistant U17 and the following dyes:
1) 0.46 % of the dye of formula
-0
Br
0~ H _ ( a) r
2) 0.52 Y, of the dye of formula
H0
0
c OH
/ \p
3) 0.17 % of the mixture of the dyes of formulae (Y1) and (YZ) (in even
portions)
CA 02049867 2002-10-09
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HO H---CH2 OH HO H--CH2 OH
o= 0 - 0-- 0
\ /HZ
HO -- (ri) H2N H (r2)
\ /
The flow rate throught the bobbins is of 40 1/kg per minute. After 30
minutes of treatment at 130 C the liquor is cooled and drained off and the
goods are cleared under reducing conditions. There is obtained a perfect-
ly level brown dyeing of full yield. During the dyeing foam-formation is
minimal.
Example 4
TM TM
A polyester fabric (type DACRON) is dyed in a GASTON-COUNTY dye-jet
machine with 0.5 X of the dye Foron Rubine SE-GFL with addition of 2 g/l
of ammonium sulphate and 2 g/l of the product U1'7 at pH 5.0 (adjusted with
formic acid). The liquor-to-goods ratio is 20:1. Dyeing is started at
20 C; during 10 minutes the dye-bath is heated to 70 C. After 20 minutes
at 130 C the dyeing is concluded. There is obtained a level dyed fabric.
Example 5
Example 4 is repeated with the difference that instead of Foron Rubine
TM TM
SE-GFL there is employed Foron Brilliant Blue S-R. There is obtained a
level and very brilliant blue dyeing of the 1'.abric.
Example 6
parts of cleaned polyester fibrous material are given in a high tempera-
ture dyeing machine (GASTON COUNTY dye-jet machine) into 100 parts of a
dyeing liquor heated at 70 C, that contains 0.1 parts of a commercial pre-
paration (with dispersing agent) of the dye C.I. Disperse Blue 148, 0.2
parts of the composition U23 and 2 parts of ammonium sulphate and the pH
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of which is set to 5 with formic acid. The dyeing machine is closed, the
temperature is raised during 20 minutes to 130 C and maintained for 20
minutes at this temperature. After cooling the treated substrate is taken
out from the dye bath, rinsed, soaped, rinsed again and dried. There is
obtained a completely level, deep blue dyeing of very good fastness
properties.
Example 7
parts of polyester fibre fabric are dyed in a closed dyeing vessel with
400 parts of an aqueous dyeing liquor, that contains 0.05 parts of the
commercial form of the dye C.I. Disperse Red 73, 0.7 parts of the composi-
tion U15 and 3 parts of ammonium sulphate and the pH of which is set to 5
with formic acid, by heating during 30 minutes from 60 C to 130 C inner
temperature and dyeing during 30 minutes at this temperature. After
cooling the dyed fabric is taken out from the bath, rinsed, rinsed again
and dried. There is obtained a perfectly level ruby red dyeing of excel-
lent fastness properties.
Example 8
100 parts of a polyester fibre fabric are given into 4000 parts of an
aqueous dye bath which is heated to 40 C and contains 0.2 parts of C.I.
Disperse Blue 73, 6 parts of the composition U21 and 8 parts of ammonium
sulphate and the pH of which is set to 5 with formic acid. This bath is
heated during 30 minutes to 97 C and maintained for 1 hour at this tempe-
rature. After washing, rinsing and drying there is obtained a level blue
penetration dyed fabric with very good fastness properties.
Example 9
A polyester ribbon (satin) of unstretched (1:3.2) and normally stretched
(1:3.66) yarn is given into an aqueous liquor (liquor to goods ratio 40:1)
heated to 60 C and which contains 3.2 % of the dye C.I. Disperse Blue 87,
2 g/1 of ammonium sulphate, 4 g/l of citric acid and 2 g/1 of the assis-
tant U17, then heated during 45 minutes to 130 C, dyed during 60 minutes
and then cooled. The treated substrate is rinsed and dried. In this way
there is obtained a perfectly level, turquoise blue dyed ribbon.
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Example 10
100 parts of a yarn consisting of 50Y, of wool and 50% of polyethylene-
terephthalate are dyed in 4000 parts of an aqueous bath that contains
2 g/1 of ammonium sulphate and the pH of which is set to 5.5 with acetic
acid and further contains the following additions:
0.6 parts of the dye of formula
ON=N_..O__NN_O_OB
( S)
and 5 parts of the assistant U17.
The yarn is given into the bath at 60 C, then the bath is heated during 45
minutes to 106 C and dyeing is carried out during 60 minutes at this tem-
perature. After cooling the yarn is rinsed and dried. There is obtained
a level yellow dyeing in which the polyester portion is dyed substantially
more than the wool portion.
Analogously as the carrier compositions U15, U16, U20, U21 and U23 there
are employed in the above examples 1, 2, 5, 6, 7 and 8 each of the other
carrier compositions U1 to U27. Analogously as the carrier composition
U17 there are employed in Example 3 the carrier compositions U1-U5,
U8-U12, U14-U19, U21, U22 and U24-U27.
In the above Examples the carrier compositions (U) may be added directly
into the liquors or may previously be diluted to aqueous stock solutions,
produced e.g. by diluting of 10 parts of each of the compositions U1-U27
with 90 parts of demineralized water at ambient temperature.
