Note: Descriptions are shown in the official language in which they were submitted.
~ ~ 7 ~ 3~'~
The invention relates to aqueous preparations of
dyestuffs or optical brighte~ers insoluble to difficultly
soluble in water, to processes for the production of
these preparations~ to the use thereof for the
preparation of aqueous printing pastes, as well as to
the use of these for the printing of carrier materials
and to their use in transfer printing, and also to the
use of these preparations for the dyeing or optical
brightening of textile materials, and to the printed
carrier materials as well as to the textile material
printed or optically brightened by means of these
preparations in the transfer printing process, or dyed,
printed or optically brightened by means of these
preparations in the dyeing or prin~ing process.
Commercial forms of dyestuffs or optical brighteners
insoluble to difficultly soluble in water are kno~n both
as liquid preparations and as powder preparations. The
latter have the disadvantage that they have to be
firstly dispersed in water before application; the former
have the disadvantage that they re~uire large am~unts
of dispersing agent, in most cases over 30 per cent by
weighL, and contain very little dyestuff, of the order
of about 20 per cent by weight, or very little optical
- 2 -
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:
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~ 7 ~ 30 ~
brightener, of the order of about 5 to 25 per cent by
weight. There was therefore a need, particularly with
regard to the production of printing pastes for
printing of carrier materials and to the use of these
S in transfer printing, to produce a commercial form
of, in pa-ticular, dyestuffs which is directly ready ``
for use, and which contains on the one hand a relatively
small amount of dispersing agent and on the other hand
a large amount of dyestuff; and which, furthermore,
has a lo~ electrolyte content, in order to thus render
possible a more general application, for the preparation
of printi.ng pastes, also of thickening ag.ents that are
sensitive to electrolytes.
Aque~us preparations of dyestuffs or optical
brighteners insoluble to difficultly soluble in water
have now been found which do not have the disadvantages
mentioneu. These new aqueous preparations have a low
content of dispersing agents and of electrolytes, but
a high CGIcentration of dyestuff ur optical brightener
as defined, are stable, finely dispersed a~d flowable,
and contain dyestuffs insoluble .o difficultly soluble
in water, especially disperse dyestuffs or vat dyestuffs,
or optical brighteners insoluble to difficultly soluble
;
.
~7 ~ ~V ~
in water, of which th~ particle size is smaller than
lO~u, particularly smaller than 2 ~. These preparations
are characterised in that they preferably conta~n
not less than 10 per cent by weight, especially 20 to
30 per cent by weight, of water, at least 30 per cent
by weight, especially 35 to 65 per cent by weight,
preferably 40 to 60 per cent by weight, of a finely
dispersed dyestuff or optical brightener insoluble
to difficultly soluble in water, and a mixture consisting
of at most 10 per cent by weight, especially 0.1 to 5
per cent by weight, of an anion-active dispersing agent9
at most 5 per cent by weight, especially 1 to 3 per
cent by weight, of a nonionic dispersing agent and a~
most 35 per cent by weight, particularly 5 to 20 per
cent by weight, of a hydrotropic agent, optionally
together with further additives.
Suitable dyestuffs insoluble to difficultly soluble
in water ~re, in particular, disperse dyestuffs. Mention
may be made, for e~ample, of the foundation dyestuffs
of Celliton ~ and Palanil ~ dyestuffs of BASF, of
Cibacet ~ and Terasil ~ dyestuffs of Ciba-Geigy, of
Artisil ~ and Foron ~ dyestuffs of Sandoz, and of
Duranol ~ dyestuffs of ICI, to mention just a few.
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Various chemical classes of dyestuffs are applicable,
such as nitro dyestuffs, amino-ketone dyestuffs,
ketoneimine dyestuffs, methine dyestuffs, nitro-
diphenylamine dyestuffs, quinoline dyestuffs, amino- ~:
naphthoquinone dyestuffs, coumarin dyestuffs and, in
particular, anthraquinone dyestuffs and azo dyestuffs,
such as monoazo and disazo dyestuffs.
Further suitable dyestuffs are vat dyestuffs.
Typical representatives belong, for example, to the
following chemical classes: indigoid dyestuffs;
anthraquinone vat dyestuffs, including also the anthrimide
dyestuffs, anthraquinoneacridone dyestuffs, anthraquinone-
thiazole dyestuffs as well as anthraquinonylazine
dyestuffs and, finally, derivatives of condensed ring
lS systems; naphthalene dyestuffs; perylene dyestuffs;
sulphurised carbazoles and quinone dyestuffs.
It is understood that the type of dyestuff within
this given definition is to a great extent governed by
the field of application for which these aqueous
dyestuff preparations according to the invention are
intended. If they are to be employed, for example, for
the produ~tion of printing pastes and subsequent use
in transfer printing, then the employed dyestuffs
-- 5
.
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insoluble to difficultly soluble in water will be those,
within the limits of the given definitiong which are
suitable for the transfer printing process, especially
disperse dyestuffs which are converted at atmospheric
pressure, at between 150 and 220~C, to the extent of
at least 60% in less than 60 seconds into the vapour
state, ~hich are stable to heat and which can be
transferred undecomposed.
Such disperse dyestuffs are, for example, the
monoazo dyestuffs of the formula
OH
N - N -
~O-Y X
wherein X and Y each represent an alkyl radical having
1 to 4 carbon atoms,
OH
~2 ~C-NH
N = N - C
l il ~ C~N
H3~ ~ CH3.
and
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N02 '~'ÇO-CH3
_N = N - CH
. ~ ~ CO-NH
`H3C
and, in particular, the quinophthalone dyestuff of the
formula
~01~ 0
OH
- and the anthraquinone dyestuffs of the formulae
, O NH-æ
O 'NH-Z
(Z c alkyl having 1 to 4 carbon atoms),
~3~ ~
~ ~R = alkyl or aryl)
O NH2
(R = Hal)
O OH
-- 7 --
- - ~ . ~ . ,
,
~L~7~30~
O ~H2
(~ ~ 1 r
O NI~2
(Rl = allcyl having 3 to 4 carbon atoms),
O N~ICH
O NHCH3
O NH
OC~13
.
~ NH
~2 crl
O NH-A
(A - alkyl or aryl), as well as brominated or chlorinated
l,5-diamino-4,8-dihydroxyanthraquinones.
Also suitable however are reactive disperse dyestuffs
that can be used in the transfer printing process, such
-- 8 --
. ~ , . .
~ ~ 7 6 3 0 4
as the dyestuffs of the formulae
H0
Cl-CH2-CO-NH ~--N = N ~
. H3
and
c~3
0 N ~ N = N ~ N'C2H5
2 ~C2H40-CO CH2 Cl
A further important factor is the choice of dyestuffs
S in the case of dyestuff combinations, for only those
dyestuffs that are similar in their transfer charactPristics
should be combined in the transfer 2rinting process.
Suitable optical brighteners insoluble to difficultly
soluble in water are, in particular, the following
classes of compounds wi.h their nonionic substitution
products:
. ~ . .
.. ..
,. ... ..
.," .,
~ ~ ~ 7 ~ 3 ~ ~
a) pyrazolines such as, for example, 1-(4-sulphamoyl-
phenyl)-3-(4-chlorophenyl)-pyrazoline or 1-(4-
methylsulphonylphenyl)-3-(4~chlorophenyl)-pyrazoline;
b) coumarins such as ~-phenyl-7-(3-methylpyrazol-1-yl)-
S coumarin, 3-phenyl~7-(3-phenyl-4-methyl-1,2,3-
triazoL-2-yl)-coumarin or 3-(4-chloro-1,2-pyrazol-1-yl)-
7~(3-phenyl-4-mPthyl-1,2,3-triazol-2-yl)-coumarin;
c) mono~ and bis-benzoxazoles such as naphthaline-1,4-
bis-benzoxazoie-(2), thiophene-2,5-bis-benæoxazole-(2),
ethylene-1,2-bis-(5-methylbenzoxazole)-(2~, 2-(4-
cyanostyryl)-596-dimethylbenzoxazole, 4-(597-dimethyl-
benzoxazol-2-yl)-4'-phenylstilbene;
d) benzimidazoles such as uran-2~5-bis-(N-methyl-
benzimidazole)-(2);
e) aryltriazoles such as 2-(4-chloro-2'-cyano-stilben-4'-yl)-
naphtho-(1'~2':4,5)-1,2,3-triazole;
f) naphthoxazoles such as 2-(~ styryl)-naphtho-(1,2-d)-
oxazole;
g) pyrenes such as 2-pyrenyl-4,6-dimethoxy-1,395-triazine;
h) naphthalimides such as 4-me~hoxy-N-methylnaph~halimide
or 4,5-diethoxy-N-methylnaphthalimide;
- 10 - .
- . .. . ~
. . .. . . ...
, .
: , , .
~ ~7~ 3
i) bis-ethylelle-aryls such as 1,4-bis-(2-cyanostyryl~
ben~ene, 4,4'-bis-(2-methoxystyryl-~)-biphenyl.
Furthermore, it is possible to use in the aqueous
brightener prepara~îons also mixtur~s of different types
of optical brighteners within the limits as defined.
Suitable anion-active dispersing agents are, e.g.:
sulphated primary or secondary, purely aliphatic alcohols
of which the alkyl chain contains 8 to 18 carbon atoms,
e.g. sodium lauryl sulphate, potassium-a-methyl stearyl
sulphate, sodium tridecyl sulphate, sodium oleyl sulphate,
potassium stearyl sulphate, or the sodium salts of coconut
oil alcohol sulphates; sulphated, unsaturated higher fatty
acids or fatty acid esters, such a~ oleic acid, elaidic
acid or ricinoleic acid, or lower alkyl esters thereof,
e.g. ethyl es~er, propyl ester or butyl ester, and the oils
containing such fatty acids, such as olive oil, castor oil
or rape oil; addition products of 1 to 20 moles of ethylene
oxide with fatty amines, fatty acids or aliphatic alcohols
having 8 to 20 carbon atoms in the alkyl chain, which
addition products are converted into an acid ester by
means of an organic dicarboxylic acid such as maleic acid,
malonic acid or succinic acid, preferably however with
an inorganic polybasic acid such as o-phosphoric acid or,
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in particu. ar, sul.phuric a~.;.d, for example s-lch a~dition
products with stearylamir.e, oieyl~nine, stearic acid,
oleic acid, lauryl alcohol, myristyl alcohol, stearyl
alcohol or oleyl alcohol, such as the ammonium salt of
S sulphated lauryl alcohol triglycol ether, or of 1 to 5
moles of ~ hylene oxide with alkylphenols, such as the
acid sulphuric acid ester of the addition product of
2 moles of ethylene oxide with 1 mole of p-nonylphenol,
the acid sulphuric acid ester o~ the addition product of
1.5 moles of ethylene oxide with 1 mole of p-tert.oc~yl-
phenol, the acid sulphuric acid ester of the addition
product of 5 moles of ethylene oxide with 1 mole o~
p-nonylphenol, the acid phosphoric acid ester of the
addition product of 2 moles of ethylene oxide with 1 mole
of p-nonylphenol, the acid maleic acid ester of the
addition product of 2 moles of ethylene oxide with 1 mole
of p-nonylphenol; sulphated esterified polyoxy compounds,
for example sulphated, partially esterified polyvalent
alcohols, such as the sodium salt of the sulphated mono-
2~ ~lyceride of palmitic acid; instead of sulphates, it isalso possible to use esters with o.her polyvalent mineral
acids, e.g~ phosphates; primary and secondary alkyl-
sulphonates of which the alkyl chain contains 8 to 20
- 12 -
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.:- ~ . , ' ';
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- ~7 ~
carbon 2~0ms, e.g. ammonium decylsulphonate, sodium
dodecylsulphorlate~ sodium hexadecanesulphonate and sodium
stearylsulphonate; alkylarylsulphonates, such as alkyl-
benzenesu'lphonate having a straight-chain or branched-chain
alkyl chain containing at least 7 carbon atoms, e.gO
3 odium doi'ecylbenzellesulphonate, 1,3,5,7-tetramethyl-
octylbenzenesulphonate, sodi~ octadecylb~nzenesulphonate;
such as alkylnaphthalenesulphonates, ~or example, sodium-l-
isopropylnaphthalene-2-sulphonate; sodium dibuty'l-
naphthalenesulphonate; or such as dinaphthylmethane-
sulphonates', for example the disodium salt of di-
(6-sulpho.aphthyl-2)-methane; sulphonates of polycarboxylic
acid esters, for example sodium dioctyl sulphosuccinate,
sodium dihexylsulphophthalate; the sodium, potassium,
ammonium, N-alkyl-, N-hydroxyalkyl-, N-alkoxyalkyl- or
N-cyclohexylammonium or hydrazinium and morpholinium
salts of fatty acids having 10 to 20 carbon atoms, which
are designated as soaps~ such as lauric, palmitic,
stearic acid, or oleic acid of na~hthenic acids, of resinic
acids, such as abietic acidj e.g. the so-called rosin
soap; es~ers of polyalcohols, p~rticularly mono- or
~iglycerides of fatty acids having 12 to 18 carbon atoms,
e.g. the monoglycerides of lauric 9 stearic, palmitic or
- 13 -
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: ,. :
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oleic acid, as well as the fatty acid esters of sugar
aleohols, sueh as sorbitol, sorbitans and saccharose,
for example sorbitan monolaurate (Span 20), sorbitan
palmitate (Span 40), sorbitan stearate (Span 60),
sorbitan oleat~ (Span 80), sorbitan sesquiolate,
sorbitan ~rioleate (~pan 85), and the hydroxye~hyla~ion
products thereof (~een).
Al~ion-active dispersing agents which have proved
particularly favourable are condensation products of
aromatic sulphonic acids with formaldehyde, such as
eondensation products from formaldehyde and naphthalene
sulphonie aeids, or from formaldehyde~ naphthalene-
sulphonic acid and benzenesulphonic acid, or a condensation
product from crude cresol, formaldehyde and naphthalene-
sulphonic aeid, and lignin sulphorates and polyphosphates.It is also possible to Pmploy mixtures of anionic
dispersing agents, such as, e.g., a mixture of the
eondensat on product from erude eresol, formaldehyde
and naphthalenesulphonic acid with lignin sulphonate.
Normally, the anionic disperslng agents are in the
form of their alkali salts, their ammonium salts or
their water-soluble amine salts. It is advantageous to use
qualities having a low eontent of foreign electrolytes.
- 14 -
f~
: :: : . . :
,..
' . :~ ', -
~7~30~
Nonionic dispersing agen~s are, for example:
addition products of, e..g., 5 to 50 moles of alkylene
oxides 5 especia].ly ethylene oxide (with some ethylene
oxide units being able to be replaced by substituted
epoxides such as styrene oxide and/or propylene oxide),
with high_r fatty acids, or with saturated or unsaturated
alcohols, mercaptans or amines having 8 to 20 carbon
atoms, or with alkylphenols or alkylthiophenols of which
the alkyl radicals contain at least 7 carbon atoms;
reaction products from higher-molecular fatty acids
and hydroxyalkylamines; these can be prepared, for
example, ~rom higher-molecular fatty acids, preferably
such ones having about 8 to ~0 carbon atom~, e.g.
caprylic ~cid, stearic acid, oleic acid and, in particular,
lS from the mixture of acids embraced by the collective
term "coconut oil fatty acid", and from hydroxyalkyl-
amines such as triethanolamine or preferably diethanol-
amine, as well as from mixtures of these amines, with the
reaction ~eing so performed that the molecular quantity
ratio between hydroxyalkylamine and fatty acid is greater
than 1, for example 2:1. Such con~?ounds are described in
the American Patent ~pecification No. 2,089,212;
condensation products of alkylene oxide, especially
- 15 -
... . . . .
. : : ... . . :
.. . ..
. . ,
3~
ethylene oxide, with some ethylene oxide units being
able to be replaced by substituted epoxides, such as
styrene oxide and/or propylene o~ide.
Fatty alcohol polyglycol ethers have proved
particularly advantageous, especially those having more
than 20 moles of ethylene oxide, such as cetyl-stearyl
alcohol etherified with 25 moles of ethylene oxide,
stearyl-oleyl alcohol etheri~ied with 80 moles of
ethylene oxide and oleyl alcohol etherified with 20 to
80 moles ~f ethylene oxide. Furthermore, phenol ethers
such as p-nonylphenol etherified with 9 moles of
ethylene oxide, ricinoleic acid ester having lS moles
of ethylene oxide and hydroabietyl alcohol etherified
with ~5 moles of ethylene oxide are also very suitable.
Thesæ nonionic dispersing agents advantageously have
a low electrolyte content. Mixtures of such agents are
possible and in some cases have synergetic effects.
By hydrotropic agents used in the aqueous
preparations according to the invention are meant those
agents ca~able of converting the dispersion of the dyestuffs
or optical bri~hteners insoluble to difficultly soluble
in water into a stable deflocculated form, without
- 16 -
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~, : , : . . . . .. ~
- ;, -,~
, ,
~ ~ 7 ~ 3~ ~
in the process a chemical reaction occurring between
the dyestuff or the optical brightener and the
hydrotropic substance. These compounds should be water-
soluble. Suitable substances having these properties
are, for example: hydrotropic salts such as the sodium
salt of benzoic acid, the sodium salt of benzene-
sulphonic acid, the sodium salt of p-toluenesulphonic
acid or the sodium salt of N-benzylsulphanilic acid.
Compounds which have proved particularly advantageous
in this connectiolt are, however, ritrogen-containing
compounds, such as urea and derivatives thereof, for
example dimethylurea or guanidine chloride, or acid amides
such as acetamide and propionamide and derivatives
thereof, especially N-methylacetamideO
With the application accordi.g to the invention of
the hydrotropic substance in combination with dispersions
of the dyestuffs or optical brighteners as defined, a
stabilisa~ion of the deflocculated dispersion is obtained
without any actual dissolving of the dyestuffs or
optical brighteners occurring.
By virtue of this combination according to the
invention, namely of the anion-active and nonionic
dispersinO agent together with the hydrotropic agent
- 17 -
. _ _ - ; , . . . :
- , . . . . ..
, .. .. ... .
: . ; - -
. ~ . . ..
31~
in the given amounts, it is possible to obtain aqueous
preparations which have on the one hand a low c~ntent
of dispersing agent and, on the other hand, a high
content~of dyestuff or of optical brightener, and
which are characterised in particular by their stability
both in the hot state and in the cold state in a
temperature range of between about minus 10C and
plus 60C; by a storage-stability of several months;
by free flowability; by their finely dispersed form;
and by their low viscosity in the range of about 10
to lO00 c~/20C.
In cons`equence of the high propor~ion by weight of
dyestuff or optical brightener, the aqueous preparations
according to the invention are very compact and provide
a saving in space. A reduction of the space required
for storage and dispatch and in transport is therefore
ensured.
If desired or required, these preparations can
contain further additives for improving properties, such
as hygroscopic agents, e.g. glycols or sorbitols;
antifrost agents, e.g. ethylene glycol or monopropylene
glycol; antimicrobics; fungicides, e.g. aqueous
formalin solution; antifoaming agents and agents improving
- 18 -
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:: ., ", : ,
. . : ;
. .. : . .:
- . : ., . :
.: , . : . , ,; ,
:, .. ,::
. :. ,,: :
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viscosity .
As a result of the presence of about 10% of sorbitol,
there can moreover be obtained a fully satis~actory
redispersibility of the completely dried-out paste.
It is obvious that in the case of brightener
preparations there are used only such anionic and
nonionic dispersing agents and hydrotropic agents
which have no noticeably disadvantageous effects on
the fluorescence of the brighteners (e.g. so-called
quenching ~ffects). Furthermore, on subsequent
applicaticn in 'Foulardtherm' (hot padding) processes,
these auxiliaries must be able to withstand the short
exposure to heat at 150 to 220C without yellowing.
By virtue of their high content of dyestuff or
optical brightener, these preparations are greatly
superior to the liquid preparations hitherto available
commercially~ since, on account of their smailer content
of dispersing agents and extenders~ they can be processed
into low-viscous printing inks having an adequate
concentration of dyestuff or of oD~ical brightener. In
the printing on paper using solvent-free, purely aqueous
printing processes, by means of roller-printing, Flexo-
- 19 -
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,. . . . .
, : . :, . .
- : :.: . , ;
. . ~ .
:,
.
1 ~ 7 ~ 3 0 ~
printing and, in particular, rotary-screen-printing
machines, highly concentrated preparation systems having
a low content of dispersing agents are required. since
paper, compared with textile materials, has a clearly
reduced absorption capacity for printing inks, the recipes
suitable for direct printing on ~extiles, especially in
the case o deep shades, camlot be used.
The new aqueous preparations are produced, for
example, by a process in which the dyestuff or optical
brightener as defined is mixed and ground in water with
at least one of the mentioned anion-active and/or
nonionic dispersing agents, an operation which is
carried out, e.g., in a ball mill or sand mill, with
the remaining constituents being added before, during or
even after the grinding process, so that a preparation
having a particle size smaller than 10 Ju, especially
smaller than 2 ~, is obtained.
The new aqueous dyestuff preparations can be used,
advantageously after dilution with water, for the dyeing
2Q or printin~ of textile materials by the continuous or
discontinuous method of operation. Depending on the
dyestufs used in the preparations, the widest variety
o textile materials can be dyed or printed therewith,
- 20 -
.. ....
. . . ~ ..
... ..
., ' .
:
~L~7630~
such as polyester or cellulose triacetate materials
or mixtures of fibres by application of preparations
containing disperse dyestuf~s.
In the preparation also of printing pastes for
S traditional textile printing, it is of advantage
to employ preparations having the lowest possible
content of d~spersing agent, since the disperse dyestuffs
at present available contain large amounts of dispersing
agent~ wh-ch have to be washed ou~ after fixing o~
the dyestuff and thus unnecessarily contaminate the
waste water.
Since the preparations according to the present
invention have an electrolyte content that is low
compared with that of commercial preparations of
disperse dyestuffs, the thickeners used for the production
of the said printing pastes can be sensitive to
- elPctrolytes. In this connection, thickeners in particular
having a polyacrylic base have proved especially valuable.
A preferred possibility of application is moreover
that these dyestuff preparations ran be used, with the
employment of thickeners~ for the production of printing
pastes having an aqueous base or a water-in-oil-emulsion
base, which printing pastes are used for the printing of
. . . : ~ , ;
..
.. . . . ... .
- ~' ' - .. :' . . ,
... .. . .
, ~, . .. .
:, . .... . . .. .
. '. . .
: , .
. . ..
1~7~3~
carrier materials which, in their turn, can be used
in the transfer printing process on textile materials~
The carrier materials that are printed with such
printing pastes are known, and consist advantageously
of a flexible sheet material that is preferably
dim.ensionally stable, such as a strip, band or sheet,
preferably having a smooth surface. These carrier
materials must be stable to heat, and they are made of
the most varied types of materials, particularly
non-textile materials, such as metal, e.g. an aluminium
or steel sheet; or they consist of a continuous strip
o~ stainless steel, plastics or paper, preferably of a
clean, non-lacquered cellulose parchment paper, which is
optio~ally coated with a film of vinyl resin, ethyl-
cellulose, polyurethane resin or Teflon.~
me optionally ~iltered printing pastes or printing
inks are applied to the carrier material, in places or
over the whole surface, by, for example, spraying,
coating or, advantageously, printing. There can also be
applied to the ~rrier material a multicoloured pattern,
or the carrier material can be printed with a ground
shade and thereafter successively with identical or
~Trademark for a tetra~luoroethylene fluorocarbon resin.
,., . . :
.. . . .
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'
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7~36~
different d~si~ns. After application of the printing
paste to the carrier material? this is dried~ e.g.
with the aid of a warm flow of air or by infra-red
irradiation.
S The carrier materials can be printed also on both
sides, whereby it is possible to select different
colours and/pr designs for the two sides~ In order to
avoid the use of a pr;nting machine, the printing
pastes can be sprayed onto the ca~-rier materials by
means of, for example, a spray gun. Particularly
interestlng effects are obtained when simultaneously
more than one shade is printed or sprayed on the carrier
material. Specific designs can be obtained, e.g., by
the use of stencils, or artistic designs can be applied
by brush. If the carrier m2teri~ is printed, then the
most diverse printing processes may be employed, such as
high-pressure processes (e.g. letter-press printing,
flexographic printing), gravure printing (e.g. roller
printing), screen printing (e.g. rotary printing or
film printing) or electrostatic yrinting processes.
The transfer is effected in the usual ma~ner by the
action of heat. For this purpose, the treated carrier
materials are brought into contact with the materials
- 23 ~
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, ,.. :. ' ~ - ,, .,,
~; ' ' ' . , ' . .
~ :.. . . . .
: :. :.... ~
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to be printed, especially textile materials, and are
held at about 120 to 210C until the defined dyestuffs
applied to the carrier material have been transferred
to the textile material. As 2 rule, 5 to 60 seconds
S are sufficient to achieve this.
The action of heat can be applied by various known
methods, for example by passage over a hot heating
cylinder, by passage through a tunnel-shaped heating
zone, or by means of a heated roller, advantageously
together with a pressure-exerting, heated or unheated
counter roller, or by means of a hot calender, or with
the`aid of a heated plate, optionally under vacuum,
which devices are preheated to the required temperature
-by steam, oil, infra-red irradiation or microwaves,
lS or which are located in a preheated heating chamber.
After completion of the heat treatmen~, the printed
material is separated from the carrier. The material
requires no aftertreatment~ neither a steam treatment to
fix the dyestuff, nor a washing to improve the fastness
properties.
The new aqueous optical brightener preparations
are used, preferably and advantageously after dilution
- 2~ - ;;
'' ' "' ''' '"';' " ~ '
. .
~ .~
, ' ." 1,. " ,' '' '
~ 7 ~3~ ~
with water, for ~he optical brightening of textile
materials by, e~g., the exhaust process, high-
temperature exhaust process and 'Forlardtherm' process.
Further suitable dispersing agents or other auxiliaries
can optionally be added for stabilisation of the liquor
and/or or obtainment of carrier effects.
The widest variety of textile materials are suitable
such as polyester materials, polyamide, polyacrylo-
nitrile, cellulose acetate and cellulose triacetate,
and these materials can be in the most diverse stages
of processing. It is moreover possible for these
preparations to be used for the production of printing
pastes, which are employed either for conventional
brightening of, in particular 9 textile materials, or for
printing of carrier materials, such as especially paper,
which in their turn are used in the transfer printing
process on textile materials.
A further application for the optical brigh~ener
preparations according to the invention is, finally,
in spinning-solution brightening.
The following examples illustrate the invention
without limiting ;ts scope to them. IPar~s' denote parts by
~eight, and temperatur~s are given in degrees Centigrade.
- 25 -
'` ' ":'''"' ~
: ~ . : : .: . ~, .. ..
. ~' ' ' ., ' ~ ' :; ,
,, ,: ' ' : ~ ::.
,, . :~ ~. ':
'I j,' '' .~. ., ' : : ;', ~ ',: ` '
' ';, ~' ::. ~ ::
~ ~ 7 ~
A Production of ~he preparations
.
Example 1
500 par~s of the coarse crystalline dry dyestuff
of the formula
O NH2
~ .~'
O OH
are slowly introduced, with intensive stirring (Dissolver
or Lodig2-Mischer (mixers)), into a pre~prepared
solution of 25 parts of an anion-active dispersing agent
(sodium salt of naphthalene sulphonic acid condensed
with formaldehyde), 10 parts of a fatty alcohol polyglycol
ether as nonionic dispersing agent (cetyl/stearyl alcohol
etherified with 25 moles of ethylene oxide), 10 parts
of a 35% aqueous formalin solution, 100 parts of 1,2-
propylene glycol as antifrost agent and 118 parts of
urea, as hydrotropic stabilising agent, and the whole is
lS then homogenised for about 1 hour and deaerated.
This 55% dyestuff mixture is ~hen ground in a sand ;;
mill, or preferably in a closed ball mill (bead mill),
by means of Ottawa sand and Siliquarzit balls (1 mm
diameter), respectively, for about 10 hours at a temper-
ature of 20 to 50. After this time there is obtained a
- 26
.. . , . ... . . .... , . . . . . ... ... . :: ... .. . .
.:, .
- . ... .
. .
,
~ ~7 ~ 3~ ~
dispersion of which an overwhelming majority of particles
are smaller than 5 ~. The finely ground dispersion is
subsequently diluted to give a dyestuff content of
50% (yield: 1000 parts) by the addition of a further
~Q parts of water, which if necessary contains an
amount (to be determined beforehand) of carboxymethyl-
cellulose as thickening agent, in order to bring the
final viscosity into the ideal range of 500 to 1000 cP
~Brookfield viscosimeter; 30 r.p.m.).
The free-flowing aqueous preparation remains completely
unchanged even throughout a storage time of several
months, and withstands without impairment temperatures
of -15 to +40.
`If, instead of the dyestuff, the anion-active
dispersing agent, the nonionic dispersing agent and
the hydrotropic agent given in the above example, there
are used identical parts of the constituents shown in the
following Table I, with otherwise the same procedure,
then likewise there are obtained storage-stable, free-
flowing, aqueous dyestuff preparations having analogousproperties, of whieh the dyestuff content and respective
grinding time are governed by the dyestuff concerned, and
are between 40 and 60 per cent by weight and 5 to 10 hours,
respectively. - 27 -
- 1 . . ,
.. . ..
,~, : ;; . ".. ~ .
, . .. .... .
- , . . , .:....... . . :,.:
: .
., ~ .: :- .
. . . . . . . .
~Q~3~
. ~ - ~ ';
l o ~ ~
/ \ ~ ~ .~
Z o=~ o ~W
_ . . .
~s~ Q ~ P 3 0 0 ~ o ~ ¦P
p~ ~_ O ~ o 5 P ~ ~ ¦~
r n' ~ O ,; P,~ ~ ~- n
~Do PrD 8~ ~ D P
~ a ~ D'~ Z~
.
, " , ,
,,
:
~, ~..... ' . ' :
- ' ' ~ ,,
~ n 0~ ~P'
~ lpJ~
l o-~o ~ o~
~:
~,ro ~ y
~)
w~
-- - o p ~ ~
';cl o 3, rC 3 - ~ c ~ ~ P' ~-- ~ ~n ,.
P ~ C p ~ 5 o ; ~, ¦
-- I .. _ . I . __ _
O ~' ~ ~v ~ tD 1~ rr O rt ô o ~ I ~ Z
C~ n ~ ~ ~ , o
O--~ ~ Y o :~ ~n ~ I ~ r'
- 5v~ ~ Y ~ . tD 1--o ~ _ ~
n o O ~ ~ ~_X H~ O ~ o r
-- __ _.. _ ,.____
~ ~ C ~ ~D
~ :r 3' o
(D ~,
. ~
.__ . . . _ _
- 29 -
.. :,.. .. : . . -
. . ,.:
.: , :...
- ` '' :'' : .
: : ~ ~ : ,
,: .
, :, :.,: -
1~7~
,- - o . ~ g
___ ~ .._ . ____ . 5
o--~ o I ~ 3
y ¦ O ~ 0 I ~ ~ C ~'
~nO
.__ ._ . r~
~ 3 0 - 3 ~ o a c,~ o ~ ~ o c o ,- o ~ 3 3 ~ g __ .
~_ O ~) r7 = ~ 5~ ~ C ~- o 3 ~ 3
~ _ r~ O ~ g ~ o ~ n 3, n-- ~ ~ 2 r r ¦
E., 5 3 ',r- rr o~ ~, ~, rt o 3~ ~, 5 0~ 1n ~o, ~1 ~ ~ .I P
n ¦ n ~1 ~ C ~ ' I ~ 2 ~ ~ I ~ r~
__ I n C~
3 5 ~ P~ ¦ ~D g g
- ~
'. , : , :
'`' ,:' " '~. ;'~ ~
,
', ~
~ ~ 7 ~ 3
Example 12
500 parts of the dried and pulverised press cake
of dichloro-indanthrone are stirred into a solution of
130 parts of urea, 10 parts of sodium dinaphthylmethane
sulphonate, 20 parts of a condensation product of
stearyl/cetyl alcohol with 25 moles of ethylene oxide,
in 100 parts of monopropylene glycol and 240 parts of
water, and the whole is ground, with the addition of
2000 part~ of glass balls of 1 mm diameter, until the
particle size is essentially about 1 to 2 microns. The
preparation is then separated from the balls.
There is obtained a free-flowing, s~orage-stable
dyestuff preparation.
~xample 13
S00 parts of the crude dyestuff of the formula
N~ ~N~ ~ N
~C'
'~ .
- : . - -- ... . ........
.,
;,
~ ~ 7 ~ 3~ ~
are ground together with a solution of lO parts of
a condensation product of naphthalenesulphonic acid
and formaldehyde, 20 parts of the reaction product of
p-nonylphenol and 9 moles of ethylene oxide, 130 parts
S of urea, lO0 parts of ethylene glycol and 370 parts
o water with 2000 parts of sand until the particle
size is around 1 to 2 microns, and the sand is then
removed.
There is obtained a pourable stable dyestuff
preparation.
Example 1~
480 parts of the coarse crystalline dry dyestuff
of the fo~mula
~ '
H "
are slowly introduced, with intensive stirring (Dissol.ver
1$ or Lodigc~Mischer (mixers)), into a pre-prepared solution
of 24 parts of an anion-activz dispersing agent (sodium
naphthalene sulphonate condensed with formaldehyde),
lO parts of a fatty alcohol polyglycol ether as a
nonionic dispersing agent (cetyl/stearyl alcohol etherified
- 32 ~
~ . ' ~" '",,; " ~', ';, . ' ,
'~ .
~ 3 ~ ~
with 25 moles of ethylene oxide), 10 parts of 35%
aqueous formalin solution, 100 parts of 1,2~propylene
glycol as an antifrost agent and 124 parts of urea,
as a hydrotropic stabilising agent, in 172 parts of
water, and the whole is homogenised for about 1 hour
and deaerated.
The approx. 52% dyestuff mixture is then ground
in a sand mill, or preferably in a closed ball mill,
91q55
1-~ by means of Ottawa sand and ~ {~ t~ bàlls (1 mm
diameter), respectively, for about 10 hours at a
temperature of 20 to 50. After this time there is
obtained a dispersion of which the overwhelming majority
of particles are smaller than 5 ,u. The finely ground
dispersion is subsequently diluted to give a dyestuff
content _f 48% (yield: lOOQ parts) by the addition of
a further 80 parts of water which; if necessary, contains
an amount (to be determined beforehand) of car~oxymethyl-
cellulose as a thickening agent, in order to bring the
final viscosity into the ideal range of 500 to 1000 cP
(Brookfield viscosimeter; 30 r.p.m.). The free-flowing
aqueous preparation remains completely unchanged even
after a storage time of several months, and withstands
without impairment temperatures of -15 to -~40.
' ': ~ . ; ' ' :
" " ' ' . .: ' .':
'': ~: ' , . . ,' ~
.: :' ` '' :, .. . . , ; :
' ' : ,,.' . ,: ,
~ 3
Exame~
.
400 parts of the coarse crystalline dry dyestuff
of the formula
O ~H
~ ~ N
are slowly introduced, with intensive stirring (Dissolver
or Lodige-Mischer tmixers]), into a pre-prepared solu~ion "
of 20 par~s of an anion-active dispersing agent (sodium
naphthalene sulphonate ~ondensed with formaldehyde),
20 parts of a fatty alcohol polyglycol ether as a
nonionic`dispersing agent (cetyl/stearyl alcohol etherified
with 25 moles of ethylene oxide), 10 parts of 35% aqueous
formalin solution, 100 parts of 192-propylene glycol as an
antifrost agent and 150 parts of urea~ as a hydrotropic
stabilising agent, in 190 parts of water, and the whole
i~ then homogenised for about 1 hour and deaerated.
This 45% dyestuff mixture is subsequently ground in
a sand mill, or preferably in a closed ball mill, by means
of Otta~A7a sand and Siliquarzit balls (1 mm diameter),
respectively, for about 10 hours at a temperature of 20
to 50. After this time there is obtained a dispersion
- 34 -
.. , .. . ....... ~.~ .. .. ............. , ........ ,.. , . .. .. ..... .. " .. ~,
~ ~ 7 ~ 3~ ~
of which an overwhelming majority of particles are
smaller than 5 ~. The finely ground dispersion is
diluted to give a final dyestuff content of 40%
(-- 1000 parts) by the addition of a further 110 parts
of water containing if necessary an amount (to be
determined beforehand) of carboxymethylcellulose as a
thickening a~ent, in order to bring the final viscosity
into the ideal range of 500 to 1000 cP (Brookfield
viscosi~eter; 30 r.p.m.). The free-flowing aqueous
preparation remains completely un~hanged even ater
a storage time of several months, and withstands
without impairment temperatures of -15 to ~40.
Example 16
482 parts of the coarse crystalline dry dyestuf
of the formula o NH-CH3
~
0 -CH3
are slow]y introduced, with intensive stirrîng (Dissolver
or Lodige-Mischer [mixers]), intc a pre-prepared solution
of 20 parts of an anion-active dispersing agent (sodium
naphthalene sulphonate condensed with formaldehyde), 15
- 35 -
:- : .' ! '
:- ' . . . ' ':'
~' '. ' ' ' , . .
~'. ' . ' . :
.,' ' ' .
: '. , ' ' . , .
,~' ' ;. ' :'.: ' ' '
::: ' ' : ,, ' , :
. . .
~763C~4
parts of a fatty alcohol polyglycol ether as a nonionic
dispersing agent (cetyl/stearyl alcohol etherified with
25 moles of ethylene oxide), 10 parts of 35% aqueous ;~
formalin solution, 100 parts of 1,2-propylene glycol as an
antifrost agent and 120 parts of urea, as a hydrotropic sta-
bilising agent, in 145 parts of water~ and the whole is then
homogenised for about 1 hour and deaerat~d.
This 54% dyestuff mixture is then ground in a sand
mill, or preferably in a closed ball milI, by means of
Ottawa s~nd and Siliquarzit balls (1 mm diameter),
respectively, for about 10 hours at a temperature of
20 to 50. After this time there is obtained a dispersion
of which the overwhelming majority of particles are smaller
,than 5 ~. The finely ground dispersion is diluted to give
the fin~l dyestuff content of 48.2% by the addition
of a further 108 parts of water containing if necessary
an amount (to be determined beforehand) of carboxymethyl
cellulose as a thickening agent, in order to thus bring
the final viscosity into the ideal range of 500 to 1000 cP
~Brookfield viscosimeter; 30 r.p.m.). The ree-flowing
aqueous preparation remains completely unchanged even
after a storage time of several months, and withstands
without impairment temperatures of -15 to ~40.
- 36 -
. _._.. ~ ._ .. _ .
~ .
.: , ` ': '
.
., , ~ . . ': ~ '"' ' ' '' '
~6~7630~
Example 17
150 parts of a yellow dispersion according to
Example 14,
~50 parts o a red dispersion according to
Example 1,
S 300 parts of a blue dispersioll according to
Example 15, and
200 parts of a blue dispersion according to
Example 16
are homogenised in a stirring vessel.
There are obtained 1000 parts of a black formulation
having a viscosity in the range of 500 to 1000 cP
(Brookfield viscosimeter; 30 r.p.m.).
The free-flowing. highly concentrated aqweous paste
remains completely unchanged even after a storage time
of several months, and withstands without impairment
temperatures of -15 to ~40.
- 37 -
.. , .. . ... . , . . , .. ,, . . .. . . . ... .. , ... , ,.,~ ,,
.. .- ., :
:: ; :,
,, , ~ . - ,,;
. ~ .
,: ::: . . -
~ ~ 7 6 ~ 4
E~ample 18 ~:
445 parts of the coarse crystalline dry dyestuff
of the formula
O N~l
` Jl ~H- ~
are slowly introduced~ with thorough stirring (Dissolver
or Lodige-Mischer [mixers~), into a pre-prepared solution
of 10 parts of an anion-active dispersing agent (sodium
naphthalene sulphonate condensed with formaldehyde), 20
parts of a fatty alcohol polyglycol ether as a nonionic
dispersing agent (cetyl/stearyl alcohol etherified with
25 moles of ethylene oxide), 10 parts of 35% aqueous
formalin solution, 100 parts of 1,2-propylene glycol as a~
antifrost agent and 137 parts of urea as a hydrotropic
stabilising agent in 205 parts of water, and the whole
is then homogenised for about 1 hour and deaerated.
lS This 48% dyestuff mixture is then ground in a sand
mill, or preferably in a closed ball mill, by means of
Ottawa sand or Siliquarzit balls ~1 mm diameter) for
about 10 hours at a temperature of 20 to 50. There is
obtained after this time a dispersion of which an
- 3~ -
.. . ~,,, , .. ,., , .. . .. . ...... . ._
.. :. .. ..
.:
. ,~ ... . ..
. . . :.: :
~ ~ 7 ~ 3~ ~
overwheming majorlty of particles are smaller than
5 ~. The finely ground dispersion is diluted to give
a inal dyestuff content of 44.5% (= 1000 parts) by
the ad~ition of a further 73 parts of water containing
if necessary an amount (to be determined beforehand) of
carboxymethylcellulose as a thickening agent, in order
to thus bring the final viscosity into the ideal range
o~ 500 to 1000 cP (Brookfield viscosimeter; 30 r.p.m.).
The free-flowing aqueous preparation remains completely
unchanged even after a storage time of several months,
and withstands without impairment temperatures of
-15 to ~40.
- 39 -
: `: ' ' '
.. ' , ' '' ' ''., 1 ' ~;
~: . ' .: - ,
: . ' '
1~763~
Example 19
415 parts of the coarse crystalline dry dyestuff
of the formula o NH
f 3
O N~12
are slowly introduced, wi`th thorough stirring (Dissolver
or Lodige-Mischer [mixers]), into a pre-prepared solution
of 5 parts of an anion-active dispersing agent (sodium
naphthalene sulpllonate condensed with formaldehyde),
20 parts of a fatty alcohol polyglycol e~her as a nonionic
dispersing agent (cetyl/stearyl alcohol etherified with
25 moles of ethylene oxide), 10 par~:s of 35% aqueous
formalin solution, 100 parts of 1,2-propylene glycol as an
antifrost agent and 150 parts of urea as a hydrotropic
stabilising agent in 222 parts of water, and the whole is
homogenised for about 1 hour and deaerated.
This 45% dyestuff mixture is subsequently ground
in a sand mill, or preferably in a closed ball mill~ by
g I~S5
A means of Ottawa sand and SiliquarK~ balls (1 mm diameter),
respectively, for about 10 hours at a temperature of 20
to 50. There is obtained after this time a dispersion
of which an overwhelming majority of particles are smaller
- 40 --
' '`,
, ,, , ,'
, ~ . ' ',
' ' ,.,., ...,., ,,.,.. .. .'. " , ' . .. ., '....
.
~t763~
than 5 ~1. The finely ground dispersion is diluted to
give a final dyestuff content of 41.5~/o (= 1000 parts)
by the addition of a further 78 parts of water containing
if necessary an amount (to be determined beforehand) of
S carbox~nethylcellulose as a thickening agent, in order
to thus bring the final viscosity into the ideal
range of 500 to 1000 cP (Brookfield viscosimeter; 30 r.p.m.).
The free flowing aqueous preparation remains completely
unchanged even after a storage time of several months,
and withstands without impairment temperatures of -15
to ~40.
- 41 -
:;:... , , .: ,
.. ..
~ ~ ~ 6 3~ ~
~3~
500 parts of the pure dry active substance of the
optical`brightener of the formula
` ~ ~c ~Lc~
are slowly introduced, with vigorous stirring, into a
solution of 17 parts of an anion active dispersing agent
(ormaldehyde condensed with sodiUm naphthalene
sulphonate~ and 125 parts of urea, as the hydro~ropic
agent, in 230 par~s of water and 50 parts of monopropylene
glycol, and the whole is homogenised for about one hour
and deaerated. This approx. 53% mixture is then ground
in a closed ball mill (DYN0 mill, ~ype KDL) by means of
Siliquarzit balls (1 mm diameter) for about 4 hours. After
this length of time there is obtal~ed a dispersion
having a particle size of less than 3 ~l. The ground
material is diluted to 1000 parts by the addition of a
further 50 parts of monopropylene glycol, 10 parts of
35% aqueous formalin solution, as well as 18 parts of a
- 42 -
.: . :: ,.
:
: '' '' : " '
~ 3~ ~
fatty alcohol polyglycol ether as a nonionic dispersing
agent (cetyl-stearyl alcohol etherified with ~5 moles
of ethylene oxide), and the whole is then homogenised
for 15 minutes. There is optionally also added an
anti-foaming agent. The grinding agent is subsequently
removed t~ leave a free-flowing aqueous preparation
having a content of active substance of about 50 per
cent by weight. This preparation ~las a low viscosity
( ~100 cP/20C). It is therefore advisable to render the
thinly liquid dispersion slightly thixotropic by grinding
in ~ 0.75% of Aerosil 200 (Degussa) [final viscosity
500-S00 cP/20C~, as a result of which a settling out,
even after a storage time of several months, is to a
great extent avoided.
If, instead of the optical brightener, anion-active
dispersing agent, nonionic dispersing agent and hydrotropic
agent given in the above example, there are used identical
parts of the constituents shown in the following Table II,
with the procedure being otherwise as described, then
likewise there are obtained storage-stabLe, free-flowing
aqueous o~tical brightener dispersions having analogous
properties, of which the active-substance content and
- 43 -
, ~;, ,
97~3~ 4
grinding ~ime are in each case governed by the ~extureof the crystalline brightener, by the type of mill
and by the nature of ~he gr;nding agents used, and
are between 40 and 60 per cent by weight and 3 to 15
hours, respectively.
- 44 -
.. . .... ... ... . , . . .... " .. , . .. ., .. ... .... . :. .... .... . . ....
..
, ,, "". . , ., ~,
,, .
~7~i3~
- U- -
.,~ . .
S~ .. ~d .~'~
., ~: ~ o ~ ~ J~
O ~ ~ ~ Q~ J~
,
o .. ~ ~ .,,
~ ~ , ~ o I ~ o ~
a
o s~ ~ Q~
5 ~1 ~ ~ X
~,~ o~ o a)a O O ~ ~ ~ O
~ 5 ~ ~d ~ .,~ a~
O ~r~ t~ ?~1 0 ,n
O ~o . t~ o c~
~ S~ ?~ ~O~ o ~ O r5
Z ~ ~ ~ O ~ ~i
u~ ~ ~1 "
¢
.
~ J ~rl
o ~ c~ o ~ 4~
~ ~ o ~ o o
o s~ ~ ~ ~n ,s::
o a~ Q~ a)
Cl.~ ~ ~ ~ ~1 ~3
~0 t~ ,~ ~ Q~ o ~ o
~ a~ a ~ a a~
~ ~a u~ t~
O b~ a~ O c~ ~ ~ tn
~J o a~ .,~ a) ~ O ~d '~
a) ~ ~ 0
~1~ u~ 5 a) ~ u~ ~ tn t~ d O O
~O S~ O ~ ~ ~ ~.
<~~1 0 ~ ~ ~ a~ ~ ~ t~
E~c~ ~ a. ~ ~a o ~ ~ ~ ~ E3 5~ 0
~: ~ ~ x ~ ~ ~a ~ o O~ ~ 5
,1 ~ O ~ O 1
~ U~ ~ tl~ ~ ~
L~
D \~ Z ~ ~
,~, :~:1 (~ t~ L~u~
O ~ \ ~
. ::~
_ __ _.
~ o C~l . C~l . ..... _ _ ~
.. . ~
.. :, , ,, ,, ,,. :
,: , :
': ': ' :~
~,
: :.'. ~ :. :
7~
~ . _ .
.
t,
.,, ,
~ a~) .~ .
o ~ ~ ~.
~ ~ ~ ~.
J~ ~ ~ ~ .~ ., ~
o a) ~ ~ ~ ~ ~ J-
b~ ~ ~ ~ a~
a~ ~ I c~
~ ~ U ~ ~ ~i
_ ~ W
,~ ~ a~
~J ~ ~ X .~
I .~ ~ .~ o o
O ~ C ~ ~ q~X ~ ~ U~ ~
C ~ ~ ~ , o .~ a) O
I ~ ~ O ~ ~r~ ~ O ~ ~ C~
a~ ~ ~ c-, o ~ ~ ~ c~
~~ ~ ~_ .~ ~ --' O J
C~ ~r~ ~ r~ ~ rl
O S~ ~ O ~ O ~ ~ ~ ~ ~
~ ~ a~ Q) ~ ~ ~ ~ ~ ~ C~ ~ ~ ~ X
O rl5 ~ 4~ O ~ I \ O O .~ ~3 ~ O O
~- ~ O ~ ; t~ ~ a3
c ~ a~ a~ ~1 0 u~ ~ .1 ~1
O ~ CO tl) .-1 Il) t~ .-1 ~1 0 ~ /H
Z ~ ~ ~ o
u~ O O ~1 a~ ~ c ,L O ~ O 5~ O 5_1 C r~
,, ~ ~ o ~ ~ c~ O e ~
Q~ rl ~ ~ t~ ~ ~ a) ~ .~ ~ ~;
X ~ ~ ~ o ~ O ~ U I
~ 0 4~ ~ a ~
JJ ~ U ~ UJ
~ ,,
~ O ~.~ g ~ .
~ o ~ ~ o ~ s~ 1 3
a) ~ q)~ s~ ~ D, ~ 0 5
a) ~ ~ F:~ Q.~ .~ C ,~
~ ~ .C(~) ~
,, ~ x ~ ~ ~ ~ e ~
~o u~ ~ ~ ~ I O ~ ~ ~n o
t. ~ O O ~ C~l .~ ~ ~ ~ ~ s~ o
J~ O a~
~ u~ ~ .~ ~ ~ ~ ~ ~ ~ .~ o
o ~ ~ ~ ~ ~ ~ ~
~1 0 ~1 C~ .,~ U7 0 ~ ~1 ~ h O U .--i td O ~) O
o --~ ~a o P-l aJ o ~ 1 o ,~
C4 O ,~ t~
.~ ~q c.æ ~ CL.,I x a) O a~
~ _, O ~ ~ ~ ~,~ 5 ~
o o ~ c~ Ei ~
~ .~ c~l
c~ c~ .. Q3
a~ ~ a~ ~) 'cL
H~ X X Z; Z _ ~ ~
p .~o o o I~Y' o
E~ ,~ ~ ~ ~ c:
o ~ ~o ~ ~æ-~ ~
'4 O' C) t~ ~Id
~d t~l ~ ~O .
~_ .. _, . .__ .
4~ ~ L~ ~ i-- . co
OX O c~l c~l c~J
C~ ~lZ
. .
4~
. . ,.... ,. :.
:. :
;
..
. ,,
. ' . .
~7di3~4
B. A?plication of_the prepar~t-iolls
Printing pastes are obtained by the mixing, by vigorous
stirring~, of a dyestuff preparation produced according
to Examples 1 to 7 or 9 into an aqueous polyacrylate
solution. These printing pastes can be used for printing
paper in the rotary screen printing process. The paper
thus prin~ed can then be used in the transfer printing
process, preferably ~ith applicatic~a to poiyester textile
materials, with sharply outlined, deeply coloured
printings being obtained.
Example 30 `
100 parts of the dyestuff preparation according to
Example 8 are disp2rsed by stirring in 1900 parts of water.
A fabric made from mercerised cotton is impregnated with
the liquor thus obtained; the material is squeezed out to
lS leave an increase in weight of 60%, and subsequen~ly
dried in a stream of hot air.
The fabric is afterwards impregnated in an aqueous
solution containing per litre 20 parts of sodium hydroxide
and 40 parts of sodium dithionite at a temperature of 20C,
and the material is then squeezed ollt to give a 60%
increase in weight; it is subsequen~ly st~med in a steamer
` - 47 -
.. -:: . ': .
. .. .
: .. ., . -
:, . .
.. .. . .
: . . .
,- . . .
~L~G7~
fl~e rrom air for 30 seconds, and is ~hen finished by
oxida~ion, rinsing, soaping and drying in the usual
manner.
There is obtained a strong, fast yellow dyeing
S having ~xcellent levelness.
Example 31
100 parts of the preparation accord;ng to Example 3
are diluted with 1900 parts of watPr. A polyester fabric
is impreg~ated with the resulting dispersion and then
squeezed out to 50% increase in weight; it is dried in
a stream ~ hot air, and additionally thermofixed for 60
seconds at 200. The yellow dyeing obtained is rinsed
and dried, the resulting dyeing is characterised by a
solid level appearance and very good fastness properties.
Example 32
In each case, 100 parts of the dyestuff preparation
according LO Examples 3 and 8 are diluted with 1800 parts
of water; there is then impregnate~ therein a mixed
fabric made from identical parts of polyester and cotton;
the material is squeezed out to 60~/o increase in weigh~,
dried and thermofixed for 60 seconds at 200; it is
subsequently impregnated in an aqueous bath containing
- 48 -
: ' ;.: , ' ~ ,
,
.
. . :- :,, ,
;,
~763~
per litre 20 parts of sodium hydroxide and 40 parts
o sodium dithionite, then steamed ~or 60 seconds,
oxidised, rinsed, soapPd and dried. There is obtained
a level yellow ~one-in-tone dyeing having very good
fastness properties and a solid appearance.
Example 33
A printing paste is prepared by stirring lS parts
of a dyestuff preparation according to Example l into
85 parts o- a 2.5% aqueous solution of a sodium
alginate thickeni-ng as the stock thickening.
This printing paste of about 8000 cP is applied
with a photogravure printing device ~o paper~ The paper
thus printed can be used in thb transfer printing process,
e;g. on polyester textiles. There are ob~ained sharply
outlined ievel prints having a high intensity of colour.
It is -~orthy of note that the viscosity of the stock
thickening, the consistency o which is very important
for a good 2rinting result, is only very slightly changed
by the stirring-in of the large amount of dyest-lf.
If, i~qtead of the stated dyestuff and the stock
thickening mentioned, those given in the following
Table III are used in the amount given, then likewise
- 49 -
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1~76~(~4
there are obtained printing pas~ which can be used
on paper OL on other suitable intermedi.ate carriers
in flat screen printing, in rotary screen printing,
in photogravure printing or in relief printing, or in
other suitable pril~ting processesg such as spraying,
brushing, etc..
- 50 -
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Example 50
The printing pastes ob,a-nPd according to Examples 33
to 49 can be printed on textile materials based on polyester,
cellulose triacetate, polyamide or polyacrylonitri]e, and
subsequently dried and fixed by methods nornally applied
for the individual fibres. Further ~dditives may optionally
be added to these printing pastes to impro~e fixing.
Example 51
It is possible, provided that the thickening agents
concerned permit it, to mix together the printing pastes
obtained according to Examples 33 to 49 in order to
obtain specifically desired effec~s~ such as levelness,
dyestuff yi~ld or run properties.
Example 52
100 parts of the dyestuff preparation according to
Example 8 are dilwted with 150 parts of water, and the
whole is stirred into 750 parts of a thickening consisting
of 60 parts of a lOV/o aqueous starch ether solution, 10 parts
o~ glycerin, 17 par.s of potassium carbonate, 4 parts of
water and 9 parts of sodium sulphoxylate.
The printing paste thus obtained is printed by means of
stencils on a cotton fabric of 120 g¦m2 in weight, which
has been pre~r~ated in the normal manner for printing,
- 53 -
~63763~
dried, ~nd afterwards steamed for 10 minutes at 100-105
with the exclusion of air and subsequently washed.
There is obtained a sharply outlined~ de~ply coloured
print.
Example 53
-
The following preparation is produced:- 30 parts of
a locust bean flour derivative are mixed with 420 parts
of water, and the whole is stirred together with a
solution of 500 parts of water and 50 parts of a starch
ether. To 7 parts of this preparation there are added,
under a high-speed stirrer, 1 part of the dyestuff
prcparation according to Example 8, 1 part of water and
1 part of a high-boiling spirit, and the whole is
then printed, by means of heliogravure rollers, onto a
fabric made from cellulose-viscose having a weight per
unit are of 250 g/m2, and subsequently dried. The material
is afterwards impregnated wi~h an aqueou3 solution
containing 40 parts of ~aOH, 65 parts of Na-dithionite,
15 parts of borax and 880 parts of water; it is then
squeezed out to lOQ% increase in weight and fixed in a
steamer free from air for 35 seconds at 120; it is
finally rinsed cold and then hot and dried. There is
obtained a strong, sharply outlined print in a yellow shade.
- 54 -
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Example 54
150 par~s of the dyestuff preparation according to
Example 8 are worked into 850 parts of a solution-
dispersion of thermGplastic substances, and the whole
is applied to a coated paper in the heliogravure
process. Af~er drying and, optionally, storage, the
paper is brought into contact under pressure for 2 to
10 seconds at 200 with a cotton fabric having a weight
per unit area of 120 g/m2, which has been normally
pretreated for printing. The transferred dyestuff is
afterwards fixed analogously to the fixing in Example
53 by means of an NaOH-Na-dithionite solution and finally
finished. The result is a strong level yellow printing
exactly reproducing the fine de~ails of the engraving.
- 55 ;
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3L~763~
Example 55
100 parts of the dyestuff preparation according LO
Example 8 are stirred into 900 parts of the preparation
describèd below, and the whole is applied by any desired
printing process to a textlle article which can be
S made from natural, regenerated or fully synthetic
fibres. After drying, the material is treated in hot
air for 5 to 10 minutes at 140 to 150. There is
obtained a printing in a deep shade.
The said preparation is obtained as follows:
40 parts of water,
10 parts of condensed alkylpolyglycol ether and
30 parts of a 3% aqueous carob bean flour ether solution
are mixed together; subsequently,
690 parts of heavy b~næene ~boiling range 120 to 180)
are worked in with a high-speed stirrer, then
30 parts of a 30% aqueous diammonium phosphate solution
and, finally,
200 parts of a 40/ synthetic resin dispersion based on
autocross-linking copolymers having an
acrylate base are added.
- 56 -
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50 parts of the dyestuff preparation according to
Examples 12 or 13 are stirred in~o 950 parts of water.
There are also added 7 parts of sodium acetate, and a
cotton fabric is then pad dyed in this dispersion. The
material is squeezed out ~o 70% liquid absorption; it
is dried on a cylinder drying machine at 110 and developed
by padding in an aqueous bath containing per litre 30 g
of sodium hydrosulphite and 60 g of lON sodium hydroxide
solution; the dyeing is subsequently steamed for 60
seconds, rinsed, oxidised, washed, soaped and dried.
There is obtained a solid bLue dyeing level on the surfaces
and sides. Similarly good results are obtained also by
the 2-phase printing process.
Example c-
3 parts of a brightener formulation produced
~5 according to Example 21 are stirred into about 30,000
parts of water containing 30 parts of a fixing accelerator
(nonionic oxyethylation product). 1000 parts of a
polyester staple fabric (Dacron 54~ are treated in the
following manner in the liquor ob~ained (ra~io of goods
to liquor 1:30) in a dyeing apparatus that permits
temperatures of over 100-
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1~763~4
The temperature of the liquor is raised within30 minutes to 120. The fabric is treated at 120 for
a further 30 minutes, and the liquor is then cooled
within 10 minutes to 70. The polyester fabric is
S rinsed cold and dried.
Compared with an untr~ated fabric, the fabric
treated in the manner described shows an increase in
the degree of whitene,ss of 150 units of the CIB~-GEIGY
scale of whiteness (see: CIBA-GEIGY Rundschau 1973/1
pages 10 to 25).
Example 58
4 parts of a brightener formulation produced
according to Example 23 and 1 part of a commercial
wetting agent are stirred into 1000 parts of water.
A piece of polyester staple fabric (Dacron 54) is padded
with the padding liquor ~hus obtained in such a manner
that the liquor absorption is 70% of the weight of the
goods. The polyester piece treated in this way is dried
at 80 ~or 10 minutes, and subsequently thermofixed in a
thermofixing apparatus for 30 seco~lds at 200. Compared
with an untreated fabric, the treated fabric shows an
increase in the degree of whiteness of 160 units of
the CIBA-GEIGY scale of whiteness.
: . . ,................ ~,
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- - ' " ~ ' "
763~
le 59
2 parts o~ a brightener formulation produced
according to Example 22 are stirred into 30,000 parts
of water containing 30 parts of a fixing accelerator
(nonionic oxyethylation product) and r~45 parts of
85% formic acid. 1000 parts of a polyacrylonitrile
staple fabric (Orlon 75) are treated in the resulting
applica~ion liquor at pH 3.5 (ratio of goods to liquor
1:30) according to the following procedure: the
temperature o the liquor is raised within 30 minutes
to 97; the fabric is treated for a further 30 minutes
at this temperature, and then cooled to 70 within 10
minutes. The fabric is rinsed cold and dried.
ComparPd with the untreated fabric, the fabric
treated in the described manner ~h~ws an increase in
the degree of whiteness of 120 units of the CIBA-GEIGY
scale of whiteness. ;
Example 60
3 parts of a brightener formulation produced
according to Example 22 are stirred into 30,000 parts of
water containing 90 parts of a commercial redwcing
bleaching agent, e.g. sodium dithionite. 1000 parts of a
polyamide 66 woven tricot are treated in the resulting
, .. ..... , ~ .. .. .. .... .. ... , .. ... .. ,, .. ...... ; . , ~"",~,
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application liquor (ratio of goods to liquor 1:30)
according to the following procedure: the temperature
of the liquor is raised within 30 minutes to 97; the
tricot is treated at 97 for a further 30 minutes
and then cooled to 70 in the course of 10 minutes.
The woven tricot piece is rinsed cold and dried.
The wnven tricot treated in the described manner
shows, compared with an untreated substrate, an i~crease
in degree of whiteness of 140 units of the CIBA-GEIGY
scale of whiteness~
- 60 -
.
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Example 61
1500 parts of a copolymer which contains 95% of
acrylonitrile and 5% of 2-vinylpyridine and has a mean
molecular weight of 47,000 are dissolved in 5500 parts
of ethylene carbonate, and the solution obtained is
filtered and deaerated. Into this solution there is s~irred
a mixture of 2500 parts of ethylene carbohate and about
1000 parts of water, in which beforehand l part of a
brightener dispersion formulated according to Rxample 27
and 7.5 parts of oxalic acid have been added and
homogenised. The formed spinning solution is then heated
to 70 and îs extruded, at a speed of 200 g/minOlnoz~le
through spinning nozzles having 412 holes ~0.0076 cm
di~meter), into a precipitating bath containing a mixture
of 75~/O of water and 25% of ethylene carbonate. The bat'n r
temperature is maintained at 60 while the freshly formed
fi~rils are dra~. through the bath to a length of 122 cm.
The coagulated tow is drawn out of the bath at a speed
of 9.3 m/min. and over two positively driven rollers
which are arranged outside the bath and run at a speed
of 9.3 mtmin. and 44.5 m/min., respectively, so that the
tow is stretched in air to the extent of 4.8 times its
former length. The tow is then drawn through a stretching
.
- ' . :, , . .: '
. . , ; :
~763~4
bath containing water and 1 to 3% of accumulated
ethylene c~rbonate at a temperature of 100. The
tow is dra~n through the bath over a distance of
63.5 cm, as a result of which there is achievPd an
additional 1.64-fold stretching, so that the overall
stretching obtained is 7.7 times the original length.
The tension is released and the tow is subsequently
passed, over a distance of 63.5 cm, through a bath
consisting essent ally of water at 90. The resulting
slack tow is squeezed out at a rate of 66 m/min., cut
to the desired length of staple, finished and finally
dried. In contras~ to Lhe severely yellowed untreated
fibre, the staple fibre brightened in this manner wi~h
0.33 o/oo of active substance of the optical brightener
from Example 8 is pure white.
- 62 -
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Example 62
A printing paste for rotary screen printing on
paper is produced by pre-diluting 0.5 to 1 part of
an optical brightener formulated according to Example 20
or 21 with about 9 parts of water, and stirring it
into 90 parts of a stock thickening (6% aqueous solution
of a paste made from a copolymer based on maleic acid).
This printing paste of abou~ 8000 cP is applied in a
desired design to paper using a rotary screen printin~
machine. T.le dried paper printed in this manner can be
used, in the transfer prin~ing process, on polyester
~ex~iles (transfer at approx. 210 during 30 seconds).
The design printed onto paper is visible after transfer
to the polyester textile material by virtue of its pure white
effect. The design is particularly effective in rooms
illuminated by UV-radiation.
63 -
'~. , ' ,'
