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Патент USA US3043660

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- 3,043,650
United States Patent 07 HI?
2
1
1:3:5-triazine ring, and above all dyestu?s which contain
a monochloro-l:3:5-triazine ring of the formula
3,043,650
PROCESS FOR DYEING CELLULOSE WITH
REACTIVE DYESTUFFS
(1)
Jacques Wegmann, Basel, and Josef Renggli, Riehen, 5
Switzerland, assignors to Ciba Corporation, a corpo
ration of Delaware
Patented July 10, 1962
N
¢ \
a
r
‘t
No Drawing. Filed Mar. 26, 1959, Ser. No. 801,985
Claims priority, application Switzerland Mar. 28, 1958
11 Claims. (Cl. 8-542)
It is known that polyhydroxylated ?brous materials,
such as cotton, can be dyed with advantage by ?xing on
the material by the action of an alkali and‘ heat a re
r01
N\ /N
X
0 in which X represents a hydroxyl group that may be
substituted or advantageously an amino group that may
be substituted.
7
-
'
In addition to at least one labile substituent of the
active dyestuif, that is to say an organic dyestutf capable 15 above kind the dyestuffs used in the process of this in
of entering into combination with cellulose.
The present invention is based on the unexpected ob
vention also contain at least one, acid, and'preferably
servation that the ?xation can be carried out practically
as an acylated sulfonic acid amide group, one or more
without the application of heat by reacting a 'polyhy->
droxylated ?brous material, such as natural or more es
pecially regenerated cellulose, at room temperature or at
most a slightly’ raised temperature in the moist state with
the reactive dyestu? in the presence of an acid-binding
agent having in aqueous solution a more alkaline re~,
action than trisodium phosphate.
As reactive dyestuffs there are‘to be understood organic.
dyestulfs which are capable of being chemically ?xed on
the material by the action'of heat. As organic dyestuffs
of this kind there are used those which are capable of
reacting with the material under the conditions of proc
ess, for example, owing to the presence of an epoxy
group, an ethylene-imine or ethylene-imide group, a
double bond in otI?-POSlliOIl relatively to a -—CO- or
—-SO2-— group or of a labile substituent. There may be
strongly acid, group imparting solubility in water, such
further sulfuric acid ester groups, a carboxylic acid group
20 or preferably a sulfonic acid group. There are advan
tageously used dyestuffs that contain'more than one such
group and they may belong to a very wide variety of
classes, for example, stilbene dyestuifs, thioxanthone dye
stuffs, azine dyestuffs, dioxazine dyestuffs, dyestu?s of the
25 porphyrazine series such as the phthalocyanine dyestu?s,
and above all acid anthraquinone dyestuffs and am
dyestu?'s, including metal-free and metalliferous mono
,and polyazo-azo-dyestu?s. Especially good results, are
obtained with soluble dyestuifs which have no a?inity or
30 no pronounced a?inity for cotton and contain at most one
reactive halogen atom.
Many dyestuffs of the aforesaid kind are known or can I
be made by methods in themselves known, for example,
by using dyestuii components which contain the aforesaid
mentioned above all organic dyestuifs which contain an 35 labile substituents or by incorporating these labile sub
ethylene-imine group, an acryl group, especially an
stituents or radicals containing such substituents in the
acrylylamino group, a vinyl-sulfone group or a labile
substituent capable of splitting o? easily with the taking
over of the electron pair of the bond, one or more such,
dyestuff molecules by methods in themselves known after
the dyestuifs have been made. Thus, by the reaction of
an azo-dyestul‘r’ or anthraquinone dyestuff which contain
labile substituents being present in the dyestutf moleculel 40 a reactive --NH2- group wtih trichloropyrimidine or
but not more than one being present in a triazine ring.
with a primary condensation product of cyanuric chlo
As labile substituents capable of splitting o?f with the
taking over of the electron pair of the bond’, there may
ride which contains two chlorine atoms and in place of
the third chlorine atom of the cyanuric chloride an or
be mentioned, for example, aliphatically ‘bound sulfonyl
ganic radical, there are obtained valuable condensation
oxy groups (including, of course, sulfuric acid ester 45 products which contain an exchangeable chlorine atom.
' groups), for example, an aliphatically bound
and are suitable for dyeing by the process of this inven
tion. Those dyestuffs used in the process of this inven
HO-SOg-O
tion which contain a sulfonylated hydroxyl group can be
group or a halogen atom, especially an aliphatically 50 made, for example, by reacting one molecular propor
bound chlorine atom. These labile substituents are ad
tion of a dyestuif which contains a hydroxyalkyl group,
vantageously present in the 'y- or ?-position of an ali
for example, a sulfonic acid N-hydroxyalkylarnide group,
phatic radical which is bound to the dyestu? molecule
with an organic sulfonic acid‘halide, for example, tosyl
directly or through an amino group or a —-SO2-— group
chloride, benzene sulfonyl chloride or ethane sulfonyl
or to the nitrogen atom of a carboxylic acid amide group,
55 chloride, or with concentrated sulfuric acid, in such man
or of a sulfonic acid amide group. In those dyestuffs
ner that the hydroxyl group is acylated.
which contain as a labile substituent a halogen atom, this
By using padding solutions or printing pastes contain
. exchangeable halogen atom may be present in an ali
ing such dyestu?s polyhydroxylated materials, especially
phatic acyl radical, for example, in an acetyl group or
cellulosic ?brous materials, which may be composed
in the [SI-position of a propionyl group or advantageously 60 either of synthetic ?bers, for example, of regenerated cel
in a heterocyclic radical, advantageously a monohalo
lulose (viscose), or of natural ?bers, for example, linen
genated heterocyclic ring. In this preferred form of the
or more especially cotton or mixtures of such ?bers or
process dyestuffs are advantageously used which contain
a labile chlorine atom bound to a heterocyclic ring, for
example, to a pyrimidine or phthalazine ring or more
mixed ‘fabrics, may be dyed on a padding machine or
for example, dyestuffs which contain a 2-phenyl~4-chloro
trolyte, such as urea or a lower carboxylic acid amide.
printed. There are advantageously used aqueous solu
65
tions of the aforesaid d-eystutis which contain a non-elec
especially to a triazine ring. There may be mentioned,
3,043,650
3
£5.
With solutions of this kind which also contain a more or
less neutral, and preferably inorganic salt, such as an
alkali metal chloride or sulfate, and, if desired, an acid
binding agent (preferably an inorganic acid-binding
agent), which has a more alkaline reaction in water than
By the process of this invention very valuable strong
and generally very full dyeings and prints having excellent
properties of wet fastness and a very good fastness to
light are obtained on cellulosic materials, even with dye
stuffs of the kind de?ned above which possess no af?nity
or no pronounced a?inity for cotton.
In some cases it may be of advantage to subject the
dyeings or prints obtained by the process to an after
trisodium phosphate, for example, an alkaline earth metal
hydroxide, alkali metal metasilicate and/ or alkali metal
hydroxide, such as sodium hydroxide, the material to be
dyed is impregnated advantageously in the cold or at a
treatment. Thus, for example, the dyeings are advantage
moderately raised temperature or, when no alkali is 10 ously thoroughly rinsed and soaped, so that any incom
present, at a higher temperature, for example, of 60—80°
pletely ?xed dyestuff is removed. When the dyestulfs
C., and the impregnated material is squeezed in the usual
used for producing the dyeings or prints by the process
manner. The material is advantageously squeezed to an
contain metallisable groups, they may be subjected to an
extent such that it retains 10.5 to 1.3 times its original
after-treatment with an agent yielding a heavy metal,
weioht of dyestu? solution. When the dyestuff solution 15 especially an agent yielding copper.
contains no alkali, it is necessary, after impregnating the
The following examples illustrate the invention, the
‘material with the solution, to treat it with an alkaline solu
parts and percentages being by weight. Although the
tion, for example, a solution containing 15~25 grams of
dyestuffs are usualy referred to or shown in the form
sodium hydroxide per liter, which solution preferably also
of the free acids, they are used in the form of alkali metal
20 salts thereof.
contains a high concentration of salt.
. The ?xation of the dyestuffs on the impregnated mate
‘ Example 1
rial 'is carried out after the impregnation. For this pur
2
parts
of
the
complex
copper compound of the dyestu?
pose, for example, the material which has been impreg
of the formula
nated with the dyestuff solution and with an alkali is
maintained for a longtime, for example, from 2 to 48 25 HO
on
(In
hours in a wet to moist condition, and, if desired, while
being slowly rotated. At the endof this period the dye
stu?“ will have become ?xed on the material without it
being necessary to subject the material to the action of
heat. It will, of course, be understood that the reaction 30
N
takes place more rapidly at room temperatures of 25° C.
80311
to 40° C. than at lower temperatures. However, by suit
are mixed with 10 parts of urea and dissolved with heating
ably prolonging, the reaction period, it is possible to
in 85 parts of water. The solution is allowed to cool,
achieve adequate ?xation at temperatures below 20° C.,
5 parts of 10 N-sodium hydroxide solution are added, and
for example,‘ down to 10° (3., especially with dyestuifs 35 a viscose rayon fabric is impregnated with this solution,
that react'easily, for example, those containing sulfonic
then squeezed to a weight increase of 75%, rolled up
acid ‘chlorethylarnide groups or monochlorotriazine
while still wet, ‘and the roll is wrapped in a plastic foil
groups, and particularly sulfuric acid esters of [it-hydroxy
to prevent the escape of moisture. The fabric is thus
ethyl-sulfone dyestuffs. In the case of the most slowly
40 kept for 4 hours at room temperature (20 to 30° C.),
_ reacting dyestuifs, for’example, pyrimidine dyestuffs or
rinsed for 15 minutes each in cold and boiling water,
sulfuric acid‘ esters of sulfonic acid-NzB-hydroxyethyl
rinsed until clear and dried. A level ruby red dyeing is
amides, smooth ?xation can be achieved with a minimum
obtained which has good fastness to washing ‘and light.
consumption of heat at 30° C. to 40° C.
'
Similar good results are achieved when a cotton or
‘The process of the invention can be carried out with 45 spun rayon fabric is thus treated.
dyestuffs that are insu?iciently stable in the presence of
alkali, provided that care is taken to introduce the dye
stuif solution and the solution of alkali into the padding
trough separately by means of devices controlling the
, quantities of the solutions supplied, so that the dyestu? '
and alkalirremain in the trough only a short time before
the impregnation, because even dyestuffs that are most
sensitiveto alkali are considerably less sensitive on the
?ber than they are in solution.
In a preferred form of the process of this invention the 55
material‘is ?rst impregnated only with the dyestuff solu
No change in the resulting dyeing is observed when the
impregnating solution is left to itself for 4 hours before
being used.
.
Example 2
4 parts of the dyestuif of the formula
HO
OH
N—N- I
Hots
/(l3\N
N
HOaS-
NH-ii
(ll-C1
\N%
tion with a very high degree of squeezing, and then the
impregnated material, with or" without being dried, is
are dissolved with heating in 85 parts of lwater and after
treated in an alkaline solution with a very low degree of
cooling 15 parts of 10 N-sodiurn hydroxide solution are
squeezing. In order to prevent bleeding out the alkaline 60 added. A spun rayon fabric is impregnated with this
solution should have a rather high concentration of salt
solution, squeezed to a weight increase of 75% , the fabric
(100 to 200 grams of sodium chloride per liter) and often
is rolled up and the roll is wrapped in a plastic foil, and
a rather high concentration of alkali. This form of the
the whole is left to itself ‘for 48 hours at room tempera
process has the advantage of making it unnecessary to
ture. The fabric is then rinsed in cold and boiling water
take into account the sensitivity to alkali of the padding
and dried. An orange dyeing is obtained which is fast
solution.
'
to washing and light.
Measurements have shown that the concentrations of
Example 3
alkali ‘and salt produced on the fiber in the process of
2
parts
of
the
dyestutf
of the formula
this invention are more than twice as high as would be
'
expected by pure calculation, because the electrolytes 70
_ diifuse from the concentrated alkali-salt solution into
the wet ?bers due to the osmotic gradient. The process
gives very good results, especially on ?bers of regenerated
cellulose in that the streakiness that can occur with such
?bers is covered up.
75
—OH R035
01
3,043,650
5
6.
Example 5
2 parts of the dyestuff of the formula
are dissolved in 98 pantsof water, and 2 parts of 10
N-sodium hydroxide solution are added to the dyestuif
solution. A viscose fabric is impregnated with this solu
tion, squeezedto a weight increase of 100%, rolled up,
left to itself for 4 hours and then rinsed in cold and boil
ing water. A red dyeing results which is fast to washing
and light.
An equally good result is achieved when a fabric of
mercerised cotton is thus treated.
I
When in the above example the sodium hydroxide solu 10
tion is replaced by 2 parts of sodium metasilicate or 2
parts of lithium hydroxide, proceeding otherwise in iden
tical manner, similar good results are achieved.
Example 4
15
2 parts of the dyestu? of the formula
SOaH
mir-
HO
are dissolved with heating in 95 parts of water. After
NH-C o-Q
cooling, 5 parts of 10 N-sodium hydroxide solution and
20 2 parts of sodium chloride are added to the dyestutf solu
N=N—
00
|
HOaSCHr-CHz-Cl
tion which is then used to impregnate a cotton fabric.
The fabric is squeezed to a Weight increase of 60% and
kept moist for 24 hours at room temperature, then washed
soan
are dissolved in 95 parts of water by being raised to a
in cold and boiling water and dried. A greenish yellow
short boil, and after cooling 5 parts of 10 N-sodium 25 dyeing of good fastness to washing and light is obtained.
hydroxide solution are added to the dyestu? solution. A
When the above dyestu?‘ is replaced by 2 parts of
viscose fabric is impregnated with this solution, squeezed i the dyestuif obtained by condensing 1 molecular propor
to a weight increase of 75%, rolled up and wrapped in
tion of copper phthalocyanine tetrasulfonyl chloride with
a plastic foil, and the whole is allowed to stand at 20° C.
1-2 molecular proportions of the condensation product of
for 48 hours. The fabric is then washed in cold and
boiling Water and dried. A brilliant red-violet dyeing
results which has good properties of fastness to washing
O
the formula
‘
01
and light.
When in the above dyeing operation the dyestutf of the
formula
\
35
-
N
HzNOSOaH
NH,
followed by hydrolysis of the unreacted sulfonyl-chloride
N=N—C>—NH~—C O~—C=CH—C 0 OH
1
51
groups to sulfonic acid groups, proceeding otherwise in
identical manner, a turquoise blue dyeing is obtained
which is ‘fast to washing ‘and light.
OH 11038
HOQE
By using the dyestuif of the formula
i0
is used, a red dyeing is obtained which has similar good 45
NH2
S0311
properties.
('31
The dyestuif of the formula
/C
so H
N/ \N
s 03H
50
Gleam-CH3
NH
HO-——C\ /N
l
'
‘
'
NH-
<3
.
NH-
a
C-NH
i\ / "
A 0311
N
Hogs
in the above example,‘ a blue tint is obtained which is
N
fast to washing and light.
(I: o
C H=C H2
0
‘\
\
Example 6
01
'
4 parts of the dyestuif of the formula '
01
A0311
.
60
('31
N//C\If
produces a yellow dyeing.
The dyestuff of the formula
S0311
0H NH---(')
(ll-NH
\ /
65
>
N
I
N=N
>
C H;
HOaS—
S0311
are dissolved with heating in 100 parts of water._ The
produces a reddish yellow dyeing.
70 cooled solution is used to impregnate a fabric of mer
cerised cotton which is" squeezed to a weight increase of
-
The 1:2-chromium complex of the dyestuif mentioned
in Example 1 produces a currant red dyeing, while the
corresponding 1:2-cobalt complex gives a red-brown dye
mg.
60%. Without intermediate ‘drying the fabric is then
impregnated with a solution of 20 parts of sodium
chloride and 2.2 partsv of sodium hydroxide (100%) 'in
- :1 01 110 parts of water, the roller pressure of the padder being
3,043,650
8
adjusted so that the fabric absorbs another 30% of liquor.
tional weight increase of 25% calculated from the dry
The fabric is then rolled up, wrapped in a polyethylene
foil and left to itself for 12 hours at room temperature.
weight of the fabric. The fabric is rolled up and wrapped
The fabric is then thoroughly rinsed in cold and warm
water, washed for 10 minutes in boiling water, rinsed
until clear and dried. A brilliant red dyeing of good .
fastness to light and washing results.
Example 7
2 parts of the dyestulf of the formula
10
temperature, then rinsed in cold and boiling water and
dried. A level red dyeing is obtained which is fast to
.
in a plastic foil and left to itself for 12 hours at room
washing.
’
When the fabric is washed after having been kept for
8 hours, an equally handsome, but slightly paler dyeing
is obtained.
'
Example 10
3 parts of the cobalt complex obtained from 1 atomic
proportion of cobalt and two molecular proportions of
the dyestulf of the formula
(.31
C
/
15
20
N02
are dissolved in 100 parts of water.
A fabric of mer
are dissolved in 100 parts of water. A fabric of viscose
spun rayon is impregnated with this solution and then
has a temperature of 20 to 30° C.) in a manner such
squeezed to a weight increase ofr80%. Immediately after
as to achieve a weight increase of 60%. The fabric is 25 wards the fabric is further impregnated with an aqueous
then further impregnated with a solution of 20 parts of
solution of sodium ‘hydroxide and sodium chloride as de
sodium chloride, 2.2 parts of sodium hydroxide (100%)
scribed in Example 9 so that the additional weight in
in 110 parts of water until the fabric has absorbed an
crease amounts to 25% calculated from the dry weight
other 30% of liquor calculated from its dry weight. The
of the-fabric. The fabric is rolled up and wrapped in a
30
fabric is rolled up, Wrapped in a plastic foil, left to itself
plastic foil, allowed to stand for 24 hours at 25° C.
for 12 hours at 20 and 30° C., rinsed in cold and warm
The fabric is then thoroughly rinsed in cold and hot
water, boiled in water for 10‘ minutes, rinsed and dried.
water, boiled in water for twice 10 minutes, rinsed and
A level violet dyeing of good fastness to washing and
dried.
light results.
A currant red dyeing is obtained which is fast to wash
cerised cotton is impregnated with this solution (which
Example 8
3 parts of the dyestuff of the formula
ing and light.
stuffs of the formulae
01
H(|)C—N—— |
cursorHO3S—~O—-CH3
N=N——C
'
40
%
\
—0CHs
'
Similarly good results are obtained by using the dye
C=N
—SO3H
l
CH3 CH3
are dissolved in 100 parts of water and a fabric of mer
(in which X represents a dichloropyrimidine residue. The
.cerised cotton is impregnated with this solution and then
squeezed to a weight increase of 60%. Without inter
mediate drying the fabric is then impregnated with the
sodium chloride solution containing sodium hydroxide de
dyeing is red.)
Gl—OHz-CH:—NH——SOz-—
OCH»,
scribed in Example 7 and squeezed to an additional in
crease in weight of 30% calculated from the dry weight
of the textile material. The fabric is rolled up, wrapped
in a plastic foil and left to itself for 14 hours at room
temperature. The sodium chloride and hydroxide are
then thoroughly rinsed out and the fabric is boiled in
water for 10 minutes, rinsed. clear and dried.
A level, brilliant yellow dyeing of good fast-ness to light
and washing results.
‘
Example 9
60
4 parts of the dyestuif of the formula
CHr-SO
HOzS-O-CHQ
OCH3 HO
65
0311
are dissolved in 100 parts of water. A fabric of viscose
70
spun rayon is impregnated with this solution and then
squeezed-to a weight increase of 85%. Without ?rst
drying the fabric is then impregnated with a solution of
(Tlnt : yellow)
20 parts of sodium chloride, 2.2 parts of sodium hydroxide
and keeping the fabric, rolled up in a plastic foil, for
(100%) in 100 parts of water andsqueezed to an addi
7 01 24 hours at 35° C.
'
.
8,043,650
.
,
Example
.
l0
.
.
-
and with (b) water~so1uble organic dyestu? containing,
1_
as a reactive substituent, a monochloro-lz3z5-triazine
2 parts of the dyestu?' of the vformula
radical; (2) mechanically removing excess impregnation
liquor; and (3) maintaining the resulting moist impreg
01-0 HrEH-C OATH-Oscar
nated cellulosic ?ber at a temperature of at most 40° C.
for at ‘least two hours.
3. A process for dyeing cellulose which comprises: (1)
impregnating, in impregnation-liquor, cellulosic'?ber with
10
01
(a) acid-binding agent which in aqueous solution has a
more alkaline reaction than trisodium phosphate and with
(b) water-soluble organic dyestu? containing, as a re
active substituent, a dichloropyrimidine radical; (2) me
chanically removing excess impregnation-liquor; and (3)
maintaining the resulting moist impregnated cellulosic
C1
03H
15
are dissolved in 100 parts of water, and'immediately be
4. A process for dyeing cellulose which comprises: (1)
fore use the solution is mixed with 5 parts of a 10 N
impregnating, in‘impregnation-liquor, cellulosic ?ber with
solution of sodium hydroxide solution. The mixture is
(a) acid-binding agent which in aqueous solution has a
more alkaline reaction than trisodium phosphate and with
(b) water-soluble organic dyestu? containing, as a re
used to impregnate a viscose rayon fabric which is then
squeezed to a weight increase of 70%, rolled up, kept in
the moist state for 4 hours at room temperature, and
then thoroughly rinsed in hot and cold water.
A yellow dyeing is obtained which is fast to washing
and light.
Similar good results are obtained with the following
?ber at a temperature of at most 40“ C. for at least two
hours.
active substituent, an
25
dyestuffs.
group; (2) mechanically removing excess impregnation
liquor; and (3) maintaining the resulting moist impreg
nated cellulosic ?ber at a temperature of at most 40° C.
for at least two hours.
nos-o-om-om-sw-Qoom (Ina
5. A process ‘for dyeing cellulose which comprises:
(1) impregnating, in impregnation-liquor, cellulosic ?ber
with (a) acid-binding agent which in aqueous solution has,
35
:a more alkaline reaction than trisodium- phosphate vand
with (b) water-soluble organic dyestuif containing, as a
reactive substituent, an
group; (2) mechanicallyremoving excess impregnation
liquor; and (3) maintaining the resulting moist impreg
40 nated cellulosic ?ber at a temperature of at most 40° C.
for ‘at least two hours‘.
‘6. A process for dyeing cellulose which comprises:
(1) impregnating, in impregnation-liquor, cellulosic ?ber
with (a) acid-binding agent which in aqueous [solution
45 has a more alkaline reaction than trisodium phosphate
and with (b) water-soluble phthalocyanine dyestuff con
(Tint : red)
taining, ‘as a reactive substituent, at monochloro-lz3z5
triazine radical; (2) mechanically removing excess im
pregnation-liquor; and (3) maintaining the resulting moist
50 impregnated cellulosic ?ber at a temperature of at most
40° C. for at least two hours.
C
C O-GH-CHz-Cl
|
[
CH3
0111
C1
(Tint : yellow)
What is claimed is:
1. A process for dyeing cellulose which comprises:
(1) impregnating, in impregnation-liquor, cellulosic ?ber
7. A process for dyeing cellulose which comprises: (1)
impregnating, in impregnation-liquor, cellulosic ?ber with
(a) acid-binding ‘agent which in ‘aqueous solution has a
more alkaline reaction than trisodium phosphate and
with (b) water-‘soluble anthraquinone dyestu? containing,
as a reactive substituent, a monochloro-l :3 :S-triazine rad
ical, (2) mechanically removing excess impregnation
liquor; and ‘(3) maintaining the resulting moist impreg
with (a) acid-binding agent which in aqueous solution 60 nated cellulosic ?ber at a temperature of at most 40°
has a more alkaline reaction than trisodium phosphate
and with (b) water-soluble organic dyestuff containing
a reactive substituent selected from the group consisting
of the acid sulfuric ester group, the acrylarnino group,
the ?-chloropropionylamino group, the B-chloroethylsul
‘fone group, the p-chloroethylamide group, the dichloro
pyrimidine and monochloro-1z3z5-triazine groups; (2)
mechanically removing excess‘ impregnation-liquor; and
(3) maintaining the resulting moist impregnated cellulosic
C. for at least two hours.
8. A process for dyeing cellulose which comprises: (1)
impregnating, in impregnation-liquor, cellulosic ?ber with
(a) acid-binding agent which in aqueous solution has‘ a
65 more alkaline reaction than trisodium phosphate and with
(b) water-soluble azo dyestuff containing, as a reactive
substituent, a monochloro-1:3 :S-triazine radical; (2) me
chanically removing excess impregnation-liquor; and (3)
maintaining the resulting moist impregnated cellulosic
?ber at a temperature of at most 40° C. for at least two 70 ?ber at a temperature of at most 40°’ C. for at least two
hours.
2. A process for dyeing cellulose which comprises: (1')
impregnating, in impregnation-liquor, cellulosic ?ber
hours.
9. A process for dyeing cellulose which comprises: (1)
impregnating, in impregnation-liquor, cellulosic ?ber with
(a) acid-binding vagent which in aqueous solution has a
with (a) acid-binding agent which in aqueous solution
has a more alkaline reaction than tr-isodium phosphate 75 more alkaline reaction than trisodium phosphate and with
3,043,850
11
12
p (b) water-soluble phthalocyanine dyestu?? containing, as a
a more alkaline reaction than trisodium phosphate and
reactive substituent, a
with (b) water-soluble phthalocyanine dyestuff contain
_
ing, as a reactive substituent, an
-‘CO-—CHZ——‘CH2CI
-NH—CH2CH2Cl
group; (2) mechanically removing excess impregnation
liquor, and (3) maintaining the resulting moist impreg
group; (2) mechanically removing excess impregnation
liquor; and (3) maintaining the resulting moist impreg
nated cellulosic, ?ber at a temperature of at most 40°
C. for at least two hours.
,
nated cellulosic ?ber at a temperature-of 'at most 40°
C. for at least two hours.
V
10. A process for dyeing cellulose which ‘comprises:
(1) impregnating, in impregnation-liquor, cellulosic ?ber
10
with a (a) acid-binding agent which in ‘aqueous solution
has a more alkaline reaction than ,trisodium phosphate
and with (b) water-soluble phthalocyanine dyestu? con
taining, as a reactive substituent, an
-
15
group; (2) mechanically removing excess impregnation
liquor; and (3), maintaining the resulting ,moist impreg
nated cellulosic ?ber at a temperature of ‘at most 40° C.
for at least two hours.
11. A process for dyeing ‘cellulose which comprises:
(1) impregnating, in impregnation-liquor, cellulosic ?ber
with (a) acid-binding agent which in'aqueous solution has
References Cited in the ?le of this patent
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