U.S. patent number 3,771,955 [Application Number 05/139,275] was granted by the patent office on 1973-11-13 for emulsions.
This patent grant is currently assigned to Imperial Chemical Industries Limited. Invention is credited to Ida May Jones.
United States Patent |
3,771,955 |
Jones |
November 13, 1973 |
EMULSIONS
Abstract
Stabilised emulsions in halogenated hydrocarbon solvents of
aqueous solutions or dispersions of dyestuffs or textile finishing
agents, in which the emulsifying agents present comprise ethyl
hydroxyethyl cellulose and one or more anionic surface-active
agents. Also treatment of textile materials with such stabilised
emulsions.
Inventors: |
Jones; Ida May (Manchester,
EN) |
Assignee: |
Imperial Chemical Industries
Limited (London, EN)
|
Family
ID: |
10165958 |
Appl.
No.: |
05/139,275 |
Filed: |
April 30, 1971 |
Foreign Application Priority Data
|
|
|
|
|
May 5, 1970 [GB] |
|
|
21,618/70 |
|
Current U.S.
Class: |
8/562; 8/401;
8/495; 8/532; 8/554; 8/587; 8/616; 8/924; 8/490; 8/496; 8/552;
8/557; 8/606; 8/617 |
Current CPC
Class: |
D06P
3/241 (20130101); D06P 1/623 (20130101); D06L
4/664 (20170101); D06P 1/924 (20130101); D06P
3/76 (20130101); D06P 3/54 (20130101); D06M
23/10 (20130101); D06L 1/06 (20130101); D06P
1/6533 (20130101); D06P 1/50 (20130101); D06P
3/64 (20130101); Y10S 8/924 (20130101) |
Current International
Class: |
D06M
23/10 (20060101); D06M 23/00 (20060101); D06P
1/92 (20060101); D06P 1/653 (20060101); D06P
3/70 (20060101); D06P 3/58 (20060101); D06P
1/50 (20060101); D06P 1/44 (20060101); D06P
3/34 (20060101); D06P 3/24 (20060101); D06P
3/64 (20060101); D06P 1/00 (20060101); D06P
3/54 (20060101); D06P 1/62 (20060101); D06P
3/76 (20060101); D06L 1/00 (20060101); D06L
3/12 (20060101); D06L 1/06 (20060101); D06L
3/00 (20060101); D06p 001/76 () |
Field of
Search: |
;8/172,83,173,93 |
References Cited
[Referenced By]
U.S. Patent Documents
Primary Examiner: Rosdol; Leon D.
Assistant Examiner: Herbert, Jr.; T. J.
Claims
We claim:
1. A stabilized emulsion in a halogenated hydrocarbon solvent of an
aqueous preparation of a textile treatment agent selected from
dyestuffs and finishing agents, wherein there are present as
emulsifying agents as ethyl hydroxyethyl cellulose having a
solution viscosity, measured on a 5% solution by weight in 80:20
(by weight) toluene/ethanol of from 20 to 35 cp, and at least one
anionic surface-active agent, the amount of water present in said
emulsion being from 0.3 to 20% of the total weight of the
emulsion.
2. A stabilised emulsion as claimed in claim 1, wherein the anionic
surface-active agent is selected from salts of sulphonated castor
oil, the triethanolamine salt of tall oil, the sodium salt of
sulphated methyl oleate, sodium dodecylbenzenesulphonate and sodium
oleate.
3. A stabilised emulsion as claimed in claim 1, wherein the
halogenated hydrocarbon solvent is selected from perchloroethylene,
trichloroethylene and 1:1:1-trichloroethane.
4. A process for the treatment of textile materials in which there
is applied to the textile material a stabilised emulsion as claimed
in claim 1 and the material is thereafter treated in known manner
to fix the treatment agent thereupon.
Description
This invention relates to improved emulsions in halogenated
hydrocarbon solvents of dyestuffs and textile finishing agents, and
to the use of such emulsions in the dyeing and finishing of textile
fabrics.
It is known to apply dyestuffs and finishing agents to textile
materials with the aid of organic solvents, such as halogenated
hydrocarbons. Such methods of application have been developed as an
alternative to the conventional procedures utilising aqueous media,
for reasons of economy, conservation of water supplies or avoidance
of effluent problems. The range of dyestuffs or finishing agents
which are adequately soluble in such solvents is, however, limited,
and it is usually necessary to employ the dyestuff or finishing
agent in the form of a dispersion or emulsion in the solvent. One
method of obtaining such dispersions or emulsions which has been
proposed consists in preparing an aqueous solution or dispersion in
the organic solvent with the aid of a suitable emulsifying
agent.
It has now been found that a combination of ethyl hydroxyethyl
cellulose with an anionic surface-active agent is of particular
value for use as such an emulsifying agent.
According to the present invention there is provided a stabilised
emulsion in a halogenated hydrocarbon solvent of an aqueous
solution or an aqueous dispersion of a dyestuff or a textile
finishing agent, characterised in that the emulsion contains as
emulsifying agents ethyl hydroxyethyl cellulose and at least one
anionic surface active agent.
By `ethyl hydroxyethyl cellulose` is meant a mixed cellulose ether
which is prepared by a process involving the following three
reactions :
1. alkali cellulose formation in which cellulose is swollen by
aqueous sodium hydroxide; Cell - OH + NaOH.revreaction.Cell -
OH.NaOH;
2. reaction of cellulose with ethylene oxide in the presence of
alkali : Cell - OH +, ##SPC1##
.sup.naOH Cell - OCH.sub.2 CH.sub.2 OH
3. ethylation of cellulose and hydroxyethyl cellulose:
(a) Cell - OCH.sub.2 CH.sub.2 OH + NaOH + C.sub.2 H.sub.5 Cl
.fwdarw. Cell - O CH.sub.2 CH.sub.2 OC.sub.2 H.sub.5 + NaCl +
H.sub.2 O
(b) Cell - OH + NaOH + C.sub.2 H.sub.5 Cl.fwdarw.Cell - OC.sub.2
H.sub.5 +NaCl + H.sub.2 O
Ethy hydroxyethyl cellulose may thus be defined as cellulose in
which most of the hydroxyl groups have been converted to ethyl
ether groups or ethoxyethyl ether groups. Ethyl hydroxyethyl
cellulose is available commercially in a number of different grades
depending on its molecular weight. These grades may be
characterised by their solution viscosities, ranging from 10 to 250
cp. as measured on a 5% solution by weight of the ethylhydroxyethyl
cellulose in a mixture of 80 : 20 (by weight) toluene/ethanol. Any
grade of ethyl hydroxyethyl cellulose is suitable for use in the
emulsions of the present invention, but the grade having a solution
viscosity as hereinbefore defined of 20 - 35 cp is preferred.
Anionic surface active agents which are suitable for use in the
emulsions of the invention include salts of sulphonated castor oil,
known collectively commercially as Turkey Red Oil, salts of
sulphated methyl oleate, salts of dodecylbenzene sulphonic acid,
salts of oleic acid and linoleic acid, salts of tall oil, salts of
sulphated mixtures of oleyl and cetyl alcohols and salts of
oleyl-p-anisidide sulphonic acid and oleyl sarcoside, more
particularly the sodium salts thereof. Either a single anionic
surface active agent or a mixture of two or more such agents may be
employed.
Halogenated hydrocarbon solvents which may be employed in the
emulsions of the invention include trichloroethylene,
perchloroethylene, 1:1:1:-trichloroethane, carbon tetrachloride,
chloroform, monochlorobenzene and 1:2:4-trichlorobenzene.
Dyestuffs which may be incorporated in the emulsions of the
invention include any of the well-known classes, for example acid,
basic, direct, reactive or disperse dyestuffs as conventionally
employed for the dyeing of textile materials composed of polyamide,
cotton, wool, silk, acetate, polyester, viscose or acrylic fibres
or filaments.
Textile finishing agents which may be incorporated in the emulsions
of the invention include fluorescent optical brightening agents,
such as the sodium salts of bis-triazinyl-aminostilbene
di-sulphonic acids, water-proofing agents such as
stearamidomethylpyridinium chloride and N-methylolstearamide,
crease-resist resins such as dimethyloldihydroxy-ethylene urea,
antistatic and antisoil/soil release agents such as condensates of
ethylene oxide with polyamides, crystallisable polyesters
containing polyoxyalkylene groups, for example polyoxyalkylene
terephthalate/polyalkylene terephthalate block copolymers and
copolymers of polymerisable acids, for example acrylic acid, with
other polymerisable vinyl monomers, softening agents such as fatty
quaternary ammonium salts, desizing agents such as enzyme
preparations, flameproofing or flame retarding agents such as
antimony trioxide or mixtures of boric acid and borax.
The emulsions of the present invention may be produced by
subjecting a mixture of a halogenated hydrocarbon solvent and an
aqueous solution or dispersion of a dyestuff or textile finishing
agent to suitable mechanical agitation in the presence of ethyl
hydroxyethyl cellulose and at least one anionic surface-active
agent.
The emulsifying agents used, that is to say the ethyl hydroxyethyl
cellulose and the anionic agent or agents, may be initially present
in either the halogenated hydrocarbon solvent or the aqueous
solution or dispersion of the dyestuff or finishing agent, or both.
However, having regard to the solubility properties of ethyl
hydroxyethyl cellulose,in particular the 20 - 35 cp. grade which is
preferred for use in the present invention, it will usually be
convenient for this constituent to be dissolved initially in the
halogenated hydrocarbon solvent. The anionic agent or agents may be
dissolved initially in either the solvent phase or the aqueous
phase, but if desired, in accordance with a well-known technique of
emulsification using such agents, it may be produced in situ by
reaction between a suitable organic acid precursor, for example
dodecylbenzene-sulphonic acid, dissolved in the halogenated
hydrocarbon solvent phase and an alkali, for example sodium
hydroxide, dissolved in the aqueous phase.
The relative proportions of the halogenated hydrocarbon solvent and
the aqueous phase incorporated in the emulsions of the invention
may vary widely, according to the manner in which the emulsions are
to be applied to the textile fabric and to the type and solubility
of the dyestuffs or finishing agents employed. Commonly, however,
the amount of water will lie in the range 0.3 to 20.0% of the total
weight of the emulsion.
The emulsions of the present invention are valuable for the
application to textile materials of the dyestuffs or finishing
agents which they contain. In general, the emulsions may be applied
to the textile materials by passing, exhaustion or any other
conventional form of impregnation, followed by evaporation of the
halogenated hydrocarbon solvent and, if necessary, a final baking
operation to fix the dyestuff or finishing agent on the textile
material. The halogenated hydrocarbon solvent which is evaporated
during this process may, of course, be recovered for re-use.
Textile materials to which the emulsions of the invention may be
applied include yarns and knitted, woven or non-woven fabrics.
The use of the emulsions of the invention instead of conventional
aqueous solutions or dispersions of dyestuffs or textile finishing
agents confers a number of advantages. Exhaustion may be more rapid
in batchwise processes and wetting out easier and pick-up better in
padding procedures. Losses in dimensional stability are reduced.
The halogenated hydrocarbon solvents have lower specific heats and
latent heats of evaporation than water, thus reducing costs of
heating and drying and also permitting economic recovery of the
organic liquid for reuse which avoids the increasingly severe
difficulties being met in the treatment of aqueous effluents. A
number of finishing treatments, and also dry cleaning of textile
materials, are carried out in non-aqueous media and in suitable
cases these may be combined with application of a treating agent to
the textile material.
Of particular advantage for such applications is the excellent
stability of the emulsions of the invention; these show no
detectable separation of the organic and aqueous phases over a
period of several days. In contrast, emulsions of similar
composition but containing only the ethyl hydroxyethyl cellulose as
stabiliser, that is to say omitting the anionic surface active
agent or agents, show appreciable separation after as little as one
day. Inferior results are also obtained by use of an anionic agent
along (i.e., omitting the ethyl hydroxyethyl cellulose); it is
possible to achieve a moderate degree of stability of the emulsions
by increasing the concentration of the anionic agent, but this
frequently has an adverse effect on the subsequent use of the
emulsion where certain types of dyestuff are involved.
The invention is illustrated but not limited by the following
examples in which all parts and percentages are by weight unless
otherwise stated:
Example 1
0.70 Part of the dyestuff which is the disodium salt of
2-[2'-acetylamino-4'-(4"-chloro-6"-amino-1":3":5"-
triazine-2"-ylamino)phenylazo naphthalene-4:8-disulphonic acid and
0.22 part of soda ash are dissolved in 13.3 parts of water, and 1.5
parts of Turkey Red Oil is then added and stirred until in
solution. 1.5 Parts of ethyl hydroxyethyl cellulose of viscosity
20-35 cp (measured at 25.degree. C on a 5 % by weight solution in
80:20 toluene/ethanol) is dissolved in 132 parts of
perchloroethylene and is stirred at high speed while the solution
of dyestuff is slowly added over 5 minutes. High speed stirring is
continued for a further 5 minutes, followed by slow stirring for 2
minutes to allow entrapped air to escape. The resulting emulsion
has excellent stability.
A sample of cellulosic textile material is padded in the emulsion,
dried and baked at 200.degree. C for 1 minute. The textile material
is thereby evenly dyed a yellow colour.
If the above procedure is followed but omitting the Turkey Red Oil
and increasing the amount of ethyl hydroxyethyl cellulose from 1.5
parts to 2.25 parts, the resulting emulsion is found to have
considerably inferior stability, separation of aqueous phase being
detectable after 18 - 20 hours, whereas the emulsion obtained using
both ethylhydroxyethylcellulose and Turkey Red Oil shows no
separation for at least 10 days.
If the procedure first described above is followed but omitting the
ethyl hydroxyethyl cellulose and increasing the amount of Turkey
Red Oil from 1.5 parts to 3 parts, a good emulsion is initially
obtained but this shows separation of the aqueous phase after 3
days.
Example 2
The procedure of Example 1 is repeated, except that in place of the
dyestuff there described there is used 1.1parts of the dyestuff
which is the tri-sodium salt of copper phthalocyanine-3-(sulphonic
acid).sub.3 -3
{N-[.beta.-6'-chloro-4'-methoxy-1':3':5'-triazin-2'-ylamino)ethyl]-sulphon
amide}.
Cellulose textile material treated with the stable emulsion so
obtained is evenly dyed a turquoise colour.
Example 3
The procedure of Example 1 is repeated, except that in place of the
dyestuff there described there is used 0.75 part of the dyestuff
which is the tetrasodium salt of
1-{2':5'-dimethyl-4'-[4"-(4'"-chloro-6'"-amino-1'":3'":5'"-triazin-2'"-yla
mino)7"-sulphonaphth-1"-ylazo]phenylazo }
naphthalene-2:5:7-tri-sulphonic acid.
Cellulosic material treated with the resulting stable emulsion is
evenly dyed an orange-brown colour.
Example 4
The procedure described in Example 1 is repeated, except that the
perchloroethylene is replaced by an equal weight of
1:1:1-trichloroethane. An emulsion of excellent stability is again
obtained.
Example 5
The procedure described in Example 1 is repeated, except that the
perchloroethylene is replaced by an equal weight of
trichloroethylene. An emulsion of excellent stability is
obtained.
Example 6
1.4 parts of the dyestuff described in Example 1 and 0.45 part of
soda ash are dissolved in 26.6 parts of water. 1.5 parts of ethyl
hydroxyethyl cellulose of viscosity 20-35cp, measured as described
in Example 1, is dissolved in 132 parts of perchloroethylene and
1.0 part of tall oil is added, followed by 0.5 part of
triethanolamine. The solution is stirred at high speed whilst the
dyestuff solution is added dropwise as quickly as practicable. High
speed stirring is continued for 5 minutes, followed by slow
stirring for 2 minutes to allow de-aeration to take place. The
resulting emulsion has excellent stability and may be employed for
the continuous dyeing of cellulose textile materials according to
the procedure described in Example 1.
Example 7
0.05 part of the dystuff which is the pentasodium salt of
1-(2'-methyl-3'-[4"-chloro-6"-sulphoanilino-1":3":5"-triazin-2"-ylamino]-5
'-sulphophenyl)
-3-carboxy-4-[2"'-sulpho-4'"-(chlorosulphoanilino-1"":3"":5""-triazin-2""-
ylamino)phenylazo]-5-pyrazolone and 1.1 parts of urea are dissolved
in 1.9 parts of water; 0.145 part of a 45 % aqueous solution of the
sodium salt of sulphated methyl oleate and 0.26 part of sodium
dodecylbenzene sulphonate are then stirred in until dissolved. This
solution is added to a solution of 0.025 part of ethyl hydroxyethyl
cellulose of viscosity 20-35 cp, measured as described in Example
1, in 25 parts of perchloroethylene and mixed to give a coarse
emulsion. This emulsion is gradually diluted with a further 164
parts of perchloroethylene to form a stable product.
Cellulosic textile material is batchwise dyed a yellow colour by
immersion in a dyebath consisting of the above-described emulsion
which is continuously agitated and gradually heated to boiling
point, then maintained at the boil for 30 minutes.
Example 8
0.036 Part of the dyestuff identified in the Colour Index as C.I.
Acid Yellow 72 is dissolved in 0.6 part of water, and 0.145 part of
a 45 % aqueous solution of the sodium salt of sulphated methyl
oleate is added. The dyestuff solution so obtained is added with
good agitation to a solution of 0.025 part of ethyl hydroxyethyl
cellulose of viscosity 20-35 cp. in 15 parts of perchloroethylene;
the emulsion so formed is added with stirring to 149 parts of
perchloroethylene at 30.degree. C, to yield a stable product.
The resulting emulsion is used for the batchwise dyeing of nylon
textile materials to a yellow colour by immersing the textile
material in the emulsion when maintained at 85.degree. C, at which
temperature a clear solution is formed.
Example 9
The procedure of Example 8 is repeated, using in place of the
dyestuff there described 0.016 part of the dyestuff which is
identified in the Colour Index as C.I. Acid Red 266. A similar
result is obtained.
Example 10
procedure of Example 8 is repeated, using in place of the dyestuff
there described 0.015 part of the dyestuff
4-[4'-(phenylazo)phenylazo]-N-ethyl-N-(m-sulphobenzyl)aniline. A
similar result is obtained.
Example 11
0.02 Part of the dyestuff identified in the Colour Index as C.I.
Acid Blue 67 is dissolved in 0.6 part of water, and 0.045 part of
dodecylbenzene sulphonic acid added. The solution so obtained is
added with good agitation to a solution of 0.025 parts of ethyl
hydroxyethyl cellulose of viscosity 20-35cp, in 15 parts of
perchloroethylene; the emulsion so formed is added with stirring to
a further 145 parts of perchloroethylene at 30.degree. C. The
resultant dye liquor is employed for the batchwise dyeing of nylon
textile material according to the following procedure :
Perchloroethylene is circulated through the nylon textile material
at 40.degree. C for 10 minutes; the dye liquor in an amount
sufficient to deposit from 1.25 to 1.5 % by weight of the dyestuff
(based on the textile material taken), is then circulated through
the material so treated at 40.degree. C for 15 minutes, after which
the temperature is raised to 85.degree. C over a period of 40
minutes and then maintained at that value for 15 minutes. The
material is dried at 70-80.degree. C.
Example 12
The procedure of Example 11 is repeated, using in place of the
dyestuff there identified 0.016 part of the dyestuff referred to in
Example 10. A similar result to that described in Example 11 is
obtained.
Example 13
The procedure of Example 11 is repeated, using in place of the
dyestuff there identifed 0.037 part of the dyestuff identified in
the Colour Index as C.I. Acid Yellow 135. A similar result is
obtained.
Example 14
The procedure of Example 11 is repeated, using in place of the
dyestuff there identified 0.017 part of the dyestuff identified in
the Colour Index as C.I. Acid Blue 40. A similar result is
obtained.
Example 15
The procedure of Example 11 is repeated, using in place of the
dyestuff there identified 0.036 part of the dyestuff identified in
the Colour index as C.I. Acid Yellow 72. A similar result is
obtained.
Example 16
1 part of Turkey Red Oil is dissolved in 30 parts of an 18 %
solution in aqueous diethylene glycol of a fluorescent brightening
agent which is an anionic stilbene derivative; this solution is
added to a solution of 5 parts of ethyl hydroxyethyl cellulose,
viscosity 20 - 35 cp., in 70 parts of per chloroethylene, whilst
the latter is agitated with a "Silverson" homogeniser. Agitation is
continued for 1 minute after the addition is complete. The
resultant emulsion is viscous but pourable, and has excellent
stability. It is suitable for the optical bleaching of cellulosic
of polyamide fabrics and for this purpose it may be diluted with
additional perchloroethylene without breakage of the emulsion
occurring.
In a typical treatment, the diluted emulsion is padded on to a
cellulosic fabric so as to deposit 0.05-0.5% by weight of the
fluorescent brightening agent on the fabric; the solvent is then
removed by passing the fabric through a steam chamber and the
fabric is dried at 60.degree. C for 5 minutes.
The treated fabric is considerably brighter in appearance than the
untreated fabric.
Example 17
1 part of Turkey Red Oil is dissolved in 30 parts of a 50 % aqueous
solution of dimethyloldihydroxyethylene urea and is added to a
solution of 1.5 parts of ethyl hydroxyethyl cellulose, viscosity
20-35 cp., in 70 parts of perchloroethylene whilst the latter is
agitated with a "Silverson" homogeniser. Agitation is continued for
1 minute after the addition is complete. The resultant emulsion,
which is viscous but pourable, has excellent stability. It is
suitable for application together with a latent acid catalyst to
cellulosic and polyester/cellulosic fabrics for the production of
crease-resist and durable press finishes, and for this purpose it
may be diluted with additional perchloroethylene without the
emulsion breaking.
In a typical treatment, a latent acid catalyst such as
monochloroacetic acid or stearamidomethylpyridinium chloride is
added to the diluted perchloroethylene emulsion and the resulting
composition is padded on to 100 % cellulosic or
polyester-cellulosic blend fabric so as to deposit 4 - 8 % by
weight of the dimethylol dihydroxyethylene urea on the fabric. The
solvent is then removed by passing the fabric through a steam
chamber, the fabric is thereafter dried at 60.degree. C for 5
minutes and then heated at a temperature of 155 - 160.degree. C for
3 minutes.
The treated fabric possesses much improved wet and dry crease
recovery properties compared with the untreated fabric.
Example 18
0.4 part of sodium hydroxide is dissolved in 50 parts of a 15 %
w/v. aqueous dispersion of a polyethylene
terephthalate/polyoxyethylene terephthalate block copolymer; 2
parts of ethyl hydroxyethyl cellulose, viscosity 20 - 35 cp., are
dissolved in 45 parts of perchloroethylene, followed by 2.6 parts
of oleic acid. The aqueous dispersion is added over a period of 10
minutes to the oil phase, using a high-speed stirrer; after the
addition is completed, stirring is continued at high speed for 3
minutes, followed by slow-speed stirring for 2 minutes. The
resulting emulsion has excellent stability and is suitable for
conferring durable antistatic and anti-soil effects on polyester,
polyester/cellulosic and polyester/wool blend fabrics; it may be
diluted for this purpose with additional perchloroethylene without
the emulsion breaking.
The diluted emulsion is padded on to polyester fabric so as to
deposit 1 - 3 % by weight of the polyethylene
terephthalate/polyoxyethylene terephthalate block copolymer on to
the fabric. The fabric is dried by heating at 70.degree. C for 20
minutes. The treated fabric is found to possess superior
antisoil-redeposition, stain release and antisoil properties to the
untreated fabric.
Example 19
0.2 Part of an azo dye, prepared by coupling 4-aminobenzene
sulphonamide on to N-methyl-N-.beta.-cyanoethyl aniline, and 0.1
part of the polyurea deflocculating agent obtained as described
below from mixed 2,4- and 2,6-tolylene diisocyanates and a fatty
secondary amine derived from soya are gravel milled in 3 parts of
perchloroethylene for 40 hours. The resulting dispersion is added
with stirring to a solution of 1 part ethyl hydroxyethyl cellulose
of viscosity 20-35 cp (measured at 25.degree. C on a 5 % by weight
solution in 80:20 toluene/ethanol) dissolved in 115 parts
perchloroethylene. A mixture of 5 parts of water and 1 part of
Turkey Red Oil are slowly added with stirring to give an emulsion
which is then further diluted with 690 parts of
perchloroethylene.
Polyester textile material is batchwise dyed a yellow colour by
immersion in a dyebath consisting of the above described emulsion
which is continuously agitated and heated to 120.degree. C over 10
minutes, and maintained at 120.degree. C for 30 minutes.
The polyurea deflocculating agent used in the above Example is
prepared by the following procedure. A solution in 32 parts of
acetone of 73.7 parts of a commercially available 40 % solution in
butyl acetate of polymerised mixed 2,4- and 2,6-tolylene
diisocyanates containing 5.7 % of isocyanate groups and less than
0.5 % of free tolylene diisocyanate is gradually added to a stirred
solution in 118 parts of acetone at 50-55.degree. C of 53.5 parts
of a fatty secondary amine derived from soya, commercially
available under the trade name Armeen 2S ("Armeen" is a Registered
Trade Mark). The acetone is then removed by distillation up to a
temperature of 100.degree. C under reduced pressure.
Example 20
0.5 Parts of the dye identified in the Colour Index as CI Basic Red
18 is dissolved in 5 parts boiling water and 5 parts Turkey Red Oil
are added. The dye solution so obtained is added with good
agitation to a solution of 1 part of ethyl hydroxy ethyl cellulose
of 20-35 cp. in 115 parts perchloroethylene and the emulsion so
formed is diluted with stirring with 687 parts
perchloroethylene.
The resulting emulsion is used for the batchwise dyeing of
polyacrylonitrile textile materials to a red colour by immersing
the textile material in the emulsion for 30 minutes at 105.degree.
C in a closed vessel with continuous agitation.
* * * * *