Note: Descriptions are shown in the official language in which they were submitted.
3~
This Application relates to fabric treatment compositions and
to a method for treating fabrics in an aqueous bath such as
the final rinse after a washing process in order to improve
various properties of the fabric. Generally similar composi-
tions are disclosed in the co-pending Canadian patent applic-
ation Serial No. 257,084 filed on July 15th, 1976 and in the
Canadian patent application No. 279,293 filed on May 27, 1977.
It has been known for some years that fabrics can be made to
feel softer by treatment in a dilute solution or dispersion
of certain cationic quaternary ammonium derivatives and
rinse-additive compositions have been marketed for this
purpose. The inventions disclosed in the above mentioned
British Patent Applications provide substantial additional
benefits by a combination of fabric conditioning agents.
These benefits may include some or all of: easier ironing,
anti-static properties, pleasanter feel of the fabrics, soil
release properties. It appears that recognition of improved
"ease of ironing" can arise from a combination of at least
three factors, namely fewer wrinkles to be removed, wrinkles
more easily removed (e.g. with less weight upon the iron), or
more completely removed, and less effort required to slide
the iron along the fabric. "Pleasanter" feel can be consis-
tently observed by experienced judges, although it is not
easy to define in words the sensation or combination of sen-
sations they like. Anti-static and soil release properties
improve the achieving and maintaining of soil-free fabrics.
The combination of fabric conditioning agents referred to
; above requires the presence of both a cationic quaternary
ammonium (or imidazolinium) derivative and a silicone. More
specifically the invention described in Canadian S.N.
257,084 provides a textile treating composition which is
an aqueous dispersion comprising:
(a) a fabric substantive quaternary ammonium textile
softening compound having in its molecular structure
èither two alkyl groups each having 12 to 20 carbon
atoms or one alkyl chain having 18 to 24 carbon atoms
or a fabric substantive quaternary imidazolinium
textile softening compound, and
(b) a silicone having a cationic character, the weight
ratio of component (b) to component (a) being in the range
from 20:1 to 1:100.
It is an object of the present invention to provide more
effective carrier materials for depositing silicones on
fabrics and, in particular, to provide compositions which
enable the use of conventional poly-dialkyl siloxanes.
-2-
. .:
~' . ' .
Accordingly, the present invention provides a tex-
tile treating composition which is an aqueous dispersion
comprising:
(a) a fabric substantive cationic compound select-
ed from the group consisting of
i) a subsituted polyamine salt having the formula
R' R' R'
2)n 1+ ~ (CH2)n - N+ j- R' A(-)
R' R' R' m
wherein R and optionally one of the R' groups fix-
ed on the same nitrogen atom as R is an alkyl or
alkenyl group having 10 to 22 carbon atoms,
the other R' groups, which may be the same or dif-
ferent, each represent hydrogen or a (C2H4O)pH or
a (C3H6O)pH group, or a Cl 3 alkyl group provided
that not all represent a Cl 3 alkyl group, where p
is a number such that up to 25 (C2H~O) or (C3H6O)
groups in all are present, m i5 from 0 to 8, n is
from 2 to 6 and A( ) represents one or more anions
having total charge balancing that of the nitrogen
atoms;
ii) a polyamine salt having the above formula (i)
wherein R is hydrogen, or a Cl 4 lower alkyl
group, n is from about 2 to 4, preferably 2,
and m is not less than 2, preferably from 8 to
16;
iii) or mixtures thereof: and
(b) a silicone as hereinafter defined,
the weight ratio of component (b) to component (a) being in
the range from 5:1 to 1:500.
For the purpose of the present invention a silicone
-- 3 --
is defined as predominantly linear poly dialkyl or alkyl,
aryl siloxane in which the alkyl groups have one to five
carbon atoms and may be wholly or partially fluorinated. The
silicone will be present in the form of ~n emulsion. This
definition also includes silicones of cationic character which
can be one of ~he following:
(a) a predominantly linear di Cl-C5 alkyl or Cl-C5
- alkyl, aryl siloxane having a viscosity at 25C of
at least 100 centistokes, prepared by emulsion
polymerisation using a cationic surfactant as
emulsifier;
(b) an a,~-di quaternised di Cl-C5 alkyl or Cl-C5
alkyl, aryl siloxane polymer or
(c) an amino-functional~-di Cl-C5 alkyl or alkyl
aryl siloxane poly~er in which the amino group may
be substituted and may be quaternised and in which
the degree of substitution (d.s.) lies in the range
0.001 to 0.1, preferably .01 - 0.075.
A limited degree of cross linking of the siloxane
polymer is permissible and up to about 10~ by weight of
mono alkyl or mono aryl siloxanes may be present in the sili-
cones.
- a) Fabric substantive cationic softening component
: Materials suitable as the fabric substantive cat-
ionic softening component are as described above.
The compounds (ii) above include protonated poly-
ethylene imine derivatives.
Acid salts of diamine compounds, as used herein,
are the addition products formed when certain acids add to
the amino moieties of the diamines and form mono- or di-ammon-
ium salts.
`: :
',~ ' `~
' ` ' . ' ' ' '
The diamine acid salts can be partially acidified
diamine salts (i.e. only one nitrogen quaternized with aeid)
of fully acidified diamine salts (i.e. both nitrogen quater-
nized with acid).
A variety of acids can be used herein to form the
acid salts so long as the anion of the diamine acid salt
formed is stable under fabric rinse conditions and is non-
interfering in the rinse. Suitable acids include organic
and inorganie aeids such as hydrochloric acid, acetic acid,
sulphuric aeid, lactrie acid, stearic acid, formic acid,
citric acid and a large variety o~ others. Particularly
preferred acids used to form diamine acid salts include
acetie acid and hydrochloric acid.
Nonlimiting examples of such diamine aeid salts
inelude:
(C 6H33 - NH(CH3)-(CH2)3 NH(CH3)2~ 3 2
(cl8H37 - NH(CH3)-(CH2)2~NH(C2H5)2~ ( 3 2
(C H - NH(CH3)-(CH2)3-H2N C12 25~ 2
(C12H25 ~ NH(C2H5)-(CH2)3 NH(C3H7)2~ 3 4 2
~ allow H2 (cH2)3-NH(c2H5)2) Br2
2oH4l-NH(cH3)-(cH2)2-NH(cH3)21 2
(C15H31-NH(C2H5) ( 2 3 3
"
~ 18 37 N~2 (CH2)3-~2N-cH3) (HCOO)2
( 16 33 NH2 (CH2)3-H2N-cl6H33~ ++ C12-
NE~(CH3)~(CH2)3~NH(C2H5)2~++ (CH COO) -
~cl6H33NH(cH3)-(cH2)5-NH(c2H5)2~ (C 3 4 2
(Cl2H25NH(c2H5)-(cH2)2-NH(c3H7)2~ 2
~Cl4H29NH(cH3)-(cH2)3-(cH3)NH (C8H17)~ 3 2
wherein in the abo~e formulas RTal1ow is the alk~l group
derived from tallow fatty acid.
Other examples of suitable compounds include those in
which the starting diamine is N-tetradecyl, N'-propyl-1,3-
propane-diamine; N-eicosyl,N,N',N'-triethyl-1,2-ethane- -
diamine and N-octadecyl,N,NI,N'-tripropyl-1,3-propane-
diamine.
The form in which the diamine acid salt is derived is
not critical. The diamine acid salt can be formed from ;
diamines in situ during the preparation of the aqueous
fabric conditioning compositions herein or can alter-
natively, for example, be obtained as the acid salt
from commercial sources (e.g. Duomac~ T marketed by
Armour-Hess Co. Mixtures of diamine acid salts can,
of course, be used as the static control agent in the
compositions of the present invention.
The fully acidified diamine salts (i.e. the diacid
salts) are particularly preferred inasmuch as these
materials permit formation of highly stable, clear,
aqueous liquid fabric conditioning compositions.
Preferred aqueous fabric conditioning compositions
contain diamine acid salts of the formula on page 3
wherein R is alkyl of from about 16 to about 18 car-
bon atoms; and each R' is the same or different and
represents hydrogen or alkyl of from about -
: : .
- .
l to about 2 carbon atoms and n is 2 or 3, more preferably 3.
Diamine acid salts useful in the invention herein
are commercially available under a variety of trade names
including Duomeens ~ and Duomacs ~ (marketed by Armour-Hess
Co.) and Dinozem ~ and Dinoremac ~ (marketed by CECA/Pierre-
fitte-Auby). Moreover, tne starting diamine compounds can
be prepared in accordance with processes disclosed in the
art, as, for example, in U.S. Patent 2,267,205 issued
December 23, 1941 to Kyrides and U.S. Patent 2,246,524
issued June 24, 1941 to Kyrides.
- .
b) Silicone comPonent ~ ~
As mentioned previously, the silicone component is an
aqueous emulsion of a predominantly linear polydialkyl or
alkyl, aryl siloxane in which the alkyl groups can have
from one to five carbon atoms and may be wholly or
partially fluorinated. Suitable silicones are polydi-
methyl siloxanes having a viscosity at 25C in the range
~rom 100 to 200,~00 centistokes preferably no more than
120,000 centistokes. Fluorinated silicones having a
viscosity of at least 100 centistokes are also useful.
The silicone component also embraces silicones of
cationic character such as are disclosed in Canadian S.N.
297,293, which can be one of:
(a) a predominantly linear di Cl-C5 alkyl or
Cl-C5 alkyl, aryl siloxane having a viscosity at
25C of at least 100 centistokes, prepared by emulsion
polymerisation using a cationic surfactant as
emulsifier.
(b) an ~ di quaternised di Cl-C5 alkyl or
Cl-C5 alkyl, aryl siloxane polymer or
(c) an amino-functional di Cl-C5 alkyl or alkyl
aryl siloxane polymer in which the amino group may be
substituted and may be quaternised and in which the
degree of substitution (d.s.) lies in the range 0.001
to 0.1, preferably .01-0.075.
~1
a) Cationic emulsion polymerised siloxanes
Cationic emulsion polymerised siloxanes are known
in the art and can be prepared by strong alkali or acid
catalysis of siloxane monomer(s) in the presence of a
cationic emulsifying agent. Hyde and Wehryl US Patent
No.2,891,920 describes general procedures for such poly-
merisations and Examples 1 - 6 of the patent provide
specific teaching of the required reaction conditions.
The siloxane monomer can be any di lower alkyl siloxane
such as dimethyl, diethyl dipropyl, or ethyl butyl silox-
ane or alkyl, aryl siloxane such as methyl, phenyl silox-
ane or ethyl phenyl siloxane. However, the preferred
starting material for emulsion polymerisation is normally
a eylie trimer or tetramer of the desired siloxane.
The emulsifying agent can be any one of a wide
range of cationic surfactants such as:
Aliphatic fatty amines and their derivatives such
as dodecylamine acetate, octadecylamine acetate and - ;
aeetates of the amines of tallow fatty acids; homologues
of aromatie amines having fatty ehains sueh as dodeeyl-
aniline; fatty amides derived from aliphatic diamines
sueh as undeeylimidazoline; fatty amines derived from
di-substituted amines such as oleylaminodiethylamine;
derivatives of ethylene diamine; quaternary ammonium
eompounds sueh as dioetadeeyldimethyl ammonium chloride,
didodeeyldimethyl ammonium chloride and dihexadeeyl-
dimethyl ammonium chloride; amide derivatives of amino
alcohols sueh as ~ -hydroxyethylstearyl-amide; amine
salts of long ehain fatty acids; quaternary ammonium
bases derived from fatty amides or di-substituted diamin-
es sueh as oleylbenzylaminoethylene diethylamine hydro-
_ 9 _ .
:; , ' ,.. , ,, :
~ `3~
chloride; quaternary ammonium bases of the benzimi~azolines
such as methylheptadecyl benzimidazol hydrobromide; basic
compounds of pyridinium and its derivatives such as cetyl-
pyridinium chloride; sulfonium compounds such as octadecyl-
sulfonium methyl sulfate; quaternary ammonium compounds of
betaine such as betaine compounds of diethylamino acetic
acid and octadecylchloromethyl ether; urethanes of ethylene
diamine such as the condensation products of stearic acid
and diethylene triamine; polyethylene diamines; and poly-
propanolpolyethanol amines.
The emulsifier is conventionally employed at alevel of 1% - 10% by weight of the siloxane, more preferably
2% - 5~ by weight.
The catalyst employed to polymerise the siloxane
is preferably an alkaline catalyst such as an alkali me,tal
hydroxide or a quaternary ammonium hydroxide of the formula
(R)4N OH. In such ammonium hydroxides the Rgroups can be
hydrogen or alkyl radicals such as methyl, ethyl, propyl,
butyl, isobutyl, decyl or octadecyl or aralkyl radicals
such as benzyl or hydroxyalkyl radicals such as hydroxyethyl,
hydroxypropyl and hydroxybutyl.
Most preferably the catalyst is a quaternary
ammonium hydroxide having at least one radical of a least 12
carbon atoms in chain length, such a material also serving
as an emulsification agent. Long chain length alkyl quater-
nary ammonium salts are also preferred as the emulsification
agents, particularly di-long chain alkyl di-lower alkyl
quaternaries, such as ditallowyl dimethyl ammonium chloride
(~TDMAC), available commercially from Armour Chemical Company
as Arquad 2HT (Arquad is a Registered Trade Mark) and imidaz-
olinium derivatives such as methyl C18 alkyl amidoethyl,
- 10 _
Cl~ alkyl imidazolinium methosulphate, available commercially
from Ashland Chemical Company as Varisoft 475 (Varisoft is a
Registered Trade Mark).
The level of catalyst usage is dependent on the
catalyst type employed. Acid catalysts are conventionally
used at high levels, e.g. at 15% or more by weight of the
aqueous phase of the emulsion. Alkaline catalysts by con-
trast are used at lower levels, eOg. from 0.001~ to 10%,
preferably from 0.1% to 5% by weight of the siloxane monomer.
Emulsion polymerisation of dimethyl siloxane using DTDMAC as
emulsifier
In a typical preparation, dichloro dimethyl siloxane
was first hydrolysed to form octamethyl cyclo tetra siloxane
using the method of Patnode and Wilcock in JACS 68 1946
pp 358 - 363. 15 grs of this material were then added to a
mixture of 131 grs of a 1% aqueous solution of ditallowyl
dimethyl ammonium chloride and 3.75 grs of tetrabutyl ammon-
ium hydroxide in the form of a 40% aqueous solution. The
mixture was stirred during addition of the ingredients by
means of a Silverson laboratory emulsifier mixer and, after
addition was complete, the reaction mixture was subjected - `
to 15 minutes further agitation using an ultrasonic vibrator.
After 18 hours at 80C poly dimethyl siloxane oil was pre-
cipitated from the reaction mixture by addition of 500 mls of
ethyl alcohol and was then dried with further alcohol before
being heated at 75C under a high vacuum to remove all vol-
atile materials. The viscosity of the silicone was deter-
mined to be 22,000 centistokes by measurement of its rate
of flow under gravity between twa marks on a calibrated tube.
The time taken for a given quantity to flow along the tube
was converted to viscosity using a calibration curve estab-
lished with commercial silicones of known viscosity. -
- 11 -
;~i ' `'
,, . : .
i:. : . ,~ : ;,:
- . .~. .
Using the above-described polymerisation technique,
stable 10~ emulsions of polydimethyl siloxane were achieved
and equivalent results were obtained when the procedure was
repeated using cetyl trimethyl ammonium bromide and the imi-
dazoline derivative Varisoft 475 respectively as the emulsifier.
b) a - ~ quaternised polysiloxanes
The preparation of ~ , ~ quaternised siloxane
polymers can be conveniently carried out using the method
disclosed in I.C.I. British Patent Specification
No. 1,006,729. In this technique a polysiloxane end-
stopped with alkyl halide groups in which the halogen
atoms are separated from the nearest silicon atoms by at
least three carbon atoms, is reacted with a tertiary amine
to give an ~ , ~ -quaternised siloxane polymer. In order
to provide the polysiloxane starting material a solution
polymerisation is normally carried out to give a polymer
of the appropriate molecular weight, and the polymerisation
reaction is terminated by reaction with a ~-halo alkyl
dimethyl silanol.
As previously stated, the polysiloxane can be
a poly di (Cl-C5 alkyl)- or (Cl-C5 alkyl, aryl) siloxane,
preferably a polydimethyl siloxane and the tertiary amine
can be any alkyl, aryl or mixed alkyl and aryl material.
Examples include trimethyl-amine, cetyl dimethyl-amine,
pyridine, phenyl dimethyl-amine.
Preparation of a ~ - ~ dipyridinium polydimethyl siloxane
A typical preparation of this class of silicone
polymers involved the polymerisation of 23.2 grs of octa-
methyl cyclotetra siloxane in the presence of 0.9 mls of
' 30 concentrated sulphuric acid and 2.5 grs of 1,3-bis, 3-
chloropropyl tetramethyl disiloxane. The mixture was
shaken in a sealed flask for 48 hours at room temperature,
- 12 -
following which 5 mls of water were added and the flask
shaken for a further hour. The resulting emulsion was split
by addition of 50 mls of diethyl ether and the organic layer
was than washed twice with 30 ml aliquots of distilled water,
dried over sodium bicarbonate and magnesium sulphate and
filtered. ~vaporation of the filtrate to remove the ether
left 23 grs of a clear oil of viscosity 100 cs. NMR exam-
ination of the oil showed it to correspond to a polymer hav-
ing 36 siloxane units.
10 grs. of the ~ bis(3 chloropropyl) sili-
cone prepared above were then refluxed in 10 mls pyridine
for 36 hours at 120~C. Excess pyridine was distilled off
under reduced pressure leaving a brown viscous oil. This
was then dissolved in toluene, washed with water and the
toluene layer dried and evaporated to remove the toluene.
NMR spectral analysis disclosed a level of proton activity
corresponding to 70-80% of the theoretical uptake of pyridine.
10% aqueous emulsions of the silicone product
were prepared by mechanical emulsification using an ethoxy-
20 lated linear alcohol emulsifying agent (Dobanol 45E4, a C14-
C15 linear alcohol tetra ethoxylate supplied by Shell Inter-
national Chemicals Limited) at a level of 20% by weight of
the siloxane.
c) Amino functional linear polysiloxanes
Amino functional linear polysiloxanes can be
prepared by the general method disclosed in British Patent
Specification No. 1,339,906 at page 3 lines 78-108, page
4 lines 1-65 and page 3 lines 3-14. In this method, a
hydrosiloxane is reacted with an alkenyl group-containing
tertiary amine in the presence of a platinum catalyst in
accordance with the equation
13
.
, ~ - .
3~
H2P-tCl
(Me3SiO)2 (SiMe20~x(SiMeHO)y + yCH2=CHR'NR2 6 _~
(Me3SiO)2 (SiMe2O)x(OSi(Me)R'' NR2)y
wherein x = 10 to 100, y = 1 to 20, R is a methyl, ethyl
or phenyl group, R' is a direct linkage or a divalent
organic group free of alisphatic unsaturation containing
1-16 carbon atoms and R" is a divalent organic group
free of aliphatic unsaturation containing 2-18 carbon atoms.
The product of the above reaction can then be
quaternised by further reaction with an alkyl halide or
ean be converted to the hydrochloride by acidifieation
with hydrochlorie acid.
Preparation of po_ydimethyl siloxane substituted with dimethyl
aminopropyl groups
In a typical preparation 50 grs of dimethyl-methyl
hydrogen siloxane eopolymer containing approximately 76 di-
methyl siloxane units and 6 hydromethyl siloxane units was
dissolved in 50 mls toluene containing a trace of chlorplat-
inie aeid. The mixture was stirred under nitrogen at 80C,
5.18 grs of N,N-dimethylallylamine in 10 mls of toluene was :
added dropwise, holding the reaetion temperature at 80-90C.,
and the reaetion mixture was stirred for a further 2 hours
and then eooled. Sodium earbonate was added to neutralise
any remaining aeid and the mixture was filtered and rotary
evaporated to remove solvents, leaving a pale yellow fluid
of low viscosity. N~R analysis showed the formation of ,
poly dimethyl siloxane eontaining dimethylaminopropyl groups
at a level eorresponding to a reaction eomple-teness of 80%+,
and a degree of substitution (d.s.) of 0.06.
20 grs of the reaction product was stirred in
100 mls of a 1:1 mixture of dichloromethane and isopropanol
and 1.3 mls of eoneentrated HCl (11.21M) in 10 mls of the
same solvent mixture was added slowly at room temperature.
- 14 -
;~ ~
Following evaporation of the solvent a pale coloured solid
was left and NMR analysis showed this material as having a
proton ratio close to the expected value for the hydrochloride
derivative with no detectable level of t~e starting material.
The siloxane polymer was then made up into a 10% aqueous
emulsion using 20% based on the siloxane weight of a nonionic
emulsification agent (Dobanol* 45E4, a linear C14-Cl~ alcohol
containing 4 moles of ethylene oxide supplied by Shell Inter-
national Chemicals Limited).
* Dobanol is a Registered Trade ~lark.
A similar experimental technique to the above was
employed to produce polydimethyl siloxanes having respective-
ly approximately 40 siloxane units and a d.s. of 0.04 and
72 siloxane units with a d.s. of 0.015.
The concentration of the aqueous dispersions (by
which term is included solutions) which constitute the com-
positions of the invention is not critical and is controlled
by practical considerations. Thus the dispersions should
be concentrated enough not to be wasteful in transit costs,
20 yet should be fluid enough to be poured and to disperse
readily in a usage bath. Usuallv a content of from about
1% to 20%, especially about 3-10% by weight of components
(a) and (b) together is convenient. As stated earlier, the
ratio of the siloxane portion of component (b) to the quat-
ernary softening agent of component (a) should be in the
ratio of 20:1 to 1:100 by weight, preferably from 2:1 to
1:10 and most preferably from 1:1 to 1:5.
The aqueous dispersions may contain other components,
such as emulsifying aids, for instance low levels of the
order of about 1% by weight of nonionic surfactants to aid
dispersion of the usually poorly soluble cationic softeners.
1 5-
, i ,
A wide range of nonionic emulsifiers can be used for this
purpose such as those disclosed in German Patent Application
OLS 2500111 published July 17th, 1975. It is found that use
of emulsifiers is sometimes desirable to aid also the dis-
persion of the silicones in the compositions of the invent-
ion, especially when silicones of relatively high viscosity
are employed.
Highly preferred optional ingredients also include
nonionic fabric treatment agents such as the fatty acid
partial esters of mono- or polyhydric alcohols or anhydrides
thereof having from 1 to about 8 carbon atoms in the alcohol.
In these compounds the fatty acid ester should have at least
1, more preferably at least 2, fatty acyl groups.
The alcohol portion of the ester can be ethylene
glycol, glycerol, diglycerol, xylitol, sucrose, erythritol ,
pentaerythritol, sorbitol or sorbitan; sorbitan esters are
particularly preferred.
- 15a -
'~
, ,
$~i
, ~
The fatty acid portion of the ester normally comprises a
fatty acid having from 12 to 22 carbon atoms, typical examples
being lauric acid, myristic acid, palmitic acid, stearic acid
and behenic acid.
Amongst these esters, the most preferred are the glyceryl
esters of stearic acid, especially glyceryl monostearate, and
the sorbitan fatty acid esters, which are esterified
dehydration products of sorbitol.
These sorbitan fatty acid esters are disclosed in Canadian
Patent 1,074,965. Nonionic fabric conditioning materials of
this type are commonly employed at levels of 1 - 5% preferably
2 - 4% by weight of the composition.
Other preferred ingredients include pyrodextrins such as
British Gum and White dextrin and substituted dextrins such as
dextrin phosphates, cationic dextrins and dextrin pyrollidone
carboxylic acid, in which the degree of substitution is from
0.01 to 2.0 preferably 0.05 to 1.5. A preferred cationic
dextrin is a white dextrin that has been reacted with glycidyl `
trimethyl ammonium chloride to provide a degree of substitu-
2Q tion (d.s.) in the dextrin molecule of from about 0.1 to 1Ø
The dextrins are used at levels of 0.5% to 5% by weight of the
compositions, preferably at levels of 1% to 3%.
Non-aqueous, water miscible solvents may be present, and
other viscosity controlling agents, such as low levels of
electrolytes. Other optional components include appropriate
optical brighteners, fungicides and germicides, colouring or ~`~
opacifying agents, and perfumes.
In use the compositions of the invention are normally
incorporated in an aqueous bath containing the ingredients of
3Q the compositions in the ratios defined hereinabove, at a con-
centration such that there is present from about 20 to 1,000
parts per million by weight of components (a) and (b) together
of which at least 10 ppm is component (b). Preferably the bath
- 16 -
",. ~
"; ,~ .
contains from about 50 to 200 ppm of components (a) and (b)together of which at least about 15 to 150 ppm is component
(b).
The invention also embraces a method of treating
textile and textiles when so treated, which method comprises
steeping them in such a bath.
The textiles may be steeped in such a bath and
then dried on any occasion, but it is envisaged that normally
the treatment will constitute the final rinse after a wash-
ing process.
EXAMPLES
Test Procedures
Clean test pieces of cotton or other fabric were
treated in a domestic washing machine. Either a whole
standard load was made up of test pieces or additional
clean fabrics were used to make up the load. The machine
cycle was set so that the load was subjected to gentle
agitation (as for a wool wash cycle) for about 20 minutes
in a solution of the test product in water, and was then
spin-dried.
Wrinkling test
Treated test pieces were compared with a standard
set of 10 plastic simulated test pieces of different degrees
of wrinkling (American Association of Textile Chemists and
Colourists - Three dimensional durable press replicas for
use with AATCC Test 124). Number 10 graded perfect, Number
1 worst. A grade 5-7 was deemed to represent about that
degree of freedom from wrinkling at which a housewife might
be expected to consider ironing unnecessary.
- 17 -
i,~ "
.. . . . ...
Ease of Ironing test
This was judged by a panel of judges, employing
a Scheffe analysis to provide gradings (panel score units -
psu) and a "yardstick", i.e. least dif~erence significant
at 95% probability.
Ena Result test
A visual preference, graded as above in psu.
Softness test
A tactile preference, graded as above in psu.
Drying of Fabrics
The "spin-dried" test pieces were dried by hanging
in the laboratory (static drying) or in a tumbler dryer.
A number of compositions in accordance with the
invention were made up and tested for ease of ironing, wrinkle
grade, ironed end result and softness, using a commercially
available fabric softening product containing 5O8% di-
tallowyl dimethyl ammonium chloride as the standard.
Positive figures denote an advantage for the test product
and vice versa. An asterisk denotes a significant differ-
ence at the 95% level of confidence.
Formulation Levels
1 2 3 4 5
N-tallowyl, N-methyl N'dimethyl
-1,3-propane diamine hydroacetate 4 4 4
N-tallowyl, N-methyl N'dimethyl
- -1,3-propane diamine
hydrochloride 4 4
Glyceryl monostearate 2 2 2 2.5 4.5
Releasil~ (anonionic emulsified
30 polydimethyl siloxane of viscosity 3
100 cs) available from Dow Corning 2 2 2 2 1.5
Unmodified White Dextrin 3~01
- 18 -
... ,~.~ .. .. ... . , , ,, ~ ,
Cationic pyro dextrin 2,92
Ease of ironing +0.78* + .82* +1.2* 1.2* +0.92*
Wrinkling +0.32* +n . 04 -0.3* +0.28 +0.02
Ironed end result-0.10 -0.26*+0.3* +0.22*
Softness +0.3 +0.56* -~1.24*
1. White dextrin supplied by Remy, Belgium.
- 2. Reaction product of glycidyl trimethyl ammonium chloride
with white dextrin to give a d.s. of 0.85.
3. Q2-1070 - A nonionic emulsified polydimethyl siloxane of
viscosity 350 cs available from Dow Corning.
It can be seen that the compositions of the inven-
tion provide an improvement in ease of ironing and, with one
exception, an improvement in wrinkle grade of the fabrics
prior to ironing, and in ironed end result. Softness of
the treated fabrics was also enhanced in those instances
where this variable was measured~
.
~,
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