Antistatic composition

A textile treatment composition comprises a water insoluble quaternary ammonium salt and a non-ionic surfactant containing at least one long-chain alkyl or fatty acid substituent and a hydrophilic group. The quaternary ammonium compound preferably has three large alkyl substituents of at least carbon atoms each and the surfactant may be selected from phosphine oxides, sulphoxides, or tertiary amine oxides, especially the latter. The compositions may be diluted with water and applied to textile materials especially wool, to give antistatic properties thereto. Compositions of the invention have lower soiling propensity than hitherto available compositions and they may therefore be applied to finished carpets, either in the piece or in situ applications.

This invention relates to an antistatic composition for textiles and more 
particularly for carpets, and to methods of using same. 
Static electrical charges are generated on a person's body when traversing 
carpeted areas, due to the contact electrification at the shoe sole-carpet 
interface, and the subsequent distribution of this charge over the body 
creates a `body voltage`. The tendency to generate high body voltages is 
particularly pronounced at low relative humidities. Such static 
electricity not only causes objectionable shocks when the body is 
discharged to earth, but can cause serious problems with electronic 
equipment, present a hazard in the presence of flammable gases (notably in 
operating theatres), and cause problems during treatment such as pick-up 
of lint and other adventitious material when dry fabrics or garments are 
being handled. 
Carpets, including wool carpets, may be rendered free from static 
electricity by incorporating therein various types of conductive fibres of 
filaments, used either with or without a conductive primary backing or 
conductive latex compound. However such an expedient is relatively 
expensive, and cannot be employed with already made carpets. 
Alternatively, chemical treatments of various kinds may be applied to the 
carpet pile fibre to assist in the prevention or dissipation of static 
charges. One such treatment involves quarternary ammonium compounds. A 
particular compound, trioctyl/decyl methyl ammonium chloride available 
commercially as Aliquat 336 (Henkel), and Adogen 464 (Sherex Chemical Co), 
contains three large alkyl substituents on the nitrogen and is thus 
water-insoluble. 
British Patent publication No. 2081731 discloses a composition in which the 
insoluble quaternary compounds is mixed with a polyether compound. Such 
compositions (usually homogeneous themselves) have the property that when 
diluted with water to working strength for the most commonly employed 
application techniques they form a homogeneous solution or a dispersion of 
the quaternary compound which can be readily applied to textiles. 
However the polyether compounds employed may give rise to soiling problems 
if not removed before use of the carpet, and thus the application of these 
compositions is effectively precluded for in situ treatments or in 
piece-finishing. 
The invention seeks to provide a composition which gives an acceptable 
antistatic finish to textiles, which is economical and easy to use, and 
which overcomes or reduces the above disadvantages. 
According to the broadest aspect of the present invention there is provided 
a textile treatment composition which comprises a water-insoluble 
quaternary ammonium salt and a non-ionic surfactant containing at least 
one long-chain alkyl or fatty acid substituent and a highly dipolar 
hydrophilic group. 
Preferably, the surfactant may be selected from the classes: phosphine 
oxides, sulphoxides or tertiary amine oxides, especially the latter. 
According to another aspect of the present invention there is provided a 
method of imparting antistatic properties to textile materials which 
includes treating the material with an aqueous solution of a composition 
as defined above. 
The textile materials are advantageously keratinous materials, for example 
wool, and may be in the form of carpets, piece goods, knitwear, yarn, 
roving, slubbing or loose stock. 
The water-insoluble quaternary ammonium salts may be those in which the 
nitrogen atom has three large alkyl substituents, preferably of at least 
eight carbon atoms each. A particularly useful product is available 
commercially under the name Aliquat 336 (Henkel). 
It has been found that one class of surface-active compound is particularly 
effective in producing homogeneous compositions when mixed with 
water-insoluble quaternary ammonium salts and appropriate amounts of 
water. Further, these compositions also produce dispersions or homogeneous 
solutions when diluted with water to the working strength appropriate for 
commercial application. Particularly effective within this class of 
surfactants are the tertiary amine oxides; for example, lauryl dimethyl 
amine oxide as typified by the commercial product Ammonyx LO (Onyx 
Chemical Compamy). Other surfactants containing similar dipolar 
hydrophilic groups, such as the sulphoxide and phospine oxide surfactants, 
may also be used. For example a typical sulphoxide surfactant, lauryl 
methyl sulphoxide, behaves similarly to lauryl dimethyl amine oxide, in 
solubilising water-insoluble quaternary ammonium compounds in dilute 
aqueous solutions. In general any nonionic sufactant containing at least 
one long alkyl or fatty acid substituent and a hydrophilic group may be 
employed, and examples of such compounds other than thosealready mentioned 
are the sugar esters. 
The weight ratio between the surfactant and the quaternary ammonium 
compound in the composition of the invention will depend on a number of 
factors, including the exact chemical types selected, expected dilution 
level, active percentage of pure chemical in commercial supplies, and so 
forth. 
Amine oxide surfactants, for example, are commonly sold as aqueous 
solutions or pastes. For example, Ammonyx LO is supplied as a 30% active 
aqueous solution. Compositions ranging from a ratio by weight of Ammonyx 
LO (30% active by mass) to Aliquat 336 of 1.7 to less than 0.5 (i.e., a 
ratio of from 0.51 to less than 0.15 based on active amine oxide) form 
clear homogeneous mixtures upon combining and stirring the two components. 
When diluted with water, mixtures ranging in the above composition ratio 
from more than 3.2 to 1 (0.96 to 1 based on active amine oxide) will on 
high dilution form true homogeneous solutions at working concentrations 
for exhaustion processes up to at least the greatest dilution of practical 
interest, which is a concentration of about 50 parts per million Aliquat 
336 in the solution. 
The concentration of Aliquat 336 in dilute solution at which separation 
into two phases just commences has been approximately determined for a 
range of initial ratios of Ammonyx LO/Aliquat 336 concentrations. If the 
ratio by mass of the two materials is R, and the solubility limit of the 
cationic compound in % (w/w) is Q, the relationship between the two over a 
considerable range is approximately given by R=2.0 Q+0.8. 
In the case of lauryl methyl sulphoxide, rather similar behaviour occurs, 
but with homogeneous phases existing over more restricted composition 
ranges. Lauryl methyl sulphoxide is soluble in Aliquat 336 at a ratio of 1 
part to 10 by weight, but at 1 part to 5 it precipitates. The solubility 
is enhanced, however, by adding small quantities of water, and for 
instance a composition of 5 parts Aliquat, 2 parts lauryl methyl 
sulphoxide, and 3 parts water is a clear homogeneous solution. Such a 
mixture when diluted to a concentration of 0.075% of Aliquat by weight 
gives a clear solution, part of which when analysed for Aliquat gives the 
correct nominal concentration. Such preparations thus appear to be genuine 
solutions comparable in their utility to the preparations with amine 
oxides. At a concentration of 0.15% in Aliquat, such a preparation gives 
by contrast a heterogeneous system. 
As the amount of Aliquat is increased, the system Aliquat/Ammonyx LO/water 
separates into two phases. At very low additions of water, a single phase 
is again produced. 
Such amine oxide compositions may be used as in the examples given below, 
to give antistatic treatments of wool or wool-rich carpet pile with a high 
degree of permanence and durability to wear and wet cleaning. The 
compositions may be applied, inter alia, by the following methods: 
1. application by exhaustion in a batch process to yarn in a hank dyeing 
machine or similar vessel, or to loose wool in a loose wool (stock) dyeing 
machine or similar vessel; 
2 application by exhaustion in a continuous process in a yarn scouring 
machine or similar device; and 
3. application as a component of a spinning lubricant formulation 
In addition, two further application procedures are particularly 
advantageous with the present compositions. The first is to laid carpets 
in situ using a shampoo machine or spray. The second is to carpets in the 
piece during manufacture by either spray or foam application techniques. 
In these procedures there is a particular advantage of compositions of the 
invention over polyether compositions, arising from the much lower amount 
of solubilising surfactant employed in the former, and its greater 
substantivity on the fibre, which factors both reduce the soiling 
propensity of the compositions to an acceptable level thus allowing the 
use of compositions as a topical shampoo application or piece finishing 
treatment. 
Another characteristic of the present compositions pertinent to in situ 
application by shampoo machine or piece treatment is that in many cases 
where two phases are present, especially at relative proportions not far 
removed from regions of single-phase formation, the system forms a 
pearlescent mixture that is readily dispersible to a stable emulsion 
suitable for practical use. This is in marked contrast to emulsions of, 
for example, Aliquat alone, which separate into relatively non-dispersible 
layers. 
Compositions employing amine oxides have a further advantage in 
piece-finishing methods involving foam application, in that the amine 
oxides, as is well-known, are excellent foam-stabilising surfactants, and 
the diluted formulation can be readily foamed to high blow ratios, thus 
minimising the wet add-on required and the consequential drying problems 
in carpet finishing. 
In exhaustion treatments carried out as disclosed in UK patent publication 
No. 2081731, the cationic Aliquat 336 substantially exhausts from the 
solution but the solubilising surfactant, whether polyether or amine 
oxide, remains predominantly in the solution and is discharged to waste. 
Thus, the superior soiling propensity of the present compositions is not 
fully realised in such exhaustion applications. Nonetheless, the lower 
soiling propensity of the present compositions, particularly amine oxide 
preparations, is an advantage over the polyether type formulations. 
A further advantage of the present compositions is that, for example, the 
tertiary amine oxides are fairly effective short-term antistatic agents in 
their own right. The tertiary amine oxides may thus be regarded to some 
extent as an additive to the antistatic effect rather than merely 
conferring a solubilising action on the antistatic agent. 
The invention will be illustrated further in the following Examples.

EXAMPLE 1 
Hank-exhaustion treatment (commercial hank treatment, pilot plant carpet 
make-up) 
Wool yarn (R600/2 tex, standard Axminster yarn) was commercially treated in 
a dye vat after hank dyeing, with 0.9% o.w.w. of 1:1 Aliquat 336:Ammonyx 
LO mixture, for 20 min. at 20.degree. C. After drying, a sample of the 
yarn was tufted a small piece of carpet, of 5/32" gauge construction with 
24 stitches/dm and 10 mm pile height. This was backed with a standard 
non-conductive carpet latex and a secondary jute back. The body voltages 
recorded at 21.degree. C., 20% rh (by a method similar to AATCC Method 
134-1979 were as follows: 
______________________________________ 
Stepping Walk 
Scuffing Walk 
______________________________________ 
Rubber soles -1000 -1600 
Leather soles 
+1800 +2000 
______________________________________ 
A comparable untreated carpet produces voltages in the range -10,000 to 
-15,000 volts, and a treatment giving body voltages of less that .+-.2500 
is regarded as adequate. 
EXAMPLE 2 
Continuous Brattice Scour Treatment (commercial batch, commercially woven 
carpet). 
A brattice scour bowl liquor was made up to a concentration of 0.06% (w/w) 
in Aliquat 336 by dissolving 2.4 kg of Aliquat 336/Ammonyx LO mixture in 
the bath at ambient temperature. Hanks of 80/20 wool/nylon yarn (450 grams 
each) were passed through this bowl, at a rate of approximately 30 hanks 
per minute, with a 2 min. residence time. A 5% w/w dispersion of Aliquat 
336/Ammonyx LO mixture (1:1) was metered in at a rate of about 1680 
ml/min, giving an add-on assuming bath equilibrium of 0.39% w/w of Aliquat 
336 on the wool component of the yarn. 
An Axminster carpet was then woven, predominently from the yarn treated as 
above, with other lots treated similarly also included in the pattern. 
This was a 7-shot, 7-pitch carpet of 7 mm pile height. When tested for 
static at 21.degree. C., 20% rh, the following results were obtained: 
______________________________________ 
Body Voltages, volts (3-sec. time constant) 
Stepping Walk 
Scuffing Walk 
______________________________________ 
Rubber soles +1700 +900 
Leather soles 
+1600 +1300 
______________________________________ 
Such a treatment has, then produced an acceptable level of body voltage. 
EXAMPLE 3 
Applications by Exhaustion on to Stock-dyed Wool 
Scoured loose crossbred wool (14 kg) was dyed in the stock carrier of a 
GRU-15 dyeing machine, with a typical premetallised dye recipe. An Aliquat 
336/Ammonyx LO mixture (equal parts by weight, 140 g in all, 0.5% Aliquat 
336 oww) was dissolved in the side tank at 20.degree. C., and the liquor 
transferred to the dyeing vessel containing the wool and circulated for 20 
min. The liquor was then dumped, and the wool hydroextracted, dried and 
converted to yarn (R600/2 tex, 140 tpm, folding twist). 
The exhaustion of the Aliquat 336 from the treatment liquor was 91%. 
The yarn was scoured in a commercial tape scour (4 bowls, 3 at 60.degree. 
C., the last at 50.degree. C., Teric GN9 nonionic detergent in first two 
bowls) and then tufted into a cut-pile carpet (5/32" gauge, 7 mm height, 
40 stitches/dm, backed with latex and a secondary backing of jute). 
Static tests were carried out on this carpet in the same way with the 
following results for body voltages: 
Rubber soles, stepping walk: =1000 
Leather soles, stepping walk: 0 
In this experiment, small yarn samples were placed uniformly within the 
loose wool in the stock carrier, and were subsequently analysed for 
Aliquat 336 by the ether extraction of the Orange II dyestuff complex. 
The results showed that the treatment was satisfactorily level, the 
quantity of Aliquat 336 recovered from the six yarn samples averaging 
0.152% (m/m) with a standard deviation of 0.024. 
It is noteworthy that in this Example the quantity of Aliquat 336 remaining 
on the yarn after scouring is such as to yield a body voltage close to 
zero. 
EXAMPLE 4 
Application as a Component of a Woollen Processing Lubricant 
Undyed loose wool (10.5 kg) was oiled during blending by hand spraying with 
3 litres of a mixture prepared by diluting with water a concentrate of 315 
g of Frescolene B and 105 g of 1:1 Aliquat 336/Ammonyx LO mixture. The 
concentrate in this case was homogeneous but the diluted material was a 
fairly stable dispersion. The wool was carded and spun on the woollen 
system to yarn as before (R600/2 tex, 140 tpm ply twist), scoured as in 
the stock dye application example above, and tufted to the same carpet 
construction. The body voltages obtained from a test at 21.degree. C., 20% 
r.h., were: 
Rubber soles, stepping walk: +800 
Leather soles, stepping walk: +1400 
A completely homogeneous lubricant formulation which yields similar results 
may be made by modifying the mixture somewhat. For example, a concentrate 
consisting of 50 g Aliquat 336, 150 g Ammonyx LO, and 250 g Frescolene B 
is homogeneous and when diluted to 2.5 liters for application to wool (10 
kg) remained homogeneous. Such formulations have advantages in practical 
applications over heterogeneous mixtures. 
EXAMPLE 5 
Application in Foam Form to Carpet Pieces 
Aliquat 336 - amine oxide preparations are suitable for application to 
carpet pieces by either spraying or foam application. The latter has 
decided advantages in terms of uniformity and control of add-on and 
penetration, and minimising of water to be subsequently removed in drying. 
A typical foam application is detailed in the following example. 
A dispersion of 1:1 Aliquat:Ammonyx LO (2% w/w) was pumped to the foaming 
head of a carpet latex foaming unit, and foamed therein at an air delivery 
pressure of from 6-10 psi to produce a foam with a blow ratio of from 15 
to 22. This foam was delivered to a foam trough mounted above a revolving 
horizontal roller. The trough was equipped with a variable aperture and 
doctor blade so as to enable a uniform foam layer from 6 to 20 mm thick to 
be carried away by the roller, and delivered down a glass scraper blade 
bearing against the roller just below the level of its horizontal axix. 
The foam layer then was allowed to flow from the lower edge of the scraper 
blade to a carpet passing horizontally immediately beneath it. The carpet 
was subsequently drawn across a vacuum slot approximiately 4 mm wide, to 
which suction was applied via an ordinary vacuum cleaner. 
By appropriately varying the foam add-on, liquor concentration, and 
suction, it is possible to get satisfactorily uniform foam penetration 
into the carpet. 
A dense carpet was treated with 20 mm height of foam at a blow ratio of 
15:1, prepared from the dispersion described above, passed slowly over the 
vacuum slot, dried, and assessed for uniformity of foam penetration by 
staining the carpet in cross-section with Orange II. This revealed fairly 
uniform uptake of Aliquat at all levels in the pile. Different antistatic 
levels can be achieved by varying the concentration of the starting 
dispersion. 
EXAMPLE 6 
Application by hand-held airless spray to wool carpet 
A stable turbid emulsion of 1.8% of an Aliquat 336/Ammonyx LO mixture 
(50/50 w/w) in water was applied by hand-held airless spray ("Fanjet" 
123/15 "D" with 1.09 mm hole), using a conical device for fully enclosing 
the spray and preventing Aliquat particles from being breathed in by the 
operator. The mixture was sprayed on to 100% wool, tufted carpet, cut 
pile, with a surface pile weight of 650 g/m.sup.2, at the rate of 50% wet 
add-on on the surface pile weight, spraying at the rate of 725 ml/min in 
18 cm wide paths, to give a total add-on of Aliquat 336 of 0.5% on weight 
of pile fibre. The same carpet was also spray extraction cleaned, with 
water only, as an additional experiment, using a conventional spray 
extraction cleaning machine with a pull-back floor tool. 
After drying and conditioning both treated and untreated carpets at 
23.degree. C. and 25% R.H. the following body voltages were measured 
(values in volts): 
______________________________________ 
Neolite 
BAM 
Rubber Rubber PVC 
______________________________________ 
Untreated (control) 
-13,000 -10,250 -9,750 
Treated +1,400 0 +400 
Treated and cleaned 
+1,700 +250 +700 
______________________________________ 
The effect of the spray extraction cleaning is to very slightly increase 
the positive body voltage generated. 
EXAMPLE 7 
Application by hand-held spray to synthetic carpets 
The general procedure of Example 6 was carried out in a range of synthetic 
carpets as follows: 
a 100% acrylic carpet, tufted, cut pile, secondary backed 
a 100% polyester carpet, tufted shag pile, secondary backed 
a 100% polypropylene carpet, tufted, loop pile, secondary backed 
a 100% nylon carpet, tufted, velved, foam backed 
to give approximately 0.7% Aliquat 336/Ammonyx LO 50/50 mix of 0.35% o.w. 
fibre, Aliquat 336. The carpets were dried at ambient temperature, and 
conditioned to 23.degree. C./25% R.H., then tested for antistatic effects. 
______________________________________ 
Static Test results 
NEOLITE BAM PVC 
______________________________________ 
U/T Polyester +3,200 +10,750 4,750 
Treated +50 0 0 
U/T Polypropylene 
+ -200 -50 
Treated -50 0 -50 
U/T Acylic +1,100 +6,400 +4,100 
Treated +100 0 0 
______________________________________ 
It can be seen that improved antistatic effects are obtained on all the 
carpets treated. 
EXAMPLE 8 
Use in Knitwear 
A batch of fully fashioned knitwear wool sweater bodies was treated in a 
side paddle machine after drying with 0.9% oww of 1:1 Aliquat 336:Ammonyx 
mixture for 4 minutes at 20.degree. C. 
The goods were hydroextracted and dried in a tumble dryer. On removing from 
the tumbler the goods were completely free from electrostatic effect and 
were easy to handle during subsequent sewing, and picked up no lint 
fromthe sewing tables. A comparable bateh which had not received the 
antistatic treatment required careful brushing and picking before the 
garments could be packed. 
EXAMPLE 9 
Effect of Tertiary Amine Oxide Preparation on Soiling 
The improvement found in the soiling properties following an Aliquat 
336/tertiary amine oxide treatment compared to those of previously 
disclosed commercial formulations of the polyether type is exemplified in 
the following. 
Woollen carpet yarn (approximately R500/2 tex, normal twist level) dyed to 
a yellow-beige colour was treated by exhaustion in a hank dying machine 
with one or other of the following treatments: 
b 1. with 0.6% oww of Aliquat 336 contained in an Aliquat 336/Ammonyx LO 
concentrate (1 part to 3.3 parts by weight, of 1:1 on an active matter 
basis); 
2 with 0.6% available Aliquat 336 from a polyether composition. 
These treated yarns were converted into carpet of construction similar to 
those used previously. 
These carpets were then laid in a floor trial in a busy commercial arcade, 
together with an untreated woollen velour carpet of comparable colour and 
structure. Tristimulus values were measured on these carpets at intervals 
and were converted to colour difference (E) values using the CIELAB 
formula. 
______________________________________ 
E values at various tread counts 
3000 
treads 
12500 24300 44000 
______________________________________ 
std woollen velour 
8.2 11.2 14.1 16.4 
amine oxide recipe 
4.8 8.6 10.9 12.9 
polyether recipe 
11.0 14.3 17.7 19.9 
______________________________________ 
This experiment, which lists the average faults for duplicate samples in 
the trial, indicates that the amine oxide type of formulation has a 
significant benefit in reducing subsequent soiling compared to the 
polyether type of formulation. 
Although all the examples of soluble formulations, stable dispersions, and 
application procedures given above are expressed in terms of specific 
products, comparable results will be achieved with other formulations 
within the scope of the invention which involve the solubilisation of any 
quaternary ammonium compound normally having very restricted water 
solubility, irrespective of the nature of the substituents on the nitrogen 
or the incorporation of the nitrogen into ring systems. Exemplary amine 
oxide-type surfactants include, in addition to the cited lauryl dimethyl 
amine oxide, related compounds such as stearyl dimethyl amine oxide, 
compounds in which the nitrogen of the amine oxide is in a heterocycle, as 
in N-dodecylmorpholine oxide, and in imidazoline oxides, compounds which 
are diamine oxides, such as N-dodecyl-N, N', N'-trimethyl-1. 3-propylene 
diamine-N, N' dioxide, and other substituted propylene diamine derivatives 
such as products of the Ethoduomeen T/13 N, N' dioxide commercial class. 
All comments made above in reference to the uncharged form of tertiary 
amine oxides as found in basic or neutral solution apply also to the 
hydroxylammonium cation forms of these compounds formed in acid solution. 
Sulphoxide surfactants behave similarly to amine oxide surfactants in 
forming homogeneous solutions of water-insoluble quaternary ammonium 
compounds, and all the application procedures and uses of the amine oxide 
formulations apply to suitable sulphoxide surfactant preparations also, as 
well as phosphine oxide surfactants and other nonionic surfactants as 
previously described.