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Patent 2024600 Summary

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(12) Patent Application: (11) CA 2024600
(54) English Title: HIGH MOLECULAR WEIGHT ACRYLIC ANTI-STAIN TREATMENT FOR NYLON CARPET
(54) French Title: TRAITEMENT ANTI-TACHES PAR COMPOSE ACRYLIQUE A POIDS MOLECULAIRE ELEVE POUR MOQUETTES EN NYLON
Status: Dead
Bibliographic Data
(52) Canadian Patent Classification (CPC):
  • 117/205
  • 402/513
  • 8/93.19
  • 8/93.78
(51) International Patent Classification (IPC):
  • C08F 220/06 (2006.01)
  • D06M 15/263 (2006.01)
(72) Inventors :
  • BLANKENSHIP, ROBERT M. (United States of America)
  • MORRIS HAL C. (United States of America)
  • BLANKENSHIP, ROBERT M. (United States of America)
  • MORRIS HAL C. (United States of America)
(73) Owners :
  • BLANKENSHIP, ROBERT M. (Not Available)
  • MORRIS HAL C. (Not Available)
  • BLANKENSHIP, ROBERT M. (United States of America)
  • MORRIS HAL C. (Not Available)
(71) Applicants :
(74) Agent: GOWLING LAFLEUR HENDERSON LLP
(74) Associate agent:
(45) Issued:
(22) Filed Date: 1990-09-04
(41) Open to Public Inspection: 1991-03-16
Availability of licence: N/A
(25) Language of filing: English

Patent Cooperation Treaty (PCT): No

(30) Application Priority Data:
Application No. Country/Territory Date
408,053 United States of America 1989-09-15

Abstracts

English Abstract



ABSTRACT

Described is a method for treating fiber with a durable anti-
stain agent containing a copolymer of 1-20 weight % acrylic
acid and about 80-99 weight % methacrylic acid, that has a weight
average molecular weight greater than 80,000, preferably above
1000,000, more preferably above 130,000, and a fiber impregnated with
such an anti-stain agent. The anti-stain agent can be used in
treating carpets made of nylon 6 and nylon 66 fiber and effectively
withstand carper shampooing.


Claims

Note: Claims are shown in the official language in which they were submitted.



We claim:
1. In a method for treating fiber with anti-stain agent, the
improvement wherein the anti-stain agent comprises a copolymer of
about l to 20 weight percent acrylic acid and about 80 to 99 weight
percent mothacrylic acid, said copolymer having a weight average
molecular weight greater between about 80,000 and 350,000.
2. A method as recited in claim 1, wherein the weight average
molecular weight is between about 100,000 and 250,000.
3. A method as recited in claim 1, wherein the weight average
molecular weight between about 130,000 and 200,000.
4. A method as recited in claim 1, wherein the fiber is nylon
6 fiber or nylon 66 fiber.
5. A method as recited in claim 1, wherein the fiber is in the
form of a carpet.
6. A method as recited in claim 1, wherein the copolymer is of
about 5 to 15 weight percent acrylic acid and about 85 to 95 weight
percent methacrylic acid.
7. A method as recited in claim 1, wherein said anti-stain
agent is applied in an about between about 0.8 and 10.0 weight
percent of the fiber.
8. A method as recited in claim 1, wherein the fiber is nylon
or amide fiber.




9. A fiber material comprising fiber impregnated with an anti-
stain agent comprising a copolymer of about 1 to 20 weight percent
acrylic acid and about 80 to 99 weight percent methacrylic acid, said
copolymer having a weight average molecular weight between about
80,000 and 350,000.
10. A fiber material according to claim 9, wherein the weight
average molecular weight is between about 100,000 and 250, 000.
11. A fiber material according to claim 9, wherein the weight
average molecular weight is between about 130,000 and 200,000,
12. A fiber material according to claim 9, wherein the fiber
is nylon or amide fiber.
13. A fiber material according to claim 9, wherein the fiber
is nylon 6 or nylon 66 fiber.
14. A fiber material according to claim 13, wherein the fiber
is in the form of a carpet.
15. A fiber material according to claim 9, wherein the fiber
is in the form of a carpet.
16. A fiber material according to claim g, wherein the
copolymer is of about 5 to 15 weight percent acrylic acid and about
85 to 95 weight percent methaorylic acid.
17. An anti-stain agent for fibers, comprising a copolymer of
about l to 20 weight percent acrylic acid and about 80 to 99 weight
percent methacrylic acid, aid copolymer having a weight average
molecular weight between about 80,000 and 350,000.
18. An anti-stain agent as recited in claim 17, wherein the
weight average molecular weight is between about 100,000 and 250,000.




19. An anti-stain agent as recited in claim 17, wherein the
weight average molecular weight is between about 130,000 and 200,000.
20. An anti-stain agent as recited in claim 17, wherein the
copolymer is of about 5 to 15 weight percent acrylic acid and about
85 to 95 weight percent methacrylic acid.

17

Description

Note: Descriptions are shown in the official language in which they were submitted.


~2~




. HI~ MOLECULAR ~E~R~
ACRYLIC ANT~-ST~ REATMENT
FOR NYLON CARPE~
__ ... ..... _

The ~r~sent invention relates ta an improve~ s~ain-re~ stant
composition for treatlng carpet. Specifically, thQ invention
. relates to high m~l~cul~r wet~ht ~eirylio materialx ~hleh are
relatively durable and resist~nt ~ ~hampooill~. In particular, th~
. 5 in~ention relat~ to A ~tain^re.si.stant carpet treatm~nt for carpets
made o~' nylon or amide fibers.
~ylon carpetln~ m~ke~ up a lar~e per¢ent~e of the carpet
. lndustry. Nylon 6h fib~r and nylon ~ iber are u.sed in carpet~.
. Nylon 66 .is more crystalllne than nylon 6, thus limiting th~ depth
of ~hade developed durin~ dy~ln~ of nylon 66 a~ ~ell ~s
beneflcially llmitlng its staining. Conver~ely, with nylon 6 an
Advanta~eous depth of shadc 1~ possible; h~wever, nylon 6 suf~erg
from the drawba~k that known stain-ro~i~tant tr4atmont~ ar~
ef~ctlvc on the fl~er~.
Known 3tain-re~ nt tre~tm~t~ for oarpet~ ~on~alning nylon

flber inolude sulfonated naphthol/phenol ormaldehyde condensates
and dihydroxy diphenyl sulfones. However, in treating fibar~ Inade
. of nylon 6, relatively hi~h level~ of ~n~wn stain-resi.stance
material ar~ req~ired. ~hi~ impart~ a stiffer han~ to the flber
and, despite the increased level, the material~ ar~ mor~e easily
removed durlng shampoolng of the carpet.
Furthermore, the known naphth~l~p~enol conden~ate~ and sulfone

compounds, which a~t ag clqa~ dyes, have sig~flcant disadvantages.


202~0a




80th material~ alter the color of the treat~ carpo~ ya~n,
espeoially ~n nylon 6 where higher levels are reguired.
Addltlonally, the kno~n materials yellow signifiGantly ~hen ex~o~d
to ultraviolet ( W ) light, an~ are of questionable e~oloyical
s~fety.
A ~tain-resi~tant treatment u~ing a ~lend o~ a methacrylic
acld oligomer with a g~aft copolymer of me~ha~rylic aoid flnd
. sulfonated castor oil has been found to have an adv~ntage over the
. phenolias and ~ulfones in color stabili~y.
An ob~ect of the present invention is to develop an effecti~e,
durable stain resistant treatment for fiber, part1cula~ly nylon
fib~r.
A fur~her ob~ect of thl~ lnvention is to pro~ide ~n improved
stain-resist~nt material for nylon ~arpet whlch conforms with
. 15 current carpet m~nufacturin~ processe~.
. According to th~ p~esent ~nvention th~r~ provlded an ~nti-
~tain ~gent for nylon c~r~et, and ~n improved method or tr~in~
nylon flber wlth an anti-st8~n a~ent, wh~r~in -the ay~n~ comprises
water-solu~le copolymer ~ from ~b~lt l to about 20 wei~ht
. 20 percent ac~ylic a~i~ and about 80 to abou~ 9~ ~eight p~rcent
meth~rylic a~id, and pre~erably from ~bout 5-15 wei~ht ~ a~rylic
acid and about 8S-9S weight ~ rne~hacrylic a~id, th~t has ~ wei~ht
average mole~ular weight ~MW) between about ~0,004 and 350,000,
prefeI~ably be~ween about lûO, 000 and 750r 000~ more ~eferably
bstw~en ~bout 130, 000 and Z00, 000, as determlned by aqueous gel
permeatlon chromatography ~PC~. The upper limitation on ~he
wel~h~ average molecular weight o~ the copolymer wh~ch ~unction~


.

2~2~6~




in the practlce of the present inves~ti~n is det~rmlned by ~h~ wate~
~olubility, ~i~cosity and practic~l process-of-manuf~cture
req~irement~.
The pre~ent inventLon al~o provide~ a f~ber impre~nate~ with
the ~nti-stain agen~. Op~ion~lly, the antl-~tain Age~t of t~q
present inventlon can be combined with an adJ~Ivant~, such as a
surfactan~, novola~ re~in, ultravi~let-light absor~er, or~anic or
ino~ganiC a~id, antioxldant, eth~xylated or ~ul.~onated fatty acid,
. polymer coating, Gr a mixtur~ thereo~.
. 10 The antl-stain agent of the present lnven~ion is u~eful ln
treatin~ fiber materials, e.~ ibers made from nylon and/or amide
flber, particularly carpet~, to make the~ staln re~istant.
Preferably, the flber used in accordanc0 with th~ pr~n~ invention
is made from nylon 6, wh~ch is a polymer of oaprolactam, or nylon
. 15 ~6, which is a condensation prod~ct of adlpic aci~ and
. hexamethylenedi~min~, which ~re well known in the m~n~factur~ of
carpe~s such a~ dis~lo~ed in U~S. I'~s~t No~ ~,501,5~1 and
. 4,780,4g9, the di~closure~ ef whieh àre incorporated her~in by
reference. Other usef~l nylon ~lbor~ lnclud0 tho~ made from,
e.~., nylon 11, ~hich is a polymer of ll-amlno undec~nolc acid,
nylon 610, which is a polycond~nsation product of ~ebaoic acld and
. hex~methylenediamine, and a copolym~r Gf nylon ~nylon 66, all of
whlch are well known as disclosed in th~ aforesaid U.S. Patent No.
4,501,5~1~
Pref~rably, flber ls treAted ln accordance w$th the pr~sent
invantion by lmmor~ion in an acidio aquaouR bath having a pH

. . 3

202~




between about 1.5 and 5.5, preferably between aho~t ~.1 and 4 . O,
more prefarably between about 2. 5 and 3. 5, oontalnin~ th~ ~nti-
staln agent, which i~ ~aintalned at a preferable temper~tl.lre
between a~out 38 and 110~, more preferably between about 80 and
100C. ~o obtain the best anti-~tain effect, imm~r~lon time v~ies
between abo~t 1 and 20 ~inute~, more preferably between about 5 and
15 mlnutes, most preferably between about 7 and 12 mln~tes. The
amount of anti-st~in agent u~ed in th~ hath veries be~ween about
. 0~ and 10 weight % of the nylon fi~e~ t~ he treated, pref~rably
between about 1.0 and 4~0 weight ~, more preferahly between abou~
1.2 and 3.0 weight ~. Acidit~ of the aqu~ s bath in combination
with eleva~ed temperature i~ mal~tatned to ~ss~re optimum
abso~ption by the nylon fl~er. ~eidQ us~ful t.n maintainin~ the
proper pH include both or~anic and lnorganiG acids, e.g., ac~tic
a~id, sulfamlc a~id, citrlc acid, nitrlç ac~d, formic acld ~nd
phosphori4 ~cid, which are add~d i.n sufficient amount to maintain
. the pH in th0 preferr~d r~n~e. A su~factant i~ ~r~ferAbly ~dd~d
to the bath to as~i~t ln w~ttin~ the nyl~n fiber at an amount
between about 0.~ ~nd 1.5 wei~ht ~ of the nylon fiber to be
t~eated. Useful ~urfa~tants in~.lude non-lonlc ~nd anionlc
surfa~tan~s, e.~., so~l.um sulfosucclnate, dlootyl and dlnonyl
sulfosuccinates, nonyl phenol ethoxalates, linear-alkyl sulfonates
and ~odecylbenzene sulfoni~ aGids. O~her preferable additives,
which ~ay be lntroduced into th~ bath a~ betw~en ~bo~t ~ and 3
weight ~ o~ the nylon f~ber to be treated, include anionic-acid dye
levelers, novol~ res~ns, such as sulPonated naphthol~ph~nol


~ '

2~2~




formaldehydc condensate~ an~ dihy~rox~1r~iphenyl ~,lfone~;
ultraviolet~ h~ a~sorb~r~, e~, ben~phen.on~, sllch a.s 2-

. hydroxy-4-methoxybenzophenono-5-sulfonic a~d, disodlum-~,2'-
dihydroxy-4,4'-~i~et~oxy-5,5'-dis~lfobenzophenone, 2,2',4,~'-
tetrahydroxy4anzophenone, ~,4-dlh~droxyber;z~ph~none, ~-hydro~y-4-
methoxybenzophenone, and 2,2'-~ih~droxy-4,4' dim~thoxy~enzoph~none~
~ntioxidants, such as sodiu~ ~hiocyanate, ethoxylat~d or ~ulfonat~d
fatty a~id3, e.g., coconut Dil, tall o1l, casto~ oil, so~ean oi
and peanut oil; and polymerio coatin~ compounds,
polyvinylchlorlde,, polyviny~3cetate, pol~vinylalc~hol, acryllc.~,
styrenes, and flusrochemic~l compound~ s~ch as ~rlfluo~oethan~.
A typical ca~pet proces~ preferably ~nvolves first dyein~ the
carpet ~o a de~ired color, then saturating the carpe~ in the bath
~ontainin~ the antl-stain a~ent. ~ein~, howev~r, çan be perfor~ed
after, or s.imultaneousl~ with, the stain~re~i~tant treat~ent. In
tr~tin~ c.arpets in accordanc~ wlth the ~r~sent inv~ntlQr
commerclally a~ilable d~eln~ uni.~, ~J~1a,h ~ vF~ hl~ t'~o111 thb
Oting Company er Ku~te.r ~or~o~ ti.on, is advant~eo1l~ly used. ~uch
unlts and their op~rati~n are we~l k1lown as dlsclos~d ln the
.0 afor~id U~5. Pa~ent No~ 4,50l,59l,
A pre~erred proces~ln~ sy~tem for treatin~ carpet is
de~cribed. Th~ c~rpet i~ f~rst wetted, f~r ex~ple with a soiutlo~
containîn~ ~y weiyh-~ 0.~ Triton~ GR-5M ~Rehm ~ Haas) and O.l ~ ~EA
. ~Triethanolamlne~. Aft~r nax~ pas~1A~ thr~ugh nip rollæ, th~
. ~5 carpet then i~ spray-dy~d, ste~med ~nd rinsed. ~he ~tain-resist

trea-tment is ~pplied in the n~xt stage, a~ ccnditlo~s o~ ~bout 160





180~F/4 sec. using a ~uster unit. The carpet i s there~fter ste~me~
a~ , e , ~ ., 2~5F~'12û sec . ~nd linsed Final ly , ths carp~ is passed
throu~h a ~;pray f luorocarbo~l ~re~ment .
In tre~ting flber in ~ccurdanee with th~ pr~3~;Qn~ ;nvention -~he
5 fiber is ~mpragn~tes~ with a ~iufflcient alrlount ~f the ar~ti-~3tain
a~ent to imp~t stain res~tan~e -to the fiber~ Preferah~y, the
amoun~ of anti-~ain ~gent impregnatl d in~ he flber varl~s
between ~bout O . ~ and ~0 . O weight ~ of the nylon f ib~r, m~r~
pr~erabl~ between abou~ O.Z and ~..O wel~ht ~i, mos~ pref~r~
between AboUt O . 3 ~Ind 0. 7S wei~ht. % .
Fiber treated in aceo~dan~3 wttl- -,he present inv~r~tion
exhibits stain l~esistanc:e to a variety of ~ ri el 5, .~:u~.h as foods
and beverages. M~ny such materi~l~ cont~in dye~, ~aleh ;3~ Foo~,
~ru~a and Cosmetic (FD&C) ~ed ~ye 40, th.~t coml~onl~ conle into
contact with carpet~3 when such p~oduct~ ar~ .~eei dentally ~pilled
on the carpet. Howeve~, such dyes are eE~sily ren)o~JP.~ f~om flt~er
carpets treated in ~ccordarlce with th~ ~resent ' ;~ t i.c)~l by l,;.Lmp.1.~n
rinsin~ with w~ter or usln~ ~n ~ eOu~ solut~ of a r~ fl, anion:iG,
carp~t shampoo. Rinse-wat~r temper~tures ar.e preferabl.y rnainl~ained
at about 15-fi54C, mor~ prefer~b:Ly at ,~bout ?.~5-38C.
To more clearly c~escrib0 the presen~ ir~vent.ion, the ~oll.-~winy
non~ itlng e~c~mplss ~re provi~ed. In th~ eic~mple~, all part.~ an~l
percentass~ are by wei~ht ~nl.~s~ lnd~ted oth~3rwi.se. Ir~ the
examples, MW denete~ weight a-~ray~ molecu~ar w~ht determined by
~5 aqueous ~:PC, Mn denote~3 number av~ra~3 r~lolecular weLght, ~nd ~W/Mn
d~3not~ the molecular w~ 3ht d~tribu~lon~



202~a




EXAMPLE 1
Anti-stain agent3 a~c~rdin~ to tha pr~sent 1~vention w~r~
prepared as foll~ws:
~ w~ tho~sand grams o~ DI (deloni2ed) w~ter and 9~ of Q.2% .iro~
sul~ate were ~dded to 3 5-liter 4-necke~ flAsk fitt~d ~ith a
$~ir~er, condense~ and nltro~en inle~. ~hls solution wa~ hea~d
~nde~ a nitrogen a~mosphere to ~0 degree~ C.
A solution of 1~.3g o SMBS ~odium ~etabisulfit~) in 22.a8g
of DI water was prepared. 17.5~g (50 weisht ~) of thi.~ solution
. lO waS th~n added to the flask (l~ SM~ ased on tot~l monomer). To
the flask were yradually and ~3eparate.y add~.d the ~ollowi;~ d~




oJer 1.5 hours: 70g of AA ~acr~rllc ~ci~) ~nd $30g of MA.A

~methacryl1~ ~cid); O.~g ~odium pers1llfate 1~ 7~ DI w~ter, and th~
remainder o~ the SMBS/DI water solutio~ SMBS on total m~nomer~,
15 whilet malnt~ininsJ the ~emperature o~ the flask contel~t~ a~ 70




. degree~ C. The polymoriz~d raaction was continu~d for lS minut~.~
after all the above feed~ were compl.et~ At ~h~ ime w~.~ adc~d




18g of 30~ ~12~ Flftoen min~te.S l~tQr, 1.379g of Dl water w~
added. The ~lask was then allowefl to cool to room temperatura~
~he copolymer so ~orm~d (S~mp.l~ l) had a MW o~ 197,000, Mn of
29,700 a~d MW/Mn of 6.~l~
The ~W o~ the ~opolymer sample~ wa~ varie~ by repeating the
~bove process and va~ying the amo~l~t ~f $MBS ~nd ~he ratio betwe~r
the initial chargo ~t~ the fla~k/kettle~ an~ the amou~t lrem~ind~r)
2S used as co-feed. A copolymer (Sample ~) with MW-~01,000, ~n=~7,300
and ~W/Mn=7.33 wa~ obtsined usln~ OL5~ SMBS ~n to~al monomQr ln the
kettle (in fl~sk initially) with 1~5~ SMBS on t~tal ~o~omer a~ co-



2 ~ 6 ~ ~3




f~ed. At 0. 6~ kettle SMBS an~ 1. 22% ca-f~3d .~MF~S or~ t~.~t~l mollomer,
a copolymer (Sa~ e 3) with MW=~17,000, Mn=29, 000 and MWj~n-~9,000
resu1ted; at U.75~s kf~ttl~ S~S r~nd ~. ~5 co-fed SM~3~ on tot~l
monomer, a copo1ymer ( Sample 4 ) with MW-94, ~300, Mn-~.4, ~00 and
5 MWf!Mn-3 . ~5 wa3 ob~ined: an~ at 0 . 33% kettle S~I~$ and 0 . 33g6 kett~.e
SMBS on total monomer, ~ copo'ylner lSamp1e 5~ wi-tn MW-~.31,000,
Mn-47, 100 and MW/Mn-4. 9 ~.~ produc~

E AMPLE
Arlti~stain ~ nt~ according to the pr~3~ent :iLnvention were ~sl.so
proAIl¢ed by the f~ owing proce~s:
TO a S-1iter 4-neCked 1EISk was added 3000~ nI w~ter, which
was heate~ to 85 degree~ ~ unAer N2. Nine ~r~qm~ of sodi~lm
per~ulfcite ( 1. 5 weiclht % based on to~al manomer ~ in :~0~ DI water
was then added. After two r~linutes, a mi~ture of 6(~g i~A anc~ 5~0q
MAA Wci~ fed ove~ a pe~io~i of or~e hour to the fIac;k, main~ainin~ e
t~r~or~ture ~t 85 de~reer; C, ~ter whi~h :lO35-~ ofi DI wEit~3r was
added. l`he Ela~k wa~ al:lowed t:o c r.~o~ n room t~3mper.ltur~ r~ MW
o the resu~tinS~ copolyn~ ampl~ ~) w~.r.~ 84,000, the Mr~ was 26,300
an~l MW~Mn was 3.1.
Ad~litlon21 c~po1ymer~ WeI'e'. al;sv pre~a:rr d by this rnf3tho~ y
varying the amount of sodi~nl pe~rsulfate~ ~t lr~ ~odillln p~rsul ~te
based on tot~l mon~m~r, a ~o~olyrn~r (Samp1a 7) resulted havin~
MW-124, 00(~, Mn-3~, 400 and MW/Mn 3 .

2~2~




EXAMPLE ~
. As in Exar~ple 1, A co-f~ed of monomer and cat~lys~ wa used,
. The catalyst solution a~ded initlally to the heated reacto~
flask wa~ l~Sg sodium per~ulfate ~n 30~ DI water (0.~5 we~gh~ ~ on
total monomor).
The co-feed wa~ 4. 5g NaaS~08 ln lOOg DI water plus 60~ AA and
154û~ MhA. The co-eeds were ~dde~ separ~tely o~r~ar ene hour. Th3
temperature was ~eld at 9~ de~ree~ C for thirty minute~, and then
gg o~ 0.1~% iron sul~ate solution and 0.8g of t-butylh~droperexid~
10 in 5g of D~ w~ter were add~d . Then, 1. 2g o i~o--ascorbic acid ( IA )
: in 25g ~I w~ter w~ addsd. T~n minut~ later, a second identis~l
amount of IA~DI water was adde~. ~lext, 1035~ DI water was ad~ed
and the reaetion flask was then allowed to ccol to room
temp~rature . The resultin~ copolylner ( Sample 3 ) had a MW-~6, 400.
lSThe above process wa~ repeated under the s~me çondition.~,
except for the oo-feedin~ tim~ and the lnltial an~ co-~
per~entages of sodlum per~.3ulfate ~)n~ed on tot~l monoltler:
Sample 9: 0 .167~ ~odium per~lfa~o ( basecl on total monomor )
wa~ added initi,311y to ~he fla~k, with 0.503% co-fed. The
~0molecular welght of the resultin~ copo1ymer wa~ MW~127,000.
Sampl~ 10~ Utlllzin~ ~odium p~r~ulfate as in S~mple 10, w1th
the ~o-f~ed time lncreased from 1 to 1.25 hours, ylel~ed a
~opo1y~er with MW-12~ 0.
Sampls 11: Utilizing ~odium per~ulf~te ln amo~lnts a~ t
~5 ~orth ln Sample 10, but with the co-feed tlme d~creased from 1 to
. 0.75 hour~, a copolymer W~-Q obtained wlth ~W-135,000.

~2~




Sample 12: 0.125% sodium persulfat~ w~.~ In~ti~lly in the
~lask, and 0.375% sc?diutn persulfat~ was co-~d. ~ha copolymer
produc~ h~d ~ ~w-157,000.

S EXAMPLE 4
Carp~t samples treate~ in accordan~e with the presellt
inven~ion were tested ~or dur~ility ~nd sta1n resist~nc~ in
compari~on with an untreated, un~tained ~ntrol and a ~taine~,
untreatsd cor,trol. ~he carpet S~mplt?S tested were mad~ o~ undy~d,
heat-set nylon ~ fi.ber.
A treatment bath was prepared cont~ining 12~1 part~ deionl~e~
water, 1.25 parts so~ium ~ fosuccinate a~ a 6ur~act~nt ~a~ail~ble
. fro~ Rohm and ~as Company under the name TritonTM ~R-5M), '~.5 parts
acetl~ acid, and ~5 parts of a 1% solid~ aqu~ou~ solution oÇ an
1~ anti-stain agent of the present inv~n~i.on. ~o tr~at a carp~t
sample, t~e bath wa~ brou~.~ht to a b~lil anrt therl t:he .~amp.l.~ a~
ad~ed to the bat.h an~ ~olled ~ b~ elllni~ t.e~-;. Att~r t?oilin~J,
the samp.l~ was centrlEuge~ ~n~t therl t.lrie~ ~t çlbo~t 1l6bC for about
8-10 minutes.
The treated ~ample was sh~po~A to demon~3trat~ th~ d~r~billty
of the anti-staln tr~atm~nt. 'rhis wa~ per~crm~d by dipping tne
s~mple into a 2.11~ aqueous s~luti~n of a ca~pat shampeo oontainin~
e~hylenediaminate~r~-aoetic acld t~rasodlum s~ av~ ble from
Blue Luster Home Care Products, Inc., Irld~anap~lis, under the name
~5 Rinse 'n V~ at about ~C for about 15 ~erond~, fvllowed by
rinslng the s~mpl~ in co~d water, centrifugin~ t~e sample, and ~hen


2 ~ ,6~




dryin~ the sample at ahout lOD~ for ahout 30 minutes.
The treated and control ~amples wer~ then stained ~y imlnersion
. in a 10~ aqueous solutLon of a food pr3duct c~ntal~in~ ~itrlc a~id
. ~nd about 0.1~ Food, Dru~ and C~smetio Basic Red ~40 ~ye ~herry
Kool-AldlM) fo~ abo~t five minutes ~t a te~.peratur~ of a~out 41~,
followed by rinslng in co~d water. The sa~ples ~.~ere then
Gontrifuged followed by dryl~g ~t ~2~C.
. The s~mples w~re e~al~ated f~r staining, by te~-tln3 for
brightnes~ ~on a scale of 1-50~ using a ~rlghtlme~br Model 54-M
Bri~htness Te~ter (~chnidyne ~orp.)~ ~urin~ the brightness
measuremen~s, the nap of the carpet was laid in th~ same ~irection
for each carpet sample. F~ ve bri~ht~ess me~surements were tak~
f~r ~ach sample (2" x ~
The result ~f the te~t~n~ o tho samples treated with anti-

~ain ag~nts prepared according tc Ex~mple 1 are gi~en in Table l~ w.




11


..

~2 f~




TABLE~ 1
. , ~
S ~rightnes~; ( S~n~ard d~viation ~
Sample Unstat ned Staine~ Sh~mpoo ~ Stained _
1 36.1 (2.13 1~ 3
. 10 2 44.7 (S.3) l4.5S0-7)
3 41.4 (4.~ lfi.~a (1.23
~ . 42.8 ~1~2) 1~.~(2.6)
~0.4 ~3.5~ 17~3(2.7)
Control A 48.~ (~,9)
Control B 1.6 (0~)
.0
Both Cor~trol A ~nd ~ontrol B w~re untxeat~ed~


EXAMPI.E_5
The procedures o~ Example 4 wsre repeated us~.n~ the antl-stain
agent~ prepared in accordance with ~xamples 2. and ~ . The resul t~
~re ~hown in T~ble 2 below.




12

'~02~t~




TABLE ~

Brightn~s;
5 Sample Uns~a n d__ _St~ined Sham~St in~d
6 36. 4 la . 1
7 ~ 17.1
~ ~3.~2 7~72
~ 23.24 12.01
~2 . ~. . 63
11 3~ 7 13. ~0
12 31~47 13,3
Contxc: 1 C 48 . 8
20~ontrol D~ 1. 6
, ~ .... ~
Both Gontrol C and ~ontrol D w~re ur~treated~

~5 The tabulated re~3ult$ given in E~amples 4 and 5 show the
excellent stain re~istan~e and durability o~ stain reslstan~e of
carpets tre~ted in accordar~ce w.ith the pre.~ent invent ;lon.


3o r,xAMPr.E 6
The procedure o~ Examplo 4 wa5 r~3Fl~tecl using an ~n~i-stain
a~ent prepa~ed ac,co~ding to Example 3 having ~ wei~ht ~vera~e
molecular welght of 135, 000, 6~xcept a commercial acid shampoo was
. utillzed in place of "Rinss IN Vac" ~ alkallne shampoo) in the last
samplQ. The aci~ ~hampoo ~ormulation wa~ ~59~ butyl acrylate/15
styrene~50P~ methacrylic ac~à~ neutralized ~ h ~mmonia an~
cataly~ed with zirc. The rasults are se~ for~l~ in ~able 3 below:

~3

2~2~




TABL 3
Si~mple B~ight ~;.s
Traated Control (no ~hamE~ooJst~ined~ ~6 . 4
~lkaline Shampoo ( stained ) 16 . ~
Acid Shampoc~ ~ stained ) ~3 . 5

The results of thi~ oxample demonstr~te the dur~bility of ~:he
c~rpet after treatment aGcording to the inven~ion, comparin~ a
cont~ol s~mple with no shampoo $ t;ep wlth sample~ that have been
10 shampooed using st~rldar~ alkaline and a~id sham~oos.




14

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Administrative Status

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Administrative Status

Title Date
Forecasted Issue Date Unavailable
(22) Filed 1990-09-04
(41) Open to Public Inspection 1991-03-16
Dead Application 1995-03-04

Abandonment History

There is no abandonment history.

Payment History

Fee Type Anniversary Year Due Date Amount Paid Paid Date
Application Fee $0.00 1990-09-04
Registration of a document - section 124 $0.00 1991-03-27
Maintenance Fee - Application - New Act 2 1992-09-04 $100.00 1992-04-24
Maintenance Fee - Application - New Act 3 1993-09-06 $100.00 1993-04-26
Owners on Record

Note: Records showing the ownership history in alphabetical order.

Current Owners on Record
BLANKENSHIP, ROBERT M.
MORRIS HAL C.
BLANKENSHIP, ROBERT M.
MORRIS HAL C.
Past Owners on Record
None
Past Owners that do not appear in the "Owners on Record" listing will appear in other documentation within the application.
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Document
Description 
Date
(yyyy-mm-dd) 
Number of pages   Size of Image (KB) 
Drawings 1991-03-16 1 16
Claims 1991-03-16 3 81
Abstract 1991-03-16 1 16
Cover Page 1991-03-16 1 15
Description 1991-03-16 14 515
Fees 1993-04-26 1 74
Fees 1992-04-24 1 61