( 1 2 ) United S ta tes Pa tent

Jona s et a 1 .
US 0082 47640B2
US 8, 2 47, 640 B2
A u g . 2 1 , 2 01 2
( 1 0) Pa tent N 0. :
( 45 ) Da te of Pa tent:
( 5 4) HIGHLY S WELLA BLE A BS ORPTION
MEDIUMWITH REDUCED CA KIN G
TEN DEN CY
( 75 ) Inv entor s : Ger d Jona s , Kr ef el d ( DE) ; Ric h a r d
Mer tens , Kr ef el d ( DE) ; Ma r ku s F r a nk,
Tonis v or s t ( DE)
( 73 ) A s s ig nee: Ev onik S toc kh a u s en GmbH, Kr ef el d
( DE)
( * ) N otic e: S u bj ec t to a ny dis c l a imer , th e ter m of th is
p a tent is ex tended or a dj u s ted u nder 3 5
U. S . C. 1 5 4( b) by 1 5 1 da y s .
( 2 1 ) A p p l . N o. : 1 2 / 71 8, 61 7
( 2 2 ) F il ed: Ma r . 5 , 2 01 0
( 65 ) Pr ior Pu bl ic a tion Da ta
US 2 01 0/ 01 60883 A 1 Ju n. 2 4, 2 01 0
Rel a ted US . A p p l ic a tion Da ta
( 60) Div is ion of a p p l ic a tion N o. 1 0/ 42 4, 45 9 , ? l ed on A p r .
2 5 , 2 003 , noW a ba ndoned, Wh ic h is a c ontinu a tion of
a p p l ic a tion N o. PCT/ EP2 001 / 01 2 3 1 5 , ? l ed on Oc t.
2 5 , 2 001 .
( 3 0) F or eig n A p p l ic a tion Pr ior ity Da ta
Oc t. 2 5 , 2 000 ( DE) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1 00 5 2 9 66
( 5 1 ) Int. Cl .
A 61 F 1 3 / 1 5 ( 2 006. 01 )
( 5 2 ) US . Cl . . . . . . . . . . . 604/ 3 72 ; 604/ 3 68; 42 3 / 2 67; 5 2 1 / 5 7;
42 7/ 2 3 ; 42 7/ 3 84
( 5 8) F iel d of Cl a s s i? c a tion S ea r c h . . . . . . . . . . . . . . . . . . 604/ 3 67,
604/ 3 68, 3 70, 3 72 ; 42 3 / 2 67; 5 2 1 / 5 7; 42 7/ 2 3 ,
42 7/ 3 84
S ee a p p l ic a tion ? l e f or c omp l ete s ea r c h h is tor y .
( 5 6) Ref er enc es Cited
U. S . PA TEN T DOCUMEN TS
3 , 65 6, 9 9 6 A 4/ 1 9 72 Va n Pa es s c h en et a l . 42 8/ 3 3 6
4, 2 86, 082 A 8/ 1 9 81 Ts u ba kimoto et a l .
4, 3 62 , 73 7 A 1 2 / 1 9 82 S c h a f er et a 1 . . . . . . . . . . . . . . . . . 5 1 4/ 1 2 0
4, 640, 81 0 A 2 / 1 9 87 La u r s en et a l .
4, 666, 9 83 A 5 / 1 9 87 Ts u ba kimoto et a l .
4, 73 4, 478 A 3 / 1 9 88 Ts u ba kimoto et a 1 . . . . . . . . 5 2 7/ 3 00
4, 771 , 1 05 A 9 / 1 9 88 S h ir a i et a 1 .
4, 83 5 , 02 0 A 5 / 1 9 89 Itoh et a 1 .
5 , 3 2 1 , 09 8 A 6/ 1 9 9 4 La l
5 , 3 80, 808 A 1 / 1 9 9 5 S u miy a et a l .
5 , 409 , 771 A 4/ 1 9 9 5 Da h men et a 1 .
5 , 63 3 , 3 1 6 A 5 / 1 9 9 7 Ga r tner et a 1 . . . . . . . . . . . . . . 5 2 5 / 5 43 2
5 , 669 , 89 4 A 9 / 1 9 9 7 Gol dma n et a 1 .
5 , 72 8, 742 A 3 / 1 9 9 8 S ta p l es et a 1 . . . . . . . . . . . . . . . . . . . . 5 2 1 / 5 7
5 , 763 , 067 A 6/ 1 9 9 8 Br u eg g ema nn et a 1 .
5 , 840, 3 2 1 A 1 1 / 1 9 9 8 Eng el h a r dt et a 1 .
5 , 9 45 , 49 5 A 8/ 1 9 9 9 Da niel et a 1 .
5 , 9 9 4, 440 A 1 1 / 1 9 9 9 S ta p l es et a 1 .
6, 03 1 , 1 47 A 2 / 2 000 Gr os s
6, 03 3 , 769 A 3 / 2 000 Br u eg g ema nn et a 1 .
6, 1 03 , 3 5 8 A 8/ 2 000 Br u eg g ema nn et a 1 .
6, 1 2 4, 3 9 1 A 9 / 2 000 S u n et a 1 .
6, 1 46, 5 70 A 1 1 / 2 000 S ter n
6, 1 5 6, 02 4 A 1 2 / 2 000 S c h u l te et a 1 . . . . . . . . . . . . 604/ 3 85 . 2 8
6, 2 9 1 , 63 6 B1 9 / 2 001 Miy a ke et a 1 .
6, 675 , 702 B1 1 / 2 004 Ma ks imow
2 004/ 0071 9 66 A 1 4/ 2 004 Ing er et a 1 .
2 005 / 002 0780 A 1 1 / 2 005 Ing er et a 1 .
F OREIGN PA TEN T DOCUMEN TS
CA 2 3 1 6 3 42 A 1 6/ 2 000
DE 40 2 0 780 C1 6/ 1 9 9 0
DE 40 2 0 780 C1 8/ 1 9 9 1
DE 441 8 3 1 9 A 1 5 / 1 9 9 4
DE 1 9 5 05 709 A 1 2 / 1 9 9 5
DE 1 9 6 01 763 A 1 1 / 1 9 9 6
DE 1 9 6 01 763 A 1 7/ 1 9 9 7
DE 1 9 7 5 0 89 0 A 1 1 1 / 1 9 9 7
DE 1 9 8 01 9 3 3 A 1 1 / 1 9 9 8
DE 1 9 7 5 0 89 0 A 1 5 / 1 9 9 9
DE 1 9 8 01 9 3 3 A 1 7/ 1 9 9 9
DE 1 00 1 6 041 A 1 3 / 2 000
DE 1 00 1 6 041 A 1 1 0/ 2 001
EP 0 3 88 1 2 0 A 1 9 / 1 9 9 0
EP 0 467 073 A 1 1 / 1 9 9 2
EP 0 5 09 708 A 1 1 0/ 1 9 9 2
EP 0 75 5 9 64 A 2 7/ 1 9 9 6
EP 0 75 5 9 64 1 / 1 9 9 7
EP 0 85 0 61 5 7/ 1 9 9 8
EP 0 85 0 61 5 A 1 7/ 1 9 9 8
JP S 63 2 70741 A 1 1 / 1 9 88
JP H04-1 75 3 1 9 A 6/ 1 9 9 2
JP H1 1 -2 9 2 9 1 9 A 1 0/ 1 9 9 9
JP 2 001 -2 1 3 9 1 4 A 8/ 2 001
W0 WO 9 9 / 472 49 9 / 1 9 9 9
W0 WO 9 9 / 49 9 05 1 0/ 1 9 9 9
W0 WO 00/ 1 061 9 3 / 2 000
Pr ima r y Ex a miner * Ly nne A nder s on
( 74) A ttor ney , A g ent, or F ir m * S mith Moor e Lea th er Wood
LLP; Ph il ip P. Mc Ca nn
( 5 7) A BS TRA CT
Th e p r es ent inv ention c onc er ns h ig h l y s Wel l a bl e a bs or p tion
mediu ms With a r edu c ed c a king tendenc y a t h ig h h u midity
a nd/ or h ig h temp er a tu r es , Wh er ein a s Wel l a bl e p ol y mer is
c oa ted With a non-ionic , nitr og en-c onta ining s u r f a c ta nt a nd
op tiona l l y a LeWis a c id a nd th en r ea c ted by h ea ting .
1 4 Cl a ims , N o Dr a wing s
US 8, 2 47, 640 B2
1
HIGHLY S WELLA BLE A BS ORPTION
MEDIUMWITH REDUCED CA KIN G
TEN DEN CY
Th is a p p l ic a tion is a div is iona l of U. S . A p p l ic a tion S er . N o.
1 0/ 42 4, 45 9 , ? l ed on A p r . 2 5 , 2 003 , noW p ending , Wh ic h is a
c ontinu a tion a p p l ic a tion of Inter na tiona l A p p l ic a tion N o.
PCT/ EP2 001 / 01 2 3 1 5 ? l ed Oc t. 2 5 , 2 001 , Wh ic h c l a ims p r i
or ity to Ger ma nA p p l ic a tion N o. DE 1 00 5 2 9 66. 6 ? l ed Oc to
ber 2 5 , 2 000, th e dis c l os u r es of Wh ic h a r e ex p r es s l y inc or p o
r a ted h er ein by r ef er enc e.
BA CKGROUN D OF THE IN VEN TION
Th e p r es ent inv ention r el a tes to h ig h l y s Wel l a bl e a bs or p
tion mediu ms h a v ing a r edu c ed c a king tendenc y in a mois t
env ir onment a nd/ or a t h ig h temp er a tu r es . Th e p r es ent inv en
tion a l s o r el a tes to th e p r odu c tion a nd a p p l ic a tion of th is
a bs or p tion mediu m in h y g iene a r tic l es a nd in tec h nic a l ? el ds .
Pol y mer s th a t a bs or b a q u eou s ? u ids , ter med s u p er a bs or b
er s , a r e knoWn f r om a l a r g e nu mber of p u bl ic a tions . Th ey a r e
modi? ed na tu r a l p ol y mer s a nd p a r tia l l y or tota l l y s y nth etic
p ol y mer s . Tota l l y s y nth etic p ol y mer s a r e u s u a l l y p r odu c ed by
r a dic a l p ol y mer iz a tion of dif f er ent h y dr op h il ic monomer s in
a q u eou s s ol u tion u s ing a v a r iety of meth ods . In g ener a l ,
c r os s -l inking a g ents a r e p ol y mer iZ ed a s Wel l s o th a t th e p ol y
mer is no l ong er Wa ter -s ol u bl e bu t onl y Wa ter s Wel l a bl e.
Pol y mer s ba s ed, f or ex a mp l e, on ( meth ) a c r y l ic a c ids c a n be
u s ed a s s u p er a bs or ber s a nd a r e p a r tia l l y in th e neu tr a l iZ ed
f or m a s th e a l ka l i s a l t.
S u p er a bs or bent p ol y mer s a r e u s u a l l y u s ed in th e f or m of
g r a nu l a tes a s a bs or bing c omp onents in ma ny h y g iene a r tic l es
s u c h a s dia p er s , f eminine p a ds or a bs or bent dr es s ing s . Pr o
du c ing s u c h a r tic l es r eq u ir es ex a c t p r op or tions to be u s ed th a t
c a n onl y be g u a r a nteed by c ons ta nt c onv ey ing in th e p r odu c
tion p l a nt. Th e h ig h l y h y g r os c op ic na tu r e of s u p er a bs or bent
p ol y mer s c a u s es p r obl ems a t c ons ta nt c onv ey ing s p eeds . Th is
h y g r os c op ic na tu r e r es u l ts in c a king of th e p ol y mer p a r tic l es ,
in p a r tic u l a r Wh en th e h u midity is r el a tiv el y h ig h a nd/ or Wh en
th e temp er a tu r e is h ig h . A g g l omer a ted s u p er a bs or ber s c a nnot
be dos ed p r ec is el y a nd s tic k to th e Wa l l s of th e p r odu c tion
p l a nt, r es u l ting in inc r ea s ed c l ea ning c os ts . Th u s , th er e h a v e
been ma ny a ttemp ts in th e p a s t to dev el op s u p er a bs or bent
p ol y mer s With a r edu c ed c a king tendenc y .
Ma ny knoWn p r oc es s es r edu c e th e h y g r os c op ic na tu r e by
a dding ? nel y div ided inor g a nic p oWder to th e s u r f a c e of th e
p ol y mer p a r tic l es . Eu r op ea n p a tent EP 0 3 88 1 2 0 A des c r ibes
th e s u r f a c e tr ea tment of p ol y mer s With s il ic on diox ide p oW
der With a n a v er a g e p a r tic l e s iZ e of 0. 1 to 3 0 u m.
US . Pa t. N o. 4, 73 4, 478 dis c l os es p ol y mer s to Wh ic h , a f ter
p ol y mer iz a tion, a mix tu r e of a p ol y a l c oh ol a nd a h y dr op h il ic
or g a nic s ol v ent is a dded f ol l oWed by h ea t tr ea tment a t > 9 0 C.
S u bs eq u entl y , th e s u r f a c e c r os s -l inked p ol y mer s a r e tr ea ted
With 0. 01 % to 1 0% by Weig h t of s il ic a du s t With a p a r tic l e
dia meter of l es s th a n 1 0 u m. S u c h p ol y mer s a r e s ta ted to h a v e
a h ig h Wa ter u p ta ke c a p a c ity a s Wel l a s a r edu c ed c a king
tendenc y .
US . Pa t. N o. 4, 2 86, 082 dis c l os es p r oc es s es f or th e p r odu c
tion of Wa ter a bs or bing r es ins , in Wh ic h a t l ea s t one Wa ter
s ol u bl e, s u r f a c e a c tiv e r ea g ent is a dded to th e monomer s ol u
tion a nd th e p ol y mer obta ined is h ea t tr ea ted a t a temp er a tu r e
of 1 00 C. to 2 3 0 C. Th e s u r f a c e a c tiv e r ea g ents a r e p r ef er
a bl y nonionic s u r f a c ta nts With a n HLB of 7 to 2 0. To r edu c e
th e c a king tendenc y of s u c h p ol y mer s , th e p ol y mer s a r e
mix ed With u l tr a mic r os c op ic s il ic a .
S inc e th e du s t c ontent of s u c h p ol y mer s is inc r ea s ed by
tr ea ting With a n inor g a nic p oWder , p r obl ems With du s t a r is e,
2 0
2 5
3 0
3 5
40
45
5 0
5 5
60
65
2
in p a r tic u l a r Wh en u nder mec h a nic a l s tr es s s u c h a s th e f r ic
tion r es u l ting f r om p neu ma tic c onv ey ing . S u c h a r el ea s e of
du s t is p r ef er a bl y a v oided f or h ea l th r ea s ons , s o s u c h p ol y
mer s a r e mor e di? ic u l t to ma nip u l a te du r ing p r odu c tion a nd
u s e.
A ttemp ts to p r odu c e p ol y mer s With a l oW du s t c ontent a r e
des c r ibed in US . Pa t. N o. 5 , 9 9 4, 440. S u c h p ol y mer s a r e
obta ined by c oa ting th e s u r f a c e of Wa ter -a bs or bent, c r os s
l inked p ol y mer s With h y dr op h il ic or g a nic c omp ou nds th a t do
not p enetr a te into th e inter na l s tr u c tu r e of th e p ol y mer . S u it
a bl e or g a nic c omp ou nds a r e a l ip h a tic p ol y ol s With a mol ec u
l a r Weig h t of mor e th a n 2 00 g / mol . Th e s u r f a c e c oa ting c a u s es
th e p ol y mer du s t to a dh er e to th e p ol y mer p a r tic l es or to th e
Wa l l of th e s tor a g e c onta iner s o th a t du s t c a n be a v oided. Th e
l oos e du s t p or tion of s u c h a p ol y mer is s ta ted to be 2 2 . 5 p p m,
With du s t p a r tic l es With a dia meter of g 1 0 u m being c ou nted.
In a noth er s er ies of knoWn p r oc es s es , th e s u r f a c e of th e
a bs or bent p a r tic l es is tr ea ted With h y dr op h obic a g ents to
r edu c e th e h y g r os c op ic na tu r e. Th u s , EP 0 75 5 9 64 A 2
des c r ibes h ig h l y s Wel l a bl e h y dr og el s th e s u r f a c e of Wh ic h is
c oa ted With Wa x . A ny Wa x With no r ea c tiv e g r ou p s th a t c a n
r ea c t With th e c a r box y l g r ou p s of th e p ol y mer s u r f a c e c a n be
u s ed. Pr ef er a bl y , Wa x es With a mel ting p oint r a ng e of 3 0 C.
to 1 80 C. a r e u s ed.
EP 0 5 09 708 A 1 dis c l os es p ol y mer s obta ined by s u r f a c e
c r os s -l inking With p ol y h y dr ox y c omp ou nds a nd by c oa ting
th e s u r f a c e With s u r f a c ta nts With a n HLB betWeen 3 a nd 1 0.
Th e p ol y h y dr ox y c omp ou nds c a n be a ny c omp ou nd th a t h a s
a t l ea s t tWo h y dr ox y l g r ou p s a nd th a t c a n r ea c t With th e
c a r box y l g r ou p s on th e p ol y mer p a r tic l es . Pr ef er r ed p ol y h y
dr ox y c omp ou nds inc l u de p ol y g l y c ol s or l oWer g l y c ol der iv a
tiv es . Pa r tic u l a r s u r f a c ta nts th a t c a n be u s ed a r e s or bita n f a tty
a c id es ter s , eth ox y l a ted s or bita n f a tty a c id es ter s , g l y c er in or
p ol y g l y c er in f a tty a c id es ter s or modi? ed s u r f a c e a c tiv e p ol y
es ter s .
A dis a dv a nta g e of th a t p r oc es s f or s u r f a c e c oa ting p ol y
mer s With h y dr op h obic s u bs ta nc es is th a t th e h y dr op h il ic
na tu r e of th e p ol y mer s u r f a c e is r edu c ed, r es u l ting in r edu c ed
l iq u id u p ta ke r a tes .
US . Pa t. N o. 5 , 72 8, 742 A dis c l os es a non c a king , non
du s ty c omp os ition obta ined by tr ea ting Wa ter a bs or bing ,
l ig h tl y c r os s -l inked p ol y mer s With a n a nti-c a king a g ent a nd a
h y dr op h il ic de-du s ting a g ent. S u c h dedu s ting a g ents a r e
eith er p ol y ol s With a mol ec u l a r Weig h t of mor e th a n 2 00
g / mol or p ol y a l ky l ene g l y c ol s With a mol ec u l a r Weig h t of 400
to 6000 g / mol . Th e a nti-c a king a g ents a r e c a tionic s u r f a c
ta nts , f or ex a mp l e q u a ter na r y a mmoniu m or p h os p h oniu m
s a l ts .
DETA ILED DES CRIPTION OF THE IN VEN TION
Th e a im of th e p r es ent inv ention is to p r ov ide s u p er a bs or
bent p ol y mer s th a t h a v e a r edu c ed c a king tendenc y c omp a r ed
With a bs or p tion mediu ms th a t a r e knoWn f r om th e p r ior a r t, in
p a r tic u l a r in a mois t env ir onment s u c h a s h ig h h u midity a nd/
or h ig h temp er a tu r es , With a t l ea s t eq u iv a l ent p r op er ties , in
p a r tic u l a r a t l ea s t a n u nc h a ng ed Wa ter u p ta ke c a p a c ity , r eten
tion a nd u p ta ke r a te f or Wa ter or a q u eou s ? u ids , in p a r tic u l a r
body ? u ids .
Th e p r es ent inv ention p r ov ides a h ig h l y s Wel l a bl e a bs or p
tion mediu m With a r edu c ed c a king tendenc y in a mois t env i
r onment a nd/ or a t h ig h temp er a tu r es ba s ed on th e f ol l oWing
c omp onents :
I a Wa ter - or a q u eou s ? u id-a bs or bing na tu r a l p ol y mer modi
? ed With a c id g r ou p s or a Wa ter -ins ol u bl e, op tiona l l y s u r
f a c e c r os s -l inked, Wa ter - or a q u eou s ? u id-a bs or bing c r os s
US 8, 2 47, 640 B2
3
l inked p ol y mer ba s ed on p ol y mer iz ed monomer s
c onta ining a t l ea s t p a r tia l l y neu tr a l iz ed a c id g r ou p s , Wh ic h
is tr ea ted with :
H a t l ea s t one c oa ting a g ent s el ec ted f r om th e g r ou p f or med
by nitr og en-c onta ining , non-ionic s u r f a c ta nts ; a nd
Wh er eby
th e mix tu r e f or med f r om c omp onents I a nd II h a s been h ea t
tr ea ted.
Pr ef er a bl y , th e s u r f a c ta nt in th e a bs or p tion mediu m of th e
inv ention is a t l ea s t one c omp ou nd With g ener a l f or mu l a 1 :
R1
/ R2
C N
u j \ R
O Y! 3 Z
in Wh ic h
R1 is a Z -s u bs titu ted a l ip h a tic r es idu e, p r ef er a bl y a Z -s u b
s titu ted, s a tu r a ted or u ns a tu r a ted, l inea r or br a nc h ed a l i
p h a tic C1 to C3 0 h y dr oc a r bon r es idu e, mor e p r ef er a bl y
C8 to C2 2 , Wh ic h op tiona l l y c a r r ies a r y l r es idu es , p r ef
er a bl y a p h eny l r es idu e, a Z - s u b s titu ted benZ ene r es idu e,
op tiona l l y c ondens ed With ? v e or s ix -member ed r ing s
op tiona l l y c onta ining h eter oa toms s u c h a s ox y g en,
p h os p h or u s or nitr og en;
R2 is
a h y dr og en; or
a n a l ip h a tic r es idu e, p r ef er a bl y a s a tu r a ted or u ns a tu r a ted,
l inea r or br a nc h ed C2 to C2 4 h y dr oc a r bon r es idu e, p r ef
er a bl y C8 to C2 2 ;
a h y dr ox y a l ky l ene r es idu e,
th e h y dr ox y l g r ou p of s a id h y dr ox y a l ky l en r es idu e is
p r ef er a bl y a n end g r ou p a nd/ or op tiona l l y a l kox y l a ted
With 1 to 5 0, p r ef er a bl y 1 to 2 0, mor e p a r tic u l a r l y With
1 to 1 0 a l ky l ene ox ide u nits , p r ef er a bl y eth y l ene a nd/
or p r op y l ene ox ide u nits , a nd/ or s a id h y dr ox y l g r ou p
is op tiona l l y es ter i? ed With a c a r bon a c id, p r ef er a bl y
a Cl - to CS -c a r bon a c id, a nd
th e a l ky l ene g r ou p of s a id h y dr ox y a l ky l en r es idu e is a
Cl - to C8-, p r ef er a bl y Cl - to C4-h y dr oc a r bon g r ou p ,
oc c u r s in th e a l ky l ene r es idu e, or a N , N -dih y dr ox y
a l ky l ene-a mino-a l ky l ene r es idu e With Cl -C4 in ea c h
a l ky l ene r es idu e;
R3 , Wh ic h ma y be identic a l or dif f er ent, h a s th e s a me
mea ning a s R2 , p r ov ided th a t With a mide c omp ou nds ,
a t l ea s t one of r es idu es R2 or R3 r ep r es ents a h y dr ox y
a l ky l ene r es idu e or a n a l kox y l a ted h y dr ox y a l ky l ene
r es idu e or a c or r es p onding es ter i? ed or a l kox y l a ted or
es ter i? ed a nd a l kox y l a ted h y dr ox y a l ky l ene r es idu e
With th e de? nition g iv en f or R2 a bov e;
n is 0 or 1 , p r ef er a bl y 1 ;
a nd Z is a Wh ol e nu mber f r om 1 to 4.
Pr ef er a bl y , c omp onent I is a p oWder . Th e p a r tic l e s iZ e of
th is p oWder is p r ef er a bl y a t l ea s t 2 0% by Weig h t, p r ef er a bl y a t
l ea s t 5 0% by Weig h t a nd mor e p r ef er a bl y a t l ea s t 70% by
Weig h t in th e r a ng e 1 5 0 to 1 000 u m. Pr ef er a bl y a g a in, l es s
th a n 2 0% by Weig h t, mor e p r ef er a bl y l es s th a n 1 0% by Weig h t
of th e p a r tic l es of th e p oWder is l es s th a n 1 5 0 p m. Th e p r o
p or tions g iv en by Weig h t in th is p a r a g r a p h a l l r ef er to th e
p oWder a s a Wh ol e. Th e p a r tic l e s iZ e c a n be deter mined u s ing
ERT-42 0. l -9 9 .
It h a s s u r p r is ing l y been dis c ov er ed th a t c oa ting Wa ter or
a q u eou s ? u id-a bs or bing p ol y mer s With a t l ea s t one c oa ting
a g ent 1 1 of th e inv ention p os s ibl y in c ombina tion With a LeWis
2 0
2 5
3 0
3 5
40
45
5 0
5 5
60
65
4
a c id 1 1 1 c a n p r odu c e a bs or p tion mediu ms With a s ig ni? c a ntl y
r edu c ed c a king tendenc y , Wh il e th e oth er tec h nic a l p r op er
ties , in p a r tic u l a r r etention a nd a bs or p tion u nder l oa d, a r e not
a f f ec ted. F u r th er , th e tr ea ted p ol y mer s h a v e a r edu c ed du s t
p r odu c tion.
Th e a bs or p tion mediu m of th e inv ention ex h ibits a t l ea s t
one, p r ef er a bl y a l l of th e f ol l oWing p r op er ties :
( a ) no a nti-c a king a f ter a t l ea s t 3 , p r ef er a bl y a t l ea s t 6 a nd
p a r tic u l a r l y p r ef er a bl y a t l ea s t 2 4 h , mos t p r ef er a bl y in
th e r a ng e 3 to 3 0 h ou r s , h ea t tr ea tment being in a c c or
da nc e With th e a nti-c a king tes ts des c r ibed bel oW;
( b) a r etention of a t l ea s t 2 0 g / g , p r ef er a bl y a t l ea s t 2 5 g / g
a nd p a r tic u l a r l y p r ef er a bl y a t l ea s t 3 0 g / g , mos t p r ef er
a bl y in th e r a ng e 2 0 to 1 00 g / g ;
( c ) a n a bs or p tion u nder l oa d a t a l oa d of 0. 9 p s i ( A ULOS PS i)
of a t l ea s t 7 g / g , p r ef er a bl y a t l ea s t 1 5 g / g a nd p a r tic u l a r
p r ef er a bl y a t l ea s t 2 0 g / g , mos t p r ef er a bl y in th e r a ng e 7
to 40 g / g .
Combina tions of tWo or mor e of th e a bov e p r op er ties ea c h
p r odu c e p r ef er r ed embodiments of th e a bs or p tion mediu m of
th e inv ention; c ombina tions a b, a c , be a r e p r ef er r ed, With
c ombina tions a b a nd a c being p a r tic u l a r l y p r ef er r ed.
Pa r tia l l y s y nth etic or tota l l y s y nth etic p ol y mer s c a n be
c ons ider ed in a ddition to na tu r a l p ol y mer s a s th e Wa ter
s Wel l a bl e h y dr op h il ic p ol y mer s . N a tu r a l p ol y mer s modi? ed
With a c idic g r ou p s , p r ef er a bl y c a r box y l g r ou p s , th a t c a n be
u s ed a r e p ol y s a c c h a r ides With c a r box y l g r ou p s , p r ef er a bl y
s ta r c h es , c el l u l os es , g u a r , f or ex a mp l e c a r box y meth y l g u a r ,
x a nth a n g u m, a l g ina tes , g u m a r a bic , c a r box y meth y l c el l u
l os e, c a r box y meth y l s ta r c h es a nd mix tu r es of th es e p ol y s a c
c h a r ides . Th es e p ol y mer s a r e Wa ter s Wel l a bl e a nd p a r tia l l y or
tota l l y Wa ter -ins ol u bl e.
Pa r tia l l y s y nth etic a nd tota l l y s y nth etic p ol y mer s a r e p r ef
er a bl y u s ed, in p a r tic u l a r a nionic ( meth ) a c r y l ic a c id ba s ed
p ol y mer s , Wh ic h a r e in th e p a r tia l l y neu tr a l iZ ed f or m a s a l ka l i
s a l ts , in p a r tic u l a r s odiu m a nd/ or p ota s s iu m s a l ts . Th e deg r ee
of neu tr a l is a tion of th e a c idic monomer c omp onents c a n v a r y ,
bu t is p r ef er a bl y in th e r a ng e 2 5 mol e % to 85 mol e %. Homo
a nd c o-p ol y mer s c a n be u s ed th a t a r e obta ined s ol el y f r om
a c r y l ic a c ids a nd/ or meth a c r y l ic a c ids , f r om s u c h monomer s
tog eth er With one or mor e oth er monomer s or a l one f r om one
or mor e oth er monomer s , bu t, f or ex a mp l e, th ey c a n a l s o be
g r a f ted a nionic p ol y mer s , f or ex a mp l e ba s ed on ( meth ) a c r y l ic
a c ids , in th e p a r tia l l y neu tr a l iZ ed f or m a s th e a l ka l i s a l t, f or
ex a mp l e g r a f t p ol y mer s With p ol y v iny l a l c oh ol , p ol y s a c c h a
r ides s u c h a s s ta r c h es or c el l u l os e or der iv a tiv es th er eof or
With p ol y a l ky l ene ox ides s u c h a s p ol y eth y l ene ox ides or
p ol y p r op y l ene ox ides .
Ex a mp l es of monomer s th a t c a n be u s ed to p r odu c e th e
p ol y mer s in a ddition to ( meth ) a c r y l ic a c ids a r e meth y l , eth y l ,
a nd ( p ol y ) h y dr ox y a l ky l es ter s of ( meth ) a c r y l ic a c ids , ( meth )
a c r y l a mide, c r otonic a c id, ma l eic a nd f u ma r ic a c ids , ita c onic
a c id, 2 -a c r y l a mido-2 -meth y l p r op a nes u l p h onic a c id, v iny l
s u l p h onic a c id a nd v iny l p h os p h onic a c ids a nd th e meth y l ,
eth y l a ndp ol y ( h y dr ox y a l ky l ) es ter s a nd a mides of th es e a c ids ,
a mino- a nd a mmoniu m g r ou p -c onta ining es ter s a nd a mides
of a l l s a id a c ids a nd Wa ter -s ol u bl e N -v iny l a mides , bu t a l s o a l l
oth er monomer s u s u a l l y emp l oy ed a s el ementa l u nits in th e
p r odu c tion of s u p er a bs or bent p ol y mer s c a n be c onta ined in
th e p ol y mer . Th e p ol y mer s a r e p r ef er a bl y c r os s -l inked.
Ex a mp l es of s u ita bl e c r os s -l inking c omp ou nds th a t c a n be
u s ed to p r odu c e th e a bs or bent p ol y mer s a nd c onta in tWo or
mor e r ea c tiv e g r ou p s a r e p ol y g l y c idy l c omp ou nds s u c h a s
p ol y g l y c idy l eth er , meth y l ene bis ( meth ) a c r y l a mide, bis
a c r y l a mido a c etic a c id, es ter s of u ns a tu r a ted a c ids With p ol y
ol s or a l kox y l a ted p ol y ol s , f or ex a mp l e eth y l ene g l y c ol
di( meth ) a c r y l a te or tr imeth y l ol p r op a ne tr i( meth ) a c r y l a te or
US 8, 2 47, 640 B2
5
a l l y l c omp ou nds , s u c h a s a l l y l ( meth ) a c r y l a te, p ol y a l l y l
es ter s , tetr a -a l l y l ox y eth a ne, tr ia l l y l a mine, tetr a -a l l y l eth y l
enedia mine or a l l y l es ter s of p h os p h or ic a c id a s Wel l a s v iny l
p h os p h onic a c id der iv a tiv es or mix tu r es th er eof . Th e p r op or
tion of c r os s -l inking a g ents a dded du r ing p r odu c tion of th e
a bs or bent p ol y mer is p r ef er a bl y 0. 01 % to 2 0% by Weig h t,
mor e p r ef er a bl y 0. 1 % to 3 % by Weig h t With r es p ec t to th e
tota l monomer q u a ntity .
Pol y mer p r odu c tion is c a r r ied ou t u s ing knoWn meth ods
s u c h a s th a t des c r ibed in Ger ma n p a tent DE-C1 -40 2 0 780
a nd Wh ic h is h er eby inc or p or a ted by r ef er enc e a nd c ons titu tes
p a r t of th e dis c l os u r e. Pr ef er a bl y , th e p ol y mer is p r odu c ed by
p ol y mer iz a tion in a n a q u eou s s ol u tion u s ing th e g el p ol y mer
iZ a tion p r oc es s .
Th e p ol y mer p oWder obta ined by dis integ r a ting , dr y ing
a nd g r inding of th e p ol y mer g el c a n th en u nder g o s u r f a c e
c r os s -l inking .
Pr ior to s u r f a c e c r os s -l inking , th e p ol y mer is p r ef er a bl y
dr ied, g r ou nd a nd s c r eened to obta in th e des ir ed g r a in s iZ e
f r a c tion, th en th e s u r f a c e c r os s -l inking r ea c tion is c a r r ied ou t.
In s ome c a s es , h oWev er , it is p er tinent to a dd th e s u r f a c e
c r os s -l inking a g ent bef or e dr y ing th e p ol y mer g el or bef or e
dis integ r a ting th e p a r tia l l y or es s entia l l y dr y p ol y mer . A s u r
f a c e c r os s -l inking s tep th a t c a n be c a r r ied ou t in a c c or da nc e
With th e inv ention h a s been des c r ibed in Us . Pa t. N o. 4, 666,
9 83 a nd DE-C-40 2 0 780. Th es e doc u ments a r e h er eby inc or
p or a ted by r ef er enc e a nd th u s c ons titu te p a r t of th e dis c l os u r e.
Pr ef er a bl y , th e s u r f a c e c r os s -l inking a g ent is of ten a dded in
th e f or m of a s ol u tion in Wa ter , a n or g a nic s ol v ent or a mix tu r e
th er eof , in p a r tic u l a r Wh en s ma l l a mou nts of s u r f a c e c r os s
l inking a g ent a r e u s ed. Ex a mp l es of s u ita bl e mix ing ma c h ines
f or a dding th e s u r f a c e c r os s -l inking a g ents a r e a Pa tter s on
Kel l ey mix er , a DRA IS tu r bu l enc e mix er , a Lodig e mix er , a
Ru ber g mix er , a Wor m mix er , a p a n mix er a nd a ? u idis ed bed
mix er , a l s o c ontinu ou s v er tic a l mix er s in Wh ic h th e p oWder is
mix ed a t a h ig h f r eq u enc y u s ing r ota ting kniv es ( S c h u g i
mix er ) . A f ter th e s u r f a c e c r os s -l inking a g ent h a s been mix ed
With th e p ol y mer , it is h ea ted to temp er a tu r es of 60 C. to 2 5 0
C. , p r ef er a bl y 1 3 5 C. to 2 00 C. a nd p a r tic u l a r l y p r ef er a bl y
1 5 0 C. to 1 85 C. to c a r r y ou t th e s u r f a c e c r os s -l inking
r ea c tion. Th e h ea ting p er iod mu s t be l imited s o th a t th e p r op
er ties of th e p ol y mer a r e not a f f ec ted by th e h ea t tr ea tment.
Pr ef er r ed p os t c r os s -l inking a g ents f or s u r f a c e c r os s -l ink
ing of th e p ol y mer s a r e or g a nic c r os s -l inking a g ents , i. e. ,
c omp ou nds th a t r ea c t With th e s u r f a c e COOH g r ou p s of th e
p ol y mer s , s u c h a s a l ky l ene c a r bona tes , f or ex a mp l e 1 , 3 -di
ox ol a n-2 -one, 4-meth y l -1 , 3 -diox ol a n-2 -one, 4, 5 -dimeth y l -1 ,
3 -diox ol a n-2 -one, 4, 4-dimeth y l -1 , 3 -diox ol a n-2 -one,
4-eth y l -1 , 3 -diox ol a n-2 -one, 4-h y dr ox y meth y l -1 , 3 -diox ol a n
2 -one, 1 , 3 -diox a n-2 -one, 4-meth y l -1 , 3 -diox a n-2 -one, 4, 6
dimeth y l -1 , 3 -diox a n-2 -one or 1 , 3 -diox ep a n-1 -one. Pa r tic u
l a r l y p r ef er r ed c omp ou nds a r e 1 , 3 -diox ol a n-2 -one a nd
4-meth y l -1 , 3 -diox ol a n-2 -one.
F u r th er , th e f ol l oWing c omp ou nds c a n be u s ed a s s u r f a c e
c r os s -l inking a g ents : p ol y h y dr ox y c omp ou nds , f or ex a mp l e
eth y l eneg l y c ol , p r op y l eneg l y c ol , dieth y l eneg l y c ol , dip r op y
l eneg l y c ol , tr ieth y l eneg l y c ol , tetr a eth y l eneg l y c ol , tetr a p r o
p y l eneg l y c ol , p ol y eth y l eneg l y c ol , p ol y p r op y l eneg l y c ol , 1 , 3
p r op a nediol , g l y c er ine, p ol y g l y c er ine, 1 , 4-bu ta nediol , 1 , 5
p enta nediol , 1 , 6-h ex a nediol , tr imeth y l ol p r op a ne,
p enta er y th r itol or s or bitol ; a mino a l c oh ol s s u c h a s dieth a no
l a mine, tr ieth a nol a mine. F u r th er or g a nic s u r f a c e c r os s -l ink
ing a g ents th a t a r e not p r ef er r ed on th e g r ou nds of th eir
tox ic ity a nd s o h a v e to be s ev er el y l imited in th eir u s e a r e:
p ol y ep ox ides s u c h a s eth y l eneg l y c ol dig l y c idy l eth er , p ol y
eth y l eneg l y c ol dig l y c idy l eth er , g l y c er ol p ol y g l y c idy l eth er
p ol y g l y c er ol p ol y g l y c idy l eth er , p r op y l eneg l y c ol dig l y
2 0
2 5
3 0
3 5
40
45
5 0
5 5
60
65
6
c idy l eth er , p ol y p r op y l eneg l y c ol dig l y c idy l eth er , g l y c idol ;
p ol y is oc y a na tes s u c h a s 2 , 4-tol u enediis oc y a na te a nd h ex a m
eth y l enediis oc y a na te; h a l og ena ted ep ox ides s u c h a s
ep ic h l or - a nd ep ibr omh y dr in a nd ot-meth y l -ep ic h l or h y dr in;
p ol y a mine c omp ou nds s u c h a s eth y l enedia mine, dieth y l en
etr ia mine, tr ieth y l enetetr a mine, p ol y a l l y l a mine or p ol y eth y l
eneimine. A dditiona l s u r f a c e c r os s -l inking a g ents th a t c a n be
u s ed a r e p ol y ox a Z ol in c omp ou nds s u c h a s 1 , 2 -eth y l enebis ox
a Z ol in. Th e or g a nic s u r f a c e c r os s -l inking a g ent is p r ef er a bl y
u s ed in a mou nt of 0. 01 % to 5 % by Weig h t, mor e p r ef er a bl y
0. 1 % to 2 . 5 % by Weig h t a nd p a r tic u l a r l y p r ef er a bl y f r om
0. 1 % to 1 % by Weig h t, With r es p ec t to th e p ol y mer .
N on-ionic , nitr og en-c onta ining s u r f a c ta nts c a n be u s ed a s
c oa ting a g ent II, p r ef er a bl y c omp ou nds With g ener a l f or mu l a
I. HoWev er , a mix tu r e of a t l ea s t tWo c omp ou nds With th is
f or mu l a c a n a l s o be u s ed. Pr ef er a bl y , c oa ting a g ent II is ba s ed
on a f a tty a c id s u c h a s c a p r y l ic a c id, c a p r inic a c id, l a u r ic a c id,
my r is tic a c id, p a l mitic a c id, p a l mitol eic a c id, ma g a r ic a c id,
s tea r ic a c id, ol eic a c id, l inol eic a c id, l inol enic a c id, a r a c h ic
a c id, or eu r ec a s ic a c id.
In p a r tic u l a r , c oa ting a g ent II is a f a tty a c id a l ka nol a mide,
th e c or r es p onding eth ox y l a ted a nd/ or p r op ox y l a ted c om
p ou nds , th e es ter i? ed c omp ou nds ; or f a tty a c id a mines , th e
c or r es p onding eth ox y l a ted a nd/ or p r op ox y l a ted c omp ou nds ,
Wh ic h c a n a l s o be es ter i? ed. Th es e inc l u de l a u r ic a c id mono
eth a nol a mide, c oc onu t a c id monoeth a nol a mide, s tea r ic a c id
monoeth a nol a mide, r ic inic a c id monoeth a nol a mide, u nde
c y l enic a c id monoeth a nol a mide, l a u r ic a c id dieth a nol a mide,
c oc onu t a c id dieth a nol a mide, s oy a a c id dieth a nol a mide,
l inol eic a c id dieth a nol a mide, l a u r y l my r is tinic a c id dieth a no
l a mide, ol eic a c id dieth a nol a mide, l a u r ic a c id is op r op a nol a
mide, c oc onu t a c id is op r op a nol a mide, ol eic a c id is op r op a no
l a mide, u ndec y l enic a c id p ol y dieth a nol a mide, c oc onu t a c id
p ol y dieth a nol a mide, s tea r y l a mine, s tea r y l p r op y l enedi
a mine, c oc onu t a c id a mine, l a u r y l a mine, ol ey l a mine, s tea r y
l a mine, ta l l oW a c id a mine, th e eth ox y l a tes a nd/ or p r op ox y
l a tes of s a id c omp ou nds , Wh ic h ma y c onta in 1 to 5 0,
p r ef er a bl y 1 to 2 0 a l ky l ene ox ide u nits , a l s o th e es ter s of s a id
c omp ou nds , s u c h a s c oc onu t a c id monoeth a nol a mide a c eta te.
Mix tu r es of s a id c omp ou nds c a n a l s o be u s ed.
Coa ting a g ents II a r e p r ef er a bl y emp l oy ed in a c onc entr a
tion of 5 0 to 5 0000 p p m, p a r tic u l a r p r ef er a bl y 1 00 to 5 000
p p m, s til l mor e p r ef er a bl y 3 00 to 3 000 p p m With r es p ec t to
c omp onent I.
In a p a r tic u l a r embodiment of th e p r es ent inv ention, a t l ea s t
one LeWis a c id is a dded a s c oa ting a g ent III to th e p ol y mer s in
a ddition to a t l ea s t one c oa ting a g ent II. In a c c or da nc e With
th e inv ention, el ec tr on p a ir a c c ep tor s c a n be emp l oy ed a s th e
LeWis a c id.
Th e c omp ou nds th a t c a n be u s ed a s LeWis a c id III or
c oa ting a g ent III in th e a bs or p tion mediu m of th e inv ention
a r e inor g a nic a c ids , Wa ter -s ol u bl e, s a tu r a ted or u ns a tu r a ted
or g a nic a c ids , Wa ter -s ol u bl e h y dr oc a r bon a c ids or Wa ter
s ol u bl e a c id s a l ts .
Th e LeWis a c ids a r e p r ef er a bl y inor g a nic a c ids s u c h a s
h y dr og en h a l ides , ox y h a l og en a c ids , s u l p h u r or s el eniu m
ox y a c ids , nitr og en or p h os p h or u s ox y a c ids , or g a nic a c ids
s u c h a s Wa ter -s ol u bl e s a tu r a ted or u ns a tu r a ted or g a nic a c ids ,
a nd/ or Wa ter -s ol u bl e a c id s a l ts s u c h a s Wa ter -s ol u bl e br o
mides , c h l or ides , nitr a tes , s u l p h a tes , p h os p h a tes or s a l ts of
or g a nic a c ids s u c h a s th e a c eta te, f or ' ma te, ox a l a te a nd l a c ta te
of th e meta l s A l , F e, Z n, S b, A s , S n, Cu , Mg , Ca , Cr , Ga , V, Ti,
Bi, T1 , In, Mn, N i, Co, Be u nd Z ir c oniu m.
Pr ef er a bl y , th e inor g a nic a c ids a r e h y dr oc h l or ic a c id, p er
c h l or ic a c id, br omic a c id, h y dr obr omic a c id, s u l p h u r ic a c id,
s u l p h u r -c onta ining a c ids , s el enic a c id, nitr ic a c id, p h os p h o
nic a c id or p h os p h or u s -c onta ining a c ids ; th e or g a nic Wa ter
US 8, 2 47, 640 B2
7
s ol u bl e a c ids a r e p r ef er a bl y c a r bonic a c id, h y dr oc a r bon
a c ids , s u l p h onic a c ids or p h os p h onic a c ids or th e c or r es p ond
ing a mino a c ids , f or ex a mp l e a c r y l ic a c id, meth a c r y l ic a c id,
f or mic a c id, a c etic a c id, p r op ionic a c id, bu ty r ic a c id, ox a l ic
a c id, ma l onic a c id, s u c c inic a c id, l a c tic a c id, ma l eic a c id,
f u ma r ic a c id, benz oic a c id, p h th a l ic a c id, s a l ic y l ic a c id, ta r
ta r ic a c id, c itr ic a c id, p -, m- u nd o-tol u enes u l p h onic a c id,
benz enes u l p h onic a c id, a minometh a nes u l p h onic a c id, a mi
nometh a nep h os p h onic a c id; a nd th e a c id s a l ts a r e a l u miniu m
s a l ts , a l u ms a nd th eir v a r iou s h y dr a tes s u c h a s A l Cl 3 > < 6H2 O,
N a A l ( S O4) 2 > < 1 2 H2 O, KA I( S O4) 2 > < 1 2 H2 O or A I2 ( S O4) 3 > < 1 4
1 8H2 O, z inc s a l ts a nd th eir h y dr a tes s u c h a s Z nCl 2 , Z nS O4> <
1 -7H2 O a nd Z n( CH3 COO) 2 > < 2 H2 O, ir on s a l ts a nd th eir
h y dr a tes s u c h a s N a F e( S O4) 2 > < 1 2 H2 O, KF e( S O4) 2 > < 1 2 H2 O
a nd F e2 ( S O4) 3 > < nH2 O, Mg -s a l ts s u c h a s Mg Cl 2 or Mg S O4,
dou bl e s a l ts , a l s o mix tu r es of th e s a l ts a nd mix tu r es of th e
inor g a nic a nd/ or or g a nic a c ids a nd mix tu r es of th e s a l ts With
th e inor g a nic a nd/ or or g a nic a c ids .
Pa r tic u l a r l y p r ef er r ed c omp ou nds a r e: f or th e inor g a nic
a c ids , s u l p h u r ic a c id or p h os p h or ic a c id; f or th e a c id s a l ts :
A l Cl 3 > < 6H2 O, A l 2 ( S O4) 3 > < 1 4-1 8H2 O, Z nCl 2 , Z nS O4> < 1
7H2 O, Z n ( CH3 COO) 2 > < 2 H2 O, Mg S O4, Mg Cl 2 ; a nd f or th e
or g a nic a c ids , a c etic a c id, ox a l ic a c id, l a c tic a c id, c itr ic a c id
a nd ta r ta r ic a c id.
Pa r tic u l a r l y p r ef er a bl y , th e LeWis a c id is s u l p h u r ic a c id,
p h os p h or ic a c id, f or mic a c id, a c etic a c id, c itr ic a c id or p -tol u
enes u l p h onic a c id, a n a l u miniu m s a l t or a l u m a nd/ or th eir
v a r iou s h y dr a tes , z inc s a l ts a nd/ or h y dr a tes th er eof , ma g ne
s iu m s a l ts a nd/ or h y dr a tes th er eof a nd/ or dou bl e s a l ts .
In a c c or da nc e With th e inv ention, a t l ea s t one LeWis a c id is
u s ed. HoWev er , a mix tu r e of a t l ea s t tWo of th e c ited LeWis
a c ids c a n be u s ed.
Th e tota l a mou nt of c oa ting a g ents II a nd III is 1 00 to
5 0000 p p m, p r ef er a bl y 3 00 to 2 5 000 p p m, mor e p a r tic u l a r l y
5 00 to 1 3 000 p p m With r es p ec t to c omp onent I.
Coa ting a g ent II c a n be a dded With LeWis a c id III or bef or e
or a f ter c a r r y ing ou t th e s u r f a c e c r os s -l inking s tep or s imu l
ta neou s l y With th e c r os s -l inking a g ent, a nd th en u nder g o th e
h ea t tr ea tment With p ol y mer I. A l ter na tiv el y , Wh en a c ombi
na tion of c oa ting a g ent II With LeWis a c id III is u s ed, th e tWo
c omp ou nds c a n be a dded s ep a r a tel y , p r ef er a bl y a s a q u eou s
s ol u tions , or th ey c a n be a dded s imu l ta neou s l y to p ol y mer I,
op tiona l l y tog eth er With th e c r os s -l inking a g ent, p r ef er a bl y a s
a n a q u eou s s ol u tion. Pr ef er a bl y , c oa ting a g ent II, op tiona l l y
in c ombina tion With LeWis a c id III, is a dded s imu l ta neou s l y
With th e c r os s -l inking a g ent a nd th e c oa ted p ol y mer th en
u nder g oes h ea t tr ea tment, th u s dis p ens ing With a n a dditiona l
p r oc es s s tep . Pa r tic u l a r l y p r ef er a bl y , c omp onent I is c oa ted
With a n a q u eou s s ol u tion of c oa ting a g ent II a nd III a nd th en
r ea c ted. S til l mor e p r ef er a bl y , c oa ting a g ent II is a f a tty a c id
a l ka nol a mide or a f a tty a c id a mine With f or mu l a I, Wh ic h ma y
be a l kox y l a ted a nd/ or es ter i? ed.
S u ita bl e s ol v ents a r e Wa ter or p ol a r , Wa ter -mis c ibl e
or g a nic s ol v ents s u c h a s a c etone, meth a nol , eth a nol or 2 -p r o
p a nol or mix tu r es th er eof , p r ef er a bl y Wa ter . Th e ter m a q u e
ou s s ol u tion a s u s ed in th e c ontex t of th e inv ention mea ns ,
Wh en r ef er r ing to s ol v ent c omp onents , th a t th ey c a n a l s o
c onta in or g a nic s ol v ents in a ddition to Wa ter . Th e c onc entr a
tion of th e op tiona l c r os s -l inking a g ent in th e c oa ting s ol u tion
c a n v a r y betWeen Wide l imits a nd is p r ima r il y in th e r a ng e 1 %
to 80% by Weig h t, p r ef er a bl y in th e r a ng e 1 % to 60% by
Weig h t, p a r tic u l a r l y p r ef er a bl y in th e r a ng e 1 0% to 5 0% by
Weig h t. Th e c onc entr a tion of c oa ting a g ent II or op tiona l
LeWis a c id III in th e s ol u tion c a n a l s o v a r y betWeen Wide
l imits , p r ef er a bl y in th e r a ng e 0. 5 % to 80% by Weig h t, p r ef
er a bl y in th e r a ng e 0. 5 % to 60% by Weig h t, p a r tic u l a r l y
p r ef er a bl y in th e r a ng e 0. 5 % to 60% by Weig h t a nd p a r tic u
2 0
2 5
3 0
3 5
40
45
5 0
5 5
60
65
8
l a r l y p r ef er a bl y in th e r a ng e 0. 5 % to 3 0% by Weig h t. Th e
p r ef er r ed s ol v ent f or th e op tiona l or g a nic c r os s -l inking a g ent
a nd c oa ting a g ent II a nd op tiona l LeWis a c id III is Wa ter ,
p r ef er a bl y in a n a mou nt of 0. 5 % to 1 0% by Weig h t, p a r tic u
l a r l y p r ef er a bl y 0. 5 % to 5 % by Weig h t a nd s til l mor e p r ef er
a bl y 0. 5 % to 4% by Weig h t With r es p ec t to p ol y mer I.
To obta in th e des ir ed p r op er ties , th e c oa ting s ol u tion( s )
mu s t be ev enl y dis tr ibu ted on th e a bs or bent p ol y mer . To th is
end, th e c omp onents a r e th or ou g h l y a nd h omog eneou s l y
mix ed in s u ita bl e mix er s , s u c h a s ? u idis ed bed mix er s , p a n
mix er s , r ol l er mix er s or tWin s c r eW mix er s .
It is a l s o p os s ibl e to c oa t th e p ol y mer s du r ing p r odu c tion of
th e p ol y mer , p r ef er a bl y a t th e ? na l s ta g e of p ol y mer iz a tion.
To th is end, r ev er s e s u s p ens ion p ol y mer iz a tion is s u ita bl e.
Hea t tr ea tment of c omp onent I c oa ted With c oa ting a g ent II
or a c or r es p onding c oa ting s ol u tion is p r ef er a bl y c a r r ied ou t
a t temp er a tu r es of 1 00 C. to 2 5 0 C. , p a r tic u l a r l y p r ef er a bl y
1 5 00 C. to 2 3 0 C. , mor e p a r tic u l a r l y p r ef er a bl y 1 5 0 C. to
2 1 0 C. , to c a u s e c omp onent Ito r ea c t With th e c oa ting a g ent.
If c oa ting a g ent II a nd III or th e c or r es p onding c oa ting
s ol u tion is u s ed, h ea t tr ea tment is p r ef er a bl y c a r r ied ou t a t a
temp er a tu r e of 40 C. to 2 5 0 C. , p a r tic u l a r l y p r ef er a bl y 1 00
C. to 2 3 0 C. , mor e p a r tic u l a r l y p r ef er a bl y 1 3 0 C. to 2 1 0 C. ,
to c a u s e c omp onent to r ea c t With th e c oa ting a g ent.
Pr ef er a bl y , c oa ting a g ent II is a dded to th e a bs or bent p ol y
mer in c ombina tion With a LeWis a c id III bef or e, a f ter or
s imu l ta neou s l y With th e c r os s -l inking a g ent p r ior to h ea t
tr ea tment, a s in th is c a s e th e temp er a tu r e a nd du r a tion of th e
h ea t tr ea tment is l oWer a nd s h or ter th a n Wh en tr ea ting th e
a bs or bent p ol y mer With c oa ting a g ent II With ou t LeWis a c id
III.
Th e p a r tic l e s iz e of th e p oWder to be c oa ted is p r ef er a bl y in
th e r a ng e 5 0 to 5 000 u m, p a r tic u l a r l y p r ef er a bl y in th e r a ng e
5 0 to 1 000 u m a nd mor e p a r tic u l a r l y p r ef er a bl y in th e r a ng e
5 0 to 85 0 p m. Th e p a r tic l e s iz e is deter mined u s ing knoWn
s c r eening meth ods .
Th e h ea t tr ea tment p er iod is a l s o dep endent on th e s el ec ted
temp er a tu r e. It s h ou l d be noted in th is r eg a r d th a t th e h ig h er
th e temp er a tu r e, th e s h or ter th e p er iod. Th e tr ea tment time
a nd temp er a tu r e a r e s el ec ted s o th a t th e tr ea ted p ol y mer h a s a
r edu c ed c a king tendenc y , i. e. , it p a s s es th e a nti-c a king tes t
( 2 3 h ou r s ) , r eta ining or imp r ov ing th e r etention, a bs or p tion
u nder l oa d a nd u p ta ke r a te f or Wa ter or a q u eou s ? u ids , in
p a r tic u l a r body ? u ids , c omp a r ed With s u p er a bs or bent p ol y
mer s th a t a r e not in a c c or da nc e With th e inv ention. F or p ol y
mer s ba s ed on p a r tia l l y neu tr a l iz ed a nd c r os s -l inked p ol y
( meth ) a c r y l ic a c ids , th is mea ns a r etention of 2 2 0 g / g a nd a n
A ULQ9 of 2 1 9 g / g u s ing th e meth ods des c r ibed bel oW.
Th e inv ention a l s o c onc er ns a bs or bent a g ent p r odu c ed by
th e p r oc es s of th e inv ention.
Th e p ol y mer s tr ea ted in a c c or da nc e With th e inv ention a r e
ea s y to ma nip u l a te, f or ex a mp l e ea s y to c onv ey a nd dos e.
Th e p ol y mer s of th e inv ention or a bs or bent a g ents a r e
p r ef er a bl y u s ed in a bs or bent h y g iene p r odu c ts s u c h a s dia
p er s , inc ontinenc e p r odu c ts f or a du l ts a nd f eminine p a ds .
A bs or bent h y g iene p r odu c ts u s u a l l y h a v e a g ener a l c on
s tr u c tion c ons titu ted by a ? u id-p er mea bl e c ov er f a c ing th e
body , a ? u id-a bs or bing a bs or bent l a y er a nd a n es s entia l l y
? u id imp er mea bl e, ou ter l a y er f a c ing a Wa y f r om th e body .
Op tiona l l y , th ey ma y h a v e f u r th er mea ns f or r a p id u p ta ke a nd
dis tr ibu tion of body ? u ids to th e a bs or bent c or e. Th es e c on
s tr u c tions a r e of ten, bu t not nec es s a r il y betWeen th e ? u id
p er mea bl e c ov er f a c ing th e body a nd th e ? u id-a bs or bing
a bs or bent c or e.
Th e ? u id-p er mea bl e c ov er u s u a l l y c ons is ts of a nonWov en,
? br ou s f a br ic or a dif f er ent p or ou s c ons tr u c tion.
US 8, 2 47, 640 B2
Ex a mp l es of ma ter ia l s f or th is c ov er a r e s y nth etic p ol y mer s
s u c h a s p ol y v iny l c h l or ide or ? u or ide, p ol y tetr a ? u or eth y l ene
( PTF E) , p ol y v iny l a l c oh ol s a nd th eir der iv a tiv es , p ol y a c r y
l a tes , p ol y a mides , p ol y es ter s , p ol y u r eth a nes , p ol y s ty r ene,
p ol y s il ox a ne or p ol y ol e? ns ( f or ex a mp l e p ol y eth y l ene ( PE)
or p ol y p r op y l ene ( PP) ) , a l s o na tu r a l ? br ou s ma ter ia l s a nd
c ombina tions of th e a bov e ma ter ia l s a s mix ed ma ter ia l s or
c omp os ites or c op ol y mer s .
Th e ? u id p er mea bl e c ov er is h y dr op h il ic in na tu r e. It c a n
a l s o c ons is t of a c ombina tion of h y dr op h il ic a nd h y dr op h obic
c omp onents . Pr ef er a bl y , th e ? u id-p er mea bl e c ov er h a s a
h y dr op h il ic f r a mewor k s o th a t body ? u ids c a n tr ic kl e q u ic kl y
th r ou g h into th e ? u id-a bs or bing a bs or bent l a y er , h oWev er
p a r tia l l y h y dr op h obic c ov er s a r e a l s o u s ed.
F l u id-a bs or bing a bs or bent l a y er .
Th e ? u id-a bs or bing a bs or bent l a y er c onta ins th e s u p er a b
s or bent p oWder ed or g r a nu l a ted p ol y mer of th e inv ention a nd
f u r th er c omp onents , f or ex a mp l e ? br ou s ma ter ia l s , f oa med
ma ter ia l s , ? l m-f or ming ma ter ia l s or p or ou s ma ter ia l s a s Wel l
a s c ombina tions of tWo or mor e of s u c h ma ter ia l s . Ea c h
ma ter ia l c a n be na tu r a l or s y nth etic in or ig in or c a n be p r o
du c ed by c h emic a l or p h y s ic a l modi? c a tion of na tu r a l ma te
r ia l s . Th e ma ter ia l s c a n be h y dr op h il ic or h y dr op h obic , p r ef
er a bl y h y dr op h il ic . Th is is p a r tic u l a r l y th e c a s e f or
c omp os itions th a t e? ic ientl y ta ke u p ex u ded body ? u ids a nd
tr a ns p or t th e body ? u id to a l oc a tion in th e a bs or bent c or e th a t
is a t a dis ta nc e f r om th e entr y p oint.
S u ita bl e ? br ou s ma ter ia l s a r e c el l u l os e ? br es , modi? ed
c el l u l os e ? br es ( f or ex a mp l e s tif f ened c el l u l os e ? br es ) , p ol y
es ter ? br es ( f or ex a mp l e Da c r on) , h y dr op h il ic ny l on or
h y dr op h il is ed h y dr op h obic ? br es , s u c h a s p ol y ol e? ns ( PE,
PP) h y dr op h il is ed With s u r f a c ta nts , p ol y es ter s , p ol y a c r y l a tes ,
p ol y a mides , p ol y s ty r ene, p ol y u r eth a nes a nd th e l ike.
Pr ef er a bl y , c el l u l os e ? br es a nd modi? ed c el l u l os e ? br es
a r e u s ed. Combina tions of c el l u l os e ? br es a nd/ or modi? ed
c el l u l os e ? br es With s y nth etic ? br es s u c h a s PE/ PP c omp os ite
ma ter ia l s , ter med bi-c omp onent ? br es , s u c h a s th os e u s ed f or
th r emobonding of a ir l a id ma ter ia l s , or oth er ma ter ia l s c a n
a l s o be u s ed.
Th e ? br ou s ma ter ia l s c a n be in dif f er ent f or ms , f or ex a mp l e
l oos e f r om a n a ir s tr ea m or a s a n a q u eou s p h a s e or dep os ited
c el l u l os e ? br es , a s a nonWov en f a br ic or a s a tis s u e. Combi
na tions of dif f er ent f or ms a r e p os s ibl e.
Op tiona l l y , in a ddition to th e s u p er a bs or ber of th e inv en
tion, oth er p oWder ed s u bs ta nc es c a n be u s ed, f or ex a mp l e
odou r -binding s u bs ta nc es s u c h a s c y c l odex tr in, Z eol ites , inor
g a nic or or g a nic s a l ts a nd th e l ike.
Th e p or ou s ma ter ia l s a nd f oa med ma ter ia l s c a n, f or
ex a mp l e, be p ol y mer f oa ms s u c h a s th os e des c r ibed in DE 44
1 8 3 1 9 A 1 a nd DE 1 9 5 05 709 A 1 , h er eby inc or p or a ted by
r ef er enc e a nd c ons ider ed to c ons titu te p a r t of th e dis c l os u r e.
Th er mop l a s tic ? br es ( f or ex a mp l e bi-c omp onent ? br es of
p ol y ol e? ns , p ol y ol e? n g r a nu l a tes , l a tex dis p er s ions or h ot
mel t a dh es iv es ) c a n be u s ed to s ta bil is e th e ? u id-a bs or bing
a bs or bent l a y er mec h a nic a l l y . Op tiona l l y , one or mor e l a y er s
of tis s u e c a n be u s ed f or s ta bil is a tion.
Th e ? u id-a bs or bing a bs or bent l a y er c a n be a s ing l e l a y er ,
or it c a n c ons is t of a p l u r a l ity of l a y er s . Pr ef er a bl y , c ons tr u c
tions a r e u s ed th a t c ons is t of h y dr op h il ic ? br es , p r ef er a bl y
c el l u l os e ? br es , op tiona l l y a c ons tr u c tion f or r a p idu p ta ke a nd
dis tr ibu tion of body ? u ids , s u c h a s c h emic a l l y s tif f ened
( modi? ed) c el l u l os e ? br es or h ig h l of t f a br ic f r om h y dr o
p h il ic or h y dr op h il is ed ? br es , a nd s u p er a bs or bent p ol y mer s .
Th e s u p er a bs or bent p ol y mer of th e inv ention c a n be h omo
g eneou s l y dis tr ibu ted in th e c el l u l os e ? br es or s tif f ened c el
l u l os e ? br es , it c a n be l a y er ed betWeen th e c el l u l os e ? br es or
s tif f ened c el l u l os e ? br es , or th e c onc entr a tion of s u p er a bs or
2 0
2 5
3 0
3 5
40
45
5 0
5 5
60
65
1 0
bent p ol y mer c a n be g r a du a ted With in th e c el l u l os e ? br es or
s tif f ened c el l u l os e ? br es . Th e r a tio of th e tota l a mou nt of
s u p er a bs or bent p ol y mer to th e tota l a mou nt of c el l u l os e ? br es
or s tif f ened c el l u l os e ? br es in th e a bs or bent c or e c a n be
betWeen 0 to 1 00 a nd 80 to 2 0, Wh il e in one embodiment, f or
ex a mp l e th a t With a g r a dient or l a y er ed s tr u c tu r e, l oc a l c on
c entr a tions of u p to 1 00% by Weig h t of p ol y mer c a n be
obta ined. S u c h c ons tr u c tions With r eg ions of h ig h c onc entr a
tions of a bs or bent p ol y mer , Wh er e th e p r op or tion of s u p er a b
s or ber in c er ta in r eg ions is betWeen 60% a nd 1 00% by
Weig h t, or betWeen 9 0% a nd 1 00% by Weig h t a t its h ig h es t,
ea c h ba s ed on th e tota l Weig h t of th e c ons tr u c tion, a r e
des c r ibed, f or ex a mp l e, in US . Pa t. N o. 5 , 669 , 89 4 A , h er eby
inc or p or a ted by r ef er enc e a nd c ons ider ed to c ons titu te p a r t of
th e dis c l os u r e.
Op tiona l l y , a p l u r a l ity of dif f er ent a bs or bent p ol y mer s dif
f er ing , f or ex a mp l e, in a bs or bing s p eed, p er mea bil ity , s tor a g e
c a p a c ity , a bs or p tion u nder l oa d, g r a in s iZ e dis tr ibu tion or
c h emic a l c omp os ition, c a n be u s ed a t th e s a me time. Th es e
dif f er ent p ol y mer s c a n be mix ed tog eth er in th e a bs or bent p a d
or c a n be in dif f er ent l oc a tions in th e a bs or bent c or e. S u c h
dif f er entia ted p os itioning c a n be a l ong th e th ic knes s of th e
a bs or bent p a d or a l ong th e l eng th or br ea dth of th e a bs or bent
p a d.
One or mor e of th e l a y er s of c el l u l os e ? br es or s tif f ened
c el l u l os e ? br es c onta ining s u p er a bs or bent p ol y mer s a r e c on
ta ined in th e a bs or bing a bs or bent l a y er . In a p r ef er r ed
embodiment, c ons tr u c tions of c ombina tions of l a y er s With
h omog eneou s s u p er a b s or bing l a y er s a nd a dditiona l l a y er s a r e
u s ed.
Op tiona l l y , th e c ited s tr u c tu r es c a n be s u p p l emented by
f u r th er l a y er s of p u r e c el l u l os e ? br es or s tif f ened c el l u l os e
? br es on th e s ide f a c ing th e body a nd/ or f a c ing a Wa y f r om th e
body .
Th e c ons tr u c tions des c r ibed a bov e c a n be r ep ea ted a p l u
r a l ity of times , by s ta c king tWo or mor e s imil a r l a y er s or by
s ta c king tWo or mor e dif f er ent c ons tr u c tions . Th e dif f er enc es
ma y be entir el y c ons tr u c tiv e or ma y r es ide in th e ty p e of th e
ma ter ia l s u s ed, s u c h a s th e u s e of a bs or bent p ol y mer s With
dif f er ent p r op er ties or dif f er ent c el l u l os e ty p es .
Op tiona l l y , th e entir e a bs or bent p a d or indiv idu a l l a y er s of
th e a bs or bing a bs or bent l a y er c a n be s ep a r a ted f r om th e oth er
c omp onents With l a y er s of tis s u e or th ey ma y be in dir ec t
c onta c t With oth er l a y er s or c omp onents .
A s a n ex a mp l e, th e s tr u c tu r e f or r a p id u p ta ke a nd dis tr ibu
tion of body ? u ids c a n be s ep a r a ted f r om th e a bs or bing a bs or
bent l a y er by tis s u e or th ey c a n be in dir ec t c onta c t With ea c h
oth er . If no s ep a r a te c ons tr u c tion f or r a p id u p ta ke a nd dis tr i
bu tion of body ? u id ex is ts betWeen th e a bs or bing a bs or bent
l a y er a nd th e ? u id-p er mea bl e c ov er f a c ing th e body , bu t th e
ef f ec t of ? u id dis tr ibu tion is to be obta ined, f or ex a mp l e by
u s ing a s p ec ia l ? u id-p er mea bl e c ov er on th e body s ide, th e
? u id-p er mea bl e c ov er f a c ing th e body c a n op tiona l l y be s ep a
r a ted f r om th e ? u id-a bs or bing a bs or bent l a y er by a tis s u e.
Op tiona l l y , ins tea d of tis s u e, a nonWov en f a br ic c a n be
a dded to th e ? u id-a bs or bing a bs or bent l a y er . Both c omp o
nents r es u l t in th e des ir ed s ide ef f ec t of s ta bil is ing a nd ? x ing
th e a bs or bent c or e Wh en mois t.
Pr oc es s f or p r odu c ing th e ? u id-a bs or bing a bs or bent l a y er .
F ibr e-c onta ining , s u p er a bs or ber -c onta ining , ? u id dis tr ib
u ting a nd s tor ing l a y er s c a n be g ener a ted by a p l u r a l ity of
p r oc es s es .
Es ta bl is h ed c onv entiona l p r oc es s es , s u mma r is ed by th e
s kil l ed p er s on a s dr u m f or ming With th e a s s is ta nc e of s h a p ing
Wh eel s , p oc kets a nd p r odu c t s h a p es a nd s u ita bl e c or r es p ond
ing dos ing a p p a r a tu s f or th e r a W ma ter ia l s , a r e s u p p l emented
by moder n p r oc es s es s u c h a s th e a ir l a id p r oc es s ( eg EP 85 0
US 8, 2 47, 640 B2
1 1
61 5 , c n. 4 l ine 3 9 to c n. 5 l ine 2 9 , US . Pa t. N o. 4, 640, 81 0)
With a l l ty p es of dos ing , dep os ition of ? br es a nd ? x ing s u c h a s
h y dr og en bonding ( e. g . DE 1 9 7 5 0 89 0, c n. 1 l ine 45 to c n. 3
l ine 5 0, th er r no bonding , l a tex bonding ( e. g . EP 85 0 61 5 , c n.
8 l ine 3 3 to c n. 9 l ine 1 7 a nd h y br id bonding , th e Wet l a id
p r oc es s ( eg PCT WO 9 9 / 49 9 05 , c n. 4 l ine 1 4 to c n. 7 l ine 1 6) ,
c a r ding , mel t bl oWn, s p u n bl oWn p r oc es s es a nd s imil a r p r o
c es s es f or th e p r odu c tion of s u p er a bs or ber -c onta ining non
Wov ens ( a s de? ned by EDA N A , Br u s s el s ) , a l s o c ombina tions
of th es e p r oc es s es With oth er nor ma l meth ods f or th e p r odu c
tion of th e c ited ? u id s tor a g e mea ns . Th e doc u ments c ited
a bov e a r e h er eby inc or p or a ted by r ef er enc e a nd s h ou l d be
c ons ider ed to c ons titu te p a r t of th e dis c l os u r e.
F u r th er p r oc es s es th a t c a nbe c ons ider ed a r e th e p r odu c tion
of l a mina tes in th e br oa des t s ens e a nd th e p r odu c tion of
ex tr u ded a nd c o-ex tr u ded, Wet a nd dr y s tr u c tu r es a nd p os t
f or med s tr u c tu r es .
A c ombina tion of th es e p r oc es s es With ea c h oth er is a l s o
p os s ibl e.
Cons tr u c tions f or r a p id u p ta ke a nd dis tr ibu tion of body
? u ids
A c ons tr u c tion f or r a p id u p ta ke a nd dis tr ibu tion of body
? u ids c ons is ts , f or ex a mp l e, of c h emic a l l y s tif f ened ( modi
? ed) c el l u l os e ? br es or h ig h l of t f a br ic s of h y dr op h il ic or
h y dr op h il is ed ? br es or a c ombina tion of th e tWo.
Ch emic a l l y s tif f ened, modi? ed c el l u l os e ? br es c a n, f or
ex a mp l e, be p r odu c ed f r om c el l u l os e ? br es , Wh ic h a r e c h emi
c a l l y tr a ns f or med by c r os s -l inking a g ents s u c h a s C2 -C8 dia l
deh y des , C2 -C8 monoa l deh y des With a n a dditiona l a c id f u nc
tion, or C2 -C9 p ol y c a r bon a c ids . Pa r tic u l a r ex a mp l es a r e:
g l u ta r a l deh y de, g l y ox a l , g l y ox a l ic a c id or c itr ic a c id. Ca tioni
c a l l y modi? ed s ta r c h es or p ol y a mide-ep ic h l or h y dr in r es ins
( f or ex a mp l e KYMEN E 5 5 7H, Her c u l es l nc . , Wil ming ton,
Del . ) a r e a l s o knoWn. Cr os s -l inking p r odu c es a tWis ted,
c r u mp l ed s tr u c tu r e th a t is s ta bl e, Wh ic h a dv a nta g eou s l y
a f f ec ts th e r a te of ? u id u p ta ke.
Weig h t p er u nit a r ea a nd dens ity of a bs or bent a r tic l es
Th e a bs or bent h y g iene p r odu c ts c a n v a r y Widel y in Weig h t
p er u nit a r ea a nd th ic knes s a nd th u s in dens ity . Ty p ic a l l y , th e
dens ity of th e a bs or bent c or e is in th e r a ng e 0. 08 to 0. 2 5
g / c m3 . Th e Weig h t p er u nit a r ea is betWeen 1 0 a nd 1 000 g / m2 ,
a nd p r ef er a bl y th e Weig h t p er u nit a r ea is betWeen 1 00 a nd
600 g / m2 ( s ee a l s o US . Pa t. N o. 5 , 669 , 89 4, h er eby inc or p o
r a ted by r ef er enc e a nd c ons ider ed to c ons titu te p a r t of th e
dis c l os u r e) . Th e dens ity nor ma l l y v a r ies ov er th e l eng th of th e
a bs or bent c or e. Th is is a s a r es u l t of p r edeter mined dos ing of
th e c el l u l os e ? br e or s tif f ened c el l u l os e ? br e or th e a mou nt of
th e s u p er a bs or bent p ol y mer , a s in p r ef er r ed embodiments ,
th es e c omp onents a r e mor e c onc entr a ted in th e f r onta l a r ea of
th e a bs or bent dis p os a bl e a r tic l es .
Th is del iber a te inc r ea s e in th e c onc entr a tion of a bs or bent
ma ter ia l in p a r tic u l a r r eg ions of th e a bs or bent c or e c a n be
a c h iev ed in oth er Wa y s , f or ex a mp l e by p r odu c ing a n a p p r o
p r ia tel y dimens ioned ? a t f or m u s ing a n a ir l a id or Wet l a id
p r oc es s c ons is ting of h y dr op h il ic c el l u l os e ? br es , op tiona l l y
f r om s tif f ened c el l u l os e ? br es , op tiona l l y f r om s y nth etic
? br es ( f or ex a mp l e p ol y ol e? ns ) a nd s u p er a bs or bent p ol y mer s
a nd th en f ol ding it ba c k or s ta c king
Tes t Meth ods
Unl es s oth er Wis e indic a ted, th e f ol l oWing tes ts a r e c a r r ied
ou t u s ing p ol y mer s With a p a r tic l e s iZ e of 3 00 to 600 u m
( deter mined u s ing th e s c r een meth od) .
A nti-Ca king Tes t:
5 g : 0. 1 of p ol y mer With a p a r tic l e s iZ e of 1 5 0 to 1 80 u m is
Weig h ed into a n a l u miniu m Weig h ing boa t ( 5 7 mm) a nd dis
tr ibu ted h omog eneou s l y ov er th e entir e boa t. Th e boa t is
Weig h ed. Th en th e boa t is p l a c ed in a h ea ted c a binet a t a
2 0
2 5
3 0
3 5
40
45
5 0
5 5
60
65
1 2
temp er a tu r e of 3 5 0 C. With a r el a tiv e h u midity of 80% f or 3 ,
6 or 2 4 h . Th en th e boa t is Weig h ed a g a in. A f u r th er boa t is
Weig h ed a nd a s iev e With a mes h of 1 . 5 mm is p l a c ed ov er it.
Th e s a mp l e is tip p ed onto th e s iev e. A f ter ta p p ing l ig h tl y on
th e s iev e a nu mber of times , th e Weig h t of th e p r odu c t th a t h a s
f a l l en th r ou g h th e s iev e is mea s u r ed.
Th e tes t is c ons ider ed to h a v e been p a s s ed Wh en mor e th a n
9 0% by Weig h t of th e p r odu c t f a l l s th r ou g h th e s iev e. Th e
Wa ter u p ta ke of th e p r odu c t is a l s o deter mined.
Meth od f or Mea s u r ing S u r f a c e Tens ion:
Mea s u r ement of S u r f a c e Tens ion of A q u eou s S ol u tions Us ing
a Tr a u be-Ger h a r dt S ta l a g mometer .
A s ta l a g mometer is a ty p e of v ol u metr ic p ip ette th a t emp
ties into a v er y c a r ef u l l y p r odu c ed dr ip s u r f a c e. On th is p ol
is h ed s u r f a c e, dr op l ets f or m one a f ter th e oth er , th e s iZ e of
Wh ic h is dep endent on th e s u r f a c e tens ion of th e p r odu c t
u nder c ons ider a tion. Th e h ig h er th e s u r f a c e tens ion, th e l a r g er
th e dr op l ets , a nd v ic e v er s a . Th e v ol u me of th e p ip ette is
c a l ibr a ted With c ir c u l a r ma r ks . S inc e th e v ol u me is c ons ta nt
a nd th e dr op l et s iZ e is dep endent on th e s u r f a c e tens ion, th e
nu mber of dr op l ets is a dir ec t mea s u r e of th e s u r f a c e tens ion.
Th e v a l u e th a t is mea s u r ed, th er ef or e, is c omp a r ed With th e
nu mber of dr op l ets of p u r e Wa ter , th e s u r f a c e tens ion of Wh ic h
is knoWn.
1 5 0 g of 0. 9 % N a Cl s ol u tion is p l a c ed in a 2 5 0 ml bea ker
a nd s tir r ed With a ma g netic s tir r er ( 2 00 r p m) . 1 g of th e tes t
p ol y mer is s l oWl y s c a tter ed in th e s p ou t f or med by th e 0. 9 %
N a Cl s ol u tion. Wh en s c a tter ing is c omp l ete, th e s ol u tion is
s tir r ed f or 3 minu tes . It is th en a l l oWed to s ta nd f or 1 5 min
u tes .
Th e tes t s ol u tion is dr a Wn u p to Wel l bey ond th e u p p er
p ip ette v ol u me ma r k u s ing a p ip ette bu l b. Th e nu mber of
dr op l ets betWeen th e u p p er a nd l oWer ma r k a r e c ou nted. Ea c h
s ol u tion is tes ted tWic e.
Ca l c u l a tion of s u r f a c e tens ion in mN / mIN u mber of
dr op l ets of p u r e Wa ter > < 72 . 75 * / tes t s a mp l e dr op
l et nu mber * ( s u r f a c e tens ion of Wa ter in mN / m) .
Mea s u r ing th e s u r f a c e tens ion es ta bl is h es h oW mu c h c oa t
ing a g ent ma y be r el ea s ed into a n a q u eou s env ir onment. In
oth er Wor ds , th is mea s u r ement es ta bl is h es h oW Wel l th e c oa t
ing a g ent is bonded to th e p ol y mer . If th e s u r f a c e tens ion is
r edu c ed by th e c oa ting , th en th e p r obl em of r e-Wetting c a n
oc c u r . Re-Wetting c a u s es ? u ids , f or ex a mp l e u r ine, th a t h a v e
a l r ea dy been a bs or bed to be r el ea s ed, f or ex a mp l e, by p r es
s u r e on th e 0s Wol l en g el , mea ning th a t th e h y g iene a r tic l e is
not c omf or ta bl e f or th e Wea r er .
Retention:
Th e r etention is obta ined u s ing th e tea ba g meth od a nd th e
a v er a g e of th r ee mea s u r ements is ta ken. A bou t 2 00 mg of
p ol y mer is s ea l ed in a tea ba g a nd s oa ked in 0. 9 % N a Cl
s ol u tion f or 3 0 minu tes . Th en th e tea ba g is c entr if u g ed in a
c entr if u g e ( 2 3 c m dia meter , 1 400 r p m) f or 3 minu tes a nd th en
Weig h ed. A tea ba g With no a bs or bent p ol y mer is r u n a t th e
s a me time a s a r ef er enc e.
Retention [ g / g ] : endoth er mic Weig h t-r ef er enc e
Weig h t/ s ta r ting Weig h t
F l u id Up ta ke Under 0. 9 p s i Loa d, A UL:
0. 1 6 g of p ol y mer is a c c u r a tel y Weig h ed into a Pl ex ig l a s
c y l inder With a n inter na l dia meter of 2 5 . 4 mm ? tted With a
400 mes h ny l on s iev e ba s e. Th e l a y er of p ol y mer ev enl y
dis tr ibu ted on th e s iev e ba s e is c ov er ed With a 2 6. 1 mm
dia meter Te? on dis k a nd Weig h ed doWn With a c y l indr ic a l
p is ton Weig h ing 3 3 2 . 4 g . Th e Te? on dis k a nd p is ton tog eth er
c ons titu te a l oa d of 63 g / c m2 , or 0. 9 p s i. Th e Weig h ed c y l inder
is th en p l a c ed on a g l a s s ? l ter p l a te in a dis h With 0. 9 % N a Cl
s ol u tion th e dep th of Wh ic h ex a c tl y c or r es p onds to th e dep th
US 8, 2 47, 640 B2
1 3
of th e ? l ter p l a te. A f ter th e c y l inder a s s embl y h a s been l ef t f or
1 h ou r to a l l ow th e 0. 9 % N a Cl s ol u tion to be a bs or bed, th e
? l ter p a p er is p a tted f r ee of ex c es s tes t s ol u tion a nd th en
r e-Weig h ed a nd th e A UL is c a l c u l a ted a s f ol l oWs :
A UL: ? na l Weig h t ( c y l inder a s s embl y + s Wol l en p ol y
mer ) s ta r t Weig h t ( c y l inder a s s embl y + non s Wol
l en p ol y mer ) / p ol y mer s ta r t Weig h t
EXA MPLES
Th e inv ention Wil l noW be il l u s tr a ted by ex a mp l es . Th e
ex a mp l es a r e g iv en p u r el y by Wa y of il l u s tr a tion a nd in no
Wa y l imit th e s c op e of th e inv ention.
Th e f ol l owing a bbr ev ia tions a r e u s ed:
A BA H 2 . 2 ' -a Z o-bis -a midinop r op a ne-dih y dr oc h l or ide
A IBN 2 . 2 ' -a Z o-bis -2 -meth y l p r op ionitr il e
A MPS 2 -a c r y l a mido-2 -meth y l p r op a nes u l p h onic a c id
BO 2 -bu ty l -oc ta nol
EO eth y l ene ox ide ( 1 , 2 -ep ox y eth a ne)
IHD is oh ex a dec a ne
ITDA is otr idec y l a l c oh ol
ITS is otr idec y l s tea r a te
DN deg r ee of neu tr a l is a tion, mol e-%
OA BOE ol eic a c id bu ty l oc ty l es ter
ROS ME r a p es eed oil a c id meth y l es ter
TA MA Ctr ia l l y l meth y l a mmoniu m c h l or ide
Comp a r a tiv e Ex a mp l e 1
US . Pa t. N o. 5 , 72 8, 742
1 000 p p m of Eth oq u a d 0/ 1 2 dis s ol v ed in 3 g of is op r op a nol
Wa s a dded, u s ing a s y r ing e, s tir r ing With a mix er , to 5 0 g of
p oWder ed p ol y a c r y l a te th a t h a d been 70% neu tr a l iZ ed a nd
s u r f a c e c r os s -l inked ( F a v or S XM 880 , a v a il a bl e f r om
S toc kh a u s en GmbH & Co. KG) , With a r etention of 3 2 g / g in
0. 9 % N a Cl -s ol u tion a nd a A ULOS PS Z - of 2 2 . 1 g / g . Th e p ol y mer
Wa s r ol l ed f or 60 minu tes on a r ol l benc h a t a mbient temp er a
tu r e. Th e p r odu c t did not p a s s th e 3 h a nti-c a king tes t
des c r ibed a bov e.
Eth oq u a d 0/ 1 2 : ol ey l meth y l di ( 2 -h y dr ox y eth y l ) a mmoniu m
c h l or ide
Comp a r a tiv e Ex a mp l e 2
US . Pa t. N o. 5 , 72 8, 742
1 000 p p m of A r q u a d 1 6-5 0 dis s ol v ed in 3 g of is op r op a nol
Wa s a dded, u s ing a s y r ing e, s tir r ing With a mix er , to 5 0 g of
p oWder ed p ol y a c r y l a te a s des c r ibed in c omp a r a tiv e ex a mp l e
1 ( F a v or S XM880 , a v a il a bl e f r om S toc kh a u s en GmbH &
Co. KG) . Th e p ol y mer Wa s r ol l ed f or 60 minu tes on a r ol l
benc h a t a mbient temp er a tu r e. Th e p r odu c t did not p a s s th e 3
h a nti-c a king tes t des c r ibed a bov e.
A r q u a d 1 6-5 0: Hex a dec y l tr imeth y l a mmoniu m Ch l or ide
Pr odu c tion of Pol y mer PoWder s 1 -5
PoWder 1 :
2 9 0 g of a c r y l ic a c id Wa s div ided into tWo eq u a l p or tions .
One p or tion Wa s a dded to 45 8. 5 g of H2 0. 0. 85 g of p ol y eth
y l ene g l y c ol 3 00-dia c r y l a te a nd 1 . 5 g of a l l y l ox y p ol y eth y l
ene g l y c ol a c r y l ic a c id es ter Wer e dis s ol v ed in th e s ec ond
p or tion of a c r y l ic a c id a nd th en a dded to th e Wa ter . Th e
s ol u tion Wa s c ool ed to 1 0 C. , th en a tota l of 2 2 5 . 4 g of 5 0%
s odiu m h y dr ox ide Wa s s l oWl y a dded With c ool ing s o th a t th e
temp er a tu r e did not ex c eed 3 00 C. Th e s ol u tion Wa s th en
? u s h ed With nitr og en a t 2 0 C. a nd th en c ool ed a g a in. Wh en
th e s ta r t temp er a tu r e of 4 C. h a d been r ea c h ed, th e initia tor
2 0
2 5
3 0
3 5
40
45
5 0
5 5
60
65
1 4
s ol u tions ( 0. 1 g of 2 . 2 ' -a Z obis -2 -a midinop r op a ne-dih y dr o
c h l or ide in 1 0 g H2 O, 1 . 0 g s odiu m p er ox y dis u l p h a te in 1 0 g
H2 O, 0. 1 g 3 0% h y dr og en p er ox ide s ol u tion in 1 g H2 0 a nd
0. 01 5 g a s c or bic a c id in 2 g Wa ter ) Wa s a dded. A f ter th e ? na l
temp er a tu r e of 1 02 C. h a d been r ea c h ed, th e g el th a t h a d
f or med Wa s dis integ r a ted a nd th en dr ied f or 9 0 minu tes a t
1 5 0 C. th e dr ied p ol y mer Wa s c oa r s el y c r u s h ed, g r ou nd a nd
s c r eened to a p oWder With a p a r tic l e s iZ e of 1 5 0 to 85 0 u m.
PoWder 2 :
3 00 g of a c r y l ic a c id Wa s div ided into tWo eq u a l p or tions .
One p or tion Wa s a dded to 42 9 . 1 g of H2 0. 0. 3 6 g of tr ia l l y
l a mine, 1 . 05 g of a l l y l ox y p ol y eth y l ene g l y c ol a c r y l ic a c id
es ter a nd 1 2 g of meth ox y p ol y eth y l ene g l y c ol ( 2 2 EO) meth
a c r y l a te Wer e dis s ol v ed in th e s ec ond p or tion of a c r y l ic a c id
a nd th en a dded to th e Wa ter . Th e s ol u tion Wa s c ool ed to 1 0 C.
Th en a tota l of 2 3 3 . 1 g of 5 0% s odiu m h y dr ox ide Wa s s l oWl y
a dded With c ool ing s o th a t th e temp er a tu r e did not ex c eed 3 0
C. Th e s ol u tion Wa s th en ? u s h ed With nitr og en a t 2 0 C. a nd
th en c ool ed a g a in. Wh en th e s ta r t temp er a tu r e of 4 C. h a d
been r ea c h ed, 0. 9 g of s odiu m c a r bona te a nd th e initia tor
s ol u tions ( 0. 1 g of 2 . 2 " -a Z obis -2 -a midinop r op a ne-dih y dr o
c h l or ide in 1 0 g H2 O, 0. 1 5 g of s odiu mp er ox y dis u l p h a te in 1 0
g H2 O, 0. 1 g of 3 0% h y dr og en p er ox ide s ol u tion in 1 g H2 0
a nd 0. 01 g a s c or bic a c id in 2 g Wa ter ) Wer e a dded. A f ter th e
? na l temp er a tu r e of 1 04 C. h a d been r ea c h ed, th e g el th a t h a d
f or med Wa s dis integ r a ted a nd th en dr ied f or 9 0 minu tes a t
1 5 0 C. Th e dr ied p ol y mer Wa s c oa r s el y c r u s h ed, g r ou nd a nd
s c r eened to a p oWder With a p a r tic l e s iZ e of 1 5 0 to 85 0 u m.
PoWder 3 :
Wa s a non s u r f a c e c r os s -l inked p ol y a c r y l ic a c id ( f a br ic a
tion p r odu c t of F a v or S XM880 ) , 70% neu tr a l iZ ed a nd With
a r etention of 40 g / g in 0. 9 % N a Cl s ol u tion a nd a nA UL of 8. 7
g / g .
PoWder 4:
2 80 g of a c r y l ic a c id Wa s div ided into tWo eq u a l p or tions .
One p or tion Wa s a dded to 5 1 7. 04 g of H2 0. 0. 2 8 g of tr ia l l y
l a mine, 0. 72 g of a l l y l ox y p ol y eth y l ene g l y c ol a c r y l ic a c id
es ter a nd 7. 5 1 g of meth ox y p ol y eth y l ene g l y c ol ( 2 2 EO)
meth a c r y l a te Wer e dis s ol v ed in th e s ec ond p or tion of a c r y l ic
a c id a nd th en a dded to th e Wa ter . Th e s ol u tion Wa s c ool ed to
1 0 C. Th en a tota l of 1 70. 9 7 g of 5 0% s odiu m h y dr ox ide Wa s
s l oWl y a dded With c ool ing s o th a t th e temp er a tu r e did not
ex c eed 3 0 C. Th e s ol u tion Wa s th en ? u s h ed With nitr og en a t
2 0 C. a nd th en c ool ed a g a in. Wh en th e s ta r t temp er a tu r e of
4 C. h a d been r ea c h ed, 0. 9 g of s odiu m c a r bona te a nd th e
initia tor s ol u tions ( 0. 1 g of 2 . 2 " -a Z obis -2 -a midinop r op a ne
dih y dr oc h l or ide in 1 0 g of H2 0, 1 . 0 g of s odiu m p er ox y dis
u l p h a te in 1 0 g H2 O, 0. 07 g of 3 0% h y dr og en p er ox ide s ol u
tion in 1 g H2 0 a nd 0. 01 g a s c or bic a c id in 2 g Wa ter ) Wer e
a dded. A f ter th e ? na l temp er a tu r e of 1 02 C. h a d been
r ea c h ed, th e g el th a t h a d f or med Wa s dis integ r a ted a nd th en
dr ied f or 9 0 minu tes a t 1 5 0 C. Th e dr ied p ol y mer Wa s
c oa r s el y c r u s h ed, g r ou nd a nd s c r eened to a p oWder With a
p a r tic l e s iZ e of 1 5 0 to 85 0 u m.
PoWder 5 :
Wa s th e non s u r f a c e c r os s -l inked p ol y a c r y l ic a c id of c om
p a r a tiv e Ex a mp l e 1 With a r etention of 3 2 g / g in 0. 9 % N a Cl
s ol u tion a nd a n A UL of 2 2 . 1 g / g ( F a v or S XM880 ) .
Ex a mp l e 1
A mix tu r e of 0. 01 5 g of Comp er l a n COD, 0. 2 5 g of eth y l
ene c a r bona te a s a c r os s -l inking a g ent, 1 . 0 g of H2 0 a nd 4. 0
g of a c etone Wa s a dded to 5 0 g of p oWder 1 , s tir r ing With a
mix er ( Kr u p s Dr y Mix Ty p e 7007) on its h ig h es t s etting . Th e
c oa ted p ol y mer Wa s ev enl y p ou r ed into a p h otog r a p h ic ta nk
a nd dr ied f or 3 0 minu tes in a c ir c u l a ting a ir dr y ing ov en a t
US 8, 2 47, 640 B2
1 5
1 80 C. Th e r etention, A UL v a l u e, s u r f a c e tens ion a nd a nti
c a king tes ts Wer e c a r r ied ou t a s des c r ibed a bov e a nd th e
r es u l ts a r e s h oWn in Ta bl e 1 .
Ex a mp l es 2 -1 7
Ex a mp l es 2 -1 7 Wer e c a r r ied ou t a s des c r ibed f or Ex a mp l e
1 . Th e p oWder u s ed, a dded c omp ou nds , th e a mou nts of th e
c omp ou nds a nd th e du r a tion a nd temp er a tu r e of th e h ea t
tr ea tment a r e s h oWn in Ta bl e I a l ong With th e c or r es p onding 1 0
r etention, A UL, s u r f a c e tens ion a nd th e r es u l ts of th e a nti
c a king tes ts .
Comp a r a tiv e Ex a mp l e 3
A mix tu r e of 0. 05 g of Imbentin CMEA / 045 in 1 . 0 g of
H2 0 Wa s a dded to 5 0 g of p oWder 5 , s tir r ing With a mix er
( Kr u p s Dr y Mix Ty p e 7007) on its h ig h es t s etting ; it Wa s th en
s tir r ed f or a f u r th er 2 minu tes . N o h ea t tr ea tment Wa s c a r r ied
ou t. Th e p ol y mer did not p a s s th e 3 h a nti-c a king tes t a nd h a d 2 0
r edu c ed p ou r a bil ity .
Th e p ol y mer h a d a r etention of 3 1 . 4 g / g a nd a nA UL of 2 1 . 3
1 6
Ex a mp l e 1 8
A mix tu r e of 0. 05 g of Imber tin CMEA / 045 in 1 . 0 g of H2 O
Wa s a dded to 5 0 g of p oWder 5 , s tir r ing With a mix er ( Kr u p s
Dr y Mix Ty p e 7007) on its h ig h es t s etting . It Wa s th en s tir r ed
f or a f u r th er 2 minu tes . Th e p r odu c t Wa s p ou r ed into a p h o
tog r a p h ic ta nk a nd dr ied f or 2 0 minu tes in a c ir c u l a ting a ir
dr y ing ov en a t 1 80 C. Th e tr ea ted p ol y mer p a s s ed th e a nti
c a king tes t. Its r etention, A UL a nd s u r f a c e tens ion a r e s h oWn
in Ta bl e 1 .
Ex a mp l e 1 9
A mix tu r e of 0. 05 g of Imbentin CMEA / 045 in 1 . 0 g of
H2 0 Wa s a dded to 5 0 g of p oWder 5 , s tir r ing With a mix er
( Kr u p s Dr y Mix Ty p e 7007) on its h ig h es t s etting . It Wa s th en
s tir r ed f or a f u r th er 2 minu tes . Th e p r odu c t Wa s p ou r ed into a
p h otog r a p h ic ta nk a nd dr ied f or 1 5 minu tes in a c ir c u l a ting a ir
dr y ing ov en a t 1 9 0 C. Th e tr ea ted p ol y mer p a s s ed th e a nti
c a king tes t. Its r etention, A UL a nd s u r f a c e tens ion a r e s h oWn
in Ta bl e 1 .
TA BLE 1
Conc n, Wt 3 h
% With Temp er a tu r e/ a nti- A UL S u r f a c e
A nti- r es p ec t to time c a king Retention 0. 9 p s i tens ion
Ex a mp l e Powder c a king s u bs ta nc e p r odu c t [ C. / t] tes t [ g g ] [ g g ] [ mN / m]
1 i 1 80/ 3 0 3 1 . 5 1 7. 7
1 1 Comp er l a n 0. 01 5 1 80/ 3 0 + 3 1 . 5 1 7. 6 72 . 5
COD
2 1 Comp er l a n 0. 06 1 80/ 3 0 + 3 2 . 8 1 7. 4 72 . 5
LD
2 i 1 80/ 3 0 3 4. 8 2 3 . 5 i
3 2 Ma r l a z in 0. 03 1 80/ 40 + 3 5 . 0 2 3 . 7 72 . 5
L1 0
4 2 Ma r l a z in 0. 1 0 1 80/ 40 + 3 4. 9 2 3 . 8 72 . 5
L1 0
5 2 S er dox 0. 1 0 1 80/ 3 0 + 3 4. 5 2 2 . 5 72 . 5
N XC3
6 2 S er dox 0. 1 0 1 80/ 40 + 3 5 . 0 2 1 . 0 72 . 5
N XC6
7 2 S er dox 0. 1 0 1 80/ 40 + 3 4. 8 2 2 . 0 72 . 5
N XC 1 4
8 2 S er dox 0. 05 1 80/ 40 + 3 5 . 2 2 2 . 3 72 . 5
N XC6
3 i 1 9 0/ 2 5 3 2 . 4 2 1 . 2 i
9 3 S er dox 0. 1 0 1 80/ 3 5 + 3 2 . 3 1 9 . 1 72 . 5
N XC6
1 0 3 Ma r l a z in 0. 1 0 1 80/ 3 5 + 3 2 . 3 2 0. 3 72 . 5
OL 2 0
1 1 3 Ma r l a z in L1 0 0. 1 0 1 80/ 3 5 + 3 2 . 3 1 9 . 5 72 . 5
1 2 3 Comp er l a n 0. 2 1 80/ 3 0 + 3 1 . 3 2 1 . 1 72 . 5
COD
1 3 3 S er dox 0. 1 1 80/ 3 0 + 3 1 . 7 2 1 . 2 72 . 5
N XC6
1 4 3 Imbentin 0. 1 1 9 0/ 2 0 + 3 2 . 1 2 1 . 0 72 . 5
CMEN 045
1 5 3 Imbentin 0. 2 1 9 0/ 2 0 + 3 2 . 0 2 0. 8 72 . 5
CMEN 045
4 i 1 70/ 2 5 3 0. 5 2 1 . 0 i
1 6 4 S tokomin 0. 1 1 70/ 2 5 + 3 0. 1 2 1 . 2 72 . 5
S 1 0
1 7 4 S er dox 0. 1 1 70/ 2 5 + 3 0. 9 2 0. 4 72 . 5
N XC3
5 i 3 2 . 0 2 2 . 1
1 8 5 Imbentin 0. 05 1 80/ 2 0 + 3 0. 9 2 0. 8 72 . 5
CMEN 045
US 8, 2 47, 640 B2
1 7 1 8
TA BLE l -c ontinu ed
Conc n, wt 3 h
% with Temp er a tu r e/ a nti- A UL S u r f a c e
A nti- r es p ec t to time c a king Retention 0. 9 p s i tens ion
Ex a mp l e Powder c a king s u bs ta nc e p r odu c t [ 0 C. / t] tes t [ g g ] [ g g ] [ mN / m]
1 9 5 Imbentin 0. 05 1 9 0/ 1 5 + 3 0. 8 2 1 . 0 72 . 5
CMEA / 045
S tokomin S 1 0 = S tea r y l a mine, eth ox y l a ted with 1 0 EO;
Comp er l a n COD = c oc onu t a c id dieth a nol a mide ( Henkel KGa A ) ;
Comp er l a n LD = l a u r ic a c id dieth a nol a mide ( Henkel KGa A ) ;
Comp er l a n 1 00 = c oc onu t a c id monoeth a nol a mide ( Henkel KGa A ) ;
Ma r l a z in L1 0 = l a u r y l a mine, eth ox y l a ted with 1 0 EO ( Contens io) ;
Ma r l a z in OL 2 0 = ol ey l a mine, eth ox y l a ted with 2 0 EO ( Contens io) ;
S er dox N ' XC 3 = Ol eic a c id monoeth a nol a mide, eth ox y l a ted with 3 EO ( Condea ) ;
S er dox N ' XC 6 = Ol eic a c id monoeth a nol a mide, eth ox y l a ted with 6 EO ( Condea ) ;
S er dox N ' XC 1 4 = Ol eic a c id monoeth a nol a mide, eth ox y l a ted with 1 4 EO ( Condea ) ;
Imbentin CMIA / 045 = c oc onu t a c id monoeth a nol a mide, eth ox y l a ted with 4. 5 EO
Comp a r a tiv e v a l u e f or s u r f a c e tens ion of wa ter : O = 72 . 5 mN / m
+ : tes t p a s s ed
: tes t f a il ed
2 0
Comp a r a tiv e Ex a mp l e 4 Ex a mp l e 2 2
0. 5 g of eth y l ene c a r bona te, 2 g of wa ter a nd 0. 2 5 g of
A l 2 ( S O4) 3 > < 1 8H2 O wer e mix ed tog eth er a nd a dded u s ing a
s y r ing e to 5 0 g of p owder 3 , s tir r ing with a mix er ( Kr u p s Dr y
Mix Ty p e 7007) on its h ig h es t s etting . Th e p r odu c t wa s
p ou r ed into a p h otog r a p h ic ta nk a nd dr ied f or 5 0 minu tes in a
c ir c u l a ting a ir dr y ing ov en a t 1 700 C.
Th e tr ea ted p ol y mer f a il ed th e 3 h a nti-c a king tes t. Its
r etention, A UL a nd s u r f a c e tens ion a r e s h own in Ta bl e 2 .
Ex a mp l e 2 0
Powder 3 wa s mix ed with 0. 7% by weig h t of eth y l ene
c a r bona te, 1 . 8% by weig h t of wa ter , 0. 2 % by weig h t of A 1 2
( S O4) 3 > < 1 4H2 O a nd 0. 2 % by weig h t of Imbentin CMEA / 02 4
( Kol b A G) in a mix er ( Kr u p s Dr y Mix Ty p e 7007) on its
h ig h es t s etting , a nd c oa ted. Th en, th e tr ea ted p ol y mer wa s
p l a c ed in a bl a de dr y er a nd l ef t f or 1 0 minu tes a t a temp er a tu r e
of 1 1 0 C.
Th e p r odu c t p a s s ed th e 3 h a nti-c a king tes t. Its r etention
a nd A UL a r e s h own in Ta bl e 2 .
Ex a mp l e 2 1
0. 5 g of eth y l ene c a r bona te, 0. 5 g of a c etone, 2 g of wa ter ,
0. 075 g of Z nCl 2 a nd 0. 05 g of Imbentin CMEA / 045 ( Kol b
A G) wer e mix ed a nd a dded to 5 0 g of p owder 3 u s ing a
s y r ing e, s tir r ing with a mix er ( Kr u p s Dr y Mix Ty p e 7007) on
its h ig h es t s etting . Th en, th e p ol y mer wa s p ou r ed into a p h o
tog r a p h ic ta nk a nd dr ied f or 5 0 minu tes in a c ir c u l a ting a ir
dr y ing ov en a t 1 700 C.
Th e tr ea ted p ol y mer p a s s ed th e 3 h a nti-c a king tes t. Its
r etention, A UL a nd s u r f a c e tens ion a r e s h own in Ta bl e 2 .
2 5
3 0
3 5
40
45
5 0
Powder 3 wa s c oa ted by a dding a mix tu r e of 2 % by weig h t
of wa ter a nd 1 % by weig h t of H2 S O4 ( 9 8%) with a s y r ing e,
s tir r ing u s ing a mix er . 0. 5 g of eth y l ene c a r bona te, 0. 5 g of
a c etone, 0. 05 g of Imbentin CMEA / 045 a nd 1 g of wa ter wer e
mix ed tog eth er a nd a dded u s ing a s y r ing e to 5 0 g of p owder 3
s tir r ing with th e mix er ( Kr u p s Dr y Mix Ty p e 7007) on its
h ig h es t s etting . Th en, th e p ol y mer wa s p ou r ed into a p h oto
g r a p h ic ta nk a nd dr ied f or 5 0 minu tes in a c ir c u l a ting a ir
dr y ing ov en a t 1 700 C.
Th e tr ea ted p ol y mer p a s s ed th e 3 h a nti-c a king tes t. Its
r etention, A UL a nd s u r f a c e tens ion a r e s h own in Ta bl e 2 .
Ex a mp l e 2 3
0. 5 g of eth y l ene c a r bona te, 0. 5 g of a c etone, 1 g of wa ter ,
1 g of H3 PO4 ( 85 %) a nd 0. 1 g of Imbentin CMEA / 045 ( Kol b
A G) wer e mix ed tog eth er a nd a dded u s ing a s y r ing e to 5 0 g of
p owder 3 s tir r ing with th e mix er ( Kr u p s Dr y Mix Ty p e 7007)
on its h ig h es t s etting . Th en, th e p ol y mer wa s p ou r ed into a
p h otog r a p h ic ta nk a nd dr ied f or 5 0 minu tes in a c ir c u l a ting a ir
dr y ing ov en a t 1 700 C.
Th e tr ea ted p ol y mer p a s s ed th e 3 h a nti-c a king tes t. Its
r etention, A UL a nd s u r f a c e tens ion a r e s h own in Ta bl e 2 .
Ex a mp l es 2 4-2 7
Ex a mp l es 2 4-2 9 wer e c a r r ied ou t a s des c r ibed f or Ex a mp l e
2 1 , with th e a mou nts of Lewis a c ids a nd Imbentin CMEA /
045 emp l oy ed s h own in Ta bl e 2 . Th e r es u l ts of th e 3 h a nti
c a king tes ts , r etention, A UL a nd s u r f a c e tens ion f or th e
r es p ec tiv e p ol y mer s a r e s h own in Ta bl e 2 .
TA BLE 2
Imbentin* / Temp . / 3 h
Lewis a c id* * time Retention A ULO_9 PS I- A nti
Ex a mp l e Lewis a c id ( Gew. %) ( 0 C. / min) ( g g ) ( g / g ) c a king
Comp . A l 2 ( S O4) 3 x 1 8H2 O 0. 0/ 0. 5 0 1 70/ 5 0 3 1 . 5 2 2 . 6
Ex . 4
2 0 A l 2 ( S O4) 3 x 1 4H2 O 0. 2 / 0. 2 0 1 1 0/ 1 0 3 5 . 7 7. 2 +
2 1 Z nCl 2 0. 1 / 0. 1 5 1 70/ 5 0 3 2 . 8 2 1 . 8 +
2 2 H2 804 0. 1 / 1 . 00 1 70/ 5 0 3 1 . 9 1 9 . 0 +
2 3 H3 PO4 0. 2 / 2 . 00 1 70/ 5 0 3 0. 0 1 7. 1 +
US 8, 2 47, 640 B2
1 9 2 0
TA BLE 2 -c ontinu ed
Imbentin* / Temp . / 3 h
Lewis a c id* * time Retention A ULQQPS Z - A nti
Ex a mp l e Lewis a c id ( Gew. %) ( C. / min) ( g g ) ( g / g ) c a king
2 4 F eCl 3 x 6H2 O 0. 1 / 0. 05 1 70/ 5 0 3 2 . 3 2 1 . 4 +
2 5 Mg S O4x 7H2 O 0. 3 / 0. 1 0 1 70/ 5 0 3 1 . 5 2 3 . 6 +
2 6 A l Cl 3 x 6H2 O 0. 1 / 0. 05 1 60/ 5 0 3 5 . 9 1 4. 0 +
2 7 F eCl 3 x 6H2 O 0. 2 / 0. 1 0 1 70/ 5 0 3 2 . 1 1 9 . 2 +
* Lmbentin 01 / 1 2 / 0045
* * with r es p ec t to c omp onent I
+ : a nti-c a l c ing tes t p a s s ed
: a nti-c a l c ing tes t f a il ed
Ex a mp l es 2 8-2 9 1 5 s u r f a c e c oa ting c omp onent I with a c oa ting a g ent s el ec ted
f r om th e g r ou p c ons is ting of nitr og en-c onta ining , non
0-5 g of eth y l ene Ca r bona te, 2 g of Wa ter , a l u miniu m 5 1 1 1 - ionic s u r f a c ta nts a s c omp onent 1 1 a nd op tiona l l y a Lewis
Ph a te a nd Imbeml n CMEA / 045 ( Kol b A G) Wer e ml Xed a c id a s c omp onent 1 1 1 ; wh er ein s a id s u r f a c ta nt h a s th e
tog eth er a nd a dded u s ing a s y r ing e to 5 0 g of p owder 3 s tir r ing g ener a l f or mu l a I;
with th e mix er ( Kr u p s Dr y Mix Ty p e 7007) on its h ig h es t 2 0
s etting . Th en, th e p ol y mer wa s p ou r ed into a p h otog r a p h ic
ta nk a nd dr ied f or 5 0 minu tes in a c ir c u l a ting a ir dr y ing ov en I
a t 1 70 C. Th e r ea c tion c onditions a nd p r odu c t p r op er ties a r e / R;
s h own 1 n Ta bl e 3 . R1 C N
2 5 | | \
Ex a mp l es 3 0-3 3 0 n R3 Z
Two p ol y a c r y l ic a c ids wer e p r odu c ed with a deg r ee of _ _
neu tr a l is a tion of 65 % or 70% a nd a r etention of 3 4% or 3 2 g / g 1 1 1 Wh l c h
in 0. 9 % a q u eou s N a Cl s ol u tion a s des c r ibed f or th e p r odu c - 3 0 R1 is a n a l ip h a tic C1 IO C3 0 h y dr oc a r bon Z -S u bS titu ted a l i
tion of p owder 1 . 5 0 g of th is p owder ( p a r tic l e s iz e in th e r a ng e p h a tic r es idu e,
1 5 0 to 85 0 u m) wa s mix ed with a mix tu r e c ons is ting of 0. 5 g R2 is s el ec ted f r om a h y dr og en, a n C2 to C2 4 a l ip h a tic
of eth y l ene c a r bona te, 2 g of wa ter , a l u miniu m s u l p h a te> < h y dr oc a r bon r es idu e, a nd
1 4H2 O a nd l mbentin CMEA / 045 u s ing a mix er ( Kr u p s Dr y a h y dr ox y a l ky l ene r es idu e
Mix Ty p e 7007) on its h ig h es t s etting . Th e p owder wa s th en 3 5 R3 , wh ic h ma y be identic a l or dif f er ent, h a s th e s a me
dr ied in a c ir c u l a ting a ir dr y ing ov en in a p h otog r a p h ic ta nk. mea ning a s R2 , p r ov ided th a t with a mide c omp ou nds , a t
Th e r ea c tion c onditions a nd p r op er ties of th e p r odu c ts a r e l ea s t one of r es idu es R2 or R3 r ep r es ents a h y dr ox y a l ky
s h own in Ta bl e 3 . l ene r es idu e or a n a l kox y l a ted h y dr ox y a l ky l ene r es idu e
TA BLE 3
S ta r t A nti- A UL
p r odu c t Retention Temp . Time c a king 0. 9 p s i
Ex . DN g g l mbentinu ) A l 2 ( S O4) 3 x 1 4H2 O( 1 ) C. min tes t( 2 ) Retention g / g
2 8 70 3 9 0. 1 0. 1 1 70 60 6 3 1 . 7 2 2 . 0
2 9 70 3 9 0. 1 0. 2 1 70 60 6 3 1 . 6 2 1 . 5
3 0 65 3 4 0. 2 5 0. 45 1 70 60 2 4 3 0 2 0. 5
3 1 65 3 4 0. 2 5 0. 5 0 1 70 60 2 4 3 0 2 1
3 2 70 3 2 0. 3 0 0. 5 0 1 80 3 0 2 4 2 8 1 9 . 5
3 3 70 3 2 0. 2 5 0. 60 1 80 3 0 2 4 3 0 2 0
Wt % with r es p ec t to p owder
( 2 ) A nti-c a l c ing tes t p a s s ed a ? er 6 or 2 4 h ou r s
Wh a t is c l a imed is : or a c or r es p onding es ter i? ed or a l kox y l a ted or es ter i? ed
1 . A p r oc es s f or th e p r odu c tion of s u p er a bs or bent p ol y mer a nd a l kox y l a ted h y dr ox y a l ky l ene r es idu e with th e de?
p owder with a r edu c ed c a king tendenc y in a mois t env ir on- 5 5 nition g iv en f or R2 a bov e;
ment a nd/ or a t h ig h temp er a tu r es , c omp r is ing th e s tep s of : n is 1 ; a nd Z is a wh ol e nu mber f r om 1 to 4
p r ov iding a c omp onent I wh ic h is a wa ter - or a q u eou s h ea t tr ea ting th e s u r f a c e c oa ted c omp onent I a t a temp er a
? u id-a bs or bing , dr ied, s u r f a c e-c r os s -l inked p ol y mer tu r e of f r om 1 000 C. to 2 5 0 C. to c a u s e c omp onent I to
p owder ba s ed on p ol y mer iz ed monomer s c onta ining a t r ea c t with th e s u r f a c e c r os s -l inking a g ent, th e c oa ting
l ea s t p a r tia l l y neu tr a l iz ed a c id g r ou p s wh er ein th e p ol y - 60 a g ent c omp onent 1 1 a nd op tiona l l y c omp onent Il l ;
mer iz ed monomer s is f or med into a g el wh ic h wa s dr ied
f or a bou t 9 0 minu tes a t a bou t 1 5 0 C. a nd th e dr ied
p ol y mer wa s g r ou nd a nd s c r eened to a p ol y mer p owder
a nd c oa ting th e p ol y mer p owder with a s u r f a c e c r os s
l inking a g ent to f or m th e wa ter - or a q u eou s ? u id-a bs or b
ing , dr ied, p ol y mer p owder c oa ted with a s u r f a c e c r os s
l inking a g ent of c omp onent I; a nd
wh er ein th e s u p er a bs or bent p ol y mer p owder p a s s es th e
A nti-c a king tes t a s s et f or th h er ein.
2 . Th e p r oc es s a c c or ding to c l a im 1 , f u r th er c omp r is ing th e
s tep of mix ing a n a q u eou s s ol u tion of th e c oa ting a g ent( s )
65 with c omp onent I.
3 . Th e p r oc es s a c c or ding to c l a im 1 , f u r th er c omp r is ing th e
s tep of tr ea ting th e p ol y mer bef or e, du r ing , or a f ter its s u r f a c e
US 8, 2 47, 640 B2
2 1
c r os s -l inking With a n a q u eou s s ol u tion of c omp onent 1 1 a nd
op tiona l c omp onent III, with th e a ddition of h ea t.
4. Th e p r oc es s a c c or ding to c l a im 1 , f u r th er c omp r is ing th e
s tep of s imu l ta neou s l y tr a ns f or ming th e a q u eou s s ol u tion of
c omp onent H a nd op tiona l c omp onent Il l a nd s u r f a c e c r os s
l inking th e p ol y mer .
5 . Th e p r oc es s a c c or ding to c l a im 1 Wh er ein s a id nitr og en
c onta ining , non-ionic s u r f a c ta nt is s el ec ted f r om s tea r y
l a mine, eth ox y l a ted With 1 0 eth y l ene ox ide ( EO) u nits , c oc o
nu t a c id dieth a nol a mide, l a u r ic a c id dieth a nol a mide, c oc onu t
a c id monoeth a nol a mide, l a u r y l a mine, eth ox y l a ted With 1 0
E0 u nits , ol ey l a mine eth ox y l a ted With 2 0 E0 u nits , ol eic a c id
monoeth a nol a mide eth ox y l a ted With 3 EO u nits , ol eic a c id
monoeth a nol a mide, eth ox y l a ted With 6 EO u nits , Ol eic a c id
monoeth a nol a mide eth ox y l a ted With 1 4 E0 u nits , or c oc onu t
a c id monoeth a nol a mide eth ox y l a ted With 4. 5 B0.
6. Th e p r oc es s a c c or ding to c l a im 1 Wh er ein s a id c omp o
nent III is s el ec ted f r om a l u minu m s u l f a te, a l u minu m c h l o
r ide, Z inc a c eta te, Z inc c h l or ide, Z inc s u l f a te, ir on c h l or ide,
ma g nes iu m s u l f a te, ma g nes iu m c h l or ide, s u l p h u r ic a c id, s u l
p h u r -c onta ining a c ids , s el enic a c id, nitr ic a c id, p h os p h onic
a c id or p h os p h or u s -c onta ining a c ids a c etic a c id, ox a l ic a c id,
l a c tic a c id, c itr ic a c id, ta r ta r ic a c id or h y dr a ted f or ms of
a l u minu m s u l f a te, a l u minu m c h l or ide, Z inc a c eta te, Z inc c h l o
r ide, Z inc s u l f a te, a nd ir on c h l or ide.
7. Th e p r oc es s a c c or ding to c l a im 6 Wh er ein s a id a l u minu m
s u l f a te is A l 2 ( S O4) 3 > < l 4-l 8H2 O, a nd a l u minu m c h l or ide is
A l Cl 3 > < 6H2 O; Z inc a c eta te is Z n ( CH3 COO) 2 > < 2 H2 O.
8. A s u p er a bs or bent p ol y mer p oWder p r odu c ed by th e p r o
c es s de? ned in c l a im 1 .
9 . Th e s u p er a bs or bent p ol y mer p oWder of c l a im 8 h a v ing a
Retention of f r om 2 0 g / g to 3 6 g / g a c c or ding to th e Retention
Tes t Meth od a nd a ? u id u p ta ke u nder l oa d a t 0. 9 p s i ( A ULO. 9
p s i) of f r om 1 5 g / g to 40 g / g a c c or ding to th e F l u id Up ta ke
u nder 0. 9 p s i l oa d A UL Tes t Meth od.
1 0. A p r oc es s f or th e p r odu c tion of s u p er a bs or bent p ol y
mer p oWder With a r edu c ed c a king tendenc y c omp r is ing th e
s tep s of :
a ) p r ep a r ing a s u p er a bs or bent p ol y mer g el inc l u ding p ol y
mer iZ ing p ol y mer iz ed monomer s c onta ining a t l ea s t
p a r tia l l y neu tr a l iZ ed a c id g r ou p s a nd a t l ea s t one
c r os s l inker ;
b) dr y ing th e s u p er a bs or bent p ol y mer g el to f or m a dr ied
s u p er a bs or bent p ol y mer ;
c ) g r inding a nd s c r eening th e dr ied s u p er a bs or bent p ol y
mer to h a v e a p a r tic l e s iZ e in th e r a ng e f r om 1 5 0 to 85 0
m;
d) il r ea ting th e dr ied s u p er a bs or bent p ol y mer of s tep c ) With
a s u r f a c e c r os s -l inking a g ent to f or m a Wa ter - or a q u eou s
? u id-a bs or bing , dr ied, s u r f a c e-c r os s -l inked p ol y mer
p oWder , r ef er r ed to a s c omp onent I; a nd
e) s u r f a c e c oa ting th e Wa ter - or a q u eou s ? u id-a bs or bing ,
dr ied, s u r f a c e-c r os s -l inked p ol y mer p oWder of s tep d)
With a c oa ting a g ent s el ec ted f r om th e g r ou p c ons is ting
of nitr og en-c onta ining , non-ionic s u r f a c ta nt a nd op tion
a l l y a LeWis a c id; Wh er ein s a id s u r f a c ta nt h a s th e g ener a l
f or mu l a I:
2 0
2 5
3 0
3 5
40
45
5 0
5 5
2 2
R2
/
C N
u i \ R
O n 3
inWh ic h
R1 is a n a l ip h a tic C1 to C3 0 h y dr oc a r bon Z -s u bs titu ted a l i
p h a tic r es idu e,
R2 is s el ec ted f r om a h y dr og en, a n C2 to C2 4 a l ip h a tic
h y dr oc a r bon r es idu e, a nd
a h y dr ox y a l ky l ene r es idu e
R3 , Wh ic h ma y be identic a l or dif f er ent, h a s th e s a me
mea ning a s R2 , p r ov ided th a t With a mide c omp ou nds , a t
l ea s t one of r es idu es R2 or R3 r ep r es ents a h y dr ox y a l ky
l ene r es idu e or a n a l kox y l a ted h y dr ox y a l ky l ene r es idu e
or a c or r es p onding es ter i? ed or a l kox y l a ted or es ter i? ed
a nd a l kox y l a ted h y dr ox y a l ky l ene r es idu e With th e de?
nition g iv en f or R2 a bov e;
n is l ; a nd Z is a Wh ol e nu mber f r om 1 to 4; a nd
f ) h ea t tr ea ting th e s u r f a c e c oa ted Wa ter - or a q u eou s ? u id
a bs or bing , dr ied, s u r f a c e-c r os s -l inked p ol y mer p oWder
of s tep e) a t a temp er a tu r e of f r om 1 00 C. to 2 5 00 C. to
c a u s e s u r f a c e c oa ted Wa ter - or a q u eou s ? u id-a bs or bing ,
dr ied, s u r f a c e-c r os s -l inked p ol y mer p oWder to r ea c t
With th e s u r f a c ta nt a nd op tiona l l y , th e LeWis a c id to f or m
th e s u p er a bs or bent p ol y mer p oWder ;
Wh er ein th e s u p er a bs or bent p ol y mer p oWder p a s s es th e
A nti-c a king Tes t a s s et f or th h er ein.
1 1 . Th e p r oc es s a c c or ding to c l a im 1 0 Wh er ein s a id s u r f a c
ta nt is s el ec ted f r om s tea r y l a mine, eth ox y l a ted With 1 0 eth
y l ene ox ide ( EO) u nits , c oc onu t a c id dieth a nol a mide, l a u r ic
a c id dieth a nol a mide, c oc onu t a c id monoeth a nol a mide, l a u
r y l a mine, eth ox y l a ted With 1 0 E0 u nits , ol ey l a mine eth ox y
l a ted With 2 0 E0 u nits , ol eic a c id monoeth a nol a mide eth ox y
l a ted With 3 EO u nits , ol eic a c id monoeth a nol a mide,
eth ox y l a ted With 6 EO u nits , Ol eic a c id monoeth a nol a mide
eth ox y l a ted With 1 4 E0 u nits , or c oc onu t a c id monoeth a no
l a mide eth ox y l a ted With 4. 5 B0.
1 2 . Th e p r oc es s a c c or ding to c l a im 1 0 Wh er ein s a id c oa ting
a g ent f u r th er inc l u des a LeWis a c id s el ec ted f r om is s el ec ted
f r om a l u minu m s u l f a te, a l u minu m c h l or ide, Z inc a c eta te, Z inc
c h l or ide, Z inc s u l f a te, ir on c h l or ide, ma g nes iu m s u l f a te, ma g
nes iu m c h l or ide, s u l p h u r ic a c id, s u l p h u r -c onta ining a c ids ,
s el enic a c id, nitr ic a c id, p h os p h onic a c id or p h os p h or u s -c on
ta ining a c ids a c etic a c id, ox a l ic a c id, l a c tic a c id, c itr ic a c id,
ta r ta r ic a c id or h y dr a ted f or ms of a l u minu m s u l f a te, a l u mi
nu m c h l or ide, Z inc a c eta te, Z inc c h l or ide, Z inc s u l f a te, a nd
ir on c h l or ide.
1 3 . A s u p er a bs or bent p ol y mer p oWder p r odu c ed by th e
p r oc es s de? ned in c l a im 1 0.
1 4. Th e s u p er a bs or bent p ol y mer p oWder of c l a im 1 3 h a v
ing a Retention of f r om 2 0 g / g to 3 6 g / g a c c or ding to th e
Retention Tes t Meth od a nd a ? u id u p ta ke u nder l oa d a t 0. 9 p s i
( A ULO. 9 p s i) of f r om 1 5 g / g to 40 g / g a c c or ding to th e F l u id
Up ta ke u nder 0. 9 p s i l oa d A UL Tes t Meth od.
* * * * *
UN ITED S TA TES PA TEN T A N D TRA DEMA RK OF F ICE
CERTIF ICA TE OF CORRECTION
PA TEN T N O. I 8, 2 47, 640 B2 Pa g e 1 Of l
A PPLICA TION N O. : 1 2 / 71 861 7
DA TED : A u g u s t 2 1 , 2 01 2
IN VEN TOR( S ) : Ger d Jona s , Ric h a r d Mer tens a nd Ma r ku s F r a nk
It is c er tif ied th a t er r or a p p ea r s in th e a bov e-identi? ed p a tent a nd th a t s a id Letter s Pa tent is h er eby c or r ec ted a s s h own bel ow:
Col u mn 8,
Line 2 0, c omp onent Ito r ea c t s h ou l d r ea d -- c omp onent I to r ea c t --.
Line 2 5 , c a u s e c omp onent to r ea c t s h ou l d r ea d -- c a u s e c omp onent I to r ea c t --.
S ig ned a nd S ea l ed th is
S ix teenth Da y of Oc tober , 2 01 2
v
Da v id J. Ka p p os
Dir ec tor of th e United S ta tes Pa tent a nd Tr a dema r k O? ic e