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h p://dx.doi.o g/10.1080/00405000.2015.1029808
h p://hdl.handle.ne /10251/77509
Taylo & F ancis
Bone A acil, MA.; Bou Belda, E.; Monllo Pé ez, P.; Gisbe ; Jaime (2016). Binde
e ec i eness o mic ocapsules applied on o co on ab ics du ing laund y. The Jou nal o he
Tex ile Ins i u e. 107(3):300-306. doi:10.1080/00405000.2015.1029808.
BINDER EFFECTIVENESS OF MICROCAPSULES APPLIED ONTO COTTON
FABRICS DURING LAUNDRY
Mª ÁNGELES BONET*, EVA BOU, PABLO MONLLOR, JAIME GISBERT,
M. Bone 1*, E. Bou-Belda1, P.Monllo 1, J. Gisbe 2,
1 Uni e si a Poli ècnica de Valencia
Plaza Fe andiz y Ca bonell s/n
03801 Alcoy.Spain
2 INNOVATEC SC,S.L.
A enida de Elche nº 3
03801 Alcoy
Spain
* To whom co espondence should be sen : maboa @ xp.up .es
M. Angeles Bone A acil
AKNOWLEDGEMENTS
Au ho s g a e ully acknowledge he inancial suppo ecei ed by his esea ch p ojec
om he Spanish go e nmen in he p og amme “Plan Nacional 2008–2011” e e ence
Ma 2009-14210-C02-01.
BINDER EFFECTIVENESS OF MICROCAPSULES APPLIED ONTO COTTON
FABRICS DURING LAUNDRY
ABSTRACT
Mic ocapsules can be added o ab ic in indus ial p ocesses howe e , hey
ha e no been widely sp ead among indus ial companies. In his s udy we
sugges he possibili y o eloading mic ocapsules on o a ab ic while clo hs a e
washed. The e ec i eness o di e en esins when mic ocapsules a e applied in
washing machine du ing domes ic laund y p ocess has been s udied.
Mic ocapsules con aining la ende ag ance and melamine o maldehyde shell
whe e adhe ed o he ab ic by means o one ac ylic acid as a esin, o some
c osslinking agen s such as bu ane e aca boxylic acid (BTCA) o succinic acid
(SUC). In o de o e alua e hei beha iou some launde ing o i oning es s
we e conduc ed acco ding o in e na ional s anda ds (ISO). E e y sample om
he labo a o y was s udied wi h Scanning Elec on Mic oscopy (SEM) and wi h a
pa icle size coun e . As a esul we could obse e which was he mos sui able
auxilia y used o bond mic ocapsules o ab ic, and conclude abou he
condi ions ( empe a u e, concen a ion, e c.) in which we ob ained he op imal
esul s. I was demons a ed ha domes ic laund y is a sui able p ocess o
inco po a e mic ocapsules o ga men s.
KEYWORDS
Co on, Mic ocapsules, laund y, binde , SEM.
1. INTRODUCTION
Mic ocapsules p oduc s we e bo n wi h ca bonless copying pape (Zhang,
Saunde s & Thomas, 1999) and became conside ably impo an in he
pha maceu ical ield (S olnick, 1995). In o he a eas such as ex iles hey we e
i s ly conside ed some ime ago (Go don, 2001). The main ad an age o
mic ocapsules is ha new unc ions can be added and con e mo e p ope ies
such as cosme ic (Gisbe , Ibañez, Bone , Monllo , Díaz, Mon a a, 2009),
ag ances (Li, Lewis, S ewa , Qian, & Boy e , 2006; Nelson, 2001; Monllo ,
Bone , Cases, 2007; Monllo , Bone , Sánchez, Cases, 2009; Monllo ,
Capablanca, Bone , Gisbe , Díaz; Mon a a, 2010), phase change ma e ials
(Fan, Zhang, Wang, Li& Zhu, 2004; Hawlade , Uddin, Khin, 2003; Xiao_Zheng,
Zhi-Cheng, Guang-Long, Li-Xian & Tao 2003; Zhang e al, 2004, Ka hukeyan,
Ramachand an, & Shanmugasunda am, 2014) e c.
The mos ex ended mic ocapsules applied o ex iles a e based on non eac i e
shells. In o de o imp o e du abili y o washing o handle some auxilia y
p oduc s a e equi ed o join mic ocapsules on o he ib es su ace (Nelson,
2001); hey a e usually based on ac ylic, polyu e hanes, o silicone esins (Li e
al. 2008; Rod igues e al, 2009). Some s udies show how polyca boxylic acids
can be used in encapsula ion p ocess (Pascu, Ga cia-Valls, & Giambe ini,
2008) o as a binde o join mic ocapsules (Voncina, K e , Kokol, Chen, 2009;
Badulescu, Vi od, Jauso ec, Voncina, 2008; Ziming, Genquan, Wai-man, Huiyi,
2011) o nanopa icles o ab ics (Mon aze , Lessan, Moghadam, 2012; Wanga,
Chen, 2005).
To da e he mos indus ial me hods known o apply inishing ea men s o
ib es a e padding, ba h exhaus , coa ing o sp aying. The main cha ac e is ic o
ba h exhaus ion is ha i is use ul when chemical eac ion can be es ablished,
and as we ha e ema ked usually mic ocapsules´ shell show no eac i i y wi h
ib es. Some au ho s demons a ed ha ba h exhaus ion was no he mos
sui able p ocedu e o ha kind o p oduc s (Bone , Capablanca, Monllo , Diaz,
Mon a a, 2012). Howe e , mic ocapsules a e pa o he ecipe o some soaps
(EP 0 376 385 A2) o in some ca ionic so ene s (US 6,620,77 B2) wha mean
ha hose p oduc s can be applied o ab ics in laund y, which in ol es ba h
exhaus ion p ocedu e. Some o hem show a ecipe wi hou binde and some o
hem include mainly ac ylic esins (US 6,620,77 B2). Mo eo e , some pa en s
show a he mal ea men in an au oma ic d ye a a empe a u e be ween 38-
100º C a e a ea men in a p e-soaking/washing p ocess (USP 4,234,627).
I can be no iceable ha he e is no s udy abou he binde e ec i eness o he
in luence o i oning in c osslinking. The aim o his pape is o s udy he
e ec i eness o di e en esins when mic ocapsules a e applied in washing
machine while laund y. This wo k will s udy how many laund y cycles allow he
mic ocapsules o emain on he ab ic when hey had been pas ed on o he
ib es while clo hes we e washed. Apa om laund y beha iou , change in
colou will be e alua ed in o de o de e mine i he p ocedu e has seconda y
e ec s such as yellowing.
2. MATERIALS AND METHODS

2.1. Ma e ials
Mic ocapsules (CENTER FINISH 164/02 LAVANDA) we e supplied by COLOR
CENTER (Ta asa, Spain). The wall ma e ial was melamine o maldehyde, and
he mic ocapsules con ained la ende ag ance. No u he in o ma ion was
supplied by he p o ide . In o de o bond he mic ocapsules o he ab ic, an
ac ylic esin was applied, also supplied by Colo Cen e and wo polyca boxylic
acids, bu ane e aca boxylic acid (BTCA) om Al a Aesa and Succinic acid
(SUC) om Pan eac. Polyca boxylic acids ecqui e he p esence o a ca alys . I
was sodium hypophosphi e monohid a e (SHP) which was supplied om Al a
Aesa .
The ab ic used was a 100% co on will ab ic wi h 210 g/m2, which had
been chemically bleached wi h pe oxide in an indus ial p ocess.
2.2. Adhe ing mic ocapsules on o ab ics.
The equipmen used o apply mic ocapsules was a domes ic washing machine.
I s capaci y was 5 Kg and i s maximum olume o wa e was 11 L.
Mic ocapsules dispe sion was p epa ed in a glass essel. Fou es s we e
conduc ed. One es was comp ised o no binde . The es con ained BTCA,
SUC, o ac ylic esin. The supplie sugges ed concen a ions o use. Di e en
samples we e p epa ed depending on he binde na u e. All he samples
con ained 5% ow (o e weigh o ib e) o mic ocapsules. One o he ba hs was
comp ised o mic ocapsules wi hou any binde . The ecipes o samples wi h
polyca boxylic acids (BTCA and SUC) as binde we e o mula ed wi h 5% ow o
mic ocapsules 4% ow o binde and 2% ow o ca alys . The es wi h ac ylic
binde (RES) was based on 5% ow o mic ocapsules and 12,5 % ow o binde .
As soon as he washing machine inished, he ab ics we e d ied in an IR d ye
a 100º C un il he ab ic was comple ely d y. La ely, ab ics should be he mally
ea ed so as o polyme ize he binde . Comme cial b ands sugges di e en
empe a u es bu in his s udy he cu ing empe a u e has been selec ed in
o de o ge he minimum yellowness on he co on ib e and di e en cu ing
empe a u es ha e been e alua ed.
Table 1 summa ises he ea men condi ions he ein s udied.
Inse able 1 abou he e
2.3. Scanning Elec on Mic oscopy (SEM).
Fo su ace obse a ion, a scanning elec on mic oscope (SEM) Phenom
mic oscope (FEI Company) was used. Each sample was ixed on a s anda d
sample holde and spu e coa ed wi h a gold –pla inum mix u e. Samples we e
hen examined wi h sui able accele a ing ol age and magni ica ion.
2.4. Mic ocapsules pe manence.
To es he e ec i eness o he binde s some launde ing es s we e conduc ed.
The specimens we e ea ed on a sho ime p og am in a He aeus Lini es o
45 min a 30 °C, in acco dance wi h ISO S anda d 105 C01. Jus inishing one
cycle, samples we e d ied on a ho izon al su ace a oom empe a u e. All
samples we e examined a e 1, 2, 3, 4 and 5 cycles.
2.5. Coun ing mic ocapsules.
The pa icle size dis ibu ion o he mic ocapsules was measu ed by a Coul e ®
Coun e appa a us (Mul isize Z2, Coul e Elec onics, No hwell, UK). The
pa icle size was exp essed as he equi alen olume diame e and wo
eplica es we e pe o med o each ba ch o mic ocapsule, o educe e o an
a e age cu e was calcula ed and analysed.
This me hod was used o measu e he mic ocapsules dispe sion jus
immedia ely i was p epa ed and he was ewa e om he washing machine.
The numbe o mic ocapsules emaining on he ab ic was calcula ed as he
di e ence be ween he numbe o mic ocapsules on he p epa ed ba h and he
numbe o mic ocapsules in was ewa e .
Fu he mo e, he was ewa e om ISO laund y was also measu ed o obse e
he mic ocapsules beha iou in each laund y cycle.
2.6.- I oning samples.
Some samples we e i oned a di e en empe a u es (110, 150 and 200º C).
The i oning p ocedu e was pe o med as UNE EN ISO 105 X11 s anda d
indica ed.
3. RESULTS
3.1.- Cu ing empe a u e.
Polyca boxylic acids should be cu ed a empe a u es om 150º C in o de o
induce c osslinking. Knowing ha he mal ea men on cellulosic ib es is
esponsible o yellowness, di e en cu ing empe a u es ha e been e alua ed.
Figu e 1 shows he whi eness index depending on he binde used and he
empe a u e o ea men . I could be p edic able ough, he whi e colou on
co on ib es dec eases as he empe a u e inc eases, and i can be app ecia ed
ha when empe a u e is highe han 160º C co on ib e whi eness
conside ably dec eases. When ab ics a e ea ed wi h binde s he whi eness
index, a lowe empe a u es han 140º C, is app oxima ely he same han he
ab ic wi hou ea men . As a esul 150º C has been conside ed a good
empe a u e o cu ing polyca boxylic acids.
I is conside ably no iceable ha when empe a u e is lowe ha 160ºC,
samples ea ed wi h ac ylic binde show he lowes alues o whi eness index.
Howe e , a abou 160º C he whi eness index is app oxima ely he same o
e e y ab ic which had been ea ed wi h a binde , and sligh ly lowe han he
index o co on wi hou ea men .
When ac ylic esin is compa ed wi h polyca boxylic acids and conside ing
he mal condi ions o each one, he e idence shows ha he la e allow
mic ocapsules o emain on he ab ic he longe . Appa en ly, succinic acid
displays he highe numbe o mic ocapsules on he ib e. Fu he mo e, ac ylic
binde de elops some agg ega es o mic ocapsules and makes impossible o
es he binde app op ia ely.
To sum up, when applying mic ocapsules o ab ics by washing machine,
succinic acid i cu ed a 150º C shows he bes esul s and ea ed ab ic has
no changed sensi i ely he colou . I oning a 150ºC is e ec i e in he cu ing
p ocess and in he app op ia e binding o mic ocapsules in ab ics. This a icle
demons a es he possibili y o applying mic ocapsules o ab ics in a domes ic
p ocess using succinic acid in a con en ional washing p ocedu e and i oning
wi h domes ic equipmen .
AKNOWLEDGEMENTS
On i le page in o de o a id p o iding au ho s in o ma ion.

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FIGURE CAPTIONS
Figu e 1.- Whi eness index depending on cu ing empe a u e
Figu e 2.- Mic ocapsules applied on ab ics by washing machine p ocess wi h BTCA binde ,
cu ed a 150º C and wi hou any laund y.
Figu e 3.- Fab ics ea ed by ISO 105 C10 a e 5 washing cycles. a) 25M; b) RES; c) BTCA; d)
BTCA-150; d) SUC; e) SUC-150.
Figu e 4.- Mic ocapsules p esence on he ab ics (mics/m2) a e di e en laund y cycles.
Figu e 5.- Fab ics ea ed by i oning and washed once.

FIGURES
Figu e 1.- Whi eness index depending on cu ing empe a u e
40
45
50
55
60
65
70
75
80
85
140 150 160 170 180 190 200
Whi eness Index (CIE)
Cu ing Tempe a u e (ºC)
Co on
RES
SUC
BTCA
Figu e 2.- Mic ocapsules applied on ab ics by washing machine p ocess wi h BTCA binde ,
cu ed a 150º C and wi hou any laund y.
a) 25 M b) RES
c) BTCA d) BTCA-150
e) SUC ) SUC-150
Figu e 3.- Fab ics ea ed by ISO 105 C10 a e 5 cycles. a) 25M; b) RES; c) BTCA; d) BTCA-
150; e) SUC; ) SUC-150.
Figu e 4.- Mic ocapsules p esence on he ab ics (mics/m2) a e di e en laund y cycles.
0,00E+00
5,00E+09
1,00E+10
1,50E+10
2,00E+10
2,50E+10
3,00E+10
1 2 3 4 5
Mic/m2
La ados
25M
RES
SUC
SUC-150