Film blowing o PHB-based sys ems o home compos able ood packaging
P.F. Teixei a1, J.A. Co as1, M.J. Sua ez2, I. Angulo2, L. Hilliou1
1Ins i u e o Polyme s and Composi es, Uni e si y o Minho, Guima ães, Po ugal.
2GAIKER Technology Cen e, Basque Resea ch and Technology Alliance (BRTA),
Zamudio, Spain.
*[email p o ec ed]; Tel: +351 253510320.
Bibliog aphy
DOI 10.3139/217.3985
In e n. Polyme P ocessing
XXXV (2020) 5; page 440–447
ª Ca l Hanse Ve lag GmbH & Co. KG
ISSN 0930-777X
This manusc ip is submi ed o inclusion in he special issue hono ing Pie e
Ca eau
Abs ac .
One o he ou es o minimize he en i onmen al impac o plas ics was e is he use o
bio-sou ced and biodeg adable al e na i es, pa icula ly o packaging applica ions.
Al hough Polyhyd oxyalkanoa es (PHA) a e a ac i e candida es o ood packaging,
hey ha e poo p ocessabili y, pa icula ly o ex usion ilm blowing. Thus, one
ela i ely success ul al e na i e has been blending PHA wi h a biodeg adable polyme .
This wo k p oposes ilm blowing o a co-ex uded Poly(hyd oxybu y a e) (PHB) laye
wi h a poly bu ylene adipa e‐co‐ e eph ala e (PBAT) laye o enhance bubble s abili y,
mechanical and ba ie p ope ies. Co-ex usion is de ailed, oge he wi h he di e en
s a egies ollowed o imp o e adhesion be ween ilm laye s and he PHB con en in he
ilms. Films wi h hicknesses below 50 mic on and elonga ion a b eak beyond 500%
we e consis en ly p oduced.
Keywo ds: ilm blowing, co-ex usion, polyhyd ybu y a e, biodeg adable packaging.
1. In oduc ion
App oxima ely 37% o ood packaging a e made o plas ics (Halonen e al., 2020), which
demons a es he posi i e con ibu ion o hese ma e ials o ood sa e y and consume s
wellbeing. Simul aneously, ood packages ep esen a signi ican sha e o plas ics was e.
Fo ins ance, 40% o he Eu opean plas ics p oduc ion is dedica ed o packaging
applica ions (Plas icsEu ope, 2019). The esul ing en i onmen al impac igge ed
esea ch and inno a ion e o s o he de elopmen o bio-sou ced and biodeg adable
al e na i es. Repo s on new bio-based and biodeg adable ilm packaging a e abundan
(Rhim e al. 2013; Mu hu aj e al., 2018; Ka an e al., 2019; Sca a o e al., 2019; Na ancic
e al., 2020; Sha ma e al. 2020), bu ew ilms ac ually made hei way up o he ma ke
(Peelman e al., 2013; Niaounakis 2015).
Among he bio-based and biodeg adable polyme s a ailable, polyhyd oxyalkanoa es
(PHA) a e a ac i e candida es o ood packaging (Bugnicou e al., 2014), since
deg ada ion o hese mic obial polyes e s does no equi e indus ial compos ing
acili ies. Howe e , his bene i is o se by poo p ocessabili y and mechanical esis ance
o hin ilms. Poly(hyd oxybu y a e) (PHB) is epo ed o be inapp op ia e o ilm
blowing (Haängi U. J., 2013; Niaounakis, 2015). Film blowing o a comme cial
polyhyd oxy(bu y a e-co- ale a e) (PHBV) was a emp ed (Cunha e al., 2015), bu he
p ocess was uns able and 100 mic on hick ilms showed poo ea esis ance.
Mel blending PHA wi h o he biodeg adable polyme s and mel compounding wi h
addi i es ha e been a emp ed o imp o e ilm-blowing pe o mance. Film blowing o
PHB/polyy(lac ic acid) (PLA) blends using maleic anhyd ide as eac i e compa ibilize
was accomplished, bu he ilms con ained 40% o less o PHB (Jandas e al., 2013).
Using a comme cial PHBV/poly bu ylene adipa e‐co‐ e eph ala e (PBAT) blend yielded
35 mic on hick ilms wi h 30 w .% PHBV con en (Russo e al., 2013). PHBV mel
compounded wi h 70 w .% o an expe imen al Ma e -Bi® compound was p ocessed in o
blown ilms wi h hickness anging om 80 o 100 mic on, bu he bubbles we e ela i ely
uns able (Cunha e al., 2016). Rela i ely hick ilms (be ween 180 and 230 mic ons) we e
p oduced using a he moplas ic s a ch/poly(3-hyd oxybu y a e-co-4-hyd oxybu y a e)
blend con aining 36 w .% o he la e (Sun e al., 2017).
Co-ex usion is an al e na i e ou e o con e biodeg adable plas ics in o ilms o ood
packaging (Sca a o e al., 2018). A epo ed comme cial applica ion o PHBV o ood
packaging is an 87 mic on hick mul ilaye ed ilm wi h PBAT (Peelman e al., 2013).
Film blowing o a co-ex uded PHA laye wi h a PBAT o biodeg adable composi e laye
displayed enhanced bubble s abili y when compa ed o ilm blowing o he co esponding
blends (Cunha e al., 2016). Howe e , ilms con aining mo e han 50% PHBV could no
be p oduced, and delamina ion be ween he wo laye s occu ed a s ains as low as 10 %.
Based upon p e ious esul s (Cunha e al., 2016), he p esen s udy explo es co-ex usion
ilm blowing o p oduce bi-laye ed PHB/PBAT ilms o ood packaging applica ions.
The esea ch was ca ied ou wi hin he amewo k o EU unded YPACK p ojec (High
pe o mance polyhyd oxyalkanoa es based packaging o minimise ood was e). The main
objec i es a e o maximize he PHB con en in he bi-laye ed ilms and o enhance
adhesion be ween laye s. The i s objec i e in ol es op imiza ion o p ocessing
pa ame e s. The second objec i e is pu sued h ough wo ou es: he addi ion a -line o a
eac i e c osslinking agen o PHB, and he co-ex usion o a compa ibilized PHB/PBAT
blend con aining 10 w .% PBAT wi h PBAT. Dicumyl pe oxide (DCP) was chosen as
c osslinke , since i has long been es ablished ha i s eac i e ex usion wi h PHBV
p omo es chain b anching (D’Haene e al., 1999), which is a c i ical chain con o ma ional
a ibu e o enhancing ilm blowing o bio-based polyme s such as PLA (Nou i e al.,
2015).
2. Expe imen al
2.1. Ma e ials and compounding
An expe imen al PHB g ade (Biome ® P309) was supplied by BIOMER (K ailling,
Ge many). The ba ch was exp essly p oduced o he YPACK p ojec , being essen ially
designed o injec ion molding and being p ocessed a a maximum empe a u e o 185
ºC. This g ade has a mel low index (MFI) o 10 g/10 min a 180 ºC o a load o 2.16
kgs. A ilm blowing g ade o PBAT (Eco lex® F blend C1200) was pu chased om
BASF (Ludwigsha en am Rhein, Ge many). This g ade has a MFI o 2.7-4.5 g/10 min a
190 ºC o a load o 2.16 kgs. BASF kindly o e ed a mul i unc ional epoxide s y ene-
ac ylic oligome ic chain ex ende (CE). This amily o chain ex ende s has been
ex ensi ely used o modi y PLA o PBAT, o o compa ibilize hei blends, o imp o ing
ex usion ilm blowing (Al-I y, 2015; A uda e al., 2015; Li e al., 2018; Malle e al.
2014; Schneide e al., 2016). Dicumyl pe oxide (DCP) was pu chased om Sigma-
Ald ich (CAS Numbe 80-43-3). All ma e ials we e d ied o e nigh a 60 °C be o e
p ocessing.
PHB modi ica ion wi h DCP was pe o med in an in e meshing co- o a ing win sc ew
ex ude Collin ZK 25. P emixes o PHB and DCP ed he ex ude a a a e o 3.5 kg/h.
The empe a u e p o ile was se o 180 ºC / 180 ºC / 170 ºC / 170 ºC /170 ºC / 160 ºC /
160 ºC om hoppe o die, and he sc ews o a ed a 100 pm. P emixes o PHB (90
w .%), PBAT (10 w .%) and CE we e p epa ed in he same ex ude , wi h iden ical
p ocessing pa ame e s.

2.2. Rheological cha ac e iza ion
Ma e ials and compounds we e cha ac e ized using an ARG2 o a ional heome e (TA
ins umen s), equipped wi h a pa allel-pla e geome y (25 mm diame e ). In o de o a oid
addi ional he mal deg ada ion associa ed wi h comp ession molding o p oduce ci cula
discs, pelle s (d ied o e nigh a 60 °C be o ehand) we e di ec ly loaded in he shea ing
geome y p e-hea ed o 180 ºC. The same amoun o ma e ial was used o all
measu emen s. A ci cula me allic ing main ained he pelle s on he bo om pla e and
allowed ma e ial compac ion du ing gap se ing. A e eaching he equi ed gap (0.9
mm), he ing was emo ed and he excess o ma e ial immed. Time was gi en o
he mal equilib ium and o elaxa ion o he sample no mal o ce. Mechanical spec a
we e de e mined wi h small ampli ude oscilla o y (sinusoidal) shea equency sweeps
om 100 Hz o 0.1 Hz, a 180ºC unde a cons an s ain ampli ude o 5 % (wi hin he
linea iscoelas ici y egimen, as e idenced om he sinusoidal s ess esponses). To
assess he he mal s abili y o he samples, ime sweep measu emen s we e pe o med
(wi h esh samples) a 1 Hz and 180 ºC, du ing app oxima ely 6 min, again wi h a
sinusoidal de o ma ion o 5%. S eady iscosi y low cu es we e measu ed a 180 ºC wi h
esh samples, by loga i hmically amping he s eady shea a e om 0.1 s-1 o 20 s-1, and
allowing a maximum o 30 seconds a each shea a e s ep o ead he iscosi y alue.
2.3. Film blowing
Films we e p oduced using a labo a o ial p o o ype ex usion blown- ilm line (Pe iplas ,
Po ugal) de ailed a leng h elsewhe e (Ca nei o e al., 2008). The equipmen was
con igu ed o con en ional ex usion ilm blowing (i can also make biaxially o ien ed
ilm), wi h one o wo ex ude s and ex usion/co-ex usion dies, o he p oduc ion o
mono-laye ed o bi-laye ed ilms, espec i ely. The se empe a u e p o ile o ex ude
A (3 hea ing zones) was 180 ºC / 160 ºC / 155 ºC om hoppe o sc ew ip, and o
ex ude B (4 zones) was 180 ºC / 160 ºC / 155 ºC / 170 ºC. Ex ude A was ed wi h
PHB, PHB/DCP and PHB/PBAT blends o p oduce he in e nal laye o bi-laye ed ilms,
as well as monolaye ilm o modi ied PHB. Ex ude B was ed wi h PBAT o c ea e he
ex e nal laye o bi-laye ed ilms and he co esponding PBAT monolaye . The
ex usion/co-ex usion head (wi h a die lip gap o 0.5 mm) was kep a 175 ºC / 165 ºC /
160 ºC om ex ude ou le o die exi , excep o he modi ied PHB monolaye (175 ºC
/ 170 ºC / 160 ºC). Ex e nal bubble cooling condi ions we e main ained cons an , whe eas
ope a ing condi ions we e a ied in o de o gene a e a ange o blow up (BUR) and ake
up (TUR) a ios. Table 1 iden i ies and p esen s da a o he 10 ilms p oduced. When
pe o ming ex usion ials aiming a maximizing he PHB con en in he ilms while
minimizing hei hicknesses ( ilms 1 o 5), he sc ew speeds whe e adjus ed and TUR
and BUR we e also maximized. The ilm blowing pa ame e s used o p oduce ilm 1 we e
employed o es he modi ied PHB ( ilm 6) and he PHB/PBAT blend ( ilms 7 and 8) as
adhesi e second laye . An ex usion un wi h PHB/PBAT blend aimed a maximizing he
PHB con en by inc easing he sc ew speed o he co esponding ex ude .
Table 1: Films p oduced in he ex usion ials.
Film label
In e nal laye
Ex e nal laye
BUR
TUR
Ex ude A
( pm)
Ex ude B
( pm)
PHB
PHB+DCP
-
1.9
6.4
30
-
PBAT
-
PBAT
2.2
12.1
-
20
Maximizing PHB con en and ilm hickness
1
PHB
PBAT
1.8
10.1
15
15
2
PHB
PBAT
2.0
9.2
15
15
3
PHB
PBAT
2.1
9.0
20
20
4
PHB
PBAT
1.9
13.9
18
15
5
PHB
PBAT
2.1
12.5
20
15
Op imizing adhesion be ween laye s
6
PHB+DCP
PBAT
1.9
10.1
15
15
7
PHB+PBAT+CE
PBAT
1.9
7.9
15
15
8
PHB+PBAT+CE
PBAT
2.0
7.1
30
15
2.3. Films cha ac e iza ion
The a e age lay la wid h o he ilms was measu ed a 30 cm leng hwise s eps o e a
o al leng h o 6 m. A he same leng hwise in e als, ilms hicknesses we e measu ed a
5 cm s eps along he ans e se di ec ion (TD).
The PHB olume ic con en was assessed om scanning elec on mic oscopy (SEM)
obse a ions o he su ace no mal o he ex usion di ec ion, pe o med wi h a NanoSEM
- FEI No a 200 using an accele a ion ol age o 15kV. P io o SEM examina ion, he
bilaye ed ilms we e ac u ed in liquid ni ogen. The ac u ed su ace was spu e ed
(Scancoa Six Edwa ds, C awley, UK), wi h a hin laye o gold unde a gon a mosphe e,
o a oid elec os a ic cha ging unde he elec on beam.
The ensile p ope ies o he ilms we e de e mined bo h in he machine (MD) and
ans e se (TD) di ec ions using a Zwick/Rowell Z005 (Ulm, Ge many) uni e sal es ing
machine, ollowing he ASTM S anda d Me hod D 882-02, wi h a 5 KN load cell, a s ain
a e o 50 mm/min and a gauge leng h o 50 mm. Rec angula es specimens (80 mm ×
10 mm) we e cu om ilms p e iously s o ed o 24 hou s a oom empe a u e
(app oxima ely 22 °C) and 60% ela i e humidi y. Each specimen hickness was
measu ed a 5 poin s. The mechanical p ope ies o welded ilms join s we e e alua ed
ollowing he same p o ocol. Welding o PHB on PHB and o PHB on PBAT we e
pe o med wi h an Impulse Hea Seale F-200 o sealing plas ic bags. The seale sends
an elec ic impulse o hea he wi e o 0.2 - 1.5 seconds. Fo welding he ilms, wo
consecu i e impulses o 1.5 s we e de ined. Films ea esis ance we e measu ed by d op
weigh impac es s acco ding o ASTM D2582-03, using a ROSAND IFW IT 5 impac
es ing machine, equipped wi h a da weighing 113.5 g, d opped om a heigh o 74 cm.
Fo he bi-laye ed ilms, es s we e pe o med wi h he PHB and PBAT side acing he
load.
Op ical p ope ies we e de e mined wi h a XL-211 Hazega d sys em, ollowing ASTM
D1003-61. This es me hod co e s he e alua ion o speci ic ligh - ansmi ing and wide-
angle-ligh -sca e ing p ope ies o plana sec ions o ilms.
Compa a i e wa e apo ansmission a e (WVTR) h ough he a ious ilms was
measu ed acco ding o ASTM E398:03, using a Pe ma an W398 appa a us. Tes s we e
ca ied ou in duplica es a 30 ºC and 90% ela i e humidi y, wi h ilm samples o 5 cm2,
a a p essu e o 760 mm Hg. Fo bi-laye ed ilms, PBAT side was acing he ni ogen
lushing chambe .
3. Resul s and Discussion
All bi-laye ed ilms in Figu e 6 show supe io elonga ion a b eak along he machine
di ec ion han ilms documen ed in he li e a u e and blown om non-compa ibilized
blends con aining up o 40% PHA (Jandas e al., 2013; Sun e al., 2017). Howe e , ilms
6 o 8 do no ma ch he 500% elonga ion a b eak epo ed o a compa ibilized blend o
PHB wi h 70 w .% PLA (Jandas e al., 2013).
Figu e 7 shows he ea esis ance measu ed on bo h sides o he ilms, no malized by he
ilm hickness. As expec ed om he ensile es ing esul s, ilms wi h op imized adhesion
be ween laye s show be e balanced ea esis ance. Con e sely, using DCP is ine icien
in imp o ing his p ope y, since he co esponding ilm ( ilm 6) p esen s he weakes ea
esis ance.
Figu e 7. No malized ea esis ance o he ilms s udied.
All ilms exhibi sa is ac o y welding pe o mance, as demons a ed in Figu e 8, which
po ays he mechanical esis ance o join s made by welding PHB laye s on PBAT laye s.
Welding p ope ies a e impo an in ood packages, bu only ew s udies wi h bio based
and/o biodeg adable polyme s a e a ailable in he li e a u e (Tabasi and Ajji, 2017).

Mos esis an weld was achie ed wi h bi-laye ed ilm 8. This esul is gene ally
consis en wi h he bes ea esis ance and he absence o delamina ion du ing mechanical
es ing.
Figu e 8. Maximum s ess M (a) and s ain a b eak B (b) o welded ilms. Welding o
PHB laye s on PBAT laye s was pe o med be o e he ensile es ing o he esul ing
join s.
The op ical p ope ies (in e ms o haze) o all ilms a e p esen ed in Figu e 9, oge he
wi h he espec i e PHB con en s and hicknesses, and pic u es epo ing he isual
aspec s o a PHB ilm and ilm 8. Films 7 and 8 a e bo h as hick as ilms 4 and 5, bu
exhibi much less haze. Ra he , he ela i e hickness o he PHB laye seems also o
impac on he ligh sca e ing p ope ies o ilms. O e all, ilms 7 and 8 a e as hazy as he
PBAT ilm a compa able hicknesses.
Figu e 9. Haze o he ilms p oduced, oge he wi h hei hickness (emp y symbols) and
PHB con en (solid symbols). The pic u e on op igh shows a modi ied PHB ilm ( op),
he PBAT side o ilm 8 (middle) and he PHB side o ilm 8 (bo om), whe eas he pic u e
on he lowe igh shows a bag o ilm 8.
The pe meabili y o he ilms o wa e apo is displayed in Figu e 10. Co-ex uding a
laye o PHB imp o es he wa e apo ba ie p ope ies o ilms. WVTR da a o ilms
4 and 5 indica e ha pe meabili y is no simply ela ed o ilm hickness. The inse in
Figu e 10, a emp s o shed some ligh on he ole o PHB con en on he ilms ba ie
p ope ies. Clea ly, wi h he excep ion o one ou lie ( ilm 4), WVTR co ela es well wi h
he hickness o he PHB laye in he ilm. These esul s a e in ag eemen wi h p e ious
expec a ions ha biodeg adable plas ics ha e poo ba ie p ope ies, PHB being he
excep ion (Jos 2018). The e o e, Figu e 10 unde lines he bene i s o using PHB and co-
ex usion o imp o e he WVTR o PBAT, a esul ha is no achie ed by blending
(Cunha e al. 2015; Jos 2018).
Figu e 10. Wa e apo ansmission a es (WVTR) o blown ilms om PHB, PBAT and
co-ex uded PBAT and PHB. Inse : PHB hickness in bi-laye ed ilms plo ed as a
unc ion o he wa e apo ansmission a es o co esponding ilms.
4. Conclusions
Polyhyd oxyalkanoa es (PHA) in gene al and Poly(hyd oxybu y a e) (PHB) in pa icula
a e a ac i e candida es o ood packaging applica ions, no only because hey a e
sui able o home compos ing, bu also due o he ac ha hey can be ob ained om aw
bio-based ood indus y by-p oduc s. Howe e , poo p ocessabili y and ilm pe o mance
mo i a ed hei ela i e success ul usage as blends wi h o he biodeg adable polyme s.
This wo k explo ed co-ex usion ilm blowing o bi-laye ed ilms con aining a laye ich
in PHB and ano he ich in PBAT. 40 mic on hick ilms con aining a leas 50% PHB
we e consis en ly p oduced. The ilms showed no delamina ion, sa is ac o y mechanical
p ope ies, as well as low pe meabili y o wa e apo . Mo eo e , good welding be ween
PBAT and PHB was obse ed. The p ocess can be eadily scaled-up o indus ial
p oduc ion.
5. Acknowledgemen s
This p ojec has ecei ed unding om he Eu opean Union’s Ho izon 2020 esea ch and
inno a ion p og amme unde g an ag eemen No. 774088. LH also acknowledges
unding om he Po uguese Founda ion o Science and Technology In es iga o
P og amme h ough g an IF/00606/2014.
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