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New characterized material from biomasses [GRIP - D2.4.2]

Author: Università degli Studi del Piemonte Orientale "Amedeo Avogadro"
Publisher: Zenodo
DOI: 10.5281/zenodo.17276817
Source: https://zenodo.org/records/17276817/files/NODES_GRIP_RM2_D2.4.2_def.pdf
NODES – No d O es Digi ale e Sos enibile
FLAGSHIP PROJECT GRIP
SPOKE 2 –GREEN TECHNOLOGIES AND SUSTAINABLE INDUSTRIES
DELIVERABLE D2.4.2 “New cha ac e ized ma e ial om biomasses”
REPORTING PERIOD
Pe iod co e ed:
om M8 o M 28
Pe iodic epo da e and e sion:
30/09/2025
Deli e able # Responsible
Boccale i-Lau en i-Binda
RM2 Responsible
A lo io
This epo is pa o he p ojec NODES which has ecei ed unding om he MUR – M4C2
1.5 o PNRR unded by he Eu opean Union - Nex Gene a ionEU (G an ag eemen no.
ECS00000036)
1
Lis o Deli e ables
D. No
Name
Type
Dissemina i
on Le el
Due Da e
Deli e y Da e
(ac ual)
[numbe ]
[name]
[R — Documen ,
epo ] [DEM —
Demons a o , pilo ,
p o o ype]
[DEC — Websi es,
pa en filings,
ideos, e c]
[DATA — da a se s,
mic oda a, e c]
[DMP — Da a
Managemen Plan]
[ETHICS] [SECURITY]
[OTHER]
[PU — Public]
[SEN —
Sensi i e]
[R]
[C]
[S]
[mon h
numbe ]
[dd/mm/yyyy]
D2.1
Da a abou chemical and
nu i ional p ofiling o aw
was es and by p oduc s
R
PU
M14
18/04/2024
D2.2.1
On line lab-scale echnical
mul i-de ice o was e
p ocessing*
O he
(ma e ial)
PU
M18
25/10/2024
D2.2.2
Deli e y o p o ocols
(lab-scale) eady o scale-up
he p oduc ion o new
high- alue ma e ial (in
collabo a ion wi h
Companies)
R
PU
M22
16/02/2025
D2.3.1
New da a abou alo ized
ma ices cha ac e iza ion
and high alue p oduc s
R
PU
M28
30/09/2025
D2.3.2
New cha ac e ized
ing edien s/ma e ials o
ood, nu aceu icals, pha ma
and cosme ic applica ions
O he (ma e ial)
PU
M30
30/09/2025
D2.4.1
New da a abou sus ainable
p oduc ion o new ma e ials
om biomasses
R
PU
M24
D2.4.2
New cha ac e ized ma e ials
om biomasses
O he (ma e ial)
PU
M30
30/09/2025
D2.5.2
Po ous so ben s om
biomasses alo iza ion
O he (ma e ial)
PU
M30
29/09/2025
D2.6.1
New ma e ial p oduced a
pilo scale eady o he
o mula ion o co- o mula ion
(in collabo a ion wi h
Companies)
O he (ma e ial)
PU
M32
D2.6.2
New well cha ac e ized
p ocess and o mula ed
pilo -p oduc s (in
collabo a ion wi h
Companies)
R/O he (Ma e ial)
PU
M32
2
D2.7
Repo on he adso p ion
and/o ca aly ic
pe o mances o po ous solids
de i ed om biomasses
alo iza ion and
non- ecyclable plas ic was es
R
PU
M32
29/09/2025
3
A) INTRODUCTION
The wo k and he ou comes epo ed in his Deli e able a e ela ed o he ac i i y
scheduled in Task 2.2 ( ocusing on Sub-Task 2.2.3 and Sub-Task 2.2.4). The main goal was
he p epa a ion and he cha ac e iza ion o he plan / ecalci an biomasses use ul o
p oduce new ma e ial eady o be used in cemen /biopolyme s/polyme composi e
p oduc ion/fine chemicals, as well as new high- alue chemicals (biosu ac an s).
B) ROLE OF PARTNERS
The ole o he Pa ne s in ol ed in his ac i i y (Disi -UPO, UNIPV, UNITO) was o apply
he bes pe o ming me hods o up-cycle he aw biomasses ( om di e en o igin,
animal and plan -de i ed ma e ials), in o de o ob ain hei comple e cha ac e iza ion,
as well as some da a abou he high- alue molecules/ma e ials eco e ed.
C) EXPLANATION OF THE WORK CARRIED OUT AND OVERVIEW OF THE PROGRESS
Following we epo he cha ac e iza ion o he main ma e ials om biomasses ( ice
husk; soy; cow milk whey and Elodea nu alii, used cooked oil).
The cha ac e iza ion o u he ma ices (e.g. cocoa bean husks) we e p o ided in o he
Deli e ables.
Disi -UPO
Rice husk has been cha ac e ized o unde s and he in insic ea u es and design he
ea men op imiza ion. Pa icula ca e was de o ed o he e alua ion o he ino ganic
con en , as he high silica amoun o he d ied ice husk basically limi s i s con e sion.
Such amoun , despi e ela ed o he ype o ice and i s geog aphical o igin,
de e mined a e calcina ion, is abou 20% w . o which abou 85% is composed by
amo phous silica. Rice husk was p o ide an indus ial sample p o ided by a ice
p oduc ion plan si ed in Mo ano Po (VC).
I s cha ac e iza ion equi ed XRPD, TGA, XRF and SS-NMR; his cha ac e iza ion
p o ocol allowed o unde s and i s composi ion and alida e he mos e ficien s a egy
o chemicals and ma e ials eco e y. Rice husk was calcined o ob ain he ino ganic
4
ac ion, on which he elemen al composi ion was e alua ed by XRF using he glass
disk ob ained a e bo a e flux usion me hod. The elemen s, epo ed as oxides, and
he ela i e pe cen ages in weigh a e epo ed in he able.
The composi ion is ypical o a na u al-based ma ix, i.e. he p esence o he soil
elemen s (K, P, Mn, Mg..).
Oxide
Weigh
Pe cen age
SiO2
85,64
K2O
4,14
CaO
4,05
SO3
1,40
P2O5
1,02
Fe2O3
0,96
Cl
0,84
Al2O3
0,74
MnO
0,59
MgO
0,37
Na2O
0,08
TiO2
0,06
Table 1: Elemen al composi ion by XFR on calcined Rice husk
The XRPD o he esidue o he ino ganic ac ion (Figu e 1 – igh ) highligh s he
p esence o c is obali e phase (a polymo ph o qua z) esul ing om he densifica ion
o he silica ac ion du ing he he mal ea men .
5

Fig. 1
On he con a y, he XRPD pa e n o ice husk (Figu e 1 XRPD - le ) does no show
signals ela ed o Si oxides o in gene al o i s ino ganic con en , while se e al b oad
peaks and some sha p signals a e due o he p esence o cellulose, cha ac e ized by a
c ys alline s uc u e. The amo phous halos o hemicellulose, lignin and silica can be
seen a he lowe angles. The inse s in he XRPD figu e a e he images o ice husk, aw
and a e calcina ion.
Figu e 2: 29Si and 13C-MAS-NMR spec a
Based on he high silica con en , he 29Si SS-NMR was collec ed o define he silicon
coo dina ion (see figu e NMR op). Silicon is in high polyme iza ion s a e because,
6
acco ding o he chemical shi , Q3 (3 bonds Si-O-Si and 1 OH) and Q4 (all Si-O-Si bonds)
coo dina ion’s a e obse ed. The o ganic ac ion was analysed by 13C SS-NMR and he
spec um is in figu e - bo om. Peaks om he main componen s o ice husk can be
obse ed a 63, 73, 83, 88 and 105 ppm o cellulose, a 21 and 171 ppm associa ed wi h
ace a e g oups o hemicellulose (besides peaks in coincidence wi h cellulose), and a 56
and be ween 116 and 152 ppm (a oma ic ca bons) o lignin.
Figu e 3: TGA p ofile o ice husk and ela i e dTG eco ded unde ai flow (RT- 900 °C – 10 °C/min)
The he mog a ime ic p ofile eco ded unde ai flow shows he p esence o h ee
main weigh losses: fi s he dehyd a ion and he o he wo a e he combus ion o
lignin and cellulose. Wi h he help o he dTG p ofile, a ough o ganic composi ion can
be de e mined, because i he fi s weigh loss is cha ac e ized by a low combus ion
a e, e ealing ha ice husk does no con ain many ola ile molecules. On he o he
hand, he high combus ion a e o he second loss is asc ibable o ice husk wi h low
lignin con en .
All hese findings pe mi ed he comple e e alua ion o he cha ac e is ics o he ice
husk sample, eady o he p epa a ion o de i ed ma e ial use ul o be inse ed in
cemen as addi i e.
7
CHEM-UniTO
Soybean hulls, ano he biomass conside ed in RM2 ac i i y, ha e been cha ac e ized
h ough di e en echniques o s udy hei composi ion and chemical-physical
p ope ies. They showed a nega i ely cha ged su ace wi h a measu ed poin o ze o
cha ge a pH alue close o 2. The elemen al composi ion was also s udied h ough he
elemen al analysis .The w % a e age con en o C, H, N, S was 41.37±0.08; H 6.09±0.05; N
1.50±0.06; S 0.00 espec i ely while he calcula ed C/H a io was 6.79.
The ou comes o soybean hulls’ composi ional analysis pe o med h ough he NREL
p o ocol a e epo ed in Figu e 5-le . The main componen s a e hemicellulose (49%)
and cellulose (42%) while lignin (4%) and he lipidic ac ion (5%) a e a mino i y. These
componen s a e o ganized in fib ils as shown in FESEM image (Figu e 5- igh ).
Figu e 4: -Composi ion (le ) and FESEM image ( igh ) o soybean hulls
Rice husks’ ashes ha e been ob ained om a was e- o-ene gy p ocess o an impo an
company loca ed in Piedmon . Mo phological analysis and mic oanalysis (Figu e 6A
8
and 6B) showed an he e ogeneous composi ion cha ac e ized by he p edominance o
C and Si a oms. The high Si con en (22 g/100 g o ashes) was confi med h ough he
XRF analysis (Figu e 6C) which also allowed o exclude he p esence o dange ous
hea y me als. Si is con ained in he o m o silica as e idenced by he ATR-FTIR spec a
which showed he cha ac e is ic pa e n o SiO2 (Figu e 6D).
Figu e 5: Rice husk ashes cha ac e iza ion: A) FESEM-EDS mic oanalysis; B) FESEM
images; C) XRF esul s; D) ATR-FTIR spec um
UNITO (DBIOS)
Ma e ial collec ion, ex ac ion and quan ifica ion o high alue molecules om Elodea
nu alii
UNITO (DBIOS) ca ied ou su eys o de ec he p esence o he alien aqua ic
plan Elodea nu alliiin he s e ch o he Ri e Po be ween Villa anca Piemon e and
Casale Mon e a o. Elodea was ound om sp ing 2023 onwa ds a a ious loca ions
along he s e ch; i s biomass inc eased significan ly du ing he summe mon hs and
hen dec eased again owa ds au umn. This end was confi med o e he ollowing
9
Figu e 15. Fa y acid composi ion o UCO. PA= palmi ic acid, SA= s ea ic acid, OA= oleic
acid, LA= linoleic acid.
16