Accepted Manuscript

Title: LIGNOCELLULOSIC MICRO/NANOFIBERS FROM

WOOD SAWDUST APPLIED TO RECYCLED FIBERS
FOR THE PRODUCTION OF PAPER BAGS

Authors: Quim Tarrés, Neus Pellicer, Ana Balea, Noemi

Merayo, Carlos Negro, Angeles Blanco, Marc
Delgado-Aguilar, Pere Mutjé

PII: S0141-8130(17)31826-3
DOI: http://dx.doi.org/doi:10.1016/j.ijbiomac.2017.07.092
Reference: BIOMAC 7900

To appear in: International Journal of Biological Macromolecules

Received date: 22-5-2017

Revised date: 13-7-2017
Accepted date: 13-7-2017

Please cite this article as: Quim Tarrés, Neus Pellicer, Ana Balea, Noemi Merayo, Carlos
Negro, Angeles Blanco, Marc Delgado-Aguilar, Pere Mutjé, LIGNOCELLULOSIC
MICRO/NANOFIBERS FROM WOOD SAWDUST APPLIED TO RECYCLED
FIBERS FOR THE PRODUCTION OF PAPER BAGS, International Journal of
Biological Macromoleculeshttp://dx.doi.org/10.1016/j.ijbiomac.2017.07.092

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 LIGNOCELLULOSIC MICRO/NANOFIBERS FROM WOOD SAWDUST
APPLIED TO RECYCLED FIBERS FOR THE PRODUCTION OF PAPER
BAGS

Quim Tarrés1* joaquimagusti.tarres@udg.edu, Neus Pellicer1 neus.pellicer@udg.edu,

Ana Balea2 anabalea@ucm.es, Noemi Merayo2 nmerayoc@ucm.es, Carlos Negro2
cnegro@ucm.es, Angeles Blanco2 ablanco@ucm.es, Marc Delgado-Aguilar1
m.delgado@udg.edu, Pere Mutjé1 pere.mutje@udg.edu

1
Group LEPAMAP, Department of Chemical Engineering. University of Girona. c/M.
Aurèlia Campmany 61. 17071 Girona, Spain

2
Department of Chemical Engineering, Complutense University of Madrid. Avda
Complutense s/n, 28040 Madrid, Spain

*
Corresponding author at: Tel.: +34 972419840.

1
Highlights
 Lignocellulosic micro/nanofibers from pine sawdust can be produced by only
mechanical treatments
 Effect of fibers chemical composition on lignocellulose micro/nanofibers production
was evaluated
 Effect of LCMNF on whiteness of white papers was determinated
 Typical paper bags tensile strength was reached by only 3 or 4.5 % LCMNF addition
 Lower effect on drainability was found when LCMNF were used

2
Abstract

In the present work, lignocellulosic micro/nanofibers (LCMNF) were produced from pine
sawdust. For that, pine sawdust was submitted to alkali treatment and subsequent
bleaching stages, tailoring its chemical composition with the purpose of obtaining
effective LCMNF. The obtained LCMNF were characterized and incorporated to
recycled cardboard boxes with the purpose of producing recycled paper. The obtained
results showed that it was possible to obtain LCMNF with the same reinforcing potential
than those cellulose nanofibers (CNF) prepared by oxidative or other chemical methods.
In fact, the obtained papers increased the breaking length of recycled cardboard from
3338 m to 5347 m, being a value significantly higher than the requirements to produce
paper bags. Overall, the studied strategies could allow a significant reduction of paper
basis weight, with the consequent material saving and, thus, contribution to the
environment.

Keywords: Lignocellulosic Micro/nanofibers; Paper Bag; Recycled Fibers; Papermaking

3
1. Introduction

Packaging is a growing sector with an annual increase of 4%. It encompasses a wide range
of material types across paper, board, plastic, metal, glass, wood and other materials. The
largest share of global packaging is accounted for paper and board packaging with a
production over 200 million tonnes and sales of 261 USD billion in 2015, equating near
40% of the market. In Europe, paper and board packaging production in 2015 was 44.5
million tonnes and it has increased by 2.6% compared to 2014 [1]. The factors
contributing to the growth of the paper and board packaging market are the increasing
demand of packaged food, the increasing number of supermarkets, the rising of online
retail and the sustainability of paper products [2].

Nowadays, the recovery of paper and board is a well stablished practice with a recycling
rate of 71.5% and a utilization rate of 52.5% [1]. Packaging has the highest recovered
paper utilization rate, near 100% for case materials category [1].

Paper recycling contributes to the aims of circular economy but by increasing the number
of recycling cycles, the quality of the fibers gradually decreases, mainly because of the
hornification of the cellulose fibers causing irreversible changes in the fiber structure and
properties [3]. Therefore, secondary fibers inherently reduce paper quality, especially
strength [4]. On the other hand, replacement of cellulose fibers by fillers is a common
practice for reducing raw material and energy costs and for improving bulk, smoothness
and optical paper properties. However, the substitution of cellulose fibers with fillers
reduces the strength and the quality of the printing properties of the finished sheet [5,6].

Refining is the most common method used to improve the strength of paper. By applying
shear forces to the fibers, more fibrillated fibers are created, improving mechanical
entanglement, hydrogen bonds, and fiber-to-fiber joint strength. This allows the
formation of a fibrous network with some improved mechanical properties, but it is
clearly detrimental to others, slowing the drainage rate, increasing energy consumption,
and decreasing the tear resistance and opacity of the finished paper [7–9]. Moreover, high
quality fibers from wood, wood wastes or agrowastes [10,11] and strength additives are
commonly used to increase mechanical paper properties [4]. Since, poor tensile strength

4
is the main source of costumer complains to paper manufacturers, alternative methods to
achieve the market requirements are still needed [12].

In this context, new strategies to improve interfiber bonding have been explored, such as
enzymatic refining or the use of cellulose nanofibers (CNF). Although, the use of
enzymes have been reported at mill scale, more research is needed to develop effective
enzymes and to optimize different process parameters [13].

CNF have emerged as an alternative additive to improve the mechanical properties of

paper and board with additional advantages, such as their renewable nature,
biodegradability and high potential availability. Several studies have demonstrated that
the use of CNF obtained by oxidation pre-treatment using 2,2,6,6,-tetramethylpiperidine-
1-oxyl radical (TEMPO) and mechanical homogenization enhances mechanical
properties of paper and board [14–16] and reduces linting propensity in recycled paper
with high filler load [6]. However, recent industrial studies have demonstrated that
TEMPO-oxidized nanocelluloses (TO-CNF) have at the moment unreachable production
costs for papermaking industry. The high cost of TO-CNF can be associated with the
chemical pretreatment of fibers before the mechanical desestructuration [17]. Therefore,
recent studies have focussed on producing low cost micro/nanofibers (LCMNF) for
brown paper strength enhancement [18,19].

In this sense, the present work shows the technical and economic viability of producing
LCMNF from pine sawdust by only mechanical treatments. Pine sawdust from sawmills
is an important by-product in Europe during the primary transformation of wood. Firstly,
the amorphous part of pine sawdust pulp, lignin and hemicellulose content, was studied
to optimize the LCMNF production. Then, LCMNF were added to recycled cardboard
furnish, and the handsheets were examined in terms of mechanical properties to be used
as commercial paper bags.

2. Experimental

Materials

Pine sawdust was supplied by Mas Clara, Domeny (Girona, Spain). Sodium hydroxide
and sodium hypochlorite for cooking and bleaching processes were purchased from
Sigma-Aldrich, Spain. Table 1 shows the mechanical properties of the commercial paper

5
bag taken as reference. Recycled cardboard was collected from BonPreu Supermarket
(Girona, Spain) to prepare the paper furnish used to obtain the handsheets.

Pulp digestion and bleaching

Pine sawdust was first cooked in a rotatory pulp digester at 180ºC in presence of 25 wt%
NaOH during 90 minutes. The treated sawdust was then washed with water to neutral pH
and black liquors were removed by filtration. Then, sawdust was fibrillated by passing
through a Sprout-Waldron refiner in order to obtain individual fibers. Finally, pulp was
bleached with 8 wt% NaClO at 70ºC. Bleaching time was set at 1, 2, 3 and 4 hours and
bleached pulps were labelled as PS-1, PS-2, PS-3 and PS-4, respectively. Unbleached
pine sawdust pulp was labelled as PS-0.

Fibers characterization

Extractive fraction, Klason lignin and kappa number were determined according to
standards (ISO 302:2015 and T222 om-15) [20–22]. Hemicellulose content was
performed by high performance anion exchange chromatography (HPAEC) and cellulose
content was calculated by difference from 100% [19,23]. Fiber morphological analysis
was conducted in a MorFi compact analyzer (TechPap, France) that provides information
about fiber length, fiber diameter and fines content (those fibers shorter than 75 µm).

Production and characterization of lignocellulosic nanofibers

Lignocellulosic micro/nanofibers were obtained by fully mechanical treatments (LCMNF)

from PS-0 to PS-4 pine sawdust pulps. First, pulps were diluted at 2.0 % of consistency
with tap water. Then, suspensions were passed through a Mazuko grinder MKCA6-5
several times during 3 hours. This time was set taking into account previous experience
acquired with private contracts, which was found to obtain the maximum efficiency at
minimum cost.

LCMNF were characterized by field emission scanning electron microscopy (FE-SEM),

yield of nanofibrilation, transmittance, carboxyl content and cationic demand. Specific
surface and diameter of LCMNF were calculated from cationic demand and carboxyl
content based on the method reported by [18,19].

6
The yield of nanofibrilation was determined by centrifugation at 4500 rpm during 20
minutes for the separation of nanofibrillated fraction in the supernatant. Transmittance
readings of 0.1% wt. LCMNF suspensions diluted were performed between 400 and 800
nm on a UV-Vis Shimadzu UV-160A spectrophotometer. The carboxylic content of
LCMNF was calculated by conductometric titration of each sample [15]. Cationic
demand was determined by colloidal titration of the diluted LCMNF suspension at 0.1
wt.% using a particle charge detector, Mütek PCD 04 (BTG Instruments GMbH,
Germany). LCMNF charge was offset in excess by polydiallyldimethylammonium
chloride (polyDADMAC) and then this excess was titrated with anionic polymer (Pes-
Na) [24].

Handheets preparation and characterization

Cardboard boxes were first torn in small pieces to be disintegrated in a laboratory pulper
at 3,000 rpm during 15 minutes. Consistency was set at 1.5 %. Then, LCMNF were added
into the pulper and disintegrated at 3,000 rpm for 60 minutes. After this, 0.5 % of cationic
starch and 0.8 % of colloidal silica were added as retention agents. The amount of
LCMNF-reinforced pulp was calculated to obtain 75g/m2 paper sheets in a normalized
Rapid-Köthen, following the standard ISO 5269-2:2004 [25]. Wet handsheets were
vacuum-dried at 90ºC for 10 minutes and conditioned for 24 hours at 23ºC and 50% RH
before mechanical testing [26].

Cationic starch was added to ensure the completely retention of LCMNF. However, the
flocculation produced by cationic starch could lead to a non-good handsheet formation.
Therefore, the addition of colloidal silica micronizes the flocs ensuring a good
distribution of fibers on the handsheet. This retention system was verified by the
production of the same handsheet without the retention system using a nitrocellulose
membrane with a 0.22 µm pore diameter [19]. The LCMNF retention level resulting by
these two systems was the same. These results prove the correct efficiency of this
retention system.

The effect of LCMNF lignin content on the papers produced with bleached pulp was
determined by measuring the brightness, following the standard ISO 11475:2010 [27].
Drainage rate of pulps was evaluated by means of Schopper-Riegler test method, ISO
5267-1:1999 [28]. Thickness and porosity of the handsheets were measured following the

7
standards ISO 534:2011 and ISO 5636-5:2013 [29,30], respectively. Breaking length
(BL), strain at break (Ɛ) and Young’s modulus (E) of handsheets were determined from
tensile experiments performed in an INSTRON universal testing machine provided with
2.5 kN cell load; according to the standard ISO 1924-2:2008 [31]. Finally, tearing
resistance was determined by Elmendorf method [32].

3. Results and discussion

Chemical and morphological characterization

The chemical composition of pine sawdust, the starting material for the production of
different LCMNF, was determined according to the abovementioned methods (Table 1).

TABLE 1 GOES AROUND HERE

Comparatively, pine sawdust presented higher lignin content than annual plants (2.5 – 12
%) [33] or fibers from several straws (16 – 20 %) [34]. Nonetheless, hemicellulose
amount was considerably lower than for triticale which, as reported elsewhere [19],
accounted for more than twice. Cellulose content was surprisingly higher, which, at first
sight, indicates that pine sawdust it is not probably the best choice for LCMNF production,
taking into account the expected high crystallinity. As reported by Boufi and Gandini
2015 [35], the presence of amorphous polysaccharides, which is not the case of cellulose,
could benefit fibrillation and, thus, LCMNF production. In any case, the selected pine
sawdust for this work presented about 43 % of amorphous constituents (hemicellulose
plus lignin), fact that justifies its use as raw material for LCMNF production. In addition,
the selected sawdust is interesting due to its origin, since it is a residue from pine pulp
production process.

Pine sawdust, once treated in the rotary digestor, was fibrillated in a Sprout-Waldron
refiner. The alkali treatment presented a yield of 45.4 %, meaning that almost 55 % of the
raw material was removed and dissolved by the cooking liquors. This removal caused
significant changes in the chemical composition of the starting material. In relative terms,
while extractives were totally removed, the treated sawdust still had the half of the initial
lignin and hemicellulose (Table 2). This decrease on amorphous regions was also
observed by Lehto et al. (2016) [36], and it is a well-known fact in fiber production.

TABLE 2 GOES AROUND HERE

8
This reduction can be associated to the severity of the alkali treatment, understood as
sodium hydroxide concentration, temperature, pressure and time. With the purpose of
removing lignin without affecting dramatically the hemicellulose content, PS-0 was
submitted to subsequent bleaching stages with sodium hypochlorite, which has been
previously reported to be a successful bleaching method for LCMNF production. In that
way, lignin was decreased from 14.7 to 2.4 %, with moderate hemicellulose removal
(from 5.9 to 4.3 %). By definition, kappa number is an indication of the residual lignin
content or bleachability of wood pulp by a standardized analysis method. In fact, kappa
number estimates the amount of chemicals required during bleaching, being this amount
related to the lignin content of the pulp. Thus, this measurement can be used to monitor
the effectiveness of the lignin extraction phase. Morphological analysis did not show any
significant change on fiber length and diameter, while fines content showed a slight
increase as bleaching time was increased.

LCMNF Production and Characterization

The obtained pulps were used for the production of different LCMNF. Taking into
account the grinding time, the amount of fibers passed through and the price of energy in
Spain (assuming cogeneration, 0.08 €/kW·h), the fibrillation cost for all the obtained
LCMNF was 1.04 €/kg. Each LCMNF was characterized as described in the previous
section and results are shown in Table 3.

TABLE 3 GOES AROUND HERE

As in other works [17,18], an optimal point was found in terms of LCMNF properties. In
this case, those LCMNF prepared from PS-1 (kappa number, 20) showed the best
performance. Thus, those LCMNF prepared from the starting pulp (PS-0) showed a yield
of fibrillation of 18.23 %, which has increased to 21.03 % by decreasing kappa number
in 5 units (PS-1), and then was decreased with further bleaching. The same tendency was
observed with cationic demand and transmittance at 800 nm. Carboxyl content remained
constant, fact that proves that sodium hypochlorite was totally consumed by lignin and
there was no fiber oxidation, meaning that no COO- groups were introduced in cellulose
chains.

FIGURE 1 GOES AROUND HERE

9
The obtained LCMNF were observed by FE-SEM (Figure 1), showing that individual
fibrils were obtained, with diameters in the nano-domain. Nonetheless, the obtained
diameters are still larger than those obtained by treating fibers by oxidative or other
chemical methods [9, 33, 34]. As it is possible to see, the obtained values for diameter
(Table 3) are in consonance with the FE-SEM micrographs, proving the method based on
carboxyl content and cationic demand. In fact PS-1 LCMNF presented the highest
cationic demand and, as it is well known, this property is strongly related to specific
surface.

Commercial paper bag characterization

Commercial paper bag was taken as a reference to stablish the minimum requirements to
be achieved (Table 4).

TABLE 4 GOES AROUND HERE

Table 4 shows the great difference if mechanical properties are measured at machine and
at cross direction. The difference between both directions comes from fiber orientation
during paper formation due to the differential speed between the head box inlet and the
paper cloth. This phenomenon cannot be observed with paper sheets prepared at
laboratory scale, since fibers get randomly oriented due to the static conditions of the
equipment. Taking into account that fiber orientation can increase the breaking length (at
machine direction) by a factor of 1.33 – 1.45 and the starch at the size press, by 1.12, the
breaking length requirement to be achieved at laboratory scale was set between 4374 and
4768 m. Both factors, anisotropy and starch contribution, were calculated and discussed
in a previous work [37].

Effect of LCMNF on recycled cardboard paper

Recycled cardboard pulps were reinforced with 3 wt% of each LCMNF and basic physic-
mechanical properties were assessed, both of the reinforced pulps and papers. Table 5
shows the effects on pulp drainability, as well as some mechanical properties.

TABLE 5 GOES AROUND HERE

The reference pulp presented an initial drainability of 35 °SR and the resulting papers,
about 3340 m of breaking length. This value is considerably lower than the established

10
minimum requirement in the previous section. When 3 wt% of LCMNF was added, as
expected, mechanical properties were significantly improved and drainability, worsened.
However, the impact of adding 3 wt% of LCMNF on pulp drainability was considerably
low compared to that caused by other types of nanofibers, especially those obtained by
chemical methods [38]. What becomes apparent is that as yield of fibrillation of LCMNF
was increased, tensile properties were enhanced and, at the same time, pulp drainability
was slightly decreased, mainly due to the higher specific surface thereof [8].

PS-1 LCMNF increased the breaking length of recycled papers in 47.5 %. Comparatively
to virgin pulps, the properties enhancement that such LCMNF can impart was
significantly lower, mainly due to fiber fibrillation and the presence of fines produced by
the subsequent refining stages that cardboard boxes have stand [39].

The main drawback of such LCMNF is the presence of lignin, which limits their use in
white papers. With the purpose of quantifying the effect of such LCMNF in white papers,
3 wt% of each LCMNF was added to a bleached kraft hardwood pulp and brightness was
measured (Figure 2).

FIGURE 2 GOES AROUND HERE

As expected, paper brightness was significantly decreased by the incorporation of 3 wt%

of LCMNF, from 82.6 to 62.3 % in the worst case. Thus, the use of such LCMNF in white
papers could be not recommended depending on the final application but, in the case of
brown-line papers, at first sight, there are no drawbacks in this sense.

LCMNF from PS-1 were incorporated at different percentages on recycled papers with
the purpose of assessing the effect of increasing percentages on pulp and paper properties
(Table 6).

TABLE 6 GOES AROUND HERE

As expected, as the amount of LCMNF was increased, Schopper – Riegler degree was
increased (13 ºSR for 4.5 % addition). Sheet density increased with further addition of
LCMNF. This effect mainly comes from the shrinkage forces that LCMNF impart
between fibers, leading to smaller pores and, thus, decreasing paper porosity (bulk).

11
In principle, mechanical properties, such is breaking length, are not affected by basis
weight. However, in a recent work it has been found that this is not completely true [40].
The incorporation of 3 and 4.5 % of LCMNF to 76 g/m2 paper sheets enhanced breaking
length to 4925 and 5347 m, being higher than the established minimum requirement for
papers of 136 g/m2 (4768 m). In the referred work, breaking length and tear index were
decreased in 11.6 and 30.5 % when basis weight was also decreased from 140 to 80 g/m2.
This means that, at first sight, if basis weight was set at 140 g/m2 for LCMNF-reinforced
papers, even higher mechanical properties could be achieved, leading to stronger bags.
Not only this, but, if technical requirements were the same, the present work shows that
basis weight could be decreased from 136 to 76 g/m2. This would mean significant
savings in terms of raw material, meaning that cost efficiency would be improved, at the
same time than contributing to the environment.

4. Conclusions

In the present work, LCMNF from pine sawdust have been successfully prepared and
used as paper strength additive for the production of paper bags. The main conclusions
can be listed as follows:

- Pine sawdust, properly treated and bleached, can lead to cost-efficient LCMNF
with similar reinforcing potential than those obtained by oxidative methods.
- Chemical composition of starting pulp for LCMNF production play a key role
during fibrillation.
- The effect of adding LCMNF to white papers has been quantified in terms of paper
brightness, proving that this optical property is strongly affected, limiting thus
their use for some applications. This fact opens an opportunity to such LCMNF
in the production of brown-line papers.
- The obtained LCMNF significantly increased mechanical properties of paper with
minor effects on pulp drainability, making them suitable to be used as bulk
additive.
- The use of LCMNF in packaging paper production opens an opportunity to
palliate natural resources consumption due to basis weight reduction. This
strategy would also save production and transport costs.

12
Acknowledgements

The authors wish to thank the Economy and Competitiveness Ministry of Spain and the
Community of Madrid (Spain) for the support of projects with references CTQ2013-
48090-C2-1-R and P2013/MAE2907.

13
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Figures Legend

Figure 1. FE-SEM micrographs of LCMNF from pine sawdust pulp: a) LCMNF PS-0;
b) LCMNF PS-1; c) LCMNF PS-2; d) LCMNF PS-3; e) LCMNF PS-4

Figure 2. a) Picture of different LCMNF obtained b) Evolution of paper brightness with

3% of different LCMNF

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Tables

Table 1. Chemical characterization of pine sawdust

Klason
Extractive Kappa Hemicellulose Cellulose
Lignin
(%) number (%) (%)
(%)
2.04 30.6 88.37 12.30 55.06
*Weighted in length
**Percentage in length under 75 µm length

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 Table 2. Chemical and morphological characterization of bleached and non-bleached
pulps from pine sawdust

Klason
Extractive Kappa Hemicellulose Cellulose Length* Diameter Fines**
Lignin
(%) number (%) (%) (mm) (µm) (%)
(%)
PS-0 0.80 14.7 25 5.89 78.64 0.576 24.1 67.4
PS-1 0.64 11.7 20 5.51 82.15 0.572 23.9 68.9
PS-2 0.54 6.4 16 4.96 88.10 0.558 23.8 72.6
PS-3 0.31 3.2 10 4.31 92.18 0.553 23.7 76.8
PS-4 0.27 2.4 8.9 4.25 93.08 0.549 23.7 77.3
*Weighted in length

** Percentage in length under 75 µm length

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 Table 3. Characterization of LCMNF

Yield of Carboxyl Cationic Specific

LCMNF Kappa Transmittance Diameter
nanofibrilation content demand surface
grade number at 800nm (nm)
(%) (µmols/g) (μeq·g/g) (m²/g)
PS-0 25 18.23 35.4 46.35 207.28 78.4 32
PS-1 20 21.03 41.6 46.74 228.11 88.3 28
PS-2 16 18.52 37.9 46.57 211.35 80.2 31
PS-3 10 17.21 29.7 46.67 199.67 74.5 34
PS-4 8.9 16.98 26.6 46.54 198.45 74.0 34

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 Table 4. Dimensions and mechanical properties of a high quality commercial paper bag

Paper bag dimensions Paper dimensions

Width Height Depth Volume Basis Thickness Density Porosity
(cm) (cm) (cm) (L) weight (µm) (g/cm³) (s)
(g/m²)
42 42.5 17 30.3 136 169 0.8 109 ± 4
Mechanical properties of paper bags
BLMD BLCD ƐMD ƐCD EMD ECD Tear I.MD Tear I.CD
(m) (m) (%) (%) (GPa) (GPa) (mN·m2/g) (mN·m2/g)
7103 ± 46 3794 ± 75 3.63 ± 0.12 2.29 ± 0.14 5.06 ± 0.09 2.30 ± 0.08 12.4 ± 0.2 11.2 ± 0.3
BLMD is breaking length on machine direction; BLCD is breaking length on cross
direction; ƐMD is deformation on machine direction; ƐCD is deformation on cross
direction; EMD is Young Modulus on machine direction; ECD is Young Modulus on
cross direction; Tear I.MD is tear index on machine direction; Tear I.CD is Tear index on
cross direction.

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Table 5. Characterization of recycled hand sheets with 3 % LCMNF addition

BL Ɛ E Tear I. Porosity
CNF °SR
(m) (%) (GPa) (mN·m2/g) (s)
Ref. 35 ± 0 3338 ± 115 1.27 ± 0.08 2.17 ± 0.03 7.4 ± 0.2 7.6 ± 0.8
PS-0 42 ± 1 4397 ± 207 1.82 ± 0.07 2.55 ± 0.07 8.0 ± 0.1 22.8 ± 0.3
PS-1 44 ± 1 4925 ± 150 1.97 ± 0.03 2.71 ± 0.06 8.3 ± 0.4 22.9 ± 0.2
PS-2 43 ± 1 4502 ± 167 1.84 ± 0.02 2.58 ± 0.04 8.2 ± 0.3 22.9 ± 0.4
PS-3 40 ± 0 4096 ± 214 1.61 ± 0.04 2.40 ± 0.02 7.5 ± 0.2 22.6 ± 0.4
PS-4 40 ± 1 3962 ± 163 1.59 ± 0.05 2.41 ± 0.09 7.5 ± 0.1 22.4 ± 0.3

ºSR is Schopper-Riegler degree; BL is breaking length; Ɛ is deformation; E is the Young

modulus; Tear I. is the tear index.

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Table 6. Mechanical properties of recycled hand sheets with PS-1 LCMNF addition

E Gurley
LCMNF Thickness Porosity BL Ɛ Tear I.
°SR (GPa) porosity
(%) (µm) (%) (m) (%) (mN·m2/g)
(s)
0 151 68.5 35 ± 0 3338 ± 133 1.27 ± 0.12 2.17 ± 0.13 7.4 ± 0.2 7.6 ± 0.1
1.5 147 67.7 38 ± 1 4204 ± 146 1.67 ± 0.15 2.48 ± 0.17 7.8 ± 0.1 15.1 ± 0.4
PS-1

3 141 66.3 44 ± 1 4925 ± 124 1.97 ± 0.24 2.71 ± 0.16 8.3 ± 0.3 22.9 ± 0.4
4.5 136 65.1 48 ± 1 5347 ± 139 2.15 ± 0.18 2.87 ± 0.21 8.7 ± 0.3 33.0 ± 0.7

26