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US 20140352903A1

(19) United States


(12) Patent Application Publication (10) Pub. No.: US 2014/0352903A1
Ernegg (43) Pub. Date: Dec. 4, 2014
(54) CELLULOSE FIBRE COMPOSITION (30) Foreign Application Priority Data
(75) Inventor: Martin Charles Ernegg, Mullumbimby Oct. 26, 2010 (AU) ----- --------- -- --- ------ --- ---- 2010904775

(AU) Publication Classification

(51) Int. Cl.


(73) Assignee: ZEO IP PTY LTD, Mullumbimby, New D2 IIH II/4 (2006.01)
South Wales (AU) (52) U.S. C.
CPC ..................................... D2 IH II/14 (2013.01)
(21) Appl. No.: 13/881,408 USPC ........... 162/149; 162/100: 162/162; 162/158:
(22) PCT Filed: Oct. 26, 2011 162/159
(57) ABSTRACT
(86). PCT No.: PCT/AU2O11?0O1360
A cellulosic composition comprising fibres having a length
S371 (c)(1), weighted average fibre length (“LWAFL) of 0.25 to 0.40
(2), (4) Date: Jul. 8, 2014 .
Patent Application Publication Dec. 4, 2014 Sheet 1 of 9 US 2014/0352903A1

Water Retention Value


Centrifuge
cup or shield

Fife'
Sample in
centrifuge tube
TAPPI Useful Method UM 256
Figure 1

(a) (b)

(a) (b)
Patent Application Publication Dec. 4, 2014 Sheet 2 of 9 US 2014/0352903A1

(a) (b)
Patent Application Publication Dec. 4, 2014 Sheet 3 of 9 US 2014/0352903A1

(a) (b)

(a) (b)
Patent Application Publication Dec. 4, 2014 Sheet 4 of 9 US 2014/0352903A1

Distribution of fibre lengths Sample A


8,8 - - - - - -

so
4.3 :

Illin. * * * 8 & 3 x : $ $8
x : : - - -
Patent Application Publication Dec. 4, 2014 Sheet 5 of 9 US 2014/0352903A1

Distribution of fibre lengths Sample B


7.3

s
Q> | - - - - -- - - - - - - - -. . .. .

r
Hill.
a- - - -r:
S$ 3 : S. 3' s s: : s s: , ;
is is..... wasaka.

Length of fibre (mm)


s

3 :

2. 8s 3.8 .38 33 8,
P
Cy
r
A.r &8

Length of fibre (mm)

Figure 9
Patent Application Publication Dec. 4, 2014 Sheet 6 of 9 US 2014/0352903A1

Distribution of fibre lengths Sample C

s>
2t 2.8

2rD 3.
|III ar is is is .......
: s , S: , s 3 - ? 8° S : y : * * :
Length of fibre (mm)

&

3.
- ?
Š
Z.
r
P
Cy
r : :

88:

Length Of fibre (mm)

Figure 10
Patent Application Publication Dec. 4, 2014 Sheet 7 of 9 US 2014/0352903A1

Distribution of fibre lengths sample D

s> W
O
Z.
Cy s
r

--------------rr-r Illiluli.
& *s as $ 3 S $ & $
Length of fibre (mm)

&

s
O
Z.
Cy
2

338 fi 88: 8,33 3.3s 87 & 8: 8,38 8.8

Length of fibre (mm)

Figure 11
Patent Application Publication Dec. 4, 2014 Sheet 8 of 9 US 2014/0352903A1

Distribution O fibre lengths Sample E

s>
Q
Z.
-
t
Cy
r
A.
r s

W v lin.
is 3 & y & 8 s: s 2 & 3 S S & 8 :
Length of fibre (mm)

D
Q
Z.
-
r :

Sr

, 8, 8,88 3,33 s 88. 8.7 8. 3.3S .

Length of fibre (mm)

Figure 12
Patent Application Publication Dec. 4, 2014 Sheet 9 of 9 US 2014/0352903A1

Distribution of fibre lengths Sample F

S k 3 && K.3 S.8.


&3 s :- SY3 sN. S.& &x
:
SY s&: s &
Length of fibre (mm)

s
s
>
tr
Cy ; :
r
A.
r
; :8
8 . -
8.8

Length of fibre (mm)

Figure 13
US 2014/0352903A1 Dec. 4, 2014

CELLULOSE FIBRE COMPOSITION numerical average (AFL) and the weight weighted average
fiber length (WWAFL). These averages are obtained through
TECHNICAL FIELD the following calculations:
0001. The disclosure relates to cellulosic compositions
that are useful as structural building components for objects
including, but not limited to, buildings, furniture, car parts,
coffins, cabinets & cases, electronic housing, structural build AFL = =
ing pillars, beams, boards, sheets, Veneers, chairs, musical X (if n.)
instruments, and toys. LWAFL= St.
BACKGROUND
X(f-n,)
0002 Large amounts of waste generated in the pulp and WWAFL– (l. n.)
paper processing industry are typically disposed to landfill.
Disposal to landfill, however, is becoming increasingly prob where
lematic due to the environmental constraints associated with
land availability and land/soil contamination. As such, there 0013 x=bin it
is significant pressure to reduce the amount of waste disposed 0014 1-bin median length
to landfill, one means of reduction being recycling. 00.15 n=bin fiber count
0003 Recycling of paper and textile materials requires the 0016 N=total number of fibers counted
breakdown of such materials into fibres or fibre-like material 0017 Preferably, the composition has a Water Retention
which may then be reformed into material to provide paper Value (WRV) of 600% to 2000%, more preferably, 700% to
and paper-like products. As an alternative to reforming into 1300%.
material to provide paper and paper-like products, a recycling (0018. The water retention value (WRV) is defined as the
process has previously been developed for producing moul amount of water that participates in the swelling of the fibrous
ded pieces out of cellulose fibres in which the specific gravity material and that which is not released under the application
of the moulded pieces approaches that of pure cellulose, 1.5. of a centrifugal force. The WRV is also highly correlated to
The process involves finely chopping and grinding cellulose the bonding ability of kraft fibers. The test to determine the
fibres in the presence of water into micro-fibres prior to form WRV is carried out by placing a pad of moist fibers in a
ing a fibre-water mixture in which the cellulose fibre content centrifuge tube that has a fritted glass filter at its base. The
is about 1-15% by weight. The process subsequently involves centrifuge is accelerated at 3000 g for 15 minutes to remove
shaping and drying the mixture of cellulose fibres and water water from the outside surfaces and lumens of the fiber. The
into the moulded pieces. Details of the process and the moul remaining water is believed to be associated with submicro
ded pieces produced by the process are set out in U.S. Pat. No. scopic pores within the cell wall. The centrifuged fibers are
6,379,594. weighed, dried at 105°C., and then reweighed. The WRV can
0004 Efforts have continued in the production of cellulo then be calculated from the ratio of the water mass to the dry
sic based compositions derived from pulp and paper process mass. The apparatus used to measure the WRV is shown
ing waste and plant fibres which have high load bearing schematically in FIG. 1.
capacities and the ability for use as structural components. 0019. In an embodiment, the composition comprises, by
weight:
SUMMARY 0020 (a) 15% to 25% fibres of a length weighted aver
0005. The disclosure provides a cellulosic composition age fibre length of 0.001 mm to 0.2 mm:
comprising fibres having a length weighted average fibre 0021 (b) 45% to 55% fibres of an a length weighted
length (“LWAFL) of 0.25 to 0.40 mm. average fibre length of 0.2 mm to 0.5 mm;
0006 Preferably, 0.28 to 0.38 mm. 0022 (c) 20% to about 30% fibres of a length weighted
0007. The disclosure also provides a cellulosic composi average fibre length of 0.5 mm to 1.2 mm and
tion comprising, by weight: 0023 (d) less than 1% fibres of a length weighted aver
0008 (a) 15% to 25% fibres of a length weighted aver age fibre length of 1.2 mm to 2.0 mm.
age fibre length of 0.001 mm to 0.2 mm: 0024. The cellulosic composition may be in a wet or dry
0009 (b) 40% to 60% fibres of a length weighted aver State.
age fibre length of 0.2 mm to 0.5 mm; 0025. In an embodiment, the cellulosic composition are
0010 (c) 8% to 35% fibres of a length weighted average dried in the form of pellets, granules or powders. In the dry
fibre length of 0.5 mm to 1.2 and state, the cellulosic composition may be conveniently stored
0011 (d) less than 3% fibres of a length weighted aver and transported.
age fibre length of 1.2 mm to 2.0 mm. 0026. The dry pellets, granules or powders may be mixed
0012. The length weighted average fibre length with water to form mouldable, fine pulps that may be dried to
(“LWAFL) provides a measure of the average length of the create materials for use as structural components.
fibres in a sample of fibres which is weighted by the length of 0027. The mouldable, fine pulps may be moulded using
the individual fibres. The LWAFL gives emphasis to the any Suitable method including, but not limited to, spray mold
longer fibers in the sample and imparts less emphasis to the ing, injection molding, extrusion or three stage molding. The
shorter fibers and fines. The LWFAFL is sometimes referred moulded or green articles may be subsequently dried to form
to as just the weighted average fibre length or “WAFL. The a product
LWAFL can be compared to other measures of the average 0028. The density of the product produced from a compo
length of the fibres in a sample such as the arithmetic or sition according to the disclosure may be from 0.5 g/cm3 to
US 2014/0352903A1 Dec. 4, 2014

1.5 g/cm3. The tensile modulus of the product may be from composition are distributed in a skewed bell curve, with the
3500 MPa to 10800 MPa and the tensile strength may be from composition comprising, by weight:
27 MPa to 115 MPa. 0041 (a) 15% to 25% fibres of a length weighted aver
0029 Whilst functional additives (such as dyes and pig age fibre length of 0.001 mm to 0.2 mm:
ments for colouring, resins and waxes for waterproofing, (0.042 (b) 40% to 60% (preferably 45% to 55%) fibres of
lime, fire retardants including natron silicate, glues, metal a length weighted average fibre length of 0.2 mm to 0.5
powders and graphites for electrical conductivity, latex for
flex and waterproofing, fillers and very long fibres of 1.5-6.0 (0.043 (c) 8% to 35% (preferably 20% to 30%) fibres of
mm in length for increased tensile strength) may be added to a length weighted average fibre length of 0.5 mm to 1.2
the pulp of dry cellulosic powders/granules/pellets mixed and
with water, there is no need for the addition of any functional 0044) (d) less than 3% (preferably less than 1%) fibres
additives or the application of pressure to dry and harden the of a length weighted average fibre length of 1.2 mm to
pulp. 2.0 mm.
0030. In an embodiment, the composition may be pre 0045 Thus the composition consists of a significant
pared by any one or combination of processing methods amount of fines (fibre length <0.2 mm) mixed with short
including, but not limited to, ultra friction grinding, high length fibres (fibre length of 0.2-1.2 mm).
pressure homogenizing, cryo grinding, extrusion, Steam 0046 Additionally, the composition has a high degree of
explosion, ultra Sonic treatment, enzyme-fibre separation, fibrillation indicated by a high Water Retention Value (WRV)
high consistency/medium consistency/low consistency refin
ing, chemical treatment or whitewater fines recovery. of 600-2000%, preferably, 700-1300%.
0031 Components of the composition may be prepared 0047. The composition is prepared by any one or combi
separately and mixed together. In an embodiment, two or nation of processing methods including, but not limited to,
more intermediary compositions with different fibre length ultra friction grinding, high pressure homogenizing, cryo
distributions may be prepared and mixed in the required pro grinding, extrusion, steam explosion, ultra Sonic treatment,
portions to form the compositions defined above. enzyme-fibre separation, high consistency/medium consis
0032 Various raw materials may be used in the prepara tency/low consistency refining, chemical treatment or white
tion of the compositions as described herein, including, but water fines recovery.
not limited to, short/ultra short cellulose fibres/fines recov 0048 Components of the composition may be prepared
ered from waste streams, for example, recovered paper, separately and mixed together. In some embodiments, two or
recovered fines in whitewater from paper & pulp processing more intermediary compositions with different fibre length
and recovered cotton fibers. Additional raw materials may distributions are prepared and mixed in the required propor
also include any cellulosic fibers used in pulp & paper pro tions to form the composition.
cessing and various plant fibers having a high cellulosic con 0049 Various raw materials may be used in the prepara
tent, for example, hemp, flax, cotton, abaca, sisal and jute. tion of the composition, including, but not limited to, short/
ultra short cellulose fibres/fines recovered from waste
0033. The disclosure also provides a product made from a
composition as described herein. streams, for example, recovered paper, recovered fines in
whitewater from paper & pulp processing and recovered cot
BRIEF DESCRIPTION OF THE FIGURES ton fibers. Additional raw materials may also include any
cellulosic fibers used in pulp & paper processing and various
0034 Embodiments will now be described, with reference plant fibers having a high cellulosic content, for example,
to the accompanying Figures, in which: hemp, flax, cotton, abaca, sisal and jute.
0035 FIG. 1 is a schematic view of an apparatus for mea 0050. The composition may be dried for transport and/or
suring the Water Retention Value (WRV) of fibre samples: storage in the form of pellets, granules or powders. From
0036 FIGS. 2-6 depict Norval Wilson stained microscope these forms, the compositions may be re-wetted to form
images of wet pulp compositions derived from wastepaper a moldable, fine pulps. Alternatively, the compositions may be
the scales indicated; prepared as a pulp and used directly in a molding process. The
0037 FIG. 7 depicts Norval Wilson stained microscope compositions as a pulp may be moulded by any moulding
images of wet pulp compositions derived from hemp cellu operations known to persons skilled in the art, for example,
lose at the scales indicated; and spray molding, injection molding, extrusion or three stage
0038 FIGS. 8-13 are graphs of the fibre length distribu molding. The moulded or green articles may be Subsequently
tions for the wet pulp compositions shown in FIGS. 2-7. dried to form a product.
0051) Advantageously, the composition can be used to
DETAILED DESCRIPTION OF THE create a material with appropriate hardness, strength and duc
EMBODIMENTS tility to be used as a structural material yet remains (as a wet
pulp) capable of being readily handled during processing and
0039 Embodiments provide cellulosic composition made manufacture of articles from the composition, including very
up of fibres having different specific lengths, a high degree of large articles. Furthermore, the composition does not require
fibrillation and a high water retention capacity. These com excessive energy to produce and is therefore economically
position may be subsequently moulded and dried to produce viable.
finished wood-like or horn-like articles of high strength and 0.052 Accordingly when molded and dried, the composi
which therefore can be used as load bearing products. tion can be used to create structural and industrial compo
0040. The composition comprise fibres having a length nents such as coffins, electronic housings, structural building
weighted average fibre length (“LWAFL) of 0.25 to 0.40 pillars, beams, boards, sheets, Veneers, boxes, chairs, cabi
mm, preferably 0.28 to 0.38 mm. The fibre lengths in the nets, cases and other furniture, car parts and toys.
US 2014/0352903A1 Dec. 4, 2014

0053. It will be appreciated that due to a variation in the TABLE 1


compositions of the raw materials in terms of for example,
lignin content, ash content, OH bonding capacity and degree Fibre length
of entanglement/fibrillation, as well as the choices of fibre Length Weighted Mass Weighted
processing parameters, the physical properties of the final Arithmetic Average Fibre Average Fibre
product produced from the composition will vary. For Fibre Length Length Length
example, the density may vary from 0.5 to 1.5 g/cm3, the (mm) (mm) (mm)
tensile modulus may vary from 3500 to 10800 MPa and the Sample (AFL) (LWAFL) (WWAFL)
tensile strength may vary from 27 to 115 MPa. A. O.25 0.37 O.47
B 0.27 O4O O.S4
EXAMPLES C O.26 O.39 O.49
D O.30 0.44 0.55
E O.25 O.36 O46
Fibre Furnish and Degree of Fibrillation F O.20 O.29 O41

0054 Five samples (A to E) based on waste paper,


RCW80 de-inked recovered waste paper from Amcor, and 0059. The results in Table 1 show that all samples (Ato F)
one sample (F) based on hemp cellulose, Hempcell B from contain extremely shortened fibres. The arithmetic average of
Celesa in Spain, were Subjected to grinding in a high consis
tency 22" refiner. The fibre (solids) content in the pulp was 16 the measured fibre lengths is skewed somewhat by the pres
wt % and the flow rate of pulp through the refiner was ence of fines (<0.2 mm). This can be mathematically cor
approximately 200 L/min. The specific energy (the amount of rected (reduced), by weighting the lengths and masses, i.e. by
energy transferred from the refiner's motor to the fibre) input referring to the LFAFL or WWAFL.
was for each of the Samples: 0060. In practice the length weighted average fibre length
(LFAFL) is typically used for the comparison offibrous mate
Sample A 1.8 kWh/kg rials with one another. From the values of the LFAFL for all
Sample B 1.8 kWh/kg Samples in Table 1, it can be seen that similar values are
Sample C 1.8 kWh/kg obtained for all Samples based on wastepaper (A to E) with a
Sample D 1.6 kWh/kg slightly shorter value for the Sample based on hemp cellulose
Sample E 2.0 kWh/kg
Sample F 1.9 kWh/kg (F).
0061. The results shown in Table 2 below are an evaluation
0055. The specific edge load (the amount of energy of the distribution of fibre lengths within certain length
applied across one meter of refiner plate's bar edge and trans ranges. The majority offibres of all six Samples (Ato F) after
ferred to the pulp in one second) was between 4-8 WS/m at the processing are 0.2-0.5 mm, which is considered to be the
beginning of the refining process and this load was gradually short fibre or fibre fragment range. This is also shown graphi
reduced to between 1-4 WS/m by the end of the process. cally in FIGS. 8-13. Each of these Figures (for respective
0056. The fibres were processed until the spread of the samples) contains two graphs. The top graph in each of FIGS.
average fibre length matched a known “bell curve'. From 8-13 shows the distribution of fibres having lengths of <0.06
experience and knowing the process inputs, this occurs after mm whilst the lower graph in each of these Figures shows the
a certain time period of processing. However, the fibres may distribution of fibres having lengths of >0.1 mm.
be sampled to confirm that they have this distribution of fibre
lengths. TABLE 2
0057. A light microscope and a Norval Wilson stain was Distribution of fibre lengths (length weighted
used on the prepared slides containing dispersed fibre average length in length ranges) by weight%
samples and images were taken of each sample as depicted in O.OO1-0.2 0.2-0.5 0.5-1.2 1.2-2.O 20-32 3.2-7.6
FIGS. 2 to 7. As can been seen from these Figures, a high l l ill ill ill ill
degree offibrillation is observed for the six samples and most Sample A 22.8% 54.1%. 23.1% 0.1% O.0% O.0%
of the fibres were broken or cut into very small fragments. Sample B 19.3% 51.0%. 29.1% 0.3% O.2% O.1%
Sample C 19.1% 53.1%. 27.8% 0.0% O.0% O.0%
Suspension Properties: Morphological Properties as Well as Sample D 15.2% 48.7%. 35.8% 0.3% O.0% O.0%
Sample E 22.5% SS.6%. 21.8% 0.2% O.0% O.0%
Resistance to Dehydration and Swelling Behaviour Sample F 33.2% 57.29% 9.3% 0.2% O.1% O.0%
0058 0.2 g (dry weight) of each Sample A-F after the
grinding process described above were strongly diluted by The fines content of the ground samples were investigated
pre-suspending in water, stirring, and Subsequently filling
with water to 5000 ml. From this suspension, 25 ml were further by determining the fraction of the fines (fibres <0.2
taken (corresponding to 1.0 mg (dry weight) fibrous material) mm) in each Sample based on the arithmetic average fibre
and photographed. The photographs were Subsequently length (AFL). This fraction for each Sample is compared to
analysed (double determination) using FibreLab 3.0" equip the length weighted fraction offines (as per Table 2) is shown
ment to determine the fibre-morphological properties and in Table 3 below. As can be seen from Table 3, the fines
distribution parameters for the separated and Suspended content of all Samples (A to F) is very high. The hemp
fibres, including the fibre length. The results for fibre length cellulose Sample F, notably contained markedly more fine
are provided in Table 1 below. material than the wastepaper samples (A to E).
US 2014/0352903A1 Dec. 4, 2014

TABLE 3 able, strongly ground celluloses. The higher WRC generally


Fine material contents
equates to a denser material which when moulded and dried
into a final product results in a product which has a lower tear
Fine material (<0.2 mm) Fine material (<0.2 mm) or tensile strength but a higher load bearing capacity and
(arithmetic average) (length weighted average) Young's modulus. A preferred range for Water Retention
Sample % % Capacity is generally between 700 and 1200% as above this
A. 49.4 22.8 range, the low tear strength makes it difficult to form sheets—
B
C
45.0
45.7
19.3
19.1
as was found with Sample C.
D 38.7 15.2
E 47.3 22.5 Material Properties: Physical/Strength Properties
F 57.3 33.2

0.066 Samples A to F were ground as described above and


0062. Further measurements of the diameter, wall thick mixed with water in a mixer to a solids concentration in the
ness and calculated (curvature) parameters using the Fibrelab range between 0.3 and 0.4 wt % (3 to 4 g/L) as per Table 8
equipment show that samples A to E derived from wastepaper below.
have similar values whereas sample F derived from hemp
cellulose has Smaller fibre dimensions and a smaller curva TABLE 8
ture. This result corresponds with the fibre lengths deter
mined as well as with the fibre fragments present. Sample A. B C D E F

TABLE 4
Solids Concentra- wt % 0.367 O.379 0.351 O.379 0.354 0.351
Further fibre data tion in the mixer

Fibre width Fibre wall thickness Fibre curvature


Sample In In %
A. 16.5 3.8 17.9 0067. The objective was to produce test sheets with an
B 16.2 3.8 18.1 average grammage of m of 80+2 g/m, for use in Subsequent
C 16.4 3.8 17.3 strength testing according to the Rapid-Köthen method (in
D 17.0 4.1 19.3
E 17.0 4.0 18.0 accordance with ISO 5269-2). It is noted that due to the very
F 13.9 3.3 16.2 low dehydration capability of all of the Samples, the ISO
5269-2 test specifications had to be adapted by reducing the
volume of filling water in the cylinder and varying the period
Determination of the Water Retention Capacity (WRC) of drop and Suction to Suit the required conditions for sheet
According to Zellcheming Fact Sheet IV/33/57 forming for each of Samples A to F.
0063 All Samples A to F (after grinding described above) 0068. After producing the test sheets for each of the
were homogenised by mixing prior to sampling for determi Samples, the test sheets were acclimatised in Standard climate
nation of their Water Retention Capacity (WRC). conditions (23 C./50% relative air humidity).
0064. The Samples of fibrous material were dehydrated 0069. The grammage of the acclimatised test sheets was
(to a solids content of approximately 25 wt %) on a G2 frit in ten determined according to DIN EN ISO 536. The results of
the absence of a vacuum and transferred to a swell tube the grammage testing are shown in Table 9.
(according to DIN 53814). The swell tube was filled to
approximately two-thirds capacity (resulting in a solids con TABLE 9
tent of approximately 0.150 wt %). The swell tube was sealed
with a plug and subjected to a centrifugal force of 3000 g for Sample Grammage
15 minutes. Six parallel determinations were performed. Sample A. B C D E F
0065. The water not participating in the swelling of the
fibres was removed from the fibrous material by the centrifu Grammage g/m 79.3 81.2 74.4 81.0 78.5 77.6
gation. The Swelling water and the water retention capacity
were gravimetrically determined by drying the fibrous mate
rial at 105° C. until a constant mass solids content was 0070. Due to the characteristics of the materials it was very
achieved. The results are shown in Table 5. difficult to produce test sheets with uniform grammage. This
was especially the case of sample C wherein the targeted
TABLE 5 value (80+2 g/m) could not be realised despite repeated
Water Retention Capacity corrections. This is due to the very high Water Retention
Capacity (WRC) of the Samples. In order to compensate for
Sample A. B C D E F the non-uniformity in grammage between the test sheets, the
Water Reten- % 841 742 1532 774 1138 1052 strength values have been corrected with respect to gram
tion Capacity mage.
0071. The test sheets were subjected to thickness and
The values of the water retention capacity are extremely high apparent sheet density testing, the results of which are shown
and atypical particularly compared to commercially avail in Table 10.
US 2014/0352903A1 Dec. 4, 2014

TABLE 10 to express language or necessary implication, the word "com


prise' or variations such as “comprises' or "comprising is
Sheet thickness and apparent sheet density used in an inclusive sense, i.e. to specify the presence of the
Sample A. B C D E F stated features but not to preclude the presence or addition of
further features in various embodiments.
Thickness In 84 88 78 89 8O 81 0079. It is to be understood that, if any prior art publication
Apparent sheet gicm3 O.94 O.92 O.95 0.91 O.98 0.96
density is referred to herein, such reference does not constitute an
admission that the publication forms part of the common
general knowledge in the art, in Australia or any other coun
0072 By virtue of the high proportion of very short, fine try.
fibres, the thickness at the grammage strived for was Small 1. A cellulosic composition comprising fibres having
and the density very high. This corresponds to the normal length weighted average fibre length (“LWAFL) of 0.25 0.40
behaviour at high packing densities that are achieved with .
very short fibres.
0073. The test sheets were subjected to tensile testing 2. The cellulosic composition as claimed in claim 1, the
according to DIN EN ISO 1924-2, the results of which are composition comprising, by weight:
shown in Table 11 below. (a) 15% to 25% fibres of a length weighted average fibre
0074 The values for breaking force, elongation, breaking length of 0.001 mm to 0.2 mm:
length and Young's modulus determined from this testing are (b) 40% to 60% fibres of a length weighted average fibre
not corrected with respect to the grammage, but are corrected length of 0.2 mm to 0.5 mm;
with respect to the breaking length (represented as the Tensile (c) 8% to 35% fibres of a length weighted average fibre
Index): length of 0.5 mm to 1.2 and
TABLE 11
Tensile test results

Sample A. B C D E F

Breaking force N 81.1 85.5 71.8 84.3 74.5 77.5


Elongation % 3.0 3.0 2.2 3.3 2.3 3.5
Breaking length l 7050 7250 6SOO 7100 6SOO 67OO
Tensile Index Nmig 69.1 71.O 63.7 69.7 63.7 65.9
Young's modulus GPa. 7.85 7.77 7.88 7.48 7.92 7.92

0075. From the results in Table 11, the tensile strength, (d) less than 3% fibres of a length weighted average fibre
expressed as tensile index, corresponds to that of ground length of 1.2 mm to 2.0 mm.
cellulose. Whilst the tensile strength values for the Samples 3. A cellulosic composition comprising, by weight:
differ, there is little variation in the Young's modulus of the (a) 15% to 25% fibres of a length weighted average fibre
Samples which is high. The high Young's modulus of each of length of 0.001 mm to 0.2 mm:
the Samples is indicative that the Samples can withstand (b) 40% to 60% fibres of a length weighted average fibre
tensile loads elastically for long periods of time. Without length of 0.2 mm to 0.5 mm;
wishing to be bound by theory, it is expected that this is due to (c) 8% to 35% fibres of a length weighted average fibre
the high amount offibrillation of the fibres and the subsequent length of 0.5 mm to 1.2 and
linkages between the fibrillated fibres.
0076. The test sheets were cut into strips and subjected to (d) less than 3% fibres of a length weighted average fibre
tear resistance testing according to DIN EN 21974. The length of 1.2 mm to 2.0 mm.
results are shown in Table 12. The resistance to tearing is not 4. The cellulosic composition as claimed in claim 1,
corrected according to the grammage, only according to the wherein the composition has a Water Retention Value (WRV)
tear index. of 600% to 2000%.
TABLE 12
Tear Resistance

Sample A. B C D E

Tear resistance (E) mN 222 28O 181 294 195 215


Tear index Mn m/g 2.67 3.41 2.46 3.62 2.55 2.80

0077. The tearing strength of all samples, measured on 5. The cellulosic composition as claimed in claim 1,
“standard” celluloses, is at a very low level, i.e. the resistance wherein the composition comprises, by weight:
to tear is low. This can be attributed primarily to very short (a) 15% to 25% fibres of a length weighted average fibre
fibres. length of 0.001 mm to 0.2 mm:
0078. In the claim which follows and in the preceding (b) 45% to 55% fibres of an a length weighted average fibre
description, except where the context requires otherwise due length of 0.2 mm to 0.5 mm;
US 2014/0352903A1 Dec. 4, 2014

(c) 20% to about 30% fibres of a length weighted average 10. The cellulosic composition as claimed in claim 1,
fibre length of 0.5 mm to 1.2 mm and wherein components of the composition are prepared sepa
(d) less than 1% fibres of a length weighted average fibre rately and mixed together.
length of 1.2 mm to 2.0 mm. 11. The cellulosic composition as claimed in claim 10,
6. The cellulosic composition as claimed in claim 1, wherein two or more intermediary compositions with differ
wherein the cellulosic composition is in the form of pellets, ent fibre length distributions are prepared and mixed in the
granules or powder. required proportions to form the composition.
7. The cellulosic composition as claimed in claim 1, 12. The cellulosic composition as claimed in claim 1,
wherein the composition also comprises one or more func wherein the raw material used in the preparation of the com
tional additives. positions comprises one or more of short/ultra short cellulose
8. The cellulosic composition as claimed in claim 7. fibres/fines recovered from waste streams, recovered paper,
wherein the functional additives are selected from dyes and recovered fines in Whitewater from paper & pulp processing
pigments for colouring, resins and waxes for waterproofing, and recovered cotton fibres, any cellulosic fibres used in pulp
lime, fire retardants including natron, silicate, glues, metal & paper processing and plant fibres having a high cellulosic
powders and graphites for electrical conductivity, latex for content such as hemp, flax, cotton, abaca, sisal and jute.
flex and waterproofing, fillers and very long fibres of 1.5-6.0 13. A product made from a composition as claimed in claim
mm in length for increased tensile strength. 1.
9. The cellulosic composition as claimed in claim 1, 14. The product as claimed in claim 13, wherein the density
wherein the composition is prepared by any one or combina of the product is from 0.5 g/cm3 to 1.5 g/cm3.
tion of processing methods including ultra friction grinding, 15. The product as claimed in claim 13, wherein the tensile
high pressure homogenizing, cryo grinding, extrusion, Steam modulus of the product is from 3500 MPa to 10800 MPa.
explosion, ultra Sonic treatment, enzyme-fibre separation, 16. The product as claimed in claim 13, wherein the tensile
high consistency/medium consistency/low consistency refin strength of the product is from 27 MPa to 115 MPa.
ing, chemical treatment or Whitewater fines recovery. k k k k k

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