[0001] The present invention relates to strong as-spun discontinuous polyethylene fibres,
especially strong discontinuous plexifilamentary film-fibril strands formed directly
from fibre-forming polyethylene. Such as-spun discontinuous fibres may be formed in
a flash spinning process.
[0002] As used herein, "discontinuous" means that the strands have a length of not more
than 100 mm.
[0003] As used herein, "plexifilamentary film-fibril strands of polyethylene" means strands
which are characterized as a three dimensional integral network of a multitude of
thin, ribbon-like film-like elements of random length and of a thickness in the range
of about 1-20 µm, with an average thickness of less than about 10 µm, generally coextensively
aligned with the longitudinal axis of the strand. The film-fibril elements intermittently
unite and separate at irregular intervals in various places throughout the length,
width and thickness of the strand to form the three dimensional network. Such strands
are known, being described in further detail in Blades and White, US-A-3 081 519.
[0004] Blades and White describe a flash-spinning process for producing continuous plexifilamentary
film-fibril strands from fibre-forming polymers. A solution of polymer in a liquid
that is a non-solvent for the polymer at or below its normal boiling point, is extruded
at a temperature above the normal boiling point of the liquid and at autogenous or
higher pressure through a spinneret into a medium of lower temperature and substantially
lower pressure. This flash spinning causes the liquid to vaporize and form a continuous
plexifilamentary film-fibril strand. Commercial spunbonded products have been made
from polyethylene plexifilamentary film-fibril strands obtained by flash-spinning
using trichlorofluoromethane as solvent, but that halocarbon has been implicated in
the depletion of the earth's ozone.
[0005] It is known that the spinneret and tunnel used in flash spinning a polymer solution
are important with respect to properties of flash spun continuous fibres, e.g. tenacity
and elongation to break. For instance, US-A-4 352 650 discusses optimization of the
tunnel for increasing fibre tenacity e.g. from 3.7 to 4.6 cN/dtex (4.2 to 5.2 grams/denier),
of flash spun continuous fibres. In general, fibre tenacity can be increased by as
much as 1.3 to 1.7 times by using a tunnel at the exit to the spinneret. Various methods
for making discrete fibres are known e.g. as discussed in the copending patent application
now EP-A-0 597 658 filed concurrently herewith.
[0006] US-A-5 043 108 discloses flash spinning of a mixture of organic solvent, polyethylene
and a non-solvent or spin aid, especially water or an alcohol, or mixtures thereof,
in which the amount of water is less than the saturation limit of water in the organic
solvent, to produce continuous as-spun fibres. A process for the manufacture of a
polyolefin pulp in which strands are formed and shredded is disclosed in US-A-5 093
060. However, while it is possible to produce continuous filaments using a flash spinning
process and to subsequently shred the continuous filaments by mechanical means to
form discontinuous filaments, such mechanical shredding tends to fuse the ends of
the shredded filaments, even if the shredding is carried out under water. Fused ends
make it difficult or impossible to open up the resultant web of fibres, as well as
reducing fibre orientation and strength. For these reasons, processes that produce
discontinuous fibres without requiring use of mechanical shredding means would be
preferred.
[0007] While a variety of discrete fibres have been produced, discrete fibres of improved
properties are still required. Improved discontinuous as-spun plexifilamentary film-fibril
strands, especially fine, strong, oriented and discontinuous fibrils, and polyethylene
pulp have now been found.
[0008] Accordingly, the present invention provides fine, strong, as-spun discontinuous fibres
formed from polyethylene, said fibres having a length of 1-25 mm, a fibre diameter
of less than 30 µm and a handsheet zero span strength of greater than 29.4 N/15 mm
(3 kg/15 mm).
[0009] In a preferred embodiment of the fibres of the present invention, the handsheet zero
span strength is greater than 58.8 N/15 mm (6 kg/15 mm).
[0010] The present invention also provides a polyethylene pulp formed from as-spun discontinuous
fibres having a surface area of greater than 4 m
2/g, a Pulmac defect value of less than 3%, a handsheet zero span value of at least
29.4 N/15 mm (3 kg/15 mm) and with the fibres of the pulp having a Kajaani coarseness
of less than 0.30 mg/m.
[0011] In a preferred embodiment of the pulp of the present invention, the pulp has a Pulmac
defect value of less than 2%.
[0012] In another embodiment, the fibre length in the pulp is less than 2 mm and with an
average length in the range of 0.80-1.20 mm.
[0013] In a further embodiment, the fibres have a fineness such that the fibres have a Kajaani
coarseness of less than 0.20 mg/m.
[0014] In yet another embodiment, the pulp has a surface area in the range of 6-8 m
2/g.
[0015] In embodiments of the fibre and of the pulp, the polyethylene has a melt index of
less than 15 dg/min, especially less than 7 dg/min and in particular less than 2 dg/min.
[0016] The measurements of handsheet zero span strength and surface area are described below.
[0017] The fibre is in the form of plexifilamentary film-fibrils in a discontinuous form.
The average length of the fibre is in the range of 1-25 mm. The fibres of the present
invention have a handsheet zero span strength of greater than 29.4 N/15 mm (3 kg/15
mm) and especially greater than 58.8 N/15 mm (6 kg/15 mm).
[0018] The diameter of the fibre is less than 30 µm and more particularly less than 20 µm.
The fibres are referred to as "as-spun" fibres, which have "free" ends in contrast
to the fused ends that tend to result from mechanical cutting of polyethylene fibres,
especially at commercial rates. The as-spun fibres are characterized by an absence
of fused ends. This freeness of the fibres contributes to improved processing of the
fibres, which usually includes a step of opening up of the fibres or separation of
fibre bundles into individual fibres.
[0019] The fibres of the present invention are short fibres, in comparison to the fibres
produced in the aforementioned Blades and White and Samuels processes.
[0020] The fibres of the present invention may be manufactured in a flash spinning process,
particular examples of which are described in the aforementioned copending European
patent application. In such an embodiment of a process of manufacture, polyolefin
is dissolved in an organic solvent. The polyolefin may be in the form of pellets or
powder, or other forms known in the art, having been previously polymerized from monomers.
Alternatively, the polyolefin is already dissolved in an organic solvent e.g. it is
a solution of polymer in organic solvent from a process for the polymerization of
monomers.
[0021] The polyethylene used in the present invention may be a high molecular weight homopolymer
of ethylene or copolymer of ethylene and at least one C
4-C
10 hydrocarbon alpha-olefin e.g. butene-1, hexene-1 and/or octene-1. A wide variety
of such polymers, including by type of monomer(s) used, molecular weight, molecular
weight distribution and other properties are commercially available. In preferred
embodiments in which the polyethylene is a homopolymer of ethylene or copolymer of
ethylene and at least one C
4-C
10 hydrocarbon alpha-olefin, the density is in the range of 0.930 to 0.965 g/cm
3, especially in the range of 0.940 to 0.960 g/cm
3. The melt index of the polyolefin is preferably less than 15 dg/min i.e. in the range
of from so-called "no-flow" e.g. less than about 0.01 dg/min, to 15 dg/min, especially
in the range of 0.50 to 7.0 dg/min; melt index is measured by the method of ASTM D-1238
(condition E).
[0022] A variety of organic solvents may be used in the process, examples of which include
pentane, hexane, cyclohexane, heptane, octane, methyl cyclohexane and hydrogenated
naphtha, and related hydrocarbon solvents, and mixtures of solvents.
[0023] The polyethylene may contain additives e.g. antioxidants, ultra violet stabilizers,
wetting agents, surfactants and other additives known for use in polyolefins, provided
that the additives are capable of passing through the orifice used in the process
and not otherwise adversely affecting the process.
[0024] The solution of polyethylene in organic solvent is at an elevated temperature and
pressure, the solution being at a pressure that is at least the autogenous pressure
and at a temperature sufficient to maintain the polyolefin in solution. In preferred
embodiments, the solution also contains a non-solvent e.g. water, as a spinning aid,
as described in the aforementioned patent of Samuels. The spinning aid may contain
wetting agents, surfactants or the like. The temperature and pressure used, and the
composition of the solution especially the percent of polymer in the solution, affect
the properties of the film-fibril strands obtained on spinning and consequently the
fibrous material subsequently formed in the process. For instance, the temperature,
pressure and solution composition may be selected so that highly oriented fibres are
obtained, such fibres being preferred.
[0025] The solution is fed through a feed section to a spinneret exit to form plexifilamentary
film-fibril strands, the strands being formed as the polymer solution passes from
the spinneret exit. A mixture of steam and water is contacted with the solution passing
from spinneret exit substantially simultaneously with the passage of the solution
from the spinneret exit. The mixture of steam and water may be fed as a stream to
the tunnel or, preferably, a stream of hot high pressure water is flashed through
an orifice into the tunnel, where the mixture of steam and water is formed. The temperature
and pressure of the stream are selected so as to produce the required ratio of steam
to water in the tunnel.
[0026] In a preferred embodiment, the ratio of steam to water is in the range of 20:80 to
80:20 on a weight basis, especially in the range of 35:65 to 65:35. The temperature
of the inert fluid is 2-40°C lower than the melting point of the polymer.
[0027] It is to be understood that the surfaces of pipes, vessels and the like used should
be free of snag points or other obstructions that might prevent or retard the passage
of the film-fibrils or fibrous material.
[0028] The fibre may be converted to a polyethylene pulp, which has a variety of uses. For
instance, the pulp may be used as part of blends with cellulose for use in e.g. diapers,
disposable wipes, feminine hygiene products and incontinence products, as a filler
e.g. in polymers, cement and the like, thixotropic agent in paints and as synthetic
paper. In some end-uses, fibres especially longer fibres with lengths in the range
of about 5-25 mm, may be used, without refining, to produce sheet structures using
either wet-lay or air-lay sheet forming technologies.
[0029] Pulp may be obtained by feeding the fibres to a refining process that reduces the
length of the fibres to less than 2 mm and with an average length in the range of
0.80-1.20 mm as well as opening up the fibre structure. The fibres are fed to the
refiner in the form of a slurry e.g. about 2% by weight, with polyvinyl alcohol added
as surfactant; other surfactants may be used in combination with or instead of polyvinyl
alcohol. The fibres must be of a length of not more than about 10 mm, preferably with
an average length of about 6 mm in order to produce an acceptable slurry. The refining
process may be carried out in a pulp and paper-type refiner. Suitable refiners include
single disk, twin-flow and conical refiners.
[0030] Synthetic pulp is synthetic fibre having a very short length. As used herein, the
fibre in the pulp preferably has an length of less than 2 mm, an average length in
the range of 0.8-1.2 mm, and preferably about 1 mm. In addition, the fibre in the
pulp has a surface area of greater than 4 m
2/g, especially than 6 m
2/g and in particular in the range of 6-8 m
2/g. Pulp fibres have a handsheet zero span value of at least 29.4 N/15 mm (3 kg/15
mm), especially at least 49 N/15 mm (5 kg/15 mm). In use, it is preferred that the
pulp have a low percentage of long fibres and a low percentage of agglomerates. Long
fibres are measured by Clark 14 mesh, and acceptable values are less than 12% and
especially less than 7%. Agglomerates are measured by Pulmac defects, and acceptable
values are less than 3% and especially less than 2%. The fineness of the fibres may
be characterized using, a coarseness test viz. the Kajaani test. As used herein "fine
fibres" have a coarseness of less than 0.3 mg/m and preferably less than 0.2 mg/m.
[0031] In the examples, the following test methods were used:
Handsheet zero span is a measurement of fibre strength, and is obtained using the
procedures of TAPPI T205 om on a Pulmac Troubleshooter, using the method suggested
by the manufacturer. Handsheets with a basis weight of 60 g/m2 are made in a handsheet mould, by forming a slurry of fibres in water and then depositing
the fibres on a screen using vacuum. Handsheet zero span is the force required to
break a strip measuring 2.54 cm x 10 cm, using a jaw width of 15 mm and a jaw separation
of 0 mm. The results are expressed in N/15 mm (kg/15 mm);
Surface area is a measure of the degree of fineness and fibrillation of the product,
and is measured by the Strohlein nitrogen adsorption method. Nitrogen is adsorbed
on the fibres at liquid nitrogen temperature. The amount adsorbed is measured as a
pressure difference between sample and reference flask. Because of the small size
of nitrogen molecules, small differences in surfaces can be detected. In effect, the
method is a one-point measurement using the principles of the BET nitrogen adsorption
of S. Brunauer, P.H. Emmett and E. Teller, J. Amer. Chem. Soc., vol 60, p 309-319
(1938). The results are reported in m2/g;
Linear Shrinkage is measured by immersion of fibre bundles in ethylene glycol at 155°C
for 5 seconds, and is expressed as the ratio of the initial length to the shrunken
length. Linear shrinkage is an indication of the orientation imparted to the fibres
during the spinning process;
Average fibre length and coarseness was measured using Kajaani apparatus in which
a very dilute slurry of fibres in distilled water is drawn through a small orifice
using a vacuum. The length and size of the fibres are detected by a diode array detector
as the fibres pass through the orifice. A distribution of fibre lengths and sizes
is obtained. For unrefined samples, where the fiber length is greater than 2 mm, a
very dilute slurry of 0.0078g of fibre in water is prepared, deposited onto a screen
and then pressed into a plastic slide measuring 12.7 x 12.7 cm; a visual estimate
of the length distribution and average length of the sample is then made;
A Clark classifier is used to measure the proportion of long fibres (mostly longer
than 2 mm) in a sample;
samples that have not been refined completely will have unacceptably high Clark values
e.g. greater than 12%. The procedure used is TAPPI T233 os and TAPPI T261 pm. Fibres
are dispersed in water, and then circulated through a series of different mesh screens.
For refined fibres, only the amount collected on the 14 Mesh screen (1.19 mm openings)
is reported; and
Pulmac defects is a measure of agglomeration in which a slurry is passed through a
slot opening that is 0.1 mm or 0.15 mm wide at a given flow rate. The fibres or agglomerates
which do not make it through the slot after two passes are considered defects.
[0032] The present invention is illustrated by the following examples.
Example I
[0033] Fibrous material was manufactured using semi-works scale apparatus equipped with
a spinneret and die having a venturi tunnel, such a tunnel being shown in Fig. 1 of
the aforementioned EP-A-0 597 658. The solution of polymer fed to the spinneret was
a solution of ethylene/butene-1 copolymer dissolved in cyclohexane and containing
7% (w/w) of water as a spin aid. Water was introduced at high temperature and pressure
into the zone immediately adjacent the spinneret so that a mixture of steam and water
contacted the fibres exiting from the spinneret.
[0034] In the spinning vessel, the product was in the form of a slurry of fibres in water
at a 0.5% consistency (w/w). The fibre slurry was conveyed, using a water-driven venturi,
through a large smooth pipe to a vessel where live steam was injected to boil off
residual traces of cyclohexane. The slurry, free of solvent, was further conveyed,
using a water-driven venturi, through a large smooth pipe to a belt filter press where
water was removed. The product was collected in the form of a loose cake with an approximately
50% solids content.
[0035] Further details of the polymer used and the conditions in the flash spinning process
are given in Table I.
Table I
Run No. |
1 |
2 |
3 |
POLYMER PROPERTIES: |
|
|
|
Melt Index (dg/min) |
0.28 |
0.33 |
0.43 |
Density (g/cm3) |
0.937 |
0.942 |
0.958 |
SPINNING CONDITIONS: |
|
|
|
Solution Temperature (°C) |
249 |
232 |
237 |
Let-down Chamber Pressure (kPa) |
6690 |
6310 |
6345 |
Solution flow (kg/hr) |
291 |
315 |
225 |
Polymer in Solution (%) |
14.8 |
14.9 |
15.6 |
SPIN SHATTERING CONDITIONS: |
|
|
|
Water flow rate (kg/hr) |
220 |
210 |
240 |
Water temperature (°C) |
300 |
298 |
302 |
Water Pressure (kPa) |
10760 |
13730 |
10030 |
Water flashing to steam (%)* |
42 |
42 |
43 |
Water to polymer ratio (kg/kg) |
5.1 |
4.5 |
6.9 |
FIBRE PROPERTIES: |
|
|
|
Linear shrinkage |
10.5 |
10.5 |
10.1 |
Handsheet zero span N/15 mm (kg/15 mm) |
61.7 (6.3) |
79.4 (8.1) |
89.8 (9.0) |
Fibre lengths (mm) |
18-25 |
18-25 |
4-10 |
Note: Solution flow = polymer plus solvent
* - assumes that pressure in tunnel is 104 kPa and the temperature is 100°C |
[0036] In this example, polymers of low melt index i.e. high molecular weight, were spun
into discontinuous fibres. The fibres were all strongly oriented, with linear shrinkages
slightly above 10. Fibre length was in the range of 18-25 mm for Runs 1 and 2, in
which the melt index was 0.28 and 0.33 dg/min respectively. However, in Run 3 in which
the polymer melt index was higher viz. 0.43 dg/min, the fibre length was shorter,
generally below 10 mm.
[0037] The largest effect of increasing polymer density was an increase in fibre strength,
as measured by handsheet zero span. Handsheet zero span strength was 61.7 N/15 mm
(6.3 kg/15 mm) at a polymer density of 0.937 g/cm
3 (Run 1), 79.4 N/15 mm (8.1 kg/15 mm) at a polymer density of 0.942 g/cm
3 (Run 2) and 81.9 N/15 mm (9.0 kg/15 mm) at a polymer density of 0.958 g/cm
3 (Run 3).
[0038] The fibres of this example were strong and discontinuous, with combinations of the
unique properties described herein.
Example II
[0039] The procedure of Example I was repeated using polymers of differing melt index. Polymers
having a melt indices in the range of 0.79 to 7.6 dg/min were spun into fibres.
[0040] Further results are given in Table II.
Table II
Run No. |
4 |
5 |
6 |
7 |
8 |
POLYMER PROPERTIES: |
|
|
|
|
|
Melt Index (dg/min) |
0.79 |
1.16 |
1.90 |
3.8 |
7.6 |
Density (g/cm3) |
0.955 |
0.956 |
0.938 |
0.947 |
0.959 |
SPINNING CONDITIONS: |
|
|
|
|
|
Solution Temperature (°C) |
262 |
260 |
237 |
229 |
234 |
Let-down Chamber Pressure (kPa) |
7165 |
6675 |
8550 |
8080 |
8240 |
Solution flow (kg/hr) |
235 |
220 |
284 |
264 |
224 |
Polymer in Solution (%) |
15.4 |
15.4 |
14.9 |
16.9 |
20.1 |
SPIN SHATTERING CONDITIONS: |
|
|
|
|
|
Water rate (kg/hr) |
280 |
265 |
250 |
250 |
268 |
Water temperature (°C) |
299 |
300 |
301 |
302 |
299 |
Water Pressure (kPa) |
- |
10070 |
10000 |
9890 |
10510 |
Water flashing to steam (%)* |
42 |
42 |
42 |
43 |
42 |
Water to polymer ratio (kg/kg) |
7.8 |
7.8 |
6.0 |
5.6 |
6.0 |
FIBRE PROPERTIES: |
|
|
|
|
|
Linear shrinkage |
- |
9.9 |
- |
- |
- |
Handsheet zero span N/15 (kg/15 mm) |
83.3 (8.5) |
82.3 (8.4) |
45.5 (5.0) |
42.1 (4.3) |
37.2 (3.8) |
Fibre lengths (mm) |
2-8 |
2-6 |
1-4 |
1-4 |
1-3 |
Note: Solution flow = polymer plus solvent
* - assumes that pressure in tunnel is 104 kPa and the temperature is 100°C |
[0041] Polymer melt index (or polymer molecular weight) had an effect on both the fibre
length and fibre strength. All the fibres were strong and discontinuous, with the
unique combination of properties described herein.
[0042] For the polymer with the lowest melt index (0.79 dg/min, in Run 4), the individual
fibres lengths ranged from 2 to 8 mm. In contrast, for the polymer of highest melt
index (7.6 dg/min, in Run 8), the individual fibre lengths ranged from 1 to 3 mm.
Fibres with the lengths reported in this Example are short enough to be dispersed
into a slurry in a well agitated vessel, preferably a pulper, and refined to pulp
length. In contrast, some of the fibres obtained in Example 1 had lengths of up to
25 mm, which would be expected to cause entanglement problems in a pulping and refining
process.
[0043] Polymers with lower melt index (higher molecular weight) give fibres with higher
strength, as measured by handsheet zero span, than fibres with higher melt index.
The polymer with a melt index of 0.79 dg/min had a handsheet zero span of 83.3 N/15
mm (8.5 kg/15 mm) (Run 4), whereas the polymer with a melt index of 7.6 dg/min had
a handsheet zero span of less than half that value (Run 8). In Run 3 of Example I,
the polymer had the same density and a melt index of 0.42 dg/min; the handsheet zero
span was 89.8 N/15 mm (9.0 kg/15 mm).
Example III
[0044] The procedure of Example I was repeated, with the fibres obtained being refined to
a pulp length viz. approximately 1 mm.
[0045] Refining was conducted by first dispersing the fibres in water in an agitated tank,
at a fibre consistency of 1.5-2%. A surfactant (polyvinyl alcohol, 2% by weight of
fibres) was used in order to make the fibres more wettable. Two different single disk
refiners were used, with a 30 cm plate diameter in Runs 9 and 10 and with a one metre
plate diameter in Run 11. The plate gap setting was between 0.05 and 0.15 mm, with
the larger gap settings being used on the smaller refiner. The samples were refined
until the average fibre length was 1 mm.
[0046] Further details and the results obtained are given in Table III.
Table III
Run No. |
9 |
10 |
11 |
POLYMER PROPERTIES: |
|
|
|
Melt Index (dg/min) |
0.78 |
1 .04 |
7.5 |
Density (g/cm3) |
0.962 |
0.956 |
0.958 |
SPINNING CONDITIONS: |
|
|
|
Solution Temperature (oC) |
237 |
249 |
245 |
Let-down Chamber Pressure (kPa) |
7115 |
7320 |
8255 |
Solution flow (kg/hr) |
250 |
219 |
231 |
Polymer in Solution (%) |
15.4 |
15.1 |
19.0 |
SPIN SHATTERING CONDITIONS: |
|
|
|
Water rate (kg/hr) |
280 |
245 |
283 |
Water temperature (°C) |
300 |
301 |
302 |
Water Pressure (kPa) |
10855 |
9510 |
- |
Water flashing to steam (%) |
42 |
42 |
43 |
Water to polymer ratio (kg/kg) |
7.2 |
7.4 |
6.4 |
UNREFINED Fibre PROPERTIES: |
|
|
|
Linear shrinkage |
9.7 |
6.9 |
- |
Handsheet zero span N/15 mm (kg/15 mm) |
73.5 (7.5) |
72.5 (7.4) |
35.3 (3.6) |
Fibre lengks (mm) |
6-12 |
4-8 |
1-3 |
REFINED Fibre PROPERTIES: |
|
|
|
Average fibre length (mm) |
0.97 |
1.02 |
0.98 |
Average fibre coarseness (mg/m) |
0.171 |
0.219 |
0.26 |
Surface area (m2/g) |
6.22 |
6.61 |
5.97 |
Pulmac defects (%) |
0.2 |
0.9 |
1.2 |
Clark 14 mesh (%) |
1.1 |
1.8 |
1.4 |
Canadian standard freeness (ml) |
402 |
432 |
525 |
Handsheet zero span N/15 mm (kg/15 mm) |
55.9 (5.7) |
55.9 (5.7) |
30.4 (3.1) |
Note: Solution flow = polymer plus solvent
* - assumes that pressure in tunnel is 104 kPa and the temperature is 100°C |
[0047] This Example compares the properties of refined fibres (pulp) to the unrefined fibres.
Most applications of the fibres are expected to be in the form of pulp. In addition,
certain fibre properties cannot be measured on unrefined fibres.
[0048] The fibre samples were obtained by spinning high density polymers with varying melt
indices viz. from 0.78 to 7.5 dg/min. For Run 9, in which the melt index was 0.78
dg/min, the handsheet zero span for unrefined fibres was 73.5 N/15 mm (7.5 kg/15 mm)
and the individual fibre lengths ranged between 6 and 12 mm. For Run 11, in which
the melt index was 7.5 dg/min, the handsheet zero span was 35.3 N/15 mm (3.6 kg/15
mm) and the individual fibres lengths ranged between 1 and 3 mm.
[0049] The fibres were refined to an average length of 1 mm viz. 0.97 mm for Run 9, 1.02
mm for Run 10 and 0.98 mm for Run 11. The Pulmac defect test, which measures long
fibres and agglomerates, gave results of less than 2% for the fibres of all three
runs. The Clark 14 mesh test, which measures the proportion of long fibres, was also
less than 2% for all three runs.
[0050] Fibre strength as measured by the handsheet zero span test was lower for the refined
fibres than for the unrefined fibres. For the lower melt index polymer of Run 9, the
handsheet zero span decreased from 73.5 N/15 mm (7.5 kg/15) mm before refining to
55.9 N/15 mm (5.7 kg/15 mm) after refining. In Run 11, the decrease was from 35.3
to 30.4 N/15 mm (3.6 to 3.1 kg/15 mm). Nonetheless, fibre strength was still acceptable.
[0051] Fibre size and surface area are typically measured only on refined fibres, because
refining opens up the fibre structure. Average fibre coarseness as measured by the
Kajaani method increased with increasing melt index, from 0.171 mg/m in Run 9 to 0.260
in Run 11. This shows that finer, more oriented fibres may be obtained with lower
melt index polymers. Surface area measured by nitrogen adsorption was between 6 and
7 m
2/g for all three runs.
1. Fine, strong, as-spun discontinuous fibres formed from polyethylene, said fibres having
a length of 1-25 mm, a fibre diameter of less than 30 microns and a handsheet zero
span strength of greater than 29.4 N/15 mm (3 kg/15 mm) using the procedure of TAPPI
205 om.
2. The fibres of Claim 1 in which the handsheet zero span strength is greater than 58.8
N/15 mm (6 kg/15 mm) using the procedure of TAPPI 205 om.
3. The fibres of Claim 1 or Claim 2 in which the polyethylene has a melt index of less
than 15 dg/min.
4. The fibres of Claim 3 in which the melt index of the polyethylene is less than 7 dg/min.
5. The fibres of Claim 3 in which the melt index of the polyethylene is less than 2 dg/min.
6. The fibres of any one of Claims 1-5 in which the polyethylene is a high molecular
weight homopolymer of ethylene or copolymer of ethylene and at least one C4-C10 hydrocarbon alpha-olefin.
7. The fibres of Claim 6 in which the polyethylene is a copolymer and the alpha-olefin
is selected from butene-1, hexene-1 and octene-1, and mixtures thereof.
8. The fibres of Claim 6 in which the density of the polyethylene is in the range of
0.930 to 0.965 g/cm3.
9. The fibres of Claim 8 in which the melt index of the polyolefin is less than 15 dg/min.
10. A polyethylene pulp formed from the fibres claimed in any one of claims 1 to 9, the
fibres in the pulp having a surface area of greater than 4 m2/g, a Pulmac defect value of less than 3%, a handsheet zero span value of at least
29.4 N/15 mm (3 kg/15 mm) using the procedure of TAPPI 205 om and with the fibres
of the pulp having a Kajaani coarseness of less than 0.30 mg/m.
11. The polyethylene pulp of Claim 10 in which the Pulmac defect value is less than 2%.
12. The polyethylene pulp of Claim 10 or Claim 11 in which the fibre length is less than
2 mm and with an average length in the range of 0.80-1.20 mm.
13. The polyethylene pulp of any one of Claims 10-12 in which the pulp has a surface area
in the range of 6-8 m2/g.
14. The polyethylene pulp of any one of Claims 10-13 in which the fibres have a fineness
such that the fibres have a Kajaani coarseness of less than 0.20 mg/m.
15. A polyethylene sheet formed from the pulp as claimed in any one of claims 10 to 14.
16. A polyethylene sheet formed from strong discontinuous fibres of any one of Claims
1-9.
17. A sheet of Claim 16 in which the fibres have lengths in the range of 5-25 mm.
18. A sheet of Claim 16 or Claim 17 which is an air-laid sheet.
19. A sheet of Claim 16 or Claim 17 which is a wet-laid sheet.
1. Feine, feste, als Nichtendlosfasern gesponnene Fasern, die aus Polyethylen gebildet
sind, wobei die Fasern eine Länge von 1-25 mm, einen Faserdurchmesser von weniger
als 30 µm und -- nach der Vorschrift gemäß TAPPI 205 om bestimmt -- eine Nullabstandsfestigkeit
eines Handblatts von mehr als 29,4 N/15 mm (3 kg/15 mm) aufweisen.
2. Fasern nach Anspruch 1, bei denen die Nullabstandsfestigkeit eines Handblatts - nach
der Vorschrift gemäß TAPPI 205 om bestimmt - größer als 58,8 N/15 mm (6 kg/15 mm)
ist.
3. Fasern nach Anspruch 1 oder 2, bei denen das Polyethylen einen Schmelzindex von weniger
als 15 dg/min aufweist.
4. Fasern nach Anspruch 3, bei denen der Schmelzindex des Polyethylens niedriger als
7 dg/min ist.
5. Fasern nach Anspruch 3, bei denen der Schmelzindex des Polyethylens niedriger als
2 dg/min ist.
6. Fasern nach einem der Ansprüche 1 bis 5, bei denen das Polyethylen ein hochmolekulares
Homopolymer von Ethylen oder ein Copolymer von Ethylen mit zumindest einem C4-C10-Kohlenwasserstoff-α-Olefin ist.
7. Fasern nach Anspruch 6, bei denen das Polyethylen ein Copolymer ist und das α-Olefin
aus Buten-1, Hexen-1 und Octen-1 sowie Gemischen davon angewählt ist.
8. Fasern nach Anspruch 6, bei denen die Dichte des Polyethylens im Bereich von 0,930
bis 0,965 g/cm3 liegt.
9. Fasern nach Anspruch 8, bei denen der Schmelzindex des Polyolefins niedriger als 15
dg/min ist.
10. Aus den Fasern nach einem der Ansprüche 1 bis 9 gebildete Polyethylenpulpe, wobei
die Fasern in der Pulpe eine Oberfläche von mehr als 4 m2/g, eine Pulmac-Abweichung von weniger als 3%, eine Nullabstandsfestigkeit eines Handblatts,
nach der Vorschrift gemäß TAPPI 205 om bestimmt, von zumindest 29,4 N/15 mm (3 kg/15
mm) aufweisen, und wobei die Fasern der Pulpe eine Kajaani-Grobfasrigkeit von weniger
als 0,30 mg/m aufweisen.
11. Polyethylenpulpe nach Anspruch 10, bei dem die Pulmac-Abweichung geringer als 2% ist.
12. Polyethylenpulpe nach Anspruch 10 oder 11, bei der die Faserlänge geringer als 2 mm
ist, wobei die durchschnittliche Länge im Bereich von 0,80-1,20 mm liegt.
13. Polyethylenpulpe nach einem der Ansprüche 10 bis 12, bei der der Pulpe eine Oberfläche
im Bereich von 6-8 m2/g aufweist.
14. Polyethylenpulpe nach einem der Ansprüche 10 bis 13, bei der die Fasern eine solche
Feinheit aufweisen, daß die Fasern eine Kajaani-Grobfasrigkeit von weniger als 0,20
mg/m aufweisen.
15. Aus der Pulpe nach einem der Ansprüche 10 bis 14 gebildetes Bahn- bzw. Blattmaterial
aus Polyethylen.
16. Aus festen, unterbrochenen Fasern nach einem der Ansprüche 1 bis 9 gebildetes Bahn-
bzw. Blattmaterial aus Polyethylen.
17. Bahn- bzw. Blattmaterial nach Anspruch 16, bei der die Fasern Längen im Bereich von
5 bis 25 mm aufweisen.
18. Bahn- bzw. Blattmaterial nach Anspruch 16 oder 17, das ein nach einem Lufttransportverfahren
gelegtes Material ist.
19. Bahn- bzw. Blattmaterial nach Anspruch 16 oder 17, das ein nach einem Naßverfahren
gelegtes Material ist.
1. Fibres fines, résistantes, discontinues telles que filées formées de polyéthylène,
lesdites fibres ayant une longueur de 1-25 mm, un diamètre de la fibre de moins de
30 microns et une résistance à écartement zéro d'une feuille d'une main de plus de
29,4 N/15 mm (3 kg/15 mm) en utilisant le processus de TAPPI 205 om.
2. Les fibres de la revendication 1 dans lesquelles la résistance à l'écartement zéro
d'une feuille d'une main est plus grande que 58,8 (N/15 mn) (6 kg/15 mn).
3. Les fibres de la revendication 1 ou de la revendication 2 dans lesquelles le polyéthylène
a un indice de fusion de moins de 15 dg/mn.
4. Les fibres de la revendication 3 dans lesquelles l'indice de fusion polyéthylène est
inférieur à 7 dg/mn.
5. Les fibres de la revendication 3 dans lesquelles l'indice de fusion du polyéthylène
est inférieur à 2 dg/mn.
6. Les fibres selon l'une quelconque des revendications 1-5 dans lesquelles le polyéthylène
est un homopolymère de fort poids moléculaire d'éthylène ou un copolymère d'éthylène
et d'au moins une hydrocarbure d'alpha-oléfine C4-C10.
7. Les fibres de la revendication 6 dans lesquelles le polyéthylène est un copolymère
et l'alpha-oléfine est sélectionnée parmi le butène-1, l'hexène-1 et l'octène-1, et
leurs mélanges.
8. Les fibres de la revendication 6 dans lesquelles la densité du polyéthylène est comprise
entre 0,930 et 0,965 g/cm3.
9. Les fibres de la revendication 8 dans lesquelles l'indice de fusion de la polyoléfine
est inférieur à 15 dg/mn.
10. Une pâte de polyéthylène formée de fibres selon l'une quelconque des revendications
1 à 9, les fibres dans la pâte ayant une aire superficielle de plus de 4 m2/g, une valeur de défaut Pulmac de moins de 3%, une valeur à écartement zéro d'une
feuille d'une main de 29,4 N/15 mn (3 kg/15 mn) en utilisant le processus de TAPPI
205 om et avec les fibres de la pâte ayant une rugosité de Kajaani de moins de 0,30
mg/m.
11. Pâte de polyéthylène de la revendication 10 dans laquelle la valeur du défaut Pulmac
est inférieure à 2%.
12. Pâte de polyéthylène de la revendication 10 ou de la revendication 11 dans laquelle
la longueur de la fibre est inférieure à 2 mm et avec une longueur moyenne comprise
entre 0,80 et 1,20 mm.
13. Pâte de polyéthylène selon l'une quelconque des revendications 10-12 dans laquelle
la pâte a une aire superficielle comprise entre 6 et 8 m2/g.
14. Pâte de polyéthylène selon l'une quelconque des revendications 10-13 dans laquelle
les fibres ont une finesse telle que les fibres ont une rugosité de Kajaani de moins
de 0,20 mg/m.
15. Feuille de polyéthylène formée de la pâte selon l'une quelconque des revendications
10 à 14.
16. Feuille de polyéthylène formée de fibres fortes discontinues selon l'une quelconque
des revendications 1-9.
17. Feuille de la revendication 16 dans laquelle les fibres ont des longueurs comprises
entre 5 et 25 mm.
18. Feuille de la revendication 16 ou de la revendication 17 qui est une feuille mise
à plat à l'air.
19. Feuille de la revendication 16 ou de la revendication 17 qui est une feuille mise
à plat à l'état humide.