FORM2
THE PATENTS ACT, 1970
(39 of 1970)
&
THE PATENTS RULES, 2003
COMPLETE SPECIFICATION
(See section 10, rule 13)

1. Title of the invention: A LAMITUBE SLEEVE AND IMPLEMENTATIONS THEREOF

2. Applicant(s)
NAME NATIONALITY ADDRESS
EPL LIMITED Indian Top Floor, Times Tower, Kamala
City, Senapati Bapat Marg, Lower
Parel, Mumbai 400013, India

3. Preamble to the description

COMPLETE SPECIFICATION
The following specification particularly describes the invention and the manner in which it
is to be performed.

FIELD OF INVENTION
[0001] The present disclosure relates to packaging materials. In particular, the
present disclosure relates to lamitube sleeve comprising nucleated polyethylene and
process of preparing thereof.
5
BACKGROUND OF THE INVENTION
[0002] The packaging industry has emerged as one of the fastest growing sectors
in the world economy. Ease of manufacture of plastics, coupled with its wide
functionality has made plastics a widely accepted packaging material. However,
10 there are growing concerns related to environmental and ecological sustainability
in the use of such plastics. Accordingly, the concept of reduce, reuse and recycle is
the guiding principle to minimize the growing environmental concerns.
[0003] Reduce is an essential guideline since it eliminates the source of plastics
even before its availability for reuse and recycle. Reduce would necessarily be
15 decreasing the amount of the plastics used in packaging material without
compromising its functional aspects. Thus, reducing the amount and thickness of
plastics yet retaining its mechanical, aesthetic, barrier and recyclable properties is
most sought for.
[0004] In view of the above, there is a need for packaging materials with reduced
20 plastics without compromising any of its existing packaging qualities.
SUMMARY OF THE INVENTION
[0005] In an aspect of the present disclosure, there is provided a lamitube sleeve
comprising: a) an outer layer and a sealant layer independently comprising at least
25 one nucleated high density polyethylene; and b) a barrier layer disposed between
the outer layer and the sealant layer, wherein the lamitube sleeve has a tensile
strength @yield of at least 22 MPa.
[0006] In another aspect of the present disclosure, there is provided a process of
preparing the lamitube sleeve as disclosed herein, the process comprising: a)
30 making multilayer film(s) from nucleated high density polyethylene; b) obtaining a

barrier layer; and c) extrusion laminating the layers together, then slitting into reels
of desired width in the range of 63 - 320 mm, followed by tubing from the reels.
[0007] These and other features, aspects, and advantages of the present subject
matter will be better understood with reference to the following detailed description
5 and appended claims. This summary is provided to introduce a selection of concepts
in a simplified form. This summary is not intended to identify key features or
essential features of the claimed subject matter.
DETAILED DESCRIPTION OF THE INVENTION
10 [0008] Those skilled in the art will be aware that the present disclosure is subject
to variations and modifications other than those specifically described. It is to be
understood that the present disclosure includes all such variations and
modifications. The disclosure also includes all such steps, features, compositions,
and compounds referred to or indicated in this specification, individually or
15 collectively, and any and all combinations of any or more of such steps or features.
Definitions
[0009] For convenience, before further description of the present disclosure,
certain terms employed in the specification, and examples are delineated here.
These definitions should be read in the light of the remainder of the disclosure and
20 understood as by a person of skill in the art. The terms used herein have the
meanings recognized and known to those of skill in the art, however, for
convenience and completeness, particular terms and their meanings are set forth
below.
[0010] The articles “a”, “an” and “the” are used to refer to one or to more than one
25 (i.e., to at least one) of the grammatical object of the article.
[0011] The terms “comprise” and “comprising” are used in the inclusive, open
sense, meaning that additional elements may be included. It is not intended to be
construed as “consists of only”.
[0012] Throughout this specification, unless the context requires otherwise the
30 word “comprise” and variations such as “comprises” and “comprising”, will be

understood to imply the inclusion of a stated element or step or group of element or
steps but not the exclusion of any other element or step or group of element or steps.
[0013] The term “including” is used to mean “including but not limited to”.
“Including” and “including but not limited to” are used interchangeably.
5 [0014] The term “at least one” used herein refers to one or more and thus, includes
individual components as well as mixtures/combinations.
[0015] The term “lamitube sleeve” used herein refers to sleeve of the lamitube
comprising an outer layer and a sealant layer independently comprising at least one
nucleated high density polyethylene; and a barrier layer disposed between the outer
10 layer and the sealant layer, wherein the lamitube sleeve has tensile strength @yield
of at least 22 MPa and density in a range of 0.941 to 0.990 g/cm3
.
[0016] The term “polyethylene” as used herein refers to an ethylene polymer
having density in a range of 0.833 - 0.990 g/cm3
, selected from high density
polyethylene, medium density polyethylene, low density polyethylene, linear low
15 density polyethylene or combinations thereof.
[0017] The term “high density polyethylene” as used herein refers to polyethylene
having a density usually in the range of from about 0.94 g/cm3 to about 0.97 g/cm3
.
The terms HDPE and high density polyethylene may be interchangeably used. High
density polyethylene of the present disclosure may also inherently include a
20 nucleating agent. Examples of such HDPE include but not limited to Elite AT6900
from Dow chemicals, SURPASS HPs167-AB-sHDPE from Nova chemicals or
combinations thereof.
[0018] The term “medium density polyethylene” as used herein refers to
polyethylene having a density usually in the range of from about 0.926 g/cm3
to
about 0.941 g/cm3
25 . The term MDPE and medium density polyethylene may be
interchangeably used.
[0019] The term “low density polyethylene” as used herein refers to polyethylene
having a density usually in the range of from about 0.910 g/cm3
to about 0.925
g/cm3
. The term LDPE and low density polyethylene may be interchangeably used.
30 [0020] The term “linear low density polyethylene” as used herein refers to
polyethylene having a density usually in the range of from about 0.910 g/cm3
to

about 0.930 g/cm3
. The term LLDPE and linear low density polyethylene may be
interchangeably used.
[0021] The melt flow index (MFI) of aforesaid polyethylene may be in the range
of 0.2 to 15 g/10min, specifically in the range of 0.2 to 7.0 g/10 min, more
5 specifically 0.2 to 2.0 g/10 min. The MFI is measured as per ASTM D 1238.
[0022] The term “nucleating agent” used herein refers to an additive added to a
polymer that changes the crystallization behaviour of the polymer. For the purpose
of the present disclosure, a nucleating agent is added to high density polyethylene
to form nucleated high density polyethylene. Examples of nucleating agents include
10 but are not limited to UltraGuard™ Solutions Natural 10036, UltraGuard™
Solutions EXP Natural 10385 (Milliken) and so on. High density polyethylene can
also be of inherently containing a nucleating agent such as Elite AT6900 from Dow,
SURPASS HPs167-AB – sHDPE from Nova Chemicals and so on.
[0023] The term “tensile strength @ yield” used herein refers to a material’s ability
15 to withstand loads and forces. For the purpose of the present disclosure, the “tensile
strength @ yield” of the lamitube sleeve is at least 22 MPa. The tensile properties
are measured as per ASTM D 882.
[0024] The term “water vapour transmission rate” or “WTR” or “WVTR” used
herein refers to amount of water vapour pass or permeate through a material in a
20 specific period of time. For the purpose of the present disclosure, WTR of the
lamitube sleeve is measured at 38℃ at 90% humidity and is found to be equal to or
less than 0.750 g/m2
.day. The test method is as per ASTM F 1249-20.
[0025] Ratios, concentrations, amounts, and other numerical data may be presented
herein in a range format. It is to be understood that such range format is used merely
25 for convenience and brevity and should be interpreted flexibly to include not only
the numerical values explicitly recited as the limits of the range, but also to include
all the individual numerical values or sub-ranges encompassed within that range as
if each numerical value and sub-range is explicitly recited. For example, a thickness
range of 50 µm to 150 µm should be interpreted to include not only the explicitly
30 recited limits of 60 µm to 130 µm, but also to include sub-ranges, such as 65 µm to
135 µm, 70 µm to 120 µm, and so forth, as well as individual amounts, including

fractional amounts, within the specified ranges, such as 65.2 µm, 140.6 µm, and
141.5 µm, for example.
[0026] As discussed in the background, there is a requirement for packaging
materials with reduced plastics. Accordingly, the present disclosure provides a
5 lamitube sleeve comprising an outer layer and a sealant layer independently
comprising nucleated high density polyethylene. Nucleated high density
polyethylene is obtained by dispersing nucleating agent with high density
polyethylene in order to achieve a polyethylene with higher crystallinity and also
evenly sized spherulites. However, such crystalline formations or desired
10 morphology (crystalline structure or spherulite structure) are not observed in the
absence of such nucleating agents. Therefore, nucleated polyethylene due to its
higher crystalline structure impart improved mechanical properties. Thus, the
present disclosure provides a lamitube sleeve comprising an outer layer and a
sealant layer independently comprising nucleated high density polyethylene, and a
15 barrier layer disposed between the outer layer and the sealant layer, wherein the
lamitube sleeve has a tensile strength @yield of at least 22 MPa. Also, the lamitube
sleeve has water vapour transmission rate equal to or less than 0.750 g/m2
.day at
38℃ at 90% humidity.
[0027] In an embodiment of the present disclosure, there is provided a lamitube
20 sleeve comprising: a) an outer layer and a sealant layer independently comprising
at least one nucleated high density polyethylene; and b) a barrier layer disposed
between the outer layer and the sealant layer, wherein the lamitube sleeve has a
tensile strength @yield of at least 22 MPa. In another embodiment of the present
disclosure, the lamitube sleeve has a tensile strength @yield in a range of 22 to 30
25 MPa. In one another embodiment of the present disclosure, the lamitube sleeve has
a tensile strength @yield in a range of 22 to 25 MPa.
[0028] In an embodiment of the present disclosure, there is provided a lamitube
sleeve as disclosed herein, the nucleated high density polyethylene comprises high
density polyethylene and a nucleating agent. In another embodiment of the present
30 disclosure, the nucleated high density polyethylene comprises a high density
polyethylene inherently with a nucleating agent. In one another embodiment of the

present disclosure, the nucleated high density polyethylene comprises a high
density polyethylene inherently with a nucleating agent such as to Elite AT6900
from Dow, SURPASS HPs167-AB – sHDPE from Nova Chemicals or
combinations thereof.
5 [0029] In an embodiment of the present disclosure, there is provided a lamitube
sleeve as disclosed herein, wherein the barrier layer is a multilayer comprising at
least one barrier component and at least one polyethylene.
[0030] In an embodiment of the present disclosure, there is provided a lamitube
sleeve as disclosed herein, wherein the polyethylene has density in a range of 0.833
– 0.990 g/cm3
10 . In another embodiment of the present disclosure, the polyethylene
has density in a range of 0.870 – 0.990 g/cm3
.
[0031] In an embodiment of the present disclosure, there is provided a lamitube
sleeve as disclosed herein, wherein the barrier component is selected from
ethylvinyl alcohol, polyvinyl alcohol, polyamides, polyethylene terephthalate or
15 combinations thereof. In another embodiment of the present disclosure, the barrier
component is ethylvinyl alcohol or polyvinyl alcohol.
[0032] In an embodiment of the present disclosure, there is provided a lamitube
sleeve as disclosed herein, wherein the outer layer comprises one to five layers.
[0033] In an embodiment of the present disclosure, there is provided a lamitube
20 sleeve as disclosed herein, wherein the sealant layer comprises one to eleven layers.
[0034] In an embodiment of the present disclosure, there is provided a lamitube
sleeve as disclosed herein, wherein the barrier layer comprises one or more layers.
[0035] In an embodiment of the present disclosure, there is provided a lamitube
sleeve as disclosed herein, wherein each of the layer may comprise at least one tie
25 layer.
[0036] In an embodiment of the present disclosure, there is provided a lamitube
sleeve as disclosed herein, wherein the tie layer comprises a polymeric adhesive
selected from the group consisting of maleated polyethylene, anhydride grafted
ethylene/1-butene copolymer, anhydride grafted ethylene/1-hexene copolymer,
30 polypropylene, propylene ethylene copolymer, ethylene vinyl acetate copolymer,

ethylene methyl acrylate copolymer, and anhydride grafted ethylene/1-octene
copolymer.
[0037] In an embodiment of the present disclosure, there is provided a lamitube
sleeve as disclosed herein, wherein at least one layer of the lamitube sleeve is
5 metallized.
[0038] In an embodiment of the present disclosure, there is provided a lamitube
sleeve as disclosed herein, wherein the outer layer has a thickness in a range of 50
µm -150 µm.
[0039] In an embodiment of the present disclosure, there is provided a lamitube
10 sleeve as disclosed herein, wherein the sealant layer has a thickness in a range of
50 µm -200 µm.
[0040] In an embodiment of the present disclosure, there is provided a lamitube
sleeve as disclosed herein, wherein the barrier layer has a thickness in a range of 50
µm -150 µm.
15 [0041] In an embodiment of the present disclosure, there is provided a lamitube
sleeve as disclosed herein, wherein the nucleating agent is selected from UltraGuard
Solutions Natural 10036, or UltraGuard™ Solutions EXP Natural 1038. In another
embodiment of the present disclosure, the nucleated high density polyethylene is
selected from Elite AT6900 from Dow, SURPASS HPs167-AB – sHDPE from
20 Nova Chemicals or combinations thereof.
[0042] In an embodiment of the present disclosure, there is provided a lamitube
sleeve as disclosed herein, wherein the lamitube sleeve has density in a range of
0.941 to 0.990 g/cm3
.
[0043] In an embodiment of the present disclosure, there is provided a lamitube
25 sleeve as disclosed herein, wherein the lamitube sleeve has thickness in a range of
150 to 500 µm. In another embodiment of the present disclosure, the lamitube
sleeve has thickness in a range of 150 to 250 µm.
[0044] In an embodiment of the present disclosure, there is provided a lamitube
sleeve as disclosed herein, wherein the lamitube sleeve has water vapour
transmission rate equal to or less than 0.750 g/m2
30 .day at 38℃ at 90% humidity. In

another embodiment of the present disclosure, the lamitube sleeve has water vapour
transmission rate in a range of 0.250 to 0.750 g/m2
.day at 38℃ at 90% humidity.
[0045] In an embodiment of the present disclosure, there is provided a process of
preparing the lamitube sleeve as disclosed herein, the process comprising: a)
5 making multilayer film(s) from nucleated high density polyethylene; b) obtaining a
barrier layer; and c) extrusion laminating the layers together, then slitting into reels
of desired width in the range of 63 mm - 320 mm, followed by tubing from the
reels.
[0046] In an embodiment of the present disclosure, there is provided a process of
10 preparing the lamitube sleeve as disclosed herein, wherein extrusion laminating the
layers together is carried out in the presence of an extrusion lamination layer
comprising a high flowing polymer selected from HDPE, LDPE, LLDPE, ethyleneacrylic acid copolymer or combinations thereof. In another embodiment of the
present disclosure, the each of the layer of the lamitube sleeve may comprise a tie
15 layer comprising an adhesive selected from polyurethane, maleated polyethylene,
anhydride grafted (ethylene/1-butene copolymer, anhydride grafted ethylene/1-
hexene copolymer, anhydride grafted polypropylene, anhydride grafted propylene
ethylene copolymer), ethylene vinyl acetate copolymer, ethylene methyl acrylate
copolymer, anhydride grafted ethylene/1-octene copolymer, or combinations
20 thereof
[0047] Although the subject matter has been described in considerable detail with
reference to certain examples and implementations thereof, other implementations
are possible.
Examples
25 [0048] The disclosure will now be illustrated with working examples, which is
intended to illustrate the working of disclosure and not intended to take restrictively
to imply any limitations on the scope of the present disclosure. Unless defined
otherwise, all technical and scientific terms used herein have the same meaning as
commonly understood to one of ordinary skill in the art to which this disclosure
30 belongs. Although methods and materials similar or equivalent to those described
herein can be used in the practice of the disclosed methods and compositions, the

exemplary methods, devices and materials are described herein. It is to be
understood that this disclosure is not limited to particular methods, and
experimental conditions described, as such methods and conditions may apply.
5 Example 1
Process of preparing a lamitube sleeve
[0049] The lamitube sleeve of the present disclosure is a multilayer laminate sleeve
wherein each of the layers are obtained by blown film extrusion. The layers of the
lamitube sleeve include an outer layer, a sealant layer and a barrier layer. The outer
10 layer and the sealant layer independently comprise at least one layer of nucleated
polyethylene. The nucleated polyethylene is obtained by mixing a nucleating agent
and high density polyethylene and subjecting the composition to blown film
extrusion to obtain a layer of nucleated high density polyethylene (Nucleated
HDPE). A barrier layer is obtained by blown film extrusion of ethylvinyl alcohol
15 along with tie layers and flanking outer polyethylene layers. The lamitube sleeve is
then obtained by extrusion laminating the layers together, then slitting into reels of
desired width in the range of 63 - 320 mm, followed by tubing from the reels. The
process of film extrusion is a well-known process as discussed in the references
[Multilayer Flexible Packaging, 2nd Edition - March 29, 2016, Page 137-145,
20 Editor: John R. Wagner Jr. ELSEVIER]].
[0050] The lamitube sleeve of the present disclosure is of below structure:
L1- 50 μm (Nucleated HDPE) /20 μm (extrusion lamination layer) /55 μm (PE/
tie/EVOH/ tie/PE) / 20 μm (extrusion lamination layer) / 50 μm (Nucleated HDPE)
[0051] The lamitube sleeve includes an outer layer and a sealant layer which are
25 independently nucleated HDPE of thickness 50 μm. The barrier layer comprises is
multilayer, wherein a layer of ethylvinyl alcohol is sandwiched between
polyethylene in the presence of a tie layer. The outer, sealant and the barrier layers
are extruded laminated in the presence of extrusion lamination layer of an
(polyurethane) adhesive or high flowing polyethylene to obtain the lamitube sleeve.
30 [0052] For comparative purpose, lamitube sleeve L2 of below structure was
prepared by extrusion lamination of layers.
10

L2- 50 μm PE/tie/EVOH tie/PE / 20 μm (extrusion lamination layer) / 50 μm
PE/tie/EVOH/tie/PE / 20 μm(extrusion lamination layer) / 70 μm PE.
Example 2
Barrier and Mechanical Properties of the lamitube sleeve
5 [0053] Barrier and mechanical properties of the lamitube sleeves L1 and L2 as
prepared in Example 1 were measured.
[0054] WTR of the lamitube sleeves were measured at 38℃ at 90% RH. The test
conditions for measuring WTR is provided in Table 1 below and measured WTR
values of the lamitube sleeves are shown in Table 2.
Test Condition For WTR testing
Standard Used ASTM F 1249 - 20
Room Temp. 23 ± 2 ℃
Test Temp. 38 ± 0.5 ℃
Test RH 90% ± 3% RH
Conditioning 1 Hr
Test Area 50 cm2
Machine Model Permatran 3/34 G
10
[0055] Mechanical strength of the lamitube sleeves is assessed by determining
tensile strength at yield by ASTM D882 and the results are shown in Table 2. Tube
burst values of the of the lamitubes comprising the lamitube sleeve of the present
disclosure was also measured.
15 [0056] Burst strength refers to the ability of a lamitube to withstand a high
pressure for a specified time period. The tube was held by the nozzle in an air-tight
manner in a Burst Strength Tester. The ability of the lamitube to withstand the
pressure was determined and the results are shown in Table 2.
[0057] The burst strength test results showed that the lamitube comprising the
20 lamitube sleeve of the present disclosure had the ability to withstand internal
pressure of 3.56 bar without bursting. No cracks, or breakage was found after the
experiment which concludes that the lamitube comprising the lamitube sleeve of
the present disclosure possessed high burst strength.

Table 2
Lamitube
Sleeve
Thickness
(μm)
Tensile
strength @
yield (MPa)
WTR
(g/m2
.day)
38℃ 90%
RH
Tube burst strength
comprising L1/L2 of
lamitube diameter –
22 mm and Length –
75 mm
L1 195 MD: 22.20
TD: 24.12
0.659 3.61
L2 210 MD: 18.56
TD: 19.68
0.960 3.56
[0058] From Table 2 it could be observed that the lamitube sleeve of the present
disclosure exhibited improved barrier and mechanical properties as compared to
lamitube comprising L2. Table 2 confirmed that L2 showed higher WTR of 0.960
g/m2
.day, whereas L1 showed lesser WTR of 0.659 g/m2
5 .day confirming the
improved barrier properties. This could be attributed to the presence of nucleated
HDPE in the outer and the sealant layer in the lamitube sleeve. Thus, presence of
nucleated HDPE was critical in achieving the enhanced WTR. Further, it could be
seen that L1 had tensile strength @ yield of greater than 22 MPa in both machine
10 direction (MD) and transverse direction (TD) confirmed that the lamitube sleeve
(L1) of the present disclosure exhibited increased stiffness and tensile nature,
whereas the lamitube sleeve L2 without nucleated HDPE deformed at a lesser force
or load.
[0059] Further the lamitube comprising L1 of lesser thickness exhibited
15 comparable burst strength value with lamitube sleeve L2, wherein the thickness was
higher. However when the thickness of the lamitube sleeve of the present disclosure
was increased further the lamitube exhibited increased burst strength. Thus, the
lamitube sleeve of the present disclosure comprising the nucleated high density
polyethylene at the outer and at the sealant layer showed improved properties
20 besides having reduced thickness of the sleeve.

I/We Claim:

1. A lamitube sleeve comprising:
a) an outer layer and a sealant layer independently comprising at least one
nucleated high density polyethylene; and
b) a barrier layer disposed between the outer layer and the sealant layer,
wherein the lamitube sleeve has a tensile strength @yield of at least 22 MPa.

2. The lamitube sleeve as claimed in claim 1, wherein the nucleated high density polyethylene comprises high density polyethylene and a nucleating agent.

3. The lamitube sleeve as claimed in claim 1, wherein the barrier layer is a
multilayer comprising at least one barrier component and at least one
polyethylene.

4. The lamitube sleeve as claimed in claims 1 to 3, wherein the polyethylene has density in a range of 0.833 – 0.990 g/cm3.

5. The lamitube sleeve as claimed in claim 3, wherein the barrier component is selected from ethylvinyl alcohol, polyvinyl alcohol, polyamides, polyethylene terephthalate or combinations thereof.

6. The lamitube sleeve as claimed in claim 1, wherein the outer layer comprises one to five layers.

7. The lamitube sleeve as claimed in claim 1, wherein the sealant layer comprises one to eleven layers.

8. The lamitube sleeve as claimed in claim 1, wherein each of the layers may
comprise at least one tie layer.

9. The lamitube sleeve as claimed in claim 8, wherein the tie layer comprises a polymeric adhesive selected from the group consisting of maleated polyethylene, anhydride grafted ethylene/1-butene copolymer, anhydride grafted ethylene/1-hexene copolymer, polypropylene, propylene ethylene copolymer, ethylene vinyl acetate copolymer, ethylene methyl acrylate copolymer, and anhydride grafted ethylene/1-octene copolymer.

10. The lamitube sleeve as claimed in claim 1, wherein the outer layer has a
thickness in a range of 50 µm -150 µm.

11. The lamitube sleeve as claimed in claim 1, wherein the sealant layer has a thickness in a range of 50 µm -200 µm.

12. The lamitube sleeve as claimed in claim 1, wherein the barrier layer has a thickness in a range of 50 µm -150 µm.

13. The lamitube sleeve as claimed in claim 1, wherein the lamitube sleeve has density in a range of 0.941 to 0.990 g/cm3
.
14. The lamitube sleeve as claimed in claim 1, wherein the lamitube sleeve has water vapour transmission rate equal to or less than 0.750 g/m2 .day at 38℃ at 90% humidity.

15. A process of preparing the lamitube sleeve as claimed in claim 1, the process comprising:
a. making multilayer film (s) from nucleated high density
polyethylene;
b. obtaining a barrier layer; and
c. extrusion laminating the layers together, then slitting into reels of
desired width in the range of 63 - 320 mm, followed by tubing from the reels