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Patent 2217640 Summary

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Claims and Abstract availability

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(12) Patent Application: (11) CA 2217640
(54) English Title: COMPOSTIBLE LAMINATE
(54) French Title: LAMINE COMPOSTIBLE
Status: Deemed Abandoned and Beyond the Period of Reinstatement - Pending Response to Notice of Disregarded Communication
Bibliographic Data
(51) International Patent Classification (IPC):
  • B32B 27/10 (2006.01)
  • B32B 7/06 (2019.01)
  • B32B 29/00 (2006.01)
  • B65D 65/46 (2006.01)
  • D21H 19/30 (2006.01)
  • D21H 19/34 (2006.01)
  • D21H 19/82 (2006.01)
(72) Inventors :
  • WADDINGTON, SIMON DOMINIC (Belgium)
  • MONTADOR, JAMES HENRY (United Kingdom)
  • KUUSIPALO, JURKKA TAPANI (Finland)
  • KARHUKETO, HANNU TAPANI (Finland)
(73) Owners :
  • ZENECA LIMITED
  • UNITED PAPER MILLS LIMITED
  • UNITED PAPER MILLS LIMITED
  • METABOLIX, INC.
(71) Applicants :
  • ZENECA LIMITED (United Kingdom)
  • UNITED PAPER MILLS LIMITED (Finland)
  • UNITED PAPER MILLS LIMITED (Finland)
  • METABOLIX, INC. (United States of America)
(74) Agent: OSLER, HOSKIN & HARCOURT LLP
(74) Associate agent:
(45) Issued:
(86) PCT Filing Date: 1996-04-04
(87) Open to Public Inspection: 1996-10-10
Availability of licence: N/A
Dedicated to the Public: N/A
(25) Language of filing: English

Patent Cooperation Treaty (PCT): Yes
(86) PCT Filing Number: PCT/GB1996/000819
(87) International Publication Number: WO 1996031347
(85) National Entry: 1997-10-06

(30) Application Priority Data:
Application No. Country/Territory Date
9507263.3 (United Kingdom) 1995-04-07
951637 (Finland) 1995-04-06

Abstracts

English Abstract


A composite laminate which comprises layers of a cellulose sheet, a
polycaprolactone, polylactic acid and/or a poly 3- or 4-hydroxyalkanoic acid
is compostible and has acceptable wet strength and resistance to cracking.


French Abstract

La présente invention décrit un laminé composite comportant des couches de feuilles de cellulose, une polycaprolactone, un acide polylactique et/ou un acide poly 3- ou 4- hydroxyalcanoïque, qui est compostible et présente une résistance à l'état humide et une résistance à la déchirure acceptables.

Claims

Note: Claims are shown in the official language in which they were submitted.


CLAIMS
1 A laminate which comprises a cellulosic
sheet directly coated on at least one surface with a
layer of polycaprolactone and a layer overlying the said
directly coated layer of a poly 3- or 4- hydroxy-alkanoic
acid.
2 A laminate as claimed in Claim 1 in which the
cellulosic sheet is paper or board.
3 A laminate as claimed in any preceding
claim in which the polyhydroxyalkanoic acid layer is
covered with a readily removable sacrificial layer
of optionally non polymer.
4 A laminate as claimed in Claim 3 in which the readily
removable layer is of polyethylene or polypropylene.
A laminate as claimed in any of Claims 1 to 5 in
which the total weight of the layers other than the
cellulosic sheet after stripping any ready removable
layer from the product is 4 to 40 grams per square
metre.
6 A laminate as claimed in any preceding claim in
which the ratio of the polyhydroxyalkanoic acid to
polycaprolactone is 2:1 to 1:2 by weight and preferably a ratio of 1:1
7 A laminate as claimed in any preceding claim in
which the polyhydroxyalkanoic acid is a homo or

copolymer of hydroxybutyric acid together with
hydroxyvaleric acid.
9 A laminate as claimed in Claim 7 in which the
polyhydroxyalkanoic acid has a molecular weight of
100,000 to 800,000.
A laminate as claimed in any preceding claim in
which the polycaprolactone has a molecular weight of at least
40, 000.
11 A process of making a laminate as claimed in any
preceding claim in which the other layers are
applied to the cellulosic sheet simultaneously.
12 A process as claimed in Claim 10 in which
temperatures of 150 to 300°C are used for
coextrusion and in which the melting points of the
polymers used are below the said extrusion
temperature.
13 A process as claimed in Claim 10 or 11 in which the
laminate is cooled to a temperature of 40 to 70°C by
contacting the laminate with a chill roll.
14 A process as claimed in any of claims 10 or 12 in
which the readily removable layer is stripped from the
laminate and re-used in the manufacturing process.

Description

Note: Descriptions are shown in the official language in which they were submitted.


J y -- -- --
CA 022l7640 l997-l0-06
, Blo~ D~ ~ L
~ff~L ,. _ J~ I~~SS~ o 1 ~9 r,A~ a ~ 1
THIS INVENTION relates to q~ ,o~ 't~l~minates.
Used packaging materials constitute a refuse
disposal problem and it is desirable to be able to
compost them. Also, in composting organic wastes, for
example food or vegetation, it is convenient to transport
the compostible material in a compostible container.
Bags made of paper or other cellulosic material, for
example cellulose film or boxes made of such materials,
for example cardboard or the like may be used but are
mechanically weak when wet. b10d~ f ~l~ l~
This invention provides ~c~..~o~t lc laminates
comprising cellulosic sheets, for example paper or board,
of satisfactory strength which comprise substantially
b io~ ra.d a ble
only ac.. ~oGtiblc~components and which comprise layers of
a cellulose sheet, a polycaprolactone, ~ polyl~ctic ~cid
and,'~r ~ c~'lulorc Q~tcr and a poly 3- or 4-hydroxy-
alkanoic acid.
The invention preferably comprises a c~_~e~tiblc
laminate which comprises a cellulosic sheet directly
coated on at least one surface with a layer of
polycaprolactone ~lyl~otio a~id afidfc~ ~ cell~'c~
~x~ and a layer overlying the said directly coated
layer of a poly 3 or 4-hydroxy~lk~noic acid. We have
found that laminates according to the invention have
acceptable wet strength and resistance to cracking.
Resistance to cracking is important if the paper or board
is folded as any cracking along the fold will allow
access to moisture and impairment of the wet strength
along the fold.
VO ~

a~:,, r~ V v ~
CA 022l7640 l997-l0-06
The invention also comprises a ~ ct~lt lamunate
as aforesaid in which the polyhydroxyalkanoic acid layer
is covered with a readily removable ~QrificiQl layer of
optionally non-compostible polymer, for example6polythene
~d ,l~ ~0 ~ ~e
or polypropylene. The oac _fiaill~layer is useful in
improving the manufacture of the l~;nate, for ex~rle in
preventing the sticking of the laminate to chill rolls in
the course of manufacture. If desired it may be left in
position to protect the l~;nate until it is to be used.
The added layers may be applied to the cellulosic
sheet simultaneously using known techniques, for example
by the use of a multi manifold co-extruder. Temperatures
of 150 to 300~C and preferably 150 to 250~C are suitably
used for co-extrusion and polymers with melting points
below the extrusion temperature should be used. After
application of the added layers the laminate is suitably
cooled for example to a temperature of 40 to 70~C. This
~y be accomplished by contacting the l~;nate with a
chill roller.
It is preferred that the total weight of the coating
r~4~ ~c~o ~ Je
layers after stripping thelo~crifi~ial layer from the
product should be about 5 to 40 yl~-~,es per square metre
and is preferably 10-25 yr ?~ per square metre. The
ratio of the polyhydroxyalkanoic acid to the polycapro-
lactone, ccllulo~ cctcr or po'ylac~io ~ yer~ ~y '_
~.~O ~o ~v.l prc ~~?~ly 5tl to 11~ ~n~ .c_c ~rcfc_~ly
2:1 to 1:2 by weight~
The polyhydroxyalkanoic acid may be a homo or co-
polymer ~ 'y of hydroxybutyric acid prq~q}ab'y
together with hydroxyvaleric acid. Suitable polymers of
A~EP'~D~D S~T

CA 022l7640 l997-l0-06
this type are described in ~r European Patents EP 52459
and EP 69497. The polyhydroxyalkanoic acid preferably
has a molecular weight of 50,000 to 1 million and more
preferably 100,000 to 800,000. The ~olyl~a~
aollulocc ~t~ or polycaprolactone preferably has a
molecular weight of ~t lc~t ~0,000 fc_ c~b~lc 30,000 to
soo,ooo, ahl f)r~f~r~obly ~ ~t ~e~s t 4~ o~.
The c~ f~ ayer may after it is stripped from
the laminate be reused in the manufacturing process if it
is a thermo-plastic. ~ead ~ - fef~
A pilot line was used for the following work which
comprises a roll of 110g/m' brown Kraft paper feeding the
paper to a unit f or corona discharge onto the paper, a
support roller supporting the paper emerging from the
corona discharge chamber, a die for extruding three
layers of polymer onto the paper beyond the support
roller, a chill roller and a nip roller for pressing the
laminate of paper and polymer together against the chill
roller and a wind-up rol' ~r for collecting the l~nate.
The corona discharge was at a power of approximately
1.5 ~ over a width of 350 mm, the paper being run
through the discharge at a rate of 15 to 75 m per minute.
The die was fed by three extruders supplying
polycaprolactone (a commercial product sold as ~Tone- 767
by Union Carbide, estimated number average molecular
weight 43,000 melt flow index of 30 at 190~C), a
copolymer comprising 92% hydroxybutyric acid units and 8%
hydroxyvaleric acid units in a D-configuration of
estimated weight average molecular weight 480,000 sold
under the trade name ~BIOPOL- by ZENECA Limited and low

CA 02217640 1997-10-06
WO 9613~347 PCT/GB96/00819
density polyethylene sold by Borealis as grade NCPE 1515,
MFI 15 at 190~C. The die was a Cloeren vane flat die of
width 350 mm with adjustable vanes and equipped with
breaker plates and screen packs and using a CCABB
configuration plug.
This arrangement enabled the polymers to be extruded
onto the paper in the order paper/polycaprolactone/-
"BIOPOL" polyhydroxyalkanoate/polyethylene in the desired
thicknesses set by the outputs from each extruder.
The chill roller was maint~;ne~ at a temperature of
60~C.
The line was operated under the conditions shown
below. For comparison a single layer consisting of
"BIOPOL n polymer was coated onto the paper using only one
of the extruders under the conditions shown below. The
"Barrel Zone" temperatures indicate the successive
increases in temperature in the barrel zones of the
extruders which feed adaptors of the extruders which
adjust the temperature of the polymer as shown. The
temperature of the die itself was set at 185~C.
8~ngle Layer Extrusion
Sample Barrel Zones ~C Adaptor Screw Line
~CSpeed speed
1 2 3 rpm m/min
#1 150 175 185 18540 30
#2 150 175 185 18540 20
#3 150 175 185 185 40 25

CA 022l7640 l997-l0-06
WO96l3~347 PCT/GB96/00819
s
3 Layer Co-Extrusion
Sample Barrel Zones ~C Adap Screw Line
-tor speed speed
~C rpm m/min
1 2 3 4
#9 150 175185 18545 35
150 170180185 18520
150 170180185 18590
#10 150 175185 18532 35
150 170185185 18532
150 170185185 18590
#20 150 175185 18550 50
150 175180185 18550
170 190195200 205200
#21 150 175185 18550 75
150 170180185 18550
170 190195200 205200
The screw speeds in the preceding table are
proportional to the approximate relative thickness of the
layers.
The products were tested as follows:
T.~m; n~te from the wind-up roller was removed and any
polyethylene layer stripped off. The coat weight (i.e.
the total polymer r~m~ining per square metre of laminate)
was recorded.
A & esion of the layers was tested by m~n

=
CA 02217640 1997-10-06
WO96/31347 PCT/GB96/00819
stripping of the deposited polymer layers from the paper.
Cracking of the polymer layer was tested by folding
the laminate over so that the polymer layer contacted the
polymer layer, the direction of folding being transverse
to the line processing direction or parallel to the line
processing direction as the case may be, and also so that
the paper layer contacted the paper layer in the
transverse and parallel directions as aforesaid.
The integrity of the polymer coating after folding
was tested by laying the laminate flat, applying coloured
turpentine to the crease from the polymer side of the
laminate and after 10 minutes measuring the proportion of
the crease in which colouring on the paper side was
observed. 10 cm lengths of crease were tested.
lS The results are reported as follows:

CA 02217640 1997-10-06
W0 96/31347 PCT/GB96/00819
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CA 02217640 1997-10-06
W 096131347 PCTI~D5G,'~C319
Adhesion O Layers not bonded at all and both
materials remain completely intact.
A & esion 1 Layers come apart easily and both
materials remain completely intact.
Adhesion 2 Some force needed to separate the layers
and materials damaged slightly.
Adhesion 3 More force needed to separate the layers
and both materials damaged.
Adhesion 4 Layers difficult to pull apart and both
damaged almost totally.
Adhesion 5 Layers impossible to pull apart, both tear
immediately.

Representative Drawing

Sorry, the representative drawing for patent document number 2217640 was not found.

Administrative Status

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Event History

Description Date
Inactive: Agents merged 2013-10-28
Inactive: IPC from MCD 2006-03-12
Inactive: IPC from MCD 2006-03-12
Inactive: IPC from MCD 2006-03-12
Inactive: IPC from MCD 2006-03-12
Time Limit for Reversal Expired 2004-04-05
Application Not Reinstated by Deadline 2004-04-05
Deemed Abandoned - Failure to Respond to Maintenance Fee Notice 2003-04-04
Inactive: Abandon-RFE+Late fee unpaid-Correspondence sent 2003-04-04
Letter Sent 2002-07-23
Letter Sent 2002-05-02
Reinstatement Requirements Deemed Compliant for All Abandonment Reasons 2002-04-19
Deemed Abandoned - Failure to Respond to Maintenance Fee Notice 2002-04-04
Inactive: Delete abandonment 1999-04-23
Inactive: Delete abandonment 1999-04-21
Inactive: Abandoned - No reply to Office letter 1999-03-23
Inactive: Abandoned - No reply to Office letter 1999-03-09
Inactive: Single transfer 1999-03-09
Inactive: Transfer information requested 1998-12-09
Inactive: Single transfer 1998-10-02
Inactive: IPC assigned 1998-01-21
Inactive: IPC assigned 1998-01-19
Inactive: IPC assigned 1998-01-19
Inactive: First IPC assigned 1998-01-19
Classification Modified 1998-01-19
Inactive: Courtesy letter - Evidence 1997-12-23
Inactive: Notice - National entry - No RFE 1997-12-16
Application Received - PCT 1997-12-15
Application Published (Open to Public Inspection) 1996-10-10

Abandonment History

Abandonment Date Reason Reinstatement Date
2003-04-04
2002-04-04

Maintenance Fee

The last payment was received on 2002-04-19

Note : If the full payment has not been received on or before the date indicated, a further fee may be required which may be one of the following

  • the reinstatement fee;
  • the late payment fee; or
  • additional fee to reverse deemed expiry.

Please refer to the CIPO Patent Fees web page to see all current fee amounts.

Fee History

Fee Type Anniversary Year Due Date Paid Date
Basic national fee - standard 1997-10-06
MF (application, 2nd anniv.) - standard 02 1998-04-06 1998-03-25
Registration of a document 1998-10-02
MF (application, 3rd anniv.) - standard 03 1999-04-06 1999-03-25
MF (application, 4th anniv.) - standard 04 2000-04-04 2000-03-22
MF (application, 5th anniv.) - standard 05 2001-04-04 2001-03-27
MF (application, 6th anniv.) - standard 06 2002-04-04 2002-04-19
Reinstatement 2002-04-19
Registration of a document 2002-06-11
Owners on Record

Note: Records showing the ownership history in alphabetical order.

Current Owners on Record
ZENECA LIMITED
UNITED PAPER MILLS LIMITED
UNITED PAPER MILLS LIMITED
METABOLIX, INC.
Past Owners on Record
HANNU TAPANI KARHUKETO
JAMES HENRY MONTADOR
JURKKA TAPANI KUUSIPALO
SIMON DOMINIC WADDINGTON
Past Owners that do not appear in the "Owners on Record" listing will appear in other documentation within the application.
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Document
Description 
Date
(yyyy-mm-dd) 
Number of pages   Size of Image (KB) 
Abstract 1997-10-06 1 45
Description 1997-10-06 8 240
Claims 1997-10-06 2 62
Cover Page 1998-01-20 1 26
Reminder of maintenance fee due 1997-12-16 1 111
Notice of National Entry 1997-12-16 1 193
Request for evidence or missing transfer 1998-10-07 1 110
Request for evidence or missing transfer 1998-12-23 1 110
Courtesy - Certificate of registration (related document(s)) 1999-04-12 1 118
Courtesy - Certificate of registration (related document(s)) 1999-04-12 1 117
Courtesy - Abandonment Letter (Maintenance Fee) 2002-05-02 1 183
Notice of Reinstatement 2002-05-02 1 172
Reminder - Request for Examination 2002-12-05 1 113
Courtesy - Abandonment Letter (Maintenance Fee) 2003-05-05 1 176
Courtesy - Abandonment Letter (Request for Examination) 2003-06-16 1 166
PCT 1997-10-06 15 525
Correspondence 1997-12-18 1 29
Correspondence 1998-10-07 1 10
Fees 2002-04-19 1 46
Fees 2000-03-22 1 53
Fees 1998-03-25 1 53
Fees 2001-03-27 1 53
Fees 1999-03-25 1 58