Container for anaerobic products

FIELD OF THE INVENTION

The present invention relates to a container for anaerobic products in particular anaerobic sealants and adhesives, in particular liquid products. Anaerobic adhesives and sealants cure, set-up or polymerise in the absence of oxygen (air).

BACKGROUND OF THE INVENTION

The term anaerobic products as used here refers to formulations which cure, set-up or polymerise in the absence of air.

EP 0 352 143 describes an anaerobic liquid acylate sealant composition. U.S. Pat. No. 4,180 640 (Loctite) describes a hardenable adhesive and sealing composition. U.S. Pat. No. 3,218,305 (Krieble) discloses an anaerobic sealant composition. U.S. Pat. No. 2,895,950 and U.S. Pat. No. 3,046,262 (Krieble) also disclose anaerobic compositions. The products described in these specifications are examples of the type of product that may be stored in the container of the invention.

Containers or packages for storing anaerobic adhesive and sealant products are known. Typically such containers may be constructed from plastic, having substantially rigid walls, and capable of holding a number of liters of anaerobic product. Larger containers with pouring spouts are suitable only for low viscosity products. High viscosity products are not-easily decanted. It is known to provide semi-rigid plastic containers for such products. High viscosity products may be dispensed from containers by manual squeezing.

Rigid and semi-rigid containers are used with automatic dispensing machines. They do not readily conform to the shape of the dispenser and thus can create pockets of trapped (and therefore undispensing) products in the dispensing machine. High viscosity products tend to adhere to the walls of the container even if the container is pressurised, leaving a substantial amount of product within the container which is then wasted, or has otherwise to be removed from the container. A further disadvantage of such containers is the shelf life of products and particularly of anaerobic products placed in such containers if the container is filled beyond a certain level. Containers for anaerobic products are ordinarily left with a headspace above the level of liquid in the container. Typically 30% to 60% of the internal volume of the container is left unfilled with anaerobic product, depending on the rigidity of the side wall of the container in order to give a sufficient shelf-life. This allows a sufficient volume of air (oxygen) to remain within the container to help stabilise the anaerobic product. There exists however a conflict between the necessity to seal in the product on the one hand and to allow air (oxygen) to permeate through the product on the other. Such containers when filled or nearly full do not provide commercially acceptable shelf life for anaerobic products, as there is not sufficient air (oxygen) present in the container, nor does sufficient air permeate into the container. There is therefore substantial wastage of packaging materials and higher costs due to the partial filling of containers with this product.

Containers made from air-permeable material allow air through their walls etc. This air may replace air in the headspace or may permeate into the product within the container. However in order to ensure stability of anaerobic products permeation into the headspace alone is not sufficient to ensure adequate shelf-life. The air must permeate through the product also to ensure curing, setting up or polymerisation of the product does not occur. The area where curing, setting up or polymerisation is most likely to first occur is at the centre of the mass of product. Thus even with an air permeable container, and headspace of air in the container, curing or setting up or polymerisation may take place prematurely giving the product a shorter than desired shelf-life. The problem of curing or setting up is exacerbated by elevated storage temperatures. It is known to refrigerate, for example at temperatures of 2-8° C., certain anaerobic products which are sensitive to polymerisation, curing or setting up (particularly those of high viscosity) in order to prevent premature curing. Temperatures greater than about 28-30° C. cause even more rapid curing or setting up of anaerobic products.

An example of one of such containers is commonly referred to as a “cubitainer” [commercially available from Dynopack Ltd. in the U.K.]. The name stems from its cubic shape. The container is constructed from a typically translucent plastic constructed from low density polyethylene/ethylene vinyl acetate (LLDPE/EVA) copolymer mixed with linear low density polyethylene (LLDPE) with a wall thickness of about 160 μm to 180 μm. A nozzle with a threaded cap is fitted at the centre of the top wall of the container. Typically the cubitainer has a 3 liter internal volume, which is used to hold 1 liter or 2 liters, of an anaerobic adhesive. The less anaerobic adhesive placed in the cubitainer the greater the shelf-life of the adhesive.

The cubitainer has a continuous welded seam which runs about the outside of the container. The seam runs along one side of the base wall, then diagonally across a first side wall, then across one side of the top wall and then diagonally down a second side wall opposite the first side wall to meet the base wall to form a continuous seam about the container.

The container is relatively rigid, though its contents can be dispensed manually by squeezing the walls of the container to some extent. However, users of the cubitainer have noticed that substantial amounts of medium to high viscosity product remain in the container despite manual pressure, causing them to resort to cutting open the container to remove the contents. The cubitainer is packaged within an external paperboard carton which prevents physical damage to the plastic walls and allows stacking. The oxygen permeability of the cubitainer at 20° C. and 350 μm wall thickness is about (546 cm

3

/m

2

.day.atm) 553 cm

3

/m

2

.day.bar.

When partially full the cubitainer provides a storage means for anaerobic containers which gives the product an excellent shelf life. However as stated above partially filled containers are wasteful of materials and energy. It is of course possible to fill the cubitainer completely, but in practice it has not been filled as this would compromise the shelf-life of the product. Furthermore the cubitainer is suitable only for low to medium viscosity products, not for medium to high viscosity products due to their “difficult to pour” nature. High viscosity products have been traditionally sold in “bucket with lid” containers i.e. a very wide mouthed container (and thus large) to allow the product to be removed manually from the container.

The containers described above are all “stand-alone” containers i.e. the rigidity of the side-walls is sufficient to allow the container to stand without falling over or deforming to any appreciable extent under internal pressure from its contents. To make a stand-alone container it is necessary to conform to a base area:height ratio which makes the container stable when standing. The cubitainer described above is packaged in a paperboard carton to protect it from damage during transport, storage and the like. The cubitainer is a stand-alone container, its cubic shape and relatively rigid side walls allowing it to stand on its base.

Another form of container used for high viscosity anaerobic products is a cartridge having a nozzle and a built-in piston from which product is dispensed by a dispensing gun etc. No headspace is left in the cartridge. This severely limits the shelf-life of the product. Furthermore the amounts placed in these cartridges are relatively small, of the order of 300 ml to 800 ml. Larger volumes would result in an even shorter shelf-life of the product.

A collapsible container is known from EP-A-0172711 which is suitable for use with medicaments or other liquids which must be preserved from contamination. Likewise EP-A-0590465 relates to a composite film barrier for packaging oxygen-sensitive products. These containers are intended to prevent the ingress of air into the interior of the container and therefore would not be suitable for use with anaerobic products which would cure or polymerise in the absence of air (oxygen).

Composite films for bag-in-box-type containers are known from JP-A-07 701 002-A (see Derwent Abstract: Accession No. 95-182607 [24]). Such films are made from outer layers of ultra-low density polyethylene or linear low density polyethylene with an intermediate gas barrier layer. The gas barrier layer may be of polyamide resin layer, saponified ethylene-vinyl acetate copolymer layer and polyamide resin layer or alternatively of polyamide resin layer, polyolefin adhesive resin layer and saponified ethylene-vinyl acetate copolymer layer. The outer and intermediate layers are bonded by adhesive resin. The films are described as having good gas barrier properties and are thus useful for storing food products and chemicals.

Similar products are known from U.S. Pat. No. 4,863,770, U.S. Pat. No. 4,851,272 and U.S. Pat. No. 4,778,699 and all are considered to have good oxygen or gas permeation barriers.

Anaerobic products in the types of container described above have been available commercially for some time. There therefore exists a need to provide a container for anaerobic products which:

(i) confers excellent shelf life stability on anaerobic products;

(ii) may be used to store any one of low, medium or high viscosity products while allowing the product to be dispensed manually or to be dispensed automatically from a dispensing apparatus, without difficulty, and which may be filled to a level where the headspace in the container is minimised; and

(iii) prevents the anaerobic product from escaping from the container, but does not exclude air by permeation into the container i.e. does not provide a substantial barrier to the permeation of air.

A minimal headspace typically does not exceed the volume of the nozzle/cap. However it will be appreciated that achieving a headspace of less than 20% of the container would be a significant improvement over prior art containers, when the shelf-life of the product is not compromised by the minimal headspace.

SUMMARY OF THE INVENTION

The present invention provides a flexible container for anaerobic products comprising at least one wall defining a cavity for receiving and retaining an anaerobic product, the wall being made of a deformable, oxygen permeable material, such that the container is sufficiently flexible to substantially conform to the shape of a further container into which it may be placed.

The flexible container may be made of a thin layer or layers of an oxygen-permeable material such as polyethylene or polypropylene and formed in the shape of a bag. Suitable materials are linear low density polyethylene, very low density polyethylene, high density polyethylene or polypropylene or blends, co-extrusions or laminates of these products. The flexible container may comprise two or more layers of oxygen permeable material. The wall thickness may be at least 50 μm and the permeability of a wall is suitably 25 cm

3

/m

2

.day.bar or greater. The flexible container may be opaque. This is desired where the product is light sensitive.

In another aspect, the invention provides a pack which comprises a flexible and a rigid container. The flexible container may be provided in an outer substantially rigid oxygen permeable container which can hold the flexible container and can retain the flexible container in use in a predetermined shape when containing anaerobic product. The outer container retains the flexible container in its optimum position for allowing oxygen to permeate through to the anaerobic product. This gives an excellent shelf-life while the container in which the adhesive is stored is flexible and allows products to be dispensed easily. The product may be decanted or dispensed irrespective of its viscosity.

A low viscosity anaerobic product contained within the flexible container may be dispensed without removing the flexible container from the outer container if the outer carton is so adapted. In particular the flexible container may be provided with a nozzle which may be opened or closed to dispense the contents of the flexible container.

In one aspect of the invention, the flexible container comprises a plastic bag and the outer container comprises a substantially rigid carton. The carton may comprise paperboard and may be of a flattened or flatpack shape. In other words, one dimension of the pack may be substantially less than the other two dimensions e.g. the width and depth may be greater than the height. Suitably, in use, the outer container retains the flexible container when containing a mass of anaerobic product to a shape in which the distance from any point in the product to a wall is less than or equal to 4 cm.

BRIEF DESCRIPTION OF THE DRAWINGS

FIG. 1

is a perspective view of a flexible container of the invention.

FIG. 2

is a magnified part-sectional view of the flexible container of FIG.

1

.

FIG. 3

is a perspective view of an outer container for the flexible container of FIG.

1

.

FIG. 4

is a sectional view of the flexible container of

FIG. 1

, filled, and enclosed in the outer container of FIG.

3

.

DETAILED DESCRIPTION OF THE DRAWINGS

A flexible container of the invention will now be described with reference to

FIGS. 1

to

4

.

The flexible container is generally designated

1

.

As can be seen from

FIG. 1

the flexible container

1

depicted therein is rectangular in shape. The flexible container

1

is made from thin layers of an oxygen permeable material, which for example may be linear low density polyethylene (LLDPE). LLDPE is air/oxygen permeable. The flexible container

1

has two opposing walls: a first wall

2

and a second wall

3

; each wall formed from two layers of LLDPE. A weld or join

4

runs about the perimeter of the flexible container

1

a short distance from its edges. The weld

4

joins the walls

2

,

3

together to form a sealed bag shape. The flexible container

1

has also a nozzle or spout

8

fitted to the first wall

2

. A flange

7

beneath wall

2

(of

FIG. 4

) supports the nozzle

8

. The flange

7

is sealingly fitted to the first wall

2

by a weld

24

about the flange. The flange

7

and the nozzle

8

are formed as a single piece. The nozzle

8

is fitted with a screw-threaded stopper or cap

10

which is used to retain the product in the flexible container

1

when the flexible container holds product. When empty the flexible container

1

is flat in the configuration of FIG.

1

. It is generally rectangular in shape. It will be appreciated that any given wall of the container may comprise one or more layers. A single layer may comprise one or more plies of material. The most preferred material is plastics material particularly polyethylene or polypropylene. Each wall/layer or ply may be a laminate a co-extruded product, or a blended product.

FIG. 2

shows a side view of the flexible container of FIG.

1

. In particular it can be seen that the first wall

2

comprises two layers

5

,

6

of LLDPE film, while second wall

3

also comprises two layers

11

,

12

. The layers of first wall

2

and the layers

11

,

12

of second walls

3

are held together only by the weld

4

. In particular layers

5

and

6

of the first wall

2

are not bound or sealed together over their surface area. Neither are the layers

11

,

12

of second wall

3

.

FIG. 3

shows a perspective view of an outer container or carton

9

, which is made from paperboard. The container

9

has a base

13

, two side walls

14

,

15

and two end walls

16

,

17

. The container

9

has a paperboard lid

18

comprising two hinged pieces

19

,

20

. The lid

18

is movable between a closed position and an open position. The container

9

has two further tuck-in flaps

21

,

22

which function to hold the lid

18

in a closed position. Other flaps (not shown) may be used to hold the lid in the closed position. The internal height of the outer container should be less than 80 mm, desirably less than 60 mm. In the embodiment described the internal height is approximately 50 mm. The other dimensions of the container

9

are determined by the flexible container

1

as the outer container

9

is adapted to receive the filled or almost filled flexible container

1

. When filled with anaerobic product the flexible container

1

fits snugly within the outer container

9

. The flexible container

1

and the outer container

9

may be of any required shape. Suitably they have complementary shapes. The bottom wall of flexible container

1

fits into the container

9

and in particular rests on base

13

. The flexible container

1

is then constrainable by two perimeters when the outer container

9

is in its closed configuration: the first is the internal perimeter about the width of the outer container

9

; the second is the internal perimeter about the length of the container. The flexible container 1 fits these dimensions within a tolerance of up to 10 mm less than the corresponding dimension of the container. Bulging of flexible container

1

is prevented by the outer container

9

which keeps the product evenly distributed within the flexible container

1

.

The flexible container

1

, filled with anaerobic product, and placed in the outer container

9

(now closed) is shown in FIG.

4

. The two layers

5

,

6

on the top wall

2

and the base wall

3

allow for trapping of any anaerobic product which may weep from the internal cavity of the container

1

, between the layers of each wall.

Known packaging presents a high barrier to air (oxygen) permeability whereas the flexible container

1

of the present invention presents a low barrier.

The outer container

9

retains the flexible container

1

in the shape shown in FIG.

4

. The flexible container

1

is restrained in height by the internal height of outer container

9

i.e. upper wall

2

of flexible carton

1

is restrained by lid

18

while lower wall

2

of flexible container

1

is restrained and supported by base

13

. The flexible container

1

cannot exceed in height the internal height of outer container

9

between lid

18

and base

13

. End walls

16

and

17

of outer container

9

fit snugly against the ends of the flexible container

1

, holding flexible container

1

against movement during transport. Without the outer container

9

the container

1

may become folded, creased or otherwise deformed during transport or storage. The outer container

9

prevents this and also provides a generally rectangular box shape which may be easily stacked, stored and the like. The flexible container

1

is maintained in a generally flat shape, having a relatively large surface area and allowing oxygen to permeate through all of the mass of anaerobic product

23

in the flexible container

1

, as the distance from the walls

2

,

3

to any point in the product is relatively small. The flat shape may be generally referred to as a “flatpack” shape. The flexible container

1

is thus maintained with optimum exposed surface area for permeation of oxygen through the flexible container

1

.

The outer container

9

need not be constructed of oxygen permeable material. It may be made of an impermeable material which allows air into the interior of the container e.g. by providing small apertures in the container etc. The outer container

9

may also be designed to carry a multiple of flexible containers

1

. Each flexible container

1

may be separated from the others by a divider which may be oxygen permeable. Alternatively the flexible containers

1

may be held in a spaced apart arrangement by other means.

The flexible container

1

takes up the shape of a pressure pot dispenser it is placed in. This allows anaerobic product (of low to high viscosity) to be dispensed without direct contact between the anaerobic product and the user. An anaerobic product having low to medium viscosity may also be decanted without removing the flexible container

1

from the outer container

9

. High viscosity anaerobic products may be squeezed by hand from the flexible container

1

or may be dispensed as above. The flexible container

1

may be removed from the outer container

9

before dispensing product therefrom.

The flexible container

1

may be used with a pressure pot dispenser such as that described in International patent application No. PCT/IE97/00015 the disclosure of which is hereby expressly incorporated herein by reference.

The container

1

can be specifically designed to have a snug fit within any of a variety of pressure pot dispensers. In general the circumference of the flexible container

1

when filled with product can be made to match closely the internal dimensions of the cylindrical cavity of any pressure pot dispenser. The nozzle

8

is designed to be held by a collar of the pressure pot dispenser, so that a dispensing nozzle may pierce the cap and allow the anaerobic product to be expressed from the flexible container

1

without the need to remove the cap

10

from the flexible container

1

.

It will be noted that the flexible container

1

is of sufficient flexibility to conform to the shape of a container in which it is placed, provided that the container has dimensions which restrict the shape of the flexible container

1

in some way. For example outer container

9

restricts the height of flexible container

1

, while a pressure pot dispenser may have a cylindrical cavity which conforms the flexible container

1

, at least in cross section, to a generally cylindrical shape. Furthermore the flexible container

1

may be folded, for example folded upon itself by the pressure piston of a pressure pot. Substantially all of the anaerobic adhesive

23

may thus be dispensed from flexible container

1

.

The flexible container

1

of the invention can be of any shape as long as it retained the flatpack shape described above. In particular the flexible container and or the mass of adhesive should have at least one dimension height/width/length which is not greater than about 8 cm. It is most convenient if it is the height of the container which does not exceed 8 cm.

A suitable method for calculating the approximate value to which one dimension of the container would be restricted is to use the formula:

maximum value of restricted dimension=5/9 (Volume of flexible container)

1/3

(i.e. calculate 5/9 of the cubic root of the volume (cm

3

) and take this number as the restricted dimension (cm) e.g. height (cm)).

The flexible container

1

may have side walls of 50 μm or greater thickness. The side walls may comprise a number of layers or plies at least one of which is about 50 μm or greater in thickness. In the embodiment illustrated the flexible container

1

has two plies each of 70 μm thickness.

The flexible container

1

may contain different volumes of product and still have a minimal headspace. It will be appreciated that due to the flexible nature of the flexible container

1

, the headspace can be minimised at any level of fill of product. Air may be expressed from the flexible container

1

so that there is effectively left only the headspace of the internal volume of the nozzle

8

.

When a nominal volume for the flexible container

1

is stated, this is to be taken as the target minimal fill of the flexible container

1

(a minimal fill is requested for manufacturing purposes). The flexible container

1

may have an internal volume which exceeds the nominal volume particularly where the shape of the flexible container

1

is unrestrained and the sides may bulge when being filled. The outer container

9

has a direct bearing on the nominal volume of flexible container

1

as it constrains the flexible container

1

to given dimensions. The flexible container

1

, combined with the restraining forces of the outer container

9

and the internal pressure (due to the volume present) of the anaerobic product are combined in the present invention to provide a flatpack shape for the flexible container

1

when in use i.e. the flexible container 1 does not crease or fold on itself to any substantial degree. A degree of overfill as compared to the nominal volume can be accommodated. The term ‘headspace’ refers to the internal volume of the container which is unoccupied by product and is normally occupied by air. The flexible container

1

may be opaque, translucent or transparent. Where the anaerobic product is light sensitive it may be opaque.

The following examples are provided only for illustrative purposes, and are in no way intended to limit the teaching as set forth herein.

The following abbreviations are used in the following examples:

PE=polyethylene

HDPE=high density polyethylene

LLDPE=linear low density polyethylene

VLDPE=very low density polyethylene

“CUBIC”=cubicontainer product described above (3 liter internal volume)

“5LHDPE”=natural HDPE bottle, rectangular shape, approx. 1 mm thickness having 5 liter capacity

“Black HIDPE”=HDPE bottle, black in colour, round in shape, walls approximately 1 mm in thickness and having a 1.75 liter capacity. The oxygen permeability of the-‘Black HDPE’ is approximately 30 m

3

/m

2

.day.bar.

“Red”=LDPE bottle, red in colour, oval in shape, walls approximately 1 mm thickness, and of 400 ml capacity. The oxygen permeability of the ‘red container’ is 150 cm

3

/m

2

.day.bar.

“Natural LDPE”=LDPE bottle, natural, round in shape, approx. 1 mm in thickness of 1.75 liter capacity.

“LDPE Bag”=LDPE bag (equivalent to flexible container 1), constructed of two layers of 70 μm LLDPE (natural), having a 2 liter capacity.

The word “natural” refers to an uncoloured product i.e. one of natural colour to which no dye has been added.

EXAMPLE 1

Dimensions of Flexible Container 1

EXAMPLE 1.(a): Example of typical dimensions of a flexible container

1

and its outer container

9

are given below:

Construction: Upper and lower walls each 2 ply, formed in a rectangular shape and welded with a 6 mm weld. The outer ply in each case was constructed of PE/HDPE/PE (code A057/1), the inner ply LLDPE (70 μm).

Length and width are measured inside weld to inside weld.

Dimensions of Flexible Container

1

:

Length (cm): 27.5-28.5 Width (cm): 24.5-25.5

Nominal volume (liter): 2

Distance from inside weld to centre of nozzle: from end 4.5 to 5.5 cm: from side 12.3 to 12.7cm

Dimensions of Outer Container

9

:

Length internal (cm): 25.5 Width internal (cm): 32 Height internal (cm): 19.0 Thickness of Walls (cm): 0.3

EXAMPLE 1(b) Example of typical dimensions of a flexible container

1

and its Outer Container

9

are Given below

Construction: Upper and lower walls each 2 ply, formed in a rectangular shape and welded with a 6 mm weld. The outer ply in each case is LLDPE (clear) 70 μm film. The inner ply in each case is LLDPE (clear) 70 μm film. (This flexible container 1 is code A057/3).

Dimensions of flexible container

1

:

Length and width are measured inside weld to inside weld.

Length(cm) 33.5±0.5 Width(cm) 20.0±0.5

Nominal Volume (Liter): 2

Distance from inside weld to centre of nozzle: From end (cm): 5.0±0.5 From side (cm): 10.0±.0.5

Dimensions of outer container

9

:

Length internal (cm): 37.5 Width internal (cm): 14.0

Height internal (cm): 5.0 Thickness of Walls (cm): 10.3

EXAMPLE 2

O

2

Permeability of Material which may be used to Construct Flexible Container 1

TEST MATERIALS: Sample D (code A057/3):clear 70 μm VLDPE/LLDPE blend. Sample E (code A057/1):clear HDPE/LLDPE co-extrusion.

TEST CONDITIONS: 23±1° C., 50±2% rh (relative humidity)

TEST METHOD

ASTM D3985-81, Coulometric method using the Oxtran 2/20 apparatus with computer control. Each specimen was mounted to create a membrane between two chambers. Both chambers were initially flushed with a carrier gas. When steady conditions were established, oxygen was flushed through the upper chamber. The sensor was activated to detect the oxygen that had permeated through the specimen and measurements were taken over the course of several hours until the system had reached equilibrium and constancy in the result was reached. The samples were tested to 1% oxygen in nitrogen and the results are quoted for 100% oxygen, 4 replicate tests per sample.

Oxygen Permeability (cm

3

/m

2

.day.atm)

Mean

Range

Sample D(code A057/3)

2728

2586-2848

Sample E(code A057/1)

1494

1446-1544

EXAMPLE 3(a)

Performance and Stability Testing of Loctite Product No. 121078. Product 121078 is a Single Component Anaerobic Retaining Adhesive Based on an Urethane Methyacrylate Monomer.

1 liter of product 121078 was stored at RT in a 3 liter flexible container

1

which has walls constructed of 2 plies of 70 μm natural LLDPE. The flexible container

1

was inflated with 2 liters 8 as to mimic a 3 liter cubitainer with a 1 liter fill.

On heating at 45° C. for 4.5 months or 3 months the flexible container

1

performed similarly to the cubitainer.

EXAMPLE 3(b)

Loctite product no. 121078: was heat aged at 55° C., 45° C. and 35° C. and was also stored at room temperature in each of the following containers with the specified amount of product 5LHDPE (2 liters of 121078), Black HDPE (1 liter of 121078), Cubic (1 liter of 121078), RED (250 ml) in natural LDPE (1 liter of 121078) and flexible container

1

(2 liter fill). The performance of the product stored in the flexible containers (as above) with a 2 liter fill was similar to that of the product in the 3 liter cubitainer with a 1 liter fill (and again with a two liter headspace of air) and superior to the performance of product stored in the other containers. Failure of the test was judged to have occurred where there was a significant increase in viscosity of the product and/or partial (lumps) or complete gellation of the product.

For the samples heat-aged at 55° C., the cubitainer and the flexible container (

1

) outperformed the other containers containing 1 liter or greater of product. The time to product gellation was approximately sevenfold that the other containers and had a performance similar to the ‘Red’ container above which held only 250 mls of product. At 45° C. the performance of the cubitainer and flexible container gave a time to product gellation in excess of eightfold that of the other containers containing 1 liter or more and similar to that of the ‘Red’ container. At 35° C., with testing not completed, the cubitainer and flexible container had outperformed the other containers containing 1 liter or more by threefold, and again had a performance similar to the ‘Red’ container.

EXAMPLE 4

The pin and collar test was used to determine the shear strength of an adhesive joint of the adhesive between a metal pin and metal collar. The pin and collar test is a standard test in the industry.

Viscosity was determined in the usual way using a Brookfield RVT using the appropriate spindle at two different settings of the revolutions per minute. Viscosity tests on a Brookfield RVT is a standard test.

The percentage weight loss of product was also determined. The pin and collar (P & C) test of the viscosity and weight test were all used to judge the storage characteristics of the containers, by testing the performance of the anaerobic product which was heat aged or stored at room temperature (22° C. in the container).

A series of proprietary products of Loctite (Ireland) Ltd. listed below were each stored in two different 2 liter flexible containers—those of Examples 1(a) and 1(b), (2 liter fill—the headspace was the amount of air in the nozzle

8

). The cubitainer was used as a reference to judge the performance of these products when heat-aged at 45° C. for 7 weeks and 35° C. for 14 weeks. Viscosity measurements, the pin and collar test and weight loss of product were used for comparative tests between products stored in the cubitainer and that stored in identical conditions in each of the flexible containers

1

. For product nos. 275 and 242 the torque strength required to break a coarse threaded nut and bolt when locked together by the product (‘BONB’ test) instead of the pin and collar test. The cubitainer was placed in its standard paperboard carton for each of the tests. The flexible containers were stored, two side by side in a paperboard carton for convenience.

The products tested were as follows:

Viscosity in Cp's @

25° C.

(H) = high viscosity

Loctite Product

(M) = medium viscosity

Reference No.

(L) = low viscosity

Description

121078

Spindle 3, 2.5 rpm

Single component anaerobic

14,000 (H)

adhesive based on urethane

methacrylate monomer.

Used to bond close fitting

metal surfaces.

574

Spindle 6, 2.5 rpm

Dimethacrylate ester

50,000-150,000 (H)

monomers. Single

component, thixotropic

anaerobic sealant. Used as a

form-inplace gasket on rigid

flanged components e.g.

gear box and engine casings

etc.

577

Spindle 5, 2.5 rpm

Dimethacrylate ester

50,000-110,000 (H)

monomer. Single

component, medium

strength thixotropic

anaerobic sealant with fast

curing properties. Used to

seal metal threaded fittings.

573

Spindle 6, 2.5 rpm

Dimethacrylate ester

30,000-90,000

monomer. Single

(H)

component, thixotropic

anaerobic sealant which

develops medium strength.

Used as form-in-place

gasket e.g. gear box and

engine casings etc.

275

Spindle 5, 2.5 rpm

Dimethacrylate ester

17,500-52,500

monomer. A one

(H)

component anaerobic

material which is

thixotropic and has high

strength. Prevents

loosening through vibration

and leakage of threaded

fasteners.

542

Spindle 5, 2.5 rpm

Dimethacrylate ester

925-2775 (M)

monomer. A single

component anaerobic pipe

sealant material. Used to

lock and seal hydraulic and

pneumatic fittings and for

sealing threaded metal

fittings.

242

Spindle 2, 2.5 rpm

Dimethacrylate ester

4,000-8,000 (M)

monomer. A one

component anaerobic

material which is thixotropic

and has medium strength.

Used as a thread locking

composition.

638

Spindle 3, 20 rpm

Urethane methacrylate

1,800-3,300 (M)

monomer. A single

component anaerobic

adhesive which develops

high strength rapidly. Used

for example to lock bushings

and sleeves into housings

and on shafts.

648

Spindle 2, 20 rpm

Urethane methacrylate

400-600 (L)

monomer. Used as a single

component anaerobic

retaining adhesive which

develops high strength

rapidly. Applications

include holding gears and

sprockets onto gearbox

shafts and rotors on electric

motor shafts.

All the above products are available from Loctite (Ireland) Ltd., Dublin, Ireland under the given product reference number. The above products include low, medium and high viscosity products.

The term low viscosity is defined as a material of 0-1000 Cps.

The term medium viscosity is defined as a material of 1,000-10,000 Cps.

The term high viscosity is defined as a material of 10,000-3,000,000 Cps. These viscosity ranges are based on the Brookfield RVT test and on the viscosity measurement taken at the lower revolution per minute figure for the test.

Results

The results of the tests are set out in the following nine tables.

Product 121078 - Stability in 2L Bags

Cubi

A057/3

A057/1

1 Liter

2 Liter

2 Liter

7 Wk at 45 C.

Code

82

85*

88

% Wt Loss

1 Wk

0.34

0.48

0.18

2 Wk

0.63

0.87

0.34

3 Wk

0.88

1.2

0.49

7 Wk

1.45

2.06

0.88

Viscosity (mPas)

#4, 2.5 rpm

8608

8480

8240

#4, 20 rpm

3290

3240

2860

P & C (N/mm2)

15 min

0

0

0

24 Hr

20.7

21.6

21.2

14 Wk at 35 C.

Code

81

84*

87*

% Wt Loss

3 Wk

0.48

0.57

0.99

4 Wk

0.55

0.66

1.05

5 Wk

0.65

0.79

1.11

10 Wk

1.18

1.44

1.45

14 Wk

1.58

1.86

1.66

Viscosity (mPas)

#4, 2.5 rpm

7120

8240

7360

#4, 20 rpm

2920

3050

2980

P & C (N/mm2)

15 min

0

0

5.00

24 Hr

20.08

21.37

20.89

A057/1

Outer Ply PE/HDPE/PE

Inner Ply LLDPE 70 u

A057/3

Outer Ply LDPE 70 u

Inner Ply LLDPE 70 u

Product 574 - Stability in 2L Bags

Cubi

A057/3

A057/1

1 Liter

2 Liter

2 Liter

7 Wk at 45 C.

Code

72

75

78

% Wt Loss

3 Wk

0.68

1.05

0.57

4 Wk

0.85

1.34

0.72

5 Wk

1.02

1.59

0.85

7 Wk

1.27

2

1.08

Viscosity(mPas)

#6, 2.5 rpm

161200

166800

152000

#6, 20 rpm

37600

40200

35600

P & C (N/mm2)

1 Hr

0.40

0.40

0.70

24 Hr

9.24

9.42

9.22

14 Wk at 35 C.

Code

71

74

77

% Wt Loss

3 Wk

0.33

0.49

0.2

4 Wk

0.39

0.56

0.24

5 Wk

0.46

0.65

0.29

10 Wk

0.87

1.16

0.52

14 Wk

1.15

1.44

0.66

Viscosity(mPas)

#6, 2.5 rpm

206400

202000

168000

#6, 20 rpm

41650

44200

42800

P & C (N/mm2)

1 Hr

3.25

3.29

3.3

24 Hr

9.08

8.29

8.94

A057/1

Outer Ply PE/HDPE/PE

Inner Ply LLDPE 70 u

A057/3

Outer Ply LDPE 70 u

Inner Ply LLDPE 70 u

Product 577 - Stability in 2L Bags

Cubi

A057/3

A057/1

1 Liter

2 Liter

2 Liter

7 Wk at 45 C.

Code

62

65

68

% Wt Loss

3 Wk

0.58

0.73

0.51

4 Wk

0.69

0.88

0.66

5 Wk

0.76

1.04

0.77

7 Wk

0.97

1.3

0.96

Viscosity(mPas)

#6, 2.5 rpm

157200

197200

197600

#6, 20 rpm

40350

46950

46000

P & C (N/mm2)

1 Hr

0.70

0.40

0.60

24 Hr

12.34

9.35

12.88

14 Wk at 35 C.

Code

61

64

67

% Wt Loss

3 Wk

0.37

0.27

0.23

4 Wk

0.39

0.32

0.26

5 Wk

0.45

0.37

0.3

10 Wk

0.7

0.64

0.56

14 Wk

0.87

0.79

0.68

Viscosity(mPas)

#6, 2.5 rpm

168400

161600

166400

#6, 20 rpm

33600

37350

38500

P & C (N/mm2)

1 Hr

2.54

3.01

3.1

24 Hr

12.29

12.04

12.43

A057/1

Outer Ply PE/HDPE/PE

Inner Ply LLDPE 70 u

A057/3

Outer Ply LDPE 70 u

Inner Ply LLDPE 70 u

Product 573 - Stability in 2L Bags

Cubi

A057/3

A057/1

1 Liter

2 Liter

2 Liter

7 wk at 45 C.

Code

52

55

58

% Wt Loss

3 Wk

0.11

0.13

0.08

4 Wk

0.13

0.15

0.09

5 Wk

0.15

0.17

0.10

7 Wk

0.17

0.17

0.10

Viscosity(mPas)

#6, 2.5 rpm

54800

51600

41200

#6, 20 rpm

18350

18000

15750

P & C (N/mm2)

6 Hr

0.23

0.25

0.16

24 Hr

1.09

0.82

0.92

14 Wk at 35 C.

Code

51

54

57

% Wt Loss

3 Wk

0.06

0.06

0.04

4 Wk

0.07

0.06

0.04

5 Wk

0.08

0.06

0.04

10 Wk

0.14

0.10

0.07

14 Wk

0.14

0.10

0.08

Viscosity(mPas)

#6, 2.5 rpm

54800

56800

58000

#6, 20 rpm

17550

17400

16450

P & C (N/mm2)

6 Hr

0.54

0.58

0.5

24 Hr

2.62

1.36

1.66

RT

Code

53

56

59

A057/1

Outer Ply PE/HDPE/PE

Inner Ply LLDPE 70 u

A057/3

Outer Ply LDPE 70 u

Inner Ply LLDPE 70 u

Product 275 - Stability in 2L Bags

Cubi

A057/3

A057/1

1 Liter

2 Liter

2 liter

7 Wk at 45 C.

Code

42

45

48*

% Wt Loss

3 Wk

0.36

0.52

0.21

4 Wk

0.44

0.58

0.26

5 Wk

0.51

0.65

0.29

7 wk

0.61

0.76

0.35

Viscosity(mPas)

#5, 2.5 rpm

49600

51840

47840

#5, 20 rpm

8020

8280

8080

BONB

15 min Prevail

2.6

3.0

3.0

1 Hr prevail

19.2

17.6

18.10

24 Hr Prevail

30.4

33.4

23.5

14 Wk at 35 C.

Code

41

44

47

% Wt Loss

3 Wk

0.21

0.27

0.08

4 Wk

0.23

0.31

0.09

5 Wk

0.26

0.34

0.1

10 Wk

0.44

0.53

0.16

14 Wk

0.55

0.61

0.18

Viscosity(mPas)

#5, 2.5 rpm

54400

48640

48480

#5, 20 rpm

8180

7700

7720

BONB (Nm)

15 min Prevail

1.4

1.3

6.1

1 Hr Prevail

23.6

27.2

31.40

24 Hr Prevail

34.2

46.8

42.0

A057/1

Outer Ply PE/HDPE/PE

Inner Ply LLDPE 70 u

A057/3

Outer Ply LDPE 70 u

Inner Ply LLDPE 70 u

Product 542 - Stability in 2L Bags

Cubi

A057/3

A057/1

1 Liter

2 Liter

2 liter

7 Wk at 45 C.

Code

32

35

38

% Wt Loss

1 Wk

0.15

0.29

0.12

2 Wk

0.29

0.48

0.22

3 Wk

0.41

0.62

0.31

7 Wk

0.64

0.95

0.53

Viscosity (mPas)

#2, 2.5 rpm

1968

2352

3072

#2, 20 rpm

656

710

866

P & C (N/mm2)

1 Hr

1.73

1.33

2.1

24 Hr

9.1

8.5

9

14 Wk at 35 C.

Code

31

34

37

% Wt Loss

3 Wk

0.17

0.29

0.12

4 Wk

0.2

0.33

0.15

5 Wk

0.25

0.39

0.18

10 Wk

0.49

0.65

0.34

14 Wk

0.62

0.81

0.41

Viscosity (mPas)

#2, 2.5 rpm

176

224

1056

#2, 20 rpm

160

220

452

P & C (N/mm2)

1 Hr

2.3.6

2.41

2.51

24 Hr

8.7

8.29

8.61

A057/1

Outer Ply PE/HDPE/PE

Inner Ply LLDPE 70 u

A057/3

Outer Ply LDPE 70 u

Inner Ply LLDPE 70 u

Product 242 - Stability in 2L Bags

Cubi

A057/3

A057/1

1 Liter

2 Liter

2 Liter

7 Wk at 45 C.

Code

22

25

28

% Wt Loss

3 Wk

0.19

0.22

0.11

4 Wk

0.25

0.27

0.14

5 Wk

0.28

0.32

0.17

7 Wk

0.36

0.38

0.21

Viscosity(mPas)

#3, 2.5 rpm

2400

3000

2800

#3, 20 rpm

655

800

750

BONB

1 Hr

13

13.8

13.4

4 Hr

16.2

17.6

16.2

24 Hr

20.4

21.4

19.6

14 Wk at 35 C.

Code

21

24

27

% Wt Loss

3 Wk

0.11

0.13

0.05

4 Wk

0.13

0.16

0.06

5 Wk

0.13

0.17

0.07

10 Wk

0.26

0.31

0.15

14 Wk

0.32

0.37

0.19

Viscosity(mPas)

#3, 2.5 rpm

2440

1440

1400

#3, 20 rpm

700

435

9

BONB

1 Hr

12

12.8

13.80

4 Hr

18.7

18.2

17.50

24 Hr

21.3

19.8

20.3

A057/1

Outer Ply PE/HDPE/PE

Inner Ply LLDPE 70 u

A057/3

Outer Ply LDPE 70 u

Inner Ply LLDPE 70 u

Product 638 - Stability in 2L Bags

Cubi

A057/3

A057/1

1 Liter

2 Liter

2 Liter

7 Wk at 45 C.

Code

12

15

18

% Wt Loss

1 Wk

0.38

0.15

0.45

2 Wk

0.70

0.32

0.9

3 Wk

0.97

0.47

1.27

7 Wk

1.69

0.9

2.18

Viscosity (mPas)

#3, 20 rpm

4990

4745

5570

P & C

15 min

0

0

0

24 Hr

28.0

25.2

24.6

14 Wk at 35 C.

Code

11

14

17*

% Wt Loss

3 Wk

0.53

1.56

0.23

4 Wk

0.62

1.65

0.27

5 Wk

0.75

1.77

0.32

10 Wk

1.38

2.41

0.60

14 Wk

1.85

2.85

0.76

Viscosity (mPas)

#3, 20 rpm

4015

4175

3485

P & C (N/mm2)

15 min

11.89

9.89

7.00

24 Hr

24.65

24.47

23.01

A057/1

Outer Ply PE/HDPE/PE

Inner Ply LLDPE 70 u

A057/3

Outer Ply LDPE 70 u

Inner Ply LLDPE 70 u

Product 648 - Stability in 2L Bags

Cubi

A057/3

A057/1

1 Liter

2 Liter

2 Liter

7 Wk at 45 C.

Code

2

5

8*

% Wt Loss

3 Wk

0.99

1.4

0.62

4 Wk

1.30

1.76

0.78

5 Wk

1.51

2.06

0.94

7 Wk

1.89

2.5

1.33

Viscosity (mPas)

#2, 20 rpm

586

606

712

P & C

15 min

0.1

0.1

0

24 Hr

20.68

20.58

21.9

14 Wk at 35 C.

Code

1

4*

7*

% Wt Loss

3 Wk

0.60

0.71

0.28

4 Wk

0.78

0.82

0.31

5 Wk

0.78

0.95

0.38

10 Wk

1.37

1.58

0.70

14 Wk

1.76

1.96

0.91

Viscosity (mPas)

#2, 20 rpm

676

670

600

P & C (N/mm2)

15 min

2.15

3.88

4.95

24 Hr

23.51

23.51

22.88

A0571/

Outer Ply PE/HDPE/PE

Inner Ply LLDPE 70 u

A057/3

Outer Ply LDPE 70 u

Inner Ply LLDPE 70 u

Summary of Results

For all of the above products the cubitainer and the flexible container showed similar performances for all of the tests conducted. In individual tests one of the flexible containers outperformed the other and/or the cubitainer.

Overall the storage capability of the flexible containers and the cubitainers were shown to be similar.

Number	Name	Date	Kind
2895950	Krieble	Jul 1959	A
3046262	Krieble	Jul 1962	A
3173579	Curie et al.	Mar 1965	A
3218305	Krieble	Nov 1965	A
3595465	Vaillancourt	Jul 1971	A
3646723	Meroney	Mar 1972	A
3761013	Schuster	Sep 1973	A
3790067	Scheier	Feb 1974	A
4180640	Melody et al.	Dec 1979	A
4356221	Anthony et al.	Oct 1982	A
4464426	Anthony	Aug 1984	A
4724961	Shimoyamada et al.	Feb 1988	A
4778699	Knox, III et al.	Oct 1988	A
4851272	Knox, III et al.	Jul 1989	A
4863770	Knox, III et al.	Sep 1989	A
5246114	Underwood	Sep 1993	A

Number	Date	Country
27 14 537	Oct 1978	DE
0 172 711	Feb 1986	EP
0 352 143	Jan 1990	EP
0 590 465	Sep 1993	EP
2 717 781	Sep 1995	FR
07 701 002	Apr 1995	JP
09 087 395	Mar 1997	JP
9601766	Jan 1996	WO
9732807	Sep 1997	WO

Container for anaerobic products

Information

Patent Number

Date Filed

Date Issued

Inventors

Original Assignees

Examiners

Agents

CPC

US Classifications

Field of Search

US

International Classifications

Abstract

Description

Claims

Priority Claims (1)

PCT Information

US Referenced Citations (16)

Foreign Referenced Citations (9)

Non-Patent Literature Citations (1)