JP2020158197A - Method of filling curable composition - Google Patents

Abstract

To improve storage stability of a curable composition filled (accommodated) in a container by preventing a gap between the curable composition filled (accommodated) in an outer peripheral edge part of a can body and a moisture prevention film.SOLUTION: A method for filling a curable composition includes the steps of: filling a hermetically sealable container with a curable composition; laying a moisture prevention film on the surface of the curable composition; pressing the moisture prevention film by a push plate with a convex bottom surface to integrate the moisture prevention film with the curable composition; and sealing a container with a lid.SELECTED DRAWING: Figure 1

Description

The present invention relates to a method for filling a container with a curable composition.

Curable compositions are used as sealants, adhesives and putty materials for construction, civil engineering and automobiles. These curable compositions are prepared by blending a curable resin such as an isocyanate group-containing resin or a crosslinkable silyl group-containing resin with additives such as a curing catalyst, a filler, and a rocking denaturing agent. The curable composition is stored in a closed container such as a cartridge or a pail can in consideration of its usage.

For example, when the curable composition is stored in a pail, a film is laid on the surface of the curable composition in order to block the curable composition from the outside air (moisture), and then the container body and the lid are fitted and sealed. (For example, Patent Documents 1 and 2). These prior arts disclose the contained curable composition and methods for blocking moisture in the air. Specifically, in Patent Document 1, the surface of the curable composition is covered with a moisture blocking film to form a sealing surface on the peripheral edge of the film to block moisture, and in Patent Document 2, the surface of the curable composition is covered. While covering with a moisture-blocking film, the vicinity of the peripheral edge of the film is intentionally exposed to moisture in the air to form a cured product having sealing performance, and the moisture-blocking film and the cured product block the moisture in the air. The methods described in these prior arts are effective in blocking the curable composition and moisture.

Since the curable composition used for a sealing material, an adhesive, a putty material, etc. is generally a viscous material having thixotropic properties, when the surface of the curable composition is covered with a moisture blocking film. If the pressing by a pressing plate or the like is insufficient, a gap may be formed between the peripheral edge of the moisture-blocking film and the curable composition (the peripheral edge in the container). Further, even when the pressing is sufficient and no voids are formed between the peripheral edge portion of the moisture-blocking film and the curable composition, voids are generated over time and the curable composition in the void portion is thickened. It may be hardened in a ring shape, so improvement is necessary.

Japanese Unexamined Patent Publication No. 3-162269 Japanese Unexamined Patent Publication No. 9-150866

In view of the above problems, the present invention prevents the formation of voids between the filled (stored) curable composition and the moisture-proof film at the peripheral edge of the container, and the curable composition at the voids. It is an object of the present invention to provide a method for filling a curable composition, which can prevent the film from thickening or hardening in a ring shape.

As a result of diligent research, the present inventors have conducted a step of filling a sealable container with a curable composition, a step of laying a moisture-proof film on the surface of the curable composition, and a push plate having a convex portion on the bottom surface. By a method of filling the curable composition, which comprises a step of pressing the curable composition with a lid to integrate the moisture-proof film and the curable composition and a step of sealing the container with a lid, the container is filled at the peripheral edge of the container. It was found that it is possible to prevent the formation of voids between the (stored) curable composition and the moisture-proof film. That is, the present invention is the embodiment shown in the following (1) to (14).

(1) A step of filling a sealable container with a curable composition and
The process of laying a moisture-proof film on the surface of the curable composition and
A step of pressing the moisture-proof film with the push plate with the convex portion of the push plate having a convex portion on the bottom surface facing the moisture-proof film to integrate the moisture-proof film and the curable composition. When,
The process of sealing the container with a lid,
A method for filling a curable composition containing.
(2) The filling method according to (1), wherein the convex portion is a curved surface portion formed in a side view arc shape on the entire bottom surface.
(3) The convex portion forms a curved surface region having an arc shape in a side view formed on the peripheral edge of the bottom surface and a flat region having a linear side view formed from the peripheral edge of the bottom surface to the central portion continuous from the curved surface region. The filling method according to (1).
(4) A side surface in which the convex portion is formed from a side view arc-shaped first curved surface region formed on the peripheral edge of the bottom surface and from the peripheral edge to the central portion of the bottom surface continuous from the first curved surface region. The filling method according to (1), which has a second curved surface region having a side view arc shape, which has a radius of curvature larger than the radius of curvature of the first curved surface region having a visual arc shape.
(5) The sealable container has a cylindrical, elliptical or square tubular shape with the lower surface as the bottom surface, an opening is provided in the upper portion of the container, and the opening and the lid are fitted to each other. The filling method according to any one of (1) to (4), which provides a sealable container.
(6) The filling method according to any one of (1) to (5), wherein the moisture-proof film is a composite film of aluminum and resin.
(7) The filling method according to any one of (1) to (6), wherein the strength of the moisture-proof film measured in the tensile performance test is 20 to 100 N / mm ² .
(8) The filling method according to any one of (1) to (7), wherein the elongation of the moisture-proof film measured in the tensile performance test is 5% or more.
(9) The filling method according to any one of (1) to (8), wherein the viscosity at 25 ° C. measured at 1 rpm using an E-type viscometer of the curable composition is 150 to 400 Pa · s.
(10) The filling method according to any one of (1) to (9), wherein the thixotropic index at 25 ° C. measured at 1 rpm / 10 rpm using an E-type viscometer of the curable composition is 3 to 6. ..
(11) By the step of integrating the moisture-proof film and the curable composition, the moisture-proof film and the curable composition are integrated, and the curable composition is shielded from moisture (1) to (1). The filling method according to any one of 10).
(12) By the step of integrating the moisture-proof film and the curable composition, the moisture-proof film and the curable composition are integrated, the curable composition is shielded from moisture, and the moisture-prevention is prevented. The filling method according to any one of (1) to (11), wherein the film is brought into close contact with the inner peripheral side surface of the sealable container in whole or in part.
(13) By the step of integrating the moisture-proof film and the curable composition, the moisture-proof film and the curable composition are integrated, the curable composition is shielded from moisture, and the moisture-prevention is prevented. The filling method according to any one of (1) to (12), wherein the film and the curable composition become convex toward the bottom surface of the container.
(14) A structure in which the curable composition is filled in a sealable container by the filling method according to any one of (1) to (13), and the container is sealed by the lid.

In the above aspect, the "side view" means a state in which the push plate is visually recognized from the vertical direction with respect to the pushing direction.

According to the method for filling the curable composition of the present invention, it is possible to prevent the formation of voids between the filled (stored) curable composition and the moisture-proof film at the peripheral edge of the container, so that the voids are curable. It is possible to prevent the composition from thickening or hardening into a ring shape. Therefore, the storage stability of the curable composition filled (stored) in the container is improved.

It is a side sectional view of the push plate which concerns on 1st Embodiment used in the filling method of the curable composition of this invention. It is a side sectional view of the push plate which concerns on 2nd Embodiment used in the filling method of the curable composition of this invention. It is a side sectional view of the push plate which concerns on 3rd Embodiment used in the filling method of the curable composition of this invention. It is a side sectional view which shows the procedure 1 of the filling method of the curable composition of this invention. It is a side sectional view which shows the procedure 2 of the filling method of the curable composition of this invention. It is a side sectional view which shows the procedure 3 of the filling method of the curable composition of this invention. It is a side sectional view which shows the procedure 4 of the filling method of the curable composition of this invention. It is a side sectional view which shows the procedure 5 of the filling method of the curable composition of this invention. It is a side sectional view which shows the sealed structure of the curable composition which was filled by the filling method of the curable composition of this invention using the push plate which concerns on 1st Embodiment. It is a side sectional view which shows the sealed structure of the curable composition which was filled by the filling method of the curable composition of this invention using the push plate which concerns on 2nd Embodiment. It is a side sectional view which shows the sealed structure of the curable composition which was filled by the filling method of the curable composition of this invention using the push plate which concerns on 3rd Embodiment.

First, a push plate having a convex portion on the bottom surface used in the method for filling the curable composition of the present invention will be described with reference to FIGS. 1 to 3. For the push plate having a convex portion on the bottom surface shown in FIGS. 1 to 3, a moisture-proof film is laid on the surface of the push plate after filling (storing) the curable composition in a sealable container, and the moisture-proof film is pressed by the push plate. The surface of the curable composition is covered with a moisture-proof film by being integrated with the curable composition, and the curable composition is used to shield the curable composition from moisture in the air. In the present specification, the shielding from moisture by the moisture-proof film means that the moisture-proof film does not completely permeate the moisture, or even if the moisture permeates, the curable composition is significantly thickened or cured. Means a state in which can be prevented.

First, the push plate according to the first embodiment will be described. FIG. 1 is a side sectional view of a push plate according to a first embodiment used in the method for filling a curable composition of the present invention. As shown in FIG. 1, the push plate 18 according to the first embodiment is attached to the bottom surface 1, the top surface 12 facing the bottom surface 1, the side surface 2 connecting the bottom surface 1 and the top surface 12, and the top surface 12. It has a handle 3. The bottom surface 1 is provided with a convex portion 13 projecting in the direction opposite to the top surface 12. As will be described later, the convex portion 13 of the push plate 18 is in a state of facing the moisture prevention film (not shown in FIG. 1), and the moisture prevention film is pressed by the push plate 18.

In the push plate 18, the convex portion 13 is a curved surface portion 14 formed in a side view arc shape on the entire bottom surface 1. That is, the entire bottom surface 1 is a curved surface, and the bottom surface 1 has a substantially convex arc shape (curved shape) from the central portion 15 toward the outer peripheral edge 16. The radius of curvature of the convex portion 13 which is arcuate in the side view is substantially the same over the entire bottom surface 1. From the above, the central portion 15 of the bottom surface 1 is in the most protruding mode. The radius of curvature of the convex portion 13 having an arcuate side view is not particularly limited, but is, for example, 50 to 15000 mm, preferably 100 to 7000 mm.

The shape of the upper surface 12 facing the bottom surface 1 is not particularly limited, but the entire upper surface 12 of the push plate 18 is flat. At the center of the upper surface 12, the push plate 18 is carried to the place of the moisture-proof film in the container, the moisture-proof film is pressed, and the handle 3 gripped by the operator when the push plate 18 is separated from the moisture-proof film. Is provided. The handle 3 improves the convenience of the above work.

As shown in FIG. 1, the side surface 2 connecting the bottom surface 1 and the top surface 12 is provided along the outer peripheral edge 16 of the bottom surface 1. The side surface 2 is provided perpendicular to the upper surface 12 in the direction of the upper surface 12 from the outer peripheral edge 16 of the bottom surface 1.

Next, the push plate according to the second embodiment will be described. FIG. 2 is a side sectional view of a push plate according to a second embodiment used in the method for filling the curable composition of the present invention. The same components as the push plate according to the first embodiment will be described with reference to the same reference numerals.

In the push plate 18 according to the first embodiment, the convex portion 13 is a curved surface portion 14 formed in a side view arc shape on the entire bottom surface 1. Instead of this, in the push plate 28 according to the second embodiment, as shown in FIG. 2, the convex portion 23 formed on the bottom surface 1 has a side view arc shape formed on the peripheral edge 26 of the bottom surface 1. It has a curved surface region 21 and a flat region 22 having a linear side view formed from the peripheral edge 26 of the bottom surface 1 continuous from the curved surface region 21 to the central portion 25. In the push plate 28, only the curved surface region 21 is a curved surface portion. Therefore, in the push plate 28, only the peripheral edge 26 of the bottom surface 1 is a curved surface portion, and only the peripheral edge 16 of the bottom surface 1 is arcuate (curved). Since the peripheral edge 26 of the bottom surface 1 is the curved surface region 21, the convex portion 23 is formed on the bottom surface 1. The radius of curvature of the peripheral edge 26, which is arcuate in side view, is substantially the same. The radius of curvature of the curved surface region 21 having a side view arc shape is not particularly limited, but is preferably 10 to 26 mm, for example.

On the other hand, the flat region 22 is a flat surface (flat portion), and the central portion 25 of the bottom surface 1 is flat. The flat region 22 is parallel to the upper surface 12, which is also a flat surface. From the above, the bottom surface 1 has a substantially convex shape from the central portion 25 toward the peripheral edge 26. The range of the curved surface region 21 is not particularly limited, but has, for example, an area of 10% or more and 50% or less with respect to the total area of the bottom surface 1.

Next, the push plate according to the third embodiment will be described. FIG. 3 is a side sectional view of a push plate according to a third embodiment used in the method for filling the curable composition of the present invention. The same components as the push plate according to the first and second embodiments will be described with reference to the same reference numerals.

In the push plate 18 according to the first embodiment, the convex portion 13 is a curved surface portion 14 formed in a side view arc shape on the entire bottom surface 1, and the radius of curvature of the convex portion 13 is substantially the same over the entire bottom surface 1. It was. Instead of this, in the push plate 38 according to the third embodiment, as shown in FIG. 3, the convex portion 33 is formed on the peripheral edge 36 of the bottom surface 1, and the side view arc-shaped first curved surface region 31 A side view arc shape having a radius of curvature larger than the radius of curvature of the side view arc shape first curved surface region 31 formed from the peripheral edge 36 of the bottom surface 1 continuous from the first curved surface region 31 to the central portion 35. It has a second curved surface region 32 of the above. Both the first curved surface region 31 and the second curved surface region 32 are curved surface portions formed on the bottom surface 1.

That is, in the push plate 38, the entire bottom surface 1 is a curved surface, but the degree of bending of the peripheral edge 36 of the bottom surface 1 is larger than the degree of bending of the central portion 35. The radius of curvature of the first curved surface region 31 which is arcuate in the side view is substantially the same over the entire first curved surface region 31. Further, the radius of curvature of the second curved surface region 32 having a side view arc shape is substantially the same over the entire second curved surface region 32. From the above, even in the push plate 38, the central portion 35 of the bottom surface 1 is in the most protruding mode. The radius of curvature of the first curved surface region 31 having a side view arc shape is not particularly limited, but is preferably 10 to 26 mm, for example. The radius of curvature of the second curved surface region 32 having a side view arc shape is not particularly limited, but is, for example, 50 to 15000 mm, preferably 100 to 7000 mm.

The range of the first curved surface region 31 is not particularly limited, but has, for example, an area of 10% or more and 50% or less with respect to the area of the entire bottom surface 1.

The shape of the handle 3 is not particularly limited as long as the push plates 18, 28, and 38 can be carried and pressed, and can be a known shape.

The diameter of the bottom surface 1 of the push plates 18, 28, 38 is preferably 1 to 20 mm smaller than the inner diameter of the container (for example, a can body) for filling (storing) the curable composition, and particularly 1 to 10 mm smaller. Is preferable. In the case of a tapered can in which the inner diameter of the container decreases from the opening toward the bottom surface, it is pressed by the pressing plates 18, 28, 38 with respect to the inner diameter of the container at the position where the curable composition and the moisture-proof film are integrated. , 1 to 20 mm smaller, and particularly preferably 1 to 10 mm smaller.

If the material of the push plates 18, 28, 38 can press the moisture-proof film, integrate the moisture-proof film and the curable composition, and cover the surface of the curable composition with the moisture-proof film. There are no particular restrictions. Examples of the materials of the push plates 18, 28 and 38 include aluminum, stainless steel, iron, copper, porcelain, pottery, ceramics, wood, natural stone, artificial stone, concrete, glass, plastic and hard paper.

Next, the filling method of the curable composition of the present invention will be described in accordance with the procedure with reference to FIGS. 4 to 8. The procedure for filling the curable composition shown below is an example, and the present invention is not construed as being limited to this procedure. Further, here, for convenience of explanation, the push plate 18 according to the first embodiment will be used as the push plate.

Procedure 1 of the filling method of the curable composition
FIG. 4 shows a side sectional view of the concept of installing a filling nozzle 5 capable of discharging the curable composition 6 in a sealable can body 4 (container body). The filling nozzle 5 is preferably installed on the center of the bottom surface of the can body 4. In this case, when the curable composition 6 is discharged from the filling nozzle 5, the curable composition is filled (stored) in the can body 4 without bias. The can body 4 can be placed on a weighing device (not shown) and weighed while filling the can body 4 with the curable composition.

Procedure 2 of the filling method of the curable composition
FIG. 5 shows a side sectional view of the concept of filling (storing) the curable composition 6 into a sealable can body 4 (container body) via a filling nozzle 5 that can be discharged. A weighing device (not shown) on which the can body 4 is installed can be interlocked with a discharge control device (not shown) of the filling nozzle 5 to automatically fill the curable composition 6 to a preset capacity. it can. Further, a flow meter can be installed in the filling nozzle 5 to automatically fill the curable composition 6 so as to have a preset capacity.

Procedure 3 of the filling method of the curable composition
FIG. 6 shows a side sectional view of a concept in which a curable composition 6 is filled (stored) in a sealable can body 4 (container body) and a moisture-proof film 7 is laid on the surface of the curable composition 6. It is a thing. The moisture-proof film 7 is laid so that the (flat) center of the moisture-proof film 7 coincides with the center of the bottom surface of the can body 4. The size of the moisture-proof film 7 may be the same as the inner diameter of the can body 4, or may be larger than the inner diameter of the can body 4.

Procedure 4 of the filling method of the curable composition
In FIG. 7, the curable composition 6 is filled (stored) in a sealable can body 4 (container body), and the moisture-proof film 7 and the curable composition 6 laid on the surface of the curable composition 6 are pressed. It is a side sectional view of the concept of integrating the moisture-proof film 7 and the curable composition 6 by pressing with a plate 18. The moisture-proof film is pressed by the push plate 18 with the convex portion 13 of the push plate 18 facing the moisture-proof film 7. It is preferable that the pressing plate 18 is carefully pressed so that no gap is formed between the moisture-proof film 7 and the curable composition 6. As shown in FIG. 7, when the size of the moisture-proof film 7 is larger than the inner diameter of the can body 4, the moisture-proof film 7 bends along the side surface 2 of the push plate 18 when pressed by the push plate 18, and the moisture is prevented. The prevention film 7 is in close contact with the inner peripheral side surface of the can body 4 in whole or in part. When the moisture-preventing film 7 is in close contact with the inner peripheral side surface of the can body 4, the effect of preventing the curable composition 6 from moisture in the air is enhanced. Therefore, when the moisture-preventing film 7 is pressed by the pressing plate 18, the pressing plate 18 is pressed. It is preferable that the bent moisture-proof film 7 is brought into contact with the inner peripheral side surface of the can body 4 and the moisture-proof film 7 and the inner peripheral side surface of the can body 4 are brought into close contact with each other. If the moisture-preventing film 7 bent after pressing the moisture-preventing film 7 with the push plate 18 and the inner peripheral side surface of the can body 4 are not sufficiently adhered to each other, the moisture-proof film 7 is used with a tool such as a finger touch or a spatula. It is preferable that the inner peripheral side surface of the can body 4 is brought into close contact with the can body 4.

If it is difficult to bring the moisture-proof film 7 and the inner peripheral side surface of the can body into close contact with each other, insert a liquid substance between the moisture-proof film 7 and the inner peripheral side surface of the can body 4 to the extent that moisture in the air can be blocked. You can also do it. The liquid material is preferably a compound that does not react with water such as the curable composition 6 and moisture. As a liquid substance, a plasticizer such as a phthalate ester or an adipate ester, a polyoxyalkylene polyol having a number average molecular weight of 300 to 5,000, or a hydroxyl group of a polyoxyalkylene monool is reacted with an isocyanate compound or a carboxylic acid compound. Examples thereof include urethanized and esterified resins. Further, instead of the above liquid material, heavy calcium carbonate, fatty acid surface-treated calcium carbonate, fine powder silica and the like may be mixed with these plasticizers and resins and mixed uniformly to form a paste. .. The number average molecular weight in the present specification is a polystyrene-equivalent value measured by gel permeation chromatography (GPC).

Step 5 of the filling method of the curable composition
FIG. 8 shows a can body 4 (container) in which the curable composition 6 is filled (stored) in a sealable can body 4 (container body) and the surface of the curable composition 6 is integrated with a moisture-proof film 7. The side sectional view of the concept of fitting the main body) and the can lid 9 provided with the seal 10 is shown. The moisture-proof film 7 and the curable composition 6 laid on the surface of the curable composition 6 are pressed by the pressing plate 18 to integrate the moisture-proof film 7 and the curable composition 6, and then the pressing plate 18 is pressed. The lid can 9 is attached to the can body 4 away from the moisture-proof film 7. The can body 4 has a sealed structure by being fitted with the can lid 9 via the seal 10. Before fitting the can body 4 and the can lid 9 through the seal 10, dry air or dry nitrogen is blown into the can body 4 using an air gun or the like to and the air (including moisture) in the can body 4. Can be replaced.

FIG. 9 is an example of a side sectional view showing a sealed structure of the curable composition 6 packed by the filling method of the present invention. The sealed structure of FIG. 9 uses the push plate 18 according to the first embodiment shown in FIG. In FIG. 9, the surface of the curable composition 6 and the moisture-preventing film 7 pressed and integrated by the push plate 18 facing the can lid 9 has a shape corresponding to the shape of the convex portion 13 of the push plate 18, and the can. It becomes a substantially convex arc shape toward the bottom surface of the body 4. A desiccant 11 is placed on the moisture-preventing film 7 for the purpose of removing moisture in the air.

FIG. 10 is an example of a side sectional view showing a sealed structure of the curable composition 6 packed by the filling method of the present invention. FIG. 10 uses the push plate 28 according to the second embodiment shown in FIG. In FIG. 10, the surface of the curable composition 6 and the moisture-preventing film 7 pressed and integrated by the push plate 28 facing the can lid 9 has a shape corresponding to the shape of the convex portion 23 of the push plate 28.

FIG. 11 is an example of a side sectional view showing a sealed structure of the curable composition 6 packed by the filling method of the present invention. FIG. 11 uses the push plate 38 according to the third embodiment shown in FIG. In FIG. 11, the surface of the curable composition 6 and the moisture-preventing film 7 pressed and integrated by the push plate 38 facing the can lid 9 has a shape corresponding to the shape of the convex portion 33 of the push plate 38.

By the method of filling the curable composition shown in FIGS. 4 to 8, it is possible to prevent the gap between the curable composition 6 and the moisture-preventing film 7 generated at the peripheral edge of the can body 4. By preventing the generation of voids, it is possible to prevent the thickeners and cured products of the curable composition from being generated around the voids, so that the storage stability of the curable composition filled (stored) in the container is improved.

The mechanism of generation of voids between the curable composition and the moisture-proof film generated at the peripheral edge of the can body (container body) is presumed to be as follows. The curable composition that is filled (stored) in the can body is often higher than the outside air temperature of the filling work place in order to ensure fluidity during filling. After filling the curable composition and sealing the can body with a can lid, the curable composition cools from the peripheral edge of the can body to cause volume shrinkage. At this time, if the moisture-proof film integrated with the curable composition cannot follow the volume shrinkage of the curable composition, voids are likely to occur between the curable composition and the moisture-proof film at the peripheral edge of the can body. Become. There is also a method of softening the moisture-proof film to prevent the generation of voids, but if the moisture-proof film is softened, the handling when laying the moisture-proof film on the surface of the curable composition is poor and the pressure is pressed with a push plate. In some cases, the moisture-proof film may wrinkle. Further, if the thickness of the film is reduced in order to soften the moisture-proof film, the moisture-proof performance of the film is deteriorated, which is not preferable.

On the other hand, when the method for filling the curable composition of the present invention is used, the integrated curable composition and the moisture-proof film have a shape having a convex portion toward the bottom surface of the can body, that is, a convex portion of the push plate. Since it has a recess corresponding to the shape of the can and the peripheral edge of the recess rises toward the upper surface of the can body, it is necessary to prevent voids in the peripheral edge of the can body caused by volume shrinkage of the curable composition. Can be done.

The shape of the can body 4 (container body) is not particularly limited as long as it can be filled (stored) with the curable composition 6 and sealed using the can lid 9. Specifically, for example, the lower part of the can body 4 is the bottom surface because the curable composition 6 can be easily filled, easily obtained and transported, and the workability when using the curable composition 6 is easy. A cylindrical shape, an elliptical tubular shape, or a square tubular shape having a bottom surface and an open upper portion (ceiling surface) of the can body 4 can be mentioned.

The material of the can body 4 (container body) is particularly limited as long as it can be filled (stored) with the curable composition 6, sealed with the can lid 9, and then blocked from the outside air (particularly moisture such as humidity). Can be used without. Specific examples thereof include metals such as aluminum, iron, stainless steel, tin and copper, and resins such as polyethylene, polypropylene, polyamide, polyethylene terephthalate, polycarbonate and polyvinyl chloride.

A release agent may be applied to the inner peripheral side surface (inner wall surface) of the can body 4 (container body) to provide a release layer. Examples of the release agent include natural waxes such as carnauba wax, mitsuro, and paraffin wax, polyolefin-based resins such as polyethylene and polypropylene, stearic acid amide, silicone-based or fluorine-based resins. By providing the release layer, the aluminum film 7 in close contact with the inner peripheral side surface of the can body 4 (container body) can be easily peeled off.

A handle such as a wire bracelet or a plast bracelet may be provided on the outer peripheral side surface (outer wall surface) of the can body 4 (container body) in order to facilitate the carrying of the can body 4.

The shape of the can lid 9 is not particularly limited as long as it has a structure that can be fitted and sealed with the can body 4 (container body) filled (stored) with the curable composition 6. Specifically, for example, the top plate portion of the can lid 9 is flat and has a side surface substantially perpendicular to the peripheral edge portion thereof. The can lid 9 may be provided with a seal 10 on the inner peripheral edge of the side surface of the can lid 9 so that the can lid 9 can be fitted with the can body 4. In this case, the outer peripheral side surface (outer wall surface) of the opening of the can body 4 (container body) and the seal 10 are in close contact with each other to form a sealed structure in which the inside of the can body 4 is shielded from the outside air (moisture in the air).

Examples of the material of the can lid 9 include the same materials as those of the can body 4 (container body). The same material may be used for the can lid 9 and the can body 4, or different materials may be used.

Examples of the moisture-proof film 7 include an aluminum single-layer film and a composite film of aluminum and resin. A composite film of aluminum and resin is preferable because it has a good balance between moisture-proof performance, strength and elongation. Resins that can be used for the composite film of aluminum and resin include low density polyethylene (LDPE), linear low density polyethylene (L-LDPE), high density polyethylene (HDPE), nylon (NY), and polyethylene terephthalate (PET). Can be mentioned. These can be used alone or in combination of two or more.

The thickness of the moisture-proof film 7 is not particularly limited, but is preferably 30 to 200 μm, and particularly preferably 50 to 150 μm. When the moisture-proof film 7 is a composite film of aluminum and resin, the thickness of aluminum in the composite film is preferably 5 to 50 μm, particularly preferably 5 to 40 μm.

The strength of the moisture-proof film 7 is preferably ²⁰ to 100 N / mm ² , and particularly preferably 30 to 80 N / mm ² . The strength of the moisture-proof film in the present specification is a numerical value of the maximum point strength measured in the tensile performance test.

The elongation of the moisture-proof film 7 is preferably 5% or more, more preferably 10 to 50%, and particularly preferably 15 to 50%. The elongation of the moisture-proof film in the present specification is a numerical value of the maximum point elongation measured in a tensile performance test.

Regarding the strength and elongation of the moisture-proof film 7, the dumbbell-shaped No. 4 shape specified in JIS K 6251 "Tensile test method for vulcanized rubber (1993)" was prepared using the moisture-proof film 7 at 23 ° C. 50. It means the strength and elongation measured at a speed of 500 mm / min in an environment of% RH. The thickness of the dumbbell-shaped No. 4 shape was the thickness of the moisture-proof film 7.

When the strength and elongation of the moisture-proof film 7 are within the above ranges, the moisture-proof film 7 is laid on the surface of the curable composition 6 and pressed by the pressing plates 18, 28, 38 to cure the moisture-proof film 7. When the composition 6 is integrated, wrinkles are less likely to occur in the moisture-proof film 7, and voids are less likely to be generated between the curable composition 6 and the moisture-proof film 7. Further, even if the curable composition 6 shrinks in volume due to the outside air temperature after the container such as the can body 4 is filled with the curable composition 6, it is easy to follow the volume change and suppress the generation of voids in the peripheral portion in the container. it can.

Examples of the curable composition 6 include a urethane-based curable composition, a modified silicone-based curable composition, and a polysulfide-based curable composition.

The urethane-based curable composition is a composition containing an isocyanate group-containing resin as a curable resin. The isocyanate group-containing resin is a resin having one or more isocyanate groups in the resin, and the isocyanate groups react with active hydrogen (groups) to form urethane bonds, urea bonds, and the like, and cross-linking and curing. As the isocyanate group-containing resin, an isocyanate group-containing urethane prepolymer can be preferably mentioned. The isocyanate group-containing urethane prepolymer comprises an organic isocyanate compound and an active hydrogen-containing compound in a range in which the molar ratio of isocyanate group / active hydrogen is preferably 1.2 to 10 and more preferably 1.2 to 5.0. It can be produced by reacting all at once or sequentially so that the isocyanate group remains in the urethane prepolymer.

The modified silicone-based curable composition is a composition containing a crosslinkable silyl group-containing resin as a curable resin. The crosslinkable silyl group-containing resin is a resin having one or more crosslinkable (hydrolytable) silyl groups in the resin, and the crosslinkable silyl group reacts with an active hydrogen (group) to form a siloxane bond. Crosslink and cure.

（式中、Ｒは炭化水素基であり、炭素数１〜２０のアルキル基、炭素数６〜２０のアリール基または炭素数７〜２０のアラルキル基が好ましく、メチル基が最も好ましい。Ｘで示される反応性基はハロゲン原子、水素原子、水酸基、アルコキシ基、アシルオキシ基、ケトキシメート基、アミド基、酸アミド基、メルカプト基、アルケニルオキシ基およびアミノオキシ基より選ばれる加水分解性の基であり、Ｘが複数の場合には、Ｘは同じ基であっても異なった基であってもよい。このうちＸはアルコキシ基が好ましく、メトキシ基またはエトキシ基が特に好ましい。ａは０、１または２の整数であり、０または１が特に好ましい。） From the viewpoint of curability and physical properties after curing of the modified silicone-based curable composition, the crosslinkable silyl group is preferably contained in an amount of 1 or more, and more preferably 1 to 5, particularly 1 It is preferable that ~ 3 pieces are contained. Further, the crosslinkable silyl group is preferably one represented by the following general formula, which is easy to crosslink and easy to produce.

(In the formula, R is a hydrocarbon group, preferably an alkyl group having 1 to 20 carbon atoms, an aryl group having 6 to 20 carbon atoms or an aralkyl group having 7 to 20 carbon atoms, and most preferably a methyl group. Reactive groups are hydrolyzable groups selected from halogen atoms, hydrogen atoms, hydroxyl groups, alkoxy groups, acyloxy groups, ketoximate groups, amide groups, acid amide groups, mercapto groups, alkenyloxy groups and aminooxy groups. When there are a plurality of Xs, X may be the same group or different groups. Of these, X is preferably an alkoxy group, particularly preferably a methoxy group or an ethoxy group. A is 0, 1 or 2. It is an integer of 0 or 1 is particularly preferable.)

The main chain of the crosslinkable silyl group-containing resin is a polyoxyalkylene polymer or a polyoxyalkylene polymer which may be (meth) acrylic modified from the viewpoint of tensile adhesiveness after curing and rubber properties such as modulus. , (Meta) acrylic copolymer is preferable.

In the present invention, "may be (meth) acrylic modified" means a polyoxyalkylene polymer obtained by blocking or pendant copolymerizing a (meth) acrylic monomer, or a polyoxyalkylene polymer. It means a mixture of a (meth) acrylic copolymer and a polymer of a (meth) acrylic monomer in a polyoxyalkylene polymer having a crosslinkable silyl group introduced therein.

The polysulfide-based curable composition is a composition containing a polysulfide resin as a curable resin. Polysulfide resin is a polymer having a polysulfide skeleton and a mercapto group at the end. The polysulfide resin having a mercapto group at the end preferably has a structure represented by the general formula: HS- (R'/-Sy) z-R "-SH. In this general formula, y is an integer of 1 to 4. The average value thereof is 1.5 to 2.5. Z is 1 to 120, preferably 6 to 50. Further, R'and R "in this general formula are divalent fats. a family hydrocarbon group, and specific _{examples, -C 2 H 4 -, -} C 3 H 6 -, - C 4 H 8 - and the like. Those having an ether bond are particularly preferable, and specific examples thereof include the following.
_{-C 2 H 4 -O-C 2} H 4 -
-C ₃ H ₆ -O-C ₃ H _{6-
-C 4 H 8 -O-C 4} H 8 -
_{-C 2 H 4 -O-CH 2} -O-C 2 H 4 -
-C ₃ H ₆ -O-CH _2- O-C ₃ H _{6-
-C 4 H 8 -O-CH 2} -O-C 4 H 8 -

In the urethane-based curable composition, the modified silicone-based curable composition, and the polysulfide-based curable composition, additives can be further added as necessary in addition to the above-mentioned curable resin.

Additives are added to the curable composition and used to improve various performances such as viscosity adjustment, curing acceleration, and adhesiveness of the curable composition. Specific examples thereof include a curing accelerator, a plasticizer, a weather-resistant stabilizer, a filler, a rocking denaturing agent, an adhesiveness improving agent, a storage stability improving agent (dehydrating agent), a coloring agent, and an organic solvent. All of these can be used alone or in combination of two or more.

These curable compositions are roughly classified into one-component curable compositions that cure by reacting with moisture in the air and two-component curable compositions that cure by mixing the main agent with a curing agent and curing. can do. The filling method of the present invention can be applied to both a one-component curable composition and a two-component curable composition. The filling method of the present invention is a step of integrating the moisture-proof film 7 and the curable composition 6 and covering the surface of the curable composition 6 with the moisture-proof film 7 to shield the curable composition 6 from moisture in the air. As the curable composition 6 to be applied, it is stored as a one-component curable composition and a curable composition containing a resin that reacts with moisture in the air in the two-component curable composition. High stability effect.

The viscosity of the curable composition 6 is preferably 150 to 400 Pa · s at 1 rpm, particularly preferably 200 to 350 Pa · s, as measured by an E-type viscometer (25 ° C.). Further, in the measurement with an E-type viscometer (25 ° C.), 40 to 100 Pa · s is preferable at 10 rpm, and 50 to 80 Pa · s is particularly preferable.

The thixotropic index of the curable composition 6 is preferably 3 to 6, and particularly preferably 3.5 to 5. The thixotropic index of the curable composition 6 is determined as a viscosity ratio of 1 rpm to 10 rpm (viscosity of 1 rpm / viscosity of 10 rpm) of the curable composition 6 in the measurement of an E-type viscometer (25 ° C., 1 rpm, 10 rpm). be able to.

The seal 10 can be used without particular limitation as long as the can body 4 (container body) and the can lid 9 can be fitted and the can body 4 can be sealed.

Examples of the material of the seal 10 include natural rubber and synthetic rubber. Examples of the synthetic rubber include nitrile rubber, hydride nitrile rubber, fluororubber, urethane rubber, silicone rubber, ethylene propylene rubber, chloroprene rubber, acrylic rubber, butyl rubber, chlorosulphonized polyethylene rubber, and epichlorohydrin rubber.

The method of fitting the can body 4 (container body) and the can lid 9 has been described with reference to the seals 10 shown in FIGS. 8 to 11, but the fitting is performed by a conventionally known method other than the fitting by the seal 10. There is no limitation on the method as long as it can be sealed with the can body 4 and the can lid 9.

The desiccant is used to remove water (moisture absorption / water absorption) such as moisture in a container such as a sealed can body 4. Examples of the desiccant include silica gel, silica-alumina gel, calcium oxide, and calcium chloride.

1 Bottom surface 2 Side surface 3 Handle 4 Can body 5 Filling nozzle 6 Filling (curable composition)
7 Moisture prevention film 9 Can lid 10 Seal 11 Desiccant 13, 23, 33 Convex parts 18, 28, 38 Push plate

Claims (14)

The process of filling a sealable container with the curable composition,
The process of laying a moisture-proof film on the surface of the curable composition and
A step of pressing the moisture-proof film with the push plate with the convex portion of the push plate having a convex portion on the bottom surface facing the moisture-proof film to integrate the moisture-proof film and the curable composition. When,
The process of sealing the container with a lid,
A method for filling a curable composition containing. The filling method according to claim 1, wherein the convex portion is a curved surface portion formed in a side view arc shape on the entire bottom surface. A claim that the convex portion has a curved surface region having an arcuate side view formed on the peripheral edge of the bottom surface and a flat region having a linear side view linearly formed from the peripheral edge of the bottom surface to the central portion continuous from the curved surface region. The filling method according to 1. The convex portion has a side-viewing arc-shaped first curved surface region formed on the peripheral edge of the bottom surface and a side-viewing arc-shaped region formed from the peripheral edge of the bottom surface to the central portion continuous from the first curved surface region. The filling method according to claim 1, further comprising a second curved surface region having a side view arc shape, which has a radius of curvature larger than the radius of curvature of the first curved surface region of the above. The sealable container has a cylindrical, elliptical, or square tubular shape with the lower surface as the bottom surface, an opening is provided in the upper part of the container, and the container can be sealed by fitting the opening and the lid. The filling method according to any one of claims 1 to 4, which serves as a container. The filling method according to any one of claims 1 to 5, wherein the moisture-proof film is a composite film of aluminum and resin. The filling method according to any one of claims 1 to 6, wherein the strength of the moisture-proof film measured in the tensile performance test is 20 to 100 N / mm ² . The filling method according to any one of claims 1 to 7, wherein the elongation of the moisture-proof film measured in the tensile performance test is 5% or more. The filling method according to any one of claims 1 to 8, wherein the viscosity at 25 ° C. measured at 1 rpm using an E-type viscometer of the curable composition is 150 to 400 Pa · s. The filling method according to any one of claims 1 to 9, wherein the thixotropic index at 25 ° C. measured at 1 rpm / 10 rpm using an E-type viscometer of the curable composition is 3 to 6. Any of claims 1 to 10, wherein the moisture-proof film and the curable composition are integrated by the step of integrating the moisture-proof film and the curable composition, and the curable composition is shielded from moisture. The filling method according to one item. By the step of integrating the moisture-proof film and the curable composition, the moisture-proof film and the curable composition are integrated, the curable composition is shielded from moisture, and the moisture-proof film is sealed. The filling method according to any one of claims 1 to 11, wherein all or part of the inner peripheral side surface of the container is brought into close contact with the inner peripheral side surface. By the step of integrating the moisture-proof film and the curable composition, the moisture-proof film and the curable composition are integrated, the curable composition is shielded from moisture, and the moisture-proof film and the curable composition are integrated. The filling method according to any one of claims 1 to 12, wherein the curable composition becomes convex toward the bottom surface of the container. A structure in which the curable composition is filled in a sealable container by the filling method according to any one of claims 1 to 13, and the container is sealed by the lid.

Images