WO2023223974A1

WO2023223974A1 - Package

Info

Publication number: WO2023223974A1
Application number: PCT/JP2023/017948
Authority: WO
Inventors: 智大森田; 康則奥村
Original assignee: 株式会社日本触媒
Priority date: 2022-05-20
Filing date: 2023-05-12
Publication date: 2023-11-23

Abstract

This package (P) is characterized in that an ionic compound containing fluorine atoms or a composition containing the ionic compound is packaged in a flexible packaging material (2) as contents (1), the packaging material (2) includes at least one metal layer (3), the moisture permeability of the packaging material (2) is 0.1 g/m2·24 hours or less, and the bulk filling rate of the contents (1) is 50-97% with respect to the volume of the package (P).

Description

packaging

The present disclosure relates to a package containing an ionic compound containing a fluorine atom or a composition containing the ionic compound.

For example, fluorosulfonyl used in electrolytes, additives to fuel cell electrolytes, selective electrophilic fluorination agents, photoacid generators, thermal acid generators, near-infrared absorbing dyes, antistatic agents, reaction catalysts, etc. Ionic compounds containing fluorine atoms, such as imide salts, are usually crystallized and dried, and then the resulting powder is packaged as it is for storage and transportation (shipping). Here, the ionic compound containing a fluorine atom has high hygroscopicity and is easily hydrolyzed to generate hydrofluoric acid. Hydrofluoric acid is a strong acid and may corrode containers and bags used for storage and transportation. Furthermore, since the presence of water has an adverse effect in battery applications, etc., the amount of water present in the ionic compound must be reduced as much as possible.

Therefore, the present applicant has developed an ionic compound having a fluorine atom or a composition containing the ionic compound into a packaging material having at least one metal layer after reducing the initial water content to a predetermined amount or less. They have found that packaging with good storage stability can be achieved and have proposed packaging for this purpose (Patent Documents 1 and 2). In this package, hydrolysis of the ionic compound during storage and transportation is suppressed as much as possible, so the occurrence of the above-mentioned inconveniences is suppressed.

Furthermore, the applicant has discovered a method for manufacturing small-scale packages by dividing fluorosulfonylimide in an atmosphere in which fluorosulfonylimide does not easily absorb moisture, and has also proposed a method for manufacturing such packages (patent Reference 3). With this method, fluorosulfonylimide can be subdivided from the storage container in which it was stored into smaller packaging containers in a less expensive dry room, reducing product costs and improving workability. do.

Patent No. 6208929 Patent No. 6266702 Patent No. 6368466

By the way, as mentioned above, ionic compounds containing fluorine atoms are highly hygroscopic, so depending on the storage period (for example, one month or more) and the storage/transport environment, even the above packaging may absorb moisture during storage/transport. do. In addition, the powder has the property of agglomerating. Aggregated ionic compounds or compositions containing ionic compounds (agglomerates) are not only difficult to discharge from the packaging material, but also have problems in subsequent steps, e.g., because it takes time to dissolve the aggregates. It also affects workability.

The present disclosure has been made in view of the above, and its purpose is to prevent the powder of an ionic compound containing a fluorine atom or a composition containing the ionic compound from agglomerating in a package. The object of the present invention is to provide a package that can easily fluidize aggregates inside the package.

As a result of further studies, the inventors of the present application have determined that the packaging material is made of a flexible material, and that the volume of the void existing inside the package (specifically, the volume ratio of the contents to the void) is It has been found that by specifying this, even when the powder is agglomerated, the agglomerate can be easily returned to a fluid state (for example, powder) (fluidized) inside the package. Specifically, the present disclosure is as follows.

The package of the present disclosure is a package in which an ionic compound containing a fluorine atom or a composition containing the ionic compound is packaged with a flexible packaging material, and the package includes at least one layer of the packaging material. The packaging material has a moisture permeability of 0.1 g/ ^m2 ·24 hours or less, and the bulk filling rate of the contents is 50% or more and 97% or less with respect to the volume of the packaging body. It is characterized by The bulk filling rate of the above-mentioned contents may be 10% or more and 60% or less with respect to the internal volume of the above-mentioned packaging material. The ionic compound containing a fluorine atom has the general formula (I):
[Chemical formula 1]
MN(XSO ₂ )(FSO ₂ ) (M is an inorganic cation, X is an organic group or fluorine.) (I)
It may also be a fluorosulfonylimide represented by

According to the package of the present disclosure, even when powder of an ionic compound containing a fluorine atom or a composition containing the ionic compound aggregates within the package, the aggregates can be easily fluidized within the package. can be converted into

FIG. 1 is a perspective view showing a schematic configuration of a package according to an embodiment of the present disclosure. FIG. 2 is a sectional view showing a schematic configuration of a package according to an embodiment of the present disclosure.

Hereinafter, this embodiment will be described in detail based on the drawings. The following description of preferred embodiments is merely exemplary in nature and is in no way intended to limit the invention, its applications, or its uses.

[Package]
1 and 2 show a package P according to an embodiment of the present disclosure. The package P of the present disclosure stores or transports (ships) an ionic compound containing a fluorine atom or a composition containing the ionic compound (hereinafter collectively referred to as "ionic compound, etc.") as contents 1, which will be described later. ). The package P refers to a shipping form when an ionic compound or the like is distributed on the market. That is, the package P refers to a state in which the content 1 such as an ionic compound is packaged with the packaging material 2, and includes the packaging material 2 and the content 1 packaged therein.

<Packaging materials>
The packaging material 2 is for packaging the contents 1 and has flexibility. The flexible packaging material 2 is one that does not maintain a fixed shape and can be deformed in accordance with external conditions. As the flexible packaging material 2, for example, a packaging material made of a deformable material can be selected, such as a packaging material made of a plastic resin film.

The packaging material 2 includes at least one metal layer 3. This metal layer 3 suppresses moisture and water from entering from the outside. Examples of the metal layer 3 include an aluminum or aluminum alloy layer (hereinafter also simply referred to as an "aluminum layer"), a stainless steel layer, and the like. Among the metal layers 3, an aluminum layer is preferable from the viewpoint of making the packaging material 2 flexible. The flexible packaging material 2 may be constituted by a sealable bag formed of, for example, a laminate having an aluminum layer, specifically a laminate in which both sides of the aluminum layer are protected with resin films. Examples of the resin constituting the resin film include polyolefins such as polyethylene and polypropylene; polyesters such as polyethylene terephthalate and polybutylene terephthalate; nylon; and polystyrene. The number of layers in the laminate is not particularly limited as long as it has flexibility, and may be two layers or three or more layers. Further, the number of layers of the metal layer 3 is not particularly limited as long as it has at least one layer and flexibility is ensured, and may be two or more layers. Moreover, the packaging material 2 may be comprised of two or more types of bags including at least one type of bag mentioned above. For example, a plurality of the above-mentioned bags stacked may be used as one packaging material. The material of the bag (inner surface thereof) with which the contents 1 come into direct contact is preferably one containing a resin film.

The thickness of the laminate is not particularly limited, but is preferably about 50 μm to 200 μm, for example. In this case, the thickness of the aluminum layer is preferably about 5 μm to 20 μm. If the thickness of the aluminum layer is within the above range, the formation of pinholes due to a decrease in film strength will be suppressed, and the flexibility of the packaging material 2 will also be ensured.

Methods for manufacturing the laminate include, for example, attaching a resin film to aluminum foil using an appropriate adhesive, laminating the resin onto the aluminum foil while extruding it, and depositing aluminum on the resin film and then laminating the resin film. etc. Further, as a method for sealing these laminates, for example, a method using a zipper previously formed on the bag and further using means such as heat sealing or ultrasonic welding can be mentioned.

Moreover, the moisture permeability of the packaging material 2 (if it is composed of the above-mentioned laminate, the laminate) is 0.1 g/m ² ·24 hours or less. In this specification, moisture permeability refers to the amount of moisture that permeates per 1 m ² of fabric (laminate) of the packaging material 2 in 24 hours. If the moisture permeability of the packaging material 2 is within the above range, the intrusion of moisture and water from the outside will be suppressed, and the flexibility of the packaging material 2 will also be ensured. Note that moisture permeability can be measured by a generally known method.

The shape of the packaging material 2 is not particularly limited, and examples thereof include a bottle shape, a cylinder shape, a pack shape, a pouch shape, and the like. Examples of bottle-shaped and cylindrical containers include closed containers whose horizontal cross-sectional shape is circular, elliptical, polygonal, and the like. Examples of the pack type and pouch type include a prismatic sealed container whose horizontal cross-sectional shape is rectangular or the like. The internal volume of the packaging material 2 is not particularly limited.

Note that the packaging material 2 may be covered with at least one outer bag (not shown) from the viewpoint of suppressing moisture absorption of the ionic compound containing a fluorine atom. In other words, the package P of the present disclosure may further include an outer bag. Examples of the outer bag include resin bags, resin containers, glass containers, and the like. Examples of the resin constituting the resin bag or the resin container include the resin constituting the resin film described above, fluororesin, etc., and a laminate of two or more resins may be used. In addition, dry inert gas, dry air, etc. may be filled between the packaging material 2 and the outer bag, or between each outer bag in a structure in which the packaging material 2 is covered with multiple outer bags. or may be evacuated.

<Bulk filling rate of contents relative to the volume of the package>
Here, in the package P of the present disclosure, the bulk volume of the content 1 is specified as the ratio of the content 1 to the volume of the package P. Specifically, the bulk volume of the contents 1 is filled with the volume of the package P at a filling rate of 50% or more and 97% or less (the bulk filling rate of the contents with respect to the volume of the package). In this specification, the bulk filling rate of the contents with respect to the volume of the package is expressed by the formula (1):
[Number 1]
Bulk filling rate (%) of contents to volume of package = [(mass of contents/bulk specific gravity of contents)/volume of package] x 100 (1)
(hereinafter also referred to as "bulk filling rate of contents (1)").

"(Mass of contents/bulk specific gravity of contents)" refers to the bulk volume of the contents 1. "Volume of the package" refers to the bulk volume occupied by the content 1 and the inside of the package P after the content 1 is filled into the packaging material 2 (in a state where the content 1 is wrapped by the packaging material 2). This is the sum of the volume of the existing void G. In other words, the "bulk filling rate of the contents (1)" defines the ratio between the apparent bulk volume of the contents 1 (for example, powder) and the volume of the void G inside the package P. I can say that.

The volume of the package P is a value measured under measurement conditions at room temperature (approximately 25°C) in a dry room with a dew point of -30°C. The volume of the package P can be measured using, for example, a commercially available laser volume meter. Note that since the thickness of the packaging material 2 constituting the package P is sufficiently thin (for example, about 200 μm or less) to have flexibility, it is usually not necessary to remove the volume corresponding to the thickness. On the other hand, if the packaging material 2 is considerably thick, the volume corresponding to the thickness may be removed. The volume of the package P may be measured in situ, that is, when the packaging material 2 is filled with the contents 1 and then packaged (the package P is completed).

If the "bulk filling rate (1) of the contents" relative to the volume of the package P is within the above range (especially below the upper limit), there are sufficient voids (spaces) in the packaging material 2, so that the contents 1 Even if the particles aggregate, a space is secured in which the aggregates can move. In other words, in the package P of the present disclosure, a space is secured for returning the aggregate to a fluid state. Furthermore, the package P of the present disclosure is made of a flexible packaging material 2. Therefore, even when the contents 1 aggregate, the package P deforms in accordance with the external conditions, the aggregates collapse and spread in the space created by the deformation, and can be returned to a fluid state (for example, powder). In addition, the "bulk filling rate of contents (1)" is preferably equal to or higher than the lower limit value from the viewpoint of storage and transportation costs of the package P. If the "bulk filling rate of contents (1)" is less than the lower limit, the volume of the void G is large, so the package P is likely to deform, for example, the package may collapse during loading, or the package may P (packaging material 2) may become easily torn. In addition, since the volume of the void G is large, the volume of the void G changes due to changes in the temperature of the outside world, and the amount of change becomes relatively large, so it is thought that the above-mentioned loading problem will become more pronounced. It will be done. For example, if the content 1 having a bulk volume of 5L to 9.7L is filled with the packaging material 2, which is about 10000 cm ³ (10L), assuming that the volume of the package P after filling the content 1 is large, the packaging The "bulk filling rate (1) of the contents" relative to the volume of the body P falls within the above range. Moreover, as an example of a package P having a volume smaller than the above, the amounts described in each example described later can be used as a reference. Note that the lower limit of "bulk filling rate (1) of contents" is 50% or more, and may be 60% or more or 70% or more. The upper limit of "bulk filling rate (1) of contents" is 97% or less, and may be 95% or less, 90% or less, or 80% or less. In other words, the "bulk filling rate (1) of contents" is 50% or more and 97% or less, 50% or more and 95% or less, 50% or more and 90% or less, 50% or more and 80% or less, and 60% or more and 97%. % or less, 60% to 95%, 60% to 90%, 60% to 80%, 70% to 97%, 70% to 95%, 70% to 90%, 70% to 80% It may be the following.

<Bulk filling rate of contents relative to internal volume of packaging material>
In the package P of the present disclosure, the bulk volume of the contents 1 is a filling rate of 10% or more and 60% or less with respect to the internal volume of the packaging material 2 (bulk filling rate of the contents with respect to the internal volume of the packaging material). ) is preferably filled. In this specification, the bulk filling rate of the contents with respect to the internal volume of the packaging material is expressed by the formula (2):
[Number 2]
Bulk filling rate of contents to internal volume of packaging material (%) = [(mass of contents/bulk specific gravity of contents)/internal volume of packaging material] x 100 (2)
(hereinafter also referred to as "bulk filling rate of contents (2)").

The "inner volume of the packaging material" refers to the maximum volume that can fill the packaging material 2 with the contents 1 and seal the packaging material 2. In other words, it refers to the maximum volume that can accommodate the contents 1. The maximum storable volume can be determined by filling the packaging material 2 with water or the like at room temperature (approximately 25° C.) and measuring the filling amount.

When the "bulk filling rate (2) of the contents" with respect to the internal volume of the packaging material 2 is within the above range, the internal volume of the packaging material 2 becomes large enough for the bulk volume of the contents 1. In other words, even if the "bulk filling rate (1) of the contents" is at or near the upper limit of the above range, the volume of the void G itself existing inside the package P (in order to return the aggregates to a fluid state) The amount of deformation of the package P according to external conditions can be increased. Therefore, if both the "bulk filling rate (1)" and (2) of the contents are within the predetermined range, it is possible to further deform the package P in accordance with the external conditions, and the package P In combination with the presence of voids G at a predetermined ratio inside, even if the contents 1 aggregate, it is possible to further fluidize the aggregates. In addition, the preferable lower limit of "bulk filling rate of contents (2)" is 10% or more, and may be 20% or more or 30% or more. A preferable upper limit of "bulk filling rate (2) of contents" is 60% or less, and may be 50% or less or 40% or less. In other words, the preferable "bulk filling rate (2) of contents" is 10% or more and 60% or less, 10% or more and 50% or less, 10% or more and 40% or less, 20% or more and 60% or less, and 20% or more It may be 50% or less, 20% or more and 40% or less, 30% or more and 60% or less, 30% or more and 50% or less, or 30% or more and 40% or less.

Here, the "inner volume of the packaging material" is the volume of the packaging material 2 itself (before packaging), and is usually a larger value than the "volume of the package", which is the volume after packaging. The "bulk filling rate of contents (2)" based on the "inner volume of the packaging material" is also an index (design value) when determining the bulk volume of the contents 1 to be filled into a predetermined volume of the packaging material 2. I can say that. On the other hand, the "bulk filling rate of contents (1)" based on the "volume of the package" is the bulk volume of the contents 1 to be filled into a predetermined volume of the packaging material 2, and the packaging material after filling the contents 1. It is the ratio to the volume of the void G formed inside the package P in which Content 1 is hermetically packaged, and can be said to be an index (actual measurement value) when determining the bulk volume of Content 1 in the package P (shipping form). . In this way, the "bulk filling rate of contents (1)" and the "bulk filling rate of contents (2)" have different meanings.

The void G may or may not be filled with, for example, air, an inert gas (rare gas (such as helium), nitrogen, etc.), dry air, or the like. It is sufficient that a void G exists inside the package P, and gas may be filled in the void G as necessary. That is, the package P of the present disclosure does not include packaging in a vacuum state (vacuum pack).

<Contents>
In the package P of the present disclosure, the content 1 packaged with the packaging material 2 is an ionic compound containing a fluorine atom or a composition containing an ionic compound containing a fluorine atom. That is, the content 1 may be an ionic compound containing a fluorine atom itself, or may be a composition containing an ionic compound containing a fluorine atom and other components. Since an ionic compound having a fluorine atom may be hydrolyzed by moisture in the air and generate hydrofluoric acid, it is necessary to prevent moisture permeation during storage or transportation, but this is the package P of the present disclosure. As a result, moisture permeation is suppressed, and even if aggregated, it can be easily fluidized.

(Ionic compounds containing fluorine atoms)
Examples of ionic compounds containing fluorine atoms include alkali metal salts and alkaline earth metal salts of trifluoromethanesulfonic acid such as LiCF ₃ SO ₃ , NaCF ₃ SO ₃ , KCF ₃ SO ₃ ; LiC(CF ₃ Alkali metal salts and alkaline earth metal salts of perfluorosulfonic acid imides such as SO ₂ ) ₃ , LiN(CF ₃ CF ₂ SO ₂ ) ₂ , LiN(CF ₃ SO ₂ ) ₂ , LiN(FSO ₂ ) ₂ ; LiPF Alkali metal salts and alkaline earth metal salts of hexalfluorophosphoric acid such as ₆ , NaPF ₆ and KPF ₆ ; tetrafluoroborates such as LiBF ₄ and NaBF ₄ ; alkali metal salts such as LiAsF ₆ , LiSbF ₆ and NaAsF ₆ ; Quaternary ammonium salts of tetrafluoroboric acid such as (C ₂ H ₅ ) ₄ NBF ₄ , (C ₂ H ₅ ) ₃ (CH ₃ )NBF ₄ , and quaternary ammoniums such as (C ₂ H ₅ ) ₄ NPF ₆ Salts; quaternary phosphonium salts such as (CH ₃ ) ₄ P.BF ₄ and (C ₂ H ₅ ) ₄ P.BF ₄ are exemplified.

Among the ionic compounds containing a fluorine atom, general formula (I):
[Chemical 2]
MN( _XSO2 )( _FSO2 )(I)
The fluorosulfonylimide represented by is suitable for packaging in the package P of the present disclosure. This is because fluorosulfonylimide salt is highly hygroscopic and may generate sulfuric acid in addition to hydrofluoric acid upon hydrolysis, so it is necessary to package it with packaging material 2 that can reliably prevent moisture permeation. In the case of fluorosulfonylimide, whether or not hydrolysis has occurred can be confirmed by quantitative determination of fluorine ions and sulfate ions (ion chromatography).

In general formula (I), X represents fluorine or an organic group. When X is fluorine, general formula (I) represents a bis(fluorosulfonyl)imide salt. Examples of the organic group include a haloalkyl group, a cyano group, an alkoxy group, a nitro group, a hydroxyl group, an aliphatic group, an aromatic group, and the like. Among the organic groups, a fluorinated alkyl group (fluoroalkyl group) having 1 to 6 carbon atoms is preferred. When X is a fluoroalkyl group, it becomes an N-(fluorosulfonyl)-N-(fluoroalkylsulfonyl)imide salt. The term "fluoroalkyl" refers to an alkyl group having 1 to 6 carbon atoms in which one or more hydrogen atoms have been replaced with a fluorine atom, such as fluoromethyl group, difluoromethyl group, trifluoromethyl group, etc. group, fluoroethyl group, difluoroethyl group, trifluoroethyl group, pentafluoroethyl group, etc. Among X, fluorine atom, trifluoromethyl group and pentafluoroethyl group are preferred.

Furthermore, in general formula (I), M represents an inorganic cation. As the inorganic cation, alkali metal ions or alkaline earth metal ions are suitable. Examples of the alkali metal include Li, Na, K, and the like. Examples of alkaline earth metals include Ca, Mg, and the like. A more common compound is lithium fluorosulfonylimide, where M is Li.

Note that the fluorosulfonylimide salt can be produced, for example, by the production methods described in Patent Documents 1 and 2.

(Composition containing an ionic compound containing a fluorine atom)
The composition containing an ionic compound containing a fluorine atom only needs to contain the above-mentioned ionic compound containing a fluorine atom, and may contain other components. When the content 1 is a composition containing an ionic compound having a fluorine atom, the amount of the ionic compound having a fluorine atom in the composition is preferably 3% by mass or more, more preferably 5% by mass or more, and further Preferably it is 8% by mass or more, particularly preferably 10% by mass or more. Other components such as solvents, other ionic compounds, and other powders can be appropriately blended as long as the composition is in powder form.

[Method of filling ionic compounds, etc. into packaging materials]
The method of filling the packaging material 2 with the ionic compound, etc. is not particularly limited, except that the "bulk filling rate (1) of contents" after filling is adjusted within the above range. For example, a storage container for ionic compounds or the like may be subdivided into packaging materials 2 having smaller contents. In this case, for example, as described in Patent Documents 1 and 2, it is preferable that the ionic compound etc. be stored at a moisture content of 1000 ppm or less. As the subdivision method, for example, the method described in Patent Document 3 may be applied. The subdivision work may be performed by an operator, or an automatic subdivision device or the like may be used.

[Storage and transportation of packaging]
The package P of the present disclosure is preferably stored or transported at a relatively low temperature. The temperature during storage or transportation is preferably 50°C or lower, more preferably 40°C or lower, even more preferably 30°C or lower. If the storage or transfer temperature of the package P is within the above range, hydrolysis and thermal decomposition of the ionic compounds and the like that are the contents 1 are suppressed.

[Other embodiments]
The package P of the present disclosure may be covered with a drum, a cardboard box, a plastic case, or the like. This suppresses the formation of pinholes on the surface of the package P (packaging material 2) during storage and transportation, and as a result, the ionic compound containing a fluorine atom of the contents 1 or the ionic compound containing Moisture absorption of the composition is suppressed.

[summary]
The package P of the present disclosure is one in which an ionic compound or the like is packaged using the packaging material 2. Since the packaging material 2 includes at least one metal layer 3 and has a moisture permeability of 0.1 g/ ^m2 ·24 hours or less, moisture permeation is sufficiently suppressed during storage or transportation of ionic compounds, etc. Ru. In addition, since the contents 1 such as ionic compounds are filled with a bulk filling rate (bulk filling rate (1) of contents) of 50% to 97% with respect to the volume of the package P, the packaging material 2 A gap (space) large enough to allow the contents 1 to move (flow) is secured inside. Therefore, even if the contents 1 aggregate after the package P is stored for a predetermined period (for example, one month or more), the aggregates can be easily returned to a fluid state. In this way, the packaging P of the present disclosure is not only suitable for storing or transporting ionic compounds, etc., but also has the function of easily fluidizing aggregates, so that the ionic compounds from the packaging material 2 can be easily fluidized. etc., and the time for dissolving ionic compounds etc. is also shortened, so that workability can be improved. In addition, by filling the content 1 such as an ionic compound with a bulk filling rate of 10% to 60% (bulk filling rate (2) of contents) to the internal volume of the packaging material 2, the above-mentioned voids are filled. (Space) is further secured, and the amount of deformation of the package P itself in response to external conditions increases, so the above effects can be improved.

The present disclosure will be described below based on examples. Note that the present disclosure is not limited to the following examples, and the following examples can be modified and changed based on the spirit of the present disclosure, and these are excluded from the scope of the present disclosure. isn't it.

(Example 1)
In a dry room with a dew point of -30°C, lithium bis(fluorosulfonyl)imide was placed as an ionic compound (content) containing fluorine atoms in a three-sided aluminum bag measuring 34 cm x 24 cm x 7 cm (inner volume 4300 cm ³ ) as a flexible packaging material. [Nippon Shokubai Co., Ltd., LiN (FSO ₂ ) ₂ , hereinafter referred to as "LiFSI", bulk specific gravity: 1.5] 1.5 kg was put therein, the remaining one side was heat sealed, and the aluminum bag was sealed. The moisture permeability of the aluminum bag was 0.1 g/m ² ·24 hours or less (below the measurement limit). The in situ volume of the aluminum bag (package) filled with LiFSI was measured using a commercially available laser volumeter, and the volume was approximately 1050 cm ³ (volume of the package). Therefore, the bulk volume of LiFSI filled in an aluminum bag is 1000 cm ³ (=1500/1.5), and the bulk filling rate of LiFSI to the volume of the package is expressed as the proportion of LiFSI in the aluminum bag (the bulk of the contents). The filling rate (1)) was approximately 95% (≈1000/1050×100). Furthermore, as a proportion of LiFSI in the aluminum bag, the bulk filling ratio of LiFSI to the internal volume of the packaging material (bulk filling ratio of contents (2)) was about 23% (≈1000/4300×100). As described above, a package containing LiFSI in an aluminum bag was obtained. Subsequently, the package was stored for one month at a room temperature of 23° C. and a relative humidity of 50%. After being stored for one month, the LiFSI contained in the package had aggregated, but it was possible to fluidize the LiFSI by securing space within the packaging material. In addition, the fluidization method was to allow the package to fall freely from a height of 50 cm. Finally, the aluminum bag was opened in a dry room with a dew point of -30°C, and the moisture content in the recovered LiFSI was measured based on the method described below, and it was found to be 27 ppm (after one month storage). "ppm" means "mass ppm". Note that the moisture content in LiFSI before storage was 16 ppm.

[Moisture measurement]
A sample was prepared by dissolving about 3 g of LiFSI in about 8 g of ultra-dehydrated methanol (manufactured by Fuji Film Wako Pure Chemical Industries, Ltd.). Karl Fischer moisture measuring device AQ-2000 (manufactured by Hiranuma Sangyo Co., Ltd.) was used, Aqualite RS-A (manufactured by Hiranuma Sangyo Co., Ltd.) was used as the generated liquid, and Aqualite CN (manufactured by Hiranuma Sangyo Co., Ltd.) was used as the counter electrode. , the moisture content of the sample was measured.

(Example 2)
A package in which LiFSI was wrapped in an aluminum bag was obtained in the same manner as in Example 1 except that the amount of LiFSI was changed to 2.5 kg. The in situ volume of the aluminum bag (packaging body) filled with LiFSI was measured in the same manner as in Example 1, and the volume was approximately 2100 cm ³ (volume of the packaging body). Therefore, the bulk volume of LiFSI filled in an aluminum bag is 1666 cm ³ (≒2500/1.5), and the bulk filling ratio of LiFSI to the volume of the package (bulk filling ratio of contents (1)) is approximately 80 cm 3 (≒2500/1.5). % (≒1666/2100×100). Moreover, the bulk filling rate of LiFSI with respect to the internal volume of the packaging material (bulk filling rate of contents (2)) was about 39% (≈1666/4300×100). Subsequently, the package was stored in the same manner as in Example 1 for one month. After being stored for one month, the LiFSI contained in the package had aggregated, but by securing space within the packaging material, it was possible to fluidize the LiFSI using the same fluidization method as in Example 1. did it. Finally, the moisture content in the recovered LiFSI was measured in the same manner as in Example 1 and found to be 24 ppm (after one month of storage). Note that the moisture content in LiFSI before storage was 16 ppm.

(Example 3)
A package in which LiFSI was wrapped in an aluminum bag was obtained in the same manner as in Example 1 except that the weight of LiFSI was changed to 3.5 kg. The in situ volume of the aluminum bag (packaging body) filled with LiFSI was measured in the same manner as in Example 1, and the volume was approximately 2600 cm ³ (volume of the packaging body). Therefore, the bulk volume of LiFSI filled in an aluminum bag is 2333 cm ³ (=3500/1.5), and the bulk filling ratio of LiFSI to the volume of the package (bulk filling ratio of contents (1)) is approximately 90 cm 3 (=3500/1.5). % (≒2333/2600×100). Moreover, the bulk filling rate of LiFSI to the internal volume of the packaging material (bulk filling rate of contents (2)) was about 54% (≈2333/4300×100). Subsequently, the package was stored in the same manner as in Example 1 for one month. After being stored for one month, the LiFSI contained in the package had aggregated, but by securing space within the packaging material, it was possible to fluidize the LiFSI using the same fluidization method as in Example 1. did it. Finally, the moisture content in the recovered LiFSI was measured in the same manner as in Example 1, and was found to be 20 ppm (after one month of storage). Note that the moisture content in LiFSI before storage was 16 ppm.

(Example 4)
A package in which LiFSI was wrapped in an aluminum bag was obtained in the same manner as in Example 1 except that the amount of LiFSI was changed to 0.75 kg. The in-situ volume of the aluminum bag (package) filled with LiFSI was measured in the same manner as in Example 1, and the volume was approximately 980 cm ³ (volume of the package). Therefore, the bulk volume of LiFSI filled in an aluminum bag is 500 cm ³ (≒750/1.5), and the bulk filling rate of LiFSI to the volume of the package (bulk filling rate (1) of contents) is approximately 51 cm 3 (≒750/1.5). % (≒500/980×100). Moreover, the bulk filling rate of LiFSI to the internal volume of the packaging material (bulk filling rate of contents (2)) was about 12% (≈500/4300×100). Subsequently, the package was stored in the same manner as in Example 1 for one month. After being stored for one month, the LiFSI contained in the package had aggregated, but by securing space within the packaging material, it was possible to fluidize the LiFSI using the same fluidization method as in Example 1. did it. Finally, the moisture content in the recovered LiFSI was measured in the same manner as in Example 1, and was found to be 20 ppm (after storage for one month). Note that the moisture content in LiFSI before storage was 16 ppm.

(Comparative example 1)
A package in which LiFSI was wrapped in an aluminum bag was obtained in the same manner as in Example 1 except that the weight of LiFSI was changed to 4.5 kg. The in situ volume of the aluminum bag (packaging body) filled with LiFSI was measured in the same manner as in Example 1, and the volume was approximately 3060 cm ³ (volume of the packaging body). Therefore, the bulk volume of LiFSI filled in an aluminum bag is 3000 cm ³ (=4500/1.5), and the bulk filling ratio of LiFSI to the volume of the package (bulk filling ratio of contents (1)) is approximately 98 cm 3 (=4500/1.5). % (≒3000/3060×100). Moreover, the bulk filling rate of LiFSI with respect to the internal volume of the packaging material (bulk filling rate of contents (2)) was about 70% (≈3000/4300×100). Subsequently, the package was stored in the same manner as in Example 1 for one month. After being stored for one month, the LiFSI contained in the package had aggregated and there was not enough space within the packaging material, so LiFSI could not be fluidized using the same fluidization method as in Example 1. Ta. Finally, the moisture content in the recovered LiFSI was measured in the same manner as in Example 1 and found to be 21 ppm (after storage for one month). Note that the moisture content in LiFSI before storage was 16 ppm.

(Summary of Examples)
From the above results, when comparing each example and Comparative Example 1, the bulk filling rate of LiFSI to the volume of the flexible aluminum bag after filling with LiFSI (bulk filling rate of contents to the volume of the package (1)) It was found that by setting the ratio to 50% or more and 97% or less, even if LiFSI aggregated, it could be easily fluidized. Furthermore, if the bulk filling ratio of LiFSI to the internal volume of the aluminum bag itself (bulk filling ratio of the contents to the internal volume of the packaging material (2)) is 10% or more and 60% or less, the above effects can be obtained. Do you get it.

The package of the present disclosure is useful as a form for storing or transporting an ionic compound containing a fluorine atom or a composition containing the ionic compound.

P Packaging G Gap 1 Contents 2 Packaging material 3 Metal layer

Claims

A package formed by packaging an ionic compound containing a fluorine atom or a composition containing the ionic compound with a flexible packaging material,
The packaging material includes at least one metal layer, and the packaging material has a moisture permeability of 0.1 g/m 2.24 hours or less,
A package characterized in that the bulk filling rate of the contents is 50% or more and 97% or less with respect to the volume of the package.
The package according to claim 1, wherein the bulk filling rate of the contents is 10% or more and 60% or less with respect to the internal volume of the packaging material.
The package according to claim 1 or 2, wherein the ionic compound containing a fluorine atom is a fluorosulfonylimide represented by the general formula (I).
MN(XSO 2 )(FSO 2 ) (M is an inorganic cation, X is an organic group or fluorine.) (I)