WO2025205198A1 - Substance transfer device and transfer method, and method for removing internal residue in apparatus for substance - Google Patents

Abstract

The present invention pertains to a substance transfer device that is for a substance containing at least one kind selected from sulfur atoms and halogen atoms, that enables safe and efficient handling of a substance containing at least one kind selected from sulfur atoms and halogen atoms, and that comprises a spare chamber for transfer, a transfer substance inlet and a transfer substance outlet, and an introduction mechanism and a discharge mechanism for an inert gas. The transfer substance inlet and the transfer substance outlet are provided to the spare chamber for transfer and are capable of being joined to a first substance inlet and a first substance outlet of a first container for a substance, and to a second substance transfer port of a second container for a substance. The introduction mechanism for an inert gas introduces the inert gas into the spare chamber for transfer. The discharge mechanism for an inert gas discharges the inert gas from the spare chamber for transfer. Also, the present invention pertains to a transfer method and a method for removing an internal residue in an apparatus for a substance.

Description

Substance transfer device and transfer method, and method for removing internal residues from substance equipment

The present invention relates to a substance transfer device and transfer method, as well as a method for removing internal residue from substance-transfer equipment.

With the rapid spread of information-related and communication devices such as personal computers, video cameras, and mobile phones in recent years, the development of batteries to be used as their power sources has become increasingly important. Traditionally, batteries used in these applications have used electrolytes containing flammable organic solvents. However, because the electrolyte is liquid and flammable, safety concerns regarding leakage and fire have arisen when used in batteries. In particular, demand for higher capacity and output is growing for automotive applications, and safety concerns regarding batteries that use conventional electrolytes are growing. Therefore, all-solid-state batteries, which replace the electrolyte with a solid electrolyte layer, are being developed, as this eliminates the use of flammable organic solvents in the battery, simplifies safety devices, and offers superior manufacturing costs and productivity.

Known methods for producing solid electrolytes used in solid electrolyte layers include, for example, a method for producing a solid electrolyte that involves mixing a complexing agent and a solid electrolyte raw material to prepare an electrolyte precursor (see, for example, Patent Document 1), and a method for producing a solid electrolyte that involves drying a slurry containing a complexing agent and an electrolyte precursor by fluidized drying using media particles (see, for example, Patent Document 2).

In a powder handling system, a dispersion device has been disclosed that includes a stirring/mixing section that mixes powder and liquid, a sealable powder supply section that supplies powder to the stirring/mixing section, and a dry gas generator that supplies dry gas to the powder supply section (see, for example, Patent Document 3). Also, in a mixing system that mixes multiple materials, a dry gas supply section that supplies dry gas to a hopper equipped with a mixing mechanism that mixes multiple materials, a material adjustment section that adjusts the materials, and a spout that supplies the materials to the mixing mechanism (see, for example, Patent Document 4).

International Publication No. 2020/105737 International Publication No. 2021/230189 Japanese Patent Application Laid-Open No. 2021-126598 Japanese Patent Application Laid-Open No. 2020-182891

The present invention was made in light of these circumstances, and aims to provide a substance transfer device and method, as well as a method for removing internal residues from substance-handling equipment, that can safely and efficiently handle substances containing at least one atom selected from sulfur atoms and halogen atoms.

The substance transfer device according to the present invention comprises:
An apparatus for transferring a substance containing at least one atom selected from a sulfur atom and a halogen atom,
The apparatus comprises a transfer preliminary chamber, a transfer substance inlet and a transfer substance outlet, and an inert gas introduction mechanism and an exhaust mechanism,
the transfer substance inlet and transfer substance outlet are provided in the transfer prechamber and can be connected to the first substance inlet and first substance outlet of the first substance container and the second substance transfer port of the second substance container;
the inert gas introduction mechanism introduces the inert gas into the transfer preliminary chamber, and the inert gas exhaust mechanism exhausts the inert gas from the transfer preliminary chamber;
material transfer equipment,
is.

The method for transferring a substance according to the present invention comprises:
The apparatus comprises a transfer preliminary chamber, a transfer substance inlet and a transfer substance outlet, and an inert gas introduction mechanism and an exhaust mechanism,
the transfer substance inlet and transfer substance outlet are provided in the transfer prechamber and can be connected to the first substance inlet and first substance outlet of the first substance container and the second substance transfer port of the second substance container;
the inert gas introduction mechanism introduces the inert gas into the transfer preliminary chamber, and the inert gas exhaust mechanism exhausts the inert gas from the transfer preliminary chamber;
using a transfer device for a substance containing at least one atom selected from a sulfur atom and a halogen atom,
A method for transferring a substance, comprising the steps of (1A) to (3A) below:
is.
(1A) The transfer substance inlet portion is connected to a valve 1a provided at the substance outlet portion of the first substance container, and the transfer substance outlet portion is connected to a valve 2 provided at the second substance transfer port portion of the second substance container.
(2A) The valves 1a and 2 are closed, and the inert gas is supplied and discharged by the inert gas introduction mechanism and discharge mechanism, filling the inert gas into the transfer preliminary chamber.
(3A) The supply and discharge of the inert gas are stopped, the valves 1a and 2 are opened, and the substance stored in the first substance container is transferred to the second substance container.

The method for removing internal residues from a substance container according to the present invention comprises:
The apparatus comprises a transfer preliminary chamber, a transfer substance inlet and a transfer substance outlet, and an inert gas introduction mechanism and an exhaust mechanism,
the transfer substance inlet and transfer substance outlet are provided in the transfer prechamber and can be connected to the first substance inlet and first substance outlet of the first substance container and the second substance transfer port of the second substance container;
the inert gas introduction mechanism introduces the inert gas into the transfer preliminary chamber, and the inert gas exhaust mechanism exhausts the inert gas from the transfer preliminary chamber;
using a transfer device for a substance containing at least one atom selected from a sulfur atom and a halogen atom,
A method for removing internal residues from a substance container, comprising the steps of (1B) and (2B) below:
is.
(1B) The transfer substance inlet is connected to the valve 1a provided at the substance outlet of the first substance container.
(2B) The valve 1a is opened, and the inert gas is supplied and discharged by the inert gas introduction mechanism and discharge mechanism, filling the inert gas into the preliminary substance chamber and the first substance container.

The present invention provides a substance transfer device and method, as well as a method for removing internal residues from substance-handling equipment, that can safely and efficiently handle substances containing at least one atom selected from sulfur atoms and halogen atoms.

1 is a schematic diagram showing a preferred embodiment of a substance transfer device according to the present embodiment. 1 is a schematic diagram showing a preferred embodiment of a substance transfer device according to the present embodiment.

An embodiment of the present invention (hereinafter sometimes referred to as "this embodiment") will be described below. Note that in this specification, the upper and lower limit values of numerical ranges expressed as "greater than or equal to," "less than or equal to," and "to" can be arbitrarily combined, and numerical values in examples can also be used as upper and lower limit values. Furthermore, preferred specifications can be adopted arbitrarily. In other words, one preferred specification can be adopted in combination with one or more other preferred specifications. It can be said that combinations of preferred items are more preferable.

(Findings Obtained by the Inventors to Achieve the Present Invention)
As a result of extensive research aimed at solving the above problems, the present inventors have discovered the following and have completed the present invention.

As research into the practical application of all-solid-state batteries progresses, mass production of sulfide solid electrolytes has become an urgent issue. In recent years, as demand for sulfide solid electrolytes has increased, full-scale operations have begun, shifting from lab-scale facilities to plant-scale facilities geared toward mass production. Methods for producing sulfide solid electrolytes, such as those described in Patent Documents 1 and 2, are being considered. Sulfide solid electrolyte production equipment handles a variety of substances containing sulfur atoms, including solid electrolyte raw materials containing sulfur atoms, such as lithium sulfide, diphosphorus pentasulfide, and elemental sulfur; electrolyte precursors composed of these solid electrolyte raw materials and complexing agents; and the resulting sulfide solid electrolyte. Since these sulfur-containing substances can react with moisture in the air and generate hydrogen sulfide, safety must always be taken into consideration.

Furthermore, when manufacturing sulfide solid electrolytes, substances containing halogen atoms, such as lithium halides and elemental halogens, are used as solid electrolyte raw materials, primarily to improve the ionic conductivity of the solid electrolyte. Among substances containing halogen atoms, elemental halogens are highly reactive with water, so safety must be taken into consideration.

Hydrogen sulfide can be generated when a substance containing sulfur atoms comes into contact with moisture in the air, for example, when the substance is transferred between one container and another, so caution is required. Furthermore, just like substances containing sulfur atoms, caution is also required regarding safety when transferring substances containing halogen atoms.

For example, solid electrolyte raw materials containing sulfur atoms, such as lithium sulfide, diphosphorus pentasulfide, and elemental sulfur, as well as solid electrolyte raw materials containing halogen atoms, such as lithium halide and elemental halogen, are commercially available or manufactured in a separate manufacturing apparatus. When transferring these commercially available or manufactured products from one container to another container for storing the solid electrolyte raw material provided in the sulfide solid electrolyte manufacturing apparatus, if no measures are taken when attaching or detaching the one container to the other, the material will come into contact with the atmosphere in the transfer piping for transferring the material and the surrounding atmosphere, so safety must be taken into consideration. Similar cases include when the sulfide solid electrolyte obtained in the sulfide solid electrolyte manufacturing apparatus is transported to its intended use as a product, or when it is transferred from one container storing the sulfide solid electrolyte to a container for transporting the sulfide solid electrolyte.
Thus, when a substance having at least one atom selected from sulfur atoms and halogen atoms is to be transferred from one container to another, the substance may come into contact with the atmosphere.

In manufacturing equipment through which materials flow, such as sulfide solid electrolyte manufacturing equipment capable of carrying out the sulfide solid electrolyte manufacturing methods described in Patent Documents 1 and 2, materials must be handled in all situations, including during start-up, normal operation, shutdown, and maintenance work, and care must be taken to prevent the generation of hydrogen sulfide due to reactions between the materials and moisture in the air, etc. However, no consideration is given to the handling of materials.

The dispersion device described in Patent Document 3 above is designed to supply dry gas while supplying powder to prevent the powder from reacting with moisture, which can cause deterioration and decomposition of the powder, resulting in performance degradation and the generation of toxic gas (Patent Document 3, paragraph [0008]). However, the dispersion device described in Patent Document 3 is designed for normal operation, in which powder is supplied to the stirring and mixing section together with dry gas and mixed with liquid, and the only locations that are subject to a dry gas atmosphere are those through which powder passes during normal operation, i.e., the powder supply section and the stirring and mixing section. Therefore, no consideration is given to locations where substances such as powder do not flow during normal operation.

The mixing system described in Patent Document 4, above, has a hopper equipped with a dry gas supply unit and a mixing mechanism connected in a state isolated from the outside air, thereby attempting to mix materials such as liquids and powders without contacting moisture in the outside air and exposing these materials to a dry gas environment (paragraphs [0038], [0044], etc.). However, the mixing system described in Patent Document 4 also assumes normal operation, in which multiple materials and dry gas coexist and are mixed inside the device, and the only areas that are subject to a dry gas environment are the hopper and mixing mechanism, which are areas through which powder passes during normal operation. Therefore, like Patent Document 3, Patent Document 4 also makes no consideration whatsoever to areas where powder and other substances do not flow during normal operation.

The inventors investigated methods for handling the above-mentioned substances, which arise in all situations, such as during the start-up, normal operation, shutdown, and maintenance of manufacturing equipment, and methods for ensuring safety, particularly during transfer, by minimizing reactions between the substances and moisture in the atmosphere. As a result of their investigation, they focused on using a spare chamber capable of storing an inert gas, such as nitrogen, as a transfer device. They then discovered that by combining such a spare chamber with a mechanism for supplying and discharging inert gas, and by using the spare chamber as a transfer pipe for transferring the substances when transferring them from one container to another, it is possible to minimize reactions between the substances and moisture in the atmosphere when transferring them.

Patent documents 3 and 4 do not mention at all the following: the preliminary chamber, through which the substance flows when transferring from one container to another, is filled with an inert gas atmosphere; however, the preliminary chamber, through which the substance does not flow during normal operation; or the use of the system in situations other than normal operation, such as connecting one container to another when transferring a substance stored in one container to that other container.

Furthermore, for example, when performing maintenance on equipment through which the above-mentioned substances pass during the operation of a manufacturing facility, the interior may be cleaned in advance with a fluid such as water. This may cause a reaction between the water used for cleaning and the above-mentioned substances, in addition to the moisture in the atmosphere. The water used for cleaning may then remain inside the equipment. Therefore, in order to perform maintenance more safely and quickly after shutting down the manufacturing facility, it is also important to more efficiently remove the water used for cleaning that remains inside the equipment. The inventors have discovered that in such cases, by providing the above-mentioned preliminary chamber and an inert gas supply and exhaust mechanism and using the preliminary chamber as a pipe for transferring the substances, the water used for cleaning that remains inside the equipment can be more efficiently removed, resulting in a secondary effect of improving the operating rate of the manufacturing equipment.
Thus, the transfer device and method of the present invention for a substance containing at least one atom selected from sulfur atoms and halogen atoms, as well as the method for removing internal residues from a substance-transporting device, can handle the above-mentioned substance safely and efficiently.

(Various aspects of this embodiment)
The substance transfer device according to the first aspect of this embodiment includes:
An apparatus for transferring a substance containing at least one atom selected from a sulfur atom and a halogen atom,
The apparatus comprises a transfer preliminary chamber, a transfer substance inlet and a transfer substance outlet, and an inert gas introduction mechanism and an exhaust mechanism,
the transfer substance inlet and transfer substance outlet are provided in the transfer prechamber and can be connected to the first substance inlet and first substance outlet of the first substance container and the second substance transfer port of the second substance container;
the inert gas introduction mechanism introduces the inert gas into the transfer preliminary chamber, and the inert gas exhaust mechanism exhausts the inert gas from the transfer preliminary chamber;
material transfer equipment,
is.

In the material transfer device according to the first aspect of this embodiment, when transferring a material containing sulfur atoms, such as lithium sulfide, diphosphorus pentasulfide, or elemental sulfur, or a material containing halogen atoms, such as lithium halide or elemental halogen, from a first container to a second container (or from the second container to the first container), safety can be ensured by suppressing reactions between the material and moisture in the atmosphere, etc., with a simple structure that includes a transfer reserve chamber, a transfer material inlet and outlet, and an inert gas introduction and exhaust mechanism. Furthermore, because safety can be ensured, work efficiency can be improved. As a result, it becomes possible to safely and efficiently handle a material containing at least one atom selected from sulfur atoms and halogen atoms (hereinafter sometimes simply referred to as "material").

A substance transfer device according to a second aspect of this embodiment includes:
The substance transfer apparatus according to the first aspect, wherein the inert gas introduction mechanism further introduces the inert gas from an inert gas inlet provided in the first substance container.
is.

The inert gas introduction mechanism can introduce inert gas through an inert gas inlet provided in the first substance container, allowing for safer and more efficient handling of substances. Furthermore, when removing internal residue from the substance container (described below), this can be done more efficiently, which can also improve the operating rate of the manufacturing equipment.

A substance transfer device according to a third aspect of this embodiment includes:
The substance transfer apparatus according to the first or second aspect, wherein the transfer preliminary chamber is cylindrical.
is.

If the transfer pre-chamber is cylindrical, it is possible to ensure safety while, in particular, transferring materials more smoothly, making it possible to handle materials more safely and efficiently. It also improves the maintainability of the material transfer device.

A substance transfer device according to a fourth aspect of this embodiment includes:
The substance transfer device according to the third aspect, wherein the transfer substance inlet portion and the transfer substance outlet portion are provided at both ends of the cylindrical transfer pre-chamber.
is.

Such a simple structure ensures safety while also enabling smoother material transfer, making it possible to handle materials more safely and efficiently. It also improves the maintainability of the material transfer device.

A substance transfer device according to a fifth aspect of this embodiment includes:
The substance transfer apparatus according to the third or fourth aspect, wherein the inert gas introduction mechanism and discharge mechanism are provided on a side surface of the cylindrical transfer pre-chamber.
is.

This type of structure allows for more stable introduction and discharge of inert gas, ensuring safety and particularly facilitating smoother transfer of materials, making it possible to handle materials more safely and efficiently.

A method for transferring a substance according to a sixth aspect of the present embodiment includes:
The apparatus comprises a transfer preliminary chamber, a transfer substance inlet and a transfer substance outlet, and an inert gas introduction mechanism and an exhaust mechanism,
the transfer substance inlet and transfer substance outlet are provided in the transfer prechamber and can be connected to the first substance inlet and first substance outlet of the first substance container and the second substance transfer port of the second substance container;
the inert gas introduction mechanism introduces the inert gas into the transfer preliminary chamber, and the inert gas exhaust mechanism exhausts the inert gas from the transfer preliminary chamber;
using a transfer device for a substance containing at least one atom selected from a sulfur atom and a halogen atom,
A method for transferring a substance, comprising the steps of (1A) to (3A) below:
is.
(1A) The transfer substance inlet portion is connected to a valve 1a provided at the substance outlet portion of the first substance container, and the transfer substance outlet portion is connected to a valve 2 provided at the second substance transfer port portion of the second substance container.
(2A) The valves 1a and 2 are closed, and the inert gas is supplied and discharged by the inert gas introduction mechanism and discharge mechanism, filling the inert gas into the transfer preliminary chamber.
(3A) The supply and discharge of the inert gas are stopped, the valves 1a and 2 are opened, and the substance stored in the first substance container is transferred to the second substance container.

The material transfer method of this embodiment employs the material transfer device of this embodiment described above. By performing the operations of the material transfer device of this embodiment in accordance with the steps (1A) to (3A) above, safety can be ensured while particularly material transfer can be carried out more smoothly, making it possible to handle materials safely and efficiently.

A substance transfer method according to a seventh aspect of the present embodiment includes:
The method for transferring a substance according to the sixth aspect, comprising carrying out the operations (2A) and (4A) and (5A) below after the operation (3A);
is.
(4A) The second substance container and valve 2 are removed from the transfer substance outlet.
(5A) A closing flange is attached to the outlet portion of the transfer substance.

By performing the above operations (2A), (4A), and (5A) in order following operation (3A), safety can be ensured while, in particular, the transfer of substances can be carried out more smoothly, making it possible to handle substances more safely and efficiently.

A method for removing internal residue from a substance container according to an eighth aspect of this embodiment includes:
The apparatus comprises a transfer preliminary chamber, a transfer substance inlet and a transfer substance outlet, and an inert gas introduction mechanism and an exhaust mechanism,
the transfer substance inlet and transfer substance outlet are provided in the transfer prechamber and can be connected to the first substance inlet and first substance outlet of the first substance container and the second substance transfer port of the second substance container;
the inert gas introduction mechanism introduces the inert gas into the transfer preliminary chamber, and the inert gas exhaust mechanism exhausts the inert gas from the transfer preliminary chamber;
using a transfer device for a substance containing at least one atom selected from a sulfur atom and a halogen atom,
A method for removing internal residues from a substance container, comprising the steps of (1B) and (2B) below:
is.
(1B) The transfer substance inlet is connected to the valve 1a provided at the substance outlet of the first substance container.
(2B) The valve 1a is opened, and the inert gas is supplied and discharged by the inert gas introduction mechanism and discharge mechanism, filling the inert gas into the transfer pre-chamber and the first substance container.

As mentioned above, when performing maintenance on equipment, the inside of the equipment may be washed with a fluid such as water beforehand, and this may cause a reaction between not only the moisture in the air but also the water used for washing and the above-mentioned substances. In this way, the medium such as water used for washing, as well as the substances themselves, may remain inside the equipment.
The method for removing internal residue from a substance container of this embodiment employs the substance transfer apparatus of this embodiment. By performing the procedures (1B) to (2B) above with the substance transfer apparatus of this embodiment, it is possible to ensure safety and, in particular, more smoothly remove internal residue from the equipment (substance container), thereby enabling safe and efficient substance handling. Furthermore, more smoothly removing internal residue from a substance container involves purging the substance container with an inert gas, which allows for more rapid start-up of the manufacturing equipment after maintenance, thereby improving the operating rate of the manufacturing equipment.

A method for removing internal residue from a substance container according to a ninth aspect of this embodiment includes:
the inert gas introduction mechanism introduces an inert gas from an inert gas inlet provided in the first container for the substance;
is.

In addition to introducing inert gas via valve 1a and the transfer auxiliary chamber, introducing inert gas from the first substance container also makes it possible to more efficiently remove internal residue from the substance container. As a result, substances can be handled more safely and efficiently, and the operating rate of the manufacturing equipment can also be improved.

[Matter transfer device]
The substance transfer device of this embodiment is
An apparatus for transferring a substance containing at least one atom selected from a sulfur atom and a halogen atom,
The apparatus comprises a transfer preliminary chamber, a transfer substance inlet and a transfer substance outlet, and an inert gas introduction mechanism and an exhaust mechanism,
the transfer substance inlet and transfer substance outlet are provided in the transfer prechamber and can be connected to the first substance inlet and first substance outlet of the first substance container and the second substance transfer port of the second substance container;
the inert gas introduction mechanism introduces the inert gas into the transfer preliminary chamber, and the inert gas exhaust mechanism exhausts the inert gas from the transfer preliminary chamber;
This is the device.

(Substances containing at least one atom selected from sulfur atoms and halogen atoms)
The substance to be transferred in the substance transfer device of this embodiment is not particularly limited as long as it contains at least one atom selected from sulfur atoms and halogen atoms.
For example, in a sulfide solid electrolyte production apparatus in which the substance transfer device of the present embodiment is suitably used, examples of the substance containing sulfur atoms include a solid electrolyte raw material containing sulfur atoms; an electrolyte precursor when a complexing agent is used, an intermediate such as a heat-treated product obtained by heat treatment in a solvent using a pressure-resistant container when a pressure-resistant container is used; and a sulfide solid electrolyte that will be the product.

Examples of substances containing halogen atoms include solid electrolyte raw materials containing halogen atoms; electrolyte precursors when a complexing agent is used, intermediates such as heat-treated products obtained by heat treatment using a pressure-resistant vessel when a pressure-resistant vessel is used; and sulfide solid electrolyte products that will be the product. Furthermore, examples of substances containing sulfur atoms and halogen atoms include intermediates such as electrolyte precursors and heat-treated products obtained using the above-mentioned solid electrolyte raw materials containing sulfur atoms and solid electrolyte raw materials containing halogen atoms; and sulfide solid electrolyte products that will be the product. Details of these solid electrolyte raw materials, intermediates, and sulfide solid electrolytes will be provided below.

As already mentioned, substances containing at least one atom selected from sulfur atoms and halogen atoms are solid electrolyte raw materials, intermediates, and sulfide solid electrolytes, and are basically in the form of powder, but may also be in the form of a liquid or a slurry containing powder.

(Solid electrolyte raw material)
Representative examples of the solid electrolyte raw material containing at least one atom selected from the sulfur atom and the halogen atom include lithium sulfide; lithium halides such as lithium fluoride, lithium chloride, lithium bromide, and lithium iodide; phosphorus sulfides such as phosphorus _trisulfide ( _P2S3 ) and phosphorus _pentasulfide ( _P2S5 ); elemental halogens such as bromine ( _Br2 ) and iodine ( _I2 ); and elemental sulfur. _{Li3PS4 ,} which has a _PS4 structure, can also be used as the solid electrolyte raw material.
These exemplified solid electrolyte raw materials are in solid (powder) or liquid form.

(Intermediate)
Representative examples of the intermediate include an electrolyte precursor obtained using the above-mentioned solid electrolyte raw material containing a sulfur atom and a solid electrolyte raw material containing a halogen atom, and a heat-treated product obtained by heat treatment using a pressure-resistant container when a pressure-resistant container is used.
The term "electrolyte precursor" refers to a complex formed by the combination of a solid electrolyte raw material and a solvent (also referred to as a "complexing agent") containing heteroatoms such as nitrogen atoms, oxygen atoms, halogen atoms (e.g., chlorine atoms), and sulfur atoms. These heteroatoms have a high affinity for lithium atoms, resulting in the formation of a complex. The complex formed by the combination of the solid electrolyte raw material and the complexing agent is heated and dried to remove the solvent containing the heteroatoms that make up the complex, thereby producing a solid electrolyte, hence the term "electrolyte precursor."

More specifically, the heat-treated product obtained by heat treatment using a pressure-resistant vessel is preferably obtained by pulverizing the above-mentioned solid electrolyte raw material as needed, coarsely mixing the resulting pulverized product as needed, and then mixing and pulverizing the resulting solid electrolyte mixture in a solvent, followed by heat treatment using a pressure-resistant vessel. The solvent used here may be a non-polar solvent such as a hydrocarbon solvent, and preferably also at least one polar solvent selected from nitrile compounds and ether compounds.

The heat treatment is carried out at a heating temperature of preferably 150 to 300°C, more preferably 160 to 280°C.
The heat-treated product thus obtained can be called an intermediate because an argyrodite-type solid electrolyte can be obtained by firing it.

(Sulfide solid electrolyte)
The sulfide solid electrolyte can be obtained, for example, by removing the complexing agent from the electrolyte precursor or by firing the heat-treated product. Examples of the sulfide solid electrolyte include an amorphous sulfide solid electrolyte and a crystalline sulfide solid electrolyte, which will be described later.

Representative examples of amorphous sulfide solid electrolytes include sulfide solid electrolytes composed of lithium sulfide _{, phosphorus} sulfide _, and lithium halide, such as Li ₂ S—P ₂ S ₅ , Li ₂ S—P ₂ S ₅ -LiI, Li ₂ S—P ₂ S ₅ -LiCl, Li ₂ S—P ₂ S ₅ -LiBr, and Li 2 S—P 2 S 5 -LiI-LiBr; and sulfide solid electrolytes further containing other atoms such as oxygen atoms and silicon atoms, such as Li ₂ S—P ₂ S ₅ -Li ₂ O—LiI, Li ₂ S—P ₂ S ₅ -Li ₂ O—LiI-LiBr, and Li ₂ S—SiS ₂ -P ₂ S ₅ Preferred examples of the solid electrolyte include sulfide solid electrolytes such as LiI.
The types of atoms constituting the amorphous sulfide solid electrolyte can be confirmed, for example, by an ICP emission spectrometer.

The crystalline sulfide solid electrolyte may be a so-called glass ceramic obtained by heating an amorphous sulfide solid electrolyte to a temperature equal to or higher than the crystallization temperature, and examples of the crystal structure include a Li ₃ PS ₄ crystal structure, a Li ₄ P ₂ S ₆ crystal structure, a Li ₇ PS ₆ crystal structure, a Li ₇ P ₃ S ₁₁ crystal structure, and a crystal structure having peaks at 2θ=approximately 20.2° and 23.6° (for example, JP 2013-16423 A).

Other examples include a Li _4-x Ge _1-x P _x S ₄ based thio-LISICON Region II type crystal structure (see Kanno et al., Journal of The Electrochemical Society, 148(7)A742-746(2001)), a crystal structure similar to a Li _4-x Ge _1-x P _x S ₄ based thio-LISICON Region II type (see Solid State Ionics, 177(2006), 2721-2725), and the like.

Another preferred example is a crystalline sulfide solid electrolyte having the above-mentioned Li ₇ PS ₆ structural skeleton and an argyrodite-type crystal structure in which part of the P is substituted with Si.
Examples of the composition formula of the argyrodite-type crystal structure include the crystal structures represented by the composition formula Li _7-x P _1-y Si _y S ₆ and Li _7+x P _1-y Si _y S ₆ (x is −0.6 to 0.6, y is 0.1 to 0.6), and the composition formula of the argyrodite-type crystal structure also includes the composition formula Li _7-x-2y PS _6-x-y Cl _x (0.8≦x≦1.7, 0<y≦−0.25x+0.5).

(Application)
The substance transfer device of this embodiment is suitable for use in a sulfide solid electrolyte production apparatus, as described above. Specifically, the substance transfer device is used by connecting to a component of the sulfide solid electrolyte production apparatus, through which a substance containing at least one atom selected from sulfur atoms and halogen atoms flows during operation of the production apparatus, or to a substance container for storing the substance.

When the material transfer apparatus of this embodiment is used in a connected manner, the equipment constituting the sulfide solid electrolyte production apparatus to which it is connected may vary depending on the sulfide solid electrolyte production method, but mainly includes reaction equipment used for reacting the solid electrolyte raw materials; when a solvent (including a complexing agent) is used, heating equipment for removing the solvent (including a complexing agent) from a slurry or solution containing the solid electrolyte raw materials and/or intermediates such as an electrolyte precursor and the solvent (including a complexing agent); heating equipment for crystallization, etc.; separation equipment for separating the sulfide solid electrolyte; particle size adjustment equipment for adjusting the particle size of the sulfide solid electrolyte; when heat treatment is performed using a pressure-resistant container, heating equipment for firing the pressure-resistant container and the heat-treated product; piping connecting these devices; and material containers for storing the above-mentioned materials. These devices will be described in detail in the description of the sulfide solid electrolyte production method and production apparatus.

(Configuration of material transfer device)
The structure of the substance transfer device of this embodiment will be described with reference to FIG.
1 shows that the substance transfer device of this embodiment is equipped with a transfer preliminary chamber, a transfer substance inlet and outlet ports, and an inert gas introduction mechanism and exhaust mechanism. The area enclosed by the boundary line indicated as "B/L" (abbreviation for "battery limit") in FIG. 1 corresponds to the range of the substance transfer device of this embodiment.

The transfer substance inlet and outlet ports of the substance transfer device are provided in the transfer preparation chamber, and are preferably provided at both ends of the transfer preparation chamber as shown in Figure 1. Furthermore, the transfer substance inlet and outlet ports of the substance transfer device can be connected to the first substance inlet and first substance outlet ports of the first substance container and the second substance transfer port of the second substance container; in Figure 1 they are connected to the first substance outlet port of the first substance container and the second substance transfer port of the second substance container, respectively, and the substance transfer device of this embodiment is shown as being configured to connect the first substance container and the second substance container.

FIG. 1 shows that the inert gas introduction mechanism and exhaust mechanism are provided in the transfer pre-chamber, and can introduce and exhaust the inert gas into the transfer pre-chamber. FIG. 1 also shows that, in a preferred embodiment, the inert gas introduction mechanism further introduces the inert gas from an inert gas inlet provided in the first substance container.

In Figure 1, a manner in which a substance stored in a first substance container is transferred to a second substance container is shown. As shown in Figure 1, the substance is preferably transferred by gravity.

In Figure 1, it is stated that the first substance container has a "first substance inlet portion (outlet portion)" and a "first substance outlet portion (inlet portion)." This means that the first substance inlet portion can become the first substance outlet portion depending on the manner in which the substance transfer device of this embodiment is used, and the first substance outlet portion can become the first substance inlet portion. As mentioned above, in Figure 1, an embodiment is shown in which a substance stored in the first substance container is transferred to the second substance container. However, conversely, when a substance stored in the second substance container is transferred to the first substance container, i.e., when a substance stored in the second substance container is transferred to the first substance container under its own weight, the first substance inlet portion becomes the first substance outlet portion, and the first substance outlet portion becomes the first substance inlet portion.

Furthermore, Figure 1 shows that a valve 1a is provided between the transfer object inlet port of the material transfer device of this embodiment and the first material outlet port of the first material container, and a valve 2 is provided between the transfer object outlet port of the material transfer device of this embodiment and the second material transfer port of the second material container. These valves are provided to separate the material transfer device of this embodiment from the first material container and the second material container, and are used when transferring material between the first material container and the second material container. These valves may be valves provided in the first material container and the second material container as shown in Figure 1, or may be valves provided in the material transfer device of this embodiment.

(Transportation spare room)
The transfer chamber is a flow path through which the substance passes when transferring the substance between the first and second substance containers, and can also be used to temporarily store the substance depending on the situation.

The shape of the transfer pre-chamber is not particularly limited as long as it allows the substance to pass through it and can be provided with an inert gas introduction mechanism and exhaust mechanism. When it is piping-shaped, the cross-sectional shape is preferably the same as the cross-sectional shapes of the first substance inlet and first substance outlet of the first substance container and the second substance transfer port of the second substance container, which will be described later. Preferred shapes include circle, ellipse, rectangle, and square, with circle and ellipse being more preferred, and circle being even more preferred. That is, the shape of the transfer pre-chamber is preferably cylindrical. More specifically, preferred cylindrical shapes include a cylinder, elliptical cylinder, and rectangular cylinder, with cylinder and elliptical cylinder being more preferred, and cylinder being even more preferred. By using such a shape, the substance is less likely to remain in the transfer pre-chamber during substance transfer, allowing for smoother substance transfer.

When the preliminary transfer chamber is cylindrical, the preliminary transfer chamber can be configured, for example, by piping. By configuring the preliminary transfer chamber by piping, the substance transfer device of this embodiment can be easily adjusted to a desired size and shape, and the substance is less likely to remain in the preliminary transfer chamber during substance transfer, allowing for smoother substance transfer.
Furthermore, the shape of the transfer pre-chamber can be determined according to the desired shape; for example, if it is cylindrical (when constructed from piping), it can be linear (straight piping), or serpentine (serpentine piping). Considering that this makes it less likely for the substance to remain in the transfer pre-chamber when transferring the substance and allows for smoother transfer of the substance, a linear shape (straight piping) is preferable.

The size of the cross-sectional shape of the transfer pre-chamber, like the above cross-sectional shape, is preferably the same as the size of the first substance inlet and first substance outlet of the first substance container and the second substance transfer port of the second substance container, described below. When the transfer pre-chamber is cylindrical, the diameter (inner diameter) of the cross-sectional shape is typically 5 mm or more and 310 mm or less, preferably 10 mm or more, more preferably 20 mm or more, with an upper limit of preferably 260 mm or less, more preferably 220 mm or less. When the transfer pre-chamber is constructed using piping, the size of the piping is typically 1/4 inch or more and 12 inches or less, preferably 1/2 inch or more, more preferably 1 inch or more, with an upper limit of preferably 10 inches or less, more preferably 8.5 inches or less.

Regarding the shape of the transfer pre-chamber, there are no particular restrictions on its length as long as it can accommodate an inert gas introduction and exhaust mechanism, and it can be determined depending on the installation location, etc., so it is difficult to generalize, but the length of the piping portion should usually be between 10 cm and 1 m.

(Transferred substance inlet and outlet)
The transfer substance inlet and outlet provided in the preliminary transfer chamber are not particularly limited as long as they can be connected to the first substance inlet and first substance outlet of the first substance container and the second substance transfer port of the second substance container, and for example, when the preliminary transfer chamber is cylindrical (configured by piping), it is preferable that they be provided at both ends of the cylinder (piping) as shown in Figure 1. This makes it easier to connect the first substance container and the second substance container, improving the convenience of the substance transfer device of this embodiment.

In order to facilitate easier connection to the first and second substance containers and improve convenience, the transfer substance inlet and outlet ports provided in the transfer preparation chamber preferably adopt a format that corresponds to the format of the first substance inlet and outlet ports of the first substance container and the second substance transfer port of the second substance container. For example, a connection format using a piping joint such as a flange or threaded joint is preferable. By adopting such a format, the first substance inlet and outlet ports and second substance transfer port of the substance transfer device of this embodiment can be easily attached and detached, improving convenience. Furthermore, as shown in Figure 1, if gate valves such as valve 1a and valve 2 (see Figure 1) are used as needed, attachment and detachment to these valves becomes easier, improving convenience.

(Inert gas introduction mechanism and exhaust mechanism)
The inert gas introduction mechanism is not particularly limited as long as it can introduce the inert gas into the transfer preparatory chamber, and preferably includes, for example, a connection part for receiving the inert gas from an inert gas supply source, a pipe from the connection part to the transfer preparatory chamber, and a gate valve in the pipe, as shown in Fig. 1. By including the gate valve, the transfer method described below can be performed more easily, improving convenience.

When the preliminary transfer chamber is cylindrical, as shown in Fig. 1, the inert gas introduction mechanism is preferably provided on the side surface thereof. More specifically, the piping for supplying the inert gas from the connecting portion to the preliminary transfer chamber is preferably connected to the side surface of the preliminary transfer chamber. This connection allows for more stable introduction of the inert gas, thereby ensuring safety and enabling smoother transfer of substances, among other things, and enabling safer and more efficient handling of substances.
In the inert gas introduction mechanism, the piping for supplying the inert gas from the connecting part to the transfer preparation chamber may be connected to the transfer preparation chamber by a connection method such as a pipe joint with a flange or a screw, or may be directly connected to the transfer preparation chamber as shown in FIG. 1.

The inert gas exhaust mechanism is not particularly limited as long as it can exhaust the inert gas from the transfer preparatory chamber. For example, as shown in Figure 1, it is preferable that it includes a connection section that exhausts the inert gas from the transfer preparatory chamber to an inert gas exhaust line, piping to the connection section, and a gate valve within the piping. The inclusion of a gate valve makes it easier to carry out the transfer method described below, improving convenience.

When the preliminary transfer chamber is cylindrical, as shown in Fig. 1, the inert gas exhaust mechanism is preferably provided on the side of the chamber. More specifically, the piping for exhausting the inert gas from the preliminary transfer chamber is preferably connected to the side of the preliminary transfer chamber. This connection allows for more stable exhaust of the inert gas, ensuring safety and enabling smoother transfer of substances, among other things, and enabling safer and more efficient handling of substances.
In addition, in the inert gas introduction mechanism, the piping for discharging the gas from the transfer preparation chamber may be connected to the transfer preparation chamber by a connection method such as a pipe joint with a flange or a screw, or may be directly connected to the transfer preparation chamber as shown in FIG. 1.

The inert gas used in the material transfer device of this embodiment can be, for example, a rare gas such as helium or argon; nitrogen, etc., with nitrogen being preferred in particular given its versatility.

[Method for transferring substances]
The substance transfer method of this embodiment includes:
The apparatus comprises a transfer preliminary chamber, a transfer substance inlet and a transfer substance outlet, and an inert gas introduction mechanism and an exhaust mechanism,
the transfer substance inlet and transfer substance outlet are provided in the transfer prechamber and can be connected to the first substance inlet and first substance outlet of the first substance container and the second substance transfer port of the second substance container;
the inert gas introduction mechanism introduces the inert gas into the transfer preliminary chamber, and the inert gas exhaust mechanism exhausts the inert gas from the transfer preliminary chamber;
using a transfer device for a substance containing at least one atom selected from a sulfur atom and a halogen atom,
A method for transferring a substance, comprising the steps of (1A) to (3A) below:
is.
(1A) The transfer substance inlet portion is connected to a valve 1a provided at the substance outlet portion of the first substance storage container, and the transfer substance outlet portion is connected to a valve 2 provided at the second substance transfer port portion of the second substance container.
(2A) The valves 1a and 2 are closed, and the inert gas is supplied and discharged by the inert gas introduction mechanism and discharge mechanism, filling the inert gas into the transfer preliminary chamber.
(3A) The supply and discharge of the inert gas are stopped, the valves 1a and 2 are opened, and the substance stored in the first substance container is transferred to the second substance container.

As already mentioned, the material transfer method of this embodiment employs the material transfer device of this embodiment. The configuration of the material transfer device employed in the material transfer method of this embodiment is as described above for the material transfer device of this embodiment.

In the material transfer method of this embodiment, the material transfer device of this embodiment is used to perform the operations in the above steps (1A) to (3A). Valve 1a and valve 2 used in operations (1A) to (3A) are shown in Figure 1 as being provided in the first material container and second material container, but they may also be valves provided in the material transfer device.

Operation (1A) is an operation for connecting the substance transfer device of this embodiment to the first substance container and the second substance container. The next operation (2A) is an operation for filling the preliminary transfer chamber with an inert gas before transferring the substance from the first substance container to the second substance container. This operation prevents the substance from reacting with moisture in the atmosphere as it passes through the preliminary transfer chamber, allowing for safer substance transfer.

Operation (3A) is an operation in which the substance stored in the second substance container is transferred from the first substance container to the second substance container. By performing operations (1A) and (2A) above, the transfer chamber is filled with inert gas, and the substance can be transferred in an environment where all moisture, including atmospheric moisture, has been removed. This ensures safety and, in particular, allows the substance to be transferred more smoothly, making it possible to handle the substance more safely and efficiently.

In addition, in the method for transferring a substance according to the present embodiment, it is preferable to carry out the above-mentioned operation (3A) followed by the above-mentioned operation (2A) and the following operations (4A) and (5A).
(4A) The second substance container and valve 2 are removed from the transfer substance outlet.
(5A) A closing flange is attached to the outlet portion of the transfer substance.

By performing operation (2A) following operation (3A), the second substance container, which transfers and stores the substance, can be safely removed from the first substance container. This means that operation (4A) below can be performed safely, and the removed second substance container can be transported to the desired location. Furthermore, by performing operation (5A), it is possible to isolate the first substance container from the outside air. Even if substance remains inside the first substance container and passes through valve 1a, it will be stored in the substance transfer device filled with inert gas, and the closing flange prevents atmospheric air containing moisture from entering the substance transfer device. This prevents the substance from reacting with moisture in the atmosphere, allowing for safe handling of the substance.

The substance transfer method of this embodiment is intended to be a method of transferring a substance from a first substance container to a second substance container. The first substance container and the second substance container are containers used for various purposes, such as mixing, drying, grinding, storing, preserving, and transferring substances. In the substance transfer method of this embodiment, the first substance container is used for purposes such as mixing, drying, grinding, and storing substances, and the second substance container is a container used to transfer the substance stored in the first substance container to another location. More specifically, it is intended that, for example, a sulfide solid electrolyte produced by a sulfide solid electrolyte production apparatus and stored in the first substance container is shipped as a product in the second substance container into which the sulfide solid electrolyte was transferred.

Regarding the method for transferring a substance, as an embodiment different from the method for transferring a substance of this embodiment, it is also possible to transfer a substance from a second substance container to a first substance container. As mentioned above, Figure 1 describes a "first substance inlet (outlet)" and a "first substance outlet (inlet)," and the first substance inlet can be a first substance outlet, and the first substance outlet can be a first substance inlet. In this case, as shown in Figure 2, by connecting the first substance container and the second substance container via the substance transfer device of this embodiment, it is possible to transfer the substance stored in the second substance container to the first substance container.

A method for transferring a substance according to another embodiment different from the method for transferring a substance according to this embodiment includes the following steps:
The apparatus comprises a transfer preliminary chamber, a transfer substance inlet and a transfer substance outlet, and an inert gas introduction mechanism and an exhaust mechanism,
the transfer substance inlet and transfer substance outlet are provided in the transfer prechamber and can be connected to the first substance inlet and first substance outlet of the first substance container and the second substance transfer port of the second substance container;
the inert gas introduction mechanism introduces the inert gas into the transfer preliminary chamber, and the inert gas exhaust mechanism exhausts the inert gas from the transfer preliminary chamber;
using a transfer device for a substance containing at least one atom selected from a sulfur atom and a halogen atom,
A method for transferring a substance, comprising the following operations (1B) to (3B):
(1B) The transfer substance inlet portion is connected to a valve 2 provided at the second substance transfer port portion of the second substance container, and the transfer substance outlet portion is connected to a valve 1b provided at the first substance inlet portion of the first substance container.
(2B) The valves 1b and 2 are closed, and the inert gas is supplied and discharged by the inert gas introduction mechanism and discharge mechanism, filling the inert gas into the transfer preliminary chamber.
(3B) The supply and discharge of the inert gas are stopped, the valves 1b and 2 are opened, and the substance stored in the second substance container is transferred to the first substance container.

In a substance transfer method according to a different embodiment from the substance transfer method of this embodiment, the first substance container is used for purposes such as mixing, drying, grinding, and storing substances, and the second substance container is a container used to transfer an object received at a location separate from the first substance container to the first substance container. More specifically, for example, a solid electrolyte raw material that is commercially available or produced by a different manufacturing device is transferred to the second substance container, the second substance container storing the solid electrolyte raw material is connected to the first substance container via a substance transfer device, and the solid electrolyte raw material is transferred from the second substance container to the first substance container and used to produce a sulfide solid electrolyte. When a solid electrolyte raw material that is commercially available or produced by a different manufacturing device is transferred to the second substance container, the substance can be transferred to the second substance container in a manner similar to the substance transfer method of this embodiment.

[Method for removing internal residue from a substance container]
The method for removing internal residues from a substance container according to this embodiment includes the steps of:
The apparatus comprises a transfer preliminary chamber, a transfer substance inlet and a transfer substance outlet, and an inert gas introduction mechanism and an exhaust mechanism,
the transfer substance inlet and transfer substance outlet are provided in the transfer prechamber and can be connected to the first substance inlet and first substance outlet of the first substance container and the second substance transfer port of the second substance container;
the inert gas introduction mechanism introduces the inert gas into the transfer preliminary chamber, and the inert gas exhaust mechanism exhausts the inert gas from the transfer preliminary chamber;
using a transfer device for a substance containing at least one atom selected from a sulfur atom and a halogen atom,
A method for removing internal residues from a substance container, comprising the steps of (1B) and (2B) below:
is.
(1B) The transfer substance inlet is connected to the valve 1a provided at the substance outlet of the first substance container.
(2B) The valve 1a is opened, and the inert gas is supplied and discharged by the inert gas introduction mechanism and discharge mechanism, filling the inert gas into the transfer pre-chamber and the first substance container.

As already mentioned, the method for removing internal residue from a substance container of this embodiment employs the substance transfer device of this embodiment. The configuration of the substance transfer device employed in the method for removing internal residue from a substance container of this embodiment is as described above for the substance transfer device of this embodiment.

In the method for removing internal residue from a substance container of this embodiment, the substance transfer device of this embodiment is used to perform the operations (1B) and (2B) described above. Valve 1a used in operations (1B) and (2B) is shown in Figure 1 as being provided in the first substance container and the second substance container, but it may also be a valve provided in the substance transfer device.

Furthermore, in the method for removing internal residues from a substance container of this embodiment, it is preferable to introduce an inert gas through an inert gas inlet provided in the first substance container using an inert gas introduction mechanism. This makes it possible to more efficiently remove internal residues from the substance container. As a result, substances can be handled more safely and efficiently, and the operating rate of the manufacturing equipment can also be improved.

The substance transfer device, substance transfer method, and method for removing internal residue from a substance container of this embodiment are suitable for use in a sulfide solid electrolyte manufacturing device. The sulfide solid electrolyte obtained by the sulfide solid electrolyte manufacturing device has high ionic conductivity, and is therefore suitable for use as a solid electrolyte or electrode composite in lithium ion batteries, particularly lithium ion batteries used in information-related devices and communication devices such as personal computers, video cameras, and mobile phones, as well as vehicles such as automobiles, and particularly all-solid-state batteries.

Claims (9)

An apparatus for transferring a substance containing at least one atom selected from a sulfur atom and a halogen atom,
The apparatus comprises a transfer preliminary chamber, a transfer substance inlet and a transfer substance outlet, and an inert gas introduction mechanism and an exhaust mechanism,
the transfer substance inlet and transfer substance outlet are provided in the transfer prechamber and can be connected to the first substance inlet and first substance outlet of the first substance container and the second substance transfer port of the second substance container;
the inert gas introduction mechanism introduces the inert gas into the transfer preliminary chamber, and the inert gas exhaust mechanism exhausts the inert gas from the transfer preliminary chamber;
Material transfer equipment. The substance transfer device of claim 1, wherein the inert gas introduction mechanism further introduces inert gas from an inert gas inlet provided in the first substance container. The material transfer device according to claim 1 or 2, wherein the transfer pre-chamber is cylindrical. The material transfer device described in claim 3, wherein the transfer material inlet and transfer material outlet are provided at both ends of the cylindrical transfer pre-chamber. A material transfer device as described in claim 3 or 4, wherein the inert gas introduction mechanism and exhaust mechanism are provided on the side of the cylindrical transfer pre-chamber. The apparatus comprises a transfer preliminary chamber, a transfer substance inlet and a transfer substance outlet, and an inert gas introduction mechanism and an exhaust mechanism,
the transfer substance inlet and transfer substance outlet are provided in the transfer prechamber and can be connected to the first substance inlet and first substance outlet of the first substance container and the second substance transfer port of the second substance container;
the inert gas introduction mechanism introduces the inert gas into the transfer preliminary chamber, and the inert gas exhaust mechanism exhausts the inert gas from the transfer preliminary chamber;
using a transfer device for a substance containing at least one atom selected from a sulfur atom and a halogen atom,
A method for transferring a substance, comprising the following operations (1A) to (3A):
(1A) The transfer substance inlet portion is connected to a valve 1a provided at the substance outlet portion of the first substance container, and the transfer substance outlet portion is connected to a valve 2 provided at the second substance transfer port portion of the second substance container.
(2A) The valves 1a and 2 are closed, and the inert gas is supplied and discharged by the inert gas introduction mechanism and discharge mechanism, filling the inert gas into the transfer preliminary chamber.
(3A) The supply and discharge of the inert gas are stopped, the valves 1a and 2 are opened, and the substance stored in the first substance container is transferred to the second substance container. 7. The method for transferring a substance according to claim 6, wherein the steps (3A) are followed by the steps (2A) and (4A) and (5A) below.
(4A) The second substance container and valve 2 are removed from the transfer substance outlet.
(5A) A closing flange is attached to the outlet portion of the transfer substance. The apparatus comprises a transfer preliminary chamber, a transfer substance inlet and a transfer substance outlet, and an inert gas introduction mechanism and an exhaust mechanism,
the transfer substance inlet and transfer substance outlet are provided in the transfer pre-chamber and can be connected to a first substance inlet and a first substance outlet of a first substance container and a second substance transfer port of a second substance container;
the inert gas introduction mechanism introduces the inert gas into the transfer preliminary chamber, and the inert gas exhaust mechanism exhausts the inert gas from the transfer preliminary chamber;
using a transfer device for a substance containing at least one atom selected from a sulfur atom and a halogen atom,
A method for removing internal residues from a substance container, comprising the steps of (1B) and (2B) below.
(1B) The transfer substance inlet is connected to the valve 1a provided at the substance outlet of the first substance container.
(2B) The valve 1a is opened, and the inert gas is supplied and discharged by the inert gas introduction mechanism and discharge mechanism, filling the inert gas into the transfer pre-chamber and the first substance container. 9. The method for removing internal residues from a substance container according to claim 8, wherein the inert gas introducing mechanism introduces the inert gas from an inert gas inlet provided in the first substance container.