JP7277896B2 - Container with filter, filter member, purification device, and method for producing purified substance - Google Patents

Description

TECHNICAL FIELD The present invention relates to a filter- equipped container, a filter member, a purification device, and a method for producing a purified substance, which are used in the purification of substances.

The technique of Patent Document 1 is known for sublimation purification. In the technique disclosed in Patent Literature 1, a filter is arranged in the tube-diameter-reduced portion of the sublimation tube.

Japanese Patent Application Laid-Open No. 2005-111303

By the way, when the filter is clogged, the gas may pass through the filter and become nasty, which may lengthen the time required for purification. Therefore, a filter-equipped container, a filter member, a purification device, and a method for producing a purified substance, which can suppress a decrease in purification efficiency, are provided.

(1) A filter that solves the above problems is a filter used in a purification method including a step of vaporizing a substance, and is in the form of a sheet, at least a portion of which is curved or bent to allow gas to pass through. Vaporization includes evaporation and sublimation.

According to this configuration, since the filter has a curved portion or a bent portion, the area of the surface through which gas passes is increased, and clogging is less likely to occur in the filter. As a result, a decrease in purification efficiency can be suppressed.

(2) A filter-equipped container for solving the above problems is a filter material at least partially curved or bent to allow gas to pass through, the filter material containing a substance to be purified, and a plug member closing an opening of the filter material. and

According to this configuration, since the filter material has a curved portion or a bent portion, the area of the surface through which the gas passes is increased, and clogging is less likely to occur in the filter material. As a result, a decrease in purification efficiency can be suppressed.

(3) A filter-equipped container that solves the above problems is a filter material that is at least partially curved or bent and allows gas to pass through, and is composed of a plurality of filter materials containing a substance to be purified and an internal space within the filter material. a connecting member that connects the plurality of filter materials so as to be connected.

According to this configuration, since the filter material has a curved portion or a bent portion, the area of the surface through which the gas passes is increased, and clogging is less likely to occur in the filter material. As a result, a decrease in purification efficiency can be suppressed.

(4) A filter member that solves the above problems is a filter material that is at least partially curved or bent and allows gas to pass through, wherein and a mounting member for mounting the filter material.

According to this configuration, since the filter material has a curved portion or a bent portion, the area of the surface through which the gas passes is increased, and clogging is less likely to occur in the filter material. As a result, a decrease in purification efficiency can be suppressed.

(5) A purifying apparatus for solving the above problems includes at least one purifying vessel, an outer tube accommodating the purifying vessel, and a decompression device for reducing the pressure in the outer tube, wherein at least one of the purifying vessels is , the filter, container with filter, or filter member described above can be arranged.

According to this configuration, since the refining device has at least one of the filter, the container with the filter, and the filter member, which are less likely to clog, a decrease in gas flow is suppressed. In this way, a decrease in purification efficiency is suppressed.

(6) In the above refiner, the outer tube has a first open end arranged on the downstream side and a second open end opposite to the first open end, and the downstream in the outer tube It further comprises a cap positioned to face the side first open end.

According to this configuration, since the flow of the gas is blocked by the cap, substances contained in the gas tend to condense in the vicinity of the first opening end on the downstream side of the outer tube. As a result, the amount of impurities in the gas flowing downstream from the outer tube can be reduced compared to the case where the cap is not provided. As a result, contamination by substances can be suppressed in the section between the first open end of the outer tube and the decompression device.

(7) A method for producing a purified substance that solves the above-mentioned problems, wherein the filter, the container with a filter, or the filter member is arranged in the purification container where the gas passes through when diffusing the gas of the substance to be purified. and reducing the pressure in the refining vessel.

According to this configuration, one of the filter, the container with the filter, and the filter member, which is less likely to clog, is arranged in the middle of the gas circulation path, thereby suppressing a decrease in gas circulation. This makes it possible to suppress a decrease in purification efficiency.

According to the filter, the container with the filter, the filter member, the purification device, and the method for producing a purified substance, it is possible to suppress a decrease in purification efficiency.

The perspective view of the filter which concerns on 1st Embodiment. The figure which shows the usage example of the filter which concerns on 1st Embodiment. The perspective view of the filter which concerns on 2nd Embodiment. The perspective view of the filter which concerns on 3rd Embodiment. The figure which shows the usage example of the filter which concerns on 3rd Embodiment. The exploded view of the container with a filter which concerns on 4th Embodiment. Sectional drawing of the container with a filter which concerns on 4th Embodiment. The figure which shows the usage example of the container with a filter which concerns on 4th Embodiment. The exploded view of the container with a filter which concerns on 5th Embodiment. Sectional drawing of the container with a filter which concerns on 5th Embodiment. The perspective view of a filter base material about the container with a filter which concerns on 6th Embodiment. The exploded view of the container with a filter which concerns on 6th Embodiment. The perspective view of the container with a filter which concerns on 6th Embodiment. The figure which shows the usage example of the container with a filter which concerns on 7th Embodiment. The figure which shows the usage example about the filter member which concerns on 8th Embodiment. The figure which shows the usage example about the filter member which concerns on 9th Embodiment. The figure which shows the usage example about the filter member which concerns on 10th Embodiment. The side view of the refiner|purifier which concerns on 11th Embodiment. The top view of the refiner|purifier which concerns on 11th Embodiment. FIG. 11 is a partial cross-sectional view of a refining device according to an eleventh embodiment;

<First embodiment>
A filter 10 according to the first embodiment will be described with reference to FIGS. 1 and 2. FIG.
The filter 10 according to this embodiment is used in purification including a process of vaporizing substances. An example of a purification method including a step of vaporizing a substance is described below.

A purification target substance MA is accommodated in a tubular purification container extending in one direction. The inside of the purification vessel is decompressed to a predetermined pressure of 10 ⁻⁴ Pa or more and 100 Pa or less by a decompression device. Under such reduced pressure, the purification vessel is heated either by an external heater or by an internal heater located inside the outer tube. A longitudinal temperature gradient is applied in the purification vessel. A portion of the purification container where the substance to be purified MA is placed (hereinafter referred to as “substance placement portion”) is heated to a temperature at which the substance to be purified MA can be sublimated. The purification vessel is thermally graded so that the temperature decreases downstream from the material placement portion. In the refining vessel, a predetermined portion downstream of the material disposing portion is maintained at an appropriate temperature at which the desired refining material MB precipitates. By applying a temperature gradient to the purification container under reduced pressure in this way, the purified substance MB can be obtained. The substance MA to be purified may be solid or liquid.

By the way, when the purification vessel is heated under reduced pressure, the substance to be purified MA may enter a state similar to bumping (hereinafter collectively referred to as a bumping state). The bumping state includes a state in which the material to be purified MA scatters in the form of powder. In the bumping state, the purification target material MA before vaporization may fly up to the part where the purification material MB is deposited in the purification vessel, and the purity of the purification material MB may be lowered. Therefore, the filter 10 is arranged downstream of the purification target material MA in the flow of gas in which the purification target material MA is vaporized.

In purification, the filter 10 according to the present embodiment prevents powder and droplets generated from the purification target material MA from scattering downstream from the filter 10 when the purification target material MA is in a bumping state. The filter 10 is sheet-like and allows gas to pass therethrough. The filter 10 may be permeable to liquid, but at least is configured to prevent the passage of flying liquid droplets. When the substance to be purified MA is liquid, the filter 10 is configured to prevent splashing of droplets.

The filter 10 is preferably non-gassing due to heat. For example, the filter 10 is made of at least one of silica fiber, glass fiber, fluororesin fiber, and carbon fiber. Specifically, filter 10 is formed from a nonwoven or woven sheet. The particle size retained by the filter 10 is preferably 1 μm or more and 30 μm or less. This is because if the particle size retained by the filter 10 is larger than 30 μm, the purification target substance MA may pass through the filter 10 . The retained particle diameter indicates the particle diameter capable of retaining 90% mass or more of the JIS-Z-8901 class 7 powder dispersion water after gravity filtration. Filter 10 may be formed from a porous sheet. For example, filter 10 may be formed from a porous fluororesin sheet.

The thickness of the filter 10 is set to a predetermined value. If the thickness of the filter 10 is too thin, it becomes difficult to retain its shape. Moreover, if the thickness of the filter 10 is too large, the flow of gas is obstructed. For this reason, the thickness of the filter 10 is preferably 100 μm or more and 5 mm or less.

At least a portion of filter 10 is curved or folded. Having curved or bent portions in the filter 10 increases the surface area of the filter 10 . By increasing the surface area of the filter 10, the area of the portion of the filter 10 through which gas can pass is increased.

As shown in FIG. 1, in this embodiment, the filter 10 has a shape of a curved rectangle. The filter 10 has two opposing straight sides 11 and 11 and two opposing curved sides 12 and 12 . The two sides 11, 11 extend parallel. The surface area of the filter 10 is larger than that of a virtual planar filter 10x configured to include two sides 11, 11 (see FIG. 1).

As shown in FIG. 2, the filter 10 shown in this embodiment can be suitably used for a purification vessel 15 having a cylindrical portion 15a. The length of the two sides 11 , 11 is equal to the length LA of the tubular portion 15 a of the refining vessel 15 . One of the two curved sides 12 , 12 of the filter 10 contacts the bottom surface 15 b of the purification container 15 , and the other contacts the peripheral portion 15 d of the opening 15 c of the purification container 15 . Filter 10 has flexibility. When the filter 10 is placed in the purification vessel 15, it is rolled into a cylinder. The filter 10 partitions the internal space of the purification container 15 into a first space SA and a second space SB. The first space SA is connected to the opening 15c. The second space SB constitutes a storage space in which the material to be purified MA is placed.

The operation of this embodiment will be described.
Filter 10 is used in purification methods that involve vaporizing a substance. The filter 10 is sheet-shaped, at least a portion of which is curved, and allows gas to pass therethrough. Since the filter 10 has a curved portion, the area of the surface through which the gas passes is increased, and clogging is less likely to occur in the filter 10 .

Effects of the present embodiment will be described.
Even if bumping occurs during heating for refining, the filter 10 suppresses diffusion of the refining target material MA in a state before vaporization. Also, the scattered matter caused by the bumping stays in the space partitioned by the filter 10 . Even if bumping occurs, a decrease in yield can be suppressed. Furthermore, as described above, since clogging of the filter 10 is unlikely to occur, a decrease in purification efficiency can be suppressed.

<Second embodiment>
A filter 20 according to the second embodiment will be described with reference to FIG.
In the filter 20 according to this embodiment, the same reference numerals as in the first embodiment are given to the configurations common to the first embodiment, and the description thereof will be omitted. The use of the filter 20 and the material of the filter 20 conform to the first embodiment.

As shown in FIG. 3, the filter 20 according to this embodiment is bent. Specifically, the filter 20 has a plurality of mountain folds 21 and a plurality of valley folds 22 . In the filter 20, the mountain folds 21 and the valley folds 22 are alternately arranged. The mountain folds 21 and the valley folds 22 extend from one end to the other end of the filter 20 . The filter 20 expands and contracts in the direction in which the mountain folds 21 and the valley folds 22 are arranged.

The filter 20 of this embodiment is used in a purification method including a step of vaporizing substances. The filter 20 has a sheet shape, at least a portion of which is bent, and allows gas to pass therethrough. Since the filter 20 has a bent portion, the area of the surface through which the gas passes is increased, and clogging is less likely to occur in the filter 20 . As a result, a decrease in purification efficiency can be suppressed.

<Third Embodiment>
A filter 30 according to the third embodiment will be described with reference to FIGS. 4 and 5. FIG.
In the filter 30 according to this embodiment, the same reference numerals as in the first embodiment are given to the configurations common to the first embodiment, and the description thereof will be omitted. The use of the filter 30 and the material of the filter 30 conform to the first embodiment.

As shown in FIG. 4, in this embodiment, the filter 30 has a shape of a curved quasi-ellipse.
As shown in FIG. 5, the filter 30 shown in this embodiment can be suitably used for the purification vessel 15 having the cylindrical portion 15a. The outline of the filter 30 is configured to contact the inner peripheral surface of the cylindrical portion 15a. Filter 30 has flexibility. When the filter 30 is placed in the purification vessel 15, it is rolled into a cylinder. The filter 30 partitions the inner space of the purification container 15 into a third space SC and a fourth space SD. The third space SC is connected to the opening 15c. The fourth space SD constitutes an accommodation space in which the substance to be purified MA is placed.

The filter 30 according to this embodiment has curved portions. Therefore, the same effects as those of the filter 10 according to the first embodiment are obtained. Moreover, according to the shape of the filter 30, as shown in FIG. The internal space within the container 15 can be partitioned into two vertically separated spaces.

<Fourth Embodiment>
A filter-equipped container 40 according to a fourth embodiment will be described with reference to FIGS. 6 to 8. FIG.
The filter-equipped container 40 according to this embodiment is used in a purification process including a process of vaporizing a substance. The filter-equipped container 40 confines powder and droplets generated from the purification target material MA when the purification target material MA is in a bumping state in the purification process.

The filter-equipped container 40 includes a filter material 41 and a plug member 46 that closes an opening 44 of the filter material 41 . At least a portion of the filter material 41 is curved or bent to allow gas to pass therethrough. The filter material 41 has an internal space SX that accommodates the purification target substance MA.

The filter material 41 has a tubular portion 43 , an opening 44 provided at one end of the tubular portion 43 , and a closed end portion 45 that closes the end of the tubular portion 43 opposite to the opening 44 .
The filter material 41 allows gas to pass therethrough. When the substance to be purified MA is liquid, the filter material 41 is configured to prevent splashing of droplets. The material forming the filter material 41 conforms to the filter 10 of the first embodiment.

The plug member 46 includes a closing member 47 that closes the opening 44 of the filter material 41 and a fixing member 48 that fixes the closing member 47 to the filter material 41 . The closing member 47 and the fixing member 48 are made of glass or quartz.

The closing member 47 includes an inserting portion 47a to be inserted into the filter material 41 and a gripping portion 47b to be gripped by hand.
The insertion portion 47a has a circular end face portion 47c and a first peripheral wall 47d provided along the periphery of the circular end face portion 47c. 47 d of 1st surrounding walls are comprised so that the inner peripheral surface of the opening part 44 of the filter material 41 may be contacted.

The grasping portion 47b has a second peripheral wall 47e having a larger diameter than the first peripheral wall 47d of the insertion portion 47a. The second peripheral wall 47e is connected to the first peripheral wall 47d via a stepped portion 47f. The grip portion 47b is configured to protrude outside the filter material 41 when the insertion portion 47a is inserted into the filter material 41 . The grasping portion 47b is a grasping portion for facilitating separation when the closing member 47 and the fixing member 48 are separated for the purpose of removing the filter material 41 from the plug member 46. As shown in FIG.

The fixing member 48 is formed in a ring shape. Specifically, the fixing member 48 includes a third peripheral wall 48a having a larger diameter than the first peripheral wall 47d. The inner peripheral surface of the third peripheral wall 48 a is configured to contact the outer peripheral surface of the opening 44 of the filter material 41 . The fixing member 48 is fitted into the opening 44 from the outside of the filter material 41 . With the plug member 46 attached to the filter material 41 , the opening 44 of the filter material 41 is sandwiched between the first peripheral wall 47 d of the closing member 47 and the third peripheral wall 48 a of the fixing member 48 . In this manner, the plug member 46 is attached to the filter material 41 . When the opening 44 of the filter material 41 is blocked by the plug member 46 , a closed space is formed inside the filter material 41 . A purification target substance MA is contained in a container 40 with a filter.

As shown in FIG. 8, a filtered vessel 40 is placed within the purification vessel 15 . The orientation of the container 40 with filter is not limited. Preferably, the filter material 41 of the filter-fitted container 40 is arranged downstream of the plug member 46 .

The action of the filter-equipped container 40 of this embodiment will be described. In the purification process, substances vaporized by heating pass through the filter material 41 and exit the container 40 with filter. When the purification target material MA is in a state of bumping, powder and droplets generated from the purification target material MA are confined in the filter-equipped container 40 .

The effects of the filter-equipped container 40 of this embodiment will be described.
The filter-equipped container 40 includes a filter material 41 and a plug member 46 that closes an opening 44 of the filter material 41 . The filter material 41 is configured such that at least a portion thereof is curved. The filter material 41 may be configured such that at least a portion thereof is bent. According to this configuration, since the filter material 41 has a curved portion or a bent portion, the area of the surface through which the gas passes is increased, and clogging of the filter material 41 is less likely to occur. As a result, a decrease in purification efficiency can be suppressed.

<Fifth Embodiment>
A container 50 with a filter according to a fifth embodiment will be described with reference to FIGS. 9 and 10. FIG. The filter-equipped container 50 according to this embodiment is used in the purification process of the purification target substance MA, as in the fourth embodiment. In the filter-equipped container 50 according to the fifth embodiment, description of the same configuration as that of the filter-equipped container 40 according to the fourth embodiment will be omitted.

The filter-equipped container 50 includes a plurality of filter materials 51 and a connection member 56 that connects the plurality of filter materials 51 so that the internal spaces SX in the filter materials 51 are connected. The filter material 51 has a structure according to the filter material 41 according to the fourth embodiment.

The connecting member 56 of this embodiment connects the two filter materials 51 .
The connection member 56 includes a pipe member 57 that connects the internal spaces SX in the two filter materials 51 and two fixing members 58 that fix the connection member 56 to the filter material 51 . The tube member 57 and the fixing member 58 are made of glass or quartz.

The tube member 57 includes two insertion portions 57a to be inserted into the filter material 51 and a grip portion 57b to be gripped by hand. The insertion portion 57a is provided so as to protrude from both ends of the grip portion 57b. 57 h of through-holes of the pipe member 57 are provided so that it may extend from one insertion part 57a to the other insertion part 57a.

The insert portion 57a includes a fourth peripheral wall 57d having a circular open end 57c. 57 d of 4th surrounding walls are comprised so that the inner peripheral surface of the opening part 54 of the filter material 51 may be contacted.
The grasping portion 57b has an annular fifth peripheral wall 57e having a larger diameter than the fourth peripheral wall 57d of the insertion portion 57a. The fifth peripheral wall 57e is connected to one fourth peripheral wall 57d via a first stepped portion 57f and is connected to the other fourth peripheral wall 57d via a second stepped portion 57g.

The grip portion 57b is configured to protrude outside the filter material 51 when the insertion portion 57a is inserted into the filter material 51 .
The fixing member 58 is formed in a ring shape. Specifically, the fixing member 58 includes a sixth peripheral wall 58a having a larger diameter than the fourth peripheral wall 57d. The inner peripheral surface of the sixth peripheral wall 58 a is configured to contact the outer peripheral surface of the opening 54 of the filter material 51 . The fixing member 58 is fitted into the opening 54 from the outside of the filter material 51 . The opening 54 of the filter material 51 is sandwiched between the fourth peripheral wall 57 d of the pipe member 57 and the sixth peripheral wall 58 a of the fixing member 58 when the connecting member 56 is attached to the filter material 51 . Thus, the tube member 57 is attached to the filter material 51 . When the two filter materials 51 are attached to the pipe member 57, a closed space in which the internal spaces SX in the two filter materials 51 are connected is formed. A purification target substance MA is contained in a container 50 with a filter.

The operation of this embodiment will be described. According to the filter-equipped container 50 , a closed space surrounded by the filter materials 51 is formed by connecting the plurality of filter materials 51 . Therefore, the amount of the purification target substance MA that can be accommodated in the filter-equipped container 50 can be increased.

The effects of the filter-equipped container 50 of this embodiment will be described.
The filter-equipped container 50 includes a plurality of filter materials 51 and connecting members 56 . Filter material 51 is configured to be at least partially curved. The filter material 51 is configured to allow gas to pass therethrough and contains the substance to be purified MA. The connecting member 56 connects the plurality of filter materials 51 so that the internal spaces SX in the filter materials 51 are connected. The filter material 51 may be configured such that at least a portion thereof is bent.

According to this configuration, since the filter material 51 has a curved portion or a bent portion, the area of the surface through which the gas passes is increased, and clogging of the filter material 51 is less likely to occur. As a result, a decrease in purification efficiency can be suppressed.

<Sixth Embodiment>
A filter-equipped container 60 according to a sixth embodiment will be described with reference to FIGS. 11 to 13. FIG.

The filter-equipped container 60 according to this embodiment is used in the purification process of the purification target substance MA, as in the fourth embodiment. In the filter-equipped container 60 according to the sixth embodiment, description of the same configuration as that of the filter-equipped container 40 according to the fourth embodiment will be omitted.

The filter-equipped container 60 includes a filter material 61 and a plug member 66 . The plug member 66 has a structure corresponding to the plug member 46 shown in the fourth embodiment. Here, description of the plug member 66 is omitted.

Filter material 61 is configured to be at least partially curved. The filter material 61 is configured to allow gas to pass therethrough and contains the substance to be purified MA. The filter material 61 may be configured such that at least a portion thereof is bent.

The filter material 61 is formed of a flexible or bendable sheet-like filter base material 61x. The material constituting the filter base material 61x conforms to that of the first embodiment. By folding the filter base material 61x, the filter material 61 having an internal space SX that accommodates the substance to be purified MA is formed.

The filter base material 61x is formed in a bag shape with one end closed and the other end open. For example, the bag-shaped filter material 61 is formed by folding the filter base material 61x along the inner surface of the cup. The opening 64 of the filter material 61 is closed by a plug member 66 . The method of using the filter-equipped container 60 conforms to the method of using the filter-equipped container 40 according to the fourth embodiment.

The operation of this embodiment will be described. The filter material 61 of the container 60 with a filter can be formed using the sheet-like filter base material 61x. Since the sheet-like filter base material 61x is readily available, the filter-equipped container 60 can be easily prepared.

Since the filter-equipped container 60 according to the present embodiment has the same structure as the filter-equipped container 40 according to the fourth embodiment, it has the same effects as the filter-equipped container 40 according to the fourth embodiment.

<Seventh Embodiment>
A filter-equipped container 70 according to the seventh embodiment and a purification container 16 capable of accommodating the filter-equipped container 70 will be described with reference to FIG. 14 .

The filter-equipped container 70 according to this embodiment is used in the purification process of the purification target substance MA, as in the fourth embodiment. In the filter-equipped container 70 according to the seventh embodiment, description of the same configuration as that of the filter-equipped container 40 according to the fourth embodiment will be omitted.

The filter-equipped container 70 has the same configuration as the filter-equipped container 40 of the fourth embodiment. The shape of the filter-equipped container 70 differs from the filter-equipped container 40 of the fourth embodiment in relation to the purification container 15 in which the filter-equipped container 70 is placed. The filter-fitted container 40 of the fourth embodiment is configured to have a size that can be accommodated in the refining container 15 having one opening 15c smaller than the cylindrical diameter of the cylindrical portion 15a. On the other hand, the filter-equipped container 70 according to this embodiment is housed in a special refining container 16 as described below.

The purification vessel 16 includes a tubular portion 16a, a first opening 16b provided at one end of the tubular portion 16a and smaller than the tubular diameter of the tubular portion 16a, and the other end of the tubular portion 16a. and a second opening 16c having the same diameter as that of the cylindrical portion 16a. The second opening 16c is closed by the bottom member 16d. The purification vessel 16 may be used with the second opening 16c closed by the bottom member 16d, or may be used without the second opening 16c closed by the bottom member 16d.

Preferably, the diameter of the stopper member 76 of the filter vessel 70 is equal to the inner diameter of the barrel 16a of the purification vessel 16 . With this configuration, the posture of the filter-equipped container 70 can be stabilized when the filter-equipped container 70 is accommodated in the purification container 16 . Such a set of the filter-equipped container 70 and the purification container 16 is used when purifying a large amount of the substance to be purified MA.

<Eighth Embodiment>
A filter member 80 according to the eighth embodiment will be described with reference to FIG.
The filter member 80 according to this embodiment is used in a purification process including a process of vaporizing substances. The filter member 80 confines powder and droplets generated from the target substance MA when the target substance MA undergoes bumping in the purification process, in the purification container 15 containing the target substance MA.

The filter member 80 comprises a filter material 81 and an attachment member 86 for attaching the filter material 81 to the purification vessel 15 .
The filter material 81 is configured such that at least a portion thereof is curved or bent, and allows gas to pass therethrough. The filter material 81 constitutes an internal space SX.

The filter material 81 has a tubular portion 83 , an opening 84 provided at one end of the tubular portion 83 , and a closed end 85 that closes the end of the tubular portion 83 opposite to the opening 84 .
The filter material 81 allows gas to pass through. When the substance to be purified MA is liquid, the filter material 81 is configured to prevent splashing of droplets. The material forming the filter material 81 conforms to the filter 10 of the first embodiment.

The attachment member 86 is a member for attaching the filter material 81 to the opening 15 c of the purification container 15 .
The mounting member 86 includes a tubular adapter 87 to be attached to the opening 15 c of the purification container 15 and a fixing member 88 for fixing the filter material 81 to the adapter 87 .

The adapter 87 has an insertion hole 87a through which the filter material 81 is inserted. The diameter of the insertion hole 87 a is equal to the outer diameter of the opening 84 of the filter material 81 .
The fixing member 88 is configured in a tubular shape. The fixing member 88 has a first opening 88a at one end and a second opening 88b at the other end. The diameter of the first opening 88a is larger than the diameter of the second opening 88b. The second opening 88b is sized to be inserted into the filter material 81 . The outer diameter of the periphery of the second opening 88 b is equal to the inner diameter of the opening 84 of the filter material 81 .

Filter member 80 is attached to purification vessel 15 in the following manner. First, the filter material 81 is inserted through the insertion hole 87 a of the adapter 87 . The fixing member 88 is then inserted into the filter material 81 . The filter member 80 assembled in this way is attached to the opening 15c of the refining container 15 so that the outer peripheral surface of the adapter 87 contacts the inner peripheral surface of the opening 15c of the refining container 15 . When the filter member 80 is attached to the refining container 15, the opening 15c of the refining container 15 is covered with the filter material 81 so as to allow ventilation.

The operation of this embodiment will be described.
According to such a filter member 80, the gas passage area of the filter material 81 can be increased compared to the case where the opening 15c of the refining container 15 is filled with a filter. The passing area indicates the area of the portion of the filter material 81 that can directly contact the gas in the refining container 15 . The passing area of the filter member 80 according to the present embodiment indicates the area of the portion PB of the outer surface of the filter material 81 other than the portion PA of the mounting member 86 that contacts the adapter 87 .

Effects of the present embodiment will be described. Filter material 81 is configured to be at least partially curved. The filter material 81 allows gas to pass therethrough and forms an internal space SX. The filter material 81 may have a bent configuration. According to this configuration, since the filter material 81 has a curved portion or a bent portion, the passage area of the surface through which the gas passes is increased, and clogging of the filter material 81 is less likely to occur. In particular, compared with the case where the opening 15c of the refining container 15 is filled with a filter, the passing area is increased. As a result, a decrease in purification efficiency can be suppressed.

<Ninth Embodiment>
A filter member 90 according to the ninth embodiment will be described with reference to FIG.
A filter member 90 according to this embodiment is a modification of the filter member 80 according to the eighth embodiment. In the filter member 90 according to the ninth embodiment, description of the same configuration as that of the filter member 80 according to the eighth embodiment will be omitted. The filter member 80 of the eighth embodiment is supported in a cantilevered state (see FIG. 15). On the other hand, the filter member 90 of this embodiment is supported on both sides.

Specifically, the filter member 90 comprises a filter material 91 and two attachment members 96 for attaching the filter material 91 to the purification vessel 15 . At least a portion of the filter material 91 is curved or bent, and is configured to allow gas to pass therethrough. The filter material 91 constitutes an internal space SX.

The filter material 91 has a tubular portion 93 , a first opening 94 provided at one end of the tubular portion 93 , and a second opening 95 provided at the other end of the tubular portion 93 . The filter material 91 allows gas to pass through. When the substance to be purified MA is liquid, the filter material 91 is configured to prevent splashing of droplets. The material forming the filter material 91 conforms to the filter 10 of the first embodiment. The two mounting members 96, 96 have a structure according to the mounting member 86 shown in the eighth embodiment.

Such a filter member 90 can be suitably used for a purification container 17 having two openings 17c. Moreover, according to such a filter member 90, an effect equivalent to that of the filter member 80 according to the eighth embodiment can be obtained.

<Tenth Embodiment>
A filter member 100 according to the tenth embodiment will be described with reference to FIG.
A filter member 100 according to this embodiment is a modification of the filter member 90 according to the ninth embodiment. In the filter member 100 according to the tenth embodiment, the same components as those of the filter member 90 according to the ninth embodiment are denoted by the same reference numerals, and description thereof is omitted. The filter material 91 constituting the filter member 90 of the ninth embodiment has no connecting portion in the circumferential direction around the central axis. On the other hand, the filter material 101 of the filter member 100 of this embodiment has connecting portions 101a in the circumferential direction around the central axis. The filter member 100 of this embodiment is formed by rolling a rectangular filter base material.

According to this embodiment, the filter member 100 can be formed using a sheet-like filter base material. Since a sheet-like filter base material is readily available, the filter member 100 can be easily formed. Further, the filter member 100 according to this embodiment has the same effect as the filter member 90 according to the ninth embodiment.

<Eleventh Embodiment>
A refiner 110 according to the eleventh embodiment will be described with reference to FIGS. 18 to 20. FIG.
The purification device 110 includes at least one purification container 111 , an outer tube 120 that accommodates the purification container 111 , and a decompression device 140 that reduces the pressure inside the outer tube 120 . Preferably, purification vessel 111 is housed in inner tube 130 . Furthermore, an inner tube 130 in which the purification vessel 111 is accommodated is accommodated in the outer tube 120 .

At least one of the refining containers 111 includes the above-described filters 10, 20, 30, filters-equipped containers 40, 50, 60, 70, and filter members 80, 90, 100 (hereinafter referred to as "filters, etc."). One is deployable. Purification vessel 111 has at least one opening 112 . The opening 112 of the refining vessel 111 in which the filter or the like is arranged is configured so that the filters 10, 20, 30 or the vessels 40, 50, 60, 70 with filters can be inserted. Alternatively, the opening 112 of the refining container 111 in which filters and the like are arranged is configured so that the filter members 80, 90, 100 can be attached.

In this embodiment, the refining device 110 includes five refining vessels (hereinafter referred to as "first refining vessel 111A" to "fifth refining vessel 111E").
First purification vessel 111A has one opening 114 . The second refining vessel 111B to the fifth refining vessel 111E have two openings 115,116. The second refining vessel 111B to the fifth refining vessel 111E are connected downstream of the first refining vessel 111A. Downstream indicates the side closer to the depressurizing device 140 in the gas passage in the refining device 110 . The first refining vessel 111A to the fifth refining vessel 111E are connected in series to form one internal passage. The first purification container 111A accommodates a purification target substance MA.

The first purification container 111A to the fifth purification container 111E are accommodated in the inner pipe 130. As shown in FIG. The inner tube 130 is provided with a wall 131 extending perpendicularly to the longitudinal direction DA of the inner tube 130 . The wall 131 is provided on the upstream side of the intermediate position in the longitudinal direction DA in the inner pipe 130 . First purification vessel 111A to fifth purification vessel 111E are arranged downstream of wall 131 in inner tube 130 . The first purification vessel 111A to fifth purification vessel 111E are arranged in the order of first purification vessel 111A to fifth purification vessel 111E from the upstream side.

Outer tube 120 accommodates inner tube 130 . The outer tube 120 has a first open end 121 arranged on the decompression device 140 side and a second open end 122 opposite to the first open end 121 on the decompression device 140 side.

The first open end 121 is connected to a decompression device 140 via a joint 123 . The second open end 122 is closed with a lid member 124 . The decompression device 140 has a vacuum pump 141 . Preferably, the pressure reducer 140 has a trap 142 upstream of the vacuum pump 141 for liquefying the gas. The contaminant MC is trapped in the trap 142 . For example, the passageways that make up trap 142 are cooled with liquid nitrogen.

Preferably, purifier 110 further comprises cap 160 . The cap 160 faces the first open end 121 on the downstream side of the outer tube 120 . Specifically, the cap 160 is arranged to cover the first open end 132 on the downstream side of the inner tube 130 . A gap SL is provided between the peripheral portion of the cap 160 and the peripheral portion of the first opening end 132 for gas flow. Preferably, the cap 160 is provided with a handle 161 . A cap 160 is placed over the first open end 121 of the outer tube 120 when the inner tube 130 is not in use.

Outer tube 120 is heated by heating device 150 . The heating device 150 heats the first refining vessel 111A to the fifth refining vessel 111E to different temperatures. The heating unit 151 of the heating device 150 is arranged in the outer tube 120 where the first refining vessel 111A to the fifth refining vessel 111E are arranged. The upstream refining vessel 111 is heated to a higher temperature than the downstream refining vessel 111 . That is, the set of purification vessels 111 are thermally graded. For example, heating by the heating device 150 maintains the first purification container 111A at a first temperature higher than the sublimation temperature of the purification target material MA. The fifth refining container 111E is maintained at a second temperature at which the refining substance MB refined from the refining target substance MA can be deposited.

The operation of this embodiment will be described.
The substance to be purified vaporized in the first purification container 111A is deposited in the fifth purification container 111E. Impurities MC having a higher boiling point or sublimation point than the first temperature, which is the controlled temperature of the first refining vessel 111A, remain in the first refining vessel 111A. Impurity substances MC having a freezing point lower than the second temperature, which is the controlled temperature of the fifth refining vessel 111E, are flowed downstream from the fifth refining vessel 111E and captured by the cap 160 or the trap 142 .

Effects of the present embodiment will be described.
(1) The purification device 110 includes at least one purification container 111 , an outer tube 120 that accommodates the purification container 111 , and a decompression device 140 that reduces the pressure inside the outer tube 120 . At least one of the purification vessels 111 is configured such that one of the filters 10, 20, 30, the vessels with filters 40, 50, 60, 70 and the filter members 80, 90, 100 described above can be arranged.

According to this configuration, the refining device 110 has one of the filters 10, 20, 30, the containers 40, 50, 60, 70 with filters, and the filter members 80, 90, 100 that are unlikely to clog, A decrease in gas flow is suppressed. In this way, a decrease in purification efficiency is suppressed.

(2) The purification device 110 further includes a cap 160 arranged to face the first open end 121 on the decompression device 140 side in the outer tube 120 . According to this configuration, since the cap 160 impedes the flow of the gas, some of the impurities MC contained in the gas condense near the first open end 121 on the downstream side of the outer tube 120 and enter the cap 160. Impurity MC adheres. As a result, the amount of impurities MC in the gas flowing downstream of the outer tube 120 can be reduced compared to when the cap 160 is not provided. As a result, contamination of the section between the first open end 121 of the outer tube 120 and the decompression device 140 can be suppressed.

<Twelfth Embodiment>
A method for producing the purified substance MB will be described.
In the first step, one of the above-described filters or the like is arranged in the purification container 111 at a place through which the gas passes during the gas diffusion of the substance to be purified MA. For example, when using the filters 10, 20 and 30, the substance to be purified MA is contained in the first purification container 111A, and the filters 10, 20 and 30 are arranged in the first purification container 111A (see FIG. 20). The filters 10, 20, and 30 partition the internal space SX in the first purification container 111A into a storage space for containing the substance to be purified MA and a space downstream of the storage space.

When the filter-equipped containers 40, 50, 60, 70 are used, the purification target substance MA is placed in the filter-equipped container 40, 50, 60, 70, and the filter-equipped container 40, 50, 60 containing the purification target substance MA is , 70 are housed in the first refining vessel 111A.

When the filter members 80, 90 and 100 are used, the substance to be purified MA is contained in the first purification container 111A, and the filter members 80, 90 and 100 are attached to the opening of the first purification container 111A.

In the second step, the pressure inside the refining container 111 is reduced. Preferably, after reducing the pressure to a predetermined pressure, the purification vessel 111 is heated to sublime the purification target substance MA. For example, the first refining container 111A is maintained at a first temperature higher than the sublimation temperature of the material to be refined MA. The fifth refining vessel 111E is maintained at a second temperature at which the material to be refined MA can be deposited. Preferably, second refining vessel 111B, third refining vessel 111C, and fourth refining vessel 111D are maintained at a temperature lower than the first temperature and higher than the second temperature. The temperature of the second refining vessel 111B is maintained higher than the temperature of the third refining vessel 111C, and the temperature of the third refining vessel 111C is maintained higher than the temperature of the fourth refining vessel 111D. .

The operation of the method for producing the purified substance MB will be explained.
The inside of the refining container 111 is decompressed. Therefore, heating of the refining vessel 111 facilitates bumping of the refining target material MA. When the purification target material MA bumps, the purification target material MA diffuses in a state before vaporization, but the diffusion is suppressed by a filter or the like. According to this embodiment, when the liquid or solid substance to be purified MA bumps, the diffusion of the substance to be purified MA is contained within the first purification container 111A.

When the temperature of the purification target substance MA reaches the first temperature, the purification target substance MA vaporizes. The vaporized material to be purified MA passes through a filter or the like and moves to a place with a lower temperature. On the other hand, the impurity MC having a higher sublimation point or boiling point than the first temperature is not vaporized and remains in the refining container 111 as a residue. The vaporized purification target substance MA precipitates when the second temperature is maintained at which the purification target substance MA can precipitate. In the case where the purification target material MA contains impurity substances MC having a freezing point lower than the second temperature, the impurity substances MC do not precipitate where the second temperature is maintained. The precipitated material is recovered. As described above, the purified substance MB is obtained from the purified substance MA.

Effects of the present embodiment will be described.
A method for producing a purified substance MB includes a first step and a second step. In the first step, one of the filters or the like is placed in the purification container 111 where the gas passes through in the gas diffusion of the substance to be purified MA. In the second step, the pressure inside the refining container 111 is reduced. According to this configuration, one filter or the like that is less likely to clog is arranged in the middle of the gas circulation path, thereby suppressing a decrease in gas circulation. This makes it possible to suppress a decrease in purification efficiency.

Such a manufacturing method is used, for example, in purification by the purification device 110 shown in the eleventh embodiment. The effect when the method for manufacturing the purified substance MB is executed using the refining device 110 will be described. According to the refining device 110, the refining substance MB is deposited in the fifth refining container 111E. The gas containing contaminants MC flows downstream. When the gas containing the impurities MC flows downstream from the outer tube 120, it flows along the inner surface of the cap 160 to form a gap between the peripheral portion of the cap 160 and the peripheral portion of the first open end 132 of the inner tube 130. pass SL. Since the cap 160 is a separate member from the outer tube 120 , heat is less likely to be transferred from the outer tube 120 . Therefore, there is a temperature difference between the temperature of the cap 160 and the temperature of the outer tube 120 . The temperature of cap 160 is close to room temperature. For this reason, the impurity MC is deposited in the cap 160 . Impurities MC are thus removed from the gas. Substances that do not precipitate at cap 160 are captured at trap 142 .

<Other embodiments>
The above embodiments are not limited to the above configuration examples. The above embodiment can be modified as follows. In addition, in the following modifications, configurations that are substantially the same as those of the above-described embodiment will be described using the same reference numerals as those of the above-described embodiment.

- The shape of the filters 10, 20, 30 is not limited to the example shown in the embodiment. For example, filter 10 may be curved in a wavy shape.
- The structure of the container 40, 50, 60, 70 with a filter is not limited to the example shown by embodiment. For example, the plug members 46 , 66 , 76 of the containers 40 , 50 , 60 , 70 with filters may be formed from the filter base material forming the filter 10 .

- The structure of the filter members 80, 90, 100 is not limited to the example shown in the embodiment. The filter material 81, 91, 101 of the filter members 80, 90, 100 may consist of a plurality of flat surfaces.

DA...Longitudinal direction, LA...Length, MA...Substance to be purified, MB...Substance to be purified, MC...Impurity substance, PB...Part, SA...First space, SB...Second space, SC...Third space, SD... 4th space, SL... Gap, SX... Inner space, 10... Filter, 10x... Plane filter, 11... Side, 12... Side, 15... Purification container, 15a... Cylindrical part, 15b... Bottom surface, 15c... Opening, 15d Peripheral part 16 Purification container 16a Cylindrical part 16b First opening 16c Second opening 16d Bottom member 17 Purification container 17c Opening 20 Filter 21 Mountain Folding part 22... Valley fold part 30... Filter 40... Container with filter 41... Filter material 43... Cylindrical part 44... Opening part 45... Closed end part 46... Plug member 47... Closing member, 47a... Insertion part 47b... Grasping part 47c... End face part 47d... First peripheral wall 47e... Second peripheral wall 47f... Stepped part 48... Fixed member 48a... Third peripheral wall 50... Container with filter 51 Filter material 54 Opening 56 Connecting member 57 Tube member 57a Insertion portion 57b Grasping portion 57c Opening end 57d Fourth peripheral wall 57e Fifth peripheral wall 57f First Stepped portion 57g Second stepped portion 57h Through hole 58 Fixing member 58a Sixth peripheral wall 60 Container with filter 61 Filter material 61x Filter base material 64 Opening 66 Plug member 70 Container with filter 76 Plug member 80 Filter member 81 Filter material 83 Cylindrical portion 84 Opening 85 Closed end 86 Mounting member 87 Adapter 87a ... Insertion hole 88... Fixed member 88a... First opening 88b... Second opening 90... Filter member 91... Filter material 93... Cylindrical part 94... First opening 95... Second opening Part 96... Mounting member 100... Filter member 101... Filter material 101a... Connection part 110... Purification device 111... Purification container 111A... First purification container 111B... Second purification container 111C... Third Refining container 111D Fourth refining container 111E Fifth refining container 112 Opening 114 Opening 115 Opening 116 Opening 120 Outer tube 121 First opening end 122 Second open end 123 Joint 124 Lid member 130 Inner pipe 131 Wall 132 First open end 140 Decompression device 141 Vacuum pump 142 Trap 150 Heating device 151...heating part, 160...cap, 161...handle.

Claims (7)

A refiner for purifying by sublimating a liquid or solid substance to be purified,
a plurality of refining vessels connected in series to form a gas passage through which gas flows ;
an outer tube that houses the purification vessel;
a decompression device for decompressing the inside of the outer tube ;
a heating device that heats the outer tube,
The heating device heats a first refining vessel arranged upstream among the plurality of refining vessels to a temperature higher than that of the refining vessels downstream of the first refining vessel,
The first purification container is configured to accommodate a container with a filter, or a filter member is configured to be attachable to the opening of the first purification container ,
The filter-equipped container is a container having a closed space, and has, as at least one of the members constituting the closed space, a filter that allows the gas of the substance to be purified to pass through,
The filter member allows the gas of the substance to be purified to pass through, and is configured to separate at least a partial area in the first purification container from an area outside the area.
Purification equipment. The outer tube has a first open end arranged downstream and a second open end opposite to the first open end,
Further comprising a cap arranged to face the first open end on the downstream side of the outer tube
A purification apparatus according to claim 1 . A method for producing a purified substance by sublimating a liquid or solid substance to be purified,
A plurality of refining vessels connected in series so as to form a gas passage through which gas flows, an outer tube accommodating the refining vessels, a decompression device for reducing the pressure in the outer tube, and a heating device for heating the outer tube. and a filter for passing the gas of the target substance to be purified, a container with a filter, or placing a filter member;
and decompressing the interior of the purification vessel ,
The filter-equipped container is a container having a closed space, and has, as at least one of the members constituting the closed space, a filter that allows the gas of the substance to be purified to pass through,
The filter member allows the gas of the substance to be purified to pass through, and is configured to separate at least a partial area in the first purification container from an area outside the area.
A method for producing a purified material. a filter material having an opening at one end, at least a portion of which is curved or bent, and which allows gas to pass through;
a plug member that closes the opening of the filter material ,
The filter material has a tubular portion, the opening provided at one end of the tubular portion, and a closed end portion that closes the end of the tubular portion opposite to the opening,
The filter material and the plug member constitute a closed space in which the substance to be purified is accommodated.
Container with filter. two filter materials having an opening at one end, at least a portion of which is curved or bent, and which allows gas to pass through;
a connecting member disposed between the openings of the two filter materials and connecting the two filter materials so that the internal spaces in the two filter materials are connected ;
The filter material includes a tubular portion forming the internal space, the opening provided at one end of the tubular portion, and a closed end closing the end of the tubular portion opposite to the opening. has
A closed space in which the substance to be purified is accommodated is configured by the two filter materials and the connecting member,
Container with filter. a filter material having an opening at one end, at least a portion of which is curved or bent, and which allows gas to pass through, the filter material forming an internal space;
an attachment member for attaching the filter material to an opening of a purification container containing a substance to be purified ,
The filter material includes a tubular portion forming the internal space, the opening provided at one end of the tubular portion, and a closed end closing the end of the tubular portion opposite to the opening. has
The mounting member includes a tubular adapter having an insertion hole through which the opening of the filter material is inserted and which is mounted on the opening of the refining container, and an adapter mounted inside the opening of the filter material. a cylindrical fixing member that fixes the filter material to the adapter by
filter member. a filter material having openings at both ends, at least a portion of which is curved or bent, and which allows gas to pass through, the filter material forming an internal space;
an attachment member for attaching the filter material to an opening of a purification container containing a substance to be purified ,
The filter material has a tubular portion forming the internal space and two openings provided at both ends of the tubular portion, and the purification vessel having the two openings. configured to be arranged across the two openings of the purification vessel in
The mounting member includes a tubular adapter having an insertion hole through which the opening of the filter material is inserted and which is mounted on the opening of the refining container, and an adapter mounted inside the opening of the filter material. a cylindrical fixing member that fixes the filter material to the adapter by
filter member.

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