JP3838963B2 - Fine powder collector - Google Patents

Description

[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a fine powder collecting apparatus, and more specifically, a fine powder capable of efficiently collecting fine powder formed by ejecting a carbon dioxide supercritical solution obtained by dissolving a substance in carbon dioxide in a supercritical state. It relates to a collection device.
[0002]
[Prior art]
2. Description of the Related Art Conventionally, in order to increase the absorption efficiency of medicines into the human body, particularly in the pharmaceutical industry, attention has been paid to medicine powdering technology. Production methods such as RESS method (abbreviation of Rapid Expansion of Supercritical Solutions) and GAS method (abbreviation of anti-solvent method Gas Anti-Solvent) using supercritical state have been proposed as methods for producing fine powder. It is said that fine powders on the order of several microns can be manufactured.
[0003]
As a collection device in a conventional fine powder production device using a supercritical state, there are a device for collecting fine powder attached to a filter using a filter, a device for collecting fine powder by performing natural sedimentation in a container, and the like. can give.
[0004]
In the collection device using a filter, the fine powder is clogged in the filter, and it is necessary to wash the filter every time the fine powder is collected, and it is difficult to collect the fine powder clogged in the filter. There have been various problems such as the fact that the yield of the fine powder collected is reduced.
[0005]
In the collection device using the natural sedimentation method, it takes time for natural sedimentation, there is a possibility that fine powder may be released into the atmosphere together with gas, and the size of the device may be increased. There were various problems.
[0006]
[Problems to be solved by the invention]
An object of the present invention is to provide a fine powder collecting apparatus capable of efficiently collecting fine powder, which has solved the above problems.
[0007]
[Means for Solving the Problems]
Means of the present invention for solving the above-mentioned problems are: (1) a collection container in which an internal space is formed by using at least a part of a membrane that is permeable to carbon dioxide gas and capable of expansion and contraction; an injection nozzle for the carbon dioxide supercritical solution formed by dissolving the substance in the state of carbon dioxide ejected capable disposed in said collecting vessel, Ri formed the collecting vessel and a vacuum device to vacuum ,
The membrane is a fine powder collecting device, wherein the membrane is made of silicone rubber that shrinks when removed from the attachment portion in the collection container and shrinks so as to wrap the fine powder adhering to the inner surface ,
(2) The fine powder collecting apparatus according to (1), wherein the membrane is a bag-like material , and the decompression device includes a chamber that houses the collecting container and an exhaust device that exhausts the inside of the chamber. Yes,
(3) Permeation of carbon dioxide gas when the collection container is provided with an airtight support member provided with a ventable support member, and stretched over the entire surface of the support member on the inner side of the airtight container. A membrane made of silicone rubber that can be expanded and contracted and contracts so as to wrap fine powder adhering to the surface that does not contract when removed from the inner surface of the sealed container, and the pressure reducing device includes the membrane and the support member It is a fine powder collection apparatus as described in said (1) provided with the exhaust means which exhausts the inside of the said collection container through.
[0008]
DETAILED DESCRIPTION OF THE INVENTION
The fine powder collecting apparatus according to the present invention can be suitably incorporated in a fine powdering apparatus for producing fine powder such as pharmaceuticals. Then, an example of the fine powder collection apparatus which concerns on this invention is demonstrated below with an example of the said fine powdering apparatus.
[0009]
As shown in FIG. 1, the pulverization apparatus includes a supercritical carbon dioxide generation apparatus 1, a solution preparation apparatus 2, and a pulverization collection apparatus 3.
[0010]
The supercritical carbon dioxide generator 1 is a device that forms carbon dioxide in a supercritical state, and is a carbon dioxide gas cylinder 4 and a moisture remover that removes moisture in the carbon dioxide gas to form dry carbon dioxide gas. 5, a cooler 6 that liquefies carbon dioxide gas, a suction / discharge pump 7 that sucks and discharges liquefied carbon dioxide, a heat exchanger 8 that converts liquefied carbon dioxide that has been pumped into a supercritical state, An introduction line 14A for transferring carbon dioxide from the carbon dioxide gas cylinder 4 to the solution preparation device 2, and an opening / closing valve V-1 interposed in the introduction line 14A between the heat exchanger 8 and the solution preparation device 2 It has the composition provided.
[0011]
The supercritical carbon dioxide generator 1 has the above-described configuration, and the carbon dioxide gas introduced from the carbon dioxide gas cylinder 4 to the introduction line 14A is introduced into the moisture removing device 5 and dried in the moisture removing device 5. The carbon dioxide gas becomes carbon dioxide gas, and the dried carbon dioxide gas is fed into the cooler 6 through the introduction line 14 </ b> A. The carbon dioxide gas is liquefied by the cooler 6, and the liquefied carbon dioxide is cooled by the suction / discharge pump 7. The liquefied carbon dioxide fed into the heat exchanger 8 through the introduction line 14A is heated. Note that the temperature at which carbon dioxide reaches a supercritical state is 31.1 ° C. at the lowest and the pressure is 7.38 MPa at the lowest. Therefore, the carbon dioxide passing through the heat exchanger 8 is heated to at least 31.1 ° C. by the heat exchanger 8.
[0012]
The solution preparation device 2 is a device for dissolving a substance such as a pharmaceutical in supercritical carbon dioxide, and the supercritical carbon dioxide formed by the supercritical carbon dioxide generator 1 is introduced through the introduction line 14A. A dissolution tank 10, a heater 9 for heating the inside of the dissolution tank 10, a stirring means 11 for stirring the contents in the dissolution tank 10, and the substance is dissolved in carbon dioxide in a supercritical state. It has the structure provided with the derivation | leading-out line 14B which transfers a carbon dioxide supercritical solution to the fine powder collection apparatus 3, and the on-off valve V-2 interposed in the middle of this derivation | leading-out line 14B.
[0013]
The solution preparation apparatus 2 is provided with a predetermined amount of powdery substance charged in the dissolution tank 10 in advance and opens the on-off valve V-1 with the on-off valve V-2 closed. When carbon dioxide in a supercritical state is introduced into the solution, and carbon dioxide in a supercritical state introduced into the dissolution tank 10 heated by the heater 9 is introduced, the contents of the dissolution tank 10 are stirred by the stirring means 11. When a powdery substance is dissolved in carbon dioxide in a supercritical state to prepare a carbon dioxide supercritical solution, and the on-off valve V-2 is opened with the on-off valve V-1 closed, The carbon dioxide supercritical solution is sent to the fine powder collecting device 3 through the lead-out line 14B.
[0014]
In the present invention, the carbon dioxide supercritical solution is supplied to the fine powder collecting device 3, but the carbon dioxide supercritical solution is limited to being prepared by the supercritical carbon dioxide generator 1 and the solution preparation device 2. It can be prepared by other device configurations.
[0015]
Several examples of the fine powder collecting device 3 are shown below.
[0016]
As shown in FIG. 2, the fine powder collecting device 3 </ b> A includes an injection nozzle 12 attached to a distal end portion of the lead-out line 14 </ b> B, a bag 15 made of a silicone film into which the injection nozzle 12 is inserted, A chamber 13 for storing the bag 15 and a pump P for exhausting the inside of the chamber 13 are provided. The bag 15 is formed of a silicone film that is permeable to carbon dioxide gas, and can shrink and expand. Therefore, this bag 15 is a collection container in this invention. The pump P is a decompression device according to the present invention because the internal space of the bag-like object 15 can be decompressed by exhausting the chamber 13.
[0017]
The injection nozzle 12 injects the carbon dioxide supercritical solution transferred from the solution preparation device 2 through the lead-out line 14B into the bag-like object 15 in the chamber 13 whose pressure is reduced by the pump P. At the moment of injection, carbon dioxide is gasified inside the bag-like material 15, and the substance dissolved in the carbon dioxide supercritical solution becomes fine powder, and the bag-like material 15 expands to fill the chamber 13. Since the inside of the chamber 13 is forcibly evacuated by the pump P, the carbon dioxide gas present in the bag-like material 15 passes through the silicone film and is discharged out of the chamber 13. While the carbon dioxide supercritical solution is continuously ejected from the ejection nozzle 12, the pump P is continuously driven to exhaust the carbon dioxide gas in the bag 15. As a result, the formed fine powder remains in the bag 15 at the stage where the injection from the injection nozzle 12 stops. The drive of the pump P is stopped, and the inside of the chamber 13 is returned to normal pressure. Due to the shrinkage force of the silicone film, the bag 15 that has been greatly expanded contracts. The formed fine powder is stored in the shrinkable bag 15 made of a silicone film. When the bag 15 is removed from the spray nozzle 12 and the bag 15 is removed from the chamber 13, the following various steps are performed while the fine powder stored in the bag 15 is stored in the bag 15. Will be transferred.
[0018]
In this embodiment, all the fine powder is theoretically collected in the collection container which is a bag-like material, so that the fine powder is not scattered and the apparatus environment can be made clean. Theoretically, since all the formed fine powder can be collected inside the bag-like material, the collection of the fine powder becomes efficient.
[0019]
In this embodiment, the bag-like material 15 is formed of a silicone film, but as long as it is a collection container that is partially or wholly formed of a film that is permeable to carbon dioxide gas and capable of expanding and contracting, Various design changes can be made.
[0020]
FIG. 3 shows a second example of the fine powder collecting apparatus according to the present invention.
[0021]
The fine powder collecting device 3B includes an injection nozzle 12 attached to the distal end of the lead-out line 14B, a collection container 13 equipped with the injection nozzle 12, a silicone rubber film 16, and exhausts the inside of the collection container 13. And a pump P. The collection container 13 is, for example, a box-shaped airtight container 13A, and a part of the airtight container 13A is formed by a support member 17 that can be vented, and the injection nozzle 12 is mounted in the airtight container 13A. Is done. The support member 17 is a metal filter having a size that allows the silicone rubber film 16 to be stretched. The silicone rubber film 16 is stretched on the surface of the support member 17, that is, the surface facing the inner side of the sealed container 13 </ b> A, so that the silicone rubber film 16 covers the surface of the support member 17. It is stretched. The pump P is disposed so as to exhaust the inside of the collection container 13, which is a sealed container 13 </ b> A, through the silicone rubber film 16 and the support member 17.
[0022]
In this fine powder collecting device 3B, by driving the pump P, the inside of the collecting container 13, that is, the inside of the sealed container 13A is evacuated to reduce the pressure. The said injection nozzle 12 injects the carbon dioxide supercritical solution transferred from the solution preparation apparatus 2 by the derivation | leading-out line 14B in the airtight container 13A pressure-reduced. At the moment of injection, carbon dioxide is gasified inside the sealed container 13A, and the substance dissolved in the carbon dioxide supercritical solution becomes fine powder. In the airtight container 13 </ b> A, it reaches the silicone rubber film 16 along with the air flow generated by being exhausted by the pump P. The carbon dioxide gas is discharged out of the sealed container 13A through the silicone rubber film 16 and the support member 17. Until the injection of the carbon dioxide supercritical solution from the injection nozzle 12 stops, the exhaust in the sealed container 13A by the pump P is continued. As a result, the fine powder that moves with the exhaust airflow is accumulated on the surface of the silicone rubber film 16. The injection from the injection nozzle 12 and the exhaust by driving the pump P are stopped, and the inside of the sealed container 13A is returned to normal pressure by an appropriate leak means. The support member 17 and the silicone rubber film 16 are removed from the sealed container 13A. When the silicone rubber film 16 is removed from the support member 17, the silicone rubber film 16 contracts so as to wrap fine powder accumulated on the surface of the silicone rubber film 16 due to the contraction force of the silicone rubber film. The silicone rubber film 16 enclosing the fine powder serves as a packaging container for accommodating the fine powder. The fine powder wrapped by the silicone rubber film 16 can be transferred to the next appropriate process as it is.
[0023]
In this embodiment, fine powder is conveyed to the surface of the silicone rubber film along with the air flow formed by exhausting the inside of the sealed container 13A by the pump P, and the fine powder is accumulated on the surface of the silicone rubber film. Therefore, the fine powder is not scattered outside the sealed container 13A, and the apparatus environment can be cleaned. The collection of fine powder becomes efficient.
[0024]
In the fine powder collecting apparatus according to the present invention, an appropriate film can be adopted as long as it is a film that can transmit carbon dioxide gas and can expand and contract in place of the silicone rubber film. In addition, the support member 17 has an appropriate structure made of various materials so that a carbon dioxide gas permeable and expandable / shrinkable film can be stretched instead of the metal filter, and the film can be removed. Design changes can be made.
[0037]
【The invention's effect】
According to this invention, the fine powder formed from a carbon dioxide supercritical solution can be collected efficiently and rapidly.
[0038]
A fine powder collecting device comprising a decompression device that forms a collection container with a bag-like material that is permeable to carbon dioxide gas and that can expand and contract, and exhausts the inside of the chamber that houses the collection container. If there is, the collected fine powder can be transferred to the next process in a state where it is stored in the collection container, and the fine powder does not scatter outside the collection container, so that the surroundings of the device are contaminated with the fine powder. A clean working environment can be realized.
[0039]
The collection container is formed of a sealed container, and a membrane capable of expanding and contracting carbon dioxide gas is stretched on the surface of the support member forming a part of the sealed container and on the inner surface of the sealed container. The fine powder collecting device installed does not scatter fine powder outside the sealed container, and keeps the device environment clean without contaminating the periphery of the device with fine powder as described above. In addition, after the fine powder is collected, the fine powder can be taken out in a state of being covered with the film, so that the fine powder can be handled easily.
[Brief description of the drawings]
FIG. 1 is an explanatory view showing an example of a pulverizing apparatus incorporating a pulverizing apparatus according to the present invention.
FIG. 2 is an explanatory view showing a first example of a fine powder collecting apparatus according to the present invention.
FIG. 3 is an explanatory view showing a second example of the fine powder collecting apparatus according to the present invention.
[Explanation of symbols]
1 ... Supercritical carbon dioxide generator,
2 ... Solution preparation device,
3, 3A, 3B, 3C, 3D ... Fine powder collecting device,
4 ... carbon dioxide gas cylinder,
5 ... moisture remover,
6 ... Cooler,
7 ... Suction / discharge pump,
8 ... heat exchanger,
9 ... heater,
10 ... dissolution tank,
12 ... injection nozzle,
13 ... Chamber,
14A ... Introduction line,
14B: Derivation line,
15 ... bag
16 ... silicone rubber film,
17: Support member.

Claims (3)

A collection container that has an internal space formed by using at least part of a membrane that is permeable to carbon dioxide gas and that can expand and contract, and carbon dioxide supercritical that is formed by dissolving a substance in carbon dioxide in a supercritical state solution and the injection nozzle which is ejected can be arranged in the collecting vessel and Ri formed the collecting vessel and a pressure reducing device for reducing the pressure
A fine powder collecting apparatus , wherein the membrane is made of silicone rubber which shrinks when removed from an attachment portion in a collecting container and shrinks so as to wrap fine powder adhering to the inner surface . The fine powder collecting apparatus according to claim 1, wherein the membrane is a bag-like material , and the decompression device includes a chamber that houses the collecting container and an exhaust device that exhausts the inside of the chamber. The collection container is provided with an airtight support member, and the support member is stretched over the entire surface of the airtight container inside the support member so as to be contractible. A silicone rubber membrane that shrinks so as to wrap fine powder adhering to the non-shrinkable surface when it is removed from the inner surface of the sealed container, which can be shrunk. The fine powder collecting apparatus according to claim 1, further comprising exhaust means for exhausting the inside of the collection container.

Images