JPS6327044B2 - - Google Patents

Description

[Detailed description of the invention]

The present invention relates to precision filtration equipment for water, aqueous solutions, organic liquids, air, gases, etc., and particularly for sterile water and pyrogenic substances ( The present invention relates to a precision filtration device for obtaining water that does not contain (pyrogene) or water that does not contain colloidal particles. The purpose is to provide a precision device that is highly reliable, has a simple structure, and is practical. For example, conventional methods for obtaining sterile water include distillation, boiling sterilization, ultrafiltration, and ultraviolet sterilization, but energy costs and equipment costs are high, or sterilization and sterilization are insufficient. It has drawbacks such as heat, and although it can remove bacteria, it cannot remove pyrogen. Further, even the reverse osmosis membrane method, which has been used relatively recently, has drawbacks such as high equipment cost and large noise. That is, each device has its advantages and disadvantages, and the current situation is that there is a strong desire to improve the reliability of the device itself and the equipment and operating costs.
Under these circumstances, the inventors of the present invention have conducted various tests with the aim of providing a precision device with high reliability, simple structure, and low equipment and operating costs. The invention has been achieved. That is, the present invention provides a precision filtration device in which a filtration material made of porous hollow fibers with closed hollow openings is housed in a housing having at least two fluid entrances and exits. and is fixed in the housing by a separator that divides the inside of the housing into two chambers A and B, and the liquid passes through the separator and is present in the two chambers A and B. This invention relates to a precision filtering device in which the membrane area ratio of the hollow fibers is 1 on one side and 1 to 3 on the other. Hereinafter, the manufacturing method, structure, usage method, characteristics, etc. of the precision device of the present invention will be explained in more detail with reference to the drawings. FIG. 1 is a schematic diagram showing an embodiment of the present invention,
First, the hollow fibers as the overfill material are made of porous hollow fibers whose hollow openings are closed, for example, recycled fibers such as cellulose acetate, or synthetic fibers such as polyester, polyamide, polyacrylonitrile, polysulfone, polyolefin, polyvinyl alcohol, etc. However, porous hollow fibers made of polyolefin synthetic fibers such as polypropylene, polyethylene, etc. are particularly preferred because they have excellent water resistance, bacteria resistance, and chemical resistance. It can be said to be a material. The micropore diameter of the porous wall membrane of the hollow fiber is determined by the average pore diameter measured using the mercury porosimeter method.
A diameter of about 0.05 to 0.6 μ, particularly about 0.1 to 0.3 μ is preferable from the viewpoint of overflow and overaccuracy. The inner diameter of the hollow fibers is preferably about 100 to 400 μm, particularly about 150 to 300 μm from the viewpoint of pressure loss. However, in the present invention, the above-mentioned values are not particularly limited, and can be appropriately selected and used depending on the purpose of use. Next, the hollow openings of the hollow fibers can be closed by dissolving the tips of the hollow fibers with a solvent, or by gluing them with an adhesive. Alternatively, in the case of heat-melting hollow fibers, a method of closing the fibers by fusion may be used as appropriate. In FIG. 1, the hollow fibers are bundled at approximately the center portion 2, but the hollow fibers can be bound by adhesion and solidification using, for example, polyurethane resin, silicone resin, or the like. The housing 3 is made of a rigid body made of pressure-resistant plastic or metal, and has at least two fluid inlets and outlets 4, 5, etc., and the housing is divided into two chambers A and B.
Any structure may be used as long as it has a separator plate 6 for fractionating into two parts, and this separator plate can also be made of plastic, metal, or the like. This separator divides the housing into two chambers, and allows a bundle of hollow fibers 1, which serves as a surcharge material, to pass through the separator to be present in chambers A and B in the housing in a liquid-tight or air-tight manner. It plays the role of fixing it in place. Furthermore, the membrane area ratio of the hollow fibers is set to 1 in the housing of the A and B2 chambers.
The precision device of the present invention is manufactured by storing the number of parts so that one number is 1 to 3 while the other number is 1 to 3. Since the precision filtration device of the present invention has the structure as described above, for example, the fluid flowing in from the fluid inlet 4 of the housing 3 once fills the A chamber in the housing, and then flows through the porous hollow fibers in the A chamber. Once passed through the porous wall membrane part, it reaches the hollow fiber hollow part of the hollow fiber in chamber B through the hollow fiber hollow part, flows from the inside of the hollow fiber hollow part again toward the porous outer wall membrane, and is passed again in this process. Thus, the desired superfluid can be obtained from the outlet 5 in the B chamber. In other words, since a two-stage pass is performed, the reliability as a precision pass is high. For example, even if there is an unexpected defect in the porous wall membrane of the hollow fiber in chamber A and the target object is insufficiently captured, the porous wall of the hollow fiber in chamber B It can be captured in the wall membrane, making it a highly reliable precision device. Note that when the porous wall membrane of the porous hollow fiber in chamber A becomes clogged due to changes over time during the aging process, and the flow rate decreases, the operation must be temporarily stopped and the By using the section as a fluid inlet and the fourth section as an outlet, it is possible to remove particulate matter adhering to the porous wall membrane of the hollow fiber in chamber A.
That is, it has the feature that it is easy to operate when attempting to restore membrane function by backwashing that applies reverse pressure. Further, the precision filtration device of the present invention has the following advantages because the hollow openings of the porous hollow fibers serving as the filtration material are closed. For example, when this device is used to produce sterile water, recontamination of the overfill material itself due to back infiltration of bacteria from the water sampling port is prevented, especially when the device is not in operation. In other words, if the hollow openings are not closed, there is a risk that bacteria that have infiltrated back into the hollow fibers may enter the interior of the hollow fibers through the hollow openings, which is not preferable. Next, the precision precision device of the present invention is
It is necessary to set the membrane area ratio of the hollow fibers existing in the chamber to 1 on one side and 1 to 3 on the other, and usually the membrane area of the hollow fibers present in the A chamber on the fluid inlet side during operation. It is preferable to set the membrane area so that it is equal to or larger than the membrane area of the hollow fiber existing in chamber B on the fluid outlet side from the viewpoint of efficiently operating the apparatus. That is, according to studies by the present inventors, as the membrane area of the hollow fibers in chamber A on the inlet side becomes larger than the membrane area in chamber B on the outlet side, the flow rate under the same pressure tends to decrease. Therefore, from the viewpoint of securing the flow rate, it is not preferable that B be 1 and A be 3 or more. However, if B is 1 and A is 1 or less, the membrane area of the hollow fibers on the primary flow side becomes too small, which shortens the time until so-called clogging and reduces the flow rate, which is not preferable. Based on these study results, it is necessary to increase the membrane area of chamber A by 1 to 3 times that of chamber B in this device. Further, it is preferable that the chamber has an A chamber and an inlet for the overflow fluid, and a B chamber and an outlet for the overflow fluid. In reality, the above-mentioned membrane area ratio is changed in consideration of the amount of particulate matter contained in the passing fluid, viscosity, etc., but usually the membrane area ratio is 1:1 or 1:1. 2 or so is often used. In addition, in Figure 1, there are 2 fluid inlets and outlets.
Although only one is shown, the A chamber may be further provided with an outlet for the permeated fluid. Furthermore, although the above explanation has mainly focused on the filtration of water, it is also possible to precisely filtrate gases, air, and organic liquids using the apparatus of the present invention. Next, the present invention will be explained in more detail with reference to Examples. The detection and measurement methods for bacteria and pyrogen used in the Examples are as follows. Bacteria measurement method in water Place an ordinary agar medium in a sterile Petri dish, steam sterilize it at 120℃ in an autoclave, add 1 ml of sample water onto the agar medium, and culture it in an incubator at 37℃ for 24 hours. The number of bacterial colonies (co-long) was measured. Pyrogen detection method Pyrogen detection method is Limulns lysatetest
The detection reagent used in accordance with the (Least Crab Hemocyte Lysis and Gelation Test) was Pregel Reagent (trade name) manufactured by Teikoku Zoki Seiyaku KK. The detection principle is based on the fact that blood cells in the hemolymph of horseshoe crabs react with extremely small amounts of pyrodiene and form a gel. Pregel is a reagent in which the above-mentioned freeze-dried blood cell components are sealed in an ampoule.A test solution is added to this ampoule, and after culturing in an incubator at 37°C for 1 hour, it is kept at room temperature for 5 minutes. The criteria for determining the degree of gelation by tilting the ampoule at 45° are as follows. (++): Forms a hard gel and does not lose its shape even if the ampoule is tilted. (+): A gel is formed, but when the ampoule is tilted, it moves as a lump. (±): Formation of coarse granular gel and significant increase in viscosity (-): Remains liquid and no change The detection limit of pyrodiene by this method is
10 ^-3 μg/ml. Example 1 Hollow opening of a porous hollow fiber made of polyethylene with an average micropore diameter of 0.23μ and a porosity of 60Vol% as measured using a mercury porosimeter model 221 manufactured by Carlo Erba, with a film thickness of 60μ and a hollow fiber inner diameter of 280μ. was closed by heat fusion. Next, the hollow fibers are bundled, the center of the hollow fiber bundle is glued using polyurethane resin, and the inside of the housing is attached to a separator that divides the inside of the housing into two chambers, A and B, to create a precision filter device. did. In addition, the membrane area of the hollow fiber existing in chamber A on the liquid inlet side is
1.2 m ² , and the membrane area of the hollow fibers in chamber B on the outlet side was 1 m ² . This precision filtering device was connected to the well water conduit via a pressure regulator, and the back pressure was 2.5Kg/ ^cm2 .
Table 1 shows the results and interim progress of water flowing for 2 hours a day for 12 months.

[Table] As shown in Table 1, it was found that sterile, pyrogen-free water was always obtained even though no disinfection was performed for 12 months. Example 2 In order to confirm the reliability of the precision device of the present invention, the following model experiment was attempted. First, after producing a device exactly the same as in Example 1,
A pinhole was intentionally created by poking a side surface of one of the hollow fiber bundles in chamber A on the fluid inlet side with a needle. That is, a defect was intentionally created in the hollow fiber in room A, and using this device, water was passed for 2 hours a day under the same conditions as in Example 1 for 12 months. The results and progress are shown in Table 2. Also shown.

[Table] As shown in Table 2, sterile, pyrogen-free water can be obtained even after 10 months, and even if there is a defect in the hollow fibers in chamber A on the fluid inlet side, the hollow fibers in chamber B can provide two-stage water. It was found that this device has excellent overefficiency and is a highly reliable precision overpass device. (Comparative Example) Using the same porous hollow fiber as in Example 1, a precision filtering device as shown in FIG. 2 was manufactured.
In FIG. 2, reference numeral 1 indicates a hollow fiber, and reference numeral 2 indicates a portion obtained by solidifying a hollow fiber bundle with resin and cutting it to open the hollow fiber, which is fluid-tightly connected to an outlet 5 of a housing 3. In this device, fluid to be permeated enters the housing through an inlet 4, passes through a hollow fiber, and the filtered fluid passes through the hollow portion of the hollow fiber and is taken out through an outlet 5. The effective area of the hollow fiber was set to 2.2 m ² , and using this device, water was passed for 2 hours a day for 12 months under the same conditions as in Example 1. The results and intermediate progress are also shown in Table 3.

[Table] As shown in Table 3, this device also shows sufficient sterilization and pyrogen removal effects, but after 10 months, the pyrogen test in the Limulus test showed a result of (±). Precision instruments were found to be more reliable. As explained above, the precision measuring device according to the present invention is highly reliable, has a simple structure, and is low in equipment cost and operating cost, and is considered to have extremely high practical value.

[Brief explanation of the drawing]

FIG. 1 is a schematic diagram showing a precision scanning device of the present invention, and FIG. 2 is a schematic diagram of a precision scanning device other than the present invention. 1...Hollow fiber, 2...Hollow fiber bundle fixing part, 3...
Housing, 4, 5...Fluid inlet/outlet, 6... Separation plate.

Claims (1)

[Claims] 1. In a precision filtration device in which a filtration material made of porous hollow fibers with closed hollow openings is housed in a housing having at least two fluid inlets and outlets, the hollow fibers are are bundled and fixed in the housing by a separator that divides the inside of the housing into two chambers A and B, and the liquid passes through the separator and is made to exist in the two chambers A and B. The membrane area ratio of the hollow fiber is 1 for one side and 1 to 3 for the other side.
Precision equipment. 2 The membrane area of chamber A with the inlet of the permeated fluid is
2. The precision filtration device according to claim 1, wherein the membrane area is larger than that of chamber B having an outlet for excess fluid.