JPS6068006A - filtration device - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

Detailed Description of the Invention The present invention uses hollow fibers to perform external pressure total filtration, external pressure circulation filtration (supplying the liquid to be treated to the outside of the hollow fibers and removing the treated liquid from the inside of the hollow fibers), or A device that removes undesirable components from the liquid to be treated using internal pressure total filtration (supplying the liquid to be treated inside the hollow fiber and taking out the treated liquid from the outside of the hollow fiber). Wow, I'm blind.
This invention relates to a device devised so that only the hollow fiber bundle can be easily replaced in the event of damage. The present invention will be described below as a water purification device for removing undesirable components such as bacteria from raw water. You can also use

Traditionally, distillation methods and membrane permeability methods have been used to produce sterile water and pyrogen-free water, but distillation methods produce droplets,
There is a drawback that the degree of purification is reduced due to contamination due to entrainment of foam and contamination due to dissolution of equipment materials due to heating.

On the other hand, in the case of membrane filtration, if a membrane that blocks bacteria and pyrogienes is used, both bacteria and pyrogienes should theoretically be removed to a high degree, but in this case as well, the p liquid (processing liquid) May be contaminated with pyrogens. In particular, contamination often occurs when filtration is performed for a long period of time, and the causes of this are (1) defects in the membrane itself; (2)
Leakage of raw water into the filtrate may occur due to imperfections in the membrane adhesion, (3) mechanical seals within the device, such as imperfect seals on the O-ring, but these leaks are generally extremely minute. Therefore, it is extremely difficult to check the causes and routes of contamination. However, in the production of purified water, if even one bacteria leaks into the solution, it will immediately multiply and the purpose of sterilization will no longer be achieved, so leakage of raw water into the p-liquid must be strictly avoided. Recent rapid progress in research on separation membranes has almost completely prevented leakage of raw water due to defects in hollow fibers or imperfections in the focusing and fixing parts of hollow fibers; However, the problem of leakage of raw water (liquid to be treated) still remains. In particular, the equipment for Infin, in which the raw water inlet and raw solution outlet are in a straight line, is easy to install, compact, and easy to use.
Although this device has excellent features such as the ease of attaching and detaching the hollow fiber bundle, this device does not allow raw water to leak due to defects in the sealing member.
Even if it leaks to the liquid side, it cannot be detected from the outside at all, and furthermore, even if a bacterial test of the P liquid reveals that raw water is leaking to the offshore liquid side, the cause is a non-seal caused by the sealing member. At present, it is difficult to distinguish between sealability and non-sealability caused by defects in the hollow fibers.

The present inventors have provided a filtration device that can reliably prevent leakage liquid caused by a defect in a sealing member from leaking to the offshore liquid side, and can detect non-sealing properties caused by the sealing member. The present invention was arrived at as a result of intensive study. That is, the present invention accommodates a bundle of hollow fibers in which the upper ends of a large number of hollow fibers whose lower ends are substantially sealed and whose upper ends are open are collected and fixed with an adhesive in a casing having an opening at the upper end; The convergence fixing part of the bundle or the cap body connected and fixed to the convergence fixing part is connected to the bottom wall through at least two gaskets arranged at a distance from each other, to the inlet of the liquid to be treated (raw water) and the inlet of the liquid to be treated (raw water). Liquid addition) The casing is liquid-tightly inserted into one opening of a lid body having two openings that communicate with the outlet, and the housing is liquid-tightly attached to the lid body to form a convergence fixing part for a hollow fiber bundle or The filtration device is characterized in that a cap body connected and fixed to the focusing fixing part is maintained in an inserted state, and a leakage liquid outlet opening between a plurality of gaskets is bored in a side wall of the lid body. .

The novel idea of the present invention is that both the raw water inlet and the p-liquid outlet are provided in the lid. Based on this idea, when installing the device on the actual line, it is easy to attach the 02, and when replacing the hollow fiber bundle, the housing and the hollow fiber bundle are attached and detached in the same direction, so it is easy to attach and detach. It has the excellent effect that the space required at the time is small and that the p-liquid side is not easily contaminated when the hollow fiber bundle is replaced.

It is particularly effective to configure the raw water inlet and raw solution outlet to be in a straight line (in-line type). The novel concept of the candy of the present invention is that the convergence fixing part of the hollow fiber bundle or the cap body connected and fixed to the convergence fixing part are connected to the lid body through at least two gaskets arranged at a distance from each other. The lid body is inserted into the opening and maintained in this inserted state, and a leakage liquid outlet is bored in the side wall of the lid body between the plurality of gaskets. With this idea, it is possible to reliably prevent raw water that has leaked out due to a defect in the packing from leaking into the p-liquid side, and also to guide the leakage of raw water due to a defect in the packing to the outside of the equipment so that it can be seen by the operator. can be known from the outside.

Next, one embodiment of the filtration device of the present invention will be described with reference to the drawings.

The apparatuses of the present invention include so-called external pressure type and internal pressure type apparatuses that supply the liquid to be treated to the outside or inside of the hollow fibers, and below, all external pressure type apparatuses will be explained. As shown in FIGS. 1 to 9, the present invention comprises a cylindrical casing 1 with an open top, a hollow fiber bundle 3 housed in the casing 1, and a lid attached to the top opening of the casing. It is composed of 2 bodies. In addition, in the apparatus of the present invention, the convergence fixing part 5 of the hollow fiber bundle or the cap body 4 connected and fixed to the convergence fixing part (usually a cone-shaped body whose tip end is smaller in diameter than the convergence fixing part of the hollow fiber bundle) is attached to the lid body 2. There are two methods for maintaining the insertion state of the bundle fixing part or the cap body into the opening provided in the opening, namely, an upper support method that supports the bundle fixing part 5 of the hollow fiber bundle 3, and A lower support in which the yarn bundle 3 is supported by a self-supporting member 6, and a fixing part 5' fixed with adhesive so as to seal the lower end of the hollow fiber bundle is supported by a support 36 provided protruding from the lower part of the casing. There is a method. For example, as shown in Fig. 10, a top-support type hollow fiber bundle is made by condensing and heating each hollow fiber bundle with adhesive so that the top end of each hollow fiber is open, and then sealing the bottom opening with adhesive from the opening at the bottom end. Hollow fiber bundle, as shown in FIG.
A hollow fiber bundle whose lower end is formed into a loop shape, in this case, arranging the loops at the lower end in a ring shape creates a cavity inside the hollow fiber bundle, which has the advantage of improving overflow efficiency. As shown in FIG. 12, a hollow fiber bundle with its lower end sealed is housed in a self-supporting net-like or porous cylindrical body 6 made of plastic or metal, or as shown in FIG. 15, the lower end is sealed. There is a hollow fiber bundle in which the stopped hollow fiber bundle is housed in a porous protective tube 7 made of ceramic or resin and applied with primary p. On the other hand, as a hollow fiber bundle of the lower support type, as shown in FIG.
The first -
．． 4J A hollow fiber bundle is fixed with adhesive and a storage ball cap with a single-shaped body, and the upper end of the hollow fiber bundle has an opening. There is also a hollow fiber bundle in which the hollow fibers are wound in a crisscross pattern, the lower end is buried and fixed in an adhesive, and the upper end is bundled and fixed 5 so that the upper end is open.

Further, the hollow fiber bundle can be connected to, for example, a conical cap body 4 and fixed to the bundle fixing section 5 as required.

The convergence fixing part 5 of the hollow fiber bundle 5 or the protruding part 9 of the cap body 4 connected and fixed to the single bundle fixing part has a plurality of annular grooves spaced apart from each other as shown in FIGS. 16 and 17. 10 is formed, and an 01J ring is installed in the annular groove. Usually, two annular grooves 10 are formed, but three or more may be formed to ensure sealing.

FIG. 1 shows an example of an apparatus using a hollow fiber bundle 3 of an upper support type in which a conical cap body 4 is adhesively fixed to a bundle fixing part 5 of the hollow fiber bundle.

A cylindrical casing 1 having an opening at the top is provided with seven flange 11 for supporting a deer bundle fixing part 5 of the hollow fiber bundle inside the cylindrical casing 1, and the flange 11 has a plurality of holes 12 through which raw water passes or Nine notches are bored. The hollow fiber bundle shown in FIG. 10, FIG. 11, FIG. 12, or FIG. 15 is accommodated in the housing so as to be supported by a convergence fixing part 575;

On the other hand, the lid body 2, which is attached to the opening of the housing 1 in a liquid-tight manner, has an opening in the center of its bottom wall that communicates with the furnace liquid outlet 15, and an opening that communicates with the raw water inlet 14 adjacent to the opening. ing. The openings communicating with the reactor liquid outlet 13 and the raw water intake 14 are opened on the same straight line with the flow paths changed by 90° within the lid body.
They may be connected to a filtrate outlet pipe (not shown) and a raw water inlet pipe (not shown), respectively. The protrusion 9 of the conical cap body 4 connected and fixed to the convergence fixing part 5 of the hollow fiber bundle is inserted into the opening communicating with the furnace liquid outlet 13, and the gap between the protrusion and the opening provided in the lid is 2. It is sealed by two O-rings 15. If the raw water inlet and reactor liquid outlet are reversed, it can be used as an internal pressure filter.

Further, a leakage liquid outlet 16 is bored on the outside of the lid 2 and opens between two O-rings 15 that seal the lid 2 and the protrusion 9 of the cap inserted into the lid. A band coupling 17 liquid-tightly connects the housing 1 and the lid 2 via a gasket 18. These gaskets 18 and O-rings 15 make the raw water chamber 19 and the p-liquid chamber 20 have a liquid-tight structure by separating the wall membrane of the hollow fibers. That is, raw water enters the raw water chamber 19 outside the hollow fiber from the raw water introduction pipe, and a part of the components that permeate through the hollow fiber pass through the hollow fiber and pass through the passage inside the hollow fiber, and are collected in the offshore liquid chamber 20 and collected in the cap body. The liquid is taken out through the liquid supply outlet pipe 4.

On the other hand, components that do not pass through the hollow fibers are removed from the lower discharge port 2 of the housing 1.
It is taken out as appropriate.

In the above device, the part where raw water leaks to the p liquid side is the lid 2.
From the gap between the opening communicating with the liquid supply outlet 13iC provided in the bottom wall of the opening and the protrusion 9 of the cap body 4 connected and fixed to the Rin bundle fixing part 5 of the hollow fiber bundle 3 inserted into the opening. However, the gap is completely sealed by two O-rings 15. However, if the 01J ring is damaged and the sealing performance is lost, the raw water on the pressurized side will flow out of the device through the atmospheric leakage liquid outlet 16 drilled in the lid, so the raw water will not leak to the P liquid side. . Furthermore, since the raw water flows out through the leakage outlet, leakage can be detected by an operator or by a suitable measuring device. As the gasket for sealing the gap between the protrusion and the opening provided in the lid, a flat gasket or the like may be used instead of an O-ring. Further, a flat packing and an O-ring may be used in combination. When three gaskets are attached to the conical cap, it is preferable to provide a leakage liquid outlet between the gaskets on the outside of the lid.

By providing such a plurality of leakage liquid outlets, it is possible to detect which gasket has lost its sealing properties. When the hollow fiber bundle used during the production of purified water deteriorates or becomes clogged, my sister first drains the raw water inside the housing through the outlet 21, then removes the band coupling 17 and separates the lid body 2 and the housing 1. The hollow fiber bundle 3 can be easily replaced by removing the hollow fiber bundle 3 from the housing, then storing a new hollow fiber bundle in the housing and attaching the housing to the lid. can.

The above device is used with the lid mounted on top of the housing as shown in Figure 1, but the P-pass device must be installed with the lid mounted on top of the housing. There is. In this case, it is preferable to provide an outlet for the raw water inside the housing in the raw water piping.

FIG. 2 shows an example of an apparatus in which a hollow fiber bundle 5 of a lower support type having a conical cap body 4 is housed. When the fixing part 5', which is embedded and fixed in the adhesive, is attached to the lid body, the protruding part 9 of the cap body 4 will reach the furnace liquid outlet 13 provided on the bottom wall of the lid body. It is inserted into the communicating opening and maintained in this inserted state.

FIG. 3 shows an example in which a hollow fiber bundle 5 having a conical cap body 4 is glued and fixed to the housing 1 and integrated, and the upper part of the housing 1 is provided with a plurality of openings 22 for inflowing raw water. and a flange 25 for attaching the housing to the lid at the bottom of the opening.
is provided. Raw water is supplied through raw water inlet 1 provided in the lid.
4 and enters the housing through the upper opening 22 of the housing 1. In this device, when the hollow fibers deteriorate or become clogged, the entire casing 1 containing the hollow fiber bundle can be replaced.

FIG. 4 shows an example of an apparatus that accommodates a hollow fiber bundle of an upper support type in which an O-ring 15 is attached to an annular groove 10 provided on the outside of the bundle fixing part 5 of the hollow fiber bundle 6, and FIG. 5 shows a lower part of the hollow fiber bundle. This is an example of a device that accommodates a support-type hollow fiber bundle. Figures 4 and 5
In the figures, the same reference numerals are given to the same parts as in the apparatus of FIGS. 1 and 2, and the explanation thereof will be omitted. Figures 6 to 8 are for housing 1.
This is an example in which the hollow fiber bundle 5'fc and the hollow fiber bundle 5'fc are integrated, and FIG. 6 shows a case in which the hollow fiber bundle 3 is converged and fixed in the intermediate ring 24 equipped with the O ring 15, and the intermediate ring is adhesively fixed to the housing. It is integrated with the ring-shaped plate 25. The ring-shaped plate is provided with an opening 26 that corresponds to an opening that communicates with the raw water inlet 14 provided on the bottom wall of the lid 2. FIG. 7 shows a device corresponding to FIG. 3, and the same reference numerals are used in the same places, and the explanation thereof will be omitted. FIG. 8 shows an example in which the intermediate ring 24 accommodating the hollow fiber bundle 3 shown in FIG. 6 and the ring-shaped plate 25 are integrally formed with an adhesive for converging and fixing the hollow fiber bundle. Hollow fiber bundle is in housing 1
The convergence fixing part 5 of the hollow fiber bundle is formed by a protrusion 27 inserted into an opening provided in the lid body 2 and a ring-shaped part 28 that closes the upper end opening of the casing. , the ring-shaped part has an opening 2 for introducing the human into the housing at a position corresponding to the opening communicating with the raw water inlet provided on the bottom wall of the lid body.
6 is provided. FIG. 9 shows an example in which the bundle fixing portion of the hollow fiber bundle 3 is fixed to the lid body 2 with a nut 29. Various one-touch connection methods can be applied to the above Natsu songs.

When the apparatus of the present invention is used to produce purified water, it is preferable that the hollow fibers used have a fractionation property on the order of so-called ultrafiltration, which does not substantially allow substances of 80 Å or more to pass through.

Hollow fibers that do not substantially allow substances of aoA or higher to permeate are those whose average particle diameter is 95% or more when the rejection rate R of colloidal silica of 80 people is measured under the following conditions.

Method for measuring rejection rate (1) Hollow fiber bundle; hollow fiber length 20α, membrane area based on outer diameter 2
A 00d hollow fiber bundle was prepared and used.

(11) Measurement solution; colloidal silica 1 with average particle size of 80 people
% solution (Snowtex-S manufactured by Nissan Chemical Industries, Ltd. (colloidal silica with the smallest particle size) diluted with distilled water)
.

(II+) Filtration conditions: External pressure total filtration method, filtration pressure 0.5 to 9 degrees, temperature 25°C 0. Before use, the hollow fiber bundle should be thoroughly drained of water, and the inside of the hollow fiber wall should also be replaced with colloidal silica liquid. Press down and begin filtration.

Dynamic sampling; measurement stock solution just before pressurization and 'I after pressurization
The first flow of 5i is sampled 5 times every 10cc. The six samples obtained were dried at 100°C for 16 hours.
Measure the solids concentration.

(v) Calculation of exclusion rate R; solid content concentration CD of measurement stock solution and 5
Calculate the highest solid content concentration Cpmax in each stock solution using the following formula.

■= (1-CpmaxloD)
Even if the average is 97%, it does not mean that 80 particles are transmitting 6%, and if R is 95% or more, it is 80 Å.
It can be considered that the above particles do not transmit at all.

In addition, if such hollow fibers have an active layer on the outer surface, inner surface, or both of the inner and outer surfaces that substantially does not allow substances with a diameter of 80 Å or more to pass through, or have a fine structure inside the membrane that does not substantially allow substances with a diameter of 100 Å or more to pass through, Either is fine. Such substances f of 80 Å or more: By using hollow fibers that are virtually impermeable, for example, microorganisms and colloidal substances in raw water can be completely removed in 88 minutes, and poliovirus, which is said to be the smallest virus, and colloidal substances can be completely removed. Because it can remove even the smallest substance, colloidal silica, highly purified purified water can be obtained.

As the material for the hollow fibers, materials commonly known as hollow fiber membrane materials such as polysulfone, polyacrylonitrile, cellulose such as cellulose acetate, polyamide, polycarbonate, and polyvinyl alcohol can be used. The polysulfone type has excellent heat resistance and chemical resistance such as acid resistance, alkali resistance, and oxidation resistance, so it can be regenerated by cleaning the membrane with oxidizing agents, acids, alkalis, etc., and it can also be heat sterilized. It is also possible to sterilize with chemicals such as formalin, chlorine, etc., which is preferable because the sterilization method can be freely selected.

As the adhesive for converging and fixing one end of the hollow fiber bundle, conventionally used adhesives such as polyurethane, silicone, and epoxy can be used. In particular, when used in applications that require heat resistance and chemical resistance, not only the hollow fiber but also the adhesive must have heat resistance and chemical resistance.

For such uses, it is preferable to use imidazole-based cured epoxy resins. This resin consists of an epoxy base resin, a polyamine curing agent having an amine equivalent of 25 to 70 moles relative to the epoxy equivalent, and a
．． A liquid epoxy compound consisting of 5 to 10 parts by weight of an imidazole curing agent and having a polyamine curing agent/imidazole curing agent weight ratio of 10 to 15 to 100/1 is filled into the gap at the end of the hollow fiber. The ends of the hollow fibers can be fixed together by first solidifying at 0 to 50°C and then curing at 60 to 150°C.

The casing and lid that house the hollow fiber bundle are made of contact-resistant metal such as stainless steel or resin, and resin is generally used in many cases. Such Iθ fats include polypropylene, polytetrafluoroethylene, polyvinylidene fluoride, polyacetal, polycarbonate, polysulfone,
Resins having heat resistance such as poly-4-methylpentene-1 are preferred. Among them, polysulfone is particularly preferred because it has high heat resistance and high flexural modulus. In an apparatus for processing at a temperature of 50° C. or lower, non-heat resistant resins such as vinyl chloride, polystyrene, polyacrylonitrile, etc. may be used.

Further, the gasket used for the seal is made of industrial rubber, such as silicone rubber.

In the device of the present invention, when raw water is subjected to external pressure or internal pressure total filtration, or external pressure circulation filtration, the overpressure f applied to the raw water is o,
1 kg/cA or more, preferably 11.5 kg/cn
It is 1 or more. The upper limit pressure is good for high fabrication overspeed, but it is of course necessary to keep it within a range that does not destroy the hollow fiber, and is usually 5 to 10 I or less, preferably 3 ky/cA.
It is as follows. If filtration is performed at high pressure initially, the cake will accumulate densely, which will actually reduce the total amount of filtrate, which is often undesirable. Therefore, it is preferable to initially filter at a low pressure and gradually increase the filtration pressure as the filter becomes clogged. When filtering tap water, by directly connecting the device to the water supply, highly purified pure water can be easily obtained by utilizing the water pressure without using any pumps, which is extremely economical.

The raw water to be supplied to the apparatus in the production of purified water is preferably one in which the cake (slag accumulated on the membrane surface of a hollow fiber of aoX or higher) in the raw water is close to incompressible. The term "incompressible cake" here refers to a cake whose shape does not change easily when it is compressed by filtration pressure, and in the case of this rigid cake, water can permeate through the cake layer relatively easily. I can do it.

Even inorganic materials such as iron colloids and silica, activated carbon, crosslinked polymer pieces such as ion exchange resin pieces, etc. can be said to be relatively incompressible cakes. -1 Polysaccharides or generally denatured proteins secreted by microorganisms form gel-like cakes when compressed, and the cake layer hardly allows water to pass through, which is not preferable. Even when both are mixed, if the incompressible cake is predominant, it can be filtered by the present invention.

If the cake concentration is too high, the cake accumulates quickly and requires frequent discharge of concentrated water, backwashing, chemical washing, etc., so it is preferably 0.1 q6 or less. Examples of such raw water include ultrapure water, pure water, tap water, river water, industrial water, and seawater. If the device of the present invention is used as a check filter in an ultrapure water production process, ultrapure water with extremely high purity can be obtained.

As described above, the filtration device of the present invention prevents the liquid to be processed from leaking into the processing liquid side by providing a through hole with low pressure between the liquid to be processed chamber and the liquid to be processed chamber. This is a well-devised device that is particularly useful as a sterilization filter for viruses and pyrogens, which requires particularly strict filtration accuracy, or as a filter for ultrapure water lines. Further, since the inlet of the liquid to be treated and the outlet of the treated liquid are provided in the lid, it can be easily attached to the line, and the space for attaching and removing the hollow fiber bundle is small. Furthermore, hollow fibers and casings.

Using heat-resistant polysulfone as the material for the lid has excellent chemical and heat resistance, making sterilization or sterilization easy.
It has the excellent effect of being able to

[Brief explanation of the drawing]

1 to 9 are cross-sectional views of an apparatus showing one embodiment of the apparatus of the present invention, FIGS. 10 to 15 are explanatory views of a hollow fiber bundle used in the apparatus of the present invention, and 16. 17 are enlarged sectional views of the sealing structure of the hollow fiber bundle. 1... Housing 2... Lid body 3...
・Hollow fiber bundle 4...Cap body 5...
Focusing fixing part 10... Annular groove 13...
Sawa liquid outlet 14... Raw water inlet 15...
0 ring 16...Leaking liquid outlet Patent applicant Rira Co., Ltd. Agent Patent attorney Ken Honda Drawing J"4"J (no changes to 19) No. 1 Drawing 2 Drawing 3 Figure 7 Figure 9 Figure 10 Figure 11 Figure 13 Figure 14 Figure 12 Closure 15 i 16th Figure 17 Figure 1 i-author (spontaneous) Showa expense October 258 1. Input ~ Tsumaji Iwako Sbee 17Gε1; No. 2, Name of the invention E?AY? Kurashiki City Sakazu 1621 Estate (108) Rira Shi Co., Ltd. Representative Director Ueno et al. −

Claims (1)

[Claims] 1. A bundle of hollow fibers whose lower ends are substantially sealed and whose upper ends are open, the upper ends of which are collected and fixed with an adhesive, is housed in a casing having an opening at the upper end; and the convergence fixing part of the hollow fiber bundle or the cap body connected and fixed to the convergence fixing part is connected to the bottom wall through at least two gaskets arranged at a distance from each other, to the inlet of the liquid to be treated and the process liquid. The casing is fluid-tightly inserted into one opening of a lid body having two openings communicating with the outlet, and the housing is fluid-tightly attached to the lid body to form a convergence fixing part for the hollow fiber bundle or the convergence fixation part. A filtration device, characterized in that a cap body connected and fixed to the cap body is maintained in an inserted state, and a leakage liquid outlet opening between a plurality of gaskets is bored in a side wall of the lid body. 2. The packing is an O-ring accommodated in at least two annular grooves provided on the outside of a convergence fixing part of the hollow fiber bundle or a cap body connected and fixed to the convergence fixing part. The filtration device described. 3. The filtration device according to claim 1, wherein the inlet for the liquid to be treated and the outlet for the treated liquid are provided in a straight line on the side wall of the lid.