JPS63291606A - Separator for fluids - Google Patents

Abstract

PURPOSE:To make it possible to cope with the change in volume of fluid to be separated, by disposing a small tube having higher rigidity than a hollow yarn membrane and through holes on its side wall inside the hollow yarn membrane and fixedly joining the tube with the membrane in the manner that the tube is protruded outside at least at one end of the membrane. CONSTITUTION:A small tube 9 having through holes 13, 13' on its side wall is inserted into the hollow portion of a hollow yarn membrane 8. The small tube 9 is fixed to the hollow yarn membrane 8 at each end of said membrane 8 so that the through holes 13, 13' remain within the hollow portion of the membrane 8. Supplied fluid 15 introduced from one end opening 7 of the small tube 9 passes through the through holes 13, 13' and the side wall of the hollow yarn membrane 8 to become filtered fluids 16. Cleaning of the hollow yarn membrane and recovering of the remainder of the supplied liquid are conducted by letting flow clean water, cleaning liquid or air through either one of the end openings 7, 7' with both of the openings 7, 7' opened.

Description

Detailed Description of the Invention (a) Industrial Application Field The present invention relates to a fluid separator using a hollow fibrous membrane used for ultrafiltration, reverse osmosis, microfiltration, dialysis, gas separation, gas filtration, etc. Regarding. More specifically, the present invention relates to a fluid separator having a structure in which a thin tube having one or more through holes in the side wall is inserted into a hollow portion of a hollow fibrous membrane.

(B) Definition of Terms In the present invention, the term "hollow fibrous membrane" refers to a membrane having a tubular (pipe-like) shape with a diameter of 1 cm or less. Therefore,
Hollow fibrous membranes include so-called "hollow fiber" membranes, membranes with a larger hollow diameter than hollow fibers called "tubular membranes," and even flat membranes that are made into tubes by bonding, thermocompression, etc. It also includes shaped membranes.

In the present invention, the term "tubule" refers to a cylindrical molded article having an outer diameter that can be inserted into the hollow part of a hollow fibrous membrane, and its form is not limited to a tube (pipe). That is, in order to facilitate understanding, referring to the attached FIG. 1, the ones shown in FIG. In the capillary tube shown in A) and A) in the same figure, the inside of a part 3 of the side wall of the capillary is a hollow part l, while the inside of the other part 4 of the side wall is a closed part 2. Only one end 7 of the thin tube shown in FIG.

"More rigid than a hollow fibrous membrane" means that the Young's modulus of the structure constituting the thin tube is greater than the Young's modulus of the hollow fibrous membrane, and normally the Young's modulus of a thin tube is 109d.
yn/crA or more is desirable, 10I0dyn/c
It is more preferable if it is d. As long as the Young's modulus of the capillary is larger than that of the membrane, the materials constituting the capillary and the membrane may be the same.

(c) Conventional technology Hollow fibrous membranes are used in the medical/pharmaceutical industry, food industry, and as membranes for hemodialysis, ultrafiltration, reverse osmosis, and gas separation.
It is widely used in the electronic industry. Various types of membranes are produced depending on the purpose, with pore sizes ranging from several tens of microns to several tens of microns.

Compared to those using flat membranes, separation devices using hollow fibrous membranes can be smaller and require less filling capacity if they have the same membrane area, and can be assembled as modules. It is easy to handle because it is
Further, as a filtration method, there is an advantage that so-called parallel filtration, in which filtration is performed while flowing a fluid, can be efficiently performed. Generally speaking, the larger the volume of the separation fluid, the greater the advantages of these advantages.
There is a tendency for it to be revived.

With the rapid progress of membrane separation technology, membranes with superior characteristics have been developed, and the range of separation targets has been expanded.
What is needed is a separation device with the most suitable membrane and the most suitable separation capacity for each separation operation. Conventional hollow fibrous membrane modules are made by bundling a certain number of hollow fibrous membranes, embedding both ends in adhesive, etc., and fixing them in a plastic or metal tube. It is difficult to freely select the membrane area depending on the volume.

In particular, the volume of the fluid to be separated is from several tens of I to several microns! When it comes to such a small amount, it becomes necessary to extremely reduce the effective membrane area and the filling capacity of the separator, but this is difficult to do with conventional equipment.

It is possible to assemble a series of separation modules in which the effective membrane area is continuously changed by appropriately increasing or decreasing the number of embedded membranes in conventional hollow fiber membrane modules, but this is complicated and expensive, and is not industrially practical. . Furthermore, if the effective membrane area becomes smaller, the amount of filtration fluid must be WIIt. However, in a conventional module in which a hollow fibrous membrane is fixed in a plastic or metal cylinder, the filling capacity for filtration fluid is large, and therefore a small amount of filtration fluid cannot be efficiently collected.

On the other hand, in a separator using a flat membrane, it is necessary to prepare several types of demounters with different membrane areas, which is not only impractical but also unsuitable for separating microfluids of 100J11 or less. . Furthermore, filtration using a flat membrane is generally a vertical filtration system, and clogging is more pronounced than in parallel filtration.

(d) Problems to be Solved by the Invention In consideration of the above-mentioned current situation, the purpose of the present invention is to solve the problem for separating fluids of any volume, from a very small amount on the I order to a large volume on the KA order, depending on the purpose. An object of the present invention is to provide a fluid separator using a hollow fibrous membrane, which can be provided with an optimal membrane area and filling capacity.

(v) Means for Solving the Problems The fluid separator according to the present invention has a thin tube inserted into the hollow part of the hollow fibrous membrane, which is more rigid than the hollow fibrous membrane and has a through hole in the side wall. The method is characterized in that the thin tube and the hollow fibrous membrane are joined together with the thin tube protruding outward from the hollow fibrous membrane at least at one end of the hollow fibrous membrane.

The feature of the present invention is that the thin tube inserted into the hollow part of the hollow fibrous membrane functions as (1) a membrane support and (2) an entry path for the liquid cavity. In order to meet the above objective (1), the capillary tube must be more rigid than the membrane, and is preferably made of a material that can withstand acids, alkalis, and other corrosive substances. When both ends of the thin tube protrude outward from the open end of the hollow fibrous membrane, it is desirable that one or more through holes exist in the side wall of the hollow portion of the thin tube in order to achieve the above objective (2). . It is generally preferred that the through-holes have a larger pore diameter than the pores in the side wall of the hollow fibrous membrane. Therefore,
It is also possible for the capillary to function as a pretreatment filter. It is desirable that the number of pores in the capillary be as large as possible so that the capillary can function as a membrane support.

FIG. 2 is a sectional view showing another example of the separator according to the present invention. Two through holes 13, 13 in the side wall of the hollow part of the thin tube 9.
A thin tube (an enlarged perspective view of this thin tube is shown in FIG. 3) having a diameter of It has a structure in which the thin tube 9 and the membrane 8 are joined at both ends of the hollow fibrous membrane 8 in a state where the membrane 8 remains in the state. One open end 7 of the thin tube 9
The supply fluid 15 introduced from the through holes 13 and 13'
The fluid passes through the side wall of the membrane 8 and becomes the filtered fluid 16.

When performing vertical filtration, the capillary opening end 7' is sealed with silicone rubber, etc., and the supply fluid 15 is passed through the other capillary opening end 7.
can be passed through the channel 7-1-13 (13') -10 to obtain the filtrate fluid 16.

FIG. 4 shows an example of a separator using a thin tube having eight through holes 13 in its side wall. A similar structure can be constructed using a closed tube (for example, shown in FIG. 1-2) in which one end of the thin tube is closed in advance (see FIG. 6).

The one using a closed tube is no different from the one using an open tube in terms of separation ability, but there is a problem with cleaning the inside of the membrane and the residual supply remaining in the hollow part of the capillary 1 and between the capillary and the hollow fibrous membrane. For fluid recovery work, it is easier to use open pipes. The membrane can be cleaned by leaving both ends 7 and 7' of the capillary tube open and allowing clean water, cleaning liquid or gas to flow through 7 or 7'.

Further, recovery of the remaining supply fluid can be similarly achieved by a method such as pressurizing gas or the like from either opening with both openings 7 and 7' open.

The positions of the side wall through holes 13, 13' of the thin tube are not limited to the positions shown in FIGS. 2, 4 and 5, but may be any position on the side wall of the hollow portion of the thin tube sandwiched between the adhesive parts 14, 14'. Further, the number of through holes can be freely selected within a range that allows the capillary to function as a membrane support, and the diameter of the through holes on the side wall is preferably in a range larger than the pore diameter of the membrane.

FIG. 6 shows an example of a separator in which a single-closed tube having a closed portion 2 on one side of the tube is used as a thin tube. Supply fluid 15 is 7→1
It reaches the inside of the hollow fibrous membrane 8 through the route →13→10.

The use of a single-closed tube allows the filling capacity in the fluid separator to be reduced, which is particularly effective when separating extremely small amounts of fluid.

FIG. 7 is an example of a separator in which a closed tube having a closed portion in the middle of the tube is used as a thin tube. Supply fluid 15 is 7→1→1
3-10-13'→1'-7', a part of the fluid passes through the membrane 8 as the filtration fluid 16. A filtration method in which the feed fluid flows parallel to the membrane in this manner is called parallel filtration, and the greatest advantage of using a closed tube as a thin tube is that this parallel filtration can be performed efficiently. Even when a closed tube as shown in FIG. 4 is used, it is not efficient, but if the pore size is large and the filtration rate is high, parallel filtration is achieved. Naturally, even when a closed tube is used, vertical filtration can be performed by closing 7' with silicone rubber 28 or the like.

The shape of the tubule is not limited to a straight line. For example, if it is formed into a spiral or spiral shape, a large membrane area can be secured in a smaller space. Another advantage of non-linear tubules is that
For example, if the thin tube is bent at a certain angle as shown in FIG. 8, the filtrate 16 that has passed through the membrane 8 will flow toward the inflection point 17 on the outside of the membrane 8, making it easier to collect the filtrate. It can be done. The same effect can be obtained even if it is bent in a curved line as shown in FIG. Although Figures 8 and 9 show the case of an open tube, this is the same for a closed tube, a closed tube, or a partially closed tube.In particular, in the case of parallel filtration using a closed tube, the narrow tube Having an inflection point facilitates collection of filtrate fluid.

When the connecting part to the syringe barrel is connected to the open end of the capillary,
The supply fluid can be easily supplied by a syringe. Figure 10 shows a connecting part 2 at one end of an open tube with two through holes in the side wall.
0, which is connected to a syringe 18, and the open end of the other open tube is closed with silicone rubber 28. The same applies to cases where a closed tube, a closed tube, or a partially closed tube is used.

When filtration is performed by vertically standing a hollow fibrous membrane with one open end closed as shown in Figure 10, particles floating in the supplied fluid are difficult to adhere to or accumulate on the membrane. It peels off from the top of the membrane and accumulates in the lower part of the hollow part 10' of the hollow fibrous membrane. Therefore, a decrease in filtration rate due to membrane clogging can be prevented, and deposits can be easily recovered after filtration.

To collect the deposits, for example, the membrane immediately above the adhesive portion 14' may be cut open and washed away with water, or the membrane in the area where the deposits have accumulated may be removed. good.

An effective means for preventing deposits from adhering to the membrane is to periodically increase or decrease the load pressure on the membrane. For example, the 10th
In the figure, the piston 19 can be moved up and down. As the piston 19 moves up and down, the surface 112 vibrates, and the supplied fluid repeatedly washes the membrane surface, resulting in parallel filtration.
It is possible to prevent deposits from adhering to the film surface.

FIG. 11 shows a separator using an open tube connected to a syringe.
A method is shown in which a supply fluid 15' in a container 23 such as a test tube is sucked up into the hollow fibrous membrane hollow part 10 or the syringe barrel 18 using a syringe from the open end of an open tube that is not connected to a syringe.

When the supply fluid 15' is large, such suction is not necessarily necessary, and it can be sucked directly from the mouth of the syringe barrel 18, or by connecting a separate injection needle. However, when the amount of fluid to be supplied is extremely small, for example, less than a few dozen, the suction method as shown in FIG. 11 is suitable.

When using a closed tube, connecting parts 20 are attached to both open ends of the thin tube.
, 20' and two syringes as shown in FIG. 12, parallel filtration can be performed continuously. That is, when the piston 19 is pushed down, the supply fluid 15 passes through the hollow part 10 of the hollow fibrous membrane 8 and the syringe barrel 18
' flows into '. Next, the supply liquid 15 flows into the syringe barrel 18 again by pushing down the piston 19'. By repeating this process, the feed fluid 15 can be continuously filtered in parallel.

When the feed fluid is present in large enough quantities to fill the pumps and circuit tubing, parallel filtration can be achieved by constructing a closed circuit with a pump in the circuit, as is common practice. A circulating method can also be adopted, but if the feed fluid is small, for example less than 10 ml, parallel filtration should be performed using a separator as shown in Figure 12 to minimize loss of the feed fluid. is advantageous.

In the separator of the present invention, a thin tube serving as a membrane support and a supply fluid introduction path is inserted into the hollow part of one hollow fibrous membrane, so that one hollow fibrous membrane can be used as one separator. Can be used independently. Therefore, by changing the diameter and length of the hollow part of the hollow fibrous membrane, a single hollow fibrous membrane can have any desired effective membrane area.

Table 1 shows the relationship between the inner diameter and length of the hollow portion of the hollow fibrous membrane and the effective membrane area and filling capacity.

Margin Table 1 Below As shown in Table 1, for example, if 15 cm of hollow fiber with an inner diameter of 0.2 cm is used, the effective membrane area is approximately 9.5 c [
Il (this is 1 = using a planar membrane with a diameter of 41 wrm)
It is possible to construct a separator with a filling capacity of 5004, ignoring the accumulation of capillaries. When the inner diameter is 0.03 cm (300 m), the length is 10 cn+, the effective membrane area is 1 coI, and the filling capacity is 7 μ! If the length is 1cm, the filling capacity is 1! l! The following separators can be configured.

By connecting a plurality of one fluid separator in the present invention in parallel or in series, a separator with a large membrane area can be easily constructed.

As shown in FIG. 13, when the supply fluid 15 is flowing through a tube 24 made of silicone rubber or the like, it is possible to construct a separator for parallel filtration by passing both ends of the thin tube 9 through the tube 24. can.

At this time, the membrane area can be increased or decreased by arbitrarily selecting the number of hollow fibrous membranes. The amount of fluid supplied to the separator can be adjusted eight times by opening and closing the pinch cock 26.

In extracorporeal blood circulation experiments using rats and rabbits (e.g., artificial dialysis, plasma exchange, etc.), it is necessary to prepare a separator according to the blood flow rate of the animal being used, but the present invention can quickly and Effective membrane area can be increased or decreased accurately.

In conventional hollow fiber membrane separation modules, if even one of the many hollow fibers had a pinhole, the entire module had to be replaced, but with the separator of the present invention, Even if a pinhole or the like occurs, only the defective one can be replaced, thereby avoiding major interruptions in experiments, work, etc., and eliminating wasted membranes.

FIG. 14 shows how the separator is connected when the feed fluid 15 is flowing in a tube 22, such as glass or metal. The tubes 22 and 22' are closed with rubber plugs 21 and 21' made of silicone, and the thin tube 9 is passed through and connected.

FIG. 15 shows a connection method for performing vertical filtration when a tube 22 made of glass, metal, etc. is used as a flow path for the supply fluid 15.

The separator according to the present invention has a filtration method in which a supply fluid is flowed into the hollow part of a hollow fibrous membrane and the filtrate fluid is taken out of the membrane, and a filtration method in which a supply fluid is flowed outside the hollow fibrous membrane and inside the hollow fibrous membrane. It is also possible to adopt a system in which the permeated fluid is taken out. Conventional hollow fiber membranes do not have a support for each membrane, so when pressurizing from the outside of the hollow fibers to the inside or suctioning from inside the hollow fibers, the permeation efficiency decreases due to the deformation of the hollow part. This was likely to cause a drop in the flow rate and an inability to collect the permeated fluid.

FIG. 16 shows an example of a suction filtration method using a separator using a closed tube having 14 through holes in the side wall of the hollow part of the thin tube. The thin tube is connected to the syringe barrel 18, and with the membrane 8 completely immersed in the supply fluid 15, the piston 19 can be pushed up to guide the filtrate fluid 16 into the syringe barrel 18 in the order of 10=13-1. can. The side wall 3 of the hollow part of the capillary tube and the membrane 8 come into contact with each other due to suction, so the surface of the side wall 3 of the hollow part of the capillary tube is filed to create grooves, or a part of the surface is dissolved with a corrosive agent to form unevenness. Using means, filter fluid 1
If 6 channels are secured, the filtration efficiency will be increased.

The fluid separator is suitable for sample preparation in tests performed with small volumes of filtered fluid (eg, liquid chromatography, gas chromatography, thin layer chromatography, various blood tests, various enzyme reactions, etc.).

[Brief explanation of drawings]

Figures 1a), 2) and 3) are explanatory diagrams for explaining the definition of thin tubes used in the fluid separator of the present invention, and Figure 2 is an example of the structure of the fluid separator of the present invention. FIG. 3 is a diagram showing the appearance of a thin tube having two through holes shown in FIG. 2, and FIG. 4 is a further example of the structure of the fluid separator of the present invention. 5 is a sectional view showing still another example of the structure of the fluid separator of the present invention, and FIG. 6 is a sectional view showing still another example of the structure of the fluid separator of the present invention. 7 is a sectional view showing still another example of the structure of the fluid separator of the present invention, and FIG. 8 is a sectional view showing still another example of the structure of the fluid separator of the present invention. FIG. 9 is a cross-sectional view showing still another example of the structure of the fluid separator of the present invention, and FIGS. 10 and 11 are cross-sectional views of the structure of the fluid separator of the present invention. FIG. 12 is a sectional view showing still another example of the structure of the fluid separator of the present invention and an example of its usage; FIG. FIG. 14 is an explanatory diagram showing another example of how the fluid separator of the present invention is used; FIG. 14 is an explanatory diagram showing still another example of how the fluid separator of the present invention is used; FIG. 15 is an explanatory diagram showing still another example of how the fluid separator of the present invention is used, and FIG. 16 is an explanatory diagram showing still another example of how the fluid separator of the present invention is used. . 1... Thin tube hollow part, 2... Thin tube occlusion part, 3...
...Side wall of tubule hollow part, 4...Side wall of capillary occluded part, 5.
...Closed end of capillary tube, 6...Side wall of closed end of capillary tube, 7.
...tubule opening, 8... hollow fibrous membrane, 9...
- Thin tube, 13, 13'... Side wall through hole, 14, 14'... Adhesive part, 15... Supply fluid, 16... Filtered fluid, 17... Inflection point, 18... Syringe barrel, 19... piston,
20... Connection parts, 21, 21'... Rubber stopper, 22, 22'... Tube (e.g. glass tube), 23... Container, 24... Tube (e.g. silicone rubber tube), 26・
...Pinch cock, 28...Silicone rubber.

Claims (1)

[Claims] 1. A thin tube that is more rigid than the hollow fibrous membrane and has a through hole in the side wall is inserted into the hollow part of the hollow fibrous membrane,
1. A fluid separator comprising a capillary and a hollow fibrous membrane joined together with the capillary protruding outward from the hollow fibrous membrane at least at one end of the membrane.