JP2013184157A - Membrane separation apparatus, membrane fouling measurement method, membrane separation apparatus operation method, and submodule - Google Patents

Abstract

PROBLEM TO BE SOLVED: To grasp the degree of membrane fouling with precision with a submodule.SOLUTION: A membrane separation apparatus includes a separation membrane module including a separation membrane and a submodule 2 including a fouling evaluation separation membrane 23. The submodule 2 includes a container 30 that accommodates the fouling evaluation separation membrane 23, a supply side flow passage 61 through which a sampling fluid S introduced into the container 30 passes and with which a membrane surface 23f of the fouling evaluation separation membrane 23 comes into contact, and a transmission side flow passage 62 arranged on the opposite side of the supply side flow passage 61 via the fouling evaluation separation membrane 23. The container 30 includes a container body 31 having an opening 50 and a lid part 32 detachably attached to the opening 50. The opening 50 is provided at a position facing the membrane surface 23f with the supply side flow passage 61 sandwiched in between.

Description

  The present invention relates to a membrane separation apparatus comprising a separation membrane module (operation module) having a separation membrane that permeates a supply fluid to generate a permeated fluid, and a submodule for membrane surface evaluation (evaluation of the surface of the separation membrane), The present invention relates to a method for measuring membrane fouling using the membrane separator and a method for operating the membrane separator. The present invention also relates to a submodule for evaluating membrane fouling of a separation membrane module.

  The separation membrane module in the membrane separation apparatus has a separation membrane such as a reverse osmosis membrane or an ultrafiltration membrane, and can filter (separate) various fluids such as gas or liquid by membrane separation action of the separation membrane. . For example, according to the reverse osmosis membrane device, brine or seawater can be desalted to produce fresh water, or pure water or ultrapure water can be produced using industrial water (for example, see Patent Document 1).

  In such a separation membrane module, organic substances, inorganic substances, fungi, etc. present in the fluid are deposited as scales or biofilms on the surface of the separation membrane (hereinafter sometimes referred to as membrane surface or membrane surface) over time. As a result, the membrane surface is fouled, and the membrane performance (membrane separation action of the separation membrane) may be deteriorated. In order to deal with such a problem, cleaning of the separation membrane is effective. Conventionally, chemical cleaning with an alkaline solution or the like, or physical cleaning such as reverse cleaning in which a supply fluid is flowed in a direction opposite to the direction during operation, has been performed based on experience and fluid data before and after membrane separation. In recent years, apart from the separation membrane module, a small sub-module is installed outside the operation system, and the degree of membrane fouling in the sub-module is monitored to stop the membrane fouling in the separation membrane module without stopping the separation membrane module. It has been proposed to determine the timing of performing physical cleaning or chemical cleaning of the separation membrane in the separation membrane module based on the degree of the ring (see, for example, Patent Documents 1 to 3). In the case where the membrane separation action of the separation membrane in the separation membrane module is not sufficiently recovered by washing, the separation membrane may be replaced.

JP 2008-253953 A Japanese Patent Laid-Open No. 10-286445 Special table 2009-524521

  Among the parameters representing the membrane surface state in the submodule, parameters that have a strong correlation with the membrane separation action of the separation membrane in the separation membrane module were not clear. For this reason, by monitoring the membrane surface state in the submodule, the membrane surface state of the separation membrane module (particularly the formation of a biofilm derived from bacteria) may not be sufficiently grasped. That is, it is not easy to accurately determine the proper cleaning and replacement time by using the submodule.

  The present invention has a separation membrane module and a submodule that is a module different from the separation membrane module and that monitors the membrane surface state of the separation membrane, and the membrane fouling of the separation membrane module is a submodule. It is an object of the present invention to provide a membrane separation device that can be grasped with high accuracy by using the membrane separation device, to provide a method for measuring membrane fouling using the membrane separation device, and to provide a method for operating the membrane separation device. Moreover, an object of this invention is to provide said submodule.

  As a result of diligent research, the present inventors have found that, among the parameters representing the membrane surface state in the submodule, the thickness and deposition amount (biomass amount) of the membrane fouling on the separation membrane in the submodule are determined in the separation membrane module. It was found to be important as an index for grasping the membrane separation action of the separation membrane. According to this knowledge, it is conceivable to configure the sub-module so that the fluid can be continuously supplied to the sub-module and the thickness and deposition amount of the membrane fouling on the separation membrane can be grasped continuously or periodically. . For this purpose, it is conceivable that a plurality of submodules are provided in the separation membrane module, the separation membranes in each submodule are periodically taken out sequentially, and each membrane surface is observed. However, in this case, since the film surfaces of submodules arranged at different positions are observed, the data indicating the film surface state (film fouling thickness, deposition amount, etc.) is inconsistent. Therefore, there is a possibility that the accuracy of grasping the membrane separation action, that is, membrane fouling in the separation membrane module may be lowered. It is also conceivable that a part of the container containing the sub-module separation membrane is made of a transparent member and the membrane surface is observed through this transparent member. However, in this case, foulant (causal substance for fouling) adheres to the inner surface of the transparent member, and the accuracy of observation of the film surface may decrease with time.

The present invention
For a fouling evaluation in which a separation membrane module including a separation membrane that permeates a supply fluid to generate a permeation fluid and a sampling fluid that is a fluid flowing through a branch path branched from a flow path connected to the separation membrane module A membrane separation device comprising a submodule comprising a separation membrane,
The sub-module includes a container that contains the separation membrane for fouling evaluation, a supply-side flow path through which the sampling fluid introduced into the container passes, and a membrane surface of the separation membrane for fouling evaluation contacts, A permeation-side channel disposed on the opposite side of the supply-side channel via the fouling evaluation separation membrane,
The container includes a container main body having an opening, and a lid part detachably attached to the opening.
The opening is provided at a position facing the membrane surface across the supply-side flow path,
Membrane separator,
I will provide a.

The present invention also provides:
A membrane fouling measurement method using the membrane separation device and a measuring instrument having an objective lens,
An insertion step of removing the lid from the opening and inserting the objective lens into the opening;
A state of measuring the state of the film surface by the measuring instrument with the objective lens inserted into the opening.
Membrane fouling measurement method,
I will provide a.

The present invention also provides:
An operation method of the above membrane separation device,
The membrane separation apparatus further comprises data processing means for processing electronic data obtained by measurement of the membrane surface of the separation membrane for fouling evaluation,
A method for operating a membrane separator, wherein the electronic data is stored, analyzed or transmitted using the data processing means,
I will provide a.

The present invention also provides:
A fluid that flows along a branch path that branches from a flow path connected to the separation membrane module and that forms a membrane separation apparatus alongside a separation membrane module that includes a separation membrane that permeates a supply fluid to generate a permeation fluid. A sub-module including a separation membrane for fouling evaluation that allows a sampling fluid to pass therethrough,
A container containing the separation membrane for fouling evaluation; a supply-side flow path through which the sampling fluid introduced into the container passes, and a membrane surface of the separation membrane for fouling evaluation is in contact; and for fouling evaluation A permeation side flow path disposed on the opposite side of the supply side flow path through a separation membrane,
The container includes a container main body having an opening, and a lid part detachably attached to the opening.
The opening is provided at a position facing the membrane surface across the supply-side flow path,
Submodules,
I will provide a.

  A lid is detachably attached to the opening of the container body of the submodule according to the present invention. Therefore, the lid can be removed from the opening when measuring the membrane surface of the submodule. Thereby, a film surface can be measured in the state which removed the cover part from the opening part. That is, according to the membrane separation apparatus of the present invention, the membrane surface can be measured without going through the submodule container. Therefore, the foulant adhering to the container does not deteriorate the measurement accuracy. Further, the opening of the container body can be blocked by the lid during steady operation of the submodule (when the submodule has a predetermined internal pressure), so that the sampling fluid in the submodule overflows through the opening. You can avoid getting out.

Configuration diagram showing an example of a membrane separation apparatus of the present invention The perspective view which shows an example of a structure of the submodule of this invention Sectional view of the submodule in FIG. The perspective view which shows another example of a structure of the submodule of this invention Sectional view of the submodule in FIG. The perspective view which shows another example of a structure of the submodule of this invention. Sectional drawing of the submodule in FIG. The perspective view which shows another example of a structure of the submodule of this invention. Sectional view of the submodule in FIG.

  Hereinafter, embodiments of the present invention will be described with reference to the drawings. The following description relates to an example of the present invention, and the present invention is not limited to the following embodiment.

(First embodiment)
FIG. 1 shows a membrane separation apparatus 10 which is a membrane separation apparatus according to the first embodiment. As shown in FIG. 1, the membrane separation apparatus 10 includes a separation membrane module (operation module) 1 and a submodule 2. The separation membrane module 1 is a module for membrane separation of the supplied fluid, and the submodule 2 is a module for evaluating membrane fouling. The separation membrane module 1 and the submodule 2 are cross flow type modules. The separation membrane module 1 is connected to the first flow path 11 on the downstream side of the first flow path 11. The submodule 2 is provided on the downstream side of the second flow path 12 that is a branch path branched from the first flow path 11, and is connected to the second flow path 12. A part (most part) of the supply water F (corresponding to the supply fluid in the claims) is guided to the separation membrane module 1 by the first flow path 11, and the permeated water (permeation fluid in the claims) by membrane separation. Is separated into T ₁ and concentrated water C ₁ . Sampling water S (corresponding to the sampling fluid in the claims), which is another part (remainder) of the supply water F and is branched from the first flow path 11 to the second flow path 12, is led to the submodule 2. The permeated water T ₂ and the concentrated water C ₂ are separated by membrane separation. The first flow path 11 is provided with a pressurizing pump 6 for generating a flow of the supply water F. Further, the second flow path 12 is provided with a valve (a supply pressure adjusting valve, which corresponds to the flow rate adjusting means in the claims) 5 for adjusting the flow rate of the sampling water S introduced into the submodule 2. . The membrane separation device 10 further includes a stain tank 4, and the stain tank 4 is connected to the second flow path 12 by a flow path provided with a valve 7. As will be described later, the submodule 2 is configured so that the inside of the submodule 2 can be measured by a measuring device 3 having an objective lens.

  Examples of the supply water F include brine and seawater. Further, in this specification, the terms “feed water” and “sampling water” are used for the fluid supplied to the separation membrane module 1 and the sub module 2, but the fluid is supplied to the separation membrane module 1 and the sub module 2. The fluid is not limited to water. Examples of the fluid supplied to the separation membrane module 1 and the submodule 2 include liquids other than water, gas, vapor, and the like. However, when there are many factors causing membrane fouling in the supply fluid, the effect of confirming the degree of membrane fouling (details will be described later) becomes significant. Considering this, the membrane separation apparatus 10 is suitable for water treatment using brine, seawater, waste water, irrigation water, or the like as a supply fluid. Factors that cause membrane fouling include suspended substances (fine particles, microorganisms, etc.), scales (metal oxides such as iron and manganese, sparingly soluble inorganic substances such as calcium carbonate and silica), biofilms (bacteria such as bacteria) Sediment) and organic substances (oil, residual polymer, etc.).

  The separation membrane module 1 includes a separation membrane that permeates a supply fluid to generate a permeated fluid. The separation membrane is a membrane for membrane separation of fluid, and membrane separation is a general term for operations for filtering a target object by passing the fluid through a partition wall (membrane) having selectivity. Examples of the separation membrane of the separation membrane module 1 include a reverse osmosis (RO) membrane, a nanofiltration (NF) membrane, an ultrafiltration membrane (UF) membrane, and a microfiltration (MF) membrane. Examples of the material of the separation membrane of the separation membrane module 1 include polymer materials such as cellulose acetate, polyvinyl alcohol, polyamide, and polyester. These polymer materials are particularly suitable as an RO membrane for water treatment. Moreover, what is necessary is just to employ | adopt a well-known structure as a structure of the separation membrane module 1. FIG. Specifically, examples of the separation membrane module 1 include modules such as a flat membrane type such as a frame and plate type, a tubular type such as a tubular type, a hollow fiber type, a spiral type, and a pleated type.

Next, the configuration of the submodule 2 of the present embodiment will be described with reference to FIGS. 2 and 3. Submodule 2 is a module of a cross flow system with a simple structure, the inlet port 27 to sampling water S flows, the concentrated water outlet port 28 which is concentrate C ₂ flows, the permeate T ₂ flowing And a permeate outflow port 29. In the submodule 2, the permeate-side flow path member 24, the fouling evaluation separation membrane 23, and the deposition material 22 are stacked in this order, and the stacked body is accommodated in the container 30. A supply-side channel 61 and a permeate-side channel 62 are formed in the container 30. The supply-side channel 61 is a channel through which the sampling water S introduced into the container 30 passes, and is a channel in contact with the membrane surface 23f of the fouling evaluation separation membrane 23. The permeate side channel 62 is a channel disposed on the opposite side of the supply side channel 61 through the fouling evaluation separation membrane 23, and the permeated water T _{2 that} has passed through the fouling evaluation separation membrane 23 passes therethrough. It is a flow path. For convenience of viewing the drawing, the deposition material 22, the fouling evaluation separation membrane 23, and the permeate-side flow path material 24 are omitted in FIG.

  The fouling evaluation separation membrane 23 is a separation membrane that allows the sampling water S to pass therethrough. As the separation membrane 23 for fouling evaluation, a separation membrane made of the same material as the separation membrane that can be employed as the separation membrane of the separation membrane module 1 can be used.

  The deposition material 22 is provided in contact with the membrane surface 23 f of the fouling evaluation separation membrane 23 facing the supply-side flow path 61. The deposition material 22 temporarily dams the flow of the sampling water S, causes the flow of the sampling water S in the submodule 2 to stay or turbulence, and promotes the deposition of film fouling on the film surface 23f. Examples of the material for the deposition material 22 include resins (including synthetic polymers such as polypropylene (PP), polyethylene (PE), polyethylene terephthalate (PET), polyamide (PA), and natural polymers), rubber (synthetic rubber and Natural rubber), metals and the like.

  The deposition material 22 is preferably a member that covers a part of the separation membrane 23 for fouling evaluation. In this preferred embodiment, a part of the membrane surface 23 f of the fouling evaluation separation membrane 23 is exposed to the supply-side channel 61. In the present embodiment, the deposition material 22 is a lattice net. However, the deposition material 22 may be configured by a group of convex portions provided discretely. In addition, when the deposition material 22 is too thick, the shielding effect of the sampling water S becomes too high, and the portion where the flow of the sampling water S easily reaches the flow of the sampling water S in the separation film 23 for fouling evaluation and the flow of the sampling water S are difficult to reach. A portion is likely to be generated, and membrane fouling may occur in a part of the membrane surface 23f, and the reproducibility of the distribution of membrane fouling in the separation membrane module 1 by the submodule 2 is lowered. On the other hand, if it is too thin, the turbulent flow and the retention effect of the sampling water S are not sufficiently exhibited. From the above, the dimension along the thickness direction of the separation film 23 for fouling evaluation of the deposition material 22 is, for example, 0.1 mm or more, for example, about 5 mm or less, preferably 0.3 mm or more, and preferably 2 mm or less. . Moreover, the method of installing the depositing material 22 on the film surface 23f is not particularly limited, and examples thereof include a method of adhering to the film surface 23f and a method of fixing by sandwiching with the members constituting the container 30 of the submodule 2. When the deposition material 22 is provided over the entire surface 23f of the film, the deposition material 22 having the same size as the fouling evaluation separation film 23 is sandwiched between the fouling evaluation separation film 23 and a member constituting the container 30 in plan view. And fixing.

The permeate-side flow path member 24 is provided so as to contact the membrane back surface 23 b of the fouling evaluation separation membrane 23 facing the permeate-side flow path 62. The permeate-side channel material 24 is a member for guiding the permeate T ₂ to the outflow port 29 without stagnation. As the permeate-side flow path member 24, a member similar to a member that can be employed as the deposition material 22 can be used. In addition, the permeation | transmission side flow path material 24 and the deposition material 22 may consist of the same material, and may consist of a different material. Moreover, the permeation | transmission side flow-path material 24 and the deposition material 22 may have the same shape, and may have a different shape.

  The container 30 includes a container main body 31 having an opening 50 and a lid part 32. The opening 50 is an opening for inserting an objective lens (for example, an immersion lens (water immersion lens or the like)). Specifically, the opening 50 sandwiches the supply-side channel 61 so that the membrane surface 23f of the fouling evaluation separation membrane 23 facing the supply-side channel 61 can be measured (observed) using an objective lens. It is provided at a position facing the film surface 23f. The lid 32 is detachably attached to the opening 50.

  By the way, during the steady operation of the membrane separator, the submodule has a predetermined internal pressure. For example, the internal pressure is 0.1 to 10 MPa. In particular, when seawater is desalinated by a membrane separator, a high pressure is applied to the supply fluid, and the internal pressure of the submodule is particularly high (for example, 1.5 to 10 MPa). When the container has an aspect in which the container main body is closed with a detachable lid, depending on the aspect of the container main body and the lid, the container may drop off without being able to maintain the closed state of the opening. There is a possibility that the sampling water S inside overflows through the opening. Therefore, it is desirable that the container has a predetermined pressure resistance. Therefore, it is preferable that the lid portion 32 is attached to the opening portion 50 so as not to drop out from the opening portion 50 when the internal pressure of the submodule 2 reaches 1.5 MPa, particularly when it reaches 10 MPa.

  In this embodiment, the opening part 50 and the cover part 32 are designed so that the submodule 2 can ensure pressure resistance. Specifically, the opening 50 has a female screw portion 41, and the lid portion 32 has a male screw portion 42 that engages with the female screw portion 41 of the opening 50. That is, when the female screw portion 41 is screwed with the male screw portion 42, the lid portion 32 is screwed into the opening 50, thereby ensuring the pressure resistance of the container 30 (submodule 2). In addition, in order to assist sealing of the opening part 50 by the cover part 32, you may interpose an O-ring when these screw together.

  In a state where the lid portion 32 is attached to the opening portion 50, the end surface on the male screw portion 42 side (the end surface in contact with the supply-side flow path 61) 42 s and the inner surface 31 s of the container main body 31 are flush with each other. Is preferred. Since the inner surface of the container of the separation membrane module 1 facing the membrane surface normally has no irregularities, the above configuration improves the reproducibility of membrane fouling in the separation membrane module 1 by the submodule 2. Can do. Further, the position of the opening 50 may be appropriately set in consideration of the ease of measurement using the objective lens (the measuring device 3 having the objective lens). For example, the position on the upper side when the submodule 2 is installed. Should be set.

  In the present embodiment, the lid portion 32 is transparent. Therefore, even when the lid portion 32 is attached to the opening portion 50, the membrane surface 23f of the fouling evaluation separation membrane 23 can be observed. In some cases, foulant may adhere to the inner surface of the lid portion 32. In this case, the accuracy of the evaluation of the membrane fouling is lowered, and therefore the membrane surface 23f in a state where the transparent lid portion 32 is attached to the opening 50. Although it is difficult to continue observation with high accuracy of film fouling only by observation, this observation is useful in determining the timing of observation by the objective lens.

  For the same reason, in the present embodiment, the container body 31 is also transparent. That is, both the lid portion 32 and the container body 31 are transparent members.

  Examples of a material suitable for ensuring high pressure resistance of the container body 31 and the lid portion 32 include metals such as stainless steel. An example of a transparent material suitable for the container body 31 and the lid portion 32 is pressure-resistant glass. In addition, the container main body 31 and the cover part 32 may be comprised from the same material, and may be comprised from a different material.

  Although the membrane separation apparatus 10 described above includes two separation membrane modules 1, the number of separation membrane modules 1 is not particularly limited, and may be one or three or more. Similarly, the number of submodules 2 may be one or two or more. That is, the membrane separation apparatus 10 only needs to have at least one separation membrane module 1 and at least one submodule 2.

  In the present embodiment, the separation membrane module 1 and the submodule 2 are cross-flow type modules, but other types of modules such as a total filtration method are adopted as the separation membrane module 1 and / or the submodule 2. Also good. However, from the viewpoint of increasing the reproducibility of membrane fouling in the separation membrane module 1 by the submodule 2, it is preferable that the filtration method in the submodule 2 is the same filtration method as the filtration method in the separation membrane module 1.

Moreover, in this embodiment, most of the supply water F is introduced into the separation membrane module 1, and the remainder of the supply water F is introduced into the submodule 2 (the sampling water S is constituted by a part of the supply water F. As described above, the positional relationship between the separation membrane module 1 and the submodule 2 is determined. Thereby, the reproducibility of the membrane fouling of the separation membrane module 1 by the submodule 2 is improved. However, the positional relationship between the separation membrane module 1 and the submodule 2 is not limited to this. For example, the positional relationship between the separation membrane module 1 and the submodule 2 may be determined so that the concentrated fluid C ₁ discharged from the separation membrane module 1 is introduced into the submodule 2. If this positional relationship is adopted, since membrane fouling (especially biofilm or the like) appears in the submodule 2 in a short period of time, analysis of the tendency of membrane fouling that can occur can be performed at an early stage.

  In the present embodiment, the separation membrane in the separation membrane module 1 and the separation membrane 23 for fouling evaluation in the submodule 2 are made of the same material. Thereby, the reproducibility of the membrane fouling of the separation membrane module 1 by the submodule 2 is improved. However, the separation membrane in the separation membrane module 1 and the separation membrane 23 for fouling evaluation in the submodule 2 may be made of different materials.

  Further, a supply-side channel material may be provided on the surface of the separation membrane module 1 on the side of the separation membrane to which the supply water F is supplied (for example, the separation membrane module 1 is a spiral type module). Etc.) In this case, it is preferable that the deposition material 22 and the supply-side flow path material are made of the same material. Moreover, it is preferable that the deposition material 22 and the supply side flow path material have the same shape. By these, the reproducibility of the membrane fouling of the separation membrane module 1 by the submodule 2 can be improved. However, even when the separation membrane module 1 is provided with the supply-side channel material, the deposition material 22 and the supply-side channel material may be made of different materials and have different shapes. Also good.

  Next, a film fouling measurement method according to this embodiment will be described.

  In the measurement method of the present embodiment, membrane fouling is measured using the membrane separation device 10 described above and the measuring device 3 (typically a microscope) having an objective lens. This measurement method includes a membrane separation step in which the supply water F (supply fluid) and the sampling water S (sampling fluid) are subjected to membrane separation by the separation membrane module 1 and the submodule 2, and the submodule 2 by the valve 5 (flow rate adjusting means). In a state in which the flow rate adjustment step for reducing the flow rate of the introduced sampling water S, the insertion step for removing the lid 32 from the opening 50 and inserting the objective lens into the opening 50, and the objective lens being inserted in the opening 50 The measuring step of measuring the membrane surface 23f by the measuring device 3, the membrane fouling in the vicinity of the deposition material 22 (first region) on the membrane surface 23f of the separation membrane 23 for fouling evaluation, and the deposition material on the membrane surface 23f A comparative evaluation step of comparatively evaluating film fouling in a portion other than the vicinity of 22 (second region farther from the deposition material 22 than the first region).

  In the membrane separation step, membrane fouling is deposited on the membrane surface of the separation membrane of the separation membrane module 1 and the membrane surface 23f of the separation membrane 23 for fouling evaluation. The period required for the membrane separation process depending on the settings of the membrane separation apparatus 10 (output of the pressure pump 6 and the like) and the components of the feed water F (period required to measure the membrane surface 23f again after measuring the membrane surface 23f) Although it differs, according to the use of the membrane separator 10, it can predetermine. The period required for the membrane separation step is typically 7 to 20 days. Further, when the lid portion 32 and / or the container main body 31 are transparent, the determination may be made based on observation of the film surface 23 f via the lid portion 32 and / or the container main body 31. The membrane separation step is a step that can be established if the supply water F and the sampling water S are supplied to the separation membrane module 1 and the submodule 2, and a membrane separation device for the purpose of filtering the supply water F. It does not require a separate operation from the 10 operations.

  In the flow rate adjustment step, the flow rate of the sampling water S introduced into the submodule 2 is decreased. Thereby, the measurement accuracy of the film surface 23f in the measurement process is improved. If necessary, the opening of the valve 5 may be set to zero and the introduction of the sampling water S into the submodule 2 may be stopped. When gas or vapor is used as the supply fluid and the sampling fluid, it is particularly preferable that the opening degree of the valve 5 is zero in order to prevent the sampling fluid from being released through the opening 50. However, the flow rate adjustment step is not an essential step, and the flow rate of the sampling water S introduced into the submodule 2 during the steady operation of the membrane separation apparatus 10 is so small that it does not interfere with the measurement of the membrane surface 23f. If the sampling water S is not likely to overflow (when the internal pressure of the container 30 is sufficiently low), it can be omitted.

  In the insertion step, first, the lid 32 is removed from the opening 50. Next, an objective lens is inserted into the opening 50 and fixed at a position suitable for measurement of the film surface 23f.

  In the measurement step, the film surface 23f is measured by an objective lens (measuring instrument 3 having an objective lens). In this embodiment, since measurement is not hindered by foulant or the like attached to the container, film fouling on the film surface 23f can be suitably measured. In addition, according to the present embodiment, it is possible to omit the aberration correction of the lens derived from the container.

  A specific method for measuring the film surface 23f in the measurement process is not particularly limited. For example, there is a method of adjusting the opening degree of the valve 7 and injecting a staining agent from the staining agent tank 4 into the submodule 2 to improve the visibility of the membrane fouling and then measuring the membrane surface 23f. As the staining agent tank 4 and the staining agent, known ones may be used. Further, the intensity of the reflected light from the film surface 23f of the submodule 2 can be measured by the measuring device 3 having an objective lens. By measuring the reflected light intensity, the thickness, deposition amount, type, etc. of the film fouling can be estimated. In the measurement process of the present embodiment, since the lid portion 32 is removed from the opening 50, it is difficult to prevent the reflected light from the film surface 23f from reaching the objective lens. Therefore, it can be said that this embodiment is suitable for the measurement of the reflected light intensity from the film surface 23f. The measuring device 3 suitable for measuring the reflected light intensity includes a measuring device of a reflective confocal optical system such as a reflective confocal optical microscope.

  In the comparative evaluation process of the present embodiment, the portion of the film surface 23f is within the periphery of the deposition material 22 that is approximately the same as the thickness of the deposition material 22 (for example, when the deposition material 22 has a thickness of 1 mm, the periphery is about 1 mm). Then, the part A which is the part opposite to the fluid supply side in the deposition material 22 is compared with the part B which is another part in the film surface 23f. In the site A, a membrane foulin such as a biofilm or a scale is more easily deposited than the site B. Therefore, the difference between the amount of membrane fouling at the site A and the amount of membrane fouling at the site B is easy to measure, and this difference is an index for grasping the membrane fouling of the separation membrane 23 for fouling evaluation.

  More specifically, the film surface 23f is partitioned into a covered region that is a region covered with the deposition material 22 and an adjacent region that surrounds and is adjacent to the covered region. Deposition per unit area of deposits deposited in the fluid supply side adjacent region when further divided into the fluid supply side adjacent region on the fluid supply side and the opposite side adjacent region opposite to the fluid supply side as viewed from the coating region It can be said that the film fouling of the separation film 23 for the fouling evaluation of the submodule 2 can be determined at an early stage by comparing the amount and the amount of deposit deposited per unit area in the adjacent region on the opposite side. However, the comparative evaluation process is not an essential process.

  In the present embodiment, the steps described above are repeated. Thereby, the membrane fouling of the separation membrane 23 for fouling evaluation can be grasped continuously (periodically).

  In the measurement method of the present embodiment described above, since the sampling fluid is water (sampling water S), a refractive index corresponding to the refractive index of the sampling water S (for example, 1.0 to 1.. 33), the immersion lens is inserted into the opening 50 so that the immersion lens is immersed in the sampling water S in the insertion step, and the immersion lens is immersed in the sampling water S in the measurement step. The film surface 23f is measured. Thereby, the film | membrane fouling of the film | membrane surface 23f can be measured suitably. That is, when the supply fluid and the sampling fluid are liquids, an immersion lens is used as the objective lens, and the immersion lens is inserted into the opening 50 so that the immersion lens is immersed in the sampling fluid in the insertion step. It is preferable to measure the film surface 23f with the immersion lens immersed in the sampling fluid.

  Further, the membrane separation apparatus 10 may include data processing means for processing electronic data obtained by measuring the membrane surface 23f of the fouling evaluation separation membrane 23. Electronic data can be obtained, for example, by measuring the film surface 23f in a state where an imaging device or the like is connected to the measuring device 3. When the membrane separation apparatus 10 includes data processing means, the data processing means can be used to store, analyze, or transmit electronic data (received if necessary) to a predetermined management place. That is, if a storage device for storing electronic data is used as a data processing means, electronic data can be easily stored, and if an analysis device for analyzing electronic data is used, membrane fouling can be analyzed in real time and transmission for transmitting electronic data can be performed. If an apparatus (transmission / reception apparatus if necessary) is used, film fouling can be evaluated by an external apparatus. The data processing means may be a component of the membrane separation apparatus 10 or an external means attached to the membrane separation apparatus 10 when measuring the membrane surface 23f. Moreover, said analysis is a concept which may include a comparative evaluation process, and the comparative evaluation process may be performed by an analyzer.

(Second embodiment)
In the submodule 2 in the first embodiment, the cover 32 can be detachably attached to the opening 50 by providing the female screw 41 in the opening 50 and providing the male screw 42 in the lid 32. It has gained. However, an aspect in which the lid can be detachably attached to the opening may be obtained by adopting another configuration. For example, the submodule 102 shown in FIGS. 4 and 5 may be used as the submodule. The submodule 102 is a module in which the container 30 in the submodule 2 is replaced with a container 130.

  The container 130 includes a container body 131 having an opening 150 and a lid 132. The opening 150 is an opening for inserting an objective lens. The opening 150 is also an opening for inserting the lid 132. A part of the opening 150 is provided at a position facing the film surface 23 f with the supply-side channel 61 interposed therebetween.

  The opening 150 has an opening surface 155 into which the objective lens is inserted, and an opening surface 145 that opens in a direction along the opening surface 155 and into which the lid portion 132 is inserted. In the opening 150, the opening surface 145, the opening surface 155, and the boundary surface 156 between the opening 150 and the supply-side flow path 61 communicate with each other. The width of the opening surface 145 in the direction from the opening surface 155 to the boundary surface 156 (the short direction of the opening surface 145) is narrower than the distance between the opening surface 155 and the boundary surface 156. Further, the width of the opening surface 145 in the direction along the opening surface 155 (the longitudinal direction of the opening surface 145) is wider than the width of the opening surface 155 and the width of the boundary surface 156 in the same direction. In the opening 150, a space is formed that extends from the opening surface 145 along a direction perpendicular to the opening surface 145. That is, the opening 150 is formed with a slide groove 140 for supporting the lid 132.

  The lid portion 132 is a plate-like member, and is inserted into the opening portion 150 by being slid in a direction perpendicular to the opening surface 145 from the opening surface 145 and supported by the slide groove 140. In this embodiment, the aspect which can attach the cover part 132 to the opening part 150 so that attachment or detachment is possible is obtained.

  In addition, although the cover part 132 of this embodiment has a rectangular shape by planar view, it may have other shapes, such as an ellipse by planar view. In this case, what is necessary is just to change suitably the shape of the opening part 150 so that the shape of the cover part 132 may be adapted.

  The opening 150 may be provided at a position where the opening surface 155 is on the upper side when the submodule 102 is installed, for example.

  The material of the container body 131 and the lid part 132 may be selected from materials that can be employed as the material of the container body 31 and the lid part 32.

  In addition, the submodule 102 may be provided with a motor that provides power for inserting the lid 132 into the opening 150.

(Third embodiment)
Moreover, you may use the submodule 202 shown in FIG. 6 and 7 as a submodule. The submodule 202 is a module in which the container 30 in the submodule 2 is replaced with a container 230.

  The container 230 includes a container body 231 having two openings 250a and 250b and two lids 232a and 232b. The openings 250a and 250b are openings for inserting the objective lens. Specifically, the openings 250a and 250b are provided at positions facing the film surface 23f with the supply-side channel 61 interposed therebetween. The opening portion 250a has a female screw portion 241a, and the lid portion 232a has a male screw portion 242a that engages with the female screw portion 241a of the opening portion 250a. The opening portion 250b has a female screw portion 241b, and the lid portion 232b has a male screw portion 242b that engages with the female screw portion 241b of the opening portion 250b. In addition, in order to assist the sealing of the opening parts 250a and 250b by the cover parts 232a and 232b, an O-ring may be interposed when they are screwed together.

  In the submodule 202, the opening 250a is at a position on the side where the sampling water S flows in the container 230 (inflow port 27 side), and the opening 250b is at a position opposite to the side where the sampling water S flows in the container 230 ( At the concentrated water outflow port 28 side). Biofilm tends to deposit on the side where the sampling water S flows, and scale tends to deposit on the side opposite to the side where the sampling water S flows. That is, according to such a structure, a biofilm can be grasped | ascertained favorably by the measurement in the opening part 250a, and a scale can be grasped | ascertained favorably by the measurement in the opening part 250b. In addition, providing an opening part in both the position of the side into which sampling water S flows in, and the position on the opposite side to the side into which sampling water S flows in is applicable also to 1st embodiment and 2nd embodiment.

  Further, in the present embodiment, in the state where the lid portions 232a and 232b are attached to the openings 250a and 250b, the end surfaces (supply-side flow path 61) of the lid portions 232a and 232b opposite to the male screw portions 242a and 242b side. 242aso and 242bso and the outer surface 231so of the container body 231 are flush with each other, and end surfaces on the male screw portions 242a and 242b side (end surfaces in contact with the supply-side flow path 61) 242asi in the lid portions 232a and 232b And 242bsi and the inner surface 231si of the container main body 231 are flush with each other. Further, the openings 250a and 250b may be provided at a position on the upper side when the submodule 202 is installed, for example.

  The material of the container body 231 and the lids 232a and 232b may be selected from materials that can be used as the material of the container body 31 and the lid 32.

(Fourth embodiment)
Further, the submodule 302 shown in FIGS. 8 and 9 may be used as the submodule. The submodule 302 is a module in which the container 30 in the submodule 2 is replaced with a container 330.

  The container 330 includes a container body 331 having an opening 350 and a lid 332. The opening 350 is an opening for inserting an objective lens. Specifically, the opening 350 is provided at a position facing the film surface 23 f with the supply-side channel 61 interposed therebetween. The lid portion 332 includes a rectangular plate-shaped ceiling portion 333 and a cylindrical body portion 334. The body portion 334 is a portion that is fitted into the opening portion 350. Through holes 336 for allowing the screws 335 to pass therethrough are formed at the four corners of the ceiling portion 333. The container body 331 is formed with a screw hole 337 that is screwed with the screw 335. The position of the screw hole 337 corresponds to the position of the through hole 336. According to the container 330, the screw 335 and the screw hole 337 are screwed together via the ceiling part 333, so that the lid part 332 is screwed into the opening 350, thereby ensuring the pressure resistance of the container 330. . In addition, the objective lens can be inserted into the opening 350 by removing the lid 332 when observing the film fouling. In addition, in order to assist sealing of the opening part 350 by the cover part 332, you may interpose an O-ring when these screw together.

  Further, in the present embodiment, in a state where the lid portion 332 is attached to the opening portion 350, the end surface on the trunk portion 334 side (the end surface in contact with the supply-side flow path 61) 334s and the inner surface 331s of the container body 331 in the lid portion 332 Is the same. The opening 350 may be provided at a position on the upper side when the submodule 302 is installed, for example.

(Other embodiments)
Submodules other than those described above may be used as the submodule. For example, you may use the submodule which has the aspect which ensures the pressure resistance of a container with the fitting force obtained by fitting a cover part in an opening part.

  According to the present invention, the membrane fouling of the separation membrane module can be properly grasped.

DESCRIPTION OF SYMBOLS 1 Separation membrane module 2,102,202,302 Submodule 3 Measuring instrument 4 Staining agent tank 5,7 Valve 6 Pressure pump 10 Membrane separation apparatus 11 1st flow path 12 2nd flow path 22 Deposited material 23 Fouling Separation membrane for evaluation 23f Membrane surface 23b Membrane back surface 24 Permeate side channel material 27 Inflow port 28 Concentrated water outflow port 29 Permeate outflow port 30, 130, 230, 330 Container 31, 131, 231, 331 Container body 31s, 42s, 231si, 231so, 242asi, 242aso, 242bsi, 242bso, 331s, 334s End surface 32, 132, 232a, 232b, 332 Lid 41, 241a, 241b Female screw part 42, 242a, 242b Male screw part 50, 150, 250a, 250b , 350 Opening 61 Supply side channel 62 Permeation side channel 14 Slide grooves 145, 155 open face 156 interface 333 ceiling 334 barrel 335 screw 336 through hole 337 threaded holes

Claims (13)

For a fouling evaluation in which a separation membrane module including a separation membrane that permeates a supply fluid to generate a permeation fluid and a sampling fluid that is a fluid flowing through a branch path branched from a flow path connected to the separation membrane module A membrane separation device comprising a submodule comprising a separation membrane,
The sub-module includes a container that contains the separation membrane for fouling evaluation, a supply-side flow path through which the sampling fluid introduced into the container passes and is in contact with the membrane surface of the separation membrane for fouling evaluation, A permeation-side channel disposed on the opposite side of the supply-side channel via the fouling evaluation separation membrane,
The container includes a container main body having an opening, and a lid part detachably attached to the opening.
The opening is provided at a position facing the membrane surface across the supply-side flow path,
Membrane separator.   The membrane separation device according to claim 1, wherein the lid is attached to the opening so as not to drop from the opening when the internal pressure of the submodule reaches 1.5 MPa.   The membrane separation device according to claim 1 or 2, wherein the lid is screwed into the opening.   The membrane separation apparatus as described in any one of Claims 1-3 provided with the flow volume adjustment means which adjusts the flow volume of the said sampling fluid introduce | transduced into the said submodule.   The said lid | cover part is a membrane separator as described in any one of Claims 1-4 which is transparent.   The membrane separation apparatus according to any one of claims 1 to 5, wherein a deposition material is provided on the membrane surface of the separation membrane for fouling evaluation. A membrane fouling measurement method using the membrane separation device according to any one of claims 1 to 6 and a measuring instrument having an objective lens,
An insertion step of removing the lid from the opening and inserting the objective lens into the opening;
A state of measuring the state of the film surface by the measuring instrument with the objective lens inserted into the opening.
Method for measuring membrane fouling. The membrane separation device further includes a flow rate adjusting means for adjusting the flow rate of the sampling fluid introduced into the submodule,
The membrane fouling measurement method according to claim 7, further comprising a flow rate adjusting step of reducing the flow rate of the sampling fluid introduced into the submodule by the flow rate adjusting means before the inserting step. In the membrane separator, a deposition material is provided on the membrane surface of the separation membrane for fouling evaluation,
Comparative evaluation for comparing and evaluating film fouling in the vicinity of the deposition material on the membrane surface of the separation film for fouling evaluation and film fouling in a portion other than the vicinity of the deposition material on the membrane surface after the measurement step Further comprising a step,
The method for measuring membrane fouling according to claim 7 or 8.   The film fouling measurement method according to any one of claims 7 to 9, wherein in the measurement step, the reflected light intensity from the film surface of the submodule is measured by the measuring device. The supply fluid and the sampling fluid are liquid;
The objective lens is an immersion lens;
In the inserting step, the immersion lens is inserted into the opening so that the immersion lens is immersed in the sampling fluid,
The measurement method of the film | membrane fouling as described in any one of Claims 7-10 which measures the said film | membrane surface in the said measurement process in the state which immersed the said immersion lens in the said sampling fluid. An operation method of the membrane separation device according to any one of claims 1 to 6,
The membrane separation apparatus further comprises data processing means for processing electronic data obtained by measurement of the membrane surface of the separation membrane for fouling evaluation,
A method for operating a membrane separation apparatus, wherein the electronic data is stored, analyzed or transmitted using the data processing means. A fluid that flows along a branch path that branches from a flow path connected to the separation membrane module and that forms a membrane separation apparatus alongside a separation membrane module that includes a separation membrane that permeates a supply fluid to generate a permeation fluid. A sub-module including a separation membrane for fouling evaluation that allows a sampling fluid to pass therethrough,
A container containing the separation membrane for fouling evaluation; a supply-side flow path through which the sampling fluid introduced into the container passes, and a membrane surface of the separation membrane for fouling evaluation is in contact; and for fouling evaluation A permeation side flow path disposed on the opposite side of the supply side flow path through a separation membrane,
The container includes a container main body having an opening, and a lid part detachably attached to the opening.
The opening is provided at a position facing the membrane surface across the supply-side flow path,
Submodule.

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