WO2012086763A1 - 分離膜モジュールの滅菌方法、滅菌用装置および化学品製造用装置 - Google Patents
分離膜モジュールの滅菌方法、滅菌用装置および化学品製造用装置 Download PDFInfo
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- WO2012086763A1 WO2012086763A1 PCT/JP2011/079827 JP2011079827W WO2012086763A1 WO 2012086763 A1 WO2012086763 A1 WO 2012086763A1 JP 2011079827 W JP2011079827 W JP 2011079827W WO 2012086763 A1 WO2012086763 A1 WO 2012086763A1
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- separation membrane
- membrane module
- temperature
- sterilization
- water
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2/00—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
- A61L2/02—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor using physical phenomena
- A61L2/04—Heat
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D65/00—Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
- B01D65/02—Membrane cleaning or sterilisation ; Membrane regeneration
- B01D65/022—Membrane sterilisation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/024—Oxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2321/00—Details relating to membrane cleaning, regeneration, sterilization or to the prevention of fouling
- B01D2321/08—Use of hot water or water vapor
Definitions
- the present invention relates to a sterilization method for a separation membrane module provided with a separation membrane containing at least ceramics, a sterilization apparatus for performing the sterilization method for the separation membrane module, and an apparatus for manufacturing chemical products.
- Ceramic membranes are solid and liquid in terms of being excellent in physical strength and chemical strength as compared with organic polymer membranes and enabling precise control of pore diameter. It can be suitably used for purposes such as separation. In particular, since it does not easily deteriorate even when cleaning with strong acid or strong alkali is performed, it can be suitably used for the treatment of a liquid containing a large amount of turbidity, which frequently cleans the separation membrane. As an example of a stock solution containing a lot of turbidity, a solution containing a food such as a dairy product, a solution of a pharmaceutical, and the like can be given.
- Patent Document 1 proposes a technique for performing continuous fermentation of lactic acid bacteria using a ceramic membrane as a separation membrane. In the production of chemical products by continuous fermentation, it is required to perform culturing in a state where necessary portions in the apparatus are sterilized to prevent contamination (contamination). However, Patent Document 1 merely describes that heat sterilization is possible because the separation membrane is a ceramic membrane, and there is no mention of specific means.
- sterilization methods include flame sterilization, steam sterilization, hot water sterilization, ultraviolet sterilization, gamma ray sterilization, and gas sterilization.
- flame sterilization, ultraviolet sterilization, and gamma ray sterilization are unsuitable as sterilization methods for separation membrane modules because it is difficult to sterilize ceramic membranes uniformly.
- gas sterilization in which ethylene oxide gas or the like is introduced into the separation membrane module may cause the gas to remain in the separation membrane module and may affect the properties of the filtrate. As inappropriate. Therefore, steam sterilization and warm water sterilization are preferably used as the method for sterilizing the ceramic membrane.
- Patent Document 2 introduces a technology for continuous fermentation of brewed liquor using a ceramic membrane. It is described that a ceramic film is used after steam sterilization in order to prevent contamination of germs in the brewed sake. However, although the ceramic film has a high heat-resistant temperature, it has a drawback that it is vulnerable to rapid temperature changes. If it is suddenly brought into contact with high-temperature steam used for sterilization, the ceramic film may break or There was a problem that the fractionation performance of the membrane was impaired.
- the present invention has been made in view of the above, and provides a sterilization method for a separation membrane module that enables sterilization while suppressing damage to the separation membrane module including a separation membrane containing at least ceramics, and the sterilization method. It is an object of the present invention to provide an apparatus for sterilization and an apparatus for producing a chemical product for performing the method.
- the separation membrane module sterilization method of the present invention is a separation membrane module that sterilizes a separation membrane module including a separation membrane containing at least ceramics using sterilization water.
- a sterilization method wherein the sterilizing water is supplied to the separation membrane module, and the temperature and pressure of the supplied sterilizing water are controlled so that the temperature of the separation membrane module rises at 6.0 ° C. or less per minute.
- the separation membrane module sterilization method of the present invention includes a temperature measurement step of measuring the temperature T of the separation membrane module, and a temperature Tw of the sterilization water T
- the temperature measurement step measures the temperature on the primary side of the separation membrane module on the side to which the stock solution to be treated is supplied as the temperature T.
- the sterilization water is supplied to the primary side of the separation membrane module.
- the separation membrane module sterilization method of the present invention in the above invention, in the temperature measurement step, as the temperature T, one of the temperatures T on the primary side and the secondary side of the separation membrane module is used.
- the measurement and the temperature raising step and the sterilization step are characterized in that the sterilizing water is supplied to a primary side and a secondary side of the separation membrane module.
- the separation membrane module sterilization method of the present invention is the separation membrane module sterilization method according to the above invention, wherein the separation membrane module including a separation membrane containing at least ceramics is sterilized using sterilization water,
- the supply of the sterilizing water is started on the primary side where the stock solution to be treated of the membrane module is supplied and on the secondary side where the filtrate after treatment is collected, and the primary side and the secondary side of the separation membrane module A temperature increasing step of controlling the temperature and pressure of the supplied sterilizing water so that the temperature of the separation membrane module is raised to a predetermined sterilization temperature, And sterilizing the separation membrane module at a predetermined temperature for a predetermined time after the primary side and the secondary side of the membrane module reach a predetermined sterilization temperature.
- the separation membrane module sterilization method of the present invention is supplied to the primary side of the separation membrane module, the temperature measuring step for measuring the temperature T1 on the primary side and the temperature T2 on the secondary side of the separation membrane module.
- the sterilization water temperature Tw1 and the sterilization water temperature Tw2 supplied to the secondary side of the separation membrane module are expressed as
- the initial temperature control step of controlling T1 and / or T2 and / or Tw is performed, and the temperature raising step is performed after the initial temperature control step.
- the separation membrane module sterilization method of the present invention is the cooling method for cooling the separation membrane module in the above invention, so that the temperature of the separation membrane module drops at 6.0 ° C. or less after the sterilization step. Including a process.
- the sterilization apparatus of the present invention is a sterilization apparatus for sterilizing a separation membrane module including a separation membrane containing at least ceramics, and includes a temperature measuring means for measuring the temperature of the separation membrane module, and a temperature and a pressure.
- a sterilization water control unit that generates controlled gas-phase or liquid-phase sterilization water and supplies the sterilization water module to the separation membrane module, wherein the sterilization water control unit has a temperature of the separation membrane module of 6.0 per minute.
- the sterilizing water is supplied so as to rise and fall at a temperature of less than or equal to ° C.
- the chemical product production apparatus of the present invention includes a separation membrane module including a separation membrane containing at least ceramics, the sterilization device described above, and fermenting and culturing the fermentation raw material with microorganisms, thereby chemically treating the fermentation raw material. It is provided with the fermenter converted into the fermented liquor containing goods, and the fermented liquid circulation means which sends fermented liquid from the said fermenter to the said separation membrane module.
- the present invention by performing the separation membrane module sterilization method described above, in the separation membrane module provided with the ceramic membrane, the temperature difference with the sterilization water at the start of sterilization is suppressed, Since the temperature change is kept moderate, it is possible to suppress the breakage of the ceramic film accompanying the rapid temperature change.
- FIG. 1 is a schematic diagram of an apparatus for sterilizing a separation membrane module according to Embodiment 1 of the present invention.
- FIG. 2 is a diagram showing an aspect of the separation membrane module used in Embodiment 1 of the present invention.
- 3 is a) a sectional view and b) a side view of one embodiment of the monolith membrane in the separation membrane module of FIG. 2.
- FIG. 4 is a flowchart of the sterilization process according to the first embodiment.
- FIG. 5 is a schematic diagram of an apparatus for sterilizing a separation membrane module according to Modification 1 of Embodiment 1 of the present invention.
- FIG. 6 is a flowchart of sterilization processing according to the second modification of the first embodiment.
- FIG. 1 is a schematic diagram of an apparatus for sterilizing a separation membrane module according to Embodiment 1 of the present invention.
- FIG. 2 is a diagram showing an aspect of the separation membrane module used in Embodiment 1 of the present invention.
- 3 is a) a sectional
- FIG. 7 is a schematic diagram of an apparatus for sterilizing a separation membrane module according to Embodiment 2 of the present invention.
- FIG. 8 is a flowchart of the sterilization process according to the second embodiment.
- FIG. 9 is a flowchart of the sterilization process according to the first modification of the second embodiment.
- FIG. 10 is a schematic diagram of an apparatus for sterilizing a separation membrane module according to Modification 2 of Embodiment 2 of the present invention.
- FIG. 11 is a schematic diagram of an apparatus for sterilizing a separation membrane module according to Modification 3 of Embodiment 2 of the present invention.
- FIG. 12 is a schematic diagram of a chemical product manufacturing apparatus according to Embodiment 3 of the present invention.
- FIG. 1 is a schematic view for illustrating an apparatus for sterilization of a separation membrane module according to Embodiment 1 of the present invention.
- the sterilization apparatus 2 sterilizes the separation membrane module 1 by flowing sterilization water to the primary side of the separation membrane module 1 having a ceramic membrane.
- the sterilization apparatus 2 includes a sterilization water control unit 3, a sterilization water supply line 4, a temperature measurement unit 5, and a valve 6.
- the primary side of the sterilization water control unit 3 and the separation membrane module 1 are communicated with each other by a sterilization water supply line 4, and the temperature measurement unit 5 is provided at a position where the temperature of the primary side of the separation membrane module 1 can be measured.
- the valve 6 is provided between the sterilization water control unit 3 and the temperature measurement unit 5.
- the temperature information obtained by the temperature measurement unit 5 is transmitted to the sterilization water control unit 3, and based on the temperature information, the sterilization water control unit 3 controls the temperature of the sterilization water.
- the sterilization water supplied from the sterilization apparatus 2 to the separation membrane module 1 is discharged out of the separation membrane module 1 via the sterilization water discharge line 7.
- the side in contact with the undiluted solution to be processed in the separation membrane module 1 is called a primary side
- the side in contact with the filtrate after processing is called a secondary side.
- FIG. 2 is a diagram showing an aspect of the separation membrane module 1 used in Embodiment 1 of the present invention.
- 3 is a cross-sectional view and b) side view of the monolith membrane in the separation membrane module 1 of FIG.
- the separation membrane module 1 includes a ceramic membrane 10 and a module container 11, and the O-ring 12 is separated so that the primary side and the secondary side of the ceramic membrane 10 are hermetically and liquid-tightly separated.
- a seal member as exemplified in FIG.
- the module container 11 is supplied with a raw solution to be processed, or a raw liquid supply port / concentrated liquid discharge port 13 a for discharging the concentrated liquid discharged from the filtrate in the separation membrane module 1, and in the separation membrane module 1.
- a filtrate discharge port / backwash solution supply port 13b for discharging the filtered filtrate or supplying a backwash solution for cleaning the ceramic film 10 is provided.
- the number of ceramic membranes 10 filled in one separation membrane module 1 is one or more.
- the inner diameter of the module container 11 may be determined based on the number of filled ceramic films 10 or the like, it can be said that it is preferably 300 mm or less in consideration of the weight and ease of handling of the module container 11.
- a partition, a dish, or the like may be provided as appropriate so that the ceramic films 10 do not contact each other.
- the module container 11 of the separation membrane module 1 is preferably made of a material that can withstand repeated sterilization treatment, that is, contact with high-temperature water or water vapor, and examples include stainless steel, a resin having heat resistance, and an inorganic material. Is done.
- the method for performing the sealing is not particularly limited.
- a method of sealing using a sealant and a method of directly placing the O-ring 12 between the ceramic film 10 and the module container 11 are conceivable.
- an eye plate (not shown) is provided in the separation membrane module 1
- an O-ring is provided between the eye plate and the ceramic membrane 10.
- a method of arranging 12 is conceivable.
- organic adhesives such as epoxy resins and urethane resins and inorganic adhesives such as ceramic adhesives
- inorganic adhesives such as ceramic adhesives
- the inorganic adhesive is excellent in heat resistance and is preferably used because it has good adhesion to the ceramic film 10.
- inorganic adhesives are made by adding additives such as alumina, zirconia, and magnesia to paste that vitrifies by heating. The difference in expansion coefficient can be reduced. Accordingly, the ceramic film 10 and the module container 11 are less likely to be peeled off due to thermal expansion and contraction due to heating and cooling with sterilizing water, which is preferable as a means for bonding the ceramic film 10 and the module container 11.
- the sterilization temperature of the separation membrane module 1 is usually 121 ° C. or higher, and silicone rubber, fluorine rubber, ethylene / propylene rubber (EPM), ethylene / propylene / diene rubber (EPDM), etc. can be exemplified as preferable materials. .
- the sterilization temperature may be higher and higher pressure, so it is necessary to select the material of the O-ring 12 in consideration of this point. Is done.
- the definition of ceramics in the present invention includes a metal oxide and is baked and hardened by heat treatment at a high temperature.
- the metal oxide include alumina, magnesia, titania, zirconia and the like.
- the separation membrane may be formed of only a metal oxide, and may include silica, silicon carbide, mullite, cordierite, or the like, which is a compound of silica and a metal oxide.
- Components other than the ceramics forming the separation membrane are not particularly limited as long as they can form a porous body as the separation membrane. Examples include metal, resin, glass, etc. However, since most of the resins have sintering conditions higher than the melting point, it is preferable to use metal or glass.
- the ceramic membrane 10 in the separation membrane module 1 used in Embodiment 1 is a monolith membrane as shown in FIGS.
- the ceramic film 10 By using the ceramic film 10 as a monolith film, the efficiency of filling the ceramic film 10 into the module container 11 is improved.
- a flat film, a tubular film, or the like can be used as the ceramic film 10.
- the ceramic film 10 which is a monolith film is provided with a plurality of through holes 21 in the longitudinal direction in a ceramic base material 20 containing at least ceramics. Since the monolith membrane has such a structure, the flow area per monolith membrane can be increased, which is advantageous in terms of both ease of forming the separation membrane module 1 and securing the flow area.
- the ceramic film 10 in which the separation functional layer 22 is laminated on the end face of the ceramic substrate 20 and the surface of the through hole 21 is also preferable.
- the surface pore diameter of the ceramic film 10 can be controlled more precisely, and only the substance to be filtered can be filtered and separated more accurately.
- the separation functional layer 22 also on the end surface of the ceramic substrate 20 it is possible to prevent a problem that a material that should not be filtered is filtered from the end surface of the monolith membrane and mixed into the filtrate. .
- the monolith membrane is provided with one or more water collecting slits 23, and the water collecting holes 24 communicating with the water collecting slits 23 are formed so as to be blocked so that the stock solution does not enter the end face of the ceramic substrate 20. Also good.
- the raw solution to be processed passes through the through hole 21 of the monolith membrane, is filtered through the separation function layer 22, and is collected in the water collecting hole 24 as a filtrate.
- the water collection hole 24 inside the monolith membrane is communicated with an external water collection slit 23 and a water collection slit communication hole 25, and the filtrate passes through the water collection hole 24 and the water collection slit 23, and then the secondary of the separation membrane module 1. Liquid is collected on the side.
- the separation membrane area per unit volume is reduced, but until the filtrate is filtered to the secondary side through the separation membrane from each through-hole. Is shorter than that without slits, so that the liquid flow resistance can be reduced.
- the quantity ratio between the through hole 21 and the water collecting hole 24 is not particularly specified.
- the porosity of the ceramic film 10 is not particularly specified, but if it is too low, the filtration efficiency will deteriorate, and if it is too high, the strength will decrease. In order to achieve both the filtration efficiency and the strength of the separation membrane and to have durability that can be repeatedly sterilized, it is preferably 20% or more and 60% or less.
- the wet membrane refers to a membrane in which pure water is filled in the pores but no pure water is contained in the hollow portion, and the dry membrane does not contain pure water in the pores.
- the membrane volume is determined by subtracting the volume occupied by the hollow portion from the volume occupied by the separation membrane.
- the pure water permeation performance of the ceramic membrane 10 may be set to an appropriate value from the required amount of filtrate and the properties of the processing stock solution.
- the average pore diameter of the ceramic film 10 may also be determined appropriately from the properties of the processing stock solution and the required properties of the filtrate.
- the ceramic film 10 used in the first embodiment is obtained by laminating one separation functional layer 22 on the ceramic substrate 20, but the separation functional layer 22 may be laminated by two or more layers.
- the separation functional layer 22 may be laminated by two or more layers.
- By laminating two or more separation functional layers having different pore diameters not only the average pore diameter of the ceramic membrane 10 as a whole is adjusted, but also a hydrophilic layer is provided on the surface of the separation membrane to improve stain resistance. Etc. are also possible.
- the thickness of the separation functional layer 22 is not particularly limited. However, when the thickness is less than 1 ⁇ m, the strength is not preferable because it is insufficient, and when it exceeds 200 ⁇ m, the water permeability is deteriorated.
- the thickness is preferably 1 ⁇ m or more and 200 ⁇ m or less.
- the separation functional layer 22 of the ceramic film 10 is preferably formed of the above-mentioned alumina, magnesia, titania, zirconia, etc., and titania can be particularly preferably used because it is particularly excellent in stain resistance.
- the monolithic ceramic substrate 20 preferably has a circular or polygonal cross-sectional shape perpendicular to the longitudinal direction. Therefore, regular polygons are particularly preferable, and among them, regular polygons that can be spread without gaps with one type of figure such as regular triangle, square, regular hexagon, and the like are more preferable. Further, the outer diameter of the ceramic substrate 20 is preferably 10 mm or more and 300 mm or less, more preferably 20 mm or more and 250 mm or less, and further preferably 30 mm or more and 200 mm or less.
- the ceramic substrate 20 is a polygonal column, if the end surface is a triangle, the diameter of the outer circle of the end surface is the outer diameter, and if the end surface is a polygon other than a triangle, any two vertices are connected.
- the length of the longest line segment is the outer diameter. If the outer diameter of the ceramic substrate 20 is less than 10 mm, the number of through holes that can be formed decreases, and if it exceeds 300 mm, manufacture becomes difficult. Further, the length of the ceramic substrate 20 in the longitudinal direction is preferably 20 mm or more and 2000 mm or less, more preferably 30 mm or more and 1700 mm or less, and further preferably 40 mm or more and 1500 mm or less. If the length of the ceramic substrate 20 in the longitudinal direction is less than 20 mm, the film area per one ceramic film 10 becomes small, and if it exceeds 2000 mm, manufacture and handling become difficult.
- the number of through holes 21 (including the number of water collecting holes 24) provided in the ceramic substrate 20 of the monolithic membrane is preferably 10 or more and 5000 or less, 30 More preferably, no less than 2000 and no more. If the number of through-holes 21 exceeds 5000, it is difficult to manufacture and the strength is lowered, which is not preferable.
- the shape of the through-hole 21 can be suitably selected from shapes such as a circle, an ellipse, a polygon and a star, and the equivalent diameter is preferably 0.5 mm or more and 5 mm or less.
- the equivalent diameter of the through hole 21 is the inner diameter (inner diameter) when the cross section of the through hole 21 is a circle, and the same area as the cross section when the cross section of the through hole 21 is not a circle.
- sterilization is performed by the method for sterilizing a separation membrane module according to the first embodiment before the filtration treatment is started or at any stage during the filtration treatment. It can be carried out.
- sterilizing the separation membrane module during the filtration treatment it is preferable to sterilize after stopping the supply of the processing stock solution and washing the inside of the separation membrane module.
- Sterilization water may be used for cleaning the separation membrane module, and the temperature of the sterilization water is preferably controlled according to a temperature control method described later.
- FIG. 4 is a flowchart for explaining the sterilization process of the separation membrane module 1 according to the first embodiment.
- the temperature and the sterilization water control unit 3 adjust the temperature and the temperature change rate ⁇ T1 on the primary side of the separation membrane module 1 to 6.0 ° C. or less per minute.
- the pressure-controlled sterilizing water is supplied to the primary side of the separation membrane module 1, and the temperature of the ceramic membrane 10 of the separation membrane module 1 is raised to a predetermined sterilization temperature (step S1).
- the inventors of the present invention have found that the effect of suppressing the deterioration of the ceramic film 10 is high if the temperature change rate ⁇ T1 is 6.0 ° C. or less per minute.
- the temperature information is fed back to the sterilizing water control unit 3, and sterilization is performed so that ⁇ T1 is 6.0 ° C. or less per minute.
- ⁇ T1 is 6.0 ° C. or less per minute.
- the lower limit value of the temperature change rate ⁇ T1 is not particularly limited. However, if ⁇ T1 is too small, problems such as too much time for sterilization of the ceramic film 10 and difficulty in controlling ⁇ T1 can be considered. Therefore, it is preferable that the temperature of the sterilizing water is controlled in the sterilizing water control unit 3 so that ⁇ T1 is 0.01 ° C. or more per minute.
- ⁇ T1 at the temperature rise (and the temperature fall) of the separation membrane module 1 may be controlled to be constant or may be controlled to vary. Even when ⁇ T1 is varied, the instantaneous temperature change rate of the separation membrane module 1 is required to be controlled to correspond to 6.0 ° C. or less per minute.
- a sterilization water supply line 4 is provided with a pressure measurement unit, and pressure data measured by the pressure measurement unit is sent to the sterilization water control unit 3 for sterilization.
- a method of feeding back to the pressure control in the water controller 3 is preferably used.
- the sterilizing water supplied to the separation membrane module 1 refers to sterilized water that takes either a liquid phase state or a gas phase state and is controlled in temperature and pressure. It is preferable to use ion-exchanged water, reverse osmosis membrane permeated water, distilled water, or water having the same level of cleanliness as the sterilizing water.
- the sterilization water control unit 3 brings the sterilization water into a liquid phase or a gas phase, and controls it to a predetermined temperature and pressure.
- ion-exchanged water, reverse osmosis membrane permeated water, distilled water, etc. are sterilized in advance, and then treated so as to become liquid phase or gas phase water having a predetermined temperature and pressure.
- ion-exchanged water, reverse osmosis membrane permeated water, distilled water, etc. should be treated in advance to become liquid or vapor phase water having a predetermined temperature and pressure, and then sterilized through a sterilizing filter or the like. May be.
- water may be heated with a heater, and a widely known boiler can also be used.
- a method for performing temperature control and pressure control the above-described boiler may be provided with a function, or a heat exchanger, a compressor, a pressure pump, or the like may be provided separately.
- temperature control those applicable not only to heating but also to a cooling step are preferably used.
- the sterilization water whose temperature and pressure are controlled by the sterilization water control unit 3 is supplied to the primary side of the separation membrane module 1 via the sterilization water supply line 4.
- the separation membrane module 1 is set up vertically, and the sterilization apparatus 2 is arranged on the upper portion of the separation membrane module 1 to supply sterilization water from the upper portion.
- the sterilization water is supplied to the separation membrane module 1 mainly in the gas phase state, the drainage generated by the condensation of the sterilization water is discharged vertically downward by supplying the sterilization water from above as in the first embodiment. Further, the retention of drain in the separation membrane module 1 is difficult to occur, and sterilization failure can be prevented.
- the sterilizing device 2 when sterilizing water is supplied to the separation membrane module 1 as a liquid phase, the sterilizing device 2 is arranged so that the sterilizing water is supplied from below the separation membrane module 1 as shown in FIG. Since the gas existing in the separation membrane module 1 can be pushed upward by the sterilizing water and the gas does not easily stay in the separation membrane module 1, sterilization defects are less likely to occur, which is preferable.
- the separation membrane module 1 After the separation membrane module 1 reaches a predetermined sterilization temperature, the separation membrane module 1 is sterilized at a predetermined temperature for a predetermined time (step S2).
- the sterilization temperature In sterilization using water vapor, the sterilization temperature is usually 121 ° C. and the sterilization time is 15 to 20 minutes. However, depending on the level of sterilization required for the separation membrane module 1, the sterilization temperature and sterilization time are appropriately set. It may be changed. In order to easily maintain the temperature, it is preferable to continue supplying the sterilization water to the separation membrane module 1, but if the sterilization condition can be satisfied, the supply of the sterilization water may be stopped to perform the sterilization process.
- the temperature of the ceramic membrane 10 of the separation membrane module 1 is cooled to a predetermined temperature while controlling ⁇ T1 to be 6.0 ° C. or less per minute (step S3).
- ⁇ T1 sterilization water whose temperature and pressure are controlled by the sterilization water control unit 3 is supplied to the primary side of the separation membrane module 1, and ⁇ T1 is 6.0 ° C./min. It is preferable to lower T1 as follows.
- the temperature change in the separation membrane module 1 is maintained gently, so that it is possible to suppress the breakage of the ceramic membrane 10 due to the rapid temperature change. It becomes.
- the separation membrane module 1 when the separation membrane module 1 after being used for the filtration treatment is sterilized, turbidity or the like may adhere to the surface and pores, so the separation membrane module 1 is washed and then sterilized. It is preferable to do.
- the separation membrane module 1 may be cleaned with a cleaning solution of about 80 ° C., for example. After such cleaning, the temperature of the separation membrane module is about the same as the temperature of the cleaning solution. Therefore, if sterilization water at normal temperature (20 to 30 ° C.) is supplied to the separation membrane module 1 immediately after that, There is a case where the ceramic film 10 is exposed to an abrupt temperature change due to the supply of water and is damaged.
- FIG. 6 is a flowchart for explaining a sterilization process of the separation membrane module 1 according to the second modification of the first embodiment.
- the temperature T1 on the primary side of the separation membrane module 1 is measured (step S11).
- the temperature measuring unit 5 may be provided so as to communicate with the primary side of the separation membrane module 1, but the temperature on the primary side of the ceramic membrane 10 may be provided. Arrangement so that the measurement unit 5 is in contact is preferable because the temperature on the primary side of the ceramic film 10 can be obtained and a high-precision index for suppressing breakage of the ceramic film 10 is obtained.
- between the temperature Tw of the sterilizing water supplied to the separation membrane module 1 and the primary side temperature T1 of the separation membrane module 1 measured in the temperature measurement step is 30.0 ° C.
- the temperature Tw of the sterilizing water and / or the temperature of the primary side temperature T1 of the separation membrane module 1 are controlled so as to be as follows (step S12).
- step S12 the temperature difference when the sterilizing water and the ceramic membrane 10 in the separation membrane module 1 are in contact with each other is reduced, and damage due to a rapid temperature change of the ceramic membrane 10 can be suppressed.
- is appropriately determined depending on various factors such as the size of the separation membrane module, the volume of the portion to be sterilized, the material of the ceramic membrane 10, the porosity, and the like.
- 0 ° C. is the best in reducing the risk of damage to the ceramic film 10, but if it is difficult to control
- the sterilization water temperature Tw can be controlled by the sterilization water controller 3, it is preferable to control the sterilization water temperature Tw so that
- the sterilizing water controlled to the predetermined temperature Tw by the sterilizing water control unit 3 is supplied to the primary side of the separation membrane module 1 through the sterilizing water supply line 4.
- the supply of the sterilization water to the separation membrane module 1 is started and the separation The sterilizing water whose temperature and pressure are controlled by the sterilizing water control unit 3 is supplied to the primary side of the separation membrane module 1 so that the temperature change rate ⁇ T1 on the primary side of the membrane module 1 is 6.0 ° C. or less per minute.
- the temperature of the ceramic membrane 10 of the separation membrane module 1 is raised to a predetermined sterilization temperature (step S13). After the separation membrane module 1 reaches the predetermined sterilization temperature, the separation membrane module 1 is moved to the predetermined temperature. To sterilize for a predetermined time (step S14).
- the temperature of the ceramic membrane 10 of the separation membrane module 1 is cooled to a predetermined temperature so that ⁇ T1 is 6.0 ° C. or less per minute (step S15).
- the temperature change in the separation membrane module 1 is maintained gently, so that it is possible to suppress the breakage of the ceramic membrane 10 due to the rapid temperature change. It becomes.
- the sterilization water supplied to the primary side of the separation membrane module 1 is discharged from the sterilization water discharge line 7.
- the sterilization apparatus 2 in order to supply sterilization water in the gas phase, the sterilization apparatus 2 is arranged at the upper part of the separation membrane module 1 and the sterilization water discharge line 7 is arranged at the lower part of the separation membrane module 1.
- the sterilization apparatus 2A is disposed in the lower part of the separation membrane module 1 and the sterilization water discharge line 7 is disposed in the upper part of the separation membrane module 1, as shown in FIG. It is preferable because the discharge efficiency of water can be improved.
- the sterilizing water when the sterilizing water is discharged from the separation membrane module 1, it may be returned to the sterilizing water control unit 3 again. Since the sterilizing water is continuously supplied to the separation membrane module 1, it is preferable to return the sterilizing water to the sterilizing water control unit 3 because energy required for controlling the temperature and pressure of the sterilizing water can be reduced.
- the sterilization water discharge line 7 of the separation membrane module 1 and the sterilization water control unit 3 are connected by a sterilization water return line (not shown) so that the sterilization water can be reused. It becomes possible.
- a filter may be provided in the middle of the sterilizing water return line so that the sterilizing water is removed and then returned to the sterilizing water control unit 3. Further, assuming that the sterilization water to be discharged has high turbidity, the sterilization water discharge line 7 and the sterilization water return line are provided side by side, and when the sterilization water to be discharged has high turbidity, When the turbidity of the discharged sterilizing water is low turbidity, it may be returned to the sterilizing water control unit 3 via the sterilizing water return line.
- the turbidity of the sterilized water discharged is measured with a turbidimeter, the obtained turbidity data is fed back to the solenoid valve, and the sterilization water discharge line and the sterilization water return line are switched by opening and closing the solenoid valve. Used for.
- the temperature T1 on the primary side of the separation membrane module 1 is measured. If T1 cannot be directly measured, a ceramic membrane 10 having the same specifications as the measurement target is prepared and separated from T1. A correlation between the temperature To at an arbitrary point on the outer surface of the membrane module 1 is examined in advance, and when actually sterilizing, a method may be used in which To is measured and T1 is calculated backward from the correlation. Alternatively, water having a constant temperature may be passed through the separation membrane module 1, the separation membrane module 1 may be set to a constant temperature, and the temperature T of the constant temperature water may be regarded as the temperature T of the separation membrane module 1.
- FIG. 7 is a schematic diagram of an apparatus for sterilizing a separation membrane module according to Embodiment 2 of the present invention.
- the sterilization apparatus 2B includes sterilization water controllers 3a and 3b for supplying sterilization water with controlled temperature and pressure to the primary side and the secondary side of the separation membrane module 1, respectively, Temperature measuring units 5a and 5b that measure the temperature on the secondary side, and primary and secondary sterilization water supply lines 4a and 4b of the separation membrane module 1 are provided.
- FIG. 8 is a flowchart for explaining the sterilization process of the separation membrane module 1 according to the second embodiment.
- the temperature is controlled by the sterilization water control units 3a and 3b so that the primary temperature change rate ⁇ T1 and the secondary temperature change rate ⁇ T2 of the separation membrane module 1 are 6.0 ° C. or less per minute.
- the pressure-controlled sterilizing water is supplied to the primary side and the secondary side of the separation membrane module 1, and the temperature of the ceramic membrane 10 of the separation membrane module 1 is raised to a predetermined sterilization temperature (step S21).
- ⁇ T1 and ⁇ T2 of the ceramic film 10 may be controlled independently, ⁇ T1 is set so that
- ⁇ T2 are preferably controlled.
- the separation membrane module 1 After the separation membrane module 1 reaches a predetermined sterilization temperature, the separation membrane module 1 is sterilized at a predetermined temperature for a predetermined time (step S22). In order to maintain the separation membrane module 1 at a predetermined temperature, it is preferable to sterilize by supplying sterilization water having a predetermined temperature and a predetermined pressure to the primary side and the secondary side of the separation membrane module 1.
- the temperature of the ceramic membrane 10 of the separation membrane module 1 is cooled to a predetermined temperature so that ⁇ T1 and ⁇ T2 of the separation membrane module are 6.0 ° C. or less per minute (step S23).
- sterilization water whose temperature and pressure are controlled by the sterilization water controllers 3a and 3b is supplied to the primary side and the secondary side of the separation membrane module 1 to cool the separation membrane module 1. Is preferred.
- sterilization water is supplied to each of the primary side and the secondary side of the separation membrane module, and the ceramic membrane 10 is damaged by performing sterilization while bringing the temperature of the entire ceramic membrane 10 close to uniform. Concerns can be further suppressed.
- FIG. 9 is a flowchart for explaining sterilization processing of the separation membrane module 1 according to the first modification of the second embodiment.
- the temperatures T1 and T2 on the primary side and the secondary side of the separation membrane module 1 are measured (step S31), the temperature Tw1 of sterilization water supplied to the primary side of the separation membrane module 1, and the separation membrane
- the temperature is controlled (step S32).
- the temperature difference when the sterilizing water and the ceramic membrane 10 in the separation membrane module 1 are in contact with each other is reduced, and damage due to a rapid temperature change of the ceramic membrane 10 can be suppressed.
- T1 or T2 of the separation membrane module 1 is measured by either one of the temperature measuring units 5a and 5b, and
- the sterilizing water controlled to the predetermined temperatures Tw1 and Tw2 by the sterilizing water control units 3a and 3b is supplied to the primary side and the secondary side of the separation membrane module 1 via the sterilizing water supply lines 4a and 4b and the valves 6a and 6b. Supplied respectively.
- the temperature Tw1 and Tw2 of the sterilizing water and the temperature T1 and / or T2 on the primary side of the separation membrane module 1 are
- the supply of sterilizing water to the separation membrane module 1 is started, and the sterilizing water whose temperature and pressure are controlled by the sterilizing water control units 3a and 3b so that ⁇ T1 and ⁇ T2 are 6.0 ° C. or less per minute.
- the separation membrane module 1 After the separation membrane module 1 reaches a predetermined sterilization temperature, the separation membrane module 1 is sterilized at a predetermined temperature for a predetermined time (step S34). After the sterilization process is finished, ⁇ T1 and ⁇ T2 of the separation membrane module are changed every minute. The temperature of the ceramic membrane 10 of the separation membrane module 1 is cooled to a predetermined temperature so as to be 6.0 ° C. or lower (step S35).
- FIG. 11 is a schematic diagram of an apparatus for sterilizing a separation membrane module according to Modification 3 of Embodiment 2 of the present invention.
- the sterilization apparatus 2D supplies sterilization water whose temperature and pressure are adjusted to the primary side of the separation membrane module 1.
- sterilization water discharge lines 7a and 7b are provided, respectively.
- a sterilization water supply pump 8 is installed between the sterilization water control unit 3 and the valve 6.
- the sterilization water When the sterilization water is supplied from the sterilization apparatus 2D to the primary side in the separation membrane module 1, the sterilization water is discharged out of the system through the sterilization water discharge line 7a. Further, the sterilization water supplied to the primary side is pressurized by driving the sterilization water supply pump 8, and the sterilization water is filtered to the secondary side by the pressure. The sterilizing water filtered to the secondary side is discharged out of the system through the sterilizing water discharge line 7b.
- sterilization water is supplied to the primary side of the separation membrane module 1.
- T2 of the separation membrane module 1 is measured and sterilization water is supplied to the secondary side of the separation membrane module 1, the primary side and the secondary side of the following examples may be exchanged.
- the sterilization water When the sterilization water is in a liquid phase, the sterilization water may be supplied so that a pressure necessary for filtration is applied. In this case, before supplying sterilization water, measure at least the temperature T1 on the primary side of the separation membrane module 1 and control Tw so that
- sterilization water is supplied to the primary side, and the supplied sterilization water is supplied to the secondary side. It is preferable to continue the transmission.
- the temperature lowering process after holding for a predetermined time also follows the sterilization method described above.
- the gas phase sterilizing water may be used in either a saturated state or an unsaturated state.
- sterilization water permeates from the primary side to the secondary side of the separation membrane module 1 when a pressure of about 400 kPa is applied. This corresponds to a saturated water vapor pressure of water vapor of about 145 ° C.
- the ceramic membrane 10 When vapor-phase and saturated sterilization water is allowed to permeate through the ceramic membrane 10, the ceramic membrane 10 is heated in advance while supplying the sterilization water to the primary side and the secondary side of the separation membrane module 1 in advance.
- the sterilizing water supplied for raising the temperature may be in the gas phase or the liquid phase, but it is preferable to supply the sterilizing water in the gas phase because the preferred mode of piping differs between the gas phase and the liquid phase.
- the initial temperature and the rate of temperature change of the sterilization water are controlled according to the sterilization method in which the sterilization water is supplied to both the primary side and the secondary side.
- the sterilization water is supplied only to the primary side of the separation membrane module 1 and 2 from the primary side of the ceramic membrane 10. What is necessary is just to permeate
- FIG. 10 is a schematic diagram of a chemical product manufacturing apparatus according to Embodiment 3 of the present invention.
- the chemical product manufacturing apparatus 200 includes a separation membrane module 1 having a separation membrane containing ceramics, a sterilization device 2C according to the first modification of the second embodiment, and a chemical raw material by fermentation fermentation of microorganisms.
- a fermenter 100 that performs conversion into a fermented liquid, and a circulation pump 101 that is a fermented liquid circulating means for feeding the fermented liquid from the fermenter 100 to the separation membrane module 1 are provided.
- the chemical product manufacturing apparatus 200 manufactures a chemical product by fermentation in the fermenter 100, and continuously filtrates the unfiltered solution to the fermenter 100 while filtering the fermented solution containing the manufactured chemical product through the separation membrane module 1. It is a continuous fermentation apparatus that performs fermentation.
- the chemical product manufacturing apparatus 200 is connected with a sterilization apparatus 2C for supplying sterilization water to the primary side and the secondary side upper part of the separation membrane module 1, respectively. It is also possible to sterilize the separation membrane module 1 by connecting 2B or the like.
- the sterilization of the separation membrane module 1 may be performed by the other method described above in addition to the method of the illustrated embodiment 2.
- the system of the chemical product manufacturing apparatus 200 other than the separation membrane module 1 can be sterilized by steam sterilization or hot water sterilization.
- a valve (not shown) or the like is provided between the separation membrane module 1 and other portions so that water vapor or hot water can be shut off, and control is performed so that the ceramic membrane 10 does not rapidly change in temperature. preferable.
- the sterilization treatment is performed only before the start of continuous fermentation, and is not performed during the continuous fermentation.
- the production of chemical products by continuous fermentation is started.
- the medium is supplied to the fermenter 100 by the medium supply pump 107 as necessary, and the fermenter in the fermenter 100 is stirred by the stirring device 103 as necessary.
- the neutralizing agent is supplied by the pH sensor / control device 104 and the neutralizing agent supply pump 108 to adjust the pH of the fermentation broth, and if necessary, the fermenter gas supply device 115 By supplying gas, it is performed while maintaining high productivity.
- the internal pressure in the fermenter 100 may increase.
- the inside of the fermenter 100 is preferably a positive pressure because the supplied gas is easily dissolved in the fermentation broth, but if it is an excessive positive pressure, the fermenter Since 100 is damaged, the internal pressure is preferably controlled by the fermenter pressure adjustment valve 116 and the fermenter pressure gauge 117.
- the fermented liquid in the fermenter 100 is circulated between the separation membrane module 1 and the fermenter 100 by the circulation pump 101.
- the fermentation liquid containing the chemical product is filtered and separated into a filtrate containing the microorganism and the chemical product by the separation membrane module 1 and can be taken out from the chemical product manufacturing apparatus 200.
- the microorganism concentration in the apparatus system can be maintained high, and fermentation production with a high production rate is possible.
- the filtration / separation by the separation membrane module 1 can be carried out by using the pressure of the circulation pump 101 without using any special power.
- the filtration pump 109 is provided and the differential pressure sensor 106 is used.
- the amount of fermentation broth can be adjusted appropriately.
- the transmembrane pressure difference is the pressure difference between the primary side and the secondary side of the ceramic membrane. When the transmembrane pressure difference is outside the above range, clogging of microorganisms and medium components occurs rapidly. In some cases, the permeate flow rate is reduced, causing problems in continuous fermentation.
- the transmembrane pressure may be adjusted by controlling the suction pressure of the filtration pump 109 and the pressure of gas or liquid introduced into the apparatus system.
- the temperature control device 102 can maintain the temperature of the fermenter 100 at a temperature at which microorganisms / cultured cells are activated, so that the microorganism concentration can be maintained high.
- the temperature change rate of the fermentation broth is preferably controlled at 6.0 ° C. or less per minute.
- a backwashing pipe may be provided on the secondary side so that the separation membrane module 1 can be backwashed, and the backwashing liquid 111 may be supplied as necessary.
- Backwashing is a method of removing dirt substances on the film surface by allowing liquid to permeate from the secondary side to the primary side of the ceramic film.
- the backwash valve 112 is closed, the backwash pump 111 is stopped, the filtration valve 110 is opened, the filtration pump 109 is operated, and when the separation membrane filtration is not performed, the filtration valve
- the backwashing can also be performed by closing 110, stopping the filtration pump 109, opening the backwash valve 112, and operating the backwash pump 111.
- the pipe gas supply control valve 113 and the pipe scrubbing gas supply device 114 it is possible to supply gas into the separation membrane module 1 and clean the clogging substances deposited on the surface of the separation membrane.
- the piping gas supply control valve and the piping scrubbing gas supply device are controlled by a timer or a control device as necessary to control the supply of the scrubbing gas. If necessary, the differential pressure of the separation membrane module 1 can be measured by the differential pressure sensor 106, and the piping gas supply control valve can be adjusted as necessary.
- Fermentation raw materials for microorganisms and cultured cells used in continuous fermentation that is, substances before conversion, promote the growth of microorganisms and cultured cells for fermentation and culture, and can produce chemical products that are the desired fermentation products. I just need it.
- a fermentation raw material for example, a normal liquid medium that appropriately contains a carbon source, a nitrogen source, inorganic salts, and if necessary, organic micronutrients such as amino acids and vitamins is preferably used.
- waste water or sewage is used as it is or as a fermentation raw material. May be used.
- Examples of the carbon source include sugars such as glucose, sucrose, fructose, galactose and lactose, starch containing these sugars, starch hydrolysates, sugar cane molasses, sugar beet molasses, cane juice, sugar beet molasses or cane juice. Extracts or concentrates, sugar beet molasses or cane juice filtrate, syrup (high test molasses), sugar beet molasses or cane juice purified or crystallized raw sugar, vegetable molasses or cane juice purified or crystallized Purified saccharides, organic acids such as acetic acid and fumaric acid, alcohols such as ethanol, glycerin and the like are used.
- saccharide is the first oxidation product of polyhydric alcohol, which is a carbohydrate that has one aldehyde group or ketone group, categorized as aldose, saccharide with aldehyde group, and ketose as saccharide with ketone group. Point to.
- nitrogen source examples include ammonia gas, aqueous ammonia, ammonium salts, urea, nitrates, and other auxiliary organic nitrogen sources such as oil cakes, soybean hydrolysates, casein decomposition products, Other amino acids, vitamins, corn steep liquor, yeast or yeast extract, meat extract, peptides such as peptone, various fermented cells and hydrolysates thereof are used.
- inorganic salt a phosphate, magnesium salt, calcium salt, iron salt, manganese salt etc.
- microorganism fermentation conditions can usually be carried out at a pH of 3 to 8 and a temperature of 20 to 65 ° C.
- the pH of the fermentation broth is adjusted to a predetermined value within the above range by an inorganic acid or an organic acid, an alkaline substance, urea, calcium hydroxide, calcium carbonate, ammonia gas, or the like.
- eukaryotic cells or prokaryotic cells are used, for example, yeasts such as baker's yeast often used in the fermentation industry, bacteria such as Escherichia coli, lactic acid bacteria, coryneform bacteria, and filamentous Examples include fungi, actinomycetes, animal cells and insect cells.
- yeasts such as baker's yeast often used in the fermentation industry
- bacteria such as Escherichia coli, lactic acid bacteria, coryneform bacteria, and filamentous Examples include fungi, actinomycetes, animal cells and insect cells.
- the microorganisms and cells used may be those isolated from the natural environment, or may be those whose properties have been partially modified by mutation or genetic recombination.
- yeast is more preferably used among the eukaryotic cells. Suitable yeasts in the present invention include, for example, yeasts belonging to the genus Saccharomyces and yeasts belonging to Saccharomyces cerevisiae.
- prokaryotic cells do not have a structure called a cell nucleus (nucleus) in the cell, which is clearly distinguished from a eukaryote having a cell nucleus (nucleus).
- lactic acid bacteria can be preferably used among the prokaryotic cells.
- the chemical product obtained by the chemical product manufacturing apparatus is a substance produced in the fermentation broth by the above microorganisms or cultured cells.
- the chemicals include substances that are mass-produced in the fermentation industry, such as alcohols, organic acids, amino acids, and nucleic acids.
- the chemical manufacturing apparatus can also be applied to the production of substances such as enzymes, antibiotics and recombinant proteins.
- alcohols include ethanol, 1,3-butanediol, 1,4-butanediol, glycerol, and the like.
- organic acids include acetic acid, lactic acid, pyruvic acid, succinic acid, malic acid, itaconic acid, and citric acid
- nucleic acids include inosine, guanosine, and cytidine.
- the post-conversion substance obtained by the chemical production apparatus is preferably a fluid containing at least one of chemical products, dairy products, pharmaceuticals, foods or brewed products, or waste water.
- chemical products for example, substances that can be applied to make chemical products by the process after membrane separation filtration, such as organic acids, amino acids and nucleic acids, and as dairy products, for example, membranes such as low-fat milk
- substances and pharmaceuticals that can be applied as dairy products by the process after separation and filtration for example, as substances and foods that can be applied to make pharmaceuticals by the process after membrane separation and filtration, such as enzymes, antibiotics, and recombinant proteins.
- wastewater include wastewater after washing of product such as food washing wastewater and dairy product washing wastewater, and domestic wastewater containing abundant organic substances.
- yeast for eukaryotic cells and lactic acid bacteria for prokaryotic cells.
- yeast in which a gene encoding lactate dehydrogenase is introduced into cells is preferable.
- lactic acid bacteria are preferably lactic acid bacteria that produce 50% or more lactic acid as a yield to sugar relative to glucose consumed, and more preferably 80% or more as a yield against sugar. is there.
- lactic acid bacteria preferably used for producing lactic acid include, for example, in the wild type strain, Lactobacillus, Bacillus, Pediococcus, Tetragenococcus having the ability to synthesize lactic acid.
- Genus Tetragenococcus, Genus Carnobacterium, Genus Vagococus, Genus Leuconostoc, Genus Oenococcus, Genus Oenococcus ), Enterococcus (Ge us Enterococcus) include the Lactococcus (Genus Lactococcus) and to a polo Lactobacillus (Genus Sporolactobacillus) belonging to the bacteria.
- lactic acid bacteria having high lactic acid yield to sugar and high optical purity can be selected and used.
- D-lactic acid belonging to the genus Sporolactocillus examples include Spore lactobacillus laevolacticus or Sporolactobacillus inulinus as a preferred specific example.
- Sporolactobacillus laevolacticus ATCC 23492, ATCC 23493, ATCC 23494, ATCC 23495, ATCC 23396, ATCC 223549, IAM 12326, IAM 12327, IAM 12328, IAM 12329, IAM 12331, IAM 12379 , DSM 2315, DSM 6477, DSM 6510, DSM 6511, DSM 6763, DSM 6764, DSM 6771, and Sporolactocillus inulinas JCM 6014.
- lactic acid bacteria having a high yield of L-lactic acid to sugar examples include, for example, Lactobacillus yamanasiensis, Lactobacillus animaris, Lactobacillus bilis Lactobacillus Lactobacillus Lactobacillus Lactobacillus Lactobacillus Lactobacillus Lactobacillus Lactobacillus Lactobacillus Lactobacillus Lactobacillus Lactobacillus Lactobacillus Lactobacillus Lactobacillus Lactobacillus Lactobacillus Lactobacillus Lactobacillus Lactobacillus Casei (Lactobacillus casei), Lactobacillus delbrecki (Lactobacillus delbrueki), Lactobacillus paracasei, Lactobacillus rhamnosus (Lactobacillus rhusus) ), Lactobacillus ruminis, Lactobacillus salivarius, Lactobacillus sharpeae, Lactobacillus
- the culture solution refers to a solution obtained as a result of growth of microorganisms or cultured cells as fermentation raw materials. You may change suitably the composition of the fermentation raw material to add from the fermentation raw material composition at the time of a culture
- the sugar concentration in the fermentation broth is preferably maintained at 5 g / l or less. The reason why it is preferable to keep the saccharide concentration in the fermentation broth at 5 g / l or less is to minimize the loss of saccharide due to withdrawal of the fermentation broth.
- the cultivation of microorganisms or cultured cells is usually carried out in the range of pH 3 to 8 and a temperature of 20 ° C. to 60 ° C.
- the pH of the fermentation broth is usually adjusted to a predetermined value in the range of 3 to 8 with an inorganic acid or an organic acid, an alkaline substance, urea, calcium carbonate, ammonia gas, and the like. If it is necessary to increase the oxygen supply rate, means such as adding oxygen to the air to keep the oxygen concentration at 21% or higher, pressurizing the fermentation broth, increasing the stirring rate, or increasing the aeration rate can be used. .
- the ceramic membrane is washed back-washed or washed with a chemical solution so that it must be durable.
- a chemical solution so that it must be durable.
- an alkali, an acid, or an oxidizing agent can be used for the backwashing solution as long as the fermentation is not significantly inhibited.
- the alkali include a sodium hydroxide aqueous solution and a calcium hydroxide aqueous solution.
- the acid include oxalic acid, citric acid, hydrochloric acid, nitric acid and the like.
- the oxidizing agent include hypochlorite aqueous solution and hydrogen peroxide solution.
- This backwash solution can also be used at a high temperature if temperature control similar to that for sterilization water is performed.
- the separation membrane module of the present invention may have durability against steam sterilization as well as 0-14 at pH, alkali, acid or oxidizing agent, and high temperature water. preferable.
- the backwashing speed of the backwashing liquid is in the range of 0.5 to 10 times the membrane filtration speed, and more preferably in the range of 1 to 5 times. If the backwashing speed is higher than this range, the ceramic film may be damaged, and if it is lower than this range, the cleaning effect may not be sufficiently obtained.
- the backwashing cycle of the backwashing liquid can be determined by the membrane differential pressure and the change in the membrane differential pressure.
- the backwash cycle is in the range of 0.5 to 12 times per hour, more preferably in the range of 1 to 6 times per hour. If the backwash cycle is greater than this range, the separation membrane may be damaged, and if it is less than this range, the cleaning effect may not be sufficiently obtained.
- the backwashing time of the backwashing liquid can be determined by the backwashing cycle, the membrane differential pressure, and changes in the membrane differential pressure.
- the backwash time is in the range of 5 seconds to 600 seconds per time, and more preferably in the range of 30 seconds to 300 seconds per time. If the backwash time is longer than this range, the separation membrane may be damaged.
- the cleaning effect may not be sufficiently obtained. Since the time required for washing depends on the amount of liquid that needs to be supplied to the secondary side in the separation membrane module, that is, the size of the separation side volume of the separation membrane module, the secondary side volume in the separation membrane module is as much as possible. It can be said that the smaller one is preferable because it increases the efficiency of backwashing.
- the backwashing liquid sent to the primary side of the ceramic film 10 is not discharged, the filtration is stopped, and the ceramic film 10 can be continuously washed by immersion.
- the immersion time can be determined by the immersion cleaning cycle, the film differential pressure, and the change in the film differential pressure.
- the immersion time is preferably in the range of 1 minute to 24 hours per time, more preferably 10 minutes to 12 hours per time.
- continuous fermentation may be started after performing batch culture or fed-batch culture at the initial stage of culture to increase the microorganism concentration.
- a high concentration of cells may be seeded and continuous fermentation may be performed at the start of the culture.
- the nutrients necessary for cell growth may be added to the raw material culture solution so that the cell growth can be performed continuously. Maintaining a high concentration of microorganisms or cultured cells in the fermented liquid is necessary so that the ratio of the environment of the fermented liquid becomes inappropriate for the growth of microorganisms or cultured cells and does not increase so that the efficiency is high. This is a preferred embodiment for obtaining.
- the concentration of microorganisms or cultured cells in the fermentation broth maintains a microorganism concentration of 5 g / L or more as a dry weight in D-lactic acid fermentation using Sporolactobacillus laevolacticus JCM2513 (SL strain), which is a kind of lactic acid bacteria. As a result, good production efficiency can be obtained.
- microorganisms or cultured cells can be extracted from the fermenter as necessary. For example, if the concentration of microorganisms or cultured cells in the fermenter becomes too high, clogging of the ceramic membrane is likely to occur. Therefore, the clogging of the separation membrane can be avoided by drawing out the microorganisms or cultured cells.
- the production performance of a chemical may change depending on the concentration of microorganisms or cultured cells in the fermenter, and the production performance can be maintained by extracting the microorganisms or cultured cells using the production performance as an index.
- the continuous culture operation that is performed while growing fresh bacterial cells capable of fermentation production is a continuous culture method that produces products while growing bacterial cells. Any number.
- the continuous culture operation is usually performed in a single fermentation reaction tank in terms of culture management. It is also possible to use a plurality of fermentation reaction tanks because the capacity of the fermentation reaction tank is small. In this case, high productivity of the fermentation product can be obtained even if continuous fermentation is performed by connecting a plurality of fermentation reaction tanks in parallel or in series by piping.
- SiO 2 / Al 2 O 3 is used as a main raw material and 10% by mass or less of ZrO 2 is contained, and the average particle size is set to 1 ⁇ m or less with a ball mill or the like.
- 10% by mass of the frit thus prepared was added to the mixture, and an ammonium polycarboxylate and a polysaccharide binder as organic binders were added to the total amount of 0.5% by mass and water to 80% by mass, respectively.
- a slurry for forming a functional layer was prepared.
- the slurry was circulated in the through-holes of the monolith substrate, and the circulation was stopped when an amount of film-forming raw material reaching a thickness of 150 ⁇ m was deposited on the through-holes of the monolith substrate. Thereafter, the slurry was discharged from the monolith substrate and vacuum-dried for about 10 minutes. Furthermore, after drying at 60 ° C. for 20 hours, the first separation functional layer was formed on the monolith substrate by baking at 960 ° C. for 1 hour.
- alumina having an average particle diameter of about 0.6 ⁇ m 0.5 mass% of ammonium polycarboxylate as an organic binder, 1.0 mass% of polycarboxylic acid binder, and 95 mass% of water.
- a slurry for forming the second separation membrane functional layer was prepared. Using this film-forming slurry, film formation is performed by the above-described method until an amount of film-forming raw material reaching a thickness of 30 ⁇ m adheres to the substrate, dried at 60 ° C. for 20 hours, and then fired at 1400 ° C. for 1 hour. Then, the second separation functional layer was laminated to obtain a monolith membrane.
- Reference Example 2 Preparation of Separation Membrane Module
- the monolith membrane obtained in Reference Example 1 was placed in a stainless steel module container with an inner diameter of 40 mm, and an EPDM O-ring was placed between the module container and the monolith membrane. Thus, a separation membrane module 1 was prepared.
- the SL strain was first cultured overnight in a test tube with 5 mL of lactic acid fermentation medium (pre-culture).
- the obtained culture solution was inoculated into 100 mL of a fresh lactic acid fermentation medium, and cultured with shaking in a 500 mL Sakaguchi flask at 30 ° C. for 24 hours (pre-culture).
- the culture medium is inoculated after the culture medium is put in the fermenter 100 of the chemical production apparatus 200 shown in FIG. 10, the fermenter 100 is stirred by the attached stirring device 103, and the aeration amount of the fermenter 100 is adjusted. Then, temperature adjustment and pH adjustment were performed, and the culture was performed for 24 hours without operating the circulation pump 101 (pre-culture).
- the circulation pump 101 is operated, the lactic acid fermentation medium is continuously supplied in addition to the operating conditions at the time of pre-culture, and the amount of membrane permeate is controlled so that the amount of fermentation liquid in the continuous fermentation apparatus becomes 1.5L.
- Continuous culture was carried out while producing D-lactic acid by continuous fermentation.
- the amount of membrane permeated water when performing the continuous fermentation test was controlled by the filtration pump 109 so that the filtration amount was the same as the fermentation medium supply flow rate.
- the produced D-lactic acid concentration and residual glucose concentration in the membrane permeation fermentation broth were measured appropriately.
- the secondary side of the separation membrane module is filled with sterilized water, sterilized air is sent to the primary side of the separation membrane module, and the gauge pressure on the primary side of the separation membrane module is increased to 50 kPa for 1 minute. It was held and it was confirmed whether or not bubbles were generated from the secondary side of the separation membrane module.
- this operation is referred to as an air leak test.
- bubbles are generated on the secondary side of the separation membrane within 1 minute, the airtightness of the separation membrane is impaired (leaked), which is not acceptable for the air leak test. Suppose that it passes.
- An air leak test was performed on the separation membrane module, and a leak due to a crack was confirmed in the monolith membrane.
- Table 2 The sterilization conditions at this time are summarized in Table 2.
- Comparative Example 2 The monolith membrane described in Reference Example 1 was made into a separation membrane module by the method described in Reference Example 2, and connected to the sterilization apparatus 2A shown in FIG.
- the temperature T1 on the primary side of the separation membrane module 1 was 25.0 ° C.
- 5.0 ° C. Thereafter, sterilizing water was continuously supplied while controlling ⁇ T1 to be 7.0 ° C. per minute, and the internal temperature of the separation membrane module was raised. After T1 reached 100 ° C., the sterilization water was controlled to be pressurized.
- a separation membrane module 1 using a monolith membrane was prepared in the same manner as in Comparative Example 2, and connected to the sterilization apparatus 2 shown in FIG.
- the temperature T1 on the primary side of the separation membrane module 1 was 50.0 ° C.
- 40.0 ° C. Thereafter, sterilizing water was continuously supplied while controlling ⁇ T1 to be 5.5 ° C. per minute, and the internal temperature of the separation membrane module was raised. After T1 reached 100 ° C., the sterilization water was controlled to be pressurized.
- 10.0 ° C. Thereafter, sterilization water was continuously supplied while controlling ⁇ T1 to be 5.5 ° C. per minute, and the internal temperature of the separation membrane module 1 was raised. After T1 reached 100 ° C., the sterilization water was controlled to be pressurized.
- the separation membrane module was repeatedly sterilized in the same manner as described above.
- the monolith film was free from cracks and could be sterilized 10 times.
- Example 2 A monolith membrane separation membrane module 1 was prepared in the same manner as in Example 1 and connected to the separation sterilization apparatus 2 of the apparatus shown in FIG. In the sterilization process, control is performed on the primary side of the separation membrane module 1 so that the initial temperature T and the temperature change rate ⁇ T are the same as those in the first embodiment.
- the separation membrane module was sterilized by supplying from the upper part of the next side. At 100 ° C. or higher, gas-phase sterilization water was used under pressure. It should be noted that the sterilization water in the gas phase is allowed to be mixed with the sterilization water condensed into the liquid phase.
- sterilization water in a liquid phase state may be similarly mixed.
- continuous fermentation of D-lactic acid was performed as described in Reference Example 3.
- Table 2 The results of continuous fermentation are summarized in Table 2.
- the durability of the separation membrane module against steam sterilization was confirmed.
- the monolith film was free from cracks and could be sterilized 10 times.
- Example 3 A monolith membrane separation membrane module 1 was prepared in the same manner as in Example 1, and sterilization was performed by connecting the sterilization device 2C of the device shown in FIG.
- the temperature T1 on the primary side of the separation membrane module 1 was 20.2 ° C.
- the temperature T2 on the secondary side was 20.4 ° C.
- 9.6 ° C.
- 9.4 ° C. Thereafter, sterilizing water was continuously supplied while controlling ⁇ T1 and ⁇ T2 to be 5.5 ° C.
- Example 4 A monolith membrane separation membrane module 1 was prepared in the same manner as in Example 1, and connected to the sterilization apparatus 2C shown in FIG. Supply sterilization water in a gas phase state in which the temperature and pressure are controlled so that the initial temperature T and the temperature change rate ⁇ T are the same as those in Example 3 to the upper primary side and the secondary side of the separation membrane module 1 Then, the separation membrane module 1 was sterilized. Thereafter, continuous fermentation of D-lactic acid was performed as described in Reference Example 3. When continuous fermentation was performed under these conditions, it was confirmed that continuous fermentation was possible for 400 hours from the start of continuous fermentation. The results of continuous fermentation are summarized in Table 2. In the same manner as in Example 1, the durability of the separation membrane module against steam sterilization was confirmed. As a result, in the method described in this example, the monolith film was free from cracks and could be sterilized 10 times.
- Example 5 A monolith membrane separation membrane module 1 was prepared in the same manner as in Example 1, and a sterilization apparatus 2D shown in FIG.
- the temperature T1 on the primary side of the separation membrane module 1 was 20.0 ° C.
- 10.0 ° C.
- sterilization water in a liquid phase state which was controlled to have the same temperature change rate ⁇ T as in Example 1, was continuously supplied to the primary side of the separation membrane module 1.
- Example 6 A monolith membrane separation membrane module 1 was prepared in the same manner as in Example 1, and a sterilization apparatus 2D shown in FIG.
- the temperature T1 on the primary side of the separation membrane module was 20.0 ° C.
- 10.0 ° C.
- sterilization water in a liquid phase which was controlled so that the temperature increase rate ⁇ T1 was 3.5 ° C. per minute, was continuously supplied to the primary side of the separation membrane module 1.
- Example 7 A monolith membrane separation membrane module 1 was prepared in the same manner as in Example 1, and a sterilization apparatus 2D shown in FIG.
- the temperature T1 on the primary side of the separation membrane module was 20.0 ° C.
- 25.0 ° C.
- Example 8 A monolith membrane separation membrane module 1 was prepared in the same manner as in Example 1, and a sterilization apparatus 2D shown in FIG.
- the temperature T1 on the primary side of the separation membrane module was 20.0 ° C.
- 5.0 ° C.
- sterilization water in a liquid phase state in which the temperature was controlled so as to achieve the same temperature change rate ⁇ T as in Example 1 was continuously supplied to the primary side of the separation membrane module 1.
- Example 9 A monolithic membrane separation membrane module 1 was prepared in the same manner as in Example 1, and a sterilization apparatus 2C shown in FIG. 10 was connected to the separation membrane module 1.
- the temperature T1 on the primary side of the separation membrane module 1 and the temperature T2 on the secondary side were 20.0 ° C.
- 10.0 ° C. Thereafter, sterilizing water was continuously supplied while controlling so that ⁇ T1 and ⁇ T2 were increased at 5.5 ° C. per minute, and the internal temperature of the separation membrane module 1 was raised.
- the sterilization water was controlled to be pressurized. After T1 and T2 reached 200.0 ° C., the supply of sterilization water to the secondary side of the separation membrane module 1 was stopped, and the sterilization water was allowed to permeate from the primary side to the secondary side and maintained for 5 minutes. . Thereafter, the supply of sterilization water to the secondary side of the separation membrane module is started again, and sterilization water in a pressurized state is supplied to the primary side and the secondary side of the separation membrane module, and ⁇ T1 and ⁇ T2 are 5.5 per minute.
- the separation membrane module was cooled by supplying continuously while controlling the temperature to be 0 ° C. When T1 and T2 became 100 ° C. or lower, the sterilization water was controlled to return to normal pressure. When T1 and T2 became 37 ° C. or lower, the supply of sterilizing water was stopped.
- the primary side of the separation membrane module 1 is supplied with sterilization water in the vapor phase state, in which the temperature and pressure are controlled in the same manner as in Example 2, and permeated from the primary side to the secondary side of the monolith membrane for separation.
- the membrane module 1 was sterilized.
- the sterilization water was discharged from the secondary side of the separation membrane module 1 and returned to the sterilization water control unit 3 through the sterilization filter.
- continuous fermentation of D-lactic acid was performed as described in Reference Example 3.
- the results of continuous fermentation are summarized in Table 2.
- the durability of steam sterilization of the separation membrane module was confirmed. As a result, the method described in this example could be sterilized 10 times repeatedly.
- the separation membrane module sterilization method of the present invention sterilization can be performed while suppressing damage to the separation membrane module including at least a ceramic-containing separation membrane, and it can be suitably used for the purification process of foods and pharmaceuticals. It becomes possible. Further, by using a sterilization apparatus for realizing the sterilization method and a chemical production apparatus which is one of application examples, it is possible to stably maintain high productivity over a long period of time under simple operation conditions, and Continuous fermentation that can be sterilized becomes possible, and in the fermentation industry, it is possible to stably produce chemical products that are fermentation products at low cost.
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Abstract
Description
本発明に係る分離膜モジュールの滅菌方法および滅菌用装置について、図1を参照して説明する。図1は、本発明の実施の形態1に係る分離膜モジュールの滅菌用装置を例示するための概略図である。滅菌用装置2は、セラミックス膜を備えた分離膜モジュール1の1次側に滅菌用水を流し、分離膜モジュール1を滅菌する。滅菌用装置2は、滅菌用水制御部3と、滅菌用水供給ライン4と、温度測定部5と、バルブ6と、を備える。滅菌用水制御部3と分離膜モジュール1の1次側は、滅菌用水供給ライン4によって連通されており、分離膜モジュール1の1次側の温度が測定できるような位置に温度測定部5が設けられており、滅菌用水制御部3と温度測定部5の間にバルブ6が設けられている。温度測定部5で得られた温度情報は、滅菌用水制御部3に送信され、該温度情報に基づき、滅菌用水制御部3は、滅菌用水の温度を制御する。滅菌用装置2から分離膜モジュール1に供給された滅菌用水は、滅菌用水排出ライン7を介して分離膜モジュール1の系外に排出される。なお、以下、分離膜モジュール1内の、処理対象である原液と接する側を1次側と呼び、処理後の濾過液と接する側を2次側と呼ぶ。
セラミックス基材20の端面および貫通孔21の表面に、分離機能層22が積層されたセラミックス膜10も好ましい。分離機能層22を積層させることによって、セラミックス膜10の表面孔径がより精密に制御されるようになり、濾過すべき物質のみをより正確に濾過、分離できるようになる。分離機能層22をセラミックス基材20の端面にも積層することで、濾過すべきでない物質がモノリス膜の端面から濾過されてしまい、濾液の中に混入するといった問題を未然に防止できるようになる。
なお気孔率は、以下の式より決定される。
気孔率[%]=(100×(湿潤膜重量[g]-乾燥膜重量[g]))/(水比重[g/cm3]×膜体積[cm3])
本発明の実施の形態2にかかる滅菌用装置は、2つの滅菌用水供給ラインを有し、該2つの滅菌用水供給ラインにより、分離膜モジュールの1次側および2次側に滅菌用水をそれぞれ供給する点で実施の形態1と異なる。以下、図面を参照して、実施の形態2について説明する。図7は、本発明の実施の形態2にかかる分離膜モジュールの滅菌用装置の概略図である。
分離膜モジュール1の1次側に滅菌用水を供給しながら、1次側から加圧または/および2次側から吸引することで滅菌用水をセラミックス膜10に透過させる。滅菌用水の温度変化率や、分離膜モジュール1の2次側の滅菌用水の排出については、前述の滅菌方法に準じるものとする。
次に、本発明の実施の形態3にかかる連続発酵による化学品製造装置について説明する。図10は、本発明の実施の形態3にかかる化学品製造装置の概略図である。
連続発酵で使用される微生物や培養細胞の発酵原料、すなわち変換前物質は、発酵培養する微生物や培養細胞の生育を促し、目的とする発酵生産物である化学品を良好に生産させ得るものであればよい。発酵原料としては、例えば、炭素源、窒素源、無機塩類、および必要に応じてアミノ酸、およびビタミンなどの有機微量栄養素を適宜含有する通常の液体培地等が好ましく用いられる。前記発酵培養する微生物や培養細胞の生育を促し、目的とする発酵生産物である化学品を良好に生産させ得るものを一部含む液体であれば、例えば廃水または下水も、そのまま、または発酵原料を添加して使用してもよい。
微生物の発酵条件は、通常、pHが3~8で温度が20~65℃の範囲で行うことができる。発酵液のpHは、無機の酸あるいは有機の酸、アルカリ性物質、さらには尿素、水酸化カルシウム、炭酸カルシウムおよびアンモニアガスなどによって、上記範囲内のあらかじめ定められた値に調節される。
連続発酵による化学品の製造に使用する微生物または培養細胞が生育のために特定の栄養素を必要とする場合には、その栄養物を標品もしくはそれを含有する天然物として添加する。また、消泡剤を必要に応じて使用することができる。連続発酵による化学品の製造において、培養液とは、発酵原料に微生物または培養細胞が増殖した結果得られる液のことを言う。追加する発酵原料の組成は、目的とする化学品の生産性が高くなるように、培養開始時の発酵原料組成から適宜変更しても良い。
連続発酵による化学品の製造において、発酵原料に糖を用いる場合は、発酵液中の糖類濃度は5g/l以下に保持されることが好ましい。発酵液中の糖類濃度を5g/l以下に保持することが好ましい理由は、発酵液の引き抜きによる糖類の流失を最小限にするためである。
なお、逆洗液の逆洗速度は、膜濾過速度の0.5倍以上10倍以下の範囲であり、より好ましくは1倍以上5倍以下の範囲である。逆洗速度がこの範囲より高いと、セラミックス膜に損傷を与える可能性があり、またこの範囲より低いと洗浄効果が充分に得られないことがある。
逆洗液の逆洗時間は、逆洗周期、膜差圧および膜差圧の変化により決定することができる。逆洗時間は、1回あたり5秒以上600秒以下の範囲であり、より好ましくは1回あたり30秒以上300秒以下の範囲である。逆洗時間がこの範囲より長いと、分離膜に損傷を与える可能性があり、またこの範囲より短いと、洗浄効果が充分に得られないことがある。洗浄に要する時間は、分離膜モジュール内の2次側に供給する必要がある液量、すなわち分離膜モジュール2次側容積の大きさに依存するため、分離膜モジュール内の2次側容積がなるべく小さいほうが逆洗の効率を高めることから好ましいといえる。
外径36mm、長さ200mmの円柱状かつ、基材の長手方向に直径3mmの円形貫通孔を37本設けた、アルミナを主成分とする押出成形物を製作し、これを1250℃で1時間焼結することによりモノリス基材を得た。
参考例1で得られたモノリス膜を、内径40mmの、ステンレス製のモジュール容器内に収め、モジュール容器とモノリス膜の間にEPDM製のO-リングを配して分離膜モジュール1を作成した。
D-乳酸の連続発酵は、以下の条件のとおり行った。連続発酵は、図10の化学品製造装置200を用いて行った。
発酵槽容量:2(L)
発酵槽有効容積:1.5(L)
温度調整:37(℃)
発酵槽通気量:窒素ガス0.2(L/min)
発酵槽攪拌速度:600(rpm)
pH調整:3N Ca(OH)2によりpH6に調整
乳酸発酵培地供給:発酵槽液量が約1.5Lで一定になる様に制御して添加
発酵液循環装置による循環液量:2(L/min)
膜濾過流量制御:吸引ポンプによる流量制御
間欠的な濾過処理:濾過処理(9分間)~濾過停止処理(1分間)の周期運転
膜濾過流束:0.01(m/day)以上5(m/day)以下の範囲で膜間差圧が500kPa以下となる様に可変。膜間差圧が範囲を超えて上昇し続けた場合は、連続発酵を終了した。
培地組成は、以下の表1に示すとおりである。
カラム:Shim-Pack SPR-H(島津社製)
移動相:5 mM p-トルエンスルホン酸(0.8 mL/min)
反応相:5 mM p-トルエンスルホン酸、20 mM ビストリス、0.1 mM EDTA・2Na(0.8 mL/min)
検出方法:電気伝導度
カラム温度:45℃
なお、乳酸の光学純度の分析は、以下の条件下で行った。
カラム:TSK-gel Enantio L1(東ソー社製)
移動相 :1 mM 硫酸銅水溶液
流束:1.0 mL/分
検出方法:UV 254 nm
温度:30℃
L-乳酸の光学純度は、次式(i)で計算される。
光学純度(%)=100×(L-D)/(D+L) ・・・(i)
また、D-乳酸の光学純度は、次式(ii)で計算される。
光学純度(%)=100×(D-L)/(D+L) ・・・(ii)
ここで、LはL-乳酸の濃度を表し、DはD-乳酸の濃度を表す。
参考例1で得られたモノリス膜を電気オーブンの中に収め、300.0℃になるまで加熱した。加熱速度は毎分15.0℃であった。300.0℃に達した後に30分保持し、その後、電気オーブンの電源を切り、電気オーブンに付属した換気ファンを用いてオーブン内を冷却した。オーブンの電源を切ってから20分後に電気オーブンの内温は25.0℃になり、冷却時の平均温度変化率は毎分13.8℃であった。この手順で乾熱滅菌を行ったモノリス膜は、急激な温度変化に耐えられずにクラックが入ってしまった。
このモノリス膜を用いて、参考例2と同様の手順で分離膜モジュールを作成した。その後、分離膜モジュールの2次側に滅菌水を満たし、分離膜モジュールの1次側に滅菌空気を送り、分離膜モジュールの1次側のゲージ圧が50kPaとなるように加圧して、1分間保持し、分離膜モジュールの2次側から気泡が発生するか否かを確認した。これ以降、この操作をエアリークテストと呼び、1分以内に分離膜の2次側に気泡が発生したものについては、分離膜の気密性が損なわれて(リークして)おり、エアリークテストに不合格であるとする。
この分離膜モジュールのエアリークテストを実施したが、モノリス膜にクラックによるリークが確認された。このときの滅菌処理条件をまとめて表2に記載した。
参考例1に記載のモノリス膜を、参考例2に記載の方法で分離膜モジュールとし、図6に示す滅菌用装置2Aに接続した。分離膜モジュール1の1次側の温度T1は25.0℃であった。滅菌用水制御部3において、滅菌用水をTw=30.0℃、液相状態とし、分離膜モジュール1下部の1次側への連続的供給を開始した。|T1-Tw|=5.0℃であった。その後、△T1が毎分7.0℃となるように制御しながら滅菌用水を供給し続け、分離膜モジュールの内温を昇温させた。T1が100℃に達した後は、滅菌用水を加圧するように制御した。T1が121℃に達したのち、121℃の状態を20分維持させた。その後、分離膜モジュール1の1次側に、加圧状態の滅菌用水を、△T1が毎分7.0℃となるように制御しながら連続的に供給し、分離膜モジュール1を冷却した。T1が100℃以下になったら、滅菌用水を常圧に戻すよう制御した。T1が37℃になったら滅菌用水の供給を止めた。
その後、比較例1と同様の手順で分離膜モジュール1のエアリークテストを実施したが、モノリス膜にクラックによるリークが確認された。このときの滅菌処理条件をまとめて表2に記載した。
比較例2と同様にモノリス膜を用いた分離膜モジュール1を作成し、図7に記載の滅菌用装置2に接続した。分離膜モジュール1の1次側の温度T1は50.0℃であった。滅菌用水制御部3において、滅菌用水をTw=90.0℃、気相状態とし、分離膜モジュール1の上部1次側への連続的供給を開始した。|T1-Tw|=40.0℃であった。その後、△T1が毎分5.5℃となるように制御しながら滅菌用水を供給し続け、分離膜モジュールの内温を昇温させた。T1が100℃に達した後は、滅菌用水を加圧するように制御した。T1が121℃に達したのち、121℃の状態を20分維持させた。その後、分離膜モジュール1の1次側に加圧状態の滅菌用水を、△T1が毎分5.5℃となるように制御しながら連続的に供給し、分離膜モジュール1を冷却した。T1が100℃以下になったら、滅菌用水を常圧に戻すよう制御した。T1が37℃になったら滅菌用水の供給を止めた。
その後、比較例1と同様の手順で分離膜モジュール1のエアリークテストを実施したが、モノリス膜にクラックによるリークが確認された。このときの滅菌処理条件をまとめて表2に記載した。
(実施例1)
比較例2と同様にモノリス膜の分離膜モジュール1を作成し、図7に記載の滅菌用装置2Bに接続して滅菌処理を行った。分離膜モジュール1の1次側の温度T1は20.0℃であった。滅菌用水制御部3において、滅菌用水をTw=30.0℃、液相状態とし、分離膜モジュール1の下部1次側に連続的供給を開始した。|T1-Tw|=10.0℃であった。
その後、△T1が毎分5.5℃となるように制御しながら滅菌用水を供給し続け、分離膜モジュール1の内温を昇温させた。T1が100℃に達した後は、滅菌用水を加圧するように制御した。T1が121℃に達したのち、121℃の状態を20分維持させた。その後、分離膜モジュール1の1次側に加圧状態の滅菌用水を、△T1が毎分5.5℃となるように制御しながら連続的に供給し、分離膜モジュール1を冷却した。T1が100℃以下になったら、滅菌用水を常圧に戻すよう制御した。T1が37℃になったら滅菌用水の供給を止めた。
その後、参考例3の記載に沿ってD-乳酸の連続発酵を行った。この条件で連続発酵を行った場合、連続発酵開始から400時間の連続発酵が可能であることを確認できた。連続発酵の結果をまとめて表2に記載した。
なお、分離膜モジュールの蒸気滅菌に対する耐久性を確認するために、前述の方法と同様にして分離膜モジュールを繰り返し滅菌処理した。その結果、本実施例に記載の方法ではモノリス膜にクラックの発生は無く、10回の繰り返し滅菌処理が可能であった。
(実施例2)
実施例1と同様にモノリス膜の分離膜モジュール1を作成し、図1に記載の装置の分離滅菌用装置2に接続して滅菌処理を行った。滅菌処理は、分離膜モジュール1の1次側に、実施例1と同様の初期温度Tおよび温度変化率△Tとなるように制御を行い、気相状態の滅菌用水を分離膜モジュール1の1次側上部から供給して分離膜モジュールの滅菌処理を実施した。100℃以上においては、気相状態の滅菌用水を加圧して用いた。なお、気相状態の滅菌用水には、滅菌用水が凝縮して液相状態となったものの混入を許容している。以下、他の実施例において気相状態の滅菌用水を用いる場合も、同様に液相状態の滅菌用水が混入してもよいものとした。
その後、参考例3の記載に沿ってD-乳酸の連続発酵を行った。この条件で連続発酵を行った場合、連続発酵開始から400時間の連続発酵が可能であることを確認できた。連続発酵の結果をまとめて表2に記載した。
実施例1と同様にして、分離膜モジュールの蒸気滅菌に対する耐久性を確認した。その結果、本実施例に記載の方法ではモノリス膜にクラックの発生は無く、10回の繰り返し滅菌処理が可能であった。
実施例1と同様にモノリス膜の分離膜モジュール1を作成し、図10に記載の装置の滅菌用装置2Cを分離膜モジュール1の下部に接続して滅菌処理を行った。分離膜モジュール1の1次側の温度T1は20.2℃、2次側の温度T2は20.4℃であった。滅菌用水制御部3において、滅菌用水をTw=30.0℃、液相状態とし、分離膜モジュール1下部の1次側および2次側への連続的供給を開始した。|T1-Tw|=9.6℃、|T2-Tw|=9.4℃であった。
その後、△T1および△T2がそれぞれ毎分5.5℃となるように制御しながら滅菌用水を供給し続け、分離膜モジュール1の内温を昇温させた。T1、T2のいずれかが100℃に達した後は、滅菌用水を加圧するように制御した。T1およびT2が121℃に達したのち、T1、T2とも121℃以上となる状態を20分維持させた。その後、分離膜モジュール1の1次側および2次側に加圧状態の滅菌用水を、△T1および△T2が毎分5.5℃となるように制御しながら連続的に供給し、分離膜モジュール1を冷却した。T1およびT2が100℃以下になったら、滅菌用水を常圧に戻すよう制御した。T1およびT2が37℃以下になったら滅菌用水の供給を止めた。
その後、参考例3の記載に沿ってD-乳酸の連続発酵を行った。この条件で連続発酵を行った場合、連続発酵開始から400時間の連続発酵が可能であることを確認できた。連続発酵の結果をまとめて表2に記載した。
実施例1と同様にして、分離膜モジュールの蒸気滅菌に対する耐久性を確認した。その結果、本実施例に記載の方法ではモノリス膜にクラックの発生は無く、10回の繰り返し滅菌処理が可能であった。
(実施例4)
実施例1と同様にモノリス膜の分離膜モジュール1を作成し、図10に記載の滅菌用装置2Cに接続した。分離膜モジュール1の上部1次側および2次側に、実施例3と同様の初期温度T、温度変化率△Tとなるように、温度および圧力制御を行った気相状態の滅菌用水を供給し、分離膜モジュール1の滅菌処理を実施した。
その後、参考例3の記載に沿ってD-乳酸の連続発酵を行った。この条件で連続発酵を行った場合、連続発酵開始から400時間の連続発酵が可能であることを確認できた。連続発酵の結果をまとめて表2に記載した。
実施例1と同様にして、分離膜モジュールの蒸気滅菌に対する耐久性を確認した。その結果、本実施例に記載の方法ではモノリス膜にクラックの発生は無く、10回の繰り返し滅菌処理が可能であった。
(実施例5)
実施例1と同様にモノリス膜の分離膜モジュール1を作成し、図11に記載の滅菌用装置2Dを分離膜モジュール1の下部に接続した。分離膜モジュール1の1次側の温度T1は20.0℃であった。滅菌用水制御部3において、滅菌用水をTw=30.0℃、液相状態とし、分離膜モジュール1下部の1次側への連続的供給を開始した。|T1-Tw|=10.0℃であった。次いで、分離膜モジュール1の1次側に実施例1と同様の温度変化率△Tとなるように制御を行った液相状態の滅菌用水を連続的に供給した。併せて分離膜モジュール1の1次側に滅菌用水供給ポンプ8により100kPaの圧力を印加し、滅菌用水をモノリス膜の1次側から2次側に透過させて、分離膜モジュール1の滅菌処理を実施した。
その後、参考例3の記載に沿ってD-乳酸の連続発酵を行った。この条件で連続発酵を行った場合、連続発酵開始から400時間の連続発酵が可能であることを確認できた。連続発酵の結果をまとめて表2に記載した。
実施例1と同様にして、分離膜モジュールの蒸気滅菌に対する耐久性を確認した。その結果、本実施例に記載の方法ではモノリス膜にクラックの発生は無く、10回の繰り返し滅菌処理が可能であった。
(実施例6)
実施例1と同様にモノリス膜の分離膜モジュール1を作成し、図11に記載の滅菌用装置2Dを分離膜モジュール1の下部に接続した。分離膜モジュールの1次側の温度T1は20.0℃であった。滅菌用水制御部3において、滅菌用水をTw=30.0℃、液相状態とし、分離膜モジュール下部の1次側への連続的供給を開始した。|T1-Tw|=10.0℃であった。次いで、分離膜モジュール1の1次側に、温度上昇率△T1が毎分3.5℃となるように制御を行った液相状態の滅菌用水を連続的に供給した。併せて分離膜モジュール1の1次側に滅菌用水供給ポンプ8により100kPaの圧力を印加し、滅菌用水をモノリス膜の1次側から2次側に透過させて、分離膜モジュール1の滅菌処理を実施した。
その後、参考例3の記載に沿ってD-乳酸の連続発酵を行った。この条件で連続発酵を行った場合、連続発酵開始から400時間の連続発酵が可能であることを確認できた。連続発酵の結果をまとめて表2に記載した。
実施例1と同様にして、分離膜モジュールの蒸気滅菌の耐久性を確認した。その結果、本実施例に記載の方法では10回の繰り返し滅菌処理が可能であった。
(実施例7)
実施例1と同様にモノリス膜の分離膜モジュール1を作成し、図11に記載の滅菌用装置2Dを分離膜モジュール1の下部に接続した。分離膜モジュールの1次側の温度T1は20.0℃であった。滅菌用水制御部3において、滅菌用水をTw=45.0℃、液相状態とし、分離膜モジュール1下部の1次側への連続的供給を開始した。|T1-Tw|=25.0℃であった。次いで、分離膜モジュール1の1次側に実施例1と同様の温度変化率△Tとなるように温度制御を行った液相状態の滅菌用水を連続的に供給した。併せて分離膜モジュール1の1次側に滅菌用水供給ポンプ8により100kPaの圧力を印加し、滅菌用水をモノリス膜の1次側から2次側に透過させて、分離膜モジュール1の滅菌処理を実施した。
その後、参考例3の記載に沿ってD-乳酸の連続発酵を行った。この条件で連続発酵を行った場合、連続発酵開始から400時間の連続発酵が可能であることを確認できた。連続発酵の結果をまとめて表2に記載した。
実施例1と同様にして、分離膜モジュールの蒸気滅菌の耐久性を確認した。その結果、本実施例に記載の方法では10回の繰り返し滅菌処理が可能であった。
(実施例8)
実施例1と同様にモノリス膜の分離膜モジュール1を作成し、図11に記載の滅菌用装置2Dを分離膜モジュール1の下部に接続した。分離膜モジュールの1次側の温度T1は20.0℃であった。滅菌用水制御部3において、滅菌用水をTw=25.0℃、液相状態とし、分離膜モジュール1下部の1次側への連続的供給を開始した。|T1-Tw|=5.0℃であった。次いで、分離膜モジュール1の1次側に実施例1と同様の温度変化率△Tとなるように温度制御を行った液相状態の滅菌用水を連続的に供給した。併せて分離膜モジュール1の1次側に滅菌用水供給ポンプ8により100kPaの圧力を印加し、滅菌用水をモノリス膜の1次側から2次側に透過させて、分離膜モジュール1の滅菌処理を実施した。
その後、参考例3の記載に沿ってD-乳酸の連続発酵を行った。この条件で連続発酵を行った場合、連続発酵開始から400時間の連続発酵が可能であることを確認できた。連続発酵の結果をまとめて表2に記載した。
実施例1と同様にして、分離膜モジュールの蒸気滅菌の耐久性を確認した。その結果、本実施例に記載の方法では10回の繰り返し滅菌処理が可能であった。
実施例1と同様にモノリス膜の分離膜モジュール1を作成し、図10に記載の滅菌用装置2Cを分離膜モジュール1に接続した。分離膜モジュール1の1次側の温度T1、2次側の温度T2とも20.0℃であった。滅菌用水制御部3において、滅菌用水をTw=30.0℃、気相状態とし、分離膜モジュール上部の1次側および2次側への連続的供給を開始した。|T1-Tw|=|T2-Tw|=10.0℃であった。
その後、△T1および△T2が毎分5.5℃で上昇するように制御しながら滅菌用水を供給し続け、分離膜モジュール1の内温を昇温させた。T1、T2のいずれかが100℃に達した後は、滅菌用水を加圧するように制御した。T1およびT2が200.0℃に達したのち、分離膜モジュール1の2次側への滅菌用水供給を止め、滅菌用水を1次側から2次側に透過させるようにして5分維持させた。その後、再び分離膜モジュールの2次側にも滅菌用水供給を開始し、分離膜モジュールの1次側および2次側に加圧状態の滅菌用水を、△T1および△T2が毎分5.5℃となるように制御しながら連続的に供給し、分離膜モジュールを冷却した。T1およびT2が100℃以下になったら、滅菌用水を常圧に戻すよう制御した。T1およびT2が37℃以下になったら滅菌用水の供給を止めた。
次いで、分離膜モジュール1の1次側に、実施例2と同様の温度、圧力制御を行った気相状態の滅菌用水を供給し、モノリス膜の1次側から2次側に透過させて分離膜モジュール1の滅菌処理を実施した。滅菌用水は分離膜モジュール1の2次側から排出し、滅菌フィルターを通して滅菌用水制御部3に返送した。
その後、参考例3の記載に沿ってD-乳酸の連続発酵を行った。この条件で連続発酵を行った場合、連続発酵開始から400時間の連続発酵が可能であることを確認できた。連続発酵の結果をまとめて表2に記載した。
実施例1と同様にして、分離膜モジュールの蒸気滅菌の耐久性を確認した。その結果、本実施例に記載の方法では10回の繰り返し滅菌処理が可能であった。
2、2A、2B、2C、2D 滅菌用装置
3 滅菌用水制御部
3a 滅菌用水制御部(1次側)
3b 滅菌用水制御部(2次側)
4 滅菌用水供給ライン
4a 滅菌用水供給ライン(1次側)
4b 滅菌用水供給ライン(2次側)
5 温度測定部
5a 温度測定部(1次側)
5b 温度測定部(2次側)
6 バルブ
6a バルブ(1次側)
6b バルブ(2次側)
7 滅菌用水排出ライン
7a 滅菌用水排出ライン(1次側)
7b 滅菌用水排出ライン(2次側)
8 滅菌用水供給ポンプ
10 セラミックス膜
11 モジュール容器
12 O-リング
13 通液口
13a 原液供給口/濃縮液排出口
13b 濾過液排出口/逆洗液供給口
20 セラミックス基材
21 貫通孔
22 分離機能層
23 集水スリット
24 集水孔
25 集水スリット連通孔
100 発酵槽
101 循環ポンプ
102 温度制御装置
103 攪拌装置
104 pHセンサー・制御装置
105 レベルセンサー・制御装置
106 差圧センサー
107 培地供給ポンプ
108 中和剤供給ポンプ
109 濾過ポンプ
110 濾過バルブ
111 逆洗ポンプ
112 逆洗バルブ
113 配管気体供給制御バルブ
114 配管スクラビング気体供給装置
115 発酵槽気体供給装置
116 発酵槽圧力調整バルブ
117 発酵槽圧力計
200 化学品製造装置
Claims (9)
- 少なくともセラミックスを含む分離膜を備えた分離膜モジュールを、滅菌用水を用いて滅菌する分離膜モジュールの滅菌方法であって、
前記分離膜モジュールに前記滅菌用水を供給し、前記分離膜モジュールの温度が毎分6.0℃以下で上昇するように、供給する前記滅菌用水の温度および圧力を制御して、所定の滅菌温度まで前記分離膜モジュールを昇温する昇温工程と、
前記分離膜モジュールが所定の滅菌温度に達したのちに、前記分離膜モジュールを所定温度で所定時間滅菌する滅菌工程と、
を含むことを特徴とする分離膜モジュールの滅菌方法。 - 前記分離膜モジュールの温度Tを測定する温度測定工程と、
前記滅菌用水の温度Twが|T-Tw|≦30.0℃となるようにTおよび/またはTwを制御する初期温度制御工程とを含み、
前記初期温度制御工程後に、前記昇温工程を実施することを特徴とする請求項1に記載の分離膜モジュールの滅菌方法。 - 前記温度測定工程は、前記温度Tとして処理対象の原液が供給される側である前記分離膜モジュールの1次側の温度を測定し、
前記昇温工程および前記滅菌工程は、前記分離膜モジュールの1次側に前記滅菌用水を供給することを特徴とする請求項1または2に記載の分離膜モジュールの滅菌方法。 - 前記温度測定工程は、前記温度Tとして前記分離膜モジュールの1次側および2次側の温度のうちいずれか一方の温度Tを測定し、
前記昇温工程および前記滅菌工程は、前記分離膜モジュールの1次側および2次側に前記滅菌用水を供給することを特徴とする請求項1または2に記載の分離膜モジュールの滅菌方法。 - 少なくともセラミックスを含む分離膜を備えた分離膜モジュールを、滅菌用水を用いて滅菌する分離膜モジュールの滅菌方法であって、
前記分離膜モジュールの処理対象の原液が供給される1次側および処理後の濾過液が集液される2次側に前記滅菌用水を供給し、前記分離膜モジュールの1次側および2次側の温度が毎分6.0℃以下で上昇するように、供給する前記滅菌用水の温度および圧力を制御して、所定の滅菌温度まで前記分離膜モジュールを昇温する昇温工程と、
前記分離膜モジュールの1次側および2次側が所定の滅菌温度に達したのちに、前記分離膜モジュールを所定温度で所定時間滅菌する滅菌工程と、
を含むことを特徴とする分離膜モジュールの滅菌方法。 - 前記分離膜モジュールの1次側の温度T1および2次側の温度T2を測定する温度測定工程と、
前記分離膜モジュールの1次側に供給される滅菌用水の温度Tw1、および前記分離膜モジュールの2次側に供給される滅菌用水の温度Tw2を、|T1-Tw1|≦30.0℃、および|T2-Tw2|≦30.0℃となるように、T1および/またはT2および/またはTwを制御する初期温度制御工程とを含み、
前記初期温度制御工程後に、前記昇温工程を実施することを特徴とする請求項5に記載の分離膜モジュールの滅菌方法。 - [規則91に基づく訂正 06.02.2012]
前記滅菌工程後、前記分離膜モジュールの温度が毎分6.0℃以下で降下するように、前記分離膜モジュールを冷却する冷却工程を含むことを特徴とする請求項1~6のいずれか一つに記載の分離膜モジュールの滅菌方法。 - 少なくともセラミックスを含む分離膜を備えた分離膜モジュールを滅菌する滅菌用装置であって、
前記分離膜モジュールの温度を測定する温度測定手段と、
温度および圧力が制御された気相または液相の滅菌用水を生成し、前記分離膜モジュールに供給する滅菌用水制御部と、
を備え、前記滅菌用水制御部は、前記分離膜モジュールの温度が毎分6.0℃以下で上昇および降下するように、前記滅菌用水を供給することを特徴とする滅菌用装置。 - 少なくともセラミックスを含む分離膜を備えた分離膜モジュールと、
請求項8に記載の滅菌用装置と、
発酵原料を微生物による発酵培養することにより、該発酵原料を化学品を含有する発酵液に変換する発酵槽と、
前記発酵槽から前記分離膜モジュールに発酵液を送液する発酵液循環手段と、
を備えることを特徴とする化学品製造装置。
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US13/997,094 US20130302882A1 (en) | 2010-12-24 | 2011-12-22 | Method for sterilizing separation membrane modules, sterilization device, and apparatus for producing chemicals |
JP2012513119A JPWO2012086763A1 (ja) | 2010-12-24 | 2011-12-22 | 分離膜モジュールの滅菌方法、滅菌用装置および化学品製造用装置 |
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WO2013105651A1 (ja) | 2012-01-13 | 2013-07-18 | 東レ株式会社 | 化学品の製造方法 |
WO2013105652A1 (ja) | 2012-01-13 | 2013-07-18 | 東レ株式会社 | 化学品の製造方法 |
WO2013105653A1 (ja) | 2012-01-13 | 2013-07-18 | 東レ株式会社 | 化学品の製造方法 |
US20150050694A1 (en) * | 2012-03-16 | 2015-02-19 | Toray Industries, Inc. | Method of sterilizing separation membrane module, method of producing chemical by continuous fermentation, and membrane separation-type continuous fermentation apparatus |
JP2020072654A (ja) * | 2013-12-04 | 2020-05-14 | ポカード・ディアグノスティクス・リミテッドPocared Diagnostics, Ltd. | タンジェンシャルフィルタリングによって抽出された粒子を処理し分析するための方法と装置 |
US10927389B2 (en) | 2014-04-14 | 2021-02-23 | Toray Industries, Inc. | Method of producing chemical substance by continuous fermentation |
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US9340297B2 (en) * | 2013-02-19 | 2016-05-17 | The Boeing Company | Counter-flow gas separation modules and methods |
CA2989669A1 (en) * | 2015-06-19 | 2016-12-22 | Nanostone Water Inc. | System and method for backwashing a ceramic membrane |
US11465099B2 (en) * | 2017-06-15 | 2022-10-11 | Baxter International Inc. | Water purification apparatus and a method for controlling at least one fluid property in a water purification apparatus |
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WO2013105651A1 (ja) | 2012-01-13 | 2013-07-18 | 東レ株式会社 | 化学品の製造方法 |
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JP2020072654A (ja) * | 2013-12-04 | 2020-05-14 | ポカード・ディアグノスティクス・リミテッドPocared Diagnostics, Ltd. | タンジェンシャルフィルタリングによって抽出された粒子を処理し分析するための方法と装置 |
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US10927389B2 (en) | 2014-04-14 | 2021-02-23 | Toray Industries, Inc. | Method of producing chemical substance by continuous fermentation |
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