JP4562561B2 - Solution casting apparatus and filter replacement method for filtration device - Google Patents

Description

  The present invention relates to a solution casting apparatus and a filter replacement method for a filtration device, and more particularly to a filtration device for filtering a polymer solution.

In producing a film by a solution casting method using a solution casting apparatus, a natural material such as cellulose ester may be used as a raw material for the solution. Cellulose esters contain a small amount of components that do not dissolve or are difficult to dissolve in the main organic solvent. In addition, impurities may be contained in the cellulose ester, and further, foreign matters may be mixed during the process of transporting and dissolving the solution (Patent Document 1). Therefore, impurities and foreign substances are removed by a filtration device in the liquid feeding process of the solution casting equipment. As this filtering device, a filter press having a configuration in which a filter is sandwiched between two filter plates is generally used, and foreign matter is removed by passing through the filter press.
JP 2003-221455 A

  However, the filter is formed in a fine mesh, and when the mesh is clogged with impurities and foreign matter, the pressure difference increases. For this reason, it is necessary to replace the filter when the differential pressure increases and the filtering ability of the filter is below the reference value. When replacing the filter, the press pressure between the filter plate and the filter is loosened, and the filter plate and the filter are opened and replaced with a new filter. In recent years, it is necessary to set a high reference value for the filtration capacity in accordance with the improvement in quality required for the film. For this reason, the frequency of exchanging the filter has increased, which is troublesome for the operator.

  In addition, if the pressure of the two filter plates is loosened to replace the filter and the filter plate and the filter are opened, the residual solution remaining between the filter plate and the filter will flow out, which is harmful to humans. It was dangerous when using a simple solution. Further, even when the residual solution does not flow out, there is a problem because it is dangerous due to evaporation of the solution and leads to air pollution. Further, when the filter is replaced, it is necessary to stop the operation of the filtration device, and there is a problem that the operation time is reduced. Furthermore, since the filter is thin, a plurality of new replacement filters are placed on top of each other. When replacing a filter, even if only one of the plurality of filters is to be gripped, There was a problem that.

  The present invention has been made in order to solve the above-described problem, and can filter the filter without stopping the operation, and can reduce the residual solution in the filter plate when the filter is replaced. The object is to provide a solution film-forming facility provided with a filter replacement method for a filtration device.

In order to achieve the above object, the solution casting apparatus of the present invention selectively uses a plurality of filtration devices having a filter for filtering a polymer solution in a filtration passage, and the plurality of filtration devices. And a switching device for switching the piping system, and casting the polymer solution filtered by at least one of the plurality of filtration devices onto a support and stripping it off as a polymer film. In the solution casting apparatus to be dried, the filtration device has a filtration position for clamping the filter and filtering the polymer solution, and an open position for opening the filter and allowing the filter to be replaced. A filter holding member that is displaced between the filter holding member, a cleaning unit that sends a cleaning liquid to clean the filter at the filtration position, and a filter holding member that has been cleaned by the cleaning unit. And a member to the open position have a filter exchange means for exchanging the filter, the cleaning means, said filtering the filtered passage and said polymer solution feed gas into the filter before feeding the washing liquid A polymer solution discharging means for discharging from the apparatus, and a drying means for sending a gas to the filtration passage and the filter after the cleaning with the cleaning liquid to dry the cleaning liquid .

  Further, the amount of the cleaning liquid component in the gas sent to the filtration passage and the filter for the drying is detected, the degree of drying is determined based on the detected value, and when the drying is determined to be completed, the filter replacement command is issued. It is preferable to have a drying determination means for outputting to the filter replacement means.

  Further, the filter is made of sheet-like filter paper, and the filter replacement means includes a collecting means for collecting the used filter from the filter holding member in the open position, and the unused filter being stacked and stored. A suction holding unit that sucks and holds the uppermost layer in the stored filter, and the filter sucked by the suction holding unit is a filter that has been used by the collecting means at the open position. It is preferable to have filter setting means for setting the recovered filter holding member.

  In addition, a displacement portion that displaces the suction holding portion in a state where the filter is sucked up is provided, and the filter setting means sets the filter on the filter holding member in a state where the suction portion is displaced upward. It is preferable. Furthermore, it is preferable that the air around the filtration device during the filter replacement is sucked and the organic solvent in the cleaning liquid is recovered from the sucked air. Moreover, it is preferable that the said polymer film is a cellulose ester and the said filter is the filter paper comprised from a cellulose.

  Further, the filter replacement method of the filtration device of the present invention includes a filtration position where the polymer solution is filtered by sandwiching the filter in the filtration passage, and an opening where the filter can be replaced by opening the filter. In a filter replacement method for a filtration apparatus having a filter clamping member that is displaced between positions, a polymer solution discharge step for sending gas into the filtration passage and discharging the polymer solution from the filtration passage; After discharging the molecular solution, a cleaning process is performed in which the cleaning liquid is sent into the filtration path, and the filtration path and the filter are cleaned. A dry gas is sent into the filtration path after the cleaning with the cleaning liquid, and the filtration path and the filter The drying process for drying the cleaning liquid of the liquid, and the amount of the cleaning liquid component in the dry gas during the drying process are detected, and the completion of the drying is determined based on the detected value. When it is determined, characterized in that it has a filter replacement step of replacing the filter by the filter clamping member to the open position after stopping the feeding of the gas.

  In the filter replacement step, it is preferable that air around the filtration device is sucked and the organic solvent in the cleaning liquid is recovered from the sucked air.

  According to the solution casting apparatus of the present invention, a plurality of filtration devices having a filter for filtering a polymer solution in a filtration passage, and switching for switching a piping system to selectively use the plurality of filtration devices A solution casting apparatus for casting a polymer solution that has been filtered by at least one of a plurality of filtration devices on a support and peeling it off as a polymer film, and drying the polymer film. The filtration device includes a filter holding member that moves between a filtration position for holding the filter and filtering the polymer solution, and an open position that opens the filter and allows the filter to be replaced. There are cleaning means for sending cleaning liquid to clean the filter, and filter replacement means for replacing the filter with the filter clamping member in the open position after cleaning by the cleaning means. From, it is possible to prevent the harmful gas to the outside flows out, it can be carried out safely replace the filter without stopping the operation.

  The cleaning means includes a polymer solution discharging means for sending a gas to the filtration passage and the filter before sending the cleaning solution and discharging the polymer solution from the filtration device, and a gas to the filtration passage and the filter after the washing with the washing solution. Therefore, even if the polymer solution remains in the filtration passage and the filter, the filtration passage and the filter can be reliably washed.

  Further, the amount of cleaning liquid component in the gas sent to the filter passage and the filter for drying is detected, the degree of drying is determined based on this detected value, and when it is determined that the drying is completed, a filter replacement command is sent to the filter replacement means. Since the drying determination means for outputting is provided, the filter can be replaced more safely.

  Further, according to the filter replacement method of the filtration device of the present invention, the filtration position where the polymer solution is filtered by sandwiching the filter in the filtration passage, and the opening where the filter can be replaced by opening the filter. In a filter replacement method for a filtration apparatus having a filter clamping member that is displaced between positions, a polymer solution discharge step for sending a gas into the filtration passage and discharging the polymer solution from the filtration passage; and After discharging, a cleaning process for sending the cleaning liquid into the filtration path and cleaning the filtration path and the filter, a drying process for sending the dry gas into the filtration path after cleaning with the cleaning liquid and drying the cleaning liquid for the filtration path and the filter, and a drying process The amount of the cleaning liquid component in the dry gas is detected, and the completion of drying is determined based on this detected value. And a filter replacement process for replacing the filter with the open position, so that harmful gas, polymer solution, and cleaning liquid can be prevented from flowing out to the outside, and the filter can be replaced safely. .

  FIG. 1 is a schematic plan view showing a dope production line 3 which is a part of a solution casting apparatus 2 in which the present invention is implemented. The dope production line 3 includes a solvent tank 4 for storing the solvent, a dissolution tank 5 for mixing the solvent with TAC and the like, a hopper 6 for supplying TAC, and an additive tank for storing the additive. 7, a heating device 8 for heating the swelling liquid 58 as a mixture, which will be described later, a temperature controller 9 for adjusting the temperature of the heated swelling liquid 58, a filtration unit 10, and adjusting the dope concentration A flash device 13 and a post-flush filtration unit 14 are provided. The dope production line 3 is further provided with a recovery device 15 for recovering the solvent and a regeneration device 16 for regenerating the recovered solvent. The dope production line 3 is connected to a stock tank 65.

  Since the filtration unit 10 and the post-flush filtration unit 14 are configured by members having the same structure, only the filtration unit 10 will be described as an example, and the explanation of the post-flush filtration unit 14 will be simplified. The filtration unit 10 includes a first filtration device 11, a second filtration device 12, a filtration control unit 18, a dope switching valve (switching device) 19, an aspirator 20, a cleaning switching valve 25, a cleaning liquid tank 26, a gas tank 27, and a solvent amount detection. A container (drying determination means) 28, a recovery switching valve 29, and a recovery tank 30 are provided. Connected to the filtration control unit 18 are a dope switching valve 19, a solvent amount detector 28, a cleaning switching valve (cleaning means) 25, and a recovery switching valve 29. Each valve 19, 25, 29 is connected to the filtration control unit 18. The switching is controlled by. In the present embodiment, the cleaning switching valve 25 sends gas to the dope passage part 22b before filtration, the dope passage part 22c after filtration, and the filter 21 before sending the cleaning liquid, and the dope (polymer solution) 60 is sent to the first. It also functions as a polymer solution discharging means for discharging from the filtering device 11 and the second filtering device 12, and further sends a gas to the pre-filtration dope passage portion 22b, the post-filtration dope passage portion 22c and the filter 21 after washing with the washing liquid. It also functions as a drying means for drying the cleaning liquid. The number of filtration devices is not limited to two, but may be a plurality (two or more) and may be changed as appropriate. Also, for example, when the number of filtration devices is three, one may be filtered and two may be in a standby state, and two may be filtered and one may be in a standby state. It may be changed as appropriate.

  In the dissolution tank 5, as will be described in detail later, a swelling liquid 58 is obtained, and this swelling liquid 58 is heated by the heating device 8 to become a dope (polymer solution) 60 and is sent to the temperature controller 9. . Then, the temperature of the dope 60 is adjusted by the temperature controller 9 and sent to the dope switching valve (switching device) 19. The dope switching valve 19 switches whether the dope 60 is sent to the first filtration device 11 or the second filtration device 12 of the filtration unit 10 and is controlled by the filtration control unit 18. When the filtration capacity of the filter 21 (see FIG. 2) of the first filtration device 11 detected by a filtration capacity detector (not shown) falls below a preset standard capacity value, the filtration control unit 18 The dope switching valve 19 is switched so as to send the dope 60 to the second filtration device 12. Similarly, when the filtration capacity of the filter 21 of the second filtration device 12 detected by the filtration capacity detector is equal to or less than the reference capacity value, the filtration control unit 18 sends the dope 60 to the first filtration device 11. The dope switching valve 19 is switched so as to send it. Thereby, the dope 60 can be continuously manufactured without stopping the dope manufacturing line 3.

  Since the 1st filtration apparatus 11 and the 2nd filtration apparatus 12 are comprised by the member of the same structure, only the 1st filtration apparatus 11 is demonstrated to an example and description of the 2nd filtration apparatus 12 is simplified. As shown in FIGS. 2 and 3, the first filtration device 11 includes a sheet-like filter 21 that filters the dope 60, five clamping plates (filter clamping members) 22 that sandwich the filter 21, and a used filter. A filter replacement unit (filter replacement means) 23 (see FIG. 4) for replacing the filter 21 with an unused filter 21 is provided. The filter 21 is made of 100% cellulose, and a plurality of through holes having a nominal pore diameter of 10 μm are formed at a predetermined pitch. The sandwiching plate 22 is sandwiched between a sandwiching position (see FIG. 3) as a filtering position for sandwiching the filter 21 and filtering the dope 60 by the sandwiching shift unit 24 and an open position (see FIG. 2) for releasing the sandwiching. Moved. Note that the number of the sandwiching plates 22 is not limited to five and can be changed as appropriate.

  The sandwiching plate 22 is formed with an inlet 22a, a pre-filtration dope passage portion (filtration passage) 22b, a post-filtration dope passage portion (filtration passage) 22c, and a discharge port 22d. When the unfiltered dope 60 sent from the dope switching valve 19 through the cleaning switching valve 25 is injected from the injection port 22a, the unfiltered dope 60 passes through the unfiltered dope passage portion 22b, and the filter 21 The filtered dope 60 passes through the filtered dope passage 22c and is discharged from the discharge port 22d.

  The dope 60 before filtration sent from the dope switching valve 19 is sent to each inlet 22 a of the first to fourth clamping plates 22. When the filter 21 is sandwiched between the five sandwich plates 22, the dope 60 injected from the inlet 22 a of the first sandwich plate 22 is filtered by the filter 21, and the discharge port 22 d of the second sandwich plate 22. Discharged from. Similarly, the dope 60 injected from the injection port 22a of the second clamping plate 22 is filtered by the filter 21, and from the discharge port 22d of the third clamping plate 22, the injection port 22a of the third clamping plate 22 The dope 60 injected from is filtered by the filter 21, the dope 60 injected from the outlet 22d of the fourth clamping plate 22 and the inlet 22a of the fourth clamping plate 22 is filtered by the filter 21, It discharges | emits from the discharge port 22d of the 5th clamping board 22, respectively. The first sandwiching plate 22 is the uppermost one in FIG. 3, the second sandwiching plate 22 is the second from the top in FIG. 3, and the third sandwiching plate 22 is the one in FIG. In FIG. 3, the fourth step from the top in FIG. 3 is the fourth step from the top, and the fifth step 22 is the fifth step from the top in FIG. Each is shown.

  As shown in FIG. 1, a suction device 20 is provided in the vicinity of the first and second filtration devices 11 and 12. The suction device 20 sucks air around the first and second filtration devices 11 and 12. Thereby, even when harmful gas is generated from the first and second filtration devices 11 and 12, it is possible to prevent the gas from flowing out to the outside (atmosphere). The air sucked by the suction device 20 is filtered by a filter (not shown) and discharged. Instead of sucking air with the suction device 20, a shielding cover that covers the first and second filtration devices 11 and 12 may be provided to prevent gas from flowing out.

  A cleaning switching valve 25 is provided upstream of the first and second filtration devices 11 and 12, and a cleaning liquid tank 26 and a gas tank 27 are connected to the cleaning switching valve 25. The cleaning switching valve 25 is connected to the filtration control unit 18, and switching is controlled by the filtration control unit 18. By switching the cleaning switching valve 25, either the cleaning liquid stored in the cleaning liquid tank 26 and the inert gas (for example, nitrogen gas) as the gas stored in the gas tank 27, or the dope 60 is first to fourth. Are sent to the respective inlets 22 a of the sandwiching plate 22.

  When the first to fifth clamping plates 22 of the first and second filtration devices 11 and 12 are washed, first, the washing control valve 25 is switched by the filtration control unit 18, and nitrogen gas (gas) is supplied from the gas tank 27. Is sent to the inlet 22a of the clamping plate 22. Nitrogen gas is injected into the inlet 22a of the first to fourth clamping plates 22 at a pressure of 0.3 to 1.0 MPa. The nitrogen gas injected from the inlet 22a of the first clamping plate 22 passes through the pre-filtration dope passage portion 22b of the first clamping plate 22 and is sent to the post-filtration dope passage portion 22c of the second clamping plate 22. It is done. By this nitrogen gas, the residual liquid of the dope 60 remaining inside the pre-filtration dope passage portion 22b of the first clamping plate 22, the residual liquid of the dope 60 adhering to the filter 21, and the second clamping The residual liquid of the dope 60 remaining inside the dope passage portion 22c after filtration of the plate 22 is blown off and discharged from the discharge port 22d of the second sandwich plate 22. Similarly, the residual liquid of the dope 60 remaining inside by the nitrogen gas injected from the inlet 22a of the second to fourth clamping plates 22 is discharged to the outlet 22d of the third to fifth clamping plates 22. Discharged from.

  Next, the cleaning control valve 18 is switched by the filtration control unit 18, and the cleaning liquid is sent from the cleaning liquid tank 26 to the inlet 22 a of the first to fourth clamping plates 22. The cleaning liquid injected from the inlet 22a of the first clamping plate 22 passes through the dope passage part 22b before filtration of the first sandwiching plate 22 and the filter 21, and passes through the dope passage part 22c after filtration of the second clamping plate 22. And discharged from the discharge port 22d of the second clamping plate 22. Similarly, the cleaning liquid injected from the inlet 22 a of the second to fourth clamping plates 22 is discharged from the outlet 22 d of the third to fifth clamping plates 22. The cleaning liquid stored in the cleaning liquid tank 26 is for cleaning the pre-filtration dope passage portion 22b, the used filter 21, and the post-filtration dope passage portion 22c (hereinafter referred to as the inside of the sandwich plate 22). Is the same as the organic solvent of the swelling liquid 58 described later.

  After the inside of the first to fifth clamping plates 22 of the first and second filtration devices 11 and 12 is washed with the washing liquid, the washing control valve 25 is switched by the filtration control unit 18 and nitrogen gas is injected again from the gas tank 27. Send to inlet 22a.

  Solvent amount detectors (drying determination means) 28 are provided on the downstream side of the first filtration device 11 and the downstream side of the second filtration device 12, respectively. The solvent amount detector 28 is sent from the gas tank 27 to the inlet 22a of the sandwiching plate 22, and passes through the dope passage part 22b before filtration, the filter 21, and the dope passage part 22c after filtration and discharged from the outlet 22d. The amount of solvent (the amount of cleaning liquid component) is detected, and the degree of drying inside the sandwiching plate 22 is determined. When the detected solvent amount is equal to or less than a preset reference solvent amount (for example, 5%), it is determined that the solvent has been dried, and a drying signal is sent to the filtration control unit 18. The filtration control unit 18 switches the cleaning switching valve 25 based on the sent dry signal, and stops the injection of nitrogen gas from the gas tank 27 into the inlet 22a. Then, the clamping plate 22 is moved to an open position (see FIG. 2) where the clamping of the filter 21 is released by the clamping shift unit 24 (see FIG. 3), and the filter 21 is exchanged. Thereby, when the clamping plate 22 is moved to the open position, there is no residual liquid of the dope 60 or the cleaning liquid inside the clamping plate 22, and no gas is generated. It is safe even in the presence of gas, and it is possible to prevent the atmosphere from being polluted by the generation of gas.

  A recovery switching valve 29 is provided on the downstream side of each of the two solvent quantity detectors 28, and a recovery tank 30 is connected to the recovery switching valve 29. The recovery switching valve 29 is connected to the filtration control unit 18, and switching is controlled by the filtration control unit 18. By switching the recovery switching valve 29, the cleaning liquid is sent to the recovery tank 30, and the dope 60 is sent to the stock tank 65 in the solution film-forming facility 2 via the valve 61 and stored therein. The cleaning liquid that has cleaned the insides of the first to fifth clamping plates 22 of the first and second filtration devices 11 and 12 is collected in the collection tank 30. Thereby, the dope 60 and the cleaning liquid are not mixed. The recovery tank 30 is connected to the solvent tank 4, and the cleaning liquid recovered in the recovery tank 30 is filtered by a filter (not shown), and then sent to the solvent tank 4 to be regenerated.

  As shown in FIG. 4, the filter replacement unit 23 includes a transport pickup 31 and a recovery pickup 32. The transport pickup 31 is for transporting the unused filter 21 placed on the filter mount 33 onto the clamping plate 22, and includes a pickup body 34, a transport suction pad (suction holding unit) 35, and movement A plate 36. In the present embodiment, the displacement portion that displaces the transport suction pad 35 in the state in which the filter 21 is sucked up includes the pickup body 34 and the moving plate 36.

  The conveyance suction pad 35 for sucking the filter 21 is rotatably attached to the pickup main body 34 around the rotation shaft 35a. The pickup main body 34 is provided with two shafts 34a, and a moving plate 36 is attached to the shaft 34a so as to be movable in the vertical direction. An elongated insertion hole 36a is formed in the moving plate 36, and the insertion shaft 35b of the transport suction pad 35 is inserted into the insertion hole 36a. As a result, when the moving plate 36 moves in the vertical direction, the transport suction pad 35 rotates about the rotation shaft 35a. A plurality of unused filters 21 are stacked on the filter mount 33. The collection pickup 32 sucks the used filter 21 placed on the sandwiching plate 22 and conveys it to the collection case 37.

  The conveyance pickup 31 is driven by a conveyance control unit 41. The transport pickup 31 is located between a transport suction position where the unused filter 21 placed on the filter mounting base 33 is sucked by the transport suction pad 35 and a placement position where the sucked unused filter 21 is placed on the sandwiching plate 22. Move with. In the present embodiment, the filter setting means for setting the unused filter 21 to the holding plate 22 at the open position where the used filter 21 is collected is constituted by the transport pickup 31 and the transport control unit 41. The

  When the unused filter 21 is sucked by the transport pickup 31, as shown in FIG. 5A, first, a plurality of unused filters stacked on the filter mount 33 are placed on the bottom surface of the transport suction pad 35. 21 is brought into contact with the upper surface of the uppermost filter 21 (conveying suction position). Next, the filter 21 is sucked by the transport suction pad 35. Examples of the suction method using the transport suction pad 35 include a suction blower and an ejector. However, the suction method is not limited thereto, and it is sufficient that the filter 21 can be sucked. The filter 21 is formed in a thin plate shape, and the filter 21 positioned below the filter 21 sucked by the transport suction pad 35 may also be sucked. In order to prevent this, the conveyance suction pad 35 is rotated in the direction A in FIG. 5 about the rotation shaft 35a. In order to rotate the conveyance suction pad 35, as shown in FIG. 5B, the moving plate 36 is moved upward. When the moving plate 36 moves upward, the transport suction pad 35 rotates in the direction A in FIG. 5 about the rotation shaft 35a. Thereby, only one filter 21 sucked by the transport suction pad 35 can be transported. Then, the transport pickup 31 in a state where the filter 21 is sucked by the transport suction pad 35 is moved to the loading position by the transport control unit 41. When the suction by the transport suction pad 35 is released after the movement to the placement position, the filter 21 is placed on the sandwiching plate 22.

  As shown in FIG. 4, the recovery pickup 32 picks up the used filter 21 placed on the sandwiching plate 22, accommodates it in the recovery case 37, and recovers it. A clip 38 that holds the filter 21. And is driven by the collection control unit 42. The recovery pickup 32 includes a gripping position for gripping the used filter 21 placed on the sandwiching plate 22 with the clip 38, and a recovery housing position for storing the gripped used filter 21 in the recovery case 37 for recovery. Move between. The clip 38 is provided so as to be movable up and down. When the clip 38 is moved downward in a state where the clip 38 is placed on the filter placement portion 32a of the collection pickup 32, the filter 21 is gripped.

  The used filter 21 placed on the holding plate 22 is gripped by the clip 38 (the clip 38 is moved downward), and the collection pickup 32 is moved to the collection accommodation position by the collection control unit 42. When the gripping by the clip 38 is released after moving to the collection housing position (the clip 38 is moved upward), the used filter 21 is housed in the collection case 37 and collected. In the present embodiment, the recovery means for recovering the used filter 21 from the clamping plate 22 includes a recovery pickup 32 and a recovery control unit 42. The collection pickup 32 only needs to be able to pick up the filter 21, accommodate it in the collection case 37, and collect it. The pin 21 is inserted into the filter 21 to pick up the used filter 21, and the pin is removed to remove the filter 21. May be accommodated in the collection case 37 and collected.

  The flow of the operation of the filtration unit 10 will be described using the flowchart shown in FIG. The filtration capacity detector detects the filtration capacity of the filter 21 of the filtration apparatus (for example, the first filtration apparatus 11) to which the dope 60 is sent. When the detected filtration capacity value becomes equal to or less than the reference capacity value, the filtration control unit 18 switches the dope switching valve 19 and sends the dope 60 to the second filtration device 12. And the washing | cleaning switching valve | bulb 25 is switched and nitrogen gas is sent to the 1st filtration apparatus 11 from the gas tank 27 for the preset time (for example, 30 minutes-120 minutes) (polymer solution discharge process). Next, the cleaning switching valve 25 is switched to send the cleaning liquid from the cleaning liquid tank 26 to the first filtration device 11 (cleaning step). After washing the first filtration device 11 with the washing liquid, the washing switching valve 25 is switched, and nitrogen gas is sent again from the gas tank 27 to the first filtration device 11 (drying step). The solvent amount detector 28 detects the solvent amount of nitrogen gas discharged from the discharge port 22 d of the first filtration device 11. If the detected solvent amount is equal to or less than the reference solvent amount, it is determined that the inside of the sandwiching plate 22 has been dried, and a drying signal is sent to the filtration control unit 18. The filtration control unit 18 switches the cleaning switching valve 25 based on the sent drying signal, and stops sending nitrogen gas from the gas tank 27. Next, the clamping plate 22 is moved to the open position (see FIG. 2) by the clamping shift unit 24. Then, the filter replacement unit 23 replaces the used filter 21 with an unused filter 21 (filter replacement process). Similarly, when the filtration capacity value of the second filtration device 12 is equal to or less than the reference capacity value, the dope 60 is sent to the first filtration device 11 and the used filter after the second filtration device 12 is washed. 21 is replaced with an unused filter 21.

  Thus, since the dope 60 is sent to one of the first filtration device 11 and the second filtration device 12, the dope 60 can be continuously produced without stopping the dope production line 3. it can. Furthermore, when the clamping plate 22 is moved to the open position, there is no residual dope 60 or cleaning liquid in the clamping plate 22 (the pre-filtration dope passage 22b, the used filter 21 and the post-filtration dope passage 22c). In addition, since the residual liquid does not flow out of the sandwiching plate 22 and gas is not generated, it is safe even when there is an operator around the solution film-forming facility 2, and further, due to the generation of gas The air can be prevented from being polluted.

  In addition, in the said embodiment, although the sheet-like filter 21 was used, you may use the roll filter wound by roll shape, without being limited to this, The filtration capability of the part which the roll filter is using When the value is equal to or less than the reference capacity value, the unused portion is positioned on the sandwiching plate 22 by rotating the roll filter.

  Next, the manufacturing method of the said swelling liquid 58 and the dope 60 is demonstrated. However, the manufacturing method and manufacturing apparatus described below are examples of the present invention, and the present invention is not limited thereto.

[material]
In the present embodiment, cellulose acylate is used as the polymer, and triacetyl cellulose (TAC) is particularly preferable as the cellulose acylate. The TAC may be obtained from either linter cotton or pulp cotton, but is preferably obtained from linter cotton. Among cellulose acylates, those in which the substitution degree of the acyl group substituted with the hydroxyl group of cellulose satisfies all of the following formulas (I) to (III) are more preferable. In the following formulas (I) to (III), A and B represent the substitution degree of the acyl group substituted with the hydroxyl group of cellulose, A is the substitution degree of the acetyl group, and B is 3 carbon atoms. The substitution degree of the acyl group of ˜22. In addition, it is preferable that 90 mass% or more of TAC is a particle | grain of 0.1 mm-4 mm. The polymer used in the present invention is not limited to cellulose acylate.
(I) 2.5 ≦ A + B ≦ 3.0
(II) 0 ≦ A ≦ 3.0
(III) 0 ≦ B ≦ 2.9

  In the solvent tank 4, a mixed liquid of methylene chloride and alcohol is stored as a solvent for preparing the dope 60. At this time, the content of the alcohol is preferably 2% by mass to 25% by mass and more preferably 5% by mass to 20% by mass with respect to the entire solvent. Specific examples of the alcohol include methanol, ethanol, n-propanol, isopropanol, n-butanol, etc. Among them, methanol, ethanol, n-butanol, or a mixture thereof is more preferably used. The solvent is not limited to the above-mentioned mixed liquid of methylene chloride and alcohol, but is an aromatic hydrocarbon (for example, benzene, toluene, etc.), a halogenated hydrocarbon (for example, dichloromethane, chlorobenzene, etc.), an alcohol. , Ketones (eg, acetone, methyl ethyl ketone, etc.), esters (eg, methyl acetate, ethyl acetate, propyl acetate, etc.) and ethers (eg, tetrahydrofuran, methyl cellosolve, etc.). Here, the dope is a polymer solution or dispersion obtained by dissolving or dispersing a polymer in a solvent.

  The details of cellulose acylate are described in paragraphs [0140] to [0195] of Japanese Patent Application No. 2004-264464. These descriptions are also applicable to the present invention. The same applies to additives such as solvents and plasticizers, deterioration inhibitors, UV absorbers (UV agents), optical anisotropy control agents, retardation control agents, dyes, matting agents, release agents, release accelerators, etc. The details are described in paragraphs [0196] to [0516] of Japanese Patent Application No. 2004-264464.

[Dope production method]
First, the dope 60 is manufactured using the above raw materials. In this embodiment, the dope 60 is manufactured by the following method using the dope manufacturing line 3 shown in FIG. First, the valve 51 is opened, and the solvent is sent from the solvent tank 4 to the dissolution tank 5. Next, the TAC contained in the hopper 6 is fed into the dissolution tank 5 while being measured. Further, the required amount of the additive solution is sent from the additive tank 7 to the dissolution tank 5 by opening and closing the valve 52. In this embodiment, the dope 60 is mixed so that TAC is 20.0% by weight, the plasticizer is 11.0% by weight (= 2.2% by weight) of the TAC, and the solvent is 77.8% by weight. Is done.

  In addition to the method of sending the additive as a solution, for example, when the additive is liquid at room temperature, it can be sent to the dissolution tank 5 in the liquid state. Further, when the additive is solid, a method of feeding into the dissolution tank 5 using a hopper or the like is also possible. When a plurality of types of additives are added, a solution in which a plurality of types of additives are dissolved can be placed in the additive tank 7. Alternatively, a solution in which an additive is dissolved can be put in each of a plurality of additive tanks and sent to the dissolution tank 5 through independent pipes.

  In the above description, the order of putting in the dissolution tank 5 is the solvent (used in the meaning including the case of the mixed solvent), TAC, and additive, but is not limited to this order. For example, a preferred amount of solvent can be fed after the TAC is metered into the dissolution tank 5. Further, it is not always necessary to add the additive to the dissolution tank 5 in advance, and it can be mixed with a mixture of TAC and a solvent (hereinafter, the mixture may also be referred to as a dope) in a later step.

  As shown in FIG. 1, the dissolution tank 5 includes a jacket 53 that wraps the outer surface thereof, and a first stirrer 55 that is rotated by a motor 54. Furthermore, it is preferable that a second agitator 57 that is rotated by a motor 56 is attached to the dissolution tank 5. The first stirrer 55 is preferably provided with anchor blades, and the second stirrer 57 is preferably a dissolver type eccentric stirrer. And the melting tank 5 used by this embodiment is temperature-controlled by flowing a heat-transfer medium inside the jacket 53, The preferable temperature range is the range of -10 degreeC-55 degreeC. By appropriately selecting and using the types of the first stirrer 55 and the second stirrer 57, the swelling liquid 58 in which the TAC is swollen in the solvent is obtained.

  Next, the swelling liquid 58 is sent to the heating device 8 by the pump 59. The heating device 8 is preferably a jacketed pipe, and further preferably has a configuration capable of pressurizing the swelling liquid 58. By using such a heating device 8, the solid content in the swelling liquid 58 is dissolved under heating conditions or pressurized heating conditions. Thereby, the dope 60 is manufactured. In this case, the temperature of the swelling liquid 58 is preferably 50 ° C to 120 ° C. Moreover, the cooling dissolution method which cools the swelling liquid 58 to the temperature of -100 degreeC--30 degreeC can also be performed. And after making dope 60 into substantially room temperature with the temperature controller 9, it filters by the 1st filtration apparatus 11 or the 2nd filtration apparatus 12 of the filtration unit 10, and the impurity contained in the dope 60 is removed. The dope 60 after filtration is sent to the stock tank 65 in the solution casting equipment 2 via the valve 61 and stored therein.

  When the dope 60 is being filtered by the first filtration device 11 of the filtration unit 10, if the filtration capacity of the filter 21 detected by the filtration capacity detector is less than or equal to a preset capacity value, the dope switching is performed. The valve 19 is switched to send the dope 60 to the second filtration device 12. And as above-mentioned, after wash | cleaning the clamping board 22 of the 1st filtration apparatus 11, the filter 21 is replaced | exchanged for the new filter 21 by the filter replacement | exchange unit 23. FIG.

  By the way, as mentioned above, once the swelling liquid 58 is prepared and then the swelling liquid 58 is used as a solution, the time required increases as the concentration of TAC is increased, which is a problem in terms of manufacturing cost. There is. In that case, it is preferable to prepare a dope having a concentration lower than the target concentration and then perform a concentration step for obtaining the target concentration. When using such a method, the dope 60 filtered by the filtration unit 10 is sent to the flash device 13 via the valve 61, and a part of the solvent in the dope is evaporated in the flash device 13. The solvent gas generated by the evaporation is condensed by a condenser (not shown) to become a liquid and recovered by the recovery device 15. The recovered solvent is regenerated and reused as a solvent for dope preparation by the regenerator 16. This reuse is effective in terms of cost.

  The concentrated dope 60 is extracted from the flash unit 13 by the pump 62. Furthermore, it is preferable that a bubble removal process for removing bubbles generated in the dope 60 is performed. As this defoaming method, various known methods are applied, for example, an ultrasonic irradiation method. The dope 60 is subsequently sent to the filtration unit 14 after flushing to remove foreign matters. In addition, it is preferable that the temperature of dope 60 in the case of filtration is 0 degreeC-200 degreeC. Then, the filtered dope 60 is sent to the stock tank 65 and stored. The dope 60 in the stock tank 65 is sent to the pump 73.

  It is preferable to mix the raw material dope and an additive liquid (for example, an ultraviolet absorber liquid) added to the raw material dope using an in-line mixer (for example, a static mixer) that mixes during the transfer. It is more preferable to perform mixing by connecting a plurality of in-line mixers having different mixing methods in series.

  As the in-line mixer, it is preferable to include at least one of a static mixer and a through the mixer. When the static mixer is provided, the number of elements of the static mixer is preferably 6 or more and 9 or less, and more preferably 6 or more and 60 or less.

  In the case where both a static mixer and a slew mixer are provided, the slew mixer is preferably arranged on the upstream side of the static mixer. Further, the distance between the through-the-mixer and the addition port for adding the additive liquid is preferably 5 mm or more and 150 mm or less, and further, the distance between the through-the-mixer and the addition port for adding the additive liquid is 5 mm or more and 15 mm or less. Is more preferable. Moreover, it is preferable that the upstream edge part of the element which comprises a through-zer mixer is located in the inner wall vicinity of the piping through which the said raw material dope flows.

  Furthermore, it is preferable that a first filtration device for filtering the raw material dope is provided on the upstream side of the in-line mixer, and an additive is added to the raw material dope after filtration by the first filtering device, and further, the downstream side of the in-line mixer It is more preferable that a second filtering device for filtering the dope is provided, and the dope mixed by the in-line mixer is filtered by the second filtering device.

In the present embodiment, it is preferable that the following is satisfied.
(1) When the flow rate of the additive solution is V1 and the flow rate of the raw material dope is V2, 1 ≦ V1 / V2 ≦ 5.
(2) The additive ratio of the additive liquid is 0.1% to 50% in flow rate ratio.
(3) When the viscosity of the additive solution is N1 and the viscosity of the raw material dope is N2, 1000 ≦ N2 / N1 ≦ 100000 is satisfied, and at 20 ° C., 5000 cP ≦ N1 ≦ 500000 cP, and 0 .1 cP ≦ N2 ≦ 100 cP.
(4) The shear rate of the raw material dope is 0.1 (1 / s) to 30 (1 / s).
(5) The polymer is cellulose acylate.
(6) The additive solution is a solution containing the main solvent of the polymer solution.
(7) The additive solution is a solution containing the main solvent of the polymer solution and has a composition different from that of the raw material dope.
(8) The additive solution is a solution containing the main solvent of the polymer solution, and contains at least one ultraviolet absorber.
(9) The additive solution is a solution containing the main solvent of the polymer solution, and is formed by dispersing at least one kind of inorganic or organic fine particles.
(10) The additive solution is a solution containing the main solvent of the polymer solution and contains at least one type of peeling accelerator.
(11) The additive solution is a solution containing the main solvent of the polymer solution and contains at least one kind of poor solvent.

  By the above method, the dope 60 whose TAC concentration is 5 mass% to 40 mass% can be manufactured. More preferably, the TAC concentration is from 15% by mass to 30% by mass, and most preferably from 17% by mass to 25% by mass. The concentration of the additive (mainly a plasticizer) is preferably in the range of 1% by mass or more and 20% by mass or less when the total solid content in the dope 60 is 100% by mass. In addition, from the [0517] paragraph of Japanese Patent Application No. 2004-264464 about the raw material in the solution casting method which obtains a TAC film, the raw material, the additive dissolution method and addition method, the filtration method, and the dope production methods such as defoaming [0616] The paragraph is detailed. These descriptions are also applicable to the present invention.

[Solution casting method]
Next, a method for producing a film using the dope 60 obtained above will be described. FIG. 7 is a schematic view showing the solution casting apparatus 2. However, the present invention is not limited to the solution casting apparatus as shown in FIG. The solution casting equipment 2 includes a stock tank 65, a filtration unit 74, a casting die 80, a casting band 83 stretched around rotating rollers 81 and 82, and a tenter device 110. Further, an ear clip device 112, a drying chamber 115, a cooling chamber 117, and a winding chamber 120 are arranged.

  An agitator 72 that is rotated by a motor 71 is attached to the stock tank 65. The stock tank 65 is connected to the casting die 80 via a pump 73 and a filtration unit 74. Since the filtration unit 74 filters the dope 60 and is composed of members having the same structure as the filtration unit 10, the description thereof is simplified.

The material of the casting die 80 is preferably double-layer stainless steel or precipitation hardening stainless steel, and preferably has a thermal expansion coefficient of 2 × 10 ⁻⁵ (° C. ⁻¹ ) or less. And what has corrosion resistance substantially equivalent to SUS316 in the forced corrosion test with electrolyte aqueous solution can be used as the material of the casting die 80, and further immersed in a mixed solution of dichloromethane, methanol and water for 3 months. Even if it has corrosion resistance, no pitting (perforation) occurs at the gas-liquid interface. Furthermore, it is preferable that the casting die 80 is manufactured by grinding a material that has passed one month or more after casting. This prevents the dope 60 from flowing uniformly in the casting die 80 and prevents streaks and the like from occurring in the casting film described later. The finishing accuracy of the liquid contact surface between the casting die 80 and the feed block described later is preferably 1 μm or less in terms of surface roughness and the straightness is 1 μm / m or less in any direction. The clearance of the slit of the casting die 80 can be adjusted in the range of 0.5 mm to 3.5 mm by automatic adjustment. About the corner | angular part of the liquid-contact part of the lip | tip end of the casting die 80, the R shall be 50 micrometers or less over the whole width. Moreover, it is preferable that the shear rate inside the casting die 80 is adjusted to be 1 (1 / sec) to 5000 (1 / sec).

  The width of the casting die 80 is not particularly limited, but is preferably about 1.1 to 2.0 times the width of the film as the final product. Further, it is preferable to attach a temperature controller to the casting die 80 so that the temperature during film formation is maintained at a predetermined temperature. The casting die 80 is preferably a coat hanger type. Furthermore, it is more preferable that thickness adjusting bolts (heat bolts) are provided at predetermined intervals in the width direction of the casting die 80 and the casting die 80 is provided with an automatic thickness adjusting mechanism using heat bolts. The heat bolt is preferably subjected to film formation by setting a profile according to the amount of pump 73 (preferably a high precision gear pump) according to a preset program. Further, feedback control may be performed by an adjustment program based on a profile of a thickness meter (for example, an infrared thickness meter) (not shown) in the solution casting equipment 2. The thickness difference between any two points in the width direction of the product film, excluding the casting edge portion, is adjusted within 1 μm, and the difference between the minimum value and the maximum value in the width direction thickness is adjusted to 3 μm or less. Preferably, adjusting to 2 μm or less is more preferable. In addition, it is preferable to use a lip gap whose accuracy is adjusted to ± 50 μm or less.

More preferably, a cured film is formed at the lip end of the casting die 80. A method for forming the cured film is not particularly limited, and examples thereof include ceramic coating, hard chrome plating, and a nitriding method. When ceramics are used as the cured film, those that can be ground, have low porosity, are not brittle, have good corrosion resistance, have good adhesion to the casting die 80, and have no adhesion to the dope 60 are preferable. Specifically, tungsten carbide (WC), Al ₂ O ₃ , TiN, Cr ₂ O _{3 and the} like can be mentioned, among which WC is particularly preferable. The WC coating can be performed by a thermal spraying method.

  In order to prevent the dope 60 flowing out to the slit end of the casting die 80 from being locally dried and solidified, a solvent supply device (not shown) is preferably attached to the slit end. In this case, a solvent for solubilizing the dope 60 (for example, a mixed solvent of 86.5 parts by mass of dichloromethane, 13 parts by mass of acetone, and 0.5 parts by mass of n-butanol) is formed at both ends of the casting bead and at the end of the die slit. It is preferable to supply near the periphery of the three-phase contact line formed by the part and outside air. Supplying at 0.1 mL / min to 1.0 mL / min to each one side of the end is preferable in order to prevent mixing of foreign matters into the cast film. In addition, as a pump which supplies this liquid, it is preferable to use a pump with a pulsation rate of 5% or less.

  A casting band 83 is provided below the casting die 80 so as to span the rotating rollers 81 and 82. The rotating rollers 81 and 82 are rotated by a driving device (not shown), and the casting band 83 travels endlessly with the rotation. It is preferable that the casting band 83 can move at a moving speed, that is, a casting speed of 10 m / min to 200 m / min. Further, in order to set the surface temperature of the casting band 83 to a predetermined value, it is preferable that a heat transfer medium circulation device 84 is attached to the rotary rollers 81 and 82, and the surface temperature of the casting band 83 is It is preferable that the temperature can be adjusted to -20 ° C to 40 ° C. A heat transfer medium flow path (not shown) is formed in the rotary rollers 81 and 82 used in the present embodiment, and the heat transfer medium maintained at a predetermined temperature passes through the flow path. Thus, the temperature of the rotating rollers 81 and 82 is maintained at a predetermined value.

It is also possible to use the rotating rollers 81 and 82 directly as a support. In this case, it is preferable that the rotation can be performed with high accuracy so that the rotation speed variation is 0.2% or less. In this case, it is preferable that the average roughness of the surfaces of the rotating rollers 81 and 82 is 0.01 μm or less. It is preferable to perform a hard chrome plating process or the like on the surfaces of the rotary rollers 81 and 82, thereby further providing sufficient hardness and durability. In addition, it is preferable to suppress the surface defects of the support (the casting band 83 and the rotating rollers 81 and 82) to the minimum. Specifically, there is no pinhole of 30 μm or more, and the number of pinholes of 10 μm or more and less than 30 μm is 1 / m ² or less, and the number of pinholes of less than 10 μm is preferably ² / m ² or less.

  Casting devices such as the casting die 80 and the casting band 83 are accommodated in the casting chamber 85. The casting chamber 85 is provided with a temperature control facility 86 for keeping the internal temperature at a predetermined value, and a first condenser (condenser) 87 for condensing and recovering the volatile organic solvent. Yes. A recovery device 88 for recovering the condensed organic solvent is provided outside the casting chamber 85. Further, it is preferable that a decompression chamber 90 for controlling the pressure of the back surface of the casting bead formed from the casting die 80 to the casting band 83 is disposed, and this is also used in this embodiment. .

  Further, blowers 91, 92, and 93 are provided to evaporate the solvent in the casting film 89. The mounting position of the blower is illustrated in a form in which the blower 91 is provided on the upper upstream side of the casting band 83, the blower 92 is provided on the downstream side, and the blower 93 is provided on the lower side of the casting band 83. is not. Further, it is preferable that a wind shield device 94 is provided in order to suppress the surface variation of the film surface caused by blowing dry air to the casting film 89 immediately after formation.

  The crossover portion 100 is provided with a blower 101, and the ear clip device 112 downstream of the tenter device 110 is provided with a crusher 113 for finely cutting the side edge scraps of the cut film 111. .

  The drying chamber 115 is provided with a number of rollers 114, and an adsorption / recovery device 116 for adsorbing / recovering the solvent gas generated by evaporation is attached. In FIG. 2, the cooling chamber 117 is provided downstream of the drying chamber 115, but a humidity control chamber (not shown) may be provided between the drying chamber 115 and the cooling chamber 117. A forced static elimination device (static elimination bar) 118 for adjusting the charged voltage of the film 111 to a predetermined range (for example, −3 kV to +3 kV) is provided downstream of the cooling chamber 117. In FIG. 9, an example in which the forced static elimination device 118 is on the downstream side of the cooling chamber 117 is illustrated, but is not limited to this installation position. Furthermore, in this embodiment, a knurling application roller 119 for applying knurling to both edges of the film 111 by embossing is appropriately provided downstream of the forced static elimination device 118. The winding chamber 120 includes a winding roller 121 for winding the film 111 and a press roller 122 for controlling the tension at the time of winding.

  Next, an example of a method for producing a film using the solution casting apparatus 2 as described above will be described below. The dope 60 is always made uniform by the rotation of the stirrer 72. The dope 60 may be mixed with additives such as a plasticizer and an ultraviolet absorber during the stirring.

Then, the dope 60 is sent to the filtration unit 74 by the pump 73 and filtered there, and then cast from the casting die 80 to the casting band 83. The driving of the rotating rollers 81 and 82 is preferably adjusted so that the tension generated in the casting band 83 is 10 ⁴ N / m to 10 ⁵ N / m. Further, the relative speed difference between the casting band 83 and the rotary rollers 81 and 82 is adjusted to be 0.01 m / min or less. It is preferable that the speed fluctuation of the casting band 83 is 0.5% or less, and the meandering in the width direction that occurs when the casting band 83 makes one rotation is 1.5 mm or less. In order to suppress this meandering, it is more preferable to provide a detector (not shown) for detecting the positions of both ends of the casting band 83 and to control the speed of the rotating roller by feedback control based on the measured value. Further, it is preferable to adjust the casting band 83 immediately below the casting die 80 so that the vertical position fluctuation accompanying the rotation of the rotary roller 81 is 200 μm or less. Further, the temperature of the casting chamber 85 is preferably set to −10 ° C. to 57 ° C. by the temperature control equipment 86. The solvent evaporated inside the casting chamber 85 is recovered by the recovery device 88 and then regenerated and reused as a dope preparation solvent.

  A casting bead is formed from the casting die 80 to the casting band 83, and a casting film 89 is formed on the casting band 83. The temperature of the dope 60 during casting is preferably −10 ° C. to 57 ° C. In order to stabilize the casting bead, the back surface of the bead is preferably controlled to a predetermined pressure value by the decompression chamber 90. It is preferable that the bead back surface is depressurized by −10 Pa to −1500 Pa than the front surface. Furthermore, it is preferable to attach a jacket (not shown) to the decompression chamber 90 and control the temperature so that the internal temperature is kept at a predetermined temperature. In order to keep the shape of the casting bead desired, it is preferable to attach a suction device (not shown) to the edge portion of the casting die 80. This edge suction air volume is 1 L / min. ~ 100 L / min. It is preferable that it is the range of these.

  After the casting film 89 has self-supporting properties, the casting film 89 is peeled off from the casting band 83 while being supported by the peeling roller 95 as a wet film (polymer film) 96. The amount of residual solvent at the time of stripping is preferably 20% by mass to 250% by mass based on the solid content. Thereafter, after the transfer section 100 provided with a large number of rollers is conveyed, the wet film 96 is fed into the tenter device 110. In the transition part 100, the drying of the wet film 96 is advanced by sending the drying air of desired temperature from the air blower 101. FIG. At this time, the temperature of the drying air is preferably 20 ° C to 250 ° C.

  The wet film 96 sent to the tenter device 110 is dried while being conveyed while being gripped by clips at both ends. In addition, in at least any one of the transition part 100 and the tenter apparatus 110, it is preferable to extend | stretch at least 1 direction of the casting direction and the width direction of the wet film 96 by 100.5%-300%.

  The wet film 96 is dried to a predetermined residual solvent amount by the tenter device 110 and then sent out downstream as the film 111. Both edges of the film 111 are cut at both edges by the edge cutting device 112, and the cut side edges are sent to the crusher 113 by a cutter blower (not shown). The crusher 113 pulverizes the side edges to form chips. Since this chip is reused for dope preparation, this method is effective in terms of cost. In addition, although it can also abbreviate | omit about the cutting process of this both-sides edge part, it is preferable to carry out in any one from the said casting process to the process of winding up the said film.

  On the other hand, in this embodiment, the film 111 from which both end portions have been cut and removed is sent to the drying chamber 115 and further dried. The temperature in the drying chamber 115 is not particularly limited. In the drying chamber 115, the film 111 is conveyed while being wound around a roller 114, and the solvent gas generated by evaporation here is adsorbed and collected by an adsorption recovery device 116. The air from which the solvent component has been removed is blown again as dry air inside the drying chamber 115. The drying chamber 115 is more preferably divided into a plurality of sections in order to change the drying temperature. In addition, when a preliminary drying chamber (not shown) is provided between the ear opener 112 and the drying chamber 115 and the film 111 is preliminarily dried, the film temperature is prevented from rising rapidly in the drying chamber 115. The shape change of the film 111 can be further suppressed.

  The film 111 is cooled to substantially room temperature in the cooling chamber 117. Note that a humidity control chamber (not shown) may be provided between the drying chamber 115 and the cooling chamber 117, and in this humidity control chamber, air adjusted to a desired humidity and temperature can be blown onto the film 111. It is preferable. Thereby, generation | occurrence | production of the curling of the film 111 and the winding-up defect at the time of winding can be suppressed.

  In the solution casting method, various steps such as a drying step and a side edge cutting and removing step are performed before the film (polymer film) peeled off from the support is wound up. In each of these processes or between each process, the film is mainly supported or conveyed by a roller. These rollers include a driving roller and a non-driving roller, and the non-driving roller is mainly used for determining a film conveyance path and improving conveyance stability.

  On the other hand, the drive roller is used to transmit drive to the film and convey it downstream, and a suction roller is usually used. In film transport in film formation, separation of transport tension may be necessary within each process such as casting process, stripping process, drying process, winding process, etc., and in that case, suction Separation of conveyance tension is achieved by applying a driving force to the film by a roller. This suction roller has a large number of air suction holes on the peripheral surface of the roller for adsorbing and transporting the film to itself.

  When a suction roller is used, the film is more easily deformed than a non-driven roller because a complex force whose directionality cannot be specified acts on the film. The film is also deformed by a difference in tension before and after the conveyance applied to the film. Furthermore, a large number of air suction holes are formed on the peripheral surface of the suction roller. If the film slips or contracts or deforms when the film is in contact with the edge of the suction holes, Fine scratches occur.

  The driving roller used in the transporting process is a roller whose peripheral surface is previously cured by nitriding treatment, cured chrome plating, or quenching treatment. The surface hardness of the circumferential surface is 500 to 2000 in terms of Vickers hardness. Or less, more preferably 800 or more and 1200 or less.

  The drive roller used is a suction roller, and this suction roller has a large number of air suction holes on its peripheral surface. At this time, the surface roughness Ry of the peripheral surface of the suction roller is preferably 0.3 μm or more and 1.0 μm or less, more preferably 0.5 μm or more and 0.8 μm or less. As for the surface roughness Ry of the peripheral surface, the surface roughness of the smooth portion having no hole in the roller is the peripheral surface roughness. The hole diameter is preferably 1 mm or more and 6 mm or less, more preferably 2 mm or more and 4 mm or less, and the chamfering amount of the hole is preferably 2% or more and 20% or less of the hole diameter.

  When using the suction roller, it is preferable to control the peripheral surface temperature, and therefore, it is preferable to have at least one temperature adjusting device for one suction roller. It is preferable to form the film while making the peripheral surface temperature of the roller higher than the film temperature immediately before contacting the suction roller.

  Moreover, the charged voltage while the film 111 is conveyed is set to a predetermined range (for example, −3 kV to +3 kV) by the forced charge removal device (charge removal bar) 148. In FIG. 7, an example provided on the downstream side of the cooling chamber 117 is illustrated, but the position is not limited thereto. Furthermore, it is preferable to provide a knurling roller 119 to give knurling to both edges of the film 111 by embossing. In addition, it is preferable that the unevenness | corrugation of the knurled location is 1 micrometer-200 micrometers.

  Finally, the film 111 is taken up by the take-up roller 121 in the take-up chamber 120. At this time, it is preferable to wind the sheet while applying a desired tension with the press roller 122. More preferably, the tension is gradually changed from the start to the end of winding. The film 111 to be wound is preferably at least 100 m in the longitudinal direction (casting direction). Moreover, it is preferable that the width | variety of a film is 600 mm or more, and it is more preferable that they are 1400 mm or more and 1800 mm or less. Furthermore, the present invention is also effective when it is larger than 1800 mm. The present invention is also applied when a thin film having a thickness of 15 μm or more and 100 μm or less is manufactured.

  In the present invention, when casting the dope, a method of simultaneously laminating two or more types of dopes or co-casting sequentially may be used. When performing simultaneous lamination and co-casting, a casting die to which a feed block is attached may be used, or a multi-manifold casting die may be used. In the film composed of multiple layers by co-casting, it is preferable that either the thickness of the layer on the air surface side or the thickness of the layer on the support side is 0.5% to 30% of the thickness of the entire film. Furthermore, when performing simultaneous lamination co-casting, it is preferable that the high-viscosity dope is wrapped with the low-viscosity dope when the dope is cast from the die slit to the support. Moreover, when performing simultaneous lamination | stacking co-casting, it is preferable that the dope which contact | connects an external world among the beads formed from a die slit to a support body has a larger alcohol composition ratio than an internal dope.

  From casting die, decompression chamber, support structure, co-casting, peeling method, stretching, drying conditions for each process, handling method, curl, winding method after flatness correction, solvent recovery method, film recovery method The details are described in paragraphs [0617] to [0889] of Japanese Patent Application No. 2004-264464. These descriptions are also applicable to the present invention.

[Performance / Measurement method]
(Curl degree / thickness)
The performance of the wound cellulose acylate film and the measuring method thereof are described in paragraphs [0112] to [0139] of Japanese Patent Application No. 2004-264464. These are also applicable to the present invention.

[surface treatment]
It is preferable that at least one surface of the cellulose acylate film is surface-treated. The surface treatment is preferably at least one of vacuum glow discharge treatment, atmospheric pressure plasma discharge treatment, ultraviolet irradiation treatment, corona discharge treatment, flame treatment, acid treatment or alkali treatment.

[Functional layer]
(Antistatic, hardened layer, antireflection, easy adhesion, antiglare)
At least one surface of the cellulose acylate film may be undercoated.

  Furthermore, it is preferable to use the cellulose acylate film as a base film as a functional material provided with another functional layer. The functional layer is preferably provided with at least one layer selected from an antistatic layer, a cured resin layer, an antireflection layer, an easy adhesion layer, an antiglare layer and an optical compensation layer.

  A method for applying a surface-treated functional layer for realizing various functions and properties on a cellulose acylate film is described in Japanese Patent Application No. 2004-264464, from [0890] paragraph to [1087] paragraph. It is included. These are also applicable to the present invention.

(Use)
The cellulose acylate film is particularly useful as a polarizing plate protective film. Usually, two polarizing plates each having a cellulose acylate film bonded to a polarizer are bonded to a liquid crystal layer to produce a liquid crystal display device. However, the arrangement of the liquid crystal layer and the polarizing plate is not limited, and various known arrangements can be employed. Japanese Patent Application No. 2004-264464 describes in detail TN type, STN type, VA type, OCB type, reflection type, and other examples of liquid crystal display devices. This method can also be applied to the present invention. The application also describes a cellulose acylate film provided with an optically anisotropic layer and a cellulose acylate film provided with antireflection and antiglare functions. Furthermore, the use as an optical compensation film is also described as a biaxial cellulose acylate film imparting moderate optical performance. This can also be used as a polarizing plate protective film. These descriptions are also applicable to the present invention. Details are described in paragraphs [1088] to [1265] of Japanese Patent Application No. 2004-264464.

  Moreover, the cellulose triacetate film (TAC film) excellent in an optical characteristic can be obtained with the manufacturing method of this invention. The TAC film can be used as a polarizing plate protective film or a base film for a photographic photosensitive material. Furthermore, it can also be used as an optical compensation film for improving the viewing angle dependency of a liquid crystal display device for television applications. In particular, it is effective for applications that also serve as a protective film for a polarizing plate. Therefore, it is used not only for the conventional TN mode but also for the IPS mode, OCB mode, VA mode, and the like. Moreover, you may comprise a polarizing plate using the said film for polarizing plate protective films.

Next, the Example regarding the film manufacture of this invention is described based on the flow of operation | movement of the dope manufacturing line 3 and the solution casting apparatus 2. FIG. First, the formulation for preparing the polymer solution (dope) used for film production is shown below.
[composition]
Cellulose triacetate (substitution degree 2.84, viscosity average polymerization degree 306, water content 0.2 mass%, viscosity 6 mass% in dichloromethane solution 315 mPa · s, average particle diameter 1.5 mm with standard deviation 0.5 mm Some powders) 100 parts by mass dichloromethane (first solvent) 320 parts by mass methanol (second solvent) 83 parts by mass 1-butanol (third solvent) 3 parts by mass plasticizer A (triphenyl phosphate) 7.6 parts by mass Plasticizer B (diphenyl phosphate) 3.8 parts by mass UV agent a: 2 (2′-hydroxy-3 ′, 5′-di-tert-butylphenyl) benzotriazole 0.7 part by mass UV agent b: 2 ( 2′-Hydroxy-3 ′, 5′-di-tert-amylphenyl) -5-chlorobenzotriazole 0.3 parts by mass of citric acid ester mixture (citric acid, citric acid Monoethyl ester, citric acid diethyl ester, citric acid triethyl ester mixture) 0.006 parts by weight fine particles (silicon dioxide (particle size 15 nm), Mohs hardness: about 7) 0.05 parts by weight

[Cellulose triacetate]
The cellulose triacetate used here has a residual acetic acid content of 0.1% by mass or less, a Ca content of 58 ppm, a Mg content of 42 ppm, a Fe content of 0.5 ppm, a free acetic acid of 40 ppm, It contained 15 ppm of sulfate ions. The degree of substitution of the 6-position acetyl group was 0.91, 32.5% of the total acetyl. Moreover, the acetone extraction part which extracted this TAC with acetone was 8 mass%, and the weight average molecular weight / number average molecular weight ratio was 2.5. The obtained TAC has a yellow index of 1.7, a haze of 0.08, a transparency of 93.5%, a Tg (glass transition point; measured by DSC) of 160 ° C., and a crystallization calorific value of It was 6.4 J / g. This TAC is synthesized using cellulose collected from cotton as a raw material. In the following description, this is called cotton raw material TAC.

(1-1) Dope Preparation A dope 60 was prepared using a dope production line 3 shown in FIG. In a 4000 L stainless steel dissolution tank 5 having a stirring blade, the plurality of solvents were mixed and stirred well to obtain a mixed solvent. In addition, all the solvents used that the water content is 0.5 mass% or less. Next, TAC flaky powder was gradually added from the hopper 6. The TAC powder was put into the dissolution tank 5 and dispersed for 30 minutes under a predetermined stirring condition by the first stirrer 55 as an anchor blade and the second stirrer 57 as an eccentric stirrer of a dissolver type. The temperature at the start of dispersion was 25 ° C., and the final temperature reached 48 ° C. Further, the additive solution prepared in advance was adjusted from the additive tank 7 with the valve 52 by the valve 52 and sent to the dissolution tank 5 so that the total amount became 2000 kg. After the dispersion of the additive solution was completed, the peripheral speed of the first stirrer 55 was set to a predetermined value, and the mixture was further stirred for 100 minutes to swell the TAC flakes to obtain a swelling liquid 58. The tank was pressurized to 0.12 MPa with nitrogen gas until the end of swelling. The inside of the dissolution tank 5 at this time was kept in a state where there was no problem in terms of explosion prevention because the oxygen concentration was less than 2 vol%. The amount of water in the swelling liquid was 0.3% by mass.

(1-2) Dissolution / Filtration The swelling liquid 58 was fed from the dissolution tank 5 to the heating device 8 which is a jacketed pipe using a pump 59. The swelling liquid 58 was heated to 50 ° C. with the heating device 8, further heated to 90 ° C. under a pressure of 2 MPa, and completely dissolved to obtain a dope 60. The heating time at this time was 15 minutes. Next, the temperature of the dope 60 was lowered to 36 ° C. with the temperature controller 9, and the dope 60 was filtered with the first filtering device 11 or the second filtering device 12 of the filtration unit 10, thereby obtaining the dope 60.

(1-3) Concentration / Filtration / Defoaming / Additive The dope 60 thus obtained is flash-evaporated in the flash device 13 at normal pressure at 80 ° C., and the evaporated solvent is condensed in the condenser. And recovered. In this way, the dope concentration was adjusted. The condensed solvent was recovered by the recovery device 15 to be reused as a dope preparation solvent, regenerated by the regeneration device 16, and then sent to the solvent tank 4. In the recovery device 15 and the regeneration device 16, distillation or dehydration is performed. The flash tank of the flash unit 13 was provided with a stirrer equipped with an anchor blade on the stirring shaft, and the flashed dope 60 was stirred by this stirrer to perform defoaming. The temperature of the dope 60 in this flash tank was 25 ° C., and the average residence time of the dope 60 in the tank was 50 minutes. The shear viscosity of the dope 60 taken and measured at 25 ° C. was 450 Pa · s at a shear rate of 10 ⁻¹ (sec ⁻¹ ).

  Next, bubbles were removed by irradiating the dope 60 with weak ultrasonic waves. Then, after flushing, the filtration unit 14 was passed in a state where the pressure was increased to 1.5 MPa using the pump 62. The dope temperature after filtration was adjusted to 36 ° C., and the dope 60 was fed into a 2000 L stainless steel stock tank 65 and stored therein. The stock tank 65 has a stirrer having an anchor blade on the central axis, and the inside is constantly stirred by this stirrer. Incidentally, no problem such as corrosion occurred at all in the wetted part of the dope during the preparation of the dope 60.

  Moreover, the mixed solvent A of 86.5 mass parts of dichloromethane, 13 mass parts of acetone, and 0.5 mass part of 1-butanol was produced.

(1-4) Discharge / immediate addition / casting / bead depressurization A film 111 was produced using the solution casting apparatus 2 shown in FIG. The dope 60 in the stock tank 65 was sent to the filtration unit 74 by the pump 73. This pump 73 has a function of increasing the pressure on the primary side of the pump 73, and sent the liquid by performing feedback control on the upstream side of the pump 73 with an inverter motor so that the pressure on the primary side becomes 0.8 MPa. . The pump 73 has a volumetric efficiency of 99.2% and a discharge rate variation rate of 0.5% or less. The discharge pressure was 1.5 MPa. Then, the dope 60 filtered by the filtration unit 74 was fed to the casting die 80.

  The casting die 80 is cast by adjusting the flow rate of the dope 60 at the discharge port of the casting die 80 so that the width of the casting die 80 is 1.8 m and the thickness of the dried film 111 is 80 μm. It was. The casting width of the dope 60 from the discharge port of the casting die 80 was 1700 mm. The casting speed was a predetermined speed. In order to adjust the temperature of the dope 60 to 36 ° C., a jacket (not shown) is provided on the casting die 80 and the inlet temperature of the heat transfer medium supplied into the jacket is set to 36 ° C.

  The casting die 80 and the piping were all kept at 36 ° C. during operation. The casting die 80 is a coat hanger type die. And as this casting die | dye 80, the thickness adjustment bolt was provided in 20 mm pitch, and the thing equipped with the automatic thickness adjustment mechanism by a heat bolt was used. The heat bolt can set a profile corresponding to the pumping amount by a preset program, and is feedback controlled by an adjustment program based on the profile of an infrared thickness gauge (not shown) installed in the solution casting apparatus 2 Also used were those having possible performance. In the film 111 excluding the casting side end 20 mm, the difference in thickness between two arbitrary points separated by 50 mm was within 1 μm, and the thickness variation in the width direction was adjusted to 3 μm / m or less. The overall thickness was adjusted to ± 1.5% or less.

  Further, a decompression chamber 90 for decompressing this portion was installed on the primary side of the casting die 80. The degree of decompression of the decompression chamber 90 is adjusted so that a pressure difference of 1 Pa to 5000 Pa is generated before and after the casting bead from the casting die 80 until reaching the casting start position PS. Made according to speed. At that time, the pressure difference on both sides of the bead was set so that the length of the bead became a predetermined value. Further, the decompression chamber 90 was provided with a mechanism that can be set to a temperature higher than the condensation temperature of the gas around the casting portion. Labyrinth packings (not shown) were provided on the front and back sides of the bead at the discharge port of the casting die 80, and openings were provided on both ends of the discharge port. Further, the casting die 80 is attached with an edge suction device (not shown) for adjusting the disturbance of both edges of the casting bead.

(1-5) Casting Die The material of the casting die 80 is a two-layer stainless steel having a thermal expansion coefficient of 2 × 10 ⁻⁵ (° C. ⁻¹ ) or less. This is a material that has almost the same corrosion resistance as that of SUS316 in the forced corrosion test with an aqueous electrolyte solution, and it is also pitting at the gas-liquid interface even if immersed in a mixture of dichloromethane, methanol, and water for 3 months. Corrosion resistance that does not cause (perforation). The finishing accuracy of the wetted surface of the casting die 80 was 1 μm or less in terms of surface roughness, the straightness was 1 μm / m or less in any direction, and the slit clearance was adjusted to 1.5 mm. About the corner | angular part of the liquid-contact part of the lip | tip end of the casting die 80, it is processed so that R may be 50 micrometers or less over the slit full width. The shear rate inside the casting die 80 was in the range of 1 (1 / sec) to 5000 (1 / sec). Further, a WC (tungsten carbide) coating was performed on the lip end of the casting die 80 by a thermal spraying method to provide a cured film.

  Furthermore, in order to prevent the dope 60 flowing out from being locally dried and solidified, the mixed solvent A for solubilizing the dope 60 is provided at both ends of the casting bead at the discharge port of the casting die 80. And 0.5 ml / min. Supplied one by one. The pulsation rate of the pump supplying the mixed solvent A was 5% or less. Further, the pressure on the back side of the bead was reduced by 150 Pa from the front side by the decompression chamber 90. In addition, a jacket (not shown) was attached to keep the internal temperature of the decompression chamber 90 constant at a predetermined temperature. A heat transfer medium adjusted to 35 ° C. was supplied into the jacket. The edge suction device is 1 L / min. ~ 100 L / min. The edge suction air volume can be adjusted so as to fall within the range of 30 L / min. ~ 40 L / min. It adjusted suitably so that it might become the range of.

(1-6) Metal Support A casting band 83 as a stainless steel endless band having a width of 2.1 m and a length of 70 m was used as a support. The casting band 83 was polished so that the thickness was 1.5 mm and the surface roughness was 0.05 μm or less. The material is made of SUS316 and has sufficient corrosion resistance and strength. The thickness unevenness of the entire casting band 83 was 0.5% or less. The casting band 83 was conveyed by two rotating rollers 81 and 82. At this time, the relative speed difference between the casting band 83 and the rotary rollers 81 and 82 is 0.01 m / min or less so that the tension in the conveying direction of the casting band 83 is 1.5 × 10 ⁵ N / m ^2. It was adjusted to become. The speed fluctuation of the casting band 83 was 0.5% or less. Further, both end positions of the casting band 83 were detected and controlled so that the meandering in the width direction of one rotation was limited to 1.5 mm or less. Further, the positional variation in the vertical direction between the lip tip of the casting die 80 and the casting band 83 immediately below the casting die 80 was set to 200 μm or less. The casting band 83 is installed in a casting chamber 85 having wind pressure fluctuation suppressing means (not shown). The dope 60 was cast from the casting die 80 on the casting band 83.

As the rotating rollers 81 and 82, those capable of feeding a heat transfer medium therein were used so that the temperature of the casting band 83 could be adjusted. A 5 ° C. heat transfer medium was passed through the rotary roller 81 on the casting die 80 side, and a 40 ° C. heat transfer medium was passed through the other rotary roller 82 for drying. The surface temperature of the central part of the casting band 83 immediately before casting was 15 ° C., and the temperature difference between both side ends was 6 ° C. or less. The casting band 83 preferably has no surface defects, has no pinholes of 30 μm or more, has 1 to 10 μm to 30 μm pinholes / m ² or less, and has 2 pinholes of less than 10 μm / Those with m ² or less were used.

(1-7) Casting drying The temperature of the casting chamber 85 was kept at 35 ° C. by the temperature control equipment 86. To the casting film 89 formed from the dope 60 cast on the casting band 83, the blower 91, 92 first sent the drying air flowing parallel to the casting film 89 to dry it. . The overall heat transfer coefficient from the dry air to the casting film 89 was 24 kcal / m ² · hr · ° C. The temperature of the drying air was 135 ° C. on the upstream side of the upper part of the casting band 83 and 140 ° C. on the downstream side. Further, the lower part of the casting band 83 was blown from the blower 93 so that the temperature was 65 ° C. The saturation temperature of each drying wind was around -8 ° C. The oxygen concentration in the dry atmosphere on the casting band 83 was kept at 5 vol%. In order to maintain this oxygen concentration at 5 vol%, the air was replaced with nitrogen gas. Further, in order to condense and recover the solvent in the casting chamber 85, a condenser (condenser) 87 was provided, and its outlet temperature was set to -10 ° C.

In order to prevent the air flow from directly hitting the dope 60 and the casting film 89 during the casting time of 5 seconds from the casting starting point PS, a wind shield 94 is provided, and the static pressure in the vicinity of the casting die 80 is provided. The fluctuation was suppressed to ± 1 Pa or less. When the solvent ratio in the casting film 89 reached 50% by mass on the dry basis, the film was peeled off as a wet film 96 while being supported by the peeling roller 95 from the casting band 83. The solvent content based on the dry weight standard is a value obtained by {(xy) / y} × 100, where x is the film weight at the time of sampling and y is the weight after the sampling film is dried. . The stripping tension at this time is 1 × 10 ² N / m ² , and the stripping speed (stripping roller draw) with respect to the speed of the casting band 83 is 100.1% to 110% in order to suppress stripping failure. Adjusted appropriately within the range. The surface temperature of the peeled film was 15 ° C. The drying rate on the casting band 83 was 60% by mass on the basis of dry weight reference solvent / min. Met. The solvent gas generated by the drying was condensed and liquefied by a -10 ° C. condenser and recovered by a recovery device (not shown). The recovered solvent was adjusted so that the water content was 0.5% or less. The drying air from which the solvent has been removed is heated again and reused as drying air. The wet film 96 was conveyed through the crossing part 100 and sent to the tenter device 110. At the time of conveyance, 40 ° C. dry air was sent from the blower 101 to the wet film 96. Note that a predetermined value of tension is applied to the wet film 96 during conveyance by the rollers of the crossover unit 100.

(1-8) Tenter Transport / Drying / Ear Cutting The wet film 96 sent to the tenter device 110 is transported in the drying zone of the tenter device 110 while being fixed at both ends with clips, and during that time, it is dried by drying air, The film 111 is conveyed to the ear clip device 112. The clip was cooled by supplying a heat transfer medium at 20 ° C. The clip of the tenter device 110 was conveyed by a chain, and the speed fluctuation of the sprocket was 0.5% or less. The gas composition of the drying air was set to a saturated gas concentration at −10 ° C. The average drying speed in the tenter apparatus 110 was 120% by mass (dry weight reference solvent) / min. The conditions of the drying zone were adjusted so that the residual solvent amount of the wet film 96 at the outlet of the tenter device 110 was 7% by mass. In the tenter device 110, the wet film 96 was conveyed and stretched in the width direction. In addition, when the width | variety of this wet film 96 before extending | stretching was 100%, it extended | stretched so that the width | variety after extending | stretching might be 103%. The stretching ratio (tenter driven draw) from the peeling roller to the entrance of the tenter device 110 was 102%. The ratio of the length from the clip nipping start position to the nipping release position with respect to the length from the tenter inlet to the outlet was 90%. The solvent evaporated in the tenter apparatus 110 was condensed at a temperature of −10 ° C., liquefied and recovered. A condenser (condenser) was provided for condensation recovery, and the outlet temperature was set to -8 ° C. The condensed solvent was reused after adjusting the water content to 0.5% by mass or less.

  Then, the ear-cutting device 112 cuts the ears of the film 111 within 30 seconds from the tenter outlet 17 of the tenter device 110.

(1-9) Post-drying / static elimination The film 111 was dried at high temperature in the drying chamber 115. The drying chamber 115 was divided into four sections, and drying air at 120 ° C., 130 ° C., 130 ° C., and 130 ° C. was supplied from a blower (not shown) from the upstream side. The transport tension of the film 111 by the roller 114 was set to 100 N / m, and the film was dried for about 10 minutes until the residual solvent amount finally reached 0.3% by mass. The wrap angle (the film winding center angle) in the roller 114 was 90 ° and 180 °. The material of the roller 114 was made of aluminum or carbon steel, and hard chrome plating was applied to the surface. As the surface shape of the roller 114, a flat surface and a surface formed by matting by blasting were used. All film position fluctuations due to the rotation of the roller 114 were 50 μm or less. The roller deflection at a tension of 100 N / m was selected to be 0.5 mm or less.

  The solvent gas contained in the drying air was adsorbed and recovered using the adsorption recovery device 116. The adsorbent used here was activated carbon, and desorption was performed using dry nitrogen. The recovered solvent was adjusted to a water content of 0.3% by mass or less and reused as a dope preparation solvent. Since the drying air contains solvent gas, plasticizer, UV absorber, and other high-boiling substances, these were removed by a cooler and a pre-adsorber for cooling and removing them, and recycled and used. And adsorption / desorption conditions were set so that VOC (volatile organic compound) in the outdoor exhaust gas was finally 10 ppm or less. Moreover, the solvent amount collect | recovered by a condensation method among all the evaporation solvents was 90 mass%, and most of the remainder was collect | recovered by adsorption collection.

  The dried film 111 was conveyed to a first humidity control chamber (not shown). A drying air of 110 ° C. was supplied to the transition portion between the roller dryer and the first humidity control chamber. Air having a temperature of 50 ° C. and a dew point of 20 ° C. was supplied to the first humidity control chamber. Further, the film 111 was transported to a second humidity control chamber (not shown) for suppressing the curling of the film 111. In the second humidity control chamber, air of 90 ° C. and humidity 70% was directly applied to the film 111.

(1-10) Knurling and Winding Conditions The film 111 after humidity control was cooled to 30 ° C. or lower in the cooling chamber 117, and then subjected to ear cutting with a second ear cutting device. The forced charge removal device (charge removal bar) 118 was installed so that the charged voltage of the film 111 during conveyance was always in the range of −3 kV to +3 kV. Further, knurling was applied to both ends of the film 111 by a knurling roller 119. The knurling is applied by embossing from one side of the film 111, the width for applying the knurling is 10 mm, and the knurling is applied by the knurling roller 119 so that the height of the unevenness is 12 μm higher than the average thickness of the film 111 on average. The pressing pressure was set.

  Then, the film 111 was conveyed to the winding chamber 120. The winding chamber 120 is maintained at an apparatus internal temperature of 28 ° C. and a humidity of 70%. Further, an ion wind static elimination device (not shown) was also installed in the winding chamber 120 so that the charged voltage of the film 111 was −1.5 kV to +1.5 kV. The product width of the film (thickness 80 μm) 111 thus obtained was 1475 mm. The winding roller 121 in the winding chamber 120 has a diameter of 169 mm. The tension pattern was such that the winding start tension was 300 N / m and the winding end was 200 N / m. The total length of the wound film 111 was 3940 m. The fluctuation range of winding deviation (sometimes referred to as oscillating width) during winding was ± 5 mm, and the winding deviation period with respect to the winding axis was 400 m. The pressing pressure of the press roller 122 against the winding shaft was set to 50 N / m. The temperature of the film 111 at the time of winding was 25 ° C., the water content was 1.4% by mass, and the residual solvent amount was 0.3% by mass. The average drying rate was 20% by mass (dry weight reference solvent) / min throughout the entire process. Moreover, there was no winding looseness and wrinkles, and no winding slip occurred in the impact test at 10G. Moreover, the external appearance of the film roll was also favorable.

  The film roll was stored in a storage rack at 25 ° C. and a relative humidity of 55% (hereinafter referred to as 55% RH) for one month and further examined in the same manner as described above. As a result, no change was observed. Further, no film adhesion was observed in the film roll. In addition, after the film 111 was formed, the cast film formed from the dope 60 was not peeled off on the casting band 83 at all.

  In the above embodiment, the sheet-like filter 21 is replaced by the filter replacement unit 23. However, the filter is rotated by rotating the filter roll using the filter roll wound in a roll shape, so that the filter is replaced. Also good.

It is a top view which shows the dope manufacturing line which implemented this invention. It is side surface sectional drawing which shows a filter and the clamping board located in an open position. It is side surface sectional drawing which shows a filter, the clamping board located in a clamping position, and a clamping shift part. It is side surface sectional drawing which shows a filter replacement | exchange unit, a clamping shift part, a conveyance shift part, and a collection | recovery shift part. It is a side view which shows a conveyance pick-up. It is a flowchart which shows the procedure which switches and wash | cleans a 1st filtration apparatus and a 2nd filtration apparatus. It is a top view which shows solution casting equipment.

Explanation of symbols

2 solution casting equipment 3 dope production line 10 filtration unit 11 first filtration device (filtration device)
12 Second filtration device (filtration device)
14 Filtration unit after flash 18 Filtration control unit 19 Dope switching valve (switching device)
20 aspirator 21 filter 22 clamping plate (filter clamping member)
22a inlet 22b Dope passage part before filtration (filtration passage)
22c Dope passage after filtration (filtration passage)
22d Discharge port 23 Filter replacement unit (filter replacement means)
25 Cleaning switching valve 26 Cleaning liquid tank 27 Gas tank 28 Solvent quantity detector (drying determination means)
29 Recovery switching valve 30 Recovery tank 31 Transport pickup 32 Recovery pickup 34 Pickup body 35 Transport suction pad (suction holder)
36 moving plate 60 dope (polymer solution)
74 Filtration unit 96 Wet film (polymer film)

Claims (8)

A plurality of filtration devices having a filter for filtering a polymer solution in a filtration passage; and a switching device for switching a piping system in order to selectively use the plurality of filtration devices. In the solution casting equipment for casting the polymer solution filtered by at least one of them onto a support and peeling it off as a polymer film, and drying the polymer film,
The filtering device includes a filtering position for clamping the filter to filter the polymer solution, and a filter clamping member that is displaced between an opening position that allows the filter to be replaced by opening the filter. , possess a cleaning means for sending the cleaning liquid to clean the filter at the filter position, and filter replacement means for replacing the filter by the filter clamping member after cleaning by said cleaning means to the open position,
The cleaning means includes a polymer solution discharge means for sending a gas to the filter passage and the filter before sending the cleaning liquid and discharging the polymer solution from the filtration device, and the filtration after the washing with the cleaning liquid. A solution film-forming facility, comprising: a passage and a drying means for drying the cleaning liquid by sending a gas to the filter . The amount of cleaning liquid component in the gas sent to the filtration passage and the filter for the drying is detected, the degree of drying is determined based on the detected value, and when it is determined that the drying is completed, the filter replacement command is issued. solution casting apparatus according to claim 1, characterized in that it comprises a drying judging means for outputting to the switching means. The filter is composed of sheet filter paper,
The filter replacement means includes
A collecting means for collecting the used filter from the filter holding member in the open position;
The unused filters are stacked and stored, and a suction holding unit that sucks and holds the top layer of the stored filters,
3. A filter setting unit that sets the filter sucked by the suction holding unit to a filter holding member in which the used filter is collected by the collecting unit at the open position. The solution casting apparatus described. A displacement part for displacing the suction holding part in a state of sucking the filter upward;
4. The solution casting apparatus according to claim 3 , wherein the filter setting means sets the filter on a filter holding member in a state where the suction part is displaced upward. The air suction of the peripheral of the filter in the filter exchange, the sucked solution casting apparatus of claims 1, and recovering the organic solvent in said cleaning liquid from the air 4 any one claim, wherein. The polymer film is a cellulose ester;
The filter, solution casting apparatus according any one claims 1 to 5, characterized in that a filter paper made from cellulose. Filtration device having a filter holding member which is displaced between a filtration position where the filter is sandwiched in the filtration passage and the polymer solution is filtered, and an open position where the filter can be exchanged by opening the filter. In the filter replacement method of
A polymer solution discharging step of sending a gas into the filtration passage and discharging the polymer solution from the filtration passage;
After discharging the polymer solution, a cleaning step of sending a cleaning solution into the filtration passage and washing the filtration passage and the filter;
A drying step of sending a dry gas into the filtration passage after washing with the washing solution, and drying the washing solution of the filtration passage and the filter;
The amount of the cleaning liquid component in the dry gas during the drying process is detected, and the completion of drying is determined based on the detected value. When it is determined that the drying is completed, the filter clamping member is opened after the gas feed is stopped. A filter replacement method for a filtration device, comprising: a filter replacement step of replacing the filter at a position. 8. The filter replacement method for a filter device according to claim 7 , wherein in the filter replacement step, air around the filter device is sucked and the organic solvent in the cleaning liquid is recovered from the sucked air.

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