WO2018029955A1 - Procédé de fabrication de film optique - Google Patents

Procédé de fabrication de film optique Download PDF

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Publication number
WO2018029955A1
WO2018029955A1 PCT/JP2017/020867 JP2017020867W WO2018029955A1 WO 2018029955 A1 WO2018029955 A1 WO 2018029955A1 JP 2017020867 W JP2017020867 W JP 2017020867W WO 2018029955 A1 WO2018029955 A1 WO 2018029955A1
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WO
WIPO (PCT)
Prior art keywords
stirring
resin
jig
optical film
blade
Prior art date
Application number
PCT/JP2017/020867
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English (en)
Japanese (ja)
Inventor
西村　浩
崇 南條
Original Assignee
コニカミノルタ株式会社
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by コニカミノルタ株式会社 filed Critical コニカミノルタ株式会社
Priority to CN201780049107.7A priority Critical patent/CN109641374B/zh
Priority to JP2018533437A priority patent/JP6911863B2/ja
Priority to KR1020187028465A priority patent/KR102136476B1/ko
Publication of WO2018029955A1 publication Critical patent/WO2018029955A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C41/00—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor
    • B29C41/34—Component parts, details or accessories; Auxiliary operations
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/40—Mixing liquids with liquids; Emulsifying
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
    • B01F27/85—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with two or more stirrers on separate shafts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
    • B01F27/90—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with paddles or arms 
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
    • B01F27/91—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with propellers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
    • B29B7/34—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices
    • B29B7/38—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary
    • B29B7/40—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with single shaft
    • B29B7/44—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with single shaft with paddles or arms
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C41/00—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor
    • B29C41/24—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor for making articles of indefinite length
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
    • B29D11/00—Producing optical elements, e.g. lenses or prisms
    • B29D11/0074—Production of other optical elements not provided for in B29D11/00009- B29D11/0073
    • B29D11/00788—Producing optical films

Definitions

  • the present invention relates to an optical film manufacturing method in which an optical film is formed by a solution-flow casting method, and more particularly to stirring of a dope cast on a support.
  • Patent Document 1 Conventionally, as a stirring device for stirring a solution, for example, there is one disclosed in Patent Document 1.
  • the first flat plate blade member and the second flat plate blade member are arranged side by side along the rotation axis direction on the rotation shaft extending in the vertical direction in the stirring tank into which the solution is charged.
  • the first flat plate blade member and the second flat plate blade member are attached to the rotary shaft at an inclination angle that raises the solution based on the rotation of the rotary shaft.
  • the circulation flow of the solution is generated without being divided in the vertical direction of the stirring tank, and the vertical circulation of the solution is efficiently performed. Mixing can be performed.
  • JP 2010-42337 A see claim 1, paragraphs [0001], [0004], [0007], FIG. 1, FIG. 2, etc.
  • Patent Document 1 is applied to the stirring of the resin and the solvent when preparing the dope used in the solution casting film forming method, and an optical film is formed using the dope prepared by stirring.
  • this inventor estimates as follows.
  • both the first flat plate blade member and the second flat plate blade member of the stirring device are composed of the stirring blades that generate upstream and downstream, even if stirring by vertical circulation can be performed, Stirring in the vertical direction (horizontal direction, shear direction) cannot be performed efficiently.
  • unevenness occurs in stirring in the stirring tank, and the viscosity of the dope becomes unstable due to the unevenness in stirring, and unevenness in film thickness occurs in an optical film formed using such a dope.
  • poor dissolution occurs such that the resin aggregates in the stirring tank to form an aggregate (undissolved material).
  • an optical film is formed using a dope containing an undissolved material, the undissolved material appears as a bright spot foreign material in the optical film.
  • a pellet-like resin for example, an acrylic resin
  • a solvent having a high specific gravity for example, methylene chloride
  • the resin tends to float on the liquid surface, and spatter is generated.
  • the spatter remaining as an undissolved product due to uneven stirring, bright spot foreign matter tends to be generated in the formed optical film.
  • the present invention has been made to solve the above-mentioned problems, and its purpose is to reduce the unevenness of stirring in the stirring tank, and thereby the film thickness unevenness of the optical film formed and the bright spot foreign matter. It is providing the manufacturing method of the optical film which can reduce generation
  • the method for producing an optical film according to one aspect of the present invention is a method for producing an optical film by a solution casting method, A stirring preparation step of preparing a dope by stirring at least a resin and a solvent in a stirring tank; A casting step of casting the dope prepared in the stirring preparation step on a support,
  • the resin is any one of an acrylic resin, a cycloolefin resin, and a polyarylate resin, When the specific gravity of the resin is A, the specific gravity of the solvent is B, and the specific gravity difference (BA) is ⁇ , 0.1 ⁇ ⁇ 0.5
  • the stirring tank is provided with a first stirring jig and a second stirring jig,
  • the first stirring jig includes a first rotating shaft located on a vertical axis passing through the center of the bottom surface of the stirring tank, and a lowermost portion of the first rotating shaft, and the first stirring jig is moved in the stirring tank.
  • the second agitating jig is arranged such that the second agitation jig is aligned along the vertical direction with the second rotation axis extending in the vertical direction so as to pass through the space between the first rotation axis and the arm portion.
  • the length along the vertical direction of the arm portion of the first stirring jig is L, and among the at least two stirring blades of the second stirring jig, the uppermost stirring blade and one lower side thereof
  • the first stirring blade is located above and including a position vertically lowered by (1/3) L from the uppermost portion of the arm portion of the first stirring jig
  • the second stirring blade It is composed of a stirring blade that causes a vertical flow of the resin by rotation about the rotation axis of
  • the second agitating blade is located below a position vertically lowered by (1/3) L from the uppermost part of the arm portion of the first agitating jig
  • the second rotating shaft is It is composed of an agitating blade that causes the resin drawn vertically downward by the first agitating blade to flow in a direction perpendicular to the second rotation axis by rotation around the center.
  • the unevenness of stirring in the stirring tank can be reduced, and thereby the film thickness unevenness of the optical film to be formed and the generation of bright spot foreign matter can be reduced.
  • the numerical value range includes the values of the lower limit A and the upper limit B.
  • FIG. 1 is an explanatory diagram illustrating a schematic configuration of an optical film manufacturing apparatus 1 according to the present embodiment.
  • FIG. 2 is a flowchart which shows the flow of the manufacturing process of an optical film.
  • the manufacturing method of the optical film of this embodiment is a method of manufacturing an optical film by a solution casting film forming method. As shown in FIG. 2, a stirring preparation step (S1), a casting step (S2), and a peeling step. (S3), stretching step (S4), drying step (S5), cutting step (S6), embossing step (S7), winding step (S8) are included.
  • S1 stirring preparation step
  • S2 a casting step
  • S3 a peeling step.
  • S4 stretching step
  • drying step (S5) drying step
  • cutting step (S6) embossing step
  • S7 embossing step
  • winding step S8
  • the dope prepared in the stirring preparation step is fed to the casting die 2 by a conduit through a pressurized metering gear pump or the like, and transferred onto the support 3 made of a rotationally driven stainless steel endless belt for infinite transfer.
  • the dope is cast from the casting die 2 at the casting position, thereby forming the web 5 as a casting film on the support 3.
  • the support 3 is held by a pair of rolls 3a and 3b and a plurality of rolls (not shown) positioned therebetween.
  • One or both of the rolls 3a and 3b are provided with a driving device (not shown) for applying tension to the support 3 so that the support 3 is used in a tensioned state.
  • the web 5 formed by the dope cast on the support 3 is heated on the support 3, and the solvent is evaporated until the web 5 can be peeled from the support 3 by the peeling roll 4.
  • the solvent is evaporated until the web 5 can be peeled from the support 3 by the peeling roll 4.
  • the residual solvent amount of the web 5 on the support 3 at the time of peeling is preferably in the range of 50 to 120% by mass depending on the strength of the drying conditions, the length of the support 3 and the like.
  • the amount of solvent is determined.
  • the residual solvent amount is defined by the following formula.
  • Residual solvent amount (% by mass) (mass before web heat treatment ⁇ mass after web heat treatment) / (mass after web heat treatment) ⁇ 100
  • the heat treatment for measuring the residual solvent amount represents performing heat treatment at 115 ° C. for 1 hour.
  • the web 5 peeled from the support 3 is stretched by the tenter 6.
  • the stretching direction at this time is one of a film transport direction (MD direction; Machine Direction), a lateral direction (TD direction; Transverse Direction) perpendicular to the transport direction in the film plane, and both of these directions.
  • MD direction film transport direction
  • TD direction lateral direction
  • Transverse Direction lateral direction perpendicular to the transport direction in the film plane
  • both side edges of the web 5 are fixed with a clip or the like and stretched is preferable in order to improve the flatness and dimensional stability of the film.
  • the stretching step by stretching the web 5 in both the MD direction and the TD direction, the web 5 can also be stretched (obliquely stretched) in a direction that obliquely intersects the MD direction and the TD direction.
  • the web 5 stretched by the tenter 6 is dried by a drying device 7.
  • the drying device 7 the web 5 is transported by a plurality of transport rolls arranged in a staggered manner as viewed from the side, and the web 5 is dried in the meantime.
  • the web 5 is dried using a hot air, infrared rays, a heating roll, a microwave. From the viewpoint of simplicity, a method of drying the web 5 with hot air is preferable.
  • the web 5 is transported toward the winding device 10 as the optical film F after being dried by the drying device 7.
  • a cutting unit 8 and an embossing unit 9 are arranged in this order between the drying device 7 and the winding device 10.
  • disconnects the both ends of the width direction with a slitter is performed, conveying the optical film F formed into a film.
  • the part remaining after the cutting of both ends constitutes a product part to be a film product.
  • disconnected from the optical film F is collect
  • embossing is performed by the embossing part 9 at both ends in the width direction of the optical film F.
  • Embossing is performed by pressing a heated embossing roller against both ends of the optical film F. Fine irregularities are formed on the surface of the embossing roller, and by pressing the embossing roller against both ends of the optical film F, the irregularities are formed at both ends.
  • the optical film F that has been embossed is wound up by the winding device 10 to obtain the original roll (film roll) of the optical film F. That is, in the winding process, the film roll is manufactured by winding the optical film F around the core while transporting the optical film F.
  • the winding method of the optical film F may be a commonly used winder, and there are methods for controlling tension such as a constant torque method, a constant tension method, a taper tension method, a program tension control method with a constant internal stress, and the like. You can use them properly.
  • the winding length of the optical film F is preferably 1000 to 7200 m. Further, the width at that time is desirably 1000 to 3200 mm, and the film thickness is desirably 10 to 60 ⁇ m.
  • FIG. 3 is a cross-sectional view schematically showing an example of the stirring device 100.
  • a stirring tank 101 of the stirring device 100 is provided with a first stirring jig 111 and a second stirring jig 121.
  • the bottom surface 101a side of the stirring tank 101 is “lower” and the top surface 101b side is “upper”.
  • a direction in which the bottom surface 101a and the top surface 101b face each other is a vertical direction (up and down direction), and a direction perpendicular to the vertical direction is a horizontal direction.
  • the first stirring jig 111 has a first rotating shaft 112 and an arm portion 113, and only one is provided in the stirring tank 101.
  • the first rotation shaft 112 is located on a vertical axis AX that passes through the center O of the bottom surface 101 a of the stirring vessel 101.
  • the first rotating shaft 112 is connected to a driving source (not shown) (for example, a motor) and rotates by driving the driving source.
  • the arm portion 113 is located at a position higher than the lowermost portion 112a in the stirring tank 101 from the lowermost portion 112a, which is the lower end portion of the first rotating shaft 112, and in the rotational radius direction from the first rotating shaft 112 ( It is attached to the first rotating shaft 112 so as to extend to the uppermost portion 113a at a position separated in a direction (perpendicular to the first rotating shaft 112).
  • two arm portions 113 are attached to the first rotation shaft 112 so as to be positioned symmetrically in a direction perpendicular to the first rotation shaft 112.
  • the 1st rotating shaft 112 and each arm part 113 may be comprised integrally, and may be comprised by joining of another member.
  • Each arm portion 113 is configured to have a U-shaped cross section that protrudes downward as a whole as a result of extending upward in a curved and monotonous manner from the lowermost portion 112 a of the first rotating shaft 112.
  • the first stirring jig 111 having the above-described configuration is also referred to as an anchor type because it looks like an anchor in the appearance.
  • FIG. 4 is a cross-sectional view showing another configuration of the first stirring jig 111.
  • Each arm portion 113 of the first stirring jig 111 may be configured with a W-shaped cross section as a whole. That is, each arm portion 113 may have a shape that once falls downward from the lowermost portion 112a of the first rotating shaft 112 toward the outer side in the rotational radius direction and extends toward the uppermost portion 113a therefrom.
  • Such a first stirring jig 111 is also a kind of anchor type.
  • FIG. 5 to 7 are perspective views showing still another configuration of the first stirring jig 111.
  • the first stirring jig 111 includes an arm portion 113 having a shape that extends from the lowermost portion of the first rotating shaft 112 outward in the rotational radial direction and then bends upward. May be.
  • Such a first stirring jig 111 is also a kind of anchor type.
  • the first stirring jig 111 is configured as a so-called anchor paddle type in which the area of the arm portion 113 is increased to improve the efficiency of stirring (watering). It may be.
  • two second agitation jigs 121 are provided in the agitation tank 101 and are positioned on opposite sides of the first rotation axis 112 of the first agitation jig 111. Yes.
  • the second rotating shaft 122 of the second stirring jig 121 extends in the vertical direction so as to pass through the space between the first rotating shaft 112 of the first stirring jig 111 and the arm portion 113. That is, the first rotating shaft 112 and the second rotating shaft 122 are parallel to each other.
  • the second rotating shaft 122 is connected to a driving source (not shown) (for example, a motor) and rotates by driving the driving source.
  • the at least two stirring blades 123 are attached to the second rotating shaft 122 so as to be aligned along the vertical direction.
  • the uppermost stirring blade 123 is referred to as a first stirring blade 123a
  • the stirring blade located one below the first stirring blade 123a is referred to as a second stirring blade 123b.
  • the length along the vertical direction from the lowermost part of the arm part 113 of the first stirring jig 111 to the uppermost part 113a is defined as L (mm). That is, the length L of the arm portion 113 is from the position Q corresponding to the lowermost portion of the arm portion 113 (equivalent to the lowermost portion 112a of the first rotating shaft 112 in FIG. 3) to the position P of the uppermost portion 113a. It is the length along the vertical direction.
  • the arm portion 113 is curved to a position R further below the lowermost portion 112a of the first rotating shaft 112 and then extends upward toward the uppermost portion 113a.
  • the length L of 113 is a length along the vertical direction from the position R to the position P.
  • the length L of the arm portion 113 is preferably 1/4 or more of the vertical length (depth) of the stirring tank 101, more preferably 1/3 or more, and 1/2 or more. It is further desirable that
  • a position that is vertically lowered by (1/3) L from the uppermost portion 113a (equal to the position P) of the arm portion 113 of the first stirring jig 111 is defined as a position A.
  • the first stirring blade 123a of the second stirring jig 121 is positioned above and including the position A, and the resin is rotated by rotation about the second rotating shaft 122. It consists of stirring blades that cause the vertical flow of As the stirring blade, a paddle type stirring blade shown in FIG. 8 or a propeller type stirring blade shown in FIG. 9 can be used.
  • the second stirring blade 123b of the second stirring jig 121 is positioned below the position A, and is vertically driven by the first stirring blade 123a by the rotation about the second rotation shaft 122. It is composed of stirring blades that cause the resin drawn downward to flow in a direction perpendicular to the second rotation shaft 122.
  • the agitating blade is composed of a turbine type agitating blade shown in FIG. 10 or a disk type (dissolving) agitating blade shown in FIG.
  • the dope composition is put into the stirring tank 101 of the stirring device 100 having the above configuration.
  • the dope composition includes a resin, a solvent, and an additive.
  • a pellet-shaped resin such as an acrylic resin, a cycloolefin resin, or a polyarylate resin is used as the resin.
  • the solvent methylene chloride, chloroform or the like is used.
  • fine particles (mat agent), a plasticizer, or the like is used. Since the specific gravity of the pellet-shaped resin is smaller than the specific gravity of the solvent (that is, the resin is lighter than the solvent), even if a part of the resin is dissolved in the solvent at the beginning of adding the resin, Most of the water floats on the solvent level.
  • the resin and solvent in the agitation tank 101 are uniform. And it stirs efficiently and stirring nonuniformity is reduced. Thereby, since the viscosity of the dope prepared by stirring is stabilized, film thickness unevenness can be reduced when an optical film is formed using the dope.
  • the resin can be uniformly stirred in the stirring tank 101, it becomes difficult to cause poor dissolution such as aggregation of the resin in the stirring tank 101 to form an aggregate (undissolved material), which is caused by the undissolved material. The generation of bright spot foreign matter can also be reduced.
  • the dope viscosity is unstable, it is necessary to adjust the dope viscosity (thickness adjustment) in order to reduce the film thickness unevenness, and the productivity of the optical film is lowered by the amount of such adjustment time.
  • the dope viscosity is stabilized by uniform stirring, it is possible to avoid the reduction in productivity of the optical film described above.
  • the specific gravity of the resin is A
  • the specific gravity of the solvent is B
  • the specific gravity difference (BA) is ⁇
  • the resin floats on the liquid surface of the solvent due to the specific gravity difference.
  • spalling is likely to occur.
  • the unevenness of stirring is reduced as described above, and the inside of the stirring tank 101 can be uniformly stirred. Therefore, even if the condition of ⁇ > 0.1, the generated spatter is reduced by stirring. , Generation of undissolved substances can be suppressed. As a result, in the optical film formed, the bright spot foreign matter resulting from the undissolved material can be reduced.
  • ⁇ is less than 0.5. That is, it can be said that the stirring method of the present embodiment is particularly effective when a resin and a solvent satisfying 0.1 ⁇ ⁇ 0.5 are selected to prepare a dope and form an optical film.
  • the specific gravity of polymethyl methacrylate resin (PMMA; PolymethylPomethacrylate), which is an acrylic resin, is 1.17, the specific gravity of cycloolefin resin is 1.01, and the specific gravity of polyarylate resin is 1.21. .
  • the specific gravity of methylene chloride is 1.32 and the specific gravity of chloroform is 1.48. Therefore, since any of the above resins satisfies 0.1 ⁇ ⁇ 0.5 with any of the above solvents, the resin and the solvent are used to stir by the method of this embodiment. In this way, by forming a dope and forming an optical film, it is possible to reduce film thickness unevenness and bright spot foreign matter caused by uneven stirring. It can be said that the more desirable range of the specific gravity difference ⁇ is 0.1 ⁇ ⁇ 0.31 from the minimum value and the maximum value of the specific gravity difference in the combination of each resin and each solvent.
  • the momentum of the resin flowing from the upper side to the lower side becomes strong, and the reaction at the bottom of the stirring tank causes the resin to flow from the lower side to the upper side.
  • the resin may flow vigorously and the resin may adhere to the top surface (lid portion) of the stirring tank.
  • the agitating blade (first agitating blade 123a) that generates the upstream and downstream and the agitating blade (second agitating blade 123b) that generates the horizontal flow are used,
  • the resin and the solvent can be uniformly stirred in the stirring tank 101 while moderately suppressing the flow of the resin. Therefore, the resin hardly adheres to the top surface 101b of the stirring tank 101.
  • the 1st stirring blade 123a located in the uppermost part among the several stirring blades of the 2nd stirring jig 121 is located above it including the position A, and 2nd Since the first agitating blade 123b is positioned below the position A, the first agitating blade 123a is rotated between the second agitating blade 123b and the arm portion 113 of the first agitating jig 111.
  • the resin can be reliably drawn, and the drawn resin and solvent can be reliably stirred in the horizontal direction and the shearing direction by the rotation of the second stirring blade 123b and the rotation of the arm portion 113.
  • the first stirring blade 123a located at the top of the plurality of stirring blades of the second stirring jig 121 is a paddle-type or propeller-type stirring blade, and therefore the first stirring blade 123a rotates.
  • the flow in the vertical direction in the stirring tank 101, in particular, the flow of the resin from the upper side to the lower side can be reliably generated.
  • the second stirring blade 123b located below the first stirring blade 123a is a turbine-type or disk-type stirring blade, so that the rotation of the second stirring blade 123b causes the horizontal resin flow to flow. It can surely occur.
  • the first stirring jig 111 is composed of an anchor type or anchor paddle type stirring blade (bottom blade), a space is formed between the first rotating shaft 112 and the arm portion 113. . Therefore, the second stirring jig 121 can be positioned in a part of the space as in the present embodiment. And it becomes possible to implement
  • FIG. 12 is a cross-sectional view showing another configuration of the second stirring jig 121.
  • the second stirring jig 121 may further include a third stirring blade 123c in addition to the first stirring blade 123a and the second stirring blade 123b described above.
  • the third agitating blade 123c is located one lower than the second agitating blade 123b, and, like the second agitating blade 123b, the turbine-type agitating blade shown in FIG. 10 or the disk-type agitating blade shown in FIG. Consists of.
  • the second stirring jig 121 has three stirring blades (a first stirring blade 123a, a second stirring blade 123b, and a third stirring blade 123c).
  • the third stirring blade 123b and the third stirring blade 123c) are turbine-type or disk-type stirring blades, so that the resin drawn downward by the rotation of the first stirring blade 123a is used as the second stirring blade 123b.
  • the third stirring blade 123c is rotated to flow in the horizontal direction in a wide range in the vertical direction (depth direction) in the stirring tank 101, and the resin and the solvent are moved in the vertical direction by the rotation of the arm portion 113. It can be stirred in the shear direction over a wide range.
  • the rotation of the third agitating blade 123 c causes a horizontal resin flow even at a deeper position in the agitation tank 101, and the agitation in the shearing direction due to the rotation of the arm portion 113 can be performed. Thereby, uniform stirring in the stirring tank 101 can be efficiently performed in a shorter time.
  • the number of the arm parts 113 of the first stirring jig 111 is two has been described above, the number of the arm parts 113 may be one, or may be three or more. . However, in consideration of the efficiency of stirring, it is desirable that the number of arm portions 113 is plural.
  • the plurality of arm portions 113 are provided on the first rotation shaft 112
  • the plurality of arm portions 113 are equiangularly spaced around the first rotation shaft 112 in a plane perpendicular to the first rotation shaft 112. It is desirable from the viewpoint of further reducing the unevenness of stirring in the stirring tank 101.
  • each arm portion 113 is arranged around the first rotation shaft 112 at intervals of 180 °.
  • the arm portions 113 are arranged around the first rotation shaft 112 at 120 ° intervals.
  • the four arm portions 113 are provided on the first rotation shaft 112, it is desirable that the arm portions 113 are arranged around the first rotation shaft 112 at 90 ° intervals.
  • the number of the 2nd stirring jig 121 in the stirring tank 101 is two
  • the number of the 2nd stirring jig 121 may be one, There may be three or more.
  • the number of the second stirring jigs 121 is preferably plural.
  • the second stirring jig 121 is provided in the stirring tank 101 within a plane perpendicular to the first rotation shaft 112 of the first stirring jig 111.
  • a plurality of equiangular intervals around the first rotating shaft 112 is desirable from the viewpoint of further reducing unevenness in stirring in the stirring tank 101.
  • the second stirring jigs 121 are arranged around the first rotation shaft 112 at intervals of 180 °. It is desirable.
  • the second stirring jigs 121 are arranged around the first rotation shaft 112 at intervals of 120 °. Further, when four second stirring jigs 121 are provided in the stirring tank 101, it is desirable that the second stirring jigs 121 are arranged around the first rotation shaft 112 at 90 ° intervals. Note that the number of the second stirring jigs 121 may be the same as or different from the number of the arm portions 113 of the first stirring jig 111.
  • any of acrylic resins, cycloolefin resins, and polyarylate resins can be used as the resin used for manufacturing the optical film, that is, the resin that is added to the stirring tank 101 and stirred and mixed with the solvent. .
  • the (meth) acrylic resin preferably has a Tg (glass transition temperature) of 115 ° C. or higher, more preferably 120 ° C. or higher, still more preferably 125 ° C. or higher, and particularly preferably 130 ° C. or higher.
  • Tg glass transition temperature
  • the upper limit of Tg of the (meth) acrylic resin is not particularly limited, it is preferably 170 ° C. or less from the viewpoint of moldability.
  • any appropriate (meth) acrylic resin can be adopted as long as the effects of the present embodiment are not impaired.
  • poly (meth) acrylic acid ester such as polymethyl methacrylate, methyl methacrylate- (meth) acrylic acid copolymer, methyl methacrylate- (meth) acrylic acid ester copolymer, methyl methacrylate-acrylic acid ester- (Meth) acrylic acid copolymer, (meth) methyl acrylate-styrene copolymer (MS resin, etc.), a polymer having an alicyclic hydrocarbon group (for example, methyl methacrylate-cyclohexyl methacrylate copolymer, Methyl methacrylate- (meth) acrylate norbornyl copolymer, etc.).
  • Preferable examples include C1-6 alkyl poly (meth) acrylates such as poly (meth) acrylate methyl. More preferred is a methyl methacrylate-based resin containing methyl methacrylate as a main component (in the range of 50 to 100% by mass, preferably 70 to 100% by mass).
  • the acrylic resin includes not only the acrylic resin itself but also a copolymer of the acrylic resin and another resin (compound).
  • the (meth) acrylic resin examples include, for example, Acrypet VH and Acrypet VRL20A, Dianal BR52, BR80, BR83, BR85, BR88 (manufactured by Mitsubishi Rayon Co., Ltd.), KT75 (manufactured by Electrochemical Industry Co., Ltd.) ), Delpet 60N, 80N (manufactured by Asahi Kasei Chemicals Corporation), (meth) acrylic resin having a ring structure in the molecule described in JP-A-2004-70296, by intramolecular crosslinking or intramolecular cyclization reaction. Examples include the obtained high Tg (meth) acrylic resin system.
  • the (meth) acrylic resin it is also preferable to use a (meth) acrylic resin having a lactone ring structure.
  • examples of the (meth) acrylic resin having a lactone ring structure include JP 2000-230016, JP 2001-151814, JP 2002-120326, JP 2002-254544, and JP 2005. No. 146084 and the like.
  • an acrylic resin having an unsaturated carboxylic acid alkyl ester structural unit and a glutaric anhydride structural unit can be used as the (meth) acrylic resin.
  • the acrylic resin include JP-A-2004-70290, JP-A-2004-70296, JP-A-2004-163924, JP-A-2004-292812, JP-A-2005-314534, JP-A-2006-. Examples described in JP-A-131898, JP-A-2006-206881, JP-A-2006-265532, JP-A-2006-283013, JP-A-2006-299905, JP-A-2006-335902, and the like. It is done.
  • thermoplastic resin having a glutarimide unit, a (meth) acrylic acid ester unit, and an aromatic vinyl unit
  • thermoplastic resin examples include JP-A-2006-309033, JP-A-2006-317560, JP-A-2006-328329, JP-A-2006-328334, JP-A-2006-337491, and JP-A-2006. -337374, JP-A-2006-337493, JP-A-2006-337569, and the like.
  • cycloolefin resin examples include a polymer or copolymer of a monomer having a structure represented by the following general formula (S).
  • each of R 1 to R 4 independently represents a hydrogen atom, a hydrocarbon group, a halogen atom, a hydroxy group, a carboxy group, an acyloxy group, an aryloxycarbonyl group, an alkoxycarbonyl group, an alkoxy group, a cyano group, or an amide group.
  • an imide group a silyl group, or a polar group (that is, a halogen atom, a hydroxy group, an acyloxy group, an aryloxycarbonyl group, an alkoxycarbonyl group, an alkoxy group, a cyano group, an amide group, an imide group, or a silyl group) Hydrocarbon group.
  • a polar group that is, a halogen atom, a hydroxy group, an acyloxy group, an aryloxycarbonyl group, an alkoxycarbonyl group, an alkoxy group, a cyano group, an amide group, an imide group, or a silyl group
  • R 1 to R 4 may be bonded to each other to form an unsaturated bond, monocycle or polycycle, and this monocycle or polycycle has a double bond.
  • an aromatic ring may be formed.
  • R 1 and R 2 , or R 3 and R 4 may form an alkylidene group.
  • p and m are integers of 0 or more.
  • the hydrocarbon group represented by R 1 and R 3 is preferably a hydrocarbon group having 1 to 10 carbon atoms, more preferably 1 to 4 carbon atoms, and particularly preferably 1 to 2 carbon atoms.
  • R 2 and R 4 are each a hydrogen atom or a monovalent organic group, and at least one of R 2 and R 4 preferably represents a polar group having a polarity other than a hydrogen atom or a hydrocarbon group, and m is 0
  • the glass transition temperature here is a value obtained by a method based on JIS K 7121-2012 using DSC (Differential Scanning Colorimetry).
  • Examples of the polar group of the specific monomer include a carboxy group, a hydroxy group, an alkoxycarbonyl group, an allyloxycarbonyl group, an amino group, an amide group, and a cyano group. These polar groups have a linking group such as a methylene group. It may be bonded via.
  • a hydrocarbon group in which a divalent organic group having polarity such as a carbonyl group, an ether group, a silyl ether group, a thioether group, or an imino group is bonded as a linking group can also be mentioned as a polar group.
  • a carboxy group, a hydroxy group, an alkoxycarbonyl group or an allyloxycarbonyl group is preferable, and an alkoxycarbonyl group or an allyloxycarbonyl group is particularly preferable.
  • a monomer in which at least one of R 2 and R 4 is a polar group represented by the formula — (CH 2 ) n COOR is obtained by using a cycloolefin resin having a high glass transition temperature, a low hygroscopic property, and various materials. It is preferable at the point from which it has the outstanding adhesiveness.
  • R is a hydrocarbon group having 1 to 12 carbon atoms, more preferably 1 to 4 carbon atoms, particularly preferably 1 to 2 carbon atoms, and preferably an alkyl group.
  • copolymerizable monomer examples include cycloolefin resins such as cyclobutene, cyclopentene, cycloheptene, cyclooctene, and dicyclopentadiene.
  • the number of carbon atoms of the cycloolefin is preferably 4-20, and more preferably 5-12.
  • the cycloolefin resin can be used alone or in combination of two or more.
  • a preferred molecular weight of the cycloolefin resin is an intrinsic viscosity [ ⁇ ] inh of 0.2 to 5 cm 3 / g, more preferably 0.3 to 3 cm 3 / g, particularly preferably 0.4 to 1.5 cm 3 / g.
  • the number average molecular weight (Mn) in terms of polystyrene measured by gel permeation chromatography (GPC) is 8000 to 100,000, more preferably 10,000 to 80,000, particularly preferably 12,000 to 50,000, and the weight average molecular weight (Mw). Is from 20,000 to 300,000, more preferably from 30,000 to 250,000, particularly preferably from 40,000 to 200,000.
  • Inherent viscosity [ ⁇ ] inh , number average molecular weight and weight average molecular weight are within the above ranges, so that heat resistance, water resistance, chemical resistance, mechanical properties of the cycloolefin resin, and molding of the optical film of the present embodiment And is good.
  • the glass transition temperature (Tg) of the cycloolefin resin is usually 110 ° C. or higher, preferably 110 to 350 ° C., more preferably 120 to 250 ° C., and particularly preferably 120 to 220 ° C.
  • Tg is 110 ° C. or higher because deformation is unlikely to occur due to use under high temperature conditions or secondary processing such as coating or printing.
  • Tg is 350 ° C. or lower, the case where the molding process becomes difficult can be avoided, and the possibility that the resin deteriorates due to heat during the molding process can be reduced.
  • cycloolefin resin a specific hydrocarbon resin described in, for example, Japanese Patent Application Laid-Open No. 9-221577 and Japanese Patent Application Laid-Open No. 10-287732, or a known heat can be used without departing from the effect of the present embodiment.
  • Plastic resins, thermoplastic elastomers, rubbery polymers, organic fine particles, inorganic fine particles, etc. may be blended.
  • An additive such as an absorbent may be included.
  • cycloolefin resin a commercially available product can be preferably used as the cycloolefin resin.
  • examples of commercially available products are sold under the trade names Arton (registered trademark) G, Arton F, Arton R, and Arton RX by JSR Corporation.
  • ZEONOR (registered trademark) ZF14, ZF16, ZEONEX (registered trademark) 250 or ZEONEX 280 is commercially available from ZEON Corporation, and these can be used.
  • the polyarylate resin contains at least an aromatic dialcohol component unit and an aromatic dicarboxylic acid component unit.
  • the aromatic dialcohol for obtaining the aromatic dialcohol component unit is preferably a bisphenol represented by the following formula (1), more preferably a bisphenol represented by the following formula (1 ′).
  • L in the general formulas (1) and (1 ′) is a divalent organic group.
  • the divalent organic group is preferably a single bond, an alkylene group, —S—, —SO—, —SO 2 —, —O—, —CO— or —CR 1 R 2 — (R 1 and R 2 are To form an aliphatic ring or an aromatic ring.
  • the alkylene group is preferably an alkylene group having 1 to 10 carbon atoms, and examples thereof include a methylene group, an ethylene group, and an isopropylidene group.
  • the alkylene group may further have a substituent such as a halogen atom or an aryl group.
  • R 1 and R 2 of —CR 1 R 2 — are bonded to each other to form an aliphatic ring or an aromatic ring.
  • the aliphatic ring is preferably an aliphatic hydrocarbon ring having 5 to 20 carbon atoms, and preferably a cyclohexane ring which may have a substituent.
  • the aromatic ring is an aromatic hydrocarbon ring having 6 to 20 carbon atoms, preferably a fluorene ring which may have a substituent.
  • Examples of —CR 1 R 2 — that forms a cyclohexane ring which may have a substituent include cyclohexane-1,1-diyl group, 3,3,5-trimethylcyclohexane-1,1-diyl group and the like. included.
  • Examples of —CR 1 R 2 — forming a fluorene ring which may have a substituent include a fluorenediyl group represented by the following formula.
  • R in the general formulas (1) and (1 ′) may independently be an alkyl group having 1 to 5 carbon atoms or an aryl group having 6 to 10 carbon atoms.
  • n is independently an integer of 0 to 4, preferably an integer of 0 to 3.
  • Examples of bisphenols in which L is an alkylene group include 1,1-bis (4-hydroxyphenyl) methane, 1,1-bis (4-hydroxyphenyl) ethane, 1,1-bis (4-methyl-2 -Hydroxyphenyl) methane, 1,1-bis (3,5-dimethyl-4-hydroxyphenyl) methane, 2,2-bis (4-hydroxyphenyl) -4-methylpentane, 2,2-bis (4- Hydroxyphenyl) propane (BPA), 2,2-bis (3-methyl-4-hydroxyphenyl) propane (BPC), 2,2-bis (3,5-dimethyl-4-hydroxyphenyl) propane (TMBPA), etc. Is included.
  • BPA 2,2-bis (4-hydroxyphenyl) propane
  • BPC 2,2-bis (3-methyl-4-hydroxyphenyl) propane
  • TMBPA isopropylidene-containing bisphenols such as 4-hydroxyphenyl) propane
  • Examples of bisphenols where L is —S—, —SO— or —SO 2 — include bis (4-hydroxyphenyl) sulfone, bis (2-hydroxyphenyl) sulfone, bis (3,5-dimethyl-4 -Hydroxyphenyl) sulfone (TMBPS), bis (3,5-diethyl-4-hydroxyphenyl) sulfone, bis (3-methyl-4-hydroxyphenyl) sulfone, bis (3-ethyl-4-hydroxyphenyl) sulfone, Bis (4-hydroxyphenyl) sulfide, bis (3,5-dimethyl-4-hydroxyphenyl) sulfide, bis (3,5-diethyl-4-hydroxyphenyl) sulfide, bis (3-methyl-4-hydroxyphenyl) Sulfide, bis (3-ethyl-4-hydroxyphenyl) sulfide, 2,4-dihydro Shi diphenyl sulfone and the
  • Examples of bisphenols in which L is —CR 1 R 2 — and R 1 and R 2 are bonded to form an aliphatic ring include 1,1-bis (4-hydroxyphenyl) cyclohexane (BPZ) And bisphenols having a cyclohexane skeleton such as 1,1-bis (4-hydroxyphenyl) -3,3,5-trimethylcyclohexane (BPTMC).
  • BPZ 1,1-bis (4-hydroxyphenyl) cyclohexane
  • BPTMC 1,1-bis (4-hydroxyphenyl) -3,3,5-trimethylcyclohexane
  • Examples of bisphenols in which L is —CR 1 R 2 — and R 1 and R 2 are bonded to each other to form an aromatic ring include 9,9-bis (3-methyl-4-hydroxyphenyl) Bisphenols having a fluorene skeleton such as fluorene (BCF) and 9,9-bis (3,5-dimethyl-4-hydroxyphenyl) fluorene (BXF) are included.
  • BCF fluorene
  • BXF 9,9-bis (3,5-dimethyl-4-hydroxyphenyl) fluorene
  • the aromatic dialcohol component constituting the polyarylate may be one kind or two or more kinds.
  • a sulfur atom (—S—, —SO— or —SO 2 —) is present in the main chain.
  • Bisphenols contained are preferred.
  • bisphenols containing a sulfur atom in the main chain and bisphenols having a cycloalkylene skeleton are preferred.
  • bisphenols having a fluorene skeleton are preferred.
  • Bisphenols having a cyclohexane skeleton and bisphenols having a fluorene skeleton are preferably used in combination with bisphenols containing an isopropylidene group.
  • the content ratio of the bisphenol having a cyclohexane skeleton or the bisphenol having a fluorene skeleton to the bisphenol having an isopropylidene group is 10/90 to 90/10 (molar ratio), preferably 20/80 to 80/20 (molar ratio).
  • the polyarylate may further contain an aromatic polyhydric alcohol component unit other than the aromatic dialcohol component as long as the effects of the present embodiment are not impaired.
  • aromatic polyhydric alcohol component examples include the compounds described in paragraph [0015] of Japanese Patent No. 4551503. Specifically, tris (4-hydroxyphenyl) methane, 4,4 ′-[1- [4- [1- (4-hydroxyphenyl) -1-methylethyl] phenyl] ethylidene] bisphenol, 2,3, 4,4′-tetrahydroxybenzophenone, 4- [bis (4-hydroxyphenyl) methyl] -2-methoxyphenol, tris (3-methyl-4-hydroxyphenyl) methane and the like are included.
  • the content ratio of these aromatic polyhydric alcohol component units can be appropriately set according to the required characteristics, but is 5 for example with respect to the total of the aromatic dialcohol component unit and the other aromatic polyhydric alcohol component units. It may be less than mol%.
  • the aromatic dicarboxylic acid constituting the aromatic dicarboxylic acid component unit may be terephthalic acid, isophthalic acid or a mixture thereof.
  • a mixture of terephthalic acid and isophthalic acid is preferable.
  • terephthalic acid / isophthalic acid 90/10 to 10/90 (molar ratio), more preferably 70/30 to 30/70, and still more preferably 50/50.
  • the polyarylate may further contain an aromatic dicarboxylic acid component unit other than terephthalic acid and isophthalic acid as long as the effects of the present embodiment are not impaired.
  • aromatic dicarboxylic acid components include orthophthalic acid, 2,6-naphthalenedicarboxylic acid, diphenic acid, 4,4′-dicarboxydiphenyl ether, bis (p-carboxyphenyl) alkane, 4,4′- Dicarboxyphenyl sulfone and the like are included.
  • the content ratio of aromatic dicarboxylic acid component units other than terephthalic acid and isophthalic acid can be appropriately set according to the required properties, but the total of terephthalic acid component, isophthalic acid component unit and other aromatic dicarboxylic acid component units For example, it may be 5 mol% or less.
  • the glass transition temperature of the polyarylate is preferably 260 ° C. or higher and 350 ° C. or lower, more preferably 265 ° C. or higher and lower than 300 ° C., further preferably 270 ° C. or higher and lower than 300 ° C.
  • the glass transition temperature of polyarylate can be measured according to JIS K7121 (1987). Specifically, using a DSC 6220 manufactured by Seiko Instruments Inc. as a measuring device, it can be measured under the conditions of a 10 mg polyarylate sample and a heating rate of 20 ° C./min.
  • the glass transition temperature of polyarylate can be adjusted by the type of aromatic dialcohol component constituting polyarylate.
  • aromatic dialcohol component units For example, it is preferable to include “units derived from bisphenols containing a sulfur atom in the main chain” as aromatic dialcohol component units.
  • the intrinsic viscosity of the polyarylate is preferably from 0.3 to 1.0 dl / g, more preferably from 0.4 to 0.9 dl / g, still more preferably from 0.45 to 0.8 dl / g. More preferably, it is 5 to 0.7 dl / g.
  • the intrinsic viscosity of polyarylate is 0.3 dl / g or more, the molecular weight of the resin composition tends to be a certain level or more, and a film having sufficient mechanical properties and heat resistance is easily obtained.
  • the intrinsic viscosity of the polyarylate is 1.0 dl / g or less, an excessive increase in the solution viscosity during film formation can be suppressed.
  • the intrinsic viscosity can be measured in accordance with ISO1628-1. Specifically, a solution in which a polyarylate sample is dissolved in 1,1,2,2-tetrachloroethane so as to have a concentration of 1 g / dl is prepared. The intrinsic viscosity of this solution at 25 ° C. is measured using an Ubbelohde type viscosity tube.
  • the polyarylate production method may be a known method, preferably an interface in which an aromatic dicarboxylic acid halide dissolved in an organic solvent incompatible with water and an aromatic dialcohol dissolved in an alkaline aqueous solution are mixed. It may be a polymerization method (W. M. EARECKSON, J. Poly. Sci. XL 399, 1959, Japanese Patent Publication No. 40-1959).
  • the content of polyarylate may be 50% by mass or more, preferably 60% by mass or more, more preferably 80% by mass or more with respect to the entire polyarylate film.
  • a solvent used for manufacturing an optical film that is, a solvent for dissolving the above-described resin in a stirring tank of a stirring device
  • a solvent used for manufacturing an optical film for example, dichloromethane (methylene chloride, methylene chloride), chloroform, ethanol, butanol, isopropanol N-methyl-2-pyrrolidone, 1,3-dimethylimidazolidinone, N, N-dimethylacetamide, N, N-diethylacetamide, N, N-dimethylformamide, N, N-diethylformamide, N-methylcaprolactam , Hexamethylphosphoramide, tetramethylene sulfone, dimethyl sulfoxide, m-cresol, phenol, p-chlorophenol, 2-chloro-4-hydroxytoluene, diglyme, triglyme, tetraglyme, dioxane, ⁇ -buty Lactone, 1,3-d
  • additives to be contained in the dope fine particles, plasticizer, ultraviolet absorber, antioxidant, sugar ester compound, retardation adjusting agent, light stabilizer, antistatic agent, release agent A thickener or the like may be used.
  • plasticizer ultraviolet absorber
  • antioxidant antioxidant
  • sugar ester compound sugar ester compound
  • retardation adjusting agent retardation adjusting agent
  • light stabilizer antioxidant
  • antistatic agent antistatic agent
  • release agent A thickener or the like
  • the optical film of this embodiment preferably contains a matting agent in order to impart irregularities to the film surface during film formation, ensure slipperiness, and achieve a stable winding shape.
  • a matting agent By containing the matting agent, when the produced optical film is handled, it is possible to suppress damage and deterioration of transportability.
  • Examples of the matting agent include fine particles of inorganic compounds and fine particles of resin.
  • Examples of fine particles of inorganic compounds include silicon dioxide, titanium dioxide, aluminum oxide, zirconium oxide, calcium carbonate, calcium carbonate, talc, clay, calcined kaolin, calcined calcium silicate, hydrated calcium silicate, aluminum silicate, silicic acid Examples thereof include magnesium and calcium phosphate. Fine particles containing silicon are preferable in terms of low turbidity, and silicon dioxide is particularly preferable.
  • the average primary particle size of the fine particles is preferably in the range of 5 to 400 nm, and more preferably in the range of 10 to 300 nm. These may be mainly contained as secondary aggregates having a particle size of 0.05 to 0.3 ⁇ m. If the particles have an average particle size of 80 to 400 nm, the primary particles are not aggregated. It is also preferable that it is contained as.
  • the content of these fine particles in the optical film is preferably in the range of 0.01 to 3.0% by mass, and particularly preferably in the range of 0.01 to 2.0% by mass.
  • Silicon dioxide fine particles are commercially available under the trade names of, for example, Aerosil R972, R972V, R974, R812, 200, 200V, 300, R202, OX50, TT600 (manufactured by Nippon Aerosil Co., Ltd.). .
  • Zirconium oxide fine particles are commercially available, for example, under the trade names Aerosil R976 and R811 (manufactured by Nippon Aerosil Co., Ltd.) and can be used.
  • resin fine particles examples include silicone resin, fluororesin and acrylic resin.
  • Silicone resins are preferred, and those having a three-dimensional network structure are particularly preferred. For example, these are commercially available under the trade names of Tospearl 103, 105, 108, 120, 145, 3120 and 240 (manufactured by Toshiba Silicone Co., Ltd.), and these can be used.
  • Aerosil 200V, Aerosil R972V, and Aerosil R812 are particularly preferably used because they have a large effect of reducing the friction coefficient while keeping the haze of the optical film low.
  • a polyester resin can be used as a plasticizer to be added to the optical film.
  • the polyester resin is obtained by polymerizing a dicarboxylic acid and a diol, and 70% or more of the dicarboxylic acid structural unit (the structural unit derived from the dicarboxylic acid) is derived from the aromatic dicarboxylic acid, and the diol structural unit (derived from the diol). 70% or more of the structural unit is derived from an aliphatic diol.
  • the proportion of the structural unit derived from the aromatic dicarboxylic acid is 70% or more, preferably 80% or more, and more preferably 90% or more.
  • the proportion of the structural unit derived from the aliphatic diol is 70% or more, preferably 80% or more, and more preferably 90% or more.
  • Two or more polyester resins may be used in combination.
  • aromatic dicarboxylic acids include terephthalic acid, isophthalic acid, 2,6-naphthalenedicarboxylic acid, 1,5-naphthalenedicarboxylic acid, naphthalenedicarboxylic acid such as 2,7-naphthalenedicarboxylic acid, 4,4′-biphenyldicarboxylic acid, Examples include 3,4'-biphenyldicarboxylic acid and the like, and ester-forming derivatives thereof.
  • polyester resin aliphatic dicarboxylic acids such as adipic acid, azelaic acid, and sebacic acid, and monocarboxylic acids such as benzoic acid, propionic acid, and butyric acid can be used without departing from the object of the present invention.
  • Examples of the aliphatic diol include ethylene glycol, 1,3-propylene diol, 1,4-butanediol, 1,4-cyclohexanedimethanol, 1,6-hexanediol, and ester-forming derivatives thereof.
  • polyester resin monoalcohols such as butyl alcohol, hexyl alcohol, and octyl alcohol, and polyhydric alcohols such as trimethylolpropane, glycerin, and pentaerythritol can be used as long as the object of the present embodiment is not impaired. .
  • a known esterification method or transesterification method can be applied to the production of the polyester resin.
  • the polycondensation catalyst used in the production of the polyester resin include known antimony compounds such as antimony trioxide and antimony pentoxide, germanium compounds such as germanium oxide, titanium compounds such as titanium acetate, and aluminum compounds such as aluminum chloride. Although it can, it is not limited to these.
  • Preferred polyester resins include polyethylene terephthalate resin, polyethylene terephthalate-isophthalate copolymer resin, polyethylene-1,4-cyclohexanedimethylene-terephthalate copolymer resin, polyethylene-2,6-naphthalene dicarboxylate resin, polyethylene-2, 6-naphthalene dicarboxylate-terephthalate copolymer resin, polyethylene-terephthalate-4,4'-biphenyldicarboxylate resin, poly-1,3-propylene-terephthalate resin, polybutylene terephthalate resin, polybutylene-2,6-naphthalene There are dicarboxylate resins and the like.
  • polyester resins include polyethylene terephthalate resin, polyethylene terephthalate-isophthalate copolymer resin, polyethylene-1,4-cyclohexanedimethylene-terephthalate copolymer resin, polybutylene terephthalate resin, and polyethylene-2,6-naphthalene dicarboxylate. Resin.
  • the intrinsic viscosity is 0.7 cm 3 / g or more
  • a molded product made of the polyester resin composition obtained by using the polyester resin has mechanical properties necessary as the molded product. And has good transparency.
  • the intrinsic viscosity is 2.0 cm 3 / g or less, the moldability is good.
  • compounds described in the general formulas (PEI) and (PEII) in paragraphs [0056] to [0080] of JP2013-97279A may be used.
  • stirring devices A to I satisfying the conditions shown in Table 1 were prepared.
  • the width of the stirring tank 101 (diameter of the bottom surface 101a) is 2100 mm, and the height of the liquid level when the resin and the solvent are put into the stirring tank 101 is the first stirring speed. It is a position 500 mm above the uppermost portion 113a of the arm portion 113 of the jig 111, the height from the bottom surface 101a of the uppermost portion 113a of the arm portion 113 is 2000 mm, and the length L of the arm portion 113 is 1800 mm.
  • the distance between the uppermost portions 113a of the two arm portions 113 is 2050 mm, and the distance between the first rotation shaft 112 and the second rotation shaft 122 is The distance was 750 mm.
  • each of the stirring inversions A to I is schematically shown in FIGS. 13 to 18.
  • the position of the central portion in the height direction of the arm portion 113 of the first stirring jig 111 is indicated by a position B.
  • the polymer solution continuously discharged from the polymerization reactor is supplied to a vent type screw type extruder having a reduced pressure of 2.7 to 4.0 kPa to remove volatile matter, and the pellet-shaped copolymer A1 is removed.
  • the constituent ratio of the monomer unit in the copolymer A1 was 90 mol% for the styrene monomer, 10 mol% for the acrylic acid monomer, and the weight average molecular weight was 300,000.
  • the following components were stirred using the stirrer A prepared above and dissolved sufficiently with heating to prepare a dope 1.
  • the stirring speed (rotation speed) of the first stirring jig of the stirring device A was 50 rpm
  • the stirring speed (rotation speed) of the second stirring jig was 500 rpm.
  • the stirring time in the stirring apparatus A was 5 hours.
  • composition of dope 1 (styrene: 90 mol%, acrylic acid: 10 mol%, weight average molecular weight: 300,000) 100 parts by mass Matting agent R812 (manufactured by Nippon Aerosil Co., Ltd., silica particles, average particle size 8 nm) 0.30 parts by mass Methylene chloride 150 parts by mass Ethanol 5 parts by mass
  • the prepared dope 1 was uniformly cast on a stainless steel band support at a temperature of 22 ° C. and a width of 2 m using a belt casting apparatus.
  • the solvent was evaporated on the stainless steel band support until the residual solvent amount reached 50%, and the obtained film-like material was peeled off from the stainless steel band support with a peeling tension of 162 N / m.
  • the peeled film-like product was dried at a drying temperature of 135 ° C. while evaporating the solvent at 35 ° C. and stretching it 1.25 times in the width direction (TD direction) by tenter stretching.
  • the residual solvent amount at the start of stretching by zone stretching was 20.0%, and the residual solvent amount at the start of stretching by tenter was 8.0%.
  • the obtained film was slit to a width of 1.5 m and subjected to a knurling process having a width of 10 mm and a height of 5 ⁇ m at both ends of the film, and then wound around a core to prepare an optical film 1 as an acrylic film.
  • the produced optical film 1 had a film thickness of 40 ⁇ m and a winding length of 4000 m.
  • Optical films 2 to 6 were respectively prepared in the same manner as the optical film 1 except that the stirrers B to F were used instead of the stirrer A to stir the resin and prepare dope.
  • the obtained ring-opening copolymer solution was put in an autoclave, and 100 g of toluene was further added.
  • a hydrogenation catalyst, RuHCl (CO) [P (C 6 H 5 )] 3 was added at 2500 ppm based on the monomer charge, the hydrogen gas pressure was adjusted to 9-10 MPa, and the reaction was carried out at 160-165 ° C. for 3 hours. went. After completion of the reaction, a hydrogenated product was obtained by precipitation in a large amount of methanol solution.
  • a main dope having the following composition was prepared. First, dichloromethane and ethanol were added to the stirrer A. The cycloolefin resin COP1 and the fine particle addition liquid were added to the stirring apparatus A containing dichloromethane while stirring. The resin was dissolved while heating and stirring, and this was dissolved in Azumi Filter Paper No. The main dope was prepared by filtration using 244. In addition, the stirring conditions in the stirring apparatus A are the same as the production of the optical film 1.
  • the prepared dope 1 was uniformly cast on a stainless steel band support at a temperature of 22 ° C. and a width of 2 m using a belt casting apparatus. The solvent was evaporated on the stainless steel band support until the residual solvent amount was 30%, and the obtained film-like material was peeled off from the stainless steel band support with a peeling tension of 162 N / m.
  • the peeled film-like material was dried at a drying temperature of 160 ° C. while evaporating the solvent at 35 ° C. and stretching it 1.25 times in the width direction (TD direction) by tenter stretching.
  • the residual solvent amount when starting stretching by zone stretching was 10.0%, and the residual solvent amount when starting stretching by a tenter was 5.0%.
  • the obtained film was slit to a width of 1.5 m and subjected to a knurling process having a width of 10 mm and a height of 5 ⁇ m at both ends of the film, and then wound on a core to prepare an optical film 7 as a cycloolefin.
  • the produced optical film 7 had a film thickness of 40 ⁇ m and a winding length of 4000 m.
  • optical film 8 was prepared in the same manner as optical film 1 except that the dope was prepared by stirring using chloroform in the same amount as methylene chloride instead of methylene chloride.
  • An optical film 9 was produced in the same manner as the production of the optical film 1 except that the dope 2 having the following composition including the acrylic resin 2 was used instead of the dope 1.
  • Composition of dope 2 Acrylic resin 2 (Dianar BR85, manufactured by Mitsubishi Rayon Co., Ltd.) 100 parts by mass Matting agent R812 (manufactured by Nippon Aerosil Co., Ltd., silica particles, average particle size 8 nm) 0.30 parts by mass Methylene chloride 150 parts by mass Ethanol 5 parts by mass
  • the obtained organic phase was washed with twice the amount of ion-exchanged water of the organic phase for each washing, and then the operation of separating the organic phase and the aqueous phase was repeated.
  • the washing was terminated when the electric conductivity of the washing water became less than 50 ⁇ S / cm.
  • the organic phase after washing was put into a hot water tank equipped with a homomixer at 50 ° C., and methylene chloride was evaporated to obtain a powdery polymer. Furthermore, dehydration and drying were performed to obtain polyarylate.
  • the obtained polymer solution was uniformly cast on a stainless belt of a belt casting apparatus.
  • a stainless steel belt having a length of 20 m was used.
  • the surface temperature of the stainless steel belt is 35 ° C. and 35 ° C. wind is applied to the casting film to evaporate the solvent until the residual solvent amount is 38%, and then the film is peeled off from the stainless steel belt to obtain a film-like material. It was.
  • the obtained film-like material was stretched 1.2 times at 170 ° C. in the MD direction using the peripheral speed difference between the rolls, and then stretched 1.2 times at 230 ° C. in the TD direction with a tenter.
  • the stretched film is dried for 30 minutes while being transported in a drying apparatus at 125 ° C. by a number of rolls, and then subjected to knurling with a width of 15 mm and a height of 10 ⁇ m at both ends in the width direction of the film. As a result, an optical film 10 having a film thickness of 40 ⁇ m was obtained.
  • Optical films 11 to 13 were respectively produced in the same manner as the optical film 1 except that the stirrers G to I were used instead of the stirrer A to stir the resin and prepare dope.
  • optical film 14 was prepared in the same manner as optical film 1 except that instead of methylene chloride, the same amount of THF (tetrahydrofuran) as methylene chloride was used for stirring to prepare a dope.
  • THF tetrahydrofuran
  • ⁇ Evaluation> Evaluation of film thickness unevenness
  • the film thickness ( ⁇ m) was measured using a micrometer at intervals of 10 mm in the width direction of the film, and the difference between the maximum value and the minimum value of each film thickness ( ⁇ m) was defined as film thickness unevenness.
  • the film thickness unevenness is 1.0 ⁇ m or less, there is no problem in actual use, and if it exceeds 1.0 ⁇ m, the level is problematic in actual use.
  • Evaluation criteria A: The number of foreign matters is 0.15 or less per 1 cm 2 . ⁇ The number of foreign matters is larger than 0.15 per 1 cm 2 and equal to or smaller than 0.20. ⁇ : The number of foreign matters is greater than 0.20 and less than or equal to 0.25 per cm 2 . X: The number of foreign matters is larger than 0.25 per 1 cm 2 and not larger than 0.35, but there is a problem in actual use. XX: The number of foreign matters is larger than 0.35 per cm 2 , which is a considerable problem in actual use.
  • Table 2 shows the resin, solvent, stirring device used for the production of each of the optical films 1 to 14, and the results of each evaluation.
  • the film thickness unevenness and the evaluation of foreign matters are poor. This is because the dope used for forming the optical film 11 was prepared using the stirring device G. However, in the stirring device G, as shown in FIG. Since the uppermost first stirring blade 123a is located at a position lower than the position A, which is vertically lowered by (1/3) L from the uppermost portion 113a of the arm portion 113 of the first stirring jig 111, It is considered that the resin having a small specific gravity and floating above the solvent could not be efficiently drawn downward by the first stirring blade 123a, resulting in uneven stirring.
  • the film thickness unevenness and the evaluation of foreign matters are poor.
  • the dope used for forming the optical film 12 was prepared by using the stirring device H.
  • the outermost portion of the second stirring jig 121 was used. Since the upper first stirring blade 123a is composed of a disk-type stirring blade that creates a flow in a direction perpendicular to the second rotating shaft 122, the resin having a small specific gravity and floating above the solvent is also used. This is probably because the first agitating blade 123a could not efficiently draw downward, and as a result, uneven stirring occurred.
  • the film thickness unevenness and the evaluation of foreign matters are poor.
  • the dope used for forming the optical film 13 was prepared by using the stirring device I.
  • the stirring blade is composed only of the first stirring blade 123a, and the resin drawn downward by the first stirring blade 123a cannot be stirred in the shear direction with the arm portion 113, and as a result, This is thought to be due to large unevenness in stirring.
  • the film thickness unevenness and the evaluation of the foreign matter are poor. This is because the resin used in the formation of the optical film 13 has a specific gravity greater than that of the solvent and is heavier. Therefore, even if the resin is stirred in the stirring tank 101, the resin does not flow upward, resulting in uneven stirring. It is done.
  • the dope used in the production of the optical films 1 to 10 was prepared by using any of the stirring devices A to F.
  • the second stirring treatment was performed.
  • the first stirring blade 123a of the tool 121 includes a position A and is positioned above this, and is configured with a stirring blade (propeller type, paddle type) that causes the resin to flow in the vertical direction.
  • the second stirring blade 123b is configured by a stirring blade (disk type, turbine type) that is positioned below the position B and causes a flow in a direction perpendicular to the second rotation shaft 122. This is considered to be because uniform stirring is achieved in the stirring tank 101.
  • the vertical stirring by the first stirring blade 123a and the shearing stirring by the second stirring blade 123b and the arm portion 113 are performed, so that the solvent and the resin Even if the specific gravity difference ⁇ is 0.1 ⁇ ⁇ 0.5, it is considered that the resin and the solvent in the stirring tank 101 were uniformly and efficiently stirred, and the stirring unevenness was reduced.
  • the stirring device F since the second stirring jig 121 has three stirring blades and stirring is performed more efficiently, the evaluation of film thickness unevenness and foreign matter is further improved by further reducing stirring unevenness. It is considered that.
  • stirring devices J to L satisfying the conditions shown in Table 3 were prepared.
  • the stirring device J has the same configuration as the stirring device A except that the number of arms of the first stirring jig of the stirring device A is changed from two to one.
  • the stirring device K has the same configuration as the stirring device A except that the number of arms of the first stirring jig of the stirring device A is changed from two to three. At this time, it is assumed that the three arm portions are provided at equal intervals of 120 degrees around the first rotation axis.
  • the stirring device L has the same configuration as the stirring device A except that the number of arms of the first stirring jig of the stirring device A is changed from two to four. At this time, it is assumed that the four arm portions are provided at equal intervals of 90 degrees around the first rotation axis.
  • Optical films 15 to 17 were respectively prepared in the same manner as the optical film 1 except that the stirrers J to L were used instead of the stirrer A to stir the resin and prepare dope.
  • stirring devices M to O satisfying the conditions shown in Table 4 were prepared.
  • the stirring device M has the same configuration as the stirring device A except that the number of second stirring jigs of the stirring device A is changed from two to one.
  • the stirring device N has the same configuration as the stirring device A except that the number of second stirring jigs of the stirring device A is changed from two to three. At this time, it is assumed that the three second stirring jigs are provided at equal intervals of 120 degrees around the second rotation axis.
  • the stirring device O has the same configuration as the stirring device A except that the number of second stirring jigs of the stirring device A is changed from two to four. At this time, it is assumed that the four second stirring jigs are provided at equal intervals of 90 degrees around the second rotation axis.
  • Optical films 18 to 20 were respectively prepared in the same manner as the optical film 1 except that the dope was prepared by stirring the resin and the like using the stirring devices M to O instead of the stirring device A.
  • optical films 15 to 20 produced above were evaluated for film thickness unevenness and foreign matter in the same manner as the optical film 1 and the like. The evaluation results are shown in Table 5.
  • the stirring device J used for forming the optical film 15 has fewer arm portions than the stirring device A. Further, the stirring device M used for forming the optical film 18 has a smaller number of second stirring jigs than the stirring device A. However, these stirring devices J and M are not substitute for satisfying the above conditions (1) and (2). Therefore, in the optical films 15 and 18, the film thickness unevenness and the evaluation of foreign matters are lower than those of the optical film 1, but the level is not problematic in actual use, and the stirring unevenness J and M are also reduced. It can be said that the effect is obtained.
  • the stirring devices K and L used in the production of the optical films 16 to 17 have more arms than the stirring device A, the stirring efficiency is further improved compared to the stirring device A, and uneven stirring is caused. It is considered that the film thickness was further reduced, and the evaluation of film thickness unevenness and foreign matter was further improved.
  • the stirring devices N and O used in the production of the optical films 19 to 20 have more second stirring jigs than the stirring device A, so that the stirring efficiency is further improved compared to the stirring device A. It is considered that the unevenness of stirring was further reduced, and the evaluation of unevenness of film thickness and foreign matters was further improved.
  • the manufacturing method of the optical film of the present embodiment described above can be expressed as follows.
  • a method for producing an optical film by a solution casting method A stirring preparation step of preparing a dope by stirring at least a resin and a solvent in a stirring tank; A casting step of casting the dope prepared in the stirring preparation step on a support,
  • the resin is any one of an acrylic resin, a cycloolefin resin, and a polyarylate resin, When the specific gravity of the resin is A, the specific gravity of the solvent is B, and the specific gravity difference (BA) is ⁇ , 0.1 ⁇ ⁇ 0.5
  • the stirring tank is provided with a first stirring jig and a second stirring jig,
  • the first stirring jig includes a first rotating shaft located on a vertical axis passing through the center of the bottom surface of the stirring tank, and a lowermost portion of the first rotating shaft, and the first stirring jig is moved in the stirring tank.
  • the second agitating jig is arranged such that the second agitation jig is aligned along the vertical direction with the second rotation axis extending in the vertical direction so as to pass through the space between the first rotation axis and the arm portion.
  • the length along the vertical direction of the arm portion of the first stirring jig is L, and among the at least two stirring blades of the second stirring jig, the uppermost stirring blade and one lower side thereof
  • the first stirring blade is located above and including a position vertically lowered by (1/3) L from the uppermost portion of the arm portion of the first stirring jig
  • the second stirring blade It is composed of a stirring blade that causes a vertical flow of the resin by rotation about the rotation axis of
  • the second agitating blade is located below a position vertically lowered by (1/3) L from the uppermost part of the arm portion of the first agitating jig
  • the second rotating shaft is
  • An optical system comprising: an agitating blade that causes a flow of the resin drawn vertically downward by the first agitating blade in a direction perpendicular to the second rotation axis by rotation about the center.
  • the second stirring jig further includes a third stirring blade positioned one lower than the second stirring blade, The method for producing an optical film as described in any one of 1 to 6, wherein the third stirring blade is a turbine-type or disk-type stirring blade.
  • the first stirring jig has a plurality of the arm portions at equiangular intervals around the first rotation axis in a plane perpendicular to the first rotation axis.
  • the manufacturing method of the optical film in any one of 1-7.
  • a plurality of the second stirring jigs are provided at equal angular intervals around the first rotation axis in a plane perpendicular to the first rotation axis of the first stirring jig in the stirring tank.
  • the present invention can be used for the production of an optical film by a solution casting film forming method.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Ophthalmology & Optometry (AREA)
  • Moulding By Coating Moulds (AREA)
  • Polarising Elements (AREA)
  • Optical Elements Other Than Lenses (AREA)
  • Mixers Of The Rotary Stirring Type (AREA)

Abstract

La présente invention concerne un procédé de fabrication d'un film optique qui comprend une étape de préparation par agitation et une étape d'expansion de flux. Lorsque la densité relative de la résine agitée est exprimée par A, la densité relative d'un solvant est exprimée par B et une différence de densité (B - A) est exprimée par ∆, la formule 0,1 < ∆ < 0,5 est satisfaite. Un premier appareil d'agitation (111) possède un premier arbre de rotation (112) et une partie bras (113). Un second appareil d'agitation (121) possède un second arbre de rotation (122), une première lame d'agitation (123a), et une seconde lame d'agitation (123b). Lorsqu'une longueur de la partie bras (113), dans une direction verticale, est exprimée par L, la première lame d'agitation (123a) est placée à un emplacement qui comprend ou qui est au-dessus d'un emplacement A qui est inférieur à une partie supérieure (113a) de la partie bras (113) de (1/3) L dans la direction verticale. La seconde lame d'agitation (123b) est placée en dessous de l'emplacement A.
PCT/JP2017/020867 2016-08-10 2017-06-05 Procédé de fabrication de film optique WO2018029955A1 (fr)

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WO2007108323A1 (fr) * 2006-03-22 2007-09-27 Konica Minolta Opto, Inc. Film d'ester de cellulose et procédé servant à produire celui-ci
JP2012081743A (ja) * 2010-09-15 2012-04-26 Fujifilm Corp 混合装置、流延ドープの製造方法及び溶液製膜方法

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JPH0677823U (ja) * 1994-02-07 1994-11-01 株式会社日立製作所 撹拌装置
JP3648279B2 (ja) * 1995-01-09 2005-05-18 佐竹化学機械工業株式会社 中・高粘度用撹拌翼
CN2463040Y (zh) * 2000-12-28 2001-12-05 上海理日科技发展有限公司 特殊锚形搅拌机
KR100626613B1 (ko) * 2005-04-06 2006-09-25 동양제강 주식회사 초고강도 폴리에틸렌섬유 제조장치
JP2010042337A (ja) 2008-08-11 2010-02-25 Sumitomo Electric Ind Ltd フッ素樹脂多孔膜、その製造方法及びフィルター
JP5134468B2 (ja) * 2008-08-18 2013-01-30 日東電工株式会社 撹拌装置
DE102009002630B4 (de) * 2009-04-24 2019-12-24 Robert Bosch Gmbh Vorrichtung zur Dosierung pulverförmiger Substanzen
JP2013094697A (ja) * 2011-10-28 2013-05-20 Satake Chemical Equipment Mfg Ltd 撹拌装置
CN202725176U (zh) * 2012-08-09 2013-02-13 厦门路桥翔通建材科技有限公司 搪玻璃反应罐用搅拌器
CN102861902B (zh) * 2012-09-10 2014-05-07 北京科技大学 一种复合搅拌半固态浆料连续制备装置
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JPS6039326U (ja) * 1983-08-26 1985-03-19 株式会社新潟鐵工所 固液混合タンク
WO2007108323A1 (fr) * 2006-03-22 2007-09-27 Konica Minolta Opto, Inc. Film d'ester de cellulose et procédé servant à produire celui-ci
JP2012081743A (ja) * 2010-09-15 2012-04-26 Fujifilm Corp 混合装置、流延ドープの製造方法及び溶液製膜方法

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KR102136476B1 (ko) 2020-07-21
JPWO2018029955A1 (ja) 2019-06-06
JP6911863B2 (ja) 2021-07-28
CN109641374A (zh) 2019-04-16
CN109641374B (zh) 2020-10-30

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