CN101851342A - Solution film-forming method - Google Patents
Solution film-forming method Download PDFInfo
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- CN101851342A CN101851342A CN201010144917A CN201010144917A CN101851342A CN 101851342 A CN101851342 A CN 101851342A CN 201010144917 A CN201010144917 A CN 201010144917A CN 201010144917 A CN201010144917 A CN 201010144917A CN 101851342 A CN101851342 A CN 101851342A
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Abstract
The invention discloses a kind of solution film-forming method.Liquor charging direction along doping liquid in the doping liquid stream of dynamic mixer is provided with four rotors.Rotor is installed on turning axle with certain spacing on the axial X of turning axle.Motor makes the rotor rotation by giving motivating force to turning axle.Rotor comprises: at turning axle fixed rotor subject; At the interface of rotor subject with about 90 ° spacing away from and be fixed in four agitating vanes of turning axle.The preferred 0.1m/ of outer roll surface speed second of dynamic mixer, above and 1.0m/ was below second.
Description
Technical field
The present invention relates to use and added the doping liquid of film being given the additive of various functions, make the solution film-forming method of film.
Background technology
Polymeric film has superior photopermeability or flexibility, can the light weight filming.Therefore, polymeric film utilizes in various fields as optical functional film.In polymeric film; comprise that cellulose ester especially has the TAC film of the cellulosic triacetate (hereinafter referred to as " TAC ") of 57.5%～62.5% average acidylate degree (degree of acetylation), as being the protective film or the optical compensating film utilization of polarization plates with the structure unit of liquid crystal indicator headed by the film, the market expansion in recent years (LCD) with picture photosensitive.
As the manufacture method of TAC film, for example, open disclosing in the 2006-076280 communique as the spy, knowing has solution film-forming method.Solution film-forming method is compared with other manufacture method such as solution film-forming methods, can know the superior films of rerum natura such as optical property.In solution film-forming method, at first, the doping liquid for dissolved polymkeric substance in solvent mixes various additives, and preparation stream is moulded doping liquid.As solvent, methylene dichloride or ritalin etc. are arranged.As additive, UV light absorber (UV agent), roughening agent are arranged, delay control agent, reach softening agent etc.Secondly, utilize the stream mold, make stream mould doping liquid and mould, form the stream plastic film at the supporter upper reaches.Also have, the stream plastic film will flow plastic film from supporter and peel off as wetting film after having self-supporting on the supporter.Also have, the wetting film that drying is peeled off as the goods film, is a roll form with this goods winding film with it.
As the blending means to the additive of doping liquid, knowing has the doping liquid stream that flows through at doping liquid that the interpolation nozzle is set, and via adding nozzle, additive liquid is sent into continuous (in-line) interpolation of doping liquid.Additive liquid is to disperse or dissolve the solid additive in the liquid of regulation.After having added additive liquid, utilize and specially to open 2006-076280 number, spy and open 2006-88583 communique, spy and drive the static mixer shown in each communique of 2007-215574 number, mix doping liquid and additive.Also have, put down in writing in patent documentation 1 by making up Suhl type mixing tank (sulzer mixer) and Kai Nike type mixing tank (kenics mixer) now, efficient mixes well.In addition, open to have put down in writing in the 2006-88583 communique the spy and in doping liquid, do not produce the foreign matter ground method that the stream of liquid moulds that stops to mix.In addition, open the spy and to have put down in writing in the 2007-215574 communique, be suppressed at the situation that additive is supplied with the condensation product that production line produces by vacuum breaker being formed the structure of regulation.
In recent years, according to the variation of the purposes of polymeric film, seek to make the film of various qualities.The quality of film is stipulated by the kind or the addition of additive liquid.Therefore, in order in a thin film fabrication production line, to make the film of many kinds, need suitably switch the kind or the addition of additive liquid according to the quality of film.
Quality change by film, switch additive liquid addition during in, the addition of additive etc. does not reach the benchmark value of the film of quality change object, therefore, the film of Zhi Zaoing becomes waste disposal betwixt.Thereby, in order to reduce the film that becomes waste disposal, suppress manufacturing cost, the time that the addition etc. of additive liquid is reached till the benchmark value of film of quality change object is minimum limit.In order to make the described time is minimum limit, additive need be mixed in the doping liquid equably, reliably and promptly carries out the mixing to the additive liquid of doping liquid.
Summary of the invention
The object of the present invention is to provide can be reliably and promptly carry out blended solution film-forming method to the additive liquid of doping liquid.
Solution film-forming method of the present invention comprises: the step of preparation doping liquid; The step of feeding additive liquid; Make the step of stream mold; Make the step of film.In the step of preparation doping liquid, preparation comprises the doping liquid of polymkeric substance and solvent.In the step of feeding additive liquid, in pipe arrangement with described doping liquid liquor charging, feeding additive liquid.In the step of making the stream mold, mix described doping liquid and described additive liquid, form the stream mold.Described mixing utilizes dynamic mixer to carry out.Described dynamic mixer has the stator (stator) and the rotor (rotor) of multistage on the liquor charging direction of described doping liquid.In the step of making film, use described stream mold, make film.
Preferably in above-mentioned solution film-forming method, the viscosity of carrying the described doping liquid of described additive liquid is more than the 30Pas.The viscosity ratio (%) of more preferably described additive liquid and described doping liquid is below 10%.Described viscosity ratio is obtained by { 100 * (viscosity of described additive liquid)/(viscosity of described doping liquid) }.
The outer roll surface speed of preferred described dynamic mixer is the 0.1m/ second of above and 1.0m/ below second.Static pressure in more preferably making in the described dynamic mixer is the driving that 0.1MPa controls described rotor abovely.
Preferred described stator is accommodated described rotor in the mode that can rotate, and is formed with the gap that 0.3mm is above and 1.5mm is following between described stator and the described rotor.
The residence time of preferred described doping liquid is more than 0.1 second.This residence time is the time of described doping liquid in described each stator and rotor delay.
Preferred described mixing is except described dynamic mixer, also utilizes the static mixer that is provided with in the upstream of described dynamic mixer to carry out.The mutual different first described additive liquid and the second described additive liquid is mixed in described doping liquid, and described static mixer possesses: described pipe arrangement; First nozzle that the first additive liquid is supplied with in described pipe arrangement; And second nozzle that the second described additive liquid is supplied with in described pipe arrangement, described second nozzle arrangement is in the downstream of first nozzle.
Preferred described mixing is except described dynamic mixer, also utilizes the static mixer that is provided with in the downstream of described dynamic mixer to carry out.
According to the present invention as can be known, can be reliably and promptly carry out mixing to the additive liquid of doping liquid.
Description of drawings
Above-mentioned purpose, advantage can be read the detailed explanation of preferred embodiment by with reference to accompanying drawing, and those of ordinary skills are easily understood.
Fig. 1 is the sketch chart of solution film-forming equipment.
Fig. 2 is the sketch chart of continuous stirred tank reactor.
Fig. 3 is the sectional view of dynamic mixer.
Fig. 4 is the stereographic map of rotor and stator.
Fig. 5 is the sketch chart of system film unit.
Embodiment
As shown in Figure 1, solution film-forming equipment 10 possesses: doping liquid preparation unit 11; Additive liquid adds mixed cell 12; System film unit 13.
Doping liquid preparation unit 11 comprises: mixing portion 15; Dissolving portion 16; Concentrate portion 17; Reservoir 18.Mixing portion 15 mixes polymkeric substance 26 and solvent 27 and makes thick lysate.The thick lysate of dissolving portion 16 dissolvings, preparation doping liquid 31.Concentrate portion 17 the concentrating of liquid 31 of mixing.Reservoir 18 is stored doping liquid 31.Mixing portion 15 has: first and second jar 21,22, dissolving vessel 23, hold tank 24, pump 25.In first jar 21, put into polymkeric substance 26.In dissolving vessel 23, drop into the polymkeric substance 26 about the specified amount that utilizes accessory gauger (omitting diagram) metering.In second jar 22, put into solvent 27.To drop into dissolving vessel 23 by the solvent 27 about the specified amount of accessory pump (omitting diagram) metering.
Polymkeric substance 26 does not limit especially, goes for solution film-forming method and gets final product.If can carry out in the polymkeric substance of solution film-forming, use cellulose acylate, then can access the transparency height, the film that optical characteristics is superior.Therefore, cellulose acylate is fit to the component of polymer of polarization plates with the film of optical applications such as protective film or optical compensating film.In cellulose acylate, using cellulose ethanoate, the mean value that especially uses degree of acetylation is under the situation of 57.5%～62.5% cellulosic triacetate, can access the superior film of optical characteristics.Above-mentioned degree of acetylation be meant the Mierocrystalline cellulose per unit weight in conjunction with the acetic acid amount.Degree of acetylation can be obtained according to the mensuration and the calculating of the degree of acetylation among the ASTM:D-817-91 (test methods of cellulose ethanoate etc.).In the present embodiment, use granulous TAC.Under the situation of using granulous TAC, from the viewpoint of the intermiscibility of solvent 27, the particle diameter of the above preferred 0.1～4mm of the 90 weight % of granulous TAC, the more preferably particle diameter of 1～4mm.
Also have,, be recorded in the spy and open [0140] paragraph of 2005-104148 communique in [0195] paragraph about the details of cellulose acylate.In addition, about solvent and softening agent, deterioration preventing agent, UV light absorber (UV agent), optical anisotropy control agent, delay control agent, dyestuff, roughening agent, peel off additive such as promotor, at length be recorded in the spy too and open [0196] paragraph of 2005-104148 communique in [0516] paragraph.About manufacture method, at length be recorded in the spy too and open [0517] paragraph of 2005-104148 number in [0916] paragraph based on the film of the solution film-forming method that has used cellulose acylate.These records also go among the present invention.
Solvent 27 is fit to halohydrocarbon, ester class, ketone, ethers, alcohols etc.Wherein, solvent 27 does not limit especially, and the solvability of the polymkeric substance 26 of consideration and use waits suitably to be selected to get final product.Solvent 27 can be a kind of compound, can be mixed solvent for the mixture that has mixed a plurality of compounds also.As solvent 27, specifically, (for example can enumerate halohydrocarbon, methylene dichloride etc.), the ester class (for example, ritalin, toluic acid ester, ethylhexoate, amyl group acetic ester, butylacetic acid ester etc.), ketone (for example, acetone, butanone, pimelinketone etc.), ethers (for example, diox, two oxa-s, penta ring, tetrahydrofuran (THF), Anaesthetie Ether, methyl tertiary butyl ether etc.), alcohols (for example, methyl alcohol, ethanol etc.) etc.
Dissolving vessel 23 possesses agitating vane (omitting diagram).By this agitating vane rotation, polymkeric substance and solvent in the stirring and dissolving jar 23.Stir by this, obtain the thick lysate that polymkeric substance is not dissolved in solvent fully.
Thick lysate interim storage in the dissolving vessel 23 is in hold tank 24, and thus, dissolving vessel 23 becomes sky, therefore, can begin the making of thick lysate in dissolving vessel 23.Thereby,, can carry out making based on the thick lysate of batch type by two jars of dissolving vessel 23 and hold tank 24 are set.Hold tank 24 also possesses agitating vane.By this agitating vane rotation, in hold tank 24, also stir thick lysate.
Thick lysate in the hold tank 24 is carried to the primary heater 30 of dissolving portion 16 by pump 25.Primary heater 30 possesses multi tube heat exchanger and silent oscillation mixing tank etc., heating when stirring thick lysate.Preferred 50～120 ℃ of Heating temperature, preferred 5～30 minutes of heat-up time.By this heating, required polymkeric substance 26 solutes such as grade of solution film-forming never degenerate and dissolving fully, and thick lysate becomes doping liquid 31.
The doping liquid 31 that utilizes primary heater 30 to heat is sent to water cooler 32.Water cooler 32 cooling doping liquid 31 are cooled to below the boiling point of the primary solvent that constitutes doping liquid 31.Primary solvent comprises at solvent 27 and is described composition under the situation of a composition.Comprise the composition that comprises for maximum in a plurality of compositions under the situation of a plurality of compositions at solvent 27.
The doping liquid 31 that is cooled is sent to first strainer 34 by pump 33.First strainer 34 filters doping liquid 31, removes the impurity in the doping liquid 31.Be provided with strainer changer (omitting diagram) at first strainer 34.The strainer changer will be adhered to a large amount of impurity, cause being difficult to carry out filtering filter body and be replaced by new filter body.Doping liquid 31 after the filtration is sent to the portion 17 that concentrates by pump 35.
In concentrated portion 17, utilize the doping liquid 31 after secondary heater 40 heating and filtering, the doping liquid 31 of heating is sent to flash distillation (flash) jars 41.In flash tank 41,, concentrate doping liquid 31 by the flash concentration method.The doping liquid 31 that is concentrated passes through pump 42 to reservoir 18 liquor chargings.The doping liquid 31 that the hold tank 43 of reservoir 18 is stored from flash tank 41 as required, utilizes pump 45, and the doping liquid 31 in the hold tank 43 is added mixed cell 12 liquor chargings to additive liquid.The reservoir 18 and the additive liquid that utilize pipe arrangement 84 to connect doping liquid preparation unit 11 add mixed cell 12, utilize this pipe arrangement 84 to carry doping liquid 31.Also have, concentrated portion can be provided with as required, omits also can.
Additive liquid adds mixed cell 12 to be possessed: first～the 4th additive liquid supply unit 47～50; Continuous mixing device 51; Second strainer 53; Controller 58.First～the 4th additive liquid supply unit 47～50 is supplied with additive to doping liquid 31.Continuous mixing device 51 is supplied with the mixing of doping liquid 31 of additive.Second strainer 53 is removed foreign matter from doping liquid 31.
The first additive liquid supply unit 47 possesses: softening agent supply unit 74; Solvent supply unit 75; Mixing tank 76; Additive flow container 77.Softening agent supply unit 74 possesses the softening agent jar (not having diagram) of storing softening agent.Solvent supply unit 75 possesses: the solvent tank (omitting diagram) of having stored solvent 27.Each jar is equipped with gauger at these.To drop into mixing tank 76 respectively by softening agent and the solvent 27 about the specified amount of accessory gauger (omitting diagram) metering.
Mixing tank 76 mixes softening agent and the solvent of supplying with from each supply unit 74,75, blending additive liquid 78a.Also has the scope that the preferred 10 weight % of the concentration of the softening agent among the additive liquid 78a are above and 60 weight % are following.The additive liquid 78a interim storage of blending is in the additive flow container 77 that can mix.Thus, can make the additive liquid 78a in the mixing tank 76 become empty, therefore, in mixing tank 76, can concoct new additive liquid 78a.Additive liquid 78a in the additive flow container 77 supplies with to adding nozzle 62a by pump 64.The rotating speed of pump 64 is controlled by controller 58.According to the rotating speed of pump 64, regulate addition to the additive liquid 78a of doping liquid 31.
The pipe arrangement 65 of interpolation nozzle 62a (with reference to Fig. 2) in connecting the additive flow container 77 and first static mixer 80 is provided with vacuum breaker (check valve) 61.Vacuum breaker 61 prevents to be sent to the additive liquid 78a that adds nozzle 62a and flows backwards.Also have, the supply of the additive liquid 78a that adds nozzle 62a is preferably carried out after the beginning of the rotation of the rotor in dynamic mixer described later 91～94 (with reference to Fig. 3).
Other second～the 4th additive liquid supply units 48～50 also constitute in the same manner with the first additive liquid supply unit 47.Omit the detailed explanation of second～the 4th additive liquid supply unit 48～50.The second additive liquid supply unit 48 is supplied with the additive liquid 78b that has mixed roughening agent and solvent 27 from adding nozzle 62b.In addition, the 3rd additive liquid supply unit 49 is supplied with the additive liquid 78c that has mixed UV agent and solvent 27 from adding nozzle 62c.In addition, the 4th additive liquid supply unit 50 is supplied with from adding nozzle 62d having mixed the additive liquid 78d that delays control agent and solvent 27.Also have, in the present embodiment, be provided with four additive liquid supply units 47～50, but as required, increase and decrease additive liquid supply unit also can.
As shown in Figure 2, continuous mixing device 51 begins to possess successively first static mixer 80, dynamic mixer 81, second static mixer 82 from the upstream side with respect to the liquor charging direction of doping liquid 31.Doping liquid 31 and additive liquid 78a～78d that first static mixer 80 mixes from reservoir 18.To come rotating rotor 91～94 (with reference to Fig. 3) to send into dynamic mixer 81 by utilizing motivating force at first static mixer, 80 blended doping liquid 31.To pass through the doping liquid 31 of dynamic mixer 81 and send into second static mixer 82.Each mixing tank 80～82 utilizes pipe arrangement 84 to connect.Be formed with doping liquid stream 80a～82a that doping liquid 31 flows through at each mixing tank 80～82.Be provided with interpolation nozzle 62a～62d of ejection additive liquid 78a～78d at the doping liquid stream 80a of first static mixer 80.
A plurality of elements (omitting diagram) that first static mixer 80 possesses pipe 83 and rectangular plate distortion 180 degree are formed.Pipe 83 is connected with pipe arrangement 84.Each element is contained in the inside of pipe 83.A plurality of elements are in series configuration in doping liquid stream 80a, additive liquid 78a～78d is disperseed, mixed additive liquid 78a～78d and doping liquid 31 in doping liquid 31.Under the time point that comes out from this first static mixer 80, additive liquid 78a～78d is dissolved in doping liquid 31 by halves.The doping liquid 31 that has passed through first static mixer 80 is sent to dynamic mixer 81.
The details of dynamic mixer 81 is described in detail in detail in the back.Dynamic mixer 81 comes rotating rotor 91～94 (with reference to Fig. 3 and Fig. 4) by the motivating force of utilizing motor 102, mixes doping liquid 31.In this dynamic mixer 81, additive liquid 78a～78d roughly fully is dissolved in doping liquid 31.The doping liquid 31 that has passed through dynamic mixer 81 is sent to second static mixer 82.Second static mixer 82 has the structure identical with first static mixer 80.In second static mixer 82, utilize a plurality of elements (omit illustrate) identical with first static mixer 80,78a～78d fully is dissolved in the doping liquid 31 with additive liquid.Passed through the doping liquid 31 of second dynamic mixer 81 and removed foreign matter, become the stream of should stream moulding and mould doping liquid 54 by second strainer 53 (with reference to Fig. 1).This stream is moulded the stream mold 147 (with reference to Fig. 5) that doping liquid 54 is sent to system film unit 13.Also have, under the time point that has passed through dynamic mixer 81, additive liquid 78a～78d also fully is dissolved in the doping liquid 31 sometimes.In this case, obtain stream at dynamic mixer 81 and mould doping liquid 54, therefore, do not dispose second static mixer 82 and also can.
As shown in Figure 3, dynamic mixer 81 possesses: box 90; Rotor 91～94; Turning axle 95; Stator 96～99; Motor 102; Electro-magnet portion 103.Be provided with doping liquid stream 81a, supply-pipe 106, vent pipe 107 and axle supported chamber 108 at box 90.Supply-pipe 106 will guide to doping liquid stream 81a from the doping liquid 31 of first static mixer 80.Vent pipe 107 from doping liquid stream 81a to exterior guiding doping liquid 31.108 supporting rotating shafts 95 of axle supported chamber.Be formed with an inserting hole 110a at the partition wall 110 of dividing doping liquid stream 81a and axle supported chamber 108.In axle inserting hole 110a, insert logical turning axle 95.In addition, utilize between machinery sealing agent 112 sealing turning axles 95 and the partition wall 110.Thus, prevent to mix liquid 31 types to the 108 sides leakage of axle supported chamber.Also have, in the present embodiment, dynamic mixer 81 is set for horizontal, but is not limited thereto, the liquor charging direction of doping liquid vertically also can for being set to from top to bottom.Towards the side is the long side direction and the roughly consistent situation of horizontal direction that makes dynamic mixer 81.
As shown in Figures 3 and 4, four rotors 91～94 are installed on turning axle 95 with certain spacing on the axial X of turning axle 95.The inlet side of doping liquid 31 forms big relatively footpath in the rotor 91, and outlet side forms relative path.Rotor 91～94 is installed in series with a determining deviation at its long side direction of turning axle 95 upper edges.On the side face of each rotor 91～94, on week, four agitating vanes 116 are installed with 90 ° of intervals.Each agitating vane 116 at one end to being half-twist ground, center distortion with turning axle 95 between the other end, is installed with spirrillum on the side face of rotor 91～94.Also have, the quantity of rotor does not need to be limited to 4, can be for more than 2～3 or 5.In addition, the quantity of agitating vane does not need to be limited to 4.
Four stators 96～99 are arranged in the doping liquid stream 81a along the liquor charging direction of doping liquid 31.Be formed with the supplying opening 120 that the doping liquid 31 from supply-pipe 106 enters in a side's of stator 96 side.Be formed with ejiction opening 121 that doping liquid 31 comes out and the axis hole 122 of inserting logical turning axle 95 in the opposing party's of stator 96 side.In addition, in stator 96, between supplying opening 120 and ejiction opening 121, be formed with the hollow bulb 124 of accommodating rotor 91.In addition, the inner peripheral surface 127 of stator 96 forms the conical surface that axial X tilts.
Motor 102 makes rotor 91～94 rotations by giving motivating force to turning axle 95.The doping liquid 31 that has entered in the doping liquid stream 81a at first is stirred by the rotation of agitating vane 116.Thus, additive liquid 78a～78d is mixed in doping liquid 31.Also have, doping liquid 31 from the ejiction opening 121 of stator 96 come out the back equally the rotation of the agitating vane by rotor 92～94 be stirred doping liquid 31, additive liquid 78a～78d is mixed in doping liquid 31.Like this, enter supply-pipe 106 at doping liquid 31, till coming out from vent pipe 107, utilize four agitating vanes to stir doping liquid, additive liquid 78a～78d roughly fully is dissolved in doping liquid 31 thus.
Use dynamic mixer 81 as described above, even be full-bodied doping liquid 31 more than the 30Pas to viscosity, also mixed additive liquid 78a～78d fully, dissolving fully or be scattered in doping liquid 31 equably.
In addition, utilize dynamic mixer 81, the viscosity ratio (%) { 100 * (viscosity of additive)/(viscosity of doping liquid) } of the viscosity of the viscosity of additive liquid 78a～78d and doping liquid 31 preferably is made as below 10%, and then can improves Combination the additive liquid 78a～78d of doping liquid 31.With respect to this, if viscosity ratio less than 10%, then can not be mixed in doping liquid 31 with additive liquid 78a～78d fully.Also have, described in the present embodiment " Combination " is meant additive liquid 78a～78d with which kind of degree is mixed in the doping liquid 31.In addition, viscosity ratio is made as 0% or also can near 0% value.
In addition, the outer roll surface speed of dynamic mixer 81 preferably is made as 0.1m/ second above and 1.0m/ below second, not only aforesaid full-bodied doping liquid 31 is also had sufficient Combination thus, and can not lose the mixing of stably carrying out additive liquid 78a～78d under the situation of performance of dynamic mixer 81.Roll surface speed is under above situation 0.1m/ second outside, compares with the situation less than 0.1m/ second, additive liquid 78a～78d can be mixed in doping liquid 31 more fully.
On the other hand, roll surface speed is under following situation 1.0m/ second outside, compares with the situation that surpasses 1.0m/ second, and the generation of the frictional heat in suppressing between agitating vane 116 and the doping liquid 31 suppresses the foaming that the heating of doping liquid 31 causes.Thus, suppress the reduction of the performance of dynamic mixer 81, can more stably carry out the mixing of additive liquid 78a～78d.And, roll surface speed is under the situation of 1.0m/ below second outside, compare with the situation that surpasses 1.0m/ second, the generation of the frictional heat in also suppressing between agitating vane 116 and the machinery sealing agent 112, therefore, suppress the reduction of the weather resistance of machinery sealing agent 112, the situation that the liquid 31 that prevents from more reliably to mix spills to axle supported chamber 108.
In addition, the static pressure in the doping liquid stream 81a preferably is made as the driving that 0.1MPa controls rotor 91～94 abovely, can more stably carry out the mixing of additive liquid 78a～78d thus under the situation of the performance of not losing dynamic mixer 81.Under static pressure is situation more than the 0.1MPa, compare with situation less than 0.1MPa, suppress the foaming of the doping liquid 31 that the heating based on the frictional heat that causes with contacting of agitating vane 116 causes more reliably, therefore, suppress the performance of dynamic mixer 81, can more stably carry out the mixing of additive liquid 78a～78d.
In addition, by the clearance C L between the agitating vane 116 of the inner peripheral surface 127 of stator and rotor preferably is made as more than the 0.3mm and below the 1.5mm, doping liquid 31 does not have resistance ground to flow to ejiction opening 121 from supplying opening 120, and, above-mentioned full-bodied doping liquid 31 is also had sufficient Combination.If clearance C L is more than the 0.3mm, then to compare with situation less than 0.3mm, resistance is little, and therefore, flowing of doping liquid 31 further improves, and therefore, Combination is higher.In addition, under clearance C L is situation below the 1.5mm, compare with the situation that surpasses 1.5mm, big based on the shear strength of agitating vane 116, therefore, the Combination height.Also have, clearance C L shown in Figure 3 is illustrated in and is positioned near the agitating vane 116 of central part and the distance of inner peripheral surface 127 on the axial X.But this only only is an example.Clearance C L can be the agitating vane 116 that is positioned at leading section and distance of inner peripheral surface 127 etc.
In addition, by the time of doping liquid 31 in each stator and rotor delay preferably was made as more than 0.1 second, above-mentioned full-bodied doping liquid 31 also had sufficient Combination.Under the time of being detained is situation more than 0.1 second, and compare less than 0.1 second situation, additive liquid 78a～78d can be mixed in doping liquid 31 fully.Also have, the residence time is that doping liquid 31 enters the time of each rotor till come out.Be under the situation of stator 96, the residence time is meant that doping liquid 31 enters the time of supplying opening 120 till come out from ejiction opening 121.
Electro-magnet portion 103 is to be installed on a supported chamber 108 with the magnet portion 130 opposed modes that are installed on turning axle 95.By the power that attracts each other between electro-magnet portion 103 and magnet portion 130 or push mutually, turning axle 95 can be supported in electro-magnet portion 103 rotatably.
As shown in Figure 5, system film unit 13 possesses stream and moulds chamber 140, transition part 141, tenter machine 142, kiln 143, up-coiler 144, uses stream to mould doping liquid 54 and makes film 146.Moulding chamber 140 at stream disposes stream mold 147, stream and moulds drum 148, peels off cylinder 149.Be formed with the ejiction opening that stream is moulded doping liquid 54 in stream mold 147.Stream is moulded drum 148 and is played a role as supporter.
Stream is moulded doping liquid 54 and is moulded on the drum 148 via stream mold 147 streams at the stream of rotation continuously and mould.Thus, mould formation stream plastic film 151 on the drum 148 at stream.The surface temperature that stream is moulded drum 148 preferably more than-10 ℃ in the scope below 10 ℃ constant.If mould at such stream and on the drum 148 stream to be moulded doping liquid 54 streams and mould, then stream is moulded doping liquid 54 and is cooled off rapidly.Therefore, form cohesion shape stream plastic film 151 at short notice.When stream plastic film 151 had self-supporting, stream plastic film 151 supported by peeling off cylinder 149, simultaneously, peels off as wetting film.
In transition part 141, carry when utilizing a plurality of cylinders to support wetting film 153, carry out drying betwixt.In tenter machine 142, when being kept by maintaining bodies such as pins, the both side ends of wetting film 153 carries, carry out drying betwixt.In addition, in tenter machine 142, on the expansion of the width of wetting film 153 or the direction of shrinking, maintaining body is moved, wetting film 153 is extended on width or relax.The wetting film 153 that comes out from tenter machine 142 is dried air-dry dry kiln 143.Thus, obtain film 146 as goods.Film 146 utilizes up-coiler 144 to be wound in core 155 with the roller shape.
Stream mould chamber, stream mold, stream mould the structure of drum etc., altogether stream mould, peel off method, stretching, each operation drying conditions, facture, batch, the method for winding of planarity after correcting at length be recorded in [0617] paragraph that the spy opens the 2005-104148 communique to method for recovering solvents, film recovery method and arrive in [0889] paragraph, these records also go among the present invention.Also have, in the above-described embodiment, be made as to mould and make stream plastic film 151 cooling gels on the drum 148, make it have the cooling gel mode of self-supporting at stream, but mould dry stream plastic film on the drum 148 at band (not shown) or stream, make its drying mode also can implement the present invention equally with self-supporting.
The transparency height of the film 146 that obtains by the present invention shows the value that delays of expectation, and temperature dependency is low.Therefore, especially, can be suitably use, can also utilize as the protective film on the surface that is used to protect polarization plates as the phase-contrast film of polarization plates.About cellulose ester of the present invention is the concrete purposes of film, open in the 2005-104148 communique the spy, for example, arrive in [1265] paragraph at [1088] paragraph, at length put down in writing TN type, STN type, VA type, OCB type, reflection-type, other examples as liquid crystal indicator, these records also go for the present invention.
In the above-described embodiment, use four interpolation nozzle 62a～62d that are provided with corresponding to four additive liquid supply units 47～50, various additive liquid 78a～78d are made an addition to doping liquid 31.Replace it, for example, add four additive liquid supply units 47～50 of connection on the nozzle, use an one nozzle, described various additive liquid 78a～78d are together added also can at one.
In the above-described embodiment, for doping liquid 31, add additive liquid 78a～78d in the front of stream mold 147, but doping liquid 31 maybe stored doping liquid 31 before flash tank concentrates in hold tank 43 before, additive liquid 78a～78d is made an addition to doping liquid 31 also can.
In the above-described embodiment, after doping liquid 31 has added additive liquid 78a～78d, first static mixer 80 that use sets gradually on the liquor charging direction of doping liquid 31, dynamic mixer 81, second static mixer 82, additive liquid 78a～78d is mixed in the doping liquid 31, thus additive liquid 78a～78d fully is dissolved in the doping liquid 31, but does not need to be limited to this.For example, in the low situation of the viscosity ratio of doping liquid 31 and additive liquid 78a～78d etc. down, only the mixing of carrying out additive liquid with dynamic mixer 81 also can.In this case, utilize dynamic mixer 81 that additive liquid 78a～78d fully is dissolved in doping liquid 31, utilize dynamic mixer 81 to obtain stream and mould doping liquid 54.
In the above-described embodiment, individual layer stream moulded as an example be illustrated, but in addition, also can be for except basic unit, simultaneously or one by one stream is moulded outer field stream altogether and is moulded and also can on the two sides of this basic unit.Preferably in this case, also with above-mentioned embodiment in the same manner, at first, polymkeric substance 26 is dissolved in solvent 27, preparation doping liquid 31 then, for the doping liquid 31 corresponding with each layer, adds additive respectively and also can.
Below, by embodiment, the present invention is described more specifically.
[embodiment 1]
As shown in Figure 2, on the liquor charging direction of doping liquid 31, begin to be disposed with first static mixer 80, dynamic mixer 81, reach second static mixer 82 from upstream side.Be respectively arranged with doping liquid stream 80a～82a at each mixing tank 80～82.Be provided with the additive liquid 78a, the additive liquid 78b that comprises the roughening agent that are used for to comprise softening agent, comprise the additive liquid 78c of UV agent and comprise interpolation nozzle 62a～62d that the additive liquid 78d that delays control agent makes an addition to doping liquid 31 at the doping liquid stream 80a of first static mixer 80.In first static mixer 80, the element by using 24 rectangular plate distortion 180 degree are formed has mixed doping liquid 31 and additive liquid 78a～78d.
At this, the plasticizer concentration among the additive liquid 78a is made as 60 weight %.The viscosity of doping liquid 31 is made as 30Pas.The viscosity of additive liquid 78a is made as 3Pas.Thereby, the viscosity ratio of the viscosity of additive liquid 78a and doping liquid 31 is made as 10%.In addition, the interpolation ratio with the addition of the addition of additive liquid 78a and doping liquid 31 is made as 5%.
As shown in Figure 3, the stator 96～99 that is provided with four rotors 91～94 and is used for those rotors 91～94 can be accommodated rotatably along the liquor charging side of doping liquid 31 at the doping liquid stream 81a of dynamic mixer 81.On the rotor subject 115 of each rotor, upwards four agitating vanes 116 are installed with 90 ° of spacings (pitch) in week.Give motivating force from motor 102 to turning axle 95, make agitating vane 116 rotations.By the rotation of agitating vane 116, doping liquid 31 and additive liquid 78a～78d have been mixed.
At this, the outer roll surface speed of dynamic mixer 81 is made as 1.0m/ second.Static pressure in the doping liquid stream 81a is made as 0.4MPa.Clearance C L between the inner peripheral surface 127 of stator 96～99 and the agitating vane 116 of rotor 91～94 is made as 0.3mm.The time (hereinafter referred to as " residence time ") of doping liquid 31 in each rotor and stator delay was made as 0.1 second.
[embodiment 2]
The quantity of rotor and stator is made as 3 respectively, only carries out the mixing of additive liquid 78a～78d with dynamic mixer 81, in addition, identical with embodiment 1.
[embodiment 3]
The quantity of rotor and stator is made as 2 respectively, and L is made as 1.5mm with clearance C, only carries out the mixing of additive liquid 78a～78d with dynamic mixer 81, and is in addition, identical with embodiment 1.
[embodiment 4]
The quantity of rotor and stator is made as 2 respectively, the outer roll surface speed of dynamic mixer 81 is made as 0.1m/ second, only carry out the mixing of additive liquid 78a～78d with dynamic mixer 81, in addition, identical with embodiment 1.
[embodiment 5]
The quantity of rotor and stator is made as 2 respectively, the step-down in the doping liquid stream 81a is made as 0.1MPa, only carry out the mixing of additive liquid 78a～78d with dynamic mixer 81, in addition, identical with embodiment 1.
[embodiment 6]
The quantity of rotor and stator is made as 2 respectively, the static pressure in the doping liquid stream 81a is made as 0.09MPa, only carry out the mixing of additive liquid 78a～78d with dynamic mixer 81, in addition, identical with embodiment 1.
[embodiment 7]
The quantity of rotor and stator is made as 2 respectively, and L is made as 0.29mm with clearance C, only carries out the mixing of additive liquid 78a～78d with dynamic mixer 81, and is in addition, identical with embodiment 1.
[embodiment 8]
The quantity of rotor and stator is made as 2 respectively, and L is made as 1.51mm with clearance C, only carries out the mixing of additive liquid 78a～78d with dynamic mixer 81, and is in addition, identical with embodiment 1.
[embodiment 9]
The quantity of rotor and stator is made as 2 respectively, the rotating speed of agitating vane 116 is made as 1.1m/ second, only carry out the mixing of additive liquid 78a～78d with dynamic mixer 81, in addition, identical with embodiment 1.
[embodiment 10]
The quantity of rotor and stator is made as 2 respectively, the rotating speed of agitating vane 116 is made as 0.09m/ second, only carry out the mixing of additive liquid 78a～78d with dynamic mixer 81, in addition, identical with embodiment 1.
[embodiment 11]
The quantity of rotor and stator is made as 2 respectively, will be made as the residence time 0.09 second, only carry out the mixing of additive liquid 78a～78d with dynamic mixer 81, in addition, identical with embodiment 1.
[embodiment 12]
The quantity of rotor and stator is made as 1 respectively, only carries out the mixing of additive liquid 78a～78d with dynamic mixer 81, in addition, identical with embodiment 1.
[comparative example 1]
The quantity of rotor and stator is made as 2 respectively, only uses dynamic mixer (Nuo Litake corporate system 6-N16-22 (6)-1) to carry out the mixing of additive liquid 78a～78d, in addition, identical with embodiment 1.
[result]
The results are shown in the table 1 of embodiment 1～12, comparative example 1.
[table 1]
In [mixing tank pattern] hurdle of table 1, " static/dynamic/static state " expression begins to set gradually the situation of static mixer, dynamic mixer, static mixer from upstream side." dynamically " is meant the situation of having used dynamic mixer." static state " is meant the situation of having used static mixer.
In addition, in value column, " ◎ " expression doping liquid and additive liquid is the blended situation equably." zero " expression doping liquid and additive liquid mix, but have only few part to become uneven situation.There are not the situation of blended part mutually in " △ " expression doping liquid and additive liquid.The not mutual blended situation of " * " expression doping liquid and additive liquid major part.The performance of " performance is bad " expression mixing tank reduces the situation that the mixing of doping liquid and additive liquid can not be carried out.The fault of " production stops " expression mixing tank recurs situation about can not produce.
In embodiment 1～5, the Combination height to the additive liquid of doping liquid in addition, does not have the ground such as fault of mixing tank to stablize the mixing of carrying out additive liquid.In addition, in embodiment 1 and 2,, can further improve Combination by increasing the quantity of rotor.
With respect to this, in embodiment 6, to compare with each embodiment, static pressure is low, therefore, foams easily, and this foaming becomes reason, causes the performance of mixing tank to reduce.In addition, 7 kinds of embodiment, compare with each embodiment, clearance C L is too small, and therefore, Combination reduces, and in embodiment 8, compares with each embodiment, and clearance C L is excessive, and therefore, Combination is extremely low.In addition, in embodiment 9, compare with each embodiment, the periphery excessive velocities, therefore, the fault of mixing tank recurs, and can not produce.In addition, in embodiment 10, compare with each embodiment, outer roll surface speed is slow excessively, and therefore, Combination reduces.In addition, in embodiment 11, compare with each embodiment, the residence time of doping liquid is too short, and therefore, Combination is extremely low.In addition, in embodiment 12, only carry out the mixing of additive with a rotor, therefore, Combination reduces.In addition, in comparative example 1, only mix with static mixer, therefore, Combination is extremely poor.
Claims (10)
1. a solution film-forming method comprises the steps, that is:
Preparation contains the step of the doping liquid of polymkeric substance and solvent;
The step of feeding additive liquid in the pipe arrangement of described doping liquid liquor charging;
Mix described doping liquid and described additive liquid and form the operation that stream is moulded doping liquid, wherein, described mixing utilizes dynamic mixer to carry out, and described dynamic mixer has the stator and the rotor of multistage on the liquor charging direction of described doping liquid; And
Use described stream to mould the step that doping liquid is made film.
2. solution film-forming method according to claim 1, wherein,
The viscosity that is transferred the described doping liquid of described additive liquid is more than the 30Pas.
3. solution film-forming method according to claim 2, wherein,
The viscosity ratio % of described additive liquid and described doping liquid is below 10%, and described viscosity ratio is to obtain by { 100 * (viscosity of described additive liquid)/(viscosity of described doping liquid) }.
4. solution film-forming method according to claim 1, wherein,
The outer roll surface speed of described dynamic mixer is the 0.1m/ second of above and 1.0m/ below second.
5. solution film-forming method according to claim 4, wherein,
Static pressure in making in the described dynamic mixer becomes the driving that 0.1MPa controls described rotor abovely.
6. solution film-forming method according to claim 1, wherein,
Described stator is accommodated described rotor in the mode that can rotate, and is formed with the gap that 0.3mm is above and 1.5mm is following between described stator and the described rotor.
7. solution film-forming method according to claim 1, wherein,
Described doping liquid is more than 0.1 second in the time of described each stator and rotor delay.
8. solution film-forming method according to claim 1, wherein,
Described mixing is except described dynamic mixer, also utilizes the static mixer that is provided with in the upstream of described dynamic mixer to carry out.
9. solution film-forming method according to claim 8, wherein,
The mutual different first described additive liquid and the second described additive liquid is mixed in described doping liquid,
Described static mixer possesses:
Described pipe arrangement,
First nozzle that the first additive liquid is supplied with in described pipe arrangement; And
Second nozzle that the second described additive liquid is supplied with in described pipe arrangement;
Described second nozzle arrangement is in the downstream of first nozzle.
10. solution film-forming method according to claim 1, wherein,
Described mixing is except described dynamic mixer, also utilizes the static mixer that is provided with in the downstream of described dynamic mixer to carry out.
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| CN102160971A (en) * | 2011-03-15 | 2011-08-24 | 中国纺织科学研究院 | Dynamic mixer |
| CN103585908A (en) * | 2013-11-20 | 2014-02-19 | 哈尔滨工程大学 | Multistage guide vane static mixer |
| CN104645844A (en) * | 2011-03-15 | 2015-05-27 | 中国纺织科学研究院 | Dynamic mixer |
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| JP5518652B2 (en) * | 2010-09-15 | 2014-06-11 | 富士フイルム株式会社 | Mixing apparatus, casting dope manufacturing method and solution casting method |
| JP2013006347A (en) * | 2011-06-24 | 2013-01-10 | Fujifilm Corp | Mixing device, method of manufacturing casting dope and solution film forming method |
| JP6615756B2 (en) * | 2014-07-28 | 2019-12-04 | 住友化学株式会社 | Film production method and coating solution storage method |
| JP6053045B2 (en) * | 2014-09-19 | 2016-12-27 | 富士フイルム株式会社 | Solution casting method |
| CN114701099B (en) * | 2022-04-07 | 2023-08-08 | 华南理工大学 | Modularized high polymer material double-rotor pump type conveying equipment and conveying method |
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| JP2010234693A (en) | 2010-10-21 |
| CN101851342B (en) | 2013-11-06 |
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