CN103950136A - Cellulose triacetate film preparation method - Google Patents
Cellulose triacetate film preparation method Download PDFInfo
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- CN103950136A CN103950136A CN201410117613.3A CN201410117613A CN103950136A CN 103950136 A CN103950136 A CN 103950136A CN 201410117613 A CN201410117613 A CN 201410117613A CN 103950136 A CN103950136 A CN 103950136A
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- liquid
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- dividing plate
- curtain coating
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Abstract
The invention relates to a cellulose triacetate film preparation method, which comprises casting, drying and winding, and is characterized in that a liquid seal device is arranged in a transition section between a casting section and a post-drying section, and comprises a liquid storage tank, a folding type separation plate and a liquid seal liquid, one end of the folding type separation plate is fixed on the sheet gap of the casting section, and the other end of the folding type separation plate extends into the liquid seal liquid. According to the present invention, diffusion of the high concentration solvent gas in the casting section toward the transition section and the post-drying chamber is effectively blocked, the optical isotropic property, the transmittance and the apparent quality of the prepared film are significantly improved, the solvent recovery rate is significantly increased, the production cost is reduced, and the environmental pollution is reduced.
Description
Technical field
The invention belongs to field of optical films, particularly a kind of preparation method of cellulose triacetate thin film.
Background technology
Triafol T is the cellulose acetate that average acetify degree is 57.5%～62.5%; its cellulose triacetate thin film of making (TAC film) has excellent optical isotropy, is suitable as polaroid inner protection film or the types of functionality rete such as chromatic color filter, anti-dazzling film, antireflection film, phase retardation film for liquid crystal display.
TAC film generally adopts solution casting method preparation, being about to cellulose triacetate, plasticizer, each analog assistant etc. is dissolved in solvent, form high thickness cotton glue, then high viscosity cotton glue curtain coating for no reason on support, is formed to film through series of processes such as super-dry, rollings at band shape or cydariform.Compare as melting the tape casting, melt extrusion method with other method, the optical isotropy of the film that solution casting method obtains is fabulous, and has splendid optical characteristics and physical and chemical performance, is particularly useful for the application that optics shows.
As shown in Figure 1, in the preparation process of film, the celloidin solution of high viscosity, forms the liquid film of thickness homogeneous by dispense tip curtain coating on support for no reason to band shape or drum type.At the initial drying stage of liquid film, due to the evaporation of volatile solvent, liquid film trend is shunk, and causes thus film to form plane positioning structure and produces internal stress.Result of study shows, the TAC film of 50 microns, and when the curtain coating stage is dried carry out very fast, its internal stress is 450kg/cm
2, and dry 350 kg/cm that are about when slower
2, after tested, the film that internal stress is little obtains good optics with tropism and light transmittance.In recent years, for meeting liquid crystal display slimming, large-sized market demand, around optical properties such as " TAC Film Optics homogeneity, light transmittances ", improve, film production process has been done to further improvement, in the initial dry curtain coating stage of liquid film, rely on and improve solvent strength inhibition liquid film drying speed in drying medium, make it to be more tending towards mitigation, balance.In process after improvement, the solvent strength numerical value in medium can be controlled in security interval rolls off the production line, also can be controlled at solvent safety interval reach the standard grade above, the preferred solvent security interval 850 above～1000g/m that reaches the standard grade
3.Yet also produce thus new technical problem, the solvent gas of higher concentration in curtain coating section, the sheet seam 13 by curtain coating section 4 spreads to low concentration regions such as the changeover portion 5 in downstream and rear dryer section 6, and product is caused to following adverse effect:
1. the interior high concentration solvent gas diffusion of curtain coating section 4, makes to maintain compared with high solvent concentration and become difficult in curtain coating section, is unfavorable for the stable of technology controlling and process, and Film Optics performance improvement is not obvious.
2. in the dry section 6 of the follow-up low concentration of film, because the diffusion of high concentration solvent gas causes the accumulation of solvent to make solvent strength increase, reduced follow-up dry drying efficiency, film solvent remaining quantity is not up to standard.
3. high concentration solvent gas spreads to low concentration region, is unfavorable for the recovery of area with high mercury solvent, and solvent consumption is higher, environment is had a negative impact.
For addressing this problem, prior art is to stop sovent diffusion by adjusting the gap size of the equipment sheet seam 13 of film outlet, import, is secondly that the blast that makes sheet stitch 13 places by adjusting process parameter reaches balance, stops sovent diffusion.Although these measures have certain effect, but can not thoroughly solve the diffusion problem of high concentration solvent gas, cause casting technique to control unstable, film performance and improve and be restricted.
Summary of the invention
The present invention is directed to the above-mentioned technical problem that prior art exists, a kind of preparation method of cellulose triacetate thin film is provided.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
A preparation method for cellulose triacetate thin film, comprises curtain coating, dry, wrapup procedure, after improvement, in the changeover portion between curtain coating Duan Yuhou dryer section, liquid seal device is set; Described liquid seal device comprises: liquid storage groove, fold-type dividing plate and fluid-tight liquid, and one end of fold-type dividing plate is fixed on the sheet seam of curtain coating section, and the other end of fold-type dividing plate is invaded fluid-tight liquid internal.
In above-mentioned preparation method, the distance H 1 of one end of fold-type dividing plate and sheet seam is 10cm～25cm, and the depth H 2 that the other end of fold-type dividing plate is immersed in storage tank liquid internal is not less than 5cm.
In above-mentioned preparation method, the bottom lengths A of liquid storage groove is less than or equal to the length L of changeover portion.
In above-mentioned preparation method, at fold-type dividing plate, be provided with manhole cover with one end that sheet seam is connected, aperture should be not less than 30cm.
In above-mentioned preparation method, in changeover portion, be provided with by two or more deflector rolls, formed cut water device.
In above-mentioned preparation method, described fluid-tight liquid can be water, butanols or high boiling solvent, preferred water.
Compared with prior art, tool of the present invention has the following advantages:
By liquid seal device is set, can effectively intercept high concentration solvent gas in curtain coating section to the diffusion of changeover portion and rear hothouse, solvent strength in curtain coating section is maintained in the number range of setting, realize the stable control of curtain coating segment process, the solvent strength rising of effectively avoiding film to cause due to solvent accumulation in rear dryer section 6, improved the drying efficiency of follow-up dry run, can make film solvent remaining quantity strictly be controlled; Can effectively control rate of drying, make that rate of drying is tending towards relaxing more, balance, obtain that internal stress is less, the same tropism of optics, light transmittance and apparent mass obtain the comprehensive film product improving; Meanwhile, reduce the consumption of solvent in preparation process, be beneficial to the recovery of area with high mercury solvent, reduced production cost, reduced the pollution to environment.
Accompanying drawing explanation
Fig. 1 is existing film preparation process schematic diagram;
Fig. 2 is film preparation process schematic diagram of the present invention;
Fig. 3 is liquid seal device side view of the present invention;
Fig. 4 is that the present invention cuts water device schematic diagram.
In figure, a label is: 1 extrusion nozzle; 2 stainless steel bands; 3 liquid films; 4 curtain coating sections; 5 changeover portions; 6 rear dryer section; 7 liquid seal devices; 8 liquid storage grooves; 9 fold-type dividing plates; 10 fluid-tight liquid; 11 cut water device; 12 manhole covers; 13 seams; L changeover portion 5 length; H1 fold-type dividing plate 9 and sheet stitch the distance between 13 tie points and sheet seam; H2 fold-type dividing plate 9 immerses the interior degree of depth of liquid 10; The bottom lengths of A liquid seal device.
The specific embodiment
In the present invention, film forming matter preferably has good optically isotropic material.In the present invention, the material of film is cellulose esters, preferably uses acylated cellulose, is more preferably cellulose acetate, is specially Triafol T, the cellulose triacetate that particularly acetyl degree is 57.5%～62.5%.
In the present invention, the preparation process of TAC film is as follows:
Celloidin solution (being cellulose triacetate solution) is by extrusion nozzle 1, and under certain pressure, uniform spreading is to the liquid film 3 that forms thickness homogeneous on the stainless steel band 2 of continuous operation; Liquid film 3 is interior through preliminarily dried in curtain coating section 4, is stripped from steel band when reaching 20%～40% water capacity, and by sheet, stitching 13, by curtain coating section 4, to enter changeover portion 5 and follow-up dryer section 6 dry successively.Film, through the follow-up dry remaining solvent of removing, obtains TAC film through trimming, balance, embossing, rolling.
Will keep under strict control in the film production process concentration of curtain coating section 4 internal solvents, general control is more high better, but too high, and drying efficiency reduces, and production efficiency declines, and is preferably controlled at 850 g/m
3～1200g/m
3; It is that drying medium continues to be dried that film enters rear dryer section 6 dependence air, and film solvent remaining quantity requires 8%, is to guarantee drying effect, and airborne solvent strength is controlled at 20 g/m
3below, be preferably in 10 g/m
3below.
Generally, high concentration solvent gas in curtain coating section 4 stitches 13 by sheet and spreads to changeover portion 5, rear dryer section 6, rear dryer section 6 concentration are raise, the adverse effect producing has: curtain coating section 4 process conditions are unstable, film improved combination properties is not obvious, film solvent is remaining higher, is unfavorable for the recycling of solvent simultaneously, causes solvent loss, contaminated environment.
For effectively the interior high concentration solvent gas of curtain coating section 4 being intercepted, the present invention takes the interior liquid seal device 7 that arranges of the changeover portion 5 between curtain coating section 4 and rear dryer section 6, and liquid seal device 7 comprises: liquid storage groove 8, fold-type dividing plate 9, fluid-tight liquid 10.One end of fold-type dividing plate 9 is positioned on the sheet seam 13 of curtain coating section 4, can connect with welding manner, and the distance H 1 between tie point and sheet seam 13 is preferably controlled 10～25cm again; The other end of fold-type dividing plate 9 immerses fluid-tight liquid 10 inside, immersion depth H2 is not less than 5cm, high concentration solvent gas in the effective obstruct of realization curtain coating section is to the diffusion of changeover portion and rear hothouse thus, realize stable control and the effective control to rear hothouse rate of drying of curtain coating segment process, make that rate of drying is tending towards relaxing more, balance, obtain that internal stress is less, the same tropism of optics, light transmittance and apparent mass obtain the comprehensive film product improving.Meanwhile, reduce the consumption of solvent in preparation process, be beneficial to the recovery of area with high mercury solvent, reduced production cost, reduced the pollution to environment.
For removing in time the fluid-tight liquid that film surface is carried secretly, the present invention changeover portion 5 in, liquid seal device 7 after be provided with by two or more deflector rolls, formed cut water device 11.
In the present invention, for handled easily, at fold-type dividing plate 9, be provided with manhole cover 12 with sheet seam 13 one end that are connected, aperture should be not less than 30cm.
In the present invention, fluid-tight liquid can be selected from water, butanols or certain high boiling solvent, preferred water.Anti-static effect for further enhanced film, can also add methyl alcohol, water-soluble antistatic agent, as polystyrolsulfon acid class, polythiophene class in fluid-tight liquid.
Liquid seal device material in the present invention can be used any metal material, can use stainless steel, copper or titanium, preferably stainless steel.
Below in conjunction with specific embodiment, the present invention is further illustrated, but be not limited to this.
Embodiment 1
The preferred triacetate fiber ester of the present invention is that primary raw material is prepared celloidin solution (that is: cellulose triacetate solution), celloidin solution (that is: cellulose triacetate solution) is by extrusion nozzle 1 after accurate measurement, and under certain pressure, uniform spreading is to the liquid film 3 that forms thickness homogeneous on the stainless steel band 2 of continuous operation; Liquid film 3, at the interior drying medium of curtain coating section 4 preliminarily dried, is stripped from steel band when reaching 20%～40% water capacity, and by sheet, stitching 13, by curtain coating section 4, to enter changeover portion 5 and follow-up dryer section 6 dry successively.Film, through the follow-up dry remaining solvent of removing, obtains TAC film through trimming, balance, embossing, rolling.
For effectively the interior high concentration solvent gas of curtain coating section 4 being intercepted, the present invention takes the interior liquid seal device 7 that arranges of the changeover portion 5 between curtain coating section 4 and rear dryer section 6, and liquid seal device 7 comprises: liquid storage groove 8, fold-type dividing plate 9 and fluid-tight liquid 10.The bottom lengths A of liquid storage groove 8 is less than or equal to the length L of changeover portion 5; One end of fold-type dividing plate 9 is positioned on the sheet seam 13 of curtain coating section 4, and one end of fold-type dividing plate 9 is connected with welding manner with curtain coating section 4 wallboards, and H1 is 10cm, and the other end of fold-type dividing plate 9 immerses liquid 10 inside, and immersion depth H2 is 5cm; Fluid-tight liquid 10 makes water.For removing in time the fluid-tight liquid that film surface is carried under one's arms, changeover portion 5 in, the setting below of liquid seal device 7 by two deflector rolls, formed cut water device 11.The aperture of wearing sheet device for opening manhole cover 12 is 30cm.Liquid seal device adopts stainless steel; In preparation process, curtain coating section 4 internal solvent concentration are set in 900 g/m
3.
Embodiment 2
Film production process is with embodiment 1.
For effectively the interior high concentration solvent gas of curtain coating section 4 being intercepted, the present invention takes the interior liquid seal device 7 that arranges of the changeover portion 5 between curtain coating section 4 and rear dryer section 6, and liquid seal device 7 comprises: liquid storage groove 8, fold-type dividing plate 9 and fluid-tight liquid 10.The bottom lengths A of liquid storage groove 8 is less than or equal to the length L of changeover portion 5; One end of fold-type dividing plate 9 is positioned on the sheet seam 13 of curtain coating section 4, and one end of fold-type dividing plate 9 is connected with welding manner with curtain coating section 4 wallboards, and H1 is 20cm, and the other end of fold-type dividing plate 9 immerses liquid 10 inside, and immersion depth H2 is 7cm; Fluid-tight liquid 10 is used methyl alcohol.For removing in time the fluid-tight liquid that film surface is carried under one's arms, the interior setting of changeover portion 5 is comprised of four deflector rolls cuts water device 11.The aperture of wearing sheet device for opening manhole cover 12 is 35cm.Liquid seal device adopts stainless steel; In preparation process, curtain coating section 4 internal solvent concentration are set in 1050 g/m
3.
Embodiment 3
Film production process is with embodiment 1.
For effectively the interior high concentration solvent gas of curtain coating section 4 being intercepted, the present invention takes the interior liquid seal device 7 that arranges of the changeover portion 5 between curtain coating section 4 and rear dryer section 6, and liquid seal device 7 comprises: liquid storage groove 8, fold-type dividing plate 9 and fluid-tight liquid 10.The bottom lengths A of liquid storage groove 8 is less than or equal to the length L of changeover portion 5; One end of fold-type dividing plate 9 is positioned on the sheet seam 13 of curtain coating section 4, and one end of fold-type dividing plate 9 is connected with welding manner with curtain coating section 4 wallboards, and H1 is 10cm, and the other end of fold-type dividing plate 9 immerses liquid 25 inside, and immersion depth H2 is 10cm; Fluid-tight liquid 10 is used kayexalate.For removing in time the fluid-tight liquid that film surface is carried under one's arms, the interior setting of changeover portion 5 is comprised of six deflector rolls cuts water device 11.The aperture of wearing sheet device for opening manhole cover 12 is 40cm.Liquid seal device adopts stainless steel; In preparation process, curtain coating section 4 internal solvent concentration are set in 1200 g/m
3.
Comparative example
Film production process is with embodiment 1.But liquid seal device is not set in changeover portion.
Table 1: performance data table
| Embodiment | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 |
| Solvent strength (the g/m of curtain coating section 4 3） | 900 | 1050 | 1200 | 1050 |
| Solvent strength (the g/m of rear dryer section 6 3） | 10-13 | 10-17 | 10-16 | ＞30 |
| Film solvent remaining quantity (%) | 6-8 | 6-9 | 7-9 | 15-20 |
| Solvent recovering rate (%) | 75 | 77 | 77 | 60 |
| Same tropism (the R of Film Optics 0） | 0.8 | 1.6 | 1.0 | 3.5 |
| Light transmission rate (%) | 92.37 | 92.7 | 92.58 | 90.2 |
| Film surface flaw quantity (individual/10 meter) | 6 | 5 | 5 | ＞15 |
In table, the method for testing of properties is as follows:
1. solvent strength test:
Use the online concentration detector that model is Cw-2000 ZX to test.
2. solvent remaining quantity test:
Method according to standard: HG/T3558 (film, sheet base water capacity assay method) regulation is tested.
3. Film Optics is with tropism R
0test:
Use the test of delay degree tester.
4. the test of light transmission rate:
Adopt WGT-S light transmittance/mist degree tester to test.
5. the test of solvent recovering rate:
By the quantity of solvent to use, the condensation number of recovery calculates and get final product.
6. the test of film surface flaw quantity:
Range estimation statistics.Under range estimation or microscope, viewing film is apparent; Get certain area film sample, be positioned over measuring platform, by reflection ray, detect the some quantum count on face surface.
In table, data can be found out, adopt the inventive method, can effectively intercept high concentration solvent gas in curtain coating section to the diffusion of changeover portion and rear hothouse, preparation the same tropism of Film Optics, light transmittance and apparent mass be improved significantly, simultaneously, the rate of recovery of solvent obviously improves, and has reduced production cost, has reduced the pollution to environment.
Claims (7)
1. the preparation method of a cellulose triacetate thin film, comprise curtain coating, dry, wrapup procedure, it is characterized in that, in changeover portion (5) between curtain coating section (4) and rear dryer section (6), liquid seal device (7) is set, liquid seal device comprises: liquid storage groove (8), fold-type dividing plate (9) and fluid-tight liquid (10), one end of fold-type dividing plate (9) is fixed on the sheet seam (13) of curtain coating section (4), and the other end of fold-type dividing plate (9) is invaded fluid-tight liquid (10) inside.
2. preparation method according to claim 1, is characterized in that, the distance H 1 of described fold-type dividing plate (9) one end and sheet seam (13) is 10cm～25cm, and fold-type dividing plate (9) other end is immersed in the inner depth H 2 of storage tank liquid (10) and is not less than 5cm.
3. preparation method according to claim 2, is characterized in that, the bottom lengths A of described liquid storage groove (8) is less than or equal to the length L of changeover portion (5).
4. preparation method according to claim 3, is characterized in that, at fold-type dividing plate (9), is provided with manhole cover (12) with one end that sheet seam (13) is connected, and the aperture of manhole cover (12) should be not less than 30cm.
5. preparation method according to claim 4, is characterized in that, in changeover portion (5), be provided with by two or more deflector rolls, formed cut water device (11).
6. preparation method according to claim 5, is characterized in that, described fluid-tight liquid (10) can be water, butanols or high boiling solvent.
7. preparation method according to claim 6, is characterized in that, described fluid-tight liquid (10) is water.
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| CN201410117613.3A CN103950136B (en) | 2014-03-26 | 2014-03-26 | A kind of preparation method of cellulose triacetate thin film |
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| CN201410117613.3A CN103950136B (en) | 2014-03-26 | 2014-03-26 | A kind of preparation method of cellulose triacetate thin film |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104908184A (en) * | 2015-06-29 | 2015-09-16 | 中国乐凯集团有限公司 | Preparation method of cellulose triacetate ester film |
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| US20050242465A1 (en) * | 2004-03-29 | 2005-11-03 | Fuji Photo Film Co., Ltd. | Solution casting method and polymer film |
| CN101049736A (en) * | 2006-03-17 | 2007-10-10 | 富士胶片株式会社 | Manufacturing method of polymer film |
| CN101610892A (en) * | 2007-02-08 | 2009-12-23 | 柯尼卡美能达精密光学株式会社 | Cellulose ester membrane, its manufacture method, the polarizer that has used cellulose ester membrane and display unit |
| JP2011246504A (en) * | 2010-05-21 | 2011-12-08 | Fujifilm Corp | Production method of cellulose acylate film |
| JP2013001074A (en) * | 2011-06-21 | 2013-01-07 | Konica Minolta Advanced Layers Inc | Optical film manufacturing method, optical film, polarizing plate, and liquid crystal display device |
-
2014
- 2014-03-26 CN CN201410117613.3A patent/CN103950136B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050242465A1 (en) * | 2004-03-29 | 2005-11-03 | Fuji Photo Film Co., Ltd. | Solution casting method and polymer film |
| CN101049736A (en) * | 2006-03-17 | 2007-10-10 | 富士胶片株式会社 | Manufacturing method of polymer film |
| CN101610892A (en) * | 2007-02-08 | 2009-12-23 | 柯尼卡美能达精密光学株式会社 | Cellulose ester membrane, its manufacture method, the polarizer that has used cellulose ester membrane and display unit |
| JP2011246504A (en) * | 2010-05-21 | 2011-12-08 | Fujifilm Corp | Production method of cellulose acylate film |
| JP2013001074A (en) * | 2011-06-21 | 2013-01-07 | Konica Minolta Advanced Layers Inc | Optical film manufacturing method, optical film, polarizing plate, and liquid crystal display device |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104908184A (en) * | 2015-06-29 | 2015-09-16 | 中国乐凯集团有限公司 | Preparation method of cellulose triacetate ester film |
| CN104908184B (en) * | 2015-06-29 | 2017-05-17 | 中国乐凯集团有限公司 | Preparation method of cellulose triacetate ester film |
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| CN103950136B (en) | 2016-08-24 |
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