Solution film-forming method
View Patent ↗The solution film-forming method is provided in which the absolute filtration accuracy for a cellulose acylat solution can be improved and filtration throughput can be increased without reducing the pore size of a filtering material. A dope stock solution to be filtrated is first introduced into a body feed tank and a filter aid from a filter aid tank is added and dispersed. As the filter aid, an aid including SiO2 in 50% or more and a cellulose-based aid are mixed for use. The dope stock solution in which the filter aid is dispersed is introduced into a filter machine and subjected to filtration while forming a cake on the surface of the filtering material. After the filtration, a cleaning solvent is supplied in circulation from a cleaning solvent tank, and the cake is discharged as slurry. The filter aid is separated from the slurry by a separating device and burned in a burning device. Then, a regenerated filter aid is sent to the filter aid tank. After the cleaning, a precoat liquid in which the filter aid is dispersed is supplied from a precoat tank to the filter machine to form a precoat layer on the surface of the filtering material.
1. A solution film-forming method for producing a cellulose acylate film comprising steps of:
(a) preparing a cellulose acylate solution;
(b) filtering the cellulose acylate solution by a cake layer supported by a filtration support, the cake layer being formed by pre-coating a filter aid to the support, said filtering step removing all particles having a diameter of 0.01 mm or larger; and
(c) forming a film from the cellulose acylate solution obtained in step (b);
wherein said method further comprises, prior to the filtering step, a step of precoating the filtration support in a thickness of from 0.5 to 10 mm using a precoat liquid in which the filter aid is dispersed, wherein the filter aid has an average particle size in a range of from 1 to 150 μm;
wherein:
(i) the cellulose acylate film produced by said method is used for a liquid crystal display device;
(ii) a number of bright point defects observed under crossed-Nicol having a size of 20 μm or more is 0 defect/5 cm 2 , 10 μm or more is 10 defects/5 cm 2 or less, and 5 μm or more is 10 defects/5 cm 2 or less, said number being an average of five samples of 5 cm 2 in a width direction.
2. The solution film-forming method according to claim 1 , wherein the filter aid has a composition including SiO 2 in 50% or more.
3. The solution film-forming method according to claim 1 , wherein the filter aid is a cellulose-based aid.
4. The solution film-forming method according to claim 1 , wherein the filter aid is a mixture of a cellulose-based aid and another aid including SiO 2 in 50% or more.
5. The solution film-forming method according to claim 1 , wherein the filter aid comprises a mixture of two or more filter aids.
6. The solution film-forming method according to claim 1 , wherein the filter aid has a standard deviation of particle size of 0.5 times an average particle size or smaller.
7. The solution film-forming method according to claim 1 , wherein the filter aid has a bulk density in a range of from 0.01 to 0.8 g/cm 3 .
8. The solution film-forming method according to claim 1 , wherein the filter aid is added to the cellulose acylate solution in an amount of from 0.01 to 10% by weight.
9. The solution film-forming method according to claim 1 , wherein the precoat liquid has a terminal velocity of the filter aid in a range of from 10 −4 to 1 cm/s.
10. The solution film-forming method according to claim 1 , wherein the filtering step is carried out through a filtration support, the method further comprising, prior to the filtering step, a step of precoating the filtration support in a mass of from 0.1 to 5 kg/m 2 using a precoat liquid in which the filter aid is dispersed.
11. The solution film-forming method according to claim 10 , wherein the precoat liquid has a terminal velocity of the filter aid in a range of from 10 −4 to 1 cm/s.
12. The solution film-forming method according to claim 1 , wherein a flow rate in the filtering step is in a range of from 0.1 to 50 cm/hr.
13. The solution film-forming method according to claim 1 , wherein initial pressure difference in the filtering step is in a range of from 0.01 to 1 MPa.
14. The solution film-forming method according to claim 1 , wherein filtration pressure in the filtering step is in a range of from 0.01 to 4 MPa.
15. The solution film-forming method according to claim 1 , wherein pressure difference in the filtering step is in a range of from 0.01 to 3 MPa.
16. The solution film-forming method according to claim 1 , wherein a thickness of a cake layer formed in the filtering step is in a range of from 0.1 to 80 mm.
17. The solution film-forming method according to claim 1 , wherein the filtering step is carried out in a pressure condition where the cellulose acylate solution does not boil and at a temperature 20° C. lower than a boiling point of the cellulose acylate solution at normal pressure or higher.
18. The solution film-forming method according to claim 1 , wherein the filtering step comprises steps of:
(i) dispersing the filter aid in the cellulose acylate solution at a temperature in a range of from a boiling point of the cellulose acylate solution at normal pressure to a temperature 20° C. lower than the boiling point, and
(ii) filtering the filter-aid dispersed cellulose acylate solution obtained in step (i) having a saturation of dissolved air bubble of 90% or lower.
19. The solution film-forming method according to claim 1 , wherein the filtering step comprises steps of:
(i) dispersing the filter aid in the cellulose acylate solution, and
(ii) filtering the filter-aid dispersed cellulose acylate solution obtained in step (i) at a temperature lower than that of step (i).
20. The solution film-forming method according to claim 1 , wherein a concentration of the filter aid in the cellulose acylate solution is 10,000 particles/cm 3 or less after the filtering step.
21. The solution film-forming method according to claim 1 , further comprising, prior to step (c), a step of post-filtering the cellulose acylate solution after the filtering step through a filter having an absolute filtration accuracy of from 2 to 50 μm.
22. The solution film-forming method according to claim 1 , wherein the filtering step is carried out in a filter machine,
the method further comprising, following the filtering step, a step of backwashing the filter machine by supplying a cleaning solvent in circulation, in a pressure condition where the cleaning solvent does not boil, after being heated to a temperature 20° C. lower than a boiling point of the cellulose acylate solution or higher.
23. The solution film-forming method according to claim 22 , wherein the cleaning solvent is a non-chlorine organic solvent.
24. The solution film-forming method according to claim 1 , wherein the filtering step is carried out through a filtration support, the method further comprising, following the filtering step, a step of discharging a cake formed on the filtration support as a slurry having a concentration in a range of from 1 to 50 kg/m 3 .
25. The solution film-forming method according to claim 24 , wherein the slurry is reused as at least one of a precoat liquid and a body feed liquid.
26. The solution film-forming method according to claim 24 , further comprising, following the discharging step, steps of:
(i) separating the discharged slurry of the cake to a solvent and the filter aid, and
(ii) burning the filter aid at 400° C. or higher for reuse.
27. The solution film-forming method according to claim 26 , further comprising, following the burning step, a step of mixing the burned filter aid with a virgin filter aid for use.
28. The solution film-forming method according to claim 1 , wherein the forming step is carried out by co-casting.