TW201536509A - Solution casting method and apparatus - Google Patents
Solution casting method and apparatus Download PDFInfo
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- TW201536509A TW201536509A TW104109475A TW104109475A TW201536509A TW 201536509 A TW201536509 A TW 201536509A TW 104109475 A TW104109475 A TW 104109475A TW 104109475 A TW104109475 A TW 104109475A TW 201536509 A TW201536509 A TW 201536509A
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- 238000005266 casting Methods 0.000 title claims abstract description 189
- 238000000034 method Methods 0.000 title claims abstract description 44
- 239000002904 solvent Substances 0.000 claims abstract description 34
- 239000010408 film Substances 0.000 claims description 308
- 238000001035 drying Methods 0.000 claims description 63
- 239000013557 residual solvent Substances 0.000 claims description 47
- 239000007788 liquid Substances 0.000 claims description 13
- 229920000642 polymer Polymers 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 7
- 230000005855 radiation Effects 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 5
- 238000009736 wetting Methods 0.000 claims description 3
- 239000010409 thin film Substances 0.000 claims description 2
- 230000000052 comparative effect Effects 0.000 description 19
- 230000008569 process Effects 0.000 description 15
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- 239000002994 raw material Substances 0.000 description 9
- 239000011324 bead Substances 0.000 description 7
- 238000004804 winding Methods 0.000 description 7
- 229920002284 Cellulose triacetate Polymers 0.000 description 6
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 6
- NNLVGZFZQQXQNW-ADJNRHBOSA-N [(2r,3r,4s,5r,6s)-4,5-diacetyloxy-3-[(2s,3r,4s,5r,6r)-3,4,5-triacetyloxy-6-(acetyloxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6s)-4,5,6-triacetyloxy-2-(acetyloxymethyl)oxan-3-yl]oxyoxan-2-yl]methyl acetate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](OC(C)=O)[C@H]1OC(C)=O)O[C@H]1[C@@H]([C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H](COC(C)=O)O1)OC(C)=O)COC(=O)C)[C@@H]1[C@@H](COC(C)=O)O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@H]1OC(C)=O NNLVGZFZQQXQNW-ADJNRHBOSA-N 0.000 description 6
- 230000008859 change Effects 0.000 description 6
- 238000001816 cooling Methods 0.000 description 6
- 238000001514 detection method Methods 0.000 description 5
- 238000011144 upstream manufacturing Methods 0.000 description 5
- 238000009749 continuous casting Methods 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- 230000003068 static effect Effects 0.000 description 4
- 208000028659 discharge Diseases 0.000 description 3
- 230000008719 thickening Effects 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- LPSFUJXLYNJWPX-UHFFFAOYSA-N 1,1'-biphenyl;diphenyl hydrogen phosphate Chemical compound C1=CC=CC=C1C1=CC=CC=C1.C=1C=CC=CC=1OP(=O)(O)OC1=CC=CC=C1 LPSFUJXLYNJWPX-UHFFFAOYSA-N 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- 230000008030 elimination Effects 0.000 description 2
- 238000003379 elimination reaction Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000007602 hot air drying Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000012788 optical film Substances 0.000 description 2
- 238000005192 partition Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000001143 conditioned effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920006254 polymer film Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000011179 visual inspection Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- 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
- B29C41/46—Heating or cooling
-
- 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
- B29C41/50—Shaping under special conditions, e.g. vacuum
-
- 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
- B29C41/52—Measuring, controlling or regulating
-
- 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
- B29C71/00—After-treatment of articles without altering their shape; Apparatus therefor
- B29C71/02—Thermal after-treatment
-
- 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
- B29D7/00—Producing flat articles, e.g. films or sheets
- B29D7/01—Films or sheets
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Moulding By Coating Moulds (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
Abstract
Description
本發明係有關一種溶液製膜方法及設備。 The invention relates to a solution film forming method and device.
具有透光性之聚合物薄膜(以下,稱為薄膜)廣泛用作偏光板的保護膜、相位差膜、防反射膜、透明導電性薄膜等光學薄膜。對於薄膜要求厚度的均勻性和光學特性。以往,主要使用厚度為80μm以上的厚型薄膜,但近年來,隨著光學薄膜的多樣化,薄膜的薄膜化需求增強,要求厚度為15μm以上40μm以下左右的薄膜。 A translucent polymer film (hereinafter referred to as a film) is widely used as an optical film such as a protective film of a polarizing plate, a retardation film, an antireflection film, or a transparent conductive film. The uniformity and optical properties of the thickness are required for the film. In the past, a thick film having a thickness of 80 μm or more has been mainly used. However, in recent years, as the optical film is diversified, the film thickness of the film is increased, and a film having a thickness of about 15 μm or more and 40 μm or less is required.
作為薄膜的製造方法,使用溶液製膜方法。溶液製膜方法係例如藉由如下來獲得薄膜之方法,亦即,藉由流延模在金屬製支撐體上流延將聚合物溶解於溶劑中之溶液(以下,稱為濃液)來形成流延膜,使其乾燥並剝取。作為支撐體,有滾筒或傳送帶等。使溶劑從流延膜蒸發並使流延膜乾燥至能夠剝取之程度之流延膜乾燥製程係在整個溶液製膜方法中花費較長時間之製程,因此希望縮短流延膜乾燥製程。 As a method of producing a film, a solution film forming method is used. The solution film forming method is a method of obtaining a film by, for example, casting a solution in which a polymer is dissolved in a solvent (hereinafter referred to as a dope) by casting a casting die on a metal support to form a flow. The film is stretched, dried and stripped. As the support, there are a drum, a conveyor belt, and the like. The casting film drying process for evaporating the solvent from the casting film and drying the cast film to the extent that it can be peeled off is a process which takes a long time in the entire solution film forming method, and therefore it is desirable to shorten the casting film drying process.
為了縮短流延膜乾燥製程,在日本專利公開2012-066483號公報中記載的溶液製膜方法中,在自濃液從流延模流出到在支撐體上流延為止的期間照射紅外線,並使100℃左右的熱風與形成於支撐體上之流延膜接觸,從而對流延膜進行加熱及乾燥。 In the solution film forming method described in Japanese Laid-Open Patent Publication No. 2012-066483, the infrared ray is irradiated during the period from the flow of the dope to the casting on the support, and the process is performed. The hot air around °C is brought into contact with the casting film formed on the support to heat and dry the cast film.
為了獲得薄膜,需形成較薄的流延膜(以下,稱為薄流延膜)。因此,為了對用於獲得以往的厚型薄膜之較厚的流延膜(以下,稱為厚流延膜)進行乾燥而對流延膜噴吹乾燥風來進行乾燥之方法中,由於乾燥風而產生厚度不均,存在表面平滑性受損之問題。並且,後續製程有基於後述的夾子拉幅機等之拉伸製程時,該厚度不均還會成為產生拉伸不均之原因。因此,在日本專利公開2012-066483號公報中記載的溶液製膜方法中,對於由從流延模遍及支撐體上而流出之由濃液構成之液珠,藉由紅外線加熱器照射紅外線,促進液珠中的溶劑的蒸發,從而高效地進行流延膜的乾燥。 In order to obtain a film, a thin cast film (hereinafter referred to as a thin cast film) is formed. Therefore, in order to dry a thick cast film (hereinafter referred to as a thick cast film) for obtaining a conventional thick film and to dry the film by drying the wind, the dry wind is used. There is a problem that the thickness is uneven and the surface smoothness is impaired. Further, when the subsequent process is based on a drawing process such as a clip tenter described later, the thickness unevenness may also cause stretching unevenness. Therefore, in the solution film forming method described in Japanese Patent Laid-Open Publication No. 2012-066483, the liquid droplets composed of the concentrated liquid which flow out from the casting mold over the support are irradiated with infrared rays by the infrared heater to promote the liquid crystal. The evaporation of the solvent in the liquid bead is performed to efficiently dry the cast film.
在乾燥進行至可剝取流延膜之程度之階段,從支撐體剝下流延膜來作為濕潤膜而送至夾子拉幅機,以夾子拉幅機促進濕潤膜的乾燥。夾子拉幅機中,藉由夾子把持濕潤膜的兩側緣部並進行傳送,在該傳送期間藉由乾燥風進一步促進乾燥。然而,即使僅藉由紅外線加熱器從液珠階段開始促進溶劑的蒸發,當為較薄之薄膜時,在接下來的拉伸製程中,有時薄膜側緣部因夾子被咬碎,希望予以改良。 At the stage where the drying is carried out to the extent that the cast film can be peeled off, the cast film is peeled off from the support to be sent as a wet film to the clip tenter, and the clip tenter is used to promote the drying of the wet film. In the clip tenter, both side edges of the wet film are held by the clips and conveyed, and drying is further promoted by the dry air during the conveyance. However, even if the evaporation of the solvent is promoted from the liquid bead stage only by the infrared heater, when it is a thin film, in the subsequent stretching process, the side edge portion of the film may be bitten by the clip, and it is desirable to Improvement.
因此,本發明的目的在於提供一種製造較薄之薄膜時,在拉伸製程中不會產生薄膜側緣部的咬碎而能夠製造無厚度不均和拉伸不均之薄膜之溶液製膜方法及設備。 Therefore, an object of the present invention is to provide a solution film forming method capable of producing a film having no thickness unevenness and uneven stretching without causing chipping of the side edge portion of the film during the stretching process. And equipment.
本發明的溶液製膜方法具備流延膜形成步驟(A步驟)、流延膜乾燥步驟(B步驟)、剝取步驟(C步驟)、薄膜乾燥步驟(D步驟)及側緣部乾燥步驟(E步驟)。在A步驟中,從流延模朝向移動之支撐體流出 濃液,從而在支撐體上形成兩側緣部比中央部厚之流延膜。濃液包含聚合物及溶劑。在B步驟中,使溶劑從流延膜蒸發來進行乾燥。在C步驟中,從支撐體剝取經過B步驟之流延膜來作為濕潤膜。在D步驟中,藉由夾子把持濕潤膜的兩側緣部,並使溶劑蒸發來作為薄膜。在E步驟中,在B步驟中以輻射方式加熱流延膜的兩側緣部,將剝取流延膜時的流延膜的兩側緣部的殘留溶劑量設為VS1,且將剝取流延膜時的流延膜的中央部的殘留溶劑量設為VC1時,滿足以下條件。 The solution film forming method of the present invention comprises a cast film forming step (A step), a cast film drying step (B step), a stripping step (C step), a film drying step (D step), and a side edge drying step ( Step E). In step A, the flow from the casting die to the moving support The dope is formed to form a cast film having a thicker side edge than the central portion on the support. The dope contains the polymer and solvent. In the step B, the solvent is evaporated from the cast film to be dried. In the step C, the cast film which passed through step B was peeled off from the support as a wet film. In the step D, the both side edges of the wet film are held by a clip, and the solvent is evaporated to form a film. In the step E, the both side edges of the casting film are heated by radiation in the step B, and the residual solvent amount on both side edges of the casting film when the casting film is peeled off is set to VS1, and the stripping is performed. When the amount of residual solvent in the center portion of the cast film at the time of casting a film is VC1, the following conditions are satisfied.
50%DB<VC1100%DB時,設為(VC1-15)VS1(0.96×VC1+25)的範圍內。 50%DB<VC1 When 100%DB, set to (VC1-15) VS1 Within the range of (0.96 × VC1 + 25).
20%DB<VC150%DB時,設為(0.85×VC1-7.86)VS1(1.28×VC1+5.71)的範圍內。 20%DB<VC1 50% DB, set to (0.85 × VC1 - 7.86) VS1 Within the range of (1.28 × VC1 + 5.71).
VC120%DB時,設為VS1(1.28×VC1+5.71)的範圍內。 VC1 20% DB, set to VS1 Within the range of (1.28 × VC1 + 5.71).
將薄膜的中央部的最大厚度設為TC,且將側緣部的最大厚度設為TS時,設為1.1×TCTS為較佳。 When the maximum thickness of the central portion of the film is TC and the maximum thickness of the side edge portion is TS, it is set to 1.1 × TC. TS is preferred.
在E步驟中,檢測剝取前的流延膜的中央部的殘留溶劑量及側緣部的殘留溶劑量,依據檢測出之殘留溶劑量,控制對兩側緣部的加熱量為較佳。 In the step E, the amount of residual solvent in the center portion of the cast film before peeling and the amount of residual solvent in the side edge portion are detected, and it is preferable to control the amount of heating on both side edges depending on the amount of residual solvent detected.
在E步驟中,對流延膜的兩側緣部照射紅外線為較佳。 In the E step, it is preferred to irradiate infrared rays to both side edges of the cast film.
紅外線係遠紅外線為較佳。 Infrared infrared rays are preferred.
流延膜的兩側緣部包含被夾子把持之範圍為較佳。 It is preferable that both side edges of the cast film include a range held by the clip.
本發明的溶液製膜設備具備流延膜形成裝置、流延膜乾燥部、剝取輥、薄膜乾燥部及側緣部乾燥部。流延膜形成裝置從流延模朝向 移動之支撐體流出濃液,從而在支撐體上形成兩側緣部比中央部厚之流延膜。濃液包含聚合物及溶劑。流延膜乾燥部使溶劑從形成於支撐體上之流延膜蒸發來進行乾燥。剝取輥剝取被乾燥之流延膜來作為濕潤膜。薄膜乾燥部使溶劑從濕潤膜蒸發來作為薄膜。側緣部乾燥部設置於流延膜乾燥部,以輻射方式加熱流延膜的兩側緣部,將剝取流延膜時的流延膜的兩側緣部的殘留溶劑量設為VS1,且將剝取流延膜時的流延膜的中央部的殘留溶劑量設為VC1時,滿足以下條件。 The solution film forming apparatus of the present invention includes a cast film forming apparatus, a cast film drying section, a peeling roll, a film drying section, and a side edge drying section. Cast film forming device from casting die The moving support flows out of the dope to form a cast film having a thicker side edge than the central portion on the support. The dope contains the polymer and solvent. The cast film drying section evaporates the solvent from the casting film formed on the support, and dries it. The stripping roll strips the dried cast film as a wet film. The film drying section evaporates the solvent from the wet film as a film. The side edge portion drying portion is provided in the casting film drying portion, and both side edges of the casting film are heated by radiation, and the amount of residual solvent on both side edges of the casting film when the casting film is peeled off is set to VS1. When the amount of residual solvent in the center portion of the cast film when the cast film is peeled off is set to VC1, the following conditions are satisfied.
50%DB<VC1100%DB時,設為(VC1-15)VS1(0.96×VC1+25)的範圍內。 50%DB<VC1 When 100%DB, set to (VC1-15) VS1 Within the range of (0.96 × VC1 + 25).
20%DB<VC150%DB時,設為(0.85×VC1-7.86)VS1(1.28×VC1+5.71)的範圍內。 20%DB<VC1 50% DB, set to (0.85 × VC1 - 7.86) VS1 Within the range of (1.28 × VC1 + 5.71).
VC120%DB時,設為VS1(1.28×VC1+5.71)的範圍內。 VC1 20% DB, set to VS1 Within the range of (1.28 × VC1 + 5.71).
側緣部乾燥部具有對流延膜的兩側緣部照射紅外線之紅外線加熱器為較佳。 It is preferable that the side edge portion drying portion has an infrared heater that irradiates infrared rays to both side edges of the casting film.
依本發明,剝取後的濕潤膜的兩側緣部被充份乾燥,能夠防止拉伸製程中的薄膜側緣部的撕碎和咬入不良的產生,能夠製造無厚度不均和拉伸不均之薄膜。 According to the present invention, both side edges of the wet film after peeling are sufficiently dried, and it is possible to prevent the occurrence of chipping and biting defects in the side edge portion of the film in the stretching process, and it is possible to manufacture no thickness unevenness and stretching. Uneven film.
10‧‧‧溶液製膜設備 10‧‧‧solution film making equipment
12‧‧‧流延膜形成裝置 12‧‧‧cast film forming device
13‧‧‧夾子拉幅機(薄膜乾燥部) 13‧‧‧Clip tenter (film drying section)
18‧‧‧濃液 18‧‧‧Liquor
19‧‧‧濕潤膜 19‧‧‧ Wet film
23‧‧‧薄膜 23‧‧‧ Film
41、100‧‧‧流延模 41, 100‧‧‧ casting die
42‧‧‧流延帶(支撐體) 42‧‧‧casting belt (support)
44‧‧‧剝取輥 44‧‧‧ Stripping roller
45‧‧‧流延膜 45‧‧‧cast film
45a‧‧‧側緣部 45a‧‧‧lateral edge
45b‧‧‧中央部 45b‧‧‧Central Department
51、52‧‧‧側緣部用紅外線照射裝置(側緣部乾燥部) 51, 52‧‧‧Infrared irradiation device (side edge drying part)
51a~54a‧‧‧紅外線加熱器 51a~54a‧‧‧Infrared heater
53、54‧‧‧中央部用紅外線照射裝置 53, 54‧‧‧The central part uses infrared radiation
71‧‧‧流延膜形成製程 71‧‧‧cast film forming process
72‧‧‧側緣部乾燥製程 72‧‧‧ Side edge drying process
73‧‧‧流延膜乾燥製程 73‧‧‧cast film drying process
74‧‧‧剝取製程 74‧‧‧Extraction process
75‧‧‧薄膜乾燥製程 75‧‧‧film drying process
第1圖係表示溶液製膜設備的概要之側視圖。 Fig. 1 is a side view showing an outline of a solution film forming apparatus.
第2圖係表示流延膜形成裝置之側視圖。 Fig. 2 is a side view showing a cast film forming apparatus.
第3圖係表示流延模的狹縫形狀的一例之側視圖。 Fig. 3 is a side view showing an example of a slit shape of a casting die.
第4圖係表示兩側緣部較厚之流延膜的一例之立體圖。 Fig. 4 is a perspective view showing an example of a cast film having thicker side edges.
第5圖係表示流延膜的乾燥方法的一例之剖面圖。 Fig. 5 is a cross-sectional view showing an example of a method of drying a cast film.
第6圖係溶液製膜方法的流程圖。 Figure 6 is a flow chart of a solution film forming method.
第7圖係表示藉由連續流延形成兩側緣部較厚之流延膜之一例之立體圖。 Fig. 7 is a perspective view showing an example of a cast film in which both side edges are thick by continuous casting.
第8圖係表示藉由濃液追加形成兩側緣部較厚之流延膜之一例之剖面圖。 Fig. 8 is a cross-sectional view showing an example of a cast film having thicker side edges formed by addition of a dope.
第9圖係表示設置有測定流延膜的厚度之感測器之另一實施形態之側視圖。 Fig. 9 is a side view showing another embodiment of a sensor provided with a thickness for measuring a cast film.
第10圖係表示流延膜的殘留溶劑量VC1與VS1的關係之曲線圖。 Fig. 10 is a graph showing the relationship between the residual solvent amount VC1 of the cast film and VS1.
如第1圖所示,實施了本發明之溶液製膜設備10從製造生產線的上游側依次具有流延膜形成裝置12、夾子拉幅機(薄膜乾燥部)13、乾燥室15、冷卻室16及捲取室17。流延膜形成裝置12中由包含聚合物及溶劑之濃液18形成濕潤膜19。 As shown in Fig. 1, the solution film forming apparatus 10 according to the present invention has a cast film forming apparatus 12, a clip tenter (film drying section) 13, a drying chamber 15, and a cooling chamber 16 in this order from the upstream side of the manufacturing line. And the take-up chamber 17. The wet film 19 is formed in the cast film forming apparatus 12 from a dope 18 containing a polymer and a solvent.
在流延膜形成裝置12與夾子拉幅機13之間的過渡部21設置有將乾燥風送到濕潤膜19之送風機21a、及支撐濕潤膜19之複數個支撐輥21b。複數個支撐輥21b向濕潤膜19的傳送方向排列。支撐輥21b支撐從流延膜形成裝置12送出之濕潤膜19,並將其向夾子拉幅機13引導。 The transition portion 21 between the cast film forming device 12 and the clip tenter 13 is provided with a blower 21a that sends dry air to the wet film 19, and a plurality of support rollers 21b that support the wet film 19. A plurality of support rollers 21b are arranged in the conveying direction of the wet film 19. The support roller 21b supports the wetting film 19 sent from the cast film forming device 12, and guides it to the clip tenter 13.
夾子拉幅機13以夾子(未圖示)把持濕潤膜19的兩側緣部的同時將其傳送。夾子拉幅機13藉由對濕潤膜19實施乾燥和拉伸等規定處理來設為薄膜23。薄膜23從夾子拉幅機13向乾燥室15被送出。 The clip tenter 13 conveys the both sides of the wet film 19 while holding them by a clip (not shown). The clip tenter 13 is formed into a film 23 by performing a predetermined process such as drying and stretching on the wet film 19. The film 23 is fed out from the clip tenter 13 to the drying chamber 15.
乾燥室15中設置有複數個輥27。乾燥室15內的氣氛的溫度和濕度等藉由未圖示之空調機調節。薄膜23捲繞於複數個輥27而在乾燥室15內被傳送,並在乾燥室15內被實施乾燥處理。乾燥室15與吸附回收裝置28連接。吸附回收裝置28將從薄膜23蒸發之溶劑氣體吸附於吸附劑來回收。 A plurality of rollers 27 are disposed in the drying chamber 15. The temperature, humidity, and the like of the atmosphere in the drying chamber 15 are adjusted by an air conditioner (not shown). The film 23 is wound around a plurality of rolls 27 and conveyed in the drying chamber 15, and is dried in the drying chamber 15. The drying chamber 15 is connected to the adsorption recovery device 28. The adsorption recovery device 28 recovers the solvent gas evaporated from the film 23 by adsorbing it to the adsorbent.
冷卻室16將薄膜23冷卻至薄膜23的溫度成為大致室溫。在冷卻室16與捲取室17之間,從上游側依次設置有除電棒29及滾花賦予輥30。除電棒29對從冷卻室16送出且帶電之薄膜23進行除電。滾花賦予輥30對薄膜23的寬度方向兩端賦予捲取用滾花。 The cooling chamber 16 cools the film 23 until the temperature of the film 23 becomes substantially room temperature. A static eliminating rod 29 and a knurling applying roller 30 are provided between the cooling chamber 16 and the winding chamber 17 in this order from the upstream side. The static eliminating rod 29 discharges the charged film 23 which is sent out from the cooling chamber 16 and is charged. The knurling applying roller 30 applies a knurling for winding to both ends in the width direction of the film 23.
捲取室17中設置有具有壓輥34及捲芯35之捲取機36。送出至捲取室17之薄膜23被壓輥34按壓之同時捲取於捲芯35,從而成為捲狀。 A coiler 36 having a pressure roller 34 and a winding core 35 is disposed in the winding chamber 17. The film 23 sent to the take-up chamber 17 is taken up by the pressure roller 34 while being wound around the winding core 35, and is wound.
(流延膜形成裝置) (cast film forming device)
如第2圖所示,流延膜形成裝置12中,在流延室38內設置有流延模41、流延帶42、滾筒43a、43b及剝取輥44。流延室38藉由隔板39a~39c劃分為流延部38a、乾燥部38b、剝取部38c。隔板39a~39c從流延室38的內壁面朝向流延帶42延伸,在前端形成有迷宮式密封件40。迷宮式密封件40靠近流延帶42而配設,抑制流延部38a、乾燥部38b及剝取部38c彼此之間的氣氛氣體的出入。 As shown in Fig. 2, in the casting film forming apparatus 12, a casting die 41, a casting tape 42, rollers 34a and 43b, and a peeling roller 44 are provided in the casting chamber 38. The casting chamber 38 is divided into a casting portion 38a, a drying portion 38b, and a stripping portion 38c by partition plates 39a to 39c. The partition plates 39a to 39c extend from the inner wall surface of the casting chamber 38 toward the casting belt 42, and a labyrinth seal 40 is formed at the front end. The labyrinth seal 40 is disposed close to the casting belt 42 and suppresses the entry and exit of the atmosphere gas between the casting portion 38a, the drying portion 38b, and the stripping portion 38c.
流延帶42藉由連結金屬製帶板的長邊方向的一端與另一端而形成,呈環狀。流延帶42例如由具有充份的耐腐蝕性及強度之不銹鋼(SUS316)構成。流延帶42捲繞於滾筒43a、43b。滾筒43a、43b以軸向 成為水平之方式以相互相同值高度大致平行地排列。若一個滾筒43a藉由未圖示之馬達的驅動而旋轉,則流延帶42向X方向循環移動。藉此,在滾筒43a、43b的上側,流延帶42從滾筒43a朝向滾筒43b移動,與滾筒43b接觸時,流延帶42沿著滾筒43b從上側向下側移動。並且,在滾筒43a、43b的下側,流延帶42從滾筒43b朝向滾筒43a移動,與滾筒43a接觸時,流延帶42沿著滾筒43a從下側向上側移動。 The casting tape 42 is formed by connecting one end and the other end in the longitudinal direction of the metal strip. The casting belt 42 is made of, for example, stainless steel (SUS316) having sufficient corrosion resistance and strength. The casting belt 42 is wound around the drums 43a and 43b. The rollers 43a, 43b are axially The way to be horizontal is arranged substantially parallel to each other at the same height. When one of the rollers 43a is rotated by driving of a motor (not shown), the casting tape 42 is circulated in the X direction. Thereby, on the upper side of the drums 43a and 43b, the casting belt 42 moves from the drum 43a toward the drum 43b, and when it contacts the drum 43b, the casting belt 42 moves from the upper side to the lower side along the drum 43b. Further, on the lower side of the drums 43a and 43b, the casting belt 42 moves from the drum 43b toward the drum 43a, and when it comes into contact with the drum 43a, the casting belt 42 moves from the lower side to the upper side along the drum 43a.
流延模41位於滾筒43a的上方,靠近作為支撐體之流延帶42而配設。如第3圖所示,在流延模41的前端設置有狹縫出口41a。狹縫出口41a的間隙例如藉由狹縫間隙調整螺栓(未圖示)調整。藉此,狹縫出口41a的寬度方向(Y方向)的兩側緣部例如自端部25mm的範圍的間隙與寬度中央部相比,更寬。另外,第3圖中僅示出流延模41的前端面。 The casting die 41 is positioned above the drum 43a and disposed adjacent to the casting belt 42 as a support. As shown in Fig. 3, a slit outlet 41a is provided at the tip end of the casting die 41. The gap of the slit outlet 41a is adjusted by, for example, a slit gap adjusting bolt (not shown). Thereby, the both edge parts of the width direction (Y direction) of the slit exit hole 41a are the widths of the range of 25 mm from the end part, for example, and it is wider than the width center part. In addition, only the front end surface of the casting die 41 is shown in FIG.
如第4圖所示,所流延之濃液18在循環移動之流延帶42上形成沿X方向較長地延伸之帶狀流延膜45。流延膜45藉由流延帶42的移動向X方向被傳送。並且,藉由狹縫出口41a的間隙形狀,流延膜45的Y方向上之兩側緣部45a比中央部45b厚。本實施形態中,兩側緣部45a為自流延膜45的端部25mm的範圍,但該範圍係包含被夾子拉幅機13的夾子把持之範圍者即可。例如,自流延膜45的端部15mm以上60mm以下的範圍內為較佳,15mm以上40mm以下更為佳。另外,流延膜45和流延帶42的厚度與流延膜45和流延帶42的寬度相比較微小,因此與寬度相比誇張地圖示厚度,並且,為了便於理解而簡略化。 As shown in Fig. 4, the cast dope 18 forms a strip-shaped cast film 45 extending in the X direction on the casting tape 42 which is circulated and moved. The casting film 45 is conveyed in the X direction by the movement of the casting tape 42. Further, the side edge portions 45a of the casting film 45 in the Y direction are thicker than the center portion 45b by the gap shape of the slit outlets 41a. In the present embodiment, the both side edge portions 45a are in the range of 25 mm from the end portion of the casting film 45, but the range is included in the range held by the clip of the clip tenter 13. For example, it is preferable that the end portion of the casting film 45 is in the range of 15 mm or more and 60 mm or less, and more preferably 15 mm or more and 40 mm or less. Further, since the thicknesses of the casting film 45 and the casting tape 42 are relatively small as compared with the widths of the casting film 45 and the casting tape 42, the thickness is exaggeratedly illustrated as compared with the width, and is simplified for the sake of easy understanding.
如第2圖所示,在流延模41的X方向上游側,與流延模41相接而設置有減壓腔室47。藉由減壓腔室47,從流延模41至流延帶42為 止的濃液18、所謂的流延液珠的上游側區域被減壓。藉此,由於流延帶42的循環移動而產生之攜帶風引起之流延液珠的振動得到抑制,厚度不均得到抑制。 As shown in FIG. 2, a decompression chamber 47 is provided in contact with the casting die 41 on the upstream side in the X direction of the casting die 41. By the decompression chamber 47, from the casting die 41 to the casting tape 42 The concentrated liquid 18 and the upstream side region of the so-called cast liquid bead are decompressed. Thereby, the vibration of the casting bead caused by the wind-carrying due to the cyclic movement of the casting belt 42 is suppressed, and the thickness unevenness is suppressed.
在流延帶42的周圍靠近流延帶42而設置有側緣部用紅外線照射裝置(側緣部乾燥部)51、52及中央部用紅外線照射裝置53、54(參閱第5圖)。 The side of the casting belt 42 is provided with a side edge portion infrared ray irradiation device (side edge portion drying portion) 51 and 52 and a central portion infrared ray irradiation device 53 and 54 (see Fig. 5).
如第4圖所示,側緣部用紅外線照射裝置51在比流延模41更靠X方向下游側且從滾筒43a朝向滾筒43b(參閱第2圖)之流延帶42的上方配設成與流延膜45的兩側緣部45a相對。如第5圖所示,側緣部用紅外線照射裝置51具有紅外線加熱器51a。從紅外線加熱器51a對流延膜45的兩側緣部45a照射紅外線(波長為0.7μm以上1000μm以下的範圍),使兩側緣部45a的溶劑蒸發來對兩側緣部45a進行乾燥。 As shown in Fig. 4, the side edge portion infrared irradiation device 51 is disposed above the casting tape 42 on the downstream side in the X direction from the casting die 41 and from the drum 43a toward the drum 43b (see Fig. 2). It is opposed to both side edge portions 45a of the casting film 45. As shown in Fig. 5, the side edge portion infrared ray irradiation device 51 has an infrared heater 51a. Infrared heaters 51a are irradiated with infrared rays (wavelengths in a range of 0.7 μm or more and 1000 μm or less) from both side edges 45a of the casting film 45, and the solvents of the both side edge portions 45a are evaporated to dry the both side edge portions 45a.
中央部用紅外線照射裝置53被側緣部用紅外線照射裝置51夾住,配設成與流延膜45的中央部45b相對。中央部用紅外線照射裝置53亦與側緣部用紅外線照射裝置51同樣,具有紅外線加熱器53a,對除了流延膜45的兩側緣部45a之中央部45b照射紅外線對中央部45b進行乾燥。另外,第4圖中,省略中央部用紅外線照射裝置53的圖示。 The central portion is sandwiched by the infrared ray irradiation device 51 by the side edge portion of the infrared ray irradiation device 53, and is disposed to face the central portion 45b of the casting film 45. Similarly to the infrared ray irradiation device 51 for the side edge portion, the central portion of the infrared ray irradiation device 53 has an infrared ray heater 53a for drying the central portion 45b by irradiating infrared rays to the central portion 45b of the both side edge portions 45a of the casting film 45. In addition, in FIG. 4, the illustration of the infrared irradiation device 53 for center part is abbreviate|omitted.
側緣部用紅外線照射裝置52及中央部用紅外線照射裝置54配設於從滾筒43b朝向滾筒43a之流延帶42的下方附近。側緣部用紅外線照射裝置52及中央部用紅外線照射裝置54與側緣部用紅外線照射裝置51及中央部用紅外線照射裝置53同樣地構成,具有紅外線加熱器52a、54a,並且對流延膜45進行乾燥。藉由該些各紅外線照射裝置51~54構成流延 膜乾燥部,以此進行流延膜乾燥製程73(參閱第6圖)。另外,各紅外線照射裝置51~54的紅外線加熱器51a~54a由1個或複數個構成,在使用複數個時,可個別控制溫度。另外,如所周知,紅外線藉由波長區域被區分得更細,0.7μm~2.5μm的波長區域被稱作近紅外線,2.5μm~4μm的波長區域被稱作中紅外線,4μm~1000μm的波長區域被稱作遠紅外線。並且,三醋酸纖維素易吸收4μm以上20μm以下波長的紅外線,甲醇易吸收2.5μm以上4μm以下波長的紅外線。並且,當濃液18中含有三醋酸纖維素和甲醇時,所照射之紅外線包含2.5μm以上20μm以下的波長區域為較佳。作為具體的例子,當作為濃液18的聚合物原料而使用三醋酸纖維素時,紅外線加熱器51a、52a、53a、54a所射出之紅外線為遠紅外線更為佳,藉此,流延膜45的乾燥更有效地進行。當作為濃液18的聚合物原料而使用三醋酸纖維素且在濃液18的溶劑中含有甲醇時,紅外線加熱器51a、52a、53a、54a所射出之紅外線為遠紅外線和中紅外線更為佳。藉此,流延膜45的乾燥進一步有效地進行。 The side edge portion infrared ray irradiation device 52 and the central portion infrared ray irradiation device 54 are disposed near the lower side of the casting belt 42 from the drum 43b toward the drum 43a. The side edge portion infrared ray irradiation device 52 and the central portion infrared ray irradiation device 54 are configured similarly to the side edge portion infrared ray irradiation device 51 and the central portion infrared ray irradiation device 53, and have infrared heaters 52a and 54a, and a pair of casting films 45. Dry. Casting by the infrared ray irradiation devices 51 to 54 The film drying section performs the casting film drying process 73 (see Fig. 6). Further, the infrared heaters 51a to 54a of the infrared irradiation devices 51 to 54 are composed of one or a plurality of them, and when a plurality of infrared heaters 51a to 54a are used, the temperature can be individually controlled. Further, as is well known, infrared rays are distinguished by a wavelength region, a wavelength region of 0.7 μm to 2.5 μm is referred to as near-infrared rays, and a wavelength region of 2.5 μm to 4 μm is referred to as mid-infrared rays, and a wavelength region of 4 μm to 1000 μm. It is called far infrared ray. Further, cellulose triacetate easily absorbs infrared rays having a wavelength of 4 μm or more and 20 μm or less, and methanol easily absorbs infrared rays having a wavelength of 2.5 μm or more and 4 μm or less. Further, when the concentrated liquid 18 contains cellulose triacetate and methanol, it is preferred that the infrared ray to be irradiated has a wavelength region of 2.5 μm or more and 20 μm or less. As a specific example, when cellulose triacetate is used as the polymer raw material of the dope 18, the infrared rays emitted from the infrared heaters 51a, 52a, 53a, and 54a are more preferably far infrared rays, whereby the casting film 45 is used. The drying is carried out more efficiently. When cellulose triacetate is used as the polymer raw material of the dope 18 and methanol is contained in the solvent of the dope 18, the infrared rays emitted from the infrared heaters 51a, 52a, 53a, 54a are preferably far infrared rays and medium infrared rays. . Thereby, the drying of the casting film 45 is further efficiently performed.
側緣部用紅外線照射裝置51、52及中央部用紅外線照射裝置53、54分別與控制器50(參閱第2圖)連接。控制器50控制各紅外線照射裝置51~54,根據流延膜45的Y方向上之厚度變動對流延膜45進行乾燥,以使剝取時的流延膜45的殘留溶劑量成為下述範圍內。 The side edge portion infrared irradiation devices 51 and 52 and the central portion infrared irradiation devices 53 and 54 are respectively connected to the controller 50 (see Fig. 2). The controller 50 controls the respective infrared irradiation devices 51 to 54 to dry the casting film 45 in accordance with the thickness variation in the Y direction of the casting film 45 so that the residual solvent amount of the casting film 45 at the time of peeling is within the following range. .
藉由各紅外線照射裝置51~54的紅外線照射,流延膜45被乾燥至中央部45b的殘留溶劑量成為100%DB(Dry Base:乾量基準)以下。另外,本實施形態中,將以乾量基準表示殘留於流延膜45和各薄膜中之溶劑量者作為殘留溶劑量。將應求出殘留溶劑量之測定對象的流延膜45 的質量設為x,且將完全乾燥該流延膜45後的質量設為y時,藉由{(x-y)/y}×100求出殘留溶劑量。另外,所謂“完全乾燥”,溶劑的量無需嚴格成為0(零)。例如,將以110℃對測定對象的薄膜23進行3小時的乾燥處理後的質量設為y即可。 By the infrared irradiation of each of the infrared irradiation devices 51 to 54, the casting film 45 is dried until the amount of residual solvent in the central portion 45b becomes 100% DB (Dry Base). In the present embodiment, the amount of solvent remaining in the casting film 45 and each film is expressed as a residual solvent amount on a dry basis. Cast film 45 to be measured for the amount of residual solvent When the mass is x, and the mass after the casting film 45 is completely dried is y, the amount of residual solvent is determined by {(x - y) / y} × 100. Further, the so-called "completely dry", the amount of the solvent does not need to be strictly 0 (zero). For example, the mass after drying the film 23 to be measured at 110 ° C for 3 hours may be y.
控制器50控制側緣部用紅外線照射裝置51、52及中央部用紅外線照射裝置53、54,將剝取流延膜45時的流延膜45的兩側緣部45a的殘留溶劑量及中央部45b的殘留溶劑量設為一定範圍。具體而言,為以下條件。在此,將剝取流延膜45時的流延膜45的兩側緣部45a的殘留溶劑量設為VS1,將剝取流延膜45時的流延膜45的中央部45b的殘留溶劑量設為VC1。 The controller 50 controls the amount of residual solvent and the center of the both side edge portions 45a of the casting film 45 when the casting film 45 is peeled off by the infrared ray irradiation devices 51 and 52 and the central portion infrared ray irradiation devices 53 and 54. The amount of residual solvent in the portion 45b is set to a certain range. Specifically, the following conditions are met. Here, the residual solvent amount of both side edge portions 45a of the casting film 45 when the casting film 45 is peeled off is VS1, and the residual solvent of the center portion 45b of the casting film 45 when the casting film 45 is peeled off is removed. The amount is set to VC1.
50%DB<VC1100%DB時,設為(VC1-15)VS1(0.96×VC1+25)的範圍內。 50%DB<VC1 When 100%DB, set to (VC1-15) VS1 Within the range of (0.96 × VC1 + 25).
並且,20%DB<VC150%DB時,設為(0.85×VC1-7.86)VS1(1.28×VC1+5.71)的範圍內。 And, 20% DB<VC1 50% DB, set to (0.85 × VC1 - 7.86) VS1 Within the range of (1.28 × VC1 + 5.71).
而且,VC120%DB時,設為VS1(1.28×VC1+5.71)的範圍內。 Moreover, VC1 20% DB, set to VS1 Within the range of (1.28 × VC1 + 5.71).
亦即,當VC1在大於50%DB且100%DB以下的範圍內時,將VS1設為(VC1-15)%DB以上(0.96×VC1+25)%DB以下的範圍內,當VC1在大於20%DB且50%DB以下的範圍內時,將VS1設為(0.85×VC1-7.86)%DB以上(1.28×VC1+5.71)%DB以下的範圍,當VC1為20%DB以下時,將VS1設為(1.28×VC1+5.71)%DB以下。 That is, when VC1 is in a range of more than 50% DB and 100% DB or less, VS1 is set to be in a range of (VC1-15)%DB or more (0.96×VC1+25)%DB or less, when VC1 is larger than In the range of 20% DB and 50% DB or less, VS1 is set to a range of (0.85 × VC1 - 7.86)%DB or more (1.28 × VC1 + 5.71)% DB or less, and when VC1 is 20% DB or less, VS1 is set to (1.28 × VC1 + 5.71) %DB or less.
如下進行控制器50中之各紅外線照射裝置51~54的溫度控 制。首先,根據成為產品之薄膜23的厚度、流延膜45的兩側緣部45a與中央部45b的厚度比率、流延時的濃液濃度、流延帶42的長度及行走速度的各種條件,事先求出剝取時的兩側緣部45a與中央部45b的殘留溶劑量及此時的各紅外線照射裝置51~54的溫度(以下,稱為控制溫度)。關於殘留溶劑量的計算,例如,測定剝取時的流延膜45的各部的厚度、及薄膜23的各部的厚度,依據該些測定結果,計算剝取時的流延膜45的各部的殘留溶劑量。例如能夠使用(株)KEYENCE製分光干涉式晶片厚度計SI-F80R測定剝取時的流延膜45的各部的厚度。薄膜23的各部的厚度能夠利用(株)小野測器的數字式線性規DG-525進行測定。控制器50以各紅外線照射裝置51~54的溫度成為由各種條件進行確定之控制溫度之方式控制各紅外線照射裝置51~54。 Temperature control of each of the infrared ray irradiation devices 51 to 54 in the controller 50 is performed as follows system. First, depending on the thickness of the film 23 to be the product, the thickness ratio of the side edge portions 45a of the casting film 45 to the center portion 45b, the concentration of the concentrated liquid which is delayed, the length of the casting tape 42, and the traveling speed, The amount of residual solvent of the both side edge portions 45a and the center portion 45b at the time of peeling and the temperature of each of the infrared ray irradiation devices 51 to 54 at this time (hereinafter referred to as control temperature) are obtained. For the calculation of the amount of the residual solvent, for example, the thickness of each portion of the casting film 45 at the time of peeling and the thickness of each portion of the film 23 are measured, and based on these measurement results, the residue of each portion of the casting film 45 at the time of peeling is calculated. The amount of solvent. For example, the thickness of each portion of the casting film 45 at the time of peeling can be measured using the spectral interference interferometer wafer thickness meter SI-F80R manufactured by KEYENCE Corporation. The thickness of each part of the film 23 can be measured by a digital linear gauge DG-525 of Ono Co., Ltd. The controller 50 controls each of the infrared irradiation devices 51 to 54 such that the temperature of each of the infrared irradiation devices 51 to 54 becomes a control temperature determined by various conditions.
如第2圖所示,在比流延模41更靠X方向上游側之滾筒43a的附近設置有剝取輥44。剝取輥44從流延帶42剝取被各紅外線照射裝置51~54照射紅外線而獲得自我支撐性之流延膜45。被剝取流延膜45之流延帶42向流延模41的下方移動,再次流延濃液18而作為支撐體發揮功能。 As shown in Fig. 2, a peeling roller 44 is provided in the vicinity of the drum 43a on the upstream side in the X direction from the casting die 41. The stripping roller 44 peels the casting film 45 which is irradiated with infrared rays by the respective infrared irradiation devices 51 to 54 from the casting tape 42 to obtain self-supporting properties. The casting tape 42 from which the casting film 45 is peeled off moves to the lower side of the casting die 41, and the dope 18 is cast again to function as a support.
滾筒43a、43b上連接有溫度調節裝置58。溫度調節裝置58中內置有調節傳熱介質的溫度之溫度調節部。溫度調節裝置58使調節為所希望的溫度之傳熱介質在溫度調節部與設置於滾筒43a、43b內之流路之間循環。藉由該傳熱介質的循環,流延帶42的溫度保持為所希望的溫度。 A temperature adjustment device 58 is connected to the drums 43a, 43b. A temperature adjustment unit that adjusts the temperature of the heat transfer medium is built in the temperature adjustment device 58. The temperature adjusting device 58 circulates the heat transfer medium adjusted to a desired temperature between the temperature adjusting portion and the flow path provided in the drums 43a, 43b. By the circulation of the heat transfer medium, the temperature of the casting belt 42 is maintained at a desired temperature.
並且,雖省略圖示,但是在流延帶42的內側設置有加熱器。該加熱器藉由加熱流延帶42,使溶劑從流延膜45蒸發,以此進行流延膜45的乾燥。 Further, although not shown, a heater is provided inside the casting belt 42. The heater dries the casting film 45 by heating the casting tape 42 to evaporate the solvent from the casting film 45.
流延膜形成裝置12上設置有排氣裝置59。排氣裝置59排出流延膜形成裝置12的氣氛。設置於流延膜形成裝置12的外部之未圖示之凝縮回收裝置凝縮被排出之氣氛中包含之溶劑氣體,並回收已凝縮之溶劑氣體。對於流延膜形成裝置12的氣氛中包含之溶劑氣體,凝縮回收裝置將流延膜形成裝置12內的氣氛中包含之容器基體的濃度保持為一定範圍。排氣裝置59藉由排出氣氛來控制流延膜形成裝置12內的氣體流動。 The casting film forming device 12 is provided with an exhausting device 59. The exhaust device 59 discharges the atmosphere of the cast film forming device 12. The condensing recovery device (not shown) provided outside the cast film forming apparatus 12 condenses the solvent gas contained in the discharged atmosphere, and recovers the condensed solvent gas. The condensate recovery device maintains the concentration of the container substrate contained in the atmosphere in the cast film forming device 12 within a certain range for the solvent gas contained in the atmosphere of the cast film forming apparatus 12. The exhaust device 59 controls the flow of the gas in the cast film forming device 12 by discharging the atmosphere.
(溶液製膜方法) (solution film forming method)
接著,對溶液製膜方法進行說明。以第1圖所示之溶液製膜設備10進行第6圖所示之溶液製膜方法。溶液製膜方法中依次進行流延膜形成製程71、具有側緣部乾燥製程72之流延膜乾燥製程73、剝取製程74及薄膜乾燥製程75。 Next, a solution film forming method will be described. The solution film forming method shown in Fig. 6 is carried out by the solution film forming apparatus 10 shown in Fig. 1. In the solution film forming method, a cast film forming process 71, a cast film drying process 73 having a side edge drying process 72, a stripping process 74, and a film drying process 75 are sequentially performed.
(流延膜形成製程) (cast film forming process)
如第2圖所示,藉由滾筒43a、43b的旋轉,流延帶42向X方向循環移動。流延帶42的移動速度例如為10m/分鐘以上150m/分鐘以下的範圍內,40m/分鐘以上120m/分鐘以下的範圍內為較佳。若從流延模41在流延帶42上流延濃液18,則形成沿X方向較長地延伸之帶狀流延膜45。如第3圖所示,狹縫出口41a的兩側緣部的間隙比中央部寬,因此,如第4圖所示,流延膜45中,自寬度方向的端部25mm的範圍之兩側緣部45a變得比中央部45b厚。 As shown in Fig. 2, the casting belt 42 is circulated in the X direction by the rotation of the rollers 43a and 43b. The moving speed of the casting belt 42 is, for example, in the range of 10 m/min or more and 150 m/min or less, and preferably 40 m/min or more and 120 m/min or less. When the dope 18 is cast on the casting tape 42 from the casting die 41, the tape-like casting film 45 which extends long in the X direction is formed. As shown in Fig. 3, the gap between the both side edges of the slit outlet 41a is wider than the central portion. Therefore, as shown in Fig. 4, the casting film 45 is on both sides of the range of 25 mm from the end portion in the width direction. The edge portion 45a becomes thicker than the central portion 45b.
(流延膜乾燥製程) (cast film drying process)
流延膜45藉由移動之流延帶42被傳送。如第5圖所示,側緣部用紅外線照射裝置51的紅外線加熱器51a朝向被傳送來之流延膜45 的兩側緣部45a照射紅外線。中央部用紅外線照射裝置53的紅外線加熱器53a朝向流延膜45的中央部45b照射紅外線。 The casting film 45 is conveyed by the moving casting tape 42. As shown in Fig. 5, the side edge portion is directed toward the conveyed casting film 45 by the infrared heater 51a of the infrared ray irradiation device 51. The both side edges 45a are irradiated with infrared rays. The central portion is irradiated with infrared rays toward the central portion 45b of the casting film 45 by the infrared heater 53a of the infrared irradiation device 53.
被各紅外線照射裝置51、53照射紅外線而進行乾燥之流延膜45藉由移動之流延帶42通過各紅外線照射裝置52、54的上方。各紅外線照射裝置52、54與各紅外線照射裝置51、53同樣地對流延膜45進行加熱。 The casting film 45 which is irradiated with infrared rays by the respective infrared irradiation devices 51 and 53 and dried is passed over the respective infrared irradiation devices 52 and 54 by the casting tape 42 which is moved. Each of the infrared irradiation devices 52 and 54 heats the casting film 45 in the same manner as each of the infrared irradiation devices 51 and 53.
紅外線加熱器51a~54a的溫度在100℃以上500℃以下的範圍內為較佳,100℃以上350℃以下的範圍內更為佳。紅外線的波長在0.8μm以上50μm以下的範圍內為較佳,2μm以上30μm以下的範圍內更為佳。側緣部用紅外線照射裝置51、52的紅外線加熱器51a、52a的溫度例如為180℃,中央部用紅外線照射裝置53、54的紅外線加熱器53a、54a的溫度結合紅外線加熱器51a、52a的溫度適當設定。本實施形態中,紅外線加熱器51a~54a照射波長在2μm以上30μm以下的範圍且4μm以上20μm以下的範圍比其他範圍更強地照射之紅外線。 The temperature of the infrared heaters 51a to 54a is preferably in the range of 100 ° C or more and 500 ° C or less, and more preferably in the range of 100 ° C or more and 350 ° C or less. The wavelength of the infrared ray is preferably in the range of 0.8 μm or more and 50 μm or less, and more preferably in the range of 2 μm or more and 30 μm or less. The temperature of the infrared heaters 51a and 52a of the side edge portion infrared irradiation devices 51 and 52 is, for example, 180° C., and the temperatures of the infrared heaters 53 a and 54 a of the central portion infrared irradiation devices 53 and 54 are combined with the infrared heaters 51 a and 52 a. The temperature is set appropriately. In the present embodiment, the infrared heaters 51a to 54a are irradiated with infrared rays having a wavelength in a range of 2 μm or more and 30 μm or less and a range of 4 μm or more and 20 μm or less more strongly than other ranges.
不銹鋼製流延帶42會反射紅外線,因此流延帶42的加熱受到抑制。並且,流延膜45易吸收紅外線。因此,在流延帶42的溫度上升受到抑制之狀態下流延膜45被加熱,溶劑從流延膜45蒸發,流延膜45被乾燥。流延膜45中,兩側緣部45a比中央部45b厚,但對該兩側緣部45a照射紅外線之紅外線加熱器51a、52a的溫度比對中央部45b照射紅外線之紅外線加熱器53a、54a高。藉此,流延膜45中,兩側緣部45a乾燥成與中央部45b大致相同。藉由該乾燥,剝取時的中央部殘留溶劑量VC1與側緣部殘留溶劑量VS1成為以下的關係範圍內。 The stainless steel casting tape 42 reflects infrared rays, so heating of the casting tape 42 is suppressed. Further, the casting film 45 easily absorbs infrared rays. Therefore, the casting film 45 is heated in a state where the temperature rise of the casting tape 42 is suppressed, the solvent evaporates from the casting film 45, and the casting film 45 is dried. In the casting film 45, the both side edge portions 45a are thicker than the center portion 45b, but the infrared ray heaters 51a and 52a that irradiate the infrared ray infrared heaters 51a and 52a on the both side edge portions 45a are irradiated with the infrared ray infrared heaters 53a and 54a at the center portion 45b. high. Thereby, in the casting film 45, both side edge portions 45a are dried to be substantially the same as the center portion 45b. By this drying, the amount of residual solvent VC1 at the center portion at the time of peeling and the residual solvent amount VS1 at the side edge portion are within the following relationship.
50%DB<VC1100%DB時,成為(VC1-15)VS1(0.96×VC1+25)的範圍內,20%DB<VC150%DB時,成為(0.85×VC1-7.86)VS1(1.28×VC1+5.71)的範圍內,VC120%DB時,成為VS1(1.28×VC1+5.71)的範圍內。 50%DB<VC1 When 100% DB, become (VC1-15) VS1 Within the range of (0.96 × VC1 + 25), 20% DB < VC1 When 50%DB, it becomes (0.85×VC1-7.86) VS1 Within the range of (1.28 × VC1 + 5.71), VC1 20% DB, become VS1 Within the range of (1.28 × VC1 + 5.71).
亦即,當VC1在大於50%DB且100%DB以下的範圍內時,VS1成為(VC1-15)%DB以上(0.96×VC1+25)%DB以下的範圍內,當VC1在大於20%DB且50%DB以下的範圍內時,VS1成為(0.85×VC1-7.86)%DB以上(1.28×VC1+5.71)%DB以下的範圍內,當VC1為20%DB以下時,VS1成為(1.28×VC1+5.71)%DB以下。 That is, when VC1 is in the range of more than 50% DB and 100% DB or less, VS1 becomes in the range of (VC1-15)%DB or more (0.96×VC1+25)%DB or less, when VC1 is greater than 20%. In the range of DB and 50% DB or less, VS1 is in the range of (0.85 × VC1 - 7.86) % DB or more (1.28 × VC1 + 5.71) % DB or less, and when VC1 is 20% DB or less, VS1 becomes (1.28). ×VC1+5.71)%DB or less.
(剝取製程) (stripping process)
剝取輥44將獲得自我支撐性之流延膜45作為濕潤膜19而從流延帶42剝取,經由過渡部21向夾子拉幅機13送出。 The peeling roller 44 peels the self-supporting casting film 45 as the wet film 19 from the casting tape 42, and sends it to the clip tenter 13 via the transition portion 21.
(薄膜乾燥製程) (film drying process)
夾子拉幅機13中,藉由夾子把持濕潤膜19的兩側緣部,對濕潤膜19送出規定的乾燥風,從而使溶劑從濕潤膜19蒸發。其結果,從濕潤膜19獲得薄膜23。剝取流延膜45時的中央部殘留溶劑量VC1及側緣部殘留溶劑量VS1成為上述的規定範圍內,因此剝取後的濕潤膜19的兩側緣部被充份乾燥,不會產生夾子的把持引起之咬碎。並且,還可防止薄膜23的厚度不均和拉伸不均。而且,自薄膜23的寬度方向的兩端25mm的範圍之兩側緣部的最大厚度TS與薄膜23的寬度方向中央部的最大厚度TC的關係成為1.1×TCTS。如此,濕潤膜19中兩側緣部形成為比中央部厚, 因此對於防止夾子的把持引起之咬碎更有效果。並且,由於兩側緣部變得較厚,因此不會發生夾子的咬入不良。另外,TS越是比TC厚,基於夾子之把持越穩定,但是考慮到基於流延模41之濃液18的流延或流延帶42上的流延膜45的形成的穩定化,TS5×TC為較佳,TS2×TC更為佳。 In the clip tenter 13, the both sides of the wet film 19 are gripped by the clips, and a predetermined dry air is sent to the wet film 19 to evaporate the solvent from the wet film 19. As a result, the film 23 is obtained from the wet film 19. When the casting film 45 is peeled off, the amount of residual solvent VC1 in the center portion and the residual solvent amount VS1 in the side edge portion are within the above-described predetermined ranges. Therefore, both side edges of the wet film 19 after peeling are sufficiently dried and do not occur. The grip of the clip causes the bite to break. Further, uneven thickness and uneven stretching of the film 23 can be prevented. In addition, the relationship between the maximum thickness TS of both side edges in the range of 25 mm from both ends in the width direction of the film 23 and the maximum thickness TC of the central portion in the width direction of the film 23 is 1.1 × TC. TS. As described above, the both side edges of the wet film 19 are formed thicker than the central portion, and therefore it is more effective in preventing the seizure caused by the gripping of the clip. Further, since the both side edges become thicker, the bite of the clip does not occur. Further, the TS is thicker than TC, and the more stable the grip is based on the grip, but considering the casting of the dope 18 based on the casting die 41 or the stabilization of the formation of the casting film 45 on the casting tape 42, TS 5 × TC is better, TS 2 × TC is better.
從夾子拉幅機13送出之薄膜23依次通過乾燥室15及冷卻室16,在各室中實施規定處理。對從冷卻室16送出至薄膜23依次實施基於除電棒29之除電處理及基於滾花賦予輥30之滾花賦予處理,並送出至捲取室17。送出至捲取室17之薄膜23被壓輥34按壓之同時捲取於捲芯35而成為捲狀,上述實施形態中,與兩側緣部45a同樣地藉由紅外線對成為流延膜45的產品之中央部45b進行乾燥,但中央部45b的乾燥方法並不限定於上述方法,可使用熱風乾燥、或基於設置於流延帶42內側之加熱器之經由流延帶42之加熱乾燥等進行乾燥。進行熱風乾燥時,減小乾燥風相對於流延膜45之相對速度,以避免流延膜45的表面起伏,從而避免出現厚度不均。 The film 23 fed from the clip tenter 13 passes through the drying chamber 15 and the cooling chamber 16 in order, and performs predetermined processing in each chamber. The discharge treatment from the cooling chamber 16 to the film 23 is sequentially performed by the static elimination treatment by the static elimination rod 29 and the knurling treatment by the knurling application roller 30, and is sent to the winding chamber 17. The film 23 that has been fed to the take-up chamber 17 is wound up by the pressure roller 34 and wound up in the winding core 35 to form a roll. In the above embodiment, the cast film 45 is formed by the infrared rays in the same manner as the both side edge portions 45a. The central portion 45b of the product is dried, but the drying method of the central portion 45b is not limited to the above method, and may be performed by hot air drying or by heating and drying by a casting belt 42 provided by a heater provided inside the casting belt 42. dry. When hot air drying is performed, the relative speed of the drying air with respect to the casting film 45 is reduced to avoid surface undulation of the casting film 45, thereby avoiding thickness unevenness.
上述實施形態中,藉由將流延模41的狹縫出口41a的兩側緣部的間隙形成為比中央部寬,使流延膜45的兩側緣部45a比中央部45b厚,但是如第7圖所示,亦可藉由連續流延來設置兩者的厚度差。此時,使濃液18從狹縫出口形成為直線狀之流延模100流向流延帶42來形成流延膜45,對該流延膜45的兩側緣部,從側緣部用流延模101流延濃液18,從而使流延膜45的兩側緣部45a比中央部45b厚。 In the above-described embodiment, the gap between the both side edges of the slit outlet 41a of the casting die 41 is formed to be wider than the central portion, so that both side edge portions 45a of the casting film 45 are thicker than the central portion 45b, but As shown in Fig. 7, the difference in thickness between the two can also be set by continuous casting. At this time, the casting die 100 in which the dope 18 is linearly formed from the slit outlet flows into the casting tape 42 to form the casting film 45, and the side edges of the casting film 45 are flowed from the side edge portion. The die 101 casts the dope 18 so that both side edge portions 45a of the casting film 45 are thicker than the center portion 45b.
如第8圖所示,亦可藉由從濃液供給噴嘴111向從流延模 100流出之濃液18的兩側緣部供給濃液18,使流延膜45的兩側緣部45a比中央部45b厚,以此代替上述連續流延。另外,關於如此追加之濃液(以下,稱為追加濃液)的合流,除了從流延液珠的側方進行之外,還可從流延液珠的前後方向中的任一方向或兩方向進行。而且,可適當組合基於狹縫間隙之側緣部加厚化、基於連續流延之側緣部加厚化、及基於向流延液珠的追加濃液合流之側緣部加厚化中的任一個來使流延膜45的兩側緣部45a比中央部45b厚。 As shown in Fig. 8, it can also be performed from the dope supply nozzle 111 to the slave casting die. The concentrated liquid 18 is supplied to both side edges of the concentrated liquid 18 flowing out of 100, and the both side edge portions 45a of the casting film 45 are made thicker than the central portion 45b instead of the above-described continuous casting. In addition, the confluence of the doped liquid (hereinafter referred to as additional dope) added may be carried out from the side of the casting bead, or from either of the front and rear directions of the casting bead or both. Direction. Further, it is possible to appropriately combine the thickening of the side edge portion based on the slit gap, the thickening of the side edge portion based on the continuous casting, and the thickening of the side edge portion based on the joining of the concentrated dope to the casting bead. Either the both side edge portions 45a of the casting film 45 are thicker than the center portion 45b.
上述實施形態中,控制器50分別以控制溫度將各紅外線照射裝置51~54的紅外線加熱器51a~54a的溫度設定為恆定。但是,並不限定於該方法。例如,如第9圖所示,除了藉由控制溫度的控制之外,還依據藉由第1流延膜厚度感測器121、第2流延膜厚度感測器122之厚度檢測結果,控制各紅外線照射裝置51~54來對流延膜45進行乾燥,以使剝取時的流延膜45的殘留溶劑量成為上述規定範圍內。此時,在滾筒43b的上方配設第1流延膜厚度感測器121,在滾筒43a的下方配設第2流延膜厚度感測器122。控制器50依據藉由各流延膜厚度感測器121、122之厚度檢測結果,計算剝取前的流延膜45的中央部45b的殘留溶劑量、及剝取前的流延膜45的兩側緣部45a的殘留溶劑量。依據該計算結果,控制器50控制各紅外線照射裝置51~54的紅外線加熱器51a~54a,使剝取時的中央部殘留溶劑量VC1及側緣部殘留溶劑量VS1成為上述規定範圍內。例如,流延膜45的厚度比規定值還增加時,藉由各流延膜厚度感測器121、122之檢測結果亦成為厚度增加之檢測結果。此時,若紅外線加熱器51a~54a的溫度仍為控制溫度,則中央部殘留溶劑量VC1及側緣部殘留溶劑量VS1脫離 上述規定範圍。為了防止該現象,控制器50依據藉由各流延膜厚度感測器121、122之檢測結果,提高紅外線加熱器51a~54a的溫度。流延膜厚度感測器為1個以上即可,並且可適當變更流延膜厚度感測器的檢測位置。 In the above embodiment, the controller 50 sets the temperatures of the infrared heaters 51a to 54a of the respective infrared irradiation devices 51 to 54 to be constant at the control temperature. However, it is not limited to this method. For example, as shown in FIG. 9, in addition to controlling the temperature, the thickness is detected by the thickness of the first cast film thickness sensor 121 and the second cast film thickness sensor 122. Each of the infrared irradiation devices 51 to 54 dries the casting film 45 so that the amount of residual solvent of the casting film 45 at the time of peeling is within the above-described predetermined range. At this time, the first cast film thickness sensor 121 is disposed above the drum 43b, and the second cast film thickness sensor 122 is disposed below the drum 43a. The controller 50 calculates the amount of residual solvent in the central portion 45b of the cast film 45 before stripping and the cast film 45 before stripping, based on the thickness detection results of the cast film thickness sensors 121 and 122. The amount of residual solvent on both side edges 45a. In accordance with the calculation result, the controller 50 controls the infrared heaters 51a to 54a of the respective infrared irradiation devices 51 to 54 so that the center portion residual solvent amount VC1 and the side edge portion residual solvent amount VS1 at the time of stripping are within the predetermined range. For example, when the thickness of the casting film 45 is increased more than a predetermined value, the detection result by each of the casting film thickness sensors 121 and 122 also becomes a detection result of an increase in thickness. At this time, if the temperature of the infrared heaters 51a to 54a is still the control temperature, the residual solvent amount VC1 at the center portion and the residual solvent amount VS1 at the side edge portion are separated. The above specified range. In order to prevent this, the controller 50 increases the temperatures of the infrared heaters 51a to 54a in accordance with the detection results of the respective cast film thickness sensors 121 and 122. The number of cast film thickness sensors may be one or more, and the detection position of the cast film thickness sensor can be appropriately changed.
上述實施形態中,作為流延膜45的支撐體使用捲繞於滾筒43a、43b之流延帶42,但是亦可將可旋轉之流延滾筒用作流延膜的支撐體,以此代替流延帶42。 In the above embodiment, the casting tape 42 wound around the rolls 43a and 43b is used as the support of the casting film 45. However, the rotatable casting roll may be used as the support of the casting film instead of the flow. Extending band 42.
上述實施形態中,藉由從各側緣部用紅外線照射裝置51、52的紅外線加熱器51a、52a照射之紅外線對流延膜45的兩側緣部45a進行加熱,但是亦可放射近紅外線來對流延膜45的兩側緣部45a進行加熱。並且,若能夠以輻射方式進行加熱,則可以使用其他方式的加熱器。 In the above-described embodiment, the both side edges 45a of the casting film 45 are heated by the infrared rays irradiated from the infrared heaters 51a and 52a of the infrared irradiation devices 51 and 52 at the respective side edges, but the near infrared rays may be convected. The both side edges 45a of the film 45 are heated. Further, if heating can be performed by radiation, other types of heaters can be used.
[實施例] [Examples]
以下,示出用於確認本發明的效果之實驗例,對本發明進行具體說明。但是,此處示出之例子僅僅是本發明之一例,並非限定本發明者。 Hereinafter, an experimental example for confirming the effects of the present invention will be described, and the present invention will be specifically described. However, the examples shown herein are merely examples of the invention and are not intended to limit the invention.
作為濃液18的原料,使用下述聚合物原料及溶劑原料。 As a raw material of the dope 18, the following polymer raw materials and solvent raw materials are used.
〔聚合物原料〕 [polymer raw material]
三醋酸纖維素 100質量份 Cellulose triacetate 100 parts by mass
磷酸三苯酯 7質量份 Triphenyl phosphate 7 parts by mass
磷酸聯苯基二苯酯 5.0質量份 Biphenyl diphenyl phosphate 5.0 parts by mass
〔溶劑原料〕 [solvent raw material]
二氯甲烷 92質量份 Dichloromethane 92 parts by mass
甲醇 8質量份 Methanol 8 parts by mass
將聚合物原料溶解於溶劑原料,製備固形物濃度為19.0質量%之濃液18。另外,上述三醋酸纖維素係取代度為2.84、黏度平均聚合度為306、含水率為0.2質量%、二氯甲烷溶液中的6質量%的黏度為315mPa.s、平均粒徑為1.5mm、標準偏差為0.5mm的粉體。並且,磷酸三苯酯及磷酸聯苯基二苯酯係增塑劑。本實施例中,使用對於所製備之濃液18,藉由靜置來進行脫泡,並使薄膜藉由送液泵經由者。 The polymer raw material was dissolved in a solvent raw material to prepare a dope 18 having a solid concentration of 19.0% by mass. Further, the cellulose triacetate has a degree of substitution of 2.84, a viscosity average degree of polymerization of 306, a water content of 0.2% by mass, and a viscosity of 6% by mass in a dichloromethane solution of 315 mPa. s, a powder having an average particle diameter of 1.5 mm and a standard deviation of 0.5 mm. Further, a triphenyl phosphate and a biphenyl diphenyl phosphate plasticizer. In the present embodiment, defoaming is carried out by standing for the prepared dope 18, and the film is passed through a liquid feeding pump.
使用第1圖的溶液製膜設備10,依次進行第6圖的流延膜形成製程71、具有側緣部乾燥製程72之流延膜乾燥製程73、剝取製程74、及薄膜乾燥製程75,製造中央部的最大厚度為40μm的薄膜23。將流延帶42的寬度設為2000mm,將流延膜45的寬度設為1500mm。並且,將流延帶42的行走速度設為80m/分鐘。 Using the solution film forming apparatus 10 of Fig. 1, the cast film forming process 71 of Fig. 6, the casting film drying process 73 having the side edge drying process 72, the stripping process 74, and the film drying process 75 are sequentially performed. A film 23 having a maximum thickness of 40 μm at the center portion was produced. The width of the casting tape 42 was set to 2000 mm, and the width of the casting film 45 was set to 1500 mm. Further, the running speed of the casting belt 42 was set to 80 m/min.
實施例1中,將自薄膜23的寬度方向兩端25mm範圍之兩側緣部的最大厚度TS設為46.8μm,將薄膜23的寬度方向中央部的最大厚度TC設為40μm,將剝取時的流延膜45的兩側緣部45a的殘留溶劑量VS1設為100%DB,且將剝取時的流延膜45的中央部45b的殘留溶劑量VC1設為110%DB將側緣部用紅外線照射裝置51、52的紅外線加熱器51a、52a的溫度設為180℃。將中央部用紅外線照射裝置53、54的紅外線加熱器53a、54a的溫度設為250℃。 In the first embodiment, the maximum thickness TS of both side edges in the range of 25 mm from both ends in the width direction of the film 23 is 46.8 μm, and the maximum thickness TC in the central portion in the width direction of the film 23 is 40 μm. The residual solvent amount VS1 of the both side edge portions 45a of the casting film 45 is set to 100% DB, and the residual solvent amount VC1 of the center portion 45b of the casting film 45 at the time of peeling is set to 110% DB. The temperatures of the infrared heaters 51a and 52a of the infrared irradiation devices 51 and 52 were set to 180 °C. The temperature of the infrared heaters 53a and 54a of the infrared irradiation devices 53 and 54 in the center portion was set to 250 °C.
實施例2~19、比較例1~17中,以表1所示之條件進行了實驗。其他條件設為與實施例1相同。將該實驗的結果示於表1及第10圖。表1的“咬碎”係以夾子拉幅機13的夾子把持濕潤膜19的兩側緣部時,是否產生了濕潤膜19破斷之咬碎,未產生咬碎時評價為A,產生咬碎時評 價為B。該判定藉由目視進行。並且,關於Re寬度方向變動量,遍及薄膜23的整個寬度,測定面內延遲Re,其變動量在±3nm的範圍內時評價為A,超過±3nm的範圍時評價為B。 In Examples 2 to 19 and Comparative Examples 1 to 17, experiments were carried out under the conditions shown in Table 1. Other conditions were set to be the same as in the first embodiment. The results of this experiment are shown in Table 1 and Figure 10. In the "crushing" of Table 1, when the both side edges of the wet film 19 were gripped by the clips of the clip tenter 13, whether or not the wetting of the wet film 19 was broken, and when it was not crushed, it was evaluated as A, and a bite was generated. Broken comment The price is B. This determination is made by visual inspection. In addition, the in-plane retardation Re was measured over the entire width of the film 23 in the Re width direction fluctuation amount, and was evaluated as A when the fluctuation amount was within a range of ±3 nm, and was evaluated as B when it exceeded a range of ±3 nm.
作為面內延遲Re的測定方法,以溫度25℃、濕度60%RH對樣品薄膜進行2小時的調濕,藉由以自動雙折射儀(KOBRA21ADH王子計測(株))從589.3nm中的垂直方向測定之延遲值的外插值按照下述公式進行計算。 As a method of measuring the in-plane retardation Re, the sample film was conditioned for 2 hours at a temperature of 25 ° C and a humidity of 60% RH, and the vertical direction of 589.3 nm was obtained by an automatic birefringence meter (KOBRA 21ADH Prince Measurement Co., Ltd.). The extrapolated value of the measured retardation value was calculated according to the following formula.
Re=|nX-nY|×d Re=|nX-nY|×d
nX表示X方向的折射率,nY表示Y方向的折射率,d表示薄膜的厚度(膜厚)。 nX represents the refractive index in the X direction, nY represents the refractive index in the Y direction, and d represents the thickness (film thickness) of the film.
第10圖中,橫軸設為中央部殘留溶劑量VC1,縱軸設為側緣部殘留溶劑量VS1,將實施例1~19、比較例1~17的實驗結果標會為二維曲線圖。第10圖中,針對實施例1~19的標會為“○”,針對比較例1~17的標會為“×”。以上限線L1及下限線L2表示當50<VC1100時為(VC1-15)VS1(0.96×VC1+25)、當20<VC150時為(0.85×VC1-7.86)VS1(1.28×VC1+5.71)、當VC120時為VS1(1.28×VC1+5.71)的各條件公式的上限值及下限值。 In Fig. 10, the horizontal axis represents the residual solvent amount VC1 at the center portion, and the vertical axis represents the residual solvent amount VS1 at the side edge portion. The experimental results of Examples 1 to 19 and Comparative Examples 1 to 17 are plotted as a two-dimensional graph. . In Fig. 10, the labels for Examples 1 to 19 were "○", and the labels for Comparative Examples 1 to 17 were "X". It is represented by the upper limit line L1 and the lower limit line L2 when 50<VC1 100 hours (VC1-15) VS1 (0.96×VC1+25), when 20<VC1 50 o'clock (0.85 × VC1 - 7.86) VS1 (1.28×VC1+5.71), when VC1 20 o'clock for VS1 The upper limit and lower limit of each conditional formula of (1.28 × VC1 + 5.71).
比較例1~4中,當50<VC1100時,並未滿足(VC1-15)VS1(0.96×VC1+25)。比較例1中,VS1為125%DB,VC1為100%DB,(0.96×VC1+25)為121%DB,並未滿足VS1(0.96×VC1+25)。同樣地,比較例3中,亦未滿足VS1(0.96×VC1+25)。因此,比較例1及3中,剝取後的濕潤膜19的側緣部並未被充份乾燥,產生了咬碎。 In Comparative Examples 1 to 4, when 50 < VC1 100 hours, not satisfied (VC1-15) VS1 (0.96 × VC1 + 25). In Comparative Example 1, VS1 is 125% DB, VC1 is 100% DB, and (0.96 × VC1+25) is 121% DB, which does not satisfy VS1. (0.96 × VC1 + 25). Similarly, in Comparative Example 3, VS1 was not satisfied. (0.96 × VC1 + 25). Therefore, in Comparative Examples 1 and 3, the side edge portion of the wet film 19 after peeling was not sufficiently dried, and seizure occurred.
比較例2中,VS1為80%DB,VC1為100%DB,(VC1-15)為85%DB,並未滿足(VC1-15)VS1。同樣地,比較例4中,亦未滿足(VC1-15)VS1。因此,比較例2及4中,在Re寬度方向變動量上超過了±3nm的範圍。 In Comparative Example 2, VS1 is 80% DB, VC1 is 100% DB, and (VC1-15) is 85% DB, which is not satisfied (VC1-15) VS1. Similarly, in Comparative Example 4, it was not satisfied (VC1-15). VS1. Therefore, in Comparative Examples 2 and 4, the amount of variation in the Re width direction exceeded the range of ±3 nm.
比較例5及6中,當20<VC150時,未滿足(0.85×VC1-7.86)VS1(1.28×VC1+5.71)。比較例5中,VS1為66%DB,VC1為45%DB(1.28×VC1+5.71)為63.31%DB,未滿足VS1(1.28×VC1+5.71)。因此,比較例5中產生了咬碎。比較例6中,VS1為28%DB,VC1為45%DB,(0.85×VC1-7.86)為30.39%DB,未滿足(0.85×VC1-7.86)VS1。因此,比較例6中,在Re寬度方向變動量上超過了±3nm的範圍。 In Comparative Examples 5 and 6, when 20 < VC1 At 50 o'clock, it is not satisfied (0.85×VC1-7.86) VS1 (1.28 × VC1 + 5.71). In Comparative Example 5, VS1 was 66% DB, and VC1 was 45% DB (1.28 × VC1 + 5.71) was 63.31% DB, which did not satisfy VS1. (1.28 × VC1 + 5.71). Therefore, bite was produced in Comparative Example 5. In Comparative Example 6, VS1 was 28% DB, VC1 was 45% DB, and (0.85×VC1-7.86) was 30.39% DB, which was not satisfied (0.85×VC1-7.86). VS1. Therefore, in Comparative Example 6, the amount of variation in the Re width direction exceeded the range of ±3 nm.
比較例7中,當20VC1時,並未滿足VS1(1.28×VC1+5.71),因此產生了咬碎。 In Comparative Example 7, when 20 VC1 did not satisfy VS1 (1.28 × VC1 + 5.71), so there is a bite.
比較例8、9、14、15中,當50<VC1100時,亦未滿足(VC1-15)VS1(0.96×VC1+25)。並且,比較例10~13、16、17中,當20<VC150時,並未滿足(0.85×VC1-7.86)VS1(1.28×VC1+5.71)。因此,比較例8~17中,產生咬碎,或者在Re寬度方向變動量上超過了±3nm的範圍。 In Comparative Examples 8, 9, 14, and 15, when 50 < VC1 At 100 o'clock, it is not satisfied (VC1-15) VS1 (0.96 × VC1 + 25). Also, in Comparative Examples 10 to 13, 16, and 17, when 20 < VC1 At 50 o'clock, it was not satisfied (0.85×VC1-7.86) VS1 (1.28 × VC1 + 5.71). Therefore, in Comparative Examples 8 to 17, the chipping occurred or the range of variation in the Re width direction exceeded the range of ±3 nm.
相對於此,實施例1中,當50<VC1100時,滿足(VC1-15)VS1(0.96×VC1+25)。實施例1中,VS1為110%DB,VC1為100%DB,(VC1-15)為85%DB,(0.96×VC1+25)為121%DB,滿足(VC1-15)VS1(0.96×VC1+25)。藉此,剝取後的濕潤膜19的兩側緣部被充份乾燥,並未產生咬碎。並且,Re寬度方向變動量為±3nm的範圍內。 In contrast, in Embodiment 1, when 50 < VC1 100 hours, satisfied (VC1-15) VS1 (0.96 × VC1 + 25). In the first embodiment, VS1 is 110% DB, VC1 is 100% DB, (VC1-15) is 85% DB, and (0.96×VC1+25) is 121% DB, which satisfies (VC1-15) VS1 (0.96 × VC1 + 25). Thereby, both edge portions of the wet film 19 after peeling were sufficiently dried, and no seizure occurred. Further, the amount of change in the Re width direction is within a range of ±3 nm.
實施例2~4、9、10、15、16中,當50<VC1100時,滿足(VC1-15)VS1(0.96×VC1+25),與實施例1同樣地,未產生咬碎,Re寬度方向變動量亦在±3nm的範圍內。 In Examples 2 to 4, 9, 10, 15, and 16, when 50 < VC1 100 hours, satisfied (VC1-15) VS1 (0.96 × VC1 + 25), as in the case of Example 1, no seizure occurred, and the amount of change in the Re width direction was also within the range of ±3 nm.
實施例5、6、11~14、17、18中,當20<VC150時,滿足(0.85×VC1-7.86)VS1(1.28×VC1+5.71)。藉此,實施例5、6、11~14、17、18中,未產生咬碎,Re寬度方向變動量在±3nm的範圍內。 In Examples 5, 6, 11~14, 17, and 18, when 20<VC1 50 o'clock, satisfied (0.85 × VC1 - 7.86) VS1 (1.28 × VC1 + 5.71). As a result, in Examples 5, 6, 11 to 14, 17, and 18, no chipping occurred, and the amount of change in the Re width direction was within a range of ±3 nm.
實施例7、8、19中,當VC120時,滿足VS1(1.28×VC1+5.71)。藉此,實施例7、8、19中,未產生咬碎,Re寬度方向變動量為±3nm的範圍內。 In Embodiments 7, 8, and 19, when VC1 20 o'clock, meet VS1 (1.28 × VC1 + 5.71). As a result, in Examples 7, 8, and 19, no chipping occurred, and the amount of change in the Re width direction was within a range of ±3 nm.
如上述,若剝取時的流延膜45的兩側緣部45a的殘留溶劑 量VS1、與剝取時的流延膜45的中央部45b的殘留溶劑量VC1滿足當50<VC1100時為(VC1-15)VS1(0.96×VC1+25)、當20<VC150時為(0.85×VC1-7.86)VS1(1.28×VC1+5.71)、當VC120時為VS1(1.28×VC1+5.71),則不會產生咬碎,Re寬度方向變動量亦為±3nm的範圍內,能夠製造無厚度不均和拉伸不均之薄膜23。 As described above, the residual solvent amount VS1 of both side edge portions 45a of the casting film 45 at the time of peeling and the residual solvent amount VC1 of the center portion 45b of the casting film 45 at the time of peeling satisfy the condition of 50 < VC1. 100 hours (VC1-15) VS1 (0.96×VC1+25), when 20<VC1 50 o'clock (0.85 × VC1 - 7.86) VS1 (1.28×VC1+5.71), when VC1 20 o'clock for VS1 (1.28 × VC1 + 5.71), the chipping is not caused, and the amount of change in the Re width direction is also within a range of ± 3 nm, and the film 23 having no thickness unevenness and uneven stretching can be produced.
如第10圖所示,上限線L1在50<VC1100時的傾斜度小於20<VC150時的傾斜度。若使50<VC1100時的傾斜度等於20<VC150時的傾斜度,則中央部殘留溶劑量VC1為100%DB時,側緣部殘留溶劑量VS1超過130%DB,產生咬碎。本發明中,藉由使50<VC1100時的傾斜度小於20<VC150時的傾斜度,防止咬碎。並且,下限線L2在50<VC1100時的傾斜度大於20<VC150時的傾斜度。若使50<VC1100時的傾斜度等於20<VC150時的傾斜度,則與下限線L2相比,中央部殘留溶劑量VC1與側緣部殘留溶劑量VS1之差變大,在Rc寬度方向變動量上超過±3nm的範圍。本發明中,藉由使50<VC1100時的傾斜度大於20<VC150時的傾斜度,使Re寬度方向變動量成為±3nm的範圍內。 As shown in Figure 10, the upper limit line L1 is at 50 < VC1 100 degrees inclination is less than 20<VC1 50 degrees of inclination. If 50<VC1 The inclination at 100 o'clock is equal to 20<VC1 When the amount of residual solvent VC1 in the center portion is 100% DB, the amount of residual solvent VS1 in the side edge portion exceeds 130% DB, and seizure occurs. In the present invention, by making 50<VC1 100 degrees inclination is less than 20<VC1 50 degrees of inclination to prevent chipping. And, the lower limit line L2 is at 50 < VC1 100 degrees inclination is greater than 20<VC1 50 degrees of inclination. If 50<VC1 The inclination at 100 o'clock is equal to 20<VC1 When the inclination is 50 degrees, the difference between the center portion residual solvent amount VC1 and the side edge portion residual solvent amount VS1 is larger than the lower limit line L2, and the amount of variation in the Rc width direction exceeds ±3 nm. In the present invention, by making 50<VC1 100 degrees inclination is greater than 20<VC1 The inclination at 50 o'clock was such that the amount of change in the Re width direction was within a range of ±3 nm.
51‧‧‧側緣部用紅外線照射裝置(側緣部乾燥部) 51‧‧‧Infrared irradiation device for side edge (drying part at side edge)
51a‧‧‧紅外線加熱器 51a‧‧‧Infrared heater
53‧‧‧中央部用紅外線照射裝置 53‧‧‧The central part uses infrared radiation
53a‧‧‧紅外線加熱器 53a‧‧‧Infrared heater
45‧‧‧流延膜 45‧‧‧cast film
45a‧‧‧兩側緣部 45a‧‧‧ both sides
45b‧‧‧中央部 45b‧‧‧Central Department
42‧‧‧流延帶(支撐體) 42‧‧‧casting belt (support)
52‧‧‧側緣部用紅外線照射裝置(側緣部乾燥部) 52‧‧‧Infrared irradiation device for side edge (drying part at side edge)
52a‧‧‧紅外線加熱器 52a‧‧‧Infrared heater
54‧‧‧中央部用紅外線照射裝置 54‧‧‧The central part uses infrared radiation
54a‧‧‧紅外線加熱器 54a‧‧‧Infrared heater
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| KR101655735B1 (en) * | 2009-03-31 | 2016-09-08 | 후지필름 가부시키가이샤 | Solution film-forming method |
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