KR20170009624A - Cellulose ester phase difference film having superior optical reliableness - Google Patents

Cellulose ester phase difference film having superior optical reliableness Download PDF

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KR20170009624A
KR20170009624A KR1020150101951A KR20150101951A KR20170009624A KR 20170009624 A KR20170009624 A KR 20170009624A KR 1020150101951 A KR1020150101951 A KR 1020150101951A KR 20150101951 A KR20150101951 A KR 20150101951A KR 20170009624 A KR20170009624 A KR 20170009624A
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film
carbon atoms
cellulose ester
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phase difference
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KR101716118B1 (en
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김영수
김경수
김용원
하선영
이유미
이호준
강혁모
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주식회사 효성
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    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00Optical elements other than lenses
    • G02B5/30Polarising elements
    • G02B5/3083Birefringent or phase retarding elements
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B3/00Preparation of cellulose esters of organic acids
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18Manufacture of films or sheets
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L1/00Compositions of cellulose, modified cellulose or cellulose derivatives
    • C08L1/08Cellulose derivatives
    • C08L1/10Esters of organic acids, i.e. acylates
    • GPHYSICS
    • G02OPTICS
    • G02FOPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/13Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on liquid crystals, e.g. single liquid crystal display cells
    • G02F1/133Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
    • G02F1/1333Constructional arrangements; Manufacturing methods
    • G02F1/1335Structural association of cells with optical devices, e.g. polarisers or reflectors

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Abstract

The present invention relates to a cellulose ester phase difference film. More specifically, the present invention relates to a cellulose ester phase difference film which comprises a resin and an additive to improve reliability under high temperature and humidity conditions and thus enables manufacture of a polarizing plate with improved reliability.

Description

[0001] The present invention relates to a cellulose ester phase difference film having excellent optical reliability,

The present invention relates to a cellulose ester phase difference film, and more particularly, to a cellulose ester phase difference film capable of producing a polarizing plate having improved reliability by including a resin capable of improving high temperature and high humidity reliability and an additive.

In recent years, the development of thin and lightweight notebook computers is under way. Accordingly, a protective film of a polarizing plate used in a display device such as a liquid crystal display device has been increasingly demanded for further thinning and higher performance. Since a liquid crystal display device displays a display by polarization control by a liquid crystal, a polarizing plate is required, and a polarizing plate in which a PVA film containing iodine is stretched is usually used. Since the polarizing plate is fragile, a polarizing plate protective film is used to protect the polarizing plate. In general, triacetylcellulose film is widely used for a polarizing plate protective film. In addition to these polarizing plate protective films, a retardation film is also used to control the retardation of the polarized light. The retardation film used liquid crystal display device or the like may be used in order to solve the problems such as color compensation and wide viewing angle by using a retardation (R th) in the thickness direction by the use in combination with a polarizing plate, and the phase difference in-plane direction (R o) May have a function of converting linearly polarized light into circularly polarized light with respect to the wavelength of the visible light region or conversely converting circularly polarized light into linearly polarized light.

The polarizing plate protective film is intended to protect the polarizing plate and it is most preferable to use a film made of cellulose acetate in order to protect the polarizing plate made of PVA containing moisture, considering the production process of the polarizing plate. On the other hand, as a retardation film, materials other than cellulose acetate have been used to exhibit optical performance. That is, conventionally, as a material of the retardation film, for example, there are polycarbonate, polysulfone, polyethersulfone, amorphous polyolefin and the like. These polymer films have such characteristics that the longer the wavelength is, the smaller the retardation, and it is difficult to impart an ideal retardation property to the entire wavelength of the visible light region.

In the case where linearly polarized light is converted into circularly polarized light with respect to the wavelength of the visible light region or conversely circularly polarized light is converted into linearly polarized light, in order to obtain the above effect with one piece of retardation film, the retardation in the wavelength? 4 < / RTI > Such a retardation film can be obtained by using, for example, a retardation film having a phase difference of? / 4 and only one polarizing plate for a reflective liquid crystal display device having a back electrode as a reflective electrode, thereby obtaining a reflective display device having excellent image quality . Further, with respect to the observer of the guest-host type liquid crystal layer, the retardation film is used on the back side, or the circularly polarized light of the reflection type polarizing plate composed of cholesteric liquid crystal or the like that reflects only one of the left and right circularly polarized light is converted into linearly polarized light It is also used as an element.

Further, the retardation film has a function of converting linearly polarized light into elliptically polarized light or circularly polarized light, or converting linearly polarized light in a certain direction into another direction, and therefore, the viewing angle, contrast, etc. of the liquid crystal display device can be improved .

Generally, a retardation film is attached to a pair of polarizing plates, respectively. At present, N-TAC of Konica Minolta Holdings, Inc. of Japan is generally used as a phase difference film for a VA mode liquid crystal display. The NTAC retardation film was a cellulose acetate propionylate (CAP) having a retardation in the plane of 50 nm (retardation (R 0 , relative to λ = 550 nm) and a retardation in the thickness direction (R th , ) Film.

In order to improve the viewing angle characteristics (black display state (black characteristic), etc.) of the liquid crystal display device, wavelength dispersion and control techniques are required. In general, the N-TAC film exhibits an inverse wavelength dispersion characteristic in which the retardation value increases with increasing wavelength, and exhibits an excellent viewing angle characteristic improvement effect as compared with the retardation film having a regular wavelength dispersion characteristic in which the retardation value decreases with increasing wavelength. Further, in order to improve a liquid crystal display device, a retardation film having a specific retardation value and a combination thereof are used.

Conventional retardation films (PC, PSu, PA, etc.) have such characteristics that the longer the wavelength is, the smaller the retardation. It is difficult to impart an ideal retardation characteristic to the entire wavelength of the visible light region. So that necessary performance is obtained. In order to achieve such a performance in one phase difference film, it is preferable that the in-plane direction retardation (R o ) at the wavelength λ incident on the retardation film is λ / 4, Plane directional phase difference (R o ) increases as the wavelength becomes longer. In the film made of cellulose acetate, if such a retardation property can be given, the polarizing plate protective film and the retardation film can be used together, the retardation film composed of a plurality of retardation films can be omitted, It is possible to improve the total light transmittance.

With respect to this problem, Japanese Patent Laid-Open No. 2000-137116 proposes to use an oriented film of cellulose acetate having a degree of substitution (acetylation degree) of 2.5 to 2.8 as a retardation film. According to this method, the longer the wavelength, the larger the phase difference, and the ideal phase difference characteristic is obtained with respect to the entire wavelength of the visible light region. That is, the above-mentioned patent discloses a phase difference plate in which the phase difference becomes smaller as the measurement wavelength becomes shorter with one film. A retardation film comprising a polymeric orientation film having a longer birefringence (? N) at a wavelength of 400 to 700 nm, wherein the polymeric orientation film is an orientation film of a polymeric film having an average refractive index at the above- And the like. As a means for solving this problem, a technique of orienting cellulose acetate having an acetylation degree of 2.5 to 2.8 by stretching is disclosed.

In the embodiment of the above-mentioned patent, 100 parts by weight of cellulose triacetate having an intrinsic viscosity [?] = 1.335 and an acetylation degree of 2.917 obtained from Wako Junyaku Kogyo Co., Ltd. was dissolved in 500 parts by weight of methylene chloride, Hydrolysis of cellulose triacetate with acetic acid and water at 70 DEG C for 100 minutes while removing methylene chloride by depressurization and the reaction product was precipitated with a large amount of water and washed and dried , And a cellulose acetate having an acetylation degree of 2.661 was obtained. Then, a film was prepared from a solution prepared by dissolving 100 parts by weight of this polymer and 3 parts by weight of dibutyl phthalate as a plasticizer in 700 parts by weight of a mixed solvent of methylene chloride / methanol (weight ratio 9/1) by solvent casting method, And uniaxially stretched at a temperature of 170 캜 at 1.5 times. That is, in Embodiment 1 of the patent, the retardation film having the same wavelength characteristics (wavelength dispersion characteristics) as the latter is obtained by stretching. It is also disclosed that by adjusting the retardation value, it is possible to use? / 4 or another retardation film. In Example 4 of the aforementioned patent, cellulose acetate having an acetylation degree of 2.421 was obtained. When the retardation property of the film using the film is measured, the retardation is insufficient when the film thickness is about 100 mu m (50 to 150 mu m) and when the film thickness is preferable as the self-supporting film. Further, when thick enough and has a film thickness 200㎛ over to, the retardation (R th) in the thickness direction at the time to provide a desired phase difference of about 80 to 150nm is more than 350nm, in the field of view when functioning as a λ / 4 phase difference film It did not function as an enlarged film and was not sufficient. Furthermore, the molecular weight distribution of the obtained cellulose acetate is not described, and the control of the retardation characteristics by controlling the molecular weight distribution is not described or suggested.

On the other hand, although the protective film of the polarizer PVA layer of the polarizing plate was produced by using materials such as TAC and acrylic, the raw materials added to the CAP, COP, and TAC at the time of manufacturing the retardation film are expensive, .

In addition, the cellulose-based polarizing plate made of the conventional retardation film has a low resistance to high temperature and high humidity environment, and the water resistance property of the film is deteriorated when exposed to a high temperature and high humidity reliability environment, thereby deteriorating the reliability quality of the polarizing plate and LCD.

Disclosure of Invention Technical Problem [8] Accordingly, the present invention has been made keeping in mind the above problems occurring in the prior art, and an object of the present invention is to provide a cellulose ester phase difference film capable of improving reliability quality in the production of a polarizing plate by including a resin and additives capable of improving high- .

In order to achieve the above object, the present invention provides a cellulose ester having an acetyl group degree of substitution in a range of 2.70 to 2.95, an asymmetric ester compound having an aromatic group represented by the following formulas (1) and (2) The present invention provides a cellulose ester phase difference film comprising a terminal symmetrical aliphatic compound.

[Chemical Formula 1]

M A - [D O - D A] n - D B

(2)

M A - [D O - D A] n - D O

(Wherein, M A: R 1 -COOH, D O: HO-R 2 -OH, D A: HOOC-R 1 -COOH, D B: a HO-R 3 -OH, R 1 is aryl having 6 or more R 2 is a compound having 2 to 6 carbon atoms, propylene glycol, and R 3 is a compound having 2 to 12 carbon atoms, which is an adipic acid residue or an aliphatic carboxylic acid residue or an akylene dicarboxylic acid residue, and n represents an integer of 1 or more.

(3)

I - (T) n - I

(Wherein I represents an ester group having 1 to 20 carbon atoms, an alkoxycarbonyl group having 1 to 20 carbon atoms, an amide group having 1 to 20 carbon atoms, a carbamoyl group having 1 to 20 carbon atoms, a hydroxy group, T is a 2,2,4-trimethyl-1,3-pentanylene group, or a divalent saturated bridging group having 0 to 40 carbon atoms and 0 to 20 carbon atoms, and the number of atoms is 0 Means that the groups at both ends of the linkage form a single bond directly, and N represents an integer of 1 or more.

The cellulose ester phase difference film preferably has an effective retardation value Reff defined by the following formula (1) measured under the conditions of 23 ° C and 55% RH within a range of ± 30 nm.

[Equation 1]

Reff = (nx'-ny ') xd

(Where d is the thickness (nm) of the film, nx 'and ny' are the effective refractive index values formed from nx, ny and nz when observed at the positions of? = 45 ° and? to be.)

Further, it is preferable that the cellulose ester phase difference film is allowed to stand for 500 hours in a high-temperature and high-humidity chamber at 60 DEG C and 90% RH in a reliable environment, and then the change amount DELTA Reff of Reff is within a range of +/- 10 nm.

The present invention having such a constitution can improve the reliability quality of the cellulose ester phase difference film of the present invention when the polarizing plate is manufactured by including the resin and the additive which can improve the high temperature and high humidity reliability.

Fig. 1 is a view showing effective refractive index values of the effective surface area formed from nx, ny and nz when observed at the positions of [theta] = 45 [deg.] And [Phi] = 45 [
2 is a view showing a process for producing a cellulose ester according to the present invention.

Hereinafter, the present invention will be described in more detail with reference to the following examples, but the scope of the present invention is not limited thereto.

The cellulose ester phase difference film according to the present invention is characterized in that the effective retardation value Reff defined by the following formula (1) measured under the conditions of 23 ° C and 55% RH is within ± 30 nm.

[Equation 1]

Reff = (nx'-ny ') xd

(Where d is the thickness (nm) of the film, nx 'and ny' are the effective refractive index values formed from nx, ny and nz when observed at the positions of? = 45 ° and? to be.)

Here, the cellulose ester phase difference film may be a cellulose ester having an acetyl group degree of substitution in the range of 2.70 to 2.95, an asymmetric ester compound having an aromatic group represented by the following formulas (1) and (2) and a terminal symmetrical aliphatic compound And a control unit.

[Chemical Formula 1]

M A - [D O - D A] n - D B

(2)

M A - [D O - D A] n - D O

(Wherein, M A: R 1 -COOH, D O: HO-R 2 -OH, D A: HOOC-R 1 -COOH, D B: a HO-R 3 -OH, R 1 is aryl having 6 or more R 2 is a compound having 2 to 6 carbon atoms, propylene glycol, and R 3 is a compound having 2 to 12 carbon atoms, which is an adipic acid residue or an aliphatic carboxylic acid residue or an akylene dicarboxylic acid residue, and n represents an integer of 1 or more.

(3)

I - (T) n - I

(Wherein I represents an ester group having 1 to 20 carbon atoms, an alkoxycarbonyl group having 1 to 20 carbon atoms, an amide group having 1 to 20 carbon atoms, a carbamoyl group having 1 to 20 carbon atoms, a hydroxy group, T is a 2,2,4-trimethyl-1,3-pentanylene group, or a divalent saturated bridging group having 0 to 40 carbon atoms and 0 to 20 carbon atoms, and the number of atoms is 0 Means that the groups at both ends of the linkage form a single bond directly, and N represents an integer of 1 or more.

Meanwhile, the cellulose ester phase difference film according to the present invention can be produced by solution casting method. In the solution film forming method, the cellulose ester is dissolved in an additive such as a plasticizer, a UV absorber, a matting agent, etc. and a mixed solvent such as methylene chloride and methanol to prepare a dope, which can be filtered using a filtration apparatus.

In the present invention, the molecular weight range of the cellulose ester is not limited, but the weight average molecular weight is preferably in the range of 150,000 to 220,000.

By reducing the molecular weight to a certain level or more, the strength of the film can be effectively prevented from being lowered.

Further, by keeping the molecular weight at a certain level or less, the viscosity of the cellulose ester solution (dope) is maintained at a certain level or less, thereby facilitating film production by solution casting method.

The degree of molecular weight dispersion (weight average molecular weight Mw / number average molecular weight Mn) of the cellulose ester is preferably in the range of 2.5 to 4.5.

When a film is produced by a solution film forming method (or a solvent casting method), an organic solvent is preferable as the solvent for preparing the cellulose ester composition (dope). As the organic solvent, it is preferable to use halogenated hydrocarbons, and halogenated hydrocarbons include chlorinated hydrocarbons, methylene chloride and chloroform, among which methylene chloride is most preferred.

If necessary, organic solvents other than halogenated hydrocarbons may be mixed and used. Organic solvents other than halogenated hydrocarbons include esters, ketones, ethers, alcohols and hydrocarbons. Examples of the ester include methyl formate, ethyl formate, propyl formate, pentyl formate, methyl acylate, ethyl acylate, and pentaacetate. Examples of the ketone include acetone, methyl ethyl ketone, diethyl ketone, di Isobutyl ketone, cyclopentanone, cyclohexanone, methylcyclohexanone and the like can be used. As the ether, diisopropyl ether, dimethoxymethane, dimethoxyethane, 1,4-dioxane, Ethanol, 1-propanol, 2-propanol, 1-butanol, 2-butanol, t-butanol, 1-pentanol, 2-butanol and the like can be used. Methyl-2-butanol, cyclohexanol, 2-fluoroethanol, 2,2,2-trifluoroethanol and 2,2,3,3-tetrafluoro-1-propanol.

More preferably, methylene chloride may be used as the main solvent, and alcohol may be used as the minor solvent. Specifically, methylene chloride and alcohol may be mixed at a weight ratio of 80:20 to 95: 5.

The cellulose ester composition can be prepared by room temperature, high temperature or low temperature dissolution.

Next, the additives used in the production of the cellulose ester film will be explained. The cellulose ester solution (dope) used in the solution softening method may contain various additives depending on the application in each preparation step such as a plasticizer, a deterioration inhibitor, a matte fine particle, a stripper, a UV stabilizer, an ultraviolet absorber, An additive such as a dispersing agent, an optical anisotropy adjusting agent and the like may be added. The specific kind of such additives can be used without limitation as long as they are commonly used in the field, and the content thereof is preferably used within a range that does not deteriorate the physical properties of the film. The timing of adding the additives depends on the type of additive. A step of adding an additive to the end of the doping treatment may be performed.

The cellulose ester phase difference film is characterized in that the amount of change Reff of Reff is within a range of 10 nm or less after being left in a high temperature and high humidity chamber for 60 hours at a temperature of 60 DEG C and a 90% RH reliability environment.

On the other hand, the cellulose ester film contains a plasticizer for improving mechanical strength, good castability, imparting water absorbency, and reducing water permeability. As the plasticizer, any conventionally used plasticizer can be used without limitation. For example, carboxylic acid esters selected from phosphoric acid esters, phthalic acid esters or citric acid esters and the like can be used. In the present invention, the asymmetric Type ester plasticizer is particularly preferred in order to set the optical reliability characteristics of the cellulose ester film before and after the reliability treatment to a predetermined range.

Hereinafter, specific compounds of the asymmetric ester compounds containing an aromatic group according to the present invention are shown through the following formulas (4) to (9), but the present invention is not limited thereto.

[Chemical Formula 4]

Figure pat00001

[Chemical Formula 5]

Figure pat00002

[Chemical Formula 6]

Figure pat00003

(7)

Figure pat00004

[Chemical Formula 8]

Figure pat00005

[Chemical Formula 9]

Figure pat00006

Further, specific compounds of the aliphatic-containing symmetrical ester compounds used in the embodiment of the present invention are shown by the following formula (10), but the present invention is not limited thereto.

[Chemical formula 10]

Figure pat00007

The cellulose ester solution thus obtained is cast on a support through a casting die to form a cellulose ester sheet.

The cellulose ester sheet thus formed is subjected to a stretching step in a tenter. In the preheating step, the glass transition temperature (Tg) of the cellulose ester flake is 185 to 200 ° C, the glass transition temperature (Tg) of the retardation film is 150 to 190 Lt; / RTI >

The cellulose ester film of the present invention may be completed in a drying process in a dryer after removing the left and right ends of a film whose surface is damaged by a clip or pin of a tenter after being subjected to a stretching step in a tenter under the above conditions.

Hereinafter, the present invention will be described in more detail with reference to the following examples, but the scope of the present invention is not limited thereto.

Example  One

≪ Step 1 > Cellulose solution ( Lead juice )

Triacetylcellulose having an average degree of acetyl substitution (DS) of 2.86 was used for the cellulose ester, and as the plasticizer, a terminal asymmetric aromatic plasticizer 1 (A) represented by the following formula, a terminal asymmetric aromatic plasticizer 2 (B) and a terminal symmetric aliphatic plasticizer 1 (C) were mixed to prepare a cellulose solution.

Terminal asymmetric aromatic plasticizer 1 (A) =

Figure pat00008

Terminal asymmetric aromatic plasticizer 2 (B) =

Figure pat00009

Terminal symmetrical aliphatic plasticizer 1 (C) =

Figure pat00010

<Step 2> Preparation of Dilute Solution Containing Metal Oxide

20.0 parts by weight of the cellulose solution prepared in <Step 1>, 1.5 parts by weight of silica (SiO2), and 78.5 parts by weight of a mixed solvent obtained by mixing 9: 1 (by weight) of methylene chloride and methanol were added to a mixing tank, ) Was prepared. &Lt; tb &gt; &lt; TABLE &gt;

&Lt; Step 3 > Preparation of cellulose ester film

100 parts by mass of the initiator solution and 5 parts by mass of the fine particle additive solution were added, and sufficiently mixed with an inline mixer to prepare a dope. The composition of the dope was 72 wt% of methylene chloride, 8 wt% of methanol, 17.95 wt% of triacetylcellulose (TAC), 2 wt% of plasticizer (A + B + C), and 0.05 wt% of silica. Thereafter, the belt was softened uniformly on a stainless steel band support having a width of 2000 mm by using a flexible machine. Then, the solvent was evaporated on the stainless band support to peel off from the stainless band support. Then, both ends of the web were gripped with a tenter and stretched so that the stretching magnification in the (TD) direction in the temperature environment of 170 ° C was 1.1 times. Thereafter, the stretching was maintained for a few seconds while maintaining the width, , And the film was transported for 35 minutes in a drying zone set at 110 캜 for drying for 35 minutes to produce a cellulose ester film having a thickness of 20 탆 and a knurling width of 1900 mm and a width of 10 mm and a height of 8 탆 at the end.

Example  2

A cellulose ester film was produced in the same manner as in Example 1 except that the film thickness was changed to 25 탆.

Example  3

A cellulose ester film was produced in the same manner as in Example 1 except that the film thickness was changed to 30 탆.

Example  4

A cellulose ester film was produced in the same manner as in Example 1 except that the film thickness was changed to 40 탆.

Comparative Example  One

(C) of the terminal symmetrical aliphatic plasticizer 1 (C) and the terminal symmetrical aromatic plasticizer 1 (D) represented by the following formula was used as a plasticizer and the film thickness was made to be 40 탆. Was carried out to prepare a cellulose ester film.

End symmetrical aromatic plasticizer 1 (D) =

Figure pat00011

Comparative Example  2

(C) of the terminal symmetrical aliphatic plasticizer 1 (C) and a terminal symmetrical aromatic plasticizer 2 (E) represented by the following formula was used as a plasticizer, and the film thickness was made to be 40 탆. Was carried out to prepare a cellulose ester film.

Terminal symmetrical aromatic plasticizer 2 (E) =

Figure pat00012

Experimental Example

The cellulose ester film prepared in each of Examples 1 to 4 and Comparative Examples 1 and 2 was measured with an optical measuring instrument of AxoScan (OPMF-1, Axometrics) under the environment of 23 ° C and 55% RH at a wavelength of 590 nm And the effective retardation value Reff at the position of? = 45 ° and? = 45 ° was measured.

In addition, the cellulose ester film prepared above was subjected to reliability treatment for 500 hours at 60 ° C and 90% RH using a high temperature and high humidity chamber, and the Reff after the reliability treatment was measured using the same measuring equipment.

The measurement results are shown in Table 1 below.

No cellulose
ester
Plasticizer
Kinds
Film thickness
(탆)
Reliability Before / After Reff (nm)
Before processing After processing Variation Example 1 TAC (100 kg) A (2.5 kg) + B (2.5 kg) + C (5 kg) 20 2.1 0.7 -1.4 Example 2 TAC (100 kg) A (2.5 kg) + B (2.5 kg) + C (5 kg) 25 3.5 1.4 -2.1 Example 3 TAC (100 kg) A (2.5 kg) + B (2.5 kg) + C (5 kg) 30 4.1 1.8 -2.3 Example 4 TAC (100 kg) A (2.5 kg) + B (2.5 kg) + C (5 kg) 40 5.4 0.5 -4.9 Comparative Example 1 TAC (100 kg) D (5 kg) + C (5 kg) 40 14.8 2.4 -12.4 Comparative Example 2 TAC (100 kg) E (5 kg) + C (5 kg) 40 16.7 0.9 -15.8

As can be seen from the above Table 1, when the plasticizer proposed in the present invention is included, it can be seen that the cellulose ester film has excellent ΔReff characteristics and excellent optical reliability before and after the reliability treatment.

While the present invention has been particularly shown and described with reference to specific embodiments thereof, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims. It will be easy for anyone to know.

Claims (3)

A cellulose ester having an acetyl group degree of substitution in the range of 2.70 to 2.95, an asymmetric ester compound having an aromatic group represented by the following formulas (1) and (2) and a terminal symmetrical aliphatic compound represented by the following formula Ester phase difference film.
[Chemical Formula 1]
M A - [D O - D A] n - D B
(2)
M A - [D O - D A] n - D O
(Wherein, M A: R 1 -COOH, D O: HO-R 2 -OH, D A: HOOC-R 1 -COOH, D B: a HO-R 3 -OH, R 1 is aryl having 6 or more R 2 is a compound having 2 to 6 carbon atoms, propylene glycol, and R 3 is a compound having 2 to 12 carbon atoms, which is an adipic acid residue or an aliphatic carboxylic acid residue or an akylene dicarboxylic acid residue, and n represents an integer of 1 or more.
(3)
I - (T) n - I
(Wherein I represents an ester group having 1 to 20 carbon atoms, an alkoxycarbonyl group having 1 to 20 carbon atoms, an amide group having 1 to 20 carbon atoms, a carbamoyl group having 1 to 20 carbon atoms, a hydroxyl group, T is a 2,2,4-trimethyl-1,3-pentanylene group, or a divalent saturated bridging group having 0 to 40 carbon atoms and 0 to 20 carbon atoms, and the number of atoms is 0 Means that the groups at both ends of the linkage form a single bond directly, and N represents an integer of 1 or more.
The method according to claim 1,
The cellulose ester phase difference film is characterized in that the effective retardation value Reff defined by the following formula (1) measured under the conditions of 23 ° C and 55% RH is within ± 30 nm.
[Equation 1]
Reff = (nx'-ny ') xd
(Where d is the thickness (nm) of the film, nx 'and ny' are the effective refractive index values formed from nx, ny and nz when observed at the positions of? = 45 ° and? to be.)
The method according to claim 1,
Wherein the cellulose ester phase difference film has a change amount of Reff in a range of 占 10 nm or less after standing for 500 hours in a high-temperature and high-humidity chamber at 60 占 폚 and a 90% RH reliability environment.
KR1020150101951A 2015-07-17 2015-07-17 Cellulose ester phase difference film having superior optical reliableness KR101716118B1 (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20080005536A (en) * 2005-05-10 2008-01-14 코니카 미놀타 옵토 인코포레이티드 Cellulose ester film, polarizing plate, and liquid crystal display
WO2014141734A1 (en) * 2013-03-12 2014-09-18 コニカミノルタ株式会社 Organic electroluminescent display device and method for manufacturing same

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20080005536A (en) * 2005-05-10 2008-01-14 코니카 미놀타 옵토 인코포레이티드 Cellulose ester film, polarizing plate, and liquid crystal display
WO2014141734A1 (en) * 2013-03-12 2014-09-18 コニカミノルタ株式会社 Organic electroluminescent display device and method for manufacturing same

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