CN103080785B - Reflecting material - Google Patents
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- CN103080785B CN103080785B CN201180041858.7A CN201180041858A CN103080785B CN 103080785 B CN103080785 B CN 103080785B CN 201180041858 A CN201180041858 A CN 201180041858A CN 103080785 B CN103080785 B CN 103080785B
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/02—Diffusing elements; Afocal elements
- G02B5/0205—Diffusing elements; Afocal elements characterised by the diffusing properties
- G02B5/0236—Diffusing elements; Afocal elements characterised by the diffusing properties the diffusion taking place within the volume of the element
- G02B5/0242—Diffusing elements; Afocal elements characterised by the diffusing properties the diffusion taking place within the volume of the element by means of dispersed particles
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- 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
- B29C55/00—Shaping by stretching, e.g. drawing through a die; Apparatus therefor
- B29C55/02—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets
- B29C55/04—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets uniaxial, e.g. oblique
- B29C55/06—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets uniaxial, e.g. oblique parallel with the direction of feed
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/02—Diffusing elements; Afocal elements
- G02B5/0273—Diffusing elements; Afocal elements characterized by the use
- G02B5/0284—Diffusing elements; Afocal elements characterized by the use used in reflection
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2023/00—Use of polyalkenes or derivatives thereof as moulding material
- B29K2023/10—Polymers of propylene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/016—Additives defined by their aspect ratio
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- Chemical & Material Sciences (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Engineering & Computer Science (AREA)
- Dispersion Chemistry (AREA)
- Optical Elements Other Than Lenses (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The purpose of the present invention is to provide a novel reflecting material having high reflectivity and extremely low light reflectivity loss even when used for a long period under high-temperature conditions. The reflecting material is characterized by being formed from a resin composition containing a thermoplastic resin, a finely powdered filler, and an antioxidant, the antioxidant containing a phenolic antioxidant (A) having a predetermined structure, and the average grain diameter of the finely powdered filler being 0.15 to 0.50 [mu]m and the average aspect ratio being 3 or lower.
Description
Technical field
The present invention relates to the reflecting material of the component parts being especially suitable for use as liquid crystal display, ligthing paraphernalia or lighting billboard etc.
Background technology
Reflecting material headed by liquid crystal display, the various fields such as ligthing paraphernalia or lighting billboard used.Recently, particularly in field of liquid crystal, the maximization of device and the High Level of display performance are developed, at least require to supply more light to improve the performance of backlight unit to liquid crystal, for this reason, for reflecting material, also require that it has more excellent light reflective (also referred to as " reflectivity ").
At present, as reflecting material, there will be a known the liquid crystal display reflectance coating (with reference to patent documentation 1) such as employing white polyester film.
But, when using the material of aromatic polyester-based resin as reflecting material, because aromatic rings contained in the strand of aromatic polyester-based resin absorbs ultraviolet, therefore, there is following problems: under the ultraviolet effect that the light source of liquid crystal indicator etc. sends, there is deterioration, xanthochromia in film, thus the light reflective of reflectance coating is reduced.
On the other hand, also the known film by being formed adding filling agent in acrylic resin stretches, fine space is formed in film, thus create the reflecting material (with reference to patent documentation 2 and 3) of light scattering reflection, for such reflectance coating employing polyolefin resin, by the deterioration of UV-induced film and the problem of xanthochromia few.
But, because polyolefin resin exists degradation problem under mechanical properties under the action of heat, such as, deterioration is there is under heat when the heat, the use that add man-hour and the effect of oxygen, decline to prevent mechanical properties, also proposed polyolefin composition containing Hinered phenols antioxidant, acrylic ester compound and phosphorus species (such as, with reference to patent documentation 4) and in acrylic resin, be combined with the polypropylene resin composite (for example, referring to patent documentation 5) etc. of whiteruss, phenolic antioxidant, organic phosphates antioxidant.
Known in addition, even employ the reflectance coating of aromatic polyester-based resin, be subject to the impact of the heat from light source, be formed in the crosslinking chemical generation thermal oxide of the coating layer on optical reflection film, variable color, light reflective properties is made to reduce thus, for such problem, carry out adding the trial (with reference to patent documentation 6) that Hinered phenols antioxidant etc. improves thermal stability.
In addition, the applicant etc. also proposed a kind of reflectance coating, its resin combination obtained by having coordinated aliphatic polyester-based resin (A), acrylic resin (B), micro-powdered filler (C) and antioxidant (D) is formed, wherein, as described antioxidant (D), employ Phosphorus antioxidant, lactone antioxidant or phenolic antioxidant (with reference to patent documentation 7).
Prior art document
Patent documentation
Patent documentation 1: Japanese Unexamined Patent Publication 04-239540 publication
Patent documentation 2: Japanese Unexamined Patent Publication 06-298957 publication
Patent documentation 3: Japanese Unexamined Patent Publication 2005-031653 publication
Patent documentation 4: No. 3082333rd, Jap.P.
Patent documentation 5: Japanese Unexamined Patent Publication 09-255827 publication
Patent documentation 6: Japanese Unexamined Patent Publication 2006-163378 publication
Patent documentation 7: Japanese Unexamined Patent Publication 2007-199650 publication
Summary of the invention
The problem that invention will solve
In above-mentioned patent documentation 5 and 6, only disclose and can improve thermal characteristics general in polyolefin resin formed body, for the relation with reflecting material purposes without any open, its result, in reflecting material purposes, employ the antioxidant as disclosed in patent documentation 6,7.
But, these technology still may not meet through time light reflective properties reduce requirement, there is room for improvement.
Therefore, problem of the present invention is to provide a kind of novel reflecting material, and it has excellent reflectivity, even if Long-Time Service under the high temperature conditions, the reduction of light reflective is also minimum.
The method of dealing with problems
The present inventor etc. pay close attention to the antioxidant added in reflecting material again, and conduct in-depth research, and result makes us finding uncannily: according to the kind of antioxidant, can suppress the reflectance reduction of the particular wavelength region caused under the high temperature conditions.That is, the Hinered phenols antioxidant having found to have ad hoc structure can suppress the reflectance reduction of the wavelength 430nm ~ 460nm caused under the high temperature conditions.
And, finding as drawn a conclusion based on this opinion: by adding above-mentioned antioxidant in light scattering high reflecting material in the region of repeating with above-mentioned particular wavelength region, can significantly inhibitory reflex rate reduce, so that complete the present invention.
Namely, the feature of reflecting material of the present invention is, its by be 0.15 ~ 0.50 μm containing thermoplastic resin, mean grain size and average aspect ratio be micro-powdered filler of less than 3, the resin combination of the phenolic antioxidant (A) of any more than a kind that represents of following general formula (1) or (2) forms, and at least stretches unidirectional.
[chemical formula 1]
(wherein, in general formula (1) and (2), R
1and R
2represent the side chain of hydrogen atom or carbon number 1 ~ 18 or straight chain and optionally there is substituent any alkyl, R
3represent organic residue.)
According to reflecting material of the present invention, by the antioxidant containing ad hoc structure and micro-powdered filler with specific mean grain size and specific length-diameter ratio, even if Long-Time Service under the high temperature conditions, the reduction of light reflective also can be made to become minimum.Therefore, reflecting material of the present invention can be suitable as the reflecting material of liquid crystal display, ligthing paraphernalia or lighting billboard etc.
In the present invention, as the form that reflecting material can be taked, being not particularly limited, can be membranaceous or any form in sheet etc.It should be noted that, described " film " refers to, compared with length and width, thickness is minimum, and the thin and flat goods that maximum gauge can limit arbitrarily, it supplies (Japanese Industrial Standards JIS K6900) usually as rolls; Generally speaking, described " sheet " refers to, in JIS definition, thin and for length and width, the smooth goods that its thickness is usually less.But, there is no obvious boundary between sheet and film, in the present invention, there is no need on word, both to be distinguished, also comprise " sheet " when therefore, in the present invention, being called " film ", also comprise " film " when being called " sheet ".
In addition, in the present invention, when being expressed as " X ~ Y " (X, Y are Any Digit), when being not particularly limited, the implication of representative " more than X and below Y ", also comprises the implication of " being preferably greater than X " and " being preferably less than Y ".
The effect of invention
Reflecting material of the present invention contains the antioxidant of ad hoc structure and has micro-powdered filler of specific mean grain size and specific length-diameter ratio, therefore, tool has the following advantages: have excellent reflectivity, even if Long-Time Service under the high temperature conditions, the reduction of light reflective is also minimum.
Accompanying drawing explanation
[Fig. 1] Fig. 1 illustrates the reflecting material of embodiment 1 before and after promotion test in the figure of the reflectivity of wavelength 420 ~ 600nm.
[Fig. 2] Fig. 2 illustrates the reflecting material of comparative example 1 before and after promotion test in the figure of the reflectivity of wavelength 420 ~ 600nm.
[Fig. 3] Fig. 3 illustrates not containing having the reflecting material of micro-powdered filler of specific mean grain size and specific length-diameter ratio at the figure of the reflectivity of wavelength 420 ~ 600nm.
Embodiment
< reflecting material >
As reflecting material of the present invention, as long as by containing thermoplastic resin, mean grain size be 0.15 ~ 0.50 μm and average aspect ratio be less than 3 micro-powdered filler, and the resin combination of any more than the a kind phenolic antioxidant (A) to be represented by following general formula (1) or (2) is formed, and at least stretch unidirectional, then be not particularly limited, by using the phenolic antioxidant (A) of ad hoc structure and there is the constituent material of micro-powdered filler as reflecting material of specific mean grain size and average aspect ratio, excellent reflectivity can be had, even and if Long-Time Service also can make the reduction of light reflective become minimum under the high temperature conditions.
[chemical formula 2]
(wherein, in general formula (1) and (2), R
1and R
2represent the side chain of hydrogen atom or carbon number 1 ~ 18 or straight chain and optionally there is substituent arbitrary alkyl, R
3represent organic residue.)
Fig. 1 illustrates the reflecting material of embodiment 1 before and after promotion test in the figure of the reflectivity of wavelength 420 ~ 600nm, as known in the figure, when use mean grain size is 0.15 ~ 0.50 μm and average aspect ratio is micro-powdered filler of less than 3, significantly increase at the reflectivity of wavelength 430 ~ 460nm.This is because, the light scattering height in the scope repeated with wavelength 430 ~ 460nm of micro-powdered filler with such mean grain size and length-diameter ratio.
In more detail, by extending, with micro-powdered filler for core and form space, in the scope repeated with wavelength 430 ~ 460nm, particularly light scatteringly to increase.
On the other hand, Fig. 2 is the reflecting material, namely that comparative example 1 is shown, front and back are tested in the figure of the reflectivity of wavelength 420 ~ 600nm in promotion when employing the phenolic antioxidant without ad hoc structure of the present invention, as known in the figure, when employing the phenolic antioxidant without ad hoc structure of the present invention, significantly reduce at the reflectivity of wavelength 430 ~ 460nm.
From the above results, reflecting material of the present invention is by the antioxidant containing ad hoc structure and micro-powdered filler with specific mean grain size and specific length-diameter ratio, even if Long-Time Service under the high temperature conditions, the reduction of light reflective also can be made to become minimum.
It should be noted that, Fig. 3 illustrates to employ not meet mean grain size and be 0.15 ~ 0.50 μm and average aspect ratio is the figure of reflecting material at the reflectivity of wavelength 420 ~ 600nm of micro-powdered filler (the micro-powdered filler of mean grain size more than 0.50 μm) of the scope of less than 3, as known in the figure, substantially identical with the reflectivity in other wavelength region may at the reflectivity of wavelength 430 ~ 460nm.
Therefore, reflecting material of the present invention by use mean grain size to be 0.15 ~ 0.50 μm and average aspect ratio be less than 3 micro-powdered filler, especially excellent effect can have been given play to.
(phenolic antioxidant (A))
Reflecting material of the present invention needs at least containing any more than a kind phenolic antioxidant (A) that following general formula (1) or (2) represent.
[chemical formula 3]
(wherein, in general formula (1) and (2), R
1and R
2represent the side chain of hydrogen atom or carbon number 1 ~ 18 or straight chain and optionally there is substituent arbitrary alkyl, R
3represent organic residue.)
R
1and R
2represent the side chain of hydrogen atom or carbon number 1 ~ 18 or straight chain and optionally there is substituent any alkyl, particularly, hydrogen atom, methyl and ethyl etc. can be enumerated.
In addition, R
3represent organic residue, specifically can enumerate: the group with carboxylate or phosphate ester structure; The alkyl such as ethyl, propyl group, butyl; The aryl such as benzyl, tolyl; The alkoxys such as methoxyl, ethoxy, propoxyl group; The alkyl aminos such as methylamino, ethylamino, propylcarbamic; And sulfydryl, thioether group etc. have the structure etc. of sulfenyl.
The compound that above-mentioned general formula (1) represents has the compound at the ortho position of hydroxyl by the tert-butyl group and methyl substituted skeleton, by having above-mentioned skeleton, even if Long-Time Service under the high temperature conditions, also can reduce the light reflective of inhibitory reflex material.
As the phenolic antioxidant (A-1) that above-mentioned general formula (1) represents, can enumerate such as: 3, two { the 2-[3-(3-tertiary butyl-4-hydroxy-5-aminomethyl phenyl) propionyloxy]-1 of 9-, 1-dimethyl ethyl }-2, 4, 8, 10-tetra-oxaspiro [5.5] hendecane (such as, ADEKA company manufactures, trade name " ADEKA STAB AO-80 " and Sumitomo Chemical Co manufacture, trade name " Sumilizer GA-80 " etc.), ethylenebis (oxygen ethylidene) two [3-(between 5-tert-butyl hydroxy tolyl) propionic ester] (such as, Ciba Specialty Chemicals company manufactures, trade name " IRGANOX245 "), triethylene glycol two [3-(3-tertiary butyl-4-hydroxy-5-aminomethyl phenyl) propionic ester] (such as, ADEKA company manufactures, trade name " ADEKA STAB AO-70 ") etc.
The compound that above-mentioned general formula (2) represents is the compound with following skeleton: do not have methyl at the ortho position of hydroxyl, and have organic residue in the contraposition replacement of hydroxyl, because its solid is hindered little, free radical can be caught rapidly, therefore can inhibitory reflex material light reflective reduce.
As the phenolic antioxidant (A-2) that above-mentioned general formula (2) represents, can enumerate: 1, 1, butane (such as 3-tri-(2-methyl-4-hydroxyl-5-tert-butyl-phenyl), ADEKA company manufactures, trade name " ADEKA STABAO-30 "), 4, phenol (such as 4 '-butylidene two (3-methyl-6-tert butyl), ADEKA company manufactures, trade name " ADEKA STAB AO-40 ") and 4, phenol (such as 4 '-sulphur connection two (3-methyl-6-tert butyl), Ouchi Shinko Chemical Ind Co., Ltd. manufactures, trade name " Noclac300 " and Sumitomo Chemical Co manufacture, trade name " Sumilizer WX-R ") etc.
As antioxidant, more preferably except the phenolic antioxidant (A) that above-mentioned general formula (1) or (2) represent, also combinationally use the Phosphorus antioxidant of pentaerythrite type and/or sulfur type antioxidant.Combinationally used with the Phosphorus antioxidant of pentaerythrite type and/or sulfur type antioxidant by the phenolic antioxidant (A) that above-mentioned general formula (1) or (2) are represented, more excellent effect can be obtained.
As the Phosphorus antioxidant of above-mentioned pentaerythrite type, can enumerate: two octadecyl pentaerythritol diphosphites (manufacture of ADEKA company, trade name " ADEKA STAB PEP-8 "), two (2,4-di-tert-butyl-phenyl) pentaerythritol diphosphites (manufacture of ADEKA company, trade name " ADEKA STABPEP-36 ") and two (2,6-di-t-butyl-4-aminomethyl phenyl) pentaerythritol diphosphites, two (2,6-di-t-butyl-4-n-octadecane oxygen base carbonylethyl phenyl) pentaerythritol diphosphites etc.
As above-mentioned sulfur type antioxidant, can enumerate: 3, (Sumitomo Chemical Co manufactures the two myristyl ester of 3 '-sulphur di-propionic acid, trade name " Sumilizer TPM "), two [3-(dodecyl sulfo-) propionic acid] 2, two [[3-(dodecyl the sulfo-)-1-oxopropoxy] methyl]-1 of 2-, (Sumitomo Chemical Co manufactures 3-propane two base, trade name " Sumilizer TP-D " and ADEKA company manufacture, trade name " ADEKA STABAO-412S " etc.), 3, (Sumitomo Chemical Co manufactures the two stearyl of 3 '-sulphur di-propionic acid, trade name " Sumilizer TPS ") etc.
(micro-powdered filler)
For reflecting material of the present invention, except above-mentioned phenolic antioxidant (A), also need at least containing mean grain size be 0.15 ~ 0.50 μm and average aspect ratio be less than 3 micro-powdered filler.By using, there is the mean grain size of above-mentioned scope and micro-powdered filler of average aspect ratio, produce specific micro air bubble in the inside of the reflecting material obtained by stretch processing, the reflectivity at specific wavelength (430 ~ 460nm) can be improved thus.
It should be noted that, the mean grain size of micro-powdered filler and length-diameter ratio can be obtained based on the method recorded in following embodiment.
As above-mentioned micro-powdered filler, as long as its mean grain size is 0.15 ~ 0.50 μm and average aspect ratio is less than 3, then its kind is not limited, can enumerate such as: calcium carbonate, magnesium carbonate, barium carbonate, magnesium sulfate, barium sulphate, calcium sulphate, zinc paste, magnesium oxide, calcium oxide, titanium dioxide, zinc paste, aluminium oxide, aluminium hydroxide, hydroxyapatite, silicon dioxide, mica, talcum, porcelain earth, clay, glass dust, flake asbestos, zeolite, silicic acid carclazyte, polymeric beads, polymer hollow particle etc.These micro-powdered fillers can use wherein any one or mix two or more use.
It should be noted that, by containing micro-powdered filler, except the refraction scattering brought by refringence, the refraction scattering that can also be brought by the refringence be formed between the hole around micro-powdered filler and the refraction scattering that brought by the refringence between the hole be formed in around micro-powdered filler and micro-powdered filler etc. and obtain light reflective.Therefore, in micro-powdered filler, more preferably refractive index is the filling agent of more than 1.6, compared with other micro-powdered filler, the refractive index of titanium dioxide is obviously higher, can enlarge markedly the refringence between base resin, therefore, compared with using the situation of other filling agent, excellent reflectivity can be obtained with less use level.In addition, by using titanium dioxide, even if the thickness of thinning reflecting material, also high light reflective can be obtained.Due to above-mentioned reason, most preferably titanium dioxide.
It should be noted that, as long as reflecting material of the present invention is containing micro-powdered filler with specific mean grain size and specific average aspect ratio, do not hinder interpolation not to be in micro-powdered filler in above-mentioned scope.
In addition, in order to improve the dispersiveness of inorganic micro powder body in resin, can use and utilize silicon compounds, multicomponent alcoholics compound, aminated compounds, fatty acid, fatty acid ester etc. to implement surface-treated inorganic micro powder body to the surface of micro-powdered filler.
In addition, as above-mentioned micro mist shape filling dose (when being added with micro-powdered filler without specific mean grain size and specific average aspect ratio further, what represent is the total amount of the micro-powdered filler comprising so micro-powdered filler), if consider the light reflective, physical strength, productivity etc. of reflecting material, then relative to the quality of resin combination entirety, be preferably 10 ~ 80 quality %, be more preferably 20 ~ 70 quality %.If the content of micro-powdered filler is more than 20 quality %, then fully can guarantees the area at the interface between base resin and micro-powdered filler, thus highly reflective can be given to reflecting material.If the content of micro-powdered filler is below 70 quality %, then can guarantee that reflecting material has necessary physical strength.
(thermoplastic resin)
As the thermoplastic resin used in reflecting material of the present invention, can enumerate such as: polyolefin resin, polyester resin, acrylic resin, polyvinyl chloride resin, Vingon resinoid, fluororesin, polyethers resin, polyamide-based resin, polyurethane based resin, dienes resin etc., wherein, from the viewpoint of reflecting properties, polyolefin resin can be enumerated as preferred example, as polyolefin resin, can enumerate such as: be selected from the acrylic resin such as polypropylene, propylene-ethylene copolymers; The polyvinyl resins such as tygon, high density polyethylene, Low Density Polyethylene; The cycloolefin resinoids such as ethylene-cyclic olefin multipolymer; At least one polyolefin resin in the olefin type elastomers such as EP rubbers (EPR), ethylene-propylene-diene terpolymer (EPDM).In the middle of these, from the viewpoint of engineering properties, flexibility etc., optimization polypropylene resin, polyvinyl resin, most preferably polypropylene.
(mixing ratio)
As the mixing ratio of thermoplastic resin, micro-powdered filler and phenolic antioxidant (A), relative to thermoplastic resin 100 weight portion, preferably containing micro-powdered filler of 12 ~ 400 weight portions, the phenolic antioxidant (A) of 0.01 ~ 2 weight portion, in addition, more preferably containing micro-powdered filler of 26 ~ 233 weight portions, the phenolic antioxidant (A) of 0.05 ~ 1 weight portion.
(other composition)
Except mentioned component, other resin (being called " other component resin ") can also be contained, in addition, light stabilizer, thermal stabilizer, spreading agent, ultraviolet light absorber, fluorescer, compatilizer, lubricant and other adjuvant can also be contained.
(manufacture method of reflecting material)
As the manufacture method of reflecting material of the present invention, be not particularly limited, known method can be adopted.Below, the manufacture method row for reflecting material are given one example and are described, but the present invention is not by any restriction of following manufacture method.
First, in thermoplastic resin, coordinate micro-powdered filler, phenolic antioxidant (A) and other adjuvant etc. as required, make resin combination.
Particularly (below, be described as an example to use olefine kind resin as the situation of thermoplastic resin), micro-powdered filler, phenolic antioxidant (A) and other adjuvant etc. are added in olefine kind resin, after utilizing ribbon mixer, rotary drum mixer, Henschel mixer etc. to mix, use the temperature (such as 190 DEG C ~ 270 DEG C) more than the fusing point of resin such as banbury mixers, singe screw or double screw extrusion machine to carry out mixing, can resin combination be obtained thus.
Or, quantitative olefine kind resin, micro-powdered filler, phenolic antioxidant (A) and other adjuvant etc. can be added to by respective feeder etc. and obtain resin combination.In addition, micro-powdered filler, phenolic antioxidant (A) and other adjuvant etc. can also be coordinated with high concentration in advance in olefine kind resin, make so-called masterbatch, this masterbatch is mixed with olefine kind resin, make the resin combination of desired concentration.
Then, make the resin combination drying obtained like this, be then supplied in extruder, be heated to more than given temperature respectively, make its melting.
The conditions such as extrusion temperature need to consider due to decomposition, molecular weight and molecular weight etc. to be set, and such as, when olefine kind resin, the extrusion temperature of preferred resin composition is 190 ~ 270 DEG C.
Then, by the resin combination interflow to T-shaped die head after melting, extruded by the extrusion of the slit-shaped of T-shaped die head, closely sealed solidification on chill roll, form cast sheet.
The cast sheet obtained at least is carried out stretch (particularly, preferably at least unilateral stretching more than 1.1 times) unidirectional.By stretching, the olefine kind resin of resin bed inside and the interface of micro-powdered filler occur peel off and form space, albefaction with time slice is carried out, thus can improve the light reflective (particularly at the reflectivity of wavelength 430 ~ 460nm) of film.In addition, cast sheet stretches particularly preferably in two-way.Only carry out unilateral stretching and the space that formed only becomes the fibre-like morphology extended in a direction, and by carrying out two-way stretch, its space extends in both direction in length and breadth, thus forms discoid form.
That is, by carrying out two-way stretch, the stripping area at the olefine kind resin of resin bed inside and the interface of micro-powdered filler increases, and the albefaction of sheet is carried out further, its result, can improve the light reflective of film further.In addition, if carry out two-way stretch, then the anisotropy of film shrinkage direction reduces, and therefore can improve the thermotolerance of film, and can increase the physical strength of film.
Draft temperature when stretching to cast sheet is preferably more than the glass transition temperature (Tg) of resin bed.
If draft temperature is more than glass transition temperature (Tg), then can not there is the fracture of film when stretching, can stably stretch.
The drawing sequence of two-way stretch is not particularly limited, and such as, can be two-way stretch simultaneously, also can for stretch successively.After use stretcher carries out melting masking, can be stretched by roller and stretch along MD, then utilize stenter to stretch and stretch along TD; Also two-way stretch can be carried out by tubular type stretching etc.Stretching ratio during two-way stretch preferably carries out the stretching of more than 6 times with area dynameter.By carrying out the stretching that area multiplying power is more than 6 times, the voidage that sometimes can realize reflectance coating entirety is more than 40%.
After stretching, in order to give dimensional stability (morphological stability in space) to reflectance coating, preferably carry out heat setting.Treatment temperature for carrying out heat setting to film is preferably 110 DEG C ~ 170 DEG C.Processing time required for heat setting be preferably 1 second ~ 3 minutes.In addition, stretcher etc. is not particularly limited, but the stenter preferably carrying out carrying out after the stretch heat-set treatment stretches.
< rhythmo structure >
Reflecting material of the present invention has the structure having supporting layer B at least one side side lamination of resin bed A, and at least stretch unidirectional, described resin bed A by be 0.15 ~ 0.50 μm containing thermoplastic resin, mean grain size and average aspect ratio be less than 3 micro-powdered filler and the resin combination of any more than a kind phenolic antioxidant (A) that represented by following general formula (1) or (2) formed, described supporting layer B is major component resin combination is formed by with any more than a kind in polyolefin resin, polyester resin and polystyrene resins.By forming such structure, tool has the following advantages: prevent by heat cause curling, prevent from brightness disproportionation and improve adding the operability etc. in man-hour.
In addition, as other rhythmo structure, can enumerate such as: the rhythmo structure being provided with 3 layers of supporting layer (B) on the two sides of resin bed (A).In addition, can also have other layer except resin bed (A) and supporting layer (B), other layer can between each layer of resin bed (A) and supporting layer (B).Such as, adhesive linkage can be had between resin bed (A), supporting layer (B).
As the manufacture method of the reflecting material of rhythmo structure, comprise following method, such as, the fused raw material coextrusion of the fused raw material of resin bed (A) and supporting layer (B) is carried out shaping after, the products formed obtained at least is stretched unidirectional, thus obtains laminated body.In addition, when adopting such coetrusion, when adopting olefine kind resin as resin (A), consider the adaptation between resin bed (A), above-mentioned supporting layer (B) also particularly preferably uses olefine kind resin.It should be noted that, micro-powdered filler can also be added in supporting layer (B).
In addition, following method etc. can also be adopted, namely, prepare resin bed (A) and supporting layer (B), described resin bed (A) carries out stretching obtaining unidirectional by after the fused raw material extrusion molding of resin bed (A), at least in advance, then adopt the dry lamination employing common bonding agent, the extruding layer employing the molten resin with heat sealability is pressed on resin bed (A) and supporting layer (B) and arranges bonding coat, utilize nip roll etc. to carry out pressure viscosity, thus carry out the method for pressure-sensitive adhesive.It should be noted that, supporting layer (B) also can stretch at least unidirectional in advance.In addition, in such manufacture method, as supporting layer (B), when considering thermotolerance, rigidity, preferably use olefine kind resin (wherein preferred cyclic olefin resinoid), polyethylene terephthalate and polystyrene.In addition, micro-powdered filler can also be added in supporting layer (B).
(thickness)
As the thickness of reflecting material of the present invention, be not particularly limited, be preferably 30 μm ~ 1500 μm, particularly, if consider the operability of practical aspect, be then preferably in the scope of 50 μm ~ about 1000 μm.
As the reflecting material of such as liquid crystal display purposes, preferred thickness is 50 μm ~ 700 μm, and as the reflecting material of such as ligthing paraphernalia, lighting billboard purposes, preferred thickness is 100 μm ~ 1000 μm.
In addition, when rhythmo structure, the gross thickness of each layer is than as follows: preferred resin layer (A): the scope of supporting layer (B)=1:5 ~ 10:1, is more preferably the scope of 1:4 ~ 8:1.
(reflectivity)
For reflecting material of the present invention, preferably its at least one side be more than 97% relative to the average reflectance of the light of wavelength 420nm ~ 600nm.As long as have the reflecting material of such reflecting properties, just can demonstrate the good reflection characteristic as reflecting material, the picture being assembled with the liquid crystal display of this reflecting material etc. can realize sufficient lightness.
In addition, be preferably less than 0.7% in the reduction (reflection differences) of the average reflectance of wavelength 430 ~ 460nm before and after the thermal treatment carrying out 1000 hours temperature 85 DEG C, be more preferably less than 0.3%.
(voidage)
Reflecting material of the present invention can have space in inside, its voidage be preferably more than 10% and less than 90%, be particularly preferably more than 20% and less than 80%.By arranging the space of above-mentioned scope, the albefaction of reflecting material can fully be carried out, and therefore can realize high light reflective, in addition, the physical strength of reflecting material can not be made to reduce and rupture.In addition, in rhythmo structure, more preferably only resin bed (A) has the space in above-mentioned scope.By only forming the space of above-mentioned scope in resin bed (A), compared with there is the film in space in supporting layer (B), the physical strength reduction etc. of film can not be worried.It should be noted that, the voidage by stretching when the inside of reflecting material exists hole can be updated in following formula to be obtained.
Voidage (%)={ density of the film before (density of the film after the density-stretching of the film before extension)/extension } × 100
< purposes >
Even if reflecting material of the present invention is owing to having Long-Time Service under the high temperature conditions in the also minimum character of the reduction of the average reflectance of wavelength 430 ~ 460nm, is useful as the reflection part used in the liquid crystal indicators such as liquid crystal display, ligthing paraphernalia, lighting billboard etc.
This is because, the light source used in this purposes, such as the light quantity under wavelength 430 ~ 460nm such as cold-cathode fluorescence lamp (CCFL) and LED is larger.That is, less in the reflectance reduction of this wavelength region may, brightness can be suppressed to reduce.It should be noted that, generally speaking, liquid crystal display is made up of liquid crystal panel, polarisation reflector plate, diffusion sheet, light guide plate, reflector plate, light source, light source reflector etc.Light from light source can be incident in the reflector plate of the effect in liquid crystal panel, light guide plate in performance and to use by reflecting material of the present invention efficiently, also can carry out optically focused and make it be incident in the light source reflector of the effect in light guide plate using at the irradiation light of the light source of edge part having self-configuring in the future.
Embodiment
Below embodiment is shown, more specific description is carried out to the present invention, but the present invention is not limited to these embodiments, various application can be carried out in the scope not departing from technological thought of the present invention.It should be noted that, the measured value shown in embodiment and evaluation are carried out according to shown below.Wherein, (transmission) direction that accesses of film is expressed as MD, the direction orthogonal with it is expressed as TD.
< measures and evaluation method >
(constant temperature promotes test)
Use the air drier of 85 DEG C to carry out and promote test.The yellow chromaticity determining before putting into dryer and drop into after latter 1000 hours and light reflectivity.
(xanthochromia degree (Δ YI))
Utilize spectrophotometric color measurement instrument (" SC-T ", Suga testing machine Co., Ltd. manufacture), carry out eliminating the mensuration (d/8) of normal reflection light with the attached white calibration standard plate of body for benchmark, obtain yellow chromaticity (YI).Δ YI is calculated by following formula.
Δ YI={YI (after promoting test)-YI (before promoting test) }
(average reflectance (%))
Integrating sphere is arranged in spectrophotometer (" U-3900H ", Hitachi Co., Ltd manufacture), the scope of wavelength 420nm ~ 600nm with 0.5nm measuring space using aluminium oxide blank as 100% time reflectivity.Calculate the mean value of the measured value obtained, using this value as average reflectance.The average reflectance of wavelength 430 ~ 460nm is calculated by the measured value obtained.
(mean grain size of micro-powdered filler)
The particle diameter that X-ray transmission formula particle size distribution device (manufacture of SediGraph5100, Micromeritics company) will be utilized to measure the cumulative volume mark 50% obtained is obtained as mean grain size (D50).
(length-diameter ratio of micro-powdered filler)
Electron microscope can be utilized to observe micro-powdered filler, after determining the major axis footpath of micro-powdered filler, short shaft diameter, by calculating length-diameter ratio.It should be noted that, for 30 calculating particles length-diameter ratios of micro-powdered filler, using its mean value as average aspect ratio.
(length-diameter ratio=major axis footpath/short shaft diameter)
Embodiment 1
By acrylic resin (trade name " NOVATEC PP FY6HA ", Japan Polypropylene Corp. manufacture) particle, phenolic antioxidant (the trade name " AO-80 " that general formula (1) represents, Asahi Denka Co., Ltd. manufactures), the Phosphorus antioxidant of pentaerythrite type (trade name " PEP-36 ", Asahi Denka Co., Ltd. manufactures) mix with the mass ratio of 100:0.2:0.2, then add and the titanium dioxide of acrylic resin homogenous quantities (trade name " KRONOS2230 ", KRONOS company manufactures, mean grain size: 0.37 μm, average aspect ratio: 2.1), the double screw extrusion machine be used in after 270 DEG C of heating has carried out granulating.
By the pellet supply of above-mentioned making in the extruder after 200 DEG C of heating, be extruded into sheet, cooling curing, define single-layer sheet.Then, the roller that the sheet material obtained has carried out 2 times temperature 130 DEG C along MD is stretched, then carrying out the stenter stretching of 3 times at 130 DEG C along TD further, by this has been two-way stretch, obtaining the reflectance coating of thickness 185 μm.Finally, yellow chromaticity, the reflectivity evaluation that constant temperature promotes test front and back has been carried out for the reflectance coating obtained.
Embodiment 2
In embodiment 1, the phenolic antioxidant (trade name " AO-80 ", Asahi Denka Co., Ltd. manufacture) particle of acrylic resin (trade name " NOVATEC PP FY6HA ", Japan Polypropylene Corp. manufacture), general formula (1) represented, the Phosphorus antioxidant of pentaerythrite type (trade name " PEP-36 ", Asahi Denka Co., Ltd. manufacture) mix with the mass ratio of 100:0.1:0.1, in addition, define reflectance coating according to method similarly to Example 1, the reflectance coating obtained is evaluated.
Embodiment 3
In embodiment 1, the phenolic antioxidant (trade name " AO-80 ", Asahi Denka Co., Ltd. manufacture) particle of acrylic resin (trade name " NOVATEC PP FY6HA ", Japan Polypropylene Corp. manufacture), general formula (1) represented, sulfur type antioxidant (trade name " SUMILIZERTPM ", Sumitomo Chemical Co manufacture) mix with the mass ratio of 100:0.2:0.2, in addition, define reflectance coating according to method similarly to Example 1, the reflectance coating obtained is evaluated.
Embodiment 4
In embodiment 1, the phenolic antioxidant (trade name " AO-30 ", Asahi Denka Co., Ltd. manufacture) particle of acrylic resin (trade name " NOVATEC PP FY6HA ", Japan Polypropylene Corp. manufacture), general formula (2) represented, the Phosphorus antioxidant of pentaerythrite type (trade name " PEP-36 ", Asahi Denka Co., Ltd. manufacture) mix with the mass ratio of 100:0.2:0.2, in addition, define reflectance coating according to method similarly to Example 1, the reflectance coating obtained is evaluated.
Embodiment 5
In embodiment 1, the phenolic antioxidant (trade name " AO-80 ", Asahi Denka Co., Ltd. manufacture) particle of acrylic resin (trade name " NOVATEC PP FY6HA ", Japan Polypropylene Corp. manufacture), general formula (1) represented mixes with the mass ratio of 100:0.2, in addition, define reflectance coating according to method similarly to Example 1, the reflectance coating obtained is evaluated.
Embodiment 6
In embodiment 1, the phenolic antioxidant (trade name " AO-30 ", Asahi Denka Co., Ltd. manufacture) particle of acrylic resin (trade name " NOVATEC PP FY6HA ", Japan Polypropylene Corp. manufacture), general formula (2) represented mixes with the mass ratio of 100:0.2, in addition, define reflectance coating according to method similarly to Example 1, the reflectance coating obtained is evaluated.
Embodiment 7
By acrylic resin (trade name " NOVATEC PP FY6HA ", Japan Polypropylene Corp. manufacture) particle, phenolic antioxidant (the trade name " AO-80 " that general formula (1) represents, Asahi Denka Co., Ltd. manufactures), the Phosphorus antioxidant of pentaerythrite type (trade name " PEP-36 ", Asahi Denka Co., Ltd. manufactures) mix with the mass ratio of 100:0.2:0.2, then add and the titanium dioxide of acrylic resin homogenous quantities (trade name " KRONOS2230 ", KRONOS company manufactures), the double screw extrusion machine be used in after 270 DEG C of heating carries out granulating, make resin combination A.
The particle of cyclic olefin Resin A (trade name " ZEONOR1430R ", Zeon Corp manufacture), cyclic olefin resin B (trade name " ZEONOR1060R ", Zeon Corp manufacture), acrylic resin (trade name " NOVATEC PP EA9 ", Japan Polypropylene Corp. manufacture) is mixed with the mass ratio of 50:25:25; then the double screw extrusion machine be used in after 230 DEG C of heating carries out granulating, has made resin combination B.
Above-mentioned resin combination A, B are supplied to respectively in extruder A and B being heated to 200 DEG C, 230 DEG C, in each extruder, melting mixing has been carried out 200 DEG C and 230 DEG C, then the T-shaped die head of 2 kinds 3 layers is collaborated, carry out the sheet extruding the 3-tier architecture forming resin bed B/ resin bed A/ resin bed B, carry out cooling curing, define laminated sheet.
The roller that the laminated sheet obtained has carried out 2 times temperature 130 DEG C along MD is stretched, then the stenter stretching of 3 times is carried out at 130 DEG C along TD further, by this has been two-way stretch, obtain thickness 225 μm (resin bed A:185 μm, resin bed B:20 μm, lamination than B:A:B=1:9.25:1, gross thickness is than B:A=1:4.625) reflectance coating.Yellow chromaticity, the reflectivity evaluation that constant temperature promotes test front and back has been carried out for the reflectance coating obtained.
(comparative example 1)
In embodiment 1, by acrylic resin (trade name " NOVATEC PP FY6HA ", Japan Polypropylene Corp. manufacture) particle, as being subject to resistance type phenolic antioxidant (trade name " Irganox1010 ", BASF JAPAN Co., Ltd. manufactures) and Phosphorus antioxidant (trade name " IRGAFOS168 ", BASFJAPAN Co., Ltd. manufacture) 1:1 melange trade name " IRGANOX B225 " BASFJAPAN Co., Ltd. manufacture) mix with the mass ratio of 100:0.4, in addition, reflectance coating is defined according to method similarly to Example 1, the reflectance coating obtained is evaluated.
(comparative example 2)
In embodiment 1, by the particle of acrylic resin (trade name " NOVATEC PP FY6HA ", Japan Polypropylene Corp. manufacture), mix with the mass ratio of 100:0.2:0.2 by resistance type phenolic antioxidant (trade name " Irganox1010 ", BASF JAPAN Co., Ltd. manufacture) and the Phosphorus antioxidant of pentaerythrite type (trade name " PEP-36 ", Asahi Denka Co., Ltd. manufacture), in addition, define reflectance coating according to method similarly to Example 1, the reflectance coating obtained is evaluated.
[the rule-based 26th article of supplementary 13.10.2011 carried out]
(comparative example 3)
In embodiment 1, by the particle of acrylic resin (trade name " NOVATEC PP FY6HA ", Japan Polypropylene Corp. manufacture), mix with the mass ratio of 100:0.2 by resistance type phenolic antioxidant (trade name " Irganox1010 ", BASF JAPAN Co., Ltd. manufacture), in addition, define reflectance coating according to method similarly to Example 1, the reflectance coating obtained is evaluated.
[table 1]
Clear and definite by table 1, after the reflecting material of embodiment 1 ~ 7 carries out the thermal treatment of 1000 hours at 80 DEG C, be less than 0.3% in the reflectance reduction of 430 ~ 460nm, when known its uses under the high temperature conditions for a long time, also can keep excellent light reflective.
On the other hand, the reflecting material of comparative example 1 ~ 3 is more than 0.8% in the reflectance reduction of 430 ~ 460nm after heat treatment, known at high temperature/when using for a long time, poor compared with the reflecting material of embodiment 1 ~ 7.
Industrial applicibility
Reflecting material of the present invention, due to its character, goes for the purposes such as the liquid crystal indicators such as liquid crystal display, ligthing paraphernalia, lighting billboard.
Claims (11)
1. a reflecting material, its by be 0.15 ~ 0.50 μm containing thermoplastic resin, mean grain size and average aspect ratio be less than 3 micro-powdered filler and the resin combination of any more than a kind phenolic antioxidant (A) that represented by following general formula (1) or (2) formed, and at least stretch unidirectional
Wherein, in general formula (1) and (2), R
1and R
2represent the side chain of hydrogen atom or carbon number 1 ~ 18 or straight chain and optionally there is substituent any alkyl, R
3represent organic residue,
Described thermoplastic resin is made up of polyolefin resin, polyester resin, acrylic resin, polyvinyl chloride resin, Vingon resinoid, fluororesin, polyethers resin, polyamide-based resin, polyurethane based resin or dienes resin.
2. a reflecting material, it has the structure having supporting layer B at least one side side lamination of resin bed A, and at least stretches unidirectional,
Described resin bed A by be 0.15 ~ 0.50 μm containing thermoplastic resin, mean grain size and average aspect ratio be less than 3 micro-powdered filler and the resin combination of any more than a kind phenolic antioxidant (A) that represented by following general formula (1) or (2) formed
Described supporting layer B is major component resin combination is formed by with any more than a kind in polyolefin resin, polyester resin and polystyrene resins,
Wherein, in general formula (1) and (2), R
1and R
2represent the side chain of hydrogen atom or carbon number 1 ~ 18 or straight chain and optionally there is substituent any alkyl, R
3represent organic residue,
Described thermoplastic resin is made up of polyolefin resin, polyester resin, acrylic resin, polyvinyl chloride resin, Vingon resinoid, fluororesin, polyethers resin, polyamide-based resin, polyurethane based resin or dienes resin.
3. reflecting material according to claim 1, it contains the composite antioxidant that described phenolic antioxidant (A) is formed with the Phosphorus antioxidant of pentaerythrite type (B) and/or sulfur type antioxidant (C).
4. reflecting material according to claim 2, it contains the composite antioxidant that described phenolic antioxidant (A) is formed with the Phosphorus antioxidant of pentaerythrite type (B) and/or sulfur type antioxidant (C).
5. reflecting material according to claim 1, wherein, described thermoplastic resin is more than any one in polyester resin and polyolefin resin.
6. reflecting material according to claim 2, wherein, described thermoplastic resin is more than any one in polyester resin and polyolefin resin.
7. reflecting material according to claim 3, wherein, described thermoplastic resin is more than any one in polyester resin and polyolefin resin.
8. reflecting material according to claim 4, wherein, described thermoplastic resin is more than any one in polyester resin and polyolefin resin.
9. the reflecting material according to any one of claim 1 ~ 8, it carries out being reduced to less than 0.3% in the average reflectance of wavelength 430 ~ 460nm before and after the thermal treatment of 1000 hours temperature 85 DEG C.
10. the reflecting material according to any one of claim 1 ~ 8, its component parts as liquid crystal display, ligthing paraphernalia or lighting billboard uses.
11. reflecting materials according to claim 9, its component parts as liquid crystal display, ligthing paraphernalia or lighting billboard uses.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2010234568 | 2010-10-19 | ||
| JP2010-234568 | 2010-10-19 | ||
| PCT/JP2011/072732 WO2012053341A1 (en) | 2010-10-19 | 2011-10-03 | Reflecting material |
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| Publication Number | Publication Date |
|---|---|
| CN103080785A CN103080785A (en) | 2013-05-01 |
| CN103080785B true CN103080785B (en) | 2015-05-13 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201180041858.7A Active CN103080785B (en) | 2010-10-19 | 2011-10-03 | Reflecting material |
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| JP (1) | JP5531107B2 (en) |
| KR (2) | KR20130092585A (en) |
| CN (1) | CN103080785B (en) |
| TW (1) | TWI483847B (en) |
| WO (1) | WO2012053341A1 (en) |
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| JP6296325B2 (en) * | 2013-07-17 | 2018-03-20 | コニカミノルタ株式会社 | Exposure equipment |
| CN105322433B (en) * | 2014-05-28 | 2020-02-04 | 深圳光峰科技股份有限公司 | Wavelength conversion device and related light emitting device |
| CN105754241B (en) * | 2016-03-31 | 2017-12-22 | 中山市华洋塑胶颜料有限公司 | Polystyrene reflecting material and preparation method thereof |
| WO2019004473A1 (en) * | 2017-06-30 | 2019-01-03 | 富士フイルム株式会社 | Endoscope flexible tube, endoscope-type medical device, resin composition for coating endoscope flexible tube substrate, and resin composition set for coating endoscope flexible tube substrate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3082333B2 (en) * | 1991-09-03 | 2000-08-28 | 住友化学工業株式会社 | Stabilized polyolefin composition |
| JP4263882B2 (en) * | 2001-08-06 | 2009-05-13 | 株式会社ユポ・コーポレーション | Light reflector |
| EP1424571A4 (en) * | 2001-08-06 | 2008-10-29 | Yupo Corp | Light reflector |
| JP5023471B2 (en) * | 2004-11-15 | 2012-09-12 | 東レ株式会社 | Light reflection film and image display backlight device using the same |
| JP2010191113A (en) * | 2009-02-17 | 2010-09-02 | Fujifilm Corp | Reflecting sheet |
| JP5460078B2 (en) * | 2009-03-04 | 2014-04-02 | 三菱エンジニアリングプラスチックス株式会社 | Aromatic polycarbonate resin composition and molded article |
-
2011
- 2011-10-03 KR KR1020137009939A patent/KR20130092585A/en active Application Filing
- 2011-10-03 KR KR20157008417A patent/KR20150043530A/en not_active Application Discontinuation
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| TWI483847B (en) | 2015-05-11 |
| JPWO2012053341A1 (en) | 2014-02-24 |
| TW201300232A (en) | 2013-01-01 |
| WO2012053341A1 (en) | 2012-04-26 |
| KR20150043530A (en) | 2015-04-22 |
| CN103080785A (en) | 2013-05-01 |
| JP5531107B2 (en) | 2014-06-25 |
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