JP6173400B2 - 太陽電池封止材シート用エチレンビニルアセテート共重合体樹脂及びその製造方法 - Google Patents
太陽電池封止材シート用エチレンビニルアセテート共重合体樹脂及びその製造方法 Download PDFInfo
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- 229920005989 resin Polymers 0.000 title claims description 63
- 239000011347 resin Substances 0.000 title claims description 63
- 239000005038 ethylene vinyl acetate Substances 0.000 title claims description 54
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 title claims description 54
- 238000004519 manufacturing process Methods 0.000 title claims description 26
- 239000008393 encapsulating agent Substances 0.000 title description 11
- 238000006116 polymerization reaction Methods 0.000 claims description 30
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical group CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims description 16
- 239000003999 initiator Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 16
- 239000000178 monomer Substances 0.000 claims description 15
- 150000002978 peroxides Chemical class 0.000 claims description 15
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 11
- 239000005977 Ethylene Substances 0.000 claims description 11
- 238000009826 distribution Methods 0.000 claims description 10
- -1 peroxydicarbonate compound Chemical class 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 8
- 125000000217 alkyl group Chemical group 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 5
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- BEQKKZICTDFVMG-UHFFFAOYSA-N 1,2,3,4,6-pentaoxepane-5,7-dione Chemical compound O=C1OOOOC(=O)O1 BEQKKZICTDFVMG-UHFFFAOYSA-N 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 description 8
- 241000251468 Actinopterygii Species 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- ZACVGCNKGYYQHA-UHFFFAOYSA-N 2-ethylhexoxycarbonyloxy 2-ethylhexyl carbonate Chemical compound CCCCC(CC)COC(=O)OOC(=O)OCC(CC)CCCC ZACVGCNKGYYQHA-UHFFFAOYSA-N 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
- 230000000704 physical effect Effects 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- FVQMJJQUGGVLEP-UHFFFAOYSA-N (2-methylpropan-2-yl)oxy 2-ethylhexaneperoxoate Chemical compound CCCCC(CC)C(=O)OOOC(C)(C)C FVQMJJQUGGVLEP-UHFFFAOYSA-N 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000010292 electrical insulation Methods 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 238000010030 laminating Methods 0.000 description 3
- 238000003475 lamination Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- OPQYOFWUFGEMRZ-UHFFFAOYSA-N tert-butyl 2,2-dimethylpropaneperoxoate Chemical compound CC(C)(C)OOC(=O)C(C)(C)C OPQYOFWUFGEMRZ-UHFFFAOYSA-N 0.000 description 3
- CARSMBZECAABMO-UHFFFAOYSA-N 3-chloro-2,6-dimethylbenzoic acid Chemical compound CC1=CC=C(Cl)C(C)=C1C(O)=O CARSMBZECAABMO-UHFFFAOYSA-N 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- NBBJYMSMWIIQGU-UHFFFAOYSA-N Propionic aldehyde Chemical compound CCC=O NBBJYMSMWIIQGU-UHFFFAOYSA-N 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- ZGPBOPXFOJBLIV-UHFFFAOYSA-N butoxycarbonyloxy butyl carbonate Chemical compound CCCCOC(=O)OOC(=O)OCCCC ZGPBOPXFOJBLIV-UHFFFAOYSA-N 0.000 description 2
- 239000012986 chain transfer agent Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000000691 measurement method Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- JJRDRFZYKKFYMO-UHFFFAOYSA-N 2-methyl-2-(2-methylbutan-2-ylperoxy)butane Chemical compound CCC(C)(C)OOC(C)(C)CC JJRDRFZYKKFYMO-UHFFFAOYSA-N 0.000 description 1
- LEEFORXKTBPZJH-UHFFFAOYSA-N 2-methylbutan-2-yl 2,2-dimethylpropaneperoxoate 2,2,4,4-tetramethylhexaneperoxoic acid Chemical compound C(C)(C)(CC)CC(C(=O)OO)(C)C.C(C(C)(C)C)(=O)OOC(C)(C)CC LEEFORXKTBPZJH-UHFFFAOYSA-N 0.000 description 1
- WTBPWOVBWKJVPF-UHFFFAOYSA-N 3-(2-ethylhexylperoxymethyl)heptane Chemical group CCCCC(CC)COOCC(CC)CCCC WTBPWOVBWKJVPF-UHFFFAOYSA-N 0.000 description 1
- RUDMCWOFBGNJTR-UHFFFAOYSA-N C(C)C(C(=O)O)CCCC.C(C)(C)(CC)OOC(C)(C)CC Chemical compound C(C)C(C(=O)O)CCCC.C(C)(C)(CC)OOC(C)(C)CC RUDMCWOFBGNJTR-UHFFFAOYSA-N 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N butyric aldehyde Natural products CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 description 1
- UOCJDOLVGGIYIQ-PBFPGSCMSA-N cefatrizine Chemical group S([C@@H]1[C@@H](C(N1C=1C(O)=O)=O)NC(=O)[C@H](N)C=2C=CC(O)=CC=2)CC=1CSC=1C=NNN=1 UOCJDOLVGGIYIQ-PBFPGSCMSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000005227 gel permeation chromatography Methods 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical class CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 239000004611 light stabiliser Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 150000001451 organic peroxides Chemical class 0.000 description 1
- 239000003505 polymerization initiator Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F218/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an acyloxy radical of a saturated carboxylic acid, of carbonic acid or of a haloformic acid
- C08F218/02—Esters of monocarboxylic acids
- C08F218/04—Vinyl esters
- C08F218/08—Vinyl acetate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/01—Processes of polymerisation characterised by special features of the polymerisation apparatus used
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F210/00—Copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
- C08F210/02—Ethene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F4/00—Polymerisation catalysts
- C08F4/28—Oxygen or compounds releasing free oxygen
- C08F4/32—Organic compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/08—Copolymers of ethene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L31/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an acyloxy radical of a saturated carboxylic acid, of carbonic acid or of a haloformic acid; Compositions of derivatives of such polymers
- C08L31/02—Homopolymers or copolymers of esters of monocarboxylic acids
- C08L31/04—Homopolymers or copolymers of vinyl acetate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2500/00—Characteristics or properties of obtained polyolefins; Use thereof
- C08F2500/01—High molecular weight, e.g. >800,000 Da.
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2500/00—Characteristics or properties of obtained polyolefins; Use thereof
- C08F2500/03—Narrow molecular weight distribution, i.e. Mw/Mn < 3
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/04—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices
- H01L31/042—PV modules or arrays of single PV cells
- H01L31/048—Encapsulation of modules
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S526/00—Synthetic resins or natural rubbers -- part of the class 520 series
- Y10S526/943—Polymerization with metallocene catalysts
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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Polymerisation Methods In General (AREA)
- Polymerization Catalysts (AREA)
Description
管型反応器のモノマー注入方式を限定して同じビニルアセテートの含有量のオートクレーブ反応器および既存の管型反応器を利用した樹脂対比熱収縮率が低く透明性が向上した太陽電池封止材用シートとして用いられるEVA樹脂を製造する方法を提供することにある。
67〜76重量%のエチレンモノマーおよび24〜33重量%のビニルアセテートモノマーを管型反応器の前部分にだけ投入する段階を含み、重合温度が200〜300℃、重合圧力が2,500〜3,000kg/cm2、重合時間が2〜20分間であることを特徴とするエチレンビニルアセテート共重合体樹脂の製造方法を提供する。
前記方法によって製造された太陽電池封止材用シートとして使用するのに適したエチレンビニルアセテート共重合体樹脂を提供する。
重合温度が200〜300℃、重合圧力が2,500〜3,000kg/cm2、重合時間が2〜20分間であることを特徴とするエチレンビニルアセテート共重合体樹脂の製造方法を提供する。
本発明においてはEVA樹脂のZ平均分子量(Mz)が220,000g/mol以下であり、分子量分布(Mw/Mn)が4.3以下であり、ASTM D1238、190℃の温度下、2.16kgの荷重で測定した溶融指数は6〜35g/10分であることを特徴とする太陽電池封止材シート用EVA樹脂を提供する。
本発明の方法によりエチレンモノマー72重量%にビニルアセテートモノマー28重量%を管型反応器の前部分にだけ限定して注入し、ラジカル発生触媒としてジ−(2−エチルヘキシル)パーオキシジカーボネート(Di(2−ethylhexyl)peroxy−dicarbonate)、t−ブチルパーオキシピバレート(t−Butyl peroxy pivalate)、t−ブチルパーオキシ−2−エチルヘキサノエート(t−Butyl peroxy−2−ethylhexanoate)、テトラ−ブチルパーオキシ−3,5,5−トリメチルヘキサノエート(Tert−butyl peroxy−3,5,5−trimethylhexanoate)の混合物(重量比:20/20/30/30)1200ppmと、分子量調整剤の連鎖移動剤としてプロピオンアルデヒド(Propionaldehyde)70ppmを添加した後、高圧ポンプを用いて管型反応器(tubular reactor)に圧送し、重合圧力2650kg/cm2、重合温度235℃、重合時間10分の重合条件でEVA樹脂を製造した。
重合条件において、ラジカル発生触媒としてジ−(2−エチルヘキシル)パーオキシジカーボネート(Di(2−ethylhexyl)peroxy−dicarbonate)、t−ブチルパーオキシピバレート(t−Butyl peroxy pivalate)、t−ブチルパーオキシ−2−エチルヘキサノエート(t−Butyl peroxy−2−ethylhexanoate)、テトラ−ブチルパーオキシ−3,5,5−トリメチルヘキサノエート(Tert−butyl peroxy−3,5,5−trimethylhexanoate)、D−t−ブチルパーオキサイド(D−t−butyl peroxide)の混合物(重量比:15/20/30/30/5)1300ppmを添加したのを除いては、実施例1と同様の条件で行った。
連鎖移動剤を添加しないことを除いては、実施例1と同様の条件で行った。
重合圧力を2750kg/cm2、重合温度を245℃としたことを除いては、実施例1と同様にして製造した。
72重量%のエチレンモノマーに28重量%のビニルアセテートモノマーを管型反応器の前部分と中間部分に50/50に分けて注入し、その他の重合条件は実施例1と同様にして製造した。
72重量%のエチレンモノマーに28重量%のビニルアセテートモノマーを管型反応器の前部分と中間部分に50/50に分けて注入し、その他の重合条件は実施例2と同様にして製造した。
オートクレーブ反応器を用いた通常のEVA樹脂の製造方法でエチレンモノマーおよびビニルアセテートモノマーにラジカル発生触媒と分子量調整剤、重合圧力が2000kg/cm2以下、重合温度が220〜260℃の重合条件で製造された商業用EVA樹脂と比較した。
前記実施例1〜4および比較例1〜4で製造されたEVA樹脂の諸般物性の測定は、以下の方法および基準によって行った。
前記実施例1〜4および比較例1〜4のEVA樹脂を、スクリュー直径が40mmであり、T−ダイ幅が400mmの単軸押出機で押出機温度を100℃、スクリュー回転速度を50rpmにして、厚さが450μmのシート型フィルムを製造した。
Claims (2)
- エチレンビニルアセテート共重合体樹脂の製造方法であって、
67〜76重量%のエチレンモノマーおよび24〜33重量%のビニルアセテートモノマーを管型反応器の前部分にだけ投入する段階を含み、
重合温度が200〜300℃、重合圧力が2,500〜3,000kg/cm2、重合時間が2〜20分間であり、
パーオキサイド系開始剤混合物を50〜3,000ppmの濃度で添加する段階をさらに含み、
前記パーオキサイド系開始剤混合物は、少なくとも二種以上のパーオキサイド系開始剤を含み、この中のいずれか一つの前記パーオキサイド系開始剤に対する他の前記パーオキサイド系開始剤は重量比1:X(Xは、0<X≦8.0)で混合し、
前記二種以上のパーオキサイド系開始剤のうちの一つがジアルキルパーオキシジカーボネート系化合物であり、
前記エチレンビニルアセテート共重合体樹脂において、そのZ平均分子量(Mz)が220,000g/mol以下であり、その分子量分布(Mw/Mn)が4.3以下であり、その溶融指数がASTM D1238、190℃の温度下、2.16kgの荷重で6〜35g/10分であることを特徴とするエチレンビニルアセテート共重合体樹脂の製造方法。 - 前記パーオキサイド系開始剤混合物は、(A)ジアルキルパーオキシジカーボネート系化合物、(B)アルキルパーオキシピバレート系化合物、(C)アルキルパーオキシエチルヘキサノエート系化合物、および(D)ジアルキルパーオキサイド系化合物から選択される1種以上を(A):(B):(C):(D)=e:f:g:hの重量比率で混合した混合物であって、
前記e、f、g、hは0〜8.0の範囲内であり、少なくともeは0ではないことを特徴とする請求項1に記載のエチレンビニルアセテート共重合体樹脂の製造方法。
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KR10-2014-0192285 | 2014-12-29 | ||
KR1020140192285A KR20160080453A (ko) | 2014-12-29 | 2014-12-29 | 태양전지 봉지재 시트용 에틸렌비닐아세테이트 공중합체 수지의 제조방법 및 그 수지 |
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JP2016125053A JP2016125053A (ja) | 2016-07-11 |
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JP (1) | JP6173400B2 (ja) |
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CN (1) | CN105732871B (ja) |
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MY (1) | MY179898A (ja) |
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