TW201132651A - Method and apparatus for producing polyvinyl alcohol resin - Google Patents
Method and apparatus for producing polyvinyl alcohol resin Download PDFInfo
- Publication number
- TW201132651A TW201132651A TW99140646A TW99140646A TW201132651A TW 201132651 A TW201132651 A TW 201132651A TW 99140646 A TW99140646 A TW 99140646A TW 99140646 A TW99140646 A TW 99140646A TW 201132651 A TW201132651 A TW 201132651A
- Authority
- TW
- Taiwan
- Prior art keywords
- saponification
- catalyst
- flow path
- polyvinyl alcohol
- alcohol resin
- Prior art date
Links
- 229920005989 resin Polymers 0.000 title claims abstract description 31
- 239000011347 resin Substances 0.000 title claims abstract description 31
- 239000004372 Polyvinyl alcohol Substances 0.000 title claims abstract description 30
- 229920002451 polyvinyl alcohol Polymers 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title abstract description 17
- 238000007127 saponification reaction Methods 0.000 claims abstract description 58
- 239000003054 catalyst Substances 0.000 claims abstract description 44
- 230000003068 static effect Effects 0.000 claims abstract description 39
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 229920001290 polyvinyl ester Polymers 0.000 claims abstract description 11
- 239000003960 organic solvent Substances 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims description 24
- 238000004519 manufacturing process Methods 0.000 claims description 21
- -1 polyethylene Polymers 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 229920000573 polyethylene Polymers 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 239000004698 Polyethylene Substances 0.000 claims description 2
- 239000013064 chemical raw material Substances 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 claims 1
- 238000007689 inspection Methods 0.000 claims 1
- 238000005265 energy consumption Methods 0.000 abstract description 6
- 239000000178 monomer Substances 0.000 abstract description 5
- 229920001567 vinyl ester resin Polymers 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 4
- 230000000379 polymerizing effect Effects 0.000 abstract description 2
- 230000003247 decreasing effect Effects 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 239000002253 acid Substances 0.000 description 7
- MWKFXSUHUHTGQN-UHFFFAOYSA-N decan-1-ol Chemical compound CCCCCCCCCCO MWKFXSUHUHTGQN-UHFFFAOYSA-N 0.000 description 6
- 238000006116 polymerization reaction Methods 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- CERQOIWHTDAKMF-UHFFFAOYSA-N alpha-methacrylic acid Natural products CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 235000019441 ethanol Nutrition 0.000 description 4
- 239000000052 vinegar Substances 0.000 description 4
- 235000021419 vinegar Nutrition 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229920002689 polyvinyl acetate Polymers 0.000 description 3
- 239000011118 polyvinyl acetate Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 2
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- 238000004566 IR spectroscopy Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 229930182558 Sterol Natural products 0.000 description 2
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- RDHPKYGYEGBMSE-UHFFFAOYSA-N bromoethane Chemical compound CCBr RDHPKYGYEGBMSE-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- MTZQAGJQAFMTAQ-UHFFFAOYSA-N ethyl benzoate Chemical compound CCOC(=O)C1=CC=CC=C1 MTZQAGJQAFMTAQ-UHFFFAOYSA-N 0.000 description 2
- FKRCODPIKNYEAC-UHFFFAOYSA-N ethyl propionate Chemical compound CCOC(=O)CC FKRCODPIKNYEAC-UHFFFAOYSA-N 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 150000003432 sterols Chemical class 0.000 description 2
- 235000003702 sterols Nutrition 0.000 description 2
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 description 2
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- STMDPCBYJCIZOD-UHFFFAOYSA-N 2-(2,4-dinitroanilino)-4-methylpentanoic acid Chemical compound CC(C)CC(C(O)=O)NC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O STMDPCBYJCIZOD-UHFFFAOYSA-N 0.000 description 1
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 description 1
- WWMQIJFJSHVMDM-UHFFFAOYSA-N 2-ethenoxycarbonylbenzoic acid Chemical compound OC(=O)C1=CC=CC=C1C(=O)OC=C WWMQIJFJSHVMDM-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- 241000283690 Bos taurus Species 0.000 description 1
- FDNNBVIEXCQTIP-UHFFFAOYSA-N C(C(=C)C)(=O)O.C(CCCCCCCCC)N Chemical compound C(C(=C)C)(=O)O.C(CCCCCCCCC)N FDNNBVIEXCQTIP-UHFFFAOYSA-N 0.000 description 1
- 241000218645 Cedrus Species 0.000 description 1
- OMPIYDSYGYKWSG-UHFFFAOYSA-N Citronensaeure-alpha-aethylester Natural products CCOC(=O)CC(O)(C(O)=O)CC(O)=O OMPIYDSYGYKWSG-UHFFFAOYSA-N 0.000 description 1
- IMROMDMJAWUWLK-UHFFFAOYSA-N Ethenol Chemical compound OC=C IMROMDMJAWUWLK-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- 239000004990 Smectic liquid crystal Substances 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- DOOTYTYQINUNNV-UHFFFAOYSA-N Triethyl citrate Chemical compound CCOC(=O)CC(O)(C(=O)OCC)CC(=O)OCC DOOTYTYQINUNNV-UHFFFAOYSA-N 0.000 description 1
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 235000021028 berry Nutrition 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- LDHQCZJRKDOVOX-NSCUHMNNSA-N crotonic acid Chemical compound C\C=C\C(O)=O LDHQCZJRKDOVOX-NSCUHMNNSA-N 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- AJJDSYBLSHDIHJ-UHFFFAOYSA-N dodecanoic acid ethyl acetate Chemical compound C(C)(=O)OCC.C(CCCCCCCCCCC)(=O)O AJJDSYBLSHDIHJ-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- BLZSRIYYOIZLJL-UHFFFAOYSA-N ethenyl pentanoate Chemical compound CCCCC(=O)OC=C BLZSRIYYOIZLJL-UHFFFAOYSA-N 0.000 description 1
- ZOOODBUHSVUZEM-UHFFFAOYSA-N ethoxymethanedithioic acid Chemical group CCOC(S)=S ZOOODBUHSVUZEM-UHFFFAOYSA-N 0.000 description 1
- PVBRSNZAOAJRKO-UHFFFAOYSA-N ethyl 2-sulfanylacetate Chemical compound CCOC(=O)CS PVBRSNZAOAJRKO-UHFFFAOYSA-N 0.000 description 1
- 229940057975 ethyl citrate Drugs 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 239000003925 fat Substances 0.000 description 1
- 239000001530 fumaric acid Substances 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 125000003827 glycol group Chemical group 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 1
- 229920013716 polyethylene resin Polymers 0.000 description 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- LDHQCZJRKDOVOX-UHFFFAOYSA-N trans-crotonic acid Natural products CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 description 1
- 235000013769 triethyl citrate Nutrition 0.000 description 1
- 239000003981 vehicle Substances 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920006186 water-soluble synthetic resin Polymers 0.000 description 1
- 239000012866 water-soluble synthetic resin Substances 0.000 description 1
Classifications
-
- 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
- C08F8/00—Chemical modification by after-treatment
- C08F8/12—Hydrolysis
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2010062768A JP5545723B2 (ja) | 2010-03-18 | 2010-03-18 | ポリビニルアルコール樹脂の製造方法及び製造装置 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| TW201132651A true TW201132651A (en) | 2011-10-01 |
Family
ID=44648694
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| TW99140646A TW201132651A (en) | 2010-03-18 | 2010-11-24 | Method and apparatus for producing polyvinyl alcohol resin |
Country Status (8)
| Country | Link |
|---|---|
| US (1) | US9023287B2 (enExample) |
| EP (1) | EP2548898B1 (enExample) |
| JP (1) | JP5545723B2 (enExample) |
| CN (1) | CN102812054B (enExample) |
| ES (1) | ES2597602T3 (enExample) |
| SG (1) | SG184053A1 (enExample) |
| TW (1) | TW201132651A (enExample) |
| WO (1) | WO2011114575A1 (enExample) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI688577B (zh) * | 2014-06-04 | 2020-03-21 | 日商可樂麗股份有限公司 | 聚乙烯醇粉體及其製造方法 |
Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6122579B2 (ja) * | 2012-05-17 | 2017-04-26 | 積水化学工業株式会社 | ポリビニルアルコール樹脂フィルム材料、ポリビニルアルコール樹脂フィルム材料の製造方法及び偏光フィルムの製造方法 |
| MY195648A (en) * | 2014-07-14 | 2023-02-03 | Kuraray Co | Unmodified Polyvinyl Alcohol and Aqueous Emulsion |
| JP6446869B2 (ja) * | 2014-07-14 | 2019-01-09 | 株式会社クラレ | エチレン変性ポリビニルアルコール及び水性エマルジョン |
| JP6446870B2 (ja) * | 2014-07-14 | 2019-01-09 | 株式会社クラレ | ポリビニルアルコール及び水性エマルジョン |
| US9868574B2 (en) | 2014-09-01 | 2018-01-16 | Sekisui Chemical Co., Ltd. | Water-soluble packaging film |
| US11020353B2 (en) | 2014-11-05 | 2021-06-01 | Japan Vam & Poval Co., Ltd. | Film coating composition, solid oral formulation, and method for producing the same |
| US9963520B2 (en) | 2014-12-26 | 2018-05-08 | Kuraray Co., Ltd. | Aqueous emulsion and adhesive in which same is used |
| JP2017043872A (ja) * | 2015-08-28 | 2017-03-02 | 株式会社クラレ | 紙用コーティング剤 |
| JP7517329B2 (ja) * | 2019-03-29 | 2024-07-17 | 三菱ケミカル株式会社 | ポリビニルアルコール系樹脂の製造方法 |
| KR102743558B1 (ko) * | 2019-09-03 | 2024-12-17 | 주식회사 엘지화학 | 폴리비닐알코올의 분자량에 따른 검화도 분포 분석을 위한 방법 및 시스템 |
| JP7471859B2 (ja) * | 2020-02-27 | 2024-04-22 | 株式会社クラレ | ポリビニルアルコール系樹脂及び地下処理用目止め剤 |
| JP7604516B2 (ja) * | 2020-11-11 | 2024-12-23 | 株式会社クラレ | 光学フィルム製造用フィルム及び光学フィルムの製造方法 |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA847445A (en) * | 1970-07-21 | Mueller Wilhelm | Process for the manufacture of polyvinyl alcohol | |
| JPS5545562B2 (enExample) * | 1972-03-30 | 1980-11-18 | ||
| JPS4899290A (enExample) * | 1972-03-30 | 1973-12-15 | ||
| US4338405A (en) * | 1980-12-12 | 1982-07-06 | E. I. Du Pont De Nemours And Company | Process for continuous controlled alcoholysis of polyvinyl acetate |
| JP4717177B2 (ja) | 1999-06-09 | 2011-07-06 | 株式会社クラレ | ポリビニルアルコール系重合体の製造方法及びポリビニルアルコール系重合体 |
| JP2000355611A (ja) | 1999-06-15 | 2000-12-26 | Kuraray Co Ltd | 塔型鹸化反応器 |
| US7629419B2 (en) | 2001-10-16 | 2009-12-08 | Sekisui Chemical Co., Ltd. | Process for producing modified polymer, apparatus for producing modified polymer, and modified polymer |
| KR100759188B1 (ko) | 2005-10-28 | 2007-09-14 | 주식회사 엘지화학 | 고중합도를 갖는 폴리비닐알코올의 제조방법 및 제조장치 |
-
2010
- 2010-03-18 JP JP2010062768A patent/JP5545723B2/ja active Active
- 2010-11-12 WO PCT/JP2010/070174 patent/WO2011114575A1/ja not_active Ceased
- 2010-11-12 EP EP10847981.7A patent/EP2548898B1/en active Active
- 2010-11-12 CN CN201080065467.4A patent/CN102812054B/zh active Active
- 2010-11-12 SG SG2012067914A patent/SG184053A1/en unknown
- 2010-11-12 US US13/634,331 patent/US9023287B2/en active Active
- 2010-11-12 ES ES10847981.7T patent/ES2597602T3/es active Active
- 2010-11-24 TW TW99140646A patent/TW201132651A/zh unknown
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI688577B (zh) * | 2014-06-04 | 2020-03-21 | 日商可樂麗股份有限公司 | 聚乙烯醇粉體及其製造方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2011114575A1 (ja) | 2011-09-22 |
| ES2597602T3 (es) | 2017-01-19 |
| US20120329950A1 (en) | 2012-12-27 |
| CN102812054B (zh) | 2014-08-27 |
| EP2548898B1 (en) | 2016-08-24 |
| JP5545723B2 (ja) | 2014-07-09 |
| EP2548898A4 (en) | 2014-11-26 |
| SG184053A1 (en) | 2012-10-30 |
| EP2548898A1 (en) | 2013-01-23 |
| CN102812054A (zh) | 2012-12-05 |
| JP2011195672A (ja) | 2011-10-06 |
| US9023287B2 (en) | 2015-05-05 |
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