JP2011527717A - エチレン／テトラフルオロエチレンコポリマーの水分散液重合方法 - Google Patents
エチレン／テトラフルオロエチレンコポリマーの水分散液重合方法 Download PDFInfo
- Publication number
- JP2011527717A JP2011527717A JP2011517464A JP2011517464A JP2011527717A JP 2011527717 A JP2011527717 A JP 2011527717A JP 2011517464 A JP2011517464 A JP 2011517464A JP 2011517464 A JP2011517464 A JP 2011517464A JP 2011527717 A JP2011527717 A JP 2011527717A
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- JP
- Japan
- Prior art keywords
- polymerization
- polymer
- weight
- copolymer
- dispersion
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000006116 polymerization reaction Methods 0.000 title claims abstract description 68
- 229920001577 copolymer Polymers 0.000 title claims abstract description 49
- 239000006185 dispersion Substances 0.000 title claims abstract description 40
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 239000005977 Ethylene Substances 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title description 9
- 229920000642 polymer Polymers 0.000 claims abstract description 103
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims abstract description 61
- 239000000178 monomer Substances 0.000 claims abstract description 56
- 239000002245 particle Substances 0.000 claims abstract description 52
- -1 ethylene, tetrafluoroethylene Chemical group 0.000 claims abstract description 25
- 239000012736 aqueous medium Substances 0.000 claims abstract description 23
- 239000007787 solid Substances 0.000 claims abstract description 17
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 14
- 230000000977 initiatory effect Effects 0.000 claims abstract description 5
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 35
- 239000003999 initiator Substances 0.000 claims description 19
- 230000008569 process Effects 0.000 claims description 10
- 125000003709 fluoroalkyl group Chemical group 0.000 claims description 7
- 239000003960 organic solvent Substances 0.000 claims description 7
- 239000004094 surface-active agent Substances 0.000 claims description 6
- 150000003254 radicals Chemical class 0.000 claims description 3
- 125000000962 organic group Chemical group 0.000 claims description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 41
- 239000004810 polytetrafluoroethylene Substances 0.000 description 41
- 229920002554 vinyl polymer Polymers 0.000 description 32
- 229920002313 fluoropolymer Polymers 0.000 description 29
- 239000004811 fluoropolymer Substances 0.000 description 29
- 229920000840 ethylene tetrafluoroethylene copolymer Polymers 0.000 description 28
- 239000000203 mixture Substances 0.000 description 18
- 229920005548 perfluoropolymer Polymers 0.000 description 17
- 239000011159 matrix material Substances 0.000 description 16
- 239000000155 melt Substances 0.000 description 12
- 239000000843 powder Substances 0.000 description 11
- 238000013019 agitation Methods 0.000 description 10
- 238000007334 copolymerization reaction Methods 0.000 description 10
- FJKIXWOMBXYWOQ-UHFFFAOYSA-N ethenoxyethane Chemical compound CCOC=C FJKIXWOMBXYWOQ-UHFFFAOYSA-N 0.000 description 10
- 239000002609 medium Substances 0.000 description 10
- 238000002156 mixing Methods 0.000 description 10
- 239000000243 solution Substances 0.000 description 10
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 7
- 229910052760 oxygen Inorganic materials 0.000 description 7
- 239000001301 oxygen Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- YOALFLHFSFEMLP-UHFFFAOYSA-N azane;2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-pentadecafluorooctanoic acid Chemical compound [NH4+].[O-]C(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F YOALFLHFSFEMLP-UHFFFAOYSA-N 0.000 description 6
- GVEUEBXMTMZVSD-UHFFFAOYSA-N 3,3,4,4,5,5,6,6,6-nonafluorohex-1-ene Chemical group FC(F)(F)C(F)(F)C(F)(F)C(F)(F)C=C GVEUEBXMTMZVSD-UHFFFAOYSA-N 0.000 description 5
- 238000012674 dispersion polymerization Methods 0.000 description 5
- 238000002844 melting Methods 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- HCDGVLDPFQMKDK-UHFFFAOYSA-N hexafluoropropylene Chemical group FC(F)=C(F)C(F)(F)F HCDGVLDPFQMKDK-UHFFFAOYSA-N 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 239000003607 modifier Substances 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 230000007704 transition Effects 0.000 description 4
- OVGRCEFMXPHEBL-UHFFFAOYSA-N 1-ethenoxypropane Chemical compound CCCOC=C OVGRCEFMXPHEBL-UHFFFAOYSA-N 0.000 description 3
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 3
- 238000005452 bending Methods 0.000 description 3
- 239000012986 chain transfer agent Substances 0.000 description 3
- 230000006835 compression Effects 0.000 description 3
- 238000007906 compression Methods 0.000 description 3
- 230000009969 flowable effect Effects 0.000 description 3
- 239000010702 perfluoropolyether Substances 0.000 description 3
- 239000012286 potassium permanganate Substances 0.000 description 3
- 239000011164 primary particle Substances 0.000 description 3
- 239000011163 secondary particle Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- 239000004254 Ammonium phosphate Substances 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 2
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 2
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 2
- 235000019289 ammonium phosphates Nutrition 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 150000001735 carboxylic acids Chemical class 0.000 description 2
- 230000015271 coagulation Effects 0.000 description 2
- 238000005345 coagulation Methods 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000000748 compression moulding Methods 0.000 description 2
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- 229920001519 homopolymer Polymers 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 235000006408 oxalic acid Nutrition 0.000 description 2
- 125000005010 perfluoroalkyl group Chemical group 0.000 description 2
- 239000003505 polymerization initiator Substances 0.000 description 2
- RWPGFSMJFRPDDP-UHFFFAOYSA-L potassium metabisulfite Chemical compound [K+].[K+].[O-]S(=O)S([O-])(=O)=O RWPGFSMJFRPDDP-UHFFFAOYSA-L 0.000 description 2
- 235000010263 potassium metabisulphite Nutrition 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- 238000010257 thawing Methods 0.000 description 2
- KHXKESCWFMPTFT-UHFFFAOYSA-N 1,1,1,2,2,3,3-heptafluoro-3-(1,2,2-trifluoroethenoxy)propane Chemical compound FC(F)=C(F)OC(F)(F)C(F)(F)C(F)(F)F KHXKESCWFMPTFT-UHFFFAOYSA-N 0.000 description 1
- QMIWYOZFFSLIAK-UHFFFAOYSA-N 3,3,3-trifluoro-2-(trifluoromethyl)prop-1-ene Chemical group FC(F)(F)C(=C)C(F)(F)F QMIWYOZFFSLIAK-UHFFFAOYSA-N 0.000 description 1
- JYLNVJYYQQXNEK-UHFFFAOYSA-N 3-amino-2-(4-chlorophenyl)-1-propanesulfonic acid Chemical compound OS(=O)(=O)CC(CN)C1=CC=C(Cl)C=C1 JYLNVJYYQQXNEK-UHFFFAOYSA-N 0.000 description 1
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 238000007630 basic procedure Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000001112 coagulating effect Effects 0.000 description 1
- 230000001143 conditioned effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 230000003635 deoxygenating effect Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 239000004815 dispersion polymer Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 125000001153 fluoro group Chemical group F* 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 238000002356 laser light scattering Methods 0.000 description 1
- 150000002696 manganese Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- XJRBAMWJDBPFIM-UHFFFAOYSA-N methyl vinyl ether Chemical compound COC=C XJRBAMWJDBPFIM-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical class [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 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
- C08F259/00—Macromolecular compounds obtained by polymerising monomers on to polymers of halogen containing monomers as defined in group C08F14/00
- C08F259/08—Macromolecular compounds obtained by polymerising monomers on to polymers of halogen containing monomers as defined in group C08F14/00 on to polymers containing fluorine
-
- 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
-
- 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
- C08K5/10—Esters; Ether-esters
- C08K5/101—Esters; Ether-esters of monocarboxylic acids
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Graft Or Block Polymers (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Polymerisation Methods In General (AREA)
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US7950608P | 2008-07-10 | 2008-07-10 | |
| US61/079,506 | 2008-07-10 | ||
| PCT/US2009/048593 WO2010005792A1 (en) | 2008-07-10 | 2009-06-25 | Aqueous dispersion polymerization process for ethylene/tetrafluoroethylene copolymer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2011527717A true JP2011527717A (ja) | 2011-11-04 |
| JP2011527717A5 JP2011527717A5 (enExample) | 2012-07-26 |
Family
ID=41137813
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2011517464A Pending JP2011527717A (ja) | 2008-07-10 | 2009-06-25 | エチレン／テトラフルオロエチレンコポリマーの水分散液重合方法 |
Country Status (4)
| Country | Link |
|---|---|
| US (1) | US20110092644A1 (enExample) |
| JP (1) | JP2011527717A (enExample) |
| GB (1) | GB2472734A (enExample) |
| WO (1) | WO2010005792A1 (enExample) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPWO2024128265A1 (enExample) * | 2022-12-16 | 2024-06-20 |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110092614A1 (en) * | 2008-07-10 | 2011-04-21 | E. I. Dupont Denemours And Company | Applications of ethylene/terafluoroethylene copolymer |
| US20100036053A1 (en) * | 2008-08-08 | 2010-02-11 | E.I. Du Pont De Nemours And Company | Aqueous Polymerization Process for the Manufacture of Fluoropolymer Comprising Repeating Units Arising from a Perfluoromonomer and a Monomer Having a Functional Group and a Polymerizable Carbon-Carbon Double Bond |
| EP4073128A1 (en) | 2019-12-12 | 2022-10-19 | Solvay Specialty Polymers Italy S.p.A. | Method for manufacturing fluoropolymers |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02158651A (ja) * | 1988-12-12 | 1990-06-19 | Daikin Ind Ltd | 含フッ素重合体水性分散体および含フッ素重合体オルガノゾル組成物 |
| JPH08100033A (ja) * | 1994-07-12 | 1996-04-16 | Hoechst Ag | コア／シェル粒子構造を有するテトラフルオロエチレン−エチレン系コポリマー |
| JP2009516067A (ja) * | 2005-11-18 | 2009-04-16 | イー・アイ・デュポン・ドウ・ヌムール・アンド・カンパニー | コア／シェルポリマー |
| JP2009516066A (ja) * | 2005-11-18 | 2009-04-16 | イー・アイ・デュポン・ドウ・ヌムール・アンド・カンパニー | フルオロポリマー組成物 |
| JP2012503677A (ja) * | 2008-07-10 | 2012-02-09 | イー・アイ・デュポン・ドウ・ヌムール・アンド・カンパニー | エチレン／テトラフルオロエチレンコポリマーの応用 |
Family Cites Families (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3142665A (en) * | 1960-07-26 | 1964-07-28 | Du Pont | Novel tetrafluoroethylene resins and their preparation |
| US3624250A (en) * | 1970-01-20 | 1971-11-30 | Du Pont | Copolymers of ethylene/tetrafluoroethylene and of ethylene/chlorotrifluoroethylene |
| DE2037028C2 (de) * | 1970-07-25 | 1982-07-08 | Hoechst Ag, 6000 Frankfurt | Verfahren zur Herstellung fluorhaltiger Copolymerisate |
| US3819594A (en) * | 1972-05-17 | 1974-06-25 | Du Pont | Tetrafluoroethylene fine powder resin of a copolymer of tetrafluoroethylene and perfluoro(alkyl vinyl ether) |
| US4123602A (en) * | 1976-05-24 | 1978-10-31 | Asahi Glass Company, Ltd. | Terpolymers of tetrafluoroethylene, ethylene and perfluoroalkyl vinyl monomer and process for producing the same |
| DE3024450A1 (de) * | 1980-06-28 | 1982-01-28 | Hoechst Ag, 6000 Frankfurt | Verfahren zur herstellung von waessrigen, kolloidalen dispersionen von copolymerisaten des typs tetrafluorethylen-ethylen |
| US4469846A (en) * | 1983-05-20 | 1984-09-04 | E. I. Du Pont De Nemours And Company | Core/shell fluoropolymer compositions |
| JPS60248710A (ja) * | 1984-05-22 | 1985-12-09 | Daikin Ind Ltd | 新規エチレン／テトラフルオロエチレン系共重合体 |
| US5543217A (en) * | 1995-02-06 | 1996-08-06 | E. I. Du Pont De Nemours And Company | Amorphous copolymers of tetrafluoroethylene and hexafluoropropylene |
| US6395848B1 (en) * | 1999-05-20 | 2002-05-28 | E. I. Du Pont De Nemours And Company | Polymerization of fluoromonomers |
| US6841594B2 (en) * | 2002-01-04 | 2005-01-11 | E. I. Du Pont De Nemours And Company | Core-shell fluoropolymer dispersions |
| US6870020B2 (en) * | 2002-04-30 | 2005-03-22 | E. I. Du Pont De Nemours And Company | High vinyl ether modified sinterable polytetrafluoroethylene |
| US7612139B2 (en) * | 2005-05-20 | 2009-11-03 | E.I. Du Pont De Nemours And Company | Core/shell fluoropolymer dispersions with low fluorosurfactant content |
| US20110092614A1 (en) * | 2008-07-10 | 2011-04-21 | E. I. Dupont Denemours And Company | Applications of ethylene/terafluoroethylene copolymer |
-
2009
- 2009-06-25 US US12/999,416 patent/US20110092644A1/en not_active Abandoned
- 2009-06-25 GB GB1020394A patent/GB2472734A/en not_active Withdrawn
- 2009-06-25 JP JP2011517464A patent/JP2011527717A/ja active Pending
- 2009-06-25 WO PCT/US2009/048593 patent/WO2010005792A1/en not_active Ceased
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02158651A (ja) * | 1988-12-12 | 1990-06-19 | Daikin Ind Ltd | 含フッ素重合体水性分散体および含フッ素重合体オルガノゾル組成物 |
| JPH08100033A (ja) * | 1994-07-12 | 1996-04-16 | Hoechst Ag | コア／シェル粒子構造を有するテトラフルオロエチレン−エチレン系コポリマー |
| JP2009516067A (ja) * | 2005-11-18 | 2009-04-16 | イー・アイ・デュポン・ドウ・ヌムール・アンド・カンパニー | コア／シェルポリマー |
| JP2009516066A (ja) * | 2005-11-18 | 2009-04-16 | イー・アイ・デュポン・ドウ・ヌムール・アンド・カンパニー | フルオロポリマー組成物 |
| JP2012503677A (ja) * | 2008-07-10 | 2012-02-09 | イー・アイ・デュポン・ドウ・ヌムール・アンド・カンパニー | エチレン／テトラフルオロエチレンコポリマーの応用 |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPWO2024128265A1 (enExample) * | 2022-12-16 | 2024-06-20 | ||
| WO2024128265A1 (ja) * | 2022-12-16 | 2024-06-20 | Ａｇｃ株式会社 | 含フッ素重合体の製造方法、水性分散液及び粒子 |
| JP7643649B2 (ja) | 2022-12-16 | 2025-03-11 | Ａｇｃ株式会社 | 含フッ素重合体の製造方法、水性分散液及び粒子 |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2010005792A1 (en) | 2010-01-14 |
| GB2472734A (en) | 2011-02-16 |
| GB201020394D0 (en) | 2011-01-12 |
| US20110092644A1 (en) | 2011-04-21 |
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