RU2438970C2 - Улучшенный способ очистки безводного газообразного хлороводорода - Google Patents
Улучшенный способ очистки безводного газообразного хлороводорода Download PDFInfo
- Publication number
- RU2438970C2 RU2438970C2 RU2008148885/05A RU2008148885A RU2438970C2 RU 2438970 C2 RU2438970 C2 RU 2438970C2 RU 2008148885/05 A RU2008148885/05 A RU 2008148885/05A RU 2008148885 A RU2008148885 A RU 2008148885A RU 2438970 C2 RU2438970 C2 RU 2438970C2
- Authority
- RU
- Russia
- Prior art keywords
- stream
- gas
- hydrogen chloride
- heat exchanger
- column
- Prior art date
Links
- 239000007789 gas Substances 0.000 title claims abstract description 119
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 238000000034 method Methods 0.000 title claims abstract description 45
- 238000004140 cleaning Methods 0.000 title abstract 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 65
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims abstract description 65
- 239000000356 contaminant Substances 0.000 claims abstract description 42
- 238000004821 distillation Methods 0.000 claims abstract description 38
- 238000001816 cooling Methods 0.000 claims abstract description 22
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 15
- 238000009835 boiling Methods 0.000 claims abstract description 14
- 239000012535 impurity Substances 0.000 claims abstract description 13
- 239000002826 coolant Substances 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims description 25
- 239000013618 particulate matter Substances 0.000 claims description 16
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 12
- 239000000460 chlorine Substances 0.000 claims description 12
- 229910052801 chlorine Inorganic materials 0.000 claims description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 9
- 230000004907 flux Effects 0.000 claims description 6
- 238000005187 foaming Methods 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 150000001491 aromatic compounds Chemical class 0.000 claims description 4
- 239000012141 concentrate Substances 0.000 claims description 4
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical group ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 239000012948 isocyanate Substances 0.000 abstract description 8
- 150000002513 isocyanates Chemical class 0.000 abstract description 8
- 239000000126 substance Substances 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 230000008569 process Effects 0.000 description 15
- 239000006227 byproduct Substances 0.000 description 5
- 239000002699 waste material Substances 0.000 description 5
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 4
- 238000009833 condensation Methods 0.000 description 4
- 230000005494 condensation Effects 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- OCJBOOLMMGQPQU-UHFFFAOYSA-N 1,4-dichlorobenzene Chemical compound ClC1=CC=C(Cl)C=C1 OCJBOOLMMGQPQU-UHFFFAOYSA-N 0.000 description 3
- 238000007138 Deacon process reaction Methods 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 229940117389 dichlorobenzene Drugs 0.000 description 3
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 description 2
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 description 2
- 239000005057 Hexamethylene diisocyanate Substances 0.000 description 2
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 2
- 239000000443 aerosol Substances 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- 239000004814 polyurethane Substances 0.000 description 2
- 229920002635 polyurethane Polymers 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical compound ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 description 1
- GNFTZDOKVXKIBK-UHFFFAOYSA-N 3-(2-methoxyethoxy)benzohydrazide Chemical compound COCCOC1=CC=CC(C(=O)NN)=C1 GNFTZDOKVXKIBK-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 150000007938 chlorocyclic compounds Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 150000004816 dichlorobenzenes Chemical class 0.000 description 1
- -1 for example Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- DKAGJZJALZXOOV-UHFFFAOYSA-N hydrate;hydrochloride Chemical compound O.Cl DKAGJZJALZXOOV-UHFFFAOYSA-N 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
- C01B7/0712—Purification ; Separation of hydrogen chloride by distillation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Separation By Low-Temperature Treatments (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Hydrogen, Water And Hydrids (AREA)
- Catalysts (AREA)
- Detergent Compositions (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US11/433,809 US20070261437A1 (en) | 2006-05-12 | 2006-05-12 | Enhanced process for the purification of anhydrous hydrogen chloride gas |
| US11/433,809 | 2006-05-12 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| RU2008148885A RU2008148885A (ru) | 2010-06-20 |
| RU2438970C2 true RU2438970C2 (ru) | 2012-01-10 |
Family
ID=38683841
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| RU2008148885/05A RU2438970C2 (ru) | 2006-05-12 | 2007-04-30 | Улучшенный способ очистки безводного газообразного хлороводорода |
Country Status (13)
| Country | Link |
|---|---|
| US (1) | US20070261437A1 (enExample) |
| EP (1) | EP2021275B1 (enExample) |
| JP (1) | JP5303453B2 (enExample) |
| KR (1) | KR101332914B1 (enExample) |
| CN (1) | CN101448738B (enExample) |
| AT (1) | ATE502898T1 (enExample) |
| DE (1) | DE602007013388D1 (enExample) |
| ES (1) | ES2362019T3 (enExample) |
| PL (1) | PL2021275T3 (enExample) |
| PT (1) | PT2021275E (enExample) |
| RU (1) | RU2438970C2 (enExample) |
| TW (1) | TWI387558B (enExample) |
| WO (1) | WO2007131623A2 (enExample) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2838447C1 (ru) * | 2024-09-05 | 2025-04-16 | Общество С Ограниченной Ответственностью "Инк-Литий" | Способ получения сжатого влажного хлора и устройство для его осуществления |
Families Citing this family (24)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102007016973A1 (de) * | 2007-04-10 | 2008-10-16 | Bayer Materialscience Ag | Regenerativer Adsorptionsprozess zur Entfernung organischer Komponenten aus einem Gasstrom |
| DE102007020144A1 (de) * | 2007-04-26 | 2008-10-30 | Bayer Materialscience Ag | Kondensations-Adsorptionsprozess zur Entfernung organischer Komponenten aus einem Chlorwasserstoff enthaltenden Gasstrom |
| KR20120041257A (ko) * | 2009-08-11 | 2012-04-30 | 바스프 에스이 | 기상 포스겐화에 의한 디이소시아네이트의 제조 방법 |
| CN101817506B (zh) * | 2010-03-22 | 2011-07-20 | 临沭县华盛化工有限公司 | 原甲酸三乙酯生产中所用氯化氢气体的纯化方法 |
| EP2559658A1 (en) * | 2011-08-19 | 2013-02-20 | Huntsman International LLC | A process to separate phosgene and hydrogen chloride from a fluid stream comprising phosgene and hydrogen chloride |
| EP2559659A1 (en) * | 2011-08-19 | 2013-02-20 | Huntsman International Llc | A process for separating hydrogen chloride gas out of a mixture of hydrogen chloride and phosgene |
| MY156181A (en) * | 2011-10-11 | 2016-01-15 | Hong In Chemical Co Ltd | Method and system for producing high-purity hydrogen chloride |
| CN104755458B (zh) * | 2012-10-24 | 2017-06-20 | 巴斯夫欧洲公司 | 通过在液相中光气化胺制备异氰酸酯的方法 |
| JPWO2014185499A1 (ja) * | 2013-05-15 | 2017-02-23 | 旭硝子株式会社 | 塩化水素の精製方法 |
| KR101470311B1 (ko) * | 2013-07-24 | 2014-12-08 | 코아텍주식회사 | 공업용 암모니아 정제장치 |
| PT2949622T (pt) * | 2014-05-27 | 2022-05-02 | Covestro Intellectual Property Gmbh & Co Kg | Processo para processar cloreto de hidrogénio a partir da produção de isocianatos |
| PT3268349T (pt) | 2015-03-12 | 2020-04-02 | Basf Se | Processo para a separação de um fluxo de material contendo fosgénio e cloreto de hidrogénio |
| HUE046418T2 (hu) * | 2015-06-29 | 2020-03-30 | Covestro Deutschland Ag | Eljárás kémiai átalakításokhoz hidrogénklorid biztosítására |
| KR102019704B1 (ko) | 2015-08-10 | 2019-09-09 | 쇼와 덴코 가부시키가이샤 | 염화수소의 제조 방법 |
| EP3352896B1 (de) | 2015-09-24 | 2019-10-23 | Covestro Deutschland AG | Verfahren zur herstellung von isocyanaten |
| WO2017055311A1 (de) | 2015-09-30 | 2017-04-06 | Covestro Deutschland Ag | Verfahren zur herstellung von isocyanaten |
| CN107556215B (zh) * | 2016-06-30 | 2022-04-19 | 科思创德国股份有限公司 | 从氯化氢液体混合物中分离和处理杂质的方法和系统 |
| HUE053496T2 (hu) | 2016-09-01 | 2021-07-28 | Covestro Intellectual Property Gmbh & Co Kg | Eljárás izocianátok elõállítására |
| US11365172B2 (en) | 2017-07-03 | 2022-06-21 | Covestro Deutschland Ag | Production plant for producing a chemical product by reacting H-functional reactants with phosgene, and method for operating same with an interruption to production |
| CN109110732A (zh) * | 2018-09-11 | 2019-01-01 | 安徽东至广信农化有限公司 | 氯化苯生产工艺中用于降低副产物盐酸中有害物质的方法 |
| DE102019204498A1 (de) * | 2019-03-29 | 2020-10-01 | Sgl Carbon Se | HCl-Rückgewinnungseinheit |
| CN210683206U (zh) * | 2019-07-04 | 2020-06-05 | 南通星球石墨设备有限公司 | 一种废酸处理系统 |
| KR102666415B1 (ko) * | 2020-12-14 | 2024-05-17 | 한화솔루션 주식회사 | 염소화 반응의 HCl 제거방법 |
| KR102839458B1 (ko) * | 2020-12-30 | 2025-07-25 | 한화솔루션 주식회사 | 이소시아네이트 화합물의 제조 방법 |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU906364A3 (ru) * | 1978-02-13 | 1982-02-15 | Хемище Верке Хюльс Аг (Фирма) | Способ одновременного получени три- или диалкиламинов с @ и хлористого водорода |
| GB2140014A (en) * | 1983-05-18 | 1984-11-21 | Inst Ciezkiej Syntezy Orga | Separating hydrogen chloride from an allyl chloride reaction mixture |
| US4935220A (en) * | 1988-05-17 | 1990-06-19 | Wacker-Chemie Gmbh | Process for purifying crude gaseous hydrogen chloride |
| EP1149861A1 (en) * | 2000-04-28 | 2001-10-31 | Tosoh Corporation | Method for recovering hydrogen chloride from chlorine based waste and use of recovered hydrogen chloride |
| US6719957B2 (en) * | 2002-04-17 | 2004-04-13 | Bayer Corporation | Process for purification of anhydrous hydrogen chloride gas |
| WO2004056758A1 (de) * | 2002-12-19 | 2004-07-08 | Basf Aktiengesellschaft | Auftrennung eines stoffgemisches aus chlorwasserstoff und phosgen |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3508371A1 (de) * | 1985-03-08 | 1986-09-11 | Wacker Chemie Gmbh | Verfahren zur nachreinigung von chlorwasserstoff aus einer 1,2-dichlorethan-pyrolyse |
| JPH0742085B2 (ja) * | 1986-08-20 | 1995-05-10 | ダイセル化学工業株式会社 | 塩化水素ガスの精製方法 |
| DE3832804A1 (de) * | 1988-09-28 | 1990-03-29 | Hoechst Ag | Verfahren zur herstellung von aox-armer, chlorfreier salzsaeure |
| US5799507A (en) * | 1996-10-25 | 1998-09-01 | Elcor Corporation | Hydrocarbon gas processing |
| JP2006290757A (ja) * | 2005-04-07 | 2006-10-26 | Sumitomo Chemical Co Ltd | 芳香族化合物の分離・回収方法 |
| JP2006290649A (ja) * | 2005-04-07 | 2006-10-26 | Sumitomo Chemical Co Ltd | 塩化水素の分離・回収方法 |
-
2006
- 2006-05-12 US US11/433,809 patent/US20070261437A1/en not_active Abandoned
-
2007
- 2007-04-30 KR KR1020087027568A patent/KR101332914B1/ko not_active Expired - Fee Related
- 2007-04-30 DE DE602007013388T patent/DE602007013388D1/de active Active
- 2007-04-30 JP JP2009508195A patent/JP5303453B2/ja not_active Expired - Fee Related
- 2007-04-30 ES ES07724740T patent/ES2362019T3/es active Active
- 2007-04-30 RU RU2008148885/05A patent/RU2438970C2/ru not_active IP Right Cessation
- 2007-04-30 AT AT07724740T patent/ATE502898T1/de not_active IP Right Cessation
- 2007-04-30 CN CN2007800172612A patent/CN101448738B/zh not_active Expired - Fee Related
- 2007-04-30 PT PT07724740T patent/PT2021275E/pt unknown
- 2007-04-30 PL PL07724740T patent/PL2021275T3/pl unknown
- 2007-04-30 EP EP07724740A patent/EP2021275B1/en not_active Not-in-force
- 2007-04-30 WO PCT/EP2007/003813 patent/WO2007131623A2/en not_active Ceased
- 2007-05-11 TW TW096116733A patent/TWI387558B/zh not_active IP Right Cessation
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU906364A3 (ru) * | 1978-02-13 | 1982-02-15 | Хемище Верке Хюльс Аг (Фирма) | Способ одновременного получени три- или диалкиламинов с @ и хлористого водорода |
| GB2140014A (en) * | 1983-05-18 | 1984-11-21 | Inst Ciezkiej Syntezy Orga | Separating hydrogen chloride from an allyl chloride reaction mixture |
| US4935220A (en) * | 1988-05-17 | 1990-06-19 | Wacker-Chemie Gmbh | Process for purifying crude gaseous hydrogen chloride |
| EP1149861A1 (en) * | 2000-04-28 | 2001-10-31 | Tosoh Corporation | Method for recovering hydrogen chloride from chlorine based waste and use of recovered hydrogen chloride |
| US6719957B2 (en) * | 2002-04-17 | 2004-04-13 | Bayer Corporation | Process for purification of anhydrous hydrogen chloride gas |
| WO2004056758A1 (de) * | 2002-12-19 | 2004-07-08 | Basf Aktiengesellschaft | Auftrennung eines stoffgemisches aus chlorwasserstoff und phosgen |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2838447C1 (ru) * | 2024-09-05 | 2025-04-16 | Общество С Ограниченной Ответственностью "Инк-Литий" | Способ получения сжатого влажного хлора и устройство для его осуществления |
Also Published As
| Publication number | Publication date |
|---|---|
| KR20090009239A (ko) | 2009-01-22 |
| ES2362019T3 (es) | 2011-06-27 |
| PL2021275T3 (pl) | 2011-09-30 |
| CN101448738A (zh) | 2009-06-03 |
| TW200815285A (en) | 2008-04-01 |
| PT2021275E (pt) | 2011-06-01 |
| ATE502898T1 (de) | 2011-04-15 |
| US20070261437A1 (en) | 2007-11-15 |
| EP2021275B1 (en) | 2011-03-23 |
| JP5303453B2 (ja) | 2013-10-02 |
| EP2021275A2 (en) | 2009-02-11 |
| JP2009536913A (ja) | 2009-10-22 |
| WO2007131623A2 (en) | 2007-11-22 |
| RU2008148885A (ru) | 2010-06-20 |
| DE602007013388D1 (de) | 2011-05-05 |
| TWI387558B (zh) | 2013-03-01 |
| WO2007131623A3 (en) | 2008-06-19 |
| CN101448738B (zh) | 2013-03-27 |
| KR101332914B1 (ko) | 2013-11-26 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| MM4A | The patent is invalid due to non-payment of fees |
Effective date: 20120501 |