UA82774C2 - Способ получения сорбента на основе гидрогеля метилкремниевой кислоты - Google Patents
Способ получения сорбента на основе гидрогеля метилкремниевой кислоты Download PDFInfo
- Publication number
- UA82774C2 UA82774C2 UAA200610083A UAA200610083A UA82774C2 UA 82774 C2 UA82774 C2 UA 82774C2 UA A200610083 A UAA200610083 A UA A200610083A UA A200610083 A UAA200610083 A UA A200610083A UA 82774 C2 UA82774 C2 UA 82774C2
- Authority
- UA
- Ukraine
- Prior art keywords
- product
- water
- hydrogel
- methylsilicic
- methylsilicic acid
- Prior art date
Links
- 238000000034 method Methods 0.000 title abstract description 8
- 239000004215 Carbon black (E152) Substances 0.000 title abstract 2
- 239000003795 chemical substances by application Substances 0.000 title abstract 2
- 229930195733 hydrocarbon Natural products 0.000 title abstract 2
- -1 methylsilicic acid hydrocarbon Chemical class 0.000 title abstract 2
- 239000002253 acid Substances 0.000 abstract description 9
- 239000000126 substance Substances 0.000 abstract description 7
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052700 potassium Inorganic materials 0.000 abstract description 4
- 239000011591 potassium Substances 0.000 abstract description 4
- GBPOWOIWSYUZMH-UHFFFAOYSA-N sodium;trihydroxy(methyl)silane Chemical compound [Na+].C[Si](O)(O)O GBPOWOIWSYUZMH-UHFFFAOYSA-N 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 230000007935 neutral effect Effects 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 239000002594 sorbent Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 37
- 239000000017 hydrogel Substances 0.000 description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 24
- FXSGDOZPBLGOIN-UHFFFAOYSA-N trihydroxy(methoxy)silane Chemical compound CO[Si](O)(O)O FXSGDOZPBLGOIN-UHFFFAOYSA-N 0.000 description 23
- 239000000654 additive Substances 0.000 description 11
- 239000000725 suspension Substances 0.000 description 9
- 239000003755 preservative agent Substances 0.000 description 8
- 239000000243 solution Substances 0.000 description 7
- 238000001179 sorption measurement Methods 0.000 description 7
- 235000003599 food sweetener Nutrition 0.000 description 6
- 230000002335 preservative effect Effects 0.000 description 6
- 239000003765 sweetening agent Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 229910000365 copper sulfate Inorganic materials 0.000 description 4
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 235000011837 pasties Nutrition 0.000 description 4
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 4
- 229910000368 zinc sulfate Inorganic materials 0.000 description 4
- 229960001763 zinc sulfate Drugs 0.000 description 4
- 239000004376 Sucralose Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 239000000499 gel Substances 0.000 description 3
- 238000000265 homogenisation Methods 0.000 description 3
- 239000006072 paste Substances 0.000 description 3
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 3
- 235000010234 sodium benzoate Nutrition 0.000 description 3
- 239000004299 sodium benzoate Substances 0.000 description 3
- BAQAVOSOZGMPRM-QBMZZYIRSA-N sucralose Chemical compound O[C@@H]1[C@@H](O)[C@@H](Cl)[C@@H](CO)O[C@@H]1O[C@@]1(CCl)[C@@H](O)[C@H](O)[C@@H](CCl)O1 BAQAVOSOZGMPRM-QBMZZYIRSA-N 0.000 description 3
- 235000019408 sucralose Nutrition 0.000 description 3
- 238000002156 mixing Methods 0.000 description 2
- 230000005070 ripening Effects 0.000 description 2
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 2
- 102000009027 Albumins Human genes 0.000 description 1
- 108010088751 Albumins Proteins 0.000 description 1
- 101100314454 Caenorhabditis elegans tra-1 gene Proteins 0.000 description 1
- UDIPTWFVPPPURJ-UHFFFAOYSA-M Cyclamate Chemical compound [Na+].[O-]S(=O)(=O)NC1CCCCC1 UDIPTWFVPPPURJ-UHFFFAOYSA-M 0.000 description 1
- 102000018832 Cytochromes Human genes 0.000 description 1
- 108010052832 Cytochromes Proteins 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
- 101800001775 Nuclear inclusion protein A Proteins 0.000 description 1
- 241001482237 Pica Species 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- 101000577937 Xenopus laevis Midkine-A Proteins 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000002156 adsorbate Substances 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 229960000686 benzalkonium chloride Drugs 0.000 description 1
- CADWTSSKOVRVJC-UHFFFAOYSA-N benzyl(dimethyl)azanium;chloride Chemical compound [Cl-].C[NH+](C)CC1=CC=CC=C1 CADWTSSKOVRVJC-UHFFFAOYSA-N 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 239000000625 cyclamic acid and its Na and Ca salt Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 1
- 229940012189 methyl orange Drugs 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 239000006041 probiotic Substances 0.000 description 1
- 235000018291 probiotics Nutrition 0.000 description 1
- 235000019204 saccharin Nutrition 0.000 description 1
- CVHZOJJKTDOEJC-UHFFFAOYSA-N saccharin Chemical compound C1=CC=C2C(=O)NS(=O)(=O)C2=C1 CVHZOJJKTDOEJC-UHFFFAOYSA-N 0.000 description 1
- 229940081974 saccharin Drugs 0.000 description 1
- 239000000901 saccharin and its Na,K and Ca salt Substances 0.000 description 1
- 210000002966 serum Anatomy 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229960001462 sodium cyclamate Drugs 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 239000001384 succinic acid Substances 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 235000014101 wine Nutrition 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P39/00—General protective or antinoxious agents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28069—Pore volume, e.g. total pore volume, mesopore volume, micropore volume
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Analytical Chemistry (AREA)
- Polymers & Plastics (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Toxicology (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Pharmacology & Pharmacy (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Medicinal Preparation (AREA)
Abstract
Изобретение касается способа получения сорбента на основе гидрогеля метилкремниевой кислоты общей формулы:{(CHSi·nO},который заключается в том, что к раствору метилсиликоната натрия или калия в концентрации 2,35-2,95 моль/л добавляют раствор сильной кислоты до образования продукта, далее выдерживают, измельчают и активируют продукт путем добавления разбавленного раствора сильной кислоты и отмывают продукт до нейтральной реакции и, варьируя значение коэффициента n до 495, получают разные конечные формы сорбента с избирательными сорбционными свойствами относительно высокомолекулярных веществ с молекулярной массой 10000-500000 Д и более.
Priority Applications (6)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| UAA200610083A UA82774C2 (ru) | 2006-09-20 | 2006-09-20 | Способ получения сорбента на основе гидрогеля метилкремниевой кислоты |
| EP06836011A EP2075276A4 (en) | 2006-09-20 | 2006-10-30 | PROCESS FOR PRODUCING A SORBENT BASED ON METHYLSILICILIC ACID HYDROGEL |
| EA200800832A EA012985B9 (ru) | 2006-09-20 | 2006-10-30 | Способ получения сорбента на основе гидрогеля метилкремниевой кислоты |
| PCT/UA2006/000057 WO2008036056A1 (en) | 2006-09-20 | 2006-10-30 | Method for producing a sorbent based on a methyl- silicic acid hydrogel |
| US12/438,135 US20100240532A1 (en) | 2006-09-20 | 2006-10-30 | Method for producing a sorbent based on a methyl-silicic acid hydrogel |
| RU2007102041/04A RU2007102041A (ru) | 2006-09-20 | 2007-01-22 | Способ получения сорбента на основе гидрогеля метилкремниевой кислоты |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| UAA200610083A UA82774C2 (ru) | 2006-09-20 | 2006-09-20 | Способ получения сорбента на основе гидрогеля метилкремниевой кислоты |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| UA82774C2 true UA82774C2 (ru) | 2008-05-12 |
Family
ID=39200787
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| UAA200610083A UA82774C2 (ru) | 2006-09-20 | 2006-09-20 | Способ получения сорбента на основе гидрогеля метилкремниевой кислоты |
Country Status (6)
| Country | Link |
|---|---|
| US (1) | US20100240532A1 (ru) |
| EP (1) | EP2075276A4 (ru) |
| EA (1) | EA012985B9 (ru) |
| RU (1) | RU2007102041A (ru) |
| UA (1) | UA82774C2 (ru) |
| WO (1) | WO2008036056A1 (ru) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102012109727A1 (de) | 2011-11-23 | 2013-05-23 | Vadim Kozolovskyi | Enterosorbenszusammensetzung |
| RU2491941C1 (ru) * | 2011-12-27 | 2013-09-10 | Вадим Алексеевич Козловский | Композиционный энтеросорбент |
| WO2016071405A2 (en) | 2014-11-04 | 2016-05-12 | Invenres Gmbh | Pharmaceutical preparation and method of its production and use |
| WO2019045667A1 (ru) | 2017-08-30 | 2019-03-07 | Александр Михайлович МАРТЫНЕНКО | Способ получения гидрогеля метилкремниевой кислоты со свойствами супрамолекулярных структур и гидрогель, полученный этим способом |
| US10226425B2 (en) | 2013-11-06 | 2019-03-12 | Invenres Gmbh | Pharmaceutical preparation and method of its production and use |
| US12194147B2 (en) | 2018-01-29 | 2025-01-14 | Pathelen Health Care Ag | Hydrophilic/hydrophobic pharmaceutical composition and method of its production and use |
Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| UA90988C2 (ru) * | 2009-12-16 | 2010-06-10 | Геннадий Иванович Кабачный | Способ получения гидрогеля метилкремниевой кислоты |
| UA103109C2 (ru) * | 2012-03-07 | 2013-09-10 | Вадим Алексеевич Козловский | Применение метилкремниевой кислоты в виде ксерогеля или гидрогеля для лечения тканей пародонта |
| UA112474C2 (uk) | 2014-11-20 | 2016-09-12 | Юрій Захарович Толчеєв | Спосіб одержання пастоподібного сорбенту на основі гідрогелю метилкремнієвої кислоти |
| UA118953C2 (uk) * | 2014-11-20 | 2019-04-10 | Юрій Захарович Толчеєв | Спосіб одержання сорбенту на основі гідрогелю метилкремнієвої кислоти |
| CN104447834B (zh) * | 2014-11-25 | 2017-03-22 | 廊坊师范学院 | 纳米甲基硅酸锌的制备方法 |
| US20180190257A1 (en) * | 2016-12-29 | 2018-07-05 | Shadecraft, Inc. | Intelligent Umbrellas and/or Robotic Shading Systems Including Noise Cancellation or Reduction |
| EP3554684A1 (en) * | 2017-10-13 | 2019-10-23 | Health Product Group sp. z.o.o. | Method of production of a branched organosilicone polymerous polynuclear adsorbent of high molecular toxins and this adsorbent |
| RU2719436C1 (ru) * | 2019-08-06 | 2020-04-17 | Общество с ограниченной ответственностью "Тульская фармацевтическая фабрика" | Полиметилсилсесквиоксановый гидрогель |
| CN111875883B (zh) * | 2020-07-25 | 2021-11-19 | 浙江森川家具有限公司 | 一种纳米抗菌防污桌椅塑料颗粒及制备方法 |
| RU2761627C1 (ru) * | 2020-12-01 | 2021-12-13 | Общество с ограниченной ответственностью "Гротекс" (ООО "Гротекс") | Адсорбент полиметилсилоксана полигидрат и способ его получения |
| US20250144598A1 (en) * | 2023-11-02 | 2025-05-08 | Bioline Pharmaceutical Ag | Polymethylsiloxane polyhydrate having supramolecular properties of a molecular capsule, method for its production, and sorbent containing thereof |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU911290A1 (ru) * | 1980-03-18 | 1982-03-07 | Предприятие П/Я В-8855 | Чувствительный элемент дл измерени концентрации паров этанола |
| RU2111979C1 (ru) * | 1994-03-11 | 1998-05-27 | Юрий Николаевич Шевченко | Гидрогели метилкремневой кислоты как адсорбенты среднемолекулярных метаболитов и способ их получения |
| RU2104691C1 (ru) * | 1995-02-20 | 1998-02-20 | Общество с ограниченной ответственностью "ДМ плюс" | Способ получения липосомальной композиции (варианты) |
| US7328706B2 (en) * | 2002-05-06 | 2008-02-12 | Dynamic Mouth Devices Llc | Therapeutic and protective dental device useful as an intra-oral delivery system |
-
2006
- 2006-09-20 UA UAA200610083A patent/UA82774C2/ru unknown
- 2006-10-30 US US12/438,135 patent/US20100240532A1/en not_active Abandoned
- 2006-10-30 WO PCT/UA2006/000057 patent/WO2008036056A1/ru not_active Ceased
- 2006-10-30 EA EA200800832A patent/EA012985B9/ru not_active IP Right Cessation
- 2006-10-30 EP EP06836011A patent/EP2075276A4/en not_active Withdrawn
-
2007
- 2007-01-22 RU RU2007102041/04A patent/RU2007102041A/ru not_active Application Discontinuation
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102012109727A1 (de) | 2011-11-23 | 2013-05-23 | Vadim Kozolovskyi | Enterosorbenszusammensetzung |
| RU2491941C1 (ru) * | 2011-12-27 | 2013-09-10 | Вадим Алексеевич Козловский | Композиционный энтеросорбент |
| US10226425B2 (en) | 2013-11-06 | 2019-03-12 | Invenres Gmbh | Pharmaceutical preparation and method of its production and use |
| WO2016071405A2 (en) | 2014-11-04 | 2016-05-12 | Invenres Gmbh | Pharmaceutical preparation and method of its production and use |
| WO2019045667A1 (ru) | 2017-08-30 | 2019-03-07 | Александр Михайлович МАРТЫНЕНКО | Способ получения гидрогеля метилкремниевой кислоты со свойствами супрамолекулярных структур и гидрогель, полученный этим способом |
| US12194147B2 (en) | 2018-01-29 | 2025-01-14 | Pathelen Health Care Ag | Hydrophilic/hydrophobic pharmaceutical composition and method of its production and use |
Also Published As
| Publication number | Publication date |
|---|---|
| US20100240532A1 (en) | 2010-09-23 |
| WO2008036056A1 (en) | 2008-03-27 |
| EA200800832A1 (ru) | 2009-06-30 |
| RU2007102041A (ru) | 2008-07-27 |
| EP2075276A1 (en) | 2009-07-01 |
| EA012985B1 (ru) | 2010-02-26 |
| EA012985B9 (ru) | 2016-12-30 |
| EP2075276A4 (en) | 2012-07-18 |
| WO2008036056A9 (en) | 2009-05-14 |
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