TW307696B - Sludge phase reactor and its use - Google Patents
Sludge phase reactor and its use Download PDFInfo
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- TW307696B TW307696B TW84110505A TW84110505A TW307696B TW 307696 B TW307696 B TW 307696B TW 84110505 A TW84110505 A TW 84110505A TW 84110505 A TW84110505 A TW 84110505A TW 307696 B TW307696 B TW 307696B
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- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/20—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
- B01J19/1868—Stationary reactors having moving elements inside resulting in a loop-type movement
- B01J19/1875—Stationary reactors having moving elements inside resulting in a loop-type movement internally, i.e. the mixture circulating inside the vessel such that the upwards stream is separated physically from the downwards stream(s)
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- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/1836—Heating and cooling the reactor
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
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- B01J8/22—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium gas being introduced into the liquid
- B01J8/224—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium gas being introduced into the liquid the particles being subject to a circulatory movement
- B01J8/226—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium gas being introduced into the liquid the particles being subject to a circulatory movement internally, i.e. the particles rotate within the vessel
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/30—Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of nitrogen-to-oxygen or nitrogen-to-nitrogen bonds
- C07C209/32—Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of nitrogen-to-oxygen or nitrogen-to-nitrogen bonds by reduction of nitro groups
- C07C209/36—Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of nitrogen-to-oxygen or nitrogen-to-nitrogen bonds by reduction of nitro groups by reduction of nitro groups bound to carbon atoms of six-membered aromatic rings in presence of hydrogen-containing gases and a catalyst
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00008—Controlling the process
- B01J2208/00017—Controlling the temperature
- B01J2208/00026—Controlling or regulating the heat exchange system
- B01J2208/00035—Controlling or regulating the heat exchange system involving measured parameters
- B01J2208/0007—Pressure measurement
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- 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
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00008—Controlling the process
- B01J2208/00017—Controlling the temperature
- B01J2208/00026—Controlling or regulating the heat exchange system
- B01J2208/00035—Controlling or regulating the heat exchange system involving measured parameters
- B01J2208/00079—Fluid level measurement
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- 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
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00008—Controlling the process
- B01J2208/00017—Controlling the temperature
- B01J2208/00106—Controlling the temperature by indirect heat exchange
- B01J2208/00168—Controlling the temperature by indirect heat exchange with heat exchange elements outside the bed of solid particles
- B01J2208/00212—Plates; Jackets; Cylinders
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- 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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00076—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements inside the reactor
- B01J2219/00085—Plates; Jackets; Cylinders
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Description
Α7 Β7 337696 五、發明説明(1 ) 發明背景 漿相反應係爲其中參與至少一個細分固相及一個流體相 之反應。 高度放熱之漿相反應,需要有效排放反應熱。漿相反應 器因而一般性地包括昂贵之熱交換器構造,位於反應容器 内部(參閲,例如美國專利3,243,268或歐洲專利263,935) 。於已知衆相反應器之情況中,其熱交換係由於以下事實 所導致,反應質量係被泵送環繞著所謂熱交換器管件或鍋 爐管件”場”,該管件係於一端封閉,且其中熱傳遞媒質及 所形成之蒸汽係被逆流地導引。此種熱交換型式之缺點爲 反應質量之流動速度在與反應器室之關係上是不同的,且 藉其產生之熱交換器效率是低程度的。反應質量之不同流 動速度會導致其中具有實質上降低流動之區域,且涉及此 反應之固體成份可能會沈積。 附圈簡域 圖1顯示經過根據本發明漿相反應器之橫截面;及 圖2顯示圖1反應器中A-A方向上之橫截面圖。 發明説明 根據本發明,目前提出一種容器作爲熱交換器,經過其 中之熱傳遞媒質基本上僅在一個方向上流動,此容器裝有 多個具有圓形橫截面之通路導管供反應質量使用。在與習 用蒸發-熱交換器比較下,根據本發明,反應質量因此在 ---------「裝------訂------^ (請先閱讀背面之注意事項再填巧本頁) 經濟部中央梂隼局身工消費合作社印裝 中酬家縣(CNS ) ( 21G x297公慶) 經濟部中央標準局貝工消费合作社印裝 SG7696 at _______B7 五、發明説明(2 ) ~s 熱交換器中係以"逆向方式"導引。 本發明之主題事項係爲一種供放熱漿相反應用之漿相反 應器,其包括下列組件: a) —個反應容器; b) —個呈環形室形式之熱交換器,冷卻劑與反應質量 係經過其中而在反應容器内部流動,此環形室係於 其頂部與底部被反應質量復蓋; c) 一個位於環形室内部供反應質量回流用之中央自由 流動室; d) —個使反應質量在中央自由流動室與環形室之間循 環之中央攪拌器; 其中環形室包括多個具有圓形橫截面之垂直通路導管供反 應質量使用,且冷卻劑係流經供反應質量用之通路導管間 之環形室。 較佳情況是,反應質量與熱傳遞媒質係實質上以相同方 向流經熱交換器環形室。特別是,經過環形室之反應質量 係垂直向上流經通路導管。於此情況中,攪拌器較佳係配 置在中央自由流動室之下方出口。至少一種反應成份被輸 送在攪拌器附近,以致首先使反應成份迅速地分佈在反應 質量中,且其次將所輸送之反應成份與反應質量極迅速地 引進熱交換器中。 爲使反應連續地進行,故在反應容器中之流體液面上方 提供溢流,則可自其將已反應之反應質量連續地取出。 較佳情況是,將在反應溫度下蒸發及在熱交換器環形室 本紙張尺度逋用中國國家橾準(CNS ) Λ4規格(210X297公釐〉 (請先閱讀背面之注意事項再填寫本頁) 象· 訂 經濟部中央樣準局貝工消費合作社印製
U㈣G --B7 五、發明獅(3) 底部處以液體形式輸送且以氣體形式自熱交換器環形室頭 部取出之物質,作爲熱傳遞媒質使用。特佳情況是,使用 水作爲熱傳遞媒質,且此熱交換係伴随著產生蒸汽下進行 °冷卻劑溫度較佳係設定爲保持所產生蒸汽之壓力。 涉及氣相之反應,較佳係在根據本發明之漿相反應器中 進行。爲達此目的,攪拌器係呈充氣攪拌器形式或包含另 個充氣組件。 根據本發明並具有充氣攪拌器之漿相反應器,係特別適 合用以進行芳族硝基化合物之漿相氫化反應,特佳係供二 確基甲苯之氫化反應使用,並產生相應二胺類。 本發明將更詳細地參照附圖加以解釋。 根據圖1之反應器係包括反應容器1,其係由三部份所構 成,此三部份係藉凸緣11與12以凸緣裝在一起。反應容器 1之·中夬部份含有環形熱交換器2,其包括所有侧面均密閉 且被多個通路管件21穿透之環形室,反應質量係流經通路 管件,以箭頭所指示之方向上升。位於環形室2之其餘空 間22中者,係爲熱交換器媒質。正如箭頭所示,反應質量 之回流係經過環形熱交換器2内部之中央自由流動室3。反 應質量之循環流動係藉攪拌器4產生,其具有反應器外部 驅動之中央攪拌器機轴41,及攪拌器葉片42。在此方面, 授拌器葉片42係配置在底部,於中央流動室3出口之位置 處0於所示之具體實施例中,攪拌器機軸41係呈中空機輛 形式,並包括一個充氣裝置43,位於攪拌器葉片42下方。 對反應質量充氣之氣體,係利用攪拌器機軸41中之吸入口 本紙張尺度適用中國國家標牟(CNS ) Λ4说格(210X297公釐) (請先閱讀背面之注意事項再填寫本頁) 訂 i A7 ______B7^_ 五、發明説明(4 ) 44,抽離反應容器1上方部份中之氣體室。預定氣體壓力 係經由氣體輸送連接器45確保。當使用根據本發明之反應 器較佳地用以使芳族辟基化合物氫化時,氫氣使用之壓力 係在10與40巴之間。更有利之情況是,可將新鮮氫氣直接 輪送至反應質量中。將芳族硝基化合物經由輸送管線5引 進攪拌器葉片42附近。將例如在栽體粒子(誓如碳、Si〇2 、Al2〇3等)上之貴金屬或鎳或阮尼鎳觸媒,分散在反應 質量中,作爲細分固相。產物係在溢流管7處連續地取出 ,以致保持恒定流體液面。熱交換器環形室係進一步由熱 父換器媒質回路6供應。將熱交換器媒質,較佳爲正好低 於沸點之水,於61處引進熱交換器之底部。蒸汽係於62處 自熱交換器之頂部出現,並輸送至蒸氣分離器63。箭頭64 表π蒸汽之棑放以供能量回收。冷卻水流入閥65係藉液位 調節裝置66,以控制蒸氣分離器63中之水位。當根據本發 明之反應器優先供芳族硝基化合物氫化使用時,泠卻劑壓 力64係經調整,以致保持反應器中之溫度爲。 經濟部中央揉準局貝工消費合作社印製 於圖2中之數字,係指稱與圖1中相同之組件。僅示出一 部份通路管件21。熱交換器2可包含1〇〇與3000個間之通路 管件21,依管件之額定寬度(25-10毫米)及熱交換器之直 徑(至高3米)而定。 雖然本發明已在前文爲説明目的而進行詳述,但應明瞭 此種細節僅對該目的而言,在未偏離本發明之精神與範圍 下,熟諸此藝者可於其中作改變,惟其係被申請專利範圍 所限制。 本紙張尺度適财國國家轉(CNS) M規格(2丨Μ2"公疫)
Claims (1)
- 307636 έ88 j86· C8 〜.H日 __I M 案― 六、申請專利範圍 專利申請案第84110505號 ROC Patent Appln. No.84110505 修正之申請專利範团中文本一附件一 Amended Claims in Chinese — Enel. (I ) (民國86年3月日送呈) (Submitted on March , 1997) J. 一種供放熱漿相反應用之漿相反應器,其内部包括: a) —循環形式之熱交換器,熱交換媒質流經其間; b) 位於熱交換器頂部與底部之反應物質; c) 一位於熱交換器内部,供反應物質回流用之中央 自由流動導管; d) —位於熱交換器中央之攪拌器;以及 e) 多數個圓形橫截面且貫穿熱交換器之垂直通路導 管,其係供連接熱交換器頂部與底部之反應物質 〇 2. 根據申請專利範圍第1項之漿相反應器,其中攪拌係 以充氣擾動之方式進行。 經濟部中央標準局員工消費合作社印製 ^^1 1^1 m ml ml m ^ —nil m In ^^^1 --Φ 、-0 (請先閱讀背面之注意事項再填寫本頁) 3. 根據申請專利範園第1項之漿相反應器,其中攪拌器 以中央自由流動導管向下輸送反應物質,並於垂直通 路導管中向上流動。 4. 根據申請專利範園第1項之漿相反應器,其中攪拌器 係配置在中央自由流動導管之出口處。 5. 根據申請專利範園第1項之漿相反應器,其中至少一 種反應劑引進反應物質中。 -7 - 本紙張尺度適用中國國家標準(CNS ) A4規格(210X297公釐) 307696 as C8 D8 六、申請專利範圍 6. 根據申請專利範圍第1項之漿相反應器,其中用以進 行漿相氫化作用。 7. 根據申請專利範圍第6項之漿相反應器,其中用以氫 化芳族確基化合物。 S.根據申請專利範圍第1項之漿相反應器,其中用以氫 化二硝基甲苯。 9.根據申請專利範圍第1、2、3、4或5項之漿相反 應器,其中使用水做爲冷卻劑。 -------—f 裝------訂------广k (請先閱讀背面之注意事項再填寫本頁) 經濟部中央標準局員工消費合作社印製本紙張尺度適用中國國家標準(CNS ) A4規格(210X297公釐)
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
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DE4435839A DE4435839A1 (de) | 1994-10-07 | 1994-10-07 | Schlammphasenreaktor und dessen Verwendung |
Publications (1)
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TW307696B true TW307696B (en) | 1997-06-11 |
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Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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TW84110505A TW307696B (en) | 1994-10-07 | 1995-10-06 | Sludge phase reactor and its use |
Country Status (12)
Country | Link |
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US (1) | US5779995A (zh) |
EP (1) | EP0784505B1 (zh) |
JP (1) | JP3783046B2 (zh) |
KR (1) | KR100397268B1 (zh) |
CN (1) | CN1081945C (zh) |
BR (1) | BR9509270A (zh) |
CA (1) | CA2201629C (zh) |
DE (2) | DE4435839A1 (zh) |
ES (1) | ES2122685T3 (zh) |
MX (1) | MX198021B (zh) |
TW (1) | TW307696B (zh) |
WO (1) | WO1996011052A1 (zh) |
Families Citing this family (26)
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US6242649B1 (en) | 1997-10-15 | 2001-06-05 | Bayer Aktiengesellschaft | Continuous method for producing aromatic amines |
DE19844901C1 (de) * | 1998-09-30 | 1999-11-04 | Bayer Ag | Verfahren zur Dosierung von flüssigen Nitroaromaten mit mehr als einer Nitrogruppe in Reaktoren zur Sumpfphasen-Hydrierung |
US7109378B2 (en) * | 2001-08-30 | 2006-09-19 | Air Products And Chemicals, Inc. | Monolith catalytic reactor coupled to static mixer |
US20030050510A1 (en) * | 2001-08-30 | 2003-03-13 | Welp Keith Allen | Monolith catalytic reactor coupled to static mixer |
US7074962B2 (en) * | 2002-02-15 | 2006-07-11 | Air Products And Chemicals, Inc. | Catalyst holder and agitation system for converting stirred tank reactor to fixed bed reactor |
JP4015593B2 (ja) * | 2002-09-04 | 2007-11-28 | 株式会社パウレック | 流動層装置 |
DE102004039960A1 (de) * | 2004-08-18 | 2006-02-23 | Bayer Materialscience Ag | Rührvorrichtung und Verfahren zur Durchführung einer Gas-Flüssig-Reaktion |
JP4577205B2 (ja) * | 2004-12-22 | 2010-11-10 | 住友化学株式会社 | シクロヘキサノンオキシムの製造方法 |
GB2438813B (en) * | 2005-03-17 | 2009-11-11 | Sasol Technology | Method of operating a three-phase slurry reactor |
DE102006059678A1 (de) * | 2006-12-18 | 2008-06-19 | Bayer Materialscience Ag | Verfahren zur Herstellung von aromatischen Aminen |
DE102006060572A1 (de) | 2006-12-19 | 2008-06-26 | Bayer Materialscience Ag | Verfahren zur Herstellung von Toluylendiaminen durch katalytische Hydrierung von Dinitrotoluolen |
CN100453948C (zh) * | 2007-07-20 | 2009-01-21 | 中国石化扬子石油化工有限公司 | 一种立式管壳式换热器及其防堵方法 |
DE102008063991A1 (de) | 2008-12-19 | 2010-06-24 | Bayer Materialscience Ag | Verfahren zur Herstellung von Isocyanaten in der Gasphase |
DE102009025374A1 (de) * | 2009-06-18 | 2010-12-23 | Bayer Materialscience Ag | Verfahren zur Herstellung von aromatischen Aminen |
JP5805661B2 (ja) | 2010-01-14 | 2015-11-04 | バイエル・インテレクチュアル・プロパティ・ゲゼルシャフト・ミット・ベシュレンクテル・ハフツングBayer Intellectual Property GmbH | 液相での芳香族アミンの製造方法 |
FR2966752B1 (fr) * | 2010-11-03 | 2013-11-01 | IFP Energies Nouvelles | Dispositif de test de solides mis en forme fonctionnant en phase heterogene |
CN102151525B (zh) * | 2011-01-27 | 2013-07-31 | 甘肃银光聚银化工有限公司 | 一种加氢反应装置 |
JP5802397B2 (ja) * | 2011-01-31 | 2015-10-28 | 独立行政法人石油天然ガス・金属鉱物資源機構 | 温度制御システム |
JP5815324B2 (ja) * | 2011-08-05 | 2015-11-17 | 独立行政法人石油天然ガス・金属鉱物資源機構 | 温度制御システム |
CN105195071A (zh) * | 2014-06-25 | 2015-12-30 | 安徽扬子化工有限公司 | 一种高效混合反应釜 |
US10272405B2 (en) * | 2014-11-28 | 2019-04-30 | Ulusal Bor Arastirma Enstitusu | Cartridge structure designed for generation of hydrogen gas |
DE202015009585U1 (de) * | 2015-04-23 | 2018-06-13 | Thyssenkrupp Ag | Reaktor zur Polymerisation von Lactid |
DE102015219306A1 (de) * | 2015-10-06 | 2017-04-06 | Hydrogenious Technologies Gmbh | Reaktor-Vorrichtung zum Beladen und/oder Entladen eines Trägermediums mit bzw. von Wasserstoff sowie Anlage mit einer derartigen Reaktor-Vorrichtung |
DE102016210224A1 (de) * | 2016-06-09 | 2017-12-14 | Friedrich-Alexander-Universität Erlangen-Nürnberg | Reaktor und Verfahren zur Umsetzung von gleichgewichtslimitierten Reaktionen |
CN110143883B (zh) * | 2019-05-28 | 2023-03-03 | 中国神华煤制油化工有限公司 | 一种加氢反应方法 |
CN114405340A (zh) * | 2022-01-14 | 2022-04-29 | 绍兴德美新材料有限公司 | 一种整理剂抽气消泡搅拌装置 |
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US2334553A (en) * | 1941-11-08 | 1943-11-16 | Standard Oil Dev Co | Apparatus and process for catalytic reactions of low boiling hydrocarbons |
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US3476552A (en) * | 1966-09-07 | 1969-11-04 | Mountain Copper Co Of Californ | Mercury process |
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DE1793452B2 (de) * | 1968-09-19 | 1976-11-18 | Basf Ag, 6700 Ludwigshafen | Verfahren zur verbesserung der waermeabfuehrung bei katalytischen hydrierungen |
FR1599004A (zh) * | 1968-10-17 | 1970-07-15 | ||
GB1413565A (en) * | 1973-01-29 | 1975-11-12 | Voron Vnii Sint Cheskogo Kauch | Apparatus for producing organometallic compounds and method of preparing organolithium compounds in said apparatus |
JPS6343920A (ja) * | 1986-08-11 | 1988-02-25 | Hitachi Ltd | ポリエステル重縮合装置 |
US4882283A (en) * | 1987-11-17 | 1989-11-21 | Phillips Petroleum Company | Heat exchange apparatus |
JPH0416229A (ja) * | 1990-05-07 | 1992-01-21 | Hitachi Ltd | ドラフトチューブ式攪拌槽 |
DE4323687A1 (de) * | 1993-07-15 | 1995-01-19 | Bayer Ag | Kontinuierliches Verfahren zur Herstellung von aromatischen Aminen |
-
1994
- 1994-10-07 DE DE4435839A patent/DE4435839A1/de not_active Withdrawn
-
1995
- 1995-09-25 BR BR9509270A patent/BR9509270A/pt not_active IP Right Cessation
- 1995-09-25 CN CN95195517A patent/CN1081945C/zh not_active Expired - Lifetime
- 1995-09-25 EP EP95935373A patent/EP0784505B1/de not_active Expired - Lifetime
- 1995-09-25 JP JP51228896A patent/JP3783046B2/ja not_active Expired - Fee Related
- 1995-09-25 US US08/809,840 patent/US5779995A/en not_active Expired - Lifetime
- 1995-09-25 WO PCT/EP1995/003786 patent/WO1996011052A1/de active IP Right Grant
- 1995-09-25 CA CA002201629A patent/CA2201629C/en not_active Expired - Fee Related
- 1995-09-25 KR KR1019970702229A patent/KR100397268B1/ko not_active IP Right Cessation
- 1995-09-25 DE DE59503373T patent/DE59503373D1/de not_active Expired - Lifetime
- 1995-09-25 ES ES95935373T patent/ES2122685T3/es not_active Expired - Lifetime
- 1995-10-06 TW TW84110505A patent/TW307696B/zh active
-
1997
- 1997-04-04 MX MX9702470A patent/MX198021B/es not_active IP Right Cessation
Also Published As
Publication number | Publication date |
---|---|
CA2201629A1 (en) | 1996-04-18 |
EP0784505A1 (de) | 1997-07-23 |
KR970706059A (ko) | 1997-11-03 |
MX9702470A (es) | 1998-10-31 |
ES2122685T3 (es) | 1998-12-16 |
CN1081945C (zh) | 2002-04-03 |
JP3783046B2 (ja) | 2006-06-07 |
DE4435839A1 (de) | 1996-04-11 |
DE59503373D1 (de) | 1998-10-01 |
CN1159771A (zh) | 1997-09-17 |
WO1996011052A1 (de) | 1996-04-18 |
EP0784505B1 (de) | 1998-08-26 |
BR9509270A (pt) | 1997-12-23 |
KR100397268B1 (ko) | 2003-11-28 |
CA2201629C (en) | 2005-05-24 |
JPH10506837A (ja) | 1998-07-07 |
MX198021B (es) | 2000-08-10 |
US5779995A (en) | 1998-07-14 |
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