TW486515B - Process for the autothermal reforming of a hydrocarbon feedstock containing higher hydrocarbons - Google Patents

Process for the autothermal reforming of a hydrocarbon feedstock containing higher hydrocarbons Download PDF

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Publication number
TW486515B
TW486515B TW088116488A TW88116488A TW486515B TW 486515 B TW486515 B TW 486515B TW 088116488 A TW088116488 A TW 088116488A TW 88116488 A TW88116488 A TW 88116488A TW 486515 B TW486515 B TW 486515B
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Taiwan
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reactor
steam
autothermal
gas
atr
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TW088116488A
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English (en)
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Thomas Sandahl Christensen
Jens-Henrik Bak Hansen
Peter Seier Christensen
Ivar Ivarsen Primdahl
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Haldor Topsoe As
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G35/00—Reforming naphtha
    • C10G35/04—Catalytic reforming
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
    • C01B3/32—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air
    • C01B3/34—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents
    • C01B3/38—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents using catalysts
    • C01B3/382—Multi-step processes
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/02—Processes for making hydrogen or synthesis gas
    • C01B2203/0205—Processes for making hydrogen or synthesis gas containing a reforming step
    • C01B2203/0227—Processes for making hydrogen or synthesis gas containing a reforming step containing a catalytic reforming step
    • C01B2203/0233—Processes for making hydrogen or synthesis gas containing a reforming step containing a catalytic reforming step the reforming step being a steam reforming step
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/02—Processes for making hydrogen or synthesis gas
    • C01B2203/0205—Processes for making hydrogen or synthesis gas containing a reforming step
    • C01B2203/0227—Processes for making hydrogen or synthesis gas containing a reforming step containing a catalytic reforming step
    • C01B2203/0244—Processes for making hydrogen or synthesis gas containing a reforming step containing a catalytic reforming step the reforming step being an autothermal reforming step, e.g. secondary reforming processes
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
    • C01B2203/0465—Composition of the impurity
    • C01B2203/0495—Composition of the impurity the impurity being water
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/08—Methods of heating or cooling
    • C01B2203/0805—Methods of heating the process for making hydrogen or synthesis gas
    • C01B2203/0838—Methods of heating the process for making hydrogen or synthesis gas by heat exchange with exothermic reactions, other than by combustion of fuel
    • C01B2203/0844—Methods of heating the process for making hydrogen or synthesis gas by heat exchange with exothermic reactions, other than by combustion of fuel the non-combustive exothermic reaction being another reforming reaction as defined in groups C01B2203/02 - C01B2203/0294
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/12—Feeding the process for making hydrogen or synthesis gas
    • C01B2203/1205—Composition of the feed
    • C01B2203/1211—Organic compounds or organic mixtures used in the process for making hydrogen or synthesis gas
    • C01B2203/1235—Hydrocarbons
    • C01B2203/1241—Natural gas or methane
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/12—Feeding the process for making hydrogen or synthesis gas
    • C01B2203/1205—Composition of the feed
    • C01B2203/1211—Organic compounds or organic mixtures used in the process for making hydrogen or synthesis gas
    • C01B2203/1235—Hydrocarbons
    • C01B2203/1247—Higher hydrocarbons
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/12—Feeding the process for making hydrogen or synthesis gas
    • C01B2203/1258—Pre-treatment of the feed
    • C01B2203/1264—Catalytic pre-treatment of the feed
    • C01B2203/127—Catalytic desulfurisation
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/14—Details of the flowsheet
    • C01B2203/142—At least two reforming, decomposition or partial oxidation steps in series
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/14—Details of the flowsheet
    • C01B2203/142—At least two reforming, decomposition or partial oxidation steps in series
    • C01B2203/143—Three or more reforming, decomposition or partial oxidation steps in series
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/80—Aspect of integrated processes for the production of hydrogen or synthesis gas not covered by groups C01B2203/02 - C01B2203/1695
    • C01B2203/82—Several process steps of C01B2203/02 - C01B2203/08 integrated into a single apparatus

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Combustion & Propulsion (AREA)
  • General Health & Medical Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • General Chemical & Material Sciences (AREA)
  • Hydrogen, Water And Hydrids (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Solid Fuels And Fuel-Associated Substances (AREA)
  • Vehicle Body Suspensions (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Description

486515 經濟部智慧財產局員工消費合作社印製 A7 B7 五、發明說明（I ) 本發明之背景 本發明乃關於含有較高級烴類之烴類進料之無煤灰之 自熱性重組(ATR)。 在自熱性重組中，烴類進料之燃燒係與不足化學計量 之氧氣在燃燒爐之燃燒區中藉火燄反應、且隨後在蒸汽重 組催化劑之固定床中進行之部份燃燒進料之蒸汽重組。烴 類之不足化學計量將導致不利地煤灰之生成。煤灰之生成 可以藉使用特定之燃燒爐設計以及經由控制ATR方法之操 作條件以避免。煤灰係在某些特定之操作條件範圍中於自 熱性反應器之火燄中生成。當蒸汽相對於送至ATR反應器 之其他成份之量低於臨界値時，煤灰將在反應進料中生成 。可以使用於ATR中之一此種燃燒爐係描述於美國專利第 5,496，170號中。該限制量之蒸汽可以表示成臨界蒸汽對碳 之比値，其係蒸汽之莫耳進料流速對烴類進料中之碳之莫 耳流速。該烴類進料可以是天然氣或包括天然氣之形式或 丁烷、石油腦等之烴類之形式。碳之莫耳流速係計算成烴 類之莫耳流速乘上烴類之碳含量。
不會造成煤灰生成之操作條件之實例係整理於 Christensen與Primdahl所發表之論文中（1994年三月之 Hydrocarbon Processing第39-46頁）。那些條件係示於表1 中。該測試係在實驗工廠中進行，由於熱量從相當小之實 驗工廠漏失之故，絕熱之ATR出口溫度將高於測量之 ATR出口溫度。此意謂若一可以忽略熱量漏失之大單元經 由完全相同之操作條件，ATR出口溫度將接近絕熱之ATR 3 本紙m又/又週用I7國國豕彳示準（CNS)A4規格（210 X 297公爱） — II ---------^--------- (請先閱讀背面之注意事項再填寫本頁) 486515 經濟部智慧財產局員工消費合作社印製 A7 ________B7_____ 五、發明說明（少） 出口溫度。煤灰之前體係在ATR之燃燒區中生成，而大部 份之熱量漏失係發生在燃燒區後，隨後之熱量漏失對燃燒 區中之反應沒有任何影響。氧氣對碳之比値(02/C)亦示於 表1中。此比値之定義類似於蒸汽對碳之比値，不過係將 蒸汽以氧氣取代。當從反應器所漏失之熱量已知時，來自 ATR反應器之出口溫度可以從〇2/C比値計算。 表 1 實例 編號 氧氣對 碳比值 h2o/c co2/c 測量之ATR出口 溫度，°C 絕熱之ATR出 口溫度，°C A 0.60 1.43 0 9 50 1013 B 0.62 0.59 0 1065 1173 C 0.60 0.86 0 1000 1073 D 0.67 0.68 0.47 1018 1147 E 0.70 0.67 0.75 1030 1147 F 0.73 0.58 0.98 1028 1177 不會造成煤灰生成之操作條件（來自1 994年 Christensen 與 Primdahl) 該方法在低蒸汽對碳比値下操作係有利的，因爲低比 値會降低ATR工廠之投資費用且減少在操作工廠中所需之 能源消耗。此外，低蒸汽對碳比値使富含C0氣於生產例 如甲醇或二甲基醚合成及費希爾-特普希(Fischer-Tropsch ) 所製造之合成氣之組成最適化成爲可能，已發現在自熱性 重組器之上游處安置一具有蒸汽重組催化劑之低溫重組反 應器可以降低臨界蒸汽對碳比値。該重組反應器可以移除 4 本紙張尺度適用中國國家標準（CNS)A4規格（2】0 X 297公釐） . Awm —-----訂---------線 (請先閱讀背面之注意事項再填寫本頁) 486515 A7 B7 經濟部智慧財產局員工消費合作社印制π 五、發明說明（9) 或降低較高級烴類之含量。較高級烴類係由二或多個碳原 子所構成之烴類。蒸汽重組催化劑係將較高級烴類轉化成 甲烷、一氧化碳、二氧化碳與氫氣之混合物。 低溫蒸汽重組反應器可以是絕熱之預重組器或加熱之 預重組器，例如爲描述於歐洲專利公告第855,366號之催 化熱交換器線圈之形式。來自低溫蒸汽重組反應器之流出 物流之出口溫度係不高於600°C。 因此，本發明提供一藉烴類進料於自熱性重組器中之 催化自熱性重組以製備富含氫氣及/或一氧化碳之氣體之方 法，其進一步含有步驟： (a) 將烴類進料通過含有蒸汽重組催化劑之第一反應器 以充份地移除在烴類進料中之較高級烴類之含量； (b) 將來自第一反應器之流出物通過自熱性重組器；且 (c) 從自熱性重組器中取出富含氫氣與一氧化碳之產物 氣體。 本發明之一優點爲其可能在比當使用未轉化之進料物 流作爲自熱性重組器之進料時於低之蒸汽對碳比値下操自 熱性重組器。 第二個優點爲當其不含有較高級烴類時，預熱用於 ATR之進料氣體至較高之溫度係可能的。此會造成方法所 消耗之氧氣較低。 本發明在伴生氣體(associated gas)之蒸汽重組上係特 別有用的。伴生氣體係在產油過程中所製造之天然氣。此 氣體通常係在鑽孔裝置處燃燒，因爲伴生氣體是不經濟的 5 _丨、-----------Mwi— (請先閱讀背面之注意事項再填寫本頁) 訂 線-21 4 — — — — — — —— — I*-· 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） 經濟部智慧財產局員工消費合作社印製 486515 A7 _ B7 五、發明說明（氺） 。伴生氣體具有高含量之較高級烴類。 實例1 測試單元係由用於提供進料至ATR反應器之系統、 ATR反應器與用於產物氣體之後處理之設備所構成。 進料物流係由天然氣、蒸汽、氧氣、氫氣以及若有需 要可選用之丁烷所構成。天然氣之組成係示於表2中。所 有的氣體皆壓縮至操作壓力且預熱至操作溫度。天然氣在 飼入ATR反應器之前先經脫硫處理。將進料合倂成二股物 流且送至ATR之燃燒爐。第一進料物流含有天然氣、氫氣 、蒸汽與若有需要可選用之丁烷，將此進料物流加熱至 500°C。另外之進料物流含有氧氣與蒸汽且係加熱至220°C 。ATR反應器中之壓力係2.46MPa巴斯卡。含有天然氣之 物流在飼入ATR反應器之前，若有需要可選用地通過預重 組器。亦在此例子中，氣體物流在飼入ATR反應器之前係 加熱至500°C。 ^ ---------訂---------線 (請先閱讀背面之注意事項再填寫本頁) 表 2 成份 莫耳分率 N2 0.42 C02 1.16 ch4 94.55 C2 2.75 C3 0.70 C4 0.31 C5+ 0.11 6 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） 486515 經濟部智慧財產局員工消費合作社印製 A7 ___ B7 _ 五、發明說明（（） 天然氣之組成 在ATR反應器中係進行不足化學計量之燃燒與隨後之 催化蒸汽重組以及轉移反應。入口與出口氣體組成係藉氣 相色層分析法以測量。 在ATR反應器之下游，將產物氣體冷卻且冷凝產物氣 體之蒸汽含量之大部份。若有煤灰生成，則其會被捕捉在 冷凝液中。該冷凝液係同時經重量分析與分光檢驗。 進行下述之測試以說明將進料氣體通過預重組器之影 響。在一測試中該進料氣體係攙有丁烷，丁烷之濃度係佔 總烴類之4.0體積％。 每一個測試係從蒸汽富含端進行以趨近臨界蒸汽對碳 比値。該測試係以足夠高之蒸汽流動起始以確保無煤灰之 條件，蒸汽流動然後逐步降低。使系統維持穩定，其後檢 驗冷凝液中之煤灰含量。若冷凝液中仍然沒有煤灰，則進 行下一步驟。術語”無煤灰條件”是指煤灰生成可以忽略之 條件。在臨界蒸汽對碳比値時生成之煤灰量係約3-5PPm。 在下述所描述之測試中，碳流速係100-103標準立方 米/小時，氫氣流速係2標準立方米/小時。調整蒸汽流以 得到給定之蒸汽對碳比値。調整氧氣流速範圍在55至58 標準立方米/小時，以得到所欲之操作溫度。 由於熱量從相當小之實驗工廠漏失之故，絕熱ATR出 口溫度將高於表3中所給之溫度。大型之工業單元將非常 接近絕熱條件、且當工業單元另一方面係操作在與表3中 所引用者完全相同之條件時來，自此一單元之出口溫度將 7 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） ---------^---------^ ^^^1 (請先閱讀背面之注意事項再填寫本頁) 經濟部智慧財產局員工消費合作社印製 486515 A7 B7 五、發明說明（,） 因此非常接近表3中所示之絕熱。 表 3 測試 預重組器 攙配丁烷 02/C ATR 出 σ 絕熱出口 臨界蒸汽 編號 溫度 溫度 對碳比值 °C °C 1.1 無 無 0.56 954 1019 0.70 1.2 有 無 0.56 951 1011 0.64 1.3 無 有 0.55 948 1006 0.79 來自表3之測試中之ATR反應器之產物氣體之組成係 藉氣相色層分析法以測量。氣體之組成係示於表4中。氣 體組成係以乾莫耳百分率表示，其係不包括蒸汽時之氣體 成份之莫耳組成。 表 4 測試編號 h2 n2 CO C02 ch4 % % % % % 1.1 64.4 0.14 26.74 6.81 1.87 1.2 65.1 0.12 25.17 6.99 2.62 1.3 64.5 0.12 26.09 7.67 1.62 表3之測試中之產物氣體之組成(乾莫耳％) 從表3中可看出，當將進料蒸汽通過預重組器，則臨 界蒸汽對碳比値將降低。再者，可看出的是飼入ATR之進 料氣體中丁烷含量之增加會造成臨界蒸汽對碳比値增高。 8 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） ^ —--------------^ (請先閱讀背面之注意事項再填寫本頁) 486515 A7 B7 五、發明說明（</ ) 此意謂若進料中含有較大量之較高級烴類’則將進料通過 預重組器之優點將增加。 實例2 使用如實例1之相同測試單元。將乙烷或丁烷加入測 試運轉2與3中含有天然氣之進料物流中。 在下述所描述之測試中，碳流速係100_103標準立方 米/小時，氫氣流速係2標準立方米/小時。調整蒸汽流以 得到給定之蒸汽對碳比値。調整氧氣流速範圍在58至60 標準立方米/小時，以得到所欲之操作溫度。 (請先閱讀背面之注意事項再填寫本頁) 經濟部智慧財產局員工消費合作社印製 來自表5之測試中之ATR反應器之產物氣體之組成係 示於表6中。 表 6 測試編號 h2 n2 CO C02 ch4 % % % % % 2.1 62.9 0.14 31.1 4.33 1.52 2.2 63.0 0.14 30.9 4.74 1.25 2.3 63.3 0.21 30.5 4.71 1.25 表5之測試中之產物氣體之組成(乾莫耳。/〇) 9 表_5 測試 編號 攙配 烴類 濃度 o2/c ATR出 口溫度 絕熱出 口溫度 臨界蒸 汽對碳 比值 °C °C 2.1 無 0.58 1027 1109 0.33 2.2 有 乙烷 7.2 0.58 1024 1113 0.41 2.3 有 丁烷 5.1 0.57 1023 1118 0.47 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） 486515 A7 B7 五、發明說明（S ) 從表5中可以看出，乙烷與丁烷同時之較高含量會造 成臨界蒸汽對碳比値增高。 --------------------訂---------線 (請先閱讀背面之注意事項再填寫本頁) 經濟部智慧財產局員工消費合作社印製 10 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐）

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  1. 486515
    完:、申請專利範圍 (請先閲讀背面之注意事項再填寫本頁) 1. 一種製備氫氣及/或一氧化碳之方法，其係在自熱 性重組器中將含較高級烴類之烴類進料於自熱性重組器進 行催化自熱性重組，其進一步含有步驟： (a) 將烴類進料通過含有蒸汽重組催化劑之反應器以移 除或降低在烴類進料中之較高級烴類之含量； (b) 將來自第一反應器之流出物通過自熱性重組器；且 (c) 從自熱性重組器中取出富含氫氣與一氧化碳之產物 氣體。 2. 根據申請專利範圍第1項之方法，其中該烴類進料 係天然氣及/或伴生氣體(associated gas)。 .3.根據申請專利範圍第1或2項之方法，其中該第一 反應器係絕熱操作。 4. 根據申請專利範圍第1或2項之方法，其中在第一 反應器出口之溫度係低於600°C。 5. 根據申請專利範圍第3項之方法，其中在第一反應 器出口之溫度係低於600°C。 1 本紙張尺度適用中國國家標準（CNS)A4規格(210 X 297公釐）
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NO994653D0 (no) 1999-09-24
DE69924200T2 (de) 2005-08-04
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EP0989094A2 (en) 2000-03-29
ATE290998T1 (de) 2005-04-15
US20010008621A1 (en) 2001-07-19
EP1426329A1 (en) 2004-06-09
DK199801211A (da) 2000-03-26
DK173897B1 (da) 2002-02-04
ES2238800T3 (es) 2005-09-01
KR20000023408A (ko) 2000-04-25
DE989094T1 (de) 2003-08-14
JP2000185904A (ja) 2000-07-04
EP0989094B1 (en) 2005-03-16
DE04005908T1 (de) 2005-09-15
NO994653L (no) 2000-03-27
CN1840468A (zh) 2006-10-04
DE69924200D1 (de) 2005-04-21
US6375916B2 (en) 2002-04-23
EP0989094A3 (en) 2000-09-27
CN1249267A (zh) 2000-04-05
CN1250446C (zh) 2006-04-12

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