TW304935B - - Google Patents

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Publication number
TW304935B
TW304935B TW82110419A TW82110419A TW304935B TW 304935 B TW304935 B TW 304935B TW 82110419 A TW82110419 A TW 82110419A TW 82110419 A TW82110419 A TW 82110419A TW 304935 B TW304935 B TW 304935B
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TW
Taiwan
Prior art keywords
refractory
composition
patent application
item
composition according
Prior art date
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TW82110419A
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English (en)
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Foseco Int
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/628—Coating the powders or the macroscopic reinforcing agents
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D41/00—Casting melt-holding vessels, e.g. ladles, tundishes, cups or the like
    • B22D41/02—Linings
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B22/00—Use of inorganic materials as active ingredients for mortars, concrete or artificial stone, e.g. accelerators, shrinkage compensating agents
    • C04B22/0066—Compounds chosen for their high crystalwater content
    • C—CHEMISTRY; METALLURGY
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    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B33/00—Clay-wares
    • C04B33/02—Preparing or treating the raw materials individually or as batches
    • C04B33/025—Mixtures of materials with different sizes
    • C—CHEMISTRY; METALLURGY
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    • C04B33/00—Clay-wares
    • C04B33/02—Preparing or treating the raw materials individually or as batches
    • C04B33/13—Compounding ingredients
    • C04B33/132—Waste materials; Refuse; Residues
    • C04B33/135—Combustion residues, e.g. fly ash, incineration waste
    • C04B33/1352—Fuel ashes, e.g. fly ash
    • C—CHEMISTRY; METALLURGY
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    • C04B33/22—Grog products
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/6303—Inorganic additives
    • C04B35/6306—Binders based on phosphoric acids or phosphates
    • C04B35/6313—Alkali metal or alkaline earth metal phosphates
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    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/6303—Inorganic additives
    • C04B35/6316—Binders based on silicon compounds
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    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632—Organic additives
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    • C04B35/64—Burning or sintering processes
    • C04B35/65—Reaction sintering of free metal- or free silicon-containing compositions
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D1/00—Casings; Linings; Walls; Roofs
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D1/00—Casings; Linings; Walls; Roofs
    • F27D1/0003—Linings or walls
    • F27D1/0006—Linings or walls formed from bricks or layers with a particular composition or specific characteristics
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    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00431—Refractory materials
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
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    • C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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    • Y02W30/91—Use of waste materials as fillers for mortars or concrete

Description

304935
五、發明說明（1 1况明（i ) 本發明係關於呈乾燥狀態以產製耐火物件之耐火組成 物，例如，爐用襯裡或冶金容器如杓、桶盆或流槽。 通常產製耐火產物（而不管彼等係用於特定用途之預 成形物件，爐用襯裡或冶金容器）所採用之方法（如撞擊、 鏟製、噴製或鑄製）係使用呈水性漿液、模塑或銬製物質 形式之濕式耐火組成物。此種方法之缺點在於彼等頗耗時 因爲除了初次利用之外或者成形過程亦需要乾燥步驟而且 經常需要額外煆燒或燒結步驟。亦必須將組成物維持在適 合於施用之條件下且問題在於此種固體物質傾向於沉降。 於使用時其中某些方法（例如噴製）由於需要相對複雜設 備而造成阻斷，且全部濕式方法需要在原處施用水以產製 呈合宜施用形式之組成物。 因而已提議另一種方法而此涉及使用在實質上乾燥而 耐火的組成物而能於成形或使用後能以熱將彼固化或硬化。 歐洲專利申請案第00648643號説明在一種冶金容器内 施用一種單石化耐火層之方法而此係使用一種在實質上乾 燥粒狀結合體：至少7〇重量％耐火凝結體，至少〇·5重量 %熱固性樹脂、約〇 5重量％至1〇重量％無機結合體及任 意地約0.5重量％至10重量％無機水合體。 國際專利申請案第92/09542號説明-種熱活化乾性耐 火組成物而此係用以產製在爐或其它高溫容器中之—種新 的耐火襯裡或修補既存的耐火襯裡。此種組成物係由下列 所組成.約35重量％至約85重量％耐火凝結體及約15重量 %至約50«% (含有約5至約9莫耳晶賴結水）之水合 木縣 ΚΛ 地;t]，卜内!Λ1 $ d ((' \ S ) Ψ，! ^||先閲^背而之;±*货^再填、寫本頁) 裝. .π_ 經濟部中央標準局5«工消费合作社43·? s〇4935 Λ6 Β6 經濟部中央標準局 5ΗΗί:"Η"ίΐ,λ'ν: 五、發明説明（2 ) 物質，水構成總組成物之約7重量％至約35重量％。 若將組成物施用至欲加襯裡或修補之熱表面，則水合 物質係以足量存在（關於含於其中之化學結合水之數量） 以提供組成物之水份進而造成組成物具自身流動性。 兹已發現若組成物亦含有能與無機黏合劑起放熱反應 之元素或化合物，則亦能改善含有具化學或物理鍵結水之 無機黏合劑之乾性耐火組成物之效能。 根據本發明亦提供一種包括下列之在實質上乾性、自 身硬化而熱活化之耐火組成物：粒狀耐火物質、其内具有 化學或物理鍵結水之無機黏合劑，及能與無機黏合劑起放 熱反應之元素或化合物。 粒狀耐火物質以構成組成物之約7〇重量％至約95重％ 較佳而可爲例如珍石、結石、碳化妙、銘氧（c〇rundum)、 鎂土（經煆燒菱鎂礦）、經煆燒白雲石、鉻菱鎂礦、橄欖 石、鎂橄欖石、藍晶石、紅柱石、玲羊石、碳或絡鐵礦、 或一種由二種或多種這些物質之混合體。 組成物亦可含有低密度粒狀耐火物質如經展延眞珠石、 經展延蛭石、矽藻土、飄塵浮渣而此係爲了視情況需要而 降低經熟化組成物之密度。 具有隨即與化學鍵結水聯合之合宜無機黏合劑之實例 係晶形水合鹽類如碎酸鹽、碳酸鹽、硫酸鹽、硝酸鹽、棚 酸鹽或磷酸鹽類。這些鹽類包含五水合偏矽酸鈉、單水合 偏矽酸鈉、十八水合硫酸鋁、七水合硫酸鎂、十水合四硼 酸鈉、三水合碳酸鎂、六水合硝酸鎂、十二水合硫酸鋁卸、 ·· 4 — (凊先閲冶背而之注念评項再場寫本頁) 丨裝· *π- 線· 經濟部中央標準局員工消费合作杜印^ Λ6 ' __________RG ___ 五、發明説明（3 ) 十一水p疏酸銘鋼及十二水合三鹽基鱗酸納。較佳者爲五
Jc口發酸@及十—水合二鹽基鱗酸納。具有在物理上與結 。水聯。〈合宜無齡料之實例錄膠囊财酸钟溶液 (水玻璃）及微膠囊化正彻銘水溶液。通常無機黏合劑 (包含化學或物理結合水）構成耐纽成物之約1重量％ 至約15重量％。 能與無機黏合劑起放熱反應之元素或化合物例如梦鐵、 氧化妈、氧化鍰、館或水泥，而且通常構成耐火組成物之 約1重量/6至約15重量％。以鋁較佳且可用以作爲粉末或 作爲小薄片塊。 爲了防止介於無機黏合劑與能和黏合劑起放熱反應之 元素或化合物之間產生過早反應，理想方式係使組合物含 有-種抑制劑例如礦物油或植物油。若使用此種抑制劑， 則彼通常構成耐灰組合物之_」重量％至約5重量％。 製得本發明實質上乾燥耐火組合物而以將個別組份徹 底混合在一起。 可以各種不同方式使用組合物產製耐火元件，例如， 以組合物填充合宜模子，或在冶金容器中產製一種襯裡而 以組合物填充介於欲加襯表面及合宜模型間之空間，然後 將組成物局部加熱以5丨發介於無機黏合劑與能和黏合劑起 放熱反應之元素或化合物間之硬化反應。達成將組合物局 部加熱而以使用一種至少部份受熱之模子、模型或容器或 施熱至一部份組合物例如以氣炬。 本發明之耐火組合物，實質上乾燥而具流動性之粉末， (<'NS) f ·ι )t;.|a (：>|〇 x ；).)· ) 一 --- i.%先閲---2:而之注"pJfi再塡寫本頁) —裝， 訂 經 部 中 央 標 局 π ft： 社 印 Λ 6 Β6 五、發明説明（4 ) 此很容易使用至各類應用方面，特定言之，用以產製爐或 冶金容器之正面襯裡或背襯，此種冶金容器如构、桶盆、 流槽或在熔煉鋁中所使用之鍋槽，且用以產製耐火既定形 狀物件。此種組合物具有相對短的熟化期，以致於既定形 狀物件、襯裡等係很容易以相對快速使用，且可將彼等調 製以致於產製質輕而具高度熱絕緣物件。 下列實例係可資用以説明本發明。 例1 製得一種實質上乾燥、自身硬化而熱活化之耐火組合 物而以將下列組份以所指明之比例混合在一起： 重量％ 羚羊石（45.6% Al2〇3 ; 1至3毫米） 羚羊石（45.6% Al2〇3 ;至高達毫米） 藍晶石（小於35網目DIN) 紅柱石（至高達〇·16毫米） 鋁喷粉 鋁薄片粉（鋁箔粉） 五水合偏矽酸鋁油(AVILUB RS22) 使用組成物以產製具5〇毫米直徑及5〇毫米高度之圓柱 體而以將組成物撞擊入硬紙板筒内且將彼熟化而以將本生 燈火培施用至I撞擊組成物之頂端。將經熟化圓柱體於 分鐘後從硬紙板筒内剝離出。 46.00 22,50 9.00 4.50 3.0010.00 4.50 0.50 在室溫量測某些圓括<1* 士陆、 圓枉，<壓縮強度，且將其它圓柱 體 f請先聞凉背面之;±*來¾再場寫本頁) -装. 、1T. 夂紙讯(C：NS) 'P .1
Λ6 ί?6 五、發明説明（5 ) 以每小時4〇(TC之速率加熱至高達150(TC而後以相同之速率 冷卻至室溫，而後測定彼等之壓縮強度。以在裝有量表（數 値以Kp計）之水壓機上完成量測。 測定圓柱體之滲透度而以使用供測定鉾砂試驗核心滲 透性所使用型式之GF滲透性試驗器。 於加熱至1500°C前後測定圓柱體之密度，且亦量測加 熱至1500°C所造成體積膨脹0 將所得平均結果列表如下： 滲透度（室溫） 滲透度（1500°C ) 密度（室溫） 密度（ 1500°C) 體積膨脹度（膨脹體積）-8.9% 壓縮強度（室溫） 45Kp 壓縮強度（ 1500°C) 292Kp 例2 650 460 1.20克/立方厘米 1.25克/立方厘米 -裝- 訂_ 製得一種類似於例1之組成物而以所指明比例混合下列 成份： 重量％ 羚羊石（45.6% Al2〇3 ; 1至3毫米） 30.00 羚羊石（45.6% Al2〇3 ;至高1毫米） 26.00 羚羊石（70.5% Al2〇3 ;至高1毫米） 20.00 羚羊石（38.8% Al2〇3 ; 0.25至1毫米） 8.00 藍晶石（小於35網晶DIN) 3.35 .尺_尺4!!丨闪阀家·^川（<:、 (::印 Λ6 B6 經濟部中央標準局員工消费合作社印製 五、發明説明（6 ) 鋁噴粉 3.00 鋁箔粉 5.00 五水合偏矽酸鈉 4.50 油（SVILUB RS22) 0.15 以如例1中所説明方式使用及試驗組成物除了測定壓縮 強度係圓柱體上而此已分別熱至500°C、700°C、1000°C及 1200°C，然後將彼冷卻。 將所得平均結果列於下： 滲透度（室溫） 340 滲透度（1500°C ) 330 费度（室溫） 1.19克/立方厘米 密度（ 1500°C) 1.17克/立方厘米 膨脹體積 6.1% 壓縮強度（室溫） 114Kp 壓縮強度（ 500°C ) 119Kp 壓縮強度（ 700°C ) 272Kp 壓縮強度（1000°C ) 214Kp 壓縮強度（1200°C ) 400Kp 壓縮強度（ 1500°C) 800Κρ m 製得用以作爲一種金屬鑄造杓襯裡之實質上乾燥之自 身硬化熱活化耐火組成物而以將下列組成物A及B在一種混 凝土拌合器内而以1 : 1之重量比例混合在一起歷15分鐘。 ---- 8 〆 A B 如紙张適叫中R内京d ((.:NS>，ρ 1叱格（？1“ X y V ) (請乇閲‘：七背而之汶念賁項再塡寫本頁) -裝. 訂. .線.
3ϋ4δ35 寻捫τ哥系弟ν i川4 iyst ROC Patent Appln. No. 82110419 中文説明黨修正K -附件Θ of the Chinese Specification - Enc1. M平a珍正！迷呈) I i Submitted on June ι·^>, 1995) 赞明説明（7) 重量％ 重量％ 羚羊石（45.6% Al2〇3 ; 1至3毫米） 20.0 40.0 羚羊石（45.6¾ Al2〇3 ;至高1毫米） 20.0 40.0 玲羊石（70.5% A〖2〇3，至高1毫米） 25.8 10.2 羚羊石（38.8¾ Al2〇3 ; 0.25至1毫米） 16.0 藍晶石（少於35網晶D1N) 6.8 — 五水合偏梦酸納· — 9.0 鋁喷粉 - 6.0 — 铭箔粉 5.0 — 油（SVILUB RS22) 0.4 0.8 於混合後，將組合轫在锅杓底部撞擊。然後將成形體 置於杓内部後，將組成物填充在介於成形體及杓内部表面 間之空間以產生一種襯裡。以火焰將組合物局部加熱而後 容許自身硬化歷20分鐘。然後將成型體移離而後將成形襯 裡表面以結爲基之塗料（CERAMOL 258)塗敷。 使用例1中所説明方法測定襯裡材料之壓縮強度而以於 下列三種情況：於剝離後立即進行、加熱至l〇〇〇〇c後及加 熱至150ITC後。 亦使用例1中所説明方法測定滲透性、密度及膨脹體積。 在熟化厚片材上測定經由材料之熱損耗速率及於丨小時 後之總熱損耗量而以使用英國專利1018703號所説明型式之 AMITEC 裝置。 得到下列結果： 壓縮強度（室溫） 307Kp 本紙張尺度適用中國國豕襟準（CNS ) A4規格（2IOX297公慶 m 叫^1T(-^ (請先閲讀背面之注意事項再填寫本頁) 經濟部中央梂準局WC工消費合作社印裂 Λ6 Λ6 398Kp 792Κρ 142 198 1.634克/立方厘米 1.573克/立方厘米 3.9% 0.6卡/平方厘米、秒 300卡/平方厘米 「^先閱：..!'背而之：'.1:4杯^再填寫本頁> 、發明説明（8 ) 壓縮強度（1200°C ) 壓縮強度（1500°C ) 滲透度（室溫） 滲透度（1500°C ) 密度（室溫） 密度（1500°C) 膨脹體積 熱耗損速率 於1小時後熱耗損量 .裝. —種用以聯結杓所使用典型耐火混泥土型式具有熱寻員 耗速率大小爲0.8卡/平方厘米、秒且於1小時後之熱耗損量 爲4000卡/平方厘米而且此係使用相同設備量測。 訂， 例4 製得25公斤下列組成物而以將個別成份在混泥土拌合 器·土混合在一起歷15分鐘： 經濟部中央標準局員工^：费合作、} 奔羊石（45.6% Al2〇3 羚羊石（45.6% A1203 羚羊石（70.5% Al2〇3 飄塵浮;查 五水合偏矽酸鈉 油（SVILUB RS22) 1至3亳米） 至高1毫来） 至高1毫米） ϋ% 31.75 31.75 5.40 25.71 4.76 0.63 8重量％ 然後將以上述喷銘粉組合物之重量爲基準之5 加入而後持續混合歷10分鐘。 木纸丨II’卜同Rtd. (CNS) ψ
304935 Λ6 ΒΓ) 五、發明説明（9 ) 以如例1中所説明方式試驗某些組合物以測定其熟化室 溫壓縮強度及密度。經熟化組合物具有壓縮強度爲61牛頓 /平方厘米及密度爲0.9克/立方厘米。 將能形成約25毫米厚度基底之足量組合物置於鋼构底 部而此在底部每100毫米間隔具有2至3毫米直徑之排氣孔且 在侧壁每隔150毫米亦然。將一種具有直徑小於鋼杓直徑4 厘米之預成形INSURAL牌杓櫬裡（取自Foseco公司）置於杓 基底組合物上以致於介於INSURAL觀裡及杓侧壁間形成空間。 然後將可自由流動且需要少許壓縮之其餘組合物倒入此種 空間内以填充達杓頂之空間。然後將氣炬施用至杓基底外 圍以謗發在襯裡組合物中之放熱反應。於約45分鐘後，反 應已進行至整個背襯裡且組合物已完全熟化、而後使用加 襯裡之构以支持熔融銘0 例5 製成一種類似於例4中所説明之組合物而彼含有十二水 合三驗式磷酸鋼以取代五水合偏碎酸納並試驗之。 此種經熟化組合物具有壓縮強度爲186牛頓/平方厘米 及密度爲0.86克/立方厘米。 (請先閱讀背面之注-事哨再增寫本页) 丨裝· 訂. 經濟部中央標準局員工消费合作社印製 未紙讯&度過H]中阀丨(<'NS)甲格X )

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  1. 修 it 85· 2 1 補充本年用 A8 B8 C8 D8 六、申請專利範圍 ΡΑΓ ί利申气案第82110419號 Appln* No.82110419 修i户申請專利範圍中文本-附件㈠ blinded. Claims in Chine^p - Enel.(T ) TKW^«5 -f- 10 ^ il~~g~~WK)~~^ (bubutted on October 21 , 1996) 經濟部中央標隼局員工消費合作社印製 1. 一種實質上乾燥、自身^匕、\且經熱活化之耐火组合 物，其係包括以重量之粒狀耐火物質、1% 至15%之無機黏合劑機黏合劑係含有選自於石户 酸鹽與_酸鹽中之晶形水合鹽，以及1¾至15%會與無 機黏合劑行放熱反應之鋁。 2. 根據申請專利範囷第1項之耐火組合物，其中粒狀耐 火物質係爲矽石、鲒石、碳化矽、氧化鋁、氧化錢、 經锻燒之白雲石、鉻菱鎂礦、橄欖石、鎂橄欖石、藍 鐵读、藍晶石、紅柱石、玲羊石、碳或路鐵積，或二 或多種上述物質之混合物。 3. 根據申請專利範圍第1項之耐火組合物，其中晶形水 合鹽係五水合偏矽酸鈉、九水合偏矽酸鈉或十二水合 三鹽基磷酸鈉。 4. 根據申請專利範園第1項之耐火组合物，其中該组合 物係含有一選自下列之低密度粒狀耐火物：經展延眞 珠石、經展延蛭石、矽藻土與飄塵浮渣。 5. 根據申請專利範圍第1項之对火組合物，其中該組合 物亦含有積物油或植物油。 6. 根據申請專利範圍第5項之耐火組合物，其中礦物油 或植物油之存在量係以重量計0.1¾至5%。 _96-9F0SEC0 194QA-M --------裝------灯------I.A (請先聞讀背面之注意事項再填寫本頁) 本紙張尺度適用中國國家標準（CNS ) Λ4規格（210 X 297公釐）
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KR100241129B1 (ko) 2000-02-01
GB9226662D0 (en) 1993-02-17
US6284688B1 (en) 2001-09-04
WO1994014727A1 (en) 1994-07-07
ES2099570T3 (es) 1997-05-16
EP0675862A1 (en) 1995-10-11
CA2147247C (en) 2003-04-29
DE69309105T2 (de) 1997-08-21
ZA939201B (en) 1994-08-08
KR950704210A (ko) 1995-11-17
MX9307923A (es) 1994-06-30
AU669769B2 (en) 1996-06-20
JPH08507282A (ja) 1996-08-06
CA2147247A1 (en) 1994-07-07
BR9307724A (pt) 1999-08-31
DE69309105D1 (de) 1997-04-24
IN182871B (zh) 1999-07-31
AU5570794A (en) 1994-07-19
ATE150435T1 (de) 1997-04-15
EP0675862B1 (en) 1997-03-19

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