TW591147B - Alumina fiber aggregate and its production method - Google Patents

Alumina fiber aggregate and its production method Download PDF

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Publication number
TW591147B
TW591147B TW91116173A TW91116173A TW591147B TW 591147 B TW591147 B TW 591147B TW 91116173 A TW91116173 A TW 91116173A TW 91116173 A TW91116173 A TW 91116173A TW 591147 B TW591147 B TW 591147B
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Taiwan
Prior art keywords
fiber
oxygen
alumino
spinning
alumina
Prior art date
Application number
TW91116173A
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English (en)
Inventor
Mamoru Shoji
Norio Ikeda
Toshiaki Sasaki
Original Assignee
Mitsubishi Kagaku Sanshi Corp
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    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
    • 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
    • C04B35/62227—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
    • C04B35/62231—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on oxide ceramics
    • C04B35/62236—Fibres based on aluminium oxide
    • 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
    • C04B35/62227—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
    • C04B35/62231—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on oxide ceramics
    • C04B35/6224—Fibres based on silica
    • C04B35/62245—Fibres based on silica rich in aluminium oxide
    • 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
    • C04B35/63—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
    • C04B35/634—Polymers
    • C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B35/63416—Polyvinylalcohols [PVA]; Polyvinylacetates
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D—TEXTILES; PAPER
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    • D—TEXTILES; PAPER
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    • D04H1/4234—Metal fibres
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    • D04H1/46—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling by needling or like operations to cause entanglement of fibres
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/44—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling
    • D04H1/46—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling by needling or like operations to cause entanglement of fibres
    • D04H1/498—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling by needling or like operations to cause entanglement of fibres entanglement of layered webs
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
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    • D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
    • E—FIXED CONSTRUCTIONS
    • E04—BUILDING
    • E04B—GENERAL BUILDING CONSTRUCTIONS; WALLS, e.g. PARTITIONS; ROOFS; FLOORS; CEILINGS; INSULATION OR OTHER PROTECTION OF BUILDINGS
    • E04B1/00—Constructions in general; Structures which are not restricted either to walls, e.g. partitions, or floors or ceilings or roofs
    • E04B1/62—Insulation or other protection; Elements or use of specified material therefor
    • E04B1/74—Heat, sound or noise insulation, absorption, or reflection; Other building methods affording favourable thermal or acoustical conditions, e.g. accumulating of heat within walls
    • E04B1/76—Heat, sound or noise insulation, absorption, or reflection; Other building methods affording favourable thermal or acoustical conditions, e.g. accumulating of heat within walls specifically with respect to heat only
    • E04B1/7654—Heat, sound or noise insulation, absorption, or reflection; Other building methods affording favourable thermal or acoustical conditions, e.g. accumulating of heat within walls specifically with respect to heat only comprising an insulating layer, disposed between two longitudinal supporting elements, e.g. to insulate ceilings
    • E04B1/7658—Heat, sound or noise insulation, absorption, or reflection; Other building methods affording favourable thermal or acoustical conditions, e.g. accumulating of heat within walls specifically with respect to heat only comprising an insulating layer, disposed between two longitudinal supporting elements, e.g. to insulate ceilings comprising fiber insulation, e.g. as panels or loose filled fibres
    • E04B1/7662—Heat, sound or noise insulation, absorption, or reflection; Other building methods affording favourable thermal or acoustical conditions, e.g. accumulating of heat within walls specifically with respect to heat only comprising an insulating layer, disposed between two longitudinal supporting elements, e.g. to insulate ceilings comprising fiber insulation, e.g. as panels or loose filled fibres comprising fiber blankets or batts
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    • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
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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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    • C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
    • C04B2235/444—Halide containing anions, e.g. bromide, iodate, chlorite
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52—Constituents or additives characterised by their shapes
    • C04B2235/5208—Fibers
    • C04B2235/5264—Fibers characterised by the diameter of the fibers
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
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    • Y10T428/26—Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension
    • Y10T428/263—Coating layer not in excess of 5 mils thick or equivalent
    • Y10T428/264—Up to 3 mils
    • Y10T428/265—1 mil or less
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2913—Rod, strand, filament or fiber

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Textile Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Architecture (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • Electromagnetism (AREA)
  • Acoustics & Sound (AREA)
  • Civil Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Fibers (AREA)

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9 4 A7 ____B7 五、發明説明（’） 本發明係有關鋁氧纖維聚集體及其製造方法。 (請先閱讀背面之注意事項再填寫本頁) 鋁氧纖維聚集體係活化其良好耐熱性，於鋁氧纖維夾 線板等加工後做爲絕熱材料等被使用之。該鋁氧纖維夾線 板係如以下方法進行製造者。 亦即，以放漿法進行含鹼性氯化鋁、砍化合物、有機 聚合物及水之紡絲液的紡絲後，將取得鋁氧短纖維前驅物 之聚集體（層合薄片）於必要時施予植針後進行燒成。且 於燒成步驟中去除揮發成份之同時進行鋁氧粉與二氧化矽 之結晶化後變換成鋁氧纖維。其結果取得由鋁氧短纖維所 成之鋁氧纖維聚集體。該製造方法通常稱爲前驅體纖維化 法。 而，當鋁氧短纖維直徑小時，則鋁氧短纖維易於飛散 ，使用性不佳之同時，衛生環境亦差。亦即，直徑爲數 V m以下之纖維易經過呼吸進入人體肺泡等問題被指出。 經濟部智慧財產局ϋ貝工消費合作钍印製 本發明鑑於該情況，而以提供一種由鋁氧短纖維所成 之鋁氧纖維聚集體者，鋁氧短纖維之直徑被擴徑化後，可 抑制鋁氧短纖維之飛散的鋁氧纖維聚集體及其製造方法， 爲其目的者。 本發明者經過精密檢討後，結果發現鋁氧短纖維之直 徑藉由所使用紡絲液之性狀變化後，使用特定性狀之紡絲 液，且，藉由最適當之紡絲條件後，可取得纖維徑大，且 ，纖維徑分佈小之鋁氧短纖維者，進而完成本發明。 本發明係基於上述發現而完成者，其第1主旨之特徵 係由平均纖維徑爲4 . 0〜1 〇 · 〇 # m，且最低纖維徑 -4- 本紙張尺度適用中國國家標準（CNS ) Α4規格（21〇ΧΜ7公釐） 9 4 A7 ____B7 五、發明説明（2 ) 爲3 · 0 // m之鋁氧短纖維所成之鋁氧聚集體者。 (請先閱讀背面之注意事項再填寫本頁) 本發明第2主旨之特徵係以放漿法使含有鹼性氯化銘 、矽化合物、有機聚合物及水之紡絲液進行紡絲，於燒成 取得鋁氧短纖維前驅物聚集體之鋁氧短纖維聚集體的製造 方法中，做爲該紡絲液者使用鋁與矽之比以A 1 2 0 3與 S i〇2之重量比換算後爲99 : 1〜65 : 35，鹼性氯 化鋁濃度爲1 8 0〜2 0 0 g/L，有機聚合物濃度爲 2 〇〜4 0 g / L之紡絲液者，由平均纖維徑爲4 · 0〜 10 . O/zm，且，最低纖維徑爲3 · 0#m以上之鋁氧 短纖維所成之鋁氧纖維聚集體的製造方法者。 以下，進行本發明詳細說明。首先爲方便進行說明， 針對本發明鋁氧纖維聚集體之製造方法進行說明之。 本發明製造方法係以放漿法將含有鹼性氯化鋁、矽化 合物、有機聚合物及水之紡絲液進行紡絲後，燒成取得之 鋁氧短纖維前驅物之聚合物方法（前驅物纖維化法）者。 而主要係由紡絲液之調製步驟，紡絲步驟，燒成步驟所成 ，必要時於紡絲步驟與燒成步驟間設定植針步驟者。 經濟部智慧財產局員工消費合作社印製 <紡絲液之調製步驟> 鹼性氯化鋁；A 1 (〇Η ) 3 - X C 1 X係於鹽酸或氯化 鋁水溶液中使金屬鋁溶解後進行調製者。該化學式中X之 値通常爲0 · 45〜0 · 54，較佳者爲0 · 50〜 0 · 5 3。做爲矽化合物者以矽溶膠爲理想使用者，此外 ，亦可使用四乙基矽酸酯、水溶性矽氧烷衍生物等水溶性 本紙張尺度適用中國國家標準（CNS ) Α4規格（210Χ297公釐） -5- 9 47 經濟部智慧財產局員工消費合作社印製 A7 B7五、發明説明（3 ) 矽化合物者。做爲有機聚合物者如：聚乙烯醇、聚乙二醇 、聚丙烯醯胺等水溶性高分子化合物爲理想使用者。此等 聚合度爲1000〜3000者。 本發明中，做爲該紡絲液者以使用其鋁與矽之比以 A12〇3與Si〇2之重量比換算後爲99 : 1〜65 : 35，鹼性氯化鋁之濃度爲180〜200g/L，有機 聚合物濃度爲2 0〜4 0 g / L之紡絲液者爲重點。 當矽化合物之量低於該範圍時，則構成短纖維之氧化 鋁易進行α -鋁氧化，且，藉由鋁氧粒子之粗大化易使短 纖維脆化。反之，矽化合物量大於該範圍時，與多鋁紅柱 石（3Α 12〇3 · 2S i〇2)同時產生二氧化矽（ S i 0 2 )之量增加而降低耐熱性。以A 1 2 0 3與S i〇2 重·量比換算後之鋁與矽比一般爲9 9 : 1〜6 5 : 3 5， 較佳者爲99 : 1〜70 : 30，更佳者爲98 : 2〜 7 2:2 8° 當鹼性氯化鋁之濃度低於1 8 0 g / L時，或有機聚 合物濃度小於2 0 g / L時，均未能取得理想黏度，纖維 徑變小。亦即，紡絲液中之游離水太多之結果，藉由放漿 法後，紡絲時之乾燥速度延緩，過度延伸，被紡絲之前驅 物纖維徑變化後，無法取得纖維徑大，且，纖維徑分佈小 之短纖維。且，鹼性氯化鋁濃度低於1 8 0 g / L時，將 降低生產性。另外，鹼性氯化鋁濃度大於2 0 0 g / L或 有機聚合物濃度大於4 0 g / L時，則黏度均過高而無法 呈紡絲液。理想之鹼性氯化鋁濃度以1 8 5〜1 9 5 g / (請先閱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隼（CNS ) A4規格（2丨0X297公釐） -6 - 9 4 經濟部智慧財產局員工消費合作社印製 A7 B7五、發明説明（4 ) L者宜，有機聚合物濃度爲3 0〜4 0 g/L者宜。 該紡絲液係添加矽化合物及有機聚合物於鹼性氯化鋁 水溶液中，藉由上述範圍之濃縮進行調製鹼性氯化鋁及有 機聚合物之濃度。常溫下之紡絲液黏度通常爲1〜 1 0 0 0泊者宜，較佳者爲1 0〜1 0 0泊者。 <紡絲> 紡絲（紡絲液之纖維化）係於高速紡絲氣流中進行供 與紡絲液之放漿法，藉此，取得長度呈數十m m〜數百m m之鋁氧短纖維前驅物者。 於上述紡絲時所使用之紡絲噴嘴結構並無特別限定， 一般以如：歐洲專利第4 9 5 4 6 6號公報（日本專利第 2 6 0 2 4 6 0號公報）所載之由氣式噴嘴吹出空氣流與 由紡絲液供給噴嘴擠壓出紡絲液流呈並行流，且與空氣之 並行流充份被整流之紡絲液相互接觸之結構者宜。此時， 紡絲噴嘴之直徑以0 · 1〜〇 · 5 m m者宜，1根紡絲液 供給噴嘴之液量爲1〜1 2 0 m 1 / h，較佳者爲3〜 5 Om Ι/h，氣式噴嘴之狹縫氣體流速爲4 0〜2 0 0 m / s 者。 藉由此紡絲噴嘴，由紡絲液供給噴嘴擠出之紡絲液不 會呈霧狀，充份被延伸後，纖維相互不易熔合，因此，藉 由最適當之紡絲條件後，可取得纖維徑均勻狹窄分佈之鋁 氧纖維前驅物者。 又，紡絲時，先於控制水份蒸發，紡絲液分解之條件 本紙張尺度適用中國國家標準（CNS ) A4規格（21〇><297公釐） 7 (請先閲讀背面之注意事項再填寫本頁) 591147 A7 _ _B7 五、發明説明（5 ) (請先閲讀背面之注意事項再填寫本頁) 下由紡絲液形成充份被延伸之纖維，再使此纖維迅速乾燥 者宜。因此，由紡絲液到達形成纖維之纖維收集器爲止之 過程中，由控制水份蒸發之狀態至促進水份蒸發狀態之變 化者宜。而，使紡絲液開始接觸空氣流附近之溫度做成 1 0〜2 0 0 °C，纖維收集器附近之空氣流溫度爲4 0〜 5 0°C，相對濕度爲3 0%以下者宜。 由紡絲液形成充份被延伸之纖維過程中該氣氛溫度太 高時，除水份劇烈蒸發之外，不易形成被充份延伸之纖維 ，且，形成之纖維出現缺陷，最後取得之無機氧化物纖維 呈脆弱化者。反之，抑制蒸發於低溫或高濕.度氣氛下，由 紡絲液形成纖維時，纖維形成後仍持續於同氣氛下，造成 纖維相互附著，彈性恢復後，呈液滴化後易出現散彈而不 理想。 鋁氧短纖維前驅物之聚集體係設置金網製無端帶於針 對紡絲氣流略呈直角狀後，使無端帶持續旋轉，於此使含 鋁氧短纖維前驅物之紡絲氣流藉由衝擊結構之集成裝置後 可連續回收薄片（薄層薄片）。 經濟部智慧財產局員工消費合作社印製 由該集成裝置所回收之薄層薄片係連續取出後送入折 疊裝置，以所定寬度重覆折疊之，往折疊方向呈直角方向 連續移動後可做成層合薄片。藉此，薄層薄片之兩端部寬 方向被配置於所形成層合薄片之內側，因此，層合薄片之 外觀量其薄片整體呈均勻者。做爲該折疊裝置者可利用歐 洲公開專利第9 7 1 0 5 7號公報（日本公開專利 2000 — 80547號公報）所載者。 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） -8- 591147 A7 B7 五、發明説明（6 ) 〈植針步驟〉 (請先閱讀背面之注意事項再填寫本頁) 於鋁氧短纖維前驅物之聚集體（層合薄片）施予植針 後可做成厚方向亦被配向之機械強度大之鋁氧纖維聚集體 者。植針之打數通常爲1〜5 0打/cm2，一般打數愈多 所取得鋁氧纖維聚集體之容積密度與剝離強度愈大。 <燒成步驟> 一般燒成溫度以5 0 0 °C以上者宜，較佳者於7 0 〇 〜1 4 0 0 °C下進行之。當燒成溫度低於5 0 0 °C時，則 結晶化不足，只能取得強度小，脆弱之鋁氧短纖維，反之 ，燒成溫度大於1 4 0 0 °C時，則促進纖維結晶粒之成長 後，只可取得強度小，脆弱之鋁氧短纖維者。 經濟部智慧財產局員工消費合作社印說 以下針對本發明鋁氧鋁纖維聚集體進行說明。本發明 鋁氧纖維聚集體係以如上述之製造方法取得者，結構由鋁 氧短纖維所成者。而，構成鋁氧纖維聚集體之鋁氧短纖維 之纖維徑大，且纖維徑分佈小者。亦即，本發明鋁氧纖維 聚集其鋁氧短纖維之平均纖維徑爲4 . 0〜1 0 . 〇/zm 者，且，最低纖維徑爲3 . 0//m以上爲其特徵者。鋁氧 短纖維之平均纖維徑下限以4 . 0 // m者宜，更佳者爲 5 · 0 // m。又，鋁氧短纖維之平均纖維徑小以5 . 0〜 8 . 0//m者宜，更佳者爲6 · 0〜8 . 0#m者。 當纖維徑小者愈多則纖維愈容易飛散，使用性不佳， 同時作業環境衛生亦不理想。又，纖維徑過大時，則降低 本紙張尺度適用中國國家標準（CNS ) A4規格（210X 297公釐） -9- 591147 A7 ___B7 五、發明説明（7 ) (請先閱讀背面之注意事項再填寫本頁) 鋁氧短纖維之聚集體絕熱性、彈性等而不理想。以上之度 數分佈係依後述測定纖維徑分佈之方法所測定之値者。又 ，其中所取得鋁氧短纖維長度爲1 0〜5 0 Omm者。 本發明鋁氧纖維聚集體因具有上述特徵，因此，如： 製造鋁氧纖維覆蓋之步驟中，操作上較少出現纖維之飛散 ，使用上及作業性環境衛生均較理想。 〔實施例〕 以下，藉由實施例更詳細說明本發明，惟，本發明在 不超出主旨範圍下，不僅限於以下實施例者。又，以下各 例中測定鋁氧單纖維之纖維徑分佈係依以下所示依序進行 者。 <測定纖維徑分佈之方法> (1)由銘氧纖維墊藉由鑷子取1個挖耳匙之量的纖 維。 經濟部智慧財產局員工消費合作社印製 (2 )於貼於掃描型電子顯微鏡（s E Μ )觀察用試 料台之碳製導電膠帶上將上述（1 )之纖維儘量不要重疊 下放置之。 (3 )該（2 )之纖維表面具導電性，試料表面蒸鍍 厚度1〜3 nm之鉑—鈀膜。
(4 )將蒸鍍之分析試料置入s E Μ測定室中，爲測 量纖維徑以適當倍率進行觀察之後，拍攝觀察晝面。以日 本電子公司製之掃描型電子顯微鏡「j SM〜6 3 2 〇 F 本紙張尺度適用中國國家標準（CNS ) A4規格(210X 297公楚) - 591147 A7 B7 五、發明説明（8 ) (請先閲讀背面之注意事項再填寫本頁) 」做爲裝置之使用，觀察條件採加速電壓1 5 K V，操作 調整（WD) 1. 5mm者。又，倍率1〇〇〇〜3000 之範圍內進行適當選取之。 (5 )由該（4 )所攝影之S E Μ照片以游標或直尺 測至0 . 1 m m單位。再測定任意合計1 〇 〇根之纖維徑 〇 (6 )藉由下式計算平均纖維徑。此時計算値以小數 點第2位進行四捨五入，取小數點第1位者。 (7 )又，其中由纖維徑度數分佈傾向下限纖維徑出 現疑問時，通常重覆測定2〜4次，度數分佈以平均1 % 以上之徑做爲最低纖維徑。 〔數1〕 平均纖維徑（μ m)={100分之合計測定値/(100X觀察倍率 )} X 1,000 〔實施例1〕 <紡絲液之調製> 經濟部智慧財產局員工消費合作杜印製 首先添加鋁濃度爲1 6 5 g /L之鹼性氯化鋁； 1 . 0 L A 1 (〇H)3-xC1x(x = 0.51)之水 溶液爲2 0重量％矽溶膠溶液6 0 6 g，5重量％聚乙烯 醇（聚合度1 7 0 0 )水溶液6 0 8 g進行混合後，於 5 0 °C下進行減壓濃縮後取得紡絲液。紡絲液之黏度爲 6 0泊（2 5 °C下藉由旋轉黏度計之測定値），鋁與矽之 比（Al2〇3與Si〇2之重量比）爲72 . 0 : -11 - 本紙張尺度適用中國國家標準（CNS ) A4規格（210X 297公釐） 591147 A7 B7 五、發明説明（9 ) 2 8 · 0，鹼性氯化鋁之濃度爲1 9 0 g / L，有機聚合 物之濃度爲3 5 . Og/L者。 (請先閲讀背面之注意事項再填寫本頁) 〈紡絲〉 以放漿法進行該紡絲液之紡絲。做爲紡絲噴嘴者如： 使用與歐洲專利第4 9 5 4 6 6號公報（日本專利第 2 6 0 2 4 6 0號公報）圖6所載者相同結構之紡絲噴嘴 。而，紡絲係於紡絲液供給噴嘴之直徑0 . 3 m m，紡絲 液供給噴嘴1根之液量爲5 m 1 / h，空氣流速（氣式噴 嘴之狹縫部）：5 4 m/ s (壓力：2 k g / c m 2，溫度 :1 8 °C，相對濕度4 0 % )之條件下進行之。又，聚集 棉時，於高速空氣流以並行流進行乾燥後使1 5 0 °C之熱 風導入過濾網後，使纖維收集器附近之空氣流調成溫度 4 0 °C，相對濕度2 0 %者。再設置針對紡絲氣流略呈直 角之金網製無端帶，持續旋轉無端帶，於此使含鋁氧短纖 維前驅物之紡絲氣流藉由衝擊結構之集成裝置連續回收薄 片（薄層薄片）。 經濟部智慧財產局員工消費合作社印製 由集成裝置所回收之薄層薄片係連續抽出後送入折疊 裝置後，以所定寬度以折疊重疊之，針對折疊方向之直角 方向藉由連續移動後做成層合薄片。做爲該折疊裝置者使 用與歐洲公開專利第9 7 1 0 5 7號公報（日本公開專利 2 0 0 0 — 8 0 5 4 7號公報）所載者相同結構之折疊裝 置者。 本紙張尺度適用中國國家標準（CNS ) A4規格（210X 297公釐） -12- 591147 A7 ___B7^ 五、發明説明（1〇) <鋁氧纖維聚集體之製造> (請先閱讀背面之注意事項再填寫本頁) 於該層合薄片（鋁氧短纖維前驅物之聚集體）施予植 針後，於1 2 5 0 °C，空氣中進行燒成1小時後取得鋁氧 纖維聚集體。該植針係藉由針型穿孔機進行8次/ c m 2穿 孔後，進行之。測定取得鋁氧纖維聚集體之構成鋁氧短纖 維之纖維徑分佈後結果如表1所示。平均纖維徑爲6 . 9 /zm，最低纖維徑爲5 . 2#m者。 〔實施例2〕 <紡絲液之調製> 首先，添加鋁濃度爲1 6 5 g / L之鹼性氯化鋁； 經濟部智慧財產局員工消費合作社印製 1 · 0L 之 A1 (OH) 3-xC 1χ (x = 0 · 51)水溶 液爲2 0重量％矽溶膠溶液6 Ο 6 g，5重量％聚乙烯醇 (聚合度1 7 0 0 )水溶液6 0 8 g進行混合後，於5 0 °C下進行減壓濃縮後，取得紡絲液。紡絲液黏度爲4 0泊 (2 5 °C下藉由旋轉黏度計之測定値），鋁與矽之比（ Al2〇3與Si〇2之重量比）爲72 · 0 : 28 · 0 ， 鹼性氯化鋁濃度爲1 8 0 g / L，有機聚合物之濃度爲 3 3 . 2 g / L 者。 <紡絲及鋁氧纖維聚集體之製造> 與實施例1同法進行之。測定取得鋁氧纖維聚集體之 構成鋁氧短纖維纖維徑分佈後其結果示於表1。平均纖維 徑爲4 · 9 //m，最低纖維徑爲3 · 3 //m者。 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） -13- 591147 A7 B7 五、發明説明（Μ ) 〔比較例1〕 (請先閱讀背面之注意事項再填寫本頁) <紡絲液之調製> 添加鋁濃度爲7 5 g / L 之鹼性氯化鋁；1 · 0 L A1 (〇H) 3-xC lx (x = 〇 · 56)水溶液之 20 重 量％矽溶膠溶液2 7 6 g，5重量％聚乙烯醇（聚合度 1 7 0 0 )水溶液3 1 5 g進行混合後，5 0 °C下進行減 壓濃縮，取得紡絲液。紡絲液黏度爲4 0泊（2 5 °C下旋 轉黏度計之測定値），鋁與矽之比（A 1 2 0 3與S i〇2 之重量比）爲7 2 . 0 : 2 8 · 0，鹼性氯化鋁之濃度爲 160g/L，有機聚合物濃度爲33 · 6g/L者。 <紡絲及鋁氧纖維聚集體之製造> 經濟部智慧財產局員工消费合作社印製 使用與實施例1相同之紡絲噴嘴。而，紡絲係於紡絲 液供給噴嘴直徑〇 . 3 m m，紡絲液供給噴嘴1根之液量 5m Ι/h，空氣流速（氣式噴嘴之狹縫）：54m/s (壓力：2kg/cm2,溫度·· I8t：，相對濕度40% )之條件下進行之。又，收集棉時，於高速氣流以並行流 乾燥後’以9 0 °C之熱風導入過濾網後，將纖維收集器附 近之空氣流調節爲溫度3 5 °C，相對濕度3 0 %。再藉由 與實施例1相同之聚棉裝置，集成裝置連續回收薄片（薄 層薄片）。測定取得鋁氧纖維聚集體之構成鋁氧短纖維之 纖維徑分佈後，其結果示於表1。平均纖維徑爲 6 · 6//m，最低纖維徑爲2 · 2//m者。 本紙張尺度適用中國國家標準（CNS ) A4規格（2丨〇χ 297公廣） -14- 591147 A7 __________ B7 五、發明説明（12) 〔比較例2〕 (請先閱讀背面之注意事項再填寫本頁) <紡絲液之調製> 添加鋁濃度爲1 6 5 g / L之鹼性氯化鋁；1 . 〇 l 之A1 (〇1^)31〇13：(又=〇.51)水溶液爲20 重量％矽溶膠溶液6 〇 6 g，5重量％聚乙烯醇（聚合度 1 7 0 0 )水溶液2 6 0 g進行混合後，於5 0 °C下進行 減壓濃縮後，取得紡絲液。紡絲液黏度爲8泊（2 5 〇c下 旋轉黏度計之測定値），鋁與矽之比（A 1 2 0 3與 S i 0 2之重量比）爲7 2 · 0 : 2 8 · 0，鹼性氯化鋁之 濃度爲1 90g/L，有機聚合物濃度爲1 5 · Og/L 者。 <紡絲及鋁氧纖維聚集體之製造> 與實施例1同法進行之。測定取得鋁氧纖維聚集體之 構成鋁氧短纖維之纖維徑分佈後，結果示於表1。平均纖 維徑爲2 . 3//m，最低纖維徑爲〇 · 4//m者。 經濟部智慧財產局員工消費合作社印製 〔比較例3〕 <紡絲液之調製> 添加鋁濃度爲1 6 5 g / L之鹼性氯化鋁；1 · 〇 L A1 (〇^1)3-\(：1<(:^ = 〇.51)水溶液爲20重 量％矽溶膠溶液6 0 6 g，5重量％聚乙烯醇（聚合度 1 7 0 0 )水溶液5 5 0 g進行混合後，於5 0 t：下進行 本紙張尺度適用中國國家標隼（CNS ) A4規格（210X 297公釐） -15- 591147 A7 ___B7_ 五、發明説明（13) 減壓濃縮後，調整鋁與矽之比（A 1 2〇3與S i〇2之重 量比）爲7 2 . 0 ·· 2 8 . 0，鹼性氯化鋁之濃度爲 (請先閲讀背面之注意事項再填寫本頁) 2 10g/L，有機聚合物之濃度爲35 · Og/L。惟 ’取得組成物於濃縮階段呈固化狀態後，無法做成紡絲液 〇 〔比較例4〕 <紡絲液之調製> 添加鋁濃度爲1 6 5 g / L之鹼性氯化鋁；1 . 0 L 之 A1 (〇H)3-xClx(x = 0.51)水溶液爲 20 重量％矽溶膠溶液6 0 6 g，5重量％聚乙烯醇（聚合度 1 7 0 0 )水溶液8 6 8 g進行混合後，5 0 °C下進行減 壓濃縮後，調整鋁與矽之比（A 1 2 0 3與S i 0 2之重量 比）爲7 2 · 0 : 2 8 . 0，鹼性氯化鋁濃度爲1 9 0 g /L，有機聚合物濃度爲50 · Og/L者。惟，取得組 成物於濃縮階段黏度太高，無法藉由旋轉黏度計進行適當 測定黏度，無法取得紡絲性狀。 經濟部智慧財產局員工消費合作社印製 -16- 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） 591147
A B 五、發明説明（14) 經濟部智慧財產局員工消費合作杜印製 〔表1〕 <度數分布> 纖維徑（U m) 實施例1 實施例2 比較例1 比較例2 0.0^ • 垂 • 2 0.5^ • • • 9 1.0^ 一 - - 18 1.5^ • • 25 2.0^ • 1 15 2.5^ 續 • 5 5 3.0^ - 1 8 6 3.5^ • 6 3 7 4.0 ^ 13 8 3 4.5^ 33 18 2 5.0^ 5 18 11 2 5.5^ 13 21 9 3 6.0^ 32 1 7 1 6.5^ 21 4 3 - 7.0 ^ 8 - 5 1 7.5 ^ 7 3 • 8.0^ 5 _ 2 1 8.5 ^ 3 • 5 - 9.0^ 1 義 2 - 9.5 ^ 1 - 4 - 10.0^ 4 _ 6 辑 點數 100 100 100 100 平均 6.9 4.9 6.6 2.3 下限 5.2 3.3 2.2 0.4 (請先閱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 ) A4規格（210X297公釐） -17- 591147 B7 五、發明説明（15) 〔參考例1〕 (請先閲讀背面之注意事項再填寫本頁) 先行之鋁氧纖維平均纖維徑爲2〜5 // m者’針對3 公司市販之鋁氧纖維進行分析。其結果示於表2。 平均纖維徑（u m) 最低纖維徑U m) A社品 loti 3.6 1.1 lot2 3.7 1.4 lot3 4.6 1.8 lot4 3.0 0.7 B社品 3.0 1.3 C社品 loti 3.5 1.1 lot2 4.2 1.8 lot3 4.7 2.2 〔發明效果〕 經濟部智慧財產局員工消费合作社印製 以上說明之本發明係提供一種由鋁氧短纖維所成之鋁 氧纖維聚集體，鋁氧短纖維之直徑被擴徑化後，可抑制鋁 氧短纖維之飛散的鋁氧纖維聚集體及其製造方法者。該鋁 氧纖維聚集體於操作時纖維飛散少，使用上及作業環境衛 生面均佳。因此，突顯了本發明之工業價値者。 本紙張尺度適用中國國家標準（CNS ) A4規格（210X29*7公釐） -18-

Claims (1)

  1. 591147 ABCD
    「π. 申請專利範圍 第91116173號專利申請案 中文申請專利範圍修正本 民國93年1月5日修正 1 . 一種鋁氧纖維聚集體，·其特徵係由平均纖維徑爲 4 . 0〜1 0 · 〇 β m，且，最低纖維徑爲3 · 0 // m以 4之鋁氧短纖維所成者。 經濟部智慧財產局員工消費合作社印製 g 2 .如申請專利範圍第1項之鋁氧纖維聚集體 $最低纖維徑爲4 · 0 // m以上之鋁氧短纖維所成者 T 3 ·如申請專利範圍第1項之鋁氧纖維聚集體 _最低纖維徑爲5 · 0 // m以上之鋁氧短纖維所成者。 ί 4 ·如申請專利範圍第1項至第3項中任一項之鋁氧 後 7¾維聚集體，其中該平均纖維徑爲5 · 0〜8 . 0//m之 否 _呂氧短纖維所成者。 吏 5 ·如申請專利範圍第1項至第3項中任一項之鋁氧 維聚集體，其中該平均纖維徑爲6 · 0〜8 · 0 // m之 51鋁氧短纖維所成者。 6 ·如申請專利範圍第丨項至第3項中任一項之鋁氧 纖維聚集體’其中該鋁氧短纖維之組成其A 1 2 〇 3與 S i〇2重量比爲99 : 1〜65 : 35者。 7 · —種如申請專利範圍第1項至第6項中任一項所 述錕氧纖維聚集體之製造方法，其特徵係以放漿法進行含 有驗性氯化鋸、矽化合物、有機聚合物及水之紡絲液的紡 絲後’燒成取得鋁氧短纖維前驅物聚集體之鋁氧纖維聚集 其中 其中 (請先閲讀背面之注意事項再填寫本頁) 訂 本紙張尺m財目g家料（CNS ) 591147 A8 B8 C8 D8 ^、申請專利範圍 體之製造方法中，使用做爲該紡絲液者其鋁與矽之比以 Al2〇3與Si〇2重量比換算後爲99 : 1〜65 : 3 5 ，鹼性氯化鋁濃度爲1 8 0〜2 0 0 g / L，有機聚 合物濃度爲2 0〜4 0 g / L之紡絲液者。 (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 -z - 本紙張凡度適用中國國家禚準（CNS ) A4沈袼（2〗CX197公釐）
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US6746979B2 (en) 2004-06-08
CN1464924A (zh) 2003-12-31
DE60221132D1 (de) 2007-08-23
US20030219590A1 (en) 2003-11-27
KR101291200B1 (ko) 2014-11-04
DE60221132T2 (de) 2008-03-20
KR20100133510A (ko) 2010-12-21
ATE366835T1 (de) 2007-08-15
KR101078245B1 (ko) 2011-10-31
EP1411162B1 (en) 2007-07-11
CN1320189C (zh) 2007-06-06
KR20130065731A (ko) 2013-06-19
KR20040025655A (ko) 2004-03-24
WO2003010379A1 (fr) 2003-02-06
EP1411162A1 (en) 2004-04-21

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