WO2008138554A1 - Matière à filer pour la fabrication de fibres d'oxyde d'aluminium et de mullite - Google Patents

Matière à filer pour la fabrication de fibres d'oxyde d'aluminium et de mullite Download PDF

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Publication number
WO2008138554A1
WO2008138554A1 PCT/EP2008/003734 EP2008003734W WO2008138554A1 WO 2008138554 A1 WO2008138554 A1 WO 2008138554A1 EP 2008003734 W EP2008003734 W EP 2008003734W WO 2008138554 A1 WO2008138554 A1 WO 2008138554A1
Authority
WO
WIPO (PCT)
Prior art keywords
aluminum
fibers
dope
acid
spinning mass
Prior art date
Application number
PCT/EP2008/003734
Other languages
German (de)
English (en)
Inventor
Norbert Roesch
Original Assignee
Clariant Finance (Bvi) Limited
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Clariant Finance (Bvi) Limited filed Critical Clariant Finance (Bvi) Limited
Publication of WO2008138554A1 publication Critical patent/WO2008138554A1/fr

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Classifications

    • 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
    • C04B35/63448—Polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B35/63488—Polyethers, e.g. alkylphenol polyglycolether, polyethylene glycol [PEG], polyethylene oxide [PEO]
    • 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
    • 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
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
    • 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
    • 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
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
    • C04B2235/483—Si-containing organic compounds, e.g. silicone resins, (poly)silanes, (poly)siloxanes or (poly)silazanes

Definitions

  • the present invention relates to the use of modified aminosilanes for the production of oxide-ceramic fibers.
  • Ceramic fibers have been produced for many years and used in various fields. They are characterized by high chemical resistance, high thermal stability and remarkable mechanical properties. While short fibers have gained tremendous importance in high-temperature insulation as a substitute for asbestos, the available filament fibers are niche products which, due to the high price, are only used to a limited extent for special applications.
  • the ceramic fibers based on alumina and alumina / silica are used in furnace construction, in the aerospace and automotive industries.
  • water-soluble polymers such as polyethylene oxide or polyvinyl alcohol added.
  • Silica used in crystal growth or the silica content in alumina-silica mixed fibers (mullite) is usually added in the form of colloidal silica.
  • This method has the decisive disadvantage that in the aluminum salt solutions nano-particles are introduced from silica, which usually does not succeed homogeneous.
  • domains can form, which adversely affect the mechanical properties of the oxide fibers.
  • the invention therefore relates to a spinning composition for the production of aluminum oxide and mullite fibers, which contains an aluminum percursor and optionally a polymer and further auxiliaries, wherein these
  • Suitable silanes in this case are preferably the following types: Compounds of the formulas
  • R- .NH 2 , -NH-CH 2 -CH 2 -NH 2 , -N- (CH 2 -CH 2 -NH 2 ) 2 -NH-COO-CH 3 , -NH-COO-CH 2 -CH 3 , -NH- (CH 2 ) 3 Si (OR) 3
  • aminosilanes includes not only those compounds bearing primary, secondary or tertiary amino groups, but also those compounds containing nitrogen atoms in carbonamido structures.
  • aminosilicone oils from Wacker, Dow Corning, Bayer, Rhodia, etc. are used, which carry randomly distributed (cyclo) -alkylamino groups on their polymer chain on the polysiloxane chain.
  • Preferred silanes are the following silanes:
  • silanes are reacted with acids with the preferred molar ratio of silane to acid being 1: 1.
  • acids inorganic and organic acids can be used. Preference is given to using short-chain inorganic acids such as formic acid or acetic acid.
  • the reaction is carried out by simply mixing the two components. In an exothermic reaction then forms the acid-modified aminosilane.
  • acid-modified aminosilanes are then mixed with the aqueous solution of the aluminum precursors, which are usually used as starting material for the production of ceramic fibers based on Al 2 O 3 . Stirrers or dissolvers may be used to prepare the mixture. The use of ultrasound is also possible. Since the modified aminosilane decomposes to SiO 2 in the final calcination in the process of producing the oxide fibers and as such remains in the fiber, the amount of added acid-modified aminosilane depends primarily on the desired level of SiO 2 in the finished fiber , In general, one will choose the amount of acid-modified aminosilane so that the finished fiber contains 0.1 to 30 wt% SiO 2 .
  • Suitable aluminum precursors are aluminum chlorides, aluminum sulphates, aluminum nitrates and the corresponding basic salts. Furthermore, aluminum alcoholates and aluminum salts of organic acids can be used. Particularly preferred is the aluminum chlorohydrate which has the formula Al 2 (OH) x Cl y, where x is a number from 2.5 to 5.5 and y is a number from 3.5 to 0.5 and the sum of x and y always 6. Preference is given to starting from 50% aqueous solutions, as they are commercially available.
  • a polymer to the aqueous mixture to adjust the rheology for bulk spinnability.
  • Suitable polymers include polyvinyl alcohols, polyethylene oxides, polyvinylpyrrolidones, polyvinyl butyrals and other water-soluble, organic polymers, it being possible for the polymer content to be in the range from 0.2 to 40% by weight (based on the oxide content of the mixture).
  • the spinning dope according to the invention is blown or expressed through nozzles, wherein the resulting green fibers are collected as short fiber. It is also possible to produce long fibers with the spinning composition according to the invention, in which case the thread is taken up and wound on bobbins.
  • the green fiber thus obtained is converted into the desired ceramic fiber in a subsequent calcination step. This happens at the characteristic for the formation of the desired crystal phase temperature.
  • the silica forms by decomposition of the modified aminosilane. Since a homogeneous salt mixture was assumed, the effect of homogeneously distributed silica is very efficient.
  • the long fibers according to the invention are particularly suitable for the production of ceramic fiber fabrics and as starting material for the production of ceramic matrix and metal matrix composite materials.
  • colloidal silica (Klebosol 30 CAL50) was used as the source of silica.
  • the direct comparison shows that the fibers obtained have improved flexibility, a reduced tendency to breakage and a smaller "shot” (droplets at the yarn end) when using the spinning composition according to the invention.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Ceramic Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Fibers (AREA)

Abstract

L'invention concerne une matière à filer pour la fabrication de fibres d'oxyde d'aluminium et de mullite. Cette matière à filer contient un aminosilane à modification acide en plus des progéniteurs d'AI2O3 habituels se présentant sous forme de sels d'aluminium, et éventuellement des polymères et autres additifs. L'aminosilane à modification acide entraîne une meilleure stabilité de phase des fibres céramique.
PCT/EP2008/003734 2007-05-15 2008-05-09 Matière à filer pour la fabrication de fibres d'oxyde d'aluminium et de mullite WO2008138554A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE200710022821 DE102007022821B4 (de) 2007-05-15 2007-05-15 Spinnmasse für die Herstellung von Aluminiumoxid- und Mullitfasern und Verfahren zu deren Herstellung
DE102007022821.1 2007-05-15

Publications (1)

Publication Number Publication Date
WO2008138554A1 true WO2008138554A1 (fr) 2008-11-20

Family

ID=39736846

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2008/003734 WO2008138554A1 (fr) 2007-05-15 2008-05-09 Matière à filer pour la fabrication de fibres d'oxyde d'aluminium et de mullite

Country Status (3)

Country Link
DE (1) DE102007022821B4 (fr)
TW (1) TW200912060A (fr)
WO (1) WO2008138554A1 (fr)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104073918A (zh) * 2014-07-01 2014-10-01 华东理工大学 一种低温条件下合成多晶莫来石纤维的方法
CN106048780A (zh) * 2016-05-24 2016-10-26 天津工业大学 一种氧化铝基连续纤维的制备方法
CN114455846A (zh) * 2022-01-19 2022-05-10 东华大学 一种具有垂直取向结构的多孔莫来石纳米纤维基絮片材料及其制备方法
CN115259845A (zh) * 2022-06-27 2022-11-01 东华大学 一种柔性连续莫来石长丝的制备方法

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2164861A1 (fr) * 1971-12-22 1973-08-03 Bayer Ag
US4954462A (en) * 1987-06-05 1990-09-04 Minnesota Mining And Manufacturing Company Microcrystalline alumina-based ceramic articles
WO2007009577A1 (fr) * 2005-07-16 2007-01-25 Clariant International Ltd Procede pour realiser un corindon colore de taille nanometrique

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3808015A (en) 1970-11-23 1974-04-30 Du Pont Alumina fiber
EP0206634A3 (fr) 1985-06-21 1987-08-19 Imperial Chemical Industries Plc Fibres inorganiques et leur procédé de fabrication
CA1317978C (fr) 1987-06-05 1993-05-18 Thomas E. Wood Articles de ceramique a base de microcristaux d'alumine
GB8727410D0 (en) 1987-11-23 1987-12-23 Ici Plc Inorganic oxide fibres

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2164861A1 (fr) * 1971-12-22 1973-08-03 Bayer Ag
US4954462A (en) * 1987-06-05 1990-09-04 Minnesota Mining And Manufacturing Company Microcrystalline alumina-based ceramic articles
WO2007009577A1 (fr) * 2005-07-16 2007-01-25 Clariant International Ltd Procede pour realiser un corindon colore de taille nanometrique

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104073918A (zh) * 2014-07-01 2014-10-01 华东理工大学 一种低温条件下合成多晶莫来石纤维的方法
CN106048780A (zh) * 2016-05-24 2016-10-26 天津工业大学 一种氧化铝基连续纤维的制备方法
CN114455846A (zh) * 2022-01-19 2022-05-10 东华大学 一种具有垂直取向结构的多孔莫来石纳米纤维基絮片材料及其制备方法
CN114455846B (zh) * 2022-01-19 2024-01-23 东华大学 一种具有垂直取向结构的多孔莫来石纳米纤维基絮片材料及其制备方法
CN115259845A (zh) * 2022-06-27 2022-11-01 东华大学 一种柔性连续莫来石长丝的制备方法

Also Published As

Publication number Publication date
DE102007022821A1 (de) 2008-11-20
TW200912060A (en) 2009-03-16
DE102007022821B4 (de) 2013-02-28

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