CN101336322B - Ceramic oxide fibers - Google Patents

Ceramic oxide fibers Download PDF

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Publication number
CN101336322B
CN101336322B CN2006800522448A CN200680052244A CN101336322B CN 101336322 B CN101336322 B CN 101336322B CN 2006800522448 A CN2006800522448 A CN 2006800522448A CN 200680052244 A CN200680052244 A CN 200680052244A CN 101336322 B CN101336322 B CN 101336322B
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gram
fiber
tow
slurry
ceramic oxide
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CN101336322A (en
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拉里·R·维瑟
理查德·M·弗林
卡罗-琳恩·斯帕
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3M Innovative Properties Co
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3M Innovative Properties Co
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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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
    • 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
    • C04B35/62844—Coating fibres
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/39—Aldehyde resins; Ketone resins; Polyacetals
    • D06M15/423—Amino-aldehyde resins
    • D06M15/427—Amino-aldehyde resins modified by alkoxylated compounds or alkylene oxides
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
    • C03C25/10—Coating
    • C03C25/24—Coatings containing organic materials
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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
    • 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
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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
    • 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]
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    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/4584—Coating or impregnating of particulate or fibrous ceramic material
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
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    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
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    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
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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
    • C04B2235/5216—Inorganic
    • C04B2235/522—Oxidic
    • C04B2235/5224—Alumina or aluminates
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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
    • C04B2235/5216—Inorganic
    • C04B2235/522—Oxidic
    • C04B2235/5228—Silica and alumina, including aluminosilicates, e.g. mullite
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    • 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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    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • 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
    • Y10T428/2933—Coated or with bond, impregnation or core

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  • Inorganic Fibers (AREA)
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Abstract

Tow of substantially continuous ceramic oxide fibers having a sizing material. Tows according to the present invention are useful, for example, for making metal matrix wires.

Description

Ceramic oxide fibers
Technical field
The present invention relates to ceramic oxide fibers, more particularly, relate to the ceramic oxide fibers of being with slurry.
Background technology
In general, continuous basically ceramic oxide fibers is known.Example comprises polycrystalline alumina fiber, for example those that sold with trade name " NEXTEL 610 " by 3M company (Sao Paulo, the Minnesota State); Aluminosilicate fiber, for example those that sell with trade name " NEXTEL 440 ", " NEXTEL 550 " and " NEXTEL 720 " by 3M company; And aluminoborosilicate fiber, for example those that sell with trade name " NEXTEL 312 " by 3M company.These continuous fiberss are compounded in various metal-matrix composites (as aluminium and titanium) and the polymer matrix composites (as epoxy resin), to reinforce and to strengthen these composites.
Wish to keep the intensity of composite.The intensity of composite is because of having continuous fibers and the least possible interruption is improved.A root of being interrupted is commonly referred to " shelling back " from when continuous fibers unwinding and fibrous fracture or come off from the bobbin.Wish to remove, reduce as far as possible or reduce at least these interruptions that produce in the unwinding process, thus the metal and the polymer matrix composites that allow production intensity to increase.
Summary of the invention
In one aspect, the invention provides continuous basically fire-resistant (promptly, in 820 ℃ to 1400 ℃ temperature range, keep its integrality or serviceability) the ceramic oxide fibers tow, wherein every kind of ceramic oxide fibers has outer surface, and wherein has slurry at least a portion outer surface of at least some ceramic oxide fibers.Slurry comprises the composition by following chemical formulation:
R’O-(RO) n-H，
Wherein R ' is selected from C xH 2x+1, wherein x be 1-8 or-H; R is selected from by-(C yH 2y)-(can be straight or branched) (wherein y is 1-4) and-CH 2-O-(CH 2) mThe group that-(wherein m=2-5) forms; And wherein select n so that number-average molecular weight is in 500 gram/moles to 7,000, in the scope of 000 gram/mole.Usually, number-average molecular weight is in 500 gram/moles to 3, (in certain embodiments, be in 500 gram/moles in the scope of 000,000 gram/mole to 600,000 gram/mole, 500 gram/moles are to 400,000 gram/mole, 500 gram/moles are to 300,000 gram/moles, perhaps even 4,000 gram/mole is to the scope of 40,000 gram/moles).Usually slurry provides the impost in 0.5 weight % to the 10 weight % scope.
" continuous fibers " is meant at least 30 meters long fiber.In certain embodiments, refractory fibre is crystal (that is, showing to have recognizable X-powder diffraction pattern).In certain embodiments, fiber is the crystal that is at least 50 (in certain embodiments, at least 55,60,65,70,75,80,85,90,95,96,97,98,99 or even 100) weight %.In certain embodiments, refractory oxide fibre (comprising the crystalline ceramic oxide fibre) comprises at least one in following two: (a) based on the total oxide content of every fiber, the Al of at least 40 (in certain embodiments, at least 50,60,65,70,75,80,85,90,95,96,97,98,99 or even 100) weight % 2O 3, perhaps (b) is no more than the SiO of 40 (in certain embodiments, being no more than 35,30,25,20,15,10,5,4,3,2,1,0,5,0,1 or even 0) weight % altogether based on the total oxide content of every fiber 2, Bi 2O 3, B 2O 3, P 2O 5, GeO 2, TeO 2, As 2O 3And V 2O 5
Through observing, slurry provides lubricity, and protects the fiber strand during operation.For some purposes of fiber, for example, as the reinforcing in the metal-matrix composite, slurry is removed in the process before metal is applied to fiber usually.Slurry can (for example) make it to remove from the fiber disengaging by scorching hot slurry.
The specific embodiment
The example of the refractory oxide fibre that is suitable for comprises alumina fibre, aluminosilicate fiber, aluminium borate fiber, aluminoborosilicate fiber, zirconia-silicon dioxide fibre and their combination.The example of the crystal refractory oxide fibre that is suitable for comprises alumina fibre, aluminosilicate fiber, aluminium borate fiber, aluminoborosilicate fiber, zirconia-silicon dioxide fibre and their combination.The example of the noncrystal refractory oxide fibre that is suitable for comprises aluminoborosilicate fiber, zirconia-silicon dioxide fibre and their combination.In certain embodiments, the expectation fiber comprises the Al of at least 40 (in certain embodiments, at least 50,60,65,70,75,80,85,90,95,96,97,98,99 or even 100) volume % 2O 3(based on the cumulative volume of fiber).In certain embodiments, the Al of expectation fiber (in certain embodiments, 55 to 70, perhaps even in 55 to 65 scopes) the volume % that comprises 40 to 70 2O 3(based on the cumulative volume of fiber).
The part crystal fibre can comprise the mixture of crystalline ceramic and amorphous phase (that is, fiber can not only comprise crystalline ceramic but also comprise amorphous phase).Usually, continuous ceramic fiber has the fiber diameter at least about 5 microns, more generally be, about 5 microns to about 20 microns scope; In certain embodiments, about 5 microns to about 15 microns scope.
Alumina fibre is described in (for example) U.S. Patent No. 4,954,462 (Wood people such as (Wood)) and 5,185,299 people such as () Woods to some extent.In certain embodiments, alumina fibre is a polycrystalline Alpha-alumina fiber, and comprises (according to theoretical oxide) Al greater than 99 weight % 2O 3SiO with 0.2-0.5 weight % 2(based on the gross weight of alumina fibre).On the other hand, the polycrystalline Alpha-alumina fiber of some expectations comprises the Alpha-alumina of particle mean size less than 1 micron (perhaps even in certain embodiments less than 0.5 micron).On the other hand, in certain embodiments, polycrystalline Alpha-alumina fiber has at least 1.6GPa (in certain embodiments, at least 2.1GPa, perhaps even at least average tensile strength 2.8GPa), as measured according to the test of TENSILE STRENGTH described in the U.S. Patent No. 6.460,597 (McCullough people such as (McCullough)).Exemplary Alpha-alumina fiber is sold with trade name " NEXTEL 610 " by 3M company (Sao Paulo, the Minnesota State).
Aluminosilicate fiber is described in (for example) U.S. Patent No. 4,047,965 (Karst people such as (Karst)) to some extent.Exemplary aluminosilicate fiber is sold with trade name " NEXTEL 440 ", " NEXTEL 550 " and " NEXTEL 720 " by 3M company (Sao Paulo, the Minnesota State).
Aluminium borate fiber and aluminoborosilicate fiber are described in (for example) U.S. Patent No. 3,795,524 (Suo Man (Sowman)) to some extent.Exemplary aluminoborosilicate fiber is sold with trade name " NEXTEL 312 " by 3M company.
Zirconia-silicon dioxide fibre is described in (for example) U.S. Patent No. 3,709,706 (Suo Man).
Tow is known in fiber art, and generally includes many (single) fiber of non-distortion (at least 100 fibers usually, more generally be at least 400 fibers) substantially.In certain embodiments, tow comprises at least 780 filaments of every tow, and in some cases, at least 2600 filaments of every tow, or at least 5200 filaments of every tow.The tow of various ceramic fibres has multiple length available, comprises 300 meters, 500 meters, 750 meters, 1000 meters, 1500 meters and longer.The shape of cross section of fiber can be circle, ellipse or dog bone shape.
Can be prepared by the method that may further comprise the steps according to tow of the present invention:
Basically continuous ceramic oxide fibers tow is provided, and wherein every ceramic oxide fibers has outer surface;
Be applied at least a portion outer surface of fewer ceramic oxide fibers with water-based slurry; And remove at least a portion water.Water-based slurry comprises the composition with following chemical formulation:
R’O-(RO) n-H，
Wherein R ' is selected from C xH 2x+1, wherein x be 1-8 or-H; R is selected from by-(C yH 2y)-(wherein y be 1-4) and-CH 2-O-(CH 2) mThe group that-(wherein m=2-5) forms; And wherein select n so that number-average molecular weight at 500 gram/moles to 7,000, in the scope of 000 gram/mole.Usually, number-average molecular weight at 500 gram/moles to 3,000,000 gram/mole (in certain embodiments, at 500 gram/moles to 600,000 gram/moles, 500 to 400,000 gram/mole, 500 gram/moles are to 300,000 gram/mole or even 4,000 gram/moles to 40,000 gram/moles) scope in.
The slurry that is suitable for comprises that poly-(tetramethylene oxide) (can (for example) (number-average molecular weight be 2 with trade name " TERATHANE 2900 ", 900 gram/moles) derive from (Invista of English Radar Audio Company (Kansas State Wichita), Wichita, KS)), (can (for example) (number-average molecular weight be 35 to polyethylene glycol with trade name " POLYGLYKOL 35000 ", 000 gram/mole), " POLYGLYKOL 20000 " (number-average molecular weight is 20,000 gram/mole), " POLYGLYKOL 4000S " (number-average molecular weight is 4000 gram/moles), " POLYGLYKOL 8000S " (number-average molecular weight is 8000 gram/moles), " POLYGLYKOL 1500S " (number-average molecular weight is 1500 gram/moles) derives from Ke Lairui benefactor's sigong energy Division of Chemistry (Frankfurt, Germany) (Clariant GmbH FunctionalChemicals Division, Frankfurt, Germany)) and the poly(ethylene oxide) material of high number-average molecular weight (can (for example) (number-average molecular weight be 400 with trade name " POLYOX WSR N-3000 ", 000 gram/mole), " POLYOX WSR N-750 " (number-average molecular weight is 300,000 gram/mole) and " POLYOX WSR-301 " (number-average molecular weight is 4,000,000 gram/mole) derives from (the Dow Chemical of Dow Chemical's (available), Midland, MI)).
Water-soluble paste (for example poly-(ethylene glycol)) can be dissolved in the water, so that water-based slurry to be provided.The concentration of water-soluble paste can be selected as required in the water-based slurry.Usually, this class water-based slurry is to make by water-soluble paste and water are combined, so that the water-based slurry that comprises 1% to 30% (by weight) water-soluble paste to be provided; In certain embodiments, comprise scope at 1% to 10% water-soluble paste.
When using water-fast material (for example poly-(tetramethylene oxide)), water-based slurry is emulsified.This class emulsion can prepare by using surfactant.Usually, the amount of surfactant that is used to prepare emulsion is in the scope of 0.5 weight % to 10 weight % of emulsified material, but the amount of surfactant beyond this scope also comes in handy.Usually, emulsion is in 5% to 50% scope of solid weight.If it is required that the percentage of solids of emulsion is higher than, can dilute by water.
Observe in the art, in general, slurry provides (a) enough intensity, so that the fiber in the tow is combined together to form internal bunching; (b) good lubricated/peel property, make fiber/tow can not cling equipment and thread-carrier, and have lubrication to reduce in the processing procedure friction and adhesion to the surface of contact tow; And (c) relatively low or moderate temperature (as, 700 ℃) on fiber, do not stayed down the residue ability of (as, the residue of carbon containing) by oxidation promptly.Last is especially desirable in metal matrix wire rod preparation technology's embodiment, wherein by under relatively low or moderate temperature, heating tow, be easy to usually the relatively short time (as, less than 30 seconds) in remove slurry.By just being sent into, oxidizing gas (as, air) promotes removing of slurry in the zone of oxidation slurry.Though the desired flow rate of oxidizing gas will depend on actual conditions (as, concrete slurry, amount of slurry, fiber speed, temperature, hot length etc.), exemplary flow velocity comprises about 5 liters of/minute flow velocitys to about 10 liters of/minute scopes.
In addition, the slurry that the present invention indicates can be applied on the fiber (as, the fiber in about 15 ℃-200 ℃ temperature range) effectively, is included in fiber and slurry is applied on it when leaving sintering furnace.
Tow according to the present invention can be used for (for example) preparation metal-matrix composite wire rod.Exemplary metal matrix material comprises aluminium, zinc, tin, magnesium and their alloy (as, the alloy of aluminium and copper).The technology of preparation metal-matrix composite wire rod is known in this area, and comprises those that (for example) discussed in following document: U.S. Patent No. 5,501,906 (Devi (Deve)), 6,180,232 (people such as McCullough), 6,245,425 (people such as McCullough), 6,336,495 (people such as McCullough), 6,544,645 (people such as McCullough), 6,447,927 (people such as McCullough), 6,460,597 (people such as McCullough), 6,329,056 (people such as Devi), 6,344,270 (people such as McCullough), 6,485,796 (Ka Pengte people such as (Carpenter)), 6,559,385 (Johnson people such as (Johnson)), 6,796,365 (people such as McCullough), 6,723,451 (people such as McCullough) and 6,692,842 (people such as McCullough) and 6,913,838 (people such as McCullough); Sequence number is 10/403,643 U.S. Patent application (being filed on March 31st, 2003), U.S. Patent Publication No.2005-0178000-A1 (being filed on February 13rd, 2004), U.S. Patent Publication No.2005-0181228-A1 (being filed on February 13rd, 2004), U.S. Patent Publication No.2005-0279526-A1 (being filed on June 17th, 2004), U.S. Patent Publication No.2005-0279527-A1 (being filed on June 17th, 2004) and U.S. Patent No. 7,093,416.
Through observing, that the embodiment of the metal-matrix composite wire rod of being made by last pulp fibres according to the present invention compares with the metal-matrix composite wire rod of being made by the fiber that does not comprise slurry therewith among the present invention (comprising the fiber with other slurry sizing) is more firm (as, about 2-8%).
Following example further illustrates advantage of the present invention and embodiment, but concrete material of being mentioned in these examples and quantity thereof and other condition and details all should not be interpreted as improper restriction of the present invention.Except as otherwise noted, otherwise all shares and percentage all by weight.
Example
Example 1
(number-average molecular weight is 2900 gram/moles with solid-state poly-(tetramethylene oxide) of 52.2kg (115lbs.); Can trade name " TERATHANE 2900 " derive from English Radar Audio Company (Kansas State Wichita)) be placed on to spend the night in the baking oven that is heated to 60 ℃ (140) and make its fusion.The enamel water leg receiver of being furnished with agitator of 284 liters (75 gallons) is risen to 60 ℃ (140 °F).Agitator is set to 80rpm, and pack into poly-(tetramethylene oxide) (" TERATHANE 2900 ") of described fusing of reactor.Then, the ethyl acetate of 52.2kg (115lbs.) (is derived from (Sigma-Aldrich of Sigma aldrich company (Milwaukee, the state of Wisconsin), Milwaukee, WI)) add reactor, octadecyl methyl (polyoxyethylene [the 15]) ammonium chloride that adds 8.7kg (19.1lbs.) again (can trade name " ETHOQUAD 18/25 " derive from (AkzoNobel of Akzo Nobel N.V. (Chicago, Illinois State), Chicago, IL)).
The enamel water leg reactor of being furnished with agitator (80rpm) of second 284 liters (75 gallons) is risen to 60 ℃ (140 °F).The deionized water of 114kg (253lbs.) (derives from (the C.C.Day Co. of C.C.Day company (Minnesota State Minneapolis) by 0.2 micron filter, Minneapolis, MN), dash number is 25-10110-002-01-WG) filter, join in the reactor then.Agitator speed is increased to 100rpm.When the temperature of reactor and receiver all is 60 ℃ (140 °F), increase the nitrogen pressure on the receiver, make inclusions flow into second reactor from first reactor.
(model is 70-M-310-TBS with the secondary homogenizer; Derive from Man Tonggaolin manufacturing company (Massachusetts Ai Fuleite) (Manton-Gaulin Manufacturing Co., Everett, MA); Use deionized water rinsing) the water inlet joint be connected to and have pipeline and 0.2 micron filter (derives from C.C.Day company; Dash number is 25-10110-002-01-WG) homogenizer inlet.25 microns filter cylinders (are derived from C.C.Day company; Dash number is SWF-25-RYA10T) be connected between the inlet attack of the outlet of reactor and homogenizer.The operation pressure of homogenizer is set to 20.7MPa (3000 pounds/square inch), and extracts mixture down out at 20.7MPa (3000 pounds/square inch).When the output of homogenizer when not containing the blue white emulsion of solid, output is imported 208 liters (55 gallons) has in the tube of polyethylene liner.
Blue white emulsion passes through homogenizer for the second time, and once more output importing 208 liters (55 gallons) is had in the tube of polyethylene liner.First reactor is furnished with the condensate decanter, with indigo plant white emulsion pack into and wash and clear up with deionized water before (cleaning) reactor.Agitator speed is risen to 60rpm, and jacket temperature is set to 38 ℃ (100 °F).Then, off-response device and on inclusions, form vacuum (8kPa (60mmHg)).When the ethyl acetate distillate accumulates in the decanter, vacuum is increased at leisure (5.3kPa (40mmHg) is to reduce too much foam as far as possible.When having collected the ethyl acetate of 45.4kg (100lbs.), stop distillation, with reactor cooled to 21 ℃ (70 °F), and allow the emulsion of gained (derive from C.C.Day company from a tube filter of 25 microns; Dash number is SWF-25-RYA10T) discharge, flow in 19 liters of (5 gallons) polyethylene-lined buckets and capping.
According to the following step, use the coating station that the emulsion of gained is applied to Alpha-alumina fibre bundle (10,000 denier is sold with trade name " NEXTEL CERAMIC OXIDE FIBER 610 " * (NEXTEL ceramic oxide fibers 610) by 3M company (Sao Paulo, the Minnesota State)).With deionized water above-mentioned " TERATHANE 2900 " emulsion is diluted to 5% " TERATHANE 2900 " emulsion, and it is positioned in the starching dish of coating station.Sizing roller obtains emulsion by being immersed in the coating dish.By speed tow is applied to slurry on the every fibre bundle through sizing roller with 34.7 meters/minute (114 inch per minute clocks).The speed of starching application roll is set to 1.5% the clean coating weight of starching can be provided.Applied fibre bundle around drying chamber (be heated to 100 ℃, diameter and be 15cm (6 inches) be coated with chromium steel roller) ten secondaries, is wound on the cardboard cylinder again.
The amount of slurry that is applied on the fibre bundle is measured by the following method: (3 feet) starching tow (w that weighing is a meter Initially), again this tow is positioned in 700 ℃ the heating furnace and continues 5 minutes, remove the sample in the heating furnace, make it to be cooled to room temperature, then weighing sample (w again Finally).Slurry weight % (the S that is applied w) adopt following formula to calculate:
Figure S2006800522448D00091
The impost of dry finish is about 2 weight %.Burn from fiber fully through the range estimation slurry.
Example 2
Glass jar with 2858 gram deionized water fillings 4 liters (1 gallons).The overhead type mixer that to be furnished with Cauer (Cowl) wing mixer inserts in the glass jar, rotating speed is risen to 500rpm, and (number-average molecular weight is 300 slowly to add the polyethylene glycol of (about more than 30 minutes) 150 grams in the vortex that the Cauer blade produces, 000 gram/mole, " POLYOXWSR N-750 " derives from Dow Chemical's (available) with trade name).The gained mixture is placed on the platform-type shake table (, continues about 60 hours with trade name " INNOVA 2000 " the Boulogne Zi Weike scientific company (New Jersey Edison) (New Brunswick Scientific Co.Inc., Edison, NJ)) of must making a fresh start.
As described in example 1, with the gained solution coat on the alumina fibre tow.The impost of dry finish is about 1 weight %.Evaporate from fiber fully through the range estimation slurry.
Example 3
As preparation example 3 as described in the example 2, different is that (number-average molecular weight is 1500 gram/moles with 3 gram polyethylene glycol before polyethylene glycol; Derive from Sigma aldrich company (Milwaukee, the state of Wisconsin) with trade name " PEG 1500 ") join in the deionized water.
Described in example 1, with the gained solution coat on the alumina fibre tow.The impost of dry finish is about 1.5 weight %.Burn from fiber fully through the range estimation slurry.
Example 4
As preparation example 4 as described in the example 2, different is that (number-average molecular weight is 20,000 gram/moles with 150 gram polyethylene glycol; Derive from Sigma aldrich company with trade name " PEG 20,000 ") alternative polyethylene glycol.The gained material is a clear solution.
As described in example 1, with the gained solution coat on the alumina fibre tow.The impost of dry finish is about 1 weight %.Burn from fiber fully through the range estimation slurry.
Example 5
Glass jar with 2850 gram deionized water fillings 3.8 liters (1 gallons).The overhead type mixer that to be furnished with Cauer (Cowl) wing mixer inserts in the glass jar, rotating speed is risen to 500rpm, and (number-average molecular weight is 35 slowly to add the polyethylene glycol of (about more than 10 minutes) 150 grams in the vortex that the Cauer blade produces, 000 gram/mole, derive from (the Clariant Corporation of Ke Lairui benefactor department (North Carolina State Meng Heli) with trade name " POLYGLYKOL 35000 ", Mount Holly, NC)).The gained material is transparent colourless solution.
As described in example 1, dilute gained solution, and it is applied on the alumina fibre tow.The impost of dry finish is about 1 weight %.Burn from fiber fully through the range estimation slurry.
Example 6
Load 6 liters of stainless steel beakers with 2970 gram deionized waters, and (model is #ME100L, derives from (the Charles Ross﹠amp of Luo Si company (New York Hauppauge) with trade name " ROSS MIXER EMULSIFIER " (Luo Si Mixingemulsificationmachine) with mixer; Son Co.Hauppauge, NY)) insert in the beaker.The rotating speed of mixer is risen to 5000rpm, and 30 gram polyethylene glycol (number-average molecular weight is 4,000,000 gram/mole, and " POLYOX WSR-301 " derives from Dow Chemical with trade name) are slowly added in (about more than 15 minutes) water.The gained mixture is placed on shake table (referring to example 2; Under 125rpm) on, continue 12 hours.
Described in example 1, with the gained solution coat on the alumina fibre tow.The impost of dry finish is about 1.5 weight %.Burn from fiber fully through the range estimation slurry.
Example 7
With 6 liters of stainless steel beakers of 2985 gram deionized water fillings.The overhead type mixer that to be furnished with Cauer (Cowl) wing mixer inserts in the glass jar, and rotating speed is risen to 500rpm, and (number-average molecular weight is 7,000,000 gram/mole with 15 gram polyethylene glycol; " POLYOX WSR-303 " derives from Dow Chemical with trade name) slowly add in (about more than 30 minutes) water.The gained mixture is placed on shake table (referring to example 2; Under 125rpm) on, continue 12 hours.
As described in example 1, with the gained solution coat on the alumina fibre tow.The impost of dry finish is about 2 weight %.Burn from fiber fully through the range estimation slurry.
Example 8
With 6 liters of stainless steel beakers of 2850 gram deionized water fillings, and will be furnished with in mixer (" ROSS MIXER EMULSIFIER ") the insertion beaker of Luo Si (Ross) sieve head.The mixer rotating speed is risen to 5000rpm, and heat water to about 60 ℃, again 30 gram polyethylene glycol (" POLYOX WSR N-750 ") are slowly added in (about more than 15 minutes) water.The gained mixture is placed on conventional roller table (about 40rpm) went up lasting 12 hours, thereby obtain turbid solution.
As described in example 1, with the gained solution coat on the alumina fibre tow.The impost of dry finish is about 1.3 weight %.Burn from fiber fully through the range estimation slurry.
Example 9
With 6 liters of stainless steel beakers of 2850 gram deionized water fillings, and will be furnished with in mixer (" ROSS MIXER EMULSIFIER ") the insertion beaker of Luo Si disperser blade.The rotating speed of mixer is risen to 5000rpm, and 150 gram polyethylene glycol (number-average molecular weight is 400,000, and " POLYOX WSR N-3000 " derives from Dow Chemical with trade name) are slowly added in (about more than 30 minutes) water.Can obtain clear solution like this.
As described in example 1, with the gained solution coat on the alumina fibre tow.The impost of dry finish is about 1.5 weight %.Burn from fiber fully through the range estimation slurry.
Example 10
As preparation example 10 as described in the example 3, different is that (number-average molecular weight is 4000 gram/moles with polyethylene glycol; " POLYGLYKOL 4000S " derives from Ke Lairui benefactor department with trade name) rather than " PEG 1500 " polyethylene glycol add in the deionized water.
As described in example 1, with the gained solution coat on the alumina fibre tow.The impost of dry finish is about 1.3 weight %.Burn from fiber fully through the range estimation slurry.
Example 11
As preparation example 11 as described in the example 10, different is that (number-average molecular weight is 8000 gram/moles with polyethylene glycol; " POLYGLYKOL 8000S " derives from Ke Lairui benefactor department with trade name) rather than " POLYGLYKOL 4000S " polyethylene glycol add in the deionized water.
As described in example 1, with the gained solution coat on the alumina fibre tow.The impost of dry finish is about 2 weight %.Burn from fiber fully through the range estimation slurry.
Example 12
As method as described in the example 2, preparation example 12, different is with in 147 grams " POLYOXWSR N-750 " and 3.02 grams " PEG-1500 " rather than 150 gram " POLYOX WSRN-750 " polyethylene glycol adding deionized waters.The impost of dry finish is about 1.2 weight %.Burn from fiber fully through the range estimation slurry.
The of the present invention various modifications and the change that do not break away from protection scope of the present invention and spirit will become apparent those skilled in the art, and be to be understood that the present invention locality of having to is limited in the exemplary embodiment that this paper proposes.

Claims (8)

1. the tow of a continuous basically ceramic oxide fibers, wherein every ceramic oxide fibers has outer surface, wherein have slurry on the described outer surface of at least a portion of at least some described ceramic oxide fibers, and wherein said slurry comprises the composition by following chemical formulation:
R’O-(RO) n-H，
Wherein:
R ' is selected from C xH 2x+1Or-H, wherein x is 1-8;
R is selected from by-(C yH 2y)-and-CH 2-O-(CH 2) mThe group of-composition, wherein y is 1-4, m=2-5; And
Select n so that number-average molecular weight is in 500 gram/moles to 7,000, in the scope of 000 gram/mole.
2. tow according to claim 1, wherein said continuous basically ceramic oxide fibers is a crystal.
3. tow according to claim 1, the continuous basically ceramic oxide fibers of wherein said tow is selected from the group of being made up of crystal alumina fibre, crystalline silica-aluminate fiber, crystal aluminoborosilicate fiber and their combination.
4. tow according to claim 1 is wherein selected n so that number-average molecular weight is in 500 gram/moles to 3,000, in the scope of 000 gram/mole.
5. tow according to claim 1 is wherein selected n so that number-average molecular weight is in 500 gram/moles to the scope of 400,000 gram/moles.
6. method that continuous basically ceramic oxide fibers tow according to claim 1 is provided, described method comprises:
Basically continuous ceramic oxide fibers tow is provided, and wherein every ceramic oxide fibers has outer surface;
Be applied to the described outer surface of at least a portion that lacks some ceramic oxide fibers with water-based slurry, wherein said slurry comprises the composition by following chemical formulation:
R 1’O-(R 1O)n 1-H，
Wherein:
R 1' be selected from Cx 1H2x 1+ 1 or-H, wherein x 1Be 1-8;
R 1Be selected from by-(Cy 1H2y 1)-and-CH 2-O-(CH 2) m 1The group of-composition, wherein y 1Be 1-4, m 1=2-5; And wherein select n 1So that number-average molecular weight at 500 gram/moles to 7,000, in the scope of 000 gram/mole; And
Remove at least a portion water.
7. method according to claim 6, wherein said water-based slurry are solution.
8. method according to claim 6, wherein said water-based slurry are emulsion.
CN2006800522448A 2005-12-30 2006-12-28 Ceramic oxide fibers Expired - Fee Related CN101336322B (en)

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