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US4101615A Expired / Lapsed US ⏱️ 0.0 years remaining

Process for producing alumina fiber or alumina-silica fiber

Assignee: Sumitomo Chemical Co Ltd
•
Filing: 1975-08-20
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Granted: 1978-07-18
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Expires: 1995-08-20
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Abstract

Abstract A process for producing alumina fiber or alumina-silica fiber having excellent mechanical strength and heat resistance, comprising (i) spinning a solution of at least one polyaluminoxane or of a mixture of at least one polyaluminoxane and one or more kinds of silicon-containing compounds in an organic solvent, (ii) hydrolyzing the resulting precursor fiber, and then (iii) calcining the hydrolyzed fiber, said polyaluminoxane being one or more kinds of polymers or copolymers which mainly consist of the structural units of the formula: ##STR1## wherein the pendant groups Y are one or more kinds of groups selected from the group consisting of an alkyl, an alkoxy, an acyloxy, phenyl and phenoxy, and which may be partially a halogen or hydroxy.

Inventors

  • 👤 Shozo Horikiri
  • 👤 Kozo Tsuji
  • 👤 Yasuaki Abe
  • 👤 Akio Fukui
  • 👤 Eiichi Ichiki

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-24 05:34
CPC Classifications
C; C01; C01F; C01F7/00; C01F7/02; C01F7/30; C04; C04B; C04B35/00; C04B35/622; C04B35/62227; C04B35/62231; C04B35/62236; C04B35/6224; C04B35/62245; C01P; C01P2004/00; C01P2004/10; C01P2006/00; C01P2006/60; C01P2006/90; Y; Y10; Y10S; Y10S264/00; Y10S264/19

Claims Analysis

Total Claims: 19
Claim 1
Independent Claim 301 words
A process for producing alumina fiber or alumina-silica fiber, which consists essentially of (i) spinning a solution of at least one polyaluminoxane or of a mixture of at least one polyaluminoxane and one or more kinds of silicon-containing compounds in an organic solvent to give a precursor fiber, (ii) hydrolyzing the resulting precursor fiber, and then (iii) calcining the hydrolyzed fiber, said polyaluminoxane being one or more kinds of polymers or copolymers which mainly consist of the structural units of the formula: ##STR11## wherein the pendant members Y are one or more kinds of groups selected from the group consisting of alkyl having 1 to 18 carbon atoms, alkoxy having 1 to 18 carbon atoms, acyloxy having 1 to 18 carbon atoms phenyl and phenoxy, and may be partially a halogen or hydroxy, and which may also contain cross-linkages of the formula: ##STR12## the amount of which in the polymer molecule is within the range that the polymer is soluble in the organic solvent, and said pendant groups Y of the polyaluminoxane satisfying the conditions: f(HCOO) + f(CH.sub.3 COO) + f(F) + f(Cl) + f(Br) + f(I) + f(OH) ≦ 0.2 wherein f(R) means the mole fraction for a particular group: R as defined for the pendant group Y, or ##EQU3## being in the range of from 0.0 to 1.0, and .sub.n=1 (n-1)f(C.sub.n H.sub.2n+1) + .sub.n=1 nf(C.sub.n H.sub.2n+1 O) + .sub.n=3 (n+1)f(C.sub.n-1 H.sub.2n-1 COO) + 4.5 f(phenyl) + 5.5f(phenoxy)≦8 wherein n is an integer, and further the average degree of polymerization of the polyaluminoxanes being in the range of 5 to 1,000, and the amount of the silicon-containing compounds to be mixed into the solution being not greater than an amount such that the silica content in the alumina-silica fiber obtained after the calcination is not greater than 60% by weight.
Claim 2
Dependent Claim 301 words
A process for producing alumina fiber or alumina-silica fiber, which consists essentially of (i) spinning a solution of at least one polyaluminoxane or of a mixture of at least one polyaluminoxane and one or more kinds of silicon-containing compounds in an organic solvent to give a precursor fiber, (ii) hydrolyzing the resulting precursor fiber, and then (iii) calcining the hydrolyzed fiber, said polyaluminoxane being one or more kinds of polymers or copolymers which mainly consist of the structural units of the formula: ##STR11## wherein the pendant members Y are one or more kinds of groups selected from the group consisting of alkyl having 1 to 18 carbon atoms, alkoxy having 1 to 18 carbon atoms, acyloxy having 1 to 18 carbon atoms phenyl and phenoxy, and may be partially a halogen or hydroxy, and which may also contain cross-linkages of the formula: ##STR12## the amount of which in the polymer molecule is within the range that the polymer is soluble in the organic solvent, and said pendant groups Y of the polyaluminoxane satisfying the conditions: f(HCOO) + f(CH.sub.3 COO) + f(F) + f(Cl) + f(Br) + f(I) + f(OH) ≦ 0.2 wherein f(R) means the mole fraction for a particular group: R as defined for the pendant group Y, or ##EQU3## being in the range of from 0.0 to 1.0, and .sub.n=1 (n-1)f(C.sub.n H.sub.2n+1) + .sub.n=1 nf(C.sub.n H.sub.2n+1 O) + .sub.n=3 (n+1)f(C.sub.n-1 H.sub.2n-1 COO) + 4.5 f(phenyl) + 5.5f(phenoxy)≦8 wherein n is an integer, and further the average degree of polymerization of the polyaluminoxanes being in the range of 5 to 1,000, and the amount of the silicon-containing compounds to be mixed into the solution being not greater than an amount such that the silica content in the alumina-silica fiber obtained after the calcination is not greater than 60% by weight.
Claim 3
Dependent Claim 40 words
The process according to claim 1, wherein the polyaluminoxane or the mixture of polyaluminoxane and silicon-containing compounds is hydrolyzed while it is formed into fibrous form during said spinning step, instead of hydrolyzing it after being formed into fibrous form.
Claim 4
Dependent Claim 33 words
The process according to claim 1, wherein the precursor fiber which has not been hydrolyzed is hydrolyzed by humid air during the calcination step, instead of hydrolyzing the precursor fiber before the calcination.
Claim 5
Dependent Claim 85 words
The process according to claim 1, wherein the solution of polyaluminoxane or of a mixture of polyaluminoxane and silicon-containing compounds further contains at least one compound containing an element selected from the group consisting of lithium, beryllium, boron, sodium, magnesium, phosphorus, potassium, calcium, titanium, chromium, manganese, yttrium, zirconium, barium, lanthanum and tungsten, said additional compounds being contained in such an amount that the total content of the elements in the alumina fiber or alumina-silica fiber obtained after the calcination is less than 10% by mol.
Claim 6
Dependent Claim 36 words
The process according to claim 1, wherein the organic solvent is a member selected from the group consisting of diethyl ether, ethyl n-propyl ether, ethyl isopropyl ether, tetrahydrofuran, dioxane, benzene, toluene, a xylene, and mixtures thereof.
Claim 7
Dependent Claim 82 words
The process according to claim 1, wherein the solution to be spun contains as the silicon-containing compound a polysiloxane having identical or different structural units of the general formula: ##STR13## wherein R 1 and R 2 are, each independently, a hydrogen atom excluding R 1 ═R 2 ═H, an alkyl group having from 1 to 6 carbon atoms, an alkenyl group having from 2 to 6 carbon atoms, an alkoxy group having from 1 to 6 carbon atoms, or a phenyl group.
Claim 8
Dependent Claim 72 words
The process according to claim 1, wherein the solution to be spun contains as the silicon-containing compound a polysilicic acid or a polysilicic acid ester having identical or different structural units of the general formula: ##STR14## wherein R 3 and R 4 are, each independently, a hydrogen atom, an alkyl group having from 1 to 6 carbon atoms, an alkenyl group having from 2 to 6 carbon atoms, or a phenyl group.
Claim 9
Dependent Claim 77 words
The process according to claim 1, wherein the solution to be spun contains as the silicon-containing compound silane derivatives, excluding SiH 4 , of the general formula: R.sub.n.sup.5 SI(OR.sup.6).sub.4-n wherein R 5 and R 6 are, independently, a hydrogen atom, an alkyl group having from 1 to 6 carbon atoms, an alkenyl group having from 2 to 6 carbon atoms, a phenyl group or a chlorine atom, and n is an integer of from 1 to 4.
Claim 10
Dependent Claim 51 words
The process according to claim 1, wherein the solution to be spun contains as the silicon-containing compound a silicic acid or a silicic acid ester of the general formula: Si(OR.sup.7).sub.4 wherein R 7 is a hydrogen atom, an alkyl group having from 1 to 6 carbon atoms or a phenyl group.
Claim 11
Dependent Claim 33 words
The process according to claim 1, wherein the solution to be spun contains as the silicon-containing compound an ethyl silicate of the formula: ##STR15## wherein n is an integer of 1 or more.
Claim 12
Dependent Claim 24 words
The process according to claim 1, wherein the solution to be spun has a viscosity of from 1 to 5,000 poise at room temperature.
Claim 13
Dependent Claim 22 words
The process according to claim 1, wherein the diameter of the precursor fiber is in the range of 1 to 300 microns.
Claim 14
Dependent Claim 24 words
The process according to claim 1, wherein the average degree of polymerization of the polyaluminoxane is in the range of from 10 to 200.
Claim 15
Dependent Claim 52 words
The process according to claim 1, wherein the fiber formed from the polyaluminoxane or the mixture of polyaluminoxane and silicon-containing compounds is hydrolyzed by contacting it having a humid air at 50° to 90° C with relative humidity of 50 to 100% for 5 to 300 minutes or with an acidic solution.
Claim 16
Dependent Claim 21 words
The process according to claim 1, wherein the precursor fiber is calcined at a temperature of from 600° to 1700° C.
Claim 17
Dependent Claim 19 words
The process according to claim 1, wherein the calcination is carried out in an atmosphere containing molecular oxygen gas.
Claim 18
Dependent Claim 18 words
The process according to claim 1, wherein the calcination is carried out while the fiber is under tension.
Claim 19
Dependent Claim 16 words
The process of claim 1, wherein the precursor fiber is a non-crystalline, amorphous, dense, non-porous material.

References Cited (Backward Citations)

US2915475A Cited
US2944914A Cited
US3031418A Cited
US3231540A Cited
US3634112A Cited
US3846527A Cited
US3992498A Cited
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USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1981-07-17 1982-01-16 1982-07-18 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1985-07-17 1986-01-16 1986-07-18 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1989-07-17 1990-01-16 1990-07-18 $7700.00 Window Closed / Lapsed

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