← Back to Patent Explorer
US3709833A Expired / Lapsed US ⏱️ 0.0 years remaining

Process for preparing high purity silicon oxide porous beads doped with small quantities of other oxides

Assignee: OI Glass Inc
•
Filing: 1970-08-21
•
Granted: 1973-01-09
•
Expires: 1990-08-21
📄 Original PDF 🌐 Google Patents 🔄 Sync Now

Abstract

Abstract There is disclosed the preparation of high purity, high surface area, porous beads of silicon oxide doped with small quantities of other oxides, which preparation comprises hydrolyzing a silicon alkoxide dissolved in a hydroxyl containing organic solvent with less than a stoichiometric amount of water so as to provide a partially hydrolyzed intermediate product. The resulting partially hydrolyzed intermediate product is then treated with additional water and an immiscible non-polar organic medium so as to form a discontinuous phase of liquid partially hydrolyzed intermediate product dispersed in a continuous phase of organic medium. As a source of dopant oxide, a selected water soluble salt is added to the process at any convenient step prior to the next process step of pH adjustment, e.g. before, during, or after the partially hydrolyzing; before, during, or after the organic medium treatment. The dispersed intermediate product is then treated with a base and a quantity of water sufficient to hydrolyze any residual alkoxy groups in the dispersed intermediate product. The resulting mixture is stirred until the dispersed intermediate is converted to firm, hard, solid, porous beads of silicon oxide doped with at least one other oxide. The beads are typically recovered by filtration and evaporation of non-solid residues or by like method.

Inventors

  • 👤 I Thomas

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-30 22:23
CPC Classifications
C; C01; C01B; C01B33/00; C01B33/113; C01B33/12; C01B33/16; C01B33/163

Claims Analysis

Total Claims: 27
Claim 1
Independent Claim 50 words
The process of claim 1 wherein the silicon alkoxide is selected from compounds of the formula SIXn y4-n wherein X is hydrogen, phenyl, or alkyls of one to six carbons; y is OR where R is an alkyl of one to six carbons; and n is 0, 1, or 2.
Claim 2
Dependent Claim 25 words
The process of claim 1 wherein the silicon alkoxide is hydrolyzed in step I in the presence of a catalytic amount of a hydrolysis catalyst.
Claim 3
Dependent Claim 11 words
The process of claim 1 wherein the silicon alkoxide is tetraethylorthosilicate.
Claim 4
Dependent Claim 11 words
The process of claim 1 wherein the silicon alkoxide is tetramethylorthosilicate.
Claim 5
Dependent Claim 17 words
The process of claim 1 wherein the soluble source is a soluble salt of a rare earth.
Claim 6
Dependent Claim 20 words
The process of claim 6 wherein the base in step III is selected from ammonia, ammonium hydroxide, and organic amines.
Claim 7
Dependent Claim 32 words
The process of claim 7 wherein a non-ionic emulsifier is added to the mixture prior to the pH adjustment so as to enhance the uniformity of the subsequently formed solid, porous beads.
Claim 8
Dependent Claim 97 words
As a composition of matter, an ultra pure, hard, firm, solid, porous, clear, amorphous silicon oxide bead having a mean diameter of about 50 microns to about 500 microns and a B.E.T. surface area of about 500 to about 900 square meters per gram and doped with about 10 p.p.m. by weight to about 1 percent by weight elemental metal in the form of metal oxide based on the total weight of the silicon oxide and metal oxide, said doped silicon oxide bead containing less than 50 p.p.m. by weight of trace metal impurities including alkali metals.
Claim 9
Dependent Claim 23 words
The process of claim 1 wherein the total amount of water per mol of silicon alkoxide is between about 3.5 and 4.5 mols.
Claim 10
Dependent Claim 27 words
The process of claim 1 wherein the total amount of water per mol of silicon alkoxide used in step I is between about 0.9 and 1 mol.
Claim 11
Dependent Claim 29 words
The process of claim 1 wherein the total amount of water per mol of silicon alkoxide in steps I and II combined is between about 2.7 and 3.5 mols.
Claim 12
Dependent Claim 22 words
The process of claim 1 wherein the silicon alkoxide is hydrolyzed in step I at a temperature up to about 60* C.
Claim 13
Dependent Claim 13 words
The process of claim 3 wherein the hydrolysis catalyst is a mineral acid.
Claim 14
Dependent Claim 12 words
The process of claim 14 wherein the mineral acid is hydrochloric acid.
Claim 15
Dependent Claim 14 words
The process of claim 3 wherein the hydrolysis catalyst is a Lewis Acid Catalyst.
Claim 16
Dependent Claim 21 words
The process of claim 16 wherein, the Lewis Acid Catalyst comprises compounds of a transitional element consisting of Zr or Ti.
Claim 17
Dependent Claim 17 words
The process of claim 16 wherein the Lewis Acid Catalyst comprises compounds of the non-transitional element Al.
Claim 18
Dependent Claim 30 words
The process of claim 3 wherein the catalytic amount of hydrolysis catalyst is between about 1 and about 500 parts by weight per million parts by weight of silicon alkoxide.
Claim 19
Dependent Claim 22 words
The process of claim 1 wherein said hydroxyl containing organic solvent is a lower aliphatic alcohol containing less than 10 carbon atoms.
Claim 20
Dependent Claim 19 words
The process of claim 1 wherein said non-polar solvent is hexane, heptane, octane, nonane, benzene, toluene or carbon tetrachloride.
Claim 21
Dependent Claim 12 words
The process of claim 7 wherein said organic amines comprise alkyl amines.
Claim 22
Dependent Claim 11 words
The process of claim 22 wherein said alkyl amines include triethylamine.
Claim 23
Dependent Claim 28 words
The process of claim 8 wherein said non-ionic emulsifier is morpholine oleate, polyglycol, fatty acid esters, diethylene glycol monostearate, ethylene oxide condensates of amides or alkylaryl polyether alcohols.
Claim 24
Dependent Claim 73 words
The process of claim 1 wherein said metal oxide is an oxide of Al, Ga, In, Ti, Zr, Hf, V, Nb, Ta, B, P, Ge, Sn, Pb, Li, Na, K, Rb, Cs, Fr, Be, Mg, Ca, Sr, Ba, Ra, Fe, Co, Ni, Zr, Cd, Hg, Sc, Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Ac, Th, Pa, U, Np, Pu, Am, Cm, Bk or Cf.
Claim 25
Dependent Claim 127 words
The process of claim 1 wherein said soluble source of the metal oxide is a metal acetate, sulfate, nitrate, bromate, bromidE, chloride, carbonate, or selenate. m 27. The process of claim 1 wherein said soluble source of a metal oxide is a water-soluble, rare earth salt taken from the following: Rare Earth Lathanum acetate, bromate, bromide, chloride nitrate, sulfate Cerium cerous acetate, cerous bromate, cerous chloride, cerous nitrate, ceric basic nitrate, cerous selenate, cerous sulfate Praseodymium acetate, bromate, chloride, selenate, sulfate Neodymium acetate, bromate, bromide, chloride, nitrate, sulfate Samarium acetate, bromate, chloride, sulfate Europium sulfate, chloride, nitrate Gadolinium acetate, bromide, chloride, nitrate, selenate, sulfate Terbium chloride, nitrate, sulfate Dysprosium acetate, bromate, chloride, nitrate, selenate, sulfate Erbium chloride, nitrate, sulfate Thulium chloride Ytterbium acetate, chloride, sulfate Lutetium sulfate.
Claim 26
Dependent Claim 16 words
The composition of matter of claim 9 wherein said metal oxide is a rare earth oxide.
Claim 27
Dependent Claim 75 words
The composition of matter of claim 10 wherein said metal oxide is an oxide of Al, Ga, In, Ti, Zr, Hf, V, Nb, Ta, B, P, Ge, Sn, Pb, Li, Na, I, Rb, Cs, Fr, Be, Mg, Ca, Sr, Ba, Ra, Fe, Co, Ni, Zn, Cd, Hg, Sc, Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Ac, Th, Pa, U, Np, Pu, Am, Cm, Bk or Cf.

References Cited (Backward Citations)

US2419272A Cited
US2921839A Cited
US3015620A Cited
US3245918A Cited
US3483136A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1976-01-09 1976-07-10 1977-01-09 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1980-01-09 1980-07-10 1981-01-09 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1984-01-09 1984-07-10 1985-01-09 $7700.00 Window Closed / Lapsed

Assigned Categories & Tags

No categories assigned to this patent yet.

Assign Category Tag