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US4382070A Expired / Lapsed US ⏱️ 0.0 years remaining

Process for producing xerogel of silicic acid with high volume of pores

Assignee: SLOVENSKA AKADEMIA VIED BRATISLAVA CZECHOSLOVAKIA
•
Filing: 1981-12-28
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Granted: 1983-05-03
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Expires: 2001-12-28
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Abstract

Abstract The product of this invention can be applied as a column packing for high performance liquid chromatography. This material is further useful as a catalyst carrier, as a sorbent for selective concentrating diluted compounds for analytical purposes, and for immobilizing enzymes and the like. The invention discloses a process for producing silicic acid xerogel matrix with a volume of pores up to 4.0 cm 3 g -1 or even more, which process consists in that the starting soft and elastic silica hydrogel is subjected to combined effect of successive hardening in concentrated solutions of strong inorganic or organic acids, such as, for example, sulphuric acid, hydrochloric, phosphoric, nitric or trichloroacetic acids at ambient or elevated temperatures followed by acting in water-miscible solvents, such as, for example, in alcohols or ketones, and finally, by acting in water-immiscible solvents, such as, for example, in benzene, toluene, C 5 to C 12 hydrocarbons or carbon tetrachloride.

Inventors

  • 👤 Ivan Novak
  • 👤 Dusan Berek

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-06 04:45
CPC Classifications
C; C01; C01B; C01B33/00; C01B33/113; C01B33/12; C01B33/16

Claims Analysis

Total Claims: 6
Claim 1
Independent Claim 168 words
A process for producing xerogel of silicic acid with a high volume of pores, consisting essentially of: (A) hardening wet hydrogel of polymeric silicic acid by aging for about 3 to 24 hours in a concentrated acid selected from the group consisting of sulphuric, hydrochloric, phosphoric, nitric and trichloracetic acids, the minimum concentrations thereof being 90 wt %, 37 wt %, 55 wt %, 65 wt % and 98 wt %, respectively, the amount of acid being such that the final concentration of said acid in the acid-hydrogel mixture is higher than 20 wt %, (b) removing said mineral or organic acid by washing and subsequently washing the hydrogel with an organic water-miscible solvent followed by washing with an organic water-immiscible solvent, thereby forming a lyogel, (c) stabilizing said lyogel by heating and annealing at temperatures of from 200° to 950° C., wherein the xerogel produced has a higher pore volume than an xerogel produced according to said process absent the washing step with the organic water-immiscible solvent.
Claim 2
Dependent Claim 168 words
A process for producing xerogel of silicic acid with a high volume of pores, consisting essentially of: (A) hardening wet hydrogel of polymeric silicic acid by aging for about 3 to 24 hours in a concentrated acid selected from the group consisting of sulphuric, hydrochloric, phosphoric, nitric and trichloracetic acids, the minimum concentrations thereof being 90 wt %, 37 wt %, 55 wt %, 65 wt % and 98 wt %, respectively, the amount of acid being such that the final concentration of said acid in the acid-hydrogel mixture is higher than 20 wt %, (b) removing said mineral or organic acid by washing and subsequently washing the hydrogel with an organic water-miscible solvent followed by washing with an organic water-immiscible solvent, thereby forming a lyogel, (c) stabilizing said lyogel by heating and annealing at temperatures of from 200° to 950° C., wherein the xerogel produced has a higher pore volume than an xerogel produced according to said process absent the washing step with the organic water-immiscible solvent.
Claim 3
Dependent Claim 18 words
The process of claim 1, wherein the aging is effected at temperatures of from 20° to 95° C.
Claim 4
Dependent Claim 23 words
The process of claim 1, wherein said organic water-miscible solvent is selected from the group consisting of methanol, ethanol, acetone, dioxane and tetrahydrofuran.
Claim 5
Dependent Claim 28 words
The process of claim 1, wherein said water-immiscible solvents is selected from the group consisting of benzene, toluene, C 5 to C 12 light hydrocarbons and carbon tetrachloride.
Claim 6
Dependent Claim 23 words
The process of claim 1, wherein the annealing of said silica lyogel is effected at a temperature of from 700° to 750° C.

References Cited (Backward Citations)

US3526603A Cited
US3819811A Cited
US3959174A Cited
US3977993A Cited
US4089932A Cited
US4246139A Cited
US4206297A Cited
US4169926A Cited
US4301034A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1986-05-02 1986-11-01 1987-05-03 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1990-05-02 1990-11-01 1991-05-03 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1994-05-02 1994-11-01 1995-05-03 $7700.00 Window Closed / Lapsed

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