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US3794713A Expired / Lapsed US ⏱️ 0.0 years remaining

Preparation of silica gels

Assignee: National Petro-Chemicals Corp
•
Filing: 1971-10-26
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Granted: 1974-02-26
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Expires: 1991-10-26
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Abstract

Abstract Silica xerogels having narrow pore diameter distribution in the range of 300 - 600 A, surface areas in the range of from 200 500 m2/g, and pore volumes in the range of 2.0 - 3.5 cm3/g and process for preparing such silica xerogels comprising critically controlled steps of precipitation of the silica gel, aging the precipitated silica hydrogel slurry, washing the aged product, displacing the water with an organic liquid substantially completely miscible with water and drying the gel.

Inventors

  • 👤 H Aboutboul
  • 👤 J Krekeler
  • 👤 W Kirch

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-02 22:24
CPC Classifications
C; C01; C01B; C01B33/00; C01B33/113; C01B33/12; C01B33/16; B; B01; B01J; B01J20/00; B01J20/02; B01J20/10; B01J20/103; B01J21/00; B01J21/06; B01J21/08; B01J35/00; B01J35/60; C01B33/14; C01B33/152; C01B33/154; C01B33/1543; B01J35/61; B01J35/615; B01J35/63; B01J35/638; B01J35/64; B01J35/647; B01J35/651; B01J35/66; B01J35/67

Claims Analysis

Total Claims: 29
Claim 1
Independent Claim 14 words
The method of claim 1 further comprising: f. calcining the product of step (e).
Claim 2
Dependent Claim 45 words
The method of claim 1 wherein the precipitation of silica xerogel in step (a) is accomplished by neutralization of the aqueous solution of an alkaline silicate with an agent selected from the group consisting of a strong acid, a weak acid, and an ion-exchange resin.
Claim 3
Dependent Claim 28 words
The method of claim 1 wherein the alkaline silicate is an alkali metal silicate and the temperature during step (b) is maintained above the temperature during step (a).
Claim 4
Dependent Claim 26 words
The method of claim 1 wherein the SiO2 concentration in the hydrogel slurry of step (a) is from about 8 to about 9 percent by weight.
Claim 5
Dependent Claim 19 words
The method of claim 1 wherein the temperature during neutralization step (a) is from about 0* to about 10*C..
Claim 6
Dependent Claim 24 words
The method of claim 1 wherein the pH of the hydrogel slurry during step (a) is maintained at from about 5 to about 7.
Claim 7
Dependent Claim 22 words
The method of claim 1 wherein the pH of the hydrogel slurry in step (b) is from about 4 to about 7.
Claim 8
Dependent Claim 23 words
The method of claim 1 wherein the temperature of the hydrogel slurry during step (b) is maintained at about 50* to about 100*C..
Claim 9
Dependent Claim 18 words
The method of claim 1 wherein the time of step (b) is about 1 to about 6 hours.
Claim 10
Dependent Claim 36 words
The method of claim 1 wherein the reduction of concentration of alkaline ions is accomplished by washing with a solution of displacing salts selected from the group consisting of ammonium chloride, ammonium nitrate and mixtures thereof.
Claim 11
Dependent Claim 29 words
The method of claim 1 wherein step (c) is accomplished by washing with a solution of a mineral acid selected from the group consisting of HCl, H2SO4 and HNO3.
Claim 12
Dependent Claim 26 words
The method of claim 1 wherein the organic liquid in step (d) is selected from the group consisting of lower aliphatic alcohols, acetone, and mixtures thereof.
Claim 13
Dependent Claim 51 words
The method of claim 1 wherein up to about 40 percent of the neutralizing medium is added in from about 30 to about 120 minutes and wherein the remaining neutralizing medium required to provide an end pH of 3 to 8 is added in about 20 to about 90 minutes more.
Claim 14
Dependent Claim 50 words
The method of claim 1 where the xerogel water content subsequent to displacement with said organic liquid but prior to drying is at least 1 percent by weight water but no greater than about 6 percent by weight water measured as the equilibrium water content in the displacing organic liquid.
Claim 15
Dependent Claim 18 words
The method of claim 15 wherein said water content is about 2 to about 3 percent by weight.
Claim 16
Dependent Claim 12 words
The method of claim 1 where step (b) is conducted under agitation.
Claim 17
Dependent Claim 24 words
The method of claim 1 where the silicate is a sodium silicate of the formula xNa2O.ySiO2 wherein y/x is from 1/1 to about 4/1.
Claim 18
Dependent Claim 18 words
The method of claim 1 further comprising comminuting the hydrogel after step (b) but prior to step (e).
Claim 19
Independent Claim 387 words
A method for producing a silica xerogel having a narrow pore diameter distribution primarily within the range of from 300 to 600 A, a surface area within the range of from 200 to 500 m2/g, a pore volume of from 2.2 to 3.0 cm3/g and stability at temperatures up to about 2,000* F. comprising: a. precipitating a silica hydrogel by neutralization of an aqueous solution of a sodium or potassium silicate to provide a silica hydrogel slurry having an SiO2 concentration of from about 8 to about 9 percent by weight while maintaining the pH at from about 5 to about 7 and maintaining the temperature at from about 0* C. to about 10* C., wherein the neutralizing medium is selected from the group consisting of a strong acid, a weak acid, and an ion-exchAnge resin and is added to the aqueous sodium or potassium silicate solution at a rate of up to about 40 percent of the necessary amount in from about 30 to about 120 minutes, and wherein the remaining amount of neutralizing medium necessary to provide an end pH of from about 5 to about 7 is added in a period of time of at least about 20 minutes more, precipitation being under conditions of good agitation, b. heating the product of step (a) at a temperature greater than the temperature of step (a) and at a pH of from about 5 to about 7 for at least about 1 hour, while agitating the product of step (a), c. reducing the sodium or potassium concentration of the product of step (b) by washing the product of step (b) with a liquid which displaces said sodium or potassium until the resulting wash liquor, at equilibrium with the product of step (b), contains less than about 20 ppm sodium or potassium, expressed as an acid-base salt thereof, d. displacing the water from the product of step (c) by replacement of the water with a water miscible organic liquid which reduces the surface tension within the pores of the gel to provide a product with a water content of from about 1 to 6 percent by weight measured as the water content in the displacing organic liquid, and e. drying the product of step (d) to remove the organic liquid and water and provide said silica xerogel.
Claim 20
Dependent Claim 14 words
The process of claim 20 additionally comprising: f. calcining the product of step (e).
Claim 21
Dependent Claim 38 words
The method of claim 20 wherein the reduction of concentration of sodium or potassium ions is accomplished by washing with a solution of displacing salts selected from the group consisting of ammonium chloride, ammonium nitrate and mixtures thereof.
Claim 22
Dependent Claim 29 words
The method of claim 20 wherein step (c) is accomplished by washing with a solution of a mineral acid selected from the group consisting of HCl, H2SO4 and HNO3.
Claim 23
Dependent Claim 26 words
The method of claim 20 wherein the organic liquid in step (d) is selected from the group consisting of lower aliphatic alcohols, acetone, and mixtures thereof.
Claim 24
Dependent Claim 18 words
The process of claim 20 wherein said water content is about 2 to about 3 percent by weight.
Claim 25
Dependent Claim 18 words
The method of claim 20 further comprising comminuting the hydrogel after step (d) but prior to step (e).
Claim 26
Dependent Claim 19 words
The method of claim 26 where the temperature of step (b) is from about 50* to about 100* C.
Claim 27
Dependent Claim 19 words
The method of claim 10 wherein the time of step (b) is from about 2 to about 4 hours.
Claim 28
Dependent Claim 19 words
The method of claim 20 wherein the time of step (b) is from about 1 to about 6 hours.
Claim 29
Dependent Claim 19 words
The method of claim 29 wherein the time of step (b) is from about 2 to about 4 hours.

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1977-02-25 1977-08-27 1978-02-26 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1981-02-25 1981-08-27 1982-02-26 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1985-02-25 1985-08-27 1986-02-26 $7700.00 Window Closed / Lapsed

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