Patent US5256386A successfully refreshed from Google Patents.
US5256386A
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Method for preparation of silica particles
Assignee: Nouryon Pulp and Performance Chemicals AB
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Filing: 1990-06-14
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Granted: 1993-10-26
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Expires: 2010-06-14
Abstract
Abstract Silica particles which are substantially spherical, have a particle size of 1 to 100 μm, a very narrow pore size distribution and a low alkali metal content. The particles can be prepared by sol-gel technique using emulsification technique for drop formation. The process comprises a sol growth step in a basic environment based on ammonium or amines and a post-treatment in such an environment. The silica particles are particularly suitable for use in chromatography as they have very good particle and porosity properties and high purity.
Inventors
- 👤 Mats Nystrom
- 👤 Wolgang Herrmann
- 👤 Bernt Larsson
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-08 15:06
CPC Classifications
B; B01; B01J; B01J20/00; B01J20/02; B01J20/10; B01J20/103; B01J21/00; B01J21/06; B01J21/08; C; C01; C01B; C01B33/00; C01B33/113; C01B33/12; C01B33/16
Claims Analysis
Total Claims: 14
Claim 1
Independent Claim
174 words
A process for the preparation of substantially spherical silica particles, comprising the steps of: 1) preparing at least one acid aqueous silica sol with an alkali metal content below 100 ppm and a particle size essentially below 3 nm; 2) heat treating the prepared sol in an ammonium or amine basic solution resulting in growth of the sol particles to a size corresponding to an area within the range of from about 50 to about 500 m 2 /g; 3) emulsifying the sol, after optional concentration, in an organic medium which is not miscible with water, or has a limited miscibility or solubility with water, and in the presence of a surface active agent; 4) gelling the formed sol drops by dewatering at a temperature of from about 30° C. to about 100° C. and at a pH of from about 5 to about 9; 5) heat treating the produced gel particles for removal of substantially all organic material; and 6) post-treating the gel particles in a basic environment containing ammonium or an amine.
Claim 2
Dependent Claim
174 words
A process for the preparation of substantially spherical silica particles, comprising the steps of: 1) preparing at least one acid aqueous silica sol with an alkali metal content below 100 ppm and a particle size essentially below 3 nm; 2) heat treating the prepared sol in an ammonium or amine basic solution resulting in growth of the sol particles to a size corresponding to an area within the range of from about 50 to about 500 m 2 /g; 3) emulsifying the sol, after optional concentration, in an organic medium which is not miscible with water, or has a limited miscibility or solubility with water, and in the presence of a surface active agent; 4) gelling the formed sol drops by dewatering at a temperature of from about 30° C. to about 100° C. and at a pH of from about 5 to about 9; 5) heat treating the produced gel particles for removal of substantially all organic material; and 6) post-treating the gel particles in a basic environment containing ammonium or an amine.
Claim 3
Dependent Claim
23 words
A process according to claim 1, characterized in that gelling is carried out in the presence of a substance which accelerates the gelling.
Claim 4
Dependent Claim
19 words
A process according to claim 1, characterized in that ammonium hydroxide solution is used in steps 2) and 6).
Claim 5
Dependent Claim
16 words
A process according to claim 1, characterized in that the sol which is emulsified is polydisperse.
Claim 6
Dependent Claim
27 words
A process according to claim 1, characterized in that the heat treatment of the gel particles is carried out at a temperature of at least 600° C.
Claim 7
Dependent Claim
29 words
A process according to claim 1, characterized in that the post-treatment in the ammonium or amine basic environment is carried out at a pH of at least about 11.3.
Claim 8
Dependent Claim
233 words
A process for the preparation of silica particles, comprising the steps of: 1) preparing at least one acid aqueous silica sol with an alkali metal content below 100 ppm and a particle size essentially below 3 nm; 2) heat treating the prepared sol in an ammonium or amine basic solution resulting in growth of the sol particles to a size corresponding to an area within the range of from about 50 to about 500 m 2 /g; 3) emulsifying the sol, after optional concentration, in an organic medium which is not miscible with water, or has a limited miscibility or solubility with water, and in the presence of a surface active agent; 4) gelling the formed sol drops by dewatering at a temperature of from about 30° C. to about 100° C. and at a pH of from about 5 to about 9; 5) heat treating the produced gel particles for removal of substantially all organic material; and 6) post-treating the gel particles in a basic environment containing ammonium or an amine; wherein the silica particles are substantially spherical and have a particle size within the range of from about 1 to about 100 μm, a pore size distribution where the part of the pore volume within the range of from 0.5d to 1.5d, where d is the mean pore diameter, is greater than 90% and an alkali metal content below 100 ppm.
Claim 9
Dependent Claim
233 words
A process for the preparation of silica particles, comprising the steps of: 1) preparing at least one acid aqueous silica sol with an alkali metal content below 100 ppm and a particle size essentially below 3 nm; 2) heat treating the prepared sol in an ammonium or amine basic solution resulting in growth of the sol particles to a size corresponding to an area within the range of from about 50 to about 500 m 2 /g; 3) emulsifying the sol, after optional concentration, in an organic medium which is not miscible with water, or has a limited miscibility or solubility with water, and in the presence of a surface active agent; 4) gelling the formed sol drops by dewatering at a temperature of from about 30° C. to about 100° C. and at a pH of from about 5 to about 9; 5) heat treating the produced gel particles for removal of substantially all organic material; and 6) post-treating the gel particles in a basic environment containing ammonium or an amine; wherein the silica particles are substantially spherical and have a particle size within the range of from about 1 to about 100 μm, a pore size distribution where the part of the pore volume within the range of from 0.5d to 1.5d, where d is the mean pore diameter, is greater than 90% and an alkali metal content below 100 ppm.
Claim 10
Dependent Claim
21 words
A process according to claim 7, wherein gelling is carried out in the presence of a substance which accelerates the gelling.
Claim 11
Dependent Claim
17 words
A process according to claim 7, wherein ammonium hydroxide solution is used in steps 2) and 6).
Claim 12
Dependent Claim
14 words
A process according to claim 7, wherein the sol which is emulsified is polydisperse.
Claim 13
Dependent Claim
25 words
A process according to claim 7, wherein the heat treatment of the gel particles is carried out at a temperature of at least 600° C.
Claim 14
Dependent Claim
27 words
A process according to claim 7, wherein the post-treatment in the ammonium or amine basic environment is carried out at a pH of at least about 11.3.
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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) | 1996-10-25 | 1997-04-26 | 1997-10-26 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 2000-10-25 | 2001-04-26 | 2001-10-26 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2004-10-25 | 2005-04-26 | 2005-10-26 | $7700.00 | Window Closed / Lapsed |