US4029514A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Method of precipitating microfine silica using phosphate
Assignee: PQ Corp
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Filing: 1975-06-09
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Granted: 1977-06-14
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Expires: 1995-06-09
Abstract
Abstract The addition of sodium phosphate to a dilute solution of alkali metal silicate, precipitates microfine silica that is readily dispersible.
Inventors
- 👤 Klaus Robert Lange
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-27 13:55
CPC Classifications
C; C09; C09C; C09C1/00; C09C1/28; C09C1/30; C09C1/3045; C01; C01B; C01B25/00; C01B25/16; C01B25/26; C01B25/38; C01B25/40; C01B25/41; C01B33/00; C01B33/113; C01B33/12; C01B33/18; C08; C08K; C08K3/00; C08K3/34; C08K3/36; C01P; C01P2004/00; C01P2004/60; C01P2004/61; C01P2004/80; C01P2006/00; C01P2006/12; C01P2006/14; C01P2006/16; C01P2006/80; C01P2006/82; C01P2006/90; Y; Y10; Y10T; Y10T428/00; Y10T428/29; Y10T428/2982; Y10T428/2991; Y10T428/2993
Claims Analysis
Total Claims: 8
Claim 1
Independent Claim
189 words
A method of precipitating finely divided silica having an ultimate particle size between 20 and 800 mμ, loss on ignition between 6.5 and 10.5%, loss at 105° C between 3.0 and 5.0%, pH value of 6.5 to 10, void volume of 1.3 to 5.0 cc/g., surface area of 25 to 600 m 2 /g and pore volume of 0.01 to 0.4 cc/g. and having phosphate ions on the surface of said silica, said method comprising the steps of: a. forming a dilute solution of sodium slicate having a weight ratio of 1.5 to 4.0 SiO 2 /1.0 Na 2 O and containing 0.01 to 0.05 g. of Na 2 O/cc; b. heating the dilute silicate solution to a temperature between 80° and 100 ° C; c. adding 0.7 to 1.2 equivalents of phosphate salt per equivalent of Na 2 O to said heated solution while maintaining the temperature between 80° and 100° C for a period of 1.0 to 3.5 hours, thereby producing a slurry of silica; d. filtering, washing and reslurrying the silica with aqueous NH 3 , and e. filtering, rewashing and drying to obtain the product.
Claim 2
Independent Claim
189 words
A method of precipitating finely divided silica having an ultimate particle size between 20 and 800 mμ, loss on ignition between 6.5 and 10.5%, loss at 105° C between 3.0 and 5.0%, pH value of 6.5 to 10, void volume of 1.3 to 5.0 cc/g., surface area of 25 to 600 m 2 /g and pore volume of 0.01 to 0.4 cc/g. and having phosphate ions on the surface of said silica, said method comprising the steps of: a. forming a dilute solution of sodium slicate having a weight ratio of 1.5 to 4.0 SiO 2 /1.0 Na 2 O and containing 0.01 to 0.05 g. of Na 2 O/cc; b. heating the dilute silicate solution to a temperature between 80° and 100 ° C; c. adding 0.7 to 1.2 equivalents of phosphate salt per equivalent of Na 2 O to said heated solution while maintaining the temperature between 80° and 100° C for a period of 1.0 to 3.5 hours, thereby producing a slurry of silica; d. filtering, washing and reslurrying the silica with aqueous NH 3 , and e. filtering, rewashing and drying to obtain the product.
Claim 3
Dependent Claim
23 words
The method of claim 1, wherein the phosphate salt is selected from the group consisting of sodium trimetaphosphate, sodium tripolyphosphate and sodium hexametaphosphate.
Claim 4
Dependent Claim
21 words
The method of claim 1, wherein the heating temperatures recited in steps (b) and (c) is between 85° and 98° C.
Claim 5
Dependent Claim
219 words
In the process for producing precipitated silica particles from an alkali metal silicate by addition of a precipitating agent, filtering, reslurrying the precipitate with an aqueous washing agent, filtering, washing and drying; the improvement whereby, the silica particles have surface phosphate ions thereon, and are characterized by a particle size between 20 and 800 mμ, loss on ignition between 6.5 and 10.5%, loss at 105° C between 3.0 and 5.0%, pH value between 6.5 and 10, void volume of 1.3 to 5.0 cc/g, surface area of 25 to 600 m 2 /g and pore volume of 0.01 to 0.4 cc/g and comprising the steps of: a. forming a dilute solution of sodium silicate having a weight ratio of 1.5 to 4.0 SiO 2 /1.0 Na 2 O, and containing 0.01 to 0.05 g of Na 2 O/cc; b. heating said solution to a temperature between 80° and 100° C; c. adding sufficient phosphate salt to said heated solution to obtain 0.7 to 1.2 equivalents of phosphate salt per equivalent of Na 2 O, while maintaining the temperature between 80° and 100° C for a period of 1.0 to 3.5 hours, thereby producing a slurry of silica; d. filtering, washing and reslurrying the silica with aqueous NH 3 , and then e. filtering, rewashing and drying to obtain the product.
Claim 6
Dependent Claim
219 words
In the process for producing precipitated silica particles from an alkali metal silicate by addition of a precipitating agent, filtering, reslurrying the precipitate with an aqueous washing agent, filtering, washing and drying; the improvement whereby, the silica particles have surface phosphate ions thereon, and are characterized by a particle size between 20 and 800 mμ, loss on ignition between 6.5 and 10.5%, loss at 105° C between 3.0 and 5.0%, pH value between 6.5 and 10, void volume of 1.3 to 5.0 cc/g, surface area of 25 to 600 m 2 /g and pore volume of 0.01 to 0.4 cc/g and comprising the steps of: a. forming a dilute solution of sodium silicate having a weight ratio of 1.5 to 4.0 SiO 2 /1.0 Na 2 O, and containing 0.01 to 0.05 g of Na 2 O/cc; b. heating said solution to a temperature between 80° and 100° C; c. adding sufficient phosphate salt to said heated solution to obtain 0.7 to 1.2 equivalents of phosphate salt per equivalent of Na 2 O, while maintaining the temperature between 80° and 100° C for a period of 1.0 to 3.5 hours, thereby producing a slurry of silica; d. filtering, washing and reslurrying the silica with aqueous NH 3 , and then e. filtering, rewashing and drying to obtain the product.
Claim 7
Dependent Claim
23 words
The process of claim 4, wherein the phosphate salt is selected from the group consisting of sodium trimetaphosphate, sodium tripolyphosphate and sodium hexametaphosphate.
Claim 8
Dependent Claim
15 words
The process of claim 4, wherein the heating takes place between 85° and 98° C.
References Cited (Backward Citations)
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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) | 1980-06-13 | 1980-12-13 | 1981-06-14 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1984-06-13 | 1984-12-13 | 1985-06-14 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1988-06-13 | 1988-12-13 | 1989-06-14 | $7700.00 | Window Closed / Lapsed |