US3988162A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Amorphous precipitated silica products and method for their production
Assignee: JM Huber Corp
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Filing: 1974-10-31
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Granted: 1976-10-26
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Expires: 1994-10-31
Abstract
Abstract A new method for producing precipitated silicas having a unique combination of physical and chemical properties is disclosed. The silicas are produced by acidulating a solution of an alkali metal silicate having a specific SiO 2 /Na 2 O mol ratio with an acid until precipitation just begins. At this point, the reaction mass is aged for a period of time and thereafter the acid addition is continued until the precipitated product is obtained. Products produced in accordance with the invention exhibit lower wet cake moisture and are characterized by their low structure, low oil absorption, high abrasiveness and high pack density, and as such are distinctly different from silicas used as reinforcing fillers in rubber. In a particularly advantageous embodiment, an adduct material, such as aluminum, is added to control the refractive index of the precipitated pigment silica. Products produced in this manner have particular utility for use as abrasion and gelling agents in clear toothpaste compositions.
Inventors
- 👤 Satish K. Wason
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-25 15:48
CPC Classifications
C; C09; C09C; C09C1/00; C09C1/28; C09C1/30; A; A61; A61K; A61K8/00; A61K8/18; A61K8/19; A61K8/25; A61Q; A61Q11/00; C01; C01B; C01B33/00; C01B33/113; C01B33/12; C01B33/18; C01B33/187; C01B33/193; C01B33/20; C01B33/26; C01B33/28; C01B33/2807; C01B33/2838; C01B33/36; C01B33/38; C01B33/40; C01B33/42; C01B33/46; C09C1/40; C09D; C09D7/00; C09D7/40; C09D7/42; A61K2800/00; A61K2800/20; A61K2800/26; A61K2800/262; C01P; C01P2002/00; C01P2002/02; C01P2004/00; C01P2004/50; C01P2006/00; C01P2006/10; C01P2006/11; C01P2006/12; C01P2006/19; C01P2006/60; C01P2006/80; C01P2006/82; C01P2006/90
Claims Analysis
Total Claims: 9
Claim 1
Independent Claim
249 words
A method for producing amorphous, precipitated silicas having improved chemical and physical properties including high abrasiveness and low wet cake moisture content prior to the drying thereof, said method comprising the steps of: acidulating an aqueous solution of an alkali metal silicate having an SiO 2 /X 2 O mol ratio in the range of from about 2.0 to 2.7 wherein X is selected from the group consisting of sodium, potassium, and lithium with an acid selected from the group consisting of sulfuric acid, nitric acid, and hydrochloric acid; said aqueous alkali metal silicate solution having a concentration on the order of about 1.0 to 2.5 pounds silicate per gallon, said acid being added as a dilute solution thereof and having a concentration of from about 10 to 25% by weight acid based on the weight of the solution thereof; continuing the addition of said acid until that point at which precipitation of said silica just begins; interrupting and discontinuing the addition of said acid to said silicate at said point; aging the resulting aqueous reaction mass for a period of time sufficient to obtain an equilibrium condition of the reactants comprising said reaction mass; continuing the addition of said acid to said aqueous mass following said aging period while simultaneously adding an alkali metal silicate therewith and until the precipitation of said silica is complete, adjusting the pH of the mass to acid, separating the precipitated silica from said aqueous reaction mass and recovering the precipitated silica material.
Claim 2
Independent Claim
249 words
A method for producing amorphous, precipitated silicas having improved chemical and physical properties including high abrasiveness and low wet cake moisture content prior to the drying thereof, said method comprising the steps of: acidulating an aqueous solution of an alkali metal silicate having an SiO 2 /X 2 O mol ratio in the range of from about 2.0 to 2.7 wherein X is selected from the group consisting of sodium, potassium, and lithium with an acid selected from the group consisting of sulfuric acid, nitric acid, and hydrochloric acid; said aqueous alkali metal silicate solution having a concentration on the order of about 1.0 to 2.5 pounds silicate per gallon, said acid being added as a dilute solution thereof and having a concentration of from about 10 to 25% by weight acid based on the weight of the solution thereof; continuing the addition of said acid until that point at which precipitation of said silica just begins; interrupting and discontinuing the addition of said acid to said silicate at said point; aging the resulting aqueous reaction mass for a period of time sufficient to obtain an equilibrium condition of the reactants comprising said reaction mass; continuing the addition of said acid to said aqueous mass following said aging period while simultaneously adding an alkali metal silicate therewith and until the precipitation of said silica is complete, adjusting the pH of the mass to acid, separating the precipitated silica from said aqueous reaction mass and recovering the precipitated silica material.
Claim 3
Dependent Claim
23 words
The method in accordance with claim 1 wherein said aging period is in the range of from about 10 minutes to 2 hours.
Claim 4
Dependent Claim
77 words
The method in accordance with claim 2 wherein an adduct material selected from the group consisting of the water soluble salts of aluminum, magnesium, zinc and calcium, is combined with said acid during the acidulating of said silicate solution to thereby control the refractive index of the precipitated silica and to form an adduct of said silicate with said water soluble salt having particular utility for use as an abrasive and gelling agent in clear toothpaste compositions.
Claim 5
Dependent Claim
48 words
The method in accordance with claim 1 wherein the pH of the reaction medium is adjusted to a value in the range of about 5.5 to 7.0 after precipitation is complete to therefore increase the surface area to a value of greater than 200 square meters per gram.
Claim 6
Dependent Claim
23 words
The method in accordance with claim 1 wherein the low structure silicas have a radioactive dentin abrasion of between about 50 to 1200.
Claim 7
Dependent Claim
18 words
The method in accordance with claim 5 wherein said radioactive dentin abrasion is between about 200 to 500.
Claim 8
Dependent Claim
21 words
A method according to claim 1 wherein the alkali metal silicate is sodium silicate and the acidulating agent is sulfuric acid.
Claim 9
Dependent Claim
27 words
A method according to claim 3 wherein the alkali metal silicate is sodium silicate, the acidulating acid is sulfuric acid and the adduct material is aluminum sulfate.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1979-10-26 | 1980-04-26 | 1980-10-26 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1983-10-26 | 1984-04-26 | 1984-10-26 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1987-10-26 | 1988-04-26 | 1988-10-26 | $7700.00 | Window Closed / Lapsed |