US4241035A
Expired / Lapsed
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Synthetic imogolite
Assignee: BTG International Ltd
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Filing: 1979-07-03
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Granted: 1980-12-23
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Expires: 1999-07-03
Abstract
Abstract An inorganic material akin to imogolite is synthesized. Imogolite is a natural product having tubular structure and occurs in some soils. The synthetic product has tubes of 13-17% greater diameter, and is made thus: Prepare an aqueous hydroxyaluminium silicate solution containing up to 0.5 molar aluminium and of pH 3.1 to 5.0 by acid-hydrolyzing aluminium alkoxides and (introduced not earlier than the alkoxide) tetraalkyl silicate. The atomic proportion of Si: Al is up to 0.6:1. The solution thus prepared is digested, say at 96 DEG C. for a day, until a product is obtained displaying discernible electron diffraction peaks at 1.4 A, 2.1 A and 4.2 A.
Inventors
- 👤 Victor C. Farmer
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-05 12:20
CPC Classifications
C; C01; C01B; C01B33/00; C01B33/20; C01B33/26; B; B01; B01D; B01D71/00; B01D71/02; B01D71/024; C02; C02F; C02F1/00; C02F1/28; C02F1/281; C04; C04B; C04B35/00; C04B35/622; C04B35/62227; C04B35/62231; C04B35/6224
Claims Analysis
Total Claims: 22
Claim 1
Independent Claim
116 words
A method of synthesising an inorganic material which is a fibrous product having tubular structure related to, or resembling, the natural product imogolite, the method comprising: preparing an aqueous hydroxyaluminum silicate solution containing up to 0.5 molar aluminum, wherein the atomic proportion of Si:Al in the solution does not exceed 0.6:1 when the solution contains a concentration of silicon over 20 mM, the solution having a pH of 3.1 to 5.0 and having been prepared by hydrolysis in acid of aluminum alkoxide and, introduced not later than the aluminum alkoxide, tetraalkyl silicate; and digesting the solution thus prepared until a product is obtained displaying discernible electron diffraction peaks at 1.4 A, 2.1 A and 4.2 A.
Claim 2
Independent Claim
116 words
A method of synthesising an inorganic material which is a fibrous product having tubular structure related to, or resembling, the natural product imogolite, the method comprising: preparing an aqueous hydroxyaluminum silicate solution containing up to 0.5 molar aluminum, wherein the atomic proportion of Si:Al in the solution does not exceed 0.6:1 when the solution contains a concentration of silicon over 20 mM, the solution having a pH of 3.1 to 5.0 and having been prepared by hydrolysis in acid of aluminum alkoxide and, introduced not later than the aluminum alkoxide, tetraalkyl silicate; and digesting the solution thus prepared until a product is obtained displaying discernible electron diffraction peaks at 1.4 A, 2.1 A and 4.2 A.
Claim 3
Dependent Claim
17 words
A method according to claim 1, wherein the prepared solution has a pH of 3.5 to 4.6.
Claim 4
Dependent Claim
28 words
A method according to claim 1, wherein the atomic proportion of Si:Al in the solution does not exceed 0.5:1 and wherein the solution contains over 20 mM Si.
Claim 5
Dependent Claim
35 words
A method according to claim 1, wherein the aluminium alkoxide is mixed with the tetraalkyl silicate before the mixture is hydrolysed with acid to produce the aqueous hydroxyaluminium silicate solution of pH 3.0 to 5.0.
Claim 6
Dependent Claim
17 words
A method according to claim 1, wherein the acid used for the hydrolysis is a non-complexing acid.
Claim 7
Dependent Claim
16 words
A method according to claim 5, wherein the acid is a mineral acid, excluding sulphuric acid.
Claim 8
Dependent Claim
20 words
A method according to claim 6, wherein the acid is any one of perchloric acid, nitric acid and hydrochloric acid.
Claim 9
Dependent Claim
18 words
A method according to claim 7, wherein the acid comprises a mixture of perchloric acid and acetic acid.
Claim 10
Dependent Claim
33 words
A method according to claim 7, wherein the perchloric acid is present in a concentration of at least (one sixth of the aluminium plus 1) millimolar and at most (the aluminium plus 5)millimolar.
Claim 11
Dependent Claim
18 words
A method according to claim 1, wherein chloride ion if present has a concentration not exceeding 25 millimolar.
Claim 12
Dependent Claim
19 words
A method according to claim 1, wherein the atomic proportion of Si:Al in the solution is at least 0.1:1.
Claim 13
Dependent Claim
42 words
A method according to claim 1, wherein, during the digestion, additional hydroxyaluminum silicate solution containing up to 40 millimolar aluminum is added in stages on a daily basis until the hydroxyaluminum silicate reaches a concentration of at least 60 millimolar in aluminum.
Claim 14
Dependent Claim
17 words
A method according to claim 1, wherein the digestion is performed at 40° C. to 170° C.
Claim 15
Dependent Claim
17 words
A method according to claim 13, wherein the digestion is performed at 90° C. to 130° C.
Claim 16
Dependent Claim
17 words
A method according to claim 14, wherein the digestion is performed at 95° C. to 100° C.
Claim 17
Dependent Claim
20 words
A method according to claim 1, wherein the digestion is performed at a pH of not more than 4.6 throughout.
Claim 18
Dependent Claim
18 words
A method according to claim 16, wherein the pH when the digestion starts is not less than 3.5.
Claim 19
Dependent Claim
20 words
A method according to claim 1, wherein, after digestion, the resulting colloidal solution is dried to recover the inorganic material.
Claim 20
Dependent Claim
35 words
A method according to claim 1, wherein, after digestion, a gel is precipitated from the resulting colloidal solution by the addition of alkali or salt and then freeze-dried and centrifuged to recover the inorganic material.
Claim 21
Dependent Claim
26 words
A method according to claim 1, wherein, after digestion, the resulting colloidal solution is subjected to foam-flotation using an anionic detergent to recover the inorganic material.
Claim 22
Dependent Claim
28 words
A method according to claim 1, wherein, after digestion, the resulting colloidal solution is evaporated on a flat surface to recover the inorganic material as a coherent film.
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) | 1983-12-23 | 1984-06-23 | 1984-12-23 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1987-12-23 | 1988-06-23 | 1988-12-23 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1991-12-23 | 1992-06-23 | 1992-12-23 | $7700.00 | Window Closed / Lapsed |