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US4060596A
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Method of making goethite powder
Assignee: Sony Corp
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Filing: 1975-10-31
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Granted: 1977-11-29
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Expires: 1995-10-31
Abstract
Abstract A method of making goethite powder in which a ferrous hydroxide suspension is stirred for about 3 hours in an inert atmosphere and then is oxidized to form goethite powder.
Inventors
- 👤 Tokio Nakamura
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-30 08:59
CPC Classifications
G; G11; G11B; G11B5/00; G11B5/62; G11B5/68; G11B5/70; G11B5/706; G11B5/70626; G11B5/70642; G11B5/70652; G11B5/70663; C; C01; C01G; C01G49/00; C01G49/02; C01G49/06; G11B5/70647; C01P; C01P2004/00; C01P2004/10; C01P2004/60; C01P2004/62; C01P2006/00; C01P2006/42
Claims Analysis
Total Claims: 14
Claim 1
Independent Claim
214 words
In the production of goethite, the improvement comprising a method of making acicular goethite powder comprising the steps of: 1. mixing in a relatively short time an aqueous solution of an alkali hydroxide selected from the group consisting of sodium hydroxide and potassium hydroxide with an aqueous solution of ferrous salt selected from the group consisting of ferrous chloride and ferrous sulfate under an inert atmosphere to form a suspension of ferrous hydroxide in a temperature range of 60° to 80° centrigrade, 2. continuously stirring said mixed ferrous hydroxide suspension for a period of 2 to 5 hours which time is substantially greater than said mixing time under an inert gaseous atmosphere until milk-white colored fine ferrous hydroxide suspension is formed, and during said period of stirring the temperature of the solution being in the temperature range of 60° to 80° centrigrade, 3. and then oxidizing said ferrous hydroxide suspension by an oxygen containing gas for a period of 4 to 6.5 hours until yellow colored goethite is formed, the temperature range being 50° to 80° centrigrade when the alkali hydroxide is potassium hydroxide and the ferrous salt is ferrous chloride and the temperature range being 40° to 60° centrigrade when sodium hydroxide is the alkali hydroxide and the ferrous salt is ferrous sulfate.
Claim 2
Dependent Claim
214 words
In the production of goethite, the improvement comprising a method of making acicular goethite powder comprising the steps of: 1. mixing in a relatively short time an aqueous solution of an alkali hydroxide selected from the group consisting of sodium hydroxide and potassium hydroxide with an aqueous solution of ferrous salt selected from the group consisting of ferrous chloride and ferrous sulfate under an inert atmosphere to form a suspension of ferrous hydroxide in a temperature range of 60° to 80° centrigrade, 2. continuously stirring said mixed ferrous hydroxide suspension for a period of 2 to 5 hours which time is substantially greater than said mixing time under an inert gaseous atmosphere until milk-white colored fine ferrous hydroxide suspension is formed, and during said period of stirring the temperature of the solution being in the temperature range of 60° to 80° centrigrade, 3. and then oxidizing said ferrous hydroxide suspension by an oxygen containing gas for a period of 4 to 6.5 hours until yellow colored goethite is formed, the temperature range being 50° to 80° centrigrade when the alkali hydroxide is potassium hydroxide and the ferrous salt is ferrous chloride and the temperature range being 40° to 60° centrigrade when sodium hydroxide is the alkali hydroxide and the ferrous salt is ferrous sulfate.
Claim 3
Dependent Claim
30 words
A method of making goethite powder according to claim 1, wherein a mol ratio of OH - ion to Fe ++ ion (OH - /Fe ++ ) is over 3.
Claim 4
Dependent Claim
29 words
A method of making goethite powder according to claim 1, wherein a mole ratio of OH - ion to Fe ++ ion (OH - /Fe ++ ) is 3.8-5.8.
Claim 5
Dependent Claim
25 words
The method of claim 1, wherein said contacting is continued until substantially all of the ferrous ions in said suspension have been removed by oxidation.
Claim 6
Dependent Claim
25 words
The method of claim 1, wherein after said contacting is completed, the resulting mixture is filtered, and the so separated solids are dried and pulverized.
Claim 7
Dependent Claim
28 words
The method of claim 1, wherein the concentration of said ferrous salt in said starting solution thereof ranges from about 1.2 to 3.0 mol per liter of water.
Claim 8
Dependent Claim
28 words
The method of claim 1, wherein the concentration of said alkali hydroxide in said starting solution thereof ranges from about 6.0 to 12.0 mol per liter of water.
Claim 9
Dependent Claim
12 words
The method of claim 1, wherein said inert gaseous atmosphere comprises nitrogen.
Claim 10
Dependent Claim
12 words
The method of claim 1, wherein said oxygen containing gas comprises air.
Claim 11
Dependent Claim
222 words
In the production of goethite, the improvement comprising a method of making acicular goethite powder comprising a method of steps of mixing and simultaneously stirring for a relatively short time an aqueous solution of an alkali hydroxide selected from the group consisting of potassium hydroxide and sodium hydroxide with an aqueous solution of a ferrous salt, selected from the group consisting of ferrous chloride and ferrous sulfate in a temperature range of 60° to 80° centigrade and then continuing said stirring of the resulting mixture thereby to produce a colloidal aqueous suspension of ferrous hydroxide, said stirring being continued for a period of 2 to 5 hours until milk-white colored ferrous hydroxide suspension is formed, said mixing being accomplished in a time interval less than that used for said stirring, said mixing and said stirring being carried out in an inert gaseous atmosphere, during said stirring the temperature of said solution maintained in the temperature range of 60 to 80° C, and thereafter contacting the resulting suspension with an oxygen containing gas, thereby to oxidize said ferrous hydroxide for a period of 4 to 6.5 hours until yellow goethite is formed the temperature being 50° to 80° centigrade when potassium hydroxide and ferrous chloride is used and the temperature of 40° to 60° centrigrade when sodium hydroxide and ferrous sulfate is used.
Claim 12
Dependent Claim
222 words
In the production of goethite, the improvement comprising a method of making acicular goethite powder comprising a method of steps of mixing and simultaneously stirring for a relatively short time an aqueous solution of an alkali hydroxide selected from the group consisting of potassium hydroxide and sodium hydroxide with an aqueous solution of a ferrous salt, selected from the group consisting of ferrous chloride and ferrous sulfate in a temperature range of 60° to 80° centigrade and then continuing said stirring of the resulting mixture thereby to produce a colloidal aqueous suspension of ferrous hydroxide, said stirring being continued for a period of 2 to 5 hours until milk-white colored ferrous hydroxide suspension is formed, said mixing being accomplished in a time interval less than that used for said stirring, said mixing and said stirring being carried out in an inert gaseous atmosphere, during said stirring the temperature of said solution maintained in the temperature range of 60 to 80° C, and thereafter contacting the resulting suspension with an oxygen containing gas, thereby to oxidize said ferrous hydroxide for a period of 4 to 6.5 hours until yellow goethite is formed the temperature being 50° to 80° centigrade when potassium hydroxide and ferrous chloride is used and the temperature of 40° to 60° centrigrade when sodium hydroxide and ferrous sulfate is used.
Claim 13
Dependent Claim
29 words
A method of making goethite powder according to claim 10, wherein a mol ratio of OH - ion to Fe ++ ion (OH - /Fe ++ ) is 3.2-4.5.
Claim 14
Dependent Claim
24 words
A method of making goethite powder according to claim 10, wherein said fine ferrous hydroxide suspension is oxidized at the temperature of 50°-80° C.
References Cited (Backward Citations)
CA505751A
Cited
US3047428A
Cited
GB1212126A
Cited
US3692683A
Cited
US3843773A
Cited
US3912646A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1980-11-28 | 1981-05-30 | 1981-11-29 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1984-11-28 | 1985-05-30 | 1985-11-29 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1988-11-28 | 1989-05-30 | 1989-11-29 | $7700.00 | Window Closed / Lapsed |