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US4337228A Expired / Lapsed US ⏱️ 0.0 years remaining

Process for the production of sulfates

Assignee: Alumax Inc
•
Filing: 1981-06-08
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Granted: 1982-06-29
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Expires: 2001-06-08
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Abstract

Abstract A process for commercially producing sulfates useful in the water treatment and papermaking industries from by-product aluminum oxides is taught. The process comprises feeding the aluminum oxide by-product and weak process liquor into digester vessel to form a slurry which is then heated. Sulfuric acid and additional oxide feed is added into the slurry mixture allowing the reaction to go to completion. Specific variables such as temperature, pH, reactant concentrations, reaction times and process liquor recycle are controlled to substantially eliminate certain heavy metals in any form whatsoever from contaminating the final sulfate product.

Inventors

  • 👤 Luther W. Garrett, Jr.

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-02 23:26
CPC Classifications
C; C01; C01F; C01F7/00; C01F7/68; C01F7/74; C01F7/76; C01F7/762; C01F7/765

Claims Analysis

Total Claims: 17
Claim 1
Independent Claim 155 words
A process for producing sulfates from by-product aluminum oxide wherein said sulfates contain no appreciable heavy metals, their oxides or sulfates selected from the group consisting of Cu, Cr, Mn and Pb comprising: A. feeding the aluminum oxide by-product and process-weak liquor into a digester vessel to form a slurry; B. heating the resulting slurry to an initial temperature between approximately 140° F. to 160° F.; C. gradually adding sulfuric acid and additional oxide as needed into the slurry mixture maintaining: (1) approximate stoichiometric ratios between the two reactants; (2) the specific gravity of the slurry to reach an end point of between approximately 1.400 to 1.4700; (3) the pH of the slurry between approximately 1.3 to 1.9; and (4) the temperature of the reaction below approximately 220° F.; D. continuing to allow the oxides and acid to react for between approximately 3 to 5.5 hours at approximately atmospheric pressure; and E. removing the product.
Claim 2
Dependent Claim 155 words
A process for producing sulfates from by-product aluminum oxide wherein said sulfates contain no appreciable heavy metals, their oxides or sulfates selected from the group consisting of Cu, Cr, Mn and Pb comprising: A. feeding the aluminum oxide by-product and process-weak liquor into a digester vessel to form a slurry; B. heating the resulting slurry to an initial temperature between approximately 140° F. to 160° F.; C. gradually adding sulfuric acid and additional oxide as needed into the slurry mixture maintaining: (1) approximate stoichiometric ratios between the two reactants; (2) the specific gravity of the slurry to reach an end point of between approximately 1.400 to 1.4700; (3) the pH of the slurry between approximately 1.3 to 1.9; and (4) the temperature of the reaction below approximately 220° F.; D. continuing to allow the oxides and acid to react for between approximately 3 to 5.5 hours at approximately atmospheric pressure; and E. removing the product.
Claim 3
Dependent Claim 16 words
The process of claim 1 wherein a flocculating agent is added to the slurry while agitating.
Claim 4
Dependent Claim 15 words
The process of claim 1 wherein the reactants are batch injected into the digester vessel.
Claim 5
Dependent Claim 16 words
The process of claim 1 wherein excessive foaming during the reaction is controlled by water spraying.
Claim 6
Dependent Claim 14 words
The process of claim 1 wherein the reaction mixture is heated by steam injection.
Claim 7
Dependent Claim 12 words
The process of claim 1 wherein the product is removed by decanting.
Claim 8
Dependent Claim 24 words
The process of claim 6 wherein the slurry remaining in the digester after decanting of the product is processed for recovery of additional product.
Claim 9
Dependent Claim 63 words
The process of claim 7 wherein the slurry remaining in the digester vessel is: A. removed to wash tanks; B. washed with a weak product liquor followed by agitation, flocculation, settlement and decantation; and C. separated from the weak process liquor whereupon the remaining slurry is washed with fresh water and the mixture agitated, flocculated, settled and decanted and the wash liquor recovered.
Claim 10
Dependent Claim 24 words
The process of claim 8 wherein the weak liquor product is added to the digester vessel for dilution purposes during the initial reaction phase.
Claim 11
Dependent Claim 38 words
The process of claim 1 for producing aluminum ammonium sulfate, said process further comprising submerging a device having a cooled surface into the digester vessel onto which the product may crystallize and removing, washing and stripping the crystals.
Claim 12
Dependent Claim 17 words
The process of claim 1 wherein the reactants are added and product removed in a continuous mode.
Claim 13
Dependent Claim 208 words
A process for producing the binary salt aluminum ammonium sulfate and liquid aluminum sulfate wherein said binary salt contains no appreciable heavy metals, their oxides or sulfates selected form the group consisting of Cu, Cr, Mn and Pb comprising: A. feeding the aluminum oxide by-product having a high nitride content and process-weak liquor into a digester vessel to form a slurry; B. heating the resultant slurry to an initial temperature between approximately 140° F. to 160° F.; C. gradually adding sulfuric acid and additional oxide as needed into the slurry mixture maintaining: (1) approximate stoichiometric ratios between the two reactants; (2) the specific gravity of the slurry to reach an end point between approximately 1.400 to 1.4700; (3) the pH of the slurry between 1.3 to 1.9; and (4) the temperature of the reaction below approximately 220° F.; D. after the reaction has gone substantially to completion, adding flocculant and allowing the mixture to at least partially settle; E. submerging a device having a cool surface area into the vessel containing the product mixture; F. crystallizing the binary salt on the cool surface; G. removing the device having a cool surface and removing, washing and stripping the crystals; and H. decanting the supernatent liquid aluminum sulfate product liquor.
Claim 14
Dependent Claim 208 words
A process for producing the binary salt aluminum ammonium sulfate and liquid aluminum sulfate wherein said binary salt contains no appreciable heavy metals, their oxides or sulfates selected form the group consisting of Cu, Cr, Mn and Pb comprising: A. feeding the aluminum oxide by-product having a high nitride content and process-weak liquor into a digester vessel to form a slurry; B. heating the resultant slurry to an initial temperature between approximately 140° F. to 160° F.; C. gradually adding sulfuric acid and additional oxide as needed into the slurry mixture maintaining: (1) approximate stoichiometric ratios between the two reactants; (2) the specific gravity of the slurry to reach an end point between approximately 1.400 to 1.4700; (3) the pH of the slurry between 1.3 to 1.9; and (4) the temperature of the reaction below approximately 220° F.; D. after the reaction has gone substantially to completion, adding flocculant and allowing the mixture to at least partially settle; E. submerging a device having a cool surface area into the vessel containing the product mixture; F. crystallizing the binary salt on the cool surface; G. removing the device having a cool surface and removing, washing and stripping the crystals; and H. decanting the supernatent liquid aluminum sulfate product liquor.
Claim 15
Dependent Claim 187 words
A process for producing sulfates from by-product aluminum oxide wherein said sulfates contain no appreciable heavy metals, their oxides or sulfates selected from the group consisting of Cu, Cr, Mn and Pb by a continuous mode operation comprising: A. feeding the aluminum oxide by-product and process-weak liquor into a first stage digester vessel to form a slurry; B. heating the resultant slurry to an initial temperature between approximately 140° F. to 160° F.; C. continuously feeding sulfuric acid and additional oxide as needed into the first digester stage maintaining: (1) approximate stoichiometric ratios between the two reactants; (2) the pH of the slurry between approximately 1.3 to 1.9; and (3) the temperature of the reaction below approximately 220° F.; D. providing for gravity overflow into successive digester stages necessary to complete the reaction in approximately 3.0 to 5.5 hours at approximately atmospheric pressure; E. maintaining the specific gravity of the slurry in the final stage between approximately 1.400 to 1.4700; F. diluting the product with product liquor; G. overflowing the slurry mixture to a liquid-solids separator; and H. decanting the product as a substantially clear supernatent liquid.
Claim 16
Dependent Claim 187 words
A process for producing sulfates from by-product aluminum oxide wherein said sulfates contain no appreciable heavy metals, their oxides or sulfates selected from the group consisting of Cu, Cr, Mn and Pb by a continuous mode operation comprising: A. feeding the aluminum oxide by-product and process-weak liquor into a first stage digester vessel to form a slurry; B. heating the resultant slurry to an initial temperature between approximately 140° F. to 160° F.; C. continuously feeding sulfuric acid and additional oxide as needed into the first digester stage maintaining: (1) approximate stoichiometric ratios between the two reactants; (2) the pH of the slurry between approximately 1.3 to 1.9; and (3) the temperature of the reaction below approximately 220° F.; D. providing for gravity overflow into successive digester stages necessary to complete the reaction in approximately 3.0 to 5.5 hours at approximately atmospheric pressure; E. maintaining the specific gravity of the slurry in the final stage between approximately 1.400 to 1.4700; F. diluting the product with product liquor; G. overflowing the slurry mixture to a liquid-solids separator; and H. decanting the product as a substantially clear supernatent liquid.
Claim 17
Dependent Claim 27 words
The process of claim 13 wherein steam is injected in the digester stages if needed to maintain the slurry temperature between approximately 210° F. to 220° F.

References Cited (Backward Citations)

US1962498A Cited
US2273930A Cited
US3079228A Cited
US3425802A Cited
US3667905A Cited
US4160815A Cited
US4252776A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1985-06-28 1985-12-28 1986-06-29 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1989-06-28 1989-12-28 1990-06-29 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1993-06-28 1993-12-28 1994-06-29 $7700.00 Window Closed / Lapsed

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