US3976759A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Process for removal of fluoride compounds from spent alkylation catalyst
Assignee: Texaco Inc
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Filing: 1974-12-30
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Granted: 1976-08-24
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Expires: 1994-12-30
Abstract
Abstract A process for removal of fluoride compounds from spent alkylation catalyst containing fluorosulfonic acid and sulfuric acid wherein hydrogen fluoride and fluorosulfonic acid, in the presence of water, are removed by vacuum distillation following which the remaining sulfuric acid rich fraction of the spent catalyst is reacted with a silica containing material to convert most of the remaining residual hydrogen fluoride to silicon fluoride which is volatilized from the mixture to thereby provide a sulfuric acid effluent free of substantial amounts of fluoride compounds. The hydrogen fluoride recovered is reacted with sulfur trioxide to form fresh fluorosulfonic acid which is combined with sulfuric acid to provide fresh alkylation catalyst.
Inventors
- 👤 Richard H. Bennett
- 👤 James W. Brockington
- 👤 Lloyd E. Line, Jr.
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-30 21:31
CPC Classifications
B; B01; B01J; B01J27/00; B01J27/28; B01J27/32
Claims Analysis
Total Claims: 14
Claim 1
Independent Claim
221 words
A process for removal of fluoride compounds from spent alkylation catalyst containing fluorosulfonic acid, organofluoro compounds, and sulfuric acid comprising: a. subjecting said spent catalyst to distillation, at atmospheric pressure or below, at a temperature in the range of from about 50° to about 120°C. and in admixture with at least the stoichiometric amount of water necessary to hydrolyze said fluorosulfonic acid to hydrogen fluoride and for a period of time sufficient to effect at least partial decomposition of at least some organofluoro compounds in said spent catalyst into hydrogen fluoride and/or fluorosulfonic acid; b. recovering a first fraction from said distillation, said first fraction comprising primarily hydrogen fluoride; c. recovering a second fraction from said distillation, said second fraction comprising residual hydrogen fluoride and the greater part of said sulfuric acid present in said spent catalyst; d. contacting, in a reaction zone, said second fraction with a silica containing material in an amount and for a period of time sufficient to react at least a portion of said residual hydrogen fluoride with said silica to form silicon fluoride; e. volatilizing said silicon fluoride from said reaction zone; and f. recovering from said reaction zone an effluent acid fraction containing the greater part of said sulfuric acid present in said spent catalyst and being free of substantial amounts of fluoride compounds.
Claim 2
Dependent Claim
221 words
A process for removal of fluoride compounds from spent alkylation catalyst containing fluorosulfonic acid, organofluoro compounds, and sulfuric acid comprising: a. subjecting said spent catalyst to distillation, at atmospheric pressure or below, at a temperature in the range of from about 50° to about 120°C. and in admixture with at least the stoichiometric amount of water necessary to hydrolyze said fluorosulfonic acid to hydrogen fluoride and for a period of time sufficient to effect at least partial decomposition of at least some organofluoro compounds in said spent catalyst into hydrogen fluoride and/or fluorosulfonic acid; b. recovering a first fraction from said distillation, said first fraction comprising primarily hydrogen fluoride; c. recovering a second fraction from said distillation, said second fraction comprising residual hydrogen fluoride and the greater part of said sulfuric acid present in said spent catalyst; d. contacting, in a reaction zone, said second fraction with a silica containing material in an amount and for a period of time sufficient to react at least a portion of said residual hydrogen fluoride with said silica to form silicon fluoride; e. volatilizing said silicon fluoride from said reaction zone; and f. recovering from said reaction zone an effluent acid fraction containing the greater part of said sulfuric acid present in said spent catalyst and being free of substantial amounts of fluoride compounds.
Claim 3
Dependent Claim
20 words
The process of claim 1 wherein said distillation is conducted under conditions affording increased surface area of said spent catalyst.
Claim 4
Dependent Claim
32 words
The process of claim 1 wherein said distillation is conducted at a pressure of about 1 psia or lower and a temperature in the range of from about 80° to about 110°C.
Claim 5
Dependent Claim
23 words
The process of claim 3 wherein said distillation is conducted in the presence of from about 3 to about 8% by weight water.
Claim 6
Dependent Claim
23 words
The process of claim 3 wherein said distillation is conducted in the presence of from about 8 to about 15% by weight water.
Claim 7
Dependent Claim
45 words
The process of claim 5 wherein said spent catalyst is subjected to said distillation at a temperature of about 100°C. and for a period of time such that said second fraction has a fluoride content of about 100 ppmw or less calculated as hydrogen fluoride.
Claim 8
Dependent Claim
22 words
The process of claim 3 wherein said spent catalyst is subjected to said distillation for a period of 4 hours or greater.
Claim 9
Dependent Claim
32 words
The process of claim 3 wherein said distillation of said spent catalyst is conducted at a temperature of about 100°C. in admixture with from about 8 to about 15% by weight water.
Claim 10
Dependent Claim
31 words
The process of claim 1 wherein said contacting in said reaction zone is conducted at a temperature in the range of from about 50° to about 120°C. and at subatmospheric pressure.
Claim 11
Dependent Claim
20 words
The process of claim 9 wherein said contacting is carried out for a period of about 4 hours or greater.
Claim 12
Dependent Claim
33 words
The process of claim 9 wherein said silica containing material has a silica content, by weight, of about at least the stoichometric amount necessary to convert said residual hydrogen fluoride to silicon fluoride.
Claim 13
Dependent Claim
19 words
The process of claim 11 wherein said contacting is conducted at a pressure of about 1 psia or lower.
Claim 14
Dependent Claim
62 words
The process of claim 8 wherein said contacting in said reaction zone is conducted at a temperature of about 90° to about 110°C., at a pressure of about 1 psia or lower, in the presence of a silica containing material having a silica content, by weight, of at least the stoichometric amount necessary to convert said residual hydrogen fluoride to silicon fluoride.
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) | 1979-08-24 | 1980-02-23 | 1980-08-24 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1983-08-24 | 1984-02-23 | 1984-08-24 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1987-08-24 | 1988-02-23 | 1988-08-24 | $7700.00 | Window Closed / Lapsed |