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US4005176A
Expired / Lapsed
US
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Process for the recovery of antimony pentachloride from used catalyst solutions
Assignee: Kali Chemie AG
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Filing: 1975-08-14
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Granted: 1977-01-25
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Expires: 1995-08-14
Abstract
Abstract Disclosed is a process for the recovery of antimony pentachloride from catalyst solutions used in the fluorination of chlorinated hydrocarbons characterized in that the exhausted catalyst solution containing antimony ions and high boiling halogenated hydrocarbons is chlorinated to convert the Sb 3 + to Sb 5 + followed by treatment of the solution with hydrogen fluoride to give SbCl x F y compounds, wherein x is 4-2 and y is 1-3, the sum of x+y being 5, and to convert the high boiling halogenated hydrocarbons to lower boiling halogenated hydrocarbons, thereafter removing the halogenated hydrocarbons having a lower boiling temperature than the boiling point of SbCl x F y and converting the remaining SbCl x F y compound with carbon tetrachloride to form antimony pentachloride which is thereafter separated from the remaining organic compounds and inorganic residue.
Inventors
- 👤 Gunter Fernschild
- 👤 Werner Rudolph
- 👤 Joachim Massonne
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-05 10:46
CPC Classifications
B; B01; B01J; B01J27/00; B01J27/28; B01J27/32; C; C01; C01G; C01G30/00; C01G30/006; C01G30/007; Y; Y02; Y02P; Y02P20/00; Y02P20/50; Y02P20/584
Claims Analysis
Total Claims: 14
Claim 1
Independent Claim
121 words
A process for the recovery of antimony pentachloride from used catalyst solution comprising: a. chlorinating used catalyst solution containing Sb 3 + and high boiling halogen-containing hydrocarbons to convert said Sb 3 + to Sb 5 + ; b. reacting said solution with hydrogen fluoride to give SbCl x F y wherein x is 4-2 and y is 1-3, the sum of x and y being 5, and fluorinated lower boiling hydrocarbons; c. removing said fluorinated lower boiling hydrocarbons having lower boiling temperatures than said SbCl x F y compounds from said solution by distillation; d. reacting said SbCl x F y compounds with carbon tetrachloride to SbCl 5 ; and e. separating said SbCl 5 from said solution by distillation.
Claim 2
Dependent Claim
121 words
A process for the recovery of antimony pentachloride from used catalyst solution comprising: a. chlorinating used catalyst solution containing Sb 3 + and high boiling halogen-containing hydrocarbons to convert said Sb 3 + to Sb 5 + ; b. reacting said solution with hydrogen fluoride to give SbCl x F y wherein x is 4-2 and y is 1-3, the sum of x and y being 5, and fluorinated lower boiling hydrocarbons; c. removing said fluorinated lower boiling hydrocarbons having lower boiling temperatures than said SbCl x F y compounds from said solution by distillation; d. reacting said SbCl x F y compounds with carbon tetrachloride to SbCl 5 ; and e. separating said SbCl 5 from said solution by distillation.
Claim 3
Dependent Claim
26 words
The process as defined by claim 1 wherein chlorinating step (a) is carried out at temperatures of about 20°-40° C and pressures of about 1-2.5 atmospheres.
Claim 4
Dependent Claim
25 words
The process as defined by claim 1 wherein step (b) is carried out at temperatures of about 20°-140° C and pressures of about 1-6 atmospheres.
Claim 5
Dependent Claim
25 words
The process as defined by claim 1 wherein step (b) is carried out at temperatures of about 20°-100° C and pressures of about 1-4 atmospheres.
Claim 6
Dependent Claim
31 words
The process as defined by claim 3 wherein said reaction with hydrogen fluoride is carried out first at a temperature of about 20° C then slowly raised to about 60°-80° C.
Claim 7
Dependent Claim
28 words
The process as defined by claim 1 wherein step (c) is carried out by vacuum distillation at temperatures of about 20°-100° C and pressures of about 20-100 Torr.
Claim 8
Dependent Claim
28 words
The process as defined by claim 1 wherein step (c) is carried out by vacuum distillation at temperatures of about 50°-80° C and pressures of about 20-60 Torrs.
Claim 9
Dependent Claim
26 words
The process as defined by claim 1 wherein reacting step (d) is carried out at temperatures of about 50°-120° C and pressures of about 1-5 atmospheres.
Claim 10
Dependent Claim
26 words
The process as defined by claim 1 wherein reacting step (d) is carried out at temperatures of about 60°-80° C and pressures of about 2-3 atmospheres.
Claim 11
Dependent Claim
29 words
The process as defined by claim 1 wherein separating step (e) is carried out by vacuum distillation at temperatures of about 50°-80° C and pressures of about 20-60 Torrs.
Claim 12
Dependent Claim
38 words
The process as defined by claim 1 further comprising adding at the end of the distillation of step (e) CCl 4 and Cl 2 to convert SbCl 3 received by reduction in the distillation to SbCl 5 .
Claim 13
Dependent Claim
30 words
The process as defined by claim 1 further comprising treatment of the distillate resulting from step (c) with alkali hydroxide solution and recovery of precipitated alkali antimonate from said distillate.
Claim 14
Dependent Claim
28 words
The process as defined by claim 1 further comprising: f. treating the distillation residue of step (e) with alkali hydroxide solution, and g. recovering the precipitated alkali antimonate.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1980-01-25 | 1980-07-26 | 1981-01-25 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1984-01-25 | 1984-07-26 | 1985-01-25 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1988-01-25 | 1988-07-26 | 1989-01-25 | $7700.00 | Window Closed / Lapsed |