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Fluorinated silica catalyst and preparation of aromatic/aliphatic nitriles in the presence thereof

Assignee: Rhone Poulenc Specialites Chimiques
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Filing: 1982-05-14
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Granted: 1985-03-12
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Expires: 2002-05-14
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Abstract

Abstract An improved fluorinated siliceous catalyst, well adapted for the catalytic synthesis of aromatic/aliphatic nitriles from their corresponding formamides, formanilides or amides, is comprised of a plurality of silica particulates, the specific surface of which ranging from about 200 to about 300 m2/g, having a total pore volume ranging from about 1 to about 1.5 cm3/g, with an average pore diameter ranging from about 100 to about 200 ANGSTROM , having an exchange pH of less than about 3, and with the fluorine content thereof bonded to the silica, expressed in F-, ranging from about 0.05 to about 2% by weight based upon the silica, and the sodium content thereof, expressed as Na2O, being less than about 1% by weight, also based upon the silica.

Inventors

  • 👤 Roland Jacques
  • 👤 Michel Reppelin
  • 👤 Laurent Seigneurin

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-09 02:54
CPC Classifications
B; B01; B01J; B01J21/00; B01J21/06; B01J21/08; B01J27/00; B01J27/06; B01J27/08; B01J27/12; B01J35/00; B01J35/60; B01J35/61; B01J35/615; B01J35/63; B01J35/638; B01J35/64; B01J35/647; C; C01; C01B; C01B33/00; C01B33/113; C01B33/12; C01B33/14; C01B33/152; C01B33/154; C07; C07C; C07C253/00; C07C253/20

Claims Analysis

Total Claims: 11
Claim 1
Independent Claim 229 words
A process for the preparation of the fluorinated siliceous catalyst comprising (i) adding an aqueous solution of sodium silicate to an aqueous solution of hydrofluoric acid, the temperatures of said solutions ranging from about -5° C. to about 15° C.; (ii) maintaining an amount of SiO 2 in the resulting reaction medium of less than about 15% by weight thereof, until the pH of said reaction medium attains a value of from about 3 to about 4.5; (iii) next permitting the mixture of reaction to gel, and comminuting the hydrogel which results into grain particles; then (iv) washing said grain particles to eliminate the soluble fluoride values therefrom; and (v) drying said washed grain particles at a temperature ranging from about 150° C. to 600° C.; said catalyst having a specific surface ranging from about 200 to about 300 m 2 /g, having a total pore volume ranging from about 1 to about 1.5 cm 3 /g, with an average pore diameter ranging from about 100 to about 200 Å, having an exchange pH of less than about 3 and with the fluorine content thereof bonded to the silica, expressed in F - , ranging from about 0.05 to about 2% by weight based upon the silica, and the sodium content thereof, expressed as Na 2 O, being less than about 1% by weight also based upon the silica.
Claim 2
Dependent Claim 229 words
A process for the preparation of the fluorinated siliceous catalyst comprising (i) adding an aqueous solution of sodium silicate to an aqueous solution of hydrofluoric acid, the temperatures of said solutions ranging from about -5° C. to about 15° C.; (ii) maintaining an amount of SiO 2 in the resulting reaction medium of less than about 15% by weight thereof, until the pH of said reaction medium attains a value of from about 3 to about 4.5; (iii) next permitting the mixture of reaction to gel, and comminuting the hydrogel which results into grain particles; then (iv) washing said grain particles to eliminate the soluble fluoride values therefrom; and (v) drying said washed grain particles at a temperature ranging from about 150° C. to 600° C.; said catalyst having a specific surface ranging from about 200 to about 300 m 2 /g, having a total pore volume ranging from about 1 to about 1.5 cm 3 /g, with an average pore diameter ranging from about 100 to about 200 Å, having an exchange pH of less than about 3 and with the fluorine content thereof bonded to the silica, expressed in F - , ranging from about 0.05 to about 2% by weight based upon the silica, and the sodium content thereof, expressed as Na 2 O, being less than about 1% by weight also based upon the silica.
Claim 3
Dependent Claim 24 words
The process as defined by claim 1, the sodium silicate comprising SiO 2 and Na 2 O in a molar ratio of about 3.
Claim 4
Dependent Claim 24 words
The process as defined by claim 1, comprising employing from about 1 to about 1.5 mole of HF per mole of SiO 2 .
Claim 5
Dependent Claim 20 words
The process as defined by claim 1, said grain particles having an average diameter of from 2 to 6 mm.
Claim 6
Dependent Claim 23 words
The process as defined by claim 1, said washing (iv) being with water, the pH of which ranging from about 7 to 10.
Claim 7
Dependent Claim 26 words
The process as defined by claim 5, the amount of SiO 2 in the reaction medium being maintained at less than about 10% by weight thereof.
Claim 8
Dependent Claim 24 words
The process as defined by claim 5, the concentrations of said silicate and HF solutions both ranging from about 40 to 50% by weight.
Claim 9
Dependent Claim 22 words
The process as defined by claim 1, wherein a reaction medium soluble organic carboxylic acid is added simultaneously with the hydrofluoric acid.
Claim 10
Dependent Claim 27 words
The process as defined by claim 8, wherein the molar ratio of the carboxylic acid added to the hydrofluoric acid ranges from about 0.05 to about 0.15.
Claim 11
Dependent Claim 13 words
The process as defined by claim 9, said carboxylic acid being acetic acid.

References Cited (Backward Citations)

US2386810A Cited
US2483868A Cited
US2516967A Cited
US2794002A Cited
US3494875A Cited
US4436669A Cited
US4438042A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1988-03-11 1988-09-10 1989-03-12 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1992-03-11 1992-09-10 1993-03-12 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1996-03-11 1996-09-10 1997-03-12 $7700.00 Window Closed / Lapsed

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