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US5049536A Expired / Lapsed US ⏱️ 0.0 years remaining

Catalytically active silica and alumina gel and process for preparing it

Assignee: Eni Tecnologie SpA
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Filing: 1989-04-28
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Granted: 1991-09-17
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Expires: 2009-04-28
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Abstract

Abstract A silica and alumina gel is disclosed, which is amorphous at X-rays, has a molar ratio of SiO 2 /Al 2 O 3 comprised within the range of from 30/1 to 500/1, a surface area comprised within the range of from 500 to 1000 m 2 /g, a total volume of pores comprised within the range of from 0.3 to 0.6 ml/g, an average diameter of the pores of the order of magnitude of 10 Å or less and which is free, or substantially free, from pores having a diameter larger than 30 Å. Such a silica and alumina gel is catalytically active in reactions of conversion of the hydrocarbons, such as: oligomerization, alkylation, isomerization and dewaxing. Also a process for preparing such a silica and alumina gel is disclosed.

Inventors

  • 👤 Giuseppe Bellussi
  • 👤 Mario G. Clerici
  • 👤 Angela Carati
  • 👤 Fabrizio Cavani

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-05 21:50
CPC Classifications
B; B01; B01J; B01J21/00; B01J21/12; B01J35/00; B01J35/60; B01J35/63; B01J35/64; B01J35/643; B01J37/00; B01J37/0009; B01J37/08; C; C07; C07C; C07C2/00; C07C2/02; C07C2/04; C07C2/06; C07C2/08; C07C2/10; C07C2521/00; C07C2521/12

Claims Analysis

Total Claims: 13
Claim 1
Independent Claim 221 words
Silica and alumina gel, which is amorphous at X-rays, has a molecular ratio of SiO 2 /Al 2 O 3 comprised within the range of from 30/1 to 500/1, a surface area comprised within the range of from 500 to 1000 m 2 /g, a total volume of pores comprised within the range of from 0.3 to 0.6 ml/g, an average diameter of the pores of the order of magnitude of 10 Å or less and is free, or substantially free, from pores having a diameter larger than 30 Å, obtained by: (a) preparing an aqueous solution of tetra-alkyl-ammonium hydroxide (TAA-OH) in which the alkyl is selected from among ethyl, n.-propyl and n.-butyl, of a soluble compound of aluminum capable of yielding Al 2 O 3 by hydrolysis and of a soluble silicon compound capable of yielding SiO 2 by hydrolysis; with the amount of the constituents of the solution being such as to comply with the following values of the following molar ratios: ______________________________________ SiO.sub.2 /Al.sub.2 O.sub.3 from 30:1 to 500:1; TAA--OH/SiO.sub.2 from 0.05:1 to 0.2:1; H.sub.2 O/SiO.sub.2 from 5:1 to 40:1; ______________________________________ (b) heating the so-obtained solution in order to cause the gelification to occur; (c) drying the obtained gel; and (d) calcining the dried gel, by operating first under an inert atmosphere and then under an oxidating atmosphere.
Claim 2
Dependent Claim 221 words
Silica and alumina gel, which is amorphous at X-rays, has a molecular ratio of SiO 2 /Al 2 O 3 comprised within the range of from 30/1 to 500/1, a surface area comprised within the range of from 500 to 1000 m 2 /g, a total volume of pores comprised within the range of from 0.3 to 0.6 ml/g, an average diameter of the pores of the order of magnitude of 10 Å or less and is free, or substantially free, from pores having a diameter larger than 30 Å, obtained by: (a) preparing an aqueous solution of tetra-alkyl-ammonium hydroxide (TAA-OH) in which the alkyl is selected from among ethyl, n.-propyl and n.-butyl, of a soluble compound of aluminum capable of yielding Al 2 O 3 by hydrolysis and of a soluble silicon compound capable of yielding SiO 2 by hydrolysis; with the amount of the constituents of the solution being such as to comply with the following values of the following molar ratios: ______________________________________ SiO.sub.2 /Al.sub.2 O.sub.3 from 30:1 to 500:1; TAA--OH/SiO.sub.2 from 0.05:1 to 0.2:1; H.sub.2 O/SiO.sub.2 from 5:1 to 40:1; ______________________________________ (b) heating the so-obtained solution in order to cause the gelification to occur; (c) drying the obtained gel; and (d) calcining the dried gel, by operating first under an inert atmosphere and then under an oxidating atmosphere.
Claim 3
Dependent Claim 34 words
Silica and alumina gel according to claim 1, characterized in that the soluble compound in the (a) step is aluminum tri-alkoxide and the soluble silicon compound in the (a) step is a tetra-alkyl silicate.
Claim 4
Dependent Claim 29 words
Silica and alumina gel according to claim 2, characterized in that said soluble aluminum compound is aluminum tri-n.-propoxide or aluminum tri-isopropoxide and said soluble silicon compound is tetra-ethyl silicate.
Claim 5
Dependent Claim 53 words
Silica and alumina gel according to claim 1, characterized in that the constituents of the solution in the (a) step are in such an amount as to comply with the following molar ratios: ______________________________________ SiO.sub.2 /Al.sub.2 O.sub.3 from 50:1 to 300:1 TAA--OH/SiO.sub.2 from 0.05:1 to 0.2:1 H.sub.2 O/SiO.sub.2 from 10:1 to 25:1 ______________________________________
Claim 6
Dependent Claim 48 words
Silica and alumina gel according to claim 1, characterized in that in said (a) step the reaction is carried out at a temperature comprised within the range of from room temperature ( 20°-25° C.) up to values close to those at which the gelification begins (about 50° C.).
Claim 7
Dependent Claim 50 words
Silica and alumina gel according to claim 1, characterized in that said gelification in the (b) step is carried out at a temperature comprised within the range of from 50° C. up to 70° C., for a time comprised within the range of from 15 minutes up to 5 hours.
Claim 8
Dependent Claim 33 words
Silica and alumina gel according to claim 6, characterized in that said gelification is carried out at a temperature of 60° C., for a time of the order of magnitude of 25-60 minutes.
Claim 9
Dependent Claim 25 words
Silica and alumina gel according to claim 1, characterized in that the (c) drying step is carried out at temperatures of up to 150° C.
Claim 10
Dependent Claim 28 words
Silica and alumina gel according to claim 8, characterized in that said (c) drying step is carried out at temperatures of the order of magnitude of 90°-100° C.
Claim 11
Dependent Claim 20 words
Silica and alumina gel according to claim 1, characterized in that said (c) drying step is carried out by spray-drying.
Claim 12
Dependent Claim 40 words
Silica and alumina gel according to claim 1, characterized in that the (d) calcination step is carried out at a temperature comprised within the range of from 500° to 700° C., for a time of from 4 to 20 hours.
Claim 13
Dependent Claim 30 words
Silica and alumina gel according to claim 11, characterized in that said (d) calcination step is carried out at about 550°-600° C., and for a time of about 6-16 hours.

References Cited (Backward Citations)

US3535232A Cited
US3923691A Cited
US4766101A Cited
EP0225407A1 Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1994-09-16 1995-03-18 1995-09-17 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1998-09-16 1999-03-18 1999-09-17 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 2002-09-16 2003-03-18 2003-09-17 $7700.00 Window Closed / Lapsed

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