Patent US4954326A successfully refreshed from Google Patents.
← Back to Patent Explorer
US4954326A Expired / Lapsed US ⏱️ 0.0 years remaining

Preparation of crystalline aluminosilicate zeolite, and its product

Assignee: Teijin Petrochemical Industries Ltd
•
Filing: 1989-07-12
•
Granted: 1990-09-04
•
Expires: 2009-07-12
📄 Original PDF 🌐 Google Patents 🔄 Sync Now

Abstract

Abstract A process for producing a crystalline aluminosilicate zeolite characterized by having (a) a silica/alumina mole ratio of from 10 to 100, (b) X-ray lattice distances d shown in Table A of the specification, and (c) a specific n-hexane adsorption, under limited measuring conditions, of at least 0.07 g/g, which comprises maintaining a silica source, an alumina source, and a zeolite selected from zeolites ZSM-5 and zeolites having said characteristics, in an aqueous solution containing 1 to 200 millimoles, per gram of said zeolite, of an alkali metal hydroxide under such temperature, pressure and time conditions as to produce a crystalline aluminosilicate zeolite; and a crystalline aluminosilicate zeolite characterized by having aforesaid properties (a) to (c) and (d) a (2-methylpentane/cyclohexane) adsorption ratio of from 1.1 to 1.6.

Inventors

  • 👤 Tamio Onodera
  • 👤 Tokuji Sakai
  • 👤 Yasuo Yamasaki
  • 👤 Koji Sumitani

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-08 02:07
CPC Classifications
C; C07; C07C; C07C6/00; C07C6/08; C07C6/12; C07C6/126; C01; C01B; C01B39/00; C01B39/02; C01B39/36; C01B39/38; C07C4/00; C07C4/08; C07C4/12; C07C4/14; C07C4/18; C07C2529/00; C07C2529/04; C07C2529/06; Y; Y02; Y02P; Y02P20/00; Y02P20/50; Y02P20/52

Claims Analysis

Total Claims: 15
Claim 1
Independent Claim 231 words
A process for producing a crystalline aluminosilicate zeolite characterized by having (a) a silica/alumina mole ratio of from 10 to 100, (b) X-ray lattice distances d shown in Table A of the specification, (c) a specific n-hexane adsorption, as measured on a precisely weighed sample of the zeolite which has been calcined at 450° for 8 hours until the pressure reaches 50±1 mm Hg, and maintained at 20±1° C. for 2 hours of at least 0.07 g/g, (d) a (2-methylpentane/cyclohexane) adsorption ratio of from 1.2 to 1.6, and (e) when the intensity (I o ) of the X-ray diffraction peak at d(Å)=3.86 is taken as 100, the relative intensity (I/I o ) of the X-ray diffraction peak at d(Å)=3.83 is at least 70, which comprises maintaining a silica source, an alumina source, and a seed zeolite selected from the group consisting of zeolite ZSM-5 and zeolites having said characteristics (a)-(e) inclusive, specified above, in an aqueous solution containing 1 to 200 millimoles, per gram of said zeolite, of an alkali metal hydroxide, in such proportions that the silica source, the alumina source and the alkali metal hydroxide satisfy the following mole ratios in terms of SiO 2 , Al 2 O 3 and OH-: SiO.sub.2 /Al.sub.2 O.sub.3 =5-100 OH-/(SiO.sub.2 +Al.sub.2 O.sub.3 =about 0.5-1 and OH-/H.sub.2 O=0.005-0.05, and under such temperature, pressure and time conditions as to produce a crystalline aluminosilicate zeolite.
Claim 2
Dependent Claim 231 words
A process for producing a crystalline aluminosilicate zeolite characterized by having (a) a silica/alumina mole ratio of from 10 to 100, (b) X-ray lattice distances d shown in Table A of the specification, (c) a specific n-hexane adsorption, as measured on a precisely weighed sample of the zeolite which has been calcined at 450° for 8 hours until the pressure reaches 50±1 mm Hg, and maintained at 20±1° C. for 2 hours of at least 0.07 g/g, (d) a (2-methylpentane/cyclohexane) adsorption ratio of from 1.2 to 1.6, and (e) when the intensity (I o ) of the X-ray diffraction peak at d(Å)=3.86 is taken as 100, the relative intensity (I/I o ) of the X-ray diffraction peak at d(Å)=3.83 is at least 70, which comprises maintaining a silica source, an alumina source, and a seed zeolite selected from the group consisting of zeolite ZSM-5 and zeolites having said characteristics (a)-(e) inclusive, specified above, in an aqueous solution containing 1 to 200 millimoles, per gram of said zeolite, of an alkali metal hydroxide, in such proportions that the silica source, the alumina source and the alkali metal hydroxide satisfy the following mole ratios in terms of SiO 2 , Al 2 O 3 and OH-: SiO.sub.2 /Al.sub.2 O.sub.3 =5-100 OH-/(SiO.sub.2 +Al.sub.2 O.sub.3 =about 0.5-1 and OH-/H.sub.2 O=0.005-0.05, and under such temperature, pressure and time conditions as to produce a crystalline aluminosilicate zeolite.
Claim 3
Dependent Claim 12 words
The process of claim 1 wherein the seed zeolite is zeolite ZSM-5.
Claim 4
Dependent Claim 30 words
The process of claim 1 or 2 wherein the amount of the alkali metal hydroxide in the aqueous solution is 5 to 100 millimoles per gram of the seed zeolite.
Claim 5
Dependent Claim 17 words
The process of claim 1 wherein the alkali metal hydroxide is sodium hydroxide, potassium hydroxide, or both.
Claim 6
Dependent Claim 43 words
The process of claim 1 wherein the proportions of the silica source and the alumina source are such that 0.1 to 200 millimoles of SiO 2 and 0.01 to 20 millimoles of Al 2 O 3 are used per gram of seed zeolite.
Claim 7
Dependent Claim 44 words
The process of claim 5 wherein the proportions of the silica source and the alumina source are such that 1 to 100 millimoles of SiO 2 and 0.1 to 10 millimoles of Al 2 O 3 are used per gram of the seed zeolite.
Claim 8
Dependent Claim 27 words
The process of claim 1 wherein the silica source is selected from the group consisting of a silica powder, colloidal silica, water-soluble silicon compounds and silica acid.
Claim 9
Dependent Claim 25 words
The process of claim 1 wherein the alumina source is selected from the group consisting of alumina, mineral acid salts of aluminum and aluminate salts.
Claim 10
Dependent Claim 18 words
The process of claim 1 wherein the aluminosilicate is used as a common source of silica and alumina.
Claim 11
Dependent Claim 17 words
The process of claim 1 wherein the temperature is in the range of 90° to 250° C.
Claim 12
Dependent Claim 17 words
The process of claim 1 wherein the pressure is at least the autogenous pressure in an autoclave.
Claim 13
Dependent Claim 65 words
The process of claim 1 wherein the proportions of the silica source, the alumina source and the alkali metal hydroxide are such that the SiO 2 /Al 2 O 3 mole ratio is from 10 to 80, the OH-(SiO 2 +Al 2 O 3 ) mole ratio is from about 0.5 to 1 and the OH-/H 2 O mole ratio is from 0.01 to 0.04.
Claim 14
Dependent Claim 16 words
The process of claim 1 wherein the relative intensity (I/I o ) is 73 to 78.
Claim 15
Dependent Claim 21 words
The process of claim 13 wherein the crystalline aluminosilicate zeolite product has a (2-methylpentane/cyclohexane) adsorption ratio of from 1.25 to 1.45.

References Cited (Backward Citations)

US3702886A Cited
US4175114A Cited
NL7512644A Cited
NL7512645A Cited
US4257885A Cited
US4275047A Cited
US4420467A Cited
US4524055A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1993-09-03 1994-03-05 1994-09-04 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1997-09-03 1998-03-05 1998-09-04 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 2001-09-03 2002-03-05 2002-09-04 $7700.00 Window Closed / Lapsed

Assigned Categories & Tags

No categories assigned to this patent yet.

Assign Category Tag