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US4837000A Expired / Lapsed US ⏱️ 0.0 years remaining

Crystalline silicates and process for the production thereof

Assignee: Research Association for Petroleum Alternatives Development
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Filing: 1986-12-11
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Granted: 1989-06-06
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Expires: 2006-12-11
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Abstract

Abstract Crystalline silicates and processes for the production thereof are described. These crystalline silicates are of new crystalline structure, which, as determined after calcination in the air at 550° C., have a composition represented by the general formula (I): pM 2/n O.Al 2 O 3 .qSiO 2 (the symbols are as defined in the appended claims) and give a X-ray diffraction pattern as shown in Table 2. They are superior in heat resistance and acid resistance, and can be used as catalysts for the conversion of various organic compounds, absorbents, or as catalysts for various reactions. They are produced by reacting an aqueous mixture comprising (a) a silica source, (b) an alumina source, (c) an alkali metal and/or alkaline earth metal source, and monoethanolamine at a temperature of 100° to 300° C. until the desired crystalline silicates are formed. Although monoethanolamine does not remain in the crystalline silicates, it plays an important role in the formation of the desired crystalline structure in the course of the production thereof.

Inventors

  • 👤 Kozo Takatsu
  • 👤 Noboru Kawata

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-01 19:47
CPC Classifications
B; B01; B01J; B01J29/00; B01J29/04; B01J29/06; B01J29/70; C; C01; C01B; C01B33/00; C01B33/20; C01B33/26; C01B33/28; C01B33/2807; C01B33/2869; C01B39/00; C01B39/02; C01B39/46; C01B39/48; C07; C07C; C07C1/00; C07C1/20; C07C2529/00; C07C2529/04; C07C2529/06; Y; Y02; Y02P; Y02P30/00; Y02P30/20; Y02P30/40; Y10; Y10S; Y10S423/00; Y10S423/36

Claims Analysis

Total Claims: 12
Claim 1
Independent Claim 208 words
A process for producing a crystalline silicate, when determined after calcination in the air at 550° C., having a composition represented by the general formula (I), pM.sub.2/n O.Al.sub.2 O.sub.3.qSiO.sub.2 (I) wherein M represents at least one element selected from hydrogen, alkali metals, and alkaline earth metals, n represents the valence of M, and p and q are chosen within the ranges of 0.3≦p≦3.0, q≦10, and giving a principal X-ray diffraction pattern as shown in Table 1, below: TABLE 1 ______________________________________ Lattice Spacing d (Å) Relative Intensity ______________________________________ 11.31 ± 0.2 strong 10.92 ± 0.2 very strong 7.83 ± 0.2 medium 4.51 ± 0.15 very strong 4.24 ± 0.1 strong 3.89 ± 0.1 strong 3.73 ± 0.1 medium 3.69 ± 0.1 very strong 3.61 ± 0.1 very strong 3.53 ± 0.07 medium 3.43 ± 0.07 strong 2.52 ± 0.05 medium ______________________________________ which process consists essentially of reacting an aqueous mixture consisting essentially of (a) a silica source, (b) an alumina source, (c) an alkali metal and/or alkaline earth metal source, and (e) monoethanolamine in the following molar ratios: silica/alumina≧10/1 monoethanolamine/water=0.1/1 to 5/1, monoethanolamine/silica=2/1 to 100/1, hydroxyl ion/silica=0.01/1 to 0.5/1 excluding hydroxyl ions resulting from monoethanolamine, at a temperature of 100° to 300° C. until the crystalline silicate is formed.
Claim 2
Dependent Claim 208 words
A process for producing a crystalline silicate, when determined after calcination in the air at 550° C., having a composition represented by the general formula (I), pM.sub.2/n O.Al.sub.2 O.sub.3.qSiO.sub.2 (I) wherein M represents at least one element selected from hydrogen, alkali metals, and alkaline earth metals, n represents the valence of M, and p and q are chosen within the ranges of 0.3≦p≦3.0, q≦10, and giving a principal X-ray diffraction pattern as shown in Table 1, below: TABLE 1 ______________________________________ Lattice Spacing d (Å) Relative Intensity ______________________________________ 11.31 ± 0.2 strong 10.92 ± 0.2 very strong 7.83 ± 0.2 medium 4.51 ± 0.15 very strong 4.24 ± 0.1 strong 3.89 ± 0.1 strong 3.73 ± 0.1 medium 3.69 ± 0.1 very strong 3.61 ± 0.1 very strong 3.53 ± 0.07 medium 3.43 ± 0.07 strong 2.52 ± 0.05 medium ______________________________________ which process consists essentially of reacting an aqueous mixture consisting essentially of (a) a silica source, (b) an alumina source, (c) an alkali metal and/or alkaline earth metal source, and (e) monoethanolamine in the following molar ratios: silica/alumina≧10/1 monoethanolamine/water=0.1/1 to 5/1, monoethanolamine/silica=2/1 to 100/1, hydroxyl ion/silica=0.01/1 to 0.5/1 excluding hydroxyl ions resulting from monoethanolamine, at a temperature of 100° to 300° C. until the crystalline silicate is formed.
Claim 3
Dependent Claim 9 words
The process of claim 1, wherein M is sodium.
Claim 4
Dependent Claim 9 words
The process of claim 1, wherein M is potassium.
Claim 5
Dependent Claim 9 words
The process of claim 1, wherein M is calcium.
Claim 6
Dependent Claim 21 words
The process of claim 1, wherein said crystalline silicate has the formula 0.9Na 2 O.Al 2 O 3 .74.OSiO 2 .
Claim 7
Dependent Claim 251 words
A process for producing a crystalline silicate, when determined after calcination in the air at 550° C., having a composition represented by the general formula (I), pM.sub.2/n O.Al.sub.2 O.sub.3.qSiO.sub.2 (I) wherein M represents at least one element selected from hydrogen, alkali metals, and alkaline earth metals, n represents the valence of M, and p and q are chosen within the ranges of 0.3 p 3.0, q 10, and giving a principal X-ray diffraction pattern as shown below: ______________________________________ Lattice Spacing d (Å) Relative Intensity ______________________________________ 11.31 ± 0.2 strong 10.92 ± 0.2 very strong 10.03 ± 0.2 weak 7.83 ± 0.2 medium 6.08 ± 0.15 weak 5.61 ± 0.15 weak 5.24 ± 0.15 weak 4.90 ± 0.15 weak 4.51 ± 0.15 very strong 4.42 ± 0.1 weak 4.24 ± 0.1 strong 4.14 ± 0.1 weak 3.89 ± 0.1 strong 3.73 ± 0.1 medium 3.69 ± 0.1 very strong 3.61 ± 0.1 very strong 3.53 ± 0.07 medium 3.43 ± 0.07 strong 3.32 ± 0.07 weak 3.16 ± 0.07 weak 2.97 ± 0.07 weak 2.83 ± 0.05 weak 2.52 ± 0.05 medium ______________________________________ which process consists essentially of reacting an aqueous mixture consisting essentially of (a) a silica source, (b) an alumina source, (c) an alkali metal and/or alkaline earth metal source, and (e) monoethanolamine in the following molar ratios: silica/alumina 10/1 monoethanolamine/water=0.1/1 to 5/1 monoethanolamine/silica=2/1 to 100/1 hydroxyl ion/silica=0.01/1 to 0.5/1 excluding hydroxyl ions resulting from monoethanolamine at a temperature of 100° to 300° C. until the crystalline silicate is formed.
Claim 8
Dependent Claim 251 words
A process for producing a crystalline silicate, when determined after calcination in the air at 550° C., having a composition represented by the general formula (I), pM.sub.2/n O.Al.sub.2 O.sub.3.qSiO.sub.2 (I) wherein M represents at least one element selected from hydrogen, alkali metals, and alkaline earth metals, n represents the valence of M, and p and q are chosen within the ranges of 0.3 p 3.0, q 10, and giving a principal X-ray diffraction pattern as shown below: ______________________________________ Lattice Spacing d (Å) Relative Intensity ______________________________________ 11.31 ± 0.2 strong 10.92 ± 0.2 very strong 10.03 ± 0.2 weak 7.83 ± 0.2 medium 6.08 ± 0.15 weak 5.61 ± 0.15 weak 5.24 ± 0.15 weak 4.90 ± 0.15 weak 4.51 ± 0.15 very strong 4.42 ± 0.1 weak 4.24 ± 0.1 strong 4.14 ± 0.1 weak 3.89 ± 0.1 strong 3.73 ± 0.1 medium 3.69 ± 0.1 very strong 3.61 ± 0.1 very strong 3.53 ± 0.07 medium 3.43 ± 0.07 strong 3.32 ± 0.07 weak 3.16 ± 0.07 weak 2.97 ± 0.07 weak 2.83 ± 0.05 weak 2.52 ± 0.05 medium ______________________________________ which process consists essentially of reacting an aqueous mixture consisting essentially of (a) a silica source, (b) an alumina source, (c) an alkali metal and/or alkaline earth metal source, and (e) monoethanolamine in the following molar ratios: silica/alumina 10/1 monoethanolamine/water=0.1/1 to 5/1 monoethanolamine/silica=2/1 to 100/1 hydroxyl ion/silica=0.01/1 to 0.5/1 excluding hydroxyl ions resulting from monoethanolamine at a temperature of 100° to 300° C. until the crystalline silicate is formed.
Claim 9
Dependent Claim 9 words
The process of claim 6, wherein M is sodium.
Claim 10
Dependent Claim 9 words
The process of claim 6, wherein M is potassium.
Claim 11
Dependent Claim 9 words
The process of claim 6, wherein M is calcium.
Claim 12
Dependent Claim 21 words
The process of claim 6, wherein said crystalline silicate has the formula 0.9Na 2 O.Al 2 O 3 .74.OSiO 2 .

References Cited (Backward Citations)

US4242233A Cited
US4346021A Cited
US4407728A Cited
US4478806A Cited
US4377502A Cited
GB2114110A Cited
US4578259A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1992-06-05 1992-12-05 1993-06-06 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1996-06-05 1996-12-05 1997-06-06 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 2000-06-05 2000-12-05 2001-06-06 $7700.00 Window Closed / Lapsed

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