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US5300277A
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Synthesis of mesoporous crystalline material
Assignee: Mobil Oil AS
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Filing: 1992-10-21
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Granted: 1994-04-05
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Expires: 2012-10-21
Abstract
Abstract This invention relates to an improvement in the method for synthesis of a new synthetic composition of porous crystalline material. The new crystalline material exhibits a large sorption capacity demonstrated by its benzene adsorption capacity of greater than about 10 grams benzene/100 grams at 50 torr and 25 degrees C. and a particular, unique X-ray diffraction pattern.
Inventors
- 👤 Charles T. Kresge
- 👤 Wielsaw J. Roth
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-03 16:01
CPC Classifications
B; B01; B01J; B01J29/00; B01J29/82; B01J29/83; B01D; B01D53/00; B01D53/34; B01D53/74; B01D53/86; B01D53/8621; B01D53/8625; B01D53/8628; B01J20/00; B01J20/02; B01J20/04; B01J20/041; B01J20/06; B01J20/08; B01J20/10; B01J20/103; B01J20/12; B01J20/16; B01J20/18; B01J20/22; B01J20/223; B01J29/03; B01J29/0308; B01J29/035; B01J29/04; B01J29/041; B01J29/06; B01J29/40; B01J29/70; B01J29/84; B01J29/85; C; C01; C01B; C01B37/00; C01B37/02; C01B37/06; C01B37/08; C01B39/00; C10; C10G; C10G11/00; C10G11/02; C10G11/04; C10G11/05; C10G47/00; C10G47/02; C10G47/10; C10G47/12; C10G47/16; B01J2229/00; B01J2229/10; B01J2229/26; B01J2229/30; B01J2229/32; B01J2229/34; B01J2229/36; B01J2229/40; B01J2229/42
Claims Analysis
Total Claims: 22
Claim 1
Independent Claim
262 words
In a method for synthesizing a composition of matter comprising an inorganic, porous crystalline phase material having, after calcination, an X-ray diffraction pattern including values substantially as shown in Table 1 which comprises the steps of (1) combining a primary organic directing agent (R'), optional additional organic directing agent (R"), optional source of alkali or alkaline earth metal (M) ions, and a solvent or solvent mixture such that the mole ratio Solvent/(R'.sub.2 O+M.sub.2 O) is from about 45 to less than about 100, (2) adding one or a combination of oxides of tetravalent element Y, and optionally one or a combination of oxides of elements selected from the group consisting of divalent element W, trivalent element X and pentavalent element Z to the mixture of step (1), such that the mole ratio R.sub.2 O/(YO.sub.2 +X.sub.2 O.sub.3 +Z.sub.2 O.sub.5 +WO) is from about 0.3 to about 1, where R is the total of R'+R", (3) agitating the mixture resulting from step (2) at a temperature of from about 0° C. to about 50° C. and a pH of from about 7 to about 14, and (4) crystallizing the product from step (3) at a temperature of from about 50° C. to about 200° C., the improvement wherein Y comprises silicon and the oxide of Y is added as a colloidal dispersion of SiO 2 or a precipitated SiO 2 , ethanol is added to the mixture prior to crystallizing step (4), and wherein the Solvent/(R' 2 O+M 2 O) mole ratio of step (1) is from about 45 to less than about 110.
Claim 2
Dependent Claim
262 words
In a method for synthesizing a composition of matter comprising an inorganic, porous crystalline phase material having, after calcination, an X-ray diffraction pattern including values substantially as shown in Table 1 which comprises the steps of (1) combining a primary organic directing agent (R'), optional additional organic directing agent (R"), optional source of alkali or alkaline earth metal (M) ions, and a solvent or solvent mixture such that the mole ratio Solvent/(R'.sub.2 O+M.sub.2 O) is from about 45 to less than about 100, (2) adding one or a combination of oxides of tetravalent element Y, and optionally one or a combination of oxides of elements selected from the group consisting of divalent element W, trivalent element X and pentavalent element Z to the mixture of step (1), such that the mole ratio R.sub.2 O/(YO.sub.2 +X.sub.2 O.sub.3 +Z.sub.2 O.sub.5 +WO) is from about 0.3 to about 1, where R is the total of R'+R", (3) agitating the mixture resulting from step (2) at a temperature of from about 0° C. to about 50° C. and a pH of from about 7 to about 14, and (4) crystallizing the product from step (3) at a temperature of from about 50° C. to about 200° C., the improvement wherein Y comprises silicon and the oxide of Y is added as a colloidal dispersion of SiO 2 or a precipitated SiO 2 , ethanol is added to the mixture prior to crystallizing step (4), and wherein the Solvent/(R' 2 O+M 2 O) mole ratio of step (1) is from about 45 to less than about 110.
Claim 3
Dependent Claim
29 words
The method of claim 1 wherein the mole ratio R 2 O/(YO 2 +X 2 O 3 +Z 2 O 5 +WO) is from about 0.3 to about 0.6.
Claim 4
Dependent Claim
95 words
The method of claim 1 wherein R' comprises an ion of the formula R 1 R 2 R 3 R 4 Q + , wherein Q is nitrogen or phosphorus and wherein at least one of R 1 , R 2 , R 3 and R 4 is aryl or alkyl of from 8 to about 36 carbon atoms or combinations thereof, the remainder of R 1 , R 2 , R 3 and R 4 being selected from the group consisting of hydrogen, alkyl of from 1 to 7 carbon atoms and combinations thereof.
Claim 5
Dependent Claim
65 words
The method of claim 1 wherein R" comprises an ion of the formula R 1 R 2 R 3 R 4 Q + , wherein Q is nitrogen or phosphorus and wherein at least one of R 1 , R 2 , R 3 and R 4 are selected from the group consisting of hydrogen, alkyl of 1 to 7 carbon atoms and combinations thereof.
Claim 6
Dependent Claim
16 words
The method of claim 1 wherein R' is cetyltrimethylammonium, octadecyltrimethylammonium, cetylpyridinium, myristyltrimethylammonium, decyltrimethylammonium, dodecyltrimethylammonium or dimethyldidodecylammonium.
Claim 7
Dependent Claim
11 words
The method of claim 5 wherein R' is cetyltrimethylammonium or octadecyltrimethylammonium.
Claim 8
Dependent Claim
23 words
The method of claim 1 wherein said solvent is C 1 -C 6 alcohol, C 1 -C 6 diol, water or mixture thereof.
Claim 9
Dependent Claim
29 words
The method of claim 1 wherein said porous crystalline phase material has, after calcination, an X-ray diffraction pattern including values substantially as shown in Table 2 of the specification.
Claim 10
Dependent Claim
29 words
The method of claim 1 wherein said porous crystalline phase material has, after calcination, an X-ray diffraction pattern including values substantially as shown in Table 3 of the specification.
Claim 11
Dependent Claim
29 words
The method of claim 1 wherein said porous crystalline phase material has, after calcination, an X-ray diffraction pattern including values substantially as shown in Table 4 of the specification.
Claim 12
Dependent Claim
29 words
The method of claim 1 wherein said porous crystalline phase material has, after calcination, an X-ray diffraction pattern including values substantially as shown in Table 5 of the specification.
Claim 13
Dependent Claim
29 words
The method of claim 1 wherein said porous crystalline phase material has, after calcination, an X-ray diffraction pattern including values substantially as shown in Table 6 of the specification.
Claim 14
Dependent Claim
106 words
The method of claim 1 wherein said crystalline phase has a composition expressed as follows: M.sub.n/q (W.sub.a X.sub.b Y.sub.c Z.sub.d O.sub.h) wherein M is one or more ions; n is the charge of the composition excluding M expressed as oxides; q is the weighted molar average valence of M; n/q is the number of moles or mole fraction of M; W is one or more divalent elements; X is one or more trivalent elements; Y comprises silicon; Z is one or more pentavalent elements; a,b,c, and d are mole fractions of W,X,Y and Z, respectively; h is a number of from 1 to 2.5; and (a+b+c+d)=1.
Claim 15
Dependent Claim
15 words
The method of claim 13 wherein the sum (a+b+c) is greater than d, and h=2.
Claim 16
Dependent Claim
27 words
The method of claim 13 wherein W is a divalent first row transition metal or magnesium; X is aluminum, boron, gallium or iron; and Z is phosphorus.
Claim 17
Dependent Claim
16 words
The method of claim 13 wherein W comprises cobalt, X comprises aluminum, and Z comprises phosphorus.
Claim 18
Dependent Claim
27 words
The method of claim 14 wherein W is a divalent first row transition metal or magnesium; X is aluminum, boron, gallium or iron; and Z is phosphorus.
Claim 19
Dependent Claim
16 words
The method of claim 14 wherein W comprises cobalt, X comprises aluminum, and Z comprises phosphorus.
Claim 20
Dependent Claim
13 words
The method of claim 13 wherein a and d are 0 and h=2.
Claim 21
Dependent Claim
13 words
The method of claim 19 wherein X comprises aluminum, boron, gallium or iron.
Claim 22
Dependent Claim
29 words
The method of claim 1 wherein said crystalline phase has a regular arrangement of uniformly sized pores of at least about 13 Angstrom Units as measured by argon physisorption.
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