Application of Grose, Appeal No. 78-573.
| Citation | 592 F.2d 1161 |
| Decision Date | 01 March 1979 |
| Docket Number | Appeal No. 78-573. |
| Parties | In the Matter of the Application of Robert W. GROSE and Edith Marie Flanigen. |
| Court | United States Court of Customs and Patent Appeals |
Richard G. Miller, New York City, atty. of record, for appellants; James C. Arvantes, Arlington, Va., of counsel.
Joseph F. Nakamura, Washington, D. C., for the Commissioner of Patents; Gerald H. Bjorge, Washington, D. C., of counsel.
Before MARKEY, Chief Judge, and RICH, BALDWIN, LANE, and MILLER, Judges.
Appeal from the decision of the Patent and Trademark Office (PTO) Board of Appeals (board) sustaining the rejection under 35 U.S.C. § 103 of claims 1-2 of application serial No. 432,137, filed January 10, 1974, for "Crystalline Aluminosilicate and Process for Preparing Same." We affirm.
The invention is directed to a synthetic crystalline aluminosilicate of the molecular sieve or zeolitic type, named "zeolite Upsilon" by appellants. Claims 1 and 2 read:
Table B is disclosed in the specification:
TABLE B
d Å
obs, Relative Intensity
13.4 ± 0.2 M
9.5 ± 0.2 VS
8.5 ± 0.15 M
5.47 ± 0.1 S
4.23 ± 0.08 S
3.87 ± 0.07 S
3.53 ± 0.06 M
3.30 ± 0.05 M
3.07 ± 0.05 M
2.98 ± 0.05 S W = weak
S = strong
2.86 ± 0.05 S VS = very strong
VW = very weak
2.83 ± 0.05 M M = medium
Table B represents an abbreviated version of the X-ray powder diffraction pattern used by appellants to identify their zeolite Upsilon and distinguish it from other zeolites. A more detailed X-ray diffraction pattern is disclosed in Table A of the specification:
Measurement of the X-ray powder diffraction pattern is described as follows:
Standard techniques were employed to obtain the foregoing data. The radiation was the K-alpha doublet of copper, and a Geiger-counter spectrometer with a strip-chart pen recorder was used. The peak heights, I and the positions as a function of 2 times theta (Ø), where theta is the Bragg angle, were read from the spectrometer chart. From these the relative intensities, 100 I/Io, where Io is the intensity of the strongest line or peak, and d(obs.), the interplanar spacing in Angstrom units corresponding to the recorded lines were calculated. The particular x-ray technique and/or apparatus employed, the humidity, the temperature, the orientation of the powder crystals and other variables, all of which are well known and understood by those skilled in the art of x-ray crystallography or diffraction, can cause some variation in the intensities and positions of the x-ray lines.
Appellants disclose that zeolite Upsilon is prepared by hydrothermal crystallization from a gel with the following mole ratios of oxides:
Na2O/SiO2 0.8 - 1.4
SiO2/A12O3 3.0 - 7
H2O/Na2O 32 - 50, preferably about 43
Crystallization is conducted by heating the gel, at 100 °C and atmospheric pressure, until the crystalline product has been obtained. The presence of chromium or iron oxides, in addition to the above reactants, is disclosed as essential to obtaining zeolite Upsilon as the major zeolite product.2 After crystallization, the zeolite crystals are separated by filtration, washed with distilled water until the pH of the effluent is between 9 and 12, and dried at 110 °C.
Zeolite Upsilon is disclosed as being useful as a desiccant, particularly in drying hydrocarbon gas streams and air streams to be fractionated in the liquid state, and as an absorbent for carbon dioxide.
Claims 1 and 2 were rejected under 35 U.S.C. § 102 or at least 35 U.S.C. § 103 as unpatentable over the single reference patent to Milton, No. 3,030,181, dated April 17, 1962.
Milton discloses a synthetic crystalline aluminosilicate, called zeolite R, with the following chemical formula:
0.9 ± 0.2 Na2O : A12O3 : WSiO2 : XH2O
wherein W = 3.45 - 3.65 and X = 7 when fully hydrated
Milton's zeolite R has an X-ray powder diffraction pattern substantially like that shown in this table:
TABLE I
X-Ray Diffraction Patterns of Synthetic Zeolite R
SODIUM ZEOLITE R
d=Interplanar Spacing in A. : I/I Max. = Relative Intensity
----------------------
| d, A. | 100 |
| | (I/I max.) |
|-------|------------|
| 9.51 | 88 |
| 6.97 | 35 |
| 5.75 | 16 |
| 5.61 | 26 |
| 5.10 | 45 |
| 4.75 | 12 |
| 4.37 | 78 |
| 4.13 | 12 |
| 4.02 | 14 |
| 3.92 | 35 |
| 3.80 | 16 |
| 3.63 | 41 |
| 3.48 | 25 |
| 3.34 | 12 |
| 3.21 | 18 |
| 3.13 | 12 |
| 2.95 | 100 |
| 2.89 | 16 |
| 2.80 | 14 |
| 2.71 | 14 |
| 2.66 | 10 |
| 2.62 | 25 |
| 2.53 | 22 |
| 2.39 | 10 |
| 2.14 | 6 |
| 2.10 | 14 |
| 1.93 | 10 |
| 1.89 | 10 |
| 1.82 | 18 |
| 1.76 | 6 |
| 1.73 | 16 |
| 1.69 | 4 |
----------------------
Milton's crystallization process for preparing zeolite R may use a reactant mixture with these mole ratios of oxides:
Na2O/SiO2 0.81 - 1.0
SiO2/A12O3 3 - 4.5
H2O/Na2O 40 - 80
The process conditions are essentially the same as those described by appellants, except that Milton makes no reference to the presence of iron or chromium oxides in the reaction mixture.
The examiner viewed the chemical composition of the claimed zeolite as encompassed by that of Milton's zeolite R. The only arguable chemical difference between the two zeolites, i. e., Milton's minimum Si02/Al203 ratio of 3.45 as compared to appellants' maximum Si02/Al203 ratio of 3.4, was not found to be a significant distinguishing feature because "the claimed numerical value of `3.4' which is not limited as to the digit in the second decimal place reads on or encompasses Milton's numerical value of `3.45'."
The examiner found the differences between appellants' 12 X-ray diffraction d-spacings and those reported for Milton's zeolite R insufficient to establish that the claimed zeolite has a...
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